data_L_5a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H47 O2 P' _chemical_formula_weight 494.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.342(3) _cell_length_b 19.352(5) _cell_length_c 13.400(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.229(3) _cell_angle_gamma 90.00 _cell_volume 3159.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2664 _cell_measurement_theta_min 2.3345 _cell_measurement_theta_max 20.169 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9676 _exptl_absorpt_correction_T_max 0.9989 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scan' _diffrn_reflns_number 35920 _diffrn_reflns_av_R_equivalents 0.1293 _diffrn_reflns_av_sigmaI/netI 0.1713 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7232 _reflns_number_gt 2969 _reflns_threshold_expression >2sigma(I) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 211 67 ' ' 2 0.500 0.500 1.000 211 67 ' ' _platon_squeeze_details ; ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0072(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7232 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 0.640 _refine_ls_restrained_S_all 0.640 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.73425(5) 0.08452(4) 0.77371(5) 0.02876(19) Uani 1 1 d . . . O1 O 0.38509(14) -0.00123(10) 0.78839(14) 0.0464(5) Uani 1 1 d . . . O2 O 0.53342(15) -0.07084(10) 0.78310(15) 0.0448(5) Uani 1 1 d . . . C1 C 0.6803(2) 0.05128(15) 0.88931(19) 0.0369(7) Uani 1 1 d . . . C2 C 0.5557(2) 0.03739(16) 0.8767(2) 0.0425(7) Uani 1 1 d . . . H2A H 0.5421 0.0108 0.9348 0.051 Uiso 1 1 calc R . . H2B H 0.5193 0.0816 0.8797 0.051 Uiso 1 1 calc R . . C3 C 0.5001(2) 0.00033(15) 0.7829(2) 0.0344(7) Uani 1 1 d . . . C4 C 0.5182(2) 0.03673(14) 0.68600(19) 0.0330(6) Uani 1 1 d . . . H4A H 0.4864 0.0826 0.6861 0.040 Uiso 1 1 calc R . . H4B H 0.4772 0.0118 0.6294 0.040 Uiso 1 1 calc R . . C5 C 0.6370(2) 0.04453(13) 0.66633(19) 0.0306(6) Uani 1 1 d . . . C6 C 0.7084(3) 0.10161(17) 0.9781(2) 0.0511(9) Uani 1 1 d . . . H6A H 0.6693 0.1441 0.9626 0.077 Uiso 1 1 calc R . . H6B H 0.7859 0.1106 0.9894 0.077 Uiso 1 1 calc R . . H6C H 0.6877 0.0816 1.0378 0.077 Uiso 1 1 calc R . . C7 C 0.7450(2) -0.01611(15) 0.9193(2) 0.0513(9) Uani 1 1 d . . . H7A H 0.8223 -0.0065 0.9295 0.077 Uiso 1 1 calc R . . H7B H 0.7278 -0.0496 0.8663 0.077 Uiso 1 1 calc R . . H7C H 0.7250 -0.0340 0.9806 0.077 Uiso 1 1 calc R . . C8 C 0.3442(2) -0.06424(16) 0.7427(2) 0.0488(8) Uani 1 1 d . . . H8A H 0.3192 -0.0582 0.6709 0.059 Uiso 1 1 calc R . . H8B H 0.2839 -0.0818 0.7739 0.059 Uiso 1 1 calc R . . C9 C 0.4401(3) -0.11125(18) 0.7614(3) 0.0737(12) Uani 1 1 d . . . H9A H 0.4341 -0.1417 0.8178 0.088 Uiso 1 1 calc R . . H9B H 0.4436 -0.1394 0.7021 0.088 Uiso 1 1 calc R . . C10 C 0.6361(3) 0.09105(14) 0.57373(19) 0.0458(8) Uani 1 1 d . . . H10A H 0.5978 0.0682 0.5149 0.069 Uiso 1 1 calc R . . H10B H 0.7102 0.1004 0.5644 0.069 Uiso 1 1 calc R . . H10C H 0.5998 0.1337 0.5839 0.069 Uiso 1 1 calc R . . C11 C 0.6850(2) -0.02523(14) 0.6421(2) 0.0441(8) Uani 1 1 d . . . H11A H 0.6915 -0.0546 0.7005 0.066 Uiso 1 1 calc R . . H11B H 0.7562 -0.0183 0.6236 0.066 Uiso 1 1 calc R . . H11C H 0.6375 -0.0466 0.5870 0.066 Uiso 1 1 calc R . . C12 C 0.69976(19) 0.17763(13) 0.76409(17) 0.0260(6) Uani 1 1 d . . . C13 C 0.5980(2) 0.20466(14) 0.77957(19) 0.0316(6) Uani 1 1 d . . . H13 H 0.5441 0.1743 0.7939 0.038 Uiso 1 1 calc R . . C14 C 0.5751(2) 0.27464(14) 0.7743(2) 0.0369(7) Uani 1 1 d . . . H14 H 0.5067 0.2906 0.7845 0.044 Uiso 1 1 calc R . . C15 C 0.6539(2) 0.32054(14) 0.7537(2) 0.0355(7) Uani 1 1 d . . . H15 H 0.6394 0.3677 0.7505 0.043 Uiso 1 1 calc R . . C16 C 0.7549(2) 0.29578(13) 0.73807(19) 0.0319(6) Uani 1 1 d . . . H16 H 0.8081 0.3270 0.7247 0.038 Uiso 1 1 calc R . . C17 C 0.77959(18) 0.22498(13) 0.74176(17) 0.0245(6) Uani 1 1 d . . . C18 C 0.89168(19) 0.20486(12) 0.71941(18) 0.0261(6) Uani 1 1 d . . . C19 C 0.91590(19) 0.21135(13) 0.62032(19) 0.0286(6) Uani 1 1 d . . . C20 C 1.0219(2) 0.19746(14) 0.6031(2) 0.0352(7) Uani 1 1 d . . . H20 H 1.0371 0.2013 0.5375 0.042 Uiso 1 1 calc R . . C21 C 1.1058(2) 0.17817(15) 0.6794(2) 0.0363(7) Uani 1 1 d . . . C22 C 1.0803(2) 0.17369(14) 0.77605(19) 0.0343(7) Uani 1 1 d . . . H22 H 1.1354 0.1608 0.8285 0.041 Uiso 1 1 calc R . . C23 C 0.97662(19) 0.18751(13) 0.79843(18) 0.0269(6) Uani 1 1 d . . . C24 C 0.8326(2) 0.23597(15) 0.53143(19) 0.0366(7) Uani 1 1 d . . . H24 H 0.7605 0.2378 0.5532 0.044 Uiso 1 1 calc R . . C25 C 0.8239(2) 0.18767(17) 0.4399(2) 0.0480(8) Uani 1 1 d . . . H25A H 0.8903 0.1901 0.4115 0.072 Uiso 1 1 calc R . . H25B H 0.7630 0.2015 0.3901 0.072 Uiso 1 1 calc R . . H25C H 0.8128 0.1411 0.4609 0.072 Uiso 1 1 calc R . . C26 C 0.8616(2) 0.30903(16) 0.5006(2) 0.0488(8) Uani 1 1 d . . . H26A H 0.8617 0.3399 0.5568 0.073 Uiso 1 1 calc R . . H26B H 0.8083 0.3243 0.4449 0.073 Uiso 1 1 calc R . . H26C H 0.9331 0.3087 0.4810 0.073 Uiso 1 1 calc R . . C27 C 1.2224(2) 0.16622(19) 0.6596(2) 0.0527(9) Uani 1 1 d . . . H27 H 1.2618 0.1423 0.7191 0.063 Uiso 1 1 calc R . . C28 C 1.2288(3) 0.1208(3) 0.5704(3) 0.1089(18) Uani 1 1 d . . . H28A H 1.1903 0.0784 0.5774 0.163 Uiso 1 1 calc R . . H28B H 1.3043 0.1108 0.5668 0.163 Uiso 1 1 calc R . . H28C H 1.1959 0.1440 0.5097 0.163 Uiso 1 1 calc R . . C29 C 1.2802(3) 0.2342(2) 0.6517(3) 0.0865(14) Uani 1 1 d . . . H29A H 1.2452 0.2588 0.5930 0.130 Uiso 1 1 calc R . . H29B H 1.3556 0.2258 0.6459 0.130 Uiso 1 1 calc R . . H29C H 1.2767 0.2613 0.7111 0.130 Uiso 1 1 calc R . . C30 C 0.9588(2) 0.18792(14) 0.90816(19) 0.0342(7) Uani 1 1 d . . . H30 H 0.8798 0.1833 0.9085 0.041 Uiso 1 1 calc R . . C31 C 0.9948(2) 0.25795(16) 0.9556(2) 0.0471(8) Uani 1 1 d . . . H31A H 1.0701 0.2663 0.9494 0.071 Uiso 1 1 calc R . . H31B H 0.9872 0.2576 1.0258 0.071 Uiso 1 1 calc R . . H31C H 0.9496 0.2938 0.9213 0.071 Uiso 1 1 calc R . . C32 C 1.0161(2) 0.12879(16) 0.9712(2) 0.0492(8) Uani 1 1 d . . . H32A H 0.9971 0.0857 0.9374 0.074 Uiso 1 1 calc R . . H32B H 0.9932 0.1282 1.0364 0.074 Uiso 1 1 calc R . . H32C H 1.0942 0.1353 0.9795 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0271(4) 0.0306(4) 0.0293(4) 0.0036(3) 0.0066(3) 0.0001(3) O1 0.0281(11) 0.0571(13) 0.0547(13) -0.0051(11) 0.0090(9) -0.0099(10) O2 0.0373(11) 0.0364(12) 0.0581(13) 0.0121(10) -0.0001(9) -0.0119(9) C1 0.0354(16) 0.0483(18) 0.0258(14) 0.0064(13) 0.0014(12) -0.0137(14) C2 0.0413(17) 0.055(2) 0.0315(16) 0.0016(14) 0.0083(13) -0.0168(15) C3 0.0264(15) 0.0399(17) 0.0371(16) 0.0010(13) 0.0055(12) -0.0074(12) C4 0.0355(16) 0.0312(15) 0.0303(15) -0.0008(12) -0.0014(12) -0.0011(12) C5 0.0377(16) 0.0279(15) 0.0268(14) -0.0009(11) 0.0073(12) -0.0049(12) C6 0.053(2) 0.075(2) 0.0242(15) 0.0017(15) 0.0050(13) -0.0276(17) C7 0.0470(19) 0.051(2) 0.0501(19) 0.0217(16) -0.0100(15) -0.0158(15) C8 0.0416(18) 0.069(2) 0.0356(17) -0.0092(16) 0.0051(14) -0.0229(17) C9 0.044(2) 0.059(2) 0.118(3) -0.032(2) 0.014(2) -0.0159(18) C10 0.071(2) 0.0411(18) 0.0247(15) -0.0013(13) 0.0063(14) -0.0140(16) C11 0.0537(19) 0.0305(16) 0.0525(19) -0.0089(14) 0.0217(15) -0.0033(14) C12 0.0232(13) 0.0334(15) 0.0217(13) -0.0041(11) 0.0048(10) -0.0014(11) C13 0.0254(14) 0.0380(17) 0.0333(15) -0.0083(12) 0.0106(11) -0.0052(12) C14 0.0283(15) 0.0407(18) 0.0436(17) -0.0132(14) 0.0115(13) 0.0028(13) C15 0.0311(16) 0.0300(15) 0.0464(17) -0.0088(13) 0.0093(13) 0.0014(12) C16 0.0297(15) 0.0313(16) 0.0357(16) -0.0027(12) 0.0079(12) -0.0047(12) C17 0.0210(13) 0.0327(15) 0.0193(13) -0.0037(11) 0.0017(10) -0.0024(11) C18 0.0233(13) 0.0274(14) 0.0281(14) -0.0031(11) 0.0058(11) -0.0031(11) C19 0.0235(14) 0.0345(15) 0.0279(14) -0.0014(12) 0.0042(11) -0.0006(11) C20 0.0260(14) 0.0523(19) 0.0285(15) -0.0011(13) 0.0081(12) 0.0011(13) C21 0.0223(14) 0.0514(18) 0.0361(16) -0.0008(14) 0.0069(12) 0.0047(13) C22 0.0224(14) 0.0484(18) 0.0310(15) 0.0016(13) 0.0010(11) 0.0002(12) C23 0.0215(13) 0.0298(14) 0.0288(14) -0.0001(11) 0.0022(11) -0.0036(11) C24 0.0217(14) 0.060(2) 0.0286(15) 0.0006(14) 0.0048(11) 0.0046(13) C25 0.0301(16) 0.087(2) 0.0280(15) -0.0050(16) 0.0079(12) -0.0069(16) C26 0.0450(19) 0.060(2) 0.0406(18) 0.0135(15) 0.0038(14) 0.0099(16) C27 0.0256(16) 0.095(3) 0.0386(18) 0.0021(18) 0.0067(13) 0.0171(17) C28 0.044(2) 0.173(5) 0.111(4) -0.066(3) 0.017(2) 0.032(3) C29 0.040(2) 0.131(4) 0.096(3) -0.022(3) 0.036(2) -0.025(2) C30 0.0252(14) 0.0513(18) 0.0256(14) 0.0020(13) 0.0025(11) -0.0050(13) C31 0.0445(19) 0.066(2) 0.0329(16) -0.0118(15) 0.0123(14) -0.0108(16) C32 0.0406(18) 0.073(2) 0.0335(17) 0.0170(16) 0.0057(14) 0.0000(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C12 1.851(3) . ? P1 C5 1.886(3) . ? P1 C1 1.894(3) . ? O1 C8 1.420(3) . ? O1 C3 1.433(3) . ? O2 C9 1.383(3) . ? O2 C3 1.437(3) . ? C1 C6 1.534(4) . ? C1 C2 1.544(4) . ? C1 C7 1.548(4) . ? C2 C3 1.512(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.525(3) . ? C4 C5 1.538(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C11 1.530(4) . ? C5 C10 1.532(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.483(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.406(3) . ? C12 C17 1.412(3) . ? C13 C14 1.383(4) . ? C13 H13 0.9300 . ? C14 C15 1.378(4) . ? C14 H14 0.9300 . ? C15 C16 1.383(3) . ? C15 H15 0.9300 . ? C16 C17 1.403(3) . ? C16 H16 0.9300 . ? C17 C18 1.513(3) . ? C18 C23 1.406(3) . ? C18 C19 1.413(3) . ? C19 C20 1.391(3) . ? C19 C24 1.520(3) . ? C20 C21 1.384(3) . ? C20 H20 0.9300 . ? C21 C22 1.384(3) . ? C21 C27 1.523(4) . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 C30 1.521(3) . ? C24 C26 1.532(4) . ? C24 C25 1.532(4) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.496(5) . ? C27 C29 1.508(5) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C32 1.527(4) . ? C30 C31 1.532(4) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 P1 C5 103.60(11) . . ? C12 P1 C1 106.29(12) . . ? C5 P1 C1 102.73(12) . . ? C8 O1 C3 106.4(2) . . ? C9 O2 C3 108.2(2) . . ? C6 C1 C2 107.0(2) . . ? C6 C1 C7 106.9(2) . . ? C2 C1 C7 110.2(2) . . ? C6 C1 P1 110.69(18) . . ? C2 C1 P1 116.37(17) . . ? C7 C1 P1 105.30(19) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2A 107.6 . . ? C1 C2 H2A 107.6 . . ? C3 C2 H2B 107.6 . . ? C1 C2 H2B 107.6 . . ? H2A C2 H2B 107.0 . . ? O1 C3 O2 105.4(2) . . ? O1 C3 C2 106.8(2) . . ? O2 C3 C2 111.2(2) . . ? O1 C3 C4 109.6(2) . . ? O2 C3 C4 111.3(2) . . ? C2 C3 C4 112.3(2) . . ? C3 C4 C5 117.7(2) . . ? C3 C4 H4A 107.9 . . ? C5 C4 H4A 107.9 . . ? C3 C4 H4B 107.9 . . ? C5 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? C11 C5 C10 107.4(2) . . ? C11 C5 C4 111.2(2) . . ? C10 C5 C4 108.3(2) . . ? C11 C5 P1 107.63(19) . . ? C10 C5 P1 107.33(17) . . ? C4 C5 P1 114.66(17) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 103.6(2) . . ? O1 C8 H8A 111.0 . . ? C9 C8 H8A 111.0 . . ? O1 C8 H8B 111.0 . . ? C9 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? O2 C9 C8 107.7(3) . . ? O2 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O2 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 117.4(2) . . ? C13 C12 P1 123.55(19) . . ? C17 C12 P1 119.07(18) . . ? C14 C13 C12 122.5(2) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 121.9(2) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C12 119.1(2) . . ? C16 C17 C18 116.4(2) . . ? C12 C17 C18 124.5(2) . . ? C23 C18 C19 119.0(2) . . ? C23 C18 C17 120.5(2) . . ? C19 C18 C17 120.1(2) . . ? C20 C19 C18 119.0(2) . . ? C20 C19 C24 117.8(2) . . ? C18 C19 C24 123.1(2) . . ? C21 C20 C19 122.8(2) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C22 C21 C20 116.9(2) . . ? C22 C21 C27 121.1(2) . . ? C20 C21 C27 121.9(2) . . ? C21 C22 C23 123.1(2) . . ? C21 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C22 C23 C18 119.1(2) . . ? C22 C23 C30 119.5(2) . . ? C18 C23 C30 121.4(2) . . ? C19 C24 C26 110.0(2) . . ? C19 C24 C25 112.8(2) . . ? C26 C24 C25 109.7(2) . . ? C19 C24 H24 108.1 . . ? C26 C24 H24 108.1 . . ? C25 C24 H24 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 111.7(3) . . ? C28 C27 C21 113.6(3) . . ? C29 C27 C21 110.5(3) . . ? C28 C27 H27 106.9 . . ? C29 C27 H27 106.9 . . ? C21 C27 H27 106.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C30 C32 113.9(2) . . ? C23 C30 C31 109.2(2) . . ? C32 C30 C31 110.8(2) . . ? C23 C30 H30 107.6 . . ? C32 C30 H30 107.6 . . ? C31 C30 H30 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 P1 C1 C6 -44.3(2) . . . . ? C5 P1 C1 C6 -152.8(2) . . . . ? C12 P1 C1 C2 78.1(2) . . . . ? C5 P1 C1 C2 -30.3(2) . . . . ? C12 P1 C1 C7 -159.51(17) . . . . ? C5 P1 C1 C7 92.00(19) . . . . ? C6 C1 C2 C3 168.6(3) . . . . ? C7 C1 C2 C3 -75.5(3) . . . . ? P1 C1 C2 C3 44.2(3) . . . . ? C8 O1 C3 O2 -28.2(3) . . . . ? C8 O1 C3 C2 -146.5(2) . . . . ? C8 O1 C3 C4 91.6(3) . . . . ? C9 O2 C3 O1 15.6(3) . . . . ? C9 O2 C3 C2 131.0(3) . . . . ? C9 O2 C3 C4 -103.0(3) . . . . ? C1 C2 C3 O1 -176.3(2) . . . . ? C1 C2 C3 O2 69.3(3) . . . . ? C1 C2 C3 C4 -56.1(3) . . . . ? O1 C3 C4 C5 179.4(2) . . . . ? O2 C3 C4 C5 -64.5(3) . . . . ? C2 C3 C4 C5 60.9(3) . . . . ? C3 C4 C5 C11 70.1(3) . . . . ? C3 C4 C5 C10 -172.1(2) . . . . ? C3 C4 C5 P1 -52.3(3) . . . . ? C12 P1 C5 C11 159.10(17) . . . . ? C1 P1 C5 C11 -90.39(19) . . . . ? C12 P1 C5 C10 43.8(2) . . . . ? C1 P1 C5 C10 154.28(19) . . . . ? C12 P1 C5 C4 -76.54(19) . . . . ? C1 P1 C5 C4 34.0(2) . . . . ? C3 O1 C8 C9 29.0(3) . . . . ? C3 O2 C9 C8 2.3(4) . . . . ? O1 C8 C9 O2 -19.4(4) . . . . ? C5 P1 C12 C13 65.3(2) . . . . ? C1 P1 C12 C13 -42.6(2) . . . . ? C5 P1 C12 C17 -115.88(19) . . . . ? C1 P1 C12 C17 136.25(19) . . . . ? C17 C12 C13 C14 -0.4(4) . . . . ? P1 C12 C13 C14 178.5(2) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? C15 C16 C17 C12 -1.3(4) . . . . ? C15 C16 C17 C18 177.8(2) . . . . ? C13 C12 C17 C16 1.2(3) . . . . ? P1 C12 C17 C16 -177.71(18) . . . . ? C13 C12 C17 C18 -177.8(2) . . . . ? P1 C12 C17 C18 3.3(3) . . . . ? C16 C17 C18 C23 102.4(3) . . . . ? C12 C17 C18 C23 -78.6(3) . . . . ? C16 C17 C18 C19 -70.0(3) . . . . ? C12 C17 C18 C19 109.1(3) . . . . ? C23 C18 C19 C20 2.8(4) . . . . ? C17 C18 C19 C20 175.2(2) . . . . ? C23 C18 C19 C24 -174.5(2) . . . . ? C17 C18 C19 C24 -2.0(4) . . . . ? C18 C19 C20 C21 -0.8(4) . . . . ? C24 C19 C20 C21 176.6(3) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C19 C20 C21 C27 -177.3(3) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C27 C21 C22 C23 176.7(3) . . . . ? C21 C22 C23 C18 2.1(4) . . . . ? C21 C22 C23 C30 -174.2(2) . . . . ? C19 C18 C23 C22 -3.4(4) . . . . ? C17 C18 C23 C22 -175.8(2) . . . . ? C19 C18 C23 C30 172.8(2) . . . . ? C17 C18 C23 C30 0.4(4) . . . . ? C20 C19 C24 C26 -69.3(3) . . . . ? C18 C19 C24 C26 108.0(3) . . . . ? C20 C19 C24 C25 53.5(3) . . . . ? C18 C19 C24 C25 -129.2(3) . . . . ? C22 C21 C27 C28 134.8(4) . . . . ? C20 C21 C27 C28 -48.6(5) . . . . ? C22 C21 C27 C29 -98.6(3) . . . . ? C20 C21 C27 C29 77.9(4) . . . . ? C22 C23 C30 C32 -42.6(3) . . . . ? C18 C23 C30 C32 141.2(2) . . . . ? C22 C23 C30 C31 81.8(3) . . . . ? C18 C23 C30 C31 -94.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.401 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.062 #===END data_L_5a_prime _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H45 P' _chemical_formula_weight 436.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 30.671(4) _cell_length_b 10.2786(15) _cell_length_c 33.812(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10659(3) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6527 _cell_measurement_theta_min 2.175 _cell_measurement_theta_max 21.2115 _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.088 _exptl_crystal_F_000 3840 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6235 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scan' _diffrn_reflns_number 122642 _diffrn_reflns_av_unetI/netI 0.0742 _diffrn_reflns_av_R_equivalents 0.1435 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.204 _diffrn_reflns_theta_max 27.511 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 12238 _reflns_number_gt 7303 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+9.9426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12238 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.39601(2) 0.72110(6) 0.04510(2) 0.01812(13) Uani 1 1 d . . . . . C1 C 0.38240(7) 0.7903(2) 0.09531(7) 0.0234(5) Uani 1 1 d . . . . . C2 C 0.42192(8) 0.8358(2) 0.11929(7) 0.0270(5) Uani 1 1 d . . . . . H2A H 0.4114 0.8758 0.1442 0.032 Uiso 1 1 calc R U . . . H2B H 0.4396 0.7588 0.1265 0.032 Uiso 1 1 calc R U . . . C3 C 0.45106(8) 0.9330(2) 0.09805(8) 0.0307(6) Uani 1 1 d . . . . . H3A H 0.4730 0.9670 0.1169 0.037 Uiso 1 1 calc R U . . . H3B H 0.4331 1.0073 0.0889 0.037 Uiso 1 1 calc R U . . . C4 C 0.47438(8) 0.8732(3) 0.06272(8) 0.0322(6) Uani 1 1 d . . . . . H4A H 0.4927 0.8005 0.0723 0.039 Uiso 1 1 calc R U . . . H4B H 0.4942 0.9395 0.0514 0.039 Uiso 1 1 calc R U . . . C5 C 0.44481(8) 0.8218(2) 0.02945(7) 0.0271(5) Uani 1 1 d . . . . . C6 C 0.35773(10) 0.6869(3) 0.11859(8) 0.0410(7) Uani 1 1 d . . . . . H6A H 0.3777 0.6161 0.1256 0.062 Uiso 1 1 calc R U . . . H6B H 0.3339 0.6525 0.1024 0.062 Uiso 1 1 calc R U . . . H6C H 0.3458 0.7256 0.1428 0.062 Uiso 1 1 calc R U . . . C7 C 0.35092(8) 0.9039(2) 0.08850(8) 0.0342(6) Uani 1 1 d . . . . . H7A H 0.3410 0.9378 0.1141 0.051 Uiso 1 1 calc R U . . . H7B H 0.3257 0.8735 0.0733 0.051 Uiso 1 1 calc R U . . . H7C H 0.3659 0.9730 0.0738 0.051 Uiso 1 1 calc R U . . . C8 C 0.47270(9) 0.7448(3) 0.00002(8) 0.0402(7) Uani 1 1 d . . . . . H8A H 0.4962 0.8003 -0.0099 0.060 Uiso 1 1 calc R U . . . H8B H 0.4545 0.7161 -0.0221 0.060 Uiso 1 1 calc R U . . . H8C H 0.4852 0.6687 0.0133 0.060 Uiso 1 1 calc R U . . . C9 C 0.42527(10) 0.9385(3) 0.00678(8) 0.0401(7) Uani 1 1 d . . . . . H9A H 0.4077 0.9912 0.0249 0.060 Uiso 1 1 calc R U . . . H9B H 0.4069 0.9066 -0.0148 0.060 Uiso 1 1 calc R U . . . H9C H 0.4489 0.9918 -0.0041 0.060 Uiso 1 1 calc R U . . . C10 C 0.41735(7) 0.5582(2) 0.05753(6) 0.0176(5) Uani 1 1 d . . . . . C11 C 0.45699(7) 0.5375(2) 0.07715(7) 0.0210(5) Uani 1 1 d . . . . . H11 H 0.4738 0.6108 0.0849 0.025 Uiso 1 1 calc R U . . . C12 C 0.47259(8) 0.4142(2) 0.08570(7) 0.0262(5) Uani 1 1 d . . . . . H12 H 0.4994 0.4036 0.0993 0.031 Uiso 1 1 calc R U . . . C13 C 0.44864(7) 0.3067(2) 0.07418(7) 0.0257(5) Uani 1 1 d . . . . . H13 H 0.4589 0.2215 0.0798 0.031 Uiso 1 1 calc R U . . . C14 C 0.40957(7) 0.3242(2) 0.05435(7) 0.0223(5) Uani 1 1 d . . . . . H14 H 0.3936 0.2498 0.0462 0.027 Uiso 1 1 calc R U . . . C15 C 0.39291(7) 0.4478(2) 0.04600(6) 0.0167(4) Uani 1 1 d . . . . . C16 C 0.34980(7) 0.4573(2) 0.02502(6) 0.0158(4) Uani 1 1 d . . . . . C17 C 0.34874(7) 0.4845(2) -0.01578(6) 0.0160(4) Uani 1 1 d . . . . . C18 C 0.30845(7) 0.4959(2) -0.03460(6) 0.0180(5) Uani 1 1 d . . . . . H18 H 0.3079 0.5157 -0.0620 0.022 Uiso 1 1 calc R U . . . C19 C 0.26919(7) 0.4797(2) -0.01489(6) 0.0174(5) Uani 1 1 d . . . . . C20 C 0.27100(7) 0.4476(2) 0.02507(6) 0.0176(5) Uani 1 1 d . . . . . H20 H 0.2445 0.4343 0.0390 0.021 Uiso 1 1 calc R U . . . C21 C 0.31023(7) 0.4341(2) 0.04550(6) 0.0170(4) Uani 1 1 d . . . . . C22 C 0.39040(7) 0.4936(2) -0.03998(6) 0.0198(5) Uani 1 1 d . . . . . H22 H 0.4146 0.5166 -0.0215 0.024 Uiso 1 1 calc R U . . . C23 C 0.38882(8) 0.5978(3) -0.07213(7) 0.0312(6) Uani 1 1 d . . . . . H23A H 0.3680 0.5718 -0.0926 0.047 Uiso 1 1 calc R U . . . H23B H 0.4178 0.6079 -0.0839 0.047 Uiso 1 1 calc R U . . . H23C H 0.3796 0.6807 -0.0605 0.047 Uiso 1 1 calc R U . . . C24 C 0.40109(8) 0.3613(3) -0.05818(8) 0.0348(6) Uani 1 1 d . . . . . H24A H 0.4043 0.2965 -0.0371 0.052 Uiso 1 1 calc R U . . . H24B H 0.4284 0.3674 -0.0731 0.052 Uiso 1 1 calc R U . . . H24C H 0.3775 0.3350 -0.0760 0.052 Uiso 1 1 calc R U . . . C25 C 0.22582(7) 0.4926(2) -0.03624(6) 0.0191(5) Uani 1 1 d . . . . . H25 H 0.2321 0.5206 -0.0640 0.023 Uiso 1 1 calc R U . . . C26 C 0.19667(7) 0.5963(2) -0.01750(7) 0.0259(5) Uani 1 1 d . . . . . H26A H 0.1891 0.5701 0.0095 0.039 Uiso 1 1 calc R U . . . H26B H 0.1700 0.6058 -0.0332 0.039 Uiso 1 1 calc R U . . . H26C H 0.2122 0.6795 -0.0168 0.039 Uiso 1 1 calc R U . . . C27 C 0.20212(7) 0.3622(2) -0.03830(7) 0.0235(5) Uani 1 1 d . . . . . H27A H 0.2206 0.2983 -0.0518 0.035 Uiso 1 1 calc R U . . . H27B H 0.1748 0.3727 -0.0530 0.035 Uiso 1 1 calc R U . . . H27C H 0.1957 0.3318 -0.0114 0.035 Uiso 1 1 calc R U . . . C28 C 0.30942(7) 0.3883(2) 0.08822(6) 0.0186(5) Uani 1 1 d . . . . . H28 H 0.3382 0.4099 0.1005 0.022 Uiso 1 1 calc R U . . . C29 C 0.27341(7) 0.4514(2) 0.11333(6) 0.0251(5) Uani 1 1 d . . . . . H29A H 0.2740 0.5459 0.1095 0.038 Uiso 1 1 calc R U . . . H29B H 0.2783 0.4314 0.1413 0.038 Uiso 1 1 calc R U . . . H29C H 0.2450 0.4173 0.1052 0.038 Uiso 1 1 calc R U . . . C30 C 0.30363(8) 0.2397(2) 0.08955(7) 0.0290(6) Uani 1 1 d . . . . . H30A H 0.2765 0.2158 0.0761 0.043 Uiso 1 1 calc R U . . . H30B H 0.3024 0.2108 0.1171 0.043 Uiso 1 1 calc R U . . . H30C H 0.3283 0.1978 0.0763 0.043 Uiso 1 1 calc R U . . . P2 P 0.60208(2) 0.96252(6) 0.20195(2) 0.01775(13) Uani 1 1 d . . . . . C31 C 0.55191(7) 1.0555(2) 0.21812(7) 0.0266(5) Uani 1 1 d . . . . . C32 C 0.52068(8) 1.1001(3) 0.18512(8) 0.0346(7) Uani 1 1 d . . . . . H32A H 0.5031 1.0242 0.1767 0.042 Uiso 1 1 calc R U . . . H32B H 0.5004 1.1650 0.1964 0.042 Uiso 1 1 calc R U . . . C33 C 0.54183(9) 1.1593(2) 0.14848(8) 0.0384(7) Uani 1 1 d . . . . . H33A H 0.5186 1.1851 0.1297 0.046 Uiso 1 1 calc R U . . . H33B H 0.5578 1.2390 0.1563 0.046 Uiso 1 1 calc R U . . . C34 C 0.57319(9) 1.0683(2) 0.12758(7) 0.0323(6) Uani 1 1 d . . . . . H34A H 0.5826 1.1094 0.1025 0.039 Uiso 1 1 calc R U . . . H34B H 0.5575 0.9871 0.1208 0.039 Uiso 1 1 calc R U . . . C35 C 0.61372(8) 1.0333(2) 0.15162(7) 0.0236(5) Uani 1 1 d . . . . . C36 C 0.56907(9) 1.1754(3) 0.24040(8) 0.0368(7) Uani 1 1 d . . . . . H36A H 0.5839 1.2335 0.2218 0.055 Uiso 1 1 calc R U . . . H36B H 0.5896 1.1476 0.2609 0.055 Uiso 1 1 calc R U . . . H36C H 0.5446 1.2216 0.2527 0.055 Uiso 1 1 calc R U . . . C37 C 0.52604(8) 0.9736(3) 0.24779(8) 0.0375(7) Uani 1 1 d . . . . . H37A H 0.5014 1.0246 0.2579 0.056 Uiso 1 1 calc R U . . . H37B H 0.5451 0.9487 0.2698 0.056 Uiso 1 1 calc R U . . . H37C H 0.5151 0.8952 0.2347 0.056 Uiso 1 1 calc R U . . . C38 C 0.64259(8) 1.1540(2) 0.15777(8) 0.0325(6) Uani 1 1 d . . . . . H38A H 0.6505 1.1909 0.1320 0.049 Uiso 1 1 calc R U . . . H38B H 0.6691 1.1290 0.1720 0.049 Uiso 1 1 calc R U . . . H38C H 0.6266 1.2190 0.1732 0.049 Uiso 1 1 calc R U . . . C39 C 0.64101(9) 0.9341(3) 0.12891(8) 0.0375(7) Uani 1 1 d . . . . . H39A H 0.6517 0.9735 0.1044 0.056 Uiso 1 1 calc R U . . . H39B H 0.6230 0.8581 0.1226 0.056 Uiso 1 1 calc R U . . . H39C H 0.6658 0.9069 0.1452 0.056 Uiso 1 1 calc R U . . . C40 C 0.58313(7) 0.7960(2) 0.19014(6) 0.0160(4) Uani 1 1 d . . . . . C41 C 0.54362(7) 0.7676(2) 0.17106(6) 0.0206(5) Uani 1 1 d . . . . . H41 H 0.5259 0.8376 0.1622 0.025 Uiso 1 1 calc R U . . . C42 C 0.52946(7) 0.6416(2) 0.16463(7) 0.0226(5) Uani 1 1 d . . . . . H42 H 0.5024 0.6258 0.1518 0.027 Uiso 1 1 calc R U . . . C43 C 0.55515(7) 0.5391(2) 0.17704(7) 0.0222(5) Uani 1 1 d . . . . . H43 H 0.5458 0.4520 0.1729 0.027 Uiso 1 1 calc R U . . . C44 C 0.59444(7) 0.5640(2) 0.19546(7) 0.0223(5) Uani 1 1 d . . . . . H44 H 0.6119 0.4928 0.2038 0.027 Uiso 1 1 calc R U . . . C45 C 0.60928(7) 0.6901(2) 0.20218(6) 0.0155(4) Uani 1 1 d . . . . . C46 C 0.65268(7) 0.7054(2) 0.22227(6) 0.0163(4) Uani 1 1 d . . . . . C47 C 0.69181(7) 0.6850(2) 0.20126(6) 0.0169(4) Uani 1 1 d . . . . . C48 C 0.73140(7) 0.6998(2) 0.22086(6) 0.0192(5) Uani 1 1 d . . . . . H48 H 0.7577 0.6892 0.2063 0.023 Uiso 1 1 calc R U . . . C49 C 0.73390(7) 0.7294(2) 0.26085(6) 0.0177(5) Uani 1 1 d . . . . . C50 C 0.69515(7) 0.7439(2) 0.28135(6) 0.0179(5) Uani 1 1 d . . . . . H50 H 0.6962 0.7623 0.3089 0.021 Uiso 1 1 calc R U . . . C51 C 0.65458(7) 0.7324(2) 0.26299(6) 0.0169(5) Uani 1 1 d . . . . . C52 C 0.69244(7) 0.6363(2) 0.15858(6) 0.0188(5) Uani 1 1 d . . . . . H52 H 0.6630 0.6524 0.1468 0.023 Uiso 1 1 calc R U . . . C53 C 0.70079(8) 0.4891(2) 0.15836(7) 0.0271(6) Uani 1 1 d . . . . . H53A H 0.7287 0.4708 0.1713 0.041 Uiso 1 1 calc R U . . . H53B H 0.7016 0.4578 0.1310 0.041 Uiso 1 1 calc R U . . . H53C H 0.6773 0.4448 0.1727 0.041 Uiso 1 1 calc R U . . . C54 C 0.72664(7) 0.7024(2) 0.13227(6) 0.0262(5) Uani 1 1 d . . . . . H54A H 0.7244 0.7970 0.1352 0.039 Uiso 1 1 calc R U . . . H54B H 0.7215 0.6787 0.1046 0.039 Uiso 1 1 calc R U . . . H54C H 0.7558 0.6737 0.1402 0.039 Uiso 1 1 calc R U . . . C55 C 0.77763(7) 0.7388(2) 0.28206(7) 0.0205(5) Uani 1 1 d . . . . . H55 H 0.7717 0.7613 0.3103 0.025 Uiso 1 1 calc R U . . . C56 C 0.80684(8) 0.8447(3) 0.26491(8) 0.0355(6) Uani 1 1 d . . . . . H56A H 0.8143 0.8228 0.2375 0.053 Uiso 1 1 calc R U . . . H56B H 0.8336 0.8513 0.2807 0.053 Uiso 1 1 calc R U . . . H56C H 0.7914 0.9282 0.2655 0.053 Uiso 1 1 calc R U . . . C57 C 0.80097(8) 0.6083(2) 0.28133(7) 0.0296(6) Uani 1 1 d . . . . . H57A H 0.7819 0.5413 0.2925 0.044 Uiso 1 1 calc R U . . . H57B H 0.8278 0.6140 0.2970 0.044 Uiso 1 1 calc R U . . . H57C H 0.8083 0.5856 0.2540 0.044 Uiso 1 1 calc R U . . . C58 C 0.61346(7) 0.7406(2) 0.28831(6) 0.0203(5) Uani 1 1 d . . . . . H58 H 0.5882 0.7531 0.2700 0.024 Uiso 1 1 calc R U . . . C59 C 0.61366(8) 0.8543(3) 0.31714(7) 0.0326(6) Uani 1 1 d . . . . . H59A H 0.6369 0.8418 0.3366 0.049 Uiso 1 1 calc R U . . . H59B H 0.5855 0.8589 0.3307 0.049 Uiso 1 1 calc R U . . . H59C H 0.6187 0.9354 0.3026 0.049 Uiso 1 1 calc R U . . . C60 C 0.60651(8) 0.6119(3) 0.31012(8) 0.0336(6) Uani 1 1 d . . . . . H60A H 0.6029 0.5415 0.2908 0.050 Uiso 1 1 calc R U . . . H60B H 0.5803 0.6180 0.3266 0.050 Uiso 1 1 calc R U . . . H60C H 0.6319 0.5937 0.3269 0.050 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0171(3) 0.0178(3) 0.0195(3) 0.0012(2) -0.0027(2) -0.0013(2) C1 0.0236(12) 0.0180(12) 0.0286(13) -0.0018(10) 0.0034(10) -0.0010(10) C2 0.0340(14) 0.0255(13) 0.0216(12) -0.0059(10) -0.0054(10) 0.0047(11) C3 0.0278(13) 0.0277(14) 0.0365(15) -0.0102(12) -0.0086(11) -0.0047(11) C4 0.0230(13) 0.0319(14) 0.0418(16) -0.0039(12) 0.0026(11) -0.0128(11) C5 0.0304(13) 0.0252(13) 0.0255(13) 0.0001(10) 0.0052(11) -0.0082(11) C6 0.0553(18) 0.0302(15) 0.0375(16) -0.0068(12) 0.0275(14) -0.0085(13) C7 0.0249(13) 0.0295(15) 0.0483(17) -0.0134(13) -0.0011(12) 0.0056(11) C8 0.0396(16) 0.0421(17) 0.0388(16) -0.0067(13) 0.0177(13) -0.0165(13) C9 0.0555(19) 0.0299(15) 0.0350(15) 0.0082(12) -0.0013(13) -0.0142(14) C10 0.0155(11) 0.0208(12) 0.0163(11) -0.0004(9) 0.0005(9) -0.0001(9) C11 0.0161(11) 0.0214(12) 0.0256(12) -0.0040(10) -0.0016(9) 0.0008(9) C12 0.0228(12) 0.0277(13) 0.0280(13) -0.0010(11) -0.0081(10) 0.0048(10) C13 0.0249(13) 0.0234(13) 0.0287(13) 0.0015(10) -0.0028(10) 0.0063(10) C14 0.0243(12) 0.0196(12) 0.0231(12) -0.0014(10) -0.0022(10) 0.0013(9) C15 0.0159(11) 0.0209(11) 0.0134(10) 0.0000(9) -0.0003(8) -0.0002(9) C16 0.0180(11) 0.0150(11) 0.0143(10) -0.0010(9) -0.0010(8) -0.0006(9) C17 0.0183(11) 0.0150(11) 0.0146(11) -0.0017(9) 0.0018(9) -0.0001(9) C18 0.0204(12) 0.0190(12) 0.0147(11) 0.0006(9) -0.0014(9) -0.0027(9) C19 0.0167(11) 0.0185(11) 0.0169(11) 0.0011(9) -0.0022(9) -0.0014(9) C20 0.0165(11) 0.0196(12) 0.0165(11) 0.0016(9) 0.0014(9) -0.0036(9) C21 0.0192(11) 0.0167(11) 0.0152(10) -0.0013(9) -0.0014(9) -0.0017(9) C22 0.0165(11) 0.0255(12) 0.0174(11) 0.0010(9) 0.0007(9) -0.0005(9) C23 0.0223(13) 0.0434(16) 0.0280(13) 0.0120(12) 0.0039(10) -0.0028(11) C24 0.0327(15) 0.0367(15) 0.0348(15) -0.0081(12) 0.0094(12) 0.0017(12) C25 0.0167(11) 0.0253(13) 0.0153(11) 0.0023(9) -0.0030(9) -0.0016(9) C26 0.0222(12) 0.0300(14) 0.0255(13) -0.0020(11) -0.0040(10) 0.0037(10) C27 0.0225(12) 0.0273(13) 0.0206(12) 0.0010(10) -0.0028(10) -0.0043(10) C28 0.0179(11) 0.0245(12) 0.0134(11) 0.0017(9) -0.0009(9) -0.0021(9) C29 0.0220(12) 0.0367(14) 0.0167(11) 0.0021(10) -0.0008(10) 0.0001(11) C30 0.0416(15) 0.0248(13) 0.0206(12) 0.0057(10) -0.0004(11) -0.0056(11) P2 0.0165(3) 0.0171(3) 0.0196(3) -0.0005(2) -0.0027(2) 0.0005(2) C31 0.0214(12) 0.0237(13) 0.0346(14) -0.0087(11) -0.0026(10) 0.0042(10) C32 0.0232(13) 0.0285(14) 0.0522(17) -0.0130(13) -0.0119(12) 0.0100(11) C33 0.0402(16) 0.0235(14) 0.0513(18) 0.0044(13) -0.0247(14) 0.0023(12) C34 0.0446(16) 0.0219(13) 0.0305(14) 0.0066(11) -0.0120(12) -0.0054(12) C35 0.0273(13) 0.0201(12) 0.0234(12) 0.0030(10) 0.0000(10) -0.0038(10) C36 0.0367(15) 0.0336(15) 0.0401(16) -0.0168(13) -0.0072(12) 0.0078(12) C37 0.0283(14) 0.0455(17) 0.0388(16) -0.0093(13) 0.0129(12) 0.0025(13) C38 0.0326(14) 0.0274(14) 0.0375(15) 0.0080(12) -0.0023(12) -0.0078(11) C39 0.0520(18) 0.0314(15) 0.0291(14) 0.0048(12) 0.0179(13) 0.0027(13) C40 0.0146(10) 0.0190(11) 0.0143(10) 0.0008(9) 0.0016(8) 0.0007(9) C41 0.0208(12) 0.0205(12) 0.0204(12) 0.0012(9) -0.0039(9) 0.0019(9) C42 0.0190(12) 0.0261(13) 0.0227(12) -0.0002(10) -0.0051(10) -0.0032(10) C43 0.0247(12) 0.0188(12) 0.0231(12) -0.0036(10) -0.0002(10) -0.0052(10) C44 0.0223(12) 0.0193(12) 0.0255(12) 0.0011(10) -0.0004(10) 0.0018(9) C45 0.0155(11) 0.0183(11) 0.0128(10) -0.0003(8) 0.0018(8) -0.0004(8) C46 0.0166(11) 0.0152(11) 0.0171(11) 0.0012(9) -0.0011(9) 0.0023(9) C47 0.0191(11) 0.0151(11) 0.0166(11) -0.0007(9) -0.0005(9) 0.0007(9) C48 0.0169(11) 0.0225(12) 0.0180(11) -0.0007(9) 0.0005(9) 0.0027(9) C49 0.0170(11) 0.0186(11) 0.0176(11) -0.0003(9) -0.0019(9) 0.0004(9) C50 0.0201(11) 0.0206(12) 0.0129(10) 0.0000(9) 0.0001(9) -0.0012(9) C51 0.0181(11) 0.0157(11) 0.0167(11) 0.0005(9) 0.0018(9) 0.0014(9) C52 0.0183(11) 0.0230(12) 0.0152(11) -0.0006(9) -0.0019(9) 0.0017(9) C53 0.0334(14) 0.0271(13) 0.0207(12) -0.0048(10) -0.0027(11) 0.0065(11) C54 0.0225(12) 0.0380(15) 0.0180(12) -0.0042(11) 0.0037(10) -0.0019(11) C55 0.0169(11) 0.0258(13) 0.0186(11) -0.0031(9) -0.0032(9) 0.0012(9) C56 0.0283(14) 0.0339(15) 0.0444(16) 0.0038(13) -0.0102(12) -0.0050(12) C57 0.0270(13) 0.0350(15) 0.0268(13) 0.0002(11) -0.0075(11) 0.0062(11) C58 0.0188(11) 0.0259(13) 0.0160(11) 0.0015(9) -0.0002(9) -0.0010(9) C59 0.0232(13) 0.0494(17) 0.0251(13) -0.0123(12) 0.0023(10) 0.0008(12) C60 0.0264(14) 0.0390(15) 0.0354(15) 0.0157(12) 0.0076(12) 0.0002(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C10 1.846(2) . ? P1 C1 1.888(2) . ? P1 C5 1.895(2) . ? P1 P2 8.6159(11) . ? C1 C6 1.524(3) . ? C1 C2 1.531(3) . ? C1 C7 1.532(3) . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.539(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.532(3) . ? C5 C9 1.545(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.401(3) . ? C10 C15 1.415(3) . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.398(3) . ? C14 H14 0.9500 . ? C15 C16 1.504(3) . ? C16 C17 1.408(3) . ? C16 C21 1.417(3) . ? C17 C18 1.395(3) . ? C17 C22 1.520(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.392(3) . ? C19 C25 1.519(3) . ? C20 C21 1.394(3) . ? C20 H20 0.9500 . ? C21 C28 1.520(3) . ? C22 C23 1.527(3) . ? C22 C24 1.528(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.527(3) . ? C25 C26 1.529(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.537(3) . ? C28 C30 1.538(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? P2 C40 1.851(2) . ? P2 C35 1.885(2) . ? P2 C31 1.892(2) . ? C31 C37 1.531(4) . ? C31 C36 1.537(3) . ? C31 C32 1.540(3) . ? C32 C33 1.525(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.528(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C39 1.527(3) . ? C35 C38 1.538(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.404(3) . ? C40 C45 1.412(3) . ? C41 C42 1.383(3) . ? C41 H41 0.9500 . ? C42 C43 1.381(3) . ? C42 H42 0.9500 . ? C43 C44 1.381(3) . ? C43 H43 0.9500 . ? C44 C45 1.392(3) . ? C44 H44 0.9500 . ? C45 C46 1.503(3) . ? C46 C51 1.406(3) . ? C46 C47 1.410(3) . ? C47 C48 1.392(3) . ? C47 C52 1.527(3) . ? C48 C49 1.388(3) . ? C48 H48 0.9500 . ? C49 C50 1.384(3) . ? C49 C55 1.524(3) . ? C50 C51 1.396(3) . ? C50 H50 0.9500 . ? C51 C58 1.527(3) . ? C52 C54 1.534(3) . ? C52 C53 1.534(3) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C57 1.520(3) . ? C55 C56 1.525(3) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.522(3) . ? C58 C60 1.530(3) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 P1 C1 102.44(10) . . ? C10 P1 C5 106.17(11) . . ? C1 P1 C5 102.71(10) . . ? C10 P1 P2 82.00(7) . . ? C1 P1 P2 59.99(7) . . ? C5 P1 P2 55.61(8) . . ? C6 C1 C2 109.4(2) . . ? C6 C1 C7 107.2(2) . . ? C2 C1 C7 110.23(19) . . ? C6 C1 P1 108.15(16) . . ? C2 C1 P1 114.61(16) . . ? C7 C1 P1 106.94(17) . . ? C3 C2 C1 114.6(2) . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C2 C3 C4 112.4(2) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 115.8(2) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? C5 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C8 C5 C4 108.9(2) . . ? C8 C5 C9 107.2(2) . . ? C4 C5 C9 108.9(2) . . ? C8 C5 P1 109.90(17) . . ? C4 C5 P1 116.69(17) . . ? C9 C5 P1 104.85(17) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.9(2) . . ? C11 C10 P1 123.61(17) . . ? C15 C10 P1 118.47(16) . . ? C12 C11 C10 122.5(2) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 119.5(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 122.1(2) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C10 118.67(19) . . ? C14 C15 C16 118.38(19) . . ? C10 C15 C16 122.95(19) . . ? C17 C16 C21 119.50(19) . . ? C17 C16 C15 119.68(19) . . ? C21 C16 C15 120.78(18) . . ? C18 C17 C16 118.9(2) . . ? C18 C17 C22 119.60(19) . . ? C16 C17 C22 121.35(19) . . ? C19 C18 C17 122.7(2) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C20 117.4(2) . . ? C18 C19 C25 121.42(19) . . ? C20 C19 C25 121.14(19) . . ? C19 C20 C21 122.6(2) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C20 C21 C16 118.70(19) . . ? C20 C21 C28 119.18(19) . . ? C16 C21 C28 122.04(19) . . ? C17 C22 C23 113.54(19) . . ? C17 C22 C24 110.02(19) . . ? C23 C22 C24 110.2(2) . . ? C17 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 C27 111.22(18) . . ? C19 C25 C26 112.08(18) . . ? C27 C25 C26 110.65(18) . . ? C19 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C29 113.94(18) . . ? C21 C28 C30 109.73(18) . . ? C29 C28 C30 108.69(19) . . ? C21 C28 H28 108.1 . . ? C29 C28 H28 108.1 . . ? C30 C28 H28 108.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C40 P2 C35 102.81(10) . . ? C40 P2 C31 105.91(10) . . ? C35 P2 C31 102.70(11) . . ? C40 P2 P1 51.00(7) . . ? C35 P2 P1 72.21(7) . . ? C31 P2 P1 74.14(7) . . ? C37 C31 C36 107.3(2) . . ? C37 C31 C32 108.4(2) . . ? C36 C31 C32 109.2(2) . . ? C37 C31 P2 109.47(17) . . ? C36 C31 P2 105.55(16) . . ? C32 C31 P2 116.54(17) . . ? C33 C32 C31 116.3(2) . . ? C33 C32 H32A 108.2 . . ? C31 C32 H32A 108.2 . . ? C33 C32 H32B 108.2 . . ? C31 C32 H32B 108.2 . . ? H32A C32 H32B 107.4 . . ? C34 C33 C32 113.7(2) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 114.4(2) . . ? C33 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C39 C35 C34 109.6(2) . . ? C39 C35 C38 106.9(2) . . ? C34 C35 C38 110.5(2) . . ? C39 C35 P2 107.44(16) . . ? C34 C35 P2 114.64(17) . . ? C38 C35 P2 107.36(16) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 117.6(2) . . ? C41 C40 P2 124.21(17) . . ? C45 C40 P2 118.19(15) . . ? C42 C41 C40 122.5(2) . . ? C42 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C43 C42 C41 119.2(2) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C42 119.6(2) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 122.1(2) . . ? C43 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C44 C45 C40 119.01(19) . . ? C44 C45 C46 117.44(19) . . ? C40 C45 C46 123.55(19) . . ? C51 C46 C47 119.18(19) . . ? C51 C46 C45 120.01(19) . . ? C47 C46 C45 120.70(18) . . ? C48 C47 C46 119.11(19) . . ? C48 C47 C52 118.33(19) . . ? C46 C47 C52 122.37(19) . . ? C49 C48 C47 122.4(2) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C50 C49 C48 117.7(2) . . ? C50 C49 C55 120.87(19) . . ? C48 C49 C55 121.4(2) . . ? C49 C50 C51 122.2(2) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C50 C51 C46 119.30(19) . . ? C50 C51 C58 118.84(19) . . ? C46 C51 C58 121.74(19) . . ? C47 C52 C54 114.30(18) . . ? C47 C52 C53 109.26(18) . . ? C54 C52 C53 108.65(19) . . ? C47 C52 H52 108.2 . . ? C54 C52 H52 108.2 . . ? C53 C52 H52 108.2 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C57 C55 C49 110.52(19) . . ? C57 C55 C56 110.31(19) . . ? C49 C55 C56 112.55(19) . . ? C57 C55 H55 107.8 . . ? C49 C55 H55 107.8 . . ? C56 C55 H55 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 C51 113.48(19) . . ? C59 C58 C60 110.8(2) . . ? C51 C58 C60 109.72(19) . . ? C59 C58 H58 107.5 . . ? C51 C58 H58 107.5 . . ? C60 C58 H58 107.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 P1 C1 C6 -46.29(19) . . . . ? C5 P1 C1 C6 -156.30(18) . . . . ? P2 P1 C1 C6 -119.32(19) . . . . ? C10 P1 C1 C2 76.04(18) . . . . ? C5 P1 C1 C2 -33.96(19) . . . . ? P2 P1 C1 C2 3.02(13) . . . . ? C10 P1 C1 C7 -161.47(16) . . . . ? C5 P1 C1 C7 88.52(17) . . . . ? P2 P1 C1 C7 125.50(17) . . . . ? C6 C1 C2 C3 176.2(2) . . . . ? C7 C1 C2 C3 -66.2(3) . . . . ? P1 C1 C2 C3 54.5(2) . . . . ? C1 C2 C3 C4 -67.2(3) . . . . ? C2 C3 C4 C5 61.8(3) . . . . ? C3 C4 C5 C8 -170.4(2) . . . . ? C3 C4 C5 C9 73.1(3) . . . . ? C3 C4 C5 P1 -45.3(3) . . . . ? C10 P1 C5 C8 47.2(2) . . . . ? C1 P1 C5 C8 154.41(18) . . . . ? P2 P1 C5 C8 115.3(2) . . . . ? C10 P1 C5 C4 -77.3(2) . . . . ? C1 P1 C5 C4 29.9(2) . . . . ? P2 P1 C5 C4 -9.26(15) . . . . ? C10 P1 C5 C9 162.14(16) . . . . ? C1 P1 C5 C9 -90.69(17) . . . . ? P2 P1 C5 C9 -129.83(19) . . . . ? C1 P1 C10 C11 -68.7(2) . . . . ? C5 P1 C10 C11 38.7(2) . . . . ? P2 P1 C10 C11 -11.89(18) . . . . ? C1 P1 C10 C15 112.63(17) . . . . ? C5 P1 C10 C15 -140.00(17) . . . . ? P2 P1 C10 C15 169.40(17) . . . . ? C15 C10 C11 C12 -0.4(3) . . . . ? P1 C10 C11 C12 -179.14(18) . . . . ? C10 C11 C12 C13 0.7(4) . . . . ? C11 C12 C13 C14 0.0(4) . . . . ? C12 C13 C14 C15 -1.1(4) . . . . ? C13 C14 C15 C10 1.3(3) . . . . ? C13 C14 C15 C16 -178.8(2) . . . . ? C11 C10 C15 C14 -0.6(3) . . . . ? P1 C10 C15 C14 178.19(16) . . . . ? C11 C10 C15 C16 179.57(19) . . . . ? P1 C10 C15 C16 -1.6(3) . . . . ? C14 C15 C16 C17 -101.4(2) . . . . ? C10 C15 C16 C17 78.4(3) . . . . ? C14 C15 C16 C21 76.1(3) . . . . ? C10 C15 C16 C21 -104.1(2) . . . . ? C21 C16 C17 C18 3.9(3) . . . . ? C15 C16 C17 C18 -178.53(19) . . . . ? C21 C16 C17 C22 -172.41(19) . . . . ? C15 C16 C17 C22 5.1(3) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C22 C17 C18 C19 175.4(2) . . . . ? C17 C18 C19 C20 -1.6(3) . . . . ? C17 C18 C19 C25 -179.9(2) . . . . ? C18 C19 C20 C21 1.3(3) . . . . ? C25 C19 C20 C21 179.6(2) . . . . ? C19 C20 C21 C16 1.7(3) . . . . ? C19 C20 C21 C28 -175.1(2) . . . . ? C17 C16 C21 C20 -4.3(3) . . . . ? C15 C16 C21 C20 178.24(19) . . . . ? C17 C16 C21 C28 172.42(19) . . . . ? C15 C16 C21 C28 -5.1(3) . . . . ? C18 C17 C22 C23 40.1(3) . . . . ? C16 C17 C22 C23 -143.5(2) . . . . ? C18 C17 C22 C24 -83.8(2) . . . . ? C16 C17 C22 C24 92.5(2) . . . . ? C18 C19 C25 C27 112.8(2) . . . . ? C20 C19 C25 C27 -65.4(3) . . . . ? C18 C19 C25 C26 -122.7(2) . . . . ? C20 C19 C25 C26 59.0(3) . . . . ? C20 C21 C28 C29 -42.7(3) . . . . ? C16 C21 C28 C29 140.6(2) . . . . ? C20 C21 C28 C30 79.4(2) . . . . ? C16 C21 C28 C30 -97.3(2) . . . . ? C40 P2 C31 C37 46.80(19) . . . . ? C35 P2 C31 C37 154.28(17) . . . . ? P1 P2 C31 C37 87.22(17) . . . . ? C40 P2 C31 C36 161.96(17) . . . . ? C35 P2 C31 C36 -90.55(18) . . . . ? P1 P2 C31 C36 -157.61(18) . . . . ? C40 P2 C31 C32 -76.7(2) . . . . ? C35 P2 C31 C32 30.8(2) . . . . ? P1 P2 C31 C32 -36.23(17) . . . . ? C37 C31 C32 C33 -168.0(2) . . . . ? C36 C31 C32 C33 75.4(3) . . . . ? P2 C31 C32 C33 -44.0(3) . . . . ? C31 C32 C33 C34 59.3(3) . . . . ? C32 C33 C34 C35 -65.5(3) . . . . ? C33 C34 C35 C39 175.9(2) . . . . ? C33 C34 C35 C38 -66.5(3) . . . . ? C33 C34 C35 P2 55.0(3) . . . . ? C40 P2 C35 C39 -48.14(19) . . . . ? C31 P2 C35 C39 -157.98(17) . . . . ? P1 P2 C35 C39 -89.48(17) . . . . ? C40 P2 C35 C34 73.93(18) . . . . ? C31 P2 C35 C34 -35.91(19) . . . . ? P1 P2 C35 C34 32.59(15) . . . . ? C40 P2 C35 C38 -162.85(16) . . . . ? C31 P2 C35 C38 87.31(18) . . . . ? P1 P2 C35 C38 155.81(17) . . . . ? C35 P2 C40 C41 -68.5(2) . . . . ? C31 P2 C40 C41 38.9(2) . . . . ? P1 P2 C40 C41 -14.44(14) . . . . ? C35 P2 C40 C45 113.71(17) . . . . ? C31 P2 C40 C45 -138.88(17) . . . . ? P1 P2 C40 C45 167.7(2) . . . . ? C45 C40 C41 C42 1.4(3) . . . . ? P2 C40 C41 C42 -176.42(18) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 -0.2(3) . . . . ? C42 C43 C44 C45 0.2(3) . . . . ? C43 C44 C45 C40 0.7(3) . . . . ? C43 C44 C45 C46 -179.6(2) . . . . ? C41 C40 C45 C44 -1.4(3) . . . . ? P2 C40 C45 C44 176.56(16) . . . . ? C41 C40 C45 C46 178.92(19) . . . . ? P2 C40 C45 C46 -3.1(3) . . . . ? C44 C45 C46 C51 -99.5(2) . . . . ? C40 C45 C46 C51 80.2(3) . . . . ? C44 C45 C46 C47 76.6(3) . . . . ? C40 C45 C46 C47 -103.8(2) . . . . ? C51 C46 C47 C48 -3.8(3) . . . . ? C45 C46 C47 C48 -179.9(2) . . . . ? C51 C46 C47 C52 171.04(19) . . . . ? C45 C46 C47 C52 -5.0(3) . . . . ? C46 C47 C48 C49 2.4(3) . . . . ? C52 C47 C48 C49 -172.6(2) . . . . ? C47 C48 C49 C50 0.2(3) . . . . ? C47 C48 C49 C55 177.1(2) . . . . ? C48 C49 C50 C51 -1.3(3) . . . . ? C55 C49 C50 C51 -178.3(2) . . . . ? C49 C50 C51 C46 -0.1(3) . . . . ? C49 C50 C51 C58 175.9(2) . . . . ? C47 C46 C51 C50 2.7(3) . . . . ? C45 C46 C51 C50 178.81(19) . . . . ? C47 C46 C51 C58 -173.2(2) . . . . ? C45 C46 C51 C58 2.9(3) . . . . ? C48 C47 C52 C54 -45.3(3) . . . . ? C46 C47 C52 C54 139.8(2) . . . . ? C48 C47 C52 C53 76.6(2) . . . . ? C46 C47 C52 C53 -98.2(2) . . . . ? C50 C49 C55 C57 114.1(2) . . . . ? C48 C49 C55 C57 -62.8(3) . . . . ? C50 C49 C55 C56 -122.1(2) . . . . ? C48 C49 C55 C56 61.1(3) . . . . ? C50 C51 C58 C59 47.2(3) . . . . ? C46 C51 C58 C59 -136.9(2) . . . . ? C50 C51 C58 C60 -77.4(3) . . . . ? C46 C51 C58 C60 98.5(2) . . . . ? _refine_diff_density_max 0.276 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.060 _shelx_res_file ; XRAY3534_0ma_a.res created by SHELXL-2014/7 TITL XRAY3534_0ma_a.res in Pbca CELL 0.71073 30.6711 10.2786 33.8120 90.000 90.000 90.000 ZERR 16.000 0.0043 0.0015 0.0047 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H P UNIT 480 720 16 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 CONF SIZE 0.030 0.100 0.400 CONF BIND P2 P1 TEMP -173.000 WGHT 0.040300 9.942597 FVAR 0.17732 MOLE 1 P1 3 0.396007 0.721098 0.045095 11.00000 0.01705 0.01780 = 0.01950 0.00123 -0.00266 -0.00131 C1 1 0.382402 0.790317 0.095310 11.00000 0.02356 0.01796 = 0.02858 -0.00176 0.00344 -0.00102 C2 1 0.421923 0.835806 0.119292 11.00000 0.03400 0.02549 = 0.02156 -0.00587 -0.00538 0.00471 AFIX 23 H2A 2 0.411429 0.875804 0.144168 11.00000 -1.20000 H2B 2 0.439609 0.758773 0.126470 11.00000 -1.20000 AFIX 0 C3 1 0.451063 0.933043 0.098051 11.00000 0.02780 0.02774 = 0.03654 -0.01019 -0.00858 -0.00470 AFIX 23 H3A 2 0.473011 0.966982 0.116878 11.00000 -1.20000 H3B 2 0.433137 1.007293 0.088919 11.00000 -1.20000 AFIX 0 C4 1 0.474379 0.873238 0.062720 11.00000 0.02296 0.03191 = 0.04180 -0.00389 0.00261 -0.01283 AFIX 23 H4A 2 0.492696 0.800490 0.072320 11.00000 -1.20000 H4B 2 0.494162 0.939544 0.051364 11.00000 -1.20000 AFIX 0 C5 1 0.444808 0.821752 0.029445 11.00000 0.03042 0.02519 = 0.02555 0.00006 0.00522 -0.00820 C6 1 0.357729 0.686890 0.118595 11.00000 0.05528 0.03024 = 0.03755 -0.00684 0.02753 -0.00848 AFIX 137 H6A 2 0.377673 0.616067 0.125614 11.00000 -1.50000 H6B 2 0.333881 0.652496 0.102386 11.00000 -1.50000 H6C 2 0.345770 0.725601 0.142759 11.00000 -1.50000 AFIX 0 C7 1 0.350918 0.903869 0.088504 11.00000 0.02490 0.02954 = 0.04829 -0.01342 -0.00107 0.00564 AFIX 137 H7A 2 0.341033 0.937769 0.114067 11.00000 -1.50000 H7B 2 0.325723 0.873499 0.073255 11.00000 -1.50000 H7C 2 0.365859 0.972966 0.073836 11.00000 -1.50000 AFIX 0 C8 1 0.472696 0.744775 0.000018 11.00000 0.03957 0.04205 = 0.03883 -0.00675 0.01766 -0.01649 AFIX 137 H8A 2 0.496237 0.800319 -0.009928 11.00000 -1.50000 H8B 2 0.454471 0.716073 -0.022132 11.00000 -1.50000 H8C 2 0.485215 0.668699 0.013294 11.00000 -1.50000 AFIX 0 C9 1 0.425269 0.938501 0.006779 11.00000 0.05552 0.02992 = 0.03500 0.00817 -0.00134 -0.01425 AFIX 137 H9A 2 0.407661 0.991226 0.024891 11.00000 -1.50000 H9B 2 0.406852 0.906580 -0.014826 11.00000 -1.50000 H9C 2 0.448898 0.991760 -0.004106 11.00000 -1.50000 AFIX 0 C10 1 0.417353 0.558243 0.057527 11.00000 0.01552 0.02084 = 0.01634 -0.00038 0.00051 -0.00006 C11 1 0.456990 0.537491 0.077155 11.00000 0.01606 0.02135 = 0.02556 -0.00397 -0.00159 0.00081 AFIX 43 H11 2 0.473809 0.610805 0.084897 11.00000 -1.20000 AFIX 0 C12 1 0.472585 0.414181 0.085700 11.00000 0.02281 0.02770 = 0.02797 -0.00104 -0.00812 0.00483 AFIX 43 H12 2 0.499440 0.403568 0.099323 11.00000 -1.20000 AFIX 0 C13 1 0.448635 0.306742 0.074182 11.00000 0.02485 0.02345 = 0.02873 0.00153 -0.00280 0.00626 AFIX 43 H13 2 0.458901 0.221545 0.079832 11.00000 -1.20000 AFIX 0 C14 1 0.409567 0.324205 0.054347 11.00000 0.02428 0.01961 = 0.02307 -0.00136 -0.00217 0.00128 AFIX 43 H14 2 0.393568 0.249800 0.046150 11.00000 -1.20000 AFIX 0 C15 1 0.392911 0.447815 0.045997 11.00000 0.01590 0.02090 = 0.01335 0.00001 -0.00034 -0.00019 C16 1 0.349796 0.457287 0.025024 11.00000 0.01803 0.01497 = 0.01429 -0.00104 -0.00101 -0.00059 C17 1 0.348743 0.484482 -0.015784 11.00000 0.01829 0.01503 = 0.01460 -0.00174 0.00183 -0.00011 C18 1 0.308453 0.495930 -0.034603 11.00000 0.02042 0.01903 = 0.01467 0.00064 -0.00139 -0.00272 AFIX 43 H18 2 0.307892 0.515652 -0.062048 11.00000 -1.20000 AFIX 0 C19 1 0.269186 0.479700 -0.014886 11.00000 0.01673 0.01848 = 0.01689 0.00108 -0.00215 -0.00144 C20 1 0.271002 0.447593 0.025074 11.00000 0.01655 0.01960 = 0.01652 0.00163 0.00139 -0.00362 AFIX 43 H20 2 0.244457 0.434330 0.038979 11.00000 -1.20000 AFIX 0 C21 1 0.310234 0.434123 0.045502 11.00000 0.01923 0.01670 = 0.01522 -0.00130 -0.00143 -0.00169 C22 1 0.390400 0.493564 -0.039978 11.00000 0.01651 0.02551 = 0.01739 0.00099 0.00067 -0.00053 AFIX 13 H22 2 0.414642 0.516579 -0.021479 11.00000 -1.20000 AFIX 0 C23 1 0.388816 0.597822 -0.072125 11.00000 0.02226 0.04338 = 0.02804 0.01202 0.00395 -0.00277 AFIX 137 H23A 2 0.368006 0.571818 -0.092649 11.00000 -1.50000 H23B 2 0.417834 0.607861 -0.083867 11.00000 -1.50000 H23C 2 0.379591 0.680692 -0.060488 11.00000 -1.50000 AFIX 0 C24 1 0.401091 0.361257 -0.058179 11.00000 0.03275 0.03674 = 0.03484 -0.00810 0.00942 0.00173 AFIX 137 H24A 2 0.404278 0.296473 -0.037111 11.00000 -1.50000 H24B 2 0.428393 0.367421 -0.073117 11.00000 -1.50000 H24C 2 0.377455 0.335034 -0.075979 11.00000 -1.50000 AFIX 0 C25 1 0.225821 0.492607 -0.036242 11.00000 0.01672 0.02531 = 0.01530 0.00230 -0.00296 -0.00163 AFIX 13 H25 2 0.232127 0.520552 -0.063988 11.00000 -1.20000 AFIX 0 C26 1 0.196668 0.596330 -0.017501 11.00000 0.02225 0.03002 = 0.02552 -0.00202 -0.00402 0.00367 AFIX 137 H26A 2 0.189078 0.570118 0.009502 11.00000 -1.50000 H26B 2 0.169990 0.605818 -0.033190 11.00000 -1.50000 H26C 2 0.212249 0.679537 -0.016804 11.00000 -1.50000 AFIX 0 C27 1 0.202119 0.362189 -0.038298 11.00000 0.02252 0.02730 = 0.02061 0.00105 -0.00279 -0.00427 AFIX 137 H27A 2 0.220637 0.298327 -0.051751 11.00000 -1.50000 H27B 2 0.174816 0.372688 -0.053011 11.00000 -1.50000 H27C 2 0.195688 0.331826 -0.011449 11.00000 -1.50000 AFIX 0 C28 1 0.309422 0.388270 0.088223 11.00000 0.01788 0.02446 = 0.01341 0.00172 -0.00092 -0.00211 AFIX 13 H28 2 0.338186 0.409936 0.100492 11.00000 -1.20000 AFIX 0 C29 1 0.273408 0.451447 0.113333 11.00000 0.02196 0.03674 = 0.01666 0.00211 -0.00080 0.00011 AFIX 137 H29A 2 0.273965 0.545943 0.109510 11.00000 -1.50000 H29B 2 0.278339 0.431371 0.141312 11.00000 -1.50000 H29C 2 0.244959 0.417307 0.105187 11.00000 -1.50000 AFIX 0 C30 1 0.303634 0.239663 0.089553 11.00000 0.04157 0.02479 = 0.02056 0.00569 -0.00038 -0.00565 AFIX 137 H30A 2 0.276501 0.215760 0.076082 11.00000 -1.50000 H30B 2 0.302385 0.210760 0.117150 11.00000 -1.50000 H30C 2 0.328329 0.197804 0.076275 11.00000 -1.50000 AFIX 0 MOLE 2 P2 3 0.602077 0.962518 0.201953 11.00000 0.01653 0.01712 = 0.01960 -0.00055 -0.00269 0.00050 C31 1 0.551909 1.055478 0.218121 11.00000 0.02143 0.02375 = 0.03463 -0.00875 -0.00261 0.00416 C32 1 0.520683 1.100094 0.185124 11.00000 0.02317 0.02850 = 0.05218 -0.01304 -0.01191 0.00998 AFIX 23 H32A 2 0.503081 1.024246 0.176715 11.00000 -1.20000 H32B 2 0.500358 1.165029 0.196426 11.00000 -1.20000 AFIX 0 C33 1 0.541834 1.159254 0.148480 11.00000 0.04022 0.02355 = 0.05131 0.00445 -0.02467 0.00233 AFIX 23 H33A 2 0.518638 1.185125 0.129700 11.00000 -1.20000 H33B 2 0.557755 1.238978 0.156313 11.00000 -1.20000 AFIX 0 C34 1 0.573188 1.068253 0.127576 11.00000 0.04457 0.02185 = 0.03047 0.00661 -0.01201 -0.00537 AFIX 23 H34A 2 0.582550 1.109353 0.102495 11.00000 -1.20000 H34B 2 0.557517 0.987052 0.120802 11.00000 -1.20000 AFIX 0 C35 1 0.613716 1.033333 0.151620 11.00000 0.02733 0.02012 = 0.02340 0.00300 0.00000 -0.00385 C36 1 0.569068 1.175398 0.240399 11.00000 0.03668 0.03365 = 0.04007 -0.01675 -0.00721 0.00783 AFIX 137 H36A 2 0.583946 1.233484 0.221794 11.00000 -1.50000 H36B 2 0.589598 1.147596 0.260937 11.00000 -1.50000 H36C 2 0.544598 1.221556 0.252666 11.00000 -1.50000 AFIX 0 C37 1 0.526040 0.973634 0.247791 11.00000 0.02826 0.04548 = 0.03884 -0.00929 0.01286 0.00249 AFIX 137 H37A 2 0.501450 1.024639 0.257894 11.00000 -1.50000 H37B 2 0.545056 0.948662 0.269811 11.00000 -1.50000 H37C 2 0.515055 0.895209 0.234662 11.00000 -1.50000 AFIX 0 C38 1 0.642593 1.154016 0.157768 11.00000 0.03261 0.02744 = 0.03749 0.00805 -0.00233 -0.00778 AFIX 137 H38A 2 0.650450 1.190890 0.132008 11.00000 -1.50000 H38B 2 0.669141 1.129023 0.171995 11.00000 -1.50000 H38C 2 0.626585 1.219017 0.173219 11.00000 -1.50000 AFIX 0 C39 1 0.641011 0.934061 0.128915 11.00000 0.05203 0.03137 = 0.02906 0.00477 0.01790 0.00265 AFIX 137 H39A 2 0.651721 0.973460 0.104374 11.00000 -1.50000 H39B 2 0.623009 0.858087 0.122589 11.00000 -1.50000 H39C 2 0.665822 0.906919 0.145208 11.00000 -1.50000 AFIX 0 C40 1 0.583132 0.795961 0.190139 11.00000 0.01465 0.01896 = 0.01425 0.00075 0.00160 0.00068 C41 1 0.543620 0.767595 0.171059 11.00000 0.02077 0.02052 = 0.02041 0.00120 -0.00388 0.00186 AFIX 43 H41 2 0.525919 0.837639 0.162215 11.00000 -1.20000 AFIX 0 C42 1 0.529460 0.641612 0.164634 11.00000 0.01902 0.02611 = 0.02270 -0.00022 -0.00514 -0.00317 AFIX 43 H42 2 0.502396 0.625792 0.151846 11.00000 -1.20000 AFIX 0 C43 1 0.555152 0.539073 0.177040 11.00000 0.02467 0.01885 = 0.02310 -0.00365 -0.00022 -0.00518 AFIX 43 H43 2 0.545847 0.451964 0.172924 11.00000 -1.20000 AFIX 0 C44 1 0.594443 0.564000 0.195462 11.00000 0.02229 0.01928 = 0.02547 0.00115 -0.00042 0.00179 AFIX 43 H44 2 0.611917 0.492822 0.203826 11.00000 -1.20000 AFIX 0 C45 1 0.609280 0.690057 0.202175 11.00000 0.01550 0.01830 = 0.01279 -0.00028 0.00178 -0.00039 C46 1 0.652685 0.705366 0.222270 11.00000 0.01662 0.01520 = 0.01712 0.00120 -0.00111 0.00233 C47 1 0.691809 0.685011 0.201260 11.00000 0.01908 0.01511 = 0.01661 -0.00074 -0.00052 0.00066 C48 1 0.731399 0.699786 0.220858 11.00000 0.01694 0.02249 = 0.01802 -0.00074 0.00053 0.00268 AFIX 43 H48 2 0.757677 0.689244 0.206334 11.00000 -1.20000 AFIX 0 C49 1 0.733898 0.729361 0.260846 11.00000 0.01698 0.01863 = 0.01758 -0.00034 -0.00190 0.00043 C50 1 0.695146 0.743879 0.281352 11.00000 0.02005 0.02062 = 0.01293 -0.00003 0.00013 -0.00120 AFIX 43 H50 2 0.696198 0.762312 0.308868 11.00000 -1.20000 AFIX 0 C51 1 0.654578 0.732363 0.262988 11.00000 0.01813 0.01575 = 0.01673 0.00047 0.00176 0.00138 C52 1 0.692443 0.636307 0.158583 11.00000 0.01834 0.02304 = 0.01516 -0.00057 -0.00189 0.00170 AFIX 13 H52 2 0.663043 0.652405 0.146770 11.00000 -1.20000 AFIX 0 C53 1 0.700787 0.489116 0.158363 11.00000 0.03344 0.02709 = 0.02068 -0.00484 -0.00268 0.00652 AFIX 137 H53A 2 0.728732 0.470781 0.171264 11.00000 -1.50000 H53B 2 0.701649 0.457758 0.131003 11.00000 -1.50000 H53C 2 0.677310 0.444801 0.172683 11.00000 -1.50000 AFIX 0 C54 1 0.726640 0.702398 0.132270 11.00000 0.02253 0.03803 = 0.01802 -0.00415 0.00367 -0.00194 AFIX 137 H54A 2 0.724443 0.797018 0.135225 11.00000 -1.50000 H54B 2 0.721486 0.678661 0.104591 11.00000 -1.50000 H54C 2 0.755839 0.673736 0.140184 11.00000 -1.50000 AFIX 0 C55 1 0.777629 0.738784 0.282063 11.00000 0.01689 0.02584 = 0.01862 -0.00312 -0.00319 0.00122 AFIX 13 H55 2 0.771714 0.761285 0.310332 11.00000 -1.20000 AFIX 0 C56 1 0.806841 0.844721 0.264913 11.00000 0.02834 0.03388 = 0.04441 0.00379 -0.01021 -0.00501 AFIX 137 H56A 2 0.814347 0.822834 0.237538 11.00000 -1.50000 H56B 2 0.833557 0.851257 0.280687 11.00000 -1.50000 H56C 2 0.791395 0.928162 0.265492 11.00000 -1.50000 AFIX 0 C57 1 0.800966 0.608317 0.281332 11.00000 0.02698 0.03505 = 0.02681 0.00017 -0.00748 0.00615 AFIX 137 H57A 2 0.781911 0.541258 0.292544 11.00000 -1.50000 H57B 2 0.827774 0.614034 0.297006 11.00000 -1.50000 H57C 2 0.808256 0.585558 0.253974 11.00000 -1.50000 AFIX 0 C58 1 0.613457 0.740619 0.288307 11.00000 0.01884 0.02591 = 0.01605 0.00148 -0.00016 -0.00103 AFIX 13 H58 2 0.588176 0.753087 0.270020 11.00000 -1.20000 AFIX 0 C59 1 0.613665 0.854284 0.317139 11.00000 0.02322 0.04937 = 0.02507 -0.01233 0.00227 0.00082 AFIX 137 H59A 2 0.636931 0.841778 0.336637 11.00000 -1.50000 H59B 2 0.585480 0.858852 0.330721 11.00000 -1.50000 H59C 2 0.618717 0.935428 0.302627 11.00000 -1.50000 AFIX 0 C60 1 0.606510 0.611889 0.310122 11.00000 0.02636 0.03902 = 0.03538 0.01571 0.00755 0.00018 AFIX 137 H60A 2 0.602902 0.541521 0.290842 11.00000 -1.50000 H60B 2 0.580320 0.617988 0.326622 11.00000 -1.50000 H60C 2 0.631857 0.593694 0.326879 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY3534_0ma_a.res in Pbca REM R1 = 0.0539 for 7303 Fo > 4sig(Fo) and 0.1106 for all 12238 data REM 579 parameters refined using 0 restraints END WGHT 0.0488 5.2336 REM Highest difference peak 0.276, deepest hole -0.383, 1-sigma level 0.060 Q1 1 0.2489 0.4866 -0.0257 11.00000 0.05 0.28 Q2 1 0.3697 0.4919 -0.0271 11.00000 0.05 0.27 Q3 1 0.6184 0.4991 0.2329 11.00000 0.05 0.27 Q4 1 0.6371 0.7255 0.2757 11.00000 0.05 0.26 Q5 1 0.7794 0.4196 0.2352 11.00000 0.05 0.25 Q6 1 0.5933 1.0366 0.1428 11.00000 0.05 0.23 Q7 1 0.7537 0.7486 0.2728 11.00000 0.05 0.23 Q8 1 0.6762 0.7444 0.2712 11.00000 0.05 0.22 Q9 1 0.6283 0.5282 0.1798 11.00000 0.05 0.22 Q10 1 0.3588 0.1979 0.0920 11.00000 0.05 0.21 Q11 1 0.6300 0.7020 0.2120 11.00000 0.05 0.21 Q12 1 0.6513 1.1382 0.2133 11.00000 0.05 0.20 Q13 1 0.6795 1.0119 0.1146 11.00000 0.05 0.20 Q14 1 0.5913 0.4449 0.1705 11.00000 0.05 0.20 Q15 1 0.5811 1.0732 0.1874 11.00000 0.05 0.20 Q16 1 0.3388 0.8095 0.1647 11.00000 0.05 0.20 Q17 1 0.5889 0.4692 0.2278 11.00000 0.05 0.20 Q18 1 0.5393 1.0811 0.2033 11.00000 0.05 0.20 Q19 1 0.6009 0.5232 0.2064 11.00000 0.05 0.20 Q20 1 0.6378 0.8929 0.3314 11.00000 0.05 0.20 ; _shelx_res_checksum 40710 _shelx_hkl_file ; 0 1 0 0.40 0.90 0 1 0 -1.50 0.80 0 1 0 0.40 0.90 0 1 0 -0.30 1.10 0 2 0 107.39 8.10 0 2 0 103.79 7.60 0 2 0 103.99 7.60 0 2 0 92.79 8.20 0 3 0 -8.90 2.30 0 3 0 -0.30 3.00 0 3 0 0.60 3.50 0 3 0 -2.90 2.70 0 4 0 1599.84 84.19 0 4 0 1564.94 85.19 0 4 0 1534.45 84.09 0 4 0 1541.35 84.89 0 5 0 3.50 4.30 0 5 0 -5.70 3.70 0 5 0 2.10 3.50 0 5 0 -2.10 3.30 0 6 0 13.40 5.00 0 -6 0 9.80 4.70 0 6 0 25.50 7.30 0 6 0 18.30 6.90 0 7 0 2.30 5.80 0 7 0 -6.60 4.00 0 7 0 2.60 6.40 0 -7 0 -0.30 4.20 0 -8 0 70.39 11.30 0 8 0 82.39 13.50 0 8 0 91.29 14.50 0 8 0 96.89 12.10 0 -9 0 -7.80 5.30 0 9 0 1.50 7.20 0 9 0 7.80 8.40 0 10 0 102.49 17.50 0 10 0 101.39 17.10 0 -10 0 102.79 14.50 0 11 0 -6.70 8.60 0 11 0 -0.30 9.70 0 12 0 68.79 16.70 0 -13 0 -2.60 10.20 1 1 0 0.30 1.00 -1 1 0 -0.90 0.90 -1 1 0 1.30 1.10 -1 1 0 -1.90 0.80 -1 -1 0 -1.00 0.40 1 1 0 0.60 0.90 1 1 0 -0.90 0.90 -1 1 0 -1.10 1.00 -1 2 0 -0.60 2.10 1 2 0 -2.70 2.40 -1 2 0 2.00 2.40 1 2 0 1.80 2.10 1 2 0 -0.50 2.70 1 2 0 3.20 2.30 -1 2 0 0.10 2.20 -1 2 0 0.20 2.40 1 3 0 2.60 3.50 -1 3 0 -2.70 2.90 -1 3 0 -1.70 3.20 1 3 0 3.40 3.80 1 3 0 -3.80 2.40 1 3 0 -0.30 2.60 -1 3 0 -0.10 3.10 -1 3 0 1.40 3.00 -1 4 0 1.20 3.70 1 4 0 -0.40 3.00 -1 4 0 -1.00 3.10 1 4 0 -3.20 3.60 -1 -4 0 -1.30 2.80 -1 4 0 -0.30 2.90 1 4 0 -3.10 3.70 -1 4 0 1.00 3.50 -1 5 0 2.30 4.70 1 5 0 -5.10 3.90 -1 -5 0 -1.90 2.80 1 5 0 1.80 4.60 1 5 0 -3.30 3.40 -1 5 0 5.20 4.30 -1 5 0 3.40 3.70 -1 5 0 -3.00 2.90 -1 6 0 9.50 5.30 1 6 0 -4.60 3.60 1 6 0 4.50 5.60 -1 6 0 -2.40 4.30 1 6 0 -3.80 5.50 -1 6 0 -2.60 4.80 -1 -6 0 -1.90 3.40 -1 6 0 -0.70 3.50 1 7 0 -4.30 5.20 -1 -7 0 -0.60 4.50 1 -7 0 -1.60 4.50 1 7 0 3.70 6.50 -1 7 0 5.30 6.00 1 7 0 1.40 4.80 -1 7 0 -6.60 3.90 -1 7 0 6.80 6.30 1 -8 0 10.60 6.10 1 8 0 8.00 7.60 -1 8 0 -6.30 6.10 -1 8 0 0.70 7.00 1 8 0 -4.60 6.10 1 8 0 -5.70 4.80 -1 8 0 4.90 5.30 -1 -8 0 7.90 5.30 -1 9 0 -0.60 6.60 1 -9 0 5.00 6.70 1 9 0 0.80 7.20 1 9 0 -6.10 6.90 -1 9 0 17.00 8.60 -1 -9 0 -4.80 5.20 -1 10 0 -10.60 7.90 1 10 0 4.50 9.00 -1 -10 0 1.30 6.40 1 -10 0 6.20 6.90 1 10 0 4.70 8.50 -1 10 0 11.10 9.30 1 11 0 0.40 10.10 1 -11 0 -2.50 7.20 1 11 0 -8.10 8.70 -1 11 0 5.60 9.20 -1 11 0 -2.50 8.20 1 12 0 8.70 10.30 -1 12 0 -13.60 9.00 -1 -12 0 -10.50 9.00 -1 -13 0 15.10 11.70 1 -13 0 -11.40 8.90 2 0 0 -3.90 0.30 -2 0 0 -3.70 0.20 -2 0 0 -4.20 0.30 2 0 0 -4.10 0.40 2 1 0 285.77 15.20 -2 1 0 274.97 15.40 -2 1 0 267.57 14.90 2 2 0 62.39 6.10 2 2 0 54.59 5.20 -2 -2 0 63.29 5.10 -2 2 0 63.49 6.00 -2 2 0 67.39 6.40 -2 2 0 65.29 5.60 2 2 0 76.89 7.40 -2 2 0 53.99 5.60 -2 3 0 -1.50 3.20 -2 3 0 5.80 3.60 2 3 0 4.40 2.70 -2 -3 0 -0.70 2.40 -2 3 0 2.30 3.30 -2 3 0 -0.70 3.00 2 3 0 0.10 3.40 2 3 0 4.60 4.10 -2 4 0 343.67 22.00 -2 4 0 346.67 21.50 -2 4 0 321.77 21.00 -2 4 0 328.97 21.40 2 4 0 332.77 22.30 2 4 0 337.47 20.80 -2 -4 0 320.57 20.20 2 4 0 334.87 22.10 -2 5 0 473.65 29.20 -2 5 0 503.15 30.00 2 5 0 492.95 29.00 -2 5 0 466.85 30.30 -2 5 0 461.85 29.60 2 5 0 450.95 30.50 -2 -5 0 464.15 28.40 2 5 0 482.95 30.60 -2 6 0 -1.00 4.70 -2 6 0 2.60 5.40 2 6 0 5.20 5.30 2 6 0 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6.00 -11 -9 0 5.10 7.90 11 9 0 0.10 9.50 11 -9 0 1.20 7.10 -11 9 0 4.80 7.90 -11 -10 0 12.60 9.20 -11 10 0 3.50 8.80 11 -10 0 -0.20 8.50 11 10 0 14.80 10.90 -11 10 0 -5.50 7.60 -11 -11 0 -14.70 7.60 -11 11 0 -3.20 8.70 -11 11 0 -1.70 9.10 11 11 0 17.50 13.20 11 12 0 4.30 11.20 11 -12 0 5.70 10.70 -11 -12 0 -6.60 9.10 12 0 0 2016.00 104.49 -12 0 0 1918.71 104.39 12 0 0 1982.60 105.89 -12 0 0 1909.11 104.19 12 -1 0 184.68 13.90 -12 -1 0 175.78 12.20 12 1 0 154.78 12.80 -12 1 0 157.38 12.40 -12 1 0 163.78 11.70 12 1 0 163.58 13.10 -12 -1 0 139.39 10.90 12 -1 0 168.88 11.10 12 2 0 10.30 4.20 -12 2 0 3.90 3.00 12 2 0 1.90 4.80 12 -2 0 7.60 4.80 -12 2 0 10.00 4.40 -12 -2 0 0.50 2.90 -12 -2 0 6.40 2.60 12 -2 0 7.00 2.60 -12 3 0 766.92 45.20 12 3 0 792.62 45.70 -12 3 0 800.32 46.80 12 3 0 801.72 48.00 -12 -3 0 842.92 46.20 12 -3 0 775.52 42.40 12 -3 0 795.22 47.50 -12 -3 0 816.72 43.40 12 -4 0 46.40 8.90 12 4 0 56.49 8.30 12 4 0 71.09 11.30 12 -4 0 76.19 6.00 -12 4 0 65.89 9.10 -12 4 0 72.19 10.90 -12 -4 0 74.49 9.70 -12 -4 0 68.69 6.60 -12 -5 0 54.09 6.60 12 -5 0 61.69 10.00 12 5 0 76.49 13.00 -12 5 0 80.89 11.70 12 5 0 62.69 8.80 -12 -5 0 78.89 10.40 -12 5 0 61.59 9.50 12 -5 0 58.19 6.40 12 6 0 -16.60 6.00 -12 6 0 1.00 5.10 12 -6 0 2.70 6.80 -12 -6 0 5.70 3.80 12 6 0 -2.60 4.70 -12 6 0 -1.60 4.60 -12 -6 0 -4.60 4.70 -12 -7 0 41.50 9.90 12 7 0 34.70 10.30 12 -7 0 28.70 9.50 -12 7 0 33.30 9.30 12 7 0 46.10 12.80 -12 7 0 20.40 7.40 12 -8 0 129.69 16.50 -12 8 0 102.59 15.80 12 8 0 105.79 17.70 -12 -8 0 132.29 17.20 -12 8 0 111.89 17.00 12 9 0 0.80 9.30 -12 -9 0 11.10 8.70 -12 9 0 4.70 7.60 12 -9 0 27.60 10.50 -12 9 0 -3.90 7.00 12 10 0 23.60 12.50 -12 10 0 1.30 7.50 12 -10 0 -1.50 8.00 -12 -10 0 -9.40 7.20 -12 10 0 3.60 7.70 -12 11 0 187.08 24.30 -12 -11 0 183.48 23.60 -12 11 0 157.08 22.30 12 11 0 173.28 26.40 -12 -12 0 12.10 10.80 12 12 0 6.60 12.20 12 -12 0 12.90 10.80 13 0 0 6.90 4.80 -13 0 0 1.80 3.10 -13 0 0 1.40 2.90 13 0 0 0.00 3.70 -13 1 0 0.70 2.60 -13 1 0 1.10 2.80 13 1 0 -1.40 3.80 13 -1 0 -4.50 2.70 -13 -1 0 -1.70 2.60 13 -1 0 2.80 4.70 13 1 0 1.60 4.30 -13 -1 0 -2.50 2.00 -13 2 0 0.00 2.60 -13 2 0 -1.00 2.90 13 2 0 -4.40 4.50 -13 -2 0 -3.60 2.10 13 -2 0 -7.50 4.50 13 2 0 0.00 3.60 13 -2 0 2.40 2.40 -13 -2 0 4.50 3.40 13 -3 0 0.10 2.10 13 -3 0 -4.80 4.90 -13 -3 0 2.90 3.60 -13 -3 0 -2.30 2.10 -13 3 0 -1.00 2.80 -13 3 0 -1.70 3.50 13 3 0 2.50 3.60 13 3 0 1.10 5.80 13 -4 0 -2.80 2.40 -13 -4 0 1.70 2.70 -13 -4 0 -3.20 3.40 13 -4 0 -0.10 6.40 -13 4 0 -1.70 3.50 13 4 0 0.60 6.90 13 4 0 -5.30 3.90 -13 4 0 -5.80 4.20 -13 -5 0 2.90 2.90 -13 -5 0 -3.80 4.20 13 -5 0 1.40 2.90 -13 5 0 0.10 4.70 13 -5 0 0.00 5.20 13 5 0 -7.70 5.20 13 5 0 0.10 4.00 -13 5 0 -0.20 4.50 13 6 0 -4.10 6.60 -13 -6 0 -8.90 4.20 -13 6 0 -0.60 4.90 -13 6 0 -1.00 5.20 -13 -6 0 7.00 4.10 13 6 0 -0.40 4.90 13 -6 0 -6.10 5.40 -13 7 0 3.00 6.30 -13 -7 0 8.60 6.90 13 -7 0 2.90 7.60 -13 7 0 6.00 6.30 13 7 0 7.70 8.80 -13 8 0 4.10 6.80 -13 -8 0 -4.50 5.80 -13 8 0 4.80 7.30 13 8 0 -8.10 7.80 13 -8 0 0.20 7.00 -13 9 0 -2.60 7.00 -13 9 0 0.30 8.50 13 -9 0 -0.90 8.00 -13 -9 0 4.50 7.20 13 9 0 -3.80 8.70 -13 10 0 0.70 7.90 13 -10 0 14.70 9.20 -13 10 0 -6.70 7.50 13 10 0 -4.20 9.70 -13 -10 0 -12.30 6.90 13 11 0 9.10 10.60 -13 11 0 -0.60 9.90 -13 11 0 1.20 9.50 -13 -11 0 -5.30 8.30 13 12 0 -15.80 10.80 13 -12 0 12.40 11.40 -13 -12 0 1.90 10.70 -14 0 0 1459.45 80.79 -14 0 0 1499.35 80.79 14 0 0 1492.85 80.89 14 0 0 1526.45 82.69 14 -1 0 60.59 6.70 14 1 0 49.40 8.60 -14 -1 0 65.69 7.80 14 1 0 45.10 7.80 -14 1 0 64.19 8.00 14 -1 0 56.39 8.60 -14 1 0 48.60 6.60 -14 -1 0 58.99 6.60 -14 2 0 3.70 3.10 -14 -2 0 1.40 3.10 14 -2 0 -3.50 4.90 -14 -2 0 0.30 2.60 14 2 0 -0.30 5.20 14 -2 0 1.50 3.00 14 2 0 -0.40 3.80 -14 2 0 0.50 3.50 -14 -3 0 151.68 12.80 -14 3 0 151.08 15.20 14 -3 0 150.38 9.40 -14 -3 0 136.59 10.30 -14 3 0 153.98 12.50 14 -3 0 137.79 15.00 14 3 0 133.29 15.20 14 3 0 156.08 13.30 -14 4 0 48.10 8.80 -14 4 0 41.60 7.30 -14 -4 0 43.80 7.90 14 4 0 31.50 6.60 14 -4 0 35.10 4.20 14 4 0 46.60 10.60 14 -4 0 24.80 8.50 -14 -4 0 42.60 5.30 -14 -5 0 37.20 8.00 -14 5 0 48.30 8.70 14 5 0 36.00 7.30 -14 5 0 33.40 8.50 14 5 0 38.50 10.60 14 -5 0 29.30 9.40 -14 -5 0 30.10 5.00 14 6 0 41.50 8.80 -14 6 0 38.20 8.50 -14 6 0 13.50 7.70 14 6 0 29.50 12.00 14 -6 0 45.30 10.80 -14 -6 0 25.20 7.90 14 -7 0 634.54 43.20 -14 7 0 646.44 43.80 -14 -7 0 647.74 42.60 -14 7 0 733.73 42.90 14 7 0 567.34 44.70 -14 8 0 84.39 14.00 -14 8 0 87.89 15.90 -14 -8 0 112.19 15.90 14 -8 0 108.99 15.80 14 8 0 105.29 17.70 14 -9 0 2.70 8.80 -14 -9 0 11.10 8.60 -14 9 0 -9.80 6.70 14 9 0 -9.50 9.30 -14 9 0 4.00 7.90 14 -10 0 34.10 11.50 -14 10 0 9.10 8.50 -14 10 0 3.30 8.30 14 10 0 21.90 11.00 -14 -10 0 27.30 11.30 -14 -11 0 5.50 9.90 -14 11 0 29.60 12.30 14 11 0 9.60 11.80 -14 -12 0 73.59 17.70 14 -12 0 71.49 16.90 14 12 0 54.39 16.70 -15 0 0 6.30 3.80 15 0 0 -3.40 4.00 15 0 0 4.60 4.50 -15 0 0 2.20 3.20 -15 -1 0 -1.30 2.70 15 -1 0 5.70 3.80 15 1 0 9.70 5.10 15 1 0 -11.10 4.20 15 -1 0 -4.30 4.70 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8.10 15 9 0 4.80 11.10 -15 10 0 3.50 9.60 15 10 0 1.30 10.60 15 -10 0 12.20 11.00 -15 -10 0 -4.10 7.30 -15 10 0 16.80 9.90 15 11 0 -1.40 9.50 -15 11 0 -7.80 9.20 -15 -11 0 2.70 8.90 -15 -12 0 13.30 10.80 15 12 0 1.60 12.70 15 -12 0 -6.70 10.50 -15 12 0 15.50 11.00 -16 0 0 1050.09 58.59 -16 0 0 1025.50 58.59 16 0 0 1058.09 58.79 16 0 0 1074.99 60.89 -16 -1 0 241.18 16.70 -16 -1 0 197.18 15.40 16 -1 0 238.68 15.70 -16 1 0 228.08 16.00 16 1 0 225.58 17.70 16 -1 0 258.37 19.30 16 1 0 242.88 18.10 -16 1 0 207.58 16.50 16 2 0 12.70 6.80 16 -2 0 18.60 7.10 -16 2 0 16.10 5.50 -16 -2 0 8.30 4.50 -16 2 0 12.60 4.30 16 2 0 9.20 5.50 -16 -2 0 5.50 3.60 16 -2 0 10.60 3.90 16 3 0 301.37 20.90 16 3 0 308.27 23.30 -16 -3 0 281.57 20.30 16 -3 0 315.07 23.80 -16 3 0 294.17 20.00 -16 3 0 272.27 21.20 16 -3 0 275.57 16.60 -16 -3 0 276.27 17.80 16 4 0 287.87 19.70 -16 -4 0 233.78 19.10 -16 -4 0 264.07 16.30 16 -4 0 243.38 21.40 -16 4 0 244.78 18.90 16 4 0 229.58 21.40 -16 4 0 277.57 21.40 16 -5 0 6.10 7.80 -16 -5 0 1.10 5.00 16 5 0 11.00 9.10 -16 5 0 23.90 7.80 -16 5 0 17.10 6.60 16 5 0 18.00 6.40 16 -6 0 20.40 9.30 -16 6 0 18.60 8.20 16 6 0 8.10 10.10 -16 6 0 22.60 7.40 -16 -6 0 20.90 7.60 16 6 0 26.30 7.60 -16 7 0 154.18 17.10 16 7 0 100.29 17.80 -16 -7 0 155.38 17.60 16 -7 0 126.19 17.50 -16 7 0 115.69 16.70 16 8 0 9.90 10.40 -16 -8 0 2.70 6.80 16 -8 0 -2.60 8.60 -16 8 0 5.30 6.90 -16 8 0 1.60 7.00 16 9 0 32.00 13.60 -16 9 0 19.20 9.30 -16 -9 0 14.00 8.60 16 -9 0 48.40 13.20 -16 9 0 41.40 11.90 -16 -10 0 22.60 10.30 16 10 0 27.80 13.10 -16 10 0 13.10 11.00 -16 10 0 11.60 11.10 16 -10 0 19.00 12.10 -16 11 0 -12.50 7.50 16 11 0 9.90 12.60 -16 -11 0 -3.40 9.10 -16 12 0 59.59 15.80 16 12 0 31.70 15.50 -16 -12 0 54.19 15.80 17 0 0 -3.40 5.00 -17 0 0 4.20 3.70 17 0 0 6.50 5.30 -17 0 0 0.30 3.70 17 1 0 6.90 5.60 -17 1 0 -4.80 3.10 -17 -1 0 7.70 3.90 -17 1 0 -4.50 2.40 17 -1 0 -0.40 5.30 17 1 0 0.00 5.40 17 -1 0 -3.30 3.70 -17 -1 0 12.30 4.50 17 -2 0 -3.10 3.40 17 2 0 -9.20 5.30 -17 2 0 -2.80 3.10 17 -2 0 2.20 5.20 17 2 0 -3.60 4.70 -17 -2 0 -4.40 3.00 -17 2 0 -5.30 3.30 -17 -2 0 0.90 3.00 17 -3 0 8.20 6.90 -17 3 0 -1.00 4.50 17 3 0 -2.60 4.60 -17 3 0 -1.90 3.30 -17 -3 0 8.00 4.90 17 3 0 5.40 7.90 17 -3 0 -1.30 3.60 -17 -3 0 -1.50 3.00 -17 4 0 0.30 5.20 17 4 0 -4.70 4.40 17 -4 0 3.40 6.50 -17 -4 0 2.20 4.10 -17 -4 0 1.70 2.90 -17 4 0 -4.30 3.60 17 4 0 7.00 8.00 17 -5 0 5.30 7.80 -17 5 0 1.10 5.40 17 5 0 1.30 5.50 17 5 0 0.20 7.20 -17 5 0 -8.90 4.70 -17 -5 0 7.50 5.50 17 -6 0 -8.00 7.20 17 6 0 -0.60 5.70 -17 -6 0 0.10 5.10 -17 6 0 -2.00 5.50 -17 6 0 -4.10 5.90 17 6 0 7.20 11.00 -17 -7 0 2.70 6.20 -17 7 0 9.80 6.60 17 7 0 5.60 8.90 17 -7 0 11.70 9.00 -17 7 0 3.90 6.60 17 -8 0 -11.10 8.40 -17 8 0 -1.50 7.50 17 8 0 -7.70 8.80 -17 -8 0 -2.60 6.30 -17 8 0 -1.20 6.70 -17 -9 0 -0.50 7.30 17 -9 0 -9.80 9.00 -17 9 0 -11.40 6.80 17 9 0 -5.30 10.10 -17 9 0 -8.00 6.80 17 -10 0 1.00 10.90 -17 -10 0 -2.90 8.10 17 10 0 -8.60 8.50 -17 10 0 -10.20 8.70 17 11 0 20.00 13.10 -17 11 0 5.50 9.40 -17 -11 0 3.20 9.70 -17 12 0 19.60 12.50 17 12 0 14.60 14.00 -17 -12 0 6.70 11.40 18 0 0 3.60 5.50 -18 0 0 14.90 4.90 18 0 0 3.70 6.40 -18 0 0 10.30 4.50 18 -1 0 23.20 7.60 18 1 0 22.50 7.20 -18 -1 0 14.60 5.10 -18 -1 0 28.20 5.60 -18 1 0 25.60 6.00 18 1 0 22.20 7.60 -18 1 0 24.30 5.60 18 -1 0 31.30 6.40 18 2 0 -2.90 5.00 18 -2 0 -2.50 3.50 -18 -2 0 10.40 3.70 18 2 0 -10.50 5.70 -18 2 0 10.20 4.70 -18 -2 0 4.10 4.40 -18 2 0 0.70 3.90 18 -2 0 5.80 7.10 -18 3 0 45.70 7.80 18 -3 0 23.40 8.70 -18 -3 0 51.59 6.60 18 3 0 50.49 11.20 -18 3 0 52.09 9.60 18 3 0 23.70 7.50 -18 -3 0 47.20 8.20 -18 -4 0 952.00 56.39 -18 -4 0 922.51 52.59 -18 4 0 994.90 55.99 18 4 0 970.90 56.49 -18 4 0 972.30 58.09 18 4 0 917.11 59.09 18 -4 0 993.60 59.29 -18 5 0 32.40 9.50 -18 5 0 31.40 7.80 18 5 0 -2.10 8.90 18 -5 0 23.40 9.70 -18 -5 0 21.30 7.40 18 5 0 27.40 7.80 -18 6 0 -4.30 5.40 -18 -6 0 -2.60 5.40 18 -6 0 -0.80 6.60 18 6 0 8.50 10.70 -18 6 0 -0.10 6.60 18 6 0 -0.30 6.00 -18 -7 0 68.69 11.90 -18 7 0 92.89 15.20 18 7 0 60.29 14.70 -18 7 0 59.09 12.20 18 -7 0 42.40 12.30 -18 -8 0 50.89 11.70 18 -8 0 19.00 12.00 18 8 0 36.90 13.90 -18 8 0 67.29 14.90 -18 8 0 33.00 10.30 -18 9 0 7.10 8.50 18 9 0 -2.50 10.90 -18 -9 0 10.00 8.80 -18 9 0 4.00 8.80 18 -9 0 11.20 10.80 18 10 0 0.70 13.00 -18 -10 0 2.60 8.20 -18 10 0 1.50 9.40 18 -10 0 -4.00 10.60 -18 11 0 -4.80 9.30 -18 -11 0 -4.70 9.90 18 11 0 3.70 11.10 -19 0 0 -0.50 3.40 19 0 0 11.70 6.20 -19 0 0 -3.60 3.30 19 0 0 -3.50 5.30 -19 1 0 2.80 3.60 -19 -1 0 -0.10 3.90 19 -1 0 2.60 5.00 -19 -1 0 3.40 3.40 -19 1 0 2.70 4.00 19 -1 0 6.00 6.60 19 1 0 -14.80 5.50 19 1 0 5.20 5.70 19 2 0 2.60 7.60 -19 -2 0 1.00 3.70 19 2 0 -2.90 5.30 -19 2 0 3.20 4.50 -19 2 0 1.70 3.40 19 -2 0 -8.50 5.00 -19 -2 0 -2.50 3.50 19 -2 0 1.40 4.10 19 3 0 8.70 6.30 -19 3 0 -2.10 4.00 -19 -3 0 -1.60 4.10 19 3 0 -10.50 6.80 19 -3 0 6.50 6.80 -19 3 0 2.40 4.30 -19 -3 0 0.40 3.30 -19 4 0 -5.40 4.60 -19 -4 0 -3.80 4.30 19 4 0 3.20 8.70 -19 4 0 5.10 5.90 19 -4 0 7.40 8.40 19 4 0 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6.70 -20 2 0 9.10 5.40 -20 -2 0 13.80 5.50 20 2 0 -0.90 7.70 -20 3 0 12.90 6.20 -20 3 0 23.10 6.60 20 3 0 24.40 8.30 20 -3 0 11.20 8.90 -20 -3 0 28.40 5.30 -20 -3 0 27.80 7.20 20 3 0 12.70 9.70 20 4 0 113.59 14.00 -20 -4 0 108.99 13.20 20 -4 0 87.59 15.00 -20 4 0 97.89 12.40 -20 4 0 98.89 14.10 20 4 0 60.39 13.30 20 5 0 53.39 10.10 20 -5 0 41.30 11.90 -20 5 0 59.79 10.60 20 5 0 31.90 12.10 -20 -5 0 29.20 8.30 -20 5 0 28.60 9.80 20 -6 0 1.20 8.80 -20 -6 0 -7.50 4.50 20 6 0 -8.10 9.90 -20 6 0 6.60 7.60 -20 6 0 0.90 5.80 20 6 0 -0.80 8.90 20 -7 0 43.00 12.70 -20 -7 0 65.49 12.50 20 7 0 17.50 12.70 -20 7 0 45.80 11.80 -20 7 0 44.80 10.60 -20 8 0 -7.40 6.10 -20 -8 0 -4.00 6.10 20 8 0 5.00 12.10 -20 8 0 5.20 7.30 20 -8 0 0.90 10.00 -20 9 0 51.09 14.60 20 9 0 69.29 19.30 -20 -9 0 41.70 12.80 20 -9 0 64.69 15.20 -20 10 0 23.10 11.40 20 10 0 21.50 15.40 20 -10 0 13.20 12.90 -20 -10 0 3.10 8.30 20 -11 0 20.60 13.00 20 11 0 -4.40 12.30 -20 -11 0 28.10 11.50 -20 11 0 0.10 10.90 -21 0 0 16.70 5.40 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26.50 13.60 -22 6 0 20.10 8.70 -22 6 0 40.60 11.00 -22 -7 0 134.39 17.30 -22 7 0 117.79 17.20 -22 7 0 129.09 19.80 22 7 0 87.89 18.50 22 -7 0 134.29 19.50 -22 8 0 287.37 29.80 -22 -8 0 201.78 23.20 22 8 0 184.68 26.30 22 -8 0 174.48 24.60 22 -9 0 95.39 19.80 -22 -9 0 141.19 19.30 -22 9 0 95.79 18.10 22 9 0 34.80 15.00 -22 10 0 21.30 12.40 22 -10 0 -4.90 11.70 22 10 0 1.60 13.50 -22 -10 0 35.60 12.40 -22 11 0 0.10 11.20 22 -11 0 -17.60 11.60 -22 -11 0 -18.10 9.30 22 11 0 6.40 12.90 -23 0 0 16.40 5.90 -23 0 0 28.80 6.90 23 0 0 32.20 8.70 23 0 0 13.90 8.90 -23 -1 0 2.00 4.30 -23 1 0 1.60 5.10 23 1 0 2.90 7.70 23 1 0 4.60 8.10 -23 -1 0 4.10 4.80 23 -1 0 -9.10 6.80 -23 1 0 -0.50 4.50 23 2 0 -9.40 8.20 23 -2 0 -2.30 7.50 23 2 0 -5.90 6.80 -23 2 0 2.90 4.60 -23 -2 0 -0.20 4.00 -23 2 0 -0.50 4.40 -23 -2 0 1.90 5.20 23 -3 0 -2.00 7.30 -23 -3 0 -2.20 4.90 -23 3 0 12.80 6.60 23 3 0 -3.20 6.40 23 3 0 8.60 9.70 -23 3 0 -1.90 4.60 23 -4 0 -6.40 7.70 -23 -4 0 -7.60 4.10 23 4 0 1.50 8.90 -23 4 0 1.30 5.70 -23 4 0 -2.50 5.80 23 4 0 -0.50 6.90 23 -5 0 0.00 9.30 23 5 0 -10.80 9.40 23 5 0 -3.20 6.00 -23 -5 0 0.10 5.70 -23 5 0 -11.50 5.40 -23 5 0 -1.80 5.60 23 6 0 -9.50 10.30 23 -6 0 -9.10 8.70 -23 6 0 7.00 7.60 -23 -6 0 4.40 6.40 -23 6 0 -5.60 5.70 -23 -7 0 6.90 7.10 23 7 0 -10.30 10.30 23 -7 0 20.20 12.40 -23 7 0 3.50 7.50 -23 7 0 22.20 9.10 -23 -8 0 6.00 7.30 23 -8 0 -4.40 10.80 23 8 0 20.10 14.20 -23 8 0 10.60 8.70 -23 9 0 -10.50 8.50 23 -9 0 -7.00 9.30 -23 -9 0 -1.10 8.00 23 9 0 9.50 15.00 23 10 0 -15.70 12.00 -23 -10 0 8.50 9.50 23 -10 0 -4.70 12.50 -23 10 0 2.80 9.50 -24 0 0 3025.50 164.38 -24 0 0 3127.69 164.58 24 0 0 2966.40 167.48 24 0 0 3087.59 164.38 -24 -1 0 79.29 11.50 24 -1 0 76.99 13.70 -24 1 0 67.89 11.40 24 1 0 70.89 13.00 -24 1 0 61.09 10.20 -24 -1 0 78.29 10.50 24 1 0 56.89 12.70 -24 2 0 60.49 10.10 -24 2 0 64.89 11.10 24 2 0 60.39 13.00 -24 -2 0 44.80 9.50 24 2 0 47.20 10.90 24 -2 0 41.30 11.90 -24 -2 0 63.49 9.20 -24 3 0 141.39 15.50 -24 3 0 137.59 16.90 24 3 0 148.59 19.30 24 3 0 134.69 17.50 24 -3 0 121.09 17.50 -24 -3 0 125.59 15.50 -24 -4 0 211.78 18.60 24 4 0 206.88 21.60 24 4 0 208.78 24.20 24 -4 0 191.08 23.50 -24 4 0 184.78 21.90 -24 4 0 198.28 18.10 24 5 0 18.70 13.10 -24 5 0 28.80 8.30 -24 -5 0 26.10 8.40 24 5 0 15.30 8.70 -24 5 0 10.60 8.90 24 -5 0 17.10 11.30 24 -6 0 -1.20 8.60 -24 6 0 -1.10 7.20 24 6 0 25.20 13.80 -24 -6 0 -3.90 5.50 -24 6 0 -5.80 6.00 24 -7 0 31.20 12.70 -24 7 0 38.50 12.70 -24 -7 0 28.70 10.60 24 7 0 14.30 13.00 -24 7 0 25.00 9.90 24 -8 0 0.40 11.10 24 8 0 30.90 15.00 -24 8 0 -4.80 8.30 -24 -8 0 2.70 7.40 -24 -9 0 0.60 7.60 24 -9 0 15.90 12.70 -24 9 0 22.50 12.10 24 9 0 23.00 16.50 24 -10 0 -20.20 10.60 24 10 0 2.90 15.20 -24 10 0 -7.30 9.30 -24 -10 0 -7.20 7.80 25 0 0 37.20 11.40 -25 0 0 37.00 8.50 -25 0 0 33.90 7.50 -25 1 0 -0.20 4.90 -25 -1 0 -7.10 4.30 -25 -1 0 7.20 5.20 25 1 0 -4.30 8.00 25 -1 0 -2.30 7.00 -25 1 0 3.60 4.60 25 1 0 -0.80 7.80 -25 2 0 2.90 5.50 -25 2 0 3.60 4.70 25 -2 0 15.40 9.00 25 2 0 2.90 9.10 -25 -2 0 -5.60 5.00 25 2 0 -3.40 7.40 -25 -3 0 4.20 5.90 25 -3 0 7.90 10.00 25 3 0 24.00 11.30 -25 3 0 -2.30 4.60 25 3 0 1.80 7.80 -25 3 0 2.70 5.80 -25 4 0 1.70 5.60 25 -4 0 18.20 9.50 25 4 0 16.90 11.60 -25 -4 0 0.80 5.60 -25 4 0 -3.00 6.10 25 4 0 10.40 8.00 25 -5 0 1.00 10.30 25 5 0 -10.30 11.50 -25 -5 0 -4.60 5.30 25 5 0 5.40 7.90 -25 5 0 7.40 5.90 -25 5 0 6.60 7.50 -25 6 0 0.50 6.50 -25 -6 0 4.90 6.70 25 -6 0 11.60 11.50 -25 6 0 0.20 8.20 25 6 0 24.20 13.70 25 -7 0 13.20 13.10 -25 7 0 4.10 8.20 -25 -7 0 -5.70 6.10 25 7 0 -4.80 12.20 25 8 0 8.70 13.40 25 -8 0 1.30 9.90 -25 -8 0 -8.50 7.20 -25 8 0 -1.10 8.80 -25 9 0 7.90 10.50 -25 -9 0 -8.30 7.60 25 -9 0 9.60 12.70 25 9 0 2.90 14.70 25 10 0 -5.80 15.40 -25 -10 0 9.40 9.70 25 -10 0 -6.10 11.40 -25 10 0 10.30 11.80 26 0 0 1462.35 85.29 -26 0 0 1440.86 81.79 -26 0 0 1412.46 81.49 -26 1 0 62.29 10.30 26 1 0 33.10 11.50 -26 -1 0 55.09 10.20 -26 1 0 65.29 11.70 26 -1 0 78.39 13.30 26 1 0 56.19 13.60 -26 -1 0 72.69 11.00 26 2 0 35.20 10.60 -26 -2 0 12.50 6.90 26 -2 0 32.80 11.10 -26 2 0 21.40 7.40 -26 2 0 13.00 6.90 26 2 0 20.00 10.70 -26 3 0 846.62 54.49 -26 -3 0 847.32 53.59 26 3 0 878.51 56.09 26 -3 0 927.91 58.39 -26 3 0 835.62 52.49 26 3 0 884.81 55.79 26 -4 0 115.29 17.60 -26 -4 0 95.09 14.30 26 4 0 85.99 17.30 -26 4 0 114.89 14.80 -26 4 0 117.29 17.50 26 4 0 119.79 16.60 26 5 0 27.50 10.10 -26 5 0 17.30 7.60 -26 5 0 0.30 7.20 26 -5 0 9.90 10.40 -26 -5 0 6.90 6.90 26 5 0 1.60 11.80 -26 6 0 -0.70 7.00 26 -6 0 -8.40 8.70 -26 -6 0 -1.00 6.30 26 6 0 12.40 12.50 -26 6 0 -5.00 7.60 -26 7 0 301.17 31.60 26 -7 0 233.98 28.40 26 7 0 193.88 30.10 -26 -7 0 301.07 25.00 -26 8 0 21.00 11.60 -26 -8 0 8.40 8.50 26 8 0 7.10 12.00 26 -8 0 29.80 13.70 -26 -9 0 26.40 11.10 26 -9 0 30.50 13.90 26 9 0 49.90 20.00 -26 9 0 35.90 15.10 26 10 0 34.00 20.10 -26 -10 0 -20.30 7.20 26 -10 0 10.50 14.60 -26 10 0 8.30 11.40 -27 0 0 16.20 6.40 -27 0 0 14.80 6.10 27 0 0 3.50 9.00 -27 1 0 -2.30 5.10 27 -1 0 9.70 9.40 -27 -1 0 1.20 4.80 27 1 0 -5.80 8.70 -27 -1 0 -1.10 4.80 -27 1 0 2.80 5.00 -27 2 0 2.90 6.30 27 2 0 3.60 7.40 -27 2 0 -3.80 4.50 -27 -2 0 1.70 5.60 27 2 0 16.90 9.90 27 -2 0 -5.00 7.70 27 -3 0 -3.20 9.60 27 3 0 4.30 10.00 -27 -3 0 0.20 6.00 -27 3 0 2.50 6.00 -27 3 0 4.30 6.30 27 3 0 4.00 8.80 -27 -4 0 -6.50 5.10 27 -4 0 -9.70 9.60 27 4 0 3.20 12.00 -27 4 0 10.20 7.00 27 4 0 -0.70 8.50 -27 4 0 2.90 7.00 -27 5 0 4.00 7.60 -27 5 0 0.50 6.90 -27 -5 0 -2.80 5.40 27 5 0 -8.20 10.40 27 5 0 2.80 9.30 27 -5 0 3.20 10.90 -27 -6 0 9.00 7.60 27 6 0 30.00 14.70 -27 6 0 14.50 10.00 27 -6 0 3.10 12.00 -27 7 0 13.90 9.90 27 -7 0 16.30 11.80 -27 -7 0 7.70 8.10 27 7 0 12.90 13.70 -27 8 0 11.40 10.60 -27 -8 0 0.50 7.20 27 8 0 8.90 14.30 27 -8 0 -11.70 12.30 -27 -9 0 4.80 9.20 27 -9 0 -14.60 12.60 -27 9 0 8.60 11.50 27 9 0 -8.50 14.20 -28 0 0 56.59 10.50 -28 0 0 52.39 10.20 28 0 0 60.79 13.70 -28 1 0 139.89 16.90 -28 -1 0 108.49 14.50 28 1 0 127.29 19.00 28 -1 0 110.69 18.20 -28 1 0 117.49 14.80 -28 2 0 -2.10 6.30 28 -2 0 -7.20 7.30 -28 -2 0 -1.20 5.90 28 2 0 -5.80 8.90 28 2 0 7.30 9.40 -28 2 0 -6.00 4.80 28 3 0 234.98 26.00 -28 3 0 296.97 28.40 -28 3 0 278.77 22.50 28 -3 0 263.47 28.40 -28 -3 0 253.77 24.90 28 3 0 300.57 29.30 28 4 0 -17.00 7.90 28 4 0 -14.00 11.30 -28 4 0 -3.40 7.30 -28 -4 0 -1.10 6.50 -28 4 0 9.20 7.20 28 -4 0 1.80 11.70 28 -5 0 24.00 13.10 -28 -5 0 17.00 8.40 -28 5 0 6.60 7.20 -28 5 0 31.20 10.40 28 5 0 7.00 13.60 28 -6 0 8.20 11.50 -28 -6 0 2.90 7.00 28 6 0 -4.80 11.30 -28 6 0 -11.60 7.20 -28 -7 0 63.29 13.40 28 7 0 30.60 16.30 28 -7 0 82.99 19.60 -28 7 0 72.59 16.50 -28 -8 0 2.30 8.40 28 -8 0 16.70 12.20 -28 8 0 0.90 8.40 28 8 0 4.20 13.50 -28 9 0 14.60 12.40 28 9 0 -8.70 16.50 -28 -9 0 10.80 9.60 28 -9 0 22.10 15.30 -29 0 0 -2.90 5.70 29 0 0 3.20 10.20 -29 0 0 5.80 6.40 29 1 0 3.50 9.00 29 -1 0 -9.90 8.10 -29 1 0 -0.80 5.20 -29 -1 0 2.80 5.60 -29 1 0 7.90 5.90 29 2 0 -12.50 9.10 -29 2 0 -4.30 5.40 29 -2 0 3.40 8.80 -29 -2 0 -0.30 5.80 -29 2 0 -7.60 5.40 29 3 0 -2.10 9.10 29 3 0 4.50 12.10 -29 -3 0 2.80 6.50 29 -3 0 8.40 10.40 -29 3 0 3.50 6.80 -29 3 0 8.40 6.00 29 -4 0 5.70 11.00 -29 -4 0 -11.30 5.40 -29 4 0 -3.10 7.00 29 4 0 3.30 9.80 -29 4 0 -2.60 6.70 29 4 0 -9.50 12.40 29 -5 0 1.60 10.80 29 5 0 30.10 14.60 -29 5 0 0.80 6.80 -29 -5 0 -0.50 6.60 -29 5 0 12.50 9.00 29 6 0 -2.10 12.40 29 -6 0 -6.20 11.20 -29 6 0 5.80 8.80 -29 -6 0 0.90 7.00 -29 7 0 -0.90 8.30 -29 -7 0 -5.00 8.00 29 -7 0 19.50 13.90 29 7 0 11.70 14.10 -29 8 0 8.50 9.90 29 8 0 5.30 14.80 -29 -8 0 -8.20 6.80 29 -8 0 17.80 14.40 -29 9 0 -21.00 9.00 -29 -9 0 -8.50 7.60 29 -9 0 -14.20 13.20 29 9 0 1.70 17.60 30 0 0 19.30 11.50 -30 0 0 38.10 9.40 -30 0 0 41.40 9.40 -30 1 0 212.38 23.20 30 1 0 203.98 24.70 -30 1 0 218.58 21.10 30 -1 0 196.88 24.50 -30 -1 0 193.18 20.70 30 -2 0 8.90 8.80 30 2 0 1.30 10.20 -30 -2 0 -3.70 6.40 -30 2 0 -3.40 5.40 -30 2 0 5.80 6.20 -30 3 0 20.30 8.40 30 3 0 21.30 14.20 -30 3 0 30.50 10.30 -30 -3 0 21.60 8.40 30 3 0 18.60 12.20 30 -3 0 29.30 13.00 -30 4 0 11.00 8.50 30 4 0 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8.90 6.60 -10 -4 -3 21.20 4.40 10 5 3 82.39 13.50 10 5 3 93.09 9.20 -10 -5 3 81.19 7.00 10 -5 -3 90.69 11.60 -10 5 -3 93.59 10.70 -10 5 -3 94.59 12.50 -10 -5 3 74.49 10.50 10 5 -3 94.89 11.10 -10 5 3 75.49 11.10 -10 -5 -3 84.19 8.80 10 5 -3 77.49 13.00 10 -5 3 109.79 13.10 -10 5 3 59.29 10.00 -10 -5 -3 75.89 10.90 10 -5 3 85.39 8.90 -10 5 3 78.69 7.30 10 -6 -3 305.87 22.50 -10 6 -3 274.87 21.10 -10 -6 3 293.67 18.10 -10 -6 3 278.07 22.00 10 6 3 279.57 24.50 10 6 3 290.07 19.90 -10 6 -3 286.47 22.90 10 -6 3 300.47 20.00 -10 6 3 292.77 23.00 -10 6 3 286.17 18.80 -10 6 3 306.87 22.70 10 -6 3 327.37 24.30 10 6 -3 279.47 21.60 10 6 -3 270.97 24.60 -10 -6 -3 300.67 19.70 -10 -6 -3 282.47 22.60 -10 7 -3 0.20 5.60 10 -7 -3 -9.80 5.30 -10 -7 3 -7.70 4.60 10 7 3 -11.60 6.30 -10 7 -3 4.80 6.20 -10 -7 -3 1.10 5.90 10 -7 3 0.80 5.30 -10 7 3 7.00 6.40 -10 -7 -3 9.20 4.90 -10 7 3 -1.10 6.40 10 7 -3 -2.90 8.00 10 7 -3 0.80 5.30 10 -7 3 -3.70 6.80 10 8 3 -7.50 8.00 -10 8 -3 14.50 8.00 -10 -8 3 -2.70 5.80 -10 8 -3 1.50 5.80 10 -8 -3 -6.60 6.40 -10 8 3 8.50 6.70 10 8 -3 -2.00 8.10 -10 -8 -3 8.40 7.20 -10 -8 -3 4.50 5.20 10 8 -3 -0.10 6.50 -10 8 3 1.00 5.90 10 -8 3 -4.30 6.70 -10 9 -3 -0.30 7.10 10 -9 -3 7.00 6.80 -10 9 -3 10.70 7.10 -10 -9 3 -5.40 6.10 10 9 3 9.00 8.60 -10 -9 -3 -6.90 6.60 -10 9 3 -2.00 7.30 10 9 -3 -11.40 7.60 10 -9 3 -1.20 7.10 -10 9 3 -9.20 5.40 -10 -10 3 107.59 17.10 -10 10 -3 98.29 16.00 10 10 3 60.69 16.70 -10 10 -3 79.39 15.60 10 -10 -3 86.29 15.50 -10 -10 -3 113.59 18.00 10 -10 3 70.89 14.60 10 10 -3 60.29 15.40 -10 10 3 118.99 18.20 -10 -11 3 -8.00 8.40 10 -11 -3 7.70 10.00 -10 11 -3 -0.70 8.20 10 11 3 20.50 11.70 10 11 -3 11.50 11.70 -10 11 3 5.30 9.00 -10 -11 -3 1.10 8.80 10 -12 -3 46.50 13.90 -10 -12 3 73.39 17.10 10 12 3 62.49 16.80 -10 -12 -3 79.49 18.10 -10 12 3 87.89 18.80 10 -12 3 83.59 16.60 10 12 -3 87.19 19.00 -11 0 3 -0.80 2.30 11 0 3 -0.40 3.20 11 0 -3 0.50 3.40 -11 0 3 4.80 2.90 11 0 -3 -0.10 3.30 -11 0 -3 2.20 2.60 -11 0 -3 -1.00 2.10 11 0 3 1.70 3.40 11 -1 -3 14.80 5.10 11 1 3 17.50 5.40 -11 1 -3 16.90 3.50 -11 -1 3 20.90 3.40 -11 -1 3 18.10 4.40 11 -1 -3 20.60 3.40 11 1 3 20.70 4.70 -11 1 -3 20.10 4.70 11 -1 3 23.10 5.60 -11 -1 -3 12.60 3.60 -11 1 3 24.60 4.80 11 1 -3 17.60 4.80 -11 -1 -3 19.80 3.80 -11 1 3 16.90 4.20 11 -1 3 18.90 4.20 11 1 -3 11.50 5.10 -11 2 -3 94.39 9.50 11 2 3 86.39 8.40 -11 -2 3 78.69 6.00 11 2 3 90.99 10.70 11 -2 -3 72.49 9.40 -11 -2 3 72.09 8.20 -11 2 -3 82.79 7.20 -11 -2 -3 93.79 9.10 11 -2 3 81.69 10.00 -11 2 3 87.79 9.60 11 2 -3 90.79 9.80 -11 2 3 78.99 8.60 11 -2 3 73.39 6.90 11 2 -3 97.99 11.10 -11 -2 -3 90.69 7.30 -11 -3 3 0.60 1.60 11 3 3 -1.00 2.80 11 3 3 1.20 4.40 -11 -3 3 -0.60 3.30 -11 3 -3 6.20 3.80 -11 3 -3 1.70 2.80 11 -3 -3 3.00 4.30 11 -3 3 3.20 4.60 11 3 -3 5.10 5.30 -11 3 3 -8.00 3.00 11 3 -3 -6.50 3.00 -11 -3 -3 5.70 3.00 -11 -3 -3 -3.40 3.00 11 -3 3 -0.80 2.50 -11 3 3 6.10 3.80 11 4 3 185.18 13.10 11 -4 -3 180.58 15.70 11 4 3 163.78 17.60 11 -4 -3 170.28 10.20 -11 -4 3 193.88 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146.09 16.30 -13 -3 3 146.99 12.80 13 -3 3 164.08 15.80 -13 3 3 147.89 12.90 -13 -3 -3 144.09 11.20 -13 -3 -3 161.68 13.00 -13 3 3 173.38 15.90 13 3 -3 157.38 13.60 13 -3 3 143.69 10.60 13 3 -3 132.09 15.40 13 4 3 122.39 10.50 13 4 3 120.59 15.30 -13 4 -3 127.59 12.10 -13 -4 3 134.69 13.50 13 -4 -3 111.49 14.00 -13 -4 3 118.59 8.10 -13 4 -3 119.59 13.40 -13 4 3 117.59 13.60 13 -4 3 104.19 9.10 13 4 -3 110.79 12.60 -13 -4 -3 141.29 13.60 13 4 -3 118.29 15.50 -13 4 3 99.99 12.00 13 -4 3 118.09 14.50 -13 -4 -3 115.49 9.80 -13 5 -3 115.79 12.20 13 5 3 91.39 14.40 -13 5 -3 71.99 11.80 -13 -5 3 106.09 8.20 -13 -5 3 108.69 12.40 13 5 3 105.59 10.50 13 -5 -3 111.49 13.80 13 5 -3 98.09 15.20 13 5 -3 91.59 11.80 -13 5 3 96.99 12.00 -13 5 3 51.09 11.00 13 -5 3 107.79 9.00 13 -5 3 91.09 13.10 -13 -5 -3 102.89 12.90 -13 -5 -3 104.89 10.00 -13 6 -3 15.20 7.30 13 6 3 15.10 6.80 -13 -6 3 -4.40 5.30 13 -6 -3 1.60 7.30 13 6 3 -4.10 8.10 -13 6 -3 11.10 5.90 13 -6 3 -3.40 6.60 -13 -6 -3 13.60 4.90 13 6 -3 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142.99 17.50 14 6 -3 116.89 17.90 -14 -6 -3 165.58 12.90 -14 6 3 133.39 15.90 -14 -6 -3 182.08 18.50 14 6 -3 160.18 17.00 -14 7 -3 181.28 21.00 14 7 3 170.98 22.70 14 -7 -3 183.58 20.70 -14 -7 3 227.98 19.80 -14 7 -3 191.98 19.40 -14 -7 -3 185.18 20.40 -14 7 3 180.88 21.00 14 -7 3 208.98 21.80 14 7 -3 218.88 25.40 14 7 -3 249.88 19.70 -14 7 3 196.48 20.90 -14 -8 3 69.69 12.80 14 8 3 43.90 15.10 -14 8 -3 58.69 11.80 14 -8 -3 50.99 12.70 -14 8 -3 51.99 11.70 -14 -8 -3 48.30 12.10 14 8 -3 43.30 12.70 -14 8 3 52.59 13.00 -14 8 3 61.99 12.20 14 -8 3 63.09 13.40 -14 9 -3 3.80 7.50 -14 -9 3 10.10 8.00 -14 9 -3 12.70 9.00 14 9 3 16.10 9.70 14 -9 -3 -0.30 8.50 -14 -9 -3 -7.50 7.30 14 9 -3 -8.20 9.10 -14 9 3 26.00 9.90 -14 9 3 7.20 6.80 14 -9 3 0.80 8.70 14 10 3 74.79 17.70 -14 10 -3 80.79 16.50 -14 -10 3 93.99 16.70 -14 -10 -3 104.79 17.50 14 -10 3 98.89 17.50 -14 10 3 89.59 16.90 -14 10 3 116.89 19.10 14 10 -3 64.09 16.50 -14 11 -3 -1.50 8.80 14 -11 -3 9.20 10.90 14 11 3 -5.50 10.40 -14 -11 3 2.20 8.90 14 11 -3 15.30 11.40 14 -11 3 -5.60 10.10 -14 -11 -3 5.70 10.70 -14 11 3 11.00 10.50 -14 12 -3 6.50 11.30 -14 -12 3 -5.10 9.00 14 12 3 9.20 13.90 14 -12 -3 25.90 12.00 -14 12 3 -4.30 9.90 14 12 -3 18.10 12.60 -14 -12 -3 15.30 11.60 -15 0 -3 1.70 2.90 -15 0 3 2.10 3.10 -15 0 3 -3.30 2.80 15 0 -3 -1.50 4.40 15 0 3 7.10 4.70 15 0 3 2.00 4.10 -15 0 -3 2.50 3.00 15 0 -3 2.50 3.90 -15 -1 3 536.65 31.60 -15 -1 3 514.45 29.90 15 -1 -3 536.55 33.60 -15 1 -3 502.65 30.20 -15 1 -3 495.65 31.50 15 1 3 547.35 32.40 15 1 3 541.95 32.70 15 -1 -3 503.25 29.50 15 -1 3 571.44 33.70 -15 1 3 490.05 30.90 15 1 -3 520.75 31.90 15 1 -3 488.35 32.60 15 -1 3 523.75 30.50 -15 -1 -3 521.55 30.70 -15 -1 -3 486.55 30.70 -15 1 3 535.15 31.60 15 2 3 31.50 6.90 -15 -2 3 47.80 7.30 15 -2 -3 36.00 4.00 -15 2 -3 48.20 8.10 15 -2 -3 25.30 7.30 15 2 3 56.29 9.80 -15 2 -3 35.60 5.60 -15 -2 3 43.00 5.10 -15 2 3 46.50 7.90 -15 2 3 33.60 6.40 15 2 -3 29.80 7.00 -15 -2 -3 36.40 5.50 15 -2 3 40.90 5.90 15 -2 3 43.80 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82.49 12.60 16 6 -3 74.99 12.10 -16 6 3 72.19 12.70 -16 7 -3 -2.00 5.80 16 7 3 -11.50 7.90 -16 -7 3 3.90 6.10 16 -7 -3 5.50 8.30 -16 7 -3 -1.80 6.50 -16 -7 -3 -2.80 5.50 16 -7 3 2.40 7.80 16 7 -3 -7.10 6.30 16 7 -3 0.60 10.50 -16 7 3 -0.10 6.70 -16 7 3 -4.60 6.50 -16 -8 3 7.40 7.10 16 -8 -3 10.20 9.20 -16 8 -3 6.90 7.30 -16 8 -3 17.10 7.90 16 8 3 -1.30 10.40 -16 -8 -3 7.60 7.50 16 8 -3 20.40 11.00 16 -8 3 6.90 8.40 -16 8 3 9.20 8.30 -16 8 3 6.80 8.00 16 -9 -3 103.29 16.30 -16 -9 3 123.69 17.50 -16 9 -3 40.00 12.20 16 9 3 78.59 18.60 -16 9 3 51.89 13.70 16 -9 3 67.59 15.00 16 9 -3 63.99 17.50 -16 9 3 103.09 16.70 -16 -9 -3 105.59 16.70 -16 10 -3 29.40 11.60 16 -10 -3 13.80 11.10 -16 -10 3 27.60 10.90 16 10 3 10.90 12.00 -16 10 3 5.60 9.40 -16 -10 -3 15.40 10.40 -16 10 3 -13.20 9.10 16 -10 3 37.00 12.50 16 10 -3 4.30 10.60 16 11 3 -0.10 10.50 -16 -11 3 2.00 9.80 -16 11 -3 -4.50 10.40 -16 11 3 18.40 11.50 -16 -11 -3 18.20 12.10 16 -11 3 11.30 10.50 16 11 -3 11.10 12.00 -16 11 3 1.70 9.10 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328.77 21.90 14 -1 -10 289.37 22.50 14 1 10 318.67 21.60 -14 1 -10 301.57 18.40 -14 -1 10 302.87 21.00 14 1 10 310.27 22.50 -14 -1 -10 295.77 20.80 14 1 -10 330.77 19.00 -14 1 10 308.67 20.70 -14 1 10 321.47 21.40 14 -1 10 322.97 23.30 -14 1 10 269.87 18.40 14 -1 10 338.77 21.90 -14 -1 -10 323.57 19.80 14 1 -10 326.07 21.70 14 1 -10 284.37 22.80 -14 -2 10 2.50 3.80 14 2 10 21.50 5.30 -14 2 -10 14.60 3.30 14 -2 -10 14.70 7.00 -14 2 -10 5.00 4.90 14 2 10 15.20 7.20 14 2 -10 4.80 5.90 14 -2 10 7.80 6.70 -14 2 10 8.10 2.40 -14 2 10 13.00 4.70 -14 2 10 12.40 4.90 14 2 -10 10.30 6.70 14 -2 10 3.10 5.20 -14 -2 -10 7.30 3.90 14 2 -10 12.90 2.70 -14 -2 -10 11.30 4.40 -14 -3 10 246.78 18.10 14 3 10 210.38 19.80 14 -3 -10 235.68 19.20 -14 3 -10 241.48 15.00 -14 3 -10 249.18 19.10 14 3 10 227.08 16.10 14 3 -10 241.38 20.30 14 3 -10 200.88 19.00 -14 -3 -10 251.97 17.80 14 -3 10 238.48 21.00 -14 3 10 263.37 19.30 -14 3 10 230.78 18.50 14 -3 10 230.98 17.40 -14 -3 -10 219.88 16.80 14 4 10 8.40 5.90 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168.38 13.90 -8 3 12 167.68 11.90 8 3 -12 181.58 17.50 8 -3 12 168.48 14.30 8 4 12 172.98 17.60 -8 4 -12 171.18 16.30 -8 4 -12 157.88 10.80 -8 4 -12 167.88 17.60 -8 -4 12 170.18 13.40 8 4 12 195.88 16.50 8 -4 -12 156.18 15.80 8 -4 -12 146.69 14.20 8 4 -12 150.08 17.00 8 4 -12 175.98 18.30 -8 -4 -12 196.18 15.10 8 -4 12 183.98 14.60 -8 4 12 160.58 12.20 -8 4 12 185.48 17.80 -8 -5 12 53.49 8.30 8 5 12 59.79 11.00 -8 5 -12 38.50 8.10 8 -5 -12 59.89 10.30 8 -5 -12 50.89 8.50 -8 5 -12 43.10 6.00 8 5 12 32.20 9.60 -8 5 -12 47.30 9.80 8 -5 12 37.50 8.10 -8 -5 -12 47.10 8.30 -8 5 12 42.90 9.10 8 5 -12 29.80 11.00 8 5 -12 51.59 10.60 -8 5 12 48.40 7.10 8 -6 -12 11.30 7.60 8 6 12 -8.10 5.60 -8 6 -12 -3.00 5.60 -8 6 -12 -4.70 4.20 8 -6 -12 8.50 5.60 -8 -6 12 8.10 5.30 8 6 12 11.50 7.50 8 6 -12 4.40 7.10 8 -6 12 7.20 5.90 -8 6 12 7.60 6.70 -8 -6 -12 2.30 5.60 8 6 -12 24.10 9.70 8 7 12 312.07 28.60 8 7 12 399.86 30.20 -8 -7 12 350.26 25.50 -8 7 -12 378.96 27.30 -8 7 -12 354.16 28.90 8 -7 -12 354.76 28.50 -8 7 12 324.47 28.00 8 -7 12 335.57 26.10 -8 -7 -12 340.87 25.60 8 7 -12 392.36 29.90 8 7 -12 380.86 30.70 -8 8 -12 -6.50 6.00 -8 8 -12 10.90 9.10 -8 -8 12 3.70 5.70 8 -8 -12 -1.10 7.50 8 8 12 13.40 8.90 8 8 12 2.10 9.00 8 8 -12 -0.10 8.10 8 8 -12 -5.00 9.30 8 -8 12 6.60 7.60 -8 -8 -12 2.10 6.00 -8 8 12 1.40 6.80 8 9 12 -3.00 8.80 -8 9 -12 -8.40 8.90 -8 9 -12 7.60 8.10 8 -9 -12 -3.80 8.10 8 9 12 -0.20 9.40 -8 -9 12 12.20 8.00 -8 9 12 -5.60 9.00 8 9 -12 9.90 11.00 -8 -9 -12 7.40 7.20 8 9 -12 8.90 9.90 8 -9 12 -0.20 7.20 8 10 12 22.00 11.70 -8 10 -12 21.80 11.90 8 10 12 -2.20 10.70 8 -10 -12 -4.40 8.70 -8 10 -12 2.80 7.10 -8 -10 12 15.10 8.50 -8 -10 -12 -4.30 7.10 8 -10 12 -5.90 8.30 -8 10 12 8.00 9.80 8 10 -12 -6.70 9.40 8 10 -12 13.10 12.10 8 11 12 3.80 10.70 -8 11 -12 19.10 13.50 8 11 12 9.60 11.70 8 -11 -12 5.50 10.20 -8 -11 12 16.40 9.50 -8 11 12 18.40 11.60 8 11 -12 10.20 11.40 8 -12 -12 40.20 14.30 8 12 12 34.40 14.90 -8 -12 -12 21.20 11.70 8 -12 12 40.50 13.80 -8 12 12 55.79 17.40 8 12 -12 33.60 15.60 9 0 12 850.61 48.00 -9 0 12 791.82 46.30 -9 0 12 841.72 47.00 -9 0 -12 820.22 47.20 -9 0 -12 833.42 44.80 9 0 -12 852.11 46.00 9 0 -12 803.62 48.50 -9 0 -12 850.51 47.50 -9 -1 12 433.56 24.50 9 -1 -12 387.36 25.50 9 1 12 394.96 24.10 -9 -1 12 393.26 24.60 9 1 12 389.86 25.70 -9 1 -12 420.36 26.10 -9 1 -12 385.56 21.10 9 -1 -12 393.06 24.40 -9 1 -12 406.96 25.00 -9 -1 -12 362.26 23.10 9 1 -12 389.66 26.50 -9 1 12 403.06 23.30 9 -1 12 368.86 24.80 -9 1 12 378.06 24.70 -9 -1 -12 392.16 24.60 9 1 -12 392.76 22.40 -9 -2 12 0.80 3.10 9 -2 -12 4.00 5.00 9 -2 -12 7.70 4.60 9 2 12 -2.00 4.70 9 2 12 0.80 4.00 9 2 12 4.50 3.10 -9 2 -12 -3.00 4.20 -9 2 -12 -1.80 3.00 9 -2 12 -4.50 4.00 -9 2 12 -0.10 2.30 9 2 -12 -5.30 4.70 9 2 -12 -7.40 3.80 9 2 -12 1.90 1.60 -9 -2 -12 0.50 3.40 -9 2 12 1.00 3.60 9 -3 -12 13.80 5.60 -9 3 -12 5.90 6.20 9 3 12 20.80 6.20 9 -3 -12 22.80 6.40 9 3 12 0.40 5.10 9 3 12 8.10 2.80 -9 3 -12 12.60 5.10 -9 -3 12 19.90 5.20 -9 3 12 16.50 3.50 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12 13.10 6.00 10 3 -12 8.50 6.30 -10 -3 -12 6.70 4.70 -10 -3 -12 9.70 4.50 10 3 -12 15.70 7.30 10 -3 12 8.30 5.30 -10 4 -12 564.64 35.00 -10 4 -12 554.44 30.50 -10 -4 12 528.25 33.40 10 -4 -12 582.64 34.70 10 4 12 518.35 35.40 10 4 12 534.15 36.40 10 -4 -12 577.44 35.60 -10 4 -12 553.94 36.70 10 -4 12 514.85 33.70 -10 -4 -12 570.54 34.10 -10 4 12 533.35 31.00 10 4 -12 530.75 36.40 -10 4 12 561.24 35.80 10 4 -12 566.54 37.10 -10 5 -12 22.20 7.30 10 5 12 29.00 8.80 10 5 12 16.10 7.60 10 -5 -12 24.40 7.90 -10 -5 12 24.40 6.60 10 -5 -12 16.20 7.20 -10 5 -12 20.20 7.70 10 5 -12 39.60 11.20 -10 5 12 24.00 8.10 10 5 -12 17.60 8.50 -10 -5 -12 20.40 6.80 10 -5 12 29.20 7.50 10 -6 -12 5.80 6.80 -10 -6 12 3.80 5.20 10 -6 -12 11.90 6.60 -10 6 -12 2.20 5.70 10 6 12 -0.70 7.80 -10 6 -12 -1.10 6.60 10 6 12 -3.80 7.00 10 6 -12 10.70 8.80 10 6 -12 -2.40 6.90 10 -6 12 6.30 6.00 -10 -6 -12 23.50 7.10 -10 6 12 2.90 6.80 -10 7 -12 10.00 7.70 10 -7 -12 0.20 6.50 10 7 12 4.60 9.00 10 7 12 -5.40 7.70 10 -7 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3 12 15.50 3.60 11 -3 -12 3.50 5.30 -11 3 -12 13.80 5.60 11 3 12 23.70 8.00 -11 -3 12 23.10 5.90 11 -3 -12 14.60 6.00 -11 3 -12 30.30 7.90 11 3 -12 14.30 6.10 -11 3 12 22.50 6.20 -11 -3 -12 9.40 4.60 11 3 -12 27.20 8.50 -11 3 12 17.30 3.40 -11 -3 -12 19.00 5.50 11 -3 12 5.40 5.40 -11 4 -12 42.30 9.20 -11 4 -12 37.90 7.80 11 -4 -12 35.30 8.80 11 -4 -12 45.60 8.20 -11 -4 12 41.20 7.30 11 4 12 45.60 10.10 11 4 -12 43.40 10.60 11 -4 12 36.20 7.60 -11 -4 -12 45.10 8.30 -11 4 12 47.70 8.00 -11 -4 -12 39.60 7.50 -11 4 12 42.60 8.70 11 4 -12 36.60 9.80 11 5 12 145.99 18.50 11 5 12 158.38 17.10 11 -5 -12 117.29 15.30 -11 5 -12 124.49 15.70 -11 -5 12 145.59 14.60 -11 5 -12 146.49 17.70 11 -5 -12 156.18 15.60 11 5 -12 138.49 17.20 11 -5 12 127.39 14.20 -11 5 12 131.99 16.10 -11 -5 -12 173.38 14.40 -11 -5 -12 175.28 17.70 11 5 -12 151.88 19.20 11 6 12 17.10 9.20 -11 6 -12 17.10 7.90 11 -6 -12 14.60 7.50 11 -6 -12 17.80 7.00 -11 6 -12 6.80 6.10 11 6 12 13.70 8.70 -11 -6 12 14.70 6.60 11 -6 12 21.40 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25.60 21.70 7 12 14 17.00 12.70 7 12 14 -13.60 9.90 7 -12 -14 28.00 13.80 -7 12 -14 49.00 17.40 7 12 -14 15.50 12.40 -7 12 14 42.30 15.60 -8 0 -14 5.20 2.40 -8 0 14 1.90 3.10 -8 0 14 2.60 3.40 -8 0 -14 5.10 3.60 8 0 14 9.80 4.90 8 0 -14 3.60 3.30 8 0 -14 -2.80 4.10 -8 0 -14 8.10 4.30 -8 1 -14 137.99 12.20 8 1 14 161.58 11.60 8 1 14 129.09 13.70 -8 -1 14 162.98 12.80 8 -1 -14 149.88 12.20 -8 -1 14 149.39 11.70 -8 1 -14 146.19 13.60 8 -1 -14 140.89 14.20 8 -1 14 152.38 13.20 -8 -1 -14 157.88 12.00 -8 -1 -14 152.48 12.50 -8 1 14 127.99 11.00 8 1 -14 169.88 14.80 8 1 -14 141.49 10.30 -8 1 14 150.28 12.40 8 2 14 -2.70 3.80 8 2 14 4.40 5.70 8 2 14 6.40 3.40 8 -2 -14 -0.30 4.30 -8 -2 14 8.20 4.50 -8 -2 14 3.70 3.30 -8 2 -14 -7.60 4.20 8 -2 -14 1.80 4.50 -8 2 -14 7.10 4.00 -8 2 14 2.40 3.00 -8 -2 -14 8.70 4.20 8 2 -14 4.50 2.20 8 2 -14 11.40 6.10 8 -2 14 -0.60 4.20 -8 2 14 5.40 4.30 8 -3 -14 142.49 13.70 8 -3 -14 151.08 15.00 8 3 14 177.48 17.50 -8 3 -14 181.58 14.30 8 3 14 167.38 10.30 -8 -3 14 169.18 13.00 8 3 14 171.98 14.80 -8 3 -14 149.49 16.90 -8 -3 14 166.78 16.40 -8 3 14 146.19 11.50 8 3 -14 156.58 16.80 -8 3 14 153.38 15.40 8 -3 14 158.88 14.10 -8 -3 -14 157.68 13.80 8 3 -14 145.69 9.60 -8 4 -14 -2.20 3.80 -8 -4 14 -3.90 3.60 -8 4 -14 -9.10 4.70 8 4 14 1.10 5.30 8 4 14 -2.60 5.80 8 -4 -14 1.20 5.10 8 -4 -14 -0.70 4.70 -8 4 14 3.90 3.60 8 -4 14 6.20 5.30 8 4 -14 1.40 5.80 -8 4 14 0.90 5.30 8 4 -14 -4.80 5.60 -8 -4 -14 -2.30 4.60 8 -5 -14 5.70 5.50 8 5 14 16.20 8.40 -8 5 -14 18.60 6.30 -8 -5 14 25.20 6.20 8 -5 -14 5.40 6.70 -8 5 -14 15.30 7.40 8 5 14 16.80 7.90 8 5 -14 19.50 7.50 -8 5 14 17.00 5.20 8 -5 14 19.20 6.80 -8 -5 -14 30.10 7.30 8 5 -14 14.80 9.30 -8 5 14 17.30 7.50 -8 -6 14 29.10 7.20 8 -6 -14 30.40 9.40 -8 6 -14 42.30 11.10 8 6 14 53.69 12.20 8 6 14 39.00 10.60 8 -6 -14 54.39 8.80 -8 6 -14 27.00 7.80 8 6 -14 41.80 11.60 -8 6 14 57.59 11.50 8 6 -14 24.50 10.90 -8 -6 -14 43.50 9.40 8 -6 14 30.00 8.50 -8 7 -14 11.80 9.20 8 7 14 20.20 9.50 8 -7 -14 13.70 8.30 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13.20 8 -12 -14 3.70 11.60 -8 12 14 -6.50 10.80 8 12 -14 21.90 13.00 -8 -12 -14 2.80 9.20 8 -12 14 13.50 12.10 -9 0 -14 30.10 6.50 9 0 -14 39.30 5.90 -9 0 14 44.10 6.90 -9 0 -14 34.40 4.50 -9 0 -14 27.40 5.70 9 0 -14 42.80 8.30 9 0 14 47.70 8.30 -9 0 14 44.70 6.80 9 -1 -14 37.70 7.60 9 1 14 55.99 9.00 -9 1 -14 59.79 8.10 -9 -1 14 51.19 7.30 9 -1 -14 64.89 7.90 9 1 14 38.80 6.50 -9 1 -14 45.90 8.20 -9 -1 14 66.59 8.80 9 -1 14 54.49 8.70 -9 -1 -14 54.29 7.70 -9 -1 -14 48.90 6.20 9 1 -14 46.70 8.40 -9 -1 -14 43.60 6.50 9 1 -14 52.79 5.70 -9 1 14 53.69 6.80 -9 1 14 46.40 7.30 9 -2 -14 35.00 7.10 -9 -2 14 32.40 7.20 -9 -2 14 45.70 6.80 -9 2 -14 42.30 8.30 9 2 14 39.80 8.50 9 -2 -14 32.70 7.00 9 2 14 47.10 5.90 -9 2 -14 31.40 6.30 9 2 14 34.50 6.70 9 2 -14 42.80 4.30 9 2 -14 31.80 7.80 9 -2 14 51.79 8.70 -9 2 14 27.90 5.20 -9 2 14 46.60 7.70 -9 -2 -14 36.40 6.60 -9 3 -14 15.70 5.30 9 3 14 9.70 3.00 9 -3 -14 13.30 5.60 9 3 14 8.10 6.60 9 -3 -14 12.30 6.10 -9 -3 14 11.70 5.70 -9 -3 14 5.60 4.10 9 3 14 14.50 6.50 -9 3 -14 9.00 6.60 9 -3 14 11.00 6.00 9 3 -14 8.30 6.80 -9 -3 -14 0.90 4.20 9 3 -14 12.00 6.40 9 3 -14 8.80 1.90 -9 3 14 4.50 3.10 -9 3 14 11.00 6.00 -9 -4 14 -4.80 3.50 -9 4 -14 -0.80 4.30 9 4 14 -1.30 6.30 9 -4 -14 -3.10 5.50 9 4 14 4.50 6.30 -9 4 -14 0.60 5.60 9 -4 -14 3.90 5.20 9 4 -14 -4.00 6.30 9 4 -14 3.60 6.20 -9 -4 -14 4.50 4.60 9 -4 14 -2.80 5.10 -9 4 14 -1.00 3.00 -9 4 14 -1.40 5.10 -9 -5 14 228.18 16.80 9 5 14 196.18 21.70 9 -5 -14 190.78 19.40 -9 5 -14 180.38 20.40 -9 5 -14 174.88 18.40 9 -5 -14 206.28 17.00 9 5 14 198.18 20.20 -9 5 14 212.28 21.10 -9 -5 -14 208.68 17.40 9 -5 14 216.78 17.60 9 5 -14 197.38 21.40 9 5 -14 266.87 24.70 -9 -6 14 110.19 13.40 -9 6 -14 148.69 16.80 9 6 14 108.29 16.90 -9 6 -14 107.49 16.80 9 -6 -14 113.89 13.00 9 6 14 134.59 17.00 9 -6 -14 117.39 15.60 -9 -6 -14 166.98 16.20 -9 6 14 141.69 17.60 9 6 -14 128.99 17.60 9 -6 14 105.09 14.20 9 6 -14 141.99 19.30 9 7 14 49.70 12.90 -9 7 -14 26.10 8.80 -9 7 -14 28.60 10.10 -9 -7 14 25.50 7.40 9 7 14 21.20 9.90 9 -7 -14 27.10 9.50 9 7 -14 25.40 11.90 9 -7 14 31.10 9.10 -9 7 14 43.90 11.10 -9 -7 -14 32.30 8.40 9 7 -14 42.10 12.10 9 8 14 28.80 11.10 -9 8 -14 12.80 8.20 -9 -8 14 20.30 8.00 9 -8 -14 16.60 10.00 -9 8 -14 45.30 13.20 9 8 14 -0.70 9.30 9 8 -14 22.80 10.20 -9 -8 -14 28.80 8.40 -9 8 14 31.40 10.60 9 -8 14 36.10 9.90 9 8 -14 8.00 11.30 -9 -9 14 7.60 7.00 9 9 14 0.30 9.20 9 9 14 -9.90 8.80 -9 9 -14 2.90 8.90 9 -9 -14 13.80 10.20 -9 9 -14 -3.80 6.80 9 9 -14 -3.10 10.70 -9 -9 -14 8.20 7.90 9 -9 14 -1.10 7.60 9 9 -14 0.70 10.30 -9 9 14 9.80 10.00 -9 -10 14 18.60 8.90 9 10 14 10.90 10.90 9 10 14 8.90 11.10 -9 10 -14 21.80 10.10 -9 10 -14 13.40 12.50 9 -10 -14 6.30 11.00 -9 10 14 -0.10 10.60 9 10 -14 31.30 13.90 9 10 -14 5.80 10.10 -9 -10 -14 13.10 8.60 9 -11 -14 11.50 11.60 9 11 14 -2.00 9.60 -9 11 -14 -0.30 12.70 9 11 14 -1.70 10.10 -9 -11 14 -12.70 11.00 -9 11 14 -2.60 9.80 9 11 -14 -17.80 8.40 -9 -11 -14 10.60 9.60 9 12 14 21.70 13.40 9 -12 -14 3.30 12.90 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6.20 10 3 14 8.70 3.10 10 3 -14 4.30 7.00 -10 3 14 10.00 5.30 10 -3 14 7.40 5.60 -10 3 14 4.90 3.00 10 3 -14 -2.30 5.40 -10 -3 -14 8.60 4.80 -10 4 -14 -6.00 4.90 -10 4 -14 11.40 5.40 -10 -4 14 2.50 4.40 10 -4 -14 -4.60 5.30 10 -4 -14 -9.70 4.50 10 4 14 0.90 6.70 10 4 14 3.40 5.40 -10 -4 -14 3.80 4.90 -10 4 14 1.30 3.00 10 4 -14 -1.60 5.30 10 4 -14 5.40 8.00 -10 4 14 -2.80 4.40 10 -4 14 -6.10 4.60 -10 5 -14 24.00 8.30 10 -5 -14 16.20 7.90 -10 5 -14 27.20 7.30 -10 -5 14 24.10 6.50 10 5 14 29.10 10.20 10 5 14 17.80 8.10 10 -5 -14 28.90 7.80 10 5 -14 18.60 9.20 -10 5 14 45.50 10.00 10 -5 14 29.30 7.90 -10 -5 -14 21.10 6.90 10 5 -14 29.90 10.80 -10 6 -14 42.50 11.30 -10 -6 14 59.39 9.30 10 6 14 75.09 13.40 -10 6 -14 36.40 9.20 10 6 14 54.59 13.10 10 -6 -14 55.49 9.90 10 -6 -14 39.10 10.30 10 6 -14 64.89 13.90 -10 6 14 62.49 12.70 -10 -6 -14 58.79 10.40 10 -6 14 51.69 9.80 10 6 -14 78.69 15.50 -10 7 -14 -4.70 5.80 10 7 14 -9.80 7.20 10 -7 -14 -8.00 7.30 -10 7 -14 -8.10 5.50 10 7 14 -0.20 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49.40 12.70 14 -6 14 55.09 10.30 14 6 -14 24.50 12.00 14 -7 -14 11.10 7.90 14 7 14 42.40 14.30 -14 -7 14 19.60 7.50 -14 7 -14 10.50 7.40 14 -7 -14 26.60 9.20 -14 -7 -14 34.40 9.70 14 -7 14 33.90 11.70 -14 7 14 6.60 8.90 -14 -7 -14 23.50 8.20 14 7 -14 27.20 11.00 14 7 -14 29.30 13.60 14 -7 14 9.60 7.60 -14 8 -14 5.20 7.40 14 -8 -14 -8.40 7.80 -14 -8 14 3.10 6.20 14 8 14 -6.80 10.10 14 8 -14 -5.10 9.30 14 8 -14 13.90 12.50 -14 -8 -14 16.80 8.60 -14 8 14 11.10 8.90 -14 -8 -14 5.60 7.10 14 -8 14 16.00 10.00 14 -9 -14 5.80 10.00 14 9 14 -13.50 8.70 -14 -9 14 -11.30 6.00 -14 9 -14 -1.50 7.80 14 9 -14 1.50 12.10 -14 -9 -14 14.60 8.40 -14 -9 -14 -0.20 8.40 14 -9 14 8.50 11.10 -14 9 14 5.80 9.50 14 9 -14 17.00 11.00 14 -10 -14 21.20 12.90 -14 10 -14 23.60 11.20 -14 -10 14 14.30 9.80 14 10 14 19.20 12.10 -14 10 14 14.60 10.60 14 10 -14 8.10 14.00 14 10 -14 34.90 15.20 14 -10 14 19.90 13.90 -14 -10 -14 35.10 12.20 14 -11 -14 47.30 16.10 -14 11 -14 32.70 12.90 14 11 14 37.90 15.40 -14 -11 14 48.30 13.00 -14 11 14 46.20 17.10 -14 -11 -14 58.49 15.10 14 -11 14 52.89 17.80 14 11 -14 8.00 14.40 15 0 14 -11.30 5.20 -15 0 -14 -1.90 3.90 15 0 14 -6.10 5.10 15 0 -14 3.30 4.10 15 0 -14 2.20 6.60 -15 0 14 2.70 3.60 -15 0 14 -0.20 4.60 -15 0 -14 1.30 2.60 15 -1 -14 55.99 8.60 -15 -1 14 76.79 9.70 -15 -1 14 69.39 9.70 15 -1 -14 52.09 10.50 -15 1 -14 62.69 6.00 -15 1 -14 43.50 8.60 15 1 14 51.69 11.10 15 1 14 68.49 9.70 15 -1 14 47.60 10.10 -15 1 14 71.39 7.60 -15 -1 -14 63.99 7.70 15 -1 14 53.09 9.80 -15 -1 -14 50.29 8.80 -15 1 14 58.39 9.30 15 1 -14 44.60 9.70 15 1 -14 52.69 6.70 15 2 14 -2.50 5.80 -15 -2 14 8.60 5.10 15 2 14 2.50 4.50 15 -2 -14 1.50 6.70 15 -2 -14 6.00 4.90 -15 2 -14 2.00 4.60 15 2 -14 9.90 7.40 -15 -2 -14 2.20 4.60 -15 -2 -14 3.30 3.90 15 2 -14 -1.50 5.70 -15 2 14 1.80 4.80 15 -2 14 1.90 6.90 15 -2 14 2.50 6.30 -15 -3 14 61.69 9.80 15 -3 -14 43.10 9.60 15 -3 -14 81.09 13.00 15 3 14 60.59 12.50 -15 3 -14 68.79 11.70 -15 -3 -14 57.49 9.00 15 3 -14 75.29 12.70 -15 -3 -14 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-15 116.39 18.70 12 7 15 105.79 16.80 -12 -7 15 97.39 13.30 12 -7 -15 99.09 15.60 12 7 15 101.79 18.70 12 7 -15 114.59 18.50 12 7 -15 87.49 18.20 -12 -7 -15 83.69 14.60 -12 -7 -15 107.29 14.20 -12 7 15 108.39 17.10 12 -7 15 108.59 14.20 -12 -8 15 25.20 9.00 -12 8 -15 11.50 9.70 12 -8 -15 24.90 11.00 -12 8 -15 20.70 9.30 12 8 15 2.80 10.30 -12 -8 -15 31.00 10.50 12 -8 15 19.20 7.90 -12 8 15 8.50 9.90 -12 -8 -15 25.50 9.00 12 8 -15 16.70 12.90 12 8 -15 27.20 11.80 -12 9 -15 -19.40 7.90 12 9 15 -4.60 8.50 12 -9 -15 10.80 10.00 -12 -9 15 -3.80 6.80 -12 9 -15 -9.30 7.30 12 9 -15 4.30 10.50 -12 -9 -15 3.10 7.90 12 9 -15 -3.50 11.30 -12 -9 -15 -4.90 6.70 -12 9 15 19.50 10.60 12 10 15 11.60 12.50 12 -10 -15 15.30 11.60 -12 -10 15 17.30 9.40 -12 10 -15 7.30 9.00 12 -10 15 15.50 12.20 12 10 -15 8.70 12.30 -12 -10 -15 17.30 9.80 -12 10 15 -8.10 9.10 -12 -10 -15 17.10 10.80 12 10 -15 9.30 12.60 -12 11 -15 192.78 36.10 12 -11 -15 144.69 22.70 12 11 15 140.49 24.30 -12 -11 15 169.88 20.50 -12 11 15 193.08 27.30 12 11 -15 77.09 20.10 12 -11 15 180.88 25.30 -12 -11 -15 220.68 26.90 -13 0 15 1.10 4.00 -13 0 -15 -1.10 2.20 -13 0 -15 -3.70 3.60 13 0 -15 -4.80 5.10 -13 0 15 -3.50 2.80 13 0 15 1.70 5.70 13 0 15 -8.90 4.60 13 0 -15 3.50 3.70 13 -1 -15 17.60 6.00 -13 -1 15 27.90 6.20 -13 1 -15 26.80 3.50 13 1 15 35.80 7.30 13 -1 -15 19.50 7.40 13 1 15 30.70 9.00 -13 1 -15 28.20 6.60 -13 -1 15 29.70 6.80 13 -1 15 22.80 7.20 -13 -1 -15 35.30 7.10 13 1 -15 31.90 9.00 -13 1 15 29.60 5.30 -13 1 15 31.20 7.20 13 1 -15 32.10 5.00 13 -1 15 16.60 6.80 -13 -1 -15 24.20 4.80 13 2 15 67.79 8.80 13 -2 -15 70.89 10.10 13 -2 -15 75.29 11.90 -13 -2 15 82.19 11.00 13 2 15 64.59 11.20 -13 -2 15 65.89 9.70 -13 2 -15 62.89 10.80 -13 2 -15 76.59 10.40 -13 2 15 73.29 10.70 13 -2 15 68.99 10.70 -13 2 15 79.59 7.90 13 2 -15 67.99 12.00 13 -2 15 55.19 10.50 -13 -2 -15 88.99 10.60 -13 -2 -15 65.09 8.80 -13 -3 15 147.69 15.20 13 -3 -15 170.58 16.80 13 3 15 199.58 20.70 13 -3 -15 149.69 16.70 -13 3 -15 152.38 16.10 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10.70 -5 -2 -22 60.19 10.00 5 -3 -22 -8.00 4.80 5 3 22 -9.30 5.10 -5 3 -22 5.40 7.00 -5 -3 22 10.40 4.40 5 -3 -22 9.30 6.80 -5 -3 22 3.10 5.00 -5 3 -22 1.60 4.70 5 3 22 0.60 5.10 -5 -3 -22 2.30 5.80 -5 3 22 11.10 5.80 5 -3 22 4.10 5.60 5 3 -22 6.70 8.10 -5 3 22 4.70 5.70 5 3 -22 -2.50 3.20 -5 -4 22 2.20 6.20 5 4 22 7.90 6.50 -5 -4 22 8.60 4.60 -5 4 -22 3.40 7.20 5 -4 -22 -6.60 5.80 5 4 22 14.50 7.30 -5 4 -22 8.20 5.70 5 4 -22 -5.10 6.00 5 -4 22 1.80 6.20 -5 -4 -22 2.50 5.90 -5 4 22 2.20 6.50 -5 4 22 5.80 5.50 5 -5 -22 116.49 15.70 5 5 22 114.99 16.70 -5 5 -22 103.99 14.10 -5 5 -22 126.39 19.10 -5 -5 22 132.49 18.40 5 5 22 114.09 16.10 5 5 -22 124.79 18.40 -5 -5 -22 106.19 14.60 -5 5 22 131.29 17.40 5 -5 22 151.48 17.70 -5 5 22 126.99 15.20 -5 6 -22 19.80 11.30 -5 6 -22 23.20 7.60 5 6 22 24.50 10.10 5 -6 -22 27.20 9.00 5 6 22 47.30 11.40 -5 -6 22 19.00 8.40 -5 6 22 30.70 11.00 -5 -6 -22 34.60 9.90 5 6 -22 29.70 11.60 5 -6 22 18.10 8.30 -5 -7 22 -9.90 7.10 5 7 22 0.50 7.70 -5 7 -22 -3.20 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15.60 9.40 3 -5 -28 -2.10 7.60 3 5 28 3.50 7.70 -3 -5 28 9.70 8.00 3 5 -28 3.30 9.40 -3 5 28 6.40 8.20 3 -5 28 5.70 8.90 -3 -5 -28 0.90 7.10 -3 5 28 5.90 7.60 -3 -6 28 -2.10 7.70 3 6 28 -2.10 7.70 3 -6 -28 5.70 8.30 3 6 28 -3.00 7.60 -3 6 -28 -8.10 10.00 -3 -6 -28 -0.40 7.40 3 6 -28 4.30 11.60 3 -6 28 3.80 7.70 -3 6 28 1.60 8.00 -3 7 -28 6.30 11.80 3 7 28 9.70 8.60 3 -7 -28 24.00 10.60 -3 -7 28 33.90 13.70 3 7 28 30.30 12.30 3 7 -28 14.90 13.00 -3 7 28 22.30 11.80 3 -7 28 33.90 12.80 -3 -7 -28 28.40 11.30 3 -8 -28 14.90 10.70 -3 -8 28 2.50 10.20 3 8 28 -0.10 9.70 -3 8 -28 -16.30 11.80 3 8 28 -6.40 9.00 -3 8 28 -7.40 10.00 3 -8 28 9.40 10.50 3 8 -28 -8.90 11.80 -3 -8 -28 2.40 8.80 3 9 28 3.50 11.60 -3 -9 28 -4.50 11.70 3 -9 -28 0.00 10.20 -3 9 -28 -11.90 15.00 3 -9 28 -7.20 9.20 3 9 -28 36.20 16.80 -3 -9 -28 7.40 11.30 -3 9 28 29.80 13.30 -3 -10 28 -9.10 10.80 3 10 28 15.70 14.00 3 -10 -28 8.90 11.50 -3 10 -28 24.90 20.00 -3 10 28 26.10 15.40 3 10 -28 2.60 15.60 3 -10 28 23.80 13.60 -3 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-28 33.00 12.50 -4 4 28 18.90 9.00 -4 4 28 29.50 9.40 4 -4 28 40.60 11.20 4 5 28 6.90 7.90 4 -5 -28 2.20 7.90 -4 5 -28 14.20 6.40 -4 5 -28 -0.60 10.10 4 5 28 8.60 7.50 -4 -5 28 -0.30 6.60 -4 -5 -28 8.40 7.80 -4 5 28 0.60 6.60 -4 5 28 1.80 8.60 4 -5 28 17.90 9.10 4 5 -28 -4.70 9.10 4 6 28 9.70 9.10 -4 6 -28 -9.40 10.80 -4 -6 28 0.40 8.30 4 -6 -28 -1.00 7.50 4 6 28 3.30 9.30 4 6 -28 13.60 11.70 4 -6 28 0.60 8.40 -4 6 28 -4.40 7.40 -4 -6 -28 9.10 8.20 4 7 28 18.60 10.70 4 7 28 33.40 12.70 -4 -7 28 4.80 10.60 -4 7 -28 21.50 14.40 4 -7 -28 1.90 8.60 -4 7 28 11.90 10.50 4 7 -28 31.90 14.40 4 -7 28 8.30 9.20 -4 -7 -28 5.50 9.00 -4 8 -28 32.40 15.70 -4 -8 28 17.00 11.80 4 8 28 40.00 14.50 4 -8 -28 44.00 12.80 4 8 28 33.70 14.50 -4 -8 -28 7.50 10.30 -4 8 28 20.70 13.20 4 8 -28 42.20 16.20 4 -8 28 23.80 11.50 -4 9 -28 -20.40 12.90 -4 -9 28 11.00 11.50 4 -9 -28 0.20 10.90 4 9 28 9.60 12.70 -4 9 28 8.40 12.40 -4 -9 -28 -6.50 9.20 4 -9 28 15.10 12.30 4 9 -28 -1.60 14.30 4 -10 -28 -3.40 11.50 -4 10 -28 0.60 16.20 -4 -10 28 12.80 12.60 4 10 28 6.40 13.60 4 -10 28 16.50 11.80 -4 10 28 23.30 14.10 4 10 -28 10.20 17.70 -4 -10 -28 -4.10 10.70 -5 0 -28 2.60 6.00 5 0 -28 6.20 5.30 -5 0 -28 27.60 9.60 5 0 28 5.60 7.50 5 0 -28 12.60 9.00 -5 0 28 0.60 5.30 -5 0 28 22.90 7.80 -5 -1 28 88.69 11.60 -5 -1 28 51.09 11.60 5 -1 -28 80.79 11.60 -5 1 -28 105.59 13.50 5 1 28 66.69 12.70 5 -1 -28 88.39 14.50 -5 1 -28 60.69 13.30 -5 -1 -28 99.09 14.10 5 1 -28 68.49 10.10 -5 -1 -28 78.29 12.60 5 1 -28 90.59 16.00 5 -1 28 70.69 13.40 -5 1 28 91.09 12.40 -5 1 28 62.79 12.10 -5 2 -28 -4.50 4.30 5 -2 -28 -9.50 6.50 5 2 28 9.70 8.60 -5 -2 28 2.00 6.00 -5 2 -28 10.40 9.20 5 -2 -28 -3.40 5.40 5 2 -28 0.90 8.60 5 2 -28 -1.30 6.50 5 -2 28 2.50 7.40 -5 -2 -28 -4.00 4.90 -5 2 28 -2.00 5.50 -5 2 28 2.40 6.00 5 3 28 178.88 18.40 5 -3 -28 125.49 16.60 -5 3 -28 163.28 21.00 -5 3 -28 148.59 16.40 5 3 28 152.48 20.20 -5 -3 28 144.29 19.30 -5 3 28 138.49 17.70 -5 -3 -28 116.09 15.90 -5 3 28 176.38 18.60 5 3 -28 195.38 23.80 5 -3 28 128.69 17.70 -5 -4 28 18.90 9.20 -5 4 -28 21.00 7.30 5 4 28 8.80 8.60 -5 4 -28 28.00 12.30 5 -4 -28 30.60 9.50 5 4 28 28.00 8.80 -5 4 28 27.20 9.30 -5 4 28 24.40 8.80 -5 -4 -28 8.40 7.40 5 -4 28 21.50 10.60 5 4 -28 25.80 11.50 5 5 28 44.70 11.80 5 5 28 5.80 7.60 5 -5 -28 10.00 8.40 -5 -5 28 1.40 6.50 -5 5 -28 16.10 12.10 -5 5 -28 23.40 7.00 5 5 -28 17.00 10.90 -5 -5 -28 2.00 6.80 -5 5 28 9.50 8.50 5 -5 28 21.80 10.40 5 -6 -28 -1.90 7.90 5 6 28 -6.70 7.90 -5 -6 28 -8.60 7.30 5 6 28 9.80 9.60 -5 6 -28 -5.40 9.10 5 6 -28 14.00 10.10 5 -6 28 -2.60 8.70 -5 -6 -28 1.50 7.40 -5 6 28 3.80 8.70 -5 7 -28 47.50 16.30 5 7 28 26.20 12.10 5 7 28 59.89 15.90 5 -7 -28 43.90 12.80 -5 -7 28 34.30 13.20 5 -7 28 38.40 11.80 -5 7 28 40.20 13.70 -5 -7 -28 20.80 10.40 5 7 -28 55.19 16.80 5 8 28 8.40 11.20 -5 -8 28 9.60 10.80 5 8 28 9.60 12.40 5 -8 -28 15.90 11.00 -5 8 -28 5.80 13.10 -5 -8 -28 11.20 10.20 -5 8 28 -8.10 10.60 5 8 -28 -6.70 12.20 5 -8 28 6.60 9.40 5 9 28 17.60 12.10 -5 -9 28 51.79 14.90 5 9 28 13.30 14.10 -5 9 -28 56.99 20.30 5 -9 -28 12.80 11.40 5 -9 28 26.00 12.40 -5 9 28 74.79 19.00 -5 -9 -28 16.20 10.90 5 9 -28 29.30 17.90 5 -10 -28 8.10 13.20 -5 -10 28 17.80 13.70 -5 10 -28 -5.30 16.20 5 10 28 -9.50 12.80 -5 10 28 -1.20 12.40 -5 -10 -28 10.60 11.50 5 -10 28 7.00 11.00 5 10 -28 14.40 15.80 -6 0 -28 -5.70 6.70 6 0 -28 -0.30 4.90 -6 0 -28 7.50 5.90 6 0 -28 -3.40 7.60 -6 0 28 3.00 5.90 -6 0 28 -1.40 4.90 6 0 28 5.20 7.10 -6 1 -28 142.59 18.10 -6 1 -28 106.19 13.50 6 -1 -28 80.49 12.50 -6 -1 28 98.99 12.70 6 -1 -28 98.09 15.60 6 1 28 105.69 16.50 -6 -1 28 99.89 15.50 -6 1 28 100.69 14.40 6 -1 28 106.99 15.80 -6 1 28 112.09 14.20 -6 -1 -28 132.29 15.60 -6 -1 -28 146.59 18.90 6 1 -28 138.49 13.70 6 1 -28 133.69 18.50 6 -2 -28 19.60 8.60 -6 2 -28 -8.10 4.20 6 2 28 11.80 9.20 -6 2 -28 -9.70 7.70 -6 -2 28 17.70 8.50 6 -2 -28 -6.10 5.30 -6 -2 -28 1.60 5.50 6 2 -28 8.10 10.20 6 -2 28 -1.50 6.70 -6 2 28 4.20 6.90 -6 2 28 7.60 6.50 6 -3 -28 12.60 6.90 -6 3 -28 -8.10 4.40 -6 -3 28 4.70 6.90 6 3 28 11.00 7.80 -6 3 -28 -0.90 9.00 -6 3 28 -3.10 5.30 -6 3 28 3.40 7.10 6 3 -28 12.70 10.60 -6 -3 -28 -5.00 5.80 6 -3 28 5.30 7.40 6 4 28 13.70 8.10 -6 4 -28 26.10 8.20 6 4 28 8.90 8.40 6 -4 -28 22.80 9.20 -6 4 -28 17.10 10.40 -6 -4 28 10.30 8.10 6 -4 28 4.10 8.70 -6 -4 -28 6.20 7.00 -6 4 28 6.50 6.60 -6 4 28 17.80 9.30 6 4 -28 49.80 14.70 -6 -5 28 22.40 10.20 6 5 28 47.80 12.60 6 -5 -28 26.80 10.10 -6 5 -28 19.20 12.70 6 5 28 48.40 11.70 -6 5 -28 56.49 10.50 6 5 -28 18.90 12.50 -6 -5 -28 53.29 12.20 -6 5 28 31.10 10.70 6 -5 28 62.99 13.20 -6 6 -28 -2.80 10.20 -6 -6 28 11.40 9.60 6 -6 -28 -1.20 8.30 6 6 28 -1.50 9.60 6 6 28 12.80 9.50 -6 6 28 -16.50 7.40 -6 -6 -28 12.70 8.60 6 6 -28 12.90 11.20 6 -6 28 -11.60 7.60 6 -7 -28 34.30 13.20 6 7 28 105.59 18.80 -6 -7 28 150.58 22.30 6 7 28 80.69 16.40 -6 7 -28 99.09 22.50 6 7 -28 149.39 24.70 -6 -7 -28 75.59 15.20 6 -7 28 103.29 17.40 -6 7 28 106.79 18.90 6 -8 -28 32.60 13.60 6 8 28 7.60 11.00 -6 8 -28 25.80 17.20 6 8 28 29.60 14.00 -6 -8 28 25.30 12.90 -6 8 28 20.80 12.70 6 -8 28 32.60 12.40 6 8 -28 36.20 16.60 -6 -8 -28 56.49 13.50 6 9 28 -0.90 11.80 -6 9 -28 17.80 16.90 6 9 28 -1.60 10.80 -6 -9 28 -6.40 11.00 6 -9 -28 1.60 11.10 -6 -9 -28 4.60 9.70 6 -9 28 13.40 11.00 6 9 -28 16.50 15.90 -6 9 28 -16.60 11.00 6 -10 -28 3.50 14.10 -6 10 -28 5.40 15.00 6 10 28 -4.90 11.80 -6 -10 28 4.00 13.40 6 -10 28 -6.90 10.40 6 10 -28 2.80 17.00 -6 10 28 22.60 14.90 -6 -10 -28 24.40 12.30 7 0 -28 79.99 15.80 7 0 28 110.79 16.80 -7 0 28 105.89 14.80 -7 0 -28 96.49 15.30 7 0 -28 109.09 13.00 -7 0 -28 111.99 14.50 -7 0 28 132.39 14.50 7 1 28 -14.10 6.60 -7 -1 28 3.00 5.00 7 -1 -28 -7.40 4.80 -7 -1 28 0.30 6.00 -7 1 -28 -0.70 5.20 7 -1 -28 -7.70 6.90 -7 1 -28 -6.20 7.40 -7 1 28 1.10 5.80 -7 1 28 -5.60 4.40 -7 -1 -28 3.60 6.00 7 -1 28 5.20 7.40 7 1 -28 6.30 8.70 7 1 -28 -0.90 4.60 7 -2 -28 -3.90 6.30 -7 2 -28 16.20 10.00 -7 -2 28 -3.60 6.00 -7 2 -28 6.10 5.50 7 2 28 -3.00 6.50 7 -2 -28 1.40 8.20 -7 2 28 11.10 6.60 7 -2 28 9.20 7.80 7 2 -28 6.40 8.60 -7 2 28 9.90 6.70 -7 -2 -28 1.60 6.10 -7 -3 28 4.50 6.30 7 -3 -28 0.80 6.00 7 3 28 -0.30 6.50 -7 3 -28 4.30 5.60 -7 3 -28 8.30 10.20 -7 -3 -28 -12.90 5.20 -7 3 28 4.00 7.00 -7 3 28 -0.70 5.00 7 3 -28 -0.30 8.30 7 -3 28 3.10 7.60 -7 -4 28 12.00 8.00 -7 4 -28 -6.20 5.20 7 4 28 4.70 7.40 7 4 28 0.10 7.20 7 -4 -28 24.90 9.60 -7 4 -28 -8.70 9.70 -7 4 28 17.80 8.40 7 -4 28 13.00 8.30 -7 -4 -28 7.80 7.40 7 4 -28 12.40 10.40 -7 5 -28 8.60 12.10 7 5 28 32.10 10.70 7 -5 -28 14.10 9.10 -7 -5 28 16.10 9.20 7 5 28 5.20 8.90 -7 5 -28 20.10 7.40 -7 5 28 38.90 11.40 7 5 -28 34.70 14.40 -7 -5 -28 16.40 9.00 7 -5 28 18.20 11.00 7 -6 -28 7.60 9.30 -7 6 -28 15.40 7.60 7 6 28 2.80 8.70 7 6 28 0.30 9.30 -7 6 -28 -1.10 12.00 -7 -6 28 0.30 8.30 7 6 -28 -2.40 11.20 7 -6 28 3.70 9.50 -7 6 28 -0.90 8.40 -7 -6 -28 10.10 8.60 7 -7 -28 12.90 11.70 -7 -7 28 12.80 10.50 7 7 28 6.60 9.50 -7 7 -28 8.50 12.80 7 7 28 13.40 10.60 -7 7 28 22.80 11.30 7 7 -28 30.10 14.00 -7 -7 -28 18.10 9.10 7 -7 28 15.40 10.90 -7 8 -28 -12.40 13.30 7 -8 -28 -4.50 10.00 7 8 28 -0.70 9.60 7 8 28 -5.10 11.20 -7 -8 28 -5.30 9.60 -7 8 28 0.10 9.40 7 8 -28 -7.20 12.80 -7 -8 -28 10.20 9.80 7 -8 28 0.20 8.40 7 -9 -28 -8.90 9.60 7 9 28 -1.80 11.70 -7 9 -28 -22.30 13.70 -7 -9 28 -0.40 10.40 7 9 28 -6.00 9.50 7 9 -28 -3.00 12.70 -7 9 28 -9.20 11.40 -7 -9 -28 11.50 10.90 7 -9 28 18.00 10.50 -7 10 -28 0.00 16.00 -7 -10 28 13.20 15.70 7 10 28 0.70 12.30 7 10 28 9.00 14.20 7 -10 -28 0.30 18.10 -7 -10 -28 13.00 11.10 7 -10 28 11.30 11.50 -7 10 28 11.00 14.60 7 10 -28 35.70 19.00 8 0 28 -5.50 6.70 -8 0 -28 0.40 5.20 8 0 -28 -1.30 9.20 -8 0 28 -3.30 5.30 8 0 -28 -2.10 4.70 -8 0 -28 -8.00 7.20 -8 0 28 7.40 6.30 8 -1 -28 8.00 6.80 -8 -1 28 12.00 6.40 -8 -1 28 19.70 7.70 -8 1 -28 27.90 10.90 8 -1 -28 18.70 10.60 8 1 28 13.50 8.50 -8 1 -28 27.30 7.90 -8 1 28 15.90 7.70 8 1 -28 0.90 9.20 -8 1 28 23.10 8.00 8 -1 28 1.80 8.70 -8 -1 -28 26.80 8.10 8 -2 -28 13.80 10.00 8 -2 -28 10.90 7.80 8 2 28 2.90 8.20 -8 -2 28 19.00 6.20 -8 2 -28 22.30 7.50 -8 2 -28 5.80 9.20 -8 -2 28 22.00 8.40 -8 2 28 8.50 6.10 8 2 -28 25.00 11.10 -8 -2 -28 13.50 7.40 8 -2 28 16.30 9.60 -8 2 28 25.00 8.50 8 3 28 20.80 9.50 8 -3 -28 25.10 15.00 8 -3 -28 19.00 8.40 -8 3 -28 10.70 10.20 -8 -3 28 17.70 7.70 -8 3 -28 18.40 7.60 8 -3 28 30.10 10.50 -8 3 28 19.40 8.40 8 3 -28 2.90 10.60 -8 -3 -28 5.10 7.00 -8 3 28 24.90 8.10 -8 4 -28 6.40 6.50 -8 -4 28 25.50 9.90 8 -4 -28 12.20 8.30 8 4 28 17.20 10.50 8 4 28 14.20 9.20 -8 4 -28 -5.90 9.90 8 4 -28 5.20 10.30 -8 4 28 3.70 7.20 -8 -4 -28 15.50 8.20 8 -4 28 11.10 7.90 8 5 28 4.80 9.70 8 5 28 9.40 8.30 8 -5 -28 0.50 9.00 -8 5 -28 -23.70 8.70 -8 -5 28 -7.80 6.60 -8 5 -28 2.70 5.80 -8 5 28 -9.10 6.80 8 -5 28 7.10 9.30 8 5 -28 -0.90 9.80 -8 -5 -28 -1.10 6.80 -8 6 -28 4.90 12.20 8 6 28 -0.30 8.40 -8 6 -28 6.30 7.00 -8 -6 28 4.90 7.80 8 -6 -28 -2.60 9.00 8 6 28 16.60 10.60 -8 -6 -28 16.30 9.90 8 6 -28 21.60 13.40 8 -6 28 7.50 9.30 -8 6 28 -1.50 8.40 -8 -7 28 12.60 10.20 8 7 28 8.10 11.40 -8 7 -28 24.40 15.70 8 7 28 21.20 12.00 8 -7 -28 -5.60 9.20 -8 -7 -28 9.70 8.60 -8 7 28 19.40 10.10 8 -7 28 32.50 11.60 8 7 -28 4.30 11.80 -8 -8 28 17.40 11.70 8 8 28 16.20 12.20 8 -8 -28 2.30 10.60 8 8 28 12.80 11.10 -8 8 -28 -4.10 12.20 -8 8 28 35.10 13.60 -8 -8 -28 6.90 8.40 8 -8 28 17.60 11.50 8 8 -28 21.40 14.50 8 9 28 -8.00 9.50 -8 -9 28 2.40 11.60 8 -9 -28 9.90 11.60 8 9 28 5.40 12.70 -8 9 -28 -4.90 13.20 -8 -9 -28 2.30 9.70 8 9 -28 22.70 16.20 8 -9 28 6.60 10.90 -8 9 28 -18.50 10.30 -9 0 28 255.97 20.90 9 0 28 286.57 27.50 -9 0 28 250.57 21.30 -9 0 -28 258.87 21.70 -9 0 -28 259.37 23.30 9 0 -28 253.47 26.70 9 0 -28 241.38 19.70 -9 -1 28 9.40 6.10 -9 -1 28 5.90 6.00 9 -1 -28 -6.10 8.50 9 1 28 19.60 9.40 -9 1 -28 0.00 5.50 9 -1 -28 -2.80 5.40 -9 1 -28 -2.50 7.90 -9 1 28 15.60 7.00 9 1 -28 1.60 9.70 -9 -1 -28 3.90 5.80 -9 1 28 10.90 6.20 9 -1 28 -2.60 6.60 -9 -2 28 1.50 6.10 9 2 28 14.70 8.30 9 -2 -28 0.70 6.20 -9 2 -28 -1.70 4.70 -9 2 -28 -0.70 8.50 -9 -2 28 -0.70 4.80 9 -2 -28 19.20 9.60 -9 2 28 9.40 6.90 -9 -2 -28 1.30 6.30 9 2 -28 -4.00 9.30 9 -2 28 -5.70 7.40 -9 2 28 8.90 5.90 -9 -3 28 199.08 22.20 -9 3 -28 256.47 23.20 9 -3 -28 209.88 21.80 9 3 28 253.27 26.90 9 -3 -28 248.88 23.90 -9 3 -28 240.38 26.10 -9 -3 -28 172.38 20.20 -9 3 28 180.78 21.80 9 3 -28 196.98 24.70 9 -3 28 252.77 25.90 -9 4 -28 39.40 10.10 -9 4 -28 -4.00 8.40 9 4 28 8.70 8.80 -9 -4 28 6.40 7.90 9 -4 -28 26.00 9.80 -9 -4 -28 12.40 7.70 9 -4 28 9.70 8.60 9 4 -28 23.00 12.40 -9 4 28 0.90 8.10 -9 5 -28 -3.90 10.20 9 -5 -28 5.50 9.30 9 5 28 -7.90 9.70 9 5 28 -5.30 8.10 -9 5 -28 4.00 6.00 -9 -5 28 -3.20 6.70 9 5 -28 -16.10 7.80 -9 -5 -28 -3.50 6.90 -9 5 28 -14.50 6.90 9 -5 28 -11.50 8.00 -9 6 -28 4.80 12.10 9 6 28 -6.40 9.50 -9 6 -28 8.80 7.40 9 6 28 5.50 8.60 -9 -6 28 8.60 8.80 9 -6 -28 19.40 10.90 9 -6 28 3.70 9.80 -9 6 28 44.70 13.10 -9 -6 -28 -13.80 6.20 9 6 -28 11.50 11.80 -9 7 -28 99.19 20.90 -9 -7 28 85.69 17.40 9 7 28 80.09 17.60 9 7 28 97.39 18.30 9 -7 -28 67.29 15.50 9 7 -28 92.09 21.20 9 -7 28 75.89 15.10 -9 7 28 84.19 18.00 -9 -7 -28 85.19 16.20 9 -8 -28 2.30 10.20 9 8 28 -21.40 8.30 -9 -8 28 11.50 10.80 9 8 28 19.70 10.90 -9 8 -28 -6.00 12.40 -9 8 28 4.70 10.10 9 -8 28 -11.00 10.00 9 8 -28 -12.20 12.20 -9 -8 -28 -9.80 7.70 -9 9 -28 22.70 14.80 9 9 28 6.00 12.20 9 9 28 16.40 13.60 -9 -9 28 12.40 11.70 9 -9 -28 12.50 12.40 9 -9 28 -1.60 11.20 -9 -9 -28 18.30 10.80 9 9 -28 13.10 15.10 -9 9 28 12.20 12.50 -10 0 -28 195.58 20.30 -10 0 28 172.58 18.90 10 0 -28 158.98 16.20 10 0 28 192.48 21.70 -10 0 -28 179.18 20.10 10 0 -28 163.08 21.40 -10 0 28 172.68 18.30 10 -1 -28 -12.10 7.90 10 1 28 -4.30 7.50 10 -1 -28 -2.90 5.30 -10 1 -28 0.00 5.00 -10 -1 28 -3.60 4.50 -10 -1 28 13.50 6.20 -10 1 -28 -1.10 7.70 10 -1 28 6.00 8.10 -10 -1 -28 1.60 5.20 10 1 -28 6.30 9.40 -10 1 28 -6.00 5.30 -10 1 28 0.40 5.10 -10 2 -28 11.90 6.40 -10 -2 28 3.00 5.80 10 -2 -28 7.00 9.30 10 -2 -28 4.50 6.80 -10 -2 28 -4.50 4.50 -10 2 -28 -5.20 8.30 10 2 28 -6.60 6.60 -10 2 28 13.30 7.10 10 -2 28 7.90 8.90 -10 -2 -28 2.30 6.10 10 2 -28 -4.30 10.00 -10 2 28 11.70 6.40 10 3 28 42.20 12.10 10 -3 -28 1.30 7.70 -10 3 -28 27.50 12.70 -10 -3 28 19.70 6.20 -10 3 -28 18.20 8.20 10 -3 -28 26.10 9.90 -10 -3 28 25.90 9.70 -10 3 28 14.10 8.70 -10 -3 -28 4.80 7.20 10 -3 28 21.90 10.10 10 3 -28 16.90 10.40 10 -4 -28 -3.70 7.00 10 4 28 6.50 9.90 -10 4 -28 0.30 6.30 -10 -4 28 4.40 7.20 -10 4 -28 10.80 11.90 -10 -4 -28 4.50 7.40 -10 4 28 10.50 8.70 10 4 -28 6.80 11.40 10 -4 28 0.10 8.20 -10 5 -28 27.00 9.10 -10 -5 28 26.20 10.40 -10 5 -28 19.10 13.30 10 5 28 19.50 9.50 10 5 28 28.40 11.30 10 -5 -28 24.20 10.80 -10 -5 -28 21.80 9.70 10 5 -28 4.00 11.80 10 -5 28 18.00 10.40 -10 5 28 24.20 10.40 -10 6 -28 -11.40 9.60 -10 -6 28 -0.60 8.10 -10 6 -28 -6.40 6.10 10 6 28 1.20 8.90 10 -6 -28 -8.10 9.30 10 6 28 10.00 10.00 -10 -6 -28 -9.00 7.30 -10 6 28 0.60 8.10 10 6 -28 9.60 11.30 10 -6 28 4.50 9.00 -10 -7 28 6.30 9.90 -10 7 -28 2.70 7.20 10 7 28 2.00 9.10 10 -7 -28 -1.70 9.90 10 7 28 11.30 11.60 -10 7 -28 1.10 13.20 -10 -7 -28 7.20 8.20 -10 7 28 7.60 10.40 10 -7 28 -2.60 8.50 10 7 -28 10.90 12.90 10 -8 -28 69.99 16.00 -10 -8 28 92.29 19.20 10 8 28 104.59 20.10 10 8 28 70.49 17.50 -10 8 -28 115.39 24.80 -10 -8 -28 93.59 17.40 10 -8 28 86.39 17.40 -10 8 28 76.49 18.00 10 8 -28 144.49 26.20 10 -9 -28 -22.70 10.00 -10 9 -28 -2.30 12.50 10 9 28 -7.30 10.70 10 9 28 7.40 12.30 -10 -9 28 -0.90 11.50 -10 -9 -28 3.70 10.20 10 9 -28 -1.40 15.30 -10 9 28 -2.80 10.50 10 -9 28 -2.20 10.90 -11 0 -28 365.66 27.80 11 0 -28 356.56 31.00 -11 0 -28 378.66 27.30 -11 0 28 338.07 26.30 -11 0 28 328.97 26.10 11 0 28 344.77 29.40 11 -1 -28 11.70 9.00 -11 -1 28 27.50 8.60 11 -1 -28 13.30 7.20 -11 -1 28 10.30 6.40 -11 1 -28 8.10 7.00 -11 1 -28 4.40 7.60 11 1 28 -1.20 8.00 11 -1 28 11.60 9.30 11 1 -28 -10.70 8.30 -11 -1 -28 14.10 6.50 -11 1 28 10.20 7.00 -11 1 28 2.90 5.40 11 2 28 27.50 11.00 -11 -2 28 34.70 9.10 11 -2 -28 16.40 8.10 -11 -2 28 40.00 8.70 -11 2 -28 16.00 10.00 -11 2 -28 19.80 7.60 11 -2 -28 23.50 10.70 -11 -2 -28 18.90 8.00 11 -2 28 26.10 11.30 -11 2 28 29.50 12.70 11 2 -28 47.10 14.50 -11 2 28 34.40 10.00 -11 3 -28 66.99 15.70 -11 -3 28 50.59 11.40 -11 3 -28 50.69 10.90 11 -3 -28 37.80 10.40 11 -3 -28 48.30 12.30 11 3 28 30.10 11.30 -11 -3 28 74.29 11.10 -11 -3 -28 47.10 10.70 11 3 -28 53.39 14.80 11 -3 28 49.00 12.40 -11 3 28 39.80 11.70 -11 4 -28 63.59 12.80 -11 -4 28 86.89 15.30 11 -4 -28 64.19 13.10 -11 4 -28 97.19 19.00 11 4 28 97.39 17.50 -11 4 28 76.29 14.60 11 -4 28 67.79 14.60 11 4 -28 99.89 19.20 -11 -4 -28 65.99 12.80 -11 5 -28 23.00 12.80 -11 5 -28 35.20 10.30 -11 -5 28 38.40 12.10 11 5 28 34.40 12.00 11 -5 -28 27.40 11.40 11 5 -28 40.70 15.70 11 -5 28 34.70 12.60 -11 5 28 43.20 12.70 -11 -5 -28 41.20 11.40 -11 6 -28 39.40 15.10 11 6 28 12.00 10.30 -11 -6 28 41.30 13.50 11 -6 -28 24.40 11.40 -11 6 -28 15.80 7.90 11 6 28 35.90 13.00 -11 6 28 26.20 11.00 11 -6 28 34.00 12.80 11 6 -28 11.60 15.00 -11 -6 -28 28.80 11.40 -11 -7 28 27.00 12.30 -11 7 -28 11.60 8.30 -11 7 -28 19.70 14.30 11 -7 -28 18.80 11.00 11 7 28 27.10 13.30 11 7 28 25.90 13.00 11 7 -28 22.80 14.30 11 -7 28 9.40 10.40 -11 -7 -28 6.40 9.60 -11 7 28 36.90 13.70 11 -8 -28 1.80 11.10 11 8 28 9.30 12.50 -11 8 -28 0.70 12.00 -11 -8 28 -5.70 9.00 11 8 28 6.10 10.30 -11 -8 -28 2.20 9.80 11 -8 28 9.70 9.90 -11 8 28 -7.90 8.90 11 8 -28 32.10 15.60 -11 9 -28 26.90 15.70 11 9 28 13.40 13.00 11 -9 -28 7.70 11.40 11 9 28 31.00 15.40 -11 -9 28 26.20 14.70 -11 9 28 30.20 14.10 -11 -9 -28 22.10 12.80 11 9 -28 5.50 17.10 11 -9 28 29.00 12.40 12 0 -28 186.18 23.40 -12 0 -28 194.38 20.50 12 0 28 194.68 22.90 -12 0 28 174.38 18.90 -12 0 28 182.48 19.40 -12 0 -28 154.28 18.40 12 -1 -28 63.99 11.50 12 -1 -28 83.19 15.60 12 1 28 81.79 15.80 -12 -1 28 70.29 12.90 -12 -1 28 97.69 13.10 -12 1 -28 83.29 13.20 -12 1 -28 84.09 14.60 -12 1 28 87.29 13.00 -12 1 28 75.69 12.90 -12 -1 -28 56.69 11.50 12 1 -28 85.79 16.50 12 -1 28 67.89 15.40 12 -2 -28 8.00 9.10 12 -2 -28 -0.20 6.90 -12 2 -28 1.20 8.80 -12 -2 28 14.30 7.20 -12 2 -28 -6.10 5.60 12 2 28 -0.40 7.90 -12 -2 28 3.30 5.60 12 2 -28 6.10 9.80 -12 -2 -28 -2.60 5.40 -12 2 28 0.50 6.40 12 -2 28 -9.50 8.00 -12 3 -28 170.48 19.10 12 -3 -28 155.58 18.00 -12 -3 28 157.38 16.60 -12 3 -28 174.18 22.10 12 3 28 112.99 18.60 -12 -3 28 147.49 19.20 12 -3 -28 164.78 20.50 -12 3 28 173.48 20.90 -12 -3 -28 144.99 18.10 12 -3 28 175.98 21.60 12 3 -28 137.39 21.70 12 4 28 8.90 8.60 -12 4 -28 15.50 11.70 -12 4 -28 31.10 9.70 -12 -4 28 14.70 8.20 12 -4 -28 -8.80 7.10 -12 -4 -28 28.90 10.10 -12 4 28 27.30 10.40 12 4 -28 32.70 12.50 12 -4 28 25.50 11.00 12 -5 -28 26.40 10.80 12 5 28 35.80 12.60 -12 5 -28 31.10 10.80 -12 -5 28 17.80 9.10 -12 5 -28 45.30 14.90 12 -5 28 30.50 12.00 12 5 -28 19.50 13.40 -12 -5 -28 47.70 12.00 -12 5 28 20.10 10.50 12 -6 -28 14.60 10.90 12 6 28 12.50 10.30 -12 6 -28 -4.90 5.70 -12 6 -28 -4.60 12.30 12 6 28 -8.60 8.70 -12 -6 28 -4.70 7.50 -12 -6 -28 -8.20 6.80 -12 6 28 -4.30 7.70 12 6 -28 -14.60 11.30 12 -6 28 3.70 9.50 12 7 28 13.40 12.20 -12 -7 28 11.40 9.50 12 7 28 19.90 12.10 -12 7 -28 -2.80 12.10 -12 7 -28 0.40 7.50 12 -7 -28 -6.10 9.70 -12 -7 -28 2.50 9.00 12 -7 28 -10.20 9.10 12 7 -28 -9.70 10.10 -12 7 28 2.40 9.30 12 8 28 4.60 11.80 -12 -8 28 -16.30 8.40 12 -8 -28 -5.80 9.50 -12 8 -28 -2.50 12.00 12 8 28 2.80 12.50 -12 8 28 0.00 10.50 12 -8 28 -11.80 10.30 -12 -8 -28 1.20 9.60 12 8 -28 10.80 14.00 12 9 28 11.90 13.80 12 9 28 36.10 16.10 12 -9 -28 40.80 15.00 -12 9 -28 21.10 15.90 -12 -9 28 35.40 15.40 -12 9 28 29.80 14.30 12 -9 28 13.90 11.30 12 9 -28 43.70 18.60 -12 -9 -28 22.80 12.60 -13 0 -28 130.09 17.00 -13 0 -28 146.79 17.70 13 0 28 132.29 18.10 -13 0 28 130.29 16.80 13 0 -28 131.29 19.20 -13 0 28 119.59 16.00 -13 -1 28 391.16 28.10 13 -1 -28 376.96 28.20 -13 1 -28 347.17 29.50 13 1 28 375.96 31.50 -13 -1 28 335.47 27.80 -13 1 -28 384.06 28.60 13 -1 -28 447.96 32.80 -13 -1 -28 377.76 28.80 -13 1 28 358.76 28.80 13 -1 28 427.06 32.10 13 1 -28 365.96 32.40 -13 -2 28 15.60 6.90 -13 2 -28 -2.80 6.50 -13 -2 28 2.50 5.30 13 -2 -28 10.20 7.40 13 -2 -28 -4.90 9.10 13 2 28 8.10 8.80 -13 2 -28 6.30 6.30 -13 -2 -28 1.90 6.00 13 -2 28 21.50 10.00 -13 2 28 14.90 7.60 13 2 -28 25.20 13.40 -13 3 -28 -1.00 6.00 13 -3 -28 14.30 9.90 -13 3 -28 22.20 12.10 -13 -3 28 16.00 6.50 13 3 28 -2.70 7.70 13 -3 -28 2.60 8.20 -13 -3 28 7.50 7.20 13 -3 28 16.00 8.80 13 3 -28 2.70 12.30 -13 3 28 23.30 9.30 -13 -3 -28 9.10 7.10 -13 4 -28 25.50 12.50 -13 -4 28 4.00 6.60 13 4 28 18.20 12.60 -13 -4 28 16.10 6.90 -13 4 -28 8.80 7.60 13 -4 -28 2.30 8.60 13 -4 28 0.10 9.20 13 4 -28 -2.00 11.10 -13 4 28 18.40 10.30 -13 -4 -28 -5.00 7.20 -13 5 -28 36.30 14.20 -13 -5 28 34.90 10.60 13 -5 -28 35.20 12.00 13 5 28 35.60 11.90 -13 5 -28 25.50 9.90 -13 -5 -28 39.10 11.00 13 5 -28 48.10 16.10 -13 5 28 48.20 13.70 13 -5 28 49.00 13.90 -13 6 -28 16.80 12.30 13 -6 -28 -0.20 9.40 -13 -6 28 5.60 7.70 13 6 28 4.40 11.00 -13 6 -28 -5.00 6.10 13 6 -28 9.50 13.10 -13 6 28 18.70 10.80 13 -6 28 -6.30 9.00 -13 -6 -28 -1.20 8.50 -13 7 -28 75.59 15.40 -13 -7 28 89.09 18.00 13 7 28 76.29 17.00 13 -7 -28 59.39 15.50 -13 7 -28 78.59 19.60 13 7 28 47.40 16.30 -13 -7 -28 98.39 16.80 -13 7 28 143.59 22.10 13 -7 28 48.80 14.50 13 7 -28 85.79 22.20 -13 -8 28 15.10 12.20 13 8 28 -5.30 11.70 13 8 28 10.60 13.30 13 -8 -28 15.60 12.30 -13 8 -28 -1.80 14.00 -13 8 -28 6.30 9.50 13 -8 28 -0.10 10.40 -13 8 28 -16.40 8.70 -13 -8 -28 5.90 10.40 13 8 -28 -6.50 13.70 -13 9 -28 25.60 15.80 13 9 28 7.90 12.10 -13 -9 28 0.50 11.00 13 -9 -28 -1.70 12.00 -13 9 28 11.80 11.50 13 -9 28 -15.20 11.00 13 9 -28 8.00 15.40 -13 -9 -28 -3.70 8.20 -13 -9 -28 -5.20 10.40 -14 0 -28 13.60 6.90 -14 0 28 8.20 6.80 14 0 -28 -1.00 8.10 -14 0 28 9.00 7.30 14 0 28 13.10 10.70 -14 1 -28 15.80 7.90 14 1 28 19.60 10.50 -14 -1 28 19.10 7.10 -14 -1 28 12.80 7.30 14 -1 -28 13.20 9.60 -14 1 -28 12.30 7.90 -14 -1 -28 13.00 7.70 -14 1 28 1.30 6.00 14 -1 28 12.60 9.70 14 1 -28 3.40 11.10 14 -2 -28 1.60 6.70 -14 2 -28 -1.30 8.20 -14 -2 28 -8.70 4.20 14 -2 -28 -0.20 10.50 -14 -2 28 -3.80 5.00 -14 2 -28 -11.30 4.80 14 2 28 10.80 9.80 -14 -2 -28 -1.70 5.30 14 2 -28 7.00 10.40 -14 2 28 0.70 6.50 14 -2 28 -0.70 8.30 -14 -3 28 52.39 10.20 14 3 28 48.40 13.00 -14 3 -28 80.79 15.60 14 -3 -28 52.19 14.00 -14 3 -28 81.79 14.10 -14 -3 28 59.49 12.80 14 -3 -28 74.19 13.20 -14 -3 -28 81.09 14.20 14 3 -28 44.70 15.50 14 -3 28 47.80 13.70 -14 3 28 67.99 13.40 -14 -4 28 8.70 8.30 -14 4 -28 7.80 7.90 14 4 28 10.70 10.80 -14 4 -28 2.20 11.10 14 -4 -28 4.90 9.00 -14 -4 28 30.50 7.80 14 -4 28 1.80 10.00 14 4 -28 -0.30 12.10 -14 -4 -28 14.00 8.90 -14 4 28 14.00 9.80 14 -5 -28 56.29 13.90 -14 5 -28 48.50 12.50 -14 5 -28 28.80 13.70 -14 -5 28 43.30 11.90 14 5 28 56.09 15.10 -14 -5 -28 50.09 12.80 -14 5 28 54.59 14.10 14 -5 28 74.39 15.30 14 5 -28 50.29 16.60 -14 6 -28 -3.60 6.30 14 6 28 -5.50 10.50 14 -6 -28 6.80 10.60 -14 6 -28 3.70 11.60 -14 -6 28 -2.40 7.20 -14 -6 -28 -3.50 8.10 -14 6 28 2.90 8.40 14 6 -28 12.10 12.50 14 -6 28 -14.80 8.50 -14 7 -28 18.20 9.30 -14 7 -28 33.40 17.50 14 7 28 -0.70 10.40 14 -7 -28 17.50 12.00 -14 -7 28 40.70 13.70 14 7 -28 27.60 16.60 -14 7 28 18.40 11.70 -14 -7 -28 24.20 11.50 -14 -7 -28 20.00 10.60 14 -7 28 41.30 14.20 14 -8 -28 2.40 11.80 -14 -8 28 3.10 9.90 -14 8 -28 4.60 14.00 14 8 28 -8.40 10.50 -14 8 -28 5.50 8.80 -14 -8 -28 -5.90 8.70 -14 8 28 5.30 10.30 14 8 -28 1.60 14.10 14 -8 28 5.30 11.10 -14 -8 -28 -7.30 8.00 -14 -9 28 14.70 14.00 14 9 28 11.30 13.30 14 -9 -28 21.80 13.50 -14 9 -28 11.40 16.10 14 -9 28 34.20 14.70 14 9 -28 39.70 18.20 -14 -9 -28 19.40 10.90 -14 9 28 25.80 13.80 -14 -9 -28 26.40 12.70 15 0 28 60.49 15.40 -15 0 -28 82.89 13.40 15 0 -28 68.89 16.30 -15 0 28 96.39 19.90 -15 0 28 94.99 14.30 15 -1 -28 17.90 12.40 -15 1 -28 15.10 7.60 15 1 28 18.40 10.30 -15 1 -28 15.30 8.70 -15 -1 28 7.40 7.00 -15 -1 28 22.70 8.10 -15 1 28 0.00 5.50 15 1 -28 13.30 10.70 15 -1 28 6.60 9.90 -15 -1 -28 38.20 9.80 -15 -2 28 11.40 6.90 -15 -2 28 17.90 7.60 -15 2 -28 0.40 9.20 15 -2 -28 6.50 9.70 -15 2 -28 6.90 7.30 15 2 28 14.50 10.10 15 -2 -28 9.80 7.90 -15 2 28 15.80 8.80 -15 -2 -28 -3.50 6.40 15 -2 28 8.70 10.00 15 2 -28 27.00 13.70 -15 3 -28 242.08 28.20 15 -3 -28 220.48 22.50 15 3 28 198.58 25.30 -15 -3 28 233.38 20.40 15 -3 -28 199.78 23.80 -15 -3 28 251.57 25.90 -15 3 -28 279.27 26.80 15 3 -28 285.77 31.20 15 -3 28 197.08 24.60 -15 -3 -28 254.57 25.20 -15 3 28 255.47 27.10 15 4 28 11.90 10.20 -15 -4 28 4.00 5.40 15 -4 -28 7.20 9.00 -15 -4 28 3.90 6.90 -15 4 -28 7.80 7.60 -15 4 -28 4.70 10.90 -15 4 28 -0.70 8.40 15 -4 28 10.10 10.50 15 4 -28 -11.20 11.80 -15 -4 -28 16.30 9.00 -15 5 -28 -5.90 10.40 15 -5 -28 19.10 10.60 -15 -5 28 15.00 9.30 -15 5 -28 34.30 11.10 15 5 28 19.10 11.10 15 5 -28 14.10 13.80 -15 -5 -28 22.80 10.30 -15 5 28 43.70 12.50 15 -5 28 26.10 11.30 -15 -6 28 10.70 9.40 15 6 28 -13.80 7.40 -15 6 -28 3.20 12.70 15 -6 -28 18.90 11.90 -15 6 -28 -2.60 7.10 -15 -6 -28 6.90 10.00 15 6 -28 2.60 13.90 -15 6 28 -7.50 8.70 15 -6 28 16.80 11.90 -15 7 -28 32.00 11.20 -15 7 -28 16.70 13.80 15 -7 -28 13.50 11.20 15 7 28 16.50 13.20 -15 -7 28 17.80 11.30 15 7 -28 49.90 18.10 -15 -7 -28 11.30 10.70 -15 7 28 8.10 12.00 15 -7 28 33.70 13.80 -15 -8 28 0.80 9.70 -15 8 -28 1.20 8.70 15 -8 -28 -3.90 11.60 15 8 28 0.10 10.50 -15 8 -28 -8.80 11.80 -15 -8 -28 3.20 8.20 15 8 -28 -0.30 14.90 15 -8 28 0.10 10.10 -15 8 28 5.50 10.90 -15 -8 -28 3.60 10.40 -16 0 -28 43.70 11.20 -16 0 28 60.39 12.00 16 0 28 43.30 13.00 16 0 -28 52.29 14.40 -16 -1 28 -6.00 5.10 -16 1 -28 2.20 6.40 16 1 28 15.00 10.40 16 -1 -28 -17.10 9.30 -16 -1 28 6.00 6.30 16 -1 28 17.30 10.60 -16 -1 -28 -4.30 5.30 -16 1 28 9.20 7.60 16 1 -28 1.50 10.80 16 -1 28 12.90 10.40 -16 2 -28 45.80 11.20 16 -2 -28 44.90 13.10 -16 -2 28 27.00 9.40 -16 2 -28 57.99 13.70 16 2 28 43.80 13.20 -16 -2 28 34.20 9.20 -16 -2 -28 13.90 7.70 16 -2 28 32.40 13.30 16 2 -28 8.70 13.10 -16 2 28 34.40 10.40 -16 -3 28 30.90 10.00 16 -3 -28 20.80 9.70 16 3 28 27.80 12.30 -16 3 -28 53.09 13.00 -16 3 -28 54.99 12.50 16 -3 -28 49.10 12.80 -16 -3 28 20.00 7.80 16 -3 28 42.90 13.40 -16 3 28 36.10 12.00 -16 -3 -28 36.20 10.80 16 3 -28 11.00 11.90 16 -4 -28 8.70 17.20 16 -4 -28 18.90 9.90 -16 4 -28 12.90 8.30 16 4 28 -8.90 9.80 -16 -4 28 11.00 7.60 -16 4 -28 5.90 11.30 -16 -4 28 8.90 6.10 -16 -4 -28 2.10 7.60 16 4 -28 -8.20 10.70 16 -4 28 14.70 10.90 -16 4 28 0.30 8.60 16 5 28 2.00 11.00 16 -5 -28 7.80 9.60 -16 5 -28 17.70 13.70 -16 -5 28 6.40 7.90 -16 -5 28 15.20 7.40 -16 5 -28 4.80 8.50 16 5 -28 26.60 14.60 -16 -5 -28 14.90 10.10 16 -5 28 22.90 11.70 -16 5 28 15.30 9.90 16 -6 -28 7.30 10.40 16 6 28 -2.90 9.70 -16 6 -28 1.50 11.90 -16 -6 28 -4.60 7.80 -16 6 -28 -9.00 6.70 -16 -6 -28 0.00 8.80 16 -6 28 4.40 9.30 -16 6 28 1.40 9.20 16 6 -28 29.00 16.60 -16 7 -28 48.70 13.10 -16 7 -28 70.59 19.70 16 -7 -28 53.79 14.50 -16 -7 28 46.70 13.90 16 7 28 36.50 16.10 16 -7 28 43.50 13.90 16 7 -28 59.39 19.00 -16 7 28 54.39 16.80 -16 -7 -28 38.20 12.90 16 -8 -28 3.50 11.80 -16 -8 28 23.20 12.00 16 8 28 7.10 11.20 -16 8 -28 -17.50 12.10 -16 8 -28 2.50 9.40 16 -8 28 2.60 11.70 -16 8 28 20.10 12.80 16 8 -28 10.20 15.50 -16 -8 -28 -3.20 9.70 -17 0 28 70.19 12.80 17 0 28 63.69 15.50 -17 0 -28 91.49 13.80 17 0 -28 60.69 15.60 17 1 28 4.20 8.60 -17 1 -28 2.70 6.80 17 -1 -28 23.80 13.30 -17 -1 28 -5.10 5.80 -17 -1 -28 10.80 6.70 17 1 -28 24.10 12.50 17 -1 28 -7.20 8.90 17 -1 28 -3.40 9.20 -17 1 28 12.20 8.00 -17 -2 28 12.80 7.30 -17 -2 28 7.10 6.70 17 -2 -28 16.60 10.90 17 2 28 7.00 11.10 -17 2 -28 21.90 8.70 17 -2 28 -3.10 10.80 -17 -2 -28 27.80 9.50 17 -2 28 11.20 10.30 17 2 -28 17.50 12.40 -17 2 28 26.20 9.60 17 -3 -28 10.20 8.80 17 -3 -28 -6.90 10.20 -17 -3 28 5.10 6.70 -17 -3 28 -6.70 4.80 -17 3 -28 1.40 9.40 -17 3 -28 -0.60 7.40 17 3 28 2.90 10.50 -17 -3 -28 -3.20 7.00 17 -3 28 17.30 12.70 17 -3 28 0.50 10.00 17 3 -28 10.10 12.20 -17 3 28 5.90 8.40 -17 -4 28 27.80 9.80 -17 4 -28 16.10 12.60 17 -4 -28 13.20 12.20 -17 -4 28 9.80 6.60 17 -4 -28 18.10 9.70 -17 4 -28 34.90 9.70 17 4 28 47.60 15.90 17 -4 28 22.70 12.60 -17 -4 -28 44.50 11.80 -17 4 28 20.40 10.00 17 4 -28 10.70 12.10 -17 5 -28 1.60 7.30 17 -5 -28 3.90 9.70 -17 5 -28 5.30 13.40 -17 -5 28 7.80 7.20 17 5 28 -1.80 10.10 -17 -5 28 -1.70 6.70 -17 5 28 13.10 11.50 -17 -5 -28 7.00 8.20 17 -5 28 -9.90 9.10 17 5 -28 -7.40 13.60 -17 6 -28 -20.80 11.00 17 -6 -28 6.50 10.30 -17 -6 28 -0.30 7.90 17 6 28 5.00 10.20 -17 6 -28 4.40 8.40 17 6 -28 5.70 14.20 -17 6 28 4.90 10.10 17 -6 28 8.90 10.90 -17 -6 -28 2.20 9.40 -17 7 -28 47.50 13.50 -17 7 -28 64.79 19.10 17 7 28 19.10 13.30 -17 -7 28 27.10 11.60 17 -7 -28 44.40 13.60 17 -7 28 32.90 14.20 17 -7 28 28.50 14.80 17 7 -28 54.69 18.80 -17 7 28 44.90 17.40 -17 -7 -28 33.10 13.20 -17 8 -28 40.90 18.00 17 8 28 11.90 13.00 -17 8 -28 9.10 10.80 17 -8 -28 2.30 11.30 -17 -8 28 -3.10 10.20 17 -8 28 32.60 17.40 -17 8 28 5.50 12.10 17 8 -28 -34.50 13.80 -17 -8 -28 21.30 12.20 -18 0 -28 307.57 27.60 18 0 -28 332.97 34.90 -18 0 28 425.76 29.90 18 0 28 359.16 32.10 -18 -1 28 37.40 10.00 18 1 28 58.39 16.60 18 -1 -28 32.90 13.20 -18 1 -28 35.90 10.30 18 1 -28 44.70 15.30 -18 1 28 34.50 10.40 18 -1 28 36.80 13.30 18 -1 28 2.10 10.60 -18 -1 -28 24.10 9.40 -18 2 -28 -1.80 6.20 18 2 28 4.70 10.60 -18 -2 28 1.70 6.00 18 -2 -28 -3.10 9.10 -18 -2 28 -8.80 5.00 -18 2 28 4.10 8.00 18 -2 28 -20.40 8.90 -18 -2 -28 10.90 8.50 18 2 -28 3.10 10.40 18 -2 28 15.90 12.10 -18 -3 28 24.80 9.80 18 -3 -28 16.30 12.50 18 3 28 12.90 12.10 -18 -3 28 21.80 8.70 18 -3 -28 8.50 9.00 -18 3 -28 15.70 8.90 -18 -3 -28 44.30 11.20 18 3 -28 22.60 12.90 -18 3 28 33.30 10.90 18 -3 28 5.30 11.20 18 -3 28 21.10 12.10 -18 4 -28 21.70 9.60 -18 -4 28 49.30 11.80 18 4 28 53.19 16.70 18 -4 -28 57.99 14.40 -18 -4 28 51.59 10.70 18 -4 -28 38.10 12.60 -18 -4 -28 15.50 9.90 18 -4 28 61.79 15.00 18 4 -28 53.19 15.30 18 -4 28 36.90 13.80 -18 4 28 43.20 13.00 18 5 28 -8.10 11.20 18 -5 -28 27.40 11.30 -18 5 -28 25.20 10.50 -18 -5 28 6.10 6.80 -18 -5 28 6.40 8.10 18 5 -28 -0.60 15.00 -18 -5 -28 0.40 8.20 18 -5 28 23.50 14.30 18 -5 28 2.60 11.20 -18 5 28 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13.30 9.20 -19 -3 28 50.09 11.50 -19 -3 28 31.30 10.00 19 -3 -28 36.20 14.90 19 3 28 51.39 16.00 -19 3 -28 34.40 11.80 19 -3 28 41.90 13.90 19 -3 28 54.59 14.00 19 3 -28 36.30 15.20 -19 3 28 79.49 14.90 -19 -3 -28 56.09 13.00 19 -4 -28 32.70 13.30 -19 -4 28 45.70 10.10 -19 4 -28 43.90 11.80 19 -4 -28 7.60 10.10 19 4 28 21.10 13.00 -19 -4 28 8.90 7.70 -19 4 28 18.20 10.30 19 4 -28 28.10 14.20 19 -4 28 11.20 12.40 -19 -4 -28 52.59 13.10 19 -4 28 20.20 12.10 -19 5 -28 9.70 8.50 -19 -5 28 -8.70 6.40 -19 -5 28 1.80 6.30 19 -5 -28 18.40 10.90 19 5 28 -1.00 12.40 19 -5 28 11.50 13.00 19 -5 28 1.70 11.10 -19 5 28 -0.20 9.50 19 5 -28 -7.20 13.50 -19 -5 -28 0.90 9.70 -19 -6 28 5.80 7.60 19 -6 -28 3.40 10.60 -19 -6 28 13.90 10.10 -19 6 -28 16.50 9.80 19 6 28 -7.90 11.10 -19 -6 -28 2.40 8.50 19 6 -28 45.80 18.40 19 -6 28 6.40 10.60 -19 6 28 20.90 12.70 19 -6 28 17.70 12.80 19 7 28 80.69 19.60 -19 -7 28 71.89 17.10 -19 7 -28 86.79 17.50 19 -7 -28 58.89 16.20 19 7 -28 110.39 24.70 -19 7 28 111.59 20.40 19 -7 28 90.99 21.70 -19 -7 -28 85.79 17.10 -19 8 -28 -3.80 9.30 -19 -8 28 -7.50 9.40 19 -8 -28 -4.50 11.80 19 8 28 -4.30 11.90 19 -8 28 -6.20 13.80 19 8 -28 -0.50 16.20 -19 -8 -28 -0.70 10.30 -19 8 28 11.90 14.20 -20 0 28 107.79 16.20 20 0 -28 64.49 16.80 -20 0 -28 60.29 13.10 20 0 28 75.09 16.60 20 -1 -28 25.20 13.60 -20 -1 28 34.60 10.60 -20 1 -28 16.40 9.00 20 1 28 11.10 12.20 -20 1 28 11.90 8.70 20 1 -28 35.20 12.50 20 -1 28 29.10 14.30 -20 -1 -28 20.30 9.70 -20 -2 28 6.70 6.90 -20 2 -28 9.10 8.40 20 2 28 13.50 13.70 20 -2 -28 -4.70 11.20 -20 -2 -28 27.30 10.80 20 2 -28 6.20 12.20 20 -2 28 3.00 12.30 20 -2 28 19.90 13.10 -20 2 28 27.50 11.10 20 -3 -28 13.00 11.60 -20 -3 28 -4.90 5.70 20 3 28 1.20 12.00 -20 3 -28 -3.10 6.40 -20 -3 28 -6.70 6.30 -20 3 28 5.10 7.50 -20 -3 -28 0.60 8.90 20 -3 28 -10.40 9.20 20 -3 28 -17.90 11.50 20 3 -28 -22.80 11.70 20 4 28 31.90 14.50 -20 -4 28 40.20 10.00 20 -4 -28 27.50 11.30 -20 -4 28 21.90 9.40 -20 4 -28 3.70 8.80 20 -4 -28 30.70 13.50 -20 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12.70 10.50 21 -7 28 -19.20 16.80 -21 7 28 13.80 12.60 21 7 -28 29.30 17.00 22 0 -28 0.10 10.80 22 0 28 13.20 13.10 -22 0 -28 8.50 8.90 -22 0 28 0.80 7.00 22 -1 -28 5.80 12.30 22 1 28 13.40 13.50 -22 -1 28 8.20 7.50 -22 1 -28 11.40 9.20 22 1 -28 -0.60 12.60 -22 -1 -28 18.80 10.10 -22 1 28 24.60 9.90 22 -1 28 25.30 13.30 -22 2 -28 3.80 8.00 22 -2 -28 -0.20 11.90 -22 -2 28 1.00 6.60 22 2 28 7.60 11.70 22 -2 28 -6.30 11.30 22 -2 28 1.10 10.80 -22 2 28 -3.50 7.70 22 2 -28 -2.20 13.10 -22 -2 -28 15.30 9.70 22 3 28 92.79 21.30 -22 3 -28 78.49 14.90 22 -3 -28 71.79 18.10 -22 -3 28 82.89 14.80 22 3 -28 98.59 21.90 -22 -3 -28 101.09 17.50 22 -3 28 75.19 17.60 22 -3 28 66.19 17.30 -22 3 28 81.89 16.70 -22 -4 28 14.80 9.30 -22 4 -28 9.90 10.40 22 -4 -28 47.80 14.80 22 4 28 8.90 12.10 -22 -4 28 38.60 11.10 -22 4 28 54.69 15.40 -22 -4 -28 16.90 11.90 22 4 -28 48.50 19.50 22 -4 28 32.20 15.40 22 -4 28 59.09 16.90 -22 -5 28 -4.80 7.80 22 -5 -28 -2.70 9.90 -22 5 -28 9.30 9.10 -22 -5 28 14.50 8.60 22 5 28 33.90 15.90 -22 -5 -28 19.00 10.60 22 -5 28 18.70 14.50 22 -5 28 13.00 12.90 -22 5 28 6.90 10.00 22 5 -28 3.00 15.40 -22 -6 28 2.70 7.50 22 -6 -28 -2.30 11.80 -22 6 -28 -8.40 7.60 22 6 28 26.00 15.40 -22 -6 28 -4.70 7.20 22 -6 28 -14.10 15.00 -22 6 28 -11.20 8.80 -22 -6 -28 6.30 10.60 22 6 -28 -7.40 14.20 -22 7 -28 22.80 12.00 22 7 28 19.90 15.40 22 -7 -28 -5.90 11.70 -22 -7 28 23.80 12.20 -22 7 28 6.20 11.70 -22 -7 -28 10.40 10.90 22 7 -28 35.50 20.80 22 -7 28 10.80 17.80 -23 0 28 111.59 17.70 23 0 -28 92.09 18.60 -23 0 -28 91.79 17.00 23 0 28 90.79 19.60 23 -1 -28 1.50 12.70 23 1 28 8.00 12.70 -23 -1 28 -0.70 6.80 -23 1 -28 14.80 10.60 -23 1 28 10.00 9.60 -23 -1 -28 15.00 10.00 23 -1 28 2.00 11.00 23 1 -28 3.70 12.00 -23 -2 28 -4.30 6.10 23 -2 -28 4.20 12.70 -23 2 -28 -6.60 7.70 23 2 28 13.10 15.40 -23 -2 -28 12.50 9.00 -23 2 28 15.80 9.40 23 -2 28 -2.00 11.20 23 2 -28 -4.10 11.60 23 -2 28 -12.70 11.90 -23 3 -28 89.59 16.70 -23 -3 28 106.59 16.40 23 3 28 93.49 21.50 23 -3 -28 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27.80 17.30 -10 -2 -41 -9.20 8.50 -10 3 -41 9.30 9.70 -10 -3 41 -2.90 8.30 10 3 41 14.90 12.70 10 3 -41 12.10 18.00 10 -3 41 -5.60 12.10 -10 -3 -41 5.40 10.90 11 0 41 -5.40 11.30 -11 0 -41 15.30 10.00 -11 -1 41 11.10 9.60 11 1 41 17.60 11.00 -11 1 -41 1.00 8.50 11 1 -41 -5.90 15.90 11 -1 41 -2.60 9.30 -11 -1 -41 1.00 8.80 -11 -2 41 66.79 16.40 -11 2 -41 75.49 15.50 11 2 41 46.40 14.80 11 2 -41 55.19 20.30 -11 -2 -41 103.89 17.80 11 -2 41 69.09 18.10 -11 3 -41 9.90 10.00 11 3 41 2.90 11.40 11 3 -41 21.10 18.40 -12 0 -41 -3.70 8.30 12 0 41 2.80 11.40 12 1 41 25.40 12.80 -12 1 -41 1.80 8.20 -12 -1 -41 -3.10 8.60 12 1 -41 -12.90 14.70 12 -1 41 17.30 12.10 12 2 41 2.10 9.60 -12 -2 41 -0.60 8.60 -12 2 -41 3.70 8.80 -12 -2 -41 -4.20 8.50 12 2 -41 -2.30 17.20 12 -2 41 1.70 12.80 -13 0 -41 0.30 8.10 13 0 41 -3.20 10.30 -13 1 -41 11.30 9.50 13 1 41 5.00 12.90 13 -1 41 -0.10 10.50 13 1 -41 19.80 16.90 -13 -1 -41 18.70 10.40 14 0 41 13.20 14.70 14 0 -41 62.99 27.70 -14 0 -41 17.00 9.60 0 0 42 -6.90 9.10 0 -1 42 10.90 10.80 0 -1 -42 10.80 8.90 0 1 42 -10.40 9.20 0 -2 42 341.77 35.40 0 2 42 262.57 32.50 0 -2 -42 278.77 29.50 0 3 42 0.30 10.40 0 -3 42 4.00 10.80 0 -3 -42 2.00 9.00 0 3 -42 1.30 15.90 1 0 42 -10.60 9.10 -1 0 -42 16.20 9.50 -1 0 42 8.80 9.30 1 1 42 -4.70 10.00 -1 -1 42 -7.50 9.10 1 -1 -42 8.40 8.50 -1 -1 -42 -3.10 8.10 1 -1 42 2.40 10.90 -1 1 42 16.80 10.90 1 2 42 18.20 11.40 1 -2 -42 -12.20 7.30 -1 -2 42 6.20 10.60 -1 2 42 13.80 12.50 1 -2 42 -7.90 8.50 1 2 -42 14.10 16.70 -1 -2 -42 0.40 8.90 1 3 42 1.00 10.90 -1 -3 42 18.20 13.00 -1 3 -42 32.20 18.10 1 -3 -42 11.20 10.50 1 3 -42 20.10 17.00 -1 -3 -42 8.80 10.20 1 -3 42 26.90 13.60 -1 3 42 -6.30 9.80 -2 0 42 3.40 9.90 2 0 42 -2.20 9.90 -2 0 -42 14.00 8.60 -2 -1 42 20.30 12.90 2 -1 -42 48.10 15.30 2 1 42 27.40 12.00 -2 1 42 30.90 13.90 2 -1 42 63.09 15.60 -2 -1 -42 49.60 13.40 -2 -2 42 0.00 9.90 2 -2 -42 4.40 8.90 2 2 42 -5.30 9.10 2 2 -42 25.10 16.70 2 -2 42 11.70 9.60 -2 2 42 12.10 11.60 -2 -2 -42 16.80 10.20 2 -3 -42 3.20 9.50 -2 3 -42 5.00 15.20 -2 -3 42 18.50 11.80 2 3 42 -7.10 10.40 2 -3 42 15.50 13.40 -2 3 42 6.60 10.60 2 3 -42 20.30 17.00 -2 -3 -42 -4.00 9.00 3 0 42 49.70 15.60 -3 0 42 28.30 12.60 -3 0 -42 36.30 11.00 -3 -1 42 14.10 9.80 3 1 42 19.20 11.50 -3 1 42 18.10 11.70 3 -1 42 13.60 12.20 -3 -1 -42 9.40 9.00 3 -2 -42 -5.20 9.30 3 2 42 15.90 12.10 -3 -2 42 11.10 10.70 -3 -2 -42 13.60 9.90 3 2 -42 15.90 14.80 -3 2 42 1.50 10.00 3 -2 42 0.90 10.70 -3 -3 42 4.00 10.70 -3 3 -42 1.10 16.70 3 3 42 3.30 9.90 3 -3 -42 -10.60 8.40 3 3 -42 23.10 16.50 3 -3 42 14.10 13.00 -3 -3 -42 -24.10 7.80 4 0 42 2.30 9.70 -4 0 -42 16.40 10.10 -4 0 42 2.50 9.30 -4 -1 42 1.90 10.20 4 1 42 18.10 12.80 -4 1 -42 -0.60 7.20 -4 -1 -42 -1.40 8.70 4 -1 42 3.00 10.40 -4 1 42 2.40 10.00 4 2 42 11.20 11.40 4 -2 -42 23.60 10.50 -4 -2 42 35.90 12.40 -4 2 42 48.40 14.70 -4 -2 -42 31.10 11.60 4 2 -42 25.20 16.90 4 -2 42 21.60 12.70 -4 -3 42 10.70 11.80 4 3 42 8.10 10.00 -4 3 -42 21.30 16.10 4 -3 -42 -0.80 8.80 4 3 -42 12.90 16.00 -4 -3 -42 -1.40 9.50 4 -3 42 9.90 13.90 5 0 42 12.80 12.10 -5 0 42 8.10 11.00 -5 0 -42 26.20 11.10 -5 1 -42 13.10 9.60 -5 -1 42 17.30 12.40 5 1 42 18.80 11.90 -5 1 42 10.60 10.60 5 -1 42 4.50 10.50 -5 -1 -42 6.10 9.00 -5 -2 42 22.30 10.90 5 2 42 2.60 10.00 5 2 -42 9.40 15.50 -5 -2 -42 3.40 8.90 5 -2 42 6.00 10.70 -5 -3 42 13.70 10.60 5 -3 -42 18.00 10.20 5 3 42 0.70 10.70 -5 3 -42 -20.00 14.30 -5 -3 -42 26.40 11.20 5 -3 42 7.30 12.60 5 3 -42 15.10 18.20 6 0 42 -2.20 10.30 -6 0 42 -9.00 9.00 -6 0 -42 -8.60 7.40 -6 1 -42 20.20 10.50 6 1 42 1.60 10.40 -6 -1 42 17.10 10.10 6 -1 42 11.60 13.10 -6 1 42 -5.90 9.80 -6 -1 -42 -1.90 8.80 6 2 42 48.80 15.70 -6 -2 42 29.90 12.20 6 2 -42 69.29 22.10 6 -2 42 57.59 16.90 -6 -2 -42 70.49 15.90 6 -3 -42 4.50 10.00 -6 3 -42 -42.00 17.20 -6 -3 42 24.90 12.60 6 3 42 -1.90 9.80 6 -3 42 -14.50 9.90 -6 -3 -42 -3.60 9.10 6 3 -42 15.60 16.90 -7 0 -42 11.00 9.40 7 0 42 12.80 11.20 -7 0 42 -1.60 9.00 -7 -1 42 -9.50 7.80 -7 1 -42 10.60 9.50 7 1 42 6.60 11.20 7 -1 42 10.90 12.20 -7 -1 -42 15.50 10.00 -7 -2 42 -2.80 9.30 -7 2 -42 0.90 8.80 7 2 42 -0.90 10.90 -7 -2 -42 -2.00 8.40 7 2 -42 25.50 16.10 7 -2 42 -3.90 9.90 7 3 42 0.70 11.40 -7 -3 42 18.20 12.30 7 -3 -42 13.10 13.20 7 3 -42 3.90 16.00 -7 -3 -42 14.10 10.40 7 -3 42 10.00 16.30 8 0 42 -4.30 9.30 -8 0 -42 2.20 9.40 -8 0 42 1.50 8.90 -8 -1 42 29.50 12.00 8 1 42 26.00 13.40 -8 1 -42 4.40 8.60 -8 -1 -42 27.30 12.20 8 -1 42 43.30 14.90 8 2 42 -3.40 10.90 -8 -2 42 -10.20 8.00 -8 2 -42 4.80 8.90 8 -2 42 -5.00 10.60 8 2 -42 -2.10 13.90 -8 -2 -42 15.10 10.50 9 0 42 14.20 12.30 -9 0 -42 -1.20 8.10 -9 -1 42 -6.30 7.70 9 1 42 6.00 10.80 -9 1 -42 1.80 7.20 9 -1 42 0.40 10.70 9 1 -42 5.20 17.00 -9 -1 -42 3.20 9.40 9 2 42 12.30 13.20 -9 2 -42 -6.70 8.10 -9 -2 42 -10.00 8.40 9 -2 42 -4.70 11.90 9 2 -42 11.30 15.40 -9 -2 -42 -6.70 8.50 10 0 42 12.90 13.30 -10 0 -42 35.60 12.10 10 1 42 8.40 11.70 -10 -1 42 -4.30 7.90 -10 1 -42 3.90 8.40 10 -1 42 -1.00 11.10 10 1 -42 -3.30 14.50 -10 -1 -42 -2.00 8.30 10 2 -42 24.30 18.00 -11 0 -42 9.10 9.40 11 0 42 2.00 13.30 -11 1 -42 17.70 9.80 11 1 42 23.60 14.50 -11 -1 -42 12.20 10.90 11 1 -42 4.60 15.70 0 0 43 1.00 11.00 0 -1 43 -11.10 8.90 0 1 43 -3.90 9.90 0 -1 -43 -8.50 8.00 0 2 43 0.30 10.00 0 -2 43 -13.90 9.00 0 -2 -43 7.70 10.40 1 0 43 -6.80 9.60 -1 0 43 9.00 10.70 1 -1 -43 16.90 11.90 -1 -1 43 22.30 13.30 1 1 43 18.40 12.70 -1 1 43 3.80 11.30 -1 -1 -43 12.40 10.30 1 -1 43 -0.20 9.10 1 -2 -43 -13.20 7.90 1 2 43 15.90 11.00 -1 -2 43 1.20 10.30 -1 -2 -43 19.50 10.10 -1 2 43 -6.70 9.10 1 -2 43 -0.80 9.60 2 0 43 -1.50 9.80 -2 0 43 13.20 11.10 -2 0 -43 3.60 9.00 -2 -1 43 14.60 11.70 2 1 43 3.40 9.00 -2 1 43 9.40 11.40 2 -1 43 1.20 9.30 -2 -1 -43 2.80 8.40 -2 -2 43 15.80 11.60 2 -2 -43 5.40 10.10 2 2 43 -5.90 9.10 2 -2 43 -7.80 10.50 -2 2 43 9.60 11.60 -2 -2 -43 3.40 9.10 3 0 43 3.10 9.20 -3 0 43 6.80 10.00 -3 0 -43 15.90 9.60 -3 -1 43 14.10 12.00 3 1 43 21.40 12.70 -3 1 43 8.50 11.20 -3 -1 -43 -9.90 7.90 3 -1 43 -1.40 10.30 3 -2 -43 -8.50 9.10 3 2 43 6.50 11.70 -3 -2 43 -1.60 9.40 -3 -2 -43 5.10 8.60 3 -2 43 8.90 11.40 -3 2 43 -11.20 9.70 3 2 -43 -8.70 19.20 4 0 43 -0.50 10.40 -4 0 -43 -6.00 7.60 -4 0 43 1.80 8.80 4 1 43 16.80 12.10 -4 -1 43 11.90 10.90 4 -1 43 4.10 11.50 -4 -1 -43 14.30 10.50 -4 1 43 10.10 10.00 4 2 43 1.70 11.30 -4 -2 43 6.40 10.00 -4 2 43 7.50 9.80 -4 -2 -43 4.80 9.10 4 2 -43 5.00 15.50 4 -2 43 -2.60 10.60 -5 0 -43 -8.50 7.80 5 0 43 8.10 11.50 -5 0 43 1.20 9.60 5 1 43 -6.70 10.70 -5 1 -43 4.90 9.50 -5 -1 43 -4.90 8.80 -5 -1 -43 10.20 10.00 5 -1 43 -4.60 10.30 -5 1 43 11.20 10.10 5 2 43 2.30 9.80 -5 -2 43 7.80 9.90 -5 -2 -43 -7.30 8.50 5 2 -43 -4.90 15.90 5 -2 43 6.10 12.50 -6 0 43 5.10 9.90 6 0 43 5.60 13.00 -6 0 -43 -2.80 7.60 6 1 43 -5.70 10.10 -6 -1 43 0.00 10.00 -6 1 -43 4.40 9.70 -6 -1 -43 4.90 8.70 6 -1 43 -5.80 10.20 -6 1 43 15.40 11.30 7 0 43 -5.40 9.20 -7 0 -43 0.90 8.90 -7 0 43 -4.70 9.90 7 1 43 3.80 11.00 -7 1 -43 7.10 9.40 -7 -1 43 -9.20 9.30 -7 -1 -43 -0.40 8.60 7 -1 43 9.70 12.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 28184 #===END data_L_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H47 O0.33 P' _chemical_formula_weight 455.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.350(3) _cell_length_b 19.350(3) _cell_length_c 38.469(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12474(5) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3974 _cell_measurement_theta_min 2.105 _cell_measurement_theta_max 20.1535 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4608 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scan' _diffrn_reflns_number 47305 _diffrn_reflns_av_R_equivalents 0.1720 _diffrn_reflns_av_sigmaI/netI 0.1200 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.63 _reflns_number_total 6406 _reflns_number_gt 2971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'Apex2 v2.1-4 (Bruker, 2007)' _computing_data_reduction 'Apex2 v2.1-4 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows v2.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1095P)^2^+44.1865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6406 _refine_ls_number_parameters 327 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1755 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.2476 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.67972(6) 1.08150(6) 0.08368(3) 0.0343(3) Uani 1 1 d . . . C1 C 0.6073(2) 0.8470(2) 0.08883(10) 0.0356(9) Uani 1 1 d . . . C2 C 0.6239(2) 0.8048(2) 0.06397(10) 0.0385(9) Uani 1 1 d . A . H2 H 0.5806 0.7594 0.0534 0.046 Uiso 1 1 calc R . . C3 C 0.7013(3) 0.8268(2) 0.05404(10) 0.0412(10) Uani 1 1 d D . . C4 C 0.7636(2) 0.8935(2) 0.06992(10) 0.0389(9) Uani 1 1 d . A . H4 H 0.8169 0.9088 0.0638 0.047 Uiso 1 1 calc R . . C5 C 0.7504(2) 0.9389(2) 0.09459(10) 0.0330(8) Uani 1 1 d . . . C6 C 0.6716(2) 0.9158(2) 0.10387(10) 0.0326(8) Uani 1 1 d . A . C7 C 0.5210(2) 0.8155(2) 0.09991(11) 0.0400(9) Uani 1 1 d . . . H7 H 0.5174 0.8612 0.1100 0.048 Uiso 1 1 calc R . . C8 C 0.4953(2) 0.7513(3) 0.12825(12) 0.0472(11) Uani 1 1 d . . . H8A H 0.4962 0.7047 0.1188 0.071 Uiso 1 1 calc R . . H8B H 0.4412 0.7355 0.1361 0.071 Uiso 1 1 calc R . . H8C H 0.5322 0.7728 0.1480 0.071 Uiso 1 1 calc R . . C9 C 0.4606(2) 0.7810(3) 0.06973(12) 0.0492(11) Uani 1 1 d . . . H9A H 0.4778 0.8201 0.0508 0.074 Uiso 1 1 calc R . . H9B H 0.4078 0.7691 0.0780 0.074 Uiso 1 1 calc R . . H9C H 0.4577 0.7319 0.0612 0.074 Uiso 1 1 calc R . . C10 C 0.7107(4) 0.7756(4) 0.02594(17) 0.0343(16) Uani 0.822(11) 1 d PD A 1 H10 H 0.6746 0.7693 0.0061 0.041 Uiso 0.822(11) 1 calc PR A 1 C11 C 0.6850(11) 0.6925(5) 0.0408(4) 0.047(3) Uani 0.822(11) 1 d PD A 1 H11A H 0.6921 0.6602 0.0230 0.070 Uiso 0.822(11) 1 calc PR A 1 H11B H 0.6288 0.6664 0.0476 0.070 Uiso 0.822(11) 1 calc PR A 1 H11C H 0.7179 0.6978 0.0611 0.070 Uiso 0.822(11) 1 calc PR A 1 C12 C 0.7958(3) 0.8129(3) 0.01219(14) 0.0421(16) Uani 0.822(11) 1 d PD A 1 H12A H 0.8129 0.8667 0.0034 0.063 Uiso 0.822(11) 1 calc PR A 1 H12B H 0.7978 0.7800 -0.0067 0.063 Uiso 0.822(11) 1 calc PR A 1 H12C H 0.8315 0.8161 0.0310 0.063 Uiso 0.822(11) 1 calc PR A 1 C10' C 0.7411(18) 0.7865(18) 0.0343(6) 0.046(9) Uani 0.178(11) 1 d PD A 2 H10' H 0.7981 0.8105 0.0417 0.055 Uiso 0.178(11) 1 calc PR A 2 C11' C 0.698(6) 0.696(2) 0.0392(17) 0.047(3) Uani 0.178(11) 1 d PD A 2 H11D H 0.7165 0.6727 0.0214 0.070 Uiso 0.178(11) 1 calc PR A 2 H11E H 0.6406 0.6744 0.0368 0.070 Uiso 0.178(11) 1 calc PR A 2 H11F H 0.7101 0.6838 0.0623 0.070 Uiso 0.178(11) 1 calc PR A 2 C12' C 0.737(2) 0.8075(18) -0.0033(6) 0.064(10) Uani 0.178(11) 1 d PD A 2 H12D H 0.7353 0.7659 -0.0184 0.096 Uiso 0.178(11) 1 calc PR A 2 H12E H 0.7844 0.8588 -0.0089 0.096 Uiso 0.178(11) 1 calc PR A 2 H12F H 0.6890 0.8113 -0.0069 0.096 Uiso 0.178(11) 1 calc PR A 2 C13 C 0.8213(2) 1.0081(2) 0.11187(10) 0.0363(9) Uani 1 1 d . A . H13 H 0.8013 1.0400 0.1244 0.044 Uiso 1 1 calc R . . C14 C 0.8577(3) 0.9778(3) 0.13911(12) 0.0493(11) Uani 1 1 d . . . H14A H 0.8181 0.9485 0.1573 0.074 Uiso 1 1 calc R A . H14B H 0.9046 1.0232 0.1495 0.074 Uiso 1 1 calc R . . H14C H 0.8735 0.9422 0.1280 0.074 Uiso 1 1 calc R . . C15 C 0.8845(2) 1.0637(3) 0.08594(12) 0.0490(11) Uani 1 1 d . . . H15A H 0.9100 1.0361 0.0753 0.074 Uiso 1 1 calc R A . H15B H 0.9248 1.1115 0.0981 0.074 Uiso 1 1 calc R . . H15C H 0.8592 1.0791 0.0678 0.074 Uiso 1 1 calc R . . C16 C 0.6554(2) 0.9602(2) 0.13188(10) 0.0321(8) Uani 1 1 d . . . C17 C 0.6435(2) 0.9284(2) 0.16550(10) 0.0372(9) Uani 1 1 d . A . H17 H 0.6476 0.8821 0.1693 0.045 Uiso 1 1 calc R . . C18 C 0.6260(2) 0.9622(2) 0.19342(10) 0.0389(9) Uani 1 1 d . . . H18 H 0.6189 0.9396 0.2160 0.047 Uiso 1 1 calc R A . C19 C 0.6191(2) 1.0296(2) 0.18801(11) 0.0414(10) Uani 1 1 d . A . H19 H 0.6056 1.0528 0.2067 0.050 Uiso 1 1 calc R . . C20 C 0.6321(2) 1.0624(2) 0.15506(11) 0.0401(10) Uani 1 1 d . . . H20 H 0.6274 1.1086 0.1517 0.048 Uiso 1 1 calc R A . C21 C 0.6518(2) 1.0308(2) 0.12634(10) 0.0340(9) Uani 1 1 d . A . C22 C 0.7431(2) 1.1921(2) 0.09345(11) 0.0407(10) Uani 1 1 d . . . C23 C 0.7832(2) 1.2303(2) 0.05848(12) 0.0474(11) Uani 1 1 d . . . H23A H 0.8297 1.2833 0.0637 0.057 Uiso 1 1 calc R . . H23B H 0.8043 1.1973 0.0486 0.057 Uiso 1 1 calc R . . C24 C 0.7349(3) 1.2420(2) 0.02997(12) 0.0484(11) Uani 1 1 d . . . H24A H 0.7711 1.2696 0.0102 0.058 Uiso 1 1 calc R . . H24B H 0.7166 1.2780 0.0391 0.058 Uiso 1 1 calc R . . C25 C 0.6621(2) 1.1668(2) 0.01605(11) 0.0443(10) Uani 1 1 d . . . H25A H 0.6780 1.1265 0.0110 0.053 Uiso 1 1 calc R . . H25B H 0.6458 1.1801 -0.0062 0.053 Uiso 1 1 calc R . . C26 C 0.5898(2) 1.1294(2) 0.04036(11) 0.0397(9) Uani 1 1 d . . . H26A H 0.5412 1.1071 0.0258 0.048 Uiso 1 1 calc R . . H26B H 0.5909 1.1729 0.0544 0.048 Uiso 1 1 calc R . . C27 C 0.5806(2) 1.0636(2) 0.06555(11) 0.0378(9) Uani 1 1 d . . . C28 C 0.8100(3) 1.2010(3) 0.11806(12) 0.0502(11) Uani 1 1 d . . . H28A H 0.8480 1.2577 0.1219 0.075 Uiso 1 1 calc R . . H28B H 0.8378 1.1755 0.1076 0.075 Uiso 1 1 calc R . . H28C H 0.7868 1.1753 0.1403 0.075 Uiso 1 1 calc R . . C29 C 0.7051(3) 1.2382(2) 0.10908(12) 0.0476(11) Uani 1 1 d . . . H29A H 0.6884 1.2204 0.1330 0.071 Uiso 1 1 calc R . . H29B H 0.6586 1.2283 0.0952 0.071 Uiso 1 1 calc R . . H29C H 0.7441 1.2955 0.1090 0.071 Uiso 1 1 calc R . . C30 C 0.5495(3) 0.9860(2) 0.04529(11) 0.0461(10) Uani 1 1 d . . . H30A H 0.5494 0.9451 0.0604 0.069 Uiso 1 1 calc R . . H30B H 0.5840 0.9948 0.0252 0.069 Uiso 1 1 calc R . . H30C H 0.4950 0.9681 0.0373 0.069 Uiso 1 1 calc R . . C31 C 0.5181(2) 1.0523(3) 0.09278(11) 0.0487(11) Uani 1 1 d . . . H31A H 0.4694 1.0437 0.0811 0.073 Uiso 1 1 calc R . . H31B H 0.5390 1.1001 0.1074 0.073 Uiso 1 1 calc R . . H31C H 0.5058 1.0060 0.1073 0.073 Uiso 1 1 calc R . . O1 O 0.0000 1.0000 0.0207(8) 0.215(18) Uani 0.50 3 d SP A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0322(5) 0.0300(5) 0.0414(6) 0.0001(4) 0.0008(4) 0.0162(4) C1 0.038(2) 0.0310(19) 0.036(2) -0.0011(17) -0.0007(17) 0.0162(16) C2 0.043(2) 0.033(2) 0.035(2) -0.0032(17) 0.0018(18) 0.0162(18) C3 0.054(2) 0.034(2) 0.036(2) 0.0033(17) 0.0099(19) 0.0222(19) C4 0.041(2) 0.038(2) 0.042(2) 0.0057(18) 0.0077(18) 0.0227(18) C5 0.0340(19) 0.0261(18) 0.038(2) 0.0049(16) 0.0048(16) 0.0140(15) C6 0.0339(19) 0.0329(19) 0.033(2) 0.0014(16) 0.0009(16) 0.0181(16) C7 0.036(2) 0.037(2) 0.045(2) -0.0029(18) -0.0001(18) 0.0162(18) C8 0.035(2) 0.047(2) 0.054(3) 0.005(2) 0.007(2) 0.0158(19) C9 0.041(2) 0.041(2) 0.056(3) -0.002(2) -0.007(2) 0.0143(19) C10 0.037(3) 0.038(3) 0.030(4) -0.011(2) -0.006(3) 0.020(3) C11 0.062(8) 0.043(2) 0.043(3) -0.004(2) 0.001(3) 0.033(3) C12 0.042(3) 0.049(3) 0.041(3) -0.003(2) 0.000(2) 0.026(2) C10' 0.04(2) 0.042(15) 0.023(16) -0.011(12) -0.004(14) 0.000(15) C11' 0.062(8) 0.043(2) 0.043(3) -0.004(2) 0.001(3) 0.033(3) C12' 0.11(3) 0.066(18) 0.033(16) 0.003(13) 0.007(16) 0.054(19) C13 0.0326(19) 0.0331(19) 0.042(2) 0.0029(17) 0.0010(17) 0.0151(16) C14 0.047(2) 0.046(2) 0.057(3) -0.001(2) -0.008(2) 0.024(2) C15 0.032(2) 0.044(2) 0.061(3) 0.006(2) 0.007(2) 0.0126(19) C16 0.0260(17) 0.0310(18) 0.039(2) -0.0006(16) 0.0014(16) 0.0143(15) C17 0.037(2) 0.038(2) 0.040(2) 0.0001(18) -0.0028(18) 0.0210(17) C18 0.041(2) 0.050(2) 0.032(2) -0.0027(18) -0.0036(17) 0.0277(19) C19 0.040(2) 0.051(2) 0.039(2) -0.0065(19) -0.0029(18) 0.027(2) C20 0.040(2) 0.039(2) 0.047(3) -0.0045(19) -0.0026(19) 0.0244(18) C21 0.0306(19) 0.035(2) 0.039(2) -0.0009(17) -0.0035(16) 0.0185(16) C22 0.040(2) 0.034(2) 0.048(3) -0.0027(18) -0.0061(19) 0.0182(18) C23 0.038(2) 0.032(2) 0.065(3) 0.008(2) 0.004(2) 0.0128(18) C24 0.042(2) 0.039(2) 0.060(3) 0.010(2) -0.002(2) 0.0182(19) C25 0.043(2) 0.043(2) 0.047(3) 0.005(2) 0.001(2) 0.0219(19) C26 0.036(2) 0.038(2) 0.044(2) -0.0022(18) -0.0028(18) 0.0184(18) C27 0.034(2) 0.036(2) 0.043(2) 0.0026(17) 0.0000(18) 0.0166(17) C28 0.044(2) 0.040(2) 0.066(3) -0.001(2) -0.014(2) 0.021(2) C29 0.050(2) 0.037(2) 0.060(3) -0.011(2) -0.011(2) 0.025(2) C30 0.047(2) 0.036(2) 0.049(3) 0.0005(19) -0.007(2) 0.0155(19) C31 0.032(2) 0.072(3) 0.042(3) 0.007(2) 0.0011(18) 0.026(2) O1 0.141(11) 0.141(11) 0.36(5) 0.000 0.000 0.070(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C21 1.849(4) . ? P1 C22 1.898(4) . ? P1 C27 1.903(4) . ? C1 C2 1.394(5) . ? C1 C6 1.413(5) . ? C1 C7 1.524(5) . ? C2 C3 1.391(6) . ? C3 C4 1.392(6) . ? C3 C10 1.538(6) . ? C3 C10' 1.542(18) . ? C4 C5 1.400(5) . ? C5 C6 1.405(5) . ? C5 C13 1.510(5) . ? C6 C16 1.505(5) . ? C7 C8 1.536(6) . ? C7 C9 1.543(6) . ? C10 C12 1.525(7) . ? C10 C11 1.536(8) . ? C10' C12' 1.516(16) . ? C10' C11' 1.524(17) . ? C13 C15 1.527(5) . ? C13 C14 1.533(5) . ? C16 C17 1.400(5) . ? C16 C21 1.420(5) . ? C17 C18 1.384(5) . ? C18 C19 1.393(5) . ? C19 C20 1.383(6) . ? C20 C21 1.405(5) . ? C22 C29 1.534(6) . ? C22 C28 1.544(6) . ? C22 C23 1.544(6) . ? C23 C24 1.529(6) . ? C24 C25 1.529(6) . ? C25 C26 1.531(5) . ? C26 C27 1.539(5) . ? C27 C30 1.524(5) . ? C27 C31 1.531(5) . ? O1 O1 1.59(6) 10_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 P1 C22 105.98(18) . . ? C21 P1 C27 103.17(17) . . ? C22 P1 C27 107.56(17) . . ? C2 C1 C6 118.7(4) . . ? C2 C1 C7 119.0(3) . . ? C6 C1 C7 122.3(3) . . ? C3 C2 C1 122.5(4) . . ? C2 C3 C4 117.7(4) . . ? C2 C3 C10 116.9(4) . . ? C4 C3 C10 125.4(4) . . ? C2 C3 C10' 135.6(13) . . ? C4 C3 C10' 105.3(12) . . ? C10 C3 C10' 22.8(10) . . ? C3 C4 C5 122.3(4) . . ? C4 C5 C6 118.8(3) . . ? C4 C5 C13 119.0(3) . . ? C6 C5 C13 122.1(3) . . ? C5 C6 C1 120.0(3) . . ? C5 C6 C16 120.2(3) . . ? C1 C6 C16 119.6(3) . . ? C1 C7 C8 111.6(3) . . ? C1 C7 C9 113.9(3) . . ? C8 C7 C9 108.4(3) . . ? C12 C10 C11 109.4(8) . . ? C12 C10 C3 112.7(4) . . ? C11 C10 C3 109.5(8) . . ? C12' C10' C11' 111(2) . . ? C12' C10' C3 103.2(18) . . ? C11' C10' C3 113(4) . . ? C5 C13 C15 112.9(3) . . ? C5 C13 C14 110.4(3) . . ? C15 C13 C14 110.9(3) . . ? C17 C16 C21 119.0(3) . . ? C17 C16 C6 116.5(3) . . ? C21 C16 C6 124.5(3) . . ? C18 C17 C16 122.4(4) . . ? C17 C18 C19 119.1(4) . . ? C20 C19 C18 119.1(4) . . ? C19 C20 C21 123.2(4) . . ? C20 C21 C16 117.1(3) . . ? C20 C21 P1 122.6(3) . . ? C16 C21 P1 120.1(3) . . ? C29 C22 C28 108.3(3) . . ? C29 C22 C23 109.6(3) . . ? C28 C22 C23 106.8(3) . . ? C29 C22 P1 120.4(3) . . ? C28 C22 P1 106.2(3) . . ? C23 C22 P1 104.7(3) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 116.8(3) . . ? C24 C25 C26 115.2(4) . . ? C25 C26 C27 118.4(3) . . ? C30 C27 C31 108.3(3) . . ? C30 C27 C26 108.6(3) . . ? C31 C27 C26 107.7(3) . . ? C30 C27 P1 103.5(3) . . ? C31 C27 P1 115.3(3) . . ? C26 C27 P1 113.1(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.629 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.080 #===END data_L_8 _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'L_8' _chemical_melting_point 402 _chemical_formula_moiety ? _chemical_formula_sum 'C32 H49 P' _chemical_formula_weight 464.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6727(18) _cell_length_b 14.184(3) _cell_length_c 23.006(5) _cell_angle_alpha 90 _cell_angle_beta 92.223(3) _cell_angle_gamma 90 _cell_volume 2827.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2940 _cell_measurement_theta_min 2.281 _cell_measurement_theta_max 22.376 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_F_000 1024 _exptl_transmission_factor_min 0.8016 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.114 _shelx_estimated_absorpt_T_min 0.961 _shelx_estimated_absorpt_T_max 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31809 _diffrn_reflns_av_unetI/netI 0.1076 _diffrn_reflns_av_R_equivalents 0.1303 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.687 _diffrn_reflns_theta_max 27.113 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6226 _reflns_number_gt 3680 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3367P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6226 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.33677(7) 0.65104(5) 0.34350(3) 0.01652(18) Uani 1 1 d . . . . . C1 C 0.4554(3) 0.75509(18) 0.32605(11) 0.0175(6) Uani 1 1 d . . . . . C2 C 0.5008(3) 0.81756(19) 0.37172(11) 0.0179(6) Uani 1 1 d . . . . . C3 C 0.6060(3) 0.8896(2) 0.36102(11) 0.0225(6) Uani 1 1 d . . . . . H3 H 0.637369 0.930866 0.391762 0.027 Uiso 1 1 calc R U . . . C4 C 0.6657(3) 0.9021(2) 0.30619(12) 0.0252(6) Uani 1 1 d . . . . . H4 H 0.738146 0.950901 0.299885 0.030 Uiso 1 1 calc R U . . . C5 C 0.6194(3) 0.8433(2) 0.26118(11) 0.0240(6) Uani 1 1 d . . . . . H5 H 0.658200 0.852037 0.223508 0.029 Uiso 1 1 calc R U . . . C6 C 0.5162(3) 0.7717(2) 0.27115(11) 0.0210(6) Uani 1 1 d . . . . . H6 H 0.484819 0.731878 0.239656 0.025 Uiso 1 1 calc R U . . . C7 C 0.4435(3) 0.80969(19) 0.43276(10) 0.0183(6) Uani 1 1 d . . . . . C8 C 0.5134(3) 0.74419(18) 0.47139(11) 0.0191(6) Uani 1 1 d . . . . . C9 C 0.6551(3) 0.68832(19) 0.45583(11) 0.0209(6) Uani 1 1 d . . . . . H9 H 0.663635 0.691120 0.412645 0.025 Uiso 1 1 calc R U . . . C10 C 0.7997(3) 0.7338(2) 0.48351(13) 0.0316(7) Uani 1 1 d . . . . . H10A H 0.808138 0.798932 0.469722 0.047 Uiso 1 1 calc R U . . . H10B H 0.890970 0.698129 0.472626 0.047 Uiso 1 1 calc R U . . . H10C H 0.792917 0.733612 0.525928 0.047 Uiso 1 1 calc R U . . . C11 C 0.6456(3) 0.5843(2) 0.47330(12) 0.0273(7) Uani 1 1 d . . . . . H11A H 0.651685 0.579117 0.515803 0.041 Uiso 1 1 calc R U . . . H11B H 0.731440 0.549648 0.456918 0.041 Uiso 1 1 calc R U . . . H11C H 0.547578 0.557745 0.458359 0.041 Uiso 1 1 calc R U . . . C12 C 0.4561(3) 0.73478(19) 0.52697(11) 0.0201(6) Uani 1 1 d . . . . . H12 H 0.503088 0.690438 0.553049 0.024 Uiso 1 1 calc R U . . . C13 C 0.3333(3) 0.78780(19) 0.54542(11) 0.0203(6) Uani 1 1 d . . . . . C14 C 0.2676(3) 0.7712(2) 0.60516(11) 0.0227(6) Uani 1 1 d . . . . . H14 H 0.328216 0.719118 0.624366 0.027 Uiso 1 1 calc R U . . . C15 C 0.2814(3) 0.8570(2) 0.64420(12) 0.0288(7) Uani 1 1 d . . . . . H15A H 0.390188 0.875142 0.649166 0.043 Uiso 1 1 calc R U . . . H15B H 0.240429 0.842141 0.682224 0.043 Uiso 1 1 calc R U . . . H15C H 0.222596 0.909310 0.626477 0.043 Uiso 1 1 calc R U . . . C16 C 0.1003(4) 0.7389(2) 0.59843(13) 0.0376(8) Uani 1 1 d . . . . . H16A H 0.037785 0.789106 0.580192 0.056 Uiso 1 1 calc R U . . . H16B H 0.061208 0.724356 0.636813 0.056 Uiso 1 1 calc R U . . . H16C H 0.094412 0.682325 0.573968 0.056 Uiso 1 1 calc R U . . . C17 C 0.2723(3) 0.85617(19) 0.50778(11) 0.0209(6) Uani 1 1 d . . . . . H17 H 0.191828 0.895574 0.520633 0.025 Uiso 1 1 calc R U . . . C18 C 0.3250(3) 0.86888(18) 0.45188(11) 0.0187(6) Uani 1 1 d . . . . . C19 C 0.2622(3) 0.95056(19) 0.41500(11) 0.0222(6) Uani 1 1 d . . . . . H19 H 0.281948 0.936311 0.373373 0.027 Uiso 1 1 calc R U . . . C20 C 0.0879(3) 0.9671(2) 0.42009(12) 0.0285(7) Uani 1 1 d . . . . . H20A H 0.032938 0.907106 0.415154 0.043 Uiso 1 1 calc R U . . . H20B H 0.051584 1.011427 0.389876 0.043 Uiso 1 1 calc R U . . . H20C H 0.068119 0.993371 0.458499 0.043 Uiso 1 1 calc R U . . . C21 C 0.3478(4) 1.0420(2) 0.43152(13) 0.0330(7) Uani 1 1 d . . . . . H21A H 0.328556 1.058121 0.472022 0.050 Uiso 1 1 calc R U . . . H21B H 0.310793 1.093209 0.405990 0.050 Uiso 1 1 calc R U . . . H21C H 0.458835 1.033164 0.427090 0.050 Uiso 1 1 calc R U . . . C22 C 0.4256(3) 0.54647(19) 0.30413(11) 0.0198(6) Uani 1 1 d . . . . . C23 C 0.6018(3) 0.5571(2) 0.30951(12) 0.0241(6) Uani 1 1 d . . . . . H23A H 0.650600 0.497985 0.298003 0.036 Uiso 1 1 calc R U . . . H23B H 0.632842 0.571841 0.349904 0.036 Uiso 1 1 calc R U . . . H23C H 0.634371 0.608159 0.284070 0.036 Uiso 1 1 calc R U . . . C24 C 0.3831(3) 0.5280(2) 0.23987(12) 0.0261(7) Uani 1 1 d . . . . . H24A H 0.409369 0.583393 0.216795 0.039 Uiso 1 1 calc R U . . . H24B H 0.272140 0.515596 0.235271 0.039 Uiso 1 1 calc R U . . . H24C H 0.440625 0.473197 0.226444 0.039 Uiso 1 1 calc R U . . . C25 C 0.3904(3) 0.45694(19) 0.34083(12) 0.0232(6) Uani 1 1 d . . . . . H25A H 0.445576 0.403619 0.323200 0.028 Uiso 1 1 calc R U . . . H25B H 0.438761 0.466879 0.380044 0.028 Uiso 1 1 calc R U . . . C26 C 0.2247(3) 0.4242(2) 0.34940(12) 0.0254(6) Uani 1 1 d . . . . . H26A H 0.228089 0.359364 0.365263 0.031 Uiso 1 1 calc R U . . . H26B H 0.170249 0.421414 0.310808 0.031 Uiso 1 1 calc R U . . . C27 C 0.1290(3) 0.4860(2) 0.38981(12) 0.0244(6) Uani 1 1 d . . . . . H27A H 0.084972 0.445028 0.419820 0.029 Uiso 1 1 calc R U . . . H27B H 0.199051 0.531487 0.410017 0.029 Uiso 1 1 calc R U . . . C28 C -0.0020(3) 0.5405(2) 0.35938(12) 0.0261(7) Uani 1 1 d . . . . . H28A H -0.041131 0.586955 0.387356 0.031 Uiso 1 1 calc R U . . . H28B H -0.086897 0.495681 0.350147 0.031 Uiso 1 1 calc R U . . . C29 C 0.0340(3) 0.5933(2) 0.30338(12) 0.0244(6) Uani 1 1 d . . . . . H29A H -0.065406 0.614457 0.285222 0.029 Uiso 1 1 calc R U . . . H29B H 0.078688 0.547184 0.276471 0.029 Uiso 1 1 calc R U . . . C30 C 0.1428(3) 0.6796(2) 0.30649(12) 0.0223(6) Uani 1 1 d . . . . . C31 C 0.1474(3) 0.7213(2) 0.24519(12) 0.0312(7) Uani 1 1 d . . . . . H31A H 0.189851 0.674607 0.218807 0.047 Uiso 1 1 calc R U . . . H31B H 0.212684 0.777740 0.246009 0.047 Uiso 1 1 calc R U . . . H31C H 0.042625 0.738299 0.231527 0.047 Uiso 1 1 calc R U . . . C32 C 0.0727(3) 0.7544(2) 0.34563(13) 0.0294(7) Uani 1 1 d . . . . . H32A H -0.034277 0.766528 0.332519 0.044 Uiso 1 1 calc R U . . . H32B H 0.132598 0.812804 0.343525 0.044 Uiso 1 1 calc R U . . . H32C H 0.075097 0.731633 0.385872 0.044 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0158(3) 0.0189(4) 0.0149(3) -0.0006(3) -0.0001(2) -0.0011(3) C1 0.0171(13) 0.0199(14) 0.0154(13) 0.0030(11) 0.0014(10) 0.0013(11) C2 0.0180(13) 0.0194(14) 0.0162(13) 0.0033(11) -0.0003(10) 0.0016(11) C3 0.0290(15) 0.0218(15) 0.0170(13) -0.0030(11) 0.0025(11) -0.0035(12) C4 0.0262(15) 0.0249(16) 0.0250(15) 0.0021(12) 0.0063(12) -0.0075(12) C5 0.0265(14) 0.0309(16) 0.0150(13) 0.0036(12) 0.0048(11) -0.0034(13) C6 0.0224(14) 0.0264(16) 0.0142(13) -0.0017(11) -0.0005(11) -0.0018(12) C7 0.0212(14) 0.0205(14) 0.0133(13) 0.0002(11) 0.0022(10) -0.0072(11) C8 0.0211(14) 0.0210(15) 0.0150(13) -0.0017(11) -0.0014(11) -0.0079(11) C9 0.0226(14) 0.0244(15) 0.0155(13) 0.0004(11) -0.0014(11) -0.0001(12) C10 0.0256(16) 0.0376(19) 0.0315(17) -0.0068(14) 0.0004(13) -0.0039(14) C11 0.0322(16) 0.0251(16) 0.0244(15) 0.0025(12) 0.0008(13) 0.0024(13) C12 0.0264(15) 0.0186(14) 0.0151(13) 0.0038(11) -0.0022(11) -0.0046(11) C13 0.0235(14) 0.0228(15) 0.0146(13) -0.0016(11) 0.0008(11) -0.0071(11) C14 0.0282(15) 0.0254(16) 0.0145(13) 0.0041(11) 0.0009(11) -0.0023(12) C15 0.0332(16) 0.0346(18) 0.0187(14) -0.0034(13) 0.0035(12) -0.0066(14) C16 0.0380(18) 0.053(2) 0.0215(15) 0.0027(15) 0.0015(13) -0.0257(16) C17 0.0240(14) 0.0218(15) 0.0173(13) -0.0049(11) 0.0053(11) -0.0010(12) C18 0.0214(13) 0.0202(15) 0.0143(12) -0.0011(11) -0.0004(10) -0.0043(11) C19 0.0282(15) 0.0229(15) 0.0156(13) 0.0004(12) 0.0044(11) 0.0010(12) C20 0.0341(17) 0.0301(17) 0.0214(15) 0.0026(13) 0.0043(12) 0.0085(13) C21 0.047(2) 0.0223(17) 0.0299(16) -0.0002(13) -0.0005(14) -0.0010(14) C22 0.0186(14) 0.0208(14) 0.0199(13) -0.0029(11) 0.0009(11) -0.0003(11) C23 0.0185(14) 0.0290(16) 0.0247(15) -0.0049(12) 0.0015(11) 0.0033(12) C24 0.0276(15) 0.0291(17) 0.0217(15) -0.0077(12) 0.0014(12) -0.0009(13) C25 0.0227(14) 0.0230(16) 0.0237(14) -0.0027(12) -0.0032(11) 0.0008(12) C26 0.0282(15) 0.0217(16) 0.0261(15) 0.0015(12) -0.0027(12) -0.0012(12) C27 0.0258(15) 0.0228(15) 0.0246(15) 0.0029(12) 0.0019(12) -0.0055(12) C28 0.0196(14) 0.0273(17) 0.0316(16) -0.0022(13) 0.0027(12) -0.0036(12) C29 0.0163(14) 0.0268(16) 0.0296(16) -0.0007(13) -0.0053(11) -0.0027(12) C30 0.0199(14) 0.0234(15) 0.0233(14) 0.0021(12) -0.0011(11) -0.0014(11) C31 0.0276(16) 0.0340(18) 0.0313(17) 0.0101(14) -0.0069(13) -0.0044(13) C32 0.0207(15) 0.0237(16) 0.0436(19) -0.0020(14) -0.0029(13) 0.0033(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.852(3) . ? P1 C30 1.900(3) . ? P1 C22 1.915(3) . ? C1 C6 1.407(4) . ? C1 C2 1.418(4) . ? C2 C3 1.398(4) . ? C2 C7 1.512(3) . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 C5 1.377(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.407(4) . ? C7 C18 1.411(4) . ? C8 C12 1.396(3) . ? C8 C9 1.516(4) . ? C9 C10 1.528(4) . ? C9 C11 1.532(4) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? C13 C17 1.391(4) . ? C13 C14 1.526(4) . ? C14 C15 1.514(4) . ? C14 C16 1.524(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.393(3) . ? C17 H17 0.9500 . ? C18 C19 1.524(4) . ? C19 C21 1.535(4) . ? C19 C20 1.539(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.532(4) . ? C22 C23 1.536(4) . ? C22 C25 1.561(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.531(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.543(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.522(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.533(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.545(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.531(4) . ? C30 C32 1.532(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C30 102.85(12) . . ? C1 P1 C22 106.12(12) . . ? C30 P1 C22 108.61(12) . . ? C6 C1 C2 117.2(2) . . ? C6 C1 P1 123.9(2) . . ? C2 C1 P1 118.54(18) . . ? C3 C2 C1 119.4(2) . . ? C3 C2 C7 117.3(2) . . ? C1 C2 C7 123.4(2) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.5(2) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 122.7(2) . . ? C5 C6 H6 118.6 . . ? C1 C6 H6 118.6 . . ? C8 C7 C18 119.8(2) . . ? C8 C7 C2 119.1(2) . . ? C18 C7 C2 121.0(2) . . ? C12 C8 C7 118.8(2) . . ? C12 C8 C9 119.1(2) . . ? C7 C8 C9 122.0(2) . . ? C8 C9 C10 109.9(2) . . ? C8 C9 C11 112.9(2) . . ? C10 C9 C11 110.4(2) . . ? C8 C9 H9 107.8 . . ? C10 C9 H9 107.8 . . ? C11 C9 H9 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C8 122.3(2) . . ? C13 C12 H12 118.8 . . ? C8 C12 H12 118.8 . . ? C12 C13 C17 117.8(2) . . ? C12 C13 C14 120.7(2) . . ? C17 C13 C14 121.5(2) . . ? C15 C14 C16 110.8(2) . . ? C15 C14 C13 112.8(2) . . ? C16 C14 C13 110.0(2) . . ? C15 C14 H14 107.7 . . ? C16 C14 H14 107.7 . . ? C13 C14 H14 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 122.3(2) . . ? C13 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C7 118.7(2) . . ? C17 C18 C19 119.3(2) . . ? C7 C18 C19 121.9(2) . . ? C18 C19 C21 110.2(2) . . ? C18 C19 C20 113.8(2) . . ? C21 C19 C20 108.6(2) . . ? C18 C19 H19 108.0 . . ? C21 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 107.2(2) . . ? C24 C22 C25 109.7(2) . . ? C23 C22 C25 104.5(2) . . ? C24 C22 P1 120.16(19) . . ? C23 C22 P1 107.66(18) . . ? C25 C22 P1 106.47(17) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C22 121.3(2) . . ? C26 C25 H25A 107.0 . . ? C22 C25 H25A 107.0 . . ? C26 C25 H25B 107.0 . . ? C22 C25 H25B 107.0 . . ? H25A C25 H25B 106.7 . . ? C25 C26 C27 115.8(2) . . ? C25 C26 H26A 108.3 . . ? C27 C26 H26A 108.3 . . ? C25 C26 H26B 108.3 . . ? C27 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C28 C27 C26 114.9(2) . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C26 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 C29 117.5(2) . . ? C27 C28 H28A 107.9 . . ? C29 C28 H28A 107.9 . . ? C27 C28 H28B 107.9 . . ? C29 C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C28 C29 C30 119.5(2) . . ? C28 C29 H29A 107.5 . . ? C30 C29 H29A 107.5 . . ? C28 C29 H29B 107.5 . . ? C30 C29 H29B 107.5 . . ? H29A C29 H29B 107.0 . . ? C31 C30 C32 107.4(2) . . ? C31 C30 C29 107.5(2) . . ? C32 C30 C29 108.7(2) . . ? C31 C30 P1 116.17(19) . . ? C32 C30 P1 104.42(18) . . ? C29 C30 P1 112.33(19) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 P1 C1 C6 -75.2(2) . . . . ? C22 P1 C1 C6 38.8(2) . . . . ? C30 P1 C1 C2 111.1(2) . . . . ? C22 P1 C1 C2 -134.9(2) . . . . ? C6 C1 C2 C3 -2.1(4) . . . . ? P1 C1 C2 C3 172.0(2) . . . . ? C6 C1 C2 C7 179.1(2) . . . . ? P1 C1 C2 C7 -6.8(3) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C7 C2 C3 C4 179.7(2) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C2 C1 C6 C5 1.9(4) . . . . ? P1 C1 C6 C5 -171.9(2) . . . . ? C3 C2 C7 C8 -97.6(3) . . . . ? C1 C2 C7 C8 81.2(3) . . . . ? C3 C2 C7 C18 80.3(3) . . . . ? C1 C2 C7 C18 -100.8(3) . . . . ? C18 C7 C8 C12 4.4(4) . . . . ? C2 C7 C8 C12 -177.6(2) . . . . ? C18 C7 C8 C9 -171.6(2) . . . . ? C2 C7 C8 C9 6.4(4) . . . . ? C12 C8 C9 C10 -76.5(3) . . . . ? C7 C8 C9 C10 99.4(3) . . . . ? C12 C8 C9 C11 47.3(3) . . . . ? C7 C8 C9 C11 -136.8(3) . . . . ? C7 C8 C12 C13 -0.2(4) . . . . ? C9 C8 C12 C13 175.9(2) . . . . ? C8 C12 C13 C17 -3.7(4) . . . . ? C8 C12 C13 C14 176.2(2) . . . . ? C12 C13 C14 C15 118.4(3) . . . . ? C17 C13 C14 C15 -61.7(3) . . . . ? C12 C13 C14 C16 -117.4(3) . . . . ? C17 C13 C14 C16 62.6(3) . . . . ? C12 C13 C17 C18 3.5(4) . . . . ? C14 C13 C17 C18 -176.4(2) . . . . ? C13 C17 C18 C7 0.6(4) . . . . ? C13 C17 C18 C19 -174.8(2) . . . . ? C8 C7 C18 C17 -4.6(4) . . . . ? C2 C7 C18 C17 177.5(2) . . . . ? C8 C7 C18 C19 170.7(2) . . . . ? C2 C7 C18 C19 -7.2(4) . . . . ? C17 C18 C19 C21 81.9(3) . . . . ? C7 C18 C19 C21 -93.3(3) . . . . ? C17 C18 C19 C20 -40.4(3) . . . . ? C7 C18 C19 C20 144.3(3) . . . . ? C24 C22 C25 C26 -68.4(3) . . . . ? C23 C22 C25 C26 176.9(2) . . . . ? P1 C22 C25 C26 63.1(3) . . . . ? C22 C25 C26 C27 -71.7(3) . . . . ? C25 C26 C27 C28 110.9(3) . . . . ? C26 C27 C28 C29 -46.3(3) . . . . ? C27 C28 C29 C30 -68.0(3) . . . . ? C28 C29 C30 C31 -176.0(2) . . . . ? C28 C29 C30 C32 -60.0(3) . . . . ? C28 C29 C30 P1 55.0(3) . . . . ? C1 P1 C30 C31 43.0(2) . . . . ? C22 P1 C30 C31 -69.2(2) . . . . ? C1 P1 C30 C32 -75.1(2) . . . . ? C22 P1 C30 C32 172.76(18) . . . . ? C1 P1 C30 C29 167.34(18) . . . . ? C22 P1 C30 C29 55.2(2) . . . . ? _refine_diff_density_max 0.366 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.059 _shelx_res_file ; TITL XRAY5527_0m_a.res in P2(1)/n XRAY5527_0m_a.res created by SHELXL-2016/6 at 13:22:34 on 10-Jul-2018 CELL 0.71073 8.6727 14.1838 23.0062 90.000 92.223 90.000 ZERR 4.000 0.0018 0.0029 0.0047 0.000 0.003 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H P UNIT 128 196 4 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 CONF WPDB SIZE 0.020 0.200 0.350 TEMP -173.0 WGHT 0.100000 0.336730 FVAR 0.55001 P1 3 0.336765 0.651036 0.343496 11.00000 0.01575 0.01886 = 0.01489 -0.00061 -0.00015 -0.00106 C1 1 0.455395 0.755092 0.326049 11.00000 0.01711 0.01991 = 0.01542 0.00299 0.00138 0.00130 C2 1 0.500799 0.817555 0.371722 11.00000 0.01804 0.01938 = 0.01623 0.00332 -0.00028 0.00158 C3 1 0.605969 0.889571 0.361020 11.00000 0.02896 0.02183 = 0.01697 -0.00297 0.00253 -0.00346 AFIX 43 H3 2 0.637369 0.930866 0.391762 11.00000 -1.20000 AFIX 0 C4 1 0.665728 0.902057 0.306187 11.00000 0.02619 0.02494 = 0.02498 0.00211 0.00632 -0.00747 AFIX 43 H4 2 0.738146 0.950901 0.299885 11.00000 -1.20000 AFIX 0 C5 1 0.619361 0.843294 0.261177 11.00000 0.02649 0.03088 = 0.01497 0.00356 0.00480 -0.00339 AFIX 43 H5 2 0.658200 0.852037 0.223508 11.00000 -1.20000 AFIX 0 C6 1 0.516177 0.771678 0.271155 11.00000 0.02240 0.02643 = 0.01419 -0.00169 -0.00052 -0.00183 AFIX 43 H6 2 0.484819 0.731878 0.239656 11.00000 -1.20000 AFIX 0 C7 1 0.443483 0.809687 0.432761 11.00000 0.02118 0.02046 = 0.01329 0.00018 0.00225 -0.00724 C8 1 0.513407 0.744187 0.471387 11.00000 0.02114 0.02098 = 0.01504 -0.00166 -0.00137 -0.00792 C9 1 0.655068 0.688318 0.455832 11.00000 0.02264 0.02436 = 0.01552 0.00041 -0.00142 -0.00011 AFIX 13 H9 2 0.663635 0.691120 0.412645 11.00000 -1.20000 AFIX 0 C10 1 0.799743 0.733828 0.483508 11.00000 0.02562 0.03756 = 0.03150 -0.00677 0.00042 -0.00393 AFIX 137 H10A 2 0.808138 0.798932 0.469722 11.00000 -1.50000 H10B 2 0.890970 0.698129 0.472626 11.00000 -1.50000 H10C 2 0.792917 0.733612 0.525928 11.00000 -1.50000 AFIX 0 C11 1 0.645589 0.584346 0.473301 11.00000 0.03223 0.02508 = 0.02442 0.00249 0.00081 0.00241 AFIX 137 H11A 2 0.651685 0.579117 0.515803 11.00000 -1.50000 H11B 2 0.731440 0.549648 0.456918 11.00000 -1.50000 H11C 2 0.547578 0.557745 0.458359 11.00000 -1.50000 AFIX 0 C12 1 0.456108 0.734782 0.526974 11.00000 0.02644 0.01862 = 0.01505 0.00383 -0.00220 -0.00463 AFIX 43 H12 2 0.503088 0.690438 0.553049 11.00000 -1.20000 AFIX 0 C13 1 0.333253 0.787804 0.545424 11.00000 0.02346 0.02282 = 0.01464 -0.00165 0.00081 -0.00711 C14 1 0.267636 0.771247 0.605157 11.00000 0.02820 0.02543 = 0.01453 0.00408 0.00089 -0.00231 AFIX 13 H14 2 0.328216 0.719118 0.624366 11.00000 -1.20000 AFIX 0 C15 1 0.281429 0.857027 0.644200 11.00000 0.03324 0.03460 = 0.01872 -0.00343 0.00354 -0.00656 AFIX 137 H15A 2 0.390188 0.875142 0.649166 11.00000 -1.50000 H15B 2 0.240429 0.842141 0.682224 11.00000 -1.50000 H15C 2 0.222596 0.909310 0.626477 11.00000 -1.50000 AFIX 0 C16 1 0.100328 0.738869 0.598432 11.00000 0.03803 0.05318 = 0.02153 0.00266 0.00147 -0.02570 AFIX 137 H16A 2 0.037785 0.789106 0.580192 11.00000 -1.50000 H16B 2 0.061208 0.724356 0.636813 11.00000 -1.50000 H16C 2 0.094412 0.682325 0.573968 11.00000 -1.50000 AFIX 0 C17 1 0.272263 0.856167 0.507779 11.00000 0.02395 0.02183 = 0.01732 -0.00494 0.00533 -0.00099 AFIX 43 H17 2 0.191828 0.895574 0.520633 11.00000 -1.20000 AFIX 0 C18 1 0.324991 0.868882 0.451881 11.00000 0.02142 0.02024 = 0.01432 -0.00109 -0.00044 -0.00429 C19 1 0.262224 0.950563 0.415001 11.00000 0.02824 0.02290 = 0.01564 0.00045 0.00442 0.00101 AFIX 13 H19 2 0.281948 0.936311 0.373373 11.00000 -1.20000 AFIX 0 C20 1 0.087884 0.967121 0.420095 11.00000 0.03414 0.03007 = 0.02142 0.00255 0.00427 0.00853 AFIX 137 H20A 2 0.032938 0.907106 0.415154 11.00000 -1.50000 H20B 2 0.051584 1.011427 0.389876 11.00000 -1.50000 H20C 2 0.068119 0.993371 0.458499 11.00000 -1.50000 AFIX 0 C21 1 0.347844 1.042036 0.431519 11.00000 0.04667 0.02235 = 0.02987 -0.00024 -0.00051 -0.00099 AFIX 137 H21A 2 0.328556 1.058121 0.472022 11.00000 -1.50000 H21B 2 0.310793 1.093209 0.405990 11.00000 -1.50000 H21C 2 0.458835 1.033164 0.427090 11.00000 -1.50000 AFIX 0 C22 1 0.425611 0.546467 0.304135 11.00000 0.01861 0.02076 = 0.01990 -0.00290 0.00086 -0.00031 C23 1 0.601791 0.557072 0.309514 11.00000 0.01853 0.02901 = 0.02469 -0.00487 0.00146 0.00334 AFIX 137 H23A 2 0.650600 0.497985 0.298003 11.00000 -1.50000 H23B 2 0.632842 0.571841 0.349904 11.00000 -1.50000 H23C 2 0.634371 0.608159 0.284070 11.00000 -1.50000 AFIX 0 C24 1 0.383106 0.527999 0.239870 11.00000 0.02757 0.02914 = 0.02174 -0.00767 0.00143 -0.00092 AFIX 137 H24A 2 0.409369 0.583393 0.216795 11.00000 -1.50000 H24B 2 0.272140 0.515596 0.235271 11.00000 -1.50000 H24C 2 0.440625 0.473197 0.226444 11.00000 -1.50000 AFIX 0 C25 1 0.390446 0.456940 0.340828 11.00000 0.02273 0.02302 = 0.02366 -0.00267 -0.00317 0.00082 AFIX 23 H25A 2 0.445576 0.403619 0.323200 11.00000 -1.20000 H25B 2 0.438761 0.466879 0.380044 11.00000 -1.20000 AFIX 0 C26 1 0.224686 0.424243 0.349396 11.00000 0.02817 0.02167 = 0.02614 0.00153 -0.00274 -0.00122 AFIX 23 H26A 2 0.228089 0.359364 0.365263 11.00000 -1.20000 H26B 2 0.170249 0.421414 0.310808 11.00000 -1.20000 AFIX 0 C27 1 0.128970 0.485984 0.389812 11.00000 0.02576 0.02280 = 0.02459 0.00288 0.00192 -0.00545 AFIX 23 H27A 2 0.084972 0.445028 0.419820 11.00000 -1.20000 H27B 2 0.199051 0.531487 0.410017 11.00000 -1.20000 AFIX 0 C28 1 -0.001974 0.540530 0.359381 11.00000 0.01961 0.02733 = 0.03159 -0.00216 0.00270 -0.00360 AFIX 23 H28A 2 -0.041131 0.586955 0.387356 11.00000 -1.20000 H28B 2 -0.086897 0.495681 0.350147 11.00000 -1.20000 AFIX 0 C29 1 0.034038 0.593331 0.303376 11.00000 0.01633 0.02683 = 0.02957 -0.00075 -0.00528 -0.00270 AFIX 23 H29A 2 -0.065406 0.614457 0.285222 11.00000 -1.20000 H29B 2 0.078688 0.547184 0.276471 11.00000 -1.20000 AFIX 0 C30 1 0.142793 0.679644 0.306491 11.00000 0.01988 0.02339 = 0.02334 0.00210 -0.00107 -0.00145 C31 1 0.147403 0.721323 0.245193 11.00000 0.02759 0.03397 = 0.03134 0.01015 -0.00695 -0.00441 AFIX 137 H31A 2 0.189851 0.674607 0.218807 11.00000 -1.50000 H31B 2 0.212684 0.777740 0.246009 11.00000 -1.50000 H31C 2 0.042625 0.738299 0.231527 11.00000 -1.50000 AFIX 0 C32 1 0.072746 0.754381 0.345625 11.00000 0.02068 0.02365 = 0.04360 -0.00200 -0.00288 0.00334 AFIX 137 H32A 2 -0.034277 0.766528 0.332519 11.00000 -1.50000 H32B 2 0.132598 0.812804 0.343525 11.00000 -1.50000 H32C 2 0.075097 0.731633 0.385872 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY5527_0m_a.res in P2(1)/n REM R1 = 0.0568 for 3680 Fo > 4sig(Fo) and 0.1280 for all 6226 data REM 308 parameters refined using 0 restraints END WGHT 0.0478 0.5306 REM Highest difference peak 0.366, deepest hole -0.508, 1-sigma level 0.059 Q1 1 0.4403 0.6562 0.3230 11.00000 0.05 0.37 Q2 1 0.4737 0.7785 0.4554 11.00000 0.05 0.35 Q3 1 0.3654 0.6835 0.3712 11.00000 0.05 0.33 Q4 1 0.2024 0.6507 0.3214 11.00000 0.05 0.31 Q5 1 0.3641 0.6168 0.3750 11.00000 0.05 0.30 Q6 1 0.3482 0.7354 0.3237 11.00000 0.05 0.29 Q7 1 0.2295 0.6545 0.3606 11.00000 0.05 0.28 Q8 1 0.3226 0.6961 0.3155 11.00000 0.05 0.28 Q9 1 0.2871 0.9042 0.4348 11.00000 0.05 0.28 Q10 1 0.3138 0.6132 0.3144 11.00000 0.05 0.28 Q11 1 0.4583 0.7198 0.4933 11.00000 0.05 0.27 Q12 1 0.3089 0.8185 0.5285 11.00000 0.05 0.25 Q13 1 0.4804 0.7891 0.3464 11.00000 0.05 0.24 Q14 1 0.5216 0.7713 0.4979 11.00000 0.05 0.24 Q15 1 0.5938 0.9089 0.3268 11.00000 0.05 0.24 Q16 1 0.1774 0.7570 0.6069 11.00000 0.05 0.23 Q17 1 0.3502 0.8932 0.4760 11.00000 0.05 0.23 Q18 1 0.5949 0.7973 0.2741 11.00000 0.05 0.22 Q19 1 0.1789 0.6759 0.6008 11.00000 0.05 0.22 Q20 1 -0.0912 0.5546 0.3827 11.00000 0.05 0.22 ; _shelx_res_checksum 31678 _shelx_hkl_file ; -1 0 0 0.80 4.60 1 0 0 -1.90 4.40 -1 0 0 10.80 6.30 -2 0 0 14.70 9.10 -2 0 0 15.50 11.50 2 0 0 30.80 9.10 -3 0 0 -6.50 10.20 3 0 0 -8.20 11.10 -3 0 0 -0.40 13.00 4 0 0 764.72 33.30 -4 0 0 742.63 35.10 -4 0 0 732.53 32.10 -5 0 0 -8.00 13.70 -5 0 0 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38.50 4 6 -26 99.09 41.00 -3 -6 26 68.99 40.50 3 -6 -26 17.00 28.90 3 6 -26 -20.70 38.20 -3 6 26 4.60 31.70 3 6 -26 71.59 35.10 -2 -6 26 110.49 40.40 2 -6 -26 87.99 27.70 2 6 -26 48.80 40.60 2 6 -26 78.99 34.60 -2 6 26 52.29 31.60 1 -6 -26 110.59 29.00 -1 -6 26 135.29 41.10 -1 6 26 118.89 30.70 1 6 -26 111.69 34.70 1 6 -26 51.79 37.30 0 -6 26 132.39 40.50 0 -6 -26 64.39 30.40 0 6 26 64.39 28.10 0 6 -26 106.89 37.50 1 -6 26 48.90 38.90 -1 -6 -26 33.00 30.70 1 6 26 74.79 28.20 -1 6 -26 7.60 35.40 -2 -6 -26 2.20 29.20 2 -6 26 98.39 40.20 2 6 26 7.80 27.50 -2 6 -26 48.70 34.90 -3 -6 -26 -23.20 30.30 3 -6 26 79.99 39.40 3 6 26 11.50 27.10 3 -7 -26 69.09 29.40 -3 -7 26 200.28 44.60 3 7 -26 54.29 42.30 3 7 -26 134.49 37.10 -3 7 26 111.79 35.20 2 -7 -26 -49.50 26.30 -2 -7 26 25.40 40.80 2 7 -26 66.39 56.69 -2 7 26 -23.20 31.00 2 7 -26 12.60 40.10 1 -7 -26 22.60 28.40 -1 -7 26 65.39 40.50 -1 7 26 23.70 28.50 1 7 -26 5.70 38.20 0 -7 -26 -8.50 28.40 0 -7 26 49.40 39.60 0 7 -26 58.49 39.00 0 7 26 2.90 28.80 1 -7 26 126.19 41.00 -1 -7 -26 10.40 29.60 1 7 26 -38.20 26.60 -1 7 -26 44.40 37.60 2 -7 26 12.70 39.10 -2 -7 -26 -1.40 30.40 -2 7 -26 19.80 36.80 2 7 26 13.90 27.90 -2 -8 26 93.59 43.20 2 -8 -26 40.80 29.70 2 8 -26 11.30 40.80 -2 8 26 52.29 33.20 1 -8 -26 -13.30 27.60 -1 -8 26 99.19 42.30 -1 8 26 87.69 30.60 1 8 -26 19.40 40.30 0 -8 -26 13.30 28.00 0 -8 26 102.89 42.80 0 8 -26 61.19 39.40 0 8 26 59.49 29.60 1 -8 26 98.59 43.30 -1 -8 -26 -13.10 29.80 1 8 26 6.90 27.80 -1 8 -26 33.00 38.90 4 0 -27 8.40 29.20 -4 0 27 37.60 33.20 3 0 -27 -8.90 28.60 -3 0 27 19.50 31.60 -2 0 27 49.60 31.60 2 0 -27 0.10 29.10 -1 0 27 72.59 32.00 1 0 -27 88.59 30.40 0 0 -27 -12.70 27.70 0 0 27 71.99 30.00 1 0 27 188.68 33.00 -1 0 -27 181.18 33.00 2 0 27 1.80 29.30 -2 0 -27 -30.90 29.00 -3 0 -27 32.70 31.60 3 0 27 89.89 30.30 4 0 27 41.10 29.80 -4 0 -27 -1.40 32.30 -4 -1 27 40.10 33.80 4 -1 -27 22.10 30.70 4 1 -27 33.70 31.10 -4 1 27 44.00 33.10 3 -1 -27 24.20 28.80 -3 -1 27 84.79 34.50 -3 1 27 57.99 32.60 3 1 -27 71.89 30.90 2 -1 -27 18.40 28.70 -2 -1 27 107.89 34.00 -2 1 27 115.49 33.20 2 1 -27 69.49 30.80 1 -1 -27 12.80 28.30 -1 -1 27 27.10 31.70 1 1 -27 -16.60 29.40 -1 1 27 51.09 29.40 0 -1 -27 -1.40 27.30 0 -1 27 66.79 30.80 0 1 -27 0.20 29.20 0 1 27 31.20 28.20 1 -1 27 30.70 29.40 -1 -1 -27 -41.80 27.90 -1 1 -27 7.40 30.70 1 1 27 42.70 27.90 -2 -1 -27 59.79 30.50 2 -1 27 74.59 31.90 2 1 27 47.20 28.80 -2 1 -27 51.89 31.00 3 -1 27 71.39 30.80 -3 -1 -27 28.60 31.70 -3 1 -27 86.79 32.40 3 1 27 135.29 31.30 4 -2 -27 49.60 29.20 -4 -2 27 47.40 36.40 4 2 -27 43.60 32.10 -4 2 27 -10.80 32.60 -3 -2 27 95.09 35.00 3 -2 -27 20.90 29.50 3 2 -27 1.00 31.40 -3 2 27 50.09 31.90 2 -2 -27 28.90 28.00 -2 -2 27 44.40 35.00 -2 2 27 -33.60 29.80 2 2 -27 10.70 31.00 1 -2 -27 3.90 27.60 -1 -2 27 25.20 32.30 -1 2 27 -7.80 28.00 1 2 -27 64.39 31.20 0 -2 27 54.39 34.90 0 -2 -27 -5.80 27.70 0 2 27 96.39 28.70 0 2 -27 56.49 31.70 1 -2 27 10.10 34.00 -1 -2 -27 -1.90 27.80 -1 2 -27 -46.30 30.50 1 2 27 6.20 26.50 2 -2 27 32.40 34.30 -2 -2 -27 -46.60 28.60 -2 2 -27 -45.00 29.20 2 2 27 48.50 27.70 -3 -2 -27 3.30 31.30 3 -2 27 48.60 32.20 3 2 27 32.20 28.40 -3 2 -27 -8.00 30.40 -4 -3 27 110.99 38.20 4 -3 -27 -8.80 28.80 -4 3 27 83.29 34.30 4 3 -27 112.59 35.20 -3 -3 27 87.99 36.50 3 -3 -27 54.19 29.50 -3 3 27 51.49 32.80 3 3 -27 13.60 32.60 -2 -3 27 67.89 36.30 2 -3 -27 8.60 28.20 -2 3 27 17.30 31.00 2 3 -27 31.50 32.30 1 -3 -27 58.79 27.40 -1 -3 27 107.59 35.90 -1 3 27 32.20 29.40 1 3 -27 26.70 32.40 0 -3 27 -16.00 33.70 0 -3 -27 -47.00 26.00 0 3 -27 27.00 31.40 0 3 27 0.70 27.70 -1 -3 -27 -39.60 29.20 1 -3 27 37.90 34.80 1 3 27 35.50 28.20 -1 3 -27 -17.60 31.60 2 -3 27 0.40 34.50 -2 -3 -27 -17.10 30.00 2 3 27 -16.10 27.30 -2 3 -27 -65.29 29.50 3 -3 27 9.10 35.10 -3 -3 -27 6.30 31.70 3 3 27 -7.30 28.20 4 -4 -27 13.80 29.60 -4 -4 27 84.89 39.60 -4 4 27 48.60 34.20 4 4 -27 6.70 40.00 4 4 -27 122.29 36.30 -3 -4 27 36.40 37.00 3 -4 -27 -27.30 28.00 3 4 -27 17.60 33.30 -3 4 27 -11.10 31.20 3 4 -27 -24.70 37.90 2 -4 -27 -9.80 28.30 -2 -4 27 14.80 36.70 2 4 -27 2.70 33.00 -2 4 27 17.80 30.80 -1 -4 27 26.50 36.10 1 -4 -27 0.40 27.80 -1 4 27 -25.20 27.80 1 4 -27 28.60 32.70 0 -4 27 242.18 41.20 0 -4 -27 191.18 31.80 0 4 27 205.48 33.10 0 4 -27 227.28 36.30 -1 -4 -27 19.00 29.90 1 -4 27 63.29 38.00 1 4 27 42.60 28.20 -1 4 -27 6.10 31.90 2 -4 27 189.48 40.20 -2 -4 -27 187.78 34.20 2 4 27 189.58 32.30 -3 -4 -27 -42.20 31.30 3 -4 27 50.79 37.60 3 4 27 -1.30 27.50 3 -5 -27 95.19 30.40 -3 -5 27 104.19 41.00 -3 5 27 80.89 33.80 3 5 -27 87.39 36.20 3 5 -27 34.70 40.50 -2 -5 27 36.10 38.70 2 -5 -27 5.40 28.30 -2 5 27 55.49 32.00 2 5 -27 -33.00 37.80 2 5 -27 65.69 34.50 -1 -5 27 58.19 38.70 1 -5 -27 -9.40 28.30 1 5 -27 -5.30 33.50 -1 5 27 31.60 28.80 1 5 -27 17.30 36.20 0 -5 -27 -19.80 26.90 0 -5 27 32.40 37.60 0 5 27 27.80 28.10 0 5 -27 -16.90 33.50 1 -5 27 84.29 39.00 -1 -5 -27 87.29 31.00 1 5 27 68.89 29.20 -2 -5 -27 -1.40 30.50 2 -5 27 35.80 37.80 2 5 27 -17.50 27.10 2 -6 -27 14.70 27.90 -2 -6 27 41.30 40.60 2 6 -27 6.90 33.80 -2 6 27 -3.20 30.90 2 6 -27 12.50 39.90 1 -6 -27 26.30 29.90 -1 -6 27 15.80 39.70 1 6 -27 32.20 38.80 1 6 -27 74.89 56.19 -1 6 27 2.10 28.40 0 -6 27 104.89 40.80 0 -6 -27 10.50 29.50 0 6 -27 31.80 37.80 0 6 27 72.69 30.30 -1 -6 -27 -14.90 30.30 1 -6 27 73.29 40.60 -1 6 -27 66.89 38.20 1 6 27 37.40 28.60 2 -6 27 62.39 40.00 -2 -6 -27 -20.20 31.10 2 6 27 17.80 27.80 -1 -7 27 111.99 43.60 1 -7 -27 -9.60 28.60 1 7 -27 27.00 39.40 -1 7 27 14.60 29.00 0 -7 -27 2.00 29.50 0 -7 27 39.30 41.30 0 7 27 41.20 29.70 0 7 -27 46.40 39.20 3 0 -28 0.70 29.70 -3 0 28 31.10 33.70 -2 0 28 -36.40 31.60 2 0 -28 64.29 32.00 -1 0 28 40.00 31.40 1 0 -28 18.00 30.30 0 0 -28 14.40 30.90 0 0 28 61.59 30.30 1 0 28 6.80 29.40 -1 0 -28 -33.00 30.60 2 0 28 55.79 31.40 -2 0 -28 -5.20 30.10 -3 0 -28 13.10 32.40 3 0 28 27.30 29.60 -3 -1 28 33.90 34.30 3 -1 -28 -22.70 28.10 -3 1 28 68.59 33.20 3 1 -28 -20.60 31.90 2 -1 -28 0.10 29.70 -2 -1 28 0.10 33.50 -2 1 28 -18.90 31.10 2 1 -28 -36.90 30.80 -1 -1 28 42.70 32.80 1 -1 -28 -29.90 28.40 -1 1 28 7.80 29.90 1 1 -28 -29.60 30.40 0 -1 -28 43.40 30.20 0 -1 28 61.89 32.70 0 1 -28 15.20 30.70 0 1 28 9.80 29.20 1 -1 28 130.49 33.00 -1 -1 -28 69.79 31.90 1 1 28 126.79 32.40 -1 1 -28 120.59 33.30 -2 -1 -28 5.70 31.00 2 -1 28 70.69 31.40 2 1 28 14.00 29.80 -2 1 -28 15.50 31.50 3 -2 -28 -38.70 28.70 -3 -2 28 42.80 36.00 -3 2 28 5.60 32.40 3 2 -28 -28.50 31.50 -2 -2 28 66.59 35.30 2 -2 -28 -16.20 29.20 -2 2 28 8.60 32.00 2 2 -28 5.70 32.10 -1 -2 28 269.07 39.20 1 -2 -28 156.98 31.70 -1 2 28 160.28 33.90 1 2 -28 206.08 36.40 0 -2 28 34.20 31.90 0 -2 -28 -34.70 28.40 0 2 -28 -48.30 30.20 0 2 28 9.00 28.30 -1 -2 -28 -8.50 30.10 1 -2 28 37.40 32.20 1 2 28 48.00 29.30 -1 2 -28 -4.80 32.60 2 -2 28 -3.80 31.60 -2 -2 -28 -4.20 30.50 -2 2 -28 -1.10 30.90 2 2 28 56.29 29.90 3 -3 -28 13.10 29.40 -3 -3 28 17.70 37.50 -3 3 28 -23.70 32.50 3 3 -28 39.40 34.50 2 -3 -28 1.20 28.30 -2 -3 28 59.59 36.90 -2 3 28 20.80 32.90 2 3 -28 -20.20 32.30 -1 -3 28 53.69 36.80 1 -3 -28 45.30 28.50 -1 3 28 57.29 31.50 1 3 -28 76.19 34.10 0 -3 28 42.10 36.00 0 -3 -28 -13.80 28.00 0 3 28 5.00 28.90 0 3 -28 -22.60 32.10 -1 -3 -28 -51.59 29.70 1 -3 28 53.79 36.20 -1 3 -28 -17.50 33.70 1 3 28 19.40 28.20 2 -3 28 30.40 36.40 -2 -3 -28 -31.80 30.70 -2 3 -28 -14.50 31.80 2 3 28 11.80 28.70 2 -4 -28 74.69 31.30 -2 -4 28 189.68 41.30 -2 4 28 116.89 34.60 2 4 -28 95.29 36.00 1 -4 -28 126.89 31.40 -1 -4 28 171.68 40.10 -1 4 28 99.29 32.60 1 4 -28 82.39 35.30 0 -4 28 90.89 38.30 0 -4 -28 31.00 29.30 0 4 -28 11.70 33.20 0 4 28 85.79 30.50 1 -4 28 24.80 37.00 -1 -4 -28 -21.00 30.60 1 4 28 33.10 29.10 -1 4 -28 -62.49 37.20 -2 -4 -28 29.10 31.80 2 -4 28 91.79 38.90 -2 5 28 39.70 32.00 -1 -5 28 38.80 39.30 1 -5 -28 -50.39 27.70 -1 5 28 62.69 30.10 1 5 -28 -45.80 34.10 0 -5 28 45.00 40.10 0 -5 -28 -7.60 28.80 0 5 28 28.80 29.00 -1 -5 -28 -3.00 30.20 1 -5 28 3.00 38.90 1 5 28 -20.10 26.80 -2 0 29 -6.80 33.00 2 0 -29 -21.30 30.80 -1 0 29 58.09 32.00 1 0 -29 19.90 31.60 0 0 -29 -82.99 30.80 0 0 29 57.89 30.70 -1 0 -29 -13.70 31.70 1 0 29 49.10 31.30 -2 -1 29 44.20 35.10 2 -1 -29 12.00 30.50 2 1 -29 -49.99 31.60 -2 1 29 46.20 33.40 -1 -1 29 69.49 34.00 1 -1 -29 -15.10 29.10 1 1 -29 -7.90 32.90 -1 1 29 21.90 31.90 0 -1 29 100.89 33.90 0 -1 -29 57.69 33.10 0 1 29 74.79 32.70 0 1 -29 84.59 33.80 -1 -1 -29 111.79 33.80 1 -1 29 103.19 35.50 -1 1 -29 53.99 34.40 1 1 29 163.18 34.90 1 -2 -29 4.70 29.30 -1 -2 29 48.10 34.30 1 2 -29 -32.90 33.90 -1 2 29 16.30 30.80 0 -2 29 37.70 34.00 0 -2 -29 0.30 30.60 0 2 -29 -33.10 32.40 0 2 29 17.10 29.00 1 -2 29 77.99 34.10 -1 -2 -29 93.09 33.30 1 2 29 78.09 30.70 -1 2 -29 60.19 34.40 1 -3 -29 44.60 29.40 1 3 -29 35.70 34.90 0 -3 -29 95.09 31.90 0 -3 29 102.99 39.70 0 3 -29 116.99 36.20 0 3 29 110.59 31.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 55521 #===END data_L_5c _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H51 O4 P' _chemical_formula_weight 554.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9251(8) _cell_length_b 11.2824(9) _cell_length_c 28.061(2) _cell_angle_alpha 90 _cell_angle_beta 96.4210(10) _cell_angle_gamma 90 _cell_volume 3122.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7689 _cell_measurement_theta_min 2.322 _cell_measurement_theta_max 26.6485 _exptl_crystal_description parallelapiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.180 _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9280 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scan' _diffrn_reflns_number 35457 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.461 _diffrn_reflns_theta_max 27.455 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7113 _reflns_number_gt 5590 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+2.2419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7113 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.42368(5) 0.39189(4) 0.16763(2) 0.02223(11) Uani 1 1 d . . . . . O1 O 0.55624(19) 0.72598(13) 0.25881(6) 0.0561(5) Uani 1 1 d . . . . . O2 O 0.3999(6) 0.5974(4) 0.27502(19) 0.0232(13) Uani 0.514(12) 1 d . . P A 1 O2' O 0.3411(6) 0.6260(3) 0.25810(18) 0.0193(12) Uani 0.486(12) 1 d . . P A 2 O3 O 0.68636(11) 0.52352(10) 0.14874(4) 0.0220(3) Uani 1 1 d . . . . . O4 O 0.57955(11) 0.12657(10) 0.03609(4) 0.0199(2) Uani 1 1 d . . . . . C1 C 0.5239(2) 0.39519(17) 0.22945(6) 0.0374(5) Uani 1 1 d . . . . . C2 C 0.5774(3) 0.51762(18) 0.24754(7) 0.0441(6) Uani 1 1 d . . . . . H2A H 0.6061 0.5107 0.2824 0.053 Uiso 1 1 calc R U . . . H2B H 0.6597 0.5353 0.2319 0.053 Uiso 1 1 calc R U . . . C3 C 0.4840(3) 0.62281(18) 0.24001(8) 0.0471(6) Uani 1 1 d . . . . . C4 C 0.4400(2) 0.64734(16) 0.18785(8) 0.0337(5) Uani 1 1 d . . . . . H4A H 0.5221 0.6665 0.1724 0.040 Uiso 1 1 calc R U . . . H4B H 0.3827 0.7194 0.1860 0.040 Uiso 1 1 calc R U . . . C5 C 0.36149(19) 0.55024(16) 0.15760(7) 0.0307(4) Uani 1 1 d . . . . . C6 C 0.6453(3) 0.31146(18) 0.23069(7) 0.0447(6) Uani 1 1 d . . . . . H6A H 0.7087 0.3412 0.2091 0.067 Uiso 1 1 calc R U . . . H6B H 0.6139 0.2323 0.2203 0.067 Uiso 1 1 calc R U . . . H6C H 0.6911 0.3072 0.2634 0.067 Uiso 1 1 calc R U . . . C7 C 0.4256(3) 0.3466(2) 0.26379(8) 0.0638(9) Uani 1 1 d . . . . . H7A H 0.4722 0.3428 0.2964 0.096 Uiso 1 1 calc R U . . . H7B H 0.3955 0.2670 0.2534 0.096 Uiso 1 1 calc R U . . . H7C H 0.3469 0.3992 0.2632 0.096 Uiso 1 1 calc R U . . . C8 C 0.3611(2) 0.58554(16) 0.10494(8) 0.0335(4) Uani 1 1 d . . . . . H8A H 0.3246 0.6659 0.1002 0.050 Uiso 1 1 calc R U . . . H8B H 0.3045 0.5300 0.0847 0.050 Uiso 1 1 calc R U . . . H8C H 0.4540 0.5833 0.0962 0.050 Uiso 1 1 calc R U . . . C9 C 0.2131(2) 0.54632(19) 0.16935(10) 0.0522(7) Uani 1 1 d . . . . . H9A H 0.1726 0.6254 0.1649 0.078 Uiso 1 1 calc R U . . . H9B H 0.2111 0.5211 0.2027 0.078 Uiso 1 1 calc R U . . . H9C H 0.1614 0.4900 0.1479 0.078 Uiso 1 1 calc R U . . . C10 C 0.4978(3) 0.76627(19) 0.29968(7) 0.0457(6) Uani 1 1 d . . . . . H10A H 0.4733 0.8512 0.2965 0.055 Uiso 1 1 calc R U . A 1 H10B H 0.5612 0.7551 0.3292 0.055 Uiso 1 1 calc R U . A 1 C11 C 0.3760(2) 0.6923(2) 0.30077(8) 0.0476(6) Uani 0.514(12) 1 d . . P A 1 H11A H 0.3633 0.6698 0.3341 0.057 Uiso 0.514(12) 1 calc R U P A 1 H11B H 0.2940 0.7347 0.2864 0.057 Uiso 0.514(12) 1 calc R U P A 1 C11' C 0.3760(2) 0.6923(2) 0.30077(8) 0.0476(6) Uani 0.486(12) 1 d . . P A 2 H11C H 0.3910 0.6367 0.3282 0.057 Uiso 0.486(12) 1 calc R U P A 2 H11D H 0.2986 0.7440 0.3063 0.057 Uiso 0.486(12) 1 calc R U P A 2 C12 C 0.54684(16) 0.36086(13) 0.12410(5) 0.0155(3) Uani 1 1 d . . . . . C13 C 0.66655(16) 0.42561(13) 0.11978(5) 0.0170(3) Uani 1 1 d . . . . . C14 C 0.75608(16) 0.39245(14) 0.08776(6) 0.0191(3) Uani 1 1 d . . . . . H14 H 0.8358 0.4377 0.0854 0.023 Uiso 1 1 calc R U . . . C15 C 0.72927(16) 0.29281(14) 0.05898(6) 0.0190(3) Uani 1 1 d . . . . . H15 H 0.7909 0.2699 0.0371 0.023 Uiso 1 1 calc R U . . . C16 C 0.61310(15) 0.22731(14) 0.06227(5) 0.0163(3) Uani 1 1 d . . . . . C17 C 0.51959(15) 0.26114(13) 0.09427(5) 0.0147(3) Uani 1 1 d . . . . . C18 C 0.81330(18) 0.58341(16) 0.15084(7) 0.0260(4) Uani 1 1 d . . . . . H18A H 0.8869 0.5271 0.1599 0.039 Uiso 1 1 calc R U . . . H18B H 0.8162 0.6470 0.1747 0.039 Uiso 1 1 calc R U . . . H18C H 0.8241 0.6173 0.1193 0.039 Uiso 1 1 calc R U . . . C19 C 0.65989(18) 0.09692(16) -0.00130(6) 0.0247(4) Uani 1 1 d . . . . . H19A H 0.6587 0.1630 -0.0240 0.037 Uiso 1 1 calc R U . . . H19B H 0.6227 0.0259 -0.0181 0.037 Uiso 1 1 calc R U . . . H19C H 0.7534 0.0815 0.0125 0.037 Uiso 1 1 calc R U . . . C20 C 0.39231(15) 0.18660(13) 0.09248(5) 0.0149(3) Uani 1 1 d . . . . . C21 C 0.39057(16) 0.08079(14) 0.11876(5) 0.0162(3) Uani 1 1 d . . . . . C22 C 0.27531(16) 0.00889(14) 0.11286(5) 0.0173(3) Uani 1 1 d . . . . . H22 H 0.2742 -0.0620 0.1311 0.021 Uiso 1 1 calc R U . . . C23 C 0.16245(16) 0.03748(14) 0.08127(6) 0.0179(3) Uani 1 1 d . . . . . C24 C 0.16687(16) 0.14250(14) 0.05534(6) 0.0186(3) Uani 1 1 d . . . . . H24 H 0.0901 0.1642 0.0338 0.022 Uiso 1 1 calc R U . . . C25 C 0.27940(16) 0.21682(14) 0.05976(5) 0.0170(3) Uani 1 1 d . . . . . C26 C 0.51283(16) 0.03802(14) 0.15187(6) 0.0194(3) Uani 1 1 d . . . . . H26 H 0.5824 0.1025 0.1543 0.023 Uiso 1 1 calc R U . . . C27 C 0.47747(19) 0.01121(16) 0.20263(6) 0.0249(4) Uani 1 1 d . . . . . H27A H 0.4354 0.0811 0.2155 0.037 Uiso 1 1 calc R U . . . H27B H 0.5603 -0.0090 0.2234 0.037 Uiso 1 1 calc R U . . . H27C H 0.4141 -0.0556 0.2015 0.037 Uiso 1 1 calc R U . . . C28 C 0.57494(17) -0.07158(16) 0.13038(6) 0.0248(4) Uani 1 1 d . . . . . H28A H 0.5084 -0.1361 0.1276 0.037 Uiso 1 1 calc R U . . . H28B H 0.6556 -0.0965 0.1513 0.037 Uiso 1 1 calc R U . . . H28C H 0.6004 -0.0521 0.0986 0.037 Uiso 1 1 calc R U . . . C29 C 0.03568(16) -0.03946(15) 0.07401(6) 0.0229(4) Uani 1 1 d . . . . . H29 H -0.0014 -0.0330 0.0395 0.028 Uiso 1 1 calc R U . . . C30 C -0.07344(19) 0.00620(19) 0.10373(8) 0.0380(5) Uani 1 1 d . . . . . H30A H -0.0429 -0.0042 0.1379 0.057 Uiso 1 1 calc R U . . . H30B H -0.1575 -0.0384 0.0954 0.057 Uiso 1 1 calc R U . . . H30C H -0.0899 0.0905 0.0969 0.057 Uiso 1 1 calc R U . . . C31 C 0.06256(18) -0.17057(16) 0.08468(7) 0.0303(4) Uani 1 1 d . . . . . H31A H 0.1321 -0.1996 0.0654 0.045 Uiso 1 1 calc R U . . . H31B H -0.0213 -0.2157 0.0767 0.045 Uiso 1 1 calc R U . . . H31C H 0.0941 -0.1806 0.1188 0.045 Uiso 1 1 calc R U . . . C32 C 0.28107(17) 0.32446(15) 0.02692(6) 0.0217(3) Uani 1 1 d . . . . . H32 H 0.3518 0.3803 0.0418 0.026 Uiso 1 1 calc R U . . . C33 C 0.14568(18) 0.39127(16) 0.02065(7) 0.0297(4) Uani 1 1 d . . . . . H33A H 0.0768 0.3422 0.0023 0.044 Uiso 1 1 calc R U . . . H33B H 0.1566 0.4656 0.0034 0.044 Uiso 1 1 calc R U . . . H33C H 0.1171 0.4087 0.0522 0.044 Uiso 1 1 calc R U . . . C34 C 0.32179(19) 0.28765(17) -0.02217(6) 0.0295(4) Uani 1 1 d . . . . . H34A H 0.2541 0.2326 -0.0377 0.044 Uiso 1 1 calc R U . . . H34B H 0.4106 0.2488 -0.0178 0.044 Uiso 1 1 calc R U . . . H34C H 0.3266 0.3581 -0.0423 0.044 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0309(2) 0.0159(2) 0.0227(2) -0.00522(17) 0.01538(18) -0.00717(17) O1 0.0934(13) 0.0335(8) 0.0496(9) -0.0271(7) 0.0437(9) -0.0382(9) O2 0.023(2) 0.0222(15) 0.026(2) -0.0076(14) 0.0108(19) -0.0024(15) O2' 0.019(2) 0.0177(14) 0.0227(19) -0.0025(13) 0.0076(17) 0.0001(14) O3 0.0224(6) 0.0184(6) 0.0260(6) -0.0073(5) 0.0058(5) -0.0064(5) O4 0.0222(6) 0.0195(6) 0.0194(6) -0.0065(4) 0.0081(4) -0.0026(5) C1 0.0739(15) 0.0237(9) 0.0165(8) -0.0039(7) 0.0130(9) -0.0205(10) C2 0.0853(17) 0.0308(11) 0.0184(9) -0.0079(8) 0.0152(10) -0.0294(11) C3 0.0762(16) 0.0274(10) 0.0465(13) -0.0221(9) 0.0454(12) -0.0315(11) C4 0.0361(10) 0.0166(8) 0.0537(12) -0.0112(8) 0.0287(9) -0.0085(7) C5 0.0268(9) 0.0177(8) 0.0513(12) -0.0093(8) 0.0202(8) -0.0031(7) C6 0.0827(17) 0.0280(10) 0.0196(9) 0.0025(8) -0.0113(10) -0.0145(11) C7 0.136(3) 0.0364(12) 0.0262(11) -0.0131(9) 0.0399(14) -0.0480(15) C8 0.0283(10) 0.0213(9) 0.0507(12) 0.0007(8) 0.0038(9) 0.0039(7) C9 0.0340(11) 0.0282(11) 0.101(2) -0.0255(12) 0.0379(12) -0.0083(9) C10 0.0841(17) 0.0281(10) 0.0288(11) -0.0103(9) 0.0227(11) -0.0109(11) C11 0.0268(10) 0.0737(17) 0.0419(12) -0.0327(12) 0.0028(9) 0.0104(10) C11' 0.0268(10) 0.0737(17) 0.0419(12) -0.0327(12) 0.0028(9) 0.0104(10) C12 0.0188(8) 0.0143(7) 0.0141(7) 0.0022(6) 0.0046(6) 0.0015(6) C13 0.0202(8) 0.0143(7) 0.0162(7) 0.0000(6) 0.0010(6) -0.0003(6) C14 0.0167(8) 0.0189(8) 0.0218(8) 0.0013(6) 0.0033(6) -0.0031(6) C15 0.0176(8) 0.0207(8) 0.0194(8) -0.0003(6) 0.0057(6) 0.0011(6) C16 0.0187(8) 0.0153(7) 0.0147(7) -0.0009(6) 0.0012(6) 0.0009(6) C17 0.0172(7) 0.0143(7) 0.0125(7) 0.0028(6) 0.0012(6) 0.0003(6) C18 0.0260(9) 0.0238(9) 0.0283(9) -0.0047(7) 0.0029(7) -0.0104(7) C19 0.0241(9) 0.0276(9) 0.0241(9) -0.0097(7) 0.0106(7) -0.0012(7) C20 0.0162(7) 0.0142(7) 0.0151(7) -0.0035(6) 0.0050(6) -0.0007(6) C21 0.0187(8) 0.0166(7) 0.0140(7) -0.0019(6) 0.0050(6) 0.0007(6) C22 0.0197(8) 0.0156(7) 0.0175(7) 0.0018(6) 0.0062(6) 0.0000(6) C23 0.0174(8) 0.0197(8) 0.0177(7) -0.0028(6) 0.0068(6) -0.0010(6) C24 0.0161(7) 0.0207(8) 0.0193(8) 0.0001(6) 0.0028(6) 0.0018(6) C25 0.0188(8) 0.0157(7) 0.0173(7) -0.0004(6) 0.0049(6) 0.0021(6) C26 0.0203(8) 0.0180(8) 0.0194(8) 0.0044(6) -0.0003(6) -0.0040(6) C27 0.0312(9) 0.0233(9) 0.0195(8) 0.0036(7) -0.0004(7) -0.0032(7) C28 0.0191(8) 0.0264(9) 0.0293(9) 0.0059(7) 0.0042(7) 0.0033(7) C29 0.0168(8) 0.0255(9) 0.0266(9) 0.0031(7) 0.0033(6) -0.0041(7) C30 0.0233(10) 0.0398(11) 0.0539(13) 0.0089(10) 0.0169(9) 0.0022(8) C31 0.0212(9) 0.0249(9) 0.0446(11) 0.0023(8) 0.0032(8) -0.0075(7) C32 0.0201(8) 0.0190(8) 0.0254(8) 0.0054(7) -0.0005(6) -0.0004(6) C33 0.0276(9) 0.0223(9) 0.0382(10) 0.0076(8) -0.0003(8) 0.0045(7) C34 0.0292(10) 0.0356(10) 0.0235(9) 0.0112(8) 0.0029(7) 0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C12 1.8554(15) . ? P1 C5 1.9009(19) . ? P1 C1 1.901(2) . ? O1 C10 1.417(2) . ? O1 C3 1.436(2) . ? O2 C11 1.327(3) . ? O2 C3 1.388(3) . ? O2' C11' 1.421(4) . ? O2' C3 1.559(5) . ? O3 C13 1.3724(19) . ? O3 C18 1.4251(19) . ? O4 C16 1.3739(18) . ? O4 C19 1.4267(18) . ? C1 C6 1.528(3) . ? C1 C2 1.545(2) . ? C1 C7 1.546(3) . ? C2 C3 1.507(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(3) . ? C4 C5 1.543(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.530(3) . ? C5 C9 1.546(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11' 1.472(3) . ? C10 C11 1.472(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12 C17 1.410(2) . ? C12 C13 1.412(2) . ? C13 C14 1.384(2) . ? C14 C15 1.392(2) . ? C14 H14 0.9500 . ? C15 C16 1.381(2) . ? C15 H15 0.9500 . ? C16 C17 1.414(2) . ? C17 C20 1.514(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.404(2) . ? C20 C25 1.409(2) . ? C21 C22 1.397(2) . ? C21 C26 1.522(2) . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 C24 1.394(2) . ? C23 C29 1.523(2) . ? C24 C25 1.391(2) . ? C24 H24 0.9500 . ? C25 C32 1.526(2) . ? C26 C27 1.535(2) . ? C26 C28 1.535(2) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.527(2) . ? C29 C30 1.528(2) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.534(2) . ? C32 C34 1.536(2) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 P1 C5 107.87(7) . . ? C12 P1 C1 106.75(9) . . ? C5 P1 C1 104.17(9) . . ? C10 O1 C3 108.94(15) . . ? C11 O2 C3 112.2(3) . . ? C11' O2' C3 98.1(3) . . ? C13 O3 C18 118.27(13) . . ? C16 O4 C19 117.73(12) . . ? C6 C1 C2 107.72(19) . . ? C6 C1 C7 108.50(19) . . ? C2 C1 C7 109.26(16) . . ? C6 C1 P1 109.84(12) . . ? C2 C1 P1 116.28(14) . . ? C7 C1 P1 105.03(16) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 H2A 107.7 . . ? C1 C2 H2A 107.7 . . ? C3 C2 H2B 107.7 . . ? C1 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? O2 C3 O1 102.84(18) . . ? O2 C3 C4 126.4(4) . . ? O1 C3 C4 106.66(16) . . ? O2 C3 C2 98.5(3) . . ? O1 C3 C2 108.2(2) . . ? C4 C3 C2 112.85(15) . . ? O1 C3 O2' 107.27(17) . . ? C4 C3 O2' 97.9(3) . . ? C2 C3 O2' 122.7(3) . . ? C3 C4 C5 118.56(16) . . ? C3 C4 H4A 107.7 . . ? C5 C4 H4A 107.7 . . ? C3 C4 H4B 107.7 . . ? C5 C4 H4B 107.7 . . ? H4A C4 H4B 107.1 . . ? C8 C5 C4 107.04(15) . . ? C8 C5 C9 108.31(19) . . ? C4 C5 C9 109.72(15) . . ? C8 C5 P1 110.68(12) . . ? C4 C5 P1 116.77(15) . . ? C9 C5 P1 104.06(13) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11' 104.26(16) . . ? O1 C10 C11 104.26(16) . . ? O1 C10 H10A 110.9 . . ? C11 C10 H10A 110.9 . . ? O1 C10 H10B 110.9 . . ? C11 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? O2 C11 C10 104.4(2) . . ? O2 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? O2 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? O2' C11' C10 113.8(2) . . ? O2' C11' H11C 108.8 . . ? C10 C11' H11C 108.8 . . ? O2' C11' H11D 108.8 . . ? C10 C11' H11D 108.8 . . ? H11C C11' H11D 107.7 . . ? C17 C12 C13 117.98(14) . . ? C17 C12 P1 116.40(11) . . ? C13 C12 P1 125.58(12) . . ? O3 C13 C14 122.83(14) . . ? O3 C13 C12 115.59(13) . . ? C14 C13 C12 121.58(14) . . ? C13 C14 C15 119.99(15) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.01(14) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? O4 C16 C15 124.14(14) . . ? O4 C16 C17 115.20(13) . . ? C15 C16 C17 120.66(14) . . ? C12 C17 C16 119.76(14) . . ? C12 C17 C20 124.53(13) . . ? C16 C17 C20 115.69(13) . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 119.49(14) . . ? C21 C20 C17 120.93(13) . . ? C25 C20 C17 119.16(13) . . ? C22 C21 C20 119.30(14) . . ? C22 C21 C26 118.33(14) . . ? C20 C21 C26 122.30(14) . . ? C23 C22 C21 122.21(14) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 117.47(14) . . ? C22 C23 C29 123.31(14) . . ? C24 C23 C29 119.23(14) . . ? C25 C24 C23 122.52(15) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C20 118.99(14) . . ? C24 C25 C32 119.25(14) . . ? C20 C25 C32 121.64(14) . . ? C21 C26 C27 112.31(14) . . ? C21 C26 C28 110.09(13) . . ? C27 C26 C28 110.45(13) . . ? C21 C26 H26 107.9 . . ? C27 C26 H26 107.9 . . ? C28 C26 H26 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C29 C31 113.72(14) . . ? C23 C29 C30 111.11(15) . . ? C31 C29 C30 109.78(15) . . ? C23 C29 H29 107.3 . . ? C31 C29 H29 107.3 . . ? C30 C29 H29 107.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C32 C33 113.07(14) . . ? C25 C32 C34 110.39(14) . . ? C33 C32 C34 110.19(14) . . ? C25 C32 H32 107.7 . . ? C33 C32 H32 107.7 . . ? C34 C32 H32 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 167.06(17) . . . . ? C7 C1 C2 C3 -75.3(2) . . . . ? P1 C1 C2 C3 43.3(2) . . . . ? C11 O2 C3 O1 24.0(6) . . . . ? C11 O2 C3 C4 -98.2(5) . . . . ? C11 O2 C3 C2 135.0(5) . . . . ? C10 O1 C3 O2 -8.6(4) . . . . ? C10 O1 C3 C4 126.14(19) . . . . ? C10 O1 C3 C2 -112.2(2) . . . . ? C10 O1 C3 O2' 22.1(4) . . . . ? C1 C2 C3 O2 74.4(3) . . . . ? C1 C2 C3 O1 -178.97(15) . . . . ? C1 C2 C3 C4 -61.2(2) . . . . ? C1 C2 C3 O2' 55.4(3) . . . . ? C11' O2' C3 O1 -26.9(4) . . . . ? C11' O2' C3 C4 -137.2(3) . . . . ? C11' O2' C3 C2 99.1(3) . . . . ? O2 C3 C4 C5 -60.6(3) . . . . ? O1 C3 C4 C5 178.83(16) . . . . ? C2 C3 C4 C5 60.1(2) . . . . ? O2' C3 C4 C5 -70.4(2) . . . . ? C3 C4 C5 C8 -166.26(17) . . . . ? C3 C4 C5 C9 76.4(2) . . . . ? C3 C4 C5 P1 -41.6(2) . . . . ? C3 O1 C10 C11' -7.3(3) . . . . ? C3 O1 C10 C11 -7.3(3) . . . . ? C3 O2 C11 C10 -28.9(6) . . . . ? O1 C10 C11 O2 21.3(4) . . . . ? C3 O2' C11' C10 23.6(4) . . . . ? O1 C10 C11' O2' -12.0(4) . . . . ? C5 P1 C12 C17 -124.91(12) . . . . ? C1 P1 C12 C17 123.64(12) . . . . ? C5 P1 C12 C13 57.57(16) . . . . ? C1 P1 C12 C13 -53.88(15) . . . . ? C18 O3 C13 C14 -9.2(2) . . . . ? C18 O3 C13 C12 171.74(14) . . . . ? C17 C12 C13 O3 178.38(13) . . . . ? P1 C12 C13 O3 -4.1(2) . . . . ? C17 C12 C13 C14 -0.7(2) . . . . ? P1 C12 C13 C14 176.77(12) . . . . ? O3 C13 C14 C15 -179.27(14) . . . . ? C12 C13 C14 C15 -0.2(2) . . . . ? C13 C14 C15 C16 0.2(2) . . . . ? C19 O4 C16 C15 -8.8(2) . . . . ? C19 O4 C16 C17 171.72(14) . . . . ? C14 C15 C16 O4 -178.64(14) . . . . ? C14 C15 C16 C17 0.8(2) . . . . ? C13 C12 C17 C16 1.7(2) . . . . ? P1 C12 C17 C16 -176.04(11) . . . . ? C13 C12 C17 C20 -176.41(14) . . . . ? P1 C12 C17 C20 5.9(2) . . . . ? O4 C16 C17 C12 177.72(13) . . . . ? C15 C16 C17 C12 -1.7(2) . . . . ? O4 C16 C17 C20 -4.03(19) . . . . ? C15 C16 C17 C20 176.51(14) . . . . ? C12 C17 C20 C21 -97.14(18) . . . . ? C16 C17 C20 C21 84.71(18) . . . . ? C12 C17 C20 C25 90.27(19) . . . . ? C16 C17 C20 C25 -87.89(17) . . . . ? C25 C20 C21 C22 -1.6(2) . . . . ? C17 C20 C21 C22 -174.20(14) . . . . ? C25 C20 C21 C26 175.29(14) . . . . ? C17 C20 C21 C26 2.7(2) . . . . ? C20 C21 C22 C23 1.0(2) . . . . ? C26 C21 C22 C23 -176.10(14) . . . . ? C21 C22 C23 C24 -0.5(2) . . . . ? C21 C22 C23 C29 179.80(15) . . . . ? C22 C23 C24 C25 0.8(2) . . . . ? C29 C23 C24 C25 -179.49(15) . . . . ? C23 C24 C25 C20 -1.5(2) . . . . ? C23 C24 C25 C32 174.64(14) . . . . ? C21 C20 C25 C24 1.9(2) . . . . ? C17 C20 C25 C24 174.60(14) . . . . ? C21 C20 C25 C32 -174.15(14) . . . . ? C17 C20 C25 C32 -1.5(2) . . . . ? C22 C21 C26 C27 -56.13(19) . . . . ? C20 C21 C26 C27 126.91(15) . . . . ? C22 C21 C26 C28 67.39(18) . . . . ? C20 C21 C26 C28 -109.57(16) . . . . ? C22 C23 C29 C31 -26.9(2) . . . . ? C24 C23 C29 C31 153.44(15) . . . . ? C22 C23 C29 C30 97.59(19) . . . . ? C24 C23 C29 C30 -82.10(19) . . . . ? C24 C25 C32 C33 42.7(2) . . . . ? C20 C25 C32 C33 -141.27(16) . . . . ? C24 C25 C32 C34 -81.27(18) . . . . ? C20 C25 C32 C34 94.77(18) . . . . ? _refine_diff_density_max 0.441 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.050 _shelx_res_file ; XRAY3930_0m.res created by SHELXL-2014/7 TITL XRAY3930_0m in P2(1)/n CELL 0.71073 9.9251 11.2824 28.0609 90.000 96.421 90.000 ZERR 4.00 0.0008 0.0009 0.0022 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O P UNIT 136 204 16 4 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.20 0.20 0.20 EXYZ C11 C11' EADP C11 C11' CONF TEMP -173.000 WGHT 0.043400 2.241900 FVAR 0.17494 0.51354 MOLE 1 P1 4 0.423684 0.391889 0.167630 11.00000 0.03092 0.01586 = 0.02271 -0.00522 0.01538 -0.00717 O1 3 0.556239 0.725978 0.258805 11.00000 0.09338 0.03347 = 0.04963 -0.02707 0.04373 -0.03819 PART 1 O2 3 0.399897 0.597443 0.275025 21.00000 0.02306 0.02223 = 0.02614 -0.00755 0.01079 -0.00242 PART 2 O2' 3 0.341111 0.625959 0.258103 -21.00000 0.01868 0.01770 = 0.02273 -0.00248 0.00765 0.00015 PART 0 O3 3 0.686359 0.523516 0.148736 11.00000 0.02236 0.01844 = 0.02595 -0.00732 0.00579 -0.00640 O4 3 0.579553 0.126574 0.036086 11.00000 0.02216 0.01954 = 0.01938 -0.00646 0.00814 -0.00260 C1 1 0.523940 0.395190 0.229451 11.00000 0.07394 0.02365 = 0.01652 -0.00387 0.01301 -0.02051 C2 1 0.577429 0.517617 0.247538 11.00000 0.08525 0.03076 = 0.01841 -0.00790 0.01522 -0.02943 AFIX 23 H2A 2 0.606070 0.510745 0.282371 11.00000 -1.20000 H2B 2 0.659703 0.535299 0.231873 11.00000 -1.20000 AFIX 0 C3 1 0.483966 0.622809 0.240007 11.00000 0.07618 0.02742 = 0.04649 -0.02209 0.04544 -0.03151 C4 1 0.439950 0.647344 0.187853 11.00000 0.03612 0.01657 = 0.05365 -0.01115 0.02875 -0.00846 AFIX 23 H4A 2 0.522098 0.666544 0.172355 11.00000 -1.20000 H4B 2 0.382713 0.719419 0.186035 11.00000 -1.20000 AFIX 0 C5 1 0.361489 0.550241 0.157602 11.00000 0.02684 0.01765 = 0.05127 -0.00932 0.02019 -0.00309 C6 1 0.645276 0.311462 0.230686 11.00000 0.08272 0.02798 = 0.01964 0.00246 -0.01131 -0.01450 AFIX 137 H6A 2 0.708694 0.341205 0.209115 11.00000 -1.50000 H6B 2 0.613869 0.232259 0.220295 11.00000 -1.50000 H6C 2 0.691091 0.307220 0.263442 11.00000 -1.50000 AFIX 0 C7 1 0.425634 0.346601 0.263786 11.00000 0.13581 0.03644 = 0.02617 -0.01311 0.03989 -0.04804 AFIX 137 H7A 2 0.472246 0.342767 0.296434 11.00000 -1.50000 H7B 2 0.395451 0.267040 0.253435 11.00000 -1.50000 H7C 2 0.346903 0.399201 0.263250 11.00000 -1.50000 AFIX 0 C8 1 0.361150 0.585545 0.104936 11.00000 0.02829 0.02132 = 0.05073 0.00065 0.00384 0.00386 AFIX 137 H8A 2 0.324647 0.665910 0.100175 11.00000 -1.50000 H8B 2 0.304548 0.530000 0.084664 11.00000 -1.50000 H8C 2 0.454036 0.583333 0.096239 11.00000 -1.50000 AFIX 0 C9 1 0.213068 0.546323 0.169352 11.00000 0.03396 0.02820 = 0.10120 -0.02551 0.03788 -0.00825 AFIX 137 H9A 2 0.172649 0.625362 0.164928 11.00000 -1.50000 H9B 2 0.211075 0.521114 0.202687 11.00000 -1.50000 H9C 2 0.161380 0.490011 0.147891 11.00000 -1.50000 AFIX 0 C10 1 0.497803 0.766274 0.299677 11.00000 0.08410 0.02805 = 0.02876 -0.01035 0.02267 -0.01093 AFIX 23 H10A 2 0.473338 0.851202 0.296525 11.00000 -1.20000 H10B 2 0.561159 0.755103 0.329177 11.00000 -1.20000 PART 1 AFIX 0 C11 1 0.375971 0.692286 0.300765 21.00000 0.02683 0.07373 = 0.04189 -0.03271 0.00279 0.01035 AFIX 23 H11A 2 0.363294 0.669779 0.334072 21.00000 -1.20000 H11B 2 0.294046 0.734707 0.286361 21.00000 -1.20000 PART 2 AFIX 0 C11' 1 0.375971 0.692286 0.300765 -21.00000 0.02683 0.07373 = 0.04189 -0.03271 0.00279 0.01035 AFIX 23 H11C 2 0.391003 0.636749 0.328159 -21.00000 -1.20000 H11D 2 0.298632 0.743988 0.306289 -21.00000 -1.20000 PART 0 AFIX 0 C12 1 0.546837 0.360860 0.124102 11.00000 0.01883 0.01433 = 0.01408 0.00218 0.00457 0.00145 C13 1 0.666547 0.425615 0.119776 11.00000 0.02024 0.01435 = 0.01622 0.00003 0.00097 -0.00032 C14 1 0.756078 0.392449 0.087761 11.00000 0.01671 0.01892 = 0.02178 0.00125 0.00326 -0.00309 AFIX 43 H14 2 0.835817 0.437662 0.085421 11.00000 -1.20000 AFIX 0 C15 1 0.729274 0.292815 0.058984 11.00000 0.01764 0.02072 = 0.01939 -0.00026 0.00575 0.00112 AFIX 43 H15 2 0.790894 0.269881 0.037089 11.00000 -1.20000 AFIX 0 C16 1 0.613103 0.227309 0.062265 11.00000 0.01870 0.01528 = 0.01467 -0.00095 0.00119 0.00088 C17 1 0.519588 0.261139 0.094269 11.00000 0.01723 0.01429 = 0.01254 0.00285 0.00121 0.00032 C18 1 0.813300 0.583413 0.150835 11.00000 0.02595 0.02381 = 0.02826 -0.00465 0.00287 -0.01037 AFIX 137 H18A 2 0.886913 0.527102 0.159883 11.00000 -1.50000 H18B 2 0.816181 0.646981 0.174727 11.00000 -1.50000 H18C 2 0.824101 0.617344 0.119338 11.00000 -1.50000 AFIX 0 C19 1 0.659886 0.096916 -0.001304 11.00000 0.02413 0.02757 = 0.02412 -0.00968 0.01059 -0.00118 AFIX 137 H19A 2 0.658741 0.162968 -0.024026 11.00000 -1.50000 H19B 2 0.622735 0.025888 -0.018058 11.00000 -1.50000 H19C 2 0.753362 0.081521 0.012490 11.00000 -1.50000 AFIX 0 C20 1 0.392305 0.186602 0.092479 11.00000 0.01624 0.01420 = 0.01511 -0.00347 0.00496 -0.00074 C21 1 0.390566 0.080792 0.118761 11.00000 0.01872 0.01657 = 0.01404 -0.00190 0.00496 0.00072 C22 1 0.275315 0.008892 0.112860 11.00000 0.01972 0.01558 = 0.01745 0.00178 0.00623 0.00000 AFIX 43 H22 2 0.274232 -0.061964 0.131103 11.00000 -1.20000 AFIX 0 C23 1 0.162453 0.037476 0.081270 11.00000 0.01742 0.01972 = 0.01773 -0.00282 0.00683 -0.00097 C24 1 0.166868 0.142504 0.055335 11.00000 0.01614 0.02067 = 0.01925 0.00008 0.00283 0.00178 AFIX 43 H24 2 0.090076 0.164163 0.033809 11.00000 -1.20000 AFIX 0 C25 1 0.279401 0.216817 0.059764 11.00000 0.01877 0.01570 = 0.01732 -0.00039 0.00490 0.00211 C26 1 0.512833 0.038019 0.151872 11.00000 0.02031 0.01802 = 0.01943 0.00437 -0.00029 -0.00402 AFIX 13 H26 2 0.582400 0.102493 0.154294 11.00000 -1.20000 AFIX 0 C27 1 0.477470 0.011210 0.202625 11.00000 0.03122 0.02333 = 0.01948 0.00362 -0.00044 -0.00325 AFIX 137 H27A 2 0.435375 0.081149 0.215453 11.00000 -1.50000 H27B 2 0.560340 -0.009023 0.223371 11.00000 -1.50000 H27C 2 0.414110 -0.055617 0.201465 11.00000 -1.50000 AFIX 0 C28 1 0.574943 -0.071584 0.130381 11.00000 0.01906 0.02637 = 0.02926 0.00585 0.00424 0.00331 AFIX 137 H28A 2 0.508399 -0.136086 0.127562 11.00000 -1.50000 H28B 2 0.655647 -0.096538 0.151305 11.00000 -1.50000 H28C 2 0.600441 -0.052104 0.098557 11.00000 -1.50000 AFIX 0 C29 1 0.035683 -0.039457 0.074010 11.00000 0.01681 0.02553 = 0.02665 0.00307 0.00328 -0.00406 AFIX 13 H29 2 -0.001434 -0.033038 0.039479 11.00000 -1.20000 AFIX 0 C30 1 -0.073443 0.006198 0.103731 11.00000 0.02329 0.03975 = 0.05387 0.00886 0.01695 0.00220 AFIX 137 H30A 2 -0.042911 -0.004176 0.137910 11.00000 -1.50000 H30B 2 -0.157498 -0.038433 0.095421 11.00000 -1.50000 H30C 2 -0.089893 0.090479 0.096918 11.00000 -1.50000 AFIX 0 C31 1 0.062559 -0.170574 0.084683 11.00000 0.02119 0.02493 = 0.04456 0.00226 0.00320 -0.00747 AFIX 137 H31A 2 0.132123 -0.199558 0.065388 11.00000 -1.50000 H31B 2 -0.021300 -0.215705 0.076710 11.00000 -1.50000 H31C 2 0.094102 -0.180615 0.118801 11.00000 -1.50000 AFIX 0 C32 1 0.281070 0.324459 0.026920 11.00000 0.02010 0.01897 = 0.02536 0.00535 -0.00054 -0.00037 AFIX 13 H32 2 0.351808 0.380334 0.041847 11.00000 -1.20000 AFIX 0 C33 1 0.145681 0.391266 0.020652 11.00000 0.02755 0.02229 = 0.03823 0.00761 -0.00032 0.00447 AFIX 137 H33A 2 0.076809 0.342194 0.002294 11.00000 -1.50000 H33B 2 0.156603 0.465598 0.003428 11.00000 -1.50000 H33C 2 0.117113 0.408697 0.052229 11.00000 -1.50000 AFIX 0 C34 1 0.321791 0.287655 -0.022169 11.00000 0.02922 0.03563 = 0.02351 0.01119 0.00291 0.00113 AFIX 137 H34A 2 0.254138 0.232600 -0.037662 11.00000 -1.50000 H34B 2 0.410607 0.248763 -0.017844 11.00000 -1.50000 H34C 2 0.326617 0.358113 -0.042332 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY3930_0m in P2(1)/n REM R1 = 0.0466 for 5590 Fo > 4sig(Fo) and 0.0639 for all 7113 data REM 374 parameters refined using 0 restraints END WGHT 0.0435 2.2376 REM Highest difference peak 0.441, deepest hole -0.402, 1-sigma level 0.050 Q1 1 0.3121 0.7036 0.3226 11.00000 0.05 0.44 Q2 1 0.3822 0.3608 0.2574 11.00000 0.05 0.37 Q3 1 0.5050 0.7178 0.2493 11.00000 0.05 0.35 Q4 1 0.5825 0.6845 0.2739 11.00000 0.05 0.35 Q5 1 0.4758 0.3400 0.2662 11.00000 0.05 0.29 Q6 1 0.4571 0.3098 0.2671 11.00000 0.05 0.29 Q7 1 0.4303 0.2691 0.2591 11.00000 0.05 0.29 Q8 1 0.4524 0.0610 0.1317 11.00000 0.05 0.29 Q9 1 0.4876 0.4061 0.2055 11.00000 0.05 0.28 Q10 1 0.4138 0.5872 0.3271 11.00000 0.05 0.28 Q11 1 0.3994 0.4889 0.1638 11.00000 0.05 0.28 Q12 1 0.4877 0.3730 0.1394 11.00000 0.05 0.27 Q13 1 0.5855 0.2283 0.0891 11.00000 0.05 0.26 Q14 1 0.4605 0.2231 0.0959 11.00000 0.05 0.26 Q15 1 0.2819 0.2673 0.0413 11.00000 0.05 0.26 Q16 1 0.4887 0.0253 0.1744 11.00000 0.05 0.26 Q17 1 0.1021 0.0000 0.0779 11.00000 0.05 0.26 Q18 1 0.4044 0.5895 0.1743 11.00000 0.05 0.26 Q19 1 0.5267 0.3198 0.3033 11.00000 0.05 0.25 Q20 1 0.4529 0.6229 0.2179 11.00000 0.05 0.25 ; _shelx_res_checksum 27995 _shelx_hkl_file ; 1 0 0 -0.07 0.08 1 0 0 -0.09 0.09 -1 0 0 -0.14 0.07 -1 0 0 -0.20 0.08 2 0 0 211.60 3.86 2 0 0 214.55 4.13 -2 0 0 212.03 3.86 -2 0 0 213.17 4.03 3 0 0 -0.10 0.20 3 0 0 0.19 0.19 -3 0 0 0.31 0.24 -3 0 0 0.03 0.17 -4 0 0 88.28 2.12 -4 0 0 88.95 1.91 4 0 0 83.92 2.17 4 0 0 87.42 1.97 -5 0 0 -0.20 0.27 -5 0 0 0.19 0.23 5 0 0 -0.30 0.23 5 0 0 0.05 0.23 -6 0 0 4.18 0.56 6 0 0 3.92 0.48 6 0 0 2.92 0.53 -6 0 0 3.41 0.44 -7 0 0 -0.34 0.34 7 0 0 0.28 0.32 7 0 0 0.67 0.42 -7 0 0 -0.27 0.27 8 0 0 20.88 1.24 -8 0 0 18.32 1.17 8 0 0 20.15 1.05 9 0 0 0.10 0.42 -9 0 0 0.35 0.51 9 0 0 -0.07 0.40 -10 0 0 0.75 0.60 10 0 0 1.90 0.65 11 0 0 -0.33 0.47 -11 0 0 -0.19 0.48 12 0 0 9.12 1.26 -12 0 0 8.77 1.19 0 -1 0 -0.02 0.06 0 -1 0 0.01 0.08 0 1 0 -0.10 0.07 0 1 0 -0.12 0.07 1 -1 0 502.24 9.45 -1 -1 0 503.91 9.20 1 -1 0 514.62 9.03 -1 -1 0 510.84 9.04 1 1 0 522.14 8.97 -1 1 0 514.92 9.23 1 1 0 545.07 9.52 -1 1 0 526.24 8.96 2 -1 0 91.62 1.81 -2 -1 0 89.97 1.91 -2 -1 0 89.35 1.83 2 1 0 90.83 1.89 2 1 0 90.43 1.89 -2 1 0 92.22 1.73 -2 1 0 89.61 1.94 -3 -1 0 8.19 0.45 3 -1 0 8.33 0.42 -3 -1 0 9.35 0.52 3 -1 0 8.22 0.54 3 1 0 8.60 0.49 -3 1 0 8.34 0.44 -3 1 0 8.65 0.57 3 1 0 8.17 0.49 4 -1 0 48.18 1.24 4 -1 0 49.65 1.51 -4 -1 0 49.87 1.43 -4 -1 0 50.66 1.29 4 1 0 51.06 1.44 -4 1 0 48.54 1.24 4 1 0 48.62 1.36 -4 1 0 47.06 1.42 -5 -1 0 6.19 0.59 5 -1 0 6.09 0.65 5 -1 0 5.33 0.47 -5 -1 0 5.68 0.49 -5 1 0 5.92 0.61 -5 1 0 6.03 0.48 5 1 0 4.66 0.53 5 1 0 5.12 0.55 6 -1 0 31.81 1.39 -6 -1 0 32.99 1.32 6 -1 0 32.84 1.14 -6 -1 0 34.67 1.15 6 1 0 34.65 1.27 6 1 0 32.38 1.32 -6 1 0 34.28 1.11 -6 1 0 37.04 1.39 7 -1 0 0.44 0.39 7 -1 0 0.72 0.33 -7 -1 0 0.90 0.42 -7 -1 0 0.37 0.35 -7 1 0 0.81 0.34 7 1 0 0.38 0.39 -7 1 0 -0.30 0.36 7 1 0 1.14 0.42 8 -1 0 57.70 1.79 -8 -1 0 55.94 2.03 8 -1 0 55.73 2.15 -8 -1 0 60.66 1.78 8 1 0 59.91 1.93 8 1 0 54.18 2.04 -8 1 0 55.62 2.04 -9 -1 0 52.51 2.10 9 -1 0 51.48 2.17 9 1 0 53.46 2.11 -9 1 0 51.44 2.09 9 1 0 54.11 1.92 -10 -1 0 4.04 0.79 10 -1 0 3.28 0.77 10 1 0 3.60 0.78 -10 1 0 2.17 0.70 11 -1 0 0.27 0.57 -11 -1 0 -0.78 0.54 -11 1 0 -0.65 0.47 11 1 0 -0.05 0.54 -12 -1 0 0.47 0.58 12 -1 0 -0.31 0.61 -12 1 0 0.53 0.68 0 -2 0 136.99 2.58 0 -2 0 137.96 2.62 0 2 0 134.86 2.53 0 2 0 133.20 2.63 1 -2 0 59.44 1.33 -1 -2 0 61.26 1.36 1 -2 0 60.85 1.39 -1 -2 0 61.25 1.36 -1 2 0 61.06 1.38 -1 2 0 61.16 1.21 1 2 0 60.12 1.16 1 2 0 60.35 1.36 -2 -2 0 3.71 0.34 2 -2 0 3.25 0.32 -2 -2 0 4.17 0.37 2 2 0 3.87 0.28 -2 2 0 3.55 0.26 -2 2 0 3.24 0.35 2 2 0 4.35 0.40 -3 -2 0 37.92 1.10 3 -2 0 35.09 1.17 3 -2 0 37.43 1.01 -3 -2 0 34.75 1.03 -3 2 0 35.18 1.14 3 2 0 35.35 1.10 -3 2 0 35.84 0.86 3 2 0 34.89 0.98 -4 -2 0 9.33 0.57 4 -2 0 8.46 0.46 -4 -2 0 8.94 0.59 4 -2 0 8.40 0.63 4 -2 0 9.94 0.55 -4 2 0 9.45 0.65 4 2 0 9.54 0.65 4 2 0 9.05 0.56 5 -2 0 26.29 1.17 -5 -2 0 27.58 1.09 -5 -2 0 26.39 0.99 5 -2 0 25.70 0.87 -5 2 0 24.71 1.13 5 2 0 27.87 1.09 -5 2 0 25.72 0.90 5 2 0 26.81 1.04 -6 -2 0 14.19 0.79 6 -2 0 12.85 0.67 -6 -2 0 13.00 0.83 6 -2 0 11.61 0.88 6 2 0 12.53 0.79 6 2 0 12.56 0.80 -6 2 0 13.33 0.89 -6 2 0 13.01 0.71 7 -2 0 0.86 0.35 -7 -2 0 0.73 0.44 7 -2 0 0.68 0.47 -7 -2 0 1.17 0.38 -7 2 0 1.18 0.49 -7 2 0 1.76 0.39 7 2 0 1.68 0.46 7 2 0 1.13 0.40 -8 -2 0 8.71 0.80 -8 -2 0 10.14 0.98 8 -2 0 10.07 1.06 8 2 0 7.92 0.85 8 2 0 9.41 0.90 -8 2 0 8.03 0.91 9 -2 0 45.57 2.06 -9 -2 0 44.34 1.91 -9 2 0 45.67 1.96 9 2 0 44.44 1.89 9 2 0 48.70 1.86 10 -2 0 0.71 0.56 -10 -2 0 0.66 0.54 -10 2 0 -0.12 0.52 10 2 0 -0.15 0.43 10 2 0 0.93 0.57 11 -2 0 2.29 0.82 -11 -2 0 1.96 0.69 -11 2 0 1.72 0.74 12 -2 0 4.77 1.03 -12 -2 0 4.93 0.99 -12 2 0 4.81 0.99 0 -3 0 -0.02 0.14 0 -3 0 -0.34 0.20 0 3 0 0.39 0.20 0 3 0 0.25 0.21 1 -3 0 253.38 4.72 1 -3 0 241.98 4.82 -1 -3 0 248.14 4.78 -1 -3 0 249.06 4.74 -1 -3 0 253.54 4.55 1 3 0 246.28 4.67 -1 3 0 251.42 4.81 -1 3 0 252.02 4.50 2 -3 0 97.90 2.24 -2 -3 0 95.77 2.13 2 -3 0 92.84 2.07 -2 -3 0 96.93 2.15 -2 3 0 95.25 1.87 -2 3 0 95.24 2.20 2 3 0 93.59 1.86 2 3 0 98.31 2.18 3 -3 0 24.20 0.83 -3 -3 0 22.69 0.86 -3 -3 0 23.32 0.88 3 -3 0 21.14 0.92 -3 3 0 23.19 0.65 3 3 0 22.17 0.68 -3 3 0 21.55 0.90 3 3 0 22.41 0.90 -4 -3 0 101.97 2.45 -4 -3 0 105.51 2.40 4 -3 0 102.66 2.31 4 -3 0 98.58 2.62 4 3 0 100.37 2.47 -4 3 0 102.45 2.07 -4 3 0 99.69 2.52 4 3 0 105.63 2.30 5 -3 0 20.88 0.87 -5 -3 0 22.43 0.94 -5 -3 0 21.18 1.00 5 -3 0 19.67 1.05 5 -3 0 19.80 0.73 -5 3 0 20.22 1.03 5 3 0 19.66 0.99 5 3 0 19.43 0.84 6 -3 0 1.84 0.34 -6 -3 0 2.07 0.49 6 -3 0 1.70 0.51 -6 -3 0 2.04 0.44 -6 3 0 1.43 0.36 6 3 0 3.00 0.53 6 3 0 1.78 0.39 -6 3 0 1.17 0.44 7 -3 0 6.09 0.83 -7 -3 0 7.09 0.71 -7 -3 0 6.85 0.79 7 3 0 7.93 0.75 7 3 0 7.81 0.81 -7 3 0 8.31 0.90 -7 3 0 8.05 0.68 -8 -3 0 52.20 1.99 -8 -3 0 51.03 1.74 8 -3 0 49.64 2.11 -8 3 0 51.62 2.02 8 3 0 53.61 1.89 8 3 0 54.82 1.97 -9 -3 0 0.14 0.47 9 -3 0 -0.10 0.48 -9 3 0 0.30 0.47 9 3 0 -0.45 0.43 -10 -3 0 2.56 0.71 10 -3 0 1.90 0.69 -10 3 0 1.22 0.63 10 3 0 1.50 0.63 -11 -3 0 6.03 0.99 11 -3 0 5.45 1.05 11 3 0 6.37 0.98 -11 3 0 5.00 0.93 12 -3 0 -0.01 0.73 -12 -3 0 3.07 0.80 -12 3 0 1.56 0.78 0 -4 0 43.18 1.06 0 4 0 43.38 1.17 0 4 0 43.29 1.23 -1 -4 0 1.85 0.17 1 -4 0 1.70 0.32 1 -4 0 2.15 0.31 -1 -4 0 1.26 0.32 -1 -4 0 1.21 0.30 -1 4 0 1.89 0.28 1 4 0 2.03 0.33 -2 -4 0 14.92 0.76 -2 -4 0 15.70 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0.63 -4 -7 0 4.25 0.61 4 7 0 3.25 0.62 -4 7 0 3.09 0.63 -5 -7 0 1.17 0.47 -5 -7 0 2.97 0.60 5 -7 0 2.69 0.54 5 -7 0 3.47 0.66 -5 7 0 2.53 0.59 6 -7 0 9.54 1.06 6 -7 0 10.80 0.94 -6 -7 0 11.41 1.03 -6 -7 0 10.73 1.01 6 7 0 12.07 1.13 -6 7 0 8.83 0.99 -7 -7 0 13.67 1.14 -7 -7 0 14.20 1.19 7 -7 0 11.44 1.21 -7 7 0 11.51 1.19 7 7 0 10.82 1.12 -8 -7 0 0.84 0.55 -8 -7 0 1.52 0.61 8 -7 0 2.14 0.70 8 7 0 1.18 0.64 -8 7 0 2.23 0.72 9 -7 0 1.27 0.73 -9 -7 0 2.11 0.71 9 7 0 2.71 0.76 -9 7 0 3.51 0.87 10 -7 0 3.15 0.90 -10 -7 0 3.01 0.81 10 7 0 1.87 0.75 -10 7 0 2.59 0.83 11 7 0 -1.02 0.64 -11 7 0 -0.66 0.56 0 -8 0 55.72 1.91 0 8 0 54.54 1.74 0 8 0 50.21 1.80 1 -8 0 0.32 0.30 -1 -8 0 0.52 0.43 1 -8 0 0.25 0.43 -1 8 0 0.05 0.31 1 8 0 0.18 0.37 -1 8 0 0.49 0.37 1 8 0 -0.26 0.32 -2 -8 0 71.82 2.29 2 -8 0 71.71 2.25 2 -8 0 68.62 2.06 2 8 0 71.28 2.21 -2 8 0 75.72 1.96 2 8 0 70.67 2.17 -2 8 0 73.94 2.30 -3 -8 0 11.68 1.04 3 -8 0 13.46 0.94 3 -8 0 11.27 0.87 -3 -8 0 10.83 0.95 3 8 0 10.99 1.00 -3 8 0 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0.61 1 0 -33 18.99 1.76 -1 0 33 20.27 1.49 0 0 33 1.13 0.71 0 0 33 0.07 0.59 1 0 33 0.53 0.64 -1 0 -33 1.11 0.68 -2 0 -33 1.21 0.68 2 0 33 0.64 0.66 3 0 33 13.76 1.60 -3 0 -33 13.32 1.45 -4 0 -33 -0.36 0.69 -6 -1 33 1.51 0.79 6 -1 -33 1.62 0.82 -6 1 33 -0.05 0.69 6 1 -33 0.97 0.75 5 -1 -33 1.16 0.73 -5 -1 33 2.54 0.88 5 1 -33 2.62 0.85 -5 1 33 2.66 0.88 -4 -1 33 3.46 0.91 4 -1 -33 6.75 1.15 -4 1 33 5.49 1.02 4 1 -33 6.14 1.07 3 -1 -33 13.90 1.53 -3 -1 33 8.87 1.19 3 1 -33 11.73 1.40 -3 1 33 11.18 1.35 2 -1 -33 5.60 1.08 -2 -1 33 8.97 1.18 -2 1 33 6.78 1.10 2 1 -33 6.57 1.13 -1 -1 33 1.75 0.73 1 -1 -33 0.67 0.64 -1 -1 33 0.74 0.63 -1 1 33 1.16 0.70 1 1 -33 1.74 0.69 0 -1 33 -0.53 0.53 0 1 33 0.34 0.64 0 1 33 -0.25 0.59 1 -1 33 3.25 0.88 -1 -1 -33 3.17 0.80 1 1 33 2.52 0.86 -1 1 -33 2.66 0.78 1 1 33 2.39 0.79 2 -1 33 2.05 0.81 -2 -1 -33 2.48 0.79 2 1 33 2.23 0.80 -2 1 -33 1.36 0.75 -3 -1 -33 2.42 0.85 3 -1 33 3.02 0.90 3 1 33 2.02 0.91 -3 1 -33 2.47 0.84 6 -2 -33 4.25 1.07 -6 -2 33 5.25 1.10 -5 -2 33 0.58 0.68 5 -2 -33 -0.06 0.71 5 2 -33 1.23 0.70 -5 2 33 1.47 0.79 4 -2 -33 10.44 1.41 -4 -2 33 8.12 1.16 -4 2 33 8.06 1.23 4 2 -33 7.23 1.16 3 -2 -33 0.37 0.66 -3 -2 33 -0.49 0.59 3 2 -33 0.15 0.61 -3 2 33 0.24 0.66 2 -2 -33 13.69 1.51 -2 -2 33 10.40 1.24 -2 2 33 12.45 1.41 2 2 -33 12.63 1.42 1 -2 -33 0.38 0.59 -1 -2 33 0.55 0.65 -1 2 33 1.40 0.71 0 -2 33 3.30 0.85 0 -2 -33 3.46 0.93 0 2 33 3.08 0.88 -1 -2 -33 2.08 0.74 1 -2 33 2.77 0.88 -1 2 -33 3.60 0.87 1 2 33 2.33 0.87 1 2 33 0.93 0.70 2 -2 33 1.91 0.77 -2 -2 -33 2.04 0.80 -2 2 -33 2.54 0.76 2 2 33 2.56 0.86 -3 -2 -33 0.48 0.71 3 -2 33 0.35 0.73 -3 2 -33 0.80 0.67 3 2 33 0.41 0.66 -6 -3 33 6.65 1.14 -5 -3 33 0.03 0.67 5 -3 -33 0.61 0.75 -5 3 33 -0.30 0.66 -4 -3 33 10.07 1.29 4 -3 -33 6.11 1.19 4 3 -33 7.26 1.17 -4 3 33 8.69 1.27 -3 -3 33 3.72 0.90 3 -3 -33 3.37 0.96 3 3 -33 3.52 0.90 -3 3 33 2.09 0.85 2 -3 -33 0.16 0.63 -2 3 33 1.01 0.71 2 3 -33 1.20 0.65 -1 -3 33 11.23 1.37 1 -3 -33 7.58 1.23 -1 3 33 8.73 1.22 0 -3 -33 12.87 1.52 0 -3 33 11.98 1.40 0 3 33 15.06 1.49 -1 -3 -33 0.83 0.63 1 -3 33 0.31 0.67 -1 3 -33 0.10 0.60 1 3 33 0.09 0.62 1 3 33 0.11 0.67 2 -3 33 0.38 0.69 -2 -3 -33 -0.50 0.64 2 3 33 0.12 0.66 2 3 33 0.24 0.64 -2 3 -33 0.50 0.62 3 -3 33 -0.38 0.59 -3 -3 -33 -0.31 0.67 3 3 33 0.09 0.68 -3 3 -33 0.89 0.74 -5 -4 33 0.28 0.74 4 -4 -33 1.95 0.88 -4 -4 33 0.53 0.70 -4 4 33 0.89 0.75 3 -4 -33 1.66 0.83 -3 4 33 1.50 0.79 2 -4 -33 -0.27 0.66 -2 4 33 -0.03 0.64 2 4 -33 0.01 0.57 -1 -4 33 8.48 1.21 1 -4 -33 11.50 1.44 -1 4 33 8.66 1.26 0 -4 33 2.48 0.81 0 -4 -33 2.70 0.88 0 4 33 2.40 0.84 -1 -4 -33 6.09 1.16 1 -4 33 9.00 1.29 1 4 33 9.87 1.26 -1 4 -33 8.37 1.17 -2 -4 -33 0.74 0.73 2 -4 33 0.18 0.67 2 4 33 0.39 0.61 2 4 33 0.17 0.69 -2 4 -33 0.34 0.70 3 -5 -33 1.35 0.86 -3 5 33 1.42 0.79 2 -5 -33 2.87 0.92 -2 5 33 3.67 0.95 1 -5 -33 0.64 0.69 -1 5 33 0.92 0.74 0 -5 33 6.11 1.09 0 -5 -33 4.70 1.05 0 5 33 5.75 1.09 -1 -5 -33 0.94 0.76 1 -5 33 1.12 0.76 -1 5 -33 0.49 0.64 1 5 33 0.14 0.70 5 0 -34 -0.52 0.60 -5 0 34 -0.87 0.61 -4 0 34 38.34 2.12 4 0 -34 39.11 2.27 3 0 -34 -0.30 0.61 -3 0 34 0.21 0.64 2 0 -34 6.21 1.10 -2 0 34 7.23 1.12 -1 0 34 0.89 0.68 1 0 -34 1.18 0.68 0 0 34 41.45 2.33 1 0 34 0.47 0.70 -1 0 -34 0.47 0.65 2 0 34 10.53 1.40 -2 0 -34 12.68 1.39 -3 0 -34 0.40 0.68 -5 -1 34 4.05 1.00 5 -1 -34 4.09 1.01 5 1 -34 2.59 0.89 -5 1 34 2.99 0.92 -4 -1 34 0.46 0.69 4 -1 -34 -0.10 0.62 -4 1 34 0.58 0.65 4 1 -34 -0.26 0.62 3 -1 -34 -0.21 0.59 -3 -1 34 -0.17 0.60 3 1 -34 0.37 0.65 -3 1 34 0.75 0.71 2 -1 -34 0.22 0.68 -2 -1 34 0.99 0.69 -2 1 34 -0.01 0.62 2 1 -34 0.94 0.63 1 -1 -34 3.62 0.98 -1 -1 34 6.17 1.03 -1 1 34 5.70 1.04 1 1 -34 5.40 1.05 0 -1 -34 -0.31 0.55 0 -1 34 0.49 0.67 0 1 34 -0.16 0.60 0 1 34 0.80 0.71 1 -1 34 3.86 0.95 1 1 34 4.71 1.00 -1 1 -34 4.95 0.95 2 -1 34 2.61 0.88 -2 -1 -34 1.61 0.79 2 1 34 0.85 0.71 -2 1 -34 2.64 0.86 -3 -1 -34 3.32 0.89 -3 1 -34 4.09 0.95 5 -2 -34 6.46 1.23 -5 -2 34 4.09 0.96 5 2 -34 7.78 1.21 4 -2 -34 1.89 0.88 -4 -2 34 0.24 0.69 4 2 -34 0.73 0.71 -4 2 34 2.32 0.87 3 -2 -34 0.93 0.70 -3 -2 34 -0.12 0.62 -3 2 34 -0.31 0.64 3 2 -34 -0.83 0.53 -2 -2 34 -0.35 0.59 2 -2 -34 0.45 0.66 2 2 -34 0.00 0.60 -2 2 34 -0.16 0.62 -1 -2 34 23.22 1.71 1 -2 -34 23.86 1.79 -1 2 34 25.33 1.70 1 2 -34 25.00 1.76 0 -2 34 5.91 1.07 0 -2 -34 4.04 0.95 0 2 34 7.34 1.14 1 -2 34 3.26 0.94 1 2 34 4.22 0.97 -1 2 -34 5.56 1.01 1 2 34 5.33 1.01 -2 -2 -34 3.34 0.92 2 -2 34 3.74 0.98 -2 2 -34 3.94 0.92 2 2 34 3.41 0.95 -5 -3 34 5.80 1.11 4 -3 -34 0.23 0.69 -4 -3 34 -0.61 0.63 -4 3 34 1.74 0.80 -3 -3 34 1.86 0.82 3 -3 -34 1.50 0.83 -3 3 34 1.24 0.78 3 3 -34 2.03 0.76 2 -3 -34 3.27 0.93 -2 3 34 4.44 0.98 2 3 -34 2.85 0.85 1 -3 -34 7.37 1.19 -1 -3 34 7.23 1.15 -1 3 34 7.90 1.20 0 -3 34 23.04 1.75 0 -3 -34 17.23 1.72 0 3 34 19.42 1.71 1 -3 34 2.33 0.86 -1 -3 -34 1.21 0.74 1 3 34 2.05 0.84 -1 3 -34 4.01 0.91 1 3 34 1.96 0.79 2 -3 34 0.01 0.63 -2 -3 -34 -0.46 0.65 -2 3 -34 -0.19 0.64 2 3 34 0.46 0.70 -4 -4 34 1.59 0.82 3 -4 -34 13.88 1.67 -3 4 34 14.41 1.56 2 -4 -34 1.87 0.88 2 4 -34 3.16 0.88 -2 4 34 2.72 0.88 -1 -4 34 1.58 0.75 1 -4 -34 1.35 0.74 -1 4 34 0.95 0.78 0 -4 -34 -0.12 0.59 0 -4 34 0.23 0.66 0 4 34 -0.16 0.67 1 -4 34 3.78 0.96 -1 4 -34 2.43 0.85 1 4 34 2.19 0.86 0 -5 34 0.61 0.71 0 5 34 0.02 0.65 -4 0 35 0.26 0.67 4 0 -35 1.69 0.79 -3 0 35 1.13 0.77 3 0 -35 1.12 0.72 -2 0 35 0.90 0.65 2 0 -35 0.83 0.73 1 0 -35 21.31 1.95 -1 0 35 21.39 1.77 0 0 35 -0.06 0.60 1 0 35 3.31 0.97 -2 0 -35 -0.16 0.67 -4 -1 35 -0.20 0.73 4 -1 -35 0.37 0.72 4 1 -35 0.43 0.72 -4 1 35 0.19 0.70 -3 -1 35 0.38 0.67 3 -1 -35 -0.11 0.65 -3 1 35 -0.24 0.65 3 1 -35 0.78 0.72 2 -1 -35 12.71 1.55 -2 -1 35 12.48 1.39 -2 1 35 12.14 1.44 2 1 -35 10.61 1.39 1 -1 -35 14.29 1.61 1 1 -35 16.79 1.71 -1 1 35 15.53 1.52 0 -1 35 1.41 0.71 0 -1 -35 0.55 0.69 0 1 35 1.79 0.77 1 -1 35 7.03 1.21 1 1 35 5.49 1.12 -4 -2 35 4.75 1.07 -4 2 35 5.79 1.10 4 2 -35 8.01 1.24 -3 -2 35 0.29 0.68 3 -2 -35 0.47 0.69 3 2 -35 0.26 0.64 -3 2 35 1.11 0.76 2 -2 -35 1.38 0.81 -2 2 35 1.38 0.77 2 2 -35 1.64 0.76 1 -2 -35 5.78 1.15 -1 2 35 5.68 1.06 1 2 -35 3.46 0.96 0 -2 -35 1.04 0.76 0 -2 35 3.17 0.93 0 2 35 2.16 0.83 1 -2 35 0.89 0.76 1 2 35 -0.35 0.60 -3 -3 35 1.06 0.75 3 3 -35 1.09 0.74 -3 3 35 1.57 0.79 2 3 -35 0.28 0.67 -2 3 35 -0.92 0.61 -1 -3 35 0.56 0.67 1 3 -35 -0.63 0.56 -1 3 35 -0.16 0.64 0 -3 35 3.02 0.90 0 3 35 3.84 0.97 -1 -4 35 3.23 0.94 -1 4 35 3.23 0.98 -3 0 36 0.03 0.70 3 0 -36 -0.83 0.57 -2 0 36 9.30 1.31 2 0 -36 8.39 1.29 -1 0 36 -0.29 0.65 1 0 -36 1.25 0.74 -3 -1 36 -0.90 0.61 3 1 -36 0.41 0.67 -3 1 36 -0.67 0.66 -2 -1 36 2.89 0.91 2 1 -36 2.68 0.92 -2 1 36 3.07 0.92 1 1 -36 19.71 1.87 -1 1 36 18.22 1.70 -2 2 36 0.30 0.76 1 2 -36 0.97 0.76 -1 2 36 1.66 0.81 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 23668 #===END data_L_5f _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'L_5f' _chemical_melting_point 470 _chemical_formula_moiety ? _chemical_formula_sum 'C36 H53 O3 P' _chemical_formula_weight 564.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5680(10) _cell_length_b 9.1013(11) _cell_length_c 23.827(3) _cell_angle_alpha 80.6490(10) _cell_angle_beta 86.3570(10) _cell_angle_gamma 63.9230(10) _cell_volume 1646.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5592 _cell_measurement_theta_min 2.520 _cell_measurement_theta_max 26.833 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_F_000 616 _exptl_transmission_factor_min 0.933 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.116 _shelx_estimated_absorpt_T_min 0.955 _shelx_estimated_absorpt_T_max 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19167 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.866 _diffrn_reflns_theta_max 27.297 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 7329 _reflns_number_gt 5112 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6256P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7329 _refine_ls_number_parameters 400 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C15A C 0.1714(9) 0.7480(10) 0.9561(3) 0.0554(17) Uani 0.636(12) 1 d D . P A 1 H15A H 0.184698 0.850915 0.947497 0.066 Uiso 0.636(12) 1 calc R U P A 1 C16A C -0.0177(13) 0.7817(17) 0.9521(6) 0.104(4) Uani 0.636(12) 1 d D . P A 1 H16A H -0.028322 0.680321 0.963251 0.156 Uiso 0.636(12) 1 calc R U P A 1 H16B H -0.058419 0.826433 0.913662 0.156 Uiso 0.636(12) 1 calc R U P A 1 H16C H -0.085881 0.859662 0.976899 0.156 Uiso 0.636(12) 1 calc R U P A 1 C17A C 0.2314(10) 0.6628(12) 1.0175(3) 0.088(3) Uani 0.636(12) 1 d D . P A 1 H17A H 0.162841 0.735576 1.043802 0.132 Uiso 0.636(12) 1 calc R U P A 1 H17B H 0.351639 0.637210 1.022060 0.132 Uiso 0.636(12) 1 calc R U P A 1 H17C H 0.217161 0.562523 1.024961 0.132 Uiso 0.636(12) 1 calc R U P A 1 C15B C 0.1599(15) 0.6922(13) 0.9684(5) 0.050(3) Uani 0.364(12) 1 d D . P A 2 H15B H 0.124784 0.609869 0.989540 0.060 Uiso 0.364(12) 1 calc R U P A 2 C16B C 0.2619(18) 0.7396(19) 1.0049(6) 0.082(4) Uani 0.364(12) 1 d D . P A 2 H16D H 0.359669 0.641941 1.021522 0.122 Uiso 0.364(12) 1 calc R U P A 2 H16E H 0.188979 0.794301 1.034563 0.122 Uiso 0.364(12) 1 calc R U P A 2 H16F H 0.302132 0.812826 0.982003 0.122 Uiso 0.364(12) 1 calc R U P A 2 C17B C 0.007(2) 0.8462(19) 0.9434(10) 0.084(6) Uani 0.364(12) 1 d D . P A 2 H17D H 0.047067 0.918609 0.919945 0.126 Uiso 0.364(12) 1 calc R U P A 2 H17E H -0.063188 0.901138 0.973476 0.126 Uiso 0.364(12) 1 calc R U P A 2 H17F H -0.061304 0.817282 0.920775 0.126 Uiso 0.364(12) 1 calc R U P A 2 P1 P 0.34459(6) 0.50312(6) 0.71004(2) 0.03113(14) Uani 1 1 d . . . . . O1 O 0.62609(18) 0.21946(17) 0.65050(6) 0.0439(4) Uani 1 1 d . . . . . O2 O 0.05498(17) 0.65392(18) 0.57549(6) 0.0440(4) Uani 1 1 d . . . . . O3 O 0.2391(2) 0.45457(19) 0.52614(6) 0.0476(4) Uani 1 1 d . . . . . C1 C 0.5572(2) 0.3322(2) 0.73619(7) 0.0293(4) Uani 1 1 d . . . . . C2 C 0.6773(2) 0.2116(2) 0.70483(8) 0.0332(4) Uani 1 1 d . . . . . C3 C 0.7383(3) 0.0983(3) 0.61765(9) 0.0474(5) Uani 1 1 d . . . . . H3A H 0.847847 0.103810 0.613337 0.071 Uiso 1 1 calc R U . . . H3B H 0.686896 0.118558 0.580862 0.071 Uiso 1 1 calc R U . . . H3C H 0.756155 -0.009506 0.636494 0.071 Uiso 1 1 calc R U . . . C4 C 0.8367(3) 0.0932(3) 0.72716(9) 0.0441(5) Uani 1 1 d . . . . . H4 H 0.912973 0.015923 0.705290 0.053 Uiso 1 1 calc R U . . . C5 C 0.8814(3) 0.0907(3) 0.78209(10) 0.0519(6) Uani 1 1 d . . . . . H5 H 0.988798 0.012624 0.797196 0.062 Uiso 1 1 calc R U . . . C6 C 0.7667(3) 0.2040(3) 0.81444(9) 0.0475(5) Uani 1 1 d . . . . . H6 H 0.797740 0.201220 0.851435 0.057 Uiso 1 1 calc R U . . . C7 C 0.6043(2) 0.3235(2) 0.79284(8) 0.0335(4) Uani 1 1 d . . . . . C8 C 0.4864(2) 0.4324(2) 0.83425(8) 0.0369(4) Uani 1 1 d . . . . . C9 C 0.4927(3) 0.5818(3) 0.84012(9) 0.0437(5) Uani 1 1 d . . . . . C10 C 0.6180(3) 0.6388(3) 0.80672(10) 0.0519(6) Uani 1 1 d . . . . . H10 H 0.669237 0.568870 0.776998 0.062 Uiso 1 1 calc R U . . . C11 C 0.5287(5) 0.8188(3) 0.77775(13) 0.0766(9) Uani 1 1 d . . . . . H11A H 0.427396 0.835863 0.757458 0.115 Uiso 1 1 calc R U . . . H11B H 0.607602 0.842398 0.751615 0.115 Uiso 1 1 calc R U . . . H11C H 0.495098 0.891071 0.806008 0.115 Uiso 1 1 calc R U . . . C12 C 0.7649(4) 0.6158(4) 0.84535(13) 0.0787(9) Uani 1 1 d . . . . . H12A H 0.717339 0.679689 0.875793 0.118 Uiso 1 1 calc R U . . . H12B H 0.843183 0.652352 0.823735 0.118 Uiso 1 1 calc R U . . . H12C H 0.826724 0.500977 0.860802 0.118 Uiso 1 1 calc R U . . . C13 C 0.3876(3) 0.6741(3) 0.88062(10) 0.0546(6) Uani 1 1 d . . . . . H13 H 0.390420 0.773260 0.884074 0.066 Uiso 1 1 calc R U . . . C14 C 0.2802(3) 0.6256(3) 0.91568(10) 0.0593(7) Uani 1 1 d . . . . . C18 C 0.2796(3) 0.4755(3) 0.91065(10) 0.0552(6) Uani 1 1 d . . . . . H18 H 0.208492 0.440090 0.934397 0.066 Uiso 1 1 calc R U . . . C19 C 0.3824(3) 0.3766(3) 0.87103(8) 0.0421(5) Uani 1 1 d . . . . . C20 C 0.3868(3) 0.2065(3) 0.87222(9) 0.0482(5) Uani 1 1 d . . . . . H20 H 0.437046 0.167235 0.836355 0.058 Uiso 1 1 calc R U . . . C21 C 0.2067(4) 0.2079(4) 0.87789(13) 0.0703(8) Uani 1 1 d . . . . . H21A H 0.164602 0.224123 0.915768 0.105 Uiso 1 1 calc R U . . . H21B H 0.214997 0.104231 0.870364 0.105 Uiso 1 1 calc R U . . . H21C H 0.127759 0.296219 0.851072 0.105 Uiso 1 1 calc R U . . . C22 C 0.5046(4) 0.0843(4) 0.92064(12) 0.0788(9) Uani 1 1 d . . . . . H22A H 0.620416 0.074615 0.914872 0.118 Uiso 1 1 calc R U . . . H22B H 0.505763 -0.021976 0.921315 0.118 Uiso 1 1 calc R U . . . H22C H 0.461601 0.123277 0.956169 0.118 Uiso 1 1 calc R U . . . C23 C 0.3821(2) 0.6220(2) 0.64118(8) 0.0298(4) Uani 1 1 d . . . . . C24 C 0.5621(2) 0.6218(2) 0.64366(8) 0.0368(4) Uani 1 1 d . . . . . H24A H 0.576861 0.646401 0.680538 0.044 Uiso 1 1 calc R U . . . H24B H 0.651683 0.512012 0.640014 0.044 Uiso 1 1 calc R U . . . C25 C 0.5869(3) 0.7473(3) 0.59714(10) 0.0482(5) Uani 1 1 d . . . . . H25A H 0.699386 0.745207 0.602150 0.058 Uiso 1 1 calc R U . . . H25B H 0.585214 0.716194 0.560215 0.058 Uiso 1 1 calc R U . . . C26 C 0.4449(3) 0.9222(3) 0.59885(12) 0.0569(6) Uani 1 1 d . . . . . H26A H 0.456028 0.958827 0.633787 0.068 Uiso 1 1 calc R U . . . H26B H 0.459453 0.996786 0.567192 0.068 Uiso 1 1 calc R U . . . C27 C 0.2647(3) 0.9294(3) 0.59562(10) 0.0503(6) Uani 1 1 d . . . . . H27A H 0.247973 0.906946 0.558608 0.060 Uiso 1 1 calc R U . . . H27B H 0.177499 1.039706 0.599940 0.060 Uiso 1 1 calc R U . . . C28 C 0.2416(3) 0.8032(2) 0.64209(9) 0.0384(4) Uani 1 1 d . . . . . H28A H 0.127818 0.807542 0.637656 0.046 Uiso 1 1 calc R U . . . H28B H 0.245272 0.834098 0.678898 0.046 Uiso 1 1 calc R U . . . C29 C 0.3700(2) 0.5593(2) 0.58586(7) 0.0318(4) Uani 1 1 d . . . . . H29A H 0.363124 0.643708 0.554185 0.038 Uiso 1 1 calc R U . . . H29B H 0.477916 0.462163 0.582048 0.038 Uiso 1 1 calc R U . . . C30 C 0.2211(2) 0.5147(2) 0.57955(8) 0.0334(4) Uani 1 1 d . . . . . C31 C 0.0221(3) 0.7248(3) 0.51725(10) 0.0543(6) Uani 1 1 d . . . . . H31A H 0.039482 0.824537 0.509792 0.065 Uiso 1 1 calc R U . . . H31B H -0.096093 0.752155 0.506735 0.065 Uiso 1 1 calc R U . . . C32 C 0.1510(3) 0.5938(3) 0.48443(9) 0.0553(6) Uani 1 1 d . . . . . H32A H 0.091458 0.567038 0.457244 0.066 Uiso 1 1 calc R U . . . H32B H 0.231791 0.631250 0.464177 0.066 Uiso 1 1 calc R U . . . C33 C 0.2218(3) 0.3782(3) 0.62498(8) 0.0401(5) Uani 1 1 d . . . . . H33A H 0.328600 0.279833 0.621367 0.048 Uiso 1 1 calc R U . . . H33B H 0.126582 0.354256 0.616852 0.048 Uiso 1 1 calc R U . . . C34 C 0.2068(3) 0.4064(3) 0.68721(8) 0.0406(5) Uani 1 1 d . . . . . C35 C 0.2550(4) 0.2363(4) 0.72339(11) 0.0655(8) Uani 1 1 d . . . . . H35A H 0.178678 0.191884 0.713976 0.098 Uiso 1 1 calc R U . . . H35B H 0.243682 0.247867 0.762963 0.098 Uiso 1 1 calc R U . . . H35C H 0.372853 0.162724 0.715828 0.098 Uiso 1 1 calc R U . . . C36 C 0.0179(3) 0.5235(4) 0.70046(11) 0.0668(8) Uani 1 1 d . . . . . H36A H -0.012536 0.631155 0.678854 0.100 Uiso 1 1 calc R U . . . H36B H 0.007888 0.531644 0.740313 0.100 Uiso 1 1 calc R U . . . H36C H -0.059036 0.480526 0.690449 0.100 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C15A 0.072(3) 0.039(4) 0.047(3) -0.016(2) 0.023(2) -0.018(3) C16A 0.058(4) 0.128(10) 0.093(8) -0.061(7) 0.007(4) 0.004(5) C17A 0.076(4) 0.113(6) 0.044(3) -0.034(4) 0.000(3) -0.006(4) C15B 0.064(5) 0.034(5) 0.046(6) -0.015(4) 0.012(4) -0.014(4) C16B 0.094(7) 0.106(10) 0.055(7) -0.047(6) 0.014(5) -0.043(7) C17B 0.062(8) 0.073(9) 0.064(7) -0.024(7) -0.004(6) 0.024(6) P1 0.0255(2) 0.0332(3) 0.0261(2) -0.00514(18) -0.00170(17) -0.00452(19) O1 0.0402(8) 0.0446(8) 0.0338(7) -0.0179(6) -0.0049(6) -0.0021(6) O2 0.0320(7) 0.0521(9) 0.0366(8) 0.0018(6) -0.0095(6) -0.0095(6) O3 0.0560(9) 0.0571(9) 0.0322(8) -0.0105(7) -0.0083(6) -0.0245(8) C1 0.0274(9) 0.0279(9) 0.0282(9) -0.0045(7) -0.0020(7) -0.0077(7) C2 0.0322(9) 0.0313(9) 0.0316(10) -0.0071(8) -0.0021(7) -0.0086(8) C3 0.0462(12) 0.0514(13) 0.0413(12) -0.0229(10) 0.0051(9) -0.0134(10) C4 0.0339(10) 0.0394(11) 0.0431(12) -0.0127(9) -0.0009(9) 0.0008(9) C5 0.0342(11) 0.0509(13) 0.0469(13) -0.0090(10) -0.0113(9) 0.0050(10) C6 0.0409(11) 0.0506(13) 0.0326(11) -0.0082(9) -0.0125(9) -0.0008(10) C7 0.0327(9) 0.0321(10) 0.0301(10) -0.0060(8) -0.0032(7) -0.0082(8) C8 0.0350(10) 0.0367(10) 0.0263(9) -0.0067(8) -0.0064(7) -0.0027(8) C9 0.0474(12) 0.0370(11) 0.0344(11) -0.0102(9) -0.0084(9) -0.0046(9) C10 0.0662(15) 0.0473(13) 0.0429(12) -0.0165(10) -0.0002(11) -0.0221(12) C11 0.115(3) 0.0508(15) 0.0642(18) -0.0099(13) -0.0034(16) -0.0348(17) C12 0.0674(18) 0.099(2) 0.073(2) -0.0264(17) -0.0006(15) -0.0344(18) C13 0.0572(14) 0.0458(13) 0.0495(14) -0.0220(11) -0.0019(11) -0.0069(11) C14 0.0523(14) 0.0620(16) 0.0459(13) -0.0287(12) -0.0001(11) -0.0021(12) C18 0.0470(13) 0.0679(16) 0.0391(12) -0.0153(11) 0.0054(10) -0.0126(12) C19 0.0393(11) 0.0451(12) 0.0306(10) -0.0080(9) -0.0055(8) -0.0065(9) C20 0.0500(13) 0.0507(13) 0.0373(11) -0.0060(10) 0.0008(9) -0.0162(11) C21 0.0651(17) 0.0807(19) 0.0698(18) -0.0165(15) 0.0164(14) -0.0363(15) C22 0.101(2) 0.0573(16) 0.0601(17) 0.0094(13) -0.0197(16) -0.0212(16) C23 0.0280(9) 0.0287(9) 0.0297(9) -0.0040(7) -0.0034(7) -0.0092(7) C24 0.0333(10) 0.0390(10) 0.0386(11) -0.0089(8) -0.0024(8) -0.0149(8) C25 0.0455(12) 0.0559(14) 0.0523(13) -0.0080(11) 0.0012(10) -0.0307(11) C26 0.0679(16) 0.0471(13) 0.0639(16) -0.0019(11) -0.0043(12) -0.0342(12) C27 0.0546(13) 0.0322(11) 0.0587(14) -0.0009(10) -0.0093(11) -0.0148(10) C28 0.0361(10) 0.0311(10) 0.0421(11) -0.0073(8) -0.0047(8) -0.0079(8) C29 0.0320(9) 0.0337(10) 0.0270(9) -0.0042(7) -0.0013(7) -0.0118(8) C30 0.0322(9) 0.0387(10) 0.0280(9) -0.0046(8) -0.0041(7) -0.0138(8) C31 0.0554(14) 0.0584(14) 0.0432(13) 0.0147(11) -0.0192(11) -0.0243(12) C32 0.0605(15) 0.0779(17) 0.0309(11) 0.0034(11) -0.0103(10) -0.0357(13) C33 0.0396(11) 0.0449(11) 0.0398(11) -0.0002(9) -0.0109(9) -0.0226(9) C34 0.0339(10) 0.0549(13) 0.0331(10) 0.0048(9) -0.0057(8) -0.0226(9) C35 0.0766(18) 0.0812(19) 0.0532(15) 0.0229(13) -0.0213(13) -0.0558(16) C36 0.0339(12) 0.115(2) 0.0473(14) -0.0082(14) 0.0023(10) -0.0297(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C15A C16A 1.517(10) . ? C15A C14 1.536(7) . ? C15A C17A 1.544(8) . ? C15A H15A 0.9800 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C15B C17B 1.501(12) . ? C15B C16B 1.502(12) . ? C15B C14 1.595(13) . ? C15B H15B 0.9800 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? P1 C1 1.8616(18) . ? P1 C34 1.902(2) . ? P1 C23 1.9046(19) . ? O1 C2 1.374(2) . ? O1 C3 1.416(2) . ? O2 C31 1.421(2) . ? O2 C30 1.426(2) . ? O3 C32 1.417(3) . ? O3 C30 1.439(2) . ? C1 C2 1.413(2) . ? C1 C7 1.413(3) . ? C2 C4 1.386(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.381(3) . ? C4 H4 0.9300 . ? C5 C6 1.376(3) . ? C5 H5 0.9300 . ? C6 C7 1.401(3) . ? C6 H6 0.9300 . ? C7 C8 1.512(3) . ? C8 C19 1.405(3) . ? C8 C9 1.414(3) . ? C9 C13 1.391(3) . ? C9 C10 1.517(3) . ? C10 C12 1.526(4) . ? C10 C11 1.531(4) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.371(4) . ? C13 H13 0.9300 . ? C14 C18 1.393(4) . ? C18 C19 1.397(3) . ? C18 H18 0.9300 . ? C19 C20 1.528(3) . ? C20 C22 1.527(3) . ? C20 C21 1.536(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C29 1.545(2) . ? C23 C24 1.546(3) . ? C23 C28 1.560(2) . ? C24 C25 1.533(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.526(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.523(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.531(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.522(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C33 1.507(3) . ? C31 C32 1.512(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.533(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.536(3) . ? C34 C36 1.544(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16A C15A C14 109.5(8) . . ? C16A C15A C17A 106.3(8) . . ? C14 C15A C17A 107.8(6) . . ? C16A C15A H15A 111.0 . . ? C14 C15A H15A 111.0 . . ? C17A C15A H15A 111.0 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15A C17A H17A 109.5 . . ? C15A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C15A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C17B C15B C16B 108.6(11) . . ? C17B C15B C14 105.2(14) . . ? C16B C15B C14 106.4(10) . . ? C17B C15B H15B 112.1 . . ? C16B C15B H15B 112.1 . . ? C14 C15B H15B 112.1 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C1 P1 C34 107.75(9) . . ? C1 P1 C23 108.51(8) . . ? C34 P1 C23 103.98(8) . . ? C2 O1 C3 118.25(15) . . ? C31 O2 C30 107.91(16) . . ? C32 O3 C30 107.12(16) . . ? C2 C1 C7 116.76(16) . . ? C2 C1 P1 126.52(13) . . ? C7 C1 P1 116.72(13) . . ? O1 C2 C4 121.97(16) . . ? O1 C2 C1 115.62(15) . . ? C4 C2 C1 122.42(17) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 119.56(18) . . ? C5 C4 H4 120.2 . . ? C2 C4 H4 120.2 . . ? C6 C5 C4 119.84(19) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.44(19) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C1 119.94(17) . . ? C6 C7 C8 115.85(16) . . ? C1 C7 C8 124.17(16) . . ? C19 C8 C9 119.67(18) . . ? C19 C8 C7 119.52(18) . . ? C9 C8 C7 120.52(18) . . ? C13 C9 C8 118.5(2) . . ? C13 C9 C10 119.0(2) . . ? C8 C9 C10 122.37(18) . . ? C9 C10 C12 110.3(2) . . ? C9 C10 C11 112.8(2) . . ? C12 C10 C11 109.9(2) . . ? C9 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 123.0(2) . . ? C14 C13 H13 118.5 . . ? C9 C13 H13 118.5 . . ? C13 C14 C18 117.8(2) . . ? C13 C14 C15A 114.6(4) . . ? C18 C14 C15A 127.6(4) . . ? C13 C14 C15B 135.1(5) . . ? C18 C14 C15B 106.7(5) . . ? C14 C18 C19 122.0(2) . . ? C14 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C8 118.9(2) . . ? C18 C19 C20 118.5(2) . . ? C8 C19 C20 122.49(18) . . ? C22 C20 C19 110.0(2) . . ? C22 C20 C21 109.5(2) . . ? C19 C20 C21 113.6(2) . . ? C22 C20 H20 107.9 . . ? C19 C20 H20 107.9 . . ? C21 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C29 C23 C24 108.51(15) . . ? C29 C23 C28 111.22(15) . . ? C24 C23 C28 107.51(15) . . ? C29 C23 P1 115.91(12) . . ? C24 C23 P1 109.48(12) . . ? C28 C23 P1 103.87(12) . . ? C25 C24 C23 113.31(16) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 111.57(18) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.36(18) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 111.07(18) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C23 113.71(17) . . ? C27 C28 H28A 108.8 . . ? C23 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C23 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C23 118.15(15) . . ? C30 C29 H29A 107.8 . . ? C23 C29 H29A 107.8 . . ? C30 C29 H29B 107.8 . . ? C23 C29 H29B 107.8 . . ? H29A C29 H29B 107.1 . . ? O2 C30 O3 104.12(14) . . ? O2 C30 C33 110.79(16) . . ? O3 C30 C33 106.37(16) . . ? O2 C30 C29 113.27(16) . . ? O3 C30 C29 108.52(15) . . ? C33 C30 C29 113.11(15) . . ? O2 C31 C32 105.36(17) . . ? O2 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? O2 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? O3 C32 C31 105.07(17) . . ? O3 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? O3 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C30 C33 C34 118.26(17) . . ? C30 C33 H33A 107.7 . . ? C34 C33 H33A 107.7 . . ? C30 C33 H33B 107.7 . . ? C34 C33 H33B 107.7 . . ? H33A C33 H33B 107.1 . . ? C33 C34 C35 106.20(19) . . ? C33 C34 C36 110.32(17) . . ? C35 C34 C36 108.8(2) . . ? C33 C34 P1 116.59(13) . . ? C35 C34 P1 109.70(14) . . ? C36 C34 P1 105.12(17) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C34 P1 C1 C2 59.58(18) . . . . ? C23 P1 C1 C2 -52.42(18) . . . . ? C34 P1 C1 C7 -121.33(15) . . . . ? C23 P1 C1 C7 126.67(15) . . . . ? C3 O1 C2 C4 2.3(3) . . . . ? C3 O1 C2 C1 -177.82(17) . . . . ? C7 C1 C2 O1 177.98(17) . . . . ? P1 C1 C2 O1 -2.9(3) . . . . ? C7 C1 C2 C4 -2.2(3) . . . . ? P1 C1 C2 C4 176.91(16) . . . . ? O1 C2 C4 C5 -179.8(2) . . . . ? C1 C2 C4 C5 0.3(3) . . . . ? C2 C4 C5 C6 0.9(4) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? C5 C6 C7 C1 -1.7(3) . . . . ? C5 C6 C7 C8 175.9(2) . . . . ? C2 C1 C7 C6 2.8(3) . . . . ? P1 C1 C7 C6 -176.37(16) . . . . ? C2 C1 C7 C8 -174.58(18) . . . . ? P1 C1 C7 C8 6.2(3) . . . . ? C6 C7 C8 C19 -84.3(2) . . . . ? C1 C7 C8 C19 93.2(2) . . . . ? C6 C7 C8 C9 89.4(2) . . . . ? C1 C7 C8 C9 -93.1(2) . . . . ? C19 C8 C9 C13 -3.3(3) . . . . ? C7 C8 C9 C13 -177.05(18) . . . . ? C19 C8 C9 C10 172.54(19) . . . . ? C7 C8 C9 C10 -1.2(3) . . . . ? C13 C9 C10 C12 69.8(3) . . . . ? C8 C9 C10 C12 -106.0(2) . . . . ? C13 C9 C10 C11 -53.5(3) . . . . ? C8 C9 C10 C11 130.7(2) . . . . ? C8 C9 C13 C14 1.0(3) . . . . ? C10 C9 C13 C14 -175.0(2) . . . . ? C9 C13 C14 C18 1.0(4) . . . . ? C9 C13 C14 C15A -178.3(3) . . . . ? C9 C13 C14 C15B 173.6(6) . . . . ? C16A C15A C14 C13 130.0(7) . . . . ? C17A C15A C14 C13 -114.8(7) . . . . ? C16A C15A C14 C18 -49.2(9) . . . . ? C17A C15A C14 C18 66.0(8) . . . . ? C17B C15B C14 C13 73.1(11) . . . . ? C16B C15B C14 C13 -42.1(13) . . . . ? C17B C15B C14 C18 -113.8(10) . . . . ? C16B C15B C14 C18 131.1(10) . . . . ? C13 C14 C18 C19 -0.7(4) . . . . ? C15A C14 C18 C19 178.5(4) . . . . ? C15B C14 C18 C19 -175.3(5) . . . . ? C14 C18 C19 C8 -1.6(3) . . . . ? C14 C18 C19 C20 174.3(2) . . . . ? C9 C8 C19 C18 3.6(3) . . . . ? C7 C8 C19 C18 177.39(18) . . . . ? C9 C8 C19 C20 -172.06(18) . . . . ? C7 C8 C19 C20 1.7(3) . . . . ? C18 C19 C20 C22 -77.9(3) . . . . ? C8 C19 C20 C22 97.8(3) . . . . ? C18 C19 C20 C21 45.3(3) . . . . ? C8 C19 C20 C21 -139.1(2) . . . . ? C29 C23 C24 C25 66.4(2) . . . . ? C28 C23 C24 C25 -54.0(2) . . . . ? P1 C23 C24 C25 -166.25(14) . . . . ? C23 C24 C25 C26 56.1(2) . . . . ? C24 C25 C26 C27 -54.7(3) . . . . ? C25 C26 C27 C28 54.4(3) . . . . ? C26 C27 C28 C23 -55.9(2) . . . . ? C29 C23 C28 C27 -64.4(2) . . . . ? C24 C23 C28 C27 54.3(2) . . . . ? P1 C23 C28 C27 170.24(15) . . . . ? C24 C23 C29 C30 167.64(16) . . . . ? C28 C23 C29 C30 -74.3(2) . . . . ? P1 C23 C29 C30 44.0(2) . . . . ? C31 O2 C30 O3 -30.0(2) . . . . ? C31 O2 C30 C33 -144.01(17) . . . . ? C31 O2 C30 C29 87.66(19) . . . . ? C32 O3 C30 O2 32.6(2) . . . . ? C32 O3 C30 C33 149.66(17) . . . . ? C32 O3 C30 C29 -88.35(19) . . . . ? C23 C29 C30 O2 66.8(2) . . . . ? C23 C29 C30 O3 -178.06(15) . . . . ? C23 C29 C30 C33 -60.3(2) . . . . ? C30 O2 C31 C32 16.3(2) . . . . ? C30 O3 C32 C31 -22.4(2) . . . . ? O2 C31 C32 O3 3.9(2) . . . . ? O2 C30 C33 C34 -68.2(2) . . . . ? O3 C30 C33 C34 179.21(16) . . . . ? C29 C30 C33 C34 60.2(2) . . . . ? C30 C33 C34 C35 -166.65(18) . . . . ? C30 C33 C34 C36 75.7(2) . . . . ? C30 C33 C34 P1 -44.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C28 H28A O2 0.97 2.47 3.139(3) 126.0 . C29 H29B O1 0.97 2.40 3.109(2) 129.2 . C33 H33A O1 0.97 2.48 3.168(2) 127.8 . C36 H36A O2 0.96 2.49 3.072(3) 119.0 . _refine_diff_density_max 0.417 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.055 _shelx_res_file ; TITL XRAY5783_0m_a.res in P-1 XRAY5783_0m_a.res created by SHELXL-2016/6 at 14:47:25 on 23-Dec-2018 CELL 0.71073 8.5680 9.1013 23.8274 80.649 86.357 63.923 ZERR 2.000 0.0010 0.0011 0.0028 0.001 0.001 0.001 LATT 1 SFAC C H O P UNIT 72 106 6 2 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 SADI C15A C16A C15A C17A C15B C16B C15B C17B SADI C16A C17A c16B c17B SIZE 0.020 0.300 0.400 HTAB C28 O2 HTAB C29 O1 HTAB C33 O1 HTAB C36 O2 WPDB CONF SIMU C16A C16B SIMU C17A C17B TEMP 23.0 WGHT 0.100000 0.625570 FVAR 0.79500 0.63600 PART 1 C15A 1 0.171419 0.748015 0.956111 21.00000 0.07248 0.03932 = 0.04730 -0.01606 0.02261 -0.01768 AFIX 13 H15A 2 0.184698 0.850915 0.947497 21.00000 -1.20000 AFIX 0 C16A 1 -0.017654 0.781699 0.952114 21.00000 0.05810 0.12834 = 0.09270 -0.06096 0.00708 0.00412 AFIX 137 H16A 2 -0.028322 0.680321 0.963251 21.00000 -1.50000 H16B 2 -0.058419 0.826433 0.913662 21.00000 -1.50000 H16C 2 -0.085881 0.859662 0.976899 21.00000 -1.50000 AFIX 0 C17A 1 0.231443 0.662767 1.017545 21.00000 0.07630 0.11316 = 0.04389 -0.03362 0.00002 -0.00615 AFIX 137 H17A 2 0.162841 0.735576 1.043802 21.00000 -1.50000 H17B 2 0.351639 0.637210 1.022060 21.00000 -1.50000 H17C 2 0.217161 0.562523 1.024961 21.00000 -1.50000 PART 2 AFIX 0 C15B 1 0.159873 0.692155 0.968440 -21.00000 0.06375 0.03378 = 0.04561 -0.01504 0.01192 -0.01403 AFIX 13 H15B 2 0.124784 0.609869 0.989540 -21.00000 -1.20000 AFIX 0 C16B 1 0.261863 0.739584 1.004923 -21.00000 0.09380 0.10609 = 0.05536 -0.04730 0.01426 -0.04303 AFIX 137 H16D 2 0.359669 0.641941 1.021522 -21.00000 -1.50000 H16E 2 0.188979 0.794301 1.034563 -21.00000 -1.50000 H16F 2 0.302132 0.812826 0.982003 -21.00000 -1.50000 AFIX 0 C17B 1 0.006828 0.846167 0.943404 -21.00000 0.06196 0.07345 = 0.06362 -0.02425 -0.00449 0.02360 AFIX 137 H17D 2 0.047067 0.918609 0.919945 -21.00000 -1.50000 H17E 2 -0.063188 0.901138 0.973476 -21.00000 -1.50000 H17F 2 -0.061304 0.817282 0.920775 -21.00000 -1.50000 PART 0 AFIX 0 P1 4 0.344591 0.503123 0.710037 11.00000 0.02548 0.03321 = 0.02612 -0.00514 -0.00170 -0.00452 O1 3 0.626094 0.219459 0.650504 11.00000 0.04024 0.04463 = 0.03381 -0.01793 -0.00490 -0.00209 O2 3 0.054980 0.653918 0.575489 11.00000 0.03202 0.05207 = 0.03657 0.00178 -0.00952 -0.00950 O3 3 0.239054 0.454566 0.526143 11.00000 0.05601 0.05708 = 0.03217 -0.01045 -0.00832 -0.02453 C1 1 0.557245 0.332188 0.736187 11.00000 0.02740 0.02787 = 0.02816 -0.00447 -0.00205 -0.00768 C2 1 0.677322 0.211618 0.704832 11.00000 0.03217 0.03129 = 0.03155 -0.00709 -0.00213 -0.00864 C3 1 0.738280 0.098328 0.617654 11.00000 0.04617 0.05143 = 0.04132 -0.02290 0.00509 -0.01344 AFIX 137 H3A 2 0.847847 0.103810 0.613337 11.00000 -1.50000 H3B 2 0.686896 0.118558 0.580862 11.00000 -1.50000 H3C 2 0.756155 -0.009506 0.636494 11.00000 -1.50000 AFIX 0 C4 1 0.836688 0.093186 0.727157 11.00000 0.03388 0.03940 = 0.04315 -0.01272 -0.00086 0.00080 AFIX 43 H4 2 0.912973 0.015923 0.705290 11.00000 -1.20000 AFIX 0 C5 1 0.881434 0.090690 0.782093 11.00000 0.03421 0.05094 = 0.04690 -0.00902 -0.01133 0.00499 AFIX 43 H5 2 0.988798 0.012624 0.797196 11.00000 -1.20000 AFIX 0 C6 1 0.766739 0.204023 0.814436 11.00000 0.04086 0.05063 = 0.03259 -0.00818 -0.01245 -0.00080 AFIX 43 H6 2 0.797740 0.201220 0.851435 11.00000 -1.20000 AFIX 0 C7 1 0.604320 0.323507 0.792839 11.00000 0.03269 0.03215 = 0.03015 -0.00597 -0.00325 -0.00824 C8 1 0.486420 0.432385 0.834253 11.00000 0.03500 0.03672 = 0.02632 -0.00670 -0.00636 -0.00268 C9 1 0.492685 0.581832 0.840116 11.00000 0.04741 0.03704 = 0.03439 -0.01016 -0.00844 -0.00464 C10 1 0.617960 0.638784 0.806715 11.00000 0.06618 0.04731 = 0.04288 -0.01645 -0.00016 -0.02210 AFIX 13 H10 2 0.669237 0.568870 0.776998 11.00000 -1.20000 AFIX 0 C11 1 0.528691 0.818815 0.777748 11.00000 0.11461 0.05081 = 0.06423 -0.00989 -0.00335 -0.03483 AFIX 137 H11A 2 0.427396 0.835863 0.757458 11.00000 -1.50000 H11B 2 0.607602 0.842398 0.751615 11.00000 -1.50000 H11C 2 0.495098 0.891071 0.806008 11.00000 -1.50000 AFIX 0 C12 1 0.764937 0.615820 0.845345 11.00000 0.06742 0.09894 = 0.07287 -0.02635 -0.00057 -0.03437 AFIX 137 H12A 2 0.717339 0.679689 0.875793 11.00000 -1.50000 H12B 2 0.843183 0.652352 0.823735 11.00000 -1.50000 H12C 2 0.826724 0.500977 0.860802 11.00000 -1.50000 AFIX 0 C13 1 0.387646 0.674111 0.880618 11.00000 0.05720 0.04582 = 0.04955 -0.02202 -0.00186 -0.00687 AFIX 43 H13 2 0.390420 0.773260 0.884074 11.00000 -1.20000 AFIX 0 C14 1 0.280206 0.625581 0.915679 11.00000 0.05235 0.06202 = 0.04591 -0.02866 -0.00014 -0.00209 C18 1 0.279581 0.475532 0.910647 11.00000 0.04698 0.06792 = 0.03907 -0.01527 0.00540 -0.01264 AFIX 43 H18 2 0.208492 0.440090 0.934397 11.00000 -1.20000 AFIX 0 C19 1 0.382417 0.376611 0.871033 11.00000 0.03930 0.04506 = 0.03058 -0.00801 -0.00546 -0.00648 C20 1 0.386821 0.206518 0.872216 11.00000 0.04998 0.05072 = 0.03726 -0.00597 0.00080 -0.01622 AFIX 13 H20 2 0.437046 0.167235 0.836355 11.00000 -1.20000 AFIX 0 C21 1 0.206662 0.207903 0.877886 11.00000 0.06508 0.08068 = 0.06977 -0.01646 0.01637 -0.03628 AFIX 137 H21A 2 0.164602 0.224123 0.915768 11.00000 -1.50000 H21B 2 0.214997 0.104231 0.870364 11.00000 -1.50000 H21C 2 0.127759 0.296219 0.851072 11.00000 -1.50000 AFIX 0 C22 1 0.504579 0.084263 0.920636 11.00000 0.10067 0.05728 = 0.06011 0.00940 -0.01969 -0.02122 AFIX 137 H22A 2 0.620416 0.074615 0.914872 11.00000 -1.50000 H22B 2 0.505763 -0.021976 0.921315 11.00000 -1.50000 H22C 2 0.461601 0.123277 0.956169 11.00000 -1.50000 AFIX 0 C23 1 0.382142 0.621979 0.641182 11.00000 0.02798 0.02867 = 0.02972 -0.00405 -0.00345 -0.00922 C24 1 0.562128 0.621843 0.643656 11.00000 0.03335 0.03900 = 0.03860 -0.00891 -0.00238 -0.01488 AFIX 23 H24A 2 0.576861 0.646401 0.680538 11.00000 -1.20000 H24B 2 0.651683 0.512012 0.640014 11.00000 -1.20000 AFIX 0 C25 1 0.586907 0.747326 0.597141 11.00000 0.04552 0.05595 = 0.05232 -0.00796 0.00117 -0.03072 AFIX 23 H25A 2 0.699386 0.745207 0.602150 11.00000 -1.20000 H25B 2 0.585214 0.716194 0.560215 11.00000 -1.20000 AFIX 0 C26 1 0.444949 0.922222 0.598851 11.00000 0.06788 0.04714 = 0.06389 -0.00185 -0.00431 -0.03418 AFIX 23 H26A 2 0.456028 0.958827 0.633787 11.00000 -1.20000 H26B 2 0.459453 0.996786 0.567192 11.00000 -1.20000 AFIX 0 C27 1 0.264729 0.929420 0.595624 11.00000 0.05464 0.03223 = 0.05874 -0.00091 -0.00933 -0.01482 AFIX 23 H27A 2 0.247973 0.906946 0.558608 11.00000 -1.20000 H27B 2 0.177499 1.039706 0.599940 11.00000 -1.20000 AFIX 0 C28 1 0.241608 0.803172 0.642089 11.00000 0.03606 0.03106 = 0.04210 -0.00728 -0.00466 -0.00793 AFIX 23 H28A 2 0.127818 0.807542 0.637656 11.00000 -1.20000 H28B 2 0.245272 0.834098 0.678898 11.00000 -1.20000 AFIX 0 C29 1 0.370037 0.559268 0.585859 11.00000 0.03198 0.03371 = 0.02698 -0.00418 -0.00128 -0.01177 AFIX 23 H29A 2 0.363124 0.643708 0.554185 11.00000 -1.20000 H29B 2 0.477916 0.462163 0.582048 11.00000 -1.20000 AFIX 0 C30 1 0.221077 0.514715 0.579553 11.00000 0.03221 0.03869 = 0.02800 -0.00460 -0.00408 -0.01382 C31 1 0.022129 0.724779 0.517245 11.00000 0.05536 0.05838 = 0.04318 0.01475 -0.01924 -0.02433 AFIX 23 H31A 2 0.039482 0.824537 0.509792 11.00000 -1.20000 H31B 2 -0.096093 0.752155 0.506735 11.00000 -1.20000 AFIX 0 C32 1 0.150953 0.593759 0.484434 11.00000 0.06050 0.07790 = 0.03091 0.00339 -0.01028 -0.03570 AFIX 23 H32A 2 0.091458 0.567038 0.457244 11.00000 -1.20000 H32B 2 0.231791 0.631250 0.464177 11.00000 -1.20000 AFIX 0 C33 1 0.221816 0.378201 0.624977 11.00000 0.03960 0.04486 = 0.03982 -0.00016 -0.01089 -0.02260 AFIX 23 H33A 2 0.328600 0.279833 0.621367 11.00000 -1.20000 H33B 2 0.126582 0.354256 0.616852 11.00000 -1.20000 AFIX 0 C34 1 0.206798 0.406351 0.687208 11.00000 0.03395 0.05486 = 0.03314 0.00479 -0.00573 -0.02262 C35 1 0.255024 0.236259 0.723385 11.00000 0.07661 0.08123 = 0.05321 0.02287 -0.02126 -0.05577 AFIX 137 H35A 2 0.178678 0.191884 0.713976 11.00000 -1.50000 H35B 2 0.243682 0.247867 0.762963 11.00000 -1.50000 H35C 2 0.372853 0.162724 0.715828 11.00000 -1.50000 AFIX 0 C36 1 0.017926 0.523491 0.700459 11.00000 0.03395 0.11455 = 0.04727 -0.00817 0.00233 -0.02972 AFIX 137 H36A 2 -0.012536 0.631155 0.678854 11.00000 -1.50000 H36B 2 0.007888 0.531644 0.740313 11.00000 -1.50000 H36C 2 -0.059036 0.480526 0.690449 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY5783_0m_a.res in P-1 REM R1 = 0.0495 for 5112 Fo > 4sig(Fo) and 0.0829 for all 7329 data REM 400 parameters refined using 7 restraints END WGHT 0.0831 0.1849 REM Highest difference peak 0.417, deepest hole -0.322, 1-sigma level 0.055 Q1 1 0.4055 0.5619 0.6936 11.00000 0.05 0.42 Q2 1 0.3044 0.5663 0.7392 11.00000 0.05 0.32 Q3 1 0.2936 0.5348 0.9292 11.00000 0.05 0.31 Q4 1 0.2659 0.4674 0.6916 11.00000 0.05 0.29 Q5 1 0.4616 0.4178 0.7180 11.00000 0.05 0.28 Q6 1 0.3851 0.5427 0.6667 11.00000 0.05 0.27 Q7 1 0.4617 0.6354 0.6400 11.00000 0.05 0.27 Q8 1 0.5414 0.3779 0.8138 11.00000 0.05 0.25 Q9 1 0.3631 0.6191 0.9082 11.00000 0.05 0.24 Q10 1 0.5854 0.1022 0.9370 11.00000 0.05 0.24 Q11 1 0.2857 0.5591 0.5809 11.00000 0.05 0.24 Q12 1 0.4801 0.3850 0.8634 11.00000 0.05 0.24 Q13 1 0.5233 0.4917 0.8493 11.00000 0.05 0.23 Q14 1 0.3722 0.5857 0.6170 11.00000 0.05 0.23 Q15 1 0.3068 0.2039 0.8753 11.00000 0.05 0.23 Q16 1 0.7004 0.2824 0.8011 11.00000 0.05 0.23 Q17 1 0.7383 0.1257 0.7215 11.00000 0.05 0.22 Q18 1 0.3730 0.2912 0.8852 11.00000 0.05 0.22 Q19 1 0.5587 0.2959 0.7721 11.00000 0.05 0.22 Q20 1 0.2370 0.6753 0.9352 11.00000 0.05 0.22 ; _shelx_res_checksum 74176 _shelx_hkl_file ; 1 0 0 5329.07 59.39 1 0 0 5271.37 59.59 1 0 0 5330.47 59.99 1 0 0 5262.27 58.49 2 0 0 1365.66 16.00 2 0 0 1387.96 16.10 2 0 0 1362.06 16.40 2 0 0 1376.36 16.40 3 0 0 91.69 3.50 3 0 0 96.49 3.00 3 0 0 91.09 3.10 3 0 0 95.69 3.40 4 0 0 134.49 4.10 4 0 0 131.89 3.70 4 0 0 134.49 4.40 4 0 0 131.59 4.50 5 0 0 618.54 9.70 5 0 0 620.54 10.40 5 0 0 598.94 9.40 5 0 0 630.34 10.40 6 0 0 10.70 3.60 6 0 0 8.50 3.30 6 0 0 9.80 3.60 6 0 0 9.10 2.80 7 0 0 113.39 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4.00 2.40 -6 -6 4 5.50 3.00 5 6 -4 99.19 7.00 -5 -6 4 111.19 4.40 -5 -6 4 111.49 5.40 4 6 -4 89.69 4.80 4 6 -4 99.89 6.40 -4 -6 4 99.59 4.30 -4 -6 4 94.19 4.70 3 6 -4 39.60 4.20 3 6 -4 32.20 3.50 -3 -6 4 37.30 3.60 -3 -6 4 35.40 3.00 2 6 -4 489.25 9.70 2 6 -4 489.85 9.30 -2 -6 4 489.75 8.00 -2 -6 4 510.25 8.80 1 6 -4 336.87 8.20 1 6 -4 343.07 8.10 -1 -6 4 345.87 7.50 -1 -6 4 336.97 6.20 0 6 -4 26.80 4.20 0 6 -4 28.90 3.90 0 -6 4 26.30 3.30 -1 6 -4 67.09 6.40 -1 6 -4 72.99 5.90 1 -6 4 80.19 5.50 -2 6 -4 92.79 7.20 2 -6 4 92.39 6.20 -3 6 -4 13.90 5.40 3 -6 4 21.90 4.30 -4 6 -4 60.59 7.00 4 -6 4 57.29 5.60 -5 6 -4 12.20 6.50 5 -6 4 21.70 5.50 10 5 -4 8.50 6.10 -10 -5 4 0.10 5.10 9 5 -4 5.30 5.60 -9 -5 4 2.10 4.50 8 5 -4 5.60 4.90 -8 -5 4 2.90 3.90 7 5 -4 138.39 7.90 6 5 -4 2.20 4.10 -6 -5 4 4.30 2.80 -6 -5 4 2.60 2.30 5 5 -4 1253.17 18.60 -5 -5 4 1241.38 16.20 -5 -5 4 1248.68 17.20 4 5 -4 858.11 13.70 4 5 -4 824.62 11.40 -4 -5 4 836.12 12.20 -4 -5 4 845.12 11.70 3 5 -4 147.29 4.50 3 5 -4 162.68 6.00 -3 -5 4 157.38 4.30 -3 -5 4 161.48 4.40 2 5 -4 25.20 2.80 2 5 -4 25.40 3.20 -2 -5 4 24.10 2.10 -2 -5 4 27.50 2.50 1 5 -4 54.99 4.60 1 5 -4 52.19 4.40 -1 -5 4 55.69 2.60 -1 -5 4 62.79 3.80 0 5 -4 609.94 10.30 0 5 -4 613.84 10.80 0 -5 4 612.54 10.00 0 -5 4 588.94 8.30 -1 5 -4 288.57 8.00 -1 5 -4 284.57 7.30 1 -5 4 285.17 7.00 -2 5 -4 191.38 7.60 -2 5 -4 179.48 6.80 2 -5 4 174.58 6.20 3 -5 4 281.07 8.00 -4 5 -4 24.70 5.50 4 -5 4 19.30 4.30 -5 5 -4 32.40 6.40 5 -5 4 35.40 5.40 -6 5 -4 3.60 6.10 6 -5 4 -7.30 4.90 10 4 -4 -1.20 6.10 -10 -4 4 4.20 5.00 9 4 -4 4.20 5.50 -9 -4 4 4.20 4.50 8 4 -4 0.80 4.60 -8 -4 4 1.20 3.70 7 4 -4 253.27 8.90 -7 -4 4 255.77 6.30 -7 -4 4 250.07 7.70 6 4 -4 39.80 4.50 -6 -4 4 40.60 3.90 -6 -4 4 37.50 3.60 5 4 -4 4.90 3.30 -5 -4 4 6.50 2.20 -5 -4 4 4.40 2.20 4 4 -4 183.58 6.10 -4 -4 4 182.58 4.90 -4 -4 4 189.58 4.40 3 4 -4 41.50 4.40 3 4 -4 49.50 3.00 -3 -4 4 39.30 2.90 -3 -4 4 37.80 2.70 2 4 -4 12.10 2.10 2 4 -4 9.70 2.70 -2 -4 4 13.00 1.70 -2 -4 4 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11.10 3.70 -2 -6 5 9.60 2.10 -2 -6 5 12.20 2.70 1 6 -5 43.80 4.20 1 6 -5 43.70 4.10 -1 -6 5 46.10 3.60 -1 -6 5 37.70 3.10 0 6 -5 37.40 4.30 0 6 -5 36.90 4.40 0 -6 5 39.70 3.70 -1 6 -5 181.88 7.70 -1 6 -5 179.48 7.10 1 -6 5 176.08 6.70 -2 6 -5 7.10 4.60 2 -6 5 5.00 3.50 -3 6 -5 61.19 6.30 3 -6 5 71.39 5.40 -4 6 -5 34.90 6.40 4 -6 5 36.40 5.30 -5 6 -5 -1.50 6.30 5 -6 5 8.40 5.10 10 5 -5 24.30 6.60 -10 -5 5 30.30 6.30 9 5 -5 65.79 6.80 -9 -5 5 64.59 6.00 8 5 -5 23.30 5.40 -8 -5 5 23.70 4.30 7 5 -5 89.69 7.40 -7 -5 5 72.09 5.60 -7 -5 5 73.09 4.70 6 5 -5 192.88 8.00 -6 -5 5 191.78 5.50 -6 -5 5 187.98 6.30 5 5 -5 86.19 6.30 -5 -5 5 89.29 4.10 -5 -5 5 79.39 4.70 4 5 -5 135.49 6.30 -4 -5 5 140.39 4.80 -4 -5 5 142.29 4.40 3 5 -5 53.59 3.60 3 5 -5 50.89 5.10 -3 -5 5 60.29 3.40 -3 -5 5 59.79 3.40 2 5 -5 105.39 5.40 2 5 -5 107.39 4.40 -2 -5 5 108.19 4.10 -2 -5 5 105.89 3.50 1 5 -5 15.40 3.20 1 5 -5 11.40 2.90 -1 -5 5 13.00 1.70 -1 -5 5 15.90 2.50 0 5 -5 49.50 5.10 0 5 -5 39.20 3.80 0 -5 5 34.00 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42.30 5.10 -4 6 -8 39.00 6.80 4 -6 8 37.50 5.40 -5 6 -8 17.50 6.80 5 -6 8 13.40 5.50 10 5 -8 7.10 6.40 -10 -5 8 9.00 5.80 9 5 -8 15.50 5.90 -9 -5 8 5.90 4.90 8 5 -8 3.00 5.10 -8 -5 8 2.80 4.20 7 5 -8 3.80 4.80 -7 -5 8 -1.80 3.30 -7 -5 8 1.00 3.10 6 5 -8 4.40 4.40 -6 -5 8 -2.10 2.80 -6 -5 8 -5.70 2.90 5 5 -8 72.09 6.70 -5 -5 8 56.59 4.70 -5 -5 8 61.09 4.40 4 5 -8 -1.10 3.60 -4 -5 8 1.60 2.30 -4 -5 8 0.40 2.40 3 5 -8 1.50 3.40 3 5 -8 -1.70 2.50 -3 -5 8 1.90 1.90 -3 -5 8 1.20 2.40 2 5 -8 9.80 3.70 2 5 -8 10.50 2.60 -2 -5 8 9.50 2.50 -2 -5 8 13.70 1.90 1 5 -8 97.59 5.20 1 5 -8 92.89 6.20 -1 -5 8 92.89 4.70 0 5 -8 492.45 10.50 0 5 -8 486.35 9.90 0 -5 8 488.85 9.20 -1 5 -8 450.45 10.10 -1 5 -8 456.35 10.20 1 -5 8 435.96 9.10 -2 5 -8 0.80 4.00 -2 5 -8 -4.30 4.20 2 -5 8 6.20 3.40 -3 5 -8 16.60 5.00 -3 5 -8 21.20 4.90 3 -5 8 19.10 4.00 -4 5 -8 191.08 9.60 4 -5 8 202.68 8.20 -5 5 -8 27.70 6.30 5 -5 8 29.30 5.20 -6 5 -8 16.30 7.00 6 -5 8 18.60 5.70 10 4 -8 20.10 6.60 -10 -4 8 22.30 5.90 9 4 -8 56.39 6.60 -9 -4 8 56.89 6.00 8 4 -8 3.30 4.10 8 4 -8 7.40 5.00 -8 -4 8 0.60 3.50 7 4 -8 2.50 4.30 7 4 -8 -0.90 3.50 -7 -4 8 -2.30 3.00 6 4 -8 117.69 6.00 6 4 -8 130.49 7.20 -6 -4 8 110.89 5.40 5 4 -8 16.70 3.20 5 4 -8 19.20 4.00 -5 -4 8 18.60 2.90 4 4 -8 2.30 3.30 4 4 -8 0.90 2.60 -4 -4 8 -0.70 2.20 3 4 -8 14.90 3.30 -3 -4 8 13.90 2.10 -3 -4 8 15.30 2.40 2 4 -8 102.19 5.50 2 4 -8 100.69 3.70 -2 -4 8 107.29 3.30 -2 -4 8 104.59 4.10 1 4 -8 11.20 3.30 1 4 -8 10.20 2.40 -1 -4 8 11.20 1.40 -1 -4 8 8.00 2.20 0 4 -8 47.70 4.40 0 4 -8 50.99 5.40 0 -4 8 52.89 3.80 -1 4 -8 23.60 4.00 1 -4 8 17.30 2.90 -2 4 -8 57.29 6.20 2 -4 8 68.59 4.90 2 -4 8 65.09 5.90 -3 4 -8 62.69 6.80 3 -4 8 71.09 6.70 3 -4 8 62.09 5.50 -4 4 -8 88.79 7.80 4 -4 8 97.49 7.70 4 -4 8 101.79 6.30 -5 4 -8 225.98 10.20 -5 4 -8 209.88 11.00 5 -4 8 219.48 8.50 -6 4 -8 4.50 5.70 6 -4 8 2.00 4.70 -7 4 -8 17.50 6.70 7 -4 8 9.30 5.60 -10 -3 8 14.50 5.50 9 3 -8 129.19 9.20 9 3 -8 126.39 8.10 8 3 -8 9.60 4.10 8 3 -8 5.00 4.60 -8 -3 8 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45.70 3.90 6 2 -8 54.19 5.70 -6 -2 8 58.59 4.60 5 2 -8 14.70 2.80 5 2 -8 20.20 3.30 -5 -2 8 23.30 2.90 4 2 -8 6.50 2.80 4 2 -8 4.40 2.30 -4 -2 8 5.90 2.20 3 2 -8 150.68 5.10 3 2 -8 157.78 4.50 -3 -2 8 159.78 4.40 2 2 -8 815.12 12.00 2 2 -8 841.82 11.00 -2 -2 8 836.02 11.30 1 2 -8 212.18 4.00 1 2 -8 216.38 5.80 -1 -2 8 212.38 4.60 -1 -2 8 208.88 4.00 0 2 -8 970.40 13.90 0 2 -8 971.10 11.50 0 -2 8 980.80 12.90 0 -2 8 1000.70 13.00 -1 2 -8 42.70 4.40 1 -2 8 37.70 3.50 1 -2 8 33.50 3.00 -2 2 -8 61.69 4.70 2 -2 8 61.19 4.30 2 -2 8 64.99 3.80 -3 2 -8 21.70 3.50 3 -2 8 20.60 2.90 3 -2 8 23.90 3.50 -4 2 -8 3.40 3.60 4 -2 8 1.10 3.40 4 -2 8 4.60 3.10 -5 2 -8 179.18 7.70 5 -2 8 179.98 7.90 5 -2 8 173.88 6.60 -6 2 -8 14.70 4.80 6 -2 8 14.40 4.20 6 -2 8 17.00 5.20 -7 2 -8 142.19 9.20 7 -2 8 152.78 10.00 7 -2 8 138.39 7.60 8 -2 8 86.79 8.20 9 1 -8 8.30 4.60 -9 -1 8 12.50 4.30 8 1 -8 6.00 4.00 -8 -1 8 4.50 3.60 7 1 -8 14.70 3.70 7 1 -8 15.50 4.10 -7 -1 8 4.70 3.30 6 1 -8 64.99 5.60 6 1 -8 66.99 5.20 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6.50 -6 -4 14 74.19 6.00 5 4 -14 6.10 4.50 5 4 -14 7.30 3.60 -5 -4 14 6.20 3.40 4 4 -14 80.39 6.90 4 4 -14 80.09 5.50 -4 -4 14 82.29 5.40 3 4 -14 84.19 5.10 3 4 -14 75.59 6.80 -3 -4 14 76.19 5.10 2 4 -14 -0.90 3.40 2 4 -14 5.20 4.30 -2 -4 14 0.70 2.80 1 4 -14 35.50 5.30 -1 -4 14 38.80 3.70 -1 -4 14 37.40 3.50 0 4 -14 7.00 5.00 0 -4 14 7.90 3.10 0 -4 14 5.40 3.40 -1 4 -14 4.40 5.00 1 -4 14 9.80 3.90 1 -4 14 14.80 3.50 -2 4 -14 216.78 10.00 2 -4 14 216.18 8.30 2 -4 14 218.48 7.60 -3 4 -14 25.60 6.00 3 -4 14 34.20 5.50 3 -4 14 40.10 4.80 -4 4 -14 -14.40 5.80 4 -4 14 1.10 4.30 4 -4 14 -1.20 5.00 -5 4 -14 -10.00 6.30 5 -4 14 8.10 6.20 5 -4 14 12.60 4.80 -6 4 -14 17.60 8.10 6 -4 14 38.90 5.80 6 -4 14 49.70 7.80 9 3 -14 3.70 5.00 -9 -3 14 0.60 4.80 8 3 -14 5.60 4.90 8 3 -14 -0.70 4.40 -8 -3 14 -3.40 4.20 7 3 -14 132.69 8.20 7 3 -14 114.29 7.40 -7 -3 14 109.29 7.00 6 3 -14 -2.30 3.40 6 3 -14 2.00 4.10 -6 -3 14 -4.10 3.40 5 3 -14 15.00 3.60 5 3 -14 22.20 4.40 -5 -3 14 15.30 3.50 4 3 -14 86.69 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20.40 6.00 -5 -4 -25 4.50 6.20 5 4 25 16.20 6.10 -6 -4 -25 -9.50 6.40 6 4 25 3.50 6.40 2 -5 -25 9.20 5.30 -2 5 25 1.10 4.40 1 -5 -25 29.80 5.70 -1 5 25 26.50 4.70 0 -5 -25 0.90 4.80 0 5 25 9.90 4.80 -1 -5 -25 11.60 4.90 1 5 25 26.80 5.50 -2 -5 -25 10.40 4.80 2 5 25 17.60 5.30 -3 -5 -25 4.20 4.90 3 5 25 11.20 5.30 -4 -5 -25 2.90 4.90 4 5 25 -0.20 5.50 -5 -5 -25 -9.10 5.70 5 5 25 4.90 5.80 -6 -5 -25 -6.00 6.60 6 5 25 -2.20 6.20 1 -6 -25 21.10 5.90 0 -6 -25 12.00 5.50 0 6 25 14.90 5.30 -1 -6 -25 21.80 5.60 1 6 25 23.90 5.60 -2 -6 -25 55.99 6.10 2 6 25 52.39 6.40 -3 -6 -25 19.40 5.60 3 6 25 16.50 5.90 -4 -6 -25 30.30 5.80 4 6 25 29.90 6.60 -5 -6 -25 3.40 5.30 5 6 25 0.70 6.30 6 6 25 13.50 6.70 0 -7 -25 18.30 5.80 0 7 25 28.50 6.30 -1 -7 -25 46.10 6.40 1 7 25 46.70 6.50 -2 -7 -25 21.00 5.80 2 7 25 21.40 6.20 -3 -7 -25 5.30 5.60 3 7 25 15.50 6.10 -4 -7 -25 19.70 5.90 4 7 25 19.90 6.70 -5 -7 -25 -0.30 5.50 5 7 25 3.00 6.40 -6 -7 -25 -2.20 5.60 6 7 25 6.00 7.10 -2 -8 -25 17.50 6.00 2 8 25 18.40 6.30 -3 -8 -25 6.10 6.00 3 8 25 11.60 6.50 -4 -8 -25 -5.70 5.80 4 8 25 14.70 6.60 3 4 -26 11.30 6.30 -3 -4 26 7.50 5.00 2 4 -26 10.10 6.90 -2 -4 26 7.70 5.00 1 4 -26 1.30 7.20 -1 -4 26 10.20 5.10 0 4 -26 1.70 7.60 0 -4 26 8.20 5.20 4 3 -26 9.10 5.80 -4 -3 26 3.90 4.80 3 3 -26 14.30 5.90 -3 -3 26 -7.20 4.50 2 3 -26 9.40 6.40 -2 -3 26 29.90 5.40 1 3 -26 -2.20 6.50 -1 -3 26 9.80 4.80 0 3 -26 6.80 7.50 0 -3 26 16.00 5.00 -1 3 -26 1.00 7.60 1 -3 26 17.70 5.10 -2 3 -26 -17.50 8.00 2 -3 26 6.00 4.90 5 2 -26 4.60 5.00 -5 -2 26 5.40 5.00 4 2 -26 13.40 5.70 -4 -2 26 14.70 5.10 3 2 -26 13.10 5.50 -3 -2 26 6.40 4.60 2 2 -26 3.70 5.80 -2 -2 26 1.20 4.40 1 2 -26 79.59 8.00 -1 -2 26 104.19 7.80 0 2 -26 13.00 6.80 0 -2 26 34.10 5.20 -1 2 -26 -8.00 7.00 1 -2 26 3.10 4.60 -2 2 -26 -12.40 7.60 2 -2 26 9.50 4.80 5 1 -26 1.20 4.80 -5 -1 26 -3.00 4.90 4 1 -26 22.20 4.90 -4 -1 26 15.20 5.00 -3 -1 26 8.40 4.60 2 1 -26 14.40 5.60 -2 -1 26 8.90 4.30 1 1 -26 1.70 5.80 -1 -1 26 13.10 4.40 0 1 -26 9.20 6.40 0 -1 26 24.90 4.70 -1 1 -26 -11.20 6.50 1 -1 26 17.00 4.60 -2 1 -26 -7.80 6.80 2 -1 26 8.80 4.40 -3 1 -26 -17.90 7.50 3 -1 26 2.20 5.20 -4 1 -26 -18.30 8.10 4 -1 26 3.20 5.70 5 0 -26 -0.10 4.90 -5 0 26 -3.00 4.80 4 0 -26 36.90 5.40 -4 0 26 27.20 5.30 3 0 -26 16.90 4.70 -3 0 26 10.70 4.70 2 0 -26 2.50 4.30 -2 0 26 1.20 4.20 1 0 -26 6.60 5.70 -1 0 26 5.70 4.20 0 0 -26 -0.70 5.90 0 0 26 7.10 4.10 -1 0 -26 68.39 7.90 1 0 26 82.69 6.80 -2 0 -26 -19.70 6.40 2 0 26 7.10 5.50 -3 0 -26 84.59 8.70 3 0 26 109.49 8.50 -4 0 -26 8.10 7.80 4 0 26 17.10 5.70 -5 0 -26 -1.50 8.90 5 0 26 24.00 6.50 4 -1 -26 42.70 5.70 -4 1 26 33.60 5.40 3 -1 -26 3.10 4.50 -3 1 26 -6.10 4.20 2 -1 -26 10.80 4.50 -2 1 26 -4.70 4.00 1 -1 -26 32.80 4.70 -1 1 26 27.30 4.60 0 -1 -26 6.60 5.70 0 1 26 7.20 4.00 -1 -1 -26 3.80 6.00 1 1 26 13.00 3.90 -2 -1 -26 8.30 6.60 2 1 26 17.40 4.80 -3 -1 -26 70.69 7.90 3 1 26 81.09 8.10 -4 -1 -26 25.60 7.60 4 1 26 30.10 5.90 -5 -1 -26 -8.50 7.40 5 1 26 -1.00 5.60 4 -2 -26 20.70 5.50 -4 2 26 9.70 5.00 3 -2 -26 13.10 5.00 -3 2 26 7.00 4.60 2 -2 -26 10.80 4.80 -2 2 26 6.80 4.20 1 -2 -26 12.30 4.60 -1 2 26 2.30 4.00 0 -2 -26 26.60 4.50 0 2 26 25.60 4.30 -1 -2 -26 -8.50 5.40 -2 -2 -26 56.99 7.20 2 2 26 73.19 7.60 -3 -2 -26 54.09 7.30 3 2 26 78.09 8.40 -4 -2 -26 -13.30 6.30 4 2 26 7.70 5.20 -5 -2 -26 -10.10 6.80 5 2 26 -2.90 5.60 -6 -2 -26 -5.00 7.40 6 2 26 1.70 6.50 3 -3 -26 25.10 5.50 -3 3 26 6.40 4.70 2 -3 -26 -1.30 4.70 -2 3 26 -4.80 4.20 1 -3 -26 -0.60 4.40 -1 3 26 -2.30 4.00 0 -3 -26 39.90 5.20 0 3 26 23.90 4.20 -1 -3 -26 40.80 5.10 1 3 26 41.70 5.30 2 3 26 11.00 4.80 -3 -3 -26 52.99 7.00 3 3 26 90.79 8.70 -4 -3 -26 6.80 6.30 4 3 26 14.40 5.90 -5 -3 -26 12.90 7.00 5 3 26 15.90 6.20 -6 -3 -26 18.20 7.40 6 3 26 27.00 7.00 3 -4 -26 7.20 5.40 -3 4 26 -0.90 4.60 2 -4 -26 21.10 5.70 -2 4 26 12.50 4.80 1 -4 -26 58.99 6.10 -1 4 26 38.00 5.00 0 -4 -26 107.79 8.30 -1 -4 -26 18.60 5.00 1 4 26 27.00 5.10 -2 -4 -26 21.80 4.90 2 4 26 21.90 5.40 3 4 26 111.09 9.00 -4 -4 -26 -13.80 5.70 4 4 26 11.20 5.70 -5 -4 -26 -2.10 6.30 5 4 26 6.50 6.20 -6 -4 -26 0.10 6.70 6 4 26 27.00 7.10 2 -5 -26 2.80 5.40 -2 5 26 -5.60 4.50 1 -5 -26 157.78 9.50 -1 5 26 119.89 8.70 0 -5 -26 103.99 9.00 0 5 26 115.09 10.10 -1 -5 -26 8.40 5.00 1 5 26 17.60 5.20 -2 -5 -26 42.40 5.60 2 5 26 40.20 5.90 -3 -5 -26 20.00 5.20 3 5 26 23.80 5.70 -4 -5 -26 17.40 7.40 4 5 26 8.80 5.90 -5 -5 -26 -9.00 7.00 5 5 26 5.20 6.30 -6 -5 -26 13.60 7.10 6 5 26 21.80 7.00 1 -6 -26 21.90 6.00 0 -6 -26 135.29 9.60 0 6 26 137.09 9.30 -1 -6 -26 2.40 5.10 1 6 26 18.60 5.70 -2 -6 -26 38.40 5.70 2 6 26 40.00 6.30 -3 -6 -26 10.40 5.40 3 6 26 10.60 5.90 -4 -6 -26 11.50 5.40 4 6 26 8.00 5.90 -5 -6 -26 0.60 5.70 5 6 26 8.60 6.40 6 6 26 6.10 7.00 -1 -7 -26 41.30 6.50 1 7 26 56.89 6.80 -2 -7 -26 0.80 5.40 2 7 26 9.80 5.90 -3 -7 -26 8.00 5.80 3 7 26 24.70 6.40 -4 -7 -26 25.40 6.10 4 7 26 25.60 6.90 -5 -7 -26 3.30 5.60 5 7 26 18.90 6.90 3 3 -27 11.20 5.90 -3 -3 27 3.80 4.80 2 3 -27 5.10 6.60 -2 -3 27 2.00 5.00 1 3 -27 5.00 7.20 -1 -3 27 6.40 5.00 0 3 -27 0.80 7.60 0 -3 27 3.40 5.00 -1 3 -27 -7.70 7.70 1 -3 27 15.50 5.20 -4 -2 27 2.20 4.90 3 2 -27 15.50 5.60 -3 -2 27 5.40 4.70 2 2 -27 3.20 6.00 -2 -2 27 5.50 4.70 1 2 -27 15.00 6.60 -1 -2 27 12.90 4.90 0 2 -27 -9.60 6.70 0 -2 27 4.70 4.80 -1 2 -27 -8.00 7.40 1 -2 27 8.90 4.90 -2 2 -27 -8.40 8.10 2 -2 27 15.20 5.10 4 1 -27 -0.10 4.70 -4 -1 27 4.60 5.10 -3 -1 27 11.80 4.90 2 1 -27 28.00 6.10 -2 -1 27 24.80 4.80 1 1 -27 4.00 6.20 -1 -1 27 1.30 4.20 0 1 -27 -9.40 6.20 0 -1 27 0.20 4.50 -1 1 -27 -8.20 7.10 1 -1 27 -1.30 4.50 -2 1 -27 -10.20 7.50 -3 1 -27 -23.00 7.80 4 0 -27 7.60 4.80 -4 0 27 -7.00 4.70 3 0 -27 4.20 4.60 -3 0 27 -1.10 4.50 -2 0 27 8.60 4.50 1 0 -27 17.40 5.90 -1 0 27 20.20 4.60 0 0 -27 -17.70 5.80 0 0 27 6.30 4.20 -1 0 -27 -14.00 6.20 1 0 27 7.20 4.30 -2 0 -27 -8.50 6.70 -3 0 -27 -12.30 7.00 3 0 27 5.50 5.10 -4 0 -27 -15.40 7.90 4 0 27 7.40 5.70 4 -1 -27 6.90 5.00 -4 1 27 2.60 4.90 3 -1 -27 39.40 5.40 -3 1 27 26.70 5.20 2 -1 -27 13.80 4.60 -2 1 27 3.70 4.40 -1 1 27 26.20 4.70 0 -1 -27 -0.50 5.80 0 1 27 7.20 4.10 -1 -1 -27 -14.70 6.00 1 1 27 2.50 5.90 -2 -1 -27 -8.20 6.50 2 1 27 2.90 6.00 -3 -1 -27 10.00 7.20 3 1 27 28.50 5.70 -4 -1 -27 34.40 7.90 4 1 27 43.10 6.60 -5 -1 -27 -2.50 7.90 5 1 27 20.50 6.40 3 -2 -27 57.59 6.10 -3 2 27 54.89 5.90 2 -2 -27 47.10 5.70 -2 2 27 30.50 5.00 1 -2 -27 -0.60 4.40 -1 2 27 1.20 4.30 0 -2 -27 29.20 5.20 0 2 27 25.70 4.40 -2 -2 -27 -8.20 6.20 2 2 27 14.50 5.00 -3 -2 -27 0.70 6.50 3 2 27 15.90 5.50 -4 -2 -27 -20.00 6.50 4 2 27 1.90 5.40 -5 -2 -27 28.00 8.00 5 2 27 46.20 6.90 3 -3 -27 58.19 6.30 -3 3 27 45.30 5.90 2 -3 -27 33.00 5.70 -2 3 27 30.80 5.20 1 -3 -27 3.70 4.80 -1 3 27 -2.40 4.10 0 -3 -27 25.60 5.00 -1 -3 -27 39.90 5.20 2 3 27 31.80 5.60 -3 -3 -27 -16.70 5.80 3 3 27 3.20 5.20 -4 -3 -27 6.70 6.60 4 3 27 8.40 5.80 -5 -3 -27 -7.50 6.90 5 3 27 8.80 6.00 2 -4 -27 15.70 5.60 -2 4 27 0.90 4.70 1 -4 -27 8.20 5.20 -1 4 27 4.60 4.50 0 -4 -27 40.20 5.60 -1 -4 -27 52.79 5.80 1 4 27 49.50 5.80 -2 -4 -27 26.20 5.20 2 4 27 22.90 5.60 3 4 27 9.80 5.50 -4 -4 -27 -17.30 6.00 4 4 27 9.80 6.00 -5 -4 -27 1.20 6.70 5 4 27 13.00 6.60 1 -5 -27 10.10 5.50 0 -5 -27 32.70 5.80 -1 -5 -27 85.19 8.30 1 5 27 98.69 8.90 -2 -5 -27 40.40 5.90 2 5 27 41.40 6.20 -3 -5 -27 14.90 5.10 3 5 27 11.30 5.60 4 5 27 31.40 6.60 5 5 27 17.40 6.70 0 -6 -27 21.10 6.00 -1 -6 -27 21.40 5.80 1 6 27 31.50 6.30 -2 -6 -27 21.30 5.60 2 6 27 25.10 6.00 -3 -6 -27 24.20 5.70 3 6 27 35.80 6.60 -4 -6 -27 8.80 5.70 4 6 27 18.90 6.40 5 6 27 45.10 7.70 -2 -7 -27 42.60 6.50 2 7 27 47.90 7.10 -3 -7 -27 10.30 5.70 3 7 27 20.60 6.40 -4 -7 -27 11.30 6.00 4 7 27 10.90 6.60 1 3 -28 21.10 7.30 -1 -3 28 11.10 5.30 3 2 -28 29.80 6.30 -3 -2 28 20.10 5.30 2 2 -28 21.00 6.70 -2 -2 28 12.70 4.90 1 2 -28 2.70 7.00 -1 -2 28 11.20 5.10 0 2 -28 -9.80 7.10 0 -2 28 8.90 5.00 -1 2 -28 -7.90 7.50 1 -2 28 16.90 5.20 -3 -1 28 10.10 5.10 2 1 -28 11.70 6.10 -2 -1 28 5.00 4.70 1 1 -28 -1.40 6.40 -1 -1 28 3.20 4.40 0 1 -28 21.40 7.20 0 -1 28 39.50 5.50 -1 1 -28 20.40 7.60 1 -1 28 31.90 5.30 -2 1 -28 1.70 7.90 3 0 -28 2.60 5.20 -3 0 28 -3.10 4.70 -2 0 28 -3.70 4.60 1 0 -28 -2.30 6.10 -1 0 28 3.00 4.40 0 0 -28 7.00 6.60 0 0 28 14.20 4.40 -1 0 -28 -14.80 6.70 1 0 28 5.50 4.60 -2 0 -28 10.30 7.50 -3 0 -28 -7.60 7.70 3 0 28 12.90 9.00 3 -1 -28 11.20 4.90 -3 1 28 5.00 5.00 2 -1 -28 6.50 4.70 -2 1 28 -1.60 4.50 -1 1 28 -0.10 4.30 0 1 28 0.40 4.10 -1 -1 -28 16.10 7.00 -2 -1 -28 -4.50 7.00 -3 -1 -28 12.10 7.80 3 1 28 34.30 5.90 -4 -1 -28 -17.30 7.40 4 1 28 10.30 5.80 3 -2 -28 15.80 5.40 -3 2 28 4.60 4.90 2 -2 -28 6.40 4.90 -2 2 28 2.90 4.80 1 -2 -28 48.50 5.50 -1 2 28 34.90 5.20 0 2 28 7.10 4.30 -3 -2 -28 -3.80 7.10 3 2 28 13.50 5.40 -4 -2 -28 -12.50 7.10 4 2 28 14.70 5.80 2 -3 -28 22.60 5.60 -2 3 28 13.80 4.90 1 -3 -28 31.40 5.50 -1 3 28 19.50 4.80 0 -3 -28 31.80 5.30 2 3 28 44.80 6.10 -3 -3 -28 -20.30 6.30 3 3 28 8.30 5.40 -4 -3 -28 -8.20 6.90 4 3 28 4.30 5.90 -5 -3 -28 0.20 7.20 5 3 28 12.30 6.40 2 -4 -28 6.30 5.60 -2 4 28 -8.30 4.60 1 -4 -28 5.00 5.10 -1 4 28 -3.40 6.00 0 -4 -28 14.90 5.30 -1 -4 -28 22.50 5.40 -2 -4 -28 5.70 7.20 2 4 28 7.00 5.20 3 4 28 25.90 6.20 4 4 28 6.90 5.90 -5 -4 -28 52.99 8.10 5 4 28 78.59 8.20 0 -5 -28 12.20 5.60 -1 -5 -28 20.80 5.60 1 5 28 22.30 5.90 -2 -5 -28 12.70 5.30 2 5 28 22.10 5.90 -3 -5 -28 10.90 5.20 3 5 28 6.60 5.80 4 5 28 10.60 6.30 5 5 28 35.50 7.30 -1 -6 -28 9.10 5.50 1 6 28 20.80 6.10 -2 -6 -28 30.70 6.10 2 6 28 31.60 6.50 -3 -6 -28 28.80 6.00 3 6 28 18.60 6.30 -4 -6 -28 5.40 5.80 4 6 28 15.40 6.60 1 2 -29 9.40 6.90 -1 -2 29 5.00 4.90 2 1 -29 14.20 10.20 -2 -1 29 3.30 4.70 1 1 -29 -0.40 6.40 -1 -1 29 8.40 4.70 0 1 -29 12.80 7.50 0 -1 29 31.00 5.40 -1 1 -29 3.60 7.40 1 -1 29 24.90 5.40 -3 0 29 25.50 5.50 -2 0 29 -1.80 4.80 -1 0 29 13.70 4.70 0 0 -29 14.10 7.20 0 0 29 22.10 4.80 -1 0 -29 5.20 7.20 -2 0 -29 -8.90 7.60 -2 1 29 9.80 5.00 -1 1 29 0.30 4.50 0 1 29 10.80 4.40 -1 -1 -29 21.60 7.40 -2 -1 -29 -18.30 7.00 -3 -1 -29 28.30 8.40 3 1 29 44.30 10.50 2 -2 -29 3.00 5.00 -2 2 29 -3.50 4.70 1 -2 -29 9.40 5.00 -1 2 29 2.70 4.60 -2 -2 -29 -9.90 6.80 -3 -2 -29 23.90 8.00 3 2 29 36.40 6.10 -4 -2 -29 -8.00 7.40 4 2 29 11.90 5.90 1 -3 -29 7.10 5.20 -1 3 29 -1.90 4.60 0 -3 -29 7.40 4.90 3 3 29 7.90 5.90 -4 -3 -29 -19.30 6.90 4 3 29 2.50 6.10 1 -4 -29 15.80 5.60 0 -4 -29 -2.50 5.00 -1 -4 -29 3.80 4.90 2 4 29 4.90 5.50 3 4 29 18.00 6.30 4 4 29 15.10 6.50 -1 -5 -29 13.30 5.80 -2 -5 -29 30.90 5.90 2 5 29 41.40 6.80 3 5 29 2.40 5.80 -1 0 30 1.80 4.70 0 0 -30 13.40 7.40 0 0 30 23.70 5.10 -1 0 -30 9.40 7.70 -1 1 30 -1.00 4.70 -1 -1 -30 -17.10 6.70 -2 -1 -30 42.80 8.40 -1 2 30 13.50 5.00 3 3 30 8.10 6.10 -1 -4 -30 2.20 5.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95150 #===END data_L_5j _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H57 O3 P' _chemical_formula_weight 604.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 28.119(7) _cell_length_b 13.086(3) _cell_length_c 9.328(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3432.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.6205 _cell_measurement_theta_max 27.5985 _exptl_crystal_description parallelapiped _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.170 _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_absorpt_coefficient_mu 0.116 _shelx_estimated_absorpt_T_min 0.955 _shelx_estimated_absorpt_T_max 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 1.0 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scan' _diffrn_reflns_number 39958 _diffrn_reflns_av_unetI/netI 0.0208 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.448 _diffrn_reflns_theta_max 27.648 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7957 _reflns_number_gt 7561 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.880 _reflns_Friedel_fraction_max 0.992 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.4244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3441 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.018(17) _chemical_absolute_configuration ? _refine_ls_number_reflns 7957 _refine_ls_number_parameters 395 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.65270(2) 0.43681(3) 0.47078(5) 0.01143(9) Uani 1 1 d . . . . . O1 O 0.66018(5) 0.48284(10) 0.80101(14) 0.0191(3) Uani 1 1 d . . . . . O2 O 0.76125(5) 0.67593(11) 0.63934(15) 0.0225(3) Uani 1 1 d . . . . . O3 O 0.75031(5) 0.63920(11) 0.40241(15) 0.0202(3) Uani 1 1 d . . . . . C1 C 0.62211(6) 0.37943(13) 0.62901(18) 0.0128(3) Uani 1 1 d . . . . . C2 C 0.62526(6) 0.41272(13) 0.77277(19) 0.0141(3) Uani 1 1 d . . . . . C3 C 0.66692(8) 0.51381(15) 0.9469(2) 0.0228(4) Uani 1 1 d . . . . . H3A H 0.6393 0.5535 0.9787 0.034 Uiso 1 1 calc R U . . . H3B H 0.6956 0.5559 0.9541 0.034 Uiso 1 1 calc R U . . . H3C H 0.6704 0.4532 1.0076 0.034 Uiso 1 1 calc R U . . . C4 C 0.59501(7) 0.37649(14) 0.8794(2) 0.0175(4) Uani 1 1 d . . . . . H4 H 0.5975 0.4013 0.9748 0.021 Uiso 1 1 calc R U . . . C5 C 0.56109(7) 0.30346(15) 0.8442(2) 0.0189(4) Uani 1 1 d . . . . . H5 H 0.5392 0.2807 0.9148 0.023 Uiso 1 1 calc R U . . . C6 C 0.55902(6) 0.26390(14) 0.7075(2) 0.0174(4) Uani 1 1 d . . . . . H6 H 0.5365 0.2120 0.6859 0.021 Uiso 1 1 calc R U . . . C7 C 0.58971(6) 0.29917(13) 0.59940(19) 0.0134(3) Uani 1 1 d . . . . . C8 C 0.58578(6) 0.24309(13) 0.4580(2) 0.0136(3) Uani 1 1 d . . . . . C9 C 0.61024(6) 0.14996(13) 0.43975(19) 0.0146(3) Uani 1 1 d . . . . . C10 C 0.64201(7) 0.10492(14) 0.5556(2) 0.0177(4) Uani 1 1 d . . . . . H10 H 0.6514 0.1614 0.6220 0.021 Uiso 1 1 calc R U . . . C11 C 0.68774(7) 0.05624(16) 0.4966(2) 0.0236(4) Uani 1 1 d . . . . . H11A H 0.6800 -0.0086 0.4495 0.035 Uiso 1 1 calc R U . . . H11B H 0.7099 0.0436 0.5757 0.035 Uiso 1 1 calc R U . . . H11C H 0.7025 0.1026 0.4271 0.035 Uiso 1 1 calc R U . . . C12 C 0.61417(8) 0.02515(17) 0.6428(2) 0.0258(4) Uani 1 1 d . . . . . H12A H 0.5863 0.0575 0.6864 0.039 Uiso 1 1 calc R U . . . H12B H 0.6347 -0.0027 0.7183 0.039 Uiso 1 1 calc R U . . . H12C H 0.6038 -0.0302 0.5793 0.039 Uiso 1 1 calc R U . . . C13 C 0.60272(6) 0.09305(14) 0.3150(2) 0.0163(3) Uani 1 1 d . . . . . H13 H 0.6197 0.0309 0.3027 0.020 Uiso 1 1 calc R U . . . C14 C 0.57145(6) 0.12380(14) 0.2082(2) 0.0163(3) Uani 1 1 d . . . . . C15 C 0.56224(8) 0.06075(15) 0.0728(2) 0.0236(4) Uani 1 1 d . . . . . H15 H 0.5679 0.1063 -0.0115 0.028 Uiso 1 1 calc R U . . . C16 C 0.51032(9) 0.0272(2) 0.0677(4) 0.0566(9) Uani 1 1 d . . . . . H16A H 0.5036 -0.0176 0.1495 0.085 Uiso 1 1 calc R U . . . H16B H 0.5044 -0.0100 -0.0218 0.085 Uiso 1 1 calc R U . . . H16C H 0.4897 0.0874 0.0721 0.085 Uiso 1 1 calc R U . . . C17 C 0.59431(8) -0.03168(15) 0.0563(2) 0.0249(4) Uani 1 1 d . . . . . H17A H 0.6276 -0.0103 0.0632 0.037 Uiso 1 1 calc R U . . . H17B H 0.5887 -0.0634 -0.0374 0.037 Uiso 1 1 calc R U . . . H17C H 0.5873 -0.0811 0.1323 0.037 Uiso 1 1 calc R U . . . C18 C 0.54701(6) 0.21562(14) 0.2306(2) 0.0172(4) Uani 1 1 d . . . . . H18 H 0.5252 0.2382 0.1594 0.021 Uiso 1 1 calc R U . . . C19 C 0.55326(6) 0.27516(14) 0.3527(2) 0.0151(3) Uani 1 1 d . . . . . C20 C 0.52270(7) 0.37001(15) 0.3745(2) 0.0198(4) Uani 1 1 d . . . . . H20 H 0.5369 0.4096 0.4557 0.024 Uiso 1 1 calc R U . . . C21 C 0.52215(8) 0.44046(15) 0.2432(2) 0.0242(4) Uani 1 1 d . . . . . H21A H 0.5059 0.4061 0.1637 0.036 Uiso 1 1 calc R U . . . H21B H 0.5549 0.4565 0.2150 0.036 Uiso 1 1 calc R U . . . H21C H 0.5053 0.5038 0.2669 0.036 Uiso 1 1 calc R U . . . C22 C 0.47206(7) 0.34011(18) 0.4187(3) 0.0282(5) Uani 1 1 d . . . . . H22A H 0.4532 0.4020 0.4352 0.042 Uiso 1 1 calc R U . . . H22B H 0.4732 0.2996 0.5069 0.042 Uiso 1 1 calc R U . . . H22C H 0.4574 0.2997 0.3421 0.042 Uiso 1 1 calc R U . . . C23 C 0.71876(6) 0.41877(13) 0.49584(18) 0.0123(3) Uani 1 1 d . . . . . C24 C 0.72608(6) 0.31584(14) 0.5726(2) 0.0183(4) Uani 1 1 d . . . . . H24A H 0.7149 0.3220 0.6728 0.022 Uiso 1 1 calc R U . . . H24B H 0.7065 0.2631 0.5247 0.022 Uiso 1 1 calc R U . . . C25 C 0.77817(7) 0.28072(15) 0.5732(2) 0.0213(4) Uani 1 1 d . . . . . H25A H 0.7975 0.3297 0.6292 0.026 Uiso 1 1 calc R U . . . H25B H 0.7805 0.2131 0.6202 0.026 Uiso 1 1 calc R U . . . C26 C 0.79774(7) 0.27346(15) 0.4209(2) 0.0223(4) Uani 1 1 d . . . . . H26A H 0.8321 0.2570 0.4250 0.027 Uiso 1 1 calc R U . . . H26B H 0.7815 0.2172 0.3697 0.027 Uiso 1 1 calc R U . . . C27 C 0.79081(6) 0.37264(14) 0.3378(2) 0.0186(4) Uani 1 1 d . . . . . H27A H 0.8009 0.3625 0.2371 0.022 Uiso 1 1 calc R U . . . H27B H 0.8110 0.4267 0.3801 0.022 Uiso 1 1 calc R U . . . C28 C 0.73864(6) 0.40701(14) 0.34096(19) 0.0155(3) Uani 1 1 d . . . . . H28A H 0.7191 0.3564 0.2885 0.019 Uiso 1 1 calc R U . . . H28B H 0.7358 0.4733 0.2905 0.019 Uiso 1 1 calc R U . . . C29 C 0.74440(6) 0.50288(14) 0.5816(2) 0.0159(3) Uani 1 1 d . . . . . H29A H 0.7364 0.4934 0.6842 0.019 Uiso 1 1 calc R U . . . H29B H 0.7791 0.4918 0.5716 0.019 Uiso 1 1 calc R U . . . C30 C 0.73395(7) 0.61317(14) 0.5425(2) 0.0168(4) Uani 1 1 d . . . . . C31 C 0.79929(9) 0.7197(2) 0.5620(3) 0.0397(6) Uani 1 1 d . . . . . H31A H 0.8299 0.7061 0.6109 0.048 Uiso 1 1 calc R U . . . H31B H 0.7950 0.7945 0.5533 0.048 Uiso 1 1 calc R U . . . C32 C 0.79860(7) 0.67050(18) 0.4175(3) 0.0290(5) Uani 1 1 d . . . . . H32A H 0.8076 0.7198 0.3416 0.035 Uiso 1 1 calc R U . . . H32B H 0.8204 0.6112 0.4138 0.035 Uiso 1 1 calc R U . . . C33 C 0.68217(6) 0.64238(13) 0.5614(2) 0.0165(4) Uani 1 1 d . . . . . H33A H 0.6788 0.7151 0.5339 0.020 Uiso 1 1 calc R U . . . H33B H 0.6746 0.6375 0.6648 0.020 Uiso 1 1 calc R U . . . C34 C 0.64398(6) 0.58101(12) 0.4785(2) 0.0141(3) Uani 1 1 d . . . . . C35 C 0.59457(7) 0.60393(14) 0.5445(2) 0.0186(4) Uani 1 1 d . . . . . H35A H 0.5706 0.5583 0.5003 0.022 Uiso 1 1 calc R U . . . H35B H 0.5955 0.5889 0.6485 0.022 Uiso 1 1 calc R U . . . C36 C 0.57925(7) 0.71545(16) 0.5225(2) 0.0259(5) Uani 1 1 d . . . . . H36A H 0.5475 0.7260 0.5657 0.031 Uiso 1 1 calc R U . . . H36B H 0.6020 0.7613 0.5719 0.031 Uiso 1 1 calc R U . . . C37 C 0.57741(7) 0.74272(18) 0.3635(3) 0.0296(5) Uani 1 1 d . . . . . H37A H 0.5685 0.8155 0.3523 0.035 Uiso 1 1 calc R U . . . H37B H 0.5529 0.7006 0.3152 0.035 Uiso 1 1 calc R U . . . C38 C 0.62587(7) 0.72386(15) 0.2938(2) 0.0236(4) Uani 1 1 d . . . . . H38A H 0.6495 0.7716 0.3350 0.028 Uiso 1 1 calc R U . . . H38B H 0.6237 0.7375 0.1896 0.028 Uiso 1 1 calc R U . . . C39 C 0.64253(6) 0.61353(14) 0.3179(2) 0.0171(4) Uani 1 1 d . . . . . H39A H 0.6747 0.6055 0.2766 0.021 Uiso 1 1 calc R U . . . H39B H 0.6210 0.5668 0.2656 0.021 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.01099(18) 0.01264(19) 0.01065(18) 0.00139(17) 0.00032(17) -0.00049(15) O1 0.0240(7) 0.0203(7) 0.0131(6) -0.0016(5) -0.0001(5) -0.0084(5) O2 0.0221(6) 0.0256(7) 0.0199(7) -0.0049(6) 0.0019(6) -0.0102(6) O3 0.0201(7) 0.0227(7) 0.0177(7) 0.0022(5) 0.0016(5) -0.0039(5) C1 0.0125(7) 0.0116(8) 0.0142(8) 0.0028(6) 0.0018(6) 0.0010(6) C2 0.0144(8) 0.0112(8) 0.0167(8) 0.0022(7) 0.0002(7) 0.0009(6) C3 0.0332(10) 0.0196(9) 0.0156(10) -0.0011(7) -0.0039(8) -0.0056(8) C4 0.0216(9) 0.0181(8) 0.0129(8) 0.0013(7) 0.0029(7) 0.0023(7) C5 0.0185(8) 0.0196(9) 0.0187(9) 0.0062(7) 0.0055(7) -0.0012(7) C6 0.0152(8) 0.0163(9) 0.0206(9) 0.0027(7) 0.0012(7) -0.0036(7) C7 0.0129(7) 0.0130(8) 0.0143(8) 0.0012(7) -0.0007(6) 0.0019(6) C8 0.0123(7) 0.0137(7) 0.0149(8) 0.0020(7) 0.0010(7) -0.0027(6) C9 0.0117(7) 0.0152(8) 0.0169(9) 0.0027(7) -0.0020(6) -0.0016(6) C10 0.0177(8) 0.0163(8) 0.0192(9) 0.0022(7) -0.0049(7) 0.0011(7) C11 0.0196(9) 0.0229(9) 0.0283(12) 0.0004(8) -0.0073(8) 0.0040(7) C12 0.0261(10) 0.0246(11) 0.0267(10) 0.0112(9) -0.0043(9) 0.0004(8) C13 0.0159(8) 0.0136(8) 0.0195(9) 0.0012(7) -0.0001(7) 0.0016(7) C14 0.0177(8) 0.0156(8) 0.0156(8) -0.0008(7) -0.0006(7) -0.0023(7) C15 0.0330(11) 0.0184(9) 0.0194(9) -0.0023(8) -0.0082(9) 0.0046(8) C16 0.0281(13) 0.0572(17) 0.084(2) -0.0472(18) -0.0211(14) 0.0096(12) C17 0.0295(10) 0.0224(9) 0.0228(10) -0.0050(8) 0.0018(8) 0.0011(8) C18 0.0156(8) 0.0185(9) 0.0176(9) 0.0025(7) -0.0038(7) 0.0016(7) C19 0.0134(8) 0.0153(8) 0.0166(9) 0.0015(7) 0.0007(7) 0.0008(6) C20 0.0202(9) 0.0184(9) 0.0209(9) -0.0032(7) -0.0043(7) 0.0057(7) C21 0.0259(10) 0.0181(9) 0.0286(11) 0.0007(8) -0.0058(8) 0.0043(8) C22 0.0223(10) 0.0328(11) 0.0294(11) 0.0010(9) 0.0033(8) 0.0106(8) C23 0.0111(7) 0.0137(8) 0.0122(9) 0.0004(6) 0.0004(6) 0.0004(6) C24 0.0163(8) 0.0177(8) 0.0207(9) 0.0057(7) 0.0005(7) 0.0003(7) C25 0.0193(9) 0.0198(9) 0.0249(10) 0.0061(8) -0.0022(8) 0.0037(7) C26 0.0185(9) 0.0198(9) 0.0284(10) -0.0003(8) 0.0013(8) 0.0038(7) C27 0.0166(8) 0.0191(9) 0.0200(9) -0.0023(7) 0.0041(7) -0.0002(7) C28 0.0158(8) 0.0160(8) 0.0147(8) -0.0010(7) 0.0020(7) -0.0001(7) C29 0.0141(8) 0.0192(8) 0.0143(8) -0.0001(7) -0.0004(7) -0.0010(6) C30 0.0176(8) 0.0160(8) 0.0167(9) -0.0024(7) 0.0009(7) -0.0030(7) C31 0.0334(12) 0.0505(15) 0.0353(13) -0.0184(12) 0.0142(10) -0.0271(11) C32 0.0225(10) 0.0387(13) 0.0259(10) 0.0059(9) 0.0028(8) -0.0068(9) C33 0.0178(8) 0.0141(8) 0.0176(9) 0.0001(7) 0.0033(7) -0.0006(6) C34 0.0134(7) 0.0117(7) 0.0171(8) 0.0031(8) 0.0026(8) 0.0014(6) C35 0.0164(8) 0.0182(9) 0.0212(10) 0.0050(7) 0.0048(7) 0.0032(7) C36 0.0212(10) 0.0212(10) 0.0352(11) 0.0071(8) 0.0126(8) 0.0080(8) C37 0.0226(10) 0.0277(11) 0.0384(12) 0.0169(10) 0.0077(9) 0.0103(8) C38 0.0213(9) 0.0230(10) 0.0267(10) 0.0118(8) 0.0056(8) 0.0037(8) C39 0.0152(8) 0.0185(9) 0.0178(9) 0.0044(7) 0.0017(7) 0.0003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.8660(18) . ? P1 C23 1.8870(17) . ? P1 C34 1.9042(17) . ? O1 C2 1.370(2) . ? O1 C3 1.432(2) . ? O2 C31 1.411(3) . ? O2 C30 1.442(2) . ? O3 C32 1.425(2) . ? O3 C30 1.427(2) . ? C1 C2 1.413(2) . ? C1 C7 1.418(2) . ? C2 C4 1.392(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.405(3) . ? C6 H6 0.9500 . ? C7 C8 1.513(2) . ? C8 C19 1.406(2) . ? C8 C9 1.410(2) . ? C9 C13 1.398(3) . ? C9 C10 1.521(2) . ? C10 C11 1.537(3) . ? C10 C12 1.538(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C18 1.400(3) . ? C14 C15 1.530(3) . ? C15 C17 1.517(3) . ? C15 C16 1.526(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.523(2) . ? C20 C21 1.533(3) . ? C20 C22 1.533(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.539(2) . ? C23 C29 1.540(2) . ? C23 C28 1.557(2) . ? C24 C25 1.535(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.526(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.525(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.535(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.518(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.515(3) . ? C31 C32 1.494(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.548(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.549(2) . ? C34 C39 1.558(3) . ? C35 C36 1.535(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.526(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.530(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.535(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C23 107.78(8) . . ? C1 P1 C34 108.03(8) . . ? C23 P1 C34 104.24(7) . . ? C2 O1 C3 117.85(14) . . ? C31 O2 C30 108.32(15) . . ? C32 O3 C30 106.60(15) . . ? C2 C1 C7 116.98(15) . . ? C2 C1 P1 126.71(13) . . ? C7 C1 P1 116.12(13) . . ? O1 C2 C4 121.94(16) . . ? O1 C2 C1 115.73(15) . . ? C4 C2 C1 122.33(16) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 119.02(17) . . ? C5 C4 H4 120.5 . . ? C2 C4 H4 120.5 . . ? C6 C5 C4 120.40(17) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.98(17) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C1 119.89(16) . . ? C6 C7 C8 114.90(15) . . ? C1 C7 C8 125.17(15) . . ? C19 C8 C9 119.39(16) . . ? C19 C8 C7 120.76(15) . . ? C9 C8 C7 119.28(15) . . ? C13 C9 C8 119.18(16) . . ? C13 C9 C10 118.29(16) . . ? C8 C9 C10 122.39(16) . . ? C9 C10 C11 113.44(16) . . ? C9 C10 C12 109.87(15) . . ? C11 C10 C12 109.51(16) . . ? C9 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 122.60(17) . . ? C14 C13 H13 118.7 . . ? C9 C13 H13 118.7 . . ? C13 C14 C18 116.93(17) . . ? C13 C14 C15 122.88(17) . . ? C18 C14 C15 120.18(16) . . ? C17 C15 C16 109.63(18) . . ? C17 C15 C14 114.43(17) . . ? C16 C15 C14 110.07(19) . . ? C17 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C14 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C14 122.72(17) . . ? C19 C18 H18 118.6 . . ? C14 C18 H18 118.6 . . ? C18 C19 C8 119.15(16) . . ? C18 C19 C20 119.59(16) . . ? C8 C19 C20 121.15(16) . . ? C19 C20 C21 112.92(16) . . ? C19 C20 C22 110.60(16) . . ? C21 C20 C22 111.04(16) . . ? C19 C20 H20 107.3 . . ? C21 C20 H20 107.3 . . ? C22 C20 H20 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C29 108.72(14) . . ? C24 C23 C28 107.29(14) . . ? C29 C23 C28 112.64(14) . . ? C24 C23 P1 107.39(11) . . ? C29 C23 P1 115.84(12) . . ? C28 C23 P1 104.53(11) . . ? C25 C24 C23 113.04(15) . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C24 111.04(15) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.99(16) . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 111.21(15) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C23 112.96(15) . . ? C27 C28 H28A 109.0 . . ? C23 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C23 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C23 117.64(15) . . ? C30 C29 H29A 107.9 . . ? C23 C29 H29A 107.9 . . ? C30 C29 H29B 107.9 . . ? C23 C29 H29B 107.9 . . ? H29A C29 H29B 107.2 . . ? O3 C30 O2 105.42(13) . . ? O3 C30 C33 110.86(15) . . ? O2 C30 C33 107.16(14) . . ? O3 C30 C29 112.64(15) . . ? O2 C30 C29 106.73(15) . . ? C33 C30 C29 113.45(15) . . ? O2 C31 C32 106.07(16) . . ? O2 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O2 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? O3 C32 C31 103.01(17) . . ? O3 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? O3 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C30 C33 C34 118.53(14) . . ? C30 C33 H33A 107.7 . . ? C34 C33 H33A 107.7 . . ? C30 C33 H33B 107.7 . . ? C34 C33 H33B 107.7 . . ? H33A C33 H33B 107.1 . . ? C33 C34 C35 108.86(15) . . ? C33 C34 C39 110.90(14) . . ? C35 C34 C39 107.81(14) . . ? C33 C34 P1 116.34(12) . . ? C35 C34 P1 108.81(11) . . ? C39 C34 P1 103.75(12) . . ? C36 C35 C34 112.49(15) . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 111.20(18) . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C38 110.18(17) . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37B 109.6 . . ? C38 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 111.19(16) . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38B 109.4 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C34 113.95(16) . . ? C38 C39 H39A 108.8 . . ? C34 C39 H39A 108.8 . . ? C38 C39 H39B 108.8 . . ? C34 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 P1 C1 C2 64.95(17) . . . . ? C34 P1 C1 C2 -47.14(17) . . . . ? C23 P1 C1 C7 -120.17(13) . . . . ? C34 P1 C1 C7 127.74(13) . . . . ? C3 O1 C2 C4 3.9(3) . . . . ? C3 O1 C2 C1 -175.87(16) . . . . ? C7 C1 C2 O1 173.58(15) . . . . ? P1 C1 C2 O1 -11.6(2) . . . . ? C7 C1 C2 C4 -6.2(3) . . . . ? P1 C1 C2 C4 168.67(14) . . . . ? O1 C2 C4 C5 -178.41(17) . . . . ? C1 C2 C4 C5 1.3(3) . . . . ? C2 C4 C5 C6 3.2(3) . . . . ? C4 C5 C6 C7 -2.6(3) . . . . ? C5 C6 C7 C1 -2.5(3) . . . . ? C5 C6 C7 C8 175.61(16) . . . . ? C2 C1 C7 C6 6.7(2) . . . . ? P1 C1 C7 C6 -168.72(13) . . . . ? C2 C1 C7 C8 -171.26(16) . . . . ? P1 C1 C7 C8 13.3(2) . . . . ? C6 C7 C8 C19 88.8(2) . . . . ? C1 C7 C8 C19 -93.1(2) . . . . ? C6 C7 C8 C9 -82.5(2) . . . . ? C1 C7 C8 C9 95.5(2) . . . . ? C19 C8 C9 C13 2.0(2) . . . . ? C7 C8 C9 C13 173.46(15) . . . . ? C19 C8 C9 C10 -173.55(16) . . . . ? C7 C8 C9 C10 -2.1(2) . . . . ? C13 C9 C10 C11 44.0(2) . . . . ? C8 C9 C10 C11 -140.37(17) . . . . ? C13 C9 C10 C12 -78.9(2) . . . . ? C8 C9 C10 C12 96.7(2) . . . . ? C8 C9 C13 C14 -0.9(3) . . . . ? C10 C9 C13 C14 174.83(17) . . . . ? C9 C13 C14 C18 -0.3(3) . . . . ? C9 C13 C14 C15 -178.64(18) . . . . ? C13 C14 C15 C17 -6.9(3) . . . . ? C18 C14 C15 C17 174.77(18) . . . . ? C13 C14 C15 C16 117.1(2) . . . . ? C18 C14 C15 C16 -61.3(3) . . . . ? C13 C14 C18 C19 0.4(3) . . . . ? C15 C14 C18 C19 178.79(18) . . . . ? C14 C18 C19 C8 0.7(3) . . . . ? C14 C18 C19 C20 -175.49(17) . . . . ? C9 C8 C19 C18 -1.9(2) . . . . ? C7 C8 C19 C18 -173.24(16) . . . . ? C9 C8 C19 C20 174.24(16) . . . . ? C7 C8 C19 C20 2.9(2) . . . . ? C18 C19 C20 C21 -50.3(2) . . . . ? C8 C19 C20 C21 133.50(18) . . . . ? C18 C19 C20 C22 74.8(2) . . . . ? C8 C19 C20 C22 -101.4(2) . . . . ? C1 P1 C23 C24 34.41(14) . . . . ? C34 P1 C23 C24 149.04(12) . . . . ? C1 P1 C23 C29 -87.27(14) . . . . ? C34 P1 C23 C29 27.36(14) . . . . ? C1 P1 C23 C28 148.17(11) . . . . ? C34 P1 C23 C28 -97.20(12) . . . . ? C29 C23 C24 C25 -65.58(19) . . . . ? C28 C23 C24 C25 56.50(19) . . . . ? P1 C23 C24 C25 168.39(13) . . . . ? C23 C24 C25 C26 -56.8(2) . . . . ? C24 C25 C26 C27 53.6(2) . . . . ? C25 C26 C27 C28 -53.3(2) . . . . ? C26 C27 C28 C23 55.7(2) . . . . ? C24 C23 C28 C27 -56.03(19) . . . . ? C29 C23 C28 C27 63.57(19) . . . . ? P1 C23 C28 C27 -169.86(12) . . . . ? C24 C23 C29 C30 -168.18(15) . . . . ? C28 C23 C29 C30 73.06(19) . . . . ? P1 C23 C29 C30 -47.2(2) . . . . ? C32 O3 C30 O2 28.92(19) . . . . ? C32 O3 C30 C33 144.56(16) . . . . ? C32 O3 C30 C29 -87.09(18) . . . . ? C31 O2 C30 O3 -12.6(2) . . . . ? C31 O2 C30 C33 -130.78(19) . . . . ? C31 O2 C30 C29 107.4(2) . . . . ? C23 C29 C30 O3 -66.0(2) . . . . ? C23 C29 C30 O2 178.81(14) . . . . ? C23 C29 C30 C33 61.0(2) . . . . ? C30 O2 C31 C32 -7.5(3) . . . . ? C30 O3 C32 C31 -32.9(2) . . . . ? O2 C31 C32 O3 24.7(3) . . . . ? O3 C30 C33 C34 70.1(2) . . . . ? O2 C30 C33 C34 -175.38(15) . . . . ? C29 C30 C33 C34 -57.8(2) . . . . ? C30 C33 C34 C35 164.79(15) . . . . ? C30 C33 C34 C39 -76.76(19) . . . . ? C30 C33 C34 P1 41.5(2) . . . . ? C33 C34 C35 C36 66.0(2) . . . . ? C39 C34 C35 C36 -54.3(2) . . . . ? P1 C34 C35 C36 -166.26(15) . . . . ? C34 C35 C36 C37 58.6(2) . . . . ? C35 C36 C37 C38 -57.4(2) . . . . ? C36 C37 C38 C39 55.4(3) . . . . ? C37 C38 C39 C34 -55.1(2) . . . . ? C33 C34 C39 C38 -65.94(19) . . . . ? C35 C34 C39 C38 53.14(19) . . . . ? P1 C34 C39 C38 168.43(13) . . . . ? _refine_diff_density_max 0.369 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.037 _shelx_res_file ; XRAY5666_0ma.res created by SHELXL-2014/7 TITL XRAY5666_0ma in Pna2(1) CELL 0.71073 28.11920 13.08640 9.32770 90.0000 90.0000 90.0000 ZERR 4.00 0.00660 0.00310 0.00220 0.0000 0.0000 0.0000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H O P UNIT 156 228 12 4 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.40 0.40 0.40 CONF TEMP -173.000 WGHT 0.050500 0.424400 FVAR 0.17111 MOLE 1 P1 4 0.652698 0.436815 0.470783 11.00000 0.01099 0.01264 = 0.01065 0.00139 0.00032 -0.00049 O1 3 0.660184 0.482843 0.801011 11.00000 0.02397 0.02032 = 0.01311 -0.00160 -0.00013 -0.00841 O2 3 0.761254 0.675934 0.639336 11.00000 0.02207 0.02560 = 0.01992 -0.00486 0.00191 -0.01022 O3 3 0.750310 0.639199 0.402409 11.00000 0.02006 0.02266 = 0.01775 0.00220 0.00157 -0.00386 C1 1 0.622113 0.379431 0.629011 11.00000 0.01248 0.01157 = 0.01423 0.00283 0.00184 0.00105 C2 1 0.625258 0.412721 0.772766 11.00000 0.01438 0.01121 = 0.01667 0.00223 0.00024 0.00085 C3 1 0.666925 0.513814 0.946863 11.00000 0.03317 0.01964 = 0.01556 -0.00107 -0.00388 -0.00560 AFIX 137 H3A 2 0.639336 0.553547 0.978710 11.00000 -1.50000 H3B 2 0.695648 0.555915 0.954070 11.00000 -1.50000 H3C 2 0.670402 0.453175 1.007614 11.00000 -1.50000 AFIX 0 C4 1 0.595011 0.376490 0.879356 11.00000 0.02157 0.01806 = 0.01287 0.00133 0.00287 0.00233 AFIX 43 H4 2 0.597519 0.401319 0.974762 11.00000 -1.20000 AFIX 0 C5 1 0.561087 0.303461 0.844183 11.00000 0.01854 0.01961 = 0.01870 0.00616 0.00549 -0.00118 AFIX 43 H5 2 0.539189 0.280679 0.914848 11.00000 -1.20000 AFIX 0 C6 1 0.559017 0.263900 0.707474 11.00000 0.01524 0.01629 = 0.02062 0.00275 0.00121 -0.00362 AFIX 43 H6 2 0.536502 0.211997 0.685943 11.00000 -1.20000 AFIX 0 C7 1 0.589711 0.299172 0.599399 11.00000 0.01290 0.01304 = 0.01427 0.00120 -0.00066 0.00192 C8 1 0.585783 0.243090 0.458023 11.00000 0.01231 0.01366 = 0.01487 0.00198 0.00105 -0.00267 C9 1 0.610236 0.149960 0.439746 11.00000 0.01172 0.01525 = 0.01688 0.00267 -0.00198 -0.00164 C10 1 0.642010 0.104920 0.555595 11.00000 0.01770 0.01630 = 0.01915 0.00220 -0.00494 0.00110 AFIX 13 H10 2 0.651367 0.161431 0.622019 11.00000 -1.20000 AFIX 0 C11 1 0.687742 0.056239 0.496622 11.00000 0.01961 0.02289 = 0.02833 0.00040 -0.00726 0.00404 AFIX 137 H11A 2 0.679993 -0.008584 0.449488 11.00000 -1.50000 H11B 2 0.709935 0.043625 0.575673 11.00000 -1.50000 H11C 2 0.702459 0.102636 0.427102 11.00000 -1.50000 AFIX 0 C12 1 0.614166 0.025147 0.642823 11.00000 0.02610 0.02455 = 0.02672 0.01116 -0.00427 0.00037 AFIX 137 H12A 2 0.586267 0.057545 0.686402 11.00000 -1.50000 H12B 2 0.634650 -0.002699 0.718313 11.00000 -1.50000 H12C 2 0.603835 -0.030242 0.579342 11.00000 -1.50000 AFIX 0 C13 1 0.602716 0.093051 0.314959 11.00000 0.01593 0.01363 = 0.01946 0.00120 -0.00008 0.00164 AFIX 43 H13 2 0.619675 0.030871 0.302748 11.00000 -1.20000 AFIX 0 C14 1 0.571452 0.123798 0.208192 11.00000 0.01767 0.01561 = 0.01559 -0.00078 -0.00061 -0.00228 C15 1 0.562245 0.060754 0.072837 11.00000 0.03300 0.01840 = 0.01935 -0.00231 -0.00823 0.00462 AFIX 13 H15 2 0.567935 0.106329 -0.011490 11.00000 -1.20000 AFIX 0 C16 1 0.510323 0.027155 0.067703 11.00000 0.02813 0.05722 = 0.08445 -0.04724 -0.02109 0.00956 AFIX 137 H16A 2 0.503565 -0.017581 0.149460 11.00000 -1.50000 H16B 2 0.504360 -0.009964 -0.021758 11.00000 -1.50000 H16C 2 0.489689 0.087424 0.072109 11.00000 -1.50000 AFIX 0 C17 1 0.594308 -0.031676 0.056255 11.00000 0.02954 0.02241 = 0.02276 -0.00503 0.00180 0.00109 AFIX 137 H17A 2 0.627622 -0.010252 0.063238 11.00000 -1.50000 H17B 2 0.588729 -0.063367 -0.037440 11.00000 -1.50000 H17C 2 0.587291 -0.081138 0.132252 11.00000 -1.50000 AFIX 0 C18 1 0.547007 0.215619 0.230564 11.00000 0.01564 0.01846 = 0.01760 0.00250 -0.00385 0.00156 AFIX 43 H18 2 0.525247 0.238222 0.159399 11.00000 -1.20000 AFIX 0 C19 1 0.553263 0.275155 0.352742 11.00000 0.01342 0.01529 = 0.01657 0.00151 0.00073 0.00083 C20 1 0.522698 0.370014 0.374471 11.00000 0.02024 0.01841 = 0.02088 -0.00315 -0.00428 0.00570 AFIX 13 H20 2 0.536851 0.409561 0.455681 11.00000 -1.20000 AFIX 0 C21 1 0.522148 0.440455 0.243182 11.00000 0.02590 0.01813 = 0.02859 0.00069 -0.00579 0.00430 AFIX 137 H21A 2 0.505898 0.406115 0.163700 11.00000 -1.50000 H21B 2 0.554886 0.456479 0.215020 11.00000 -1.50000 H21C 2 0.505309 0.503806 0.266889 11.00000 -1.50000 AFIX 0 C22 1 0.472061 0.340113 0.418673 11.00000 0.02229 0.03281 = 0.02939 0.00101 0.00334 0.01060 AFIX 137 H22A 2 0.453224 0.402007 0.435199 11.00000 -1.50000 H22B 2 0.473216 0.299561 0.506931 11.00000 -1.50000 H22C 2 0.457376 0.299657 0.342142 11.00000 -1.50000 AFIX 0 C23 1 0.718758 0.418770 0.495838 11.00000 0.01108 0.01374 = 0.01222 0.00036 0.00039 0.00044 C24 1 0.726083 0.315841 0.572606 11.00000 0.01630 0.01772 = 0.02074 0.00566 0.00045 0.00033 AFIX 23 H24A 2 0.714854 0.322018 0.672825 11.00000 -1.20000 H24B 2 0.706452 0.263132 0.524706 11.00000 -1.20000 AFIX 0 C25 1 0.778173 0.280720 0.573238 11.00000 0.01927 0.01977 = 0.02495 0.00615 -0.00218 0.00365 AFIX 23 H25A 2 0.797532 0.329743 0.629170 11.00000 -1.20000 H25B 2 0.780508 0.213080 0.620248 11.00000 -1.20000 AFIX 0 C26 1 0.797738 0.273456 0.420937 11.00000 0.01852 0.01985 = 0.02839 -0.00032 0.00131 0.00377 AFIX 23 H26A 2 0.832079 0.257035 0.425039 11.00000 -1.20000 H26B 2 0.781482 0.217152 0.369716 11.00000 -1.20000 AFIX 0 C27 1 0.790809 0.372644 0.337781 11.00000 0.01657 0.01913 = 0.02002 -0.00227 0.00409 -0.00022 AFIX 23 H27A 2 0.800919 0.362528 0.237111 11.00000 -1.20000 H27B 2 0.811033 0.426710 0.380138 11.00000 -1.20000 AFIX 0 C28 1 0.738635 0.407008 0.340958 11.00000 0.01581 0.01599 = 0.01473 -0.00097 0.00204 -0.00009 AFIX 23 H28A 2 0.719081 0.356419 0.288495 11.00000 -1.20000 H28B 2 0.735764 0.473272 0.290487 11.00000 -1.20000 AFIX 0 C29 1 0.744399 0.502875 0.581648 11.00000 0.01410 0.01918 = 0.01432 -0.00014 -0.00041 -0.00102 AFIX 23 H29A 2 0.736444 0.493446 0.684189 11.00000 -1.20000 H29B 2 0.779068 0.491799 0.571617 11.00000 -1.20000 AFIX 0 C30 1 0.733946 0.613170 0.542501 11.00000 0.01758 0.01602 = 0.01667 -0.00242 0.00092 -0.00300 C31 1 0.799294 0.719662 0.562001 11.00000 0.03339 0.05047 = 0.03526 -0.01839 0.01425 -0.02711 AFIX 23 H31A 2 0.829894 0.706140 0.610945 11.00000 -1.20000 H31B 2 0.795005 0.794494 0.553318 11.00000 -1.20000 AFIX 0 C32 1 0.798601 0.670505 0.417471 11.00000 0.02254 0.03870 = 0.02589 0.00592 0.00277 -0.00680 AFIX 23 H32A 2 0.807628 0.719759 0.341647 11.00000 -1.20000 H32B 2 0.820400 0.611158 0.413793 11.00000 -1.20000 AFIX 0 C33 1 0.682171 0.642380 0.561389 11.00000 0.01780 0.01411 = 0.01764 0.00006 0.00330 -0.00059 AFIX 23 H33A 2 0.678825 0.715105 0.533948 11.00000 -1.20000 H33B 2 0.674593 0.637481 0.664809 11.00000 -1.20000 AFIX 0 C34 1 0.643981 0.581012 0.478514 11.00000 0.01344 0.01168 = 0.01709 0.00314 0.00259 0.00137 C35 1 0.594571 0.603935 0.544543 11.00000 0.01643 0.01817 = 0.02123 0.00504 0.00485 0.00321 AFIX 23 H35A 2 0.570637 0.558268 0.500335 11.00000 -1.20000 H35B 2 0.595509 0.588920 0.648529 11.00000 -1.20000 AFIX 0 C36 1 0.579245 0.715453 0.522516 11.00000 0.02122 0.02124 = 0.03520 0.00706 0.01262 0.00796 AFIX 23 H36A 2 0.547463 0.726048 0.565689 11.00000 -1.20000 H36B 2 0.601986 0.761262 0.571859 11.00000 -1.20000 AFIX 0 C37 1 0.577411 0.742718 0.363505 11.00000 0.02257 0.02769 = 0.03842 0.01694 0.00769 0.01032 AFIX 23 H37A 2 0.568500 0.815470 0.352316 11.00000 -1.20000 H37B 2 0.552945 0.700611 0.315181 11.00000 -1.20000 AFIX 0 C38 1 0.625867 0.723865 0.293832 11.00000 0.02128 0.02296 = 0.02669 0.01180 0.00564 0.00374 AFIX 23 H38A 2 0.649522 0.771619 0.334952 11.00000 -1.20000 H38B 2 0.623652 0.737457 0.189638 11.00000 -1.20000 AFIX 0 C39 1 0.642528 0.613531 0.317932 11.00000 0.01519 0.01848 = 0.01778 0.00442 0.00168 0.00026 AFIX 23 H39A 2 0.674741 0.605539 0.276592 11.00000 -1.20000 H39B 2 0.620955 0.566818 0.265582 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5666_0ma in Pna2(1) REM R1 = 0.0295 for 7561 Fo > 4sig(Fo) and 0.0317 for all 7957 data REM 395 parameters refined using 1 restraints END WGHT 0.0496 0.4614 REM Highest difference peak 0.369, deepest hole -0.194, 1-sigma level 0.037 Q1 1 0.7866 0.7259 0.4350 11.00000 0.05 0.37 Q2 1 0.6462 0.5086 0.4834 11.00000 0.05 0.31 Q3 1 0.7466 0.7066 0.4035 11.00000 0.05 0.26 Q4 1 0.7394 0.5568 0.5499 11.00000 0.05 0.25 Q5 1 0.7809 0.7794 0.4805 11.00000 0.05 0.23 Q6 1 0.5689 0.0924 0.1414 11.00000 0.05 0.23 Q7 1 0.5883 0.2731 0.5246 11.00000 0.05 0.22 Q8 1 0.6189 0.3990 0.6972 11.00000 0.05 0.22 Q9 1 0.6884 0.4259 0.4899 11.00000 0.05 0.22 Q10 1 0.6406 0.4040 0.5607 11.00000 0.05 0.22 Q11 1 0.6005 0.1979 0.4449 11.00000 0.05 0.21 Q12 1 0.5527 0.1554 0.2468 11.00000 0.05 0.21 Q13 1 0.6300 0.1255 0.4854 11.00000 0.05 0.21 Q14 1 0.6411 0.3997 0.3984 11.00000 0.05 0.21 Q15 1 0.5605 0.2466 0.4178 11.00000 0.05 0.21 Q16 1 0.7380 0.6193 0.4675 11.00000 0.05 0.21 Q17 1 0.7218 0.3655 0.5265 11.00000 0.05 0.20 Q18 1 0.5773 0.7567 0.4490 11.00000 0.05 0.20 Q19 1 0.5684 0.2722 0.7751 11.00000 0.05 0.20 Q20 1 0.7411 0.7034 0.5583 11.00000 0.05 0.20 ; _shelx_res_checksum 43747 _shelx_hkl_file ; -1 0 0 0.01 0.01 1 0 0 0.00 0.01 -2 0 0 234.17 1.29 2 0 0 224.20 1.00 -3 0 0 0.27 0.06 3 0 0 0.31 0.07 -4 0 0 68.59 0.51 -4 0 0 68.89 0.47 4 0 0 68.45 0.30 4 0 0 70.11 0.51 -5 0 0 0.00 0.11 -5 0 0 0.03 0.10 5 0 0 0.01 0.05 5 0 0 -0.07 0.11 -6 0 0 529.95 2.58 -6 0 0 508.95 2.68 6 0 0 531.14 1.77 6 0 0 500.00 1.62 -7 0 0 0.05 0.14 -7 0 0 -0.13 0.13 7 0 0 0.03 0.06 7 0 0 0.14 0.16 -8 0 0 9.50 0.35 -8 0 0 10.09 0.31 8 0 0 10.05 0.16 8 0 0 9.85 0.35 -9 0 0 0.02 0.15 -9 0 0 -0.06 0.13 9 0 0 -0.06 0.06 9 0 0 0.14 0.17 -10 0 0 23.27 0.51 -10 0 0 24.18 0.48 10 0 0 23.79 0.24 10 0 0 23.68 0.52 -11 0 0 0.04 0.16 -11 0 0 -0.07 0.14 11 0 0 0.02 0.07 11 0 0 0.18 0.18 -12 0 0 27.94 0.61 -12 0 0 28.12 0.55 12 0 0 28.00 0.27 12 0 0 28.76 0.61 -13 0 0 0.17 0.18 -13 0 0 -0.16 0.14 13 0 0 0.08 0.07 13 0 0 0.12 0.19 -14 0 0 21.16 0.59 -14 0 0 22.10 0.54 14 0 0 22.06 0.60 -15 0 0 0.28 0.20 -15 0 0 0.20 0.18 15 0 0 0.04 0.22 -16 0 0 18.16 0.60 -16 0 0 18.84 0.55 16 0 0 18.43 0.61 -17 0 0 0.09 0.22 -17 0 0 0.32 0.19 17 0 0 0.27 0.24 -18 0 0 17.85 0.65 -18 0 0 18.97 0.59 18 0 0 18.93 0.67 -19 0 0 0.06 0.25 -19 0 0 0.29 0.23 19 0 0 0.17 0.28 -20 0 0 44.11 1.00 -20 0 0 44.03 0.91 20 0 0 47.64 1.03 -21 0 0 0.36 0.29 -21 0 0 0.32 0.25 21 0 0 0.16 0.31 -22 0 0 21.45 0.80 -22 0 0 20.93 0.72 22 0 0 21.70 0.81 -23 0 0 0.17 0.32 -23 0 0 0.23 0.26 23 0 0 0.05 0.34 -24 0 0 9.76 0.67 -24 0 0 9.51 0.56 24 0 0 9.40 0.67 -25 0 0 -0.05 0.32 -25 0 0 0.24 0.27 25 0 0 0.08 0.35 -26 0 0 -0.02 0.33 -26 0 0 0.37 0.28 26 0 0 0.21 0.36 -27 0 0 0.26 0.36 -27 0 0 0.19 0.30 27 0 0 0.44 0.38 -28 0 0 17.64 0.93 -28 0 0 16.63 0.78 28 0 0 17.40 0.89 -29 0 0 0.18 0.40 -29 0 0 0.53 0.33 29 0 0 0.36 0.41 -30 0 0 20.29 1.03 -30 0 0 20.96 0.89 30 0 0 21.68 1.04 -31 0 0 0.18 0.41 -31 0 0 0.18 0.34 31 0 0 0.02 0.42 -32 0 0 9.86 0.85 32 0 0 9.76 0.90 -33 0 0 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1 0 186.30 1.41 15 1 0 188.15 1.62 -15 -1 0 180.25 1.59 -15 -1 0 181.01 1.55 15 -1 0 190.78 0.97 15 -1 0 186.08 1.65 -16 1 0 44.07 0.87 -16 1 0 43.77 0.74 16 1 0 43.47 0.86 -16 -1 0 43.39 0.85 -16 -1 0 44.02 0.83 16 -1 0 44.18 0.49 16 -1 0 43.74 0.88 -17 1 0 19.99 0.66 -17 1 0 20.05 0.56 17 1 0 19.48 0.64 -17 -1 0 19.48 0.64 -17 -1 0 19.81 0.61 17 -1 0 19.59 0.35 17 -1 0 20.97 0.68 -18 1 0 1.13 0.29 -18 1 0 1.13 0.24 18 1 0 0.89 0.28 -18 -1 0 1.07 0.29 -18 -1 0 1.11 0.26 18 -1 0 1.05 0.31 -19 1 0 5.48 0.49 -19 1 0 6.24 0.42 19 1 0 5.29 0.48 -19 -1 0 5.90 0.51 -19 -1 0 5.91 0.45 19 -1 0 6.44 0.54 -20 1 0 11.59 0.61 -20 1 0 11.10 0.51 20 1 0 11.81 0.63 -20 -1 0 10.71 0.62 -20 -1 0 10.77 0.54 20 -1 0 11.20 0.65 -21 1 0 0.61 0.30 -21 1 0 0.49 0.24 21 1 0 0.31 0.30 -21 -1 0 0.60 0.31 -21 -1 0 0.42 0.26 21 -1 0 0.77 0.32 -22 1 0 78.52 1.37 -22 1 0 78.77 1.19 22 1 0 79.95 1.38 -22 -1 0 79.77 1.38 -22 -1 0 77.55 1.29 22 -1 0 83.72 1.43 -23 1 0 5.27 0.57 -23 1 0 5.39 0.47 23 1 0 4.82 0.55 -23 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33.88 1.32 -33 -1 0 34.38 1.29 -33 -1 0 34.88 1.19 33 -1 0 34.08 1.32 -34 1 0 0.33 0.47 34 1 0 0.71 0.50 -34 -1 0 0.60 0.48 34 -1 0 0.70 0.51 -35 1 0 2.74 0.62 35 1 0 2.23 0.61 -35 -1 0 2.10 0.58 35 -1 0 2.06 0.60 -36 1 0 0.87 0.54 36 1 0 0.53 0.53 -36 -1 0 0.06 0.50 36 -1 0 -0.05 0.50 0 2 0 6.08 0.21 0 2 0 6.18 0.20 0 -2 0 6.81 0.22 0 -2 0 6.30 0.16 -1 2 0 143.95 0.73 -1 2 0 143.93 0.70 1 2 0 141.10 0.70 1 2 0 138.27 0.65 -1 -2 0 145.88 0.72 -1 -2 0 142.80 0.65 1 -2 0 149.06 0.77 1 -2 0 143.23 0.46 -2 2 0 38.51 0.42 -2 2 0 39.14 0.41 2 2 0 40.50 0.42 2 2 0 39.82 0.39 -2 -2 0 40.67 0.39 -2 -2 0 38.28 0.40 -3 2 0 16.54 0.32 3 2 0 17.77 0.32 3 2 0 17.07 0.29 -3 -2 0 17.95 0.26 -3 -2 0 17.88 0.32 -4 2 0 233.31 1.11 -4 2 0 235.34 1.09 -4 2 0 218.94 0.54 4 2 0 234.04 1.04 4 2 0 227.40 0.99 -4 -2 0 232.49 0.81 -4 -2 0 216.43 1.06 4 -2 0 235.91 1.05 -5 2 0 0.36 0.14 -5 2 0 0.35 0.15 -5 2 0 0.47 0.07 5 2 0 0.61 0.15 5 2 0 0.39 0.13 -5 -2 0 0.45 0.09 -5 -2 0 0.38 0.16 5 -2 0 0.71 0.14 -6 2 0 699.35 3.26 -6 2 0 798.18 4.55 -6 2 0 720.03 2.61 6 2 0 707.11 3.29 -6 -2 0 788.38 2.95 -6 -2 0 711.76 3.10 -6 -2 0 768.51 4.53 6 -2 0 752.27 3.93 -7 2 0 7.84 0.34 -7 2 0 7.75 0.20 7 2 0 8.35 0.34 -7 -2 0 8.13 0.17 -7 -2 0 7.88 0.31 -7 -2 0 7.41 0.33 7 -2 0 8.07 0.27 -8 2 0 549.78 2.13 -8 2 0 542.35 2.10 -8 2 0 554.51 2.24 8 2 0 550.90 2.03 -8 -2 0 578.27 1.74 -8 -2 0 557.84 2.01 -8 -2 0 547.20 2.12 8 -2 0 568.85 1.98 -9 2 0 0.16 0.17 -9 2 0 0.11 0.11 9 2 0 0.20 0.17 -9 -2 0 0.05 0.16 -9 -2 0 0.06 0.17 9 -2 0 0.12 0.12 9 -2 0 -0.03 0.17 -10 2 0 21.96 0.53 -10 2 0 22.85 0.38 10 2 0 22.99 0.53 -10 -2 0 22.36 0.50 -10 -2 0 21.64 0.52 10 -2 0 22.79 0.41 -11 2 0 69.23 0.90 -11 2 0 71.25 0.68 11 2 0 69.32 0.87 -11 -2 0 70.74 0.87 -11 -2 0 69.58 0.89 11 -2 0 74.21 0.70 11 -2 0 73.75 0.93 -12 2 0 198.42 1.54 -12 2 0 199.17 1.18 12 2 0 201.73 1.50 -12 -2 0 197.90 1.48 -12 -2 0 199.53 1.52 12 -2 0 205.50 1.15 12 -2 0 208.52 1.59 -13 2 0 35.69 0.73 -13 2 0 36.52 0.56 13 2 0 38.18 0.74 -13 -2 0 36.95 0.71 -13 -2 0 37.25 0.72 13 -2 0 38.24 0.53 13 -2 0 37.46 0.76 -14 2 0 15.33 0.55 -14 2 0 15.38 0.41 14 2 0 15.00 0.54 -14 -2 0 14.79 0.53 -14 -2 0 15.61 0.53 14 -2 0 15.93 0.37 14 -2 0 16.02 0.56 -15 2 0 150.68 1.51 -15 2 0 149.50 1.19 15 2 0 153.67 1.48 -15 -2 0 148.38 1.45 -15 -2 0 149.54 1.47 15 -2 0 152.84 1.04 15 -2 0 153.01 1.53 -16 2 0 18.11 0.62 -16 2 0 18.87 0.49 16 2 0 18.19 0.63 -16 -2 0 18.22 0.60 -16 -2 0 18.59 0.60 16 -2 0 18.43 0.41 16 -2 0 18.84 0.65 -17 2 0 91.24 1.28 -17 2 0 90.66 1.02 17 2 0 94.80 1.28 -17 -2 0 92.64 1.25 -17 -2 0 94.76 1.26 17 -2 0 92.79 0.84 17 -2 0 92.04 1.29 -18 2 0 7.49 0.40 18 2 0 8.49 0.54 -18 -2 0 7.95 0.50 -18 -2 0 8.41 0.49 18 -2 0 8.03 0.32 18 -2 0 8.40 0.54 -19 2 0 39.04 0.94 -19 2 0 38.22 0.74 19 2 0 40.24 0.95 -19 -2 0 38.66 0.91 -19 -2 0 39.10 0.91 19 -2 0 40.88 0.96 -20 2 0 14.33 0.53 20 2 0 15.95 0.69 -20 -2 0 14.35 0.67 -20 -2 0 14.20 0.62 20 -2 0 15.04 0.69 -21 2 0 -0.05 0.28 -21 2 0 0.08 0.21 21 2 0 -0.03 0.30 -21 -2 0 0.03 0.29 -21 -2 0 -0.01 0.25 21 -2 0 -0.02 0.30 -22 2 0 18.21 0.78 -22 2 0 17.34 0.62 22 2 0 18.37 0.77 -22 -2 0 16.62 0.73 -22 -2 0 17.12 0.71 22 -2 0 16.89 0.77 -23 2 0 5.57 0.58 -23 2 0 6.21 0.46 23 2 0 7.35 0.65 -23 -2 0 6.42 0.61 -23 -2 0 6.40 0.55 23 -2 0 6.43 0.65 -24 2 0 23.46 0.89 -24 2 0 23.84 0.74 24 2 0 24.32 0.89 -24 -2 0 22.53 0.85 -24 -2 0 23.01 0.82 24 -2 0 24.09 0.91 -25 2 0 9.94 0.73 -25 2 0 9.41 0.54 25 2 0 10.36 0.71 -25 -2 0 9.41 0.67 -25 -2 0 9.72 0.65 25 -2 0 9.66 0.71 -26 2 0 4.47 0.54 26 2 0 5.59 0.63 -26 -2 0 5.50 0.61 -26 -2 0 4.93 0.57 26 -2 0 4.90 0.57 -27 2 0 26.17 1.01 27 2 0 24.40 0.99 -27 -2 0 26.60 0.99 -27 -2 0 25.15 0.94 27 -2 0 25.94 1.04 -28 2 0 6.20 0.69 28 2 0 6.47 0.73 -28 -2 0 6.34 0.68 -28 -2 0 5.99 0.63 28 -2 0 6.46 0.75 -29 2 0 17.80 0.93 29 2 0 17.80 0.96 -29 -2 0 18.44 0.92 -29 -2 0 17.50 0.87 29 -2 0 18.13 0.98 -30 2 0 1.74 0.48 30 2 0 1.43 0.48 -30 -2 0 1.36 0.45 -30 -2 0 1.43 0.39 30 -2 0 1.22 0.48 -31 2 0 61.82 1.57 31 2 0 64.96 1.58 -31 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1.20 3 -3 0 259.80 1.29 -4 3 0 38.96 0.56 -4 3 0 38.81 0.53 4 3 0 39.50 0.53 4 3 0 39.78 0.50 -4 -3 0 38.41 0.46 -4 -3 0 39.62 0.55 4 -3 0 40.83 0.55 -5 3 0 175.18 1.14 -5 3 0 179.30 1.12 5 3 0 183.78 1.10 5 3 0 178.05 1.03 -5 -3 0 181.49 0.91 -5 -3 0 176.74 1.13 5 -3 0 182.01 1.12 -6 3 0 89.57 0.86 -6 3 0 87.85 0.84 6 3 0 92.09 0.83 6 3 0 90.95 0.79 -6 -3 0 90.56 0.63 -6 -3 0 92.52 0.87 6 -3 0 90.37 0.81 -7 3 0 5.48 0.32 -7 3 0 4.84 0.31 -7 3 0 5.18 0.14 7 3 0 5.38 0.31 7 3 0 5.32 0.30 -7 -3 0 5.43 0.21 -7 -3 0 5.08 0.31 7 -3 0 5.55 0.28 -8 3 0 4.08 0.31 -8 3 0 3.99 0.31 -8 3 0 3.89 0.15 8 3 0 3.53 0.29 8 3 0 3.95 0.28 -8 -3 0 4.04 0.18 -8 -3 0 3.87 0.30 8 -3 0 3.94 0.25 -9 3 0 61.81 0.82 -9 3 0 64.68 0.83 -9 3 0 65.64 0.49 9 3 0 67.12 0.81 9 3 0 64.47 0.78 -9 -3 0 67.72 0.49 -9 -3 0 63.71 0.78 -9 -3 0 63.23 0.84 9 -3 0 65.54 0.73 -10 3 0 98.93 1.07 -10 3 0 101.08 1.07 -10 3 0 104.23 0.67 10 3 0 99.14 1.01 -10 -3 0 106.65 0.58 -10 -3 0 102.74 1.01 -10 -3 0 100.18 1.07 10 -3 0 104.71 0.93 -11 3 0 25.09 0.60 -11 3 0 25.32 0.61 -11 3 0 26.06 0.39 11 3 0 24.83 0.58 -11 -3 0 27.01 0.29 -11 -3 0 26.29 0.58 -11 -3 0 25.61 0.61 11 -3 0 26.83 0.51 11 -3 0 25.06 0.61 -12 3 0 0.66 0.22 -12 3 0 0.76 0.13 12 3 0 0.88 0.22 -12 -3 0 0.46 0.20 -12 -3 0 0.55 0.20 12 -3 0 1.21 0.18 12 -3 0 0.64 0.23 -13 3 0 32.11 0.72 -13 3 0 31.97 0.49 13 3 0 32.64 0.71 -13 -3 0 32.50 0.68 -13 -3 0 32.02 0.71 13 -3 0 32.98 0.57 13 -3 0 32.84 0.74 -14 3 0 25.11 0.67 -14 3 0 25.27 0.47 14 3 0 26.58 0.68 -14 -3 0 25.02 0.63 -14 -3 0 24.99 0.67 14 -3 0 26.91 0.53 14 -3 0 26.25 0.69 -15 3 0 0.79 0.26 -15 3 0 0.92 0.17 15 3 0 1.01 0.27 -15 -3 0 0.80 0.24 -15 -3 0 0.94 0.26 15 -3 0 1.11 0.19 15 -3 0 0.80 0.25 -16 3 0 12.54 0.58 -16 3 0 12.62 0.39 16 3 0 12.52 0.57 -16 -3 0 12.30 0.53 -16 -3 0 11.47 0.53 16 -3 0 12.57 0.40 16 -3 0 12.56 0.57 -17 3 0 12.53 0.58 -17 3 0 13.12 0.42 17 3 0 13.31 0.58 -17 -3 0 13.53 0.57 -17 -3 0 12.96 0.57 17 -3 0 13.78 0.42 17 -3 0 12.73 0.59 -18 3 0 22.72 0.75 -18 3 0 22.76 0.55 18 3 0 23.14 0.73 -18 -3 0 22.45 0.73 -18 -3 0 22.40 0.72 18 -3 0 24.06 0.54 18 -3 0 24.15 0.78 -19 3 0 52.46 1.08 -19 3 0 55.00 0.83 19 3 0 55.31 1.09 -19 -3 0 53.74 1.05 -19 -3 0 52.82 1.07 19 -3 0 54.30 0.77 19 -3 0 56.83 1.13 -20 3 0 42.55 1.02 -20 3 0 43.54 0.78 20 3 0 42.88 1.01 -20 -3 0 43.05 0.99 -20 -3 0 43.18 1.00 20 -3 0 44.77 1.06 -21 3 0 0.62 0.33 -21 3 0 0.39 0.21 21 3 0 0.29 0.31 -21 -3 0 0.46 0.31 -21 -3 0 0.74 0.30 21 -3 0 0.45 0.34 -22 3 0 8.07 0.64 -22 3 0 7.78 0.49 22 3 0 7.83 0.62 -22 -3 0 8.40 0.63 -22 -3 0 7.43 0.60 22 -3 0 8.57 0.68 -23 3 0 40.88 1.10 23 3 0 40.91 1.08 -23 -3 0 42.23 1.09 -23 -3 0 40.21 1.05 23 -3 0 42.16 1.12 -24 3 0 74.98 1.48 24 3 0 73.90 1.42 -24 -3 0 74.40 1.40 -24 -3 0 74.95 1.42 24 -3 0 72.75 1.44 -25 3 0 64.84 1.41 25 3 0 64.92 1.37 -25 -3 0 65.10 1.37 -25 -3 0 63.95 1.34 25 -3 0 67.84 1.44 -26 3 0 10.11 0.73 26 3 0 10.38 0.76 -26 -3 0 10.76 0.72 -26 -3 0 10.22 0.67 26 -3 0 10.79 0.76 -27 3 0 0.44 0.39 27 3 0 0.16 0.37 -27 -3 0 0.39 0.37 -27 -3 0 0.42 0.33 27 -3 0 -0.01 0.38 -28 3 0 26.74 1.05 28 3 0 26.92 1.03 -28 -3 0 28.06 1.07 -28 -3 0 28.38 1.04 28 -3 0 28.81 1.13 -29 3 0 18.86 0.96 29 3 0 19.23 0.98 -29 -3 0 18.32 0.95 -29 -3 0 18.09 0.91 29 -3 0 18.20 0.96 -30 3 0 4.04 0.61 30 3 0 2.90 0.56 -30 -3 0 3.71 0.57 -30 -3 0 3.54 0.52 30 -3 0 3.30 0.60 -31 3 0 9.69 0.83 31 3 0 9.35 0.85 -31 -3 0 9.83 0.83 -31 -3 0 10.09 0.76 31 -3 0 8.64 0.83 -32 3 0 2.37 0.54 32 3 0 2.73 0.59 -32 -3 0 2.61 0.56 -32 -3 0 2.45 0.50 32 -3 0 2.50 0.61 -33 3 0 7.75 0.88 33 3 0 8.38 0.84 -33 -3 0 8.25 0.83 -33 -3 0 7.65 0.74 33 -3 0 7.49 0.89 -34 3 0 17.04 1.09 34 3 0 18.07 1.06 -34 -3 0 17.34 1.03 -34 -3 0 16.71 0.95 34 -3 0 17.88 1.09 -35 3 0 6.45 0.78 35 3 0 6.62 0.79 -35 -3 0 6.00 0.75 -35 -3 0 6.79 0.75 35 -3 0 6.02 0.80 36 3 0 17.69 1.14 -36 -3 0 19.38 1.18 -36 -3 0 19.70 1.05 0 4 0 0.06 0.15 0 4 0 0.19 0.15 0 -4 0 0.21 0.15 0 -4 0 0.41 0.12 -1 4 0 74.48 0.75 -1 4 0 73.07 0.71 1 4 0 72.07 0.74 1 4 0 72.81 0.70 -1 -4 0 75.27 0.77 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1.29 -9 -4 0 183.51 1.00 -9 -4 0 175.26 1.43 9 -4 0 182.30 1.34 -10 4 0 2.62 0.29 -10 4 0 2.09 0.26 -10 4 0 2.30 0.14 10 4 0 1.88 0.25 10 4 0 2.01 0.24 -10 -4 0 2.17 0.19 -10 -4 0 2.34 0.29 10 -4 0 2.74 0.29 -11 4 0 1.56 0.26 -11 4 0 1.83 0.27 -11 4 0 1.54 0.15 11 4 0 1.81 0.26 11 4 0 1.37 0.22 -11 -4 0 1.64 0.18 -11 -4 0 2.01 0.28 11 -4 0 1.60 0.22 -12 4 0 8.90 0.46 -12 4 0 8.69 0.46 -12 4 0 9.36 0.25 12 4 0 9.28 0.44 12 4 0 9.57 0.42 -12 -4 0 9.85 0.25 -12 -4 0 8.77 0.45 12 -4 0 9.34 0.39 -13 4 0 69.25 1.05 -13 4 0 69.37 1.05 -13 4 0 70.44 0.62 13 4 0 71.93 1.02 13 4 0 69.32 0.97 -13 -4 0 73.89 0.55 -13 -4 0 66.51 1.03 13 -4 0 70.95 0.90 -14 4 0 21.14 0.65 -14 4 0 22.14 0.40 14 4 0 23.73 0.65 14 4 0 23.18 0.62 -14 -4 0 23.12 0.30 -14 -4 0 22.49 0.62 -14 -4 0 22.10 0.67 14 -4 0 23.46 0.56 14 -4 0 22.81 0.69 -15 4 0 3.72 0.41 -15 4 0 3.30 0.23 15 4 0 3.77 0.43 -15 -4 0 3.56 0.38 -15 -4 0 3.20 0.39 15 -4 0 3.40 0.32 15 -4 0 3.41 0.42 -16 4 0 0.22 0.24 -16 4 0 0.19 0.14 16 4 0 -0.12 0.25 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3.63 0.50 25 -4 0 3.42 0.53 -26 4 0 3.23 0.50 26 4 0 3.07 0.50 -26 -4 0 3.36 0.50 -26 -4 0 3.58 0.49 26 -4 0 3.26 0.53 -27 4 0 23.73 1.00 27 4 0 23.79 0.97 -27 -4 0 23.41 0.95 -27 -4 0 23.15 0.97 27 -4 0 25.48 1.07 -28 4 0 31.62 1.13 28 4 0 32.50 1.14 -28 -4 0 31.59 1.12 -28 -4 0 31.77 1.10 28 -4 0 32.65 1.17 -29 4 0 2.33 0.52 29 4 0 2.75 0.53 -29 -4 0 2.02 0.49 -29 -4 0 2.26 0.46 29 -4 0 1.67 0.51 -30 4 0 3.56 0.60 30 4 0 3.36 0.57 -30 -4 0 3.95 0.58 -30 -4 0 3.33 0.54 30 -4 0 4.13 0.65 -31 4 0 7.83 0.79 31 4 0 8.00 0.84 -31 -4 0 8.70 0.80 -31 -4 0 7.67 0.73 31 -4 0 8.47 0.87 -32 4 0 0.00 0.43 32 4 0 0.20 0.47 -32 -4 0 -0.01 0.42 -32 -4 0 0.39 0.40 32 -4 0 -0.11 0.46 -33 4 0 0.07 0.45 33 4 0 0.24 0.49 -33 -4 0 0.17 0.47 -33 -4 0 0.13 0.39 33 -4 0 0.28 0.51 -34 4 0 2.12 0.57 34 4 0 2.05 0.59 -34 -4 0 2.66 0.61 -34 -4 0 2.28 0.53 34 -4 0 2.63 0.65 -35 4 0 2.10 0.60 35 4 0 1.57 0.59 -35 -4 0 1.69 0.58 -35 -4 0 1.48 0.51 35 -4 0 1.21 0.59 0 5 0 0.00 0.16 0 5 0 0.14 0.16 0 -5 0 0.09 0.16 0 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255.86 1.59 -8 -5 0 260.74 1.41 -8 -5 0 252.74 1.73 8 -5 0 260.98 1.75 -9 5 0 250.17 1.80 -9 5 0 249.37 1.76 9 5 0 260.49 1.73 9 5 0 248.78 1.61 -9 -5 0 256.30 1.37 -9 -5 0 252.85 1.80 9 -5 0 262.29 1.76 -10 5 0 13.07 0.52 -10 5 0 13.74 0.52 10 5 0 12.42 0.49 10 5 0 13.39 0.46 -10 -5 0 13.71 0.37 -10 -5 0 13.00 0.50 10 -5 0 12.99 0.48 -11 5 0 17.27 0.58 -11 5 0 16.45 0.56 11 5 0 18.44 0.58 11 5 0 17.14 0.53 -11 -5 0 17.17 0.39 -11 -5 0 17.20 0.58 11 -5 0 17.62 0.54 -12 5 0 4.61 0.41 -12 5 0 5.03 0.41 -12 5 0 4.44 0.16 12 5 0 4.46 0.39 12 5 0 4.53 0.37 -12 -5 0 4.64 0.25 -12 -5 0 5.12 0.41 12 -5 0 4.85 0.37 -13 5 0 13.42 0.57 -13 5 0 14.01 0.57 -13 5 0 13.66 0.26 13 5 0 13.30 0.55 13 5 0 13.14 0.52 -13 -5 0 14.13 0.34 -13 -5 0 14.21 0.58 13 -5 0 14.11 0.51 -14 5 0 0.14 0.24 -14 5 0 0.26 0.23 -14 5 0 0.17 0.12 14 5 0 0.20 0.24 14 5 0 0.29 0.22 -14 -5 0 0.28 0.13 -14 -5 0 0.10 0.22 14 -5 0 0.39 0.21 -15 5 0 4.31 0.48 -15 5 0 5.16 0.48 15 5 0 5.41 0.46 15 5 0 4.84 0.43 -15 -5 0 4.89 0.46 15 -5 0 5.76 0.40 -16 5 0 -0.10 0.26 16 5 0 -0.05 0.26 16 5 0 -0.05 0.22 -16 -5 0 -0.01 0.24 16 -5 0 0.27 0.22 16 -5 0 0.34 0.27 -17 5 0 9.09 0.58 17 5 0 10.17 0.60 17 5 0 10.04 0.54 -17 -5 0 9.49 0.57 17 -5 0 10.64 0.50 17 -5 0 9.59 0.59 -18 5 0 17.51 0.72 18 5 0 18.28 0.73 18 5 0 18.22 0.67 -18 -5 0 17.85 0.72 18 -5 0 18.44 0.60 18 -5 0 18.21 0.76 -19 5 0 2.38 0.41 19 5 0 2.52 0.40 19 5 0 1.72 0.34 -19 -5 0 1.95 0.36 19 -5 0 2.28 0.32 19 -5 0 2.38 0.42 -20 5 0 10.60 0.66 20 5 0 10.28 0.64 20 5 0 10.75 0.62 -20 -5 0 10.56 0.65 20 -5 0 10.41 0.51 20 -5 0 11.01 0.70 -21 5 0 28.79 0.93 21 5 0 27.57 0.90 21 5 0 27.02 0.86 -21 -5 0 27.98 0.93 21 -5 0 28.33 0.92 21 -5 0 28.81 0.95 -22 5 0 23.01 0.88 22 5 0 21.79 0.84 22 5 0 20.74 0.79 -22 -5 0 20.77 0.84 22 -5 0 21.70 0.89 -23 5 0 2.06 0.42 23 5 0 1.90 0.43 23 5 0 2.06 0.40 -23 -5 0 2.30 0.44 23 -5 0 2.49 0.47 -24 5 0 -0.21 0.33 24 5 0 0.14 0.35 24 5 0 0.06 0.30 -24 -5 0 0.15 0.32 24 -5 0 0.23 0.39 -25 5 0 2.51 0.47 25 5 0 2.56 0.47 25 5 0 2.88 0.45 -25 -5 0 2.67 0.46 25 -5 0 2.63 0.51 -26 5 0 1.82 0.44 26 5 0 1.26 0.44 26 5 0 2.23 0.44 -26 -5 0 1.57 0.42 26 -5 0 1.45 0.45 -27 5 0 0.04 0.36 27 5 0 -0.13 0.38 27 5 0 0.10 0.34 -27 -5 0 0.26 0.36 27 -5 0 -0.38 0.41 -28 5 0 9.34 0.81 28 5 0 9.49 0.81 28 5 0 8.09 0.73 -28 -5 0 9.72 0.75 28 -5 0 10.11 0.83 -29 5 0 4.75 0.62 29 5 0 4.98 0.63 29 5 0 4.59 0.58 -29 -5 0 4.01 0.57 29 -5 0 5.14 0.66 -30 5 0 11.94 0.87 30 5 0 12.50 0.87 30 5 0 11.16 0.79 -30 -5 0 11.88 0.82 30 -5 0 12.59 0.96 -31 5 0 3.04 0.57 31 5 0 3.45 0.61 31 5 0 3.28 0.54 -31 -5 0 3.40 0.56 31 -5 0 3.24 0.62 -32 5 0 23.49 1.13 32 5 0 25.70 1.14 32 5 0 25.75 1.12 -32 -5 0 24.83 1.12 32 -5 0 24.80 1.23 -33 5 0 3.68 0.64 33 5 0 3.62 0.66 33 5 0 3.51 0.60 -33 -5 0 3.76 0.60 33 -5 0 3.82 0.67 -34 5 0 13.72 1.03 34 5 0 14.33 1.01 34 5 0 15.20 0.99 -34 -5 0 15.19 0.97 34 -5 0 15.03 1.10 35 5 0 -0.09 0.51 35 5 0 0.59 0.46 -35 -5 0 0.25 0.46 0 6 0 204.40 1.48 0 6 0 188.47 1.34 0 -6 0 210.77 1.57 0 -6 0 199.32 1.14 -1 6 0 84.15 0.99 -1 6 0 78.42 0.90 1 6 0 82.43 0.97 1 6 0 83.34 0.91 -1 -6 0 84.20 1.01 -1 -6 0 83.11 0.79 1 -6 0 82.21 1.01 1 -6 0 83.30 0.70 -2 6 0 55.31 0.82 -2 6 0 56.37 0.79 2 6 0 55.04 0.80 2 6 0 53.59 0.75 -2 -6 0 57.24 0.83 -2 -6 0 56.32 0.70 2 -6 0 54.49 0.84 2 -6 0 56.67 0.54 -3 6 0 0.24 0.19 -3 6 0 0.00 0.18 3 6 0 0.32 0.19 3 6 0 0.18 0.19 -3 -6 0 0.18 0.18 -3 -6 0 0.06 0.15 3 -6 0 0.12 0.19 3 -6 0 0.26 0.10 -4 6 0 215.36 1.60 -4 6 0 206.78 1.48 4 6 0 218.47 1.55 4 6 0 210.05 1.42 -4 -6 0 213.10 1.51 -4 -6 0 210.64 1.44 4 -6 0 218.21 1.67 4 -6 0 211.25 0.81 -5 6 0 1.68 0.25 -5 6 0 1.94 0.25 5 6 0 1.73 0.26 5 6 0 1.99 0.24 -5 -6 0 2.37 0.29 -5 -6 0 2.26 0.25 5 -6 0 1.96 0.26 5 -6 0 2.04 0.11 -6 6 0 5.42 0.38 -6 6 0 5.27 0.38 6 6 0 5.50 0.39 6 6 0 5.25 0.35 -6 -6 0 5.81 0.34 -6 -6 0 5.77 0.35 6 -6 0 6.14 0.41 -7 6 0 0.75 0.22 -7 6 0 0.74 0.22 7 6 0 0.68 0.22 7 6 0 0.96 0.21 -7 -6 0 0.88 0.19 -7 -6 0 0.72 0.21 7 -6 0 0.79 0.22 -8 6 0 22.56 0.63 -8 6 0 21.58 0.61 8 6 0 21.52 0.60 8 6 0 21.34 0.55 -8 -6 0 21.85 0.52 -8 -6 0 20.94 0.58 8 -6 0 22.32 0.63 -9 6 0 8.96 0.48 -9 6 0 8.23 0.44 9 6 0 8.03 0.43 9 6 0 8.23 0.41 -9 -6 0 8.53 0.36 -9 -6 0 8.61 0.45 9 -6 0 8.60 0.45 -10 6 0 1.97 0.29 -10 6 0 2.01 0.29 10 6 0 2.29 0.30 10 6 0 2.23 0.27 -10 -6 0 2.44 0.27 -10 -6 0 2.36 0.30 10 -6 0 2.46 0.30 -11 6 0 181.14 1.72 -11 6 0 183.07 1.68 11 6 0 173.33 1.58 11 6 0 181.60 1.54 -11 -6 0 178.55 1.26 -11 -6 0 178.36 1.69 11 -6 0 181.88 1.64 -12 6 0 21.79 0.70 -12 6 0 21.46 0.67 12 6 0 22.93 0.68 12 6 0 22.31 0.63 -12 -6 0 22.30 0.48 -12 -6 0 22.10 0.69 12 -6 0 22.83 0.66 -13 6 0 3.28 0.38 -13 6 0 4.02 0.44 13 6 0 3.79 0.45 13 6 0 3.61 0.39 -13 -6 0 3.63 0.28 -13 -6 0 3.40 0.42 13 -6 0 2.98 0.33 -14 6 0 123.71 1.54 -14 6 0 127.14 1.54 14 6 0 130.18 1.48 14 6 0 130.49 1.43 -14 -6 0 128.61 1.01 -14 -6 0 127.69 1.57 14 -6 0 130.52 1.45 -15 6 0 39.55 0.96 -15 6 0 38.59 0.93 15 6 0 39.56 0.91 15 6 0 40.29 0.87 -15 -6 0 37.78 0.93 15 -6 0 40.85 0.86 -16 6 0 14.55 0.68 -16 6 0 15.83 0.68 16 6 0 15.33 0.65 16 6 0 14.43 0.62 -16 -6 0 15.45 0.68 16 -6 0 15.04 0.58 -17 6 0 30.52 0.90 -17 6 0 30.67 0.91 17 6 0 30.58 0.87 17 6 0 30.43 0.82 -17 -6 0 30.66 0.90 17 -6 0 31.21 0.79 17 -6 0 31.16 0.92 -18 6 0 6.96 0.57 18 6 0 7.17 0.59 18 6 0 6.61 0.53 -18 -6 0 6.80 0.57 18 -6 0 7.07 0.49 18 -6 0 6.04 0.58 -19 6 0 11.04 0.66 19 6 0 11.07 0.67 19 6 0 11.49 0.61 -19 -6 0 10.77 0.66 19 -6 0 11.43 0.56 19 -6 0 11.56 0.69 -20 6 0 4.43 0.51 20 6 0 3.77 0.46 20 6 0 3.54 0.43 -20 -6 0 3.86 0.47 20 -6 0 4.06 0.44 20 -6 0 4.60 0.57 -21 6 0 15.97 0.77 21 6 0 15.10 0.76 21 6 0 14.49 0.69 -21 -6 0 14.69 0.75 21 -6 0 15.71 0.63 21 -6 0 16.41 0.80 -22 6 0 13.27 0.74 22 6 0 13.19 0.74 22 6 0 13.26 0.69 -22 -6 0 13.86 0.76 22 -6 0 13.36 0.77 -23 6 0 34.17 1.07 23 6 0 32.35 1.03 23 6 0 33.72 1.00 -23 -6 0 34.28 1.08 23 -6 0 33.58 1.08 -24 6 0 9.69 0.72 24 6 0 9.09 0.72 24 6 0 9.50 0.69 -24 -6 0 10.51 0.74 24 -6 0 10.37 0.79 -25 6 0 18.94 0.91 25 6 0 19.29 0.88 25 6 0 18.94 0.84 -25 -6 0 18.82 0.90 25 -6 0 19.57 0.97 -26 6 0 0.56 0.39 26 6 0 0.49 0.41 26 6 0 0.42 0.37 -26 -6 0 0.66 0.38 26 -6 0 0.30 0.41 -27 6 0 8.19 0.78 27 6 0 8.30 0.77 27 6 0 8.30 0.72 -27 -6 0 8.21 0.72 27 -6 0 8.58 0.79 -28 6 0 1.76 0.48 28 6 0 2.45 0.53 28 6 0 2.22 0.46 -28 -6 0 1.88 0.47 28 -6 0 2.98 0.59 -29 6 0 -0.08 0.39 29 6 0 -0.50 0.39 29 6 0 -0.08 0.38 -29 -6 0 0.29 0.40 29 -6 0 0.08 0.44 -30 6 0 8.36 0.80 30 6 0 7.56 0.79 30 6 0 8.30 0.78 -30 -6 0 9.04 0.79 30 -6 0 9.36 0.93 -31 6 0 6.93 0.82 31 6 0 5.86 0.71 31 6 0 6.42 0.75 -31 -6 0 7.36 0.77 31 -6 0 6.21 0.77 -32 6 0 0.97 0.50 32 6 0 0.63 0.50 32 6 0 1.15 0.47 -32 -6 0 1.44 0.49 32 -6 0 1.16 0.55 -33 6 0 0.27 0.49 33 6 0 -0.21 0.46 33 6 0 -0.08 0.45 -33 -6 0 0.16 0.43 33 -6 0 0.30 0.51 34 6 0 1.99 0.61 34 6 0 2.42 0.57 -34 -6 0 2.17 0.55 0 7 0 0.01 0.19 0 7 0 0.09 0.19 0 -7 0 0.19 0.20 0 -7 0 0.11 0.14 -1 7 0 57.64 0.90 -1 7 0 58.93 0.86 1 7 0 57.90 0.90 1 7 0 56.89 0.84 -1 -7 0 58.06 0.92 -1 -7 0 59.44 0.73 1 -7 0 58.74 0.95 1 -7 0 57.90 0.65 -2 7 0 12.46 0.50 -2 7 0 12.04 0.48 2 7 0 12.83 0.50 2 7 0 11.79 0.47 -2 -7 0 12.26 0.50 -2 -7 0 12.68 0.41 2 -7 0 12.65 0.51 2 -7 0 12.52 0.32 -3 7 0 3.09 0.37 -3 7 0 3.42 0.35 3 7 0 3.82 0.37 3 7 0 3.27 0.36 -3 -7 0 3.60 0.37 -3 -7 0 3.43 0.30 3 -7 0 4.06 0.39 3 -7 0 3.69 0.21 -4 7 0 112.27 1.26 -4 7 0 115.98 1.21 4 7 0 112.25 1.22 4 7 0 113.84 1.15 -4 -7 0 113.44 1.22 -4 -7 0 112.65 1.13 4 -7 0 115.99 1.33 4 -7 0 112.66 0.69 -5 7 0 90.01 1.15 -5 7 0 90.46 1.10 5 7 0 90.52 1.12 5 7 0 88.61 1.03 -5 -7 0 91.77 1.10 -5 -7 0 88.74 1.04 5 -7 0 89.02 1.18 5 -7 0 86.55 0.52 -6 7 0 9.91 0.48 -6 7 0 10.39 0.49 6 7 0 9.84 0.48 6 7 0 10.06 0.44 -6 -7 0 10.33 0.44 -6 -7 0 10.54 0.46 6 -7 0 10.15 0.50 -7 7 0 4.33 0.42 -7 7 0 4.07 0.40 7 7 0 4.92 0.41 7 7 0 4.67 0.38 -7 -7 0 4.48 0.35 -7 -7 0 5.06 0.37 7 -7 0 4.60 0.41 -8 7 0 0.18 0.22 -8 7 0 0.16 0.21 8 7 0 0.36 0.23 8 7 0 0.17 0.21 -8 -7 0 0.14 0.18 -8 -7 0 0.14 0.22 8 -7 0 0.21 0.24 -9 7 0 3.29 0.36 -9 7 0 2.74 0.32 9 7 0 2.77 0.33 9 7 0 2.18 0.28 -9 -7 0 3.04 0.32 -9 -7 0 2.25 0.31 9 -7 0 3.39 0.36 -10 7 0 1.84 0.30 -10 7 0 1.73 0.30 10 7 0 2.30 0.32 10 7 0 1.84 0.28 -10 -7 0 1.74 0.25 -10 -7 0 1.76 0.29 10 -7 0 2.06 0.31 -11 7 0 51.06 1.01 -11 7 0 49.65 0.97 11 7 0 51.94 0.96 11 7 0 50.91 0.90 -11 -7 0 51.40 0.79 -11 -7 0 51.57 0.99 11 -7 0 51.19 0.98 -12 7 0 19.31 0.70 -12 7 0 18.62 0.68 12 7 0 19.97 0.69 12 7 0 19.78 0.64 -12 -7 0 20.36 0.53 -12 -7 0 18.54 0.67 12 -7 0 20.00 0.67 -13 7 0 52.09 1.07 -13 7 0 51.40 1.04 13 7 0 53.05 1.02 13 7 0 53.25 0.96 -13 -7 0 52.33 0.77 -13 -7 0 53.30 1.08 13 -7 0 53.89 1.02 -14 7 0 11.26 0.62 -14 7 0 12.50 0.63 14 7 0 11.95 0.63 14 7 0 11.67 0.57 -14 -7 0 11.39 0.52 -14 -7 0 11.57 0.61 14 -7 0 11.92 0.60 -15 7 0 18.69 0.77 -15 7 0 18.87 0.74 15 7 0 18.96 0.73 15 7 0 18.86 0.68 -15 -7 0 18.38 0.74 15 -7 0 19.47 0.71 -16 7 0 0.13 0.30 -16 7 0 0.09 0.28 16 7 0 0.11 0.29 16 7 0 0.15 0.26 -16 -7 0 -0.01 0.29 16 -7 0 -0.13 0.27 -17 7 0 2.86 0.43 -17 7 0 2.93 0.44 17 7 0 2.95 0.42 17 7 0 2.74 0.39 -17 -7 0 2.64 0.40 17 -7 0 2.44 0.37 -18 7 0 0.02 0.31 -18 7 0 0.19 0.30 18 7 0 0.25 0.32 18 7 0 0.24 0.28 -18 -7 0 0.18 0.32 18 -7 0 0.14 0.27 -19 7 0 10.28 0.66 19 7 0 10.98 0.67 19 7 0 10.32 0.62 -19 -7 0 10.15 0.67 19 -7 0 10.64 0.60 19 -7 0 10.15 0.71 -20 7 0 0.33 0.33 20 7 0 0.35 0.34 20 7 0 0.53 0.31 -20 -7 0 0.66 0.35 20 -7 0 0.40 0.29 20 -7 0 0.63 0.37 -21 7 0 2.41 0.46 21 7 0 1.69 0.41 21 7 0 2.06 0.40 -21 -7 0 2.33 0.44 21 -7 0 1.96 0.37 21 -7 0 2.54 0.46 -22 7 0 15.40 0.80 22 7 0 15.91 0.80 22 7 0 15.83 0.74 -22 -7 0 15.74 0.82 22 -7 0 16.17 0.72 22 -7 0 16.67 0.85 -23 7 0 5.16 0.62 23 7 0 4.44 0.54 23 7 0 4.35 0.52 -23 -7 0 4.28 0.53 23 -7 0 4.43 0.56 -24 7 0 8.56 0.71 24 7 0 9.11 0.71 24 7 0 8.39 0.68 -24 -7 0 8.29 0.72 24 -7 0 9.15 0.79 -25 7 0 1.71 0.45 25 7 0 1.42 0.44 25 7 0 1.22 0.40 -25 -7 0 1.25 0.42 25 -7 0 1.07 0.45 -26 7 0 0.40 0.39 26 7 0 0.37 0.42 26 7 0 0.32 0.38 -26 -7 0 0.62 0.41 26 -7 0 0.20 0.42 -27 7 0 9.24 0.79 27 7 0 9.35 0.80 27 7 0 9.11 0.72 -27 -7 0 8.58 0.78 27 -7 0 9.00 0.85 -28 7 0 8.83 0.83 28 7 0 8.91 0.82 28 7 0 8.10 0.76 -28 -7 0 7.72 0.76 28 -7 0 10.24 0.91 -29 7 0 8.47 0.80 29 7 0 7.55 0.80 29 7 0 7.54 0.77 -29 -7 0 8.01 0.77 29 -7 0 7.81 0.84 -30 7 0 0.70 0.45 30 7 0 0.50 0.46 30 7 0 0.61 0.44 -30 -7 0 1.17 0.46 30 -7 0 0.91 0.53 -31 7 0 4.81 0.66 31 7 0 5.05 0.68 31 7 0 5.48 0.67 -31 -7 0 5.86 0.71 31 -7 0 4.43 0.69 -32 7 0 0.18 0.45 32 7 0 0.00 0.45 32 7 0 0.27 0.46 -32 -7 0 0.75 0.47 32 -7 0 0.04 0.51 -33 7 0 7.98 0.98 33 7 0 7.66 0.88 33 7 0 7.33 0.85 -33 -7 0 9.59 0.92 33 -7 0 9.80 1.21 0 8 0 31.09 0.74 0 8 0 31.10 0.70 0 -8 0 32.10 0.79 0 -8 0 31.45 0.56 -1 8 0 14.71 0.57 -1 8 0 15.15 0.55 1 8 0 14.61 0.56 1 8 0 13.80 0.52 -1 -8 0 15.00 0.58 -1 -8 0 14.18 0.43 1 -8 0 15.19 0.59 1 -8 0 14.54 0.40 -2 8 0 0.01 0.21 -2 8 0 0.08 0.23 2 8 0 0.27 0.22 2 8 0 0.28 0.23 -2 -8 0 0.10 0.22 -2 -8 0 0.14 0.17 2 -8 0 0.22 0.24 2 -8 0 0.28 0.13 -3 8 0 62.70 1.02 -3 8 0 60.14 0.95 3 8 0 60.85 0.99 3 8 0 61.03 0.93 -3 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0.55 11 8 0 8.36 0.51 -11 -8 0 8.39 0.44 -11 -8 0 8.59 0.54 11 -8 0 8.42 0.55 -12 8 0 7.43 0.58 -12 8 0 7.38 0.55 12 8 0 7.23 0.53 12 8 0 7.10 0.51 -12 -8 0 7.94 0.44 -12 -8 0 7.10 0.53 12 -8 0 7.48 0.54 -13 8 0 0.17 0.27 -13 8 0 -0.31 0.25 13 8 0 -0.10 0.27 13 8 0 0.13 0.26 -13 -8 0 0.02 0.20 -13 -8 0 -0.05 0.28 13 -8 0 -0.09 0.28 -14 8 0 13.34 0.69 -14 8 0 14.05 0.69 14 8 0 13.30 0.67 14 8 0 14.18 0.63 -14 -8 0 13.58 0.68 14 -8 0 13.96 0.66 -15 8 0 40.47 1.05 -15 8 0 41.31 1.04 15 8 0 41.97 1.01 15 8 0 41.03 0.95 -15 -8 0 43.38 1.07 15 -8 0 44.16 1.03 -16 8 0 14.90 0.76 -16 8 0 16.43 0.77 16 8 0 16.07 0.74 16 8 0 15.27 0.67 -16 -8 0 15.02 0.74 16 -8 0 16.75 0.73 -17 8 0 2.51 0.44 -17 8 0 2.50 0.42 17 8 0 3.45 0.45 17 8 0 2.79 0.40 -17 -8 0 2.60 0.43 17 -8 0 2.86 0.42 -18 8 0 1.68 0.40 -18 8 0 1.79 0.39 18 8 0 1.75 0.40 18 8 0 1.79 0.37 -18 -8 0 1.50 0.39 18 -8 0 1.71 0.37 -19 8 0 30.25 1.01 -19 8 0 31.03 0.99 19 8 0 31.54 0.98 19 8 0 32.86 0.94 -19 -8 0 30.91 1.01 19 -8 0 32.54 0.94 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0 1.38 0.39 -15 9 0 0.75 0.35 15 9 0 0.78 0.35 15 9 0 1.35 0.34 -15 -9 0 0.66 0.33 15 -9 0 0.65 0.34 -16 9 0 1.84 0.40 -16 9 0 2.05 0.41 16 9 0 1.33 0.38 16 9 0 1.79 0.36 -16 -9 0 1.48 0.37 16 -9 0 2.01 0.40 -17 9 0 84.83 1.56 -17 9 0 91.53 1.58 17 9 0 90.82 1.51 17 9 0 87.06 1.41 -17 -9 0 87.19 1.57 17 -9 0 90.05 1.51 -18 9 0 1.20 0.40 -18 9 0 1.33 0.38 18 9 0 1.38 0.39 18 9 0 1.25 0.35 -18 -9 0 1.34 0.39 18 -9 0 1.46 0.39 -19 9 0 26.68 1.00 -19 9 0 27.01 0.98 19 9 0 26.06 0.95 19 9 0 26.82 0.90 -19 -9 0 26.05 0.98 19 -9 0 28.31 0.95 -20 9 0 5.90 0.69 -20 9 0 6.78 0.68 20 9 0 7.38 0.68 20 9 0 7.78 0.63 -20 -9 0 7.69 0.69 20 -9 0 7.09 0.64 -21 9 0 7.93 0.72 21 9 0 7.66 0.71 21 9 0 7.53 0.64 -21 -9 0 7.67 0.74 21 -9 0 7.52 0.62 21 -9 0 7.96 0.73 -22 9 0 0.87 0.41 22 9 0 0.53 0.41 22 9 0 0.94 0.37 -22 -9 0 0.85 0.42 22 -9 0 0.79 0.37 22 -9 0 0.77 0.42 -23 9 0 1.16 0.42 23 9 0 0.45 0.41 23 9 0 0.78 0.38 -23 -9 0 0.89 0.44 23 -9 0 0.93 0.41 23 -9 0 0.45 0.43 -24 9 0 0.93 0.42 24 9 0 0.44 0.42 24 9 0 0.61 0.38 -24 -9 0 0.76 0.44 24 -9 0 0.81 0.44 -25 9 0 2.51 0.51 25 9 0 1.75 0.49 25 9 0 2.02 0.47 -25 -9 0 2.69 0.55 25 -9 0 1.81 0.54 -26 9 0 0.43 0.42 26 9 0 -0.48 0.41 26 9 0 -0.31 0.35 -26 -9 0 -0.04 0.40 26 -9 0 0.53 0.47 -27 9 0 44.65 1.40 27 9 0 44.02 1.36 27 9 0 43.57 1.62 -27 -9 0 44.02 1.43 27 -9 0 46.95 1.46 -28 9 0 1.40 0.51 28 9 0 1.78 0.53 -28 -9 0 2.37 0.56 28 -9 0 2.74 0.61 -29 9 0 1.48 0.51 29 9 0 1.37 0.54 -29 -9 0 1.43 0.51 29 -9 0 1.92 0.59 -30 9 0 0.81 0.48 30 9 0 1.02 0.52 -30 -9 0 1.03 0.50 30 -9 0 1.63 0.56 -31 9 0 1.07 0.65 31 9 0 0.22 0.51 0 10 0 4.82 0.51 0 10 0 4.96 0.48 0 -10 0 4.94 0.52 -1 10 0 8.48 0.55 -1 10 0 9.16 0.55 1 10 0 9.20 0.56 1 10 0 8.14 0.55 -1 -10 0 8.38 0.58 -1 -10 0 8.62 0.42 1 -10 0 8.27 0.59 -2 10 0 7.08 0.55 -2 10 0 7.44 0.53 2 10 0 7.54 0.55 2 10 0 7.13 0.54 -2 -10 0 7.77 0.56 -2 -10 0 7.22 0.43 2 -10 0 7.18 0.57 -3 10 0 0.29 0.27 -3 10 0 0.26 0.28 3 10 0 0.18 0.26 3 10 0 0.02 0.28 -3 -10 0 0.33 0.29 -3 -10 0 0.11 0.22 3 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2.62 0.62 -3 3 11 2.33 0.57 3 3 11 1.63 0.55 -3 -3 11 1.90 0.53 3 -3 11 1.85 0.56 -4 3 -11 8.83 0.85 4 3 -11 8.96 0.88 -4 -3 -11 7.77 0.93 4 -3 -11 8.01 0.91 -4 3 11 9.85 0.91 4 3 11 8.76 0.86 -4 -3 11 8.98 0.84 4 -3 11 7.92 0.85 -5 3 -11 4.12 0.66 5 3 -11 3.61 0.62 -5 -3 -11 3.59 0.65 5 -3 -11 3.73 0.66 -5 3 11 3.48 0.61 5 3 11 4.79 0.69 -5 -3 11 3.71 0.62 5 -3 11 4.15 0.66 -6 3 -11 11.47 0.90 6 3 -11 13.34 0.98 -6 -3 -11 12.54 1.05 6 -3 -11 12.56 1.00 -6 3 11 11.98 0.93 6 3 11 13.77 0.97 -6 -3 11 11.44 0.90 6 -3 11 12.81 0.96 -7 3 -11 1.29 0.54 7 3 -11 1.70 0.54 -7 -3 -11 1.19 0.57 7 -3 -11 1.13 0.56 -7 3 11 1.71 0.55 7 3 11 1.79 0.56 -7 -3 11 1.41 0.51 7 -3 11 0.60 0.48 -8 3 -11 1.06 0.52 8 3 -11 1.81 0.55 -8 -3 -11 0.65 0.54 8 -3 -11 1.29 0.58 -8 3 11 0.83 0.47 8 3 11 0.88 0.50 -8 -3 11 1.43 0.52 8 -3 11 1.60 0.55 -9 3 -11 7.03 0.86 9 3 -11 9.03 0.94 -9 -3 -11 8.11 0.95 9 -3 -11 6.75 0.81 -9 3 11 7.12 0.83 9 3 11 8.99 0.88 -9 -3 11 9.17 0.90 9 -3 11 8.41 0.93 -10 3 -11 15.36 0.99 10 3 -11 16.19 1.09 -10 -3 -11 15.84 1.11 10 -3 -11 15.41 1.07 -10 3 11 15.59 1.01 10 3 11 14.30 0.98 -10 -3 11 13.89 0.99 10 -3 11 15.16 1.05 -11 3 -11 3.29 0.62 11 3 -11 4.15 0.66 -11 -3 -11 3.88 0.71 11 -3 -11 3.20 0.64 -11 3 11 3.74 0.67 11 3 11 3.25 0.62 -11 -3 11 4.21 0.66 11 -3 11 3.45 0.65 -12 3 -11 -0.36 0.46 12 3 -11 0.42 0.50 -12 -3 -11 -0.17 0.54 12 -3 -11 0.29 0.54 -12 3 11 0.36 0.49 12 3 11 0.39 0.48 -12 -3 11 0.89 0.51 12 -3 11 0.09 0.48 -13 3 -11 1.17 0.55 13 3 -11 0.64 0.67 -13 -3 -11 0.34 0.56 13 -3 -11 1.66 0.61 -13 3 11 1.78 0.57 13 3 11 1.17 0.50 -13 -3 11 1.27 0.54 13 -3 11 1.16 0.52 -14 3 -11 3.98 0.74 14 -3 -11 4.47 0.72 -14 3 11 4.29 0.68 14 3 11 3.88 0.64 -14 -3 11 3.24 0.62 14 -3 11 4.10 0.68 0 4 -11 -0.24 0.43 0 -4 -11 -0.36 0.50 0 4 11 0.24 0.47 0 -4 11 -0.29 0.41 -1 4 -11 0.13 0.48 1 4 -11 0.12 0.45 -1 -4 -11 -0.32 0.49 1 -4 -11 -0.04 0.52 -1 4 11 -0.07 0.46 1 4 11 0.54 0.49 -1 -4 11 0.18 0.44 1 -4 11 0.06 0.44 -2 4 -11 2.45 0.58 2 4 -11 2.49 0.58 -2 -4 -11 1.99 0.58 2 -4 -11 1.90 0.61 -2 4 11 2.84 0.61 2 4 11 2.49 0.60 -2 -4 11 2.64 0.56 2 -4 11 3.42 0.64 -3 4 -11 5.22 0.67 3 4 -11 5.04 0.69 -3 -4 -11 5.51 0.75 3 -4 -11 5.51 0.76 -3 4 11 4.82 0.70 3 4 11 4.94 0.69 -3 -4 11 5.07 0.68 3 -4 11 5.25 0.71 -4 4 -11 0.42 0.48 4 4 -11 1.31 0.52 -4 -4 -11 0.62 0.56 4 -4 -11 1.55 0.58 -4 4 11 1.99 0.56 4 4 11 1.51 0.56 -4 -4 11 1.67 0.55 4 -4 11 0.77 0.51 -5 4 -11 -0.34 0.43 5 4 -11 0.53 0.49 -5 -4 -11 0.33 0.54 5 -4 -11 -0.25 0.50 -5 4 11 0.15 0.46 5 4 11 0.13 0.46 -5 -4 11 0.35 0.48 5 -4 11 0.31 0.47 -6 4 -11 10.86 0.89 6 4 -11 11.45 0.94 -6 -4 -11 11.16 1.02 6 -4 -11 10.26 1.01 -6 4 11 10.77 0.93 6 4 11 10.43 0.92 -6 -4 11 10.51 0.90 6 -4 11 11.47 0.95 -7 4 -11 6.47 0.73 7 4 -11 4.81 0.69 -7 -4 -11 5.30 0.76 7 -4 -11 6.17 0.77 -7 4 11 6.14 0.76 7 4 11 5.80 0.73 -7 -4 11 5.73 0.72 7 -4 11 5.51 0.73 -8 4 -11 4.40 0.68 8 4 -11 5.56 0.74 -8 -4 -11 5.23 0.78 8 -4 -11 4.01 0.71 -8 4 11 4.88 0.71 8 4 11 4.26 0.66 -8 -4 11 4.97 0.69 8 -4 11 5.32 0.73 -9 4 -11 8.89 0.90 9 4 -11 9.59 0.91 -9 -4 -11 8.30 0.97 9 -4 -11 9.96 0.97 -9 4 11 9.20 0.91 9 4 11 8.77 0.88 -9 -4 11 9.33 0.90 9 -4 11 8.65 0.89 -10 4 -11 3.07 0.63 10 4 -11 3.93 0.68 -10 -4 -11 3.05 0.69 10 -4 -11 3.21 0.67 -10 4 11 3.62 0.66 10 4 11 4.06 0.66 -10 -4 11 4.05 0.65 10 -4 11 2.74 0.62 -11 4 -11 7.73 0.94 11 4 -11 7.64 0.94 -11 -4 -11 8.18 0.99 11 -4 -11 8.38 0.95 -11 4 11 9.38 0.95 11 4 11 9.22 0.93 -11 -4 11 9.46 0.90 11 -4 11 9.57 0.97 12 4 -11 4.34 0.90 -12 -4 -11 4.20 1.18 12 -4 -11 4.16 0.72 -12 4 11 4.48 0.70 12 4 11 4.16 0.66 -12 -4 11 4.84 0.71 12 -4 11 3.87 0.68 13 -4 -11 2.03 0.63 -13 4 11 2.16 0.58 13 4 11 2.26 0.58 -13 -4 11 2.13 0.59 13 -4 11 2.59 0.61 0 5 -11 2.81 0.59 0 -5 -11 1.84 0.63 0 5 11 2.03 0.60 0 -5 11 2.45 0.59 -1 5 -11 2.99 0.61 1 5 -11 2.57 0.58 -1 -5 -11 2.97 0.67 1 -5 -11 2.45 0.64 -1 5 11 2.61 0.60 1 5 11 2.13 0.60 -1 -5 11 3.12 0.62 1 -5 11 3.40 0.64 -2 5 -11 7.17 0.86 2 5 -11 6.68 0.75 -2 -5 -11 5.60 0.76 2 -5 -11 6.10 0.79 -2 5 11 6.29 0.77 2 5 11 6.39 0.79 -2 -5 11 7.44 0.84 2 -5 11 6.52 0.76 -3 5 -11 2.16 0.55 3 5 -11 2.29 0.59 -3 -5 -11 1.75 0.63 3 -5 -11 2.82 0.66 -3 5 11 2.72 0.62 3 5 11 2.66 0.61 -3 -5 11 3.32 0.62 3 -5 11 3.07 0.63 -4 5 -11 8.51 0.89 4 5 -11 9.22 0.90 -4 -5 -11 8.81 0.91 4 -5 -11 8.82 0.96 -4 5 11 8.54 0.92 4 5 11 9.07 0.91 -4 -5 11 10.40 0.95 4 -5 11 8.69 0.90 -5 5 -11 7.04 0.75 5 5 -11 8.32 0.87 -5 -5 -11 7.19 0.85 5 -5 -11 7.74 0.86 -5 5 11 8.95 0.94 5 5 11 7.34 0.87 -5 -5 11 7.56 0.85 5 -5 11 7.73 0.88 -6 5 -11 0.20 0.48 6 5 -11 0.27 0.49 -6 -5 -11 0.00 0.57 6 -5 -11 0.05 0.50 -6 5 11 0.14 0.48 6 5 11 0.71 0.50 -6 -5 11 0.77 0.48 6 -5 11 0.20 0.48 -7 5 -11 9.59 0.86 7 5 -11 9.52 0.92 -7 -5 -11 8.72 1.05 7 -5 -11 9.17 0.96 -7 5 11 9.38 0.91 7 5 11 8.65 0.89 -7 -5 11 10.08 0.90 7 -5 11 8.83 0.92 -8 5 -11 3.78 0.87 8 5 -11 4.45 0.68 -8 -5 -11 4.50 0.73 8 -5 -11 3.75 0.70 -8 5 11 5.11 0.75 8 5 11 4.01 0.66 -8 -5 11 5.00 0.72 8 -5 11 4.60 0.71 9 5 -11 4.77 0.72 -9 -5 -11 5.24 0.79 9 -5 -11 5.37 0.77 -9 5 11 6.06 0.78 9 5 11 6.38 0.77 -9 -5 11 5.91 0.75 9 -5 11 5.15 0.75 10 5 -11 4.50 0.71 -10 -5 -11 3.08 1.11 10 -5 -11 4.52 0.73 -10 5 11 3.29 0.64 10 5 11 4.20 0.67 -10 -5 11 3.46 0.64 10 -5 11 3.99 0.70 11 5 -11 1.66 0.89 11 5 -11 3.70 1.03 11 -5 -11 3.36 0.69 -11 5 11 2.80 0.64 11 5 11 3.07 0.64 -11 -5 11 2.62 0.59 11 -5 11 2.44 0.64 0 6 -11 -0.05 0.46 0 -6 -11 -0.48 0.55 0 6 11 -0.15 0.47 0 -6 11 0.09 0.46 -1 6 -11 2.18 0.59 1 6 -11 1.82 0.55 -1 -6 -11 1.26 0.61 1 -6 -11 1.17 0.60 -1 6 11 1.82 0.60 1 6 11 1.59 0.58 -1 -6 11 1.63 0.55 1 -6 11 1.67 0.56 -2 6 -11 5.89 0.72 2 6 -11 5.32 0.71 -2 -6 -11 5.27 0.78 2 -6 -11 4.23 0.74 -2 6 11 5.53 0.77 2 6 11 4.72 0.71 -2 -6 11 4.98 0.73 2 -6 11 4.67 0.69 -3 6 -11 3.84 0.63 3 6 -11 2.58 0.79 3 6 -11 4.07 0.67 -3 -6 -11 3.11 0.67 3 -6 -11 3.16 0.67 -3 6 11 2.85 0.64 3 6 11 3.78 0.67 -3 -6 11 3.62 0.66 3 -6 11 3.48 0.63 -4 6 -11 5.61 0.71 4 6 -11 5.11 0.79 4 6 -11 6.21 0.75 -4 -6 -11 6.22 0.84 4 -6 -11 6.51 0.81 -4 6 11 7.51 0.88 4 6 11 5.84 0.77 -4 -6 11 5.69 0.74 4 -6 11 6.44 0.79 5 6 -11 6.31 0.77 5 6 -11 7.43 0.89 -5 -6 -11 6.49 0.83 5 -6 -11 6.58 0.82 -5 6 11 7.03 0.85 5 6 11 7.70 0.89 -5 -6 11 6.84 0.79 5 -6 11 6.72 0.81 6 6 -11 19.29 1.11 6 6 -11 24.92 1.24 -6 -6 -11 23.63 1.34 6 -6 -11 23.05 1.22 -6 6 11 23.97 1.23 6 6 11 23.55 1.23 -6 -6 11 24.13 1.18 6 -6 11 22.71 1.23 7 6 -11 -0.96 0.48 7 6 -11 0.29 0.49 -7 -6 -11 0.12 0.64 7 -6 -11 0.59 0.56 -7 6 11 -0.01 0.50 7 6 11 0.65 0.52 -7 -6 11 0.75 0.51 7 -6 11 0.28 0.55 8 6 -11 4.21 0.70 8 6 -11 5.30 0.72 8 -6 -11 5.01 0.76 -8 6 11 6.09 1.27 8 6 11 6.05 0.75 -8 -6 11 6.11 0.76 0 7 -11 6.17 0.74 0 7 -11 6.70 0.82 0 -7 -11 4.63 0.75 0 -7 11 6.93 1.26 -1 7 -11 6.32 0.74 -1 7 -11 6.00 0.80 1 7 -11 5.94 0.76 1 7 -11 8.00 0.89 -1 -7 -11 5.86 0.82 1 -7 -11 5.66 0.81 1 7 11 4.62 0.97 -1 -7 11 8.22 1.32 -2 7 -11 3.16 0.63 2 7 -11 2.84 0.64 2 7 -11 2.74 0.62 -2 -7 -11 2.06 0.66 2 -7 -11 2.19 0.68 2 7 11 3.24 0.80 -2 -7 11 3.17 0.74 -3 7 -11 1.27 0.76 3 7 -11 0.26 0.55 3 7 -11 0.35 0.50 -3 -7 -11 0.44 0.65 3 -7 -11 -0.01 0.56 3 7 11 0.68 0.59 -3 -7 11 1.32 0.70 4 7 -11 0.51 0.53 4 7 -11 2.37 0.58 -4 -7 -11 0.56 0.99 4 -7 -11 1.12 0.60 4 7 11 1.13 0.59 -4 -7 11 0.61 0.59 0 0 -12 40.82 1.62 0 0 12 41.52 1.82 -1 0 -12 0.20 0.57 1 0 -12 0.12 0.56 -1 0 12 0.88 0.63 1 0 12 0.64 0.59 -2 0 -12 21.57 1.23 2 0 -12 22.20 1.40 -2 0 12 23.77 1.50 2 0 12 23.20 1.39 -3 0 -12 -0.10 0.57 3 0 -12 0.73 0.70 -3 0 12 0.67 0.78 3 0 12 0.85 0.62 -4 0 -12 49.24 1.85 -4 0 12 49.92 2.35 4 0 12 48.13 2.36 -5 0 -12 -0.24 0.56 0 1 -12 0.78 0.54 0 -1 -12 -0.27 0.56 0 1 12 -0.19 0.69 0 -1 12 0.29 0.77 -1 1 -12 3.98 0.70 1 1 -12 3.86 0.77 -1 -1 -12 4.02 1.15 1 -1 -12 2.80 0.85 -1 1 12 3.27 0.81 1 1 12 3.18 0.77 -1 -1 12 3.93 0.89 1 -1 12 3.91 1.09 -2 1 -12 2.77 0.67 2 1 -12 2.94 0.75 -2 -1 -12 2.56 0.89 2 -1 -12 2.53 1.03 -2 1 12 2.42 0.76 2 1 12 2.96 0.80 -2 -1 12 2.88 0.79 2 -1 12 2.58 0.78 -3 1 -12 16.48 1.13 3 1 -12 21.16 1.86 -3 -1 -12 15.10 1.47 3 1 12 14.52 1.60 -3 -1 12 18.23 1.42 3 -1 12 14.89 1.60 -4 1 -12 0.91 0.56 4 1 12 1.94 0.76 -4 -1 12 1.95 0.85 -5 1 -12 3.53 0.68 5 1 12 3.24 0.99 0 2 -12 15.40 1.13 -1 2 -12 4.39 0.71 1 2 -12 4.62 0.78 -2 2 -12 5.48 0.76 2 2 -12 5.90 1.02 -3 2 -12 6.13 0.77 3 2 -12 7.00 1.28 -4 2 -12 16.14 1.14 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 61586 #===END data_L_5k _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'L_5k' _chemical_melting_point ? _chemical_formula_moiety 'C40 H59 O4 P, 0.5(C H2 Cl2)' _chemical_formula_sum 'C40.50 H60 Cl O4 P' _chemical_formula_weight 677.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6617(18) _cell_length_b 12.3698(19) _cell_length_c 14.951(2) _cell_angle_alpha 100.424(2) _cell_angle_beta 92.731(2) _cell_angle_gamma 115.736(2) _cell_volume 1891.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4613 _cell_measurement_theta_min 2.239 _cell_measurement_theta_max 27.001 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_F_000 734 _exptl_transmission_factor_min 0.940 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 0.182 _shelx_estimated_absorpt_T_min 0.931 _shelx_estimated_absorpt_T_max 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22210 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.399 _diffrn_reflns_theta_max 27.130 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 8299 _reflns_number_gt 5781 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6996P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8299 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C15A C 0.8211(4) 0.9366(5) 0.1350(4) 0.0215(12) Uani 0.543(9) 1 d . . P A 1 H15A H 0.770271 0.978311 0.162665 0.026 Uiso 0.543(9) 1 calc R U P A 1 C16A C 0.7469(6) 0.8456(6) 0.0445(3) 0.0425(18) Uani 0.543(9) 1 d . . P A 1 H16A H 0.792706 0.798088 0.022235 0.064 Uiso 0.543(9) 1 calc R U P A 1 H16B H 0.739778 0.890885 -0.001168 0.064 Uiso 0.543(9) 1 calc R U P A 1 H16C H 0.660676 0.789498 0.054452 0.064 Uiso 0.543(9) 1 calc R U P A 1 C17A C 0.948(3) 1.029(3) 0.1194(18) 0.0327(15) Uani 0.543(9) 1 d . . P A 1 H17A H 0.997741 1.082694 0.178486 0.049 Uiso 0.543(9) 1 calc R U P A 1 H17B H 0.935038 1.078863 0.079672 0.049 Uiso 0.543(9) 1 calc R U P A 1 H17C H 0.995115 0.986681 0.089896 0.049 Uiso 0.543(9) 1 calc R U P A 1 C15B C 0.8384(5) 0.9014(5) 0.0947(5) 0.0191(14) Uani 0.457(9) 1 d . . P A 2 H15B H 0.859210 0.848230 0.046240 0.023 Uiso 0.457(9) 1 calc R U P A 2 C16B C 0.948(3) 1.038(3) 0.117(2) 0.0327(15) Uani 0.457(9) 1 d . . P A 2 H16D H 0.949275 1.073608 0.063526 0.049 Uiso 0.457(9) 1 calc R U P A 2 H16E H 1.030873 1.038070 0.131397 0.049 Uiso 0.457(9) 1 calc R U P A 2 H16F H 0.931385 1.085869 0.169761 0.049 Uiso 0.457(9) 1 calc R U P A 2 C17B C 0.7098(5) 0.8969(5) 0.0647(3) 0.0219(15) Uani 0.457(9) 1 d . . P A 2 H17D H 0.693338 0.953364 0.111246 0.033 Uiso 0.457(9) 1 calc R U P A 2 H17E H 0.641299 0.812921 0.057772 0.033 Uiso 0.457(9) 1 calc R U P A 2 H17F H 0.711640 0.921586 0.005910 0.033 Uiso 0.457(9) 1 calc R U P A 2 Cl1 Cl 0.45881(15) 0.53475(16) 0.03013(12) 0.0546(4) Uani 0.5 1 d . . P B -1 Cl2 Cl 0.6363(2) 0.4610(2) -0.06553(11) 0.0731(6) Uani 0.5 1 d . . P B -1 C41 C 0.6134(6) 0.5424(5) 0.0375(4) 0.0431(13) Uani 0.5 1 d . . P B -1 H41A H 0.626092 0.507107 0.089385 0.052 Uiso 0.5 1 calc R U P B -1 H41B H 0.678764 0.629680 0.050316 0.052 Uiso 0.5 1 calc R U P B -1 P1 P 0.69984(5) 0.44027(5) 0.26001(3) 0.01447(13) Uani 1 1 d . . . . . O1 O 0.75235(14) 0.33904(13) 0.42335(10) 0.0231(3) Uani 1 1 d . . . . . O2 O 0.95507(15) 0.84499(14) 0.50209(10) 0.0276(4) Uani 1 1 d . . . . . O3 O 0.56953(15) 0.02250(13) 0.23727(11) 0.0268(4) Uani 1 1 d . . . . . O4 O 0.53180(14) 0.10263(13) 0.12015(10) 0.0253(3) Uani 1 1 d . . . . . C1 C 0.80424(19) 0.46478(19) 0.44768(14) 0.0174(4) Uani 1 1 d . . . . . C2 C 0.7552(2) 0.2743(2) 0.49244(16) 0.0269(5) Uani 1 1 d . . . . . H2A H 0.844631 0.299972 0.517314 0.040 Uiso 1 1 calc R U . . . H2B H 0.712964 0.185590 0.465642 0.040 Uiso 1 1 calc R U . . . H2C H 0.709827 0.292866 0.541912 0.040 Uiso 1 1 calc R U . . . C3 C 0.8694(2) 0.5324(2) 0.53407(14) 0.0218(5) Uani 1 1 d . . . . . H3 H 0.878343 0.491493 0.579934 0.026 Uiso 1 1 calc R U . . . C4 C 0.9216(2) 0.6596(2) 0.55407(14) 0.0242(5) Uani 1 1 d . . . . . H4 H 0.966144 0.705869 0.613578 0.029 Uiso 1 1 calc R U . . . C5 C 0.90877(19) 0.71928(19) 0.48727(14) 0.0209(4) Uani 1 1 d . . . . . C6 C 1.0180(2) 0.9163(2) 0.59244(17) 0.0361(6) Uani 1 1 d . . . . . H6A H 0.958288 0.890081 0.637026 0.054 Uiso 1 1 calc R U . . . H6B H 1.045334 1.003682 0.594297 0.054 Uiso 1 1 calc R U . . . H6C H 1.093354 0.903803 0.607793 0.054 Uiso 1 1 calc R U . . . C7 C 0.84485(18) 0.65237(19) 0.39777(13) 0.0175(4) Uani 1 1 d . . . . . C8 C 0.84196(19) 0.72533(18) 0.32764(14) 0.0195(4) Uani 1 1 d . . . . . C9 C 0.7395(2) 0.75563(19) 0.31488(16) 0.0268(5) Uani 1 1 d . . . . . C10 C 0.6330(2) 0.7256(2) 0.37507(17) 0.0297(5) Uani 1 1 d . . . . . H10 H 0.637866 0.665564 0.409985 0.036 Uiso 1 1 calc R U . . . C11 C 0.4981(2) 0.6665(2) 0.31908(19) 0.0346(6) Uani 1 1 d . . . . . H11A H 0.485307 0.728669 0.293558 0.052 Uiso 1 1 calc R U . . . H11B H 0.433174 0.633767 0.359098 0.052 Uiso 1 1 calc R U . . . H11C H 0.489981 0.599375 0.268889 0.052 Uiso 1 1 calc R U . . . C12 C 0.6537(3) 0.8421(3) 0.4449(2) 0.0492(8) Uani 1 1 d . . . . . H12A H 0.738001 0.876992 0.482545 0.074 Uiso 1 1 calc R U . . . H12B H 0.586250 0.821085 0.484616 0.074 Uiso 1 1 calc R U . . . H12C H 0.649934 0.902659 0.412252 0.074 Uiso 1 1 calc R U . . . C13 C 0.7389(2) 0.8199(2) 0.2477(2) 0.0403(7) Uani 1 1 d . . . . . H13 H 0.669221 0.839095 0.238775 0.048 Uiso 1 1 calc R U . . . C14 C 0.8350(2) 0.8569(2) 0.1935(2) 0.0483(8) Uani 1 1 d . . . . . C18 C 0.9381(2) 0.8316(2) 0.21021(19) 0.0369(6) Uani 1 1 d . . . . . H18 H 1.006329 0.857954 0.174483 0.044 Uiso 1 1 calc R U . . . C19 C 0.9453(2) 0.76904(18) 0.27718(15) 0.0225(5) Uani 1 1 d . . . . . C20 C 1.0686(2) 0.75789(19) 0.29634(14) 0.0207(4) Uani 1 1 d . . . . . H20 H 1.050181 0.691715 0.331190 0.025 Uiso 1 1 calc R U . . . C21 C 1.1205(2) 0.7242(2) 0.20893(16) 0.0309(5) Uani 1 1 d . . . . . H21A H 1.049927 0.656265 0.165135 0.046 Uiso 1 1 calc R U . . . H21B H 1.186342 0.698822 0.224330 0.046 Uiso 1 1 calc R U . . . H21C H 1.158251 0.795857 0.181368 0.046 Uiso 1 1 calc R U . . . C22 C 1.1729(2) 0.8795(2) 0.35669(15) 0.0254(5) Uani 1 1 d . . . . . H22A H 1.192973 0.945611 0.323551 0.038 Uiso 1 1 calc R U . . . H22B H 1.250661 0.870398 0.371109 0.038 Uiso 1 1 calc R U . . . H22C H 1.141410 0.899894 0.413823 0.038 Uiso 1 1 calc R U . . . C23 C 0.53394(18) 0.32110(18) 0.27292(14) 0.0188(4) Uani 1 1 d . . . . . C24 C 0.4918(2) 0.3743(2) 0.35953(15) 0.0235(5) Uani 1 1 d . . . . . H24A H 0.539734 0.371173 0.414674 0.028 Uiso 1 1 calc R U . . . H24B H 0.515002 0.461789 0.361361 0.028 Uiso 1 1 calc R U . . . C25 C 0.3472(2) 0.3053(2) 0.36336(19) 0.0362(6) Uani 1 1 d . . . . . H25A H 0.324856 0.219918 0.368317 0.043 Uiso 1 1 calc R U . . . H25B H 0.325774 0.346236 0.418626 0.043 Uiso 1 1 calc R U . . . C26 C 0.2686(2) 0.3027(2) 0.2779(2) 0.0401(7) Uani 1 1 d . . . . . H26A H 0.175918 0.254419 0.280783 0.048 Uiso 1 1 calc R U . . . H26B H 0.284817 0.387679 0.276123 0.048 Uiso 1 1 calc R U . . . C27 C 0.3033(2) 0.2458(2) 0.19126(19) 0.0371(6) Uani 1 1 d . . . . . H27A H 0.254622 0.249546 0.136763 0.045 Uiso 1 1 calc R U . . . H27B H 0.278608 0.158146 0.189940 0.045 Uiso 1 1 calc R U . . . C28 C 0.4478(2) 0.3138(2) 0.18710(16) 0.0250(5) Uani 1 1 d . . . . . H28A H 0.469411 0.398445 0.180553 0.030 Uiso 1 1 calc R U . . . H28B H 0.467713 0.271515 0.131735 0.030 Uiso 1 1 calc R U . . . C29 C 0.52012(19) 0.19274(19) 0.27793(15) 0.0219(5) Uani 1 1 d . . . . . H29A H 0.551159 0.196944 0.341861 0.026 Uiso 1 1 calc R U . . . H29B H 0.427253 0.134695 0.265729 0.026 Uiso 1 1 calc R U . . . C30 C 0.5884(2) 0.13711(18) 0.21429(15) 0.0212(4) Uani 1 1 d . . . . . C31 C 0.4669(3) -0.0746(3) 0.1761(3) 0.0751(13) Uani 1 1 d . . . . . H31A H 0.395024 -0.117491 0.209365 0.090 Uiso 1 1 calc R U . . . H31B H 0.494566 -0.134873 0.144358 0.090 Uiso 1 1 calc R U . . . C32 C 0.4253(2) -0.0175(2) 0.10747(18) 0.0336(6) Uani 1 1 d . . . . . H32A H 0.411019 -0.065783 0.043917 0.040 Uiso 1 1 calc R U . . . H32B H 0.345517 -0.011937 0.120904 0.040 Uiso 1 1 calc R U . . . C33 C 0.73180(19) 0.21561(18) 0.22260(14) 0.0192(4) Uani 1 1 d . . . . . H33A H 0.766046 0.170091 0.179506 0.023 Uiso 1 1 calc R U . . . H33B H 0.770178 0.223791 0.285469 0.023 Uiso 1 1 calc R U . . . C34 C 0.78036(18) 0.34609(18) 0.20444(13) 0.0159(4) Uani 1 1 d . . . . . C35 C 0.7596(2) 0.34260(19) 0.10041(14) 0.0207(4) Uani 1 1 d . . . . . H35A H 0.667189 0.291158 0.076236 0.025 Uiso 1 1 calc R U . . . H35B H 0.782883 0.427092 0.092598 0.025 Uiso 1 1 calc R U . . . C36 C 0.8383(2) 0.2916(2) 0.04393(15) 0.0266(5) Uani 1 1 d . . . . . H36A H 0.823392 0.294704 -0.021106 0.032 Uiso 1 1 calc R U . . . H36B H 0.809921 0.204515 0.046656 0.032 Uiso 1 1 calc R U . . . C37 C 0.9820(2) 0.3662(2) 0.08045(16) 0.0318(5) Uani 1 1 d . . . . . H37A H 1.030274 0.327430 0.046305 0.038 Uiso 1 1 calc R U . . . H37B H 1.012931 0.450588 0.070132 0.038 Uiso 1 1 calc R U . . . C38 C 1.0077(2) 0.3728(2) 0.18260(16) 0.0272(5) Uani 1 1 d . . . . . H38A H 1.099787 0.428138 0.205445 0.033 Uiso 1 1 calc R U . . . H38B H 0.989393 0.289798 0.191625 0.033 Uiso 1 1 calc R U . . . C39 C 0.92568(19) 0.41984(19) 0.23855(14) 0.0197(4) Uani 1 1 d . . . . . H39A H 0.953195 0.507051 0.236484 0.024 Uiso 1 1 calc R U . . . H39B H 0.941714 0.416757 0.303451 0.024 Uiso 1 1 calc R U . . . C40 C 0.79017(18) 0.52261(18) 0.37739(13) 0.0154(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C15A 0.036(2) 0.019(2) 0.012(2) 0.0018(19) 0.0016(18) 0.0161(19) C16A 0.066(4) 0.042(3) 0.019(2) 0.007(2) -0.008(2) 0.026(3) C17A 0.0334(14) 0.027(3) 0.0394(16) 0.0192(19) 0.0056(12) 0.0108(17) C15B 0.025(3) 0.016(3) 0.014(3) 0.002(2) -0.003(2) 0.009(2) C16B 0.0334(14) 0.027(3) 0.0394(16) 0.0192(19) 0.0056(12) 0.0108(17) C17B 0.029(3) 0.020(3) 0.019(3) 0.006(2) -0.0006(19) 0.013(2) Cl1 0.0485(8) 0.0604(10) 0.0604(10) 0.0295(8) 0.0054(8) 0.0236(8) Cl2 0.1096(16) 0.1062(15) 0.0363(8) 0.0200(9) 0.0069(9) 0.0770(14) C41 0.053(3) 0.040(3) 0.038(3) 0.005(3) -0.005(3) 0.026(3) P1 0.0145(2) 0.0145(3) 0.0125(2) 0.00219(19) -0.00136(18) 0.0055(2) O1 0.0300(8) 0.0213(8) 0.0192(8) 0.0087(6) -0.0015(6) 0.0115(7) O2 0.0297(8) 0.0208(8) 0.0247(8) -0.0086(6) -0.0090(6) 0.0110(7) O3 0.0280(8) 0.0153(7) 0.0359(9) 0.0090(7) 0.0037(7) 0.0075(6) O4 0.0214(8) 0.0159(7) 0.0281(8) 0.0003(6) -0.0038(6) 0.0012(6) C1 0.0165(9) 0.0221(10) 0.0166(10) 0.0035(8) 0.0020(8) 0.0118(8) C2 0.0325(12) 0.0328(13) 0.0260(12) 0.0168(10) 0.0073(10) 0.0201(10) C3 0.0238(11) 0.0345(12) 0.0125(10) 0.0049(9) 0.0004(8) 0.0182(10) C4 0.0257(11) 0.0327(12) 0.0153(10) -0.0053(9) -0.0053(8) 0.0191(10) C5 0.0181(10) 0.0219(11) 0.0214(11) -0.0036(8) -0.0021(8) 0.0115(9) C6 0.0361(14) 0.0304(13) 0.0300(13) -0.0155(10) -0.0124(10) 0.0146(11) C7 0.0151(9) 0.0220(10) 0.0153(10) -0.0001(8) -0.0007(7) 0.0101(8) C8 0.0196(10) 0.0128(10) 0.0207(10) -0.0013(8) -0.0063(8) 0.0054(8) C9 0.0221(11) 0.0158(10) 0.0364(13) -0.0023(9) -0.0112(9) 0.0078(9) C10 0.0228(11) 0.0235(12) 0.0415(14) -0.0023(10) -0.0057(10) 0.0138(10) C11 0.0243(12) 0.0291(13) 0.0496(16) 0.0031(11) -0.0058(11) 0.0147(10) C12 0.0394(15) 0.0362(15) 0.065(2) -0.0154(14) -0.0098(14) 0.0229(13) C13 0.0226(12) 0.0202(12) 0.0710(19) 0.0159(12) -0.0191(12) 0.0035(10) C14 0.0258(13) 0.0320(14) 0.076(2) 0.0368(14) -0.0169(13) -0.0042(11) C18 0.0233(12) 0.0301(13) 0.0473(16) 0.0245(12) -0.0087(11) -0.0017(10) C19 0.0213(10) 0.0138(10) 0.0244(11) 0.0019(8) -0.0079(8) 0.0027(8) C20 0.0207(10) 0.0185(10) 0.0201(10) 0.0055(8) 0.0000(8) 0.0061(9) C21 0.0378(13) 0.0235(12) 0.0243(12) 0.0058(9) 0.0091(10) 0.0067(10) C22 0.0204(11) 0.0227(11) 0.0266(12) 0.0029(9) -0.0053(9) 0.0056(9) C23 0.0131(9) 0.0181(10) 0.0234(11) 0.0057(8) 0.0009(8) 0.0053(8) C24 0.0191(10) 0.0253(11) 0.0287(12) 0.0089(9) 0.0062(9) 0.0110(9) C25 0.0236(12) 0.0365(14) 0.0558(17) 0.0178(12) 0.0172(11) 0.0159(11) C26 0.0145(11) 0.0361(14) 0.0698(19) 0.0136(13) 0.0055(11) 0.0108(10) C27 0.0178(11) 0.0305(13) 0.0566(17) 0.0053(12) -0.0099(11) 0.0084(10) C28 0.0186(10) 0.0211(11) 0.0314(12) 0.0027(9) -0.0062(9) 0.0076(9) C29 0.0159(10) 0.0182(10) 0.0290(12) 0.0078(9) 0.0024(8) 0.0046(8) C30 0.0208(10) 0.0135(10) 0.0253(11) 0.0049(8) -0.0001(8) 0.0043(8) C31 0.0435(17) 0.0190(14) 0.133(3) 0.0237(17) -0.050(2) -0.0090(12) C32 0.0213(11) 0.0181(11) 0.0471(15) 0.0029(10) -0.0084(10) -0.0011(9) C33 0.0196(10) 0.0164(10) 0.0212(10) 0.0035(8) 0.0011(8) 0.0083(8) C34 0.0156(9) 0.0146(9) 0.0153(10) 0.0015(7) 0.0001(7) 0.0059(8) C35 0.0209(10) 0.0192(10) 0.0168(10) 0.0004(8) 0.0001(8) 0.0060(9) C36 0.0298(12) 0.0273(12) 0.0186(11) -0.0013(9) 0.0029(9) 0.0118(10) C37 0.0268(12) 0.0320(13) 0.0327(13) -0.0006(10) 0.0128(10) 0.0120(10) C38 0.0170(10) 0.0260(12) 0.0334(13) -0.0017(10) 0.0014(9) 0.0086(9) C39 0.0158(10) 0.0173(10) 0.0210(10) 0.0006(8) -0.0005(8) 0.0048(8) C40 0.0141(9) 0.0187(10) 0.0133(9) 0.0009(8) 0.0002(7) 0.0086(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C15A C14 1.484(5) . ? C15A C17A 1.49(3) . ? C15A C16A 1.529(8) . ? C15A H15A 1.0000 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C15B C17B 1.519(8) . ? C15B C16B 1.57(3) . ? C15B C14 1.664(6) . ? C15B H15B 1.0000 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? Cl1 C41 1.761(6) . ? Cl2 C41 1.781(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? P1 C40 1.863(2) . ? P1 C34 1.898(2) . ? P1 C23 1.901(2) . ? O1 C1 1.369(2) . ? O1 C2 1.424(2) . ? O2 C5 1.376(3) . ? O2 C6 1.433(3) . ? O3 C31 1.401(3) . ? O3 C30 1.445(2) . ? O4 C30 1.431(3) . ? O4 C32 1.435(3) . ? C1 C3 1.382(3) . ? C1 C40 1.414(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C7 1.414(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C40 1.411(3) . ? C7 C8 1.510(3) . ? C8 C19 1.408(3) . ? C8 C9 1.414(3) . ? C9 C13 1.391(3) . ? C9 C10 1.522(3) . ? C10 C12 1.535(3) . ? C10 C11 1.538(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.377(4) . ? C13 H13 0.9500 . ? C14 C18 1.391(4) . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 C20 1.522(3) . ? C20 C21 1.531(3) . ? C20 C22 1.540(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C29 1.541(3) . ? C23 C24 1.544(3) . ? C23 C28 1.556(3) . ? C24 C25 1.533(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.523(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.518(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.532(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.524(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.510(3) . ? C31 C32 1.516(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.542(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.540(3) . ? C34 C35 1.553(3) . ? C35 C36 1.529(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.531(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.523(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.529(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 C15A C17A 111.8(12) . . ? C14 C15A C16A 103.3(4) . . ? C17A C15A C16A 110.1(11) . . ? C14 C15A H15A 110.5 . . ? C17A C15A H15A 110.5 . . ? C16A C15A H15A 110.5 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15A C17A H17A 109.5 . . ? C15A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C15A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C17B C15B C16B 110.6(14) . . ? C17B C15B C14 109.8(5) . . ? C16B C15B C14 104.6(13) . . ? C17B C15B H15B 110.6 . . ? C16B C15B H15B 110.6 . . ? C14 C15B H15B 110.6 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? Cl1 C41 Cl2 111.9(3) . . ? Cl1 C41 H41A 109.2 . . ? Cl2 C41 H41A 109.2 . . ? Cl1 C41 H41B 109.2 . . ? Cl2 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C40 P1 C34 107.30(9) . . ? C40 P1 C23 107.85(9) . . ? C34 P1 C23 104.50(9) . . ? C1 O1 C2 118.48(16) . . ? C5 O2 C6 117.37(18) . . ? C31 O3 C30 108.76(18) . . ? C30 O4 C32 106.46(17) . . ? O1 C1 C3 122.96(18) . . ? O1 C1 C40 115.57(17) . . ? C3 C1 C40 121.45(19) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C4 120.3(2) . . ? C1 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.89(19) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? O2 C5 C4 123.56(18) . . ? O2 C5 C7 115.47(19) . . ? C4 C5 C7 120.97(19) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C40 C7 C5 119.31(19) . . ? C40 C7 C8 123.25(17) . . ? C5 C7 C8 117.42(18) . . ? C19 C8 C9 119.2(2) . . ? C19 C8 C7 119.85(18) . . ? C9 C8 C7 120.85(19) . . ? C13 C9 C8 118.9(2) . . ? C13 C9 C10 118.8(2) . . ? C8 C9 C10 122.2(2) . . ? C9 C10 C12 110.2(2) . . ? C9 C10 C11 112.7(2) . . ? C12 C10 C11 109.83(19) . . ? C9 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 122.8(2) . . ? C14 C13 H13 118.6 . . ? C9 C13 H13 118.6 . . ? C13 C14 C18 117.4(2) . . ? C13 C14 C15A 112.7(3) . . ? C18 C14 C15A 129.1(3) . . ? C13 C14 C15B 130.9(3) . . ? C18 C14 C15B 110.2(3) . . ? C14 C18 C19 122.6(2) . . ? C14 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C18 C19 C8 118.8(2) . . ? C18 C19 C20 118.1(2) . . ? C8 C19 C20 122.96(18) . . ? C19 C20 C21 113.23(18) . . ? C19 C20 C22 109.94(17) . . ? C21 C20 C22 109.14(18) . . ? C19 C20 H20 108.1 . . ? C21 C20 H20 108.1 . . ? C22 C20 H20 108.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C29 C23 C24 109.30(17) . . ? C29 C23 C28 111.10(17) . . ? C24 C23 C28 108.27(17) . . ? C29 C23 P1 116.64(14) . . ? C24 C23 P1 108.18(14) . . ? C28 C23 P1 102.95(14) . . ? C25 C24 C23 113.39(19) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 111.1(2) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.1(2) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 110.9(2) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C23 113.81(19) . . ? C27 C28 H28A 108.8 . . ? C23 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C23 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C23 118.47(17) . . ? C30 C29 H29A 107.7 . . ? C23 C29 H29A 107.7 . . ? C30 C29 H29B 107.7 . . ? C23 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? O4 C30 O3 104.54(15) . . ? O4 C30 C33 109.79(17) . . ? O3 C30 C33 106.89(16) . . ? O4 C30 C29 112.42(17) . . ? O3 C30 C29 107.80(16) . . ? C33 C30 C29 114.72(17) . . ? O3 C31 C32 106.4(2) . . ? O3 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O3 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.6 . . ? O4 C32 C31 103.35(18) . . ? O4 C32 H32A 111.1 . . ? C31 C32 H32A 111.1 . . ? O4 C32 H32B 111.1 . . ? C31 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? C30 C33 C34 118.16(17) . . ? C30 C33 H33A 107.8 . . ? C34 C33 H33A 107.8 . . ? C30 C33 H33B 107.8 . . ? C34 C33 H33B 107.8 . . ? H33A C33 H33B 107.1 . . ? C39 C34 C33 109.31(16) . . ? C39 C34 C35 107.62(16) . . ? C33 C34 C35 111.74(16) . . ? C39 C34 P1 107.50(13) . . ? C33 C34 P1 115.81(13) . . ? C35 C34 P1 104.44(13) . . ? C36 C35 C34 113.39(17) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 110.88(17) . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 111.09(18) . . ? C38 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? C38 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 112.24(18) . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C39 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C38 C39 C34 113.78(17) . . ? C38 C39 H39A 108.8 . . ? C34 C39 H39A 108.8 . . ? C38 C39 H39B 108.8 . . ? C34 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C7 C40 C1 118.09(18) . . ? C7 C40 P1 116.92(14) . . ? C1 C40 P1 124.96(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 O1 C1 C3 6.0(3) . . . . ? C2 O1 C1 C40 -175.69(17) . . . . ? O1 C1 C3 C4 178.91(18) . . . . ? C40 C1 C3 C4 0.7(3) . . . . ? C1 C3 C4 C5 -0.1(3) . . . . ? C6 O2 C5 C4 -1.0(3) . . . . ? C6 O2 C5 C7 178.62(19) . . . . ? C3 C4 C5 O2 178.40(19) . . . . ? C3 C4 C5 C7 -1.2(3) . . . . ? O2 C5 C7 C40 -177.71(17) . . . . ? C4 C5 C7 C40 1.9(3) . . . . ? O2 C5 C7 C8 3.8(3) . . . . ? C4 C5 C7 C8 -176.56(19) . . . . ? C40 C7 C8 C19 -92.8(2) . . . . ? C5 C7 C8 C19 85.6(2) . . . . ? C40 C7 C8 C9 90.3(2) . . . . ? C5 C7 C8 C9 -91.3(2) . . . . ? C19 C8 C9 C13 4.9(3) . . . . ? C7 C8 C9 C13 -178.2(2) . . . . ? C19 C8 C9 C10 -172.25(19) . . . . ? C7 C8 C9 C10 4.7(3) . . . . ? C13 C9 C10 C12 -73.6(3) . . . . ? C8 C9 C10 C12 103.5(2) . . . . ? C13 C9 C10 C11 49.5(3) . . . . ? C8 C9 C10 C11 -133.4(2) . . . . ? C8 C9 C13 C14 -0.8(4) . . . . ? C10 C9 C13 C14 176.4(2) . . . . ? C9 C13 C14 C18 -2.3(4) . . . . ? C9 C13 C14 C15A -173.1(3) . . . . ? C9 C13 C14 C15B 162.6(4) . . . . ? C17A C15A C14 C13 147.7(11) . . . . ? C16A C15A C14 C13 -93.9(5) . . . . ? C17A C15A C14 C18 -21.8(13) . . . . ? C16A C15A C14 C18 96.6(5) . . . . ? C17B C15B C14 C13 -0.3(7) . . . . ? C16B C15B C14 C13 118.4(13) . . . . ? C17B C15B C14 C18 165.4(5) . . . . ? C16B C15B C14 C18 -75.9(13) . . . . ? C13 C14 C18 C19 1.4(4) . . . . ? C15A C14 C18 C19 170.4(4) . . . . ? C15B C14 C18 C19 -166.5(3) . . . . ? C14 C18 C19 C8 2.6(4) . . . . ? C14 C18 C19 C20 -173.8(2) . . . . ? C9 C8 C19 C18 -5.7(3) . . . . ? C7 C8 C19 C18 177.3(2) . . . . ? C9 C8 C19 C20 170.52(18) . . . . ? C7 C8 C19 C20 -6.5(3) . . . . ? C18 C19 C20 C21 -43.9(3) . . . . ? C8 C19 C20 C21 139.8(2) . . . . ? C18 C19 C20 C22 78.4(2) . . . . ? C8 C19 C20 C22 -97.8(2) . . . . ? C29 C23 C24 C25 -68.4(2) . . . . ? C28 C23 C24 C25 52.7(2) . . . . ? P1 C23 C24 C25 163.64(16) . . . . ? C23 C24 C25 C26 -56.3(3) . . . . ? C24 C25 C26 C27 56.5(3) . . . . ? C25 C26 C27 C28 -55.9(3) . . . . ? C26 C27 C28 C23 55.3(3) . . . . ? C29 C23 C28 C27 67.6(2) . . . . ? C24 C23 C28 C27 -52.5(2) . . . . ? P1 C23 C28 C27 -166.86(16) . . . . ? C24 C23 C29 C30 -163.91(17) . . . . ? C28 C23 C29 C30 76.7(2) . . . . ? P1 C23 C29 C30 -40.9(2) . . . . ? C32 O4 C30 O3 32.8(2) . . . . ? C32 O4 C30 C33 147.15(18) . . . . ? C32 O4 C30 C29 -83.9(2) . . . . ? C31 O3 C30 O4 -22.3(3) . . . . ? C31 O3 C30 C33 -138.7(3) . . . . ? C31 O3 C30 C29 97.5(3) . . . . ? C23 C29 C30 O4 -69.9(2) . . . . ? C23 C29 C30 O3 175.37(16) . . . . ? C23 C29 C30 C33 56.4(2) . . . . ? C30 O3 C31 C32 3.8(4) . . . . ? C30 O4 C32 C31 -30.0(3) . . . . ? O3 C31 C32 O4 16.0(4) . . . . ? O4 C30 C33 C34 68.9(2) . . . . ? O3 C30 C33 C34 -178.28(16) . . . . ? C29 C30 C33 C34 -58.8(2) . . . . ? C30 C33 C34 C39 166.61(17) . . . . ? C30 C33 C34 C35 -74.4(2) . . . . ? C30 C33 C34 P1 45.0(2) . . . . ? C40 P1 C34 C39 -34.69(16) . . . . ? C23 P1 C34 C39 -149.03(14) . . . . ? C40 P1 C34 C33 87.84(15) . . . . ? C23 P1 C34 C33 -26.50(16) . . . . ? C40 P1 C34 C35 -148.83(13) . . . . ? C23 P1 C34 C35 96.83(13) . . . . ? C39 C34 C35 C36 55.1(2) . . . . ? C33 C34 C35 C36 -64.9(2) . . . . ? P1 C34 C35 C36 169.18(14) . . . . ? C34 C35 C36 C37 -57.0(2) . . . . ? C35 C36 C37 C38 54.4(3) . . . . ? C36 C37 C38 C39 -53.3(3) . . . . ? C37 C38 C39 C34 54.6(2) . . . . ? C33 C34 C39 C38 68.0(2) . . . . ? C35 C34 C39 C38 -53.5(2) . . . . ? P1 C34 C39 C38 -165.50(15) . . . . ? C5 C7 C40 C1 -1.3(3) . . . . ? C8 C7 C40 C1 177.05(18) . . . . ? C5 C7 C40 P1 176.77(15) . . . . ? C8 C7 C40 P1 -4.9(3) . . . . ? O1 C1 C40 C7 -178.29(16) . . . . ? C3 C1 C40 C7 0.0(3) . . . . ? O1 C1 C40 P1 3.8(3) . . . . ? C3 C1 C40 P1 -177.86(15) . . . . ? C34 P1 C40 C7 121.11(15) . . . . ? C23 P1 C40 C7 -126.82(15) . . . . ? C34 P1 C40 C1 -60.96(18) . . . . ? C23 P1 C40 C1 51.11(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C6 H6B O2 0.98 2.56 3.401(3) 143.6 2_776 C28 H28B O4 0.99 2.49 3.187(3) 127.3 . C29 H29A O1 0.99 2.33 3.016(3) 125.2 . C32 H32A O4 0.99 2.59 3.502(3) 153.9 2_655 C33 H33B O1 0.99 2.36 3.058(3) 127.0 . C35 H35A O4 0.99 2.41 3.082(3) 124.4 . _refine_diff_density_max 0.673 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.052 _shelx_res_file ; TITL XRAY5686_0m_a.res in P-1 XRAY5686_0m_a.res created by SHELXL-2016/6 at 12:38:09 on 05-Mar-2019 CELL 0.71073 11.6617 12.3698 14.9507 100.424 92.731 115.736 ZERR 2.000 0.0018 0.0019 0.0023 0.002 0.002 0.002 LATT 1 SFAC C H O P Cl UNIT 81 120 8 2 2 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.07 0.10 0.40 EADP C17A C16B EQIV $1 -x+2, -y+2, -z+1 HTAB C6 O2_$1 HTAB C28 O4 HTAB C29 O1 EQIV $2 -x+1, -y, -z HTAB C32 O4_$2 HTAB C33 O1 HTAB C35 O4 WPDB CONF TEMP -173.0 WGHT 0.100000 0.699620 FVAR 0.56177 0.54280 PART 1 MOLE 10 C15A 1 0.821066 0.936594 0.134981 21.00000 0.03602 0.01923 = 0.01241 0.00181 0.00157 0.01606 AFIX 13 H15A 2 0.770271 0.978311 0.162665 21.00000 -1.20000 AFIX 0 C16A 1 0.746902 0.845602 0.044508 21.00000 0.06589 0.04246 = 0.01887 0.00665 -0.00816 0.02564 AFIX 137 H16A 2 0.792706 0.798088 0.022235 21.00000 -1.50000 H16B 2 0.739778 0.890885 -0.001168 21.00000 -1.50000 H16C 2 0.660676 0.789498 0.054452 21.00000 -1.50000 AFIX 0 C17A 1 0.948083 1.029105 0.119431 21.00000 0.03343 0.02714 = 0.03941 0.01922 0.00565 0.01082 AFIX 137 H17A 2 0.997741 1.082694 0.178486 21.00000 -1.50000 H17B 2 0.935038 1.078863 0.079672 21.00000 -1.50000 H17C 2 0.995115 0.986681 0.089896 21.00000 -1.50000 PART 2 AFIX 0 C15B 1 0.838363 0.901440 0.094677 -21.00000 0.02530 0.01616 = 0.01374 0.00150 -0.00257 0.00875 AFIX 13 H15B 2 0.859210 0.848230 0.046240 -21.00000 -1.20000 AFIX 0 C16B 1 0.947746 1.037526 0.116930 -21.00000 0.03343 0.02714 = 0.03941 0.01922 0.00565 0.01082 AFIX 137 H16D 2 0.949275 1.073608 0.063526 -21.00000 -1.50000 H16E 2 1.030873 1.038070 0.131397 -21.00000 -1.50000 H16F 2 0.931385 1.085869 0.169761 -21.00000 -1.50000 AFIX 0 C17B 1 0.709752 0.896927 0.064747 -21.00000 0.02940 0.02003 = 0.01895 0.00584 -0.00060 0.01337 AFIX 137 H17D 2 0.693338 0.953364 0.111246 -21.00000 -1.50000 H17E 2 0.641299 0.812921 0.057772 -21.00000 -1.50000 H17F 2 0.711640 0.921586 0.005910 -21.00000 -1.50000 PART -1 AFIX 0 CL1 5 0.458805 0.534751 0.030131 10.50000 0.04852 0.06036 = 0.06037 0.02947 0.00539 0.02359 CL2 5 0.636341 0.461023 -0.065534 10.50000 0.10962 0.10619 = 0.03631 0.02000 0.00689 0.07697 C41 1 0.613447 0.542374 0.037544 10.50000 0.05305 0.04000 = 0.03842 0.00454 -0.00530 0.02585 AFIX 23 H41A 2 0.626092 0.507107 0.089385 10.50000 -1.20000 H41B 2 0.678764 0.629680 0.050316 10.50000 -1.20000 PART 0 AFIX 0 P1 4 0.699838 0.440272 0.260012 11.00000 0.01451 0.01454 = 0.01252 0.00219 -0.00136 0.00554 O1 3 0.752351 0.339036 0.423347 11.00000 0.02997 0.02131 = 0.01922 0.00870 -0.00151 0.01151 O2 3 0.955066 0.844995 0.502094 11.00000 0.02966 0.02079 = 0.02471 -0.00856 -0.00904 0.01101 O3 3 0.569526 0.022496 0.237272 11.00000 0.02800 0.01527 = 0.03593 0.00904 0.00371 0.00748 O4 3 0.531801 0.102631 0.120145 11.00000 0.02139 0.01585 = 0.02808 0.00034 -0.00375 0.00120 C1 1 0.804238 0.464782 0.447678 11.00000 0.01651 0.02210 = 0.01657 0.00348 0.00198 0.01185 C2 1 0.755163 0.274321 0.492439 11.00000 0.03254 0.03278 = 0.02596 0.01677 0.00729 0.02014 AFIX 137 H2A 2 0.844631 0.299972 0.517314 11.00000 -1.50000 H2B 2 0.712964 0.185590 0.465642 11.00000 -1.50000 H2C 2 0.709827 0.292866 0.541912 11.00000 -1.50000 AFIX 0 C3 1 0.869363 0.532434 0.534070 11.00000 0.02378 0.03450 = 0.01247 0.00492 0.00044 0.01818 AFIX 43 H3 2 0.878343 0.491493 0.579934 11.00000 -1.20000 AFIX 0 C4 1 0.921581 0.659631 0.554066 11.00000 0.02570 0.03271 = 0.01534 -0.00529 -0.00527 0.01906 AFIX 43 H4 2 0.966144 0.705869 0.613578 11.00000 -1.20000 AFIX 0 C5 1 0.908769 0.719278 0.487269 11.00000 0.01808 0.02187 = 0.02143 -0.00362 -0.00206 0.01150 C6 1 1.017981 0.916272 0.592441 11.00000 0.03613 0.03036 = 0.03000 -0.01549 -0.01244 0.01460 AFIX 137 H6A 2 0.958288 0.890081 0.637026 11.00000 -1.50000 H6B 2 1.045334 1.003682 0.594297 11.00000 -1.50000 H6C 2 1.093354 0.903803 0.607793 11.00000 -1.50000 AFIX 0 C7 1 0.844854 0.652373 0.397765 11.00000 0.01505 0.02198 = 0.01529 -0.00006 -0.00071 0.01006 C8 1 0.841964 0.725334 0.327644 11.00000 0.01959 0.01282 = 0.02066 -0.00134 -0.00625 0.00537 C9 1 0.739494 0.755635 0.314883 11.00000 0.02212 0.01578 = 0.03636 -0.00227 -0.01118 0.00775 C10 1 0.633042 0.725560 0.375073 11.00000 0.02277 0.02349 = 0.04152 -0.00228 -0.00569 0.01382 AFIX 13 H10 2 0.637866 0.665564 0.409985 11.00000 -1.20000 AFIX 0 C11 1 0.498145 0.666487 0.319078 11.00000 0.02431 0.02908 = 0.04961 0.00307 -0.00579 0.01472 AFIX 137 H11A 2 0.485307 0.728669 0.293558 11.00000 -1.50000 H11B 2 0.433174 0.633767 0.359098 11.00000 -1.50000 H11C 2 0.489981 0.599375 0.268889 11.00000 -1.50000 AFIX 0 C12 1 0.653672 0.842115 0.444940 11.00000 0.03943 0.03616 = 0.06538 -0.01535 -0.00983 0.02288 AFIX 137 H12A 2 0.738001 0.876992 0.482545 11.00000 -1.50000 H12B 2 0.586250 0.821085 0.484616 11.00000 -1.50000 H12C 2 0.649934 0.902659 0.412252 11.00000 -1.50000 AFIX 0 C13 1 0.738879 0.819908 0.247679 11.00000 0.02256 0.02024 = 0.07103 0.01586 -0.01905 0.00354 AFIX 43 H13 2 0.669221 0.839095 0.238775 11.00000 -1.20000 AFIX 0 C14 1 0.834974 0.856898 0.193513 11.00000 0.02579 0.03196 = 0.07597 0.03685 -0.01692 -0.00418 C18 1 0.938129 0.831550 0.210208 11.00000 0.02335 0.03006 = 0.04733 0.02445 -0.00868 -0.00171 AFIX 43 H18 2 1.006329 0.857954 0.174483 11.00000 -1.20000 AFIX 0 C19 1 0.945345 0.769039 0.277180 11.00000 0.02126 0.01377 = 0.02444 0.00193 -0.00792 0.00266 C20 1 1.068635 0.757891 0.296336 11.00000 0.02065 0.01853 = 0.02013 0.00546 0.00000 0.00611 AFIX 13 H20 2 1.050181 0.691715 0.331190 11.00000 -1.20000 AFIX 0 C21 1 1.120450 0.724176 0.208929 11.00000 0.03783 0.02345 = 0.02433 0.00581 0.00914 0.00669 AFIX 137 H21A 2 1.049927 0.656265 0.165135 11.00000 -1.50000 H21B 2 1.186342 0.698822 0.224330 11.00000 -1.50000 H21C 2 1.158251 0.795857 0.181368 11.00000 -1.50000 AFIX 0 C22 1 1.172897 0.879503 0.356691 11.00000 0.02038 0.02270 = 0.02660 0.00288 -0.00534 0.00562 AFIX 137 H22A 2 1.192973 0.945611 0.323551 11.00000 -1.50000 H22B 2 1.250661 0.870398 0.371109 11.00000 -1.50000 H22C 2 1.141410 0.899894 0.413823 11.00000 -1.50000 AFIX 0 C23 1 0.533936 0.321098 0.272922 11.00000 0.01311 0.01807 = 0.02343 0.00566 0.00092 0.00531 C24 1 0.491767 0.374265 0.359530 11.00000 0.01913 0.02528 = 0.02868 0.00895 0.00622 0.01100 AFIX 23 H24A 2 0.539734 0.371173 0.414674 11.00000 -1.20000 H24B 2 0.515002 0.461789 0.361361 11.00000 -1.20000 AFIX 0 C25 1 0.347247 0.305312 0.363361 11.00000 0.02356 0.03647 = 0.05577 0.01779 0.01721 0.01590 AFIX 23 H25A 2 0.324856 0.219918 0.368317 11.00000 -1.20000 H25B 2 0.325774 0.346236 0.418626 11.00000 -1.20000 AFIX 0 C26 1 0.268623 0.302685 0.277930 11.00000 0.01446 0.03611 = 0.06984 0.01356 0.00549 0.01078 AFIX 23 H26A 2 0.175918 0.254419 0.280783 11.00000 -1.20000 H26B 2 0.284817 0.387679 0.276123 11.00000 -1.20000 AFIX 0 C27 1 0.303278 0.245821 0.191257 11.00000 0.01784 0.03051 = 0.05663 0.00531 -0.00991 0.00836 AFIX 23 H27A 2 0.254622 0.249546 0.136763 11.00000 -1.20000 H27B 2 0.278608 0.158146 0.189940 11.00000 -1.20000 AFIX 0 C28 1 0.447756 0.313775 0.187103 11.00000 0.01860 0.02106 = 0.03143 0.00266 -0.00623 0.00758 AFIX 23 H28A 2 0.469411 0.398445 0.180553 11.00000 -1.20000 H28B 2 0.467713 0.271515 0.131735 11.00000 -1.20000 AFIX 0 C29 1 0.520119 0.192735 0.277926 11.00000 0.01595 0.01823 = 0.02899 0.00782 0.00237 0.00458 AFIX 23 H29A 2 0.551159 0.196944 0.341861 11.00000 -1.20000 H29B 2 0.427253 0.134695 0.265729 11.00000 -1.20000 AFIX 0 C30 1 0.588408 0.137112 0.214290 11.00000 0.02080 0.01349 = 0.02527 0.00485 -0.00007 0.00427 C31 1 0.466891 -0.074633 0.176097 11.00000 0.04346 0.01900 = 0.13330 0.02373 -0.04951 -0.00897 AFIX 23 H31A 2 0.395024 -0.117491 0.209365 11.00000 -1.20000 H31B 2 0.494566 -0.134873 0.144358 11.00000 -1.20000 AFIX 0 C32 1 0.425331 -0.017524 0.107469 11.00000 0.02129 0.01809 = 0.04714 0.00288 -0.00836 -0.00110 AFIX 23 H32A 2 0.411019 -0.065783 0.043917 11.00000 -1.20000 H32B 2 0.345517 -0.011937 0.120904 11.00000 -1.20000 AFIX 0 C33 1 0.731803 0.215606 0.222602 11.00000 0.01958 0.01643 = 0.02117 0.00352 0.00111 0.00826 AFIX 23 H33A 2 0.766046 0.170091 0.179506 11.00000 -1.20000 H33B 2 0.770178 0.223791 0.285469 11.00000 -1.20000 AFIX 0 C34 1 0.780358 0.346089 0.204439 11.00000 0.01564 0.01463 = 0.01532 0.00154 0.00014 0.00588 C35 1 0.759550 0.342605 0.100406 11.00000 0.02086 0.01920 = 0.01678 0.00036 0.00015 0.00598 AFIX 23 H35A 2 0.667189 0.291158 0.076236 11.00000 -1.20000 H35B 2 0.782883 0.427092 0.092598 11.00000 -1.20000 AFIX 0 C36 1 0.838346 0.291646 0.043928 11.00000 0.02982 0.02726 = 0.01862 -0.00134 0.00286 0.01176 AFIX 23 H36A 2 0.823392 0.294704 -0.021106 11.00000 -1.20000 H36B 2 0.809921 0.204515 0.046656 11.00000 -1.20000 AFIX 0 C37 1 0.982034 0.366202 0.080446 11.00000 0.02682 0.03198 = 0.03272 -0.00062 0.01280 0.01201 AFIX 23 H37A 2 1.030274 0.327430 0.046305 11.00000 -1.20000 H37B 2 1.012931 0.450588 0.070132 11.00000 -1.20000 AFIX 0 C38 1 1.007725 0.372792 0.182602 11.00000 0.01702 0.02604 = 0.03340 -0.00165 0.00137 0.00858 AFIX 23 H38A 2 1.099787 0.428138 0.205445 11.00000 -1.20000 H38B 2 0.989393 0.289798 0.191625 11.00000 -1.20000 AFIX 0 C39 1 0.925684 0.419840 0.238554 11.00000 0.01581 0.01729 = 0.02101 0.00060 -0.00051 0.00481 AFIX 23 H39A 2 0.953195 0.507051 0.236484 11.00000 -1.20000 H39B 2 0.941714 0.416757 0.303451 11.00000 -1.20000 AFIX 0 C40 1 0.790165 0.522605 0.377391 11.00000 0.01405 0.01866 = 0.01335 0.00089 0.00020 0.00856 HKLF 4 REM XRAY5686_0m_a.res in P-1 REM R1 = 0.0495 for 5781 Fo > 4sig(Fo) and 0.0830 for all 8299 data REM 465 parameters refined using 0 restraints END WGHT 0.0475 0.8788 REM Highest difference peak 0.673, deepest hole -0.559, 1-sigma level 0.052 Q1 1 0.6801 0.5441 -0.0372 11.00000 0.05 0.67 Q2 1 0.7390 0.3816 0.2298 11.00000 0.05 0.33 Q3 1 0.6946 0.4144 -0.1056 11.00000 0.05 0.32 Q4 1 0.4384 -0.1442 0.1857 11.00000 0.05 0.32 Q5 1 0.7447 0.4700 0.3285 11.00000 0.05 0.30 Q6 1 0.8476 0.8184 0.1682 11.00000 0.05 0.29 Q7 1 0.8376 0.8582 0.1435 11.00000 0.05 0.29 Q8 1 0.6947 0.5045 0.2009 11.00000 0.05 0.27 Q9 1 0.6128 0.3779 0.2761 11.00000 0.05 0.26 Q10 1 0.8476 0.6942 0.3646 11.00000 0.05 0.24 Q11 1 0.3770 -0.0783 0.2438 11.00000 0.05 0.23 Q12 1 0.7442 0.2748 0.2142 11.00000 0.05 0.23 Q13 1 0.6589 0.1824 0.2204 11.00000 0.05 0.23 Q14 1 1.0075 0.7537 0.2791 11.00000 0.05 0.23 Q15 1 0.8834 0.6936 0.4377 11.00000 0.05 0.23 Q16 1 0.7665 0.3388 0.1518 11.00000 0.05 0.23 Q17 1 0.4983 -0.0652 0.1446 11.00000 0.05 0.23 Q18 1 1.1207 0.8209 0.3224 11.00000 0.05 0.22 Q19 1 0.7025 0.5917 0.0382 11.00000 0.05 0.21 Q20 1 0.5428 0.1640 0.2340 11.00000 0.05 0.21 ; _shelx_res_checksum 64487 _shelx_hkl_file ; -1 0 0 0.50 0.70 1 0 0 0.50 0.80 1 0 0 1.00 0.70 1 0 0 0.90 0.60 1 0 0 -0.20 0.80 -2 0 0 77.79 3.10 2 0 0 78.69 3.40 2 0 0 78.89 3.70 2 0 0 79.29 2.90 -3 0 0 149.88 4.80 3 0 0 144.99 5.40 3 0 0 151.58 5.10 3 0 0 146.39 4.30 -4 0 0 1583.34 21.30 4 0 0 1621.04 20.10 4 0 0 1572.04 22.10 4 0 0 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20.10 4.90 1 7 0 15.40 3.40 1 7 0 21.70 4.20 -2 -7 0 260.07 11.50 2 7 0 274.37 10.30 2 7 0 276.67 9.20 -3 -7 0 0.30 4.30 3 7 0 0.80 3.40 3 7 0 3.30 3.20 -4 -7 0 341.27 13.70 4 7 0 350.16 11.40 4 7 0 356.36 13.50 -5 -7 0 5.90 4.90 5 7 0 7.10 3.80 5 7 0 -2.60 4.50 -6 -7 0 38.70 6.90 6 7 0 44.80 6.20 6 7 0 41.70 7.30 -7 -7 0 81.99 9.10 7 7 0 67.79 8.60 7 7 0 98.29 12.10 8 7 0 40.20 7.70 14 -8 0 5.50 6.70 -14 8 0 12.90 6.70 13 -8 0 -2.40 5.60 -13 8 0 6.50 5.50 12 -8 0 166.68 12.50 -12 8 0 165.48 11.20 11 -8 0 4.50 5.50 -11 8 0 -0.80 3.70 -11 8 0 -1.30 4.00 10 -8 0 83.59 8.60 -10 8 0 77.19 6.70 -10 8 0 80.59 7.20 9 -8 0 263.07 12.80 -9 8 0 269.87 10.50 -9 8 0 237.18 9.80 8 -8 0 44.30 6.40 -8 8 0 43.20 5.10 -8 8 0 39.90 5.00 7 -8 0 56.69 5.70 7 -8 0 60.69 6.80 -7 8 0 60.19 5.60 -7 8 0 57.09 5.40 6 -8 0 10.40 4.20 6 -8 0 0.20 3.80 -6 8 0 -2.50 3.10 -6 8 0 -0.30 2.80 5 -8 0 570.34 14.10 5 -8 0 568.54 14.30 -5 8 0 575.64 13.70 -5 8 0 568.44 12.30 4 -8 0 0.50 3.90 4 -8 0 -2.00 3.40 -4 8 0 -1.30 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137.69 7.60 -7 9 0 154.28 8.40 6 -9 0 90.89 8.00 6 -9 0 106.49 8.30 -6 9 0 87.09 7.00 -6 9 0 100.99 6.60 5 -9 0 186.28 9.20 5 -9 0 184.18 10.00 -5 9 0 175.38 7.60 -5 9 0 187.08 8.80 4 -9 0 332.27 12.60 4 -9 0 317.67 10.80 -4 9 0 333.67 11.20 -4 9 0 323.67 9.50 3 -9 0 13.00 4.10 3 -9 0 7.60 4.60 -3 9 0 7.80 3.30 -3 9 0 8.50 4.00 2 -9 0 3.60 3.50 2 -9 0 6.40 4.70 -2 9 0 8.10 4.30 -2 9 0 5.70 3.00 1 -9 0 95.39 8.90 -1 9 0 106.39 6.30 -1 9 0 100.89 8.10 0 -9 0 146.99 10.30 0 9 0 125.19 8.90 0 9 0 119.29 6.80 -1 -9 0 110.69 9.70 1 9 0 122.69 9.10 -2 -9 0 135.89 10.70 2 9 0 145.59 10.10 -3 -9 0 0.30 5.20 3 9 0 1.10 4.60 -4 -9 0 -0.40 5.10 4 9 0 0.80 5.20 -5 -9 0 -0.50 5.50 5 9 0 9.40 5.50 -6 -9 0 9.40 6.20 6 9 0 -4.10 5.40 -7 -9 0 3.50 6.90 14 -10 0 7.60 7.50 -14 10 0 -0.20 5.70 13 -10 0 23.30 8.10 -13 10 0 5.10 5.20 12 -10 0 15.40 7.30 -12 10 0 38.20 6.60 11 -10 0 107.49 10.50 -11 10 0 113.19 9.30 -11 10 0 94.19 11.90 10 -10 0 -11.50 5.10 -10 10 0 0.80 4.20 -10 10 0 -1.70 3.80 9 -10 0 101.89 9.30 -9 10 0 102.09 7.80 -9 10 0 95.79 7.90 8 -10 0 -2.00 5.00 -8 10 0 -2.60 3.20 -8 10 0 3.30 3.80 7 -10 0 32.70 5.90 7 -10 0 31.40 6.00 -7 10 0 27.00 5.20 -7 10 0 26.40 4.50 6 -10 0 22.50 5.70 6 -10 0 17.80 5.00 -6 10 0 9.30 3.60 -6 10 0 14.70 4.70 5 -10 0 12.90 5.30 5 -10 0 11.90 4.70 -5 10 0 15.50 4.60 -5 10 0 13.40 3.80 4 -10 0 20.90 5.80 4 -10 0 21.00 5.00 -4 10 0 13.90 4.70 -4 10 0 15.50 3.80 3 -10 0 108.79 9.30 -3 10 0 90.89 7.50 -3 10 0 87.09 7.80 2 -10 0 100.99 9.20 -2 10 0 116.99 8.70 1 -10 0 351.06 15.10 -1 10 0 350.36 13.30 0 -10 0 193.28 12.90 0 10 0 182.98 10.70 -1 -10 0 23.80 6.80 1 10 0 48.50 7.20 -2 -10 0 23.20 6.90 2 10 0 22.00 6.10 -3 -10 0 31.70 7.70 3 10 0 26.50 6.60 -4 -10 0 -5.00 5.80 4 10 0 -6.50 4.90 -5 -10 0 -2.60 6.10 5 10 0 1.30 5.80 14 -11 0 27.30 8.70 -14 11 0 34.70 7.50 13 -11 0 11.30 7.80 -13 11 0 -1.00 5.00 12 -11 0 47.00 8.60 -12 11 0 57.39 7.60 11 -11 0 119.59 11.00 -11 11 0 125.19 9.70 10 -11 0 121.69 10.80 -10 11 0 134.69 9.20 -10 11 0 119.09 9.00 9 -11 0 10.80 5.60 -9 11 0 1.20 3.70 -9 11 0 4.30 4.30 8 -11 0 12.40 5.90 -8 11 0 9.40 4.70 -8 11 0 16.50 4.20 7 -11 0 10.80 5.30 7 -11 0 3.90 5.20 -7 11 0 6.90 4.70 -7 11 0 11.70 3.80 6 -11 0 56.19 7.40 6 -11 0 54.19 6.60 -6 11 0 60.09 6.90 5 -11 0 -1.10 4.90 5 -11 0 3.30 4.50 -5 11 0 0.70 4.30 4 -11 0 75.49 8.60 -4 11 0 79.49 7.60 3 -11 0 115.39 10.40 -3 11 0 113.29 9.00 2 -11 0 11.20 6.10 -2 11 0 20.00 5.70 1 -11 0 2.20 5.50 -1 11 0 -5.90 4.50 0 -11 0 89.99 10.00 0 11 0 108.89 9.60 -1 -11 0 6.10 6.50 1 11 0 8.90 5.30 -2 -11 0 0.80 6.00 2 11 0 2.70 5.20 -3 -11 0 40.90 9.10 3 11 0 44.70 8.40 -4 -11 0 6.60 7.50 4 11 0 5.30 6.10 13 -12 0 42.40 9.40 -13 12 0 49.20 7.90 12 -12 0 22.50 7.70 -12 12 0 24.60 6.10 11 -12 0 68.09 9.50 -11 12 0 54.69 7.20 10 -12 0 175.88 13.10 -10 12 0 201.88 11.40 9 -12 0 6.80 5.90 -9 12 0 0.50 4.80 8 -12 0 -0.20 5.50 -8 12 0 1.80 4.30 7 -12 0 148.99 10.60 7 -12 0 150.88 11.20 -7 12 0 161.98 10.50 6 -12 0 24.90 6.60 -6 12 0 23.50 5.80 5 -12 0 189.68 12.50 -5 12 0 199.48 11.30 4 -12 0 15.00 6.20 -4 12 0 8.10 5.30 3 -12 0 30.50 7.70 -3 12 0 20.70 5.90 2 -12 0 14.10 7.10 -2 12 0 11.10 5.40 1 -12 0 58.39 9.50 -1 12 0 62.69 8.00 0 -12 0 -7.10 6.10 0 12 0 -7.00 4.90 -1 -12 0 131.39 13.50 1 12 0 138.29 12.10 -2 -12 0 -1.80 6.80 2 12 0 -3.10 5.40 -3 -12 0 0.50 7.30 3 12 0 2.20 6.40 12 -13 0 61.89 10.10 11 -13 0 63.69 9.50 10 -13 0 1.60 5.90 -10 13 0 15.80 7.00 9 -13 0 17.20 6.60 -9 13 0 16.10 5.70 8 -13 0 32.30 7.20 -8 13 0 33.90 6.70 7 -13 0 -8.30 5.40 -7 13 0 -2.90 4.80 6 -13 0 -0.80 5.80 -6 13 0 -4.70 4.90 5 -13 0 4.50 6.40 -5 13 0 0.00 5.30 4 -13 0 79.89 10.20 -4 13 0 92.09 9.00 3 -13 0 20.20 7.60 -3 13 0 15.70 6.10 2 -13 0 11.60 7.40 -2 13 0 22.80 6.50 1 -13 0 36.50 8.80 -1 13 0 38.30 7.40 0 -13 0 -4.10 6.90 0 13 0 4.30 6.00 -1 -13 0 67.09 11.10 1 13 0 55.19 9.00 11 -14 0 50.39 8.80 10 -14 0 0.20 6.00 -9 14 0 54.69 8.00 -8 14 0 24.70 6.30 7 -14 0 2.40 6.60 -7 14 0 -3.10 5.30 6 -14 0 22.20 7.60 -6 14 0 13.60 6.30 5 -14 0 49.50 9.40 -5 14 0 51.39 8.10 4 -14 0 -12.80 6.20 -4 14 0 14.70 6.60 3 -14 0 -2.70 6.90 -3 14 0 -3.70 5.50 2 -14 0 8.60 7.60 -2 14 0 3.40 5.80 1 -14 0 4.70 7.50 -1 14 0 5.90 6.50 -9 15 0 8.40 6.30 -8 15 0 39.50 7.90 7 -15 0 -2.00 6.70 -7 15 0 6.10 5.90 6 -15 0 -9.90 6.80 -6 15 0 2.70 6.00 5 -15 0 -1.20 6.70 -5 15 0 -2.30 5.40 4 -15 0 -7.50 7.00 -4 15 0 -7.80 5.60 3 -15 0 37.80 9.70 -3 15 0 50.59 8.80 -3 15 -1 -0.10 6.10 3 -15 1 -5.70 6.80 -4 15 -1 28.40 7.40 4 -15 1 12.90 8.30 -5 15 -1 3.50 6.00 5 -15 1 -9.30 6.60 -6 15 -1 28.90 7.50 6 -15 1 22.50 8.10 -7 15 -1 95.49 10.50 7 -15 1 65.89 10.20 -8 15 -1 -0.20 5.50 -9 15 -1 28.30 7.20 -10 15 -1 7.40 6.40 0 14 -1 15.70 7.30 0 -14 1 0.50 7.40 -1 14 -1 20.40 7.00 1 -14 1 6.80 7.90 -2 14 -1 14.10 6.50 2 -14 1 1.30 7.30 -3 14 -1 9.10 6.40 3 -14 1 -0.10 6.60 -4 14 -1 23.50 6.50 4 -14 1 16.10 7.60 -5 14 -1 39.50 7.80 5 -14 1 20.80 7.60 -6 14 -1 91.79 9.80 6 -14 1 82.19 10.40 -7 14 -1 85.89 9.40 7 -14 1 63.29 9.50 -8 14 -1 20.30 6.20 -9 14 -1 70.79 8.60 9 -14 1 75.59 9.40 -10 14 -1 83.69 9.20 10 -14 1 75.19 9.80 11 -14 1 6.70 6.60 12 -14 1 21.20 8.00 -2 -13 1 -0.40 7.60 1 13 -1 -3.70 5.70 -1 -13 1 -1.70 7.40 0 13 -1 17.00 6.50 0 -13 1 20.40 7.90 -1 13 -1 66.89 9.00 1 -13 1 55.39 9.60 -2 13 -1 76.19 9.60 2 -13 1 87.99 10.70 -3 13 -1 136.09 10.90 3 -13 1 123.59 11.80 -4 13 -1 25.40 6.70 4 -13 1 25.00 7.30 -5 13 -1 2.70 5.10 5 -13 1 1.30 5.70 -6 13 -1 2.00 5.50 6 -13 1 0.20 5.70 -7 13 -1 5.70 5.20 7 -13 1 5.80 5.80 7 -13 1 8.90 7.30 -8 13 -1 49.40 7.30 8 -13 1 45.10 7.90 -9 13 -1 -0.10 4.80 9 -13 1 4.10 6.40 -10 13 -1 70.29 8.50 10 -13 1 82.59 9.80 -11 13 -1 75.69 10.00 11 -13 1 68.79 9.80 12 -13 1 69.69 10.50 13 -13 1 123.99 12.50 3 12 -1 4.50 6.30 -3 -12 1 14.70 8.00 2 12 -1 17.30 6.60 -2 -12 1 24.80 8.30 1 12 -1 9.20 6.10 -1 -12 1 16.70 7.70 0 12 -1 19.80 6.40 0 -12 1 19.90 7.30 -1 12 -1 -2.70 4.90 1 -12 1 3.60 6.00 -2 12 -1 3.70 5.00 2 -12 1 5.00 6.00 -3 12 -1 61.69 7.90 3 -12 1 64.59 8.60 -4 12 -1 94.99 8.80 4 -12 1 92.39 9.60 -5 12 -1 13.20 5.00 5 -12 1 5.90 5.60 -6 12 -1 11.70 5.10 6 -12 1 13.70 6.10 6 -12 1 13.10 5.40 -7 12 -1 32.30 6.30 7 -12 1 58.19 7.80 7 -12 1 42.70 6.90 -8 12 -1 137.59 10.00 8 -12 1 151.18 11.20 -9 12 -1 145.79 10.10 9 -12 1 134.59 11.30 -10 12 -1 168.48 11.00 10 -12 1 193.68 13.60 -11 12 -1 71.49 8.20 11 -12 1 86.79 10.20 12 -12 1 -3.60 6.20 -13 12 -1 6.20 6.50 13 -12 1 5.10 7.30 4 11 -1 -5.40 5.50 -4 -11 1 -1.40 6.80 3 11 -1 8.20 5.60 -3 -11 1 11.90 6.80 2 11 -1 166.38 11.70 -2 -11 1 185.38 14.30 1 11 -1 61.79 8.20 -1 -11 1 47.60 8.80 0 11 -1 10.90 5.10 0 -11 1 5.40 5.60 -1 11 -1 10.10 5.00 1 -11 1 8.80 5.90 -2 11 -1 181.18 10.60 2 -11 1 202.88 12.80 -3 11 -1 108.79 9.20 3 -11 1 100.39 9.60 -4 11 -1 45.30 6.50 4 -11 1 53.09 6.80 4 -11 1 66.09 7.80 -5 11 -1 2.10 4.40 5 -11 1 4.50 4.80 5 -11 1 3.10 5.10 -6 11 -1 10.70 5.00 6 -11 1 8.40 5.30 6 -11 1 10.10 5.20 -7 11 -1 14.20 4.90 7 -11 1 18.70 5.90 7 -11 1 13.40 5.20 -8 11 -1 57.99 6.70 -8 11 -1 47.40 7.10 8 -11 1 58.89 7.50 -9 11 -1 48.90 5.80 -9 11 -1 41.50 6.30 9 -11 1 38.00 7.40 -10 11 -1 153.98 9.40 -10 11 -1 168.18 10.40 10 -11 1 179.38 12.90 -11 11 -1 35.30 6.00 -11 11 -1 29.90 6.20 11 -11 1 47.00 8.10 -12 11 -1 16.00 5.30 12 -11 1 20.30 7.20 -13 11 -1 104.49 10.10 13 -11 1 92.59 10.90 -14 11 -1 31.50 7.40 14 -11 1 33.50 9.30 6 10 -1 10.70 6.80 -6 -10 1 -2.00 6.10 5 10 -1 0.50 5.50 -5 -10 1 10.60 6.70 4 10 -1 -4.40 5.20 -4 -10 1 -7.50 5.20 3 10 -1 80.09 8.80 -3 -10 1 85.59 10.10 2 10 -1 73.99 8.20 -2 -10 1 78.59 9.30 1 10 -1 9.60 5.10 -1 -10 1 9.90 5.70 0 10 -1 291.27 12.70 0 -10 1 331.37 14.40 -1 10 -1 152.28 9.80 1 -10 1 156.08 10.80 -2 10 -1 12.20 5.00 2 -10 1 0.10 4.60 -3 10 -1 67.29 6.80 3 -10 1 85.79 6.80 3 -10 1 75.79 8.10 -4 10 -1 31.40 5.60 4 -10 1 33.70 5.40 4 -10 1 28.90 6.10 -5 10 -1 148.99 7.30 -5 10 -1 134.19 9.10 5 -10 1 167.18 9.60 5 -10 1 140.39 9.60 -6 10 -1 162.08 9.50 -6 10 -1 154.68 7.60 6 -10 1 161.08 9.90 6 -10 1 175.48 10.40 -7 10 -1 72.29 5.90 -7 10 -1 68.09 6.90 7 -10 1 54.79 6.80 7 -10 1 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29.10 5.10 -3 9 3 47.80 5.40 2 -9 -3 2.60 5.00 -2 9 3 -3.60 3.40 -2 9 3 -6.60 3.20 1 -9 -3 64.39 8.20 -1 9 3 69.29 6.70 -1 9 3 62.49 6.20 0 -9 -3 5.70 5.80 0 9 3 21.20 5.50 0 9 3 24.40 4.70 -1 -9 -3 127.09 11.00 1 9 3 123.29 8.30 1 9 3 120.79 9.50 -2 -9 -3 63.09 8.90 2 9 3 93.69 9.40 2 9 3 81.29 7.50 -3 -9 -3 0.20 5.80 3 9 3 11.50 4.30 3 9 3 4.60 5.40 -4 -9 -3 5.40 6.30 4 9 3 9.20 4.70 4 9 3 11.70 6.40 -5 -9 -3 14.30 7.10 5 9 3 10.30 6.40 -6 -9 -3 0.70 6.80 6 9 3 8.00 6.60 14 -10 -3 13.80 8.00 -14 10 3 15.20 6.80 13 -10 -3 11.70 7.00 -13 10 3 4.00 5.80 12 -10 -3 26.10 7.80 -12 10 3 13.20 5.80 11 -10 -3 179.38 13.10 -11 10 3 167.18 10.90 10 -10 -3 73.09 8.80 -10 10 3 74.19 7.90 9 -10 -3 44.20 7.20 -9 10 3 40.80 6.10 8 -10 -3 76.89 8.00 8 -10 -3 63.99 7.60 -8 10 3 73.89 7.20 7 -10 -3 24.20 6.50 7 -10 -3 38.40 6.10 -7 10 3 42.00 5.30 -7 10 3 40.30 5.70 6 -10 -3 96.79 8.00 6 -10 -3 80.69 8.70 -6 10 3 86.39 6.90 -6 10 3 105.79 8.10 5 -10 -3 32.70 7.00 -5 10 3 42.70 5.50 -5 10 3 42.30 5.50 4 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21.80 7.60 -12 13 3 2.70 5.70 11 -13 -3 -1.80 5.90 -11 13 3 4.10 5.20 -10 13 3 5.60 5.30 8 -13 -3 -3.30 6.70 7 -13 -3 67.39 10.30 6 -13 -3 25.50 8.30 -6 13 3 26.10 6.10 5 -13 -3 -9.10 6.30 -5 13 3 7.70 5.70 4 -13 -3 -0.30 6.70 -4 13 3 1.60 4.80 3 -13 -3 46.00 9.70 -3 13 3 50.79 7.60 2 -13 -3 28.50 8.50 -2 13 3 29.40 6.90 1 -13 -3 -6.00 7.20 -1 13 3 4.00 5.80 0 -13 -3 44.40 10.10 0 13 3 28.10 8.00 8 -14 -3 -2.50 6.90 7 -14 -3 109.99 12.50 6 -14 -3 2.40 7.80 -6 14 3 8.70 5.70 5 -14 -3 -4.50 7.30 -5 14 3 -7.00 4.80 4 -14 -3 0.10 7.00 -4 14 3 -5.30 4.90 3 -14 -3 -14.60 7.00 -3 14 3 5.00 5.70 2 -14 -3 74.59 12.20 -2 14 3 90.19 10.70 -2 15 -4 19.60 7.20 2 -15 4 27.90 9.10 -3 15 -4 2.70 6.00 3 -15 4 -9.30 6.00 -4 15 -4 15.50 7.10 4 -15 4 3.50 7.30 -5 15 -4 5.50 6.10 5 -15 4 -7.00 5.90 -6 15 -4 -8.10 5.60 6 -15 4 -2.50 6.30 -7 15 -4 -8.00 5.40 -8 15 -4 0.10 6.10 8 -15 4 -7.80 7.10 -9 15 -4 4.00 6.30 9 -15 4 24.10 8.00 -10 15 -4 15.90 6.70 10 -15 4 11.70 7.30 0 14 -4 21.90 7.30 0 -14 4 17.20 7.70 -1 14 -4 2.50 5.80 1 -14 4 -5.70 6.40 -2 14 -4 4.30 5.80 2 -14 4 8.60 6.70 -3 14 -4 54.49 8.50 3 -14 4 57.39 9.50 -4 14 -4 2.40 5.90 4 -14 4 -12.80 5.30 -5 14 -4 7.40 6.00 5 -14 4 -3.20 5.80 -6 14 -4 74.59 9.40 6 -14 4 91.99 10.10 -7 14 -4 -3.20 5.30 7 -14 4 9.90 6.10 -8 14 -4 64.29 8.70 8 -14 4 63.09 9.30 -9 14 -4 3.50 5.70 9 -14 4 13.40 7.00 -10 14 -4 15.50 6.20 10 -14 4 -0.70 6.50 -11 14 -4 24.20 6.90 11 -14 4 25.10 8.20 2 13 -4 46.60 8.50 -2 -13 4 46.10 9.60 1 13 -4 21.70 6.70 -1 -13 4 13.30 7.60 0 13 -4 10.50 6.10 0 -13 4 16.60 7.00 -1 13 -4 56.99 8.10 1 -13 4 61.89 9.70 -2 13 -4 0.00 5.30 2 -13 4 -0.70 5.80 -3 13 -4 40.80 7.20 3 -13 4 27.40 7.30 -4 13 -4 -1.00 5.00 4 -13 4 -7.30 4.70 -5 13 -4 153.58 11.40 5 -13 4 164.48 11.80 5 -13 4 152.38 11.70 -6 13 -4 32.70 7.00 6 -13 4 46.90 7.60 6 -13 4 46.10 7.80 -7 13 -4 4.00 5.40 7 -13 4 1.40 6.00 -8 13 -4 48.10 7.60 8 -13 4 58.19 8.90 -9 13 -4 0.20 5.30 9 -13 4 11.50 6.60 -10 13 -4 36.00 7.10 10 -13 4 34.00 8.10 -11 13 -4 0.40 5.40 11 -13 4 8.30 7.10 -12 13 -4 83.29 10.00 12 -13 4 86.19 11.40 3 12 -4 25.10 7.40 -3 -12 4 13.50 7.90 2 12 -4 105.29 10.40 -2 -12 4 67.99 10.20 1 12 -4 39.20 7.60 -1 -12 4 43.50 8.80 0 12 -4 -4.10 4.60 0 -12 4 4.20 6.00 -1 12 -4 -1.40 4.70 1 -12 4 1.50 5.90 -2 12 -4 20.60 6.10 2 -12 4 21.50 6.40 -3 12 -4 17.70 6.00 3 -12 4 13.30 7.30 3 -12 4 12.10 6.00 -4 12 -4 92.49 9.20 4 -12 4 84.09 8.40 4 -12 4 95.59 9.20 -5 12 -4 -1.80 4.50 5 -12 4 7.60 5.20 5 -12 4 -1.10 4.60 -6 12 -4 -1.50 4.90 6 -12 4 6.00 5.20 6 -12 4 2.50 4.80 -7 12 -4 88.39 8.80 7 -12 4 95.49 9.50 -8 12 -4 226.38 12.20 8 -12 4 208.78 13.40 -9 12 -4 11.90 5.70 9 -12 4 10.00 6.50 -10 12 -4 61.89 8.30 10 -12 4 70.99 9.70 -11 12 -4 6.90 5.70 11 -12 4 11.50 7.20 -12 12 -4 17.00 6.40 12 -12 4 8.50 8.00 -13 12 -4 25.80 7.20 13 -12 4 23.80 8.40 5 11 -4 1.20 5.80 -5 -11 4 4.90 6.70 4 11 -4 -8.70 5.10 -4 -11 4 0.00 6.30 3 11 -4 11.70 5.70 -3 -11 4 8.90 6.90 2 11 -4 133.69 10.70 -2 -11 4 131.49 12.80 1 11 -4 11.60 5.50 -1 -11 4 8.50 6.20 0 11 -4 -0.40 4.70 0 -11 4 1.40 5.70 -1 11 -4 74.99 8.20 1 -11 4 66.69 8.80 -2 11 -4 83.99 8.60 2 -11 4 88.69 9.00 2 -11 4 87.59 7.60 -3 11 -4 -1.30 4.60 3 -11 4 0.90 4.60 3 -11 4 4.60 5.00 -4 11 -4 121.79 9.50 4 -11 4 110.49 9.40 4 -11 4 101.59 8.40 -5 11 -4 404.06 14.60 5 -11 4 390.86 14.20 5 -11 4 424.66 14.30 -6 11 -4 362.96 13.70 6 -11 4 368.36 13.10 6 -11 4 385.46 14.80 -7 11 -4 7.80 4.90 7 -11 4 17.10 6.00 -8 11 -4 248.88 12.00 8 -11 4 230.58 12.80 -9 11 -4 62.89 7.50 9 -11 4 78.99 9.40 -10 11 -4 -0.10 4.80 10 -11 4 -0.80 6.00 -11 11 -4 4.60 5.10 11 -11 4 -3.60 5.80 -12 11 -4 0.40 5.20 12 -11 4 10.70 7.30 -13 11 -4 7.10 6.00 13 -11 4 20.60 7.60 6 10 -4 15.10 6.70 -6 -10 4 15.70 7.40 5 10 -4 65.99 8.90 -5 -10 4 109.39 12.10 4 10 -4 170.28 12.00 -4 -10 4 175.18 13.10 3 10 -4 45.60 7.30 -3 -10 4 42.30 8.10 2 10 -4 129.29 10.00 -2 -10 4 121.29 11.20 1 10 -4 7.50 4.70 -1 -10 4 10.10 5.80 0 10 -4 183.78 10.40 0 -10 4 183.88 12.10 0 -10 4 177.08 12.40 -1 10 -4 45.90 6.50 1 -10 4 57.39 7.50 1 -10 4 55.29 6.20 -2 10 -4 -3.40 4.20 2 -10 4 -0.90 4.30 2 -10 4 7.50 4.80 -3 10 -4 16.00 5.20 3 -10 4 10.80 5.00 3 -10 4 11.90 5.00 -4 10 -4 497.75 15.20 4 -10 4 503.45 15.00 4 -10 4 538.25 15.70 -5 10 -4 1.30 4.30 5 -10 4 10.90 5.20 5 -10 4 12.70 4.70 -6 10 -4 299.97 12.50 6 -10 4 293.67 13.00 6 -10 4 283.57 11.10 -7 10 -4 93.49 8.10 7 -10 4 95.69 8.80 -8 10 -4 6.00 4.60 8 -10 4 4.60 5.50 -9 10 -4 100.69 8.60 9 -10 4 77.89 9.00 -10 10 -4 46.50 5.70 -10 10 -4 50.49 6.90 10 -10 4 43.90 7.70 -11 10 -4 0.90 4.80 -11 10 -4 1.50 3.60 11 -10 4 6.00 6.50 -12 10 -4 -4.60 3.90 -12 10 -4 -3.60 4.50 12 -10 4 0.70 6.10 -13 10 -4 -3.80 4.90 -13 10 -4 -1.20 4.60 13 -10 4 -2.40 6.00 -14 10 -4 11.70 6.50 -14 10 -4 6.90 5.60 14 -10 4 15.30 7.20 7 9 -4 -1.00 5.40 -7 -9 4 8.00 6.90 6 9 -4 16.00 6.30 -6 -9 4 48.10 8.50 5 9 -4 -3.30 4.80 -5 -9 4 9.40 6.00 4 9 -4 200.98 11.80 -4 -9 4 214.48 13.00 3 9 -4 18.40 5.60 -3 -9 4 16.60 6.00 2 9 -4 8.10 4.70 -2 -9 4 2.80 4.80 1 9 -4 -1.60 3.90 -1 -9 4 1.70 4.50 -1 -9 4 4.50 4.00 0 9 -4 188.88 9.90 0 -9 4 181.88 8.90 0 -9 4 204.18 10.90 -1 9 -4 3.00 4.00 1 -9 4 -1.80 3.90 1 -9 4 8.70 4.80 -2 9 -4 2.20 4.10 2 -9 4 7.80 4.50 2 -9 4 5.40 4.30 -3 9 -4 235.18 10.30 3 -9 4 221.78 10.20 3 -9 4 250.07 10.80 -4 9 -4 301.57 11.20 4 -9 4 295.97 11.10 4 -9 4 304.87 11.70 -5 9 -4 27.00 5.30 5 -9 4 28.40 5.00 5 -9 4 18.60 5.40 -6 9 -4 164.48 9.20 6 -9 4 164.48 8.40 6 -9 4 148.99 10.20 -7 9 -4 148.39 7.00 -7 9 -4 162.48 9.30 7 -9 4 151.48 10.70 -8 9 -4 33.20 5.70 -8 9 -4 40.50 4.70 8 -9 4 46.70 7.30 -9 9 -4 35.10 5.90 -9 9 -4 45.60 5.20 9 -9 4 43.40 7.40 -10 9 -4 45.30 5.70 -10 9 -4 43.30 6.50 10 -9 4 32.90 6.80 -11 9 -4 11.70 4.20 -11 9 -4 6.00 4.90 11 -9 4 5.50 6.30 -12 9 -4 134.29 10.60 -12 9 -4 165.18 10.40 12 -9 4 162.78 12.80 -13 9 -4 0.60 4.80 -13 9 -4 0.00 5.40 13 -9 4 8.00 6.20 -14 9 -4 20.30 6.10 -14 9 -4 25.10 6.90 14 -9 4 23.30 7.70 8 8 -4 6.00 5.40 -8 -8 4 4.00 6.00 7 8 -4 43.00 7.30 -7 -8 4 49.10 8.40 6 8 -4 70.39 8.20 -6 -8 4 68.39 9.00 5 8 -4 25.00 5.90 -5 -8 4 16.90 5.90 4 8 -4 269.37 12.10 -4 -8 4 257.67 13.10 3 8 -4 89.79 7.90 -3 -8 4 75.19 8.30 2 8 -4 17.50 4.90 -2 -8 4 26.90 6.00 -2 -8 4 23.10 4.40 1 8 -4 91.69 7.40 -1 -8 4 127.69 9.10 -1 -8 4 87.59 6.80 0 8 -4 4.00 4.00 0 -8 4 -3.40 3.40 0 -8 4 7.40 4.20 1 -8 4 219.18 9.30 1 -8 4 216.38 10.10 -2 8 -4 22.30 4.30 2 -8 4 23.00 4.50 2 -8 4 30.20 5.00 -3 8 -4 83.59 6.90 3 -8 4 88.69 7.10 3 -8 4 76.19 6.70 -4 8 -4 35.90 5.20 -4 8 -4 43.80 3.30 4 -8 4 48.90 5.30 4 -8 4 46.00 5.80 -5 8 -4 103.19 4.90 -5 8 -4 112.39 7.50 5 -8 4 112.79 8.70 5 -8 4 133.19 7.30 -6 8 -4 3.70 2.40 -6 8 -4 2.00 3.70 6 -8 4 1.40 3.10 6 -8 4 8.40 4.80 -7 8 -4 172.38 9.00 -7 8 -4 170.78 7.30 7 -8 4 164.58 10.10 -8 8 -4 99.89 7.80 -8 8 -4 86.69 6.50 8 -8 4 92.69 8.80 -9 8 -4 15.60 3.80 -9 8 -4 10.70 4.70 9 -8 4 20.50 5.90 -10 8 -4 37.90 5.40 -10 8 -4 50.19 6.70 10 -8 4 40.70 7.20 -11 8 -4 26.20 5.20 -11 8 -4 22.70 5.90 11 -8 4 12.50 6.10 -12 8 -4 72.99 8.00 -12 8 -4 54.99 7.60 12 -8 4 64.99 9.10 -13 8 -4 72.99 8.90 -13 8 -4 65.89 8.20 13 -8 4 73.49 9.60 -14 8 -4 4.50 5.60 -14 8 -4 -9.20 5.10 14 -8 4 7.50 6.50 9 7 -4 76.79 9.10 8 7 -4 83.89 8.80 -8 -7 4 84.79 9.70 7 7 -4 257.57 12.70 -7 -7 4 252.77 13.50 6 7 -4 11.30 5.20 -6 -7 4 9.70 5.20 5 7 -4 53.99 6.60 -5 -7 4 39.50 6.50 4 7 -4 -5.30 3.70 -4 -7 4 -3.40 3.90 -4 -7 4 1.20 3.20 3 7 -4 278.87 11.10 3 7 -4 306.17 13.10 -3 -7 4 296.77 10.00 -3 -7 4 291.57 12.60 2 7 -4 242.18 11.30 2 7 -4 246.18 9.90 -2 -7 4 235.68 9.00 1 7 -4 124.29 7.50 1 7 -4 125.19 9.30 -1 -7 4 124.89 7.10 0 7 -4 590.54 15.90 0 7 -4 620.74 14.40 0 -7 4 629.54 13.80 -1 7 -4 288.47 10.80 -1 7 -4 275.27 9.70 1 -7 4 276.47 9.40 -2 7 -4 57.99 5.40 -2 7 -4 57.29 5.70 2 -7 4 48.70 5.30 2 -7 4 45.10 5.10 -3 7 -4 13.70 3.80 -3 7 -4 16.00 1.80 3 -7 4 15.10 3.70 3 -7 4 4.00 3.80 -4 7 -4 496.15 12.50 -4 7 -4 502.45 8.90 4 -7 4 519.45 12.00 4 -7 4 502.05 13.20 -5 7 -4 239.38 6.70 -5 7 -4 245.08 9.20 5 -7 4 247.18 10.10 5 -7 4 224.98 7.70 -6 7 -4 76.19 6.40 -6 7 -4 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3.20 6.10 14 -4 4 9.30 7.10 11 3 -4 44.90 7.30 10 3 -4 12.50 5.10 10 3 -4 17.00 5.40 9 3 -4 116.89 9.10 9 3 -4 122.99 9.00 -9 -3 4 123.59 8.40 8 3 -4 -3.30 3.30 8 3 -4 3.10 3.70 8 3 -4 -2.40 3.80 8 3 -4 2.00 3.70 7 3 -4 57.09 6.10 7 3 -4 61.49 6.90 7 3 -4 48.20 5.50 7 3 -4 49.10 5.50 6 3 -4 111.19 7.50 6 3 -4 110.59 6.90 6 3 -4 114.69 8.30 6 3 -4 106.79 6.90 5 3 -4 -2.50 3.40 5 3 -4 0.40 3.10 5 3 -4 -1.90 2.60 5 3 -4 -2.10 2.90 4 3 -4 160.78 6.10 4 3 -4 163.78 6.60 4 3 -4 161.28 7.30 4 3 -4 152.28 8.10 3 3 -4 773.52 12.40 3 3 -4 773.02 13.50 3 3 -4 768.72 15.80 -3 -3 4 751.22 14.30 2 3 -4 116.79 6.70 2 3 -4 115.49 5.10 -2 -3 4 112.29 5.50 -2 -3 4 121.39 3.80 1 3 -4 75.29 5.30 1 3 -4 70.79 4.40 -1 -3 4 71.99 4.70 -1 -3 4 71.49 2.50 0 3 -4 1595.74 20.90 0 3 -4 1585.14 22.50 0 -3 4 1599.34 22.00 -1 3 -4 37.10 3.50 -1 3 -4 38.90 3.30 1 -3 4 36.00 3.70 1 -3 4 33.10 2.20 -2 3 -4 44.80 3.80 -2 3 -4 50.79 4.20 2 -3 4 45.70 3.20 2 -3 4 49.20 4.20 -3 3 -4 94.59 5.10 -3 3 -4 106.09 4.10 3 -3 4 108.99 4.60 3 -3 4 102.19 5.70 -4 3 -4 5.70 2.60 -4 3 -4 10.60 1.70 4 -3 4 2.70 2.50 4 -3 4 4.00 3.00 -5 3 -4 132.59 6.50 5 -3 4 134.59 6.40 5 -3 4 127.59 6.90 -6 3 -4 48.80 5.10 6 -3 4 36.20 4.70 6 -3 4 36.30 4.50 -7 3 -4 97.59 7.00 7 -3 4 86.29 7.10 7 -3 4 84.29 6.80 -8 3 -4 144.09 8.40 8 -3 4 136.19 8.60 8 -3 4 144.39 8.60 -9 3 -4 306.67 12.00 9 -3 4 298.07 12.20 9 -3 4 306.47 11.80 -10 3 -4 5.80 4.30 10 -3 4 13.60 5.50 10 -3 4 6.60 4.40 -11 3 -4 9.00 5.30 11 -3 4 2.10 5.10 11 -3 4 0.30 4.40 -12 3 -4 33.20 7.10 12 -3 4 38.50 7.60 12 -3 4 23.10 6.00 -13 3 -4 79.39 9.60 13 -3 4 63.99 9.10 -12 -2 4 9.30 5.70 11 2 -4 6.40 4.90 -11 -2 4 -2.40 4.30 10 2 -4 21.70 5.60 10 2 -4 35.90 6.50 9 2 -4 30.40 5.70 9 2 -4 45.40 6.30 -9 -2 4 33.60 5.10 8 2 -4 7.70 4.50 8 2 -4 8.20 3.90 8 2 -4 7.40 3.90 -8 -2 4 6.90 3.50 7 2 -4 90.99 7.00 7 2 -4 86.89 7.80 7 2 -4 91.69 6.40 7 2 -4 97.79 7.20 6 2 -4 74.69 6.10 6 2 -4 77.09 7.00 6 2 -4 75.99 5.60 6 2 -4 72.39 6.30 5 2 -4 52.79 5.30 5 2 -4 60.69 4.70 5 2 -4 49.50 5.10 5 2 -4 53.49 4.60 4 2 -4 858.01 16.50 4 2 -4 825.52 15.90 4 2 -4 843.02 13.90 -4 -2 4 871.21 14.20 3 2 -4 8.50 2.90 3 2 -4 4.60 2.20 3 2 -4 5.10 2.80 -3 -2 4 6.20 1.90 2 2 -4 0.60 1.90 2 2 -4 -1.30 2.40 -2 -2 4 -1.50 2.20 -2 -2 4 2.20 1.50 1 2 -4 1665.23 20.40 1 2 -4 1632.74 22.90 -1 -2 4 1650.33 19.00 -1 -2 4 1632.24 22.10 0 2 -4 6.10 2.10 0 2 -4 1.50 2.40 0 -2 4 7.50 2.50 0 -2 4 6.80 1.60 -1 2 -4 500.15 8.90 -1 2 -4 509.15 9.50 1 -2 4 494.95 9.80 1 -2 4 520.95 7.90 -2 2 -4 323.97 6.80 -2 2 -4 312.47 7.30 2 -2 4 329.37 8.10 2 -2 4 310.77 6.80 -3 2 -4 3.50 2.30 -3 2 -4 1.90 1.60 3 -2 4 1.40 2.70 3 -2 4 1.30 2.30 -4 2 -4 25.60 2.40 -4 2 -4 31.90 3.70 4 -2 4 27.40 3.50 4 -2 4 24.90 3.50 -5 2 -4 16.60 3.40 -5 2 -4 12.20 1.60 5 -2 4 17.20 3.50 5 -2 4 11.20 3.20 -6 2 -4 85.09 6.30 6 -2 4 78.99 6.10 6 -2 4 78.09 6.20 -7 2 -4 25.70 4.50 7 -2 4 21.00 4.10 7 -2 4 34.60 5.00 -8 2 -4 2.90 3.90 8 -2 4 3.00 3.60 8 -2 4 -0.90 3.90 -9 2 -4 82.99 7.60 9 -2 4 87.19 7.40 9 -2 4 82.99 7.70 -10 2 -4 22.40 5.50 10 -2 4 17.40 5.60 10 -2 4 24.20 5.20 -11 2 -4 13.80 5.60 11 -2 4 9.50 4.80 11 -2 4 22.10 6.10 -12 2 -4 62.69 8.30 12 -2 4 75.49 9.30 -13 2 -4 2.10 6.40 13 -2 4 12.20 6.90 -13 -1 4 48.80 8.20 12 1 -4 3.40 5.10 -12 -1 4 2.50 5.10 11 1 -4 0.70 4.40 -11 -1 4 -9.20 4.10 10 1 -4 1.20 4.40 -10 -1 4 1.70 4.20 9 1 -4 -2.40 3.90 -9 -1 4 9.60 4.10 -9 -1 4 1.70 3.60 8 1 -4 234.48 10.00 8 1 -4 229.68 9.90 8 1 -4 225.48 10.60 -8 -1 4 241.38 8.90 -8 -1 4 242.98 9.90 7 1 -4 19.90 4.50 7 1 -4 18.90 4.40 -7 -1 4 17.50 4.00 -7 -1 4 25.30 3.60 6 1 -4 2.00 3.10 6 1 -4 -0.90 2.30 6 1 -4 -3.70 3.00 -6 -1 4 -5.60 2.30 5 1 -4 33.60 3.20 5 1 -4 30.30 4.30 5 1 -4 27.80 4.00 -5 -1 4 30.10 3.50 4 1 -4 403.06 10.30 4 1 -4 402.66 8.00 4 1 -4 394.36 10.20 -4 -1 4 409.46 8.90 3 1 -4 6.40 1.80 3 1 -4 19.00 3.30 3 1 -4 6.00 2.90 -3 -1 4 10.10 2.10 2 1 -4 14.10 2.90 2 1 -4 17.20 1.90 2 1 -4 22.50 3.40 -2 -1 4 15.00 2.10 1 1 -4 25.20 2.00 1 1 -4 32.50 3.50 -1 -1 4 28.90 2.30 -1 -1 4 24.20 2.90 0 1 -4 1971.50 22.80 0 1 -4 1970.80 24.90 0 -1 4 1962.50 23.00 0 -1 4 1949.20 24.30 -1 1 -4 231.08 6.20 -1 1 -4 238.18 5.70 1 -1 4 239.28 5.90 1 -1 4 235.18 6.30 -2 1 -4 75.89 3.80 2 -1 4 78.59 4.50 2 -1 4 79.29 4.40 -3 1 -4 326.77 8.20 -3 1 -4 336.17 6.70 3 -1 4 311.17 7.60 3 -1 4 324.07 8.20 -4 1 -4 56.49 4.60 -4 1 -4 64.69 3.50 4 -1 4 61.09 4.50 4 -1 4 71.89 5.20 -5 1 -4 1197.28 20.00 -5 1 -4 1204.98 15.90 5 -1 4 1176.98 18.70 5 -1 4 1148.39 20.00 -6 1 -4 207.48 5.50 -6 1 -4 213.28 8.70 6 -1 4 215.78 8.00 6 -1 4 207.78 8.80 -7 1 -4 103.39 7.40 7 -1 4 92.79 6.40 7 -1 4 89.69 7.40 -8 1 -4 10.50 4.40 8 -1 4 15.60 4.20 8 -1 4 11.00 4.60 -9 1 -4 48.90 6.60 9 -1 4 43.10 6.50 9 -1 4 49.20 5.70 -10 1 -4 68.89 7.90 10 -1 4 52.29 7.50 -11 1 -4 17.40 5.90 11 -1 4 5.70 5.30 -12 1 -4 20.90 7.20 12 -1 4 18.80 6.50 -13 1 -4 54.29 8.90 13 -1 4 41.60 8.40 13 0 -4 3.10 5.90 -13 0 4 16.80 6.10 12 0 -4 2.00 5.20 -12 0 4 -0.30 4.80 11 0 -4 46.50 7.30 -11 0 4 36.70 6.30 10 0 -4 8.90 4.80 -10 0 4 7.80 4.40 9 0 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11 -5 3.00 5.20 10 -11 5 5.80 6.50 -11 11 -5 38.30 7.10 11 -11 5 36.50 8.30 -12 11 -5 -2.60 5.30 12 -11 5 -3.30 6.40 -13 11 -5 33.70 7.50 13 -11 5 26.70 7.90 6 10 -5 8.50 6.20 -6 -10 5 1.50 5.90 5 10 -5 21.50 6.60 -5 -10 5 11.00 6.90 4 10 -5 110.39 10.50 -4 -10 5 96.19 11.00 3 10 -5 -5.80 4.50 -3 -10 5 3.50 5.90 2 10 -5 34.90 6.60 -2 -10 5 25.60 6.90 1 10 -5 5.40 4.70 -1 -10 5 0.20 4.80 0 10 -5 79.89 8.10 0 -10 5 55.09 7.50 0 -10 5 55.19 6.70 -1 10 -5 2.30 4.60 1 -10 5 0.30 4.60 1 -10 5 3.70 4.60 -2 10 -5 108.29 8.80 2 -10 5 130.49 9.50 2 -10 5 98.39 8.20 -3 10 -5 777.82 19.00 3 -10 5 737.43 18.40 3 -10 5 784.82 19.50 -4 10 -5 4.90 4.70 4 -10 5 -0.30 4.00 4 -10 5 10.50 5.30 -5 10 -5 203.28 10.70 5 -10 5 192.28 11.10 5 -10 5 199.38 10.00 -6 10 -5 242.38 11.30 6 -10 5 266.07 12.50 6 -10 5 224.58 10.10 -7 10 -5 52.59 6.70 7 -10 5 56.19 7.60 -8 10 -5 29.00 6.00 8 -10 5 14.80 6.40 -9 10 -5 -2.50 4.30 9 -10 5 7.30 6.00 -10 10 -5 6.40 5.10 10 -10 5 -0.30 5.70 -11 10 -5 1.80 5.00 11 -10 5 16.10 6.70 -12 10 -5 23.00 6.50 -12 10 -5 17.30 6.40 12 -10 5 23.20 7.80 -13 10 -5 15.20 6.30 -13 10 -5 -0.80 4.70 13 -10 5 9.10 6.60 7 9 -5 0.80 5.50 -7 -9 5 0.90 5.80 6 9 -5 16.70 6.10 -6 -9 5 18.80 6.80 5 9 -5 194.78 11.80 -5 -9 5 214.68 13.50 4 9 -5 95.59 9.10 -4 -9 5 83.69 9.40 3 9 -5 25.70 5.60 -3 -9 5 18.70 6.10 2 9 -5 212.08 11.00 -2 -9 5 208.38 10.00 -2 -9 5 202.18 12.30 1 9 -5 51.69 6.40 -1 -9 5 56.29 6.30 -1 -9 5 54.19 7.50 0 9 -5 19.30 4.90 0 -9 5 24.60 5.10 0 -9 5 16.30 5.20 -1 9 -5 343.27 12.40 1 -9 5 334.67 11.90 1 -9 5 366.06 13.60 -2 9 -5 76.09 6.90 2 -9 5 68.79 6.90 2 -9 5 85.89 7.70 -3 9 -5 218.28 10.10 3 -9 5 228.98 10.80 3 -9 5 228.78 10.30 -4 9 -5 13.90 4.80 4 -9 5 17.80 4.70 4 -9 5 12.70 4.90 -5 9 -5 62.19 6.70 5 -9 5 44.00 6.40 5 -9 5 39.80 5.40 -6 9 -5 70.09 6.90 6 -9 5 53.19 7.10 6 -9 5 47.80 5.50 -7 9 -5 152.78 9.40 7 -9 5 135.29 10.80 -8 9 -5 177.68 8.10 -8 9 -5 162.28 9.70 8 -9 5 174.08 11.70 -9 9 -5 16.10 3.80 -9 9 -5 12.30 4.90 9 -9 5 15.20 6.10 -10 9 -5 29.00 6.10 -10 9 -5 24.90 4.70 10 -9 5 28.00 6.80 -11 9 -5 9.80 4.60 -11 9 -5 14.00 5.50 11 -9 5 13.00 6.70 -12 9 -5 12.00 4.80 -12 9 -5 12.20 5.90 12 -9 5 18.20 7.10 -13 9 -5 69.79 8.20 -13 9 -5 80.69 9.30 13 -9 5 84.89 10.30 -14 9 -5 50.89 8.20 -14 9 -5 45.50 8.20 14 -9 5 47.30 9.10 8 8 -5 20.00 6.60 -8 -8 5 12.00 6.40 7 8 -5 68.69 8.40 -7 -8 5 66.49 9.10 6 8 -5 15.30 5.80 -6 -8 5 11.60 5.80 5 8 -5 1.50 4.50 -5 -8 5 -0.50 4.80 4 8 -5 -3.70 4.00 -4 -8 5 2.20 4.80 3 8 -5 0.90 5.20 3 8 -5 6.10 4.30 -3 -8 5 -3.90 3.40 -3 -8 5 2.50 4.40 2 8 -5 7.60 5.10 2 8 -5 2.70 4.00 -2 -8 5 5.80 3.90 1 8 -5 19.30 5.70 1 8 -5 23.60 4.90 -1 -8 5 33.00 5.00 0 8 -5 1.80 3.80 0 8 -5 0.50 4.30 0 -8 5 3.40 3.90 -1 8 -5 467.25 13.20 -1 8 -5 463.55 14.40 1 -8 5 451.85 13.00 -2 8 -5 63.39 6.50 -2 8 -5 59.39 5.90 2 -8 5 54.19 6.00 -3 8 -5 13.50 4.30 3 -8 5 13.50 4.70 3 -8 5 33.40 5.10 -4 8 -5 299.47 10.80 4 -8 5 307.27 10.20 4 -8 5 300.47 11.20 -5 8 -5 47.90 4.30 -5 8 -5 45.10 5.40 5 -8 5 51.99 6.50 5 -8 5 73.29 6.10 -6 8 -5 443.46 10.00 -6 8 -5 445.76 13.30 6 -8 5 430.36 11.10 6 -8 5 456.75 14.90 -7 8 -5 11.10 4.40 -7 8 -5 9.30 3.10 7 -8 5 7.20 5.30 -8 8 -5 -1.40 2.80 -8 8 -5 10.50 4.50 8 -8 5 7.70 5.20 -9 8 -5 -5.60 3.80 -9 8 -5 -4.40 2.80 9 -8 5 -13.60 4.40 -10 8 -5 73.59 6.90 -10 8 -5 59.79 7.40 10 -8 5 66.19 8.20 -11 8 -5 64.99 7.00 -11 8 -5 56.29 7.60 11 -8 5 62.69 8.80 -12 8 -5 4.30 5.50 -12 8 -5 15.30 5.00 12 -8 5 15.00 6.90 -13 8 -5 46.60 7.40 -13 8 -5 39.70 7.50 13 -8 5 45.30 8.70 -14 8 -5 5.60 6.40 -14 8 -5 10.10 5.60 14 -8 5 12.30 7.10 8 7 -5 9.00 5.40 -8 -7 5 21.60 6.50 7 7 -5 17.30 5.40 -7 -7 5 20.40 6.30 6 7 -5 31.50 6.30 -6 -7 5 24.80 6.00 5 7 -5 4.30 4.40 5 7 -5 -1.40 5.00 -5 -7 5 2.70 3.70 4 7 -5 21.20 6.30 4 7 -5 16.30 4.80 -4 -7 5 19.50 4.40 3 7 -5 163.58 10.60 3 7 -5 156.88 8.70 -3 -7 5 156.28 8.30 2 7 -5 70.49 6.30 2 7 -5 72.89 7.60 -2 -7 5 75.49 6.20 1 7 -5 249.08 9.90 1 7 -5 262.37 11.40 -1 -7 5 273.67 9.80 0 7 -5 19.90 5.00 0 7 -5 5.90 3.70 0 -7 5 4.00 3.50 -1 7 -5 103.29 6.90 -1 7 -5 106.49 8.00 1 -7 5 103.49 7.20 -2 7 -5 74.99 6.20 -2 7 -5 84.09 6.90 2 -7 5 67.69 6.00 -3 7 -5 41.10 4.90 -3 7 -5 39.50 4.80 -3 7 -5 36.50 2.30 3 -7 5 33.00 5.00 -4 7 -5 15.20 3.80 -4 7 -5 17.90 2.20 -4 7 -5 20.90 3.90 4 -7 5 16.30 4.70 -5 7 -5 155.08 8.00 -5 7 -5 156.88 5.50 5 -7 5 165.88 6.80 5 -7 5 164.28 9.10 -6 7 -5 -0.80 3.50 -6 7 -5 -2.00 2.20 6 -7 5 5.10 2.70 6 -7 5 -7.30 4.20 -7 7 -5 27.00 4.90 7 -7 5 31.50 6.00 7 -7 5 19.40 4.00 -8 7 -5 21.50 5.00 8 -7 5 18.20 4.50 8 -7 5 14.70 5.70 -9 7 -5 250.07 11.20 9 -7 5 244.68 12.70 9 -7 5 260.77 10.70 -10 7 -5 90.89 8.40 10 -7 5 73.99 7.60 10 -7 5 84.29 8.70 -11 7 -5 117.09 9.90 11 -7 5 87.99 9.30 11 -7 5 109.09 9.30 -12 7 -5 13.30 5.80 12 -7 5 15.80 6.60 12 -7 5 18.70 6.70 -13 7 -5 23.10 6.70 13 -7 5 25.50 7.20 13 -7 5 12.60 6.40 -14 7 -5 51.49 8.50 -14 7 -5 34.90 7.50 14 -7 5 34.70 8.20 14 -7 5 32.10 7.80 8 6 -5 3.20 4.90 -8 -6 5 7.20 5.30 7 6 -5 -1.10 5.10 7 6 -5 3.00 4.10 6 6 -5 99.39 8.20 6 6 -5 113.49 10.10 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4.20 -3 -4 8 8.80 2.40 -3 -4 8 9.70 4.00 2 4 -8 22.00 4.70 2 4 -8 33.50 3.90 -2 -4 8 25.90 4.70 -2 -4 8 29.20 2.70 1 4 -8 0.70 2.60 1 4 -8 2.10 3.30 -1 -4 8 -1.10 1.80 -1 -4 8 -1.80 3.10 0 4 -8 198.98 9.10 0 4 -8 217.28 7.40 0 -4 8 202.58 5.30 0 -4 8 205.38 8.70 -1 4 -8 148.39 6.60 -1 4 -8 147.89 7.60 1 -4 8 146.59 7.70 1 -4 8 147.29 5.00 -2 4 -8 4.10 2.90 -2 4 -8 4.10 3.10 2 -4 8 0.40 3.50 2 -4 8 3.90 2.40 -3 4 -8 37.40 4.30 -3 4 -8 36.00 4.30 3 -4 8 31.60 3.70 3 -4 8 20.60 4.60 -4 4 -8 279.57 9.80 -4 4 -8 281.87 8.70 4 -4 8 293.67 10.70 4 -4 8 273.67 8.60 -5 4 -8 10.90 3.80 -5 4 -8 9.00 2.90 5 -4 8 16.40 4.70 5 -4 8 1.70 3.30 -6 4 -8 160.18 8.70 6 -4 8 163.78 8.50 6 -4 8 158.98 9.30 -7 4 -8 6.50 4.00 7 -4 8 16.30 5.20 7 -4 8 18.30 4.60 -8 4 -8 77.69 7.80 8 -4 8 84.69 7.50 8 -4 8 81.29 7.60 -9 4 -8 1.10 4.70 9 -4 8 3.80 4.70 9 -4 8 0.00 4.10 -10 4 -8 9.40 5.60 10 -4 8 20.60 6.30 10 -4 8 12.60 5.10 -11 4 -8 117.09 10.80 11 -4 8 123.69 10.80 -12 4 -8 10.00 6.30 12 -4 8 13.90 6.50 11 3 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297.27 12.60 6 -9 9 293.87 14.00 -7 9 -9 2.10 4.50 7 -9 9 -2.30 5.40 -8 9 -9 96.99 9.10 8 -9 9 96.19 9.70 -9 9 -9 27.00 6.30 9 -9 9 45.00 8.20 -10 9 -9 92.79 10.10 10 -9 9 98.89 10.50 -11 9 -9 22.20 7.00 11 -9 9 20.10 7.40 -12 9 -9 61.69 9.20 12 -9 9 61.09 9.60 7 8 -9 46.40 9.60 6 8 -9 49.60 9.20 -6 -8 9 60.99 8.30 5 8 -9 -4.30 5.30 5 8 -9 7.40 6.60 -5 -8 9 5.30 5.10 4 8 -9 56.39 8.80 4 8 -9 66.79 7.30 -4 -8 9 44.60 7.20 3 8 -9 3.80 5.50 3 8 -9 16.80 5.00 -3 -8 9 4.20 5.10 2 8 -9 13.70 4.80 2 8 -9 13.20 5.90 -2 -8 9 6.90 5.00 1 8 -9 27.40 6.80 1 8 -9 25.20 5.10 -1 -8 9 25.80 6.00 0 8 -9 225.68 10.20 0 8 -9 221.78 11.80 0 -8 9 216.78 11.80 -1 8 -9 192.58 10.00 -1 8 -9 201.58 11.00 1 -8 9 186.08 11.40 -2 8 -9 35.70 6.00 -2 8 -9 33.30 5.30 2 -8 9 30.40 6.40 -3 8 -9 266.37 11.50 -3 8 -9 252.97 10.90 3 -8 9 264.77 13.10 -4 8 -9 7.20 4.20 -4 8 -9 2.30 4.00 4 -8 9 0.90 5.50 -5 8 -9 0.70 4.50 -5 8 -9 2.00 3.90 5 -8 9 -5.50 5.10 -6 8 -9 28.70 5.80 6 -8 9 31.30 7.10 -7 8 -9 20.60 5.20 7 -8 9 26.40 6.80 -8 8 -9 87.39 8.20 8 -8 9 109.19 10.10 -9 8 -9 57.69 7.80 9 -8 9 69.69 8.80 -10 8 -9 12.00 6.10 10 -8 9 11.50 6.60 -11 8 -9 13.20 6.50 11 -8 9 21.00 7.10 -12 8 -9 4.00 6.20 12 -8 9 10.20 6.50 8 7 -9 -2.30 6.50 7 7 -9 8.20 6.90 -7 -7 9 9.30 6.10 6 7 -9 298.97 16.30 -6 -7 9 310.47 15.00 5 7 -9 -2.70 5.70 -5 -7 9 1.90 4.80 4 7 -9 512.75 18.30 4 7 -9 525.45 14.80 -4 -7 9 519.75 16.90 3 7 -9 2.20 5.00 3 7 -9 1.30 3.50 -3 -7 9 -0.50 4.50 2 7 -9 355.16 14.90 2 7 -9 387.26 12.40 -2 -7 9 340.57 13.60 1 7 -9 9.80 5.30 1 7 -9 12.20 4.20 -1 -7 9 1.00 4.40 0 7 -9 16.20 4.50 0 7 -9 13.80 5.30 0 -7 9 10.00 5.10 -1 7 -9 113.89 7.60 -1 7 -9 112.09 9.10 1 -7 9 112.09 8.90 -2 7 -9 30.20 5.10 -2 7 -9 31.80 5.60 2 -7 9 32.40 6.20 -3 7 -9 63.89 6.30 -3 7 -9 67.09 6.80 3 -7 9 78.19 7.80 -4 7 -9 28.80 5.00 -4 7 -9 28.40 5.10 4 -7 9 11.20 5.70 -5 7 -9 68.19 6.90 -5 7 -9 67.89 6.30 5 -7 9 71.89 8.00 -6 7 -9 9.70 4.50 6 -7 9 3.40 5.30 -7 7 -9 19.50 5.30 7 -7 9 21.50 6.40 -8 7 -9 156.08 10.20 8 -7 9 150.98 9.00 8 -7 9 136.29 10.70 -9 7 -9 2.30 5.00 9 -7 9 1.40 4.30 9 -7 9 2.50 5.40 -10 7 -9 21.20 6.30 10 -7 9 8.20 5.90 10 -7 9 13.50 5.60 -11 7 -9 -5.20 5.40 11 -7 9 -3.80 5.00 11 -7 9 12.90 6.50 -12 7 -9 42.10 8.00 12 -7 9 40.40 8.20 12 -7 9 32.00 7.70 9 6 -9 4.50 7.00 -9 -6 9 3.70 5.70 8 6 -9 4.40 6.50 -8 -6 9 -1.10 5.20 7 6 -9 14.20 6.90 -7 -6 9 8.80 5.40 6 6 -9 188.88 13.50 -6 -6 9 211.98 12.20 5 6 -9 8.40 5.60 -5 -6 9 6.80 5.10 4 6 -9 100.69 10.00 4 6 -9 89.39 7.20 -4 -6 9 79.29 7.90 3 6 -9 7.90 3.90 3 6 -9 6.40 5.10 -3 -6 9 2.50 4.30 2 6 -9 90.19 6.80 2 6 -9 73.89 7.80 -2 -6 9 84.49 7.60 1 6 -9 54.89 6.90 1 6 -9 66.09 5.90 -1 -6 9 61.39 6.90 0 6 -9 3.80 3.40 0 6 -9 -0.40 3.90 0 -6 9 1.10 4.40 -1 6 -9 563.54 15.50 -1 6 -9 562.04 13.90 1 -6 9 547.15 15.40 -2 6 -9 98.99 7.00 -2 6 -9 96.19 7.60 2 -6 9 78.49 7.10 -3 6 -9 8.70 3.90 -3 6 -9 8.60 3.80 3 -6 9 8.70 5.00 -4 6 -9 108.39 7.10 -4 6 -9 117.99 7.80 4 -6 9 115.69 9.50 -5 6 -9 16.00 4.80 -5 6 -9 19.90 4.70 5 -6 9 19.80 5.70 5 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506.15 13.50 2 -5 9 471.55 9.20 2 -5 9 468.95 13.90 -3 5 -9 -0.60 3.20 -3 5 -9 5.10 3.60 3 -5 9 5.10 2.60 3 -5 9 10.60 4.80 -4 5 -9 74.79 6.60 -4 5 -9 67.69 6.00 4 -5 9 68.49 5.50 4 -5 9 66.29 6.90 -5 5 -9 7.00 4.10 -5 5 -9 3.00 4.50 5 -5 9 2.10 4.40 5 -5 9 5.50 3.50 -6 5 -9 602.84 16.10 6 -5 9 564.44 14.10 6 -5 9 597.14 16.50 -7 5 -9 54.59 6.80 7 -5 9 61.19 6.30 7 -5 9 57.99 7.30 -8 5 -9 260.17 12.20 8 -5 9 277.57 12.50 8 -5 9 256.57 11.30 -9 5 -9 70.39 7.90 9 -5 9 78.29 8.20 9 -5 9 69.29 7.80 -10 5 -9 -0.70 5.10 10 -5 9 -3.80 4.60 10 -5 9 -1.40 4.80 -11 5 -9 0.50 5.50 11 -5 9 0.30 5.10 11 -5 9 6.20 5.90 -12 5 -9 13.50 6.60 12 -5 9 3.60 6.10 -10 -4 9 19.10 6.80 9 4 -9 24.20 7.20 -9 -4 9 24.50 6.90 8 4 -9 7.60 6.00 -8 -4 9 5.80 5.60 7 4 -9 40.70 7.70 -7 -4 9 33.80 6.50 6 4 -9 44.70 7.50 -6 -4 9 30.70 6.00 5 4 -9 25.80 6.00 -5 -4 9 27.00 5.70 4 4 -9 15.00 3.70 4 4 -9 20.70 5.50 -4 -4 9 8.20 4.40 3 4 -9 104.59 8.50 3 4 -9 104.69 6.30 -3 -4 9 101.79 7.90 2 4 -9 6.80 4.00 2 4 -9 7.60 3.20 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10.10 4 9 -10 48.40 8.90 4 9 -10 33.70 7.70 -4 -9 10 37.50 7.50 3 9 -10 7.40 5.00 3 9 -10 -1.50 5.80 -3 -9 10 4.50 5.40 2 9 -10 4.00 5.80 2 9 -10 6.30 4.90 -2 -9 10 -4.40 5.40 1 9 -10 45.80 6.70 1 9 -10 28.90 7.20 -1 -9 10 23.40 6.50 0 9 -10 1.90 4.20 0 9 -10 1.20 5.30 0 -9 10 -5.70 5.10 -1 9 -10 24.50 5.50 -1 9 -10 18.60 6.00 1 -9 10 13.20 6.00 -2 9 -10 37.60 6.80 -2 9 -10 13.80 4.90 2 -9 10 15.30 6.10 -3 9 -10 131.79 9.40 -3 9 -10 126.59 9.80 3 -9 10 102.89 9.80 -4 9 -10 45.40 6.60 -4 9 -10 46.50 6.70 4 -9 10 58.89 8.20 -5 9 -10 43.40 6.40 5 -9 10 35.60 7.50 -6 9 -10 6.30 5.00 6 -9 10 19.70 6.70 -7 9 -10 176.28 11.10 7 -9 10 186.98 12.70 -8 9 -10 -3.70 4.80 8 -9 10 4.00 6.30 -9 9 -10 61.59 8.20 9 -9 10 71.59 9.60 -10 9 -10 50.79 8.10 10 -9 10 67.39 9.40 -11 9 -10 2.60 6.00 11 -9 10 11.70 7.20 -12 9 -10 204.68 14.30 12 -9 10 212.68 14.60 7 8 -10 -3.00 6.80 -7 -8 10 3.30 6.30 6 8 -10 18.30 7.60 -6 -8 10 25.00 7.20 5 8 -10 77.19 10.40 -5 -8 10 83.99 9.30 4 8 -10 36.90 7.80 4 8 -10 35.10 9.60 -4 -8 10 42.10 7.30 3 8 -10 21.30 5.10 3 8 -10 13.90 6.10 -3 -8 10 21.60 6.30 2 8 -10 5.90 5.60 2 8 -10 8.80 4.60 -2 -8 10 4.60 5.10 1 8 -10 13.90 5.70 1 8 -10 -2.00 3.80 -1 -8 10 -1.70 4.80 0 8 -10 71.49 6.90 0 8 -10 82.89 8.60 0 -8 10 82.39 8.60 -1 8 -10 3.60 4.80 -1 8 -10 1.30 4.10 1 -8 10 8.60 5.60 -2 8 -10 19.50 5.60 -2 8 -10 21.30 5.20 2 -8 10 19.70 6.10 -3 8 -10 72.29 7.10 -3 8 -10 77.19 7.90 3 -8 10 83.59 8.50 -4 8 -10 1.20 4.30 -4 8 -10 -0.70 3.90 4 -8 10 13.10 5.70 -5 8 -10 4.10 4.40 5 -8 10 -3.40 5.40 -6 8 -10 38.00 6.40 6 -8 10 29.80 6.90 -7 8 -10 112.39 9.30 7 -8 10 109.09 9.90 -8 8 -10 38.10 6.90 8 -8 10 33.60 7.80 -9 8 -10 35.80 6.90 9 -8 10 41.40 8.20 -10 8 -10 50.89 8.00 10 -8 10 50.79 8.50 -11 8 -10 24.70 7.30 11 -8 10 44.40 8.30 -12 8 -10 61.09 9.10 12 -8 10 100.89 10.60 8 7 -10 10.30 7.70 -8 -7 10 20.30 7.50 7 7 -10 74.49 10.40 -7 -7 10 75.09 9.60 6 7 -10 44.70 8.80 -6 -7 10 53.09 8.10 5 7 -10 26.70 7.60 -5 -7 10 30.50 6.80 4 7 -10 -5.60 5.10 -4 -7 10 -2.10 4.70 3 7 -10 107.49 7.90 3 7 -10 116.19 10.80 -3 -7 10 117.69 10.20 2 7 -10 -2.10 4.90 2 7 -10 -1.70 3.70 -2 -7 10 -2.90 4.60 1 7 -10 162.38 8.90 1 7 -10 171.28 11.20 -1 -7 10 179.58 11.10 0 7 -10 213.58 9.50 0 7 -10 220.18 11.80 0 -7 10 207.28 11.70 -1 7 -10 37.00 6.20 -1 7 -10 36.20 5.30 1 -7 10 33.40 6.40 -2 7 -10 -1.50 3.90 -2 7 -10 -5.40 3.60 2 -7 10 -1.50 5.10 -3 7 -10 231.38 10.20 -3 7 -10 245.28 11.00 3 -7 10 259.67 12.30 -4 7 -10 81.69 7.30 -4 7 -10 74.79 7.00 4 -7 10 74.09 8.00 -5 7 -10 191.68 10.20 5 -7 10 219.78 12.50 -6 7 -10 21.70 5.40 6 -7 10 12.20 5.80 -7 7 -10 12.60 5.50 7 -7 10 9.90 5.90 -8 7 -10 43.60 7.00 8 -7 10 30.70 7.20 -9 7 -10 2.00 5.10 9 -7 10 -5.60 5.50 -10 7 -10 -2.50 5.10 10 -7 10 -0.50 4.80 10 -7 10 6.40 5.90 -11 7 -10 6.70 6.30 11 -7 10 1.90 5.60 11 -7 10 -0.40 5.40 -12 7 -10 15.60 7.30 12 -7 10 18.10 6.90 12 -7 10 17.30 6.90 9 6 -10 9.50 8.00 -9 -6 10 18.40 7.10 8 6 -10 57.79 10.10 -8 -6 10 65.29 8.90 7 6 -10 211.98 14.50 -7 -6 10 207.98 13.30 6 6 -10 17.80 7.00 -6 -6 10 17.60 6.00 5 6 -10 9.20 6.30 -5 -6 10 7.10 5.40 4 6 -10 2.10 5.30 -4 -6 10 8.80 5.60 3 6 -10 3.40 4.80 3 6 -10 2.30 3.90 -3 -6 10 -1.30 4.30 2 6 -10 3.90 3.80 2 6 -10 -3.30 4.30 -2 -6 10 3.80 4.70 1 6 -10 19.10 4.40 1 6 -10 14.10 5.30 -1 -6 10 11.00 5.10 0 6 -10 67.69 6.20 0 6 -10 53.39 6.90 0 -6 10 56.89 7.00 -1 6 -10 12.90 4.30 -1 6 -10 16.90 4.80 1 -6 10 3.10 4.50 -2 6 -10 99.29 8.10 -2 6 -10 103.59 7.30 2 -6 10 106.29 8.80 -3 6 -10 1.80 3.60 -3 6 -10 1.70 3.80 3 -6 10 4.20 5.20 -4 6 -10 113.39 8.00 -4 6 -10 112.29 7.60 4 -6 10 105.69 8.80 -5 6 -10 46.80 6.20 5 -6 10 50.69 7.20 -6 6 -10 -1.80 4.10 6 -6 10 1.00 3.50 6 -6 10 1.40 5.30 -7 6 -10 31.30 5.60 7 -6 10 24.50 6.40 7 -6 10 26.00 5.00 -8 6 -10 58.89 7.60 8 -6 10 47.00 7.30 8 -6 10 46.60 6.30 -9 6 -10 -1.40 4.70 9 -6 10 -5.80 4.70 9 -6 10 1.00 5.20 -10 6 -10 20.10 6.30 10 -6 10 20.80 6.40 10 -6 10 43.20 7.60 -11 6 -10 156.38 12.50 11 -6 10 176.08 12.50 11 -6 10 173.68 11.80 -12 6 -10 43.60 8.90 12 -6 10 54.19 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16 36.80 11.70 6 5 -16 26.00 8.10 -6 -5 16 29.00 9.10 5 5 -16 25.30 8.00 -5 -5 16 26.70 8.30 4 5 -16 -5.20 6.10 -4 -5 16 7.50 6.90 3 5 -16 41.70 8.80 -3 -5 16 28.80 7.80 2 5 -16 15.90 7.30 -2 -5 16 24.60 7.40 1 5 -16 28.90 7.70 -1 -5 16 28.10 7.60 0 5 -16 9.10 6.20 0 -5 16 0.40 6.40 -1 5 -16 13.60 6.50 1 -5 16 17.90 6.60 -2 5 -16 -2.80 5.40 2 -5 16 0.40 5.80 3 -5 16 11.00 6.60 -4 5 -16 -3.20 4.90 4 -5 16 -0.30 5.90 -5 5 -16 28.50 6.70 5 -5 16 16.10 6.80 -6 5 -16 2.50 5.70 -7 5 -16 23.20 7.00 7 4 -16 49.99 9.90 -7 -4 16 27.50 9.00 6 4 -16 12.00 7.50 -6 -4 16 16.10 7.50 5 4 -16 50.39 8.90 -5 -4 16 75.49 10.20 4 4 -16 56.99 9.90 -4 -4 16 59.89 9.10 3 4 -16 -2.30 5.50 -3 -4 16 -3.40 5.50 2 4 -16 5.90 6.40 -2 -4 16 14.30 6.50 1 4 -16 9.20 6.60 -1 -4 16 -3.50 5.30 0 4 -16 58.09 9.00 0 -4 16 48.00 8.10 -1 4 -16 6.00 6.00 1 -4 16 17.20 6.60 -2 4 -16 0.30 5.40 2 -4 16 -11.30 5.20 3 -4 16 -0.70 5.60 -4 4 -16 2.60 5.30 4 -4 16 10.00 6.10 -5 4 -16 43.50 7.30 -6 4 -16 17.70 6.50 -7 4 -16 71.89 9.40 7 3 -16 40.00 8.70 -7 -3 16 39.50 8.80 6 3 -16 12.60 7.70 -6 -3 16 22.20 7.80 5 3 -16 1.60 5.80 -5 -3 16 -2.60 5.60 4 3 -16 16.00 7.20 -4 -3 16 13.70 6.70 3 3 -16 2.20 5.70 -3 -3 16 -3.50 5.30 2 3 -16 11.70 6.90 -2 -3 16 7.30 5.90 1 3 -16 66.59 9.30 -1 -3 16 79.49 8.80 0 3 -16 11.60 6.50 0 -3 16 8.00 5.40 -1 3 -16 118.89 11.40 1 -3 16 130.69 10.70 -2 3 -16 -1.00 5.60 2 -3 16 -1.00 5.50 -5 3 -16 -1.30 5.20 -6 3 -16 40.20 7.70 8 2 -16 19.00 7.90 -8 -2 16 30.80 8.20 7 2 -16 3.10 6.60 -7 -2 16 8.80 6.70 6 2 -16 11.80 7.10 -6 -2 16 36.70 7.90 5 2 -16 21.60 7.10 -5 -2 16 19.30 7.10 4 2 -16 4.90 6.20 -4 -2 16 17.50 6.60 3 2 -16 19.70 7.00 -3 -2 16 38.60 7.20 2 2 -16 -6.90 5.70 -2 -2 16 -1.30 5.20 1 2 -16 79.99 9.60 -1 -2 16 73.39 8.50 0 2 -16 14.30 6.30 0 -2 16 26.00 6.50 -1 2 -16 66.29 9.00 1 -2 16 82.79 8.80 -2 2 -16 33.00 7.30 3 -2 16 146.59 11.10 4 -2 16 36.00 7.10 -5 2 -16 -2.80 5.00 5 -2 16 1.10 5.30 -6 2 -16 6.90 5.90 6 -2 16 2.20 6.40 8 1 -16 7.30 6.40 -8 -1 16 -4.10 5.90 7 1 -16 27.90 8.20 -7 -1 16 59.89 9.20 6 1 -16 21.90 7.60 -6 -1 16 38.10 7.70 5 1 -16 17.10 6.80 -5 -1 16 -5.60 5.50 4 1 -16 5.70 6.40 -4 -1 16 12.00 5.80 3 1 -16 30.60 7.70 -3 -1 16 42.50 7.20 2 1 -16 8.30 6.60 -2 -1 16 -0.80 4.90 1 1 -16 -0.80 5.80 -1 -1 16 1.70 4.90 -1 -1 16 -3.90 4.80 0 1 -16 33.70 7.80 0 -1 16 44.70 9.00 0 -1 16 40.60 6.70 -1 1 -16 3.20 5.50 1 -1 16 -7.10 4.60 -2 1 -16 58.99 8.70 2 -1 16 57.99 7.80 3 -1 16 27.90 6.80 4 -1 16 2.50 5.60 -5 1 -16 -9.10 4.80 5 -1 16 0.20 5.70 -6 1 -16 -1.10 6.10 6 -1 16 -0.30 6.20 8 0 -16 64.89 10.30 -8 0 16 61.39 9.50 7 0 -16 181.68 14.40 -7 0 16 164.48 13.40 6 0 -16 -3.80 5.60 -6 0 16 -0.20 5.60 5 0 -16 11.40 6.50 -5 0 16 2.30 5.40 4 0 -16 -3.40 5.90 -4 0 16 -4.60 5.10 -4 0 16 1.70 5.40 3 0 -16 91.09 10.10 -3 0 16 115.39 9.60 -3 0 16 99.39 9.30 2 0 -16 -4.70 5.50 -2 0 16 0.90 4.90 -2 0 16 2.30 5.10 1 0 -16 29.80 7.40 -1 0 16 21.10 6.20 0 0 -16 15.40 6.80 0 0 16 21.20 6.10 -1 0 -16 10.70 6.00 1 0 16 6.70 5.30 -2 0 -16 22.20 7.20 2 0 16 11.60 5.90 3 0 16 8.20 5.80 4 0 16 6.10 6.20 5 0 16 35.20 7.70 8 -1 -16 37.90 8.70 -8 1 16 27.30 7.20 7 -1 -16 47.90 9.50 -7 1 16 47.20 8.00 -7 1 16 47.40 7.80 6 -1 -16 7.20 6.10 -6 1 16 6.20 5.90 -6 1 16 9.00 5.80 5 -1 -16 20.70 7.00 -5 1 16 19.00 5.80 -5 1 16 20.90 6.40 4 -1 -16 6.00 6.40 -4 1 16 -8.80 4.70 -4 1 16 -2.30 4.80 3 -1 -16 71.09 9.50 -3 1 16 97.69 9.10 -3 1 16 90.09 11.90 2 -1 -16 29.60 7.40 -2 1 16 10.40 5.60 1 -1 -16 40.60 8.20 -1 1 16 31.50 7.10 0 -1 -16 7.20 6.00 0 1 16 7.40 5.40 -1 -1 -16 60.19 9.00 1 1 16 25.50 7.00 -2 -1 -16 44.30 8.30 2 1 16 39.50 7.80 3 1 16 23.70 7.20 4 1 16 6.50 6.40 8 -2 -16 33.50 8.30 -8 2 16 22.70 7.00 -8 2 16 9.60 6.80 7 -2 -16 3.40 6.60 -7 2 16 3.50 5.50 -7 2 16 -4.30 5.40 6 -2 -16 31.20 8.10 -6 2 16 12.40 5.60 -6 2 16 14.10 6.40 5 -2 -16 5.30 6.20 -5 2 16 18.20 5.90 -5 2 16 14.10 6.40 4 -2 -16 27.70 7.90 -4 2 16 27.30 6.90 3 -2 -16 102.79 11.50 -3 2 16 118.29 10.30 2 -2 -16 29.20 7.70 -2 2 16 18.90 6.20 1 -2 -16 10.90 6.80 -1 2 16 10.80 5.90 0 -2 -16 36.60 8.10 0 2 16 19.50 6.50 -1 -2 -16 6.10 6.10 1 2 16 1.10 5.90 -2 -2 -16 14.70 6.60 2 2 16 5.30 6.30 3 2 16 -2.60 5.50 8 -3 -16 10.90 7.20 -8 3 16 -3.40 6.10 -8 3 16 10.00 5.90 7 -3 -16 57.39 9.60 -7 3 16 47.00 8.20 -7 3 16 37.10 7.20 6 -3 -16 1.40 5.80 -6 3 16 -1.20 5.60 5 -3 -16 1.20 5.90 -5 3 16 9.50 6.50 4 -3 -16 1.90 6.50 -4 3 16 -0.70 5.50 3 -3 -16 18.90 7.50 -3 3 16 10.30 6.60 2 -3 -16 230.98 15.60 -2 3 16 261.77 13.90 1 -3 -16 2.00 6.40 -1 3 16 12.20 6.30 0 -3 -16 22.20 7.60 0 3 16 21.30 7.20 -1 -3 -16 -8.00 5.80 1 3 16 0.90 5.80 -2 -3 -16 89.09 10.70 2 3 16 75.09 9.90 8 -4 -16 10.50 7.20 -8 4 16 -10.70 5.90 -8 4 16 -3.90 5.30 7 -4 -16 16.30 7.20 -7 4 16 19.00 7.30 6 -4 -16 7.30 6.70 -6 4 16 0.50 6.50 5 -4 -16 -2.90 5.90 -5 4 16 -5.30 6.00 4 -4 -16 7.30 6.80 -4 4 16 -5.40 5.60 3 -4 -16 -1.00 5.90 -3 4 16 10.20 6.80 2 -4 -16 118.69 12.40 -2 4 16 136.99 11.80 1 -4 -16 12.70 7.10 -1 4 16 4.40 6.10 0 -4 -16 57.39 9.70 0 4 16 57.19 8.70 -1 -4 -16 59.89 9.70 1 4 16 68.79 9.40 7 -5 -16 1.40 6.40 -7 5 16 -7.30 6.00 6 -5 -16 17.20 7.40 -6 5 16 2.80 6.80 5 -5 -16 7.80 6.60 -5 5 16 12.50 6.80 4 -5 -16 109.39 12.70 -4 5 16 104.99 10.70 3 -5 -16 26.60 7.90 -3 5 16 29.20 7.70 2 -5 -16 39.70 9.10 -2 5 16 37.00 8.40 1 -5 -16 9.40 7.10 -1 5 16 0.10 6.20 5 -6 -16 -4.10 6.50 -5 6 16 4.40 6.60 4 -6 -16 59.39 10.30 -4 6 16 37.70 8.30 3 -6 -16 18.20 8.30 -3 6 16 4.10 6.40 0 9 -17 -0.40 7.50 0 -9 17 -3.50 7.70 -1 9 -17 0.50 7.20 1 -9 17 -4.10 7.30 -2 9 -17 14.50 7.60 2 -9 17 10.10 8.00 3 -9 17 24.30 9.00 4 -9 17 -14.20 6.80 2 8 -17 -4.90 6.60 -2 -8 17 -7.30 7.20 1 8 -17 -0.60 7.00 -1 -8 17 1.80 7.00 0 8 -17 58.09 10.30 0 -8 17 42.10 9.80 -1 8 -17 50.59 9.00 1 -8 17 30.00 9.30 -2 8 -17 25.50 7.80 2 -8 17 15.90 8.00 3 -8 17 -10.20 7.00 4 -8 17 -2.90 7.10 -5 8 -17 44.20 8.00 5 -8 17 36.50 9.30 3 7 -17 5.40 6.70 -3 -7 17 -6.00 6.30 2 7 -17 0.90 6.70 -2 -7 17 2.40 7.50 1 7 -17 43.50 9.00 -1 -7 17 20.30 7.70 0 7 -17 39.30 8.60 0 -7 17 55.39 9.60 -1 7 -17 22.20 7.90 1 -7 17 25.00 8.50 -2 7 -17 4.80 6.90 2 -7 17 2.50 7.00 3 -7 17 -13.80 6.30 4 -7 17 -16.40 6.30 -5 7 -17 20.80 6.50 5 -7 17 24.20 8.40 -6 7 -17 240.18 13.90 6 -7 17 274.27 16.40 4 6 -17 -3.80 6.10 -4 -6 17 -16.80 6.10 3 6 -17 1.60 6.40 -3 -6 17 -4.90 6.90 2 6 -17 23.90 8.10 -2 -6 17 27.10 8.40 1 6 -17 49.70 9.00 -1 -6 17 31.80 8.20 0 6 -17 -3.50 5.80 0 -6 17 -12.70 5.70 -1 6 -17 52.79 9.00 1 -6 17 36.20 8.70 -2 6 -17 5.20 6.10 2 -6 17 -3.10 6.40 3 -6 17 2.00 6.70 4 -6 17 78.69 10.20 -5 6 -17 1.00 5.30 5 -6 17 11.60 7.30 -6 6 -17 194.68 13.30 6 -6 17 211.38 15.80 5 5 -17 3.40 6.90 -5 -5 17 -2.50 6.50 4 5 -17 5.50 6.90 -4 -5 17 4.30 6.60 3 5 -17 13.60 7.30 -3 -5 17 8.10 6.80 2 5 -17 8.60 7.10 -2 -5 17 7.10 6.60 1 5 -17 8.80 6.90 -1 -5 17 18.10 7.60 0 5 -17 4.90 6.50 0 -5 17 -1.40 6.30 -1 5 -17 3.30 6.00 1 -5 17 1.00 6.60 -2 5 -17 2.10 6.00 2 -5 17 -5.50 6.10 3 -5 17 2.00 6.50 4 -5 17 9.50 6.80 -5 5 -17 17.40 8.70 -6 5 -17 112.99 10.70 6 4 -17 30.50 8.70 -6 -4 17 23.50 8.60 5 4 -17 14.40 6.90 -5 -4 17 1.70 6.90 4 4 -17 4.70 7.20 -4 -4 17 7.50 7.10 3 4 -17 2.00 6.10 -3 -4 17 -3.20 6.10 2 4 -17 8.30 6.60 -2 -4 17 -6.60 5.50 1 4 -17 2.00 6.40 -1 -4 17 0.40 6.10 0 4 -17 3.40 6.20 0 -4 17 -2.30 6.00 -1 4 -17 5.10 6.30 1 -4 17 7.70 6.40 -2 4 -17 28.90 7.80 2 -4 17 14.70 6.60 3 -4 17 -1.50 5.80 -6 4 -17 3.90 5.90 6 3 -17 -7.30 6.30 -6 -3 17 -1.20 6.90 5 3 -17 42.60 8.70 -5 -3 17 33.20 8.30 4 3 -17 4.30 6.20 -4 -3 17 1.70 6.20 3 3 -17 36.10 8.60 -3 -3 17 30.80 7.80 2 3 -17 18.80 7.20 -2 -3 17 16.70 6.80 1 3 -17 44.90 8.80 -1 -3 17 55.39 8.10 0 3 -17 17.70 7.20 0 -3 17 25.00 7.00 -1 3 -17 -3.30 6.30 1 -3 17 3.20 5.90 -2 3 -17 -7.80 5.90 2 -3 17 -4.30 7.20 -7 -2 17 14.70 7.70 6 2 -17 5.80 6.60 -6 -2 17 9.90 7.30 5 2 -17 6.70 6.60 -5 -2 17 9.20 6.90 4 2 -17 26.70 7.90 -4 -2 17 19.70 7.30 3 2 -17 18.80 7.50 -3 -2 17 27.50 7.00 2 2 -17 30.50 8.00 -2 -2 17 26.80 6.70 1 2 -17 29.20 7.70 -1 -2 17 18.90 6.60 0 2 -17 8.90 6.40 0 -2 17 1.50 5.60 -1 2 -17 2.90 6.10 -2 2 -17 27.40 7.40 5 -2 17 -5.60 8.20 7 1 -17 1.40 6.80 -7 -1 17 2.20 6.60 6 1 -17 19.30 7.30 -6 -1 17 13.40 6.90 5 1 -17 5.10 6.50 -5 -1 17 5.50 6.20 4 1 -17 139.29 13.60 -4 -1 17 147.99 11.90 3 1 -17 30.50 8.00 -3 -1 17 31.40 7.00 2 1 -17 4.10 6.20 -2 -1 17 -8.20 4.80 1 1 -17 -7.80 5.50 -1 -1 17 0.50 5.90 0 1 -17 54.59 8.90 -1 1 -17 18.90 7.10 1 -1 17 17.90 6.20 -2 1 -17 62.79 9.40 2 -1 17 69.39 8.60 3 -1 17 -0.20 5.60 4 -1 17 6.00 5.90 7 0 -17 4.10 6.40 -7 0 17 0.80 6.30 6 0 -17 1.40 6.50 -6 0 17 8.30 6.40 5 0 -17 -3.30 5.90 -5 0 17 5.10 5.90 4 0 -17 61.89 9.80 -4 0 17 87.39 9.50 3 0 -17 -3.50 5.70 -3 0 17 13.40 5.90 2 0 -17 44.10 8.60 -2 0 17 66.09 8.10 1 0 -17 4.10 6.30 -1 0 17 1.10 5.10 0 0 -17 62.39 9.40 0 0 17 55.19 7.80 -1 0 -17 -5.30 5.60 1 0 17 1.60 5.40 -2 0 -17 62.69 9.40 2 0 17 50.69 7.90 3 0 17 6.70 6.00 4 0 17 0.20 5.70 7 -1 -17 -6.00 6.20 -7 1 17 1.40 5.40 6 -1 -17 45.00 9.20 -6 1 17 40.00 7.80 5 -1 -17 1.40 6.20 -5 1 17 4.70 5.70 -5 1 17 -11.20 5.10 4 -1 -17 30.70 8.20 -4 1 17 40.90 9.00 -4 1 17 31.80 7.00 3 -1 -17 40.80 8.60 -3 1 17 41.80 7.70 2 -1 -17 48.70 8.90 -2 1 17 47.70 7.70 1 -1 -17 4.60 6.20 -1 1 17 6.80 5.90 0 -1 -17 60.09 9.50 0 1 17 67.39 8.90 -1 -1 -17 34.20 8.10 1 1 17 20.30 6.50 -2 -1 -17 9.70 6.90 2 1 17 7.40 6.10 3 1 17 26.20 7.60 7 -2 -17 37.30 9.30 -7 2 17 39.80 7.70 -7 2 17 43.80 8.40 6 -2 -17 43.60 9.00 -6 2 17 33.50 7.30 -6 2 17 45.20 8.50 5 -2 -17 6.20 6.80 -5 2 17 2.50 6.00 4 -2 -17 6.70 6.50 -4 2 17 -3.80 5.50 3 -2 -17 11.40 7.20 -3 2 17 8.60 6.10 2 -2 -17 15.00 7.40 -2 2 17 23.00 7.20 1 -2 -17 44.40 8.90 -1 2 17 49.99 8.30 0 -2 -17 45.80 8.90 0 2 17 44.30 8.10 -1 -2 -17 99.39 11.60 1 2 17 118.69 11.00 -2 -2 -17 36.20 8.50 2 2 17 26.10 7.10 6 -3 -17 53.09 9.90 -6 3 17 40.10 8.20 5 -3 -17 4.80 6.70 -5 3 17 11.40 6.70 4 -3 -17 9.90 7.00 -4 3 17 -3.40 5.90 3 -3 -17 15.60 7.30 -3 3 17 8.50 6.30 2 -3 -17 6.30 6.90 -2 3 17 6.00 6.60 1 -3 -17 3.20 6.50 -1 3 17 4.40 6.70 0 -3 -17 12.10 7.10 0 3 17 6.00 6.40 5 -4 -17 0.00 7.10 -5 4 17 6.10 6.60 4 -4 -17 4.30 7.00 -4 4 17 3.40 6.40 3 -4 -17 28.30 9.10 -3 4 17 16.30 7.00 2 -4 -17 13.00 7.60 -2 4 17 14.20 7.00 1 -4 -17 8.80 7.10 -1 4 17 1.20 6.40 2 -8 18 52.49 10.10 1 7 -18 40.50 9.30 -1 -7 18 22.00 9.00 0 7 -18 -0.60 6.70 0 -7 18 -2.60 7.30 -1 7 -18 9.40 7.00 1 -7 18 -12.60 6.70 -2 7 -18 23.10 8.90 2 -7 18 25.30 8.90 3 -7 18 45.20 9.60 2 6 -18 6.20 7.40 -2 -6 18 -1.20 7.30 1 6 -18 14.00 7.60 -1 -6 18 1.70 7.20 0 6 -18 24.40 8.20 0 -6 18 22.30 8.40 -1 6 -18 16.10 7.70 1 -6 18 1.70 7.30 -2 6 -18 3.80 6.70 2 -6 18 -0.50 7.10 3 -6 18 120.59 12.20 4 -6 18 -0.30 6.90 3 5 -18 88.89 11.80 -3 -5 18 93.99 11.10 2 5 -18 5.90 7.70 -2 -5 18 9.40 7.30 1 5 -18 5.00 6.90 -1 -5 18 8.80 7.10 0 5 -18 4.00 7.00 0 -5 18 -4.20 6.50 -1 5 -18 8.90 6.90 1 -5 18 0.80 6.70 -2 5 -18 3.00 6.50 2 -5 18 -4.60 6.50 3 -5 18 8.90 7.10 4 4 -18 29.80 9.00 -4 -4 18 18.80 8.00 3 4 -18 39.00 9.40 -3 -4 18 38.40 9.00 2 4 -18 -1.90 6.30 -2 -4 18 3.70 6.70 1 4 -18 -8.20 6.30 -1 -4 18 -1.30 6.10 0 4 -18 14.40 7.40 0 -4 18 17.40 7.30 -1 4 -18 15.90 7.20 1 -4 18 -10.00 5.90 -2 4 -18 5.60 6.80 2 -4 18 -8.10 5.80 5 3 -18 1.30 6.90 -5 -3 18 4.30 7.00 4 3 -18 36.70 8.90 -4 -3 18 17.30 7.40 3 3 -18 7.00 6.90 -3 -3 18 20.80 7.60 2 3 -18 87.99 11.30 -2 -3 18 99.99 10.70 1 3 -18 3.00 6.70 -1 -3 18 -10.50 5.70 0 3 -18 11.40 7.40 0 -3 18 4.20 6.50 -1 3 -18 68.09 10.30 1 -3 18 67.99 11.70 -2 3 -18 4.00 7.30 5 2 -18 10.60 7.80 -5 -2 18 -5.50 6.50 4 2 -18 32.80 8.30 -4 -2 18 34.70 8.00 3 2 -18 6.70 6.90 -3 -2 18 10.50 6.60 2 2 -18 89.39 11.50 -2 -2 18 74.99 9.60 1 2 -18 -1.20 6.60 -1 -2 18 -6.70 5.40 0 2 -18 0.10 6.20 -1 2 -18 18.20 7.40 -2 2 -18 10.00 7.90 5 1 -18 44.10 9.60 -5 -1 18 63.69 9.40 4 1 -18 16.70 7.20 -4 -1 18 19.30 7.10 3 1 -18 13.70 7.40 -3 -1 18 4.60 6.00 2 1 -18 57.39 9.60 -2 -1 18 65.09 9.60 1 1 -18 77.59 10.50 0 1 -18 -3.90 6.50 -1 1 -18 60.29 9.50 -2 1 -18 81.09 14.00 5 0 -18 1.50 6.90 -5 0 18 7.60 6.10 4 0 -18 -0.10 6.50 -4 0 18 1.20 5.80 3 0 -18 43.30 9.40 2 0 -18 6.60 6.70 1 0 -18 155.08 13.70 0 0 -18 2.60 6.60 0 0 18 11.70 6.00 -1 0 -18 122.79 12.30 1 0 18 98.09 10.10 2 0 18 2.10 6.30 5 -1 -18 20.00 8.20 -5 1 18 27.00 11.40 4 -1 -18 41.60 9.30 3 -1 -18 46.80 9.70 -3 1 18 62.29 8.90 2 -1 -18 17.90 7.60 -2 1 18 19.00 7.20 1 -1 -18 89.09 11.20 -1 1 18 102.39 10.40 0 -1 -18 22.90 7.40 0 1 18 30.90 7.20 -1 -1 -18 13.40 7.30 1 1 18 5.30 6.00 4 -2 -18 3.70 7.00 -4 2 18 7.10 6.50 3 -2 -18 -4.50 6.40 -3 2 18 1.80 6.20 2 -2 -18 10.50 7.40 -2 2 18 19.00 7.00 1 -2 -18 0.60 7.10 -1 2 18 9.20 6.40 1 4 -19 7.40 7.40 -1 -4 19 -10.10 6.20 0 4 -19 -0.20 7.40 0 -4 19 3.40 6.60 -1 4 -19 38.50 8.80 1 -4 19 28.80 8.50 2 3 -19 -1.60 6.70 -2 -3 19 -5.20 6.10 1 3 -19 19.40 8.30 -1 -3 19 25.90 8.10 0 3 -19 17.00 7.60 0 -3 19 -2.00 8.00 -1 3 -19 14.50 7.80 2 2 -19 17.20 8.30 -2 -2 19 6.50 6.70 1 2 -19 4.30 7.60 0 2 -19 41.90 9.70 2 1 -19 103.09 12.70 1 1 -19 -1.50 6.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 15091 #===END data_tBuBrettPhos _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'tBuBrettPhos' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 O2 P' _chemical_formula_weight 484.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.317(3) _cell_length_b 13.782(2) _cell_length_c 22.811(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5758.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.571 _cell_measurement_theta_max 27.431 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_F_000 2128 _exptl_transmission_factor_min 0.964 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 0.120 _shelx_estimated_absorpt_T_min 0.954 _shelx_estimated_absorpt_T_max 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65543 _diffrn_reflns_av_unetI/netI 0.0156 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.785 _diffrn_reflns_theta_max 27.457 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6574 _reflns_number_gt 5666 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6574 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.60698(2) 0.65926(2) 0.74931(2) 0.01113(10) Uani 1 1 d . . . . . O1 O 0.44917(4) 0.64641(6) 0.80052(3) 0.01720(19) Uani 1 1 d . . . . . O2 O 0.46469(4) 0.55393(6) 0.56551(3) 0.01604(18) Uani 1 1 d . . . . . C1 C 0.51762(6) 0.63694(8) 0.71234(5) 0.0112(2) Uani 1 1 d . . . . . C2 C 0.44942(6) 0.62885(8) 0.74126(5) 0.0124(2) Uani 1 1 d . . . . . C3 C 0.38213(6) 0.63471(9) 0.83155(5) 0.0184(2) Uani 1 1 d . . . . . H3A H 0.346092 0.681086 0.816600 0.028 Uiso 1 1 calc R U . . . H3B H 0.390285 0.646534 0.873405 0.028 Uiso 1 1 calc R U . . . H3C H 0.363941 0.568483 0.825965 0.028 Uiso 1 1 calc R U . . . C4 C 0.38636(6) 0.60361(8) 0.71108(5) 0.0139(2) Uani 1 1 d . . . . . H4 H 0.340678 0.603052 0.730801 0.017 Uiso 1 1 calc R U . . . C5 C 0.39005(6) 0.57914(8) 0.65198(5) 0.0138(2) Uani 1 1 d . . . . . H5 H 0.347224 0.559400 0.631735 0.017 Uiso 1 1 calc R U . . . C6 C 0.45621(6) 0.58358(8) 0.62267(5) 0.0122(2) Uani 1 1 d . . . . . C7 C 0.41042(6) 0.48945(9) 0.54295(5) 0.0176(2) Uani 1 1 d . . . . . H7A H 0.402627 0.436267 0.570772 0.026 Uiso 1 1 calc R U . . . H7B H 0.426850 0.462981 0.505327 0.026 Uiso 1 1 calc R U . . . H7C H 0.364579 0.524900 0.537296 0.026 Uiso 1 1 calc R U . . . C8 C 0.51948(5) 0.61813(7) 0.65109(4) 0.0109(2) Uani 1 1 d . . . . . C9 C 0.58605(6) 0.63479(8) 0.61315(4) 0.0111(2) Uani 1 1 d . . . . . C10 C 0.64330(6) 0.56622(8) 0.61131(5) 0.0119(2) Uani 1 1 d . . . . . C11 C 0.63678(6) 0.46978(8) 0.64328(5) 0.0146(2) Uani 1 1 d . . . . . H11 H 0.601539 0.478906 0.676306 0.017 Uiso 1 1 calc R U . . . C12 C 0.70860(7) 0.43385(10) 0.66946(6) 0.0235(3) Uani 1 1 d . . . . . H12A H 0.741697 0.414411 0.637813 0.035 Uiso 1 1 calc R U . . . H12B H 0.699078 0.378068 0.694984 0.035 Uiso 1 1 calc R U . . . H12C H 0.731120 0.486006 0.692388 0.035 Uiso 1 1 calc R U . . . C13 C 0.60468(7) 0.39312(9) 0.60198(5) 0.0204(3) Uani 1 1 d . . . . . H13A H 0.557247 0.415396 0.587351 0.031 Uiso 1 1 calc R U . . . H13B H 0.598327 0.331966 0.623305 0.031 Uiso 1 1 calc R U . . . H13C H 0.637930 0.382968 0.568890 0.031 Uiso 1 1 calc R U . . . C14 C 0.70454(6) 0.58435(8) 0.57658(5) 0.0140(2) Uani 1 1 d . . . . . H14 H 0.743648 0.539075 0.576876 0.017 Uiso 1 1 calc R U . . . C15 C 0.71011(6) 0.66695(8) 0.54141(4) 0.0132(2) Uani 1 1 d . . . . . C16 C 0.77836(6) 0.68338(9) 0.50409(5) 0.0166(2) Uani 1 1 d . . . . . H16 H 0.821223 0.684635 0.531225 0.020 Uiso 1 1 calc R U . . . C17 C 0.79003(7) 0.59911(11) 0.46102(6) 0.0287(3) Uani 1 1 d . . . . . H17A H 0.749210 0.596606 0.433280 0.043 Uiso 1 1 calc R U . . . H17B H 0.792583 0.537900 0.482786 0.043 Uiso 1 1 calc R U . . . H17C H 0.835731 0.609054 0.439505 0.043 Uiso 1 1 calc R U . . . C18 C 0.77827(7) 0.77892(10) 0.47012(5) 0.0232(3) Uani 1 1 d . . . . . H18A H 0.738445 0.778416 0.441433 0.035 Uiso 1 1 calc R U . . . H18B H 0.824985 0.786621 0.449711 0.035 Uiso 1 1 calc R U . . . H18C H 0.771309 0.833013 0.497445 0.035 Uiso 1 1 calc R U . . . C19 C 0.65169(6) 0.73106(8) 0.54142(5) 0.0137(2) Uani 1 1 d . . . . . H19 H 0.653831 0.786537 0.516771 0.016 Uiso 1 1 calc R U . . . C20 C 0.58973(6) 0.71716(8) 0.57635(5) 0.0122(2) Uani 1 1 d . . . . . C21 C 0.52785(6) 0.79079(8) 0.56968(5) 0.0161(2) Uani 1 1 d . . . . . H21 H 0.493983 0.783311 0.603765 0.019 Uiso 1 1 calc R U . . . C22 C 0.55478(7) 0.89656(9) 0.56814(5) 0.0217(3) Uani 1 1 d . . . . . H22A H 0.587121 0.908379 0.601614 0.033 Uiso 1 1 calc R U . . . H22B H 0.512817 0.940540 0.570237 0.033 Uiso 1 1 calc R U . . . H22C H 0.581540 0.908104 0.531602 0.033 Uiso 1 1 calc R U . . . C23 C 0.48468(6) 0.77052(9) 0.51317(5) 0.0223(3) Uani 1 1 d . . . . . H23A H 0.517388 0.775601 0.479309 0.034 Uiso 1 1 calc R U . . . H23B H 0.445160 0.818025 0.509329 0.034 Uiso 1 1 calc R U . . . H23C H 0.463983 0.705008 0.514858 0.034 Uiso 1 1 calc R U . . . C24 C 0.60499(6) 0.79207(8) 0.76956(5) 0.0148(2) Uani 1 1 d . . . . . C25 C 0.60617(7) 0.84380(8) 0.70988(5) 0.0192(3) Uani 1 1 d . . . . . H25A H 0.560685 0.830135 0.688816 0.029 Uiso 1 1 calc R U . . . H25B H 0.647708 0.820334 0.686818 0.029 Uiso 1 1 calc R U . . . H25C H 0.610853 0.913913 0.715960 0.029 Uiso 1 1 calc R U . . . C26 C 0.67644(7) 0.81668(9) 0.80167(5) 0.0200(2) Uani 1 1 d . . . . . H26A H 0.682085 0.887295 0.803877 0.030 Uiso 1 1 calc R U . . . H26B H 0.717783 0.788825 0.780204 0.030 Uiso 1 1 calc R U . . . H26C H 0.675006 0.789612 0.841374 0.030 Uiso 1 1 calc R U . . . C27 C 0.53951(7) 0.83057(9) 0.80414(5) 0.0193(2) Uani 1 1 d . . . . . H27A H 0.537612 0.798764 0.842539 0.029 Uiso 1 1 calc R U . . . H27B H 0.494455 0.816788 0.782520 0.029 Uiso 1 1 calc R U . . . H27C H 0.544527 0.900797 0.809517 0.029 Uiso 1 1 calc R U . . . C28 C 0.61197(6) 0.58252(8) 0.81916(5) 0.0150(2) Uani 1 1 d . . . . . C29 C 0.57590(7) 0.48363(9) 0.80724(5) 0.0188(2) Uani 1 1 d . . . . . H29A H 0.585946 0.439589 0.839984 0.028 Uiso 1 1 calc R U . . . H29B H 0.595748 0.456059 0.770985 0.028 Uiso 1 1 calc R U . . . H29C H 0.523038 0.492275 0.803147 0.028 Uiso 1 1 calc R U . . . C30 C 0.69475(6) 0.56474(9) 0.82694(5) 0.0197(2) Uani 1 1 d . . . . . H30A H 0.719826 0.627061 0.831654 0.030 Uiso 1 1 calc R U . . . H30B H 0.713911 0.531251 0.792306 0.030 Uiso 1 1 calc R U . . . H30C H 0.702972 0.524631 0.861795 0.030 Uiso 1 1 calc R U . . . C31 C 0.58313(6) 0.62316(9) 0.87734(5) 0.0188(2) Uani 1 1 d . . . . . H31A H 0.530747 0.636375 0.873784 0.028 Uiso 1 1 calc R U . . . H31B H 0.608962 0.683442 0.886774 0.028 Uiso 1 1 calc R U . . . H31C H 0.591270 0.575633 0.908614 0.028 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.00956(16) 0.01386(17) 0.00998(16) -0.00010(9) 0.00012(9) -0.00135(9) O1 0.0127(4) 0.0283(4) 0.0106(4) -0.0034(3) 0.0044(3) -0.0044(3) O2 0.0141(4) 0.0239(4) 0.0101(4) -0.0037(3) -0.0001(3) -0.0050(3) C1 0.0107(5) 0.0116(5) 0.0112(5) -0.0002(4) 0.0002(4) -0.0008(4) C2 0.0126(5) 0.0134(5) 0.0111(5) -0.0008(4) 0.0012(4) -0.0004(4) C3 0.0167(5) 0.0231(6) 0.0155(5) -0.0042(4) 0.0079(4) -0.0039(5) C4 0.0100(5) 0.0168(5) 0.0150(5) -0.0004(4) 0.0023(4) -0.0001(4) C5 0.0103(5) 0.0166(5) 0.0145(5) 0.0006(4) -0.0014(4) -0.0010(4) C6 0.0135(5) 0.0136(5) 0.0094(5) 0.0003(4) -0.0004(4) 0.0002(4) C7 0.0178(5) 0.0209(6) 0.0140(5) -0.0033(4) -0.0025(4) -0.0037(4) C8 0.0101(5) 0.0111(5) 0.0116(5) 0.0011(4) 0.0010(4) 0.0010(4) C9 0.0105(5) 0.0148(5) 0.0079(5) -0.0013(4) 0.0000(4) -0.0020(4) C10 0.0121(5) 0.0143(5) 0.0093(5) -0.0005(4) -0.0017(4) 0.0000(4) C11 0.0146(5) 0.0158(5) 0.0133(5) 0.0020(4) 0.0022(4) 0.0026(4) C12 0.0211(6) 0.0256(6) 0.0237(6) 0.0078(5) -0.0028(5) 0.0060(5) C13 0.0249(6) 0.0161(5) 0.0203(6) 0.0008(5) 0.0024(4) -0.0012(5) C14 0.0109(5) 0.0178(5) 0.0133(5) -0.0019(4) 0.0004(4) 0.0017(4) C15 0.0098(5) 0.0194(6) 0.0103(5) -0.0023(4) 0.0003(4) -0.0022(4) C16 0.0113(5) 0.0249(6) 0.0136(5) -0.0002(4) 0.0027(4) -0.0022(4) C17 0.0242(6) 0.0338(7) 0.0281(7) -0.0088(6) 0.0141(5) -0.0041(5) C18 0.0160(6) 0.0325(7) 0.0210(6) 0.0071(5) 0.0044(4) -0.0041(5) C19 0.0147(5) 0.0155(5) 0.0108(5) 0.0011(4) 0.0008(4) -0.0015(4) C20 0.0115(5) 0.0144(5) 0.0107(5) -0.0015(4) -0.0003(4) 0.0006(4) C21 0.0152(5) 0.0180(6) 0.0151(5) 0.0051(4) 0.0041(4) 0.0049(4) C22 0.0275(6) 0.0174(6) 0.0202(6) 0.0038(4) 0.0049(5) 0.0053(5) C23 0.0152(6) 0.0285(6) 0.0234(6) 0.0069(5) -0.0030(5) 0.0030(5) C24 0.0143(5) 0.0149(5) 0.0152(5) -0.0013(4) -0.0001(4) -0.0025(4) C25 0.0225(6) 0.0164(6) 0.0189(6) 0.0021(4) -0.0003(4) -0.0028(4) C26 0.0194(6) 0.0201(6) 0.0206(6) -0.0019(4) -0.0032(4) -0.0060(5) C27 0.0202(6) 0.0176(6) 0.0202(6) -0.0043(4) 0.0021(4) 0.0008(4) C28 0.0136(5) 0.0198(6) 0.0117(5) 0.0025(4) -0.0009(4) -0.0012(4) C29 0.0219(6) 0.0180(6) 0.0165(5) 0.0032(4) -0.0006(4) -0.0032(4) C30 0.0158(5) 0.0260(6) 0.0172(5) 0.0053(5) -0.0028(4) 0.0011(5) C31 0.0182(6) 0.0267(6) 0.0113(5) 0.0003(4) -0.0007(4) -0.0030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.8668(11) . ? P1 C24 1.8882(12) . ? P1 C28 1.9146(12) . ? O1 C2 1.3732(13) . ? O1 C3 1.4267(13) . ? O2 C6 1.3752(13) . ? O2 C7 1.4292(13) . ? C1 C2 1.4171(14) . ? C1 C8 1.4216(15) . ? C2 C4 1.3890(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.3913(16) . ? C4 H4 0.9500 . ? C5 C6 1.3854(15) . ? C5 H5 0.9500 . ? C6 C8 1.4106(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.5128(14) . ? C9 C10 1.4123(15) . ? C9 C20 1.4134(15) . ? C10 C14 1.3957(15) . ? C10 C11 1.5208(15) . ? C11 C12 1.5274(16) . ? C11 C13 1.5328(16) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.3964(16) . ? C14 H14 0.9500 . ? C15 C19 1.3878(16) . ? C15 C16 1.5292(14) . ? C16 C18 1.5279(17) . ? C16 C17 1.5363(17) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.3999(15) . ? C19 H19 0.9500 . ? C20 C21 1.5289(15) . ? C21 C23 1.5379(16) . ? C21 C22 1.5394(17) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C27 1.5305(16) . ? C24 C25 1.5369(16) . ? C24 C26 1.5375(15) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.5343(16) . ? C28 C29 1.5388(16) . ? C28 C30 1.5462(16) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C24 104.68(5) . . ? C1 P1 C28 109.06(5) . . ? C24 P1 C28 109.44(5) . . ? C2 O1 C3 118.12(9) . . ? C6 O2 C7 116.59(8) . . ? C2 C1 C8 117.67(9) . . ? C2 C1 P1 125.14(8) . . ? C8 C1 P1 116.94(7) . . ? O1 C2 C4 121.96(10) . . ? O1 C2 C1 116.57(9) . . ? C4 C2 C1 121.47(10) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 120.04(10) . . ? C2 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.96(10) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? O2 C6 C5 122.90(10) . . ? O2 C6 C8 116.31(9) . . ? C5 C6 C8 120.78(10) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C1 119.57(9) . . ? C6 C8 C9 116.78(9) . . ? C1 C8 C9 123.64(9) . . ? C10 C9 C20 118.97(9) . . ? C10 C9 C8 120.93(9) . . ? C20 C9 C8 120.00(9) . . ? C14 C10 C9 119.59(10) . . ? C14 C10 C11 119.46(9) . . ? C9 C10 C11 120.81(9) . . ? C10 C11 C12 113.78(9) . . ? C10 C11 C13 109.75(9) . . ? C12 C11 C13 110.32(10) . . ? C10 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C13 C11 H11 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 122.05(10) . . ? C10 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C19 C15 C14 117.55(10) . . ? C19 C15 C16 122.42(10) . . ? C14 C15 C16 120.02(10) . . ? C18 C16 C15 114.15(9) . . ? C18 C16 C17 109.11(10) . . ? C15 C16 C17 110.97(9) . . ? C18 C16 H16 107.4 . . ? C15 C16 H16 107.4 . . ? C17 C16 H16 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 122.56(10) . . ? C15 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C9 119.11(10) . . ? C19 C20 C21 116.97(9) . . ? C9 C20 C21 123.84(9) . . ? C20 C21 C23 110.12(9) . . ? C20 C21 C22 113.16(10) . . ? C23 C21 C22 108.52(9) . . ? C20 C21 H21 108.3 . . ? C23 C21 H21 108.3 . . ? C22 C21 H21 108.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 C25 107.86(9) . . ? C27 C24 C26 110.19(10) . . ? C25 C24 C26 107.92(9) . . ? C27 C24 P1 118.51(8) . . ? C25 C24 P1 103.45(7) . . ? C26 C24 P1 108.30(8) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C29 109.17(9) . . ? C31 C28 C30 107.22(9) . . ? C29 C28 C30 107.51(9) . . ? C31 C28 P1 120.11(8) . . ? C29 C28 P1 108.77(8) . . ? C30 C28 P1 103.29(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C24 P1 C1 C2 -75.32(10) . . . . ? C28 P1 C1 C2 41.72(11) . . . . ? C24 P1 C1 C8 110.56(9) . . . . ? C28 P1 C1 C8 -132.40(8) . . . . ? C3 O1 C2 C4 2.22(16) . . . . ? C3 O1 C2 C1 -177.25(10) . . . . ? C8 C1 C2 O1 179.37(9) . . . . ? P1 C1 C2 O1 5.29(14) . . . . ? C8 C1 C2 C4 -0.10(16) . . . . ? P1 C1 C2 C4 -174.18(8) . . . . ? O1 C2 C4 C5 -175.03(10) . . . . ? C1 C2 C4 C5 4.41(17) . . . . ? C2 C4 C5 C6 -2.49(17) . . . . ? C7 O2 C6 C5 -20.07(15) . . . . ? C7 O2 C6 C8 159.00(10) . . . . ? C4 C5 C6 O2 175.28(10) . . . . ? C4 C5 C6 C8 -3.74(16) . . . . ? O2 C6 C8 C1 -171.03(9) . . . . ? C5 C6 C8 C1 8.06(16) . . . . ? O2 C6 C8 C9 10.04(14) . . . . ? C5 C6 C8 C9 -170.87(10) . . . . ? C2 C1 C8 C6 -6.02(15) . . . . ? P1 C1 C8 C6 168.55(8) . . . . ? C2 C1 C8 C9 172.83(10) . . . . ? P1 C1 C8 C9 -12.60(14) . . . . ? C6 C8 C9 C10 -100.44(12) . . . . ? C1 C8 C9 C10 80.68(13) . . . . ? C6 C8 C9 C20 75.94(13) . . . . ? C1 C8 C9 C20 -102.94(12) . . . . ? C20 C9 C10 C14 4.57(15) . . . . ? C8 C9 C10 C14 -179.01(9) . . . . ? C20 C9 C10 C11 -171.12(10) . . . . ? C8 C9 C10 C11 5.30(15) . . . . ? C14 C10 C11 C12 39.98(14) . . . . ? C9 C10 C11 C12 -144.32(10) . . . . ? C14 C10 C11 C13 -84.16(12) . . . . ? C9 C10 C11 C13 91.54(12) . . . . ? C9 C10 C14 C15 -2.57(16) . . . . ? C11 C10 C14 C15 173.18(10) . . . . ? C10 C14 C15 C19 -0.75(16) . . . . ? C10 C14 C15 C16 -179.92(10) . . . . ? C19 C15 C16 C18 3.55(15) . . . . ? C14 C15 C16 C18 -177.33(10) . . . . ? C19 C15 C16 C17 -120.24(12) . . . . ? C14 C15 C16 C17 58.89(14) . . . . ? C14 C15 C19 C20 2.07(16) . . . . ? C16 C15 C19 C20 -178.79(10) . . . . ? C15 C19 C20 C9 -0.03(16) . . . . ? C15 C19 C20 C21 -177.00(10) . . . . ? C10 C9 C20 C19 -3.31(15) . . . . ? C8 C9 C20 C19 -179.76(9) . . . . ? C10 C9 C20 C21 173.43(10) . . . . ? C8 C9 C20 C21 -3.02(16) . . . . ? C19 C20 C21 C23 76.78(12) . . . . ? C9 C20 C21 C23 -100.03(12) . . . . ? C19 C20 C21 C22 -44.87(13) . . . . ? C9 C20 C21 C22 138.32(11) . . . . ? C1 P1 C24 C27 52.44(10) . . . . ? C28 P1 C24 C27 -64.33(10) . . . . ? C1 P1 C24 C25 -66.82(8) . . . . ? C28 P1 C24 C25 176.40(7) . . . . ? C1 P1 C24 C26 178.84(7) . . . . ? C28 P1 C24 C26 62.06(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C31 H31A O1 0.98 2.25 3.0321(14) 136.4 . C29 H29C O1 0.98 2.52 3.2319(15) 129.4 . C27 H27B O1 0.98 2.52 3.0309(15) 112.0 . C7 H7B O2 0.98 2.57 3.4224(15) 145.2 5_666 _refine_diff_density_max 0.377 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.042 _shelx_res_file ; TITL XRAY5633_0ma_a.res in Pbca XRAY5633_0ma_a.res created by SHELXL-2016/6 at 16:08:34 on 03-Jul-2018 CELL 0.71073 18.3166 13.7825 22.8112 90.000 90.000 90.000 ZERR 8.000 0.0032 0.0024 0.0039 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O P UNIT 248 392 16 8 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 HTAB C31 O1 HTAB C29 O1 HTAB C27 O1 HTAB C7 O2_$1 EQIV $1 -x+1, -y+1, -z+1 SIZE 0.20 0.20 0.40 WPDB CONF TEMP -173.00 WGHT 0.100000 0.607040 FVAR 0.30348 P1 4 0.606983 0.659263 0.749311 11.00000 0.00956 0.01386 = 0.00998 -0.00010 0.00012 -0.00135 O1 3 0.449174 0.646415 0.800517 11.00000 0.01268 0.02833 = 0.01058 -0.00341 0.00440 -0.00438 O2 3 0.464686 0.553935 0.565513 11.00000 0.01413 0.02390 = 0.01008 -0.00372 -0.00013 -0.00504 C1 1 0.517619 0.636936 0.712344 11.00000 0.01072 0.01156 = 0.01118 -0.00023 0.00025 -0.00081 C2 1 0.449420 0.628845 0.741263 11.00000 0.01262 0.01337 = 0.01108 -0.00081 0.00121 -0.00039 C3 1 0.382125 0.634714 0.831551 11.00000 0.01665 0.02314 = 0.01552 -0.00421 0.00787 -0.00394 AFIX 137 H3A 2 0.346092 0.681086 0.816600 11.00000 -1.50000 H3B 2 0.390285 0.646534 0.873405 11.00000 -1.50000 H3C 2 0.363941 0.568483 0.825965 11.00000 -1.50000 AFIX 0 C4 1 0.386358 0.603607 0.711079 11.00000 0.01003 0.01680 = 0.01499 -0.00044 0.00235 -0.00012 AFIX 43 H4 2 0.340678 0.603052 0.730801 11.00000 -1.20000 AFIX 0 C5 1 0.390047 0.579138 0.651979 11.00000 0.01025 0.01662 = 0.01446 0.00064 -0.00143 -0.00100 AFIX 43 H5 2 0.347224 0.559400 0.631735 11.00000 -1.20000 AFIX 0 C6 1 0.456210 0.583577 0.622672 11.00000 0.01355 0.01362 = 0.00940 0.00029 -0.00040 0.00016 C7 1 0.410422 0.489454 0.542955 11.00000 0.01779 0.02092 = 0.01404 -0.00329 -0.00247 -0.00373 AFIX 137 H7A 2 0.402627 0.436267 0.570772 11.00000 -1.50000 H7B 2 0.426850 0.462981 0.505327 11.00000 -1.50000 H7C 2 0.364579 0.524900 0.537296 11.00000 -1.50000 AFIX 0 C8 1 0.519476 0.618131 0.651085 11.00000 0.01008 0.01110 = 0.01155 0.00107 0.00095 0.00097 C9 1 0.586049 0.634791 0.613147 11.00000 0.01053 0.01478 = 0.00790 -0.00131 -0.00005 -0.00203 C10 1 0.643301 0.566222 0.611305 11.00000 0.01208 0.01432 = 0.00934 -0.00049 -0.00172 -0.00005 C11 1 0.636776 0.469781 0.643278 11.00000 0.01463 0.01580 = 0.01327 0.00197 0.00224 0.00257 AFIX 13 H11 2 0.601539 0.478906 0.676306 11.00000 -1.20000 AFIX 0 C12 1 0.708603 0.433847 0.669462 11.00000 0.02114 0.02564 = 0.02373 0.00782 -0.00279 0.00598 AFIX 137 H12A 2 0.741697 0.414411 0.637813 11.00000 -1.50000 H12B 2 0.699078 0.378068 0.694984 11.00000 -1.50000 H12C 2 0.731120 0.486006 0.692388 11.00000 -1.50000 AFIX 0 C13 1 0.604676 0.393115 0.601983 11.00000 0.02489 0.01612 = 0.02025 0.00076 0.00238 -0.00117 AFIX 137 H13A 2 0.557247 0.415396 0.587351 11.00000 -1.50000 H13B 2 0.598327 0.331966 0.623305 11.00000 -1.50000 H13C 2 0.637930 0.382968 0.568890 11.00000 -1.50000 AFIX 0 C14 1 0.704539 0.584345 0.576579 11.00000 0.01087 0.01778 = 0.01333 -0.00191 0.00035 0.00167 AFIX 43 H14 2 0.743648 0.539075 0.576876 11.00000 -1.20000 AFIX 0 C15 1 0.710113 0.666947 0.541411 11.00000 0.00979 0.01941 = 0.01032 -0.00226 0.00033 -0.00218 C16 1 0.778355 0.683375 0.504089 11.00000 0.01131 0.02493 = 0.01363 -0.00019 0.00269 -0.00219 AFIX 13 H16 2 0.821223 0.684635 0.531225 11.00000 -1.20000 AFIX 0 C17 1 0.790026 0.599106 0.461016 11.00000 0.02422 0.03377 = 0.02808 -0.00880 0.01409 -0.00409 AFIX 137 H17A 2 0.749210 0.596606 0.433280 11.00000 -1.50000 H17B 2 0.792583 0.537900 0.482786 11.00000 -1.50000 H17C 2 0.835731 0.609054 0.439505 11.00000 -1.50000 AFIX 0 C18 1 0.778265 0.778922 0.470125 11.00000 0.01602 0.03247 = 0.02100 0.00706 0.00435 -0.00410 AFIX 137 H18A 2 0.738445 0.778416 0.441433 11.00000 -1.50000 H18B 2 0.824985 0.786621 0.449711 11.00000 -1.50000 H18C 2 0.771309 0.833013 0.497445 11.00000 -1.50000 AFIX 0 C19 1 0.651690 0.731058 0.541424 11.00000 0.01473 0.01550 = 0.01075 0.00109 0.00077 -0.00148 AFIX 43 H19 2 0.653831 0.786537 0.516771 11.00000 -1.20000 AFIX 0 C20 1 0.589725 0.717159 0.576351 11.00000 0.01146 0.01443 = 0.01075 -0.00148 -0.00034 0.00058 C21 1 0.527851 0.790789 0.569680 11.00000 0.01519 0.01802 = 0.01515 0.00513 0.00409 0.00486 AFIX 13 H21 2 0.493983 0.783311 0.603765 11.00000 -1.20000 AFIX 0 C22 1 0.554778 0.896562 0.568144 11.00000 0.02753 0.01740 = 0.02019 0.00378 0.00492 0.00535 AFIX 137 H22A 2 0.587121 0.908379 0.601614 11.00000 -1.50000 H22B 2 0.512817 0.940540 0.570237 11.00000 -1.50000 H22C 2 0.581540 0.908104 0.531602 11.00000 -1.50000 AFIX 0 C23 1 0.484680 0.770517 0.513169 11.00000 0.01517 0.02851 = 0.02337 0.00688 -0.00297 0.00300 AFIX 137 H23A 2 0.517388 0.775601 0.479309 11.00000 -1.50000 H23B 2 0.445160 0.818025 0.509329 11.00000 -1.50000 H23C 2 0.463983 0.705008 0.514858 11.00000 -1.50000 AFIX 0 C24 1 0.604993 0.792072 0.769565 11.00000 0.01429 0.01493 = 0.01515 -0.00131 -0.00012 -0.00246 C25 1 0.606166 0.843800 0.709883 11.00000 0.02246 0.01640 = 0.01887 0.00207 -0.00028 -0.00276 AFIX 137 H25A 2 0.560685 0.830135 0.688816 11.00000 -1.50000 H25B 2 0.647708 0.820334 0.686818 11.00000 -1.50000 H25C 2 0.610853 0.913913 0.715960 11.00000 -1.50000 AFIX 0 C26 1 0.676444 0.816682 0.801665 11.00000 0.01937 0.02011 = 0.02058 -0.00192 -0.00315 -0.00602 AFIX 137 H26A 2 0.682085 0.887295 0.803877 11.00000 -1.50000 H26B 2 0.717783 0.788825 0.780204 11.00000 -1.50000 H26C 2 0.675006 0.789612 0.841374 11.00000 -1.50000 AFIX 0 C27 1 0.539509 0.830567 0.804144 11.00000 0.02019 0.01764 = 0.02020 -0.00433 0.00206 0.00081 AFIX 137 H27A 2 0.537612 0.798764 0.842539 11.00000 -1.50000 H27B 2 0.494455 0.816788 0.782520 11.00000 -1.50000 H27C 2 0.544527 0.900797 0.809517 11.00000 -1.50000 AFIX 0 C28 1 0.611966 0.582521 0.819156 11.00000 0.01355 0.01980 = 0.01167 0.00252 -0.00090 -0.00123 C29 1 0.575900 0.483634 0.807236 11.00000 0.02195 0.01805 = 0.01648 0.00315 -0.00064 -0.00323 AFIX 137 H29A 2 0.585946 0.439589 0.839984 11.00000 -1.50000 H29B 2 0.595748 0.456059 0.770985 11.00000 -1.50000 H29C 2 0.523038 0.492275 0.803147 11.00000 -1.50000 AFIX 0 C30 1 0.694747 0.564738 0.826940 11.00000 0.01584 0.02599 = 0.01723 0.00525 -0.00280 0.00115 AFIX 137 H30A 2 0.719826 0.627061 0.831654 11.00000 -1.50000 H30B 2 0.713911 0.531251 0.792306 11.00000 -1.50000 H30C 2 0.702972 0.524631 0.861795 11.00000 -1.50000 AFIX 0 C31 1 0.583132 0.623164 0.877337 11.00000 0.01824 0.02673 = 0.01128 0.00034 -0.00068 -0.00305 AFIX 137 H31A 2 0.530747 0.636375 0.873784 11.00000 -1.50000 H31B 2 0.608962 0.683442 0.886774 11.00000 -1.50000 H31C 2 0.591270 0.575633 0.908614 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY5633_0ma_a.res in Pbca REM R1 = 0.0328 for 5666 Fo > 4sig(Fo) and 0.0408 for all 6574 data REM 321 parameters refined using 0 restraints END WGHT 0.0465 2.4925 REM Highest difference peak 0.377, deepest hole -0.254, 1-sigma level 0.042 Q1 1 0.6702 0.6482 0.7183 11.00000 0.05 0.38 Q2 1 0.7440 0.6763 0.5213 11.00000 0.05 0.35 Q3 1 0.6434 0.5189 0.6269 11.00000 0.05 0.35 Q4 1 0.6060 0.6220 0.7888 11.00000 0.05 0.34 Q5 1 0.4860 0.6012 0.6371 11.00000 0.05 0.34 Q6 1 0.4879 0.6271 0.7300 11.00000 0.05 0.34 Q7 1 0.5570 0.7531 0.5726 11.00000 0.05 0.33 Q8 1 0.6048 0.8172 0.7407 11.00000 0.05 0.32 Q9 1 0.3886 0.5996 0.6812 11.00000 0.05 0.32 Q10 1 0.5844 0.6691 0.5899 11.00000 0.05 0.32 Q11 1 0.4235 0.5853 0.6403 11.00000 0.05 0.32 Q12 1 0.5522 0.6247 0.6331 11.00000 0.05 0.32 Q13 1 0.4169 0.6220 0.7270 11.00000 0.05 0.32 Q14 1 0.5141 0.6368 0.6790 11.00000 0.05 0.31 Q15 1 0.6806 0.6954 0.5397 11.00000 0.05 0.31 Q16 1 0.6766 0.5818 0.5953 11.00000 0.05 0.30 Q17 1 0.6532 0.5778 0.8213 11.00000 0.05 0.29 Q18 1 0.6049 0.7343 0.7607 11.00000 0.05 0.29 Q19 1 0.6228 0.7221 0.5606 11.00000 0.05 0.29 Q20 1 0.5545 0.6533 0.7300 11.00000 0.05 0.29 ; _shelx_res_checksum 63527 _shelx_hkl_file ; 0 -1 0 -0.20 0.20 0 1 0 0.10 0.20 0 1 0 1.20 0.30 0 2 0 16.20 1.30 0 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1464.95 27.50 12 -1 0 1486.55 28.80 12 -1 0 1496.85 28.10 12 1 0 1478.65 28.20 -12 -1 0 1474.95 29.00 -12 2 0 120.99 4.90 -12 2 0 120.09 4.00 -12 -2 0 128.29 5.00 12 -2 0 131.39 5.00 12 2 0 128.19 4.60 12 -2 0 131.29 4.40 12 2 0 121.29 5.00 12 3 0 -1.80 1.40 12 -3 0 0.40 1.40 12 -3 0 1.60 1.90 -12 -3 0 -0.70 1.80 -12 3 0 1.20 1.30 -12 3 0 1.00 1.60 12 3 0 -2.00 1.70 12 4 0 904.21 19.10 12 -4 0 937.11 18.80 12 4 0 909.91 19.50 -12 -4 0 910.91 19.10 -12 -4 0 904.71 19.50 -12 4 0 926.81 18.80 -12 4 0 947.81 19.30 12 -4 0 933.41 19.40 -12 5 0 1024.20 20.70 12 -5 0 1017.40 21.10 12 -5 0 995.70 20.50 -12 -5 0 1012.90 21.20 -12 -5 0 1021.90 21.00 12 5 0 979.40 21.30 -12 5 0 1042.90 20.90 -12 6 0 136.39 5.20 12 6 0 133.29 5.70 -12 -6 0 141.89 5.50 12 -6 0 126.49 5.50 -12 -6 0 131.39 5.30 12 -6 0 145.59 5.10 -12 6 0 136.69 5.00 -12 7 0 728.13 15.60 12 -7 0 731.93 16.10 12 -7 0 726.33 15.90 -12 -7 0 747.13 16.40 12 7 0 700.23 16.60 -12 7 0 713.13 16.10 -12 -7 0 713.63 16.10 12 8 0 379.16 10.70 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2.20 13 -10 0 -1.20 2.20 -13 -10 0 0.20 2.30 -13 -11 0 0.00 2.60 13 -11 0 0.60 2.50 -13 11 0 -4.20 2.30 13 11 0 -3.60 2.40 13 -11 0 3.30 2.50 -13 12 0 -0.40 2.50 13 12 0 -1.00 2.60 13 -12 0 0.30 2.50 -13 -12 0 -4.30 2.50 -13 -13 0 -0.90 2.90 -13 13 0 -4.10 2.70 13 13 0 1.50 2.90 -13 14 0 -3.40 2.90 13 14 0 -2.90 2.90 -13 -14 0 -2.90 2.80 14 0 0 816.32 17.20 14 0 0 817.02 18.00 -14 0 0 851.41 18.30 -14 1 0 470.55 11.70 14 1 0 447.36 11.40 14 -1 0 444.86 11.40 -14 -1 0 474.05 11.80 14 -1 0 462.35 10.70 14 1 0 470.05 10.90 14 2 0 115.19 4.60 14 2 0 120.79 5.40 14 -2 0 116.79 5.10 -14 2 0 113.99 4.10 -14 -2 0 115.39 5.40 -14 2 0 117.09 5.30 14 -2 0 115.19 4.60 14 3 0 156.18 5.50 14 -3 0 147.19 5.30 -14 -3 0 157.78 6.20 -14 3 0 148.59 5.00 14 3 0 156.28 6.10 -14 3 0 143.89 5.80 14 -3 0 163.18 6.20 -14 -4 0 762.52 16.70 -14 4 0 759.02 16.30 14 -4 0 769.12 17.20 -14 -4 0 766.52 17.40 14 4 0 783.32 16.90 14 4 0 751.22 17.20 14 -4 0 778.12 16.40 -14 4 0 786.82 17.10 -14 -5 0 302.77 9.10 -14 -5 0 310.07 8.60 14 -5 0 317.87 9.10 -14 5 0 321.97 8.50 -14 5 0 302.67 8.70 14 -5 0 320.37 8.50 14 5 0 311.67 9.10 -14 6 0 142.69 5.60 -14 -6 0 140.59 6.10 14 -6 0 143.19 5.50 -14 -6 0 136.69 5.60 14 -6 0 138.89 6.00 -14 6 0 144.59 5.50 14 6 0 149.49 6.30 -14 7 0 83.59 4.60 -14 -7 0 73.49 4.90 -14 -7 0 86.19 4.80 -14 7 0 88.59 4.50 14 7 0 90.59 5.20 14 -7 0 85.49 4.70 14 -7 0 86.09 5.00 -14 -8 0 79.39 4.90 -14 -8 0 73.09 4.70 14 -8 0 78.49 4.80 14 8 0 73.29 5.10 -14 8 0 75.99 4.70 14 -8 0 75.59 5.00 -14 9 0 337.87 10.00 14 9 0 328.87 10.40 14 -9 0 336.37 9.80 -14 -9 0 313.07 9.50 -14 -9 0 333.57 10.10 14 -10 0 17.30 3.10 -14 -10 0 20.60 3.30 14 10 0 13.70 3.00 -14 10 0 15.20 3.10 -14 -11 0 104.09 6.10 14 11 0 99.89 6.20 14 -11 0 97.09 6.00 -14 11 0 98.29 6.00 14 12 0 67.19 5.40 -14 -12 0 58.59 5.20 -14 12 0 63.09 5.20 14 -12 0 67.89 5.90 14 13 0 241.18 9.60 -14 13 0 211.58 8.90 -14 -13 0 213.88 9.20 -14 14 0 16.60 3.70 -14 -14 0 3.00 3.40 14 14 0 10.10 3.60 -15 0 0 2.90 2.20 15 0 0 0.90 2.10 15 0 0 1.70 1.70 15 1 0 1.30 2.20 -15 1 0 -1.00 2.00 15 -1 0 -0.60 2.20 -15 -1 0 1.30 2.30 15 1 0 -0.30 1.60 15 -1 0 0.40 1.70 15 2 0 -1.20 1.70 15 2 0 0.70 2.10 -15 2 0 -3.50 1.80 15 -2 0 -0.40 2.20 -15 -2 0 1.80 2.20 15 -2 0 -1.10 1.60 15 3 0 -3.70 2.10 -15 3 0 -1.80 1.90 15 -3 0 -1.60 1.60 -15 -3 0 -0.80 2.20 15 -3 0 1.40 2.30 15 3 0 -0.60 1.70 15 -4 0 -2.30 1.60 15 4 0 -1.60 2.00 -15 -4 0 -3.10 2.20 -15 4 0 -2.10 1.60 -15 -4 0 -0.40 1.60 -15 4 0 -4.10 1.70 15 4 0 0.60 1.90 15 -4 0 3.20 2.20 -15 5 0 3.20 1.80 15 5 0 2.10 2.30 -15 -5 0 1.90 1.70 15 -5 0 -4.30 2.10 -15 -5 0 -0.70 2.30 -15 5 0 -2.60 1.70 15 -5 0 -1.20 2.00 15 6 0 1.20 2.20 -15 6 0 2.00 2.00 -15 6 0 -0.40 1.90 -15 -6 0 -2.20 2.30 15 -6 0 1.10 2.30 -15 -6 0 0.30 1.80 15 -7 0 1.80 2.40 -15 7 0 -1.40 1.80 -15 7 0 2.20 2.10 15 7 0 1.80 2.40 -15 -7 0 -1.20 2.20 -15 -7 0 -0.30 1.90 15 -8 0 -3.60 2.30 -15 8 0 2.90 2.30 15 8 0 -1.60 2.50 -15 -8 0 2.30 2.50 -15 -8 0 -0.40 2.00 15 9 0 0.30 2.40 15 -9 0 -3.40 2.30 -15 9 0 3.00 2.40 -15 -9 0 2.20 2.20 -15 -9 0 0.00 2.50 -15 10 0 -2.50 2.20 -15 -10 0 -1.50 2.20 15 10 0 -1.20 2.60 15 -10 0 -1.40 2.40 15 -11 0 -4.20 2.40 -15 -11 0 -1.10 2.60 15 11 0 3.60 2.80 -15 11 0 3.60 2.80 15 12 0 2.50 3.00 -15 12 0 1.70 2.90 -15 -12 0 -7.10 2.50 15 13 0 -2.20 2.90 -15 -13 0 0.40 3.10 -15 13 0 0.80 3.00 16 0 0 1197.08 25.30 16 0 0 1207.98 24.30 -16 0 0 1210.38 25.50 16 -1 0 32.50 3.60 16 -1 0 32.60 3.40 -16 1 0 30.90 3.20 16 1 0 27.80 3.40 16 1 0 35.40 3.00 -16 -1 0 33.90 3.60 16 2 0 137.69 5.50 -16 2 0 148.39 6.30 -16 -2 0 144.09 6.10 16 2 0 138.09 5.90 16 -2 0 144.69 6.30 16 3 0 535.35 13.30 -16 -3 0 507.85 13.40 -16 3 0 521.15 13.10 16 3 0 518.65 12.50 16 -3 0 505.85 13.00 -16 -4 0 26.10 2.80 16 4 0 31.30 3.50 16 -4 0 33.20 3.60 -16 -4 0 25.60 3.50 -16 4 0 26.00 3.20 -16 -5 0 8.80 2.70 -16 5 0 9.80 2.80 16 -5 0 9.70 2.70 -16 -5 0 14.20 2.40 16 5 0 10.50 2.80 -16 5 0 8.30 2.40 -16 6 0 11.00 2.40 -16 6 0 9.60 2.40 -16 -6 0 11.30 3.00 -16 -6 0 10.40 2.30 16 -6 0 9.80 2.80 16 6 0 8.20 2.80 16 7 0 647.84 16.30 16 -7 0 672.33 16.10 -16 7 0 645.04 15.50 -16 -7 0 680.33 16.20 -16 -7 0 659.33 15.80 -16 7 0 647.34 15.40 -16 8 0 23.40 3.20 -16 -8 0 29.30 3.40 -16 -8 0 23.80 3.50 16 8 0 26.50 3.80 16 -8 0 19.00 3.40 16 9 0 0.10 2.50 -16 -9 0 -1.20 2.50 -16 -9 0 2.70 2.30 16 -9 0 2.30 2.70 -16 9 0 1.00 2.40 -16 10 0 0.60 2.50 -16 -10 0 -3.80 2.10 16 10 0 3.90 2.80 16 -10 0 0.80 2.80 -16 -11 0 62.99 5.40 16 11 0 71.59 6.00 16 -11 0 69.39 5.90 -16 11 0 67.29 5.40 -16 -12 0 -0.70 2.70 16 12 0 5.70 3.50 -16 12 0 -3.90 2.50 -16 -13 0 318.07 11.60 -16 13 0 308.97 11.10 16 13 0 327.77 11.60 -17 0 0 2.40 2.40 17 0 0 5.40 2.50 17 -1 0 2.10 2.40 -17 -1 0 -0.70 2.00 -17 1 0 0.30 2.40 17 1 0 1.30 2.40 17 2 0 1.90 2.40 17 -2 0 2.70 2.50 -17 -2 0 0.70 2.10 -17 2 0 -1.20 1.90 -17 -3 0 -2.20 2.40 17 3 0 1.80 2.00 -17 3 0 -1.00 2.10 17 3 0 4.40 2.60 17 -3 0 -2.40 2.30 -17 4 0 -1.60 2.10 -17 -4 0 0.30 1.70 17 4 0 -3.10 1.90 17 -4 0 -0.60 2.30 -17 -4 0 -1.60 2.30 17 -5 0 1.60 2.60 -17 -5 0 3.40 2.70 17 5 0 1.60 2.50 -17 -5 0 -0.80 1.70 -17 5 0 -3.80 2.00 17 -6 0 -3.80 2.30 -17 6 0 1.00 2.30 -17 -6 0 -4.20 2.40 -17 -6 0 -0.20 1.90 17 6 0 -2.10 2.30 -17 -7 0 -1.40 2.00 -17 7 0 1.60 3.50 -17 -7 0 -0.90 2.60 -17 7 0 -5.00 2.10 17 7 0 3.70 2.70 17 -7 0 -4.30 2.40 -17 -8 0 -4.40 2.10 -17 8 0 2.10 2.50 17 -8 0 0.00 2.70 17 8 0 -1.30 2.50 -17 -8 0 -3.10 2.40 -17 9 0 -0.70 2.40 17 -9 0 -2.00 2.70 17 9 0 -0.90 2.50 -17 -9 0 0.90 2.30 -17 -9 0 1.20 2.90 -17 -10 0 1.00 2.60 -17 10 0 1.90 2.70 17 -10 0 -2.90 2.60 17 10 0 -1.20 2.70 -17 -11 0 1.20 2.60 -17 11 0 -0.50 2.70 17 11 0 4.70 3.20 17 12 0 5.50 3.40 -17 12 0 1.50 2.90 -17 -12 0 -5.40 2.70 18 0 0 255.87 8.70 -18 0 0 236.48 8.50 -18 1 0 129.29 6.20 -18 -1 0 134.29 6.60 18 -1 0 129.09 6.30 18 1 0 123.79 6.30 -18 2 0 320.87 10.10 -18 -2 0 326.77 10.40 18 -2 0 317.77 10.00 18 2 0 325.57 10.00 18 -3 0 274.67 9.20 -18 -3 0 269.27 9.40 -18 3 0 271.77 9.20 18 3 0 288.47 9.40 -18 4 0 622.24 15.40 18 -4 0 609.44 15.30 18 4 0 599.24 15.50 -18 -4 0 624.94 15.70 -18 5 0 2.40 2.40 -18 -5 0 1.90 2.80 18 5 0 1.80 2.60 18 -5 0 6.30 2.90 -18 6 0 79.89 5.20 18 6 0 81.09 5.70 18 -6 0 73.49 5.50 -18 -6 0 70.99 5.70 18 -7 0 101.59 6.10 -18 -7 0 89.59 7.10 18 7 0 100.59 6.20 -18 -7 0 94.59 6.10 -18 7 0 86.59 5.30 18 -8 0 7.80 3.10 -18 -8 0 3.90 2.50 -18 -8 0 0.20 2.90 18 8 0 9.90 3.30 18 9 0 22.40 4.00 18 -9 0 19.90 3.70 -18 -9 0 22.00 3.80 -18 -9 0 17.50 3.20 -18 10 0 -2.10 2.50 -18 -10 0 -4.50 2.40 18 -10 0 -4.00 3.10 18 10 0 1.80 3.00 18 11 0 24.60 4.30 -18 11 0 27.90 4.10 -18 -11 0 25.60 3.90 -19 0 0 -0.80 2.50 19 0 0 -3.10 2.40 19 1 0 3.90 2.70 19 -1 0 3.30 2.60 -19 -1 0 -0.60 2.70 -19 1 0 2.20 2.70 -19 2 0 -1.10 2.30 19 2 0 4.40 2.70 -19 -2 0 -0.80 2.60 19 -2 0 -1.00 2.60 19 -3 0 -1.50 2.50 -19 -3 0 -4.10 2.50 19 3 0 -0.80 2.40 -19 3 0 -1.60 2.30 -19 4 0 -0.20 2.50 -19 -4 0 -2.10 2.40 19 -4 0 1.80 2.70 19 4 0 -2.50 2.40 -19 -5 0 -3.00 2.40 -19 5 0 -2.50 2.40 19 -5 0 4.40 2.90 19 5 0 2.20 2.70 -19 6 0 -2.40 2.40 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110.99 6.60 -19 3 -3 122.19 6.30 19 3 3 112.29 6.10 19 3 -3 121.39 6.70 -19 -3 -3 106.69 6.10 -19 3 3 119.99 6.40 19 -3 3 121.09 6.30 19 4 3 2.10 2.70 19 4 3 1.60 2.60 -19 4 -3 3.20 2.60 19 -4 -3 3.80 2.90 -19 -4 3 1.70 2.60 -19 -4 -3 6.80 3.10 19 -4 3 -2.90 2.50 19 4 -3 8.80 3.10 -19 4 3 3.30 2.70 -19 5 -3 39.40 4.20 19 -5 -3 45.90 4.70 19 5 3 38.50 4.30 -19 -5 3 43.20 4.60 19 -5 3 32.70 4.00 -19 -5 -3 36.00 4.40 -19 5 3 33.50 3.80 19 5 -3 36.10 4.40 -19 -5 -3 37.50 3.80 19 -6 -3 11.60 3.30 -19 -6 3 3.10 3.00 -19 6 -3 4.50 2.60 19 6 3 3.40 2.70 19 -6 3 6.50 2.80 -19 6 3 -0.80 2.50 -19 -6 -3 -2.40 2.70 -19 -6 -3 6.60 2.50 19 6 -3 1.50 2.80 19 7 3 58.79 5.10 -19 7 -3 59.69 4.90 -19 -7 3 64.29 5.50 19 -7 -3 66.59 5.60 -19 -7 -3 58.59 4.90 -19 -7 -3 64.79 5.20 19 7 -3 57.39 5.10 19 8 3 2.80 2.80 19 -8 -3 -4.90 3.00 -19 -8 3 -3.40 2.80 -19 -8 -3 2.90 2.50 19 8 -3 0.10 2.90 -19 -8 -3 -1.70 2.90 -19 -9 3 1.50 3.20 19 9 3 3.10 2.80 19 -9 -3 -0.90 3.20 -19 -9 -3 4.30 2.90 -19 -9 -3 -4.10 2.90 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16.30 3.90 -8 15 4 24.50 3.90 8 -16 -4 64.99 5.50 -8 16 -4 64.99 5.90 8 -16 -4 84.19 9.40 8 16 4 76.49 6.40 -8 -16 4 55.09 5.90 -8 16 4 76.69 6.20 -8 -16 -4 70.89 6.30 8 16 -4 67.49 5.50 8 -16 4 81.39 6.80 9 0 -4 1025.10 19.00 -9 0 4 1030.70 20.40 9 0 -4 1018.00 20.40 -9 0 -4 1051.79 18.80 9 0 4 988.40 19.90 -9 0 -4 1017.10 20.30 -9 0 4 1004.60 19.60 9 0 4 1000.10 20.20 -9 1 -4 173.18 4.10 9 1 4 158.78 4.80 9 -1 -4 166.28 5.30 9 -1 -4 165.68 3.90 9 1 4 163.38 5.10 -9 1 -4 158.68 5.00 -9 -1 4 173.88 4.50 -9 -1 4 172.18 5.30 -9 -1 -4 167.28 3.30 9 1 -4 171.68 4.20 -9 1 4 160.88 5.10 9 -1 4 165.88 4.80 9 -1 4 163.28 5.10 9 1 -4 169.98 5.30 -9 1 4 165.88 4.70 -9 -1 -4 161.68 5.00 9 -2 -4 100.09 4.10 9 2 4 86.69 3.60 9 2 4 93.29 3.80 -9 2 -4 91.99 3.00 9 -2 -4 92.49 2.80 -9 -2 4 92.49 4.00 -9 -2 4 90.79 3.00 -9 2 -4 93.39 3.60 9 2 -4 90.59 3.00 9 -2 4 94.59 3.80 9 2 -4 91.39 4.00 -9 -2 -4 91.39 3.80 -9 2 4 84.79 3.70 9 -2 4 88.59 3.50 -9 2 4 96.89 3.60 -9 3 -4 91.79 3.60 -9 -3 4 86.69 4.00 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-1.30 3.50 -10 0 4 294.87 7.00 -10 0 4 296.67 7.70 10 0 -4 301.57 7.90 10 0 -4 299.57 6.50 10 0 4 300.27 7.50 -10 0 -4 292.17 6.10 10 0 4 302.17 7.70 -10 0 -4 304.47 7.80 10 1 4 36.70 2.70 10 -1 -4 36.50 2.90 -10 -1 4 41.70 2.20 -10 1 -4 39.00 2.70 10 -1 -4 37.50 1.90 -10 -1 4 40.20 2.90 10 1 4 37.90 2.80 -10 1 -4 34.20 1.90 -10 1 4 37.90 2.40 10 -1 4 37.10 2.60 -10 -1 -4 38.30 3.00 10 1 -4 36.10 2.90 -10 -1 -4 37.50 1.20 10 -1 4 34.40 2.70 -10 1 4 38.00 3.00 10 1 -4 40.10 2.10 -10 2 -4 20.20 1.60 10 -2 -4 13.60 2.10 -10 -2 4 16.90 1.50 10 2 4 16.30 2.00 10 2 4 13.20 1.90 -10 2 -4 17.40 2.10 10 -2 -4 15.00 1.30 -10 -2 4 16.30 2.20 -10 2 4 17.10 1.80 -10 2 4 18.10 2.10 -10 -2 -4 16.00 2.10 10 2 -4 21.50 2.40 10 -2 4 17.30 2.00 10 -2 4 14.40 1.90 10 2 -4 18.00 1.50 -10 3 -4 285.27 6.70 -10 3 -4 265.37 7.20 10 -3 -4 269.27 6.10 -10 -3 4 255.77 7.40 -10 -3 4 284.77 6.60 10 3 4 266.27 7.40 10 3 4 270.07 7.30 10 -3 -4 277.57 7.40 10 3 -4 261.87 7.40 10 -3 4 276.17 7.00 -10 -3 -4 269.87 7.30 10 -3 4 282.27 7.30 10 3 -4 268.67 6.20 -10 3 4 267.47 7.00 -10 3 4 269.57 7.20 -10 4 -4 45.00 3.00 -10 -4 4 44.00 2.60 10 4 4 38.70 2.90 10 -4 -4 42.40 2.40 -10 4 -4 49.10 2.80 10 -4 -4 44.40 3.40 10 4 4 47.40 3.30 -10 -4 4 39.80 3.40 10 4 -4 41.30 3.30 10 -4 4 40.90 2.90 -10 -4 -4 40.00 3.00 -10 4 4 43.00 3.00 10 4 -4 42.70 2.20 -10 4 4 41.80 3.00 10 -4 4 43.30 3.20 -10 -5 4 207.98 6.50 10 -5 -4 221.68 5.60 -10 5 -4 212.38 6.00 10 -5 -4 204.68 6.60 -10 -5 4 218.18 6.00 10 5 4 216.58 6.80 10 5 4 218.18 6.70 -10 5 -4 208.18 6.20 10 5 -4 206.58 6.50 -10 -5 -4 212.48 6.30 -10 5 4 211.28 6.40 10 -5 4 210.28 6.60 10 -5 4 213.28 6.00 10 5 -4 200.58 5.30 -10 5 4 218.78 6.10 10 6 4 272.57 7.90 -10 6 -4 277.97 7.70 10 -6 -4 290.07 7.10 10 -6 -4 281.67 8.10 -10 6 -4 287.47 7.50 -10 -6 4 279.57 7.60 -10 -6 4 295.97 8.00 -10 -6 -4 286.67 8.20 10 6 -4 279.77 6.80 -10 6 4 282.57 7.30 -10 -6 -4 286.57 7.60 10 -6 4 276.67 7.30 10 -6 4 285.37 8.10 -10 6 4 292.07 8.00 10 6 -4 286.27 8.10 -10 7 -4 16.00 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4.70 -10 -11 4 65.59 5.00 10 -11 -4 67.49 4.60 10 -11 -4 72.39 4.90 10 11 4 65.99 4.80 -10 11 -4 67.99 4.70 -10 -11 -4 65.19 5.10 10 11 -4 74.49 4.90 -10 11 4 68.09 5.10 10 -11 4 74.19 5.40 10 12 4 224.68 8.50 -10 -12 4 235.38 8.70 -10 12 -4 241.88 8.70 10 -12 -4 224.08 8.30 -10 -12 -4 243.38 8.90 -10 12 4 232.28 8.70 10 12 -4 237.58 8.50 10 -12 4 243.88 8.90 10 -13 -4 13.80 3.20 10 13 4 9.60 3.20 -10 -13 4 7.50 3.30 -10 13 -4 16.90 3.60 10 13 -4 12.50 3.10 -10 13 4 13.90 3.40 -10 -13 -4 11.80 3.30 10 -13 4 17.20 3.60 -10 14 -4 4.10 3.00 10 14 4 -2.00 2.80 10 -14 -4 0.80 2.80 -10 -14 4 -4.80 3.00 10 -14 4 -0.40 2.90 -10 -14 -4 0.60 2.80 -10 14 4 -2.10 2.80 10 14 -4 0.80 2.60 10 15 4 58.29 5.40 -10 15 -4 63.89 5.70 -10 -15 4 51.39 5.60 10 -15 -4 60.79 5.30 10 15 -4 62.59 5.30 -10 -15 -4 52.19 5.30 -10 15 4 66.49 5.60 10 -15 4 65.99 5.80 10 -16 -4 202.58 9.00 -10 -16 4 182.58 9.60 10 16 4 201.18 9.50 10 -16 4 208.18 9.40 10 16 -4 197.08 8.70 -11 0 -4 21.40 2.50 -11 0 4 21.70 1.90 11 0 4 19.70 2.20 -11 0 -4 19.30 1.40 11 0 -4 16.90 2.30 -11 0 4 16.80 2.20 11 0 4 22.00 2.20 11 0 -4 17.50 1.50 -11 -1 4 298.87 7.90 -11 -1 4 295.27 6.80 -11 1 -4 277.27 7.80 11 -1 -4 290.97 6.40 11 1 4 281.87 7.60 11 -1 -4 295.17 8.00 -11 1 -4 298.87 6.40 11 1 4 282.97 7.50 11 1 -4 291.17 6.60 11 -1 4 279.47 7.30 -11 -1 -4 289.17 7.90 11 -1 4 276.97 7.50 11 1 -4 285.17 7.90 -11 1 4 283.87 7.00 -11 1 4 282.77 7.70 -11 -2 4 7.50 1.30 -11 -2 4 5.80 2.00 11 -2 -4 7.80 1.20 11 -2 -4 4.70 2.10 -11 2 -4 8.20 1.70 -11 2 -4 6.80 1.30 11 2 4 3.50 1.60 11 2 4 7.20 1.80 11 2 -4 8.10 1.30 -11 2 4 8.10 2.00 11 -2 4 8.80 1.80 11 -2 4 7.60 1.80 -11 -2 -4 6.10 1.70 11 2 -4 8.00 2.00 -11 2 4 9.10 1.70 -11 3 -4 458.65 9.60 -11 3 -4 425.86 10.30 11 -3 -4 424.06 9.10 11 3 4 414.66 10.40 -11 -3 4 438.86 10.70 11 3 4 445.76 10.60 11 -3 -4 449.46 10.80 -11 -3 4 432.66 9.60 11 3 -4 427.96 10.50 11 -3 4 430.86 10.30 11 3 -4 426.66 9.10 11 -3 4 416.16 9.90 -11 3 4 438.46 10.30 -11 3 4 431.56 10.00 -11 -3 -4 418.56 10.40 -11 4 -4 11.50 1.90 -11 -4 4 15.40 1.80 11 4 4 12.00 2.10 -11 4 -4 11.70 1.80 -11 -4 4 13.40 2.30 11 4 4 11.40 2.10 11 -4 -4 13.20 1.60 11 -4 -4 15.60 2.60 11 -4 4 17.00 2.30 -11 -4 -4 12.00 2.20 11 4 -4 11.50 1.50 11 4 -4 12.50 2.30 11 -4 4 13.70 2.10 -11 4 4 12.90 2.10 -11 4 4 11.70 2.00 11 -5 -4 -0.90 1.90 -11 -5 4 2.20 1.50 11 -5 -4 -0.80 1.30 -11 5 -4 1.90 1.60 11 5 4 0.70 1.80 -11 -5 4 2.40 1.80 11 5 4 0.30 1.80 -11 5 -4 0.20 1.50 -11 5 4 1.70 1.80 -11 5 4 0.90 1.60 11 5 -4 2.50 1.90 -11 -5 -4 -0.20 1.70 11 5 -4 -0.20 1.10 11 -5 4 0.50 1.60 11 -5 4 -0.40 1.80 11 6 4 21.10 2.70 -11 -6 4 24.50 2.50 -11 6 -4 19.90 2.40 -11 6 -4 16.20 2.30 11 -6 -4 20.90 2.80 11 -6 -4 20.60 2.10 -11 -6 4 23.90 2.80 11 -6 4 17.90 2.60 11 6 -4 21.50 2.80 -11 6 4 21.80 2.60 -11 6 4 20.90 2.30 -11 -6 -4 19.70 2.60 11 -6 4 25.70 2.50 -11 -6 -4 20.40 2.50 -11 7 -4 18.30 2.30 11 -7 -4 15.50 2.80 -11 -7 4 15.00 2.30 11 -7 -4 19.30 2.30 -11 7 -4 14.40 2.40 -11 -7 4 18.90 2.70 11 7 4 14.10 2.60 -11 7 4 18.80 2.20 11 -7 4 16.70 2.70 11 7 -4 16.90 2.60 -11 7 4 14.90 2.60 -11 -7 -4 13.60 2.40 -11 -7 -4 19.60 2.50 11 -7 4 13.70 2.20 11 -8 -4 202.88 7.20 11 -8 -4 208.68 8.80 -11 -8 4 215.78 6.80 -11 8 -4 197.98 6.80 -11 -8 4 211.78 6.90 -11 8 -4 201.28 6.20 11 8 4 211.98 7.40 11 -8 4 205.88 7.20 11 -8 4 198.88 6.30 -11 -8 -4 203.38 7.30 -11 -8 -4 187.18 6.50 -11 8 4 210.48 7.20 11 8 -4 204.18 7.20 11 9 4 145.39 6.40 -11 9 -4 144.09 6.00 -11 -9 4 150.08 6.20 -11 -9 4 133.39 5.60 11 -9 -4 131.79 6.00 -11 9 4 141.19 5.90 11 9 -4 142.39 6.10 -11 -9 -4 132.59 5.40 11 -9 4 137.79 5.30 -11 -9 -4 135.89 6.00 11 -9 4 135.09 6.10 11 -10 -4 140.79 6.50 -11 10 -4 131.99 6.20 -11 -10 4 137.79 5.90 -11 -10 4 137.09 6.20 11 10 4 138.99 6.30 11 -10 4 136.99 6.20 -11 -10 -4 139.19 6.50 -11 10 4 139.59 6.40 11 10 -4 139.19 6.30 11 -11 -4 9.40 2.90 -11 -11 4 10.30 2.90 -11 11 -4 8.20 2.70 11 11 4 14.10 3.20 11 11 -4 15.00 3.00 11 -11 4 10.70 3.00 -11 -11 -4 14.70 3.20 -11 11 4 13.90 3.20 11 12 4 76.69 5.70 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4 655.13 14.40 12 -1 4 675.73 14.70 -12 1 4 662.03 14.00 -12 -1 -4 660.53 14.90 -12 2 -4 238.38 5.90 12 2 4 235.58 7.00 12 -2 -4 247.28 5.90 12 2 4 254.17 7.10 -12 -2 4 233.58 7.40 12 -2 -4 241.68 7.40 -12 2 -4 234.38 7.00 -12 -2 4 236.08 6.00 -12 2 4 243.68 7.20 12 -2 4 245.58 6.90 12 2 -4 238.98 7.30 12 -2 4 231.08 7.00 -12 -2 -4 243.48 7.20 -12 2 4 242.58 6.50 12 2 -4 238.08 5.80 -12 3 -4 58.29 3.70 12 3 4 56.69 3.70 -12 -3 4 55.79 2.90 12 -3 -4 56.89 4.20 -12 -3 4 57.99 4.10 12 3 4 51.49 3.60 -12 3 -4 58.69 3.00 12 -3 -4 56.69 3.50 12 3 -4 57.09 2.60 -12 -3 -4 57.19 3.80 12 3 -4 54.09 3.90 -12 3 4 55.39 3.40 12 -3 4 58.79 3.70 12 -3 4 52.79 3.60 -12 3 4 55.79 3.70 -12 4 -4 304.37 8.40 12 4 4 311.67 8.60 12 4 4 307.77 8.50 -12 -4 4 331.67 8.90 -12 -4 4 302.87 7.70 12 -4 -4 314.07 8.80 -12 4 -4 314.87 7.80 12 -4 4 307.77 8.40 -12 -4 -4 307.57 8.50 12 4 -4 305.57 8.70 12 -4 4 300.57 8.10 -12 4 4 286.67 8.20 -12 4 4 306.67 8.10 12 -5 -4 690.63 15.80 -12 -5 4 701.93 15.00 -12 5 -4 690.73 15.40 12 5 4 721.53 16.00 12 5 4 718.43 15.90 -12 -5 4 707.13 15.90 -12 5 -4 699.13 15.00 12 5 -4 664.03 15.60 -12 5 4 694.83 15.20 -12 -5 -4 711.43 15.60 -12 5 4 699.53 15.40 12 -5 4 702.43 15.20 12 -5 4 704.53 15.60 -12 6 -4 162.78 5.70 -12 -6 4 166.48 5.70 -12 6 -4 173.88 5.80 12 6 4 167.88 6.20 12 -6 -4 162.68 6.40 -12 -6 4 172.98 6.30 -12 -6 -4 169.68 6.10 -12 -6 -4 167.58 6.20 12 -6 4 173.28 6.20 -12 6 4 164.38 5.70 -12 6 4 163.58 6.10 12 -6 4 169.38 5.80 12 6 -4 163.58 6.30 -12 -7 4 219.28 7.30 -12 7 -4 222.08 7.00 -12 7 -4 216.38 6.70 -12 -7 4 235.58 7.10 12 7 4 224.18 7.60 12 -7 -4 212.28 7.50 -12 -7 -4 225.38 7.10 12 -7 4 236.58 7.00 -12 7 4 226.48 7.40 12 7 -4 218.98 7.40 -12 -7 -4 224.28 7.50 12 -7 4 226.08 7.40 -12 7 4 228.88 6.70 -12 -8 4 81.29 4.70 -12 8 -4 88.19 4.70 12 8 4 90.49 5.10 12 -8 -4 84.29 5.00 -12 8 -4 88.29 4.20 -12 -8 4 85.79 4.70 -12 8 4 79.59 4.90 -12 -8 -4 83.19 4.60 12 8 -4 79.99 4.90 12 -8 4 82.39 4.30 12 -8 4 87.69 5.00 -12 -8 -4 89.59 5.10 12 9 4 1.60 2.30 -12 -9 4 1.50 2.20 -12 -9 4 0.90 2.10 12 -9 -4 -2.00 2.30 -12 9 -4 -2.60 2.00 12 -9 4 0.80 2.30 -12 -9 -4 0.10 2.20 -12 -9 -4 1.30 2.00 -12 9 4 2.00 2.30 12 9 -4 2.10 2.30 12 -9 4 -1.70 2.00 12 -10 -4 11.70 2.90 -12 -10 4 12.10 2.60 12 10 4 10.90 2.70 -12 -10 4 10.30 2.70 -12 10 -4 11.40 2.70 -12 10 4 11.30 3.00 -12 -10 -4 12.20 2.80 12 10 -4 9.90 2.70 12 -10 4 15.10 3.10 12 11 4 219.38 8.70 12 -11 -4 230.18 8.30 -12 -11 4 230.08 8.40 -12 11 -4 226.88 8.30 12 -11 4 223.98 8.50 -12 -11 -4 231.18 8.60 12 11 -4 221.18 8.30 -12 11 4 230.68 8.60 -12 -12 4 43.20 4.40 12 12 4 49.99 4.80 12 -12 -4 47.20 4.50 -12 12 -4 39.30 4.20 12 12 -4 46.90 4.60 -12 12 4 41.20 4.30 -12 -12 -4 42.70 4.60 12 -12 4 49.70 4.60 -12 -13 4 0.50 2.90 12 13 4 1.20 3.00 -12 13 -4 3.40 3.00 12 -13 -4 0.80 2.80 -12 -13 -4 -2.40 2.70 12 -13 4 2.40 2.90 -12 13 4 -2.50 2.40 12 13 -4 -0.90 2.60 -12 -14 4 -1.50 3.00 -12 14 -4 2.20 3.10 12 14 4 5.80 3.50 12 -14 -4 0.20 2.90 12 -14 4 7.60 3.40 12 14 -4 12.50 3.30 -12 14 4 -2.40 3.00 -12 -14 -4 1.80 3.00 -12 -15 4 49.99 5.60 12 -15 -4 59.69 5.50 -12 15 -4 57.29 5.70 12 15 4 54.19 5.50 12 -15 4 70.99 6.10 -12 15 4 56.59 5.50 12 15 -4 52.89 5.20 -12 -15 -4 43.30 5.20 -13 0 -4 16.20 2.50 13 0 4 17.20 2.40 -13 0 4 18.80 2.80 13 0 4 14.20 2.20 -13 0 4 20.10 2.00 13 0 -4 15.10 2.70 13 1 4 60.29 3.80 -13 -1 4 54.19 2.80 -13 1 -4 49.70 3.50 13 -1 -4 45.40 3.70 13 1 4 56.99 3.60 -13 -1 4 53.29 4.10 -13 -1 -4 50.09 3.60 -13 1 4 56.09 4.00 13 -1 4 56.79 3.70 -13 1 4 53.79 3.10 13 -1 4 54.19 3.60 13 1 -4 55.99 4.10 13 1 -4 54.89 2.90 -13 -2 4 84.89 4.70 13 -2 -4 77.89 4.80 13 2 4 72.59 4.20 -13 -2 4 76.29 3.30 13 2 4 81.99 4.30 -13 2 -4 81.49 4.30 -13 2 4 79.39 3.70 13 -2 4 74.99 4.00 13 -2 4 72.89 4.00 -13 -2 -4 86.39 4.30 13 2 -4 78.79 3.40 -13 2 4 85.49 4.50 13 2 -4 73.99 4.30 13 -3 -4 269.67 8.30 -13 -3 4 270.87 8.20 -13 3 -4 264.27 7.90 -13 -3 4 269.37 7.00 -13 3 -4 285.37 7.00 13 3 4 269.97 8.00 13 3 4 282.67 8.10 -13 3 4 272.17 7.40 13 -3 4 274.37 7.80 -13 -3 -4 273.57 8.20 -13 3 4 275.17 8.00 13 -3 4 283.87 7.90 13 3 -4 266.07 8.20 -13 4 -4 31.40 2.50 -13 -4 4 30.90 2.50 13 -4 -4 26.20 3.20 -13 -4 4 24.80 3.00 13 4 4 25.00 2.90 13 4 4 30.20 3.10 -13 4 -4 27.60 2.80 13 -4 4 31.70 3.00 -13 4 4 32.80 3.10 13 4 -4 32.60 3.40 13 -4 4 31.40 2.90 -13 4 4 33.30 2.90 -13 -4 -4 29.20 3.10 -13 -5 4 1.30 2.30 13 -5 -4 2.80 2.40 13 5 4 2.40 2.00 13 5 4 2.30 2.10 -13 -5 4 2.40 1.60 -13 5 -4 2.20 1.80 -13 5 -4 1.20 1.70 -13 5 4 5.70 2.10 -13 -5 -4 3.90 2.10 -13 5 4 3.40 1.90 13 -5 4 4.00 2.10 13 5 -4 2.50 2.30 13 -5 4 0.20 1.90 13 -6 -4 4.30 2.40 -13 6 -4 7.00 2.10 -13 6 -4 8.00 2.10 13 6 4 11.40 2.50 -13 -6 4 8.20 2.00 -13 -6 4 8.20 2.50 -13 6 4 8.80 2.10 13 -6 4 8.50 2.20 -13 -6 -4 6.30 2.00 13 -6 4 4.00 2.10 -13 6 4 6.90 2.20 -13 -6 -4 8.30 2.40 13 6 -4 7.30 2.50 -13 -7 4 175.58 6.60 -13 7 -4 186.88 6.20 13 -7 -4 169.18 6.70 13 7 4 177.28 6.90 -13 -7 4 172.08 6.20 -13 7 -4 177.68 6.20 13 7 -4 180.08 6.90 -13 -7 -4 170.88 6.40 -13 7 4 171.38 6.00 13 -7 4 174.98 6.60 -13 7 4 169.08 6.50 -13 -7 -4 173.78 6.70 13 -7 4 170.08 6.20 -13 -8 4 72.99 4.80 13 8 4 72.69 5.10 -13 8 -4 72.69 4.60 -13 -8 4 77.19 4.60 13 -8 -4 70.59 5.00 -13 8 -4 89.89 4.30 -13 8 4 70.89 4.80 13 8 -4 82.79 5.10 13 -8 4 80.39 4.50 -13 -8 -4 78.79 4.70 -13 -8 -4 69.89 4.80 13 -8 4 73.59 4.80 -13 -9 4 -1.80 2.00 -13 9 -4 4.00 2.30 -13 -9 4 1.70 2.40 13 -9 -4 3.20 2.50 13 9 4 1.60 2.50 -13 9 4 4.50 2.50 13 -9 4 4.80 2.40 -13 -9 -4 -2.00 2.00 13 9 -4 0.90 2.40 -13 -9 -4 -2.60 2.20 13 10 4 11.70 3.20 -13 -10 4 16.50 3.00 -13 10 -4 17.10 3.00 13 -10 -4 21.90 3.40 -13 -10 4 13.90 3.00 13 10 -4 13.80 3.10 13 -10 4 16.80 3.10 -13 10 4 15.50 3.10 -13 -10 -4 13.30 2.90 13 11 4 15.00 3.30 -13 11 -4 10.00 3.00 -13 -11 4 9.10 3.00 13 -11 -4 5.50 2.80 13 -11 4 11.30 3.00 -13 11 4 11.60 3.10 13 11 -4 10.00 3.00 -13 -11 -4 8.10 2.60 -13 12 -4 51.09 4.70 -13 -12 4 47.40 4.70 13 12 4 42.90 4.40 13 -12 -4 49.10 4.60 13 12 -4 47.90 4.60 -13 12 4 36.70 4.20 -13 -12 -4 49.20 4.90 13 -12 4 43.50 4.60 13 13 4 4.50 3.00 -13 -13 4 -0.10 2.70 13 -13 -4 7.10 3.20 -13 13 -4 -0.40 2.70 -13 -13 -4 7.60 3.30 -13 13 4 1.90 3.10 13 13 -4 3.50 2.90 13 -13 4 6.50 3.20 -13 14 -4 12.60 3.70 13 14 4 12.00 3.80 13 -14 -4 9.20 3.50 -13 -14 4 6.60 3.60 13 14 -4 10.30 3.40 13 -14 4 14.50 3.70 -13 14 4 8.20 3.40 -13 -14 -4 6.30 3.30 -14 0 4 148.79 5.90 14 0 -4 149.69 6.20 14 0 4 144.19 5.80 14 0 4 159.48 5.70 -14 0 4 164.48 5.00 -14 0 -4 164.98 6.20 14 -1 -4 74.89 4.90 14 1 4 73.59 4.30 -14 -1 4 79.49 4.80 14 1 4 71.99 4.20 -14 1 -4 76.19 4.50 -14 1 4 77.79 3.70 -14 1 4 75.79 4.60 14 -1 4 73.19 4.30 14 1 -4 76.09 4.80 -14 -1 -4 76.29 4.30 14 -1 4 80.79 4.30 -14 2 -4 1.60 2.00 14 2 4 2.50 2.00 14 2 4 2.60 2.00 14 -2 -4 7.20 2.40 -14 -2 4 8.10 2.60 -14 -2 -4 6.20 2.40 -14 2 4 1.80 1.60 14 -2 4 4.80 2.10 -14 2 4 2.10 2.10 14 2 -4 5.10 2.40 14 -2 4 3.90 2.00 14 -3 -4 -0.90 2.20 14 3 4 -1.60 1.90 14 3 4 1.10 1.90 -14 -3 4 1.40 2.00 -14 3 -4 -0.40 1.90 14 3 -4 -0.80 2.20 14 -3 4 1.10 2.00 -14 3 4 4.60 1.80 -14 -3 -4 1.70 2.10 -14 3 4 -0.50 1.90 14 -3 4 -1.70 1.90 -14 -4 4 79.29 4.70 14 4 4 80.39 4.70 -14 4 -4 91.79 4.00 14 4 4 82.19 4.60 -14 4 -4 91.09 4.70 14 -4 -4 89.29 5.20 -14 -4 4 89.39 4.00 -14 -4 -4 87.59 4.90 14 -4 4 92.19 4.70 14 4 -4 84.69 4.80 -14 4 4 92.09 4.30 14 -4 4 93.19 4.70 -14 4 4 78.69 4.70 -14 5 -4 5.50 2.10 14 5 4 3.40 2.20 -14 -5 4 1.90 2.30 -14 -5 4 1.50 1.60 -14 5 -4 5.20 1.80 14 -5 -4 0.60 2.40 14 5 4 4.10 2.20 -14 5 4 1.40 2.00 14 -5 4 2.20 2.10 14 5 -4 0.60 2.20 -14 5 4 -0.60 1.90 14 -5 4 4.40 2.10 -14 -5 -4 0.60 2.10 -14 -6 4 411.06 10.90 -14 -6 4 383.26 9.90 -14 6 -4 386.26 10.20 14 6 4 377.76 10.60 -14 6 -4 385.46 9.90 14 -6 -4 383.36 10.80 14 -6 4 382.36 10.40 -14 -6 -4 393.66 10.60 14 6 -4 398.76 10.90 -14 6 4 387.86 10.20 -14 -6 -4 370.96 10.50 14 -6 4 390.06 10.20 -14 6 4 387.36 10.30 -14 -7 4 -1.40 1.70 14 7 4 3.20 2.50 14 -7 -4 1.00 2.60 -14 -7 4 3.50 2.40 -14 7 -4 -1.30 1.70 -14 7 -4 1.00 1.90 -14 7 4 1.10 1.90 -14 7 4 5.80 2.30 -14 -7 -4 -0.20 2.10 14 -7 4 2.30 2.20 -14 -7 -4 0.40 1.90 14 7 -4 -0.40 2.20 14 -7 4 -0.60 2.00 -14 -8 4 5.90 2.30 14 -8 -4 1.10 2.40 14 8 4 7.70 2.80 -14 -8 4 6.00 2.60 -14 8 -4 1.60 2.20 -14 8 -4 1.10 1.90 -14 -8 -4 5.30 2.40 14 8 -4 7.40 2.70 14 -8 4 4.20 2.30 14 -8 4 -0.30 2.30 -14 8 4 1.60 2.30 -14 -8 -4 2.10 2.30 14 -9 -4 1.10 2.50 -14 9 -4 -1.60 2.20 -14 -9 4 2.50 2.30 14 9 4 -5.20 2.30 -14 -9 4 1.80 2.40 14 9 -4 1.40 2.50 -14 9 4 -1.70 2.30 -14 -9 -4 -0.60 2.10 -14 -9 -4 -1.70 2.20 14 -9 4 0.90 2.50 -14 -10 4 242.08 8.60 -14 10 -4 233.98 8.50 14 10 4 259.77 9.20 14 -10 -4 243.28 8.80 -14 -10 4 227.78 8.20 -14 10 4 243.98 8.80 -14 -10 -4 255.87 9.00 14 -10 4 240.88 8.80 14 10 -4 248.98 8.90 -14 -11 4 8.40 2.70 14 -11 -4 11.30 3.20 -14 11 -4 6.20 2.80 14 11 4 11.10 3.40 -14 11 4 5.80 2.80 14 11 -4 11.10 3.20 -14 -11 -4 5.00 2.70 14 -11 4 8.80 3.00 -14 -12 4 7.90 3.10 -14 12 -4 8.10 3.00 14 -12 -4 -0.10 2.90 14 12 4 3.90 3.10 -14 12 4 4.70 3.00 14 -12 4 11.00 3.20 -14 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286.47 8.40 15 -3 4 277.07 8.30 -15 3 4 283.57 7.90 -15 3 4 291.17 8.70 15 4 4 50.79 4.10 15 -4 -4 48.90 4.20 15 4 4 46.10 4.00 -15 4 -4 50.49 4.00 -15 -4 4 47.90 4.10 15 -4 4 50.49 4.10 -15 4 4 53.19 3.60 -15 4 4 49.40 4.10 15 -4 4 49.20 3.90 -15 -4 -4 52.49 4.40 15 4 -4 47.40 4.00 15 -5 -4 0.80 2.60 15 5 4 4.70 2.40 -15 -5 4 3.00 2.40 15 5 4 0.90 2.10 -15 5 -4 9.60 2.40 -15 5 4 5.30 2.10 -15 -5 -4 5.40 2.50 -15 5 4 4.20 2.20 15 5 -4 3.20 2.40 15 -5 4 4.10 2.20 15 -5 4 10.70 2.50 -15 -6 4 143.29 6.50 -15 6 -4 143.39 5.50 -15 6 -4 133.39 5.90 15 6 4 140.79 6.40 15 -6 -4 145.49 6.60 15 -6 4 149.69 6.00 -15 6 4 136.69 5.90 -15 -6 -4 152.28 6.20 -15 6 4 141.49 5.90 -15 -6 -4 137.19 6.10 15 -6 4 134.89 6.10 15 6 -4 136.59 6.40 15 7 4 67.09 4.70 -15 7 -4 68.59 4.40 15 -7 -4 63.29 5.10 -15 -7 4 71.89 5.00 -15 -7 4 68.69 4.80 -15 7 -4 66.69 4.20 15 -7 4 61.69 4.80 -15 7 4 65.39 4.40 -15 -7 -4 57.89 4.90 -15 -7 -4 66.69 4.70 -15 7 4 74.19 4.70 15 -7 4 72.89 4.70 15 7 -4 66.69 4.70 -15 -8 4 1.10 2.60 -15 8 -4 3.80 2.10 15 -8 -4 -0.20 2.50 15 8 4 2.20 2.20 -15 8 -4 4.60 2.30 -15 -8 4 1.80 2.10 -15 8 4 0.80 2.30 -15 -8 -4 2.80 2.30 -15 -8 -4 0.70 2.30 15 -8 4 -0.80 2.30 15 8 -4 5.70 2.70 -15 9 -4 -0.20 2.10 15 9 4 1.10 2.40 -15 -9 4 1.80 2.20 15 -9 -4 -0.20 2.60 -15 -9 4 -1.80 2.40 -15 9 4 -3.00 2.30 15 9 -4 3.00 2.70 -15 -9 -4 -3.90 2.10 15 -9 4 -2.10 2.40 -15 -9 -4 -4.30 2.20 15 -10 -4 144.79 7.00 -15 10 -4 145.79 6.90 -15 -10 4 149.79 7.00 15 10 4 148.89 7.20 -15 -10 4 146.79 6.90 -15 10 4 144.29 7.00 15 -10 4 138.39 6.80 15 10 -4 146.09 7.20 -15 -10 -4 152.18 7.20 -15 11 -4 44.10 4.40 -15 -11 4 36.40 4.10 15 11 4 46.90 4.90 15 -11 -4 45.40 4.70 -15 -11 -4 36.90 4.40 15 11 -4 39.80 4.40 15 -11 4 40.20 4.40 -15 11 4 44.50 4.60 15 12 4 4.20 3.20 -15 12 -4 5.30 3.00 -15 -12 4 0.00 2.90 15 -12 -4 -2.20 2.90 15 -12 4 4.40 2.90 -15 -12 -4 -1.50 2.60 15 12 -4 7.20 3.00 -15 12 4 4.90 3.10 15 13 4 40.00 5.00 15 -13 -4 38.60 4.70 -15 13 -4 32.40 4.40 -15 -13 4 39.40 4.90 -15 -13 -4 30.20 4.40 15 -13 4 36.20 4.70 15 13 -4 41.70 5.00 -15 13 4 40.50 4.70 -16 0 4 41.50 4.00 16 0 -4 33.10 3.50 16 0 4 32.80 3.20 -16 0 -4 36.30 3.70 16 0 4 32.50 3.20 16 1 4 524.15 13.00 16 -1 -4 531.45 13.60 -16 1 -4 526.05 13.40 16 1 4 522.35 13.00 -16 -1 4 533.15 13.60 16 -1 4 535.55 13.00 16 1 -4 523.15 13.50 -16 -1 -4 514.15 13.40 -16 1 4 546.15 13.60 16 -1 4 532.75 13.00 16 -2 -4 40.10 4.00 16 2 4 46.40 3.90 16 2 4 41.50 3.70 -16 2 -4 47.10 3.90 -16 -2 4 49.10 4.30 16 -2 4 44.20 3.80 -16 -2 -4 46.60 4.00 16 -2 4 40.60 3.50 -16 2 4 45.80 4.00 16 2 -4 42.00 4.00 16 3 4 124.79 5.80 -16 3 -4 121.39 5.80 16 3 4 123.99 5.80 16 -3 -4 119.29 5.80 -16 -3 4 123.79 6.20 -16 3 4 126.09 5.50 16 -3 4 128.89 5.60 -16 -3 -4 130.09 6.10 16 3 -4 132.79 6.20 16 -3 4 121.29 5.40 -16 3 4 122.09 5.80 16 4 4 59.39 4.60 -16 -4 4 72.29 5.10 -16 4 -4 69.59 4.50 16 -4 -4 59.09 5.10 16 4 4 59.39 4.40 -16 4 4 59.69 4.50 16 -4 4 61.39 4.30 -16 4 4 60.69 4.10 16 -4 4 68.49 4.60 -16 -4 -4 68.19 4.90 16 4 -4 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19 -9 -4 3.70 3.40 -19 -9 -4 -3.30 3.10 19 9 -4 6.10 3.40 -19 -9 -4 5.90 3.00 -19 -10 4 29.10 4.50 19 -10 -4 31.20 4.70 19 10 4 34.60 4.70 -19 10 4 36.80 4.60 19 10 -4 35.90 4.80 -19 -10 -4 34.20 4.30 -20 0 4 40.50 4.70 -20 0 -4 32.90 4.00 20 0 -4 35.40 4.40 20 0 4 40.00 4.10 -20 1 -4 143.79 7.00 -20 -1 4 133.39 7.20 20 -1 -4 149.69 7.30 20 1 4 135.59 6.60 20 -1 4 119.69 6.30 20 1 -4 143.89 7.30 -20 1 4 131.89 6.80 -20 -1 -4 124.79 6.90 20 2 4 45.80 4.40 20 -2 -4 52.69 4.90 -20 2 -4 53.19 4.80 -20 -2 4 46.60 4.60 -20 -2 -4 52.69 5.10 -20 2 4 52.39 4.90 20 2 -4 48.50 4.50 20 -2 4 38.80 4.10 -20 3 -4 17.10 3.40 20 3 4 19.30 3.40 20 -3 -4 23.40 4.00 20 3 4 18.70 5.20 -20 -3 4 25.60 4.10 -20 -3 -4 18.20 3.80 20 3 -4 21.80 3.70 20 -3 4 20.80 3.30 -20 3 4 15.40 3.40 -20 -4 4 61.79 5.40 20 -4 -4 72.19 6.00 20 4 4 65.19 5.50 20 4 4 71.69 5.80 -20 4 -4 76.29 5.60 20 4 -4 78.19 5.90 -20 4 4 67.89 5.60 -20 -4 -4 74.99 6.00 20 -4 4 71.49 5.50 20 5 4 206.08 8.40 20 -5 -4 221.78 9.20 -20 -5 4 215.08 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-6 0 7 0.00 1.10 6 1 7 1909.21 36.20 -6 -1 7 1953.70 36.10 -6 1 -7 1931.11 35.20 -6 -1 7 1914.41 35.80 6 -1 -7 2011.60 36.10 -6 1 -7 1897.71 36.00 -6 -1 7 1930.11 34.60 6 1 7 1905.21 35.50 6 1 -7 1924.61 35.90 -6 1 7 1919.21 36.00 -6 -1 -7 1933.11 34.80 -6 1 7 1930.31 36.00 6 -1 7 1917.11 35.10 6 -1 7 1888.51 36.20 -6 -1 -7 1922.71 36.00 6 2 7 213.58 5.90 -6 -2 7 210.38 4.80 -6 -2 7 208.88 5.70 -6 2 -7 212.98 5.20 6 2 7 206.28 5.40 -6 2 -7 209.48 5.70 6 -2 -7 216.88 5.80 6 2 -7 211.38 5.40 6 -2 7 212.28 4.70 -6 2 7 216.48 5.70 6 -2 7 214.68 5.90 -6 2 7 206.28 5.60 -6 -2 -7 213.68 4.40 -6 -2 -7 209.88 5.70 6 2 -7 212.18 5.60 -6 3 -7 136.09 4.10 6 3 7 131.49 4.60 6 -3 -7 140.59 4.60 -6 -3 7 141.49 4.60 -6 3 -7 136.59 4.30 6 3 7 134.19 4.20 6 -3 -7 141.59 3.10 -6 -3 7 138.19 3.80 -6 -3 -7 138.69 4.30 6 3 -7 134.29 4.00 -6 3 7 133.89 4.20 -6 3 7 132.39 4.50 6 -3 7 126.39 3.30 6 3 -7 130.59 4.20 6 -3 7 136.49 4.70 -6 -3 -7 132.39 3.10 6 4 7 47.20 1.80 6 -4 -7 47.10 3.10 -6 -4 7 45.40 2.90 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7.40 -7 -2 9 300.17 6.00 -7 2 -9 266.27 7.20 7 2 9 279.37 6.90 7 2 9 274.07 7.50 7 -2 9 289.37 7.70 -7 2 9 284.97 7.40 7 2 -9 277.87 7.20 -7 -2 -9 274.67 7.30 7 -2 9 292.67 6.10 -7 -2 -9 282.67 5.90 -7 2 9 275.47 7.20 7 2 -9 268.57 6.90 -7 3 -9 20.80 2.20 -7 -3 9 18.90 2.10 7 3 9 18.90 1.90 7 3 9 19.30 2.20 -7 3 -9 23.10 1.90 7 -3 -9 21.50 2.40 -7 -3 9 17.10 1.60 7 -3 9 18.90 1.40 -7 -3 -9 19.90 2.10 -7 -3 -9 20.20 1.40 7 3 -9 20.80 2.00 -7 3 9 17.60 2.20 -7 3 9 19.60 2.10 7 -3 9 14.50 2.10 7 3 -9 19.60 2.00 -7 4 -9 27.30 2.40 -7 -4 9 27.30 2.70 -7 -4 9 30.10 2.30 7 -4 -9 32.60 2.80 7 4 9 30.90 2.60 -7 4 -9 28.50 2.40 7 4 9 24.80 2.50 7 -4 -9 33.90 1.70 -7 4 9 31.50 2.70 7 -4 9 30.60 1.70 7 -4 9 23.90 2.40 -7 -4 -9 28.60 1.50 -7 4 9 28.30 2.40 -7 -4 -9 26.20 2.30 7 4 -9 26.80 2.30 7 4 -9 31.00 2.50 7 5 9 19.10 1.60 -7 5 -9 20.20 2.10 -7 -5 9 17.50 2.00 7 -5 -9 17.00 2.20 -7 5 -9 19.00 2.10 7 -5 -9 17.70 1.50 7 5 9 17.50 2.50 -7 -5 9 16.80 2.30 7 5 9 18.40 2.30 7 5 -9 19.30 2.10 -7 5 9 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5.10 7 -16 -9 40.30 4.90 -7 -16 9 30.30 5.10 -7 16 -9 36.50 4.70 -7 -16 -9 45.10 5.40 -7 16 9 45.70 5.20 7 -16 9 53.09 5.90 8 0 9 1.00 1.00 -8 0 9 2.30 1.50 -8 0 9 -0.50 1.40 8 0 9 -2.10 1.30 -8 0 -9 0.70 0.80 8 0 -9 -1.00 1.50 -8 0 -9 -2.50 1.40 -8 -1 9 263.37 7.40 8 1 9 266.27 7.40 -8 1 -9 273.77 6.20 -8 -1 9 261.27 5.30 8 1 9 260.17 6.50 -8 -1 9 266.67 7.00 -8 1 -9 265.77 7.20 8 -1 -9 277.67 7.30 -8 1 9 268.07 7.10 8 -1 9 267.37 7.50 -8 -1 -9 268.77 7.20 8 -1 9 261.47 6.20 -8 -1 -9 273.97 5.80 -8 1 9 275.97 7.20 8 1 -9 266.67 7.10 8 -2 -9 9.70 2.00 8 2 9 11.50 1.60 8 2 9 10.80 2.00 -8 2 -9 7.80 1.80 -8 -2 9 12.50 2.00 -8 2 -9 11.70 1.50 -8 -2 9 10.80 1.10 8 2 -9 7.70 1.80 8 -2 9 11.00 2.10 8 2 -9 10.70 1.70 8 -2 9 11.50 1.30 -8 2 9 10.00 1.90 -8 2 9 13.80 2.10 -8 -2 -9 8.30 1.70 -8 -2 -9 13.00 1.00 -8 3 -9 141.19 4.40 -8 -3 9 141.29 3.90 8 -3 -9 146.89 5.20 8 3 9 137.19 4.60 -8 3 -9 145.99 5.00 8 3 9 138.19 5.10 -8 -3 9 143.69 5.10 -8 -3 -9 134.59 3.30 -8 3 9 145.19 5.00 8 3 -9 136.29 4.80 8 -3 9 131.59 5.20 8 3 -9 138.39 4.50 -8 -3 -9 135.49 4.90 8 -3 9 133.79 3.70 -8 3 9 138.69 4.80 8 -4 -9 43.50 3.50 8 4 9 38.50 3.10 -8 4 -9 43.60 2.80 -8 4 -9 39.40 3.00 8 4 9 38.20 2.90 -8 -4 9 41.40 3.40 -8 -4 9 41.30 2.70 -8 -4 -9 44.00 3.00 8 -4 9 40.00 2.00 -8 4 9 39.90 3.00 8 -4 9 44.10 3.60 8 4 -9 37.20 2.80 8 4 -9 37.50 3.10 -8 4 9 39.80 3.30 8 -5 -9 313.67 8.60 8 5 9 323.67 8.50 -8 -5 9 316.17 8.50 -8 5 -9 311.57 8.10 -8 -5 9 319.77 7.70 8 5 9 311.57 8.70 -8 5 -9 316.47 8.00 8 -5 9 296.57 8.70 -8 -5 -9 303.17 8.00 8 5 -9 312.37 8.10 -8 5 9 325.27 8.60 -8 5 9 312.27 7.80 8 5 -9 302.07 7.90 -8 6 -9 28.10 2.70 -8 -6 9 29.40 2.60 -8 6 -9 27.60 2.50 8 -6 -9 24.90 2.70 8 6 9 27.00 3.00 8 6 9 28.40 2.80 -8 -6 9 26.80 2.80 -8 6 9 29.60 2.40 8 -6 9 24.50 3.00 -8 -6 -9 24.50 2.40 -8 6 9 23.60 2.70 8 6 -9 28.60 2.50 8 6 -9 29.30 2.60 8 -7 -9 730.73 16.40 -8 7 -9 756.02 16.00 -8 -7 9 703.93 16.00 -8 -7 9 721.53 15.70 -8 7 -9 728.03 15.60 8 7 9 720.73 16.30 -8 7 9 725.33 16.40 -8 -7 -9 738.23 16.50 8 -7 9 718.43 16.60 8 7 -9 713.63 15.70 -8 7 9 733.03 15.00 8 7 -9 709.43 15.60 -8 -7 -9 719.23 15.30 8 -8 -9 55.29 4.10 -8 -8 9 57.49 3.90 -8 8 -9 52.29 4.00 8 8 9 56.89 4.20 -8 -8 9 52.99 4.00 -8 8 -9 57.69 3.50 8 8 -9 50.49 3.70 8 8 -9 53.09 3.70 -8 -8 -9 54.39 3.40 -8 -8 -9 52.69 4.30 8 -8 9 41.90 3.70 -8 8 9 51.49 4.30 8 9 9 339.97 10.20 8 -9 -9 360.36 10.20 -8 -9 9 362.76 9.60 -8 9 -9 366.76 9.10 -8 9 -9 357.16 9.90 -8 -9 9 342.77 9.80 8 9 -9 358.96 9.50 8 -9 9 349.27 10.50 8 9 -9 360.16 9.50 -8 9 9 360.36 10.20 -8 -9 -9 361.96 10.50 -8 -10 9 88.69 5.30 -8 10 -9 87.69 4.90 8 -10 -9 85.69 5.40 -8 -10 9 91.89 4.80 8 10 9 91.79 5.40 8 -10 9 91.39 5.40 -8 -10 -9 101.59 5.60 8 10 -9 88.79 4.70 -8 10 9 94.69 5.50 8 10 -9 86.49 4.60 8 -11 -9 8.90 2.60 8 11 9 7.00 2.70 -8 11 -9 9.20 2.70 -8 -11 9 5.80 2.90 8 -11 9 8.10 3.10 -8 -11 -9 10.20 2.90 -8 11 9 6.00 2.80 8 11 -9 5.60 2.20 8 11 -9 8.20 2.40 8 -12 -9 176.18 7.70 8 12 9 180.38 7.80 -8 -12 9 194.58 7.90 -8 12 -9 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7.20 -8 0 -10 324.87 7.00 8 0 -10 313.07 8.10 -8 1 -10 134.99 3.90 8 1 10 129.29 4.10 -8 -1 10 128.99 5.00 8 -1 -10 132.09 4.90 8 1 10 124.59 4.80 -8 1 -10 138.09 5.00 -8 -1 10 138.99 4.80 8 1 -10 135.39 4.60 -8 -1 -10 136.09 4.90 8 -1 10 135.29 3.80 8 1 -10 126.89 4.80 8 -1 10 135.39 5.20 -8 -1 -10 131.09 3.50 -8 1 10 137.69 4.90 -8 1 10 134.29 5.00 -8 -2 10 9.30 1.90 -8 2 -10 12.90 2.00 8 -2 -10 12.40 2.10 8 2 10 12.70 2.20 -8 -2 10 13.30 1.20 8 2 10 13.40 1.70 -8 2 -10 11.90 1.60 8 2 -10 12.60 1.90 8 -2 10 15.80 1.40 8 2 -10 13.60 2.10 -8 -2 -10 12.00 2.00 -8 2 10 15.80 2.20 8 -2 10 9.50 1.90 -8 2 10 12.10 2.00 -8 -2 -10 11.30 1.10 -8 -3 10 47.10 2.40 -8 3 -10 48.90 2.70 -8 -3 10 45.50 3.50 8 3 10 49.80 3.00 8 3 10 50.99 3.70 -8 3 -10 48.20 3.30 8 -3 -10 51.99 3.60 8 -3 10 58.09 3.80 -8 -3 -10 50.89 2.40 -8 3 10 53.99 3.30 -8 -3 -10 46.60 3.20 -8 3 10 48.00 3.40 8 3 -10 38.50 3.10 8 3 -10 44.70 2.90 8 -3 10 49.90 2.10 -8 4 -10 5.80 1.70 8 -4 -10 5.50 2.10 8 4 10 7.80 1.80 -8 4 -10 10.00 2.00 8 4 10 8.80 2.10 -8 -4 10 1.70 1.90 -8 -4 10 5.20 1.50 8 4 -10 5.30 1.70 8 -4 10 7.90 2.20 -8 4 10 8.30 2.10 8 4 -10 4.70 1.60 -8 -4 -10 9.50 1.90 -8 4 10 8.60 1.80 -8 5 -10 226.38 6.60 -8 5 -10 247.38 6.90 -8 -5 10 234.08 6.30 8 5 10 228.68 7.10 8 -5 -10 223.38 7.20 8 5 10 229.18 6.90 -8 -5 10 220.88 7.00 -8 -5 -10 227.18 6.60 8 5 -10 213.28 6.40 -8 5 10 222.88 6.50 8 -5 10 222.38 7.30 8 5 -10 244.48 6.60 -8 5 10 234.98 7.30 -8 -6 10 451.15 10.50 -8 6 -10 450.35 10.80 8 -6 -10 455.65 11.50 8 6 10 431.46 11.00 -8 6 -10 450.95 10.80 -8 -6 10 456.55 11.20 8 6 10 451.05 11.50 8 -6 10 431.96 11.50 -8 6 10 439.76 10.20 8 6 -10 439.96 10.60 -8 6 10 445.16 11.20 8 6 -10 437.46 10.60 -8 -6 -10 454.65 10.50 -8 7 -10 966.10 20.20 8 7 10 953.60 21.00 -8 -7 10 1007.70 20.00 -8 -7 10 944.11 20.30 8 7 10 923.91 20.40 -8 7 -10 967.30 19.90 8 -7 -10 955.90 20.70 8 -7 10 969.70 21.00 8 7 -10 939.31 19.80 8 7 -10 964.00 19.90 -8 7 10 936.91 19.30 -8 -7 -10 932.01 19.60 -8 7 10 985.40 20.80 -8 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8 -13 -10 157.88 7.30 -8 -13 10 155.98 7.80 8 13 10 160.78 7.60 -8 13 -10 155.58 7.50 -8 13 10 158.78 7.60 8 13 -10 153.28 6.70 -8 -13 -10 167.38 7.90 8 -13 10 161.88 8.20 8 14 10 6.60 3.20 8 -14 -10 5.90 3.10 -8 14 -10 0.40 2.70 -8 -14 10 -1.60 3.40 -8 14 10 0.80 2.80 8 -14 10 6.60 3.60 -8 -14 -10 5.00 3.30 8 -15 -10 2.90 3.10 8 15 10 6.90 3.70 -8 -15 10 -5.90 3.30 -8 15 -10 6.50 3.00 -8 15 10 0.80 2.90 8 -15 10 3.10 3.50 -8 -15 -10 4.80 3.50 -9 0 -10 86.99 2.90 -9 0 -10 86.99 4.20 9 0 10 87.59 3.30 9 0 -10 81.39 4.20 -9 0 10 81.29 4.20 9 0 10 78.29 4.00 -9 0 10 85.09 3.90 9 1 10 61.09 3.80 -9 1 -10 57.19 2.60 -9 1 -10 58.19 3.50 9 -1 -10 58.59 3.90 9 1 10 61.09 3.00 -9 -1 10 54.49 3.80 -9 -1 10 59.69 3.40 9 1 -10 61.89 3.70 -9 1 10 57.29 3.50 -9 1 10 60.19 3.80 9 -1 10 58.49 2.70 -9 -1 -10 61.59 3.70 -9 -1 -10 57.69 2.20 9 -1 10 56.59 3.80 9 -2 -10 88.09 4.40 -9 2 -10 87.49 4.20 9 2 10 83.09 4.40 -9 -2 10 89.09 4.30 9 2 10 82.89 3.70 -9 2 -10 85.59 3.40 9 -2 10 88.29 3.10 -9 2 10 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54.59 5.50 10 14 10 72.49 6.20 -10 -14 10 67.59 6.00 -10 -14 -10 61.19 5.80 10 -14 10 80.29 6.60 -10 14 10 54.79 5.30 10 -15 -10 65.19 6.00 -10 15 -10 62.19 6.60 -10 -15 10 62.19 6.10 -10 -15 -10 69.79 9.50 10 -15 10 61.89 6.10 -11 0 -10 95.89 4.70 11 0 10 94.69 4.90 -11 0 10 105.79 5.00 11 0 -10 90.39 4.90 11 0 10 97.19 3.90 -11 0 10 93.89 4.40 -11 -1 10 103.19 4.90 11 1 10 101.29 4.80 11 -1 -10 115.59 5.30 11 1 10 115.59 4.30 -11 -1 10 104.09 4.60 -11 1 -10 100.29 4.90 -11 1 10 115.99 5.10 11 1 -10 109.59 5.10 11 -1 10 104.79 5.10 11 -1 10 112.79 4.00 -11 1 10 102.19 4.60 -11 -1 -10 114.39 5.10 -11 2 -10 89.19 3.40 11 -2 -10 87.89 5.00 11 2 10 81.39 4.70 -11 -2 10 77.89 4.70 -11 2 -10 88.29 4.60 11 2 10 85.89 4.00 -11 -2 -10 91.89 4.70 -11 2 10 85.39 4.30 11 -2 10 86.19 4.80 11 2 -10 85.69 4.00 -11 2 10 91.99 4.60 11 -2 10 93.19 3.60 11 2 -10 86.59 4.70 -11 3 -10 35.70 3.30 11 3 10 31.00 2.80 -11 3 -10 28.20 2.30 -11 -3 10 26.40 3.00 11 -3 -10 27.50 3.30 11 3 10 31.80 3.30 11 -3 10 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5.90 3.50 -12 -13 -10 9.10 3.20 12 -13 10 9.30 3.50 12 -14 -10 -3.00 3.20 -12 14 -10 5.00 3.10 12 14 10 -1.00 3.30 12 -14 10 0.30 3.20 -12 14 10 0.50 3.90 -12 -14 -10 -4.00 3.10 13 0 -10 49.20 4.10 -13 0 -10 44.60 3.70 -13 0 10 46.10 3.90 13 0 10 47.70 3.40 13 0 10 48.00 4.20 -13 0 10 50.99 3.80 -13 1 -10 0.10 2.00 -13 -1 10 3.40 1.80 -13 -1 10 1.20 2.00 13 1 10 2.60 2.20 13 1 10 3.00 1.70 13 -1 -10 0.60 2.30 -13 1 10 2.60 2.20 -13 -1 -10 3.00 2.30 13 -1 10 0.40 2.20 13 1 -10 5.80 2.50 13 1 -10 2.30 1.70 13 -1 10 1.10 1.60 -13 1 10 3.20 1.90 13 2 10 91.29 5.20 13 -2 -10 98.99 5.50 -13 2 -10 100.79 5.10 13 2 10 98.09 4.60 -13 -2 10 97.59 5.30 13 2 -10 102.69 5.40 13 2 -10 97.79 4.30 -13 2 10 95.59 5.10 -13 2 10 95.49 4.70 13 -2 10 101.39 4.90 13 -2 10 92.79 5.00 -13 -2 -10 98.39 5.20 13 3 10 191.88 7.10 13 3 10 212.08 6.90 13 -3 -10 198.68 7.50 -13 -3 10 194.58 7.40 -13 3 -10 207.08 7.20 -13 -3 -10 198.88 7.10 -13 3 10 200.48 6.90 13 -3 10 207.68 7.50 13 3 -10 197.68 6.10 13 3 -10 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101.09 6.50 14 10 -10 97.99 5.90 -14 10 10 96.39 6.30 -14 11 -10 47.60 4.60 14 11 10 55.39 5.30 14 -11 -10 47.40 5.10 -14 11 10 39.40 4.70 14 11 -10 52.39 4.60 -14 -11 -10 44.80 4.90 14 -11 10 47.70 4.80 -14 12 -10 6.30 3.00 14 -12 -10 4.30 3.60 14 12 10 12.80 3.70 14 -12 10 6.10 3.20 -14 -12 -10 5.60 3.10 -14 12 10 6.00 3.00 14 12 -10 9.60 3.00 14 13 10 22.50 4.90 14 -13 -10 25.20 4.50 -14 13 -10 21.00 3.80 14 -13 10 28.60 4.60 -14 -13 -10 19.90 6.00 -14 13 10 24.20 4.40 -15 0 10 14.00 2.40 15 0 10 9.70 2.80 15 0 10 9.60 2.10 -15 0 -10 10.90 2.70 15 0 -10 10.20 3.00 -15 0 10 8.60 2.80 -15 -1 10 16.80 3.10 -15 1 -10 18.90 3.10 15 1 10 16.10 3.00 15 -1 -10 16.80 3.20 15 1 10 14.60 2.30 15 -1 10 12.60 3.00 -15 -1 -10 16.10 2.90 -15 1 10 13.30 2.70 15 1 -10 16.80 2.30 15 1 -10 18.40 3.30 -15 1 10 16.00 2.60 15 -1 10 17.10 2.40 15 2 10 8.40 2.30 -15 2 -10 8.10 2.70 -15 -2 10 7.50 2.50 15 -2 -10 2.90 2.90 15 2 10 4.30 2.30 15 2 -10 6.80 2.10 -15 2 10 4.20 2.30 -15 2 10 5.60 2.60 -15 -2 -10 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2.50 14 -5 -14 7.00 3.00 14 5 -14 4.30 2.20 -14 5 14 5.80 2.50 -14 -5 -14 7.10 2.70 -14 5 14 7.20 2.60 14 -5 14 1.90 2.80 14 5 -14 5.10 2.60 -14 -6 14 234.58 9.00 14 -6 -14 241.28 9.10 14 6 14 236.18 9.10 14 6 14 235.38 8.20 -14 6 -14 239.68 8.50 -14 6 14 234.78 8.80 14 -6 14 243.88 9.20 -14 6 14 229.98 8.00 14 6 -14 240.38 8.30 -14 -6 -14 222.58 8.30 -14 -7 14 8.20 3.00 14 7 14 12.90 3.50 -14 7 -14 15.30 3.00 14 -7 -14 18.50 3.90 14 7 14 14.80 3.10 -14 7 14 16.10 3.60 14 -7 14 10.60 3.50 -14 -7 -14 13.80 3.00 14 7 -14 14.80 3.00 14 8 14 4.10 2.60 -14 8 -14 -1.30 2.30 14 8 14 10.20 3.50 14 -8 -14 4.50 3.40 -14 -8 14 6.00 3.10 14 -8 14 1.90 3.00 -14 -8 -14 5.20 2.60 14 8 -14 5.80 2.80 -14 8 14 7.40 3.10 14 -9 -14 -1.70 3.10 -14 9 -14 0.60 2.40 14 9 14 1.30 2.70 -14 -9 14 3.30 2.90 -14 9 14 -0.60 2.90 -14 -9 -14 3.40 2.80 14 -9 14 0.90 3.10 -14 10 -14 9.50 3.00 -14 -10 14 10.60 3.20 14 10 14 8.50 3.10 14 -10 -14 7.20 3.60 14 -10 14 10.70 3.70 -14 -10 -14 9.90 3.40 -14 10 14 6.20 3.60 14 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15 -4 14 16.90 3.50 -15 -4 -14 21.50 3.50 15 5 14 3.70 2.30 -15 -5 14 5.10 3.00 -15 5 -14 9.40 2.80 15 -5 -14 0.00 2.70 15 5 14 4.60 2.70 -15 5 14 5.80 2.70 -15 5 14 1.40 2.50 15 -5 14 4.00 3.00 -15 -5 -14 6.20 2.80 15 5 -14 6.80 2.80 15 -6 -14 2.80 2.80 -15 6 -14 9.20 2.90 15 6 14 8.00 3.00 -15 -6 14 8.50 3.20 15 6 14 9.80 2.60 -15 6 14 8.40 3.00 15 6 -14 12.00 2.90 -15 -6 -14 4.80 2.70 -15 6 14 8.90 3.10 15 -6 14 2.20 3.00 15 7 14 21.70 3.90 15 7 14 35.40 3.90 15 -7 -14 38.70 4.80 -15 7 -14 26.40 3.50 -15 -7 14 28.90 4.10 15 7 -14 35.70 4.00 -15 -7 -14 22.40 3.70 15 -7 14 25.10 3.90 -15 7 14 23.20 3.90 15 8 14 30.40 4.40 -15 8 -14 25.50 3.60 -15 -8 14 26.50 3.90 15 -8 -14 23.70 4.20 15 8 14 27.00 3.70 -15 -8 -14 30.00 3.80 15 8 -14 25.30 3.70 -15 8 14 23.20 3.90 15 -8 14 28.60 4.20 -15 -9 14 -2.60 2.80 15 -9 -14 0.30 3.30 15 9 14 1.10 2.80 15 9 -14 1.60 3.30 15 -9 14 2.00 3.10 -15 9 14 2.70 3.30 -15 -9 -14 0.10 2.60 15 -10 -14 7.90 3.80 -15 -10 14 9.20 3.40 15 10 14 9.60 3.30 15 -10 14 9.30 3.40 -15 10 14 9.00 3.50 -15 -10 -14 5.90 3.20 16 0 -14 17.40 3.60 -16 0 -14 17.30 3.40 -16 0 14 15.40 3.60 16 0 14 12.90 3.40 16 0 -14 16.80 2.70 16 -1 -14 77.29 6.00 16 1 14 82.59 6.00 -16 1 -14 90.49 5.80 -16 -1 14 94.19 6.20 -16 1 14 83.29 5.40 16 -1 14 91.99 6.10 -16 -1 -14 91.29 5.90 16 1 -14 88.79 5.00 16 1 -14 76.49 5.90 -16 1 14 89.99 6.00 16 -2 -14 1.80 3.10 -16 2 -14 0.30 2.50 -16 -2 14 0.10 2.70 16 2 14 5.70 3.00 -16 2 14 -2.60 2.50 -16 -2 -14 2.60 2.60 16 2 -14 5.10 3.00 16 2 -14 2.80 2.50 16 -2 14 5.80 3.00 -16 2 14 0.90 2.40 16 3 14 69.39 5.70 16 -3 -14 52.89 4.90 -16 3 -14 66.89 5.30 -16 -3 14 62.59 5.40 16 -3 14 54.09 5.10 -16 -3 -14 63.59 5.10 16 3 -14 51.19 4.60 -16 3 14 49.40 4.60 -16 3 14 65.59 5.20 16 4 14 3.30 2.80 16 4 14 5.70 3.10 -16 4 -14 5.60 2.80 16 -4 -14 7.50 3.40 -16 -4 14 2.50 2.90 16 4 -14 7.70 3.00 -16 -4 -14 2.10 2.70 -16 4 14 3.50 2.70 16 -4 14 7.50 3.20 -16 4 14 6.00 2.80 16 5 14 78.79 5.10 16 -5 -14 72.49 6.20 -16 -5 14 73.09 6.00 16 5 14 70.69 5.90 -16 5 -14 76.69 5.60 16 5 -14 85.09 5.70 -16 5 14 78.39 5.70 -16 5 14 75.99 5.60 16 -5 14 83.59 6.20 -16 -5 -14 72.19 5.50 -16 -6 14 -2.50 2.80 -16 6 -14 -1.20 2.50 16 -6 -14 3.00 3.00 16 6 14 4.60 2.90 16 6 14 0.40 2.40 -16 6 14 1.90 2.70 -16 -6 -14 3.00 2.70 16 6 -14 3.40 2.70 16 -6 14 0.80 2.90 -16 7 -14 3.00 2.70 16 7 14 1.00 3.00 16 7 14 -0.50 2.40 -16 -7 14 1.20 2.90 16 -7 -14 1.50 3.30 16 -7 14 1.60 3.00 -16 7 14 4.30 3.10 -16 -7 -14 0.80 2.70 16 7 -14 8.40 3.00 16 8 14 63.89 5.80 16 -8 -14 48.60 5.30 -16 -8 14 72.89 6.10 -16 8 -14 60.59 5.00 16 8 14 69.19 5.90 -16 -8 -14 61.19 5.20 16 -8 14 71.79 6.10 -16 8 14 65.19 5.70 -16 -8 -14 54.39 5.10 16 8 -14 64.49 5.50 16 -9 -14 43.50 5.20 -16 -9 14 55.89 5.30 16 9 14 55.19 5.20 16 -9 14 51.19 5.40 16 9 -14 42.00 4.50 -16 9 14 53.39 5.30 -16 -9 -14 43.80 5.10 -16 -10 14 1.90 3.10 16 10 14 -1.50 2.80 16 -10 -14 -0.70 6.00 -16 10 14 4.80 3.40 -16 -10 -14 -0.70 4.70 16 -10 14 2.60 3.40 17 0 -14 3.70 3.00 -17 0 -14 3.70 2.80 17 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14 34.30 4.00 -17 6 -14 35.20 4.20 17 6 14 29.90 4.30 -17 -6 -14 38.90 4.40 17 6 -14 38.30 4.30 -17 6 14 25.70 3.90 17 -6 14 39.40 4.80 -17 7 -14 32.30 4.00 17 -7 -14 29.70 4.80 17 7 14 35.20 4.10 -17 -7 14 37.40 4.80 17 7 14 33.30 4.80 17 7 -14 38.40 4.30 17 -7 14 38.50 4.80 -17 -7 -14 38.40 4.40 -17 7 14 32.60 4.30 17 8 14 49.40 5.30 17 8 14 64.89 5.50 -17 -8 14 55.59 5.60 17 -8 -14 49.00 5.40 -17 8 -14 52.49 4.80 -17 -8 -14 57.79 5.20 17 -8 14 50.39 5.50 17 8 -14 64.39 5.40 -17 8 14 55.19 5.40 -17 -8 -14 58.09 5.40 17 -9 -14 1.50 5.90 -17 -9 14 5.80 3.40 17 9 14 1.60 2.80 -17 -9 -14 0.90 3.20 17 9 -14 5.20 3.00 17 -9 14 3.20 3.40 -17 9 14 1.40 3.20 -18 0 -14 112.09 6.70 18 0 14 107.19 6.40 18 0 -14 106.19 6.90 -18 0 14 101.79 6.80 18 1 14 37.60 4.60 -18 -1 14 51.39 5.20 -18 1 -14 48.50 4.90 18 -1 -14 43.10 4.90 -18 1 14 52.29 5.00 18 1 -14 48.50 5.00 18 -1 14 34.00 4.30 -18 -1 -14 36.80 4.50 -18 -2 14 57.49 5.30 18 -2 -14 65.49 5.90 18 2 14 59.79 5.30 -18 2 -14 72.79 5.70 18 2 -14 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29.80 4.60 20 -4 14 23.60 4.20 0 0 15 -0.90 1.50 0 0 -15 -0.60 1.30 0 0 15 1.40 1.30 0 0 -15 -1.10 1.10 0 1 15 -0.10 1.40 0 -1 15 0.30 1.40 0 1 15 0.40 1.30 0 1 -15 -0.20 1.50 0 -1 -15 0.20 1.40 0 -1 15 1.50 1.70 0 -1 -15 0.50 1.20 0 1 -15 0.00 1.00 0 2 -15 691.83 15.10 0 -2 -15 711.33 14.50 0 -2 15 674.43 15.40 0 2 15 711.63 15.20 0 2 15 679.03 15.20 0 -2 15 723.83 14.90 0 2 15 705.33 14.60 0 3 15 0.90 1.40 0 3 15 -2.50 1.30 0 -3 15 -0.70 1.70 0 -3 -15 0.90 1.40 0 3 -15 0.50 1.60 0 3 15 2.50 1.70 0 -3 15 -2.50 1.50 0 -4 15 208.28 6.70 0 -4 15 206.78 6.40 0 4 15 203.18 6.20 0 4 15 197.08 5.90 0 4 15 206.88 6.40 0 4 15 199.48 6.20 0 4 -15 195.48 6.40 0 -5 15 0.40 1.80 0 -5 15 -3.40 1.40 0 5 15 -2.00 1.40 0 5 15 -0.20 1.60 0 5 15 0.40 1.80 0 5 -15 1.10 1.90 0 5 15 0.00 1.50 0 -6 15 0.80 1.90 0 -6 -15 2.40 1.50 0 6 -15 2.10 2.10 0 6 15 0.30 1.80 0 -6 15 3.30 1.90 0 6 15 -1.60 1.50 0 6 15 2.00 1.90 0 7 15 -2.20 1.90 0 -7 15 0.20 1.70 0 -7 15 4.90 2.20 0 7 15 0.20 1.50 0 7 15 -2.60 1.80 0 7 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4.10 -2 6 -27 18.20 3.80 -2 -6 27 25.50 4.40 2 -6 -27 26.90 3.90 2 6 -27 22.60 4.10 2 -6 27 23.30 4.10 -2 7 -27 8.50 3.50 -2 -7 27 3.20 3.00 2 -7 -27 4.30 2.80 2 7 -27 8.70 5.70 2 -7 27 7.40 3.30 3 0 -27 0.00 2.90 -3 0 -27 4.40 2.70 3 0 27 0.40 2.80 -3 0 27 4.20 3.00 3 -1 -27 26.00 3.90 -3 1 -27 28.90 3.90 3 1 27 32.80 4.20 -3 -1 27 24.50 4.00 -3 -1 -27 26.30 3.60 3 1 -27 25.60 3.80 3 -1 27 27.70 4.10 -3 1 27 23.20 3.70 -3 2 -27 22.10 3.60 3 2 27 18.80 3.60 3 -2 -27 21.70 3.70 -3 -2 27 26.60 3.90 -3 -2 -27 19.70 3.40 3 2 -27 26.60 4.10 -3 2 27 21.10 3.60 3 -2 27 29.00 4.10 3 3 27 -1.50 2.70 -3 3 -27 -2.00 2.60 -3 -3 27 -1.50 2.40 3 -3 -27 5.20 3.00 3 -3 27 1.70 2.80 -3 3 27 2.20 2.60 -3 -3 -27 0.50 3.20 3 3 -27 -0.50 2.60 3 4 27 13.70 3.30 -3 4 -27 8.90 3.20 3 -4 -27 9.70 3.20 -3 -4 27 7.30 3.40 -3 4 27 10.50 3.20 3 4 -27 9.90 3.50 3 -4 27 7.60 3.20 3 -5 -27 3.30 2.90 -3 5 -27 1.20 2.80 3 5 27 1.10 2.60 -3 -5 27 0.60 2.90 3 5 -27 -2.20 2.80 -3 5 27 2.70 2.80 3 -5 27 -1.00 3.00 3 -6 -27 6.10 3.10 -3 -6 27 1.40 3.20 -3 6 -27 6.60 3.20 3 -6 27 2.60 3.10 3 6 -27 6.60 3.20 -4 0 -27 -1.50 2.40 -4 0 27 1.10 2.70 4 0 -27 1.60 2.90 4 0 27 1.30 2.80 -4 1 -27 0.10 2.70 4 -1 -27 3.30 2.90 -4 -1 27 3.40 2.70 4 1 27 -3.00 2.70 4 -1 27 3.50 3.00 -4 1 27 5.90 3.00 4 1 -27 -2.20 2.80 -4 -1 -27 -1.10 2.40 -4 -2 27 59.69 5.40 4 -2 -27 56.09 5.10 -4 2 -27 58.09 4.90 4 2 27 60.29 5.30 4 -2 27 50.29 5.00 -4 2 27 53.59 4.90 4 2 -27 70.99 5.60 4 -3 -27 65.99 5.50 -4 -3 27 69.99 5.90 4 3 27 73.59 5.80 -4 3 -27 65.39 5.40 4 -3 27 71.59 6.00 -4 3 27 70.89 5.70 4 3 -27 59.49 5.10 -4 -4 27 79.79 6.50 4 4 27 67.89 5.60 -4 4 -27 66.79 5.30 4 -4 -27 60.29 5.20 4 4 -27 62.39 5.50 -4 4 27 78.69 6.10 4 -4 27 58.29 5.60 -4 -5 27 4.60 3.20 4 -5 -27 0.10 2.60 -4 5 -27 2.10 2.90 4 5 27 -0.20 2.60 -4 5 27 2.10 2.80 4 5 -27 2.40 3.20 -4 -5 -27 0.80 2.60 4 -5 27 5.70 3.30 -4 -6 27 4.60 3.40 4 -6 -27 0.20 2.80 -4 6 -27 10.80 3.50 4 -6 27 7.30 3.50 4 6 -27 6.10 3.30 5 0 27 -0.20 2.80 5 0 -27 1.40 2.90 -5 0 27 6.00 3.00 5 -1 -27 14.80 3.70 -5 1 -27 17.60 3.40 5 1 27 16.20 3.60 -5 -1 27 17.50 3.70 5 1 -27 15.50 3.50 5 -1 27 20.40 3.80 -5 1 27 17.80 3.60 -5 2 -27 25.90 3.70 5 -2 -27 20.50 3.90 5 2 27 26.90 4.10 -5 -2 27 33.40 4.30 5 -2 27 27.60 4.20 -5 2 27 23.40 3.90 5 2 -27 27.20 4.30 5 3 27 13.30 3.40 -5 3 -27 9.50 3.00 5 -3 -27 14.20 3.50 -5 -3 27 23.70 4.00 5 -3 27 11.20 3.40 5 -3 27 18.60 4.60 5 3 -27 12.00 3.60 -5 3 27 21.10 3.70 -5 -4 27 3.40 2.80 5 -4 -27 6.20 3.10 -5 4 -27 4.50 2.90 -5 -4 -27 3.40 2.90 5 -4 27 5.50 3.10 5 -4 27 4.30 3.10 -5 4 27 1.90 2.70 5 4 -27 0.40 3.00 -5 5 -27 9.00 3.20 5 -5 -27 12.10 3.50 -5 -5 27 7.90 3.40 -5 -5 -27 13.50 3.30 5 -5 27 19.90 4.00 -5 5 27 13.80 4.20 5 -5 27 18.10 3.60 5 5 -27 19.30 4.00 -5 -6 27 27.90 4.40 5 -6 -27 23.10 4.00 -5 6 -27 24.80 4.00 -5 6 27 39.90 5.00 5 -6 27 36.10 4.40 5 -6 27 26.60 4.30 6 0 -27 -3.80 2.70 6 0 27 -0.10 2.50 6 0 27 5.80 2.70 -6 0 27 0.90 2.70 6 -1 -27 52.49 5.00 -6 -1 27 56.29 5.10 6 1 27 44.30 5.00 -6 1 27 51.39 4.90 6 -1 27 49.90 5.10 6 1 -27 53.79 5.30 6 -1 27 47.40 4.80 -6 -1 -27 46.10 4.90 -6 -2 27 -1.00 2.70 6 -2 -27 4.80 3.20 6 -2 27 0.30 2.70 6 2 -27 1.70 2.90 -6 2 27 5.60 2.90 -6 -2 -27 -0.10 2.90 6 -2 27 4.90 2.90 6 -3 -27 -0.80 2.80 -6 3 -27 0.70 2.60 -6 -3 27 -1.20 2.80 -6 -3 -27 -4.70 2.50 -6 3 27 5.60 2.80 6 3 -27 3.40 3.20 6 -3 27 3.80 3.20 6 -3 27 1.50 2.80 6 -4 -27 3.70 3.20 -6 4 -27 5.20 2.90 -6 -4 27 7.40 3.30 -6 4 27 11.90 3.20 6 4 -27 3.80 3.00 6 -4 27 10.10 3.50 6 -4 27 5.80 3.20 -6 -4 -27 0.00 2.70 -6 5 -27 19.50 3.80 -6 -5 27 21.80 4.20 6 -5 -27 20.70 4.00 6 -5 27 21.50 4.00 6 5 -27 17.10 3.80 6 -5 27 15.70 3.80 -6 -5 -27 14.40 3.50 7 0 -27 2.80 2.90 -7 0 -27 -5.00 2.50 -7 0 27 1.20 2.90 7 0 27 3.60 2.80 -7 1 -27 16.30 3.40 -7 -1 27 20.50 3.80 7 -1 -27 17.40 3.60 7 1 27 17.90 3.50 -7 1 27 18.00 3.70 7 -1 27 22.40 3.80 -7 -1 -27 14.40 3.30 7 1 -27 16.20 3.80 -7 -2 27 18.50 3.80 7 2 27 12.70 3.30 7 -2 -27 14.20 3.70 -7 2 -27 11.50 3.40 7 -2 27 16.30 3.70 -7 2 27 19.20 3.70 7 2 -27 16.30 3.70 -7 -2 -27 13.40 3.40 7 -3 -27 11.70 3.50 -7 -3 27 12.20 3.50 -7 3 -27 10.30 3.40 7 3 27 6.60 2.90 7 -3 27 10.50 3.50 -7 -3 -27 11.20 3.40 7 3 -27 12.20 3.60 -7 3 27 14.80 3.50 7 -3 27 11.60 3.20 -7 -4 27 115.19 7.40 -7 4 -27 118.19 7.20 7 -4 -27 110.49 7.10 7 -4 27 121.09 7.10 -7 4 27 122.79 7.10 -7 -4 -27 121.69 7.00 7 -4 27 121.99 7.50 7 4 -27 116.09 7.00 -7 5 -27 2.70 2.80 7 -5 -27 7.80 5.10 -7 5 -27 9.70 5.40 7 -5 27 7.50 3.40 -7 -5 -27 6.00 3.10 7 -5 27 9.10 5.70 -8 0 27 2.70 3.00 8 0 -27 1.20 2.80 -8 0 -27 -2.50 2.80 8 0 27 5.10 3.00 8 -1 -27 4.70 3.30 -8 1 -27 11.10 3.60 -8 -1 27 6.60 3.20 8 1 27 12.50 3.30 8 1 -27 12.70 3.70 -8 -1 -27 7.00 3.30 -8 1 27 10.80 3.40 8 -1 27 5.90 3.30 8 -2 -27 110.69 7.10 -8 2 -27 120.79 7.30 -8 -2 27 115.39 7.30 8 2 27 122.49 7.00 -8 2 27 127.09 7.20 -8 -2 -27 112.89 7.00 8 -2 27 129.99 7.30 8 2 -27 119.19 7.20 8 3 27 -4.60 2.40 -8 -3 27 0.70 3.20 8 -3 -27 -2.40 2.80 -8 3 -27 -4.80 2.50 8 -3 27 0.80 2.80 -8 -3 -27 1.60 2.80 -8 3 27 1.70 2.90 8 3 -27 -1.30 3.00 -8 4 -27 38.40 7.20 8 4 27 45.20 5.00 8 -4 27 33.80 4.50 8 4 -27 28.00 6.00 -8 4 27 36.10 4.50 -8 -4 -27 26.60 4.10 -9 0 27 0.70 2.90 9 0 -27 2.10 3.30 -9 0 -27 0.20 2.90 9 0 27 0.60 2.90 9 -1 -27 14.40 4.10 -9 1 -27 8.60 3.40 9 1 27 4.90 3.20 -9 -1 27 14.60 3.60 9 -1 27 10.30 3.40 -9 1 27 13.90 3.60 -9 -1 -27 13.50 3.60 9 1 -27 10.30 3.70 9 2 27 43.40 4.80 -9 -2 27 64.29 8.60 -9 2 -27 40.10 7.00 9 -2 -27 56.19 8.40 -9 -2 -27 45.00 4.80 9 -2 27 52.39 5.30 9 2 -27 42.80 5.50 -9 2 27 46.20 4.90 0 0 -28 707.43 17.90 0 0 28 712.03 18.50 0 1 -28 0.00 2.90 0 -1 28 3.70 2.90 0 -1 -28 0.40 2.70 0 1 28 1.10 2.90 0 -2 28 7.80 3.20 0 2 -28 7.60 3.20 0 -2 -28 3.70 2.80 0 2 28 4.30 3.00 0 3 -28 -1.20 2.90 0 -3 -28 1.80 2.70 0 3 28 0.40 2.50 0 -3 28 -0.50 2.80 0 4 -28 60.19 5.50 0 4 28 79.89 5.90 0 -4 -28 68.89 5.60 0 -4 28 75.39 6.10 0 5 28 0.50 2.60 0 5 -28 -1.60 3.00 0 -5 28 -2.80 3.20 0 -5 -28 -0.10 2.70 -1 0 28 20.70 3.70 1 0 -28 26.60 4.10 1 0 28 15.30 3.70 -1 0 -28 21.90 3.70 -1 1 -28 25.70 4.00 1 -1 -28 22.60 3.90 1 1 28 21.20 3.90 -1 -1 28 30.80 4.10 1 1 -28 23.60 4.00 1 -1 28 31.30 4.20 -1 -1 -28 21.00 3.60 -1 1 28 29.70 4.40 -1 2 -28 33.90 4.40 1 2 28 37.00 4.50 -1 -2 28 31.20 4.40 1 -2 -28 36.10 4.40 -1 2 28 36.70 4.70 1 2 -28 35.20 4.40 -1 -2 -28 44.70 4.50 1 -2 28 44.60 4.80 1 3 28 1.50 2.80 -1 3 -28 -1.30 2.90 1 -3 -28 -3.00 2.50 -1 -3 28 -5.00 2.30 -1 -3 -28 2.10 2.70 1 -3 28 -0.80 2.60 1 3 -28 -4.50 2.80 -1 3 28 3.00 2.80 -1 4 -28 5.50 3.20 1 4 28 7.50 3.10 -1 -4 28 0.30 3.30 1 -4 -28 6.50 3.10 -1 4 28 9.90 3.10 1 -4 28 4.90 3.30 1 4 -28 11.20 3.60 -1 -4 -28 7.40 2.90 -1 5 -28 0.00 3.00 -1 -5 28 4.10 3.40 1 5 28 4.10 2.80 1 -5 -28 6.90 3.10 -1 5 28 2.50 2.80 1 5 -28 -5.30 2.60 -1 -5 -28 2.40 2.70 1 -5 28 4.30 3.30 -2 0 -28 29.30 3.90 2 0 28 21.50 4.10 -2 0 28 23.70 3.80 2 0 -28 18.40 3.60 2 -1 -28 155.38 7.50 2 1 28 137.39 7.50 -2 1 -28 148.59 7.30 -2 -1 28 150.48 7.60 -2 1 28 145.59 7.60 -2 -1 -28 136.69 6.90 2 1 -28 131.89 7.20 2 -1 28 133.39 7.50 2 2 28 2.00 2.90 2 -2 -28 0.80 2.70 -2 2 -28 -2.60 2.80 -2 -2 28 5.40 3.00 2 2 -28 -3.20 2.80 2 -2 28 2.20 2.90 -2 -2 -28 0.50 2.70 -2 2 28 1.30 2.90 -2 -3 28 23.30 4.10 2 -3 -28 23.10 3.90 -2 3 -28 27.30 4.10 2 3 28 27.40 4.10 2 3 -28 19.30 4.00 -2 3 28 22.40 4.00 2 -3 28 23.60 4.20 -2 -3 -28 20.90 3.70 -2 -4 28 1.00 3.10 2 4 28 -1.00 2.70 2 -4 -28 0.70 2.80 -2 4 -28 -1.50 2.90 2 -4 28 0.40 3.10 -2 4 28 -0.40 2.70 2 4 -28 1.20 3.00 -2 -5 28 34.00 4.60 -2 5 -28 50.19 5.10 2 5 28 48.10 4.80 2 -5 -28 43.90 4.60 2 -5 28 56.79 5.70 -2 5 28 58.69 5.70 2 5 -28 41.70 4.90 3 0 28 124.79 7.30 -3 0 28 126.09 7.20 3 0 -28 123.39 7.20 -3 0 -28 129.09 6.70 -3 -1 28 28.50 4.20 3 1 28 21.30 4.10 -3 1 -28 23.80 3.80 3 -1 -28 21.80 3.80 -3 -1 -28 24.80 3.70 -3 1 28 34.20 4.50 3 1 -28 21.60 3.90 3 -1 28 31.20 4.40 3 2 28 0.90 2.90 -3 2 -28 0.50 2.80 3 -2 -28 -2.40 2.80 -3 -2 28 -1.10 2.80 3 -2 28 0.90 2.80 3 2 -28 5.50 3.20 -3 -2 -28 2.30 2.60 -3 2 28 1.60 2.90 -3 -3 28 64.49 5.80 -3 3 -28 50.29 4.80 3 3 28 55.29 5.10 3 -3 -28 64.89 5.60 3 -3 28 65.19 5.90 3 3 -28 64.09 5.60 -3 3 28 60.19 5.30 3 -4 -28 1.30 2.80 -3 4 -28 2.50 3.00 3 4 28 -4.10 2.60 -3 -4 28 2.90 3.30 3 4 -28 -1.10 2.80 -3 4 28 0.90 2.80 3 -4 28 -5.00 2.90 -3 5 -28 28.30 4.30 3 5 28 32.90 4.20 3 -5 -28 27.50 4.00 -3 -5 28 25.60 5.70 -3 5 28 28.50 6.70 3 -5 28 30.10 5.10 3 5 -28 25.60 6.70 -4 0 28 161.18 8.20 4 0 28 171.78 8.30 -4 0 -28 171.08 7.60 4 0 -28 178.08 8.20 4 -1 -28 84.99 6.30 -4 -1 28 101.79 6.80 -4 1 -28 96.29 6.10 4 1 28 91.89 6.60 -4 1 28 108.39 6.80 4 -1 28 97.59 6.70 4 1 -28 89.59 6.40 -4 2 -28 2.60 2.80 4 2 28 1.10 2.80 4 -2 -28 -3.30 2.60 -4 -2 28 6.30 3.00 4 2 -28 4.00 3.10 4 -2 28 1.00 3.00 -4 2 28 -0.60 2.80 -4 -3 28 0.60 2.80 -4 3 -28 0.90 2.80 4 3 28 -2.30 2.80 4 -3 -28 -0.60 2.90 -4 3 28 -1.50 2.50 4 3 -28 -0.30 2.90 4 -3 28 0.10 3.20 4 -4 -28 38.10 4.60 -4 -4 28 40.70 5.10 -4 4 -28 41.60 4.70 4 4 28 31.90 4.30 4 -4 28 33.30 4.90 4 4 -28 39.90 4.70 -4 4 28 39.10 4.50 5 0 28 2.00 3.00 5 0 -28 -0.70 2.90 -5 0 28 6.90 2.90 5 -1 -28 1.60 2.90 5 1 28 4.90 3.20 -5 -1 28 1.60 2.90 5 -1 28 -2.20 2.90 -5 1 28 6.50 3.20 5 1 -28 -2.60 2.90 5 -2 -28 -3.20 2.90 5 2 28 -0.70 3.00 -5 2 -28 5.10 2.90 -5 -2 28 4.80 3.20 -5 2 28 -1.00 2.80 5 -2 28 1.00 3.20 5 2 -28 -2.90 2.90 -5 -3 28 21.90 4.20 -5 3 -28 22.40 3.70 5 3 28 24.30 3.90 5 -3 -28 14.60 3.60 5 3 -28 17.20 3.90 -5 -3 -28 17.30 3.80 5 -3 28 14.10 3.60 -5 3 28 22.00 3.90 -5 4 -28 38.80 4.60 -5 -4 28 39.00 7.60 5 -4 -28 33.80 4.40 5 4 -28 28.30 6.40 5 -4 28 36.70 7.50 -5 4 28 29.10 4.20 -5 -4 -28 33.10 4.40 6 0 28 7.20 3.30 6 0 -28 12.30 3.70 -6 0 28 15.20 3.60 6 -1 -28 3.60 3.10 6 1 28 3.10 3.10 -6 -1 28 3.70 2.90 6 1 -28 1.80 3.20 -6 1 28 7.70 3.00 6 -1 28 6.80 3.40 -6 -1 -28 3.50 3.10 -6 -2 28 46.60 5.10 6 -2 -28 37.70 4.60 6 2 -28 34.10 4.40 6 -2 28 38.50 4.90 -6 2 28 45.70 4.80 -6 -2 -28 36.30 4.60 6 -3 -28 15.00 3.70 -6 -3 28 21.60 6.40 6 3 -28 14.10 5.70 -6 -3 -28 9.40 3.30 -6 3 28 15.30 3.50 -7 0 28 177.08 8.60 7 0 -28 182.28 9.60 -7 0 -28 163.58 8.30 7 0 28 179.38 9.00 -7 1 -28 -1.20 3.10 7 -1 -28 1.70 3.60 -7 -1 28 4.00 3.10 7 -1 28 3.60 3.00 7 1 -28 7.60 5.40 -7 -1 -28 1.30 3.00 -7 1 28 3.70 3.00 -7 2 28 44.00 4.90 7 -2 28 50.39 5.00 -7 -2 -28 44.60 5.10 0 0 29 6.20 3.10 0 0 -29 5.30 3.10 0 -1 -29 1.20 2.90 0 1 29 7.20 3.20 0 1 -29 -1.90 2.90 0 -1 29 0.50 2.90 0 -2 -29 544.55 15.20 0 -2 29 558.04 16.20 0 2 29 526.75 15.50 0 2 -29 553.14 15.50 0 3 -29 0.60 3.30 0 -3 -29 -2.50 2.60 0 -3 29 -0.10 4.40 0 3 29 -1.50 2.60 1 0 29 2.80 3.00 1 0 -29 0.40 2.90 -1 0 29 3.50 3.20 -1 0 -29 2.70 3.00 -1 1 -29 8.30 3.30 1 1 29 0.20 2.90 1 -1 -29 5.10 3.20 -1 -1 29 1.70 3.20 1 -1 29 11.30 3.40 1 1 -29 3.60 3.30 -1 1 29 13.50 3.70 -1 -1 -29 11.10 3.30 1 -2 -29 0.10 2.90 1 2 29 2.70 3.10 -1 2 -29 -2.30 2.80 -1 -2 29 3.50 3.20 1 2 -29 2.20 3.10 -1 -2 -29 2.70 2.90 -1 2 29 5.60 3.30 1 -2 29 2.50 3.20 1 3 29 14.60 3.70 1 -3 -29 17.30 3.70 -1 3 -29 17.50 3.80 -1 -3 -29 13.90 3.40 1 3 -29 14.60 3.80 1 -3 29 11.40 5.80 -1 3 29 16.50 3.50 -2 0 -29 -4.50 2.60 2 0 29 -1.00 2.90 2 0 -29 -5.90 2.70 -2 0 29 5.00 3.30 -2 1 -29 193.78 8.50 -2 -1 29 194.38 9.00 2 1 29 200.88 9.00 2 -1 -29 201.78 8.80 2 1 -29 203.78 8.90 -2 1 29 210.28 9.10 -2 -1 -29 202.78 8.50 2 -1 29 200.68 9.10 2 2 29 -0.30 3.00 2 -2 -29 1.60 2.80 -2 2 -29 3.20 3.10 -2 -2 29 -0.70 3.20 2 -2 29 8.00 3.70 2 2 -29 4.10 3.30 -2 -2 -29 1.80 2.80 -2 2 29 -0.60 3.00 -2 3 -29 351.96 11.80 2 -3 -29 366.36 12.00 2 3 29 382.16 12.30 2 3 -29 364.16 12.50 -2 3 29 374.96 12.50 -2 -3 -29 357.66 12.00 3 0 -29 0.20 2.90 3 0 29 0.30 3.00 -3 0 29 4.60 3.10 -3 0 -29 0.20 2.70 -3 1 -29 -3.90 2.60 -3 -1 29 -1.20 2.90 3 -1 -29 2.20 3.10 3 1 29 -2.70 2.70 -3 -1 -29 -0.20 2.80 3 1 -29 3.60 3.20 3 -1 29 -0.40 3.00 -3 1 29 3.90 3.10 -3 -2 29 8.80 4.60 3 -2 -29 16.70 3.80 3 2 29 9.10 3.50 -3 2 -29 12.70 3.70 3 2 -29 13.50 3.70 -3 2 29 11.60 3.40 -4 0 29 2.00 3.10 4 0 29 -1.80 2.90 4 0 -29 0.70 3.00 4 1 29 4.50 3.30 4 -1 -29 -0.90 2.90 -4 -1 29 6.70 3.90 -4 1 -29 0.20 2.90 4 1 -29 -0.20 3.10 -4 1 29 0.70 3.10 4 -1 29 1.20 4.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46343 #===END data_AdBrettPhos _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'AdBrettPhos' _chemical_melting_point ? _chemical_formula_moiety 'C43 H61 O2 P, 0.06(H2 O)' _chemical_formula_sum 'C43 H61.12 O2.06 P' _chemical_formula_weight 641.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.838(4) _cell_length_b 16.357(5) _cell_length_c 19.029(5) _cell_angle_alpha 97.751(4) _cell_angle_beta 102.559(4) _cell_angle_gamma 102.096(4) _cell_volume 3745.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4425 _cell_measurement_theta_min 2.239 _cell_measurement_theta_max 21.518 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_F_000 1401.9 _exptl_transmission_factor_min 0.912 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.108 _shelx_estimated_absorpt_T_min 0.979 _shelx_estimated_absorpt_T_max 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43918 _diffrn_reflns_av_unetI/netI 0.1186 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.297 _diffrn_reflns_theta_max 27.131 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 16418 _reflns_number_gt 8030 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5596P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 16418 _refine_ls_number_parameters 879 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1590 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O5 O 0.975(2) 0.9720(15) 0.5055(15) 0.083(8) Uiso 0.12 1 d . . P A -1 P1 P 0.73730(6) 0.30054(5) 1.03942(4) 0.02972(19) Uani 1 1 d . . . . . O1 O 0.66213(17) 0.23023(13) 1.16849(11) 0.0415(5) Uani 1 1 d . . . . . O2 O 0.89693(18) 0.03673(14) 1.03976(12) 0.0459(6) Uani 1 1 d . . . . . C1 C 0.7489(2) 0.20030(17) 1.07387(15) 0.0291(7) Uani 1 1 d . . . . . C2 C 0.7157(2) 0.17748(18) 1.13621(15) 0.0313(7) Uani 1 1 d . . . . . C3 C 0.6306(3) 0.2120(2) 1.23205(19) 0.0606(11) Uani 1 1 d . . . . . H3A H 0.579066 0.157340 1.220754 0.091 Uiso 1 1 calc R U . . . H3B H 0.596842 0.254877 1.249790 0.091 Uiso 1 1 calc R U . . . H3C H 0.694434 0.211278 1.269013 0.091 Uiso 1 1 calc R U . . . C4 C 0.7370(2) 0.1075(2) 1.16339(16) 0.0364(7) Uani 1 1 d . . . . . H4 H 0.711028 0.092737 1.203068 0.044 Uiso 1 1 calc R U . . . C5 C 0.7971(3) 0.0588(2) 1.13197(17) 0.0400(8) Uani 1 1 d . . . . . H5 H 0.812952 0.012121 1.151101 0.048 Uiso 1 1 calc R U . . . C6 C 0.8333(2) 0.08000(19) 1.07205(16) 0.0342(7) Uani 1 1 d . . . . . C7 C 0.9427(3) -0.0225(2) 1.0775(2) 0.0579(10) Uani 1 1 d . . . . . H7A H 0.982673 0.005283 1.126563 0.087 Uiso 1 1 calc R U . . . H7B H 0.991706 -0.043390 1.052166 0.087 Uiso 1 1 calc R U . . . H7C H 0.884473 -0.069324 1.079072 0.087 Uiso 1 1 calc R U . . . C8 C 0.8059(2) 0.14777(17) 1.04012(15) 0.0284(6) Uani 1 1 d . . . . . C9 C 0.8371(2) 0.15416(18) 0.96855(16) 0.0304(7) Uani 1 1 d . . . . . C10 C 0.7739(2) 0.09550(19) 0.90486(16) 0.0360(7) Uani 1 1 d . . . . . C11 C 0.6741(3) 0.0257(2) 0.90395(18) 0.0456(8) Uani 1 1 d . . . . . H11 H 0.656217 0.036947 0.951287 0.055 Uiso 1 1 calc R U . . . C12 C 0.5719(3) 0.0227(2) 0.84407(19) 0.0554(10) Uani 1 1 d . . . . . H12A H 0.582410 0.002196 0.797059 0.083 Uiso 1 1 calc R U . . . H12B H 0.560061 0.078908 0.845409 0.083 Uiso 1 1 calc R U . . . H12C H 0.509007 -0.014694 0.852062 0.083 Uiso 1 1 calc R U . . . C13 C 0.6988(4) -0.0623(2) 0.8956(2) 0.0769(13) Uani 1 1 d . . . . . H13A H 0.720260 -0.073880 0.850753 0.115 Uiso 1 1 calc R U . . . H13B H 0.634072 -0.104818 0.894609 0.115 Uiso 1 1 calc R U . . . H13C H 0.757481 -0.063269 0.936273 0.115 Uiso 1 1 calc R U . . . C14 C 0.8082(3) 0.0962(2) 0.84012(17) 0.0443(8) Uani 1 1 d . . . . . H14 H 0.765271 0.058097 0.797961 0.053 Uiso 1 1 calc R U . . . C15 C 0.9027(3) 0.1511(2) 0.83631(18) 0.0470(9) Uani 1 1 d . . . . . C16A C 0.9334(5) 0.1381(5) 0.7630(4) 0.0552(19) Uani 0.724(8) 1 d D . P B 1 H16A H 0.899442 0.079273 0.737254 0.066 Uiso 0.724(8) 1 calc R U P B 1 C17A C 0.8943(6) 0.1974(6) 0.7159(4) 0.085(3) Uani 0.724(8) 1 d D . P B 1 H17A H 0.815473 0.185657 0.704959 0.128 Uiso 0.724(8) 1 calc R U P B 1 H17B H 0.916885 0.189349 0.671057 0.128 Uiso 0.724(8) 1 calc R U P B 1 H17C H 0.925581 0.255100 0.741407 0.128 Uiso 0.724(8) 1 calc R U P B 1 C18A C 1.0593(5) 0.1560(5) 0.7731(4) 0.0650(19) Uani 0.724(8) 1 d D . P B 1 H18A H 1.075197 0.149651 0.725952 0.097 Uiso 0.724(8) 1 calc R U P B 1 H18B H 1.087559 0.116451 0.800123 0.097 Uiso 0.724(8) 1 calc R U P B 1 H18C H 1.093306 0.213039 0.799581 0.097 Uiso 0.724(8) 1 calc R U P B 1 C16B C 0.9579(15) 0.1772(12) 0.7705(11) 0.0552(19) Uani 0.276(8) 1 d D . P B 2 H16B H 0.991742 0.237838 0.774926 0.066 Uiso 0.276(8) 1 calc R U P B 2 C17B C 1.0343(17) 0.1151(14) 0.7630(12) 0.085(3) Uani 0.276(8) 1 d D . P B 2 H17D H 0.990039 0.059202 0.739306 0.128 Uiso 0.276(8) 1 calc R U P B 2 H17E H 1.075995 0.112769 0.810826 0.128 Uiso 0.276(8) 1 calc R U P B 2 H17F H 1.083782 0.135196 0.734292 0.128 Uiso 0.276(8) 1 calc R U P B 2 C18B C 0.8634(12) 0.1356(13) 0.7016(8) 0.0650(19) Uani 0.276(8) 1 d D . P B 2 H18D H 0.879092 0.159245 0.660467 0.097 Uiso 0.276(8) 1 calc R U P B 2 H18E H 0.795793 0.146400 0.709646 0.097 Uiso 0.276(8) 1 calc R U P B 2 H18F H 0.856366 0.075318 0.691918 0.097 Uiso 0.276(8) 1 calc R U P B 2 C19 C 0.9648(3) 0.2077(2) 0.89967(18) 0.0436(8) Uani 1 1 d . . . . . H19 H 1.029022 0.245507 0.898063 0.052 Uiso 1 1 calc R U . . . C20 C 0.9345(2) 0.20986(19) 0.96563(16) 0.0332(7) Uani 1 1 d . . . . . C21 C 1.0115(3) 0.2681(2) 1.03436(18) 0.0445(8) Uani 1 1 d . . . . . H21 H 0.966760 0.277768 1.068856 0.053 Uiso 1 1 calc R U . . . C22 C 1.0679(3) 0.3554(2) 1.0229(2) 0.0656(11) Uani 1 1 d . . . . . H22A H 1.118995 0.348986 0.993727 0.098 Uiso 1 1 calc R U . . . H22B H 1.106687 0.390845 1.069627 0.098 Uiso 1 1 calc R U . . . H22C H 1.013481 0.381201 0.998253 0.098 Uiso 1 1 calc R U . . . C23 C 1.0974(3) 0.2244(3) 1.0708(2) 0.0738(13) Uani 1 1 d . . . . . H23A H 1.060889 0.171742 1.081344 0.111 Uiso 1 1 calc R U . . . H23B H 1.142657 0.260899 1.115549 0.111 Uiso 1 1 calc R U . . . H23C H 1.142595 0.213280 1.038306 0.111 Uiso 1 1 calc R U . . . C24 C 0.5853(2) 0.29149(19) 1.00165(16) 0.0331(7) Uani 1 1 d . . . . . C25 C 0.5489(3) 0.2171(2) 0.93572(17) 0.0432(8) Uani 1 1 d . . . . . H25A H 0.552972 0.164438 0.953027 0.052 Uiso 1 1 calc R U . . . H25B H 0.598641 0.225947 0.904144 0.052 Uiso 1 1 calc R U . . . C26 C 0.4306(3) 0.2095(2) 0.89157(19) 0.0549(10) Uani 1 1 d . . . . . H26 H 0.409453 0.161524 0.850232 0.066 Uiso 1 1 calc R U . . . C27 C 0.3526(3) 0.1943(3) 0.9412(2) 0.0658(11) Uani 1 1 d . . . . . H27A H 0.277679 0.189408 0.913817 0.079 Uiso 1 1 calc R U . . . H27B H 0.355292 0.141549 0.958636 0.079 Uiso 1 1 calc R U . . . C28 C 0.3860(3) 0.2676(3) 1.0056(2) 0.0571(10) Uani 1 1 d . . . . . H28 H 0.335810 0.257417 1.037403 0.069 Uiso 1 1 calc R U . . . C29 C 0.5042(2) 0.2746(2) 1.04953(17) 0.0421(8) Uani 1 1 d . . . . . H29A H 0.524541 0.320584 1.091671 0.050 Uiso 1 1 calc R U . . . H29B H 0.507774 0.222116 1.067258 0.050 Uiso 1 1 calc R U . . . C30 C 0.5753(3) 0.3729(2) 0.97115(18) 0.0415(8) Uani 1 1 d . . . . . H30A H 0.597563 0.421281 1.011370 0.050 Uiso 1 1 calc R U . . . H30B H 0.624278 0.382621 0.939219 0.050 Uiso 1 1 calc R U . . . C31 C 0.4563(3) 0.3654(2) 0.92802(19) 0.0511(9) Uani 1 1 d . . . . . H31 H 0.451976 0.418268 0.910080 0.061 Uiso 1 1 calc R U . . . C32 C 0.4240(3) 0.2911(2) 0.86276(19) 0.0580(10) Uani 1 1 d . . . . . H32A H 0.349646 0.286234 0.834363 0.070 Uiso 1 1 calc R U . . . H32B H 0.473467 0.301085 0.831169 0.070 Uiso 1 1 calc R U . . . C33 C 0.3793(3) 0.3500(3) 0.9782(2) 0.0629(11) Uani 1 1 d . . . . . H33A H 0.400310 0.397097 1.019447 0.076 Uiso 1 1 calc R U . . . H33B H 0.304282 0.346024 0.951544 0.076 Uiso 1 1 calc R U . . . C34 C 0.7965(2) 0.39278(18) 1.12243(15) 0.0311(7) Uani 1 1 d . . . . . C35 C 0.8526(3) 0.46680(19) 1.09001(17) 0.0406(8) Uani 1 1 d . . . . . H35A H 0.904169 0.448230 1.064905 0.049 Uiso 1 1 calc R U . . . H35B H 0.797327 0.482316 1.054377 0.049 Uiso 1 1 calc R U . . . C36 C 0.9139(3) 0.5447(2) 1.15010(18) 0.0481(9) Uani 1 1 d . . . . . H36 H 0.948513 0.590520 1.128100 0.058 Uiso 1 1 calc R U . . . C37 C 1.0025(3) 0.5208(2) 1.20564(19) 0.0512(9) Uani 1 1 d . . . . . H37A H 1.054877 0.502101 1.181399 0.061 Uiso 1 1 calc R U . . . H37B H 1.041988 0.570011 1.243644 0.061 Uiso 1 1 calc R U . . . C38 C 0.9483(3) 0.4496(2) 1.23955(17) 0.0428(8) Uani 1 1 d . . . . . H38 H 1.004964 0.434186 1.275135 0.051 Uiso 1 1 calc R U . . . C39 C 0.8868(2) 0.37169(19) 1.17986(17) 0.0381(8) Uani 1 1 d . . . . . H39A H 0.853559 0.326351 1.202062 0.046 Uiso 1 1 calc R U . . . H39B H 0.938589 0.351702 1.155843 0.046 Uiso 1 1 calc R U . . . C40 C 0.7175(2) 0.4257(2) 1.16322(16) 0.0379(8) Uani 1 1 d . . . . . H40A H 0.660575 0.440837 1.128547 0.045 Uiso 1 1 calc R U . . . H40B H 0.682254 0.380934 1.185097 0.045 Uiso 1 1 calc R U . . . C41 C 0.7794(3) 0.5036(2) 1.22319(18) 0.0447(8) Uani 1 1 d . . . . . H41 H 0.727192 0.522929 1.248168 0.054 Uiso 1 1 calc R U . . . C42 C 0.8330(3) 0.5751(2) 1.1896(2) 0.0538(10) Uani 1 1 d . . . . . H42A H 0.871798 0.624403 1.227765 0.065 Uiso 1 1 calc R U . . . H42B H 0.777060 0.591490 1.155162 0.065 Uiso 1 1 calc R U . . . C43 C 0.8672(3) 0.4799(2) 1.27851(17) 0.0489(9) Uani 1 1 d . . . . . H43A H 0.833144 0.434978 1.300825 0.059 Uiso 1 1 calc R U . . . H43B H 0.905811 0.528886 1.316945 0.059 Uiso 1 1 calc R U . . . P2 P 0.55968(6) 0.35733(5) 0.57936(4) 0.0332(2) Uani 1 1 d . . . . . O3 O 0.68167(17) 0.31250(13) 0.72295(11) 0.0410(5) Uani 1 1 d . . . . . O4 O 0.2944(2) 0.07449(16) 0.58443(15) 0.0694(8) Uani 1 1 d . . . . . C44 C 0.4265(2) 0.19860(19) 0.58586(17) 0.0351(7) Uani 1 1 d . . . . . C45 C 0.3942(3) 0.1300(2) 0.61966(19) 0.0449(8) Uani 1 1 d . . . . . C46 C 0.2518(4) 0.0094(3) 0.6202(3) 0.1078(19) Uani 1 1 d . . . . . H46A H 0.302391 -0.025992 0.628969 0.162 Uiso 1 1 calc R U . . . H46B H 0.182183 -0.024528 0.589805 0.162 Uiso 1 1 calc R U . . . H46C H 0.241893 0.034614 0.666099 0.162 Uiso 1 1 calc R U . . . C47 C 0.4589(3) 0.1206(2) 0.6847(2) 0.0509(9) Uani 1 1 d . . . . . H47 H 0.437178 0.073577 0.705433 0.061 Uiso 1 1 calc R U . . . C48 C 0.5554(3) 0.1806(2) 0.71874(19) 0.0455(8) Uani 1 1 d . . . . . H48 H 0.599238 0.173878 0.762372 0.055 Uiso 1 1 calc R U . . . C49 C 0.5874(2) 0.25036(19) 0.68861(17) 0.0360(7) Uani 1 1 d . . . . . C50 C 0.7310(3) 0.3154(2) 0.79782(17) 0.0536(10) Uani 1 1 d . . . . . H50A H 0.677028 0.316597 0.825583 0.080 Uiso 1 1 calc R U . . . H50B H 0.790315 0.365642 0.816009 0.080 Uiso 1 1 calc R U . . . H50C H 0.759065 0.265883 0.802580 0.080 Uiso 1 1 calc R U . . . C51 C 0.5248(2) 0.26170(18) 0.62112(16) 0.0321(7) Uani 1 1 d . . . . . C52 C 0.3452(2) 0.20022(19) 0.51507(18) 0.0379(7) Uani 1 1 d . . . . . C53 C 0.3387(3) 0.1481(2) 0.44890(19) 0.0452(8) Uani 1 1 d . . . . . C54 C 0.4163(3) 0.0901(2) 0.4401(2) 0.0646(11) Uani 1 1 d . . . . . H54 H 0.479731 0.107999 0.482971 0.077 Uiso 1 1 calc R U . . . C55 C 0.4592(4) 0.0963(3) 0.3718(3) 0.0982(18) Uani 1 1 d . . . . . H55A H 0.401922 0.066325 0.329125 0.147 Uiso 1 1 calc R U . . . H55B H 0.521028 0.071301 0.375135 0.147 Uiso 1 1 calc R U . . . H55C H 0.481614 0.154977 0.368092 0.147 Uiso 1 1 calc R U . . . C56 C 0.3594(4) -0.0027(3) 0.4379(3) 0.0974(17) Uani 1 1 d . . . . . H56A H 0.338440 -0.007460 0.482940 0.146 Uiso 1 1 calc R U . . . H56B H 0.409177 -0.037952 0.431944 0.146 Uiso 1 1 calc R U . . . H56C H 0.295023 -0.020883 0.397552 0.146 Uiso 1 1 calc R U . . . C57 C 0.2543(3) 0.1445(2) 0.38774(19) 0.0536(10) Uani 1 1 d . . . . . H57 H 0.251972 0.111090 0.343525 0.064 Uiso 1 1 calc R U . . . C58 C 0.1733(3) 0.1887(2) 0.39010(19) 0.0499(9) Uani 1 1 d . . . . . C59A C 0.0722(9) 0.1720(9) 0.3206(6) 0.0726(19) Uani 0.698(8) 1 d D . P C 1 H59A H 0.096280 0.154259 0.276728 0.087 Uiso 0.698(8) 1 calc R U P C 1 C60A C 0.0306(6) 0.2502(5) 0.3120(4) 0.112(3) Uani 0.698(8) 1 d D . P C 1 H60A H -0.018858 0.241275 0.264391 0.168 Uiso 0.698(8) 1 calc R U P C 1 H60B H 0.091625 0.297862 0.317211 0.168 Uiso 0.698(8) 1 calc R U P C 1 H60C H -0.007546 0.261355 0.349014 0.168 Uiso 0.698(8) 1 calc R U P C 1 C61A C -0.0167(9) 0.0990(6) 0.3285(7) 0.132(4) Uani 0.698(8) 1 d D . P C 1 H61A H -0.031491 0.111015 0.375662 0.198 Uiso 0.698(8) 1 calc R U P C 1 H61B H 0.007764 0.047398 0.324137 0.198 Uiso 0.698(8) 1 calc R U P C 1 H61C H -0.082724 0.092369 0.290742 0.198 Uiso 0.698(8) 1 calc R U P C 1 C59B C 0.086(2) 0.183(2) 0.3285(14) 0.0726(19) Uani 0.302(8) 1 d D . P C 2 H59B H 0.087135 0.243432 0.329078 0.087 Uiso 0.302(8) 1 calc R U P C 2 C60B C -0.026(2) 0.1484(15) 0.3394(14) 0.132(4) Uani 0.302(8) 1 d D . P C 2 H60D H -0.035718 0.089099 0.341612 0.198 Uiso 0.302(8) 1 calc R U P C 2 H60E H -0.081409 0.155074 0.299098 0.198 Uiso 0.302(8) 1 calc R U P C 2 H60F H -0.032849 0.178812 0.384307 0.198 Uiso 0.302(8) 1 calc R U P C 2 C61B C 0.0950(13) 0.1548(13) 0.2521(7) 0.111(8) Uani 0.302(8) 1 d D . P C 2 H61D H 0.167794 0.179240 0.248171 0.167 Uiso 0.302(8) 1 calc R U P C 2 H61E H 0.042099 0.172982 0.217797 0.167 Uiso 0.302(8) 1 calc R U P C 2 H61F H 0.080648 0.093794 0.241614 0.167 Uiso 0.302(8) 1 calc R U P C 2 C62 C 0.1810(3) 0.2380(2) 0.45605(19) 0.0466(9) Uani 1 1 d . . . . . H62 H 0.127921 0.268306 0.458942 0.056 Uiso 1 1 calc R U . . . C63 C 0.2631(2) 0.24503(19) 0.51837(17) 0.0376(7) Uani 1 1 d . . . . . C64 C 0.2589(3) 0.2969(2) 0.58902(19) 0.0481(9) Uani 1 1 d . . . . . H64 H 0.331521 0.307985 0.623356 0.058 Uiso 1 1 calc R U . . . C65 C 0.2349(3) 0.3826(2) 0.5797(2) 0.0670(12) Uani 1 1 d . . . . . H65A H 0.285639 0.411987 0.555673 0.101 Uiso 1 1 calc R U . . . H65B H 0.242960 0.415993 0.626936 0.101 Uiso 1 1 calc R U . . . H65C H 0.160977 0.373781 0.550529 0.101 Uiso 1 1 calc R U . . . C66 C 0.1747(4) 0.2471(3) 0.6232(3) 0.0882(15) Uani 1 1 d . . . . . H66A H 0.103256 0.232332 0.589416 0.132 Uiso 1 1 calc R U . . . H66B H 0.172675 0.281531 0.667654 0.132 Uiso 1 1 calc R U . . . H66C H 0.195292 0.196117 0.633918 0.132 Uiso 1 1 calc R U . . . C67 C 0.6876(2) 0.34762(19) 0.54817(16) 0.0340(7) Uani 1 1 d . . . . . C68 C 0.7910(3) 0.3400(2) 0.60300(17) 0.0423(8) Uani 1 1 d . . . . . H68A H 0.772340 0.291206 0.625739 0.051 Uiso 1 1 calc R U . . . H68B H 0.817527 0.390542 0.641292 0.051 Uiso 1 1 calc R U . . . C69 C 0.8824(3) 0.3299(2) 0.56434(19) 0.0497(9) Uani 1 1 d . . . . . H69 H 0.947503 0.325965 0.600443 0.060 Uiso 1 1 calc R U . . . C70 C 0.8423(3) 0.2492(2) 0.5057(2) 0.0575(10) Uani 1 1 d . . . . . H70A H 0.824056 0.200009 0.528081 0.069 Uiso 1 1 calc R U . . . H70B H 0.900053 0.242368 0.481589 0.069 Uiso 1 1 calc R U . . . C71 C 0.7408(3) 0.2556(2) 0.44967(19) 0.0514(9) Uani 1 1 d . . . . . H71 H 0.714249 0.203638 0.412020 0.062 Uiso 1 1 calc R U . . . C72 C 0.6501(3) 0.2667(2) 0.48833(18) 0.0464(8) Uani 1 1 d . . . . . H72A H 0.629967 0.217477 0.510271 0.056 Uiso 1 1 calc R U . . . H72B H 0.585348 0.269925 0.452443 0.056 Uiso 1 1 calc R U . . . C73 C 0.7200(3) 0.4237(2) 0.51030(17) 0.0393(8) Uani 1 1 d . . . . . H73A H 0.656021 0.427731 0.474183 0.047 Uiso 1 1 calc R U . . . H73B H 0.744793 0.476058 0.546496 0.047 Uiso 1 1 calc R U . . . C74 C 0.8117(3) 0.4131(2) 0.47269(19) 0.0475(9) Uani 1 1 d . . . . . H74 H 0.831104 0.462281 0.449592 0.057 Uiso 1 1 calc R U . . . C75 C 0.9126(3) 0.4072(2) 0.5289(2) 0.0523(9) Uani 1 1 d . . . . . H75A H 0.938701 0.458652 0.566159 0.063 Uiso 1 1 calc R U . . . H75B H 0.971072 0.401521 0.505205 0.063 Uiso 1 1 calc R U . . . C76 C 0.7710(3) 0.3320(2) 0.41412(19) 0.0537(10) Uani 1 1 d . . . . . H76A H 0.707096 0.335947 0.377869 0.064 Uiso 1 1 calc R U . . . H76B H 0.828208 0.325355 0.389474 0.064 Uiso 1 1 calc R U . . . C77 C 0.5931(2) 0.45720(18) 0.65444(16) 0.0348(7) Uani 1 1 d . . . . . C78 C 0.7140(2) 0.4981(2) 0.69705(17) 0.0401(8) Uani 1 1 d . . . . . H78A H 0.742416 0.458469 0.724772 0.048 Uiso 1 1 calc R U . . . H78B H 0.758288 0.510596 0.662726 0.048 Uiso 1 1 calc R U . . . C79 C 0.7225(3) 0.5804(2) 0.74941(19) 0.0497(9) Uani 1 1 d . . . . . H79 H 0.799728 0.605071 0.775887 0.060 Uiso 1 1 calc R U . . . C80 C 0.6545(3) 0.5612(2) 0.8046(2) 0.0551(10) Uani 1 1 d . . . . . H80A H 0.661096 0.613056 0.838427 0.066 Uiso 1 1 calc R U . . . H80B H 0.681364 0.521102 0.832585 0.066 Uiso 1 1 calc R U . . . C81 C 0.5341(3) 0.5233(2) 0.7628(2) 0.0521(9) Uani 1 1 d . . . . . H81 H 0.489884 0.510794 0.797773 0.063 Uiso 1 1 calc R U . . . C82 C 0.5241(3) 0.4407(2) 0.71014(18) 0.0433(8) Uani 1 1 d . . . . . H82A H 0.447447 0.416530 0.684190 0.052 Uiso 1 1 calc R U . . . H82B H 0.548930 0.399857 0.737996 0.052 Uiso 1 1 calc R U . . . C83 C 0.5508(3) 0.5232(2) 0.61230(19) 0.0464(9) Uani 1 1 d . . . . . H83A H 0.593343 0.535908 0.577046 0.056 Uiso 1 1 calc R U . . . H83B H 0.474398 0.499546 0.585585 0.056 Uiso 1 1 calc R U . . . C84 C 0.5605(3) 0.6058(2) 0.6654(2) 0.0575(10) Uani 1 1 d . . . . . H84 H 0.533334 0.646457 0.637428 0.069 Uiso 1 1 calc R U . . . C85 C 0.6805(3) 0.6440(2) 0.7061(2) 0.0604(10) Uani 1 1 d . . . . . H85A H 0.687306 0.696587 0.739110 0.072 Uiso 1 1 calc R U . . . H85B H 0.724072 0.656906 0.671374 0.072 Uiso 1 1 calc R U . . . C86 C 0.4920(3) 0.5867(2) 0.7198(2) 0.0628(11) Uani 1 1 d . . . . . H86A H 0.497457 0.638758 0.753037 0.075 Uiso 1 1 calc R U . . . H86B H 0.415219 0.563148 0.693852 0.075 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0293(4) 0.0317(4) 0.0309(4) 0.0073(3) 0.0094(3) 0.0109(3) O1 0.0507(14) 0.0489(14) 0.0366(13) 0.0127(10) 0.0243(11) 0.0212(11) O2 0.0588(15) 0.0509(14) 0.0467(14) 0.0210(11) 0.0242(12) 0.0356(12) C1 0.0269(15) 0.0291(16) 0.0307(16) 0.0071(13) 0.0059(13) 0.0063(13) C2 0.0307(16) 0.0357(17) 0.0269(16) 0.0033(13) 0.0078(13) 0.0080(13) C3 0.089(3) 0.057(2) 0.052(2) 0.0098(19) 0.042(2) 0.026(2) C4 0.0388(18) 0.0447(19) 0.0306(17) 0.0127(15) 0.0138(14) 0.0124(15) C5 0.050(2) 0.0387(19) 0.0386(19) 0.0165(15) 0.0145(16) 0.0180(16) C6 0.0374(17) 0.0376(18) 0.0315(17) 0.0080(14) 0.0103(14) 0.0155(14) C7 0.074(3) 0.060(2) 0.065(3) 0.031(2) 0.030(2) 0.045(2) C8 0.0264(15) 0.0313(16) 0.0280(16) 0.0074(13) 0.0044(12) 0.0099(13) C9 0.0330(16) 0.0326(17) 0.0342(17) 0.0126(14) 0.0150(14) 0.0163(13) C10 0.0399(18) 0.0378(18) 0.0350(18) 0.0125(14) 0.0095(15) 0.0164(15) C11 0.052(2) 0.044(2) 0.0355(19) 0.0060(15) 0.0075(16) 0.0056(17) C12 0.050(2) 0.054(2) 0.050(2) -0.0027(18) 0.0012(18) 0.0049(18) C13 0.086(3) 0.051(3) 0.082(3) 0.018(2) 0.002(3) 0.007(2) C14 0.051(2) 0.057(2) 0.0277(18) 0.0079(16) 0.0081(16) 0.0210(18) C15 0.051(2) 0.072(3) 0.0315(19) 0.0221(18) 0.0171(17) 0.030(2) C16A 0.054(4) 0.074(6) 0.043(3) 0.023(4) 0.022(3) 0.010(4) C17A 0.121(6) 0.110(7) 0.072(5) 0.057(5) 0.055(4) 0.075(5) C18A 0.069(4) 0.088(5) 0.054(4) 0.027(4) 0.036(3) 0.027(4) C16B 0.054(4) 0.074(6) 0.043(3) 0.023(4) 0.022(3) 0.010(4) C17B 0.121(6) 0.110(7) 0.072(5) 0.057(5) 0.055(4) 0.075(5) C18B 0.069(4) 0.088(5) 0.054(4) 0.027(4) 0.036(3) 0.027(4) C19 0.0374(18) 0.054(2) 0.048(2) 0.0203(18) 0.0189(17) 0.0138(16) C20 0.0320(16) 0.0368(17) 0.0371(18) 0.0113(14) 0.0143(14) 0.0138(14) C21 0.0337(18) 0.052(2) 0.048(2) 0.0042(17) 0.0169(16) 0.0065(16) C22 0.062(3) 0.052(2) 0.081(3) 0.007(2) 0.029(2) 0.003(2) C23 0.057(3) 0.071(3) 0.074(3) 0.007(2) -0.013(2) 0.008(2) C24 0.0304(16) 0.0404(18) 0.0302(17) 0.0092(14) 0.0079(13) 0.0109(14) C25 0.0393(19) 0.044(2) 0.0411(19) 0.0016(16) 0.0028(15) 0.0098(15) C26 0.043(2) 0.064(3) 0.044(2) 0.0018(18) -0.0052(17) 0.0078(18) C27 0.038(2) 0.085(3) 0.061(3) 0.015(2) -0.0029(19) 0.002(2) C28 0.035(2) 0.085(3) 0.052(2) 0.018(2) 0.0141(17) 0.0130(19) C29 0.0326(18) 0.054(2) 0.0387(19) 0.0096(16) 0.0091(15) 0.0081(15) C30 0.0377(18) 0.046(2) 0.045(2) 0.0138(16) 0.0099(15) 0.0168(15) C31 0.045(2) 0.062(2) 0.052(2) 0.0196(19) 0.0063(18) 0.0260(18) C32 0.043(2) 0.082(3) 0.046(2) 0.017(2) 0.0001(17) 0.018(2) C33 0.040(2) 0.090(3) 0.064(3) 0.015(2) 0.0103(19) 0.032(2) C34 0.0312(16) 0.0310(16) 0.0316(17) 0.0064(13) 0.0081(13) 0.0082(13) C35 0.0442(19) 0.0363(18) 0.0404(19) 0.0090(15) 0.0108(15) 0.0069(15) C36 0.056(2) 0.0338(19) 0.047(2) 0.0064(16) 0.0106(18) -0.0008(16) C37 0.0378(19) 0.051(2) 0.055(2) -0.0038(18) 0.0091(17) 0.0020(17) C38 0.0405(19) 0.047(2) 0.0346(18) 0.0015(15) -0.0008(15) 0.0113(16) C39 0.0349(17) 0.0389(18) 0.0395(18) 0.0060(15) 0.0052(14) 0.0122(15) C40 0.0351(17) 0.0437(19) 0.0348(18) 0.0019(15) 0.0093(14) 0.0126(15) C41 0.043(2) 0.044(2) 0.044(2) -0.0040(16) 0.0086(16) 0.0146(16) C42 0.060(2) 0.039(2) 0.053(2) -0.0032(17) -0.0016(19) 0.0149(18) C43 0.054(2) 0.048(2) 0.0350(19) -0.0023(16) 0.0055(17) 0.0058(17) P2 0.0292(4) 0.0349(5) 0.0353(5) 0.0093(4) 0.0041(3) 0.0102(3) O3 0.0374(12) 0.0498(14) 0.0340(12) 0.0141(10) 0.0044(10) 0.0078(11) O4 0.0546(16) 0.0488(16) 0.090(2) 0.0190(15) 0.0054(15) -0.0087(13) C44 0.0335(17) 0.0332(17) 0.0408(18) 0.0050(14) 0.0101(14) 0.0137(14) C45 0.0379(19) 0.0331(18) 0.060(2) 0.0066(17) 0.0095(17) 0.0040(15) C46 0.075(3) 0.075(3) 0.159(5) 0.052(3) 0.017(3) -0.019(3) C47 0.060(2) 0.0344(19) 0.061(2) 0.0194(17) 0.017(2) 0.0090(17) C48 0.053(2) 0.043(2) 0.044(2) 0.0143(16) 0.0138(17) 0.0143(17) C49 0.0325(17) 0.0359(18) 0.0415(19) 0.0066(15) 0.0123(15) 0.0100(14) C50 0.048(2) 0.070(3) 0.038(2) 0.0139(18) 0.0031(17) 0.0102(19) C51 0.0290(16) 0.0330(17) 0.0365(17) 0.0074(14) 0.0091(14) 0.0113(13) C52 0.0309(17) 0.0324(17) 0.047(2) 0.0032(15) 0.0067(15) 0.0055(14) C53 0.0354(18) 0.044(2) 0.049(2) -0.0030(17) 0.0045(16) 0.0095(15) C54 0.048(2) 0.064(3) 0.069(3) -0.019(2) 0.000(2) 0.022(2) C55 0.062(3) 0.121(4) 0.091(4) -0.047(3) 0.016(3) 0.025(3) C56 0.094(4) 0.060(3) 0.129(4) -0.012(3) 0.010(3) 0.037(3) C57 0.049(2) 0.058(2) 0.043(2) -0.0099(17) 0.0040(18) 0.0111(18) C58 0.040(2) 0.062(2) 0.045(2) 0.0131(18) 0.0050(17) 0.0117(18) C59A 0.051(4) 0.108(5) 0.046(4) 0.009(3) -0.011(3) 0.019(4) C60A 0.064(5) 0.119(7) 0.137(7) 0.059(5) -0.032(4) 0.024(4) C61A 0.093(5) 0.108(9) 0.133(7) 0.039(8) -0.055(5) -0.033(7) C59B 0.051(4) 0.108(5) 0.046(4) 0.009(3) -0.011(3) 0.019(4) C60B 0.093(5) 0.108(9) 0.133(7) 0.039(8) -0.055(5) -0.033(7) C61B 0.078(11) 0.20(2) 0.026(8) 0.011(10) -0.012(7) 0.000(12) C62 0.041(2) 0.049(2) 0.053(2) 0.0100(18) 0.0104(17) 0.0201(17) C63 0.0311(17) 0.0378(18) 0.0436(19) 0.0066(15) 0.0082(15) 0.0097(14) C64 0.0371(19) 0.054(2) 0.052(2) -0.0007(18) 0.0067(17) 0.0207(17) C65 0.059(3) 0.058(3) 0.082(3) -0.005(2) 0.010(2) 0.031(2) C66 0.106(4) 0.094(4) 0.088(3) 0.018(3) 0.061(3) 0.037(3) C67 0.0361(17) 0.0360(17) 0.0337(17) 0.0117(14) 0.0107(14) 0.0120(14) C68 0.0408(19) 0.058(2) 0.0375(19) 0.0162(16) 0.0110(15) 0.0272(17) C69 0.043(2) 0.073(3) 0.046(2) 0.0198(19) 0.0143(17) 0.0315(19) C70 0.070(3) 0.063(3) 0.059(2) 0.020(2) 0.032(2) 0.037(2) C71 0.063(2) 0.052(2) 0.042(2) 0.0018(17) 0.0199(19) 0.0164(19) C72 0.050(2) 0.042(2) 0.047(2) 0.0067(16) 0.0145(17) 0.0117(17) C73 0.0370(18) 0.0433(19) 0.0403(19) 0.0127(15) 0.0079(15) 0.0146(15) C74 0.049(2) 0.053(2) 0.051(2) 0.0224(18) 0.0225(18) 0.0176(17) C75 0.041(2) 0.065(2) 0.057(2) 0.0122(19) 0.0187(18) 0.0174(18) C76 0.058(2) 0.071(3) 0.041(2) 0.0139(19) 0.0199(18) 0.023(2) C77 0.0298(16) 0.0325(17) 0.0395(18) 0.0063(14) 0.0031(14) 0.0080(13) C78 0.0305(17) 0.045(2) 0.0422(19) 0.0035(15) 0.0081(15) 0.0082(15) C79 0.041(2) 0.043(2) 0.056(2) -0.0045(17) 0.0077(17) 0.0044(16) C80 0.053(2) 0.052(2) 0.055(2) -0.0061(18) 0.0126(19) 0.0149(18) C81 0.048(2) 0.051(2) 0.061(2) 0.0016(19) 0.0250(19) 0.0160(18) C82 0.0373(18) 0.043(2) 0.051(2) 0.0066(16) 0.0140(16) 0.0107(15) C83 0.0397(19) 0.041(2) 0.059(2) 0.0144(17) 0.0066(17) 0.0138(16) C84 0.058(2) 0.038(2) 0.076(3) 0.0088(19) 0.009(2) 0.0221(18) C85 0.060(2) 0.037(2) 0.076(3) -0.0025(19) 0.015(2) 0.0048(18) C86 0.053(2) 0.051(2) 0.088(3) 0.000(2) 0.023(2) 0.0252(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.868(3) . ? P1 C24 1.894(3) . ? P1 C34 1.924(3) . ? O1 C2 1.373(3) . ? O1 C3 1.405(4) . ? O2 C6 1.375(3) . ? O2 C7 1.430(4) . ? C1 C2 1.414(4) . ? C1 C8 1.416(4) . ? C2 C4 1.372(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 C6 1.380(4) . ? C5 H5 0.9300 . ? C6 C8 1.405(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.511(4) . ? C9 C20 1.401(4) . ? C9 C10 1.407(4) . ? C10 C14 1.396(4) . ? C10 C11 1.523(4) . ? C11 C12 1.526(4) . ? C11 C13 1.532(5) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.372(5) . ? C14 H14 0.9300 . ? C15 C19 1.385(5) . ? C15 C16A 1.531(8) . ? C15 C16B 1.63(2) . ? C16A C17A 1.495(8) . ? C16A C18A 1.544(7) . ? C16A H16A 0.9800 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C16B C18B 1.541(14) . ? C16B C17B 1.567(15) . ? C16B H16B 0.9800 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19 C20 1.391(4) . ? C19 H19 0.9300 . ? C20 C21 1.517(4) . ? C21 C22 1.526(5) . ? C21 C23 1.528(5) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C29 1.533(4) . ? C24 C25 1.539(4) . ? C24 C30 1.541(4) . ? C25 C26 1.539(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C32 1.521(5) . ? C26 C27 1.525(5) . ? C26 H26 0.9800 . ? C27 C28 1.511(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C33 1.520(5) . ? C28 C29 1.537(4) . ? C28 H28 0.9800 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.539(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C33 1.525(5) . ? C31 C32 1.532(5) . ? C31 H31 0.9800 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C39 1.542(4) . ? C34 C40 1.542(4) . ? C34 C35 1.548(4) . ? C35 C36 1.531(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.529(5) . ? C36 C42 1.533(5) . ? C36 H36 0.9800 . ? C37 C38 1.521(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C43 1.527(4) . ? C38 C39 1.528(4) . ? C38 H38 0.9800 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.532(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.518(5) . ? C41 C43 1.519(4) . ? C41 H41 0.9800 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? P2 C51 1.864(3) . ? P2 C67 1.893(3) . ? P2 C77 1.925(3) . ? O3 C49 1.373(3) . ? O3 C50 1.418(4) . ? O4 C45 1.375(4) . ? O4 C46 1.418(5) . ? C44 C45 1.400(4) . ? C44 C51 1.417(4) . ? C44 C52 1.521(4) . ? C45 C47 1.379(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.375(5) . ? C47 H47 0.9300 . ? C48 C49 1.372(4) . ? C48 H48 0.9300 . ? C49 C51 1.417(4) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C52 C53 1.398(4) . ? C52 C63 1.411(4) . ? C53 C57 1.392(5) . ? C53 C54 1.531(5) . ? C54 C55 1.526(6) . ? C54 C56 1.532(6) . ? C54 H54 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.390(5) . ? C57 H57 0.9300 . ? C58 C62 1.369(5) . ? C58 C59B 1.41(3) . ? C58 C59A 1.587(13) . ? C59A C60A 1.500(14) . ? C59A C61A 1.518(10) . ? C59A H59A 0.9800 . ? C60A H60A 0.9600 . ? C60A H60B 0.9600 . ? C60A H60C 0.9600 . ? C61A H61A 0.9600 . ? C61A H61B 0.9600 . ? C61A H61C 0.9600 . ? C59B C61B 1.501(17) . ? C59B C60B 1.506(15) . ? C59B H59B 0.9800 . ? C60B H60D 0.9600 . ? C60B H60E 0.9600 . ? C60B H60F 0.9600 . ? C61B H61D 0.9600 . ? C61B H61E 0.9600 . ? C61B H61F 0.9600 . ? C62 C63 1.378(4) . ? C62 H62 0.9300 . ? C63 C64 1.508(4) . ? C64 C65 1.522(5) . ? C64 C66 1.528(5) . ? C64 H64 0.9800 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C72 1.538(4) . ? C67 C68 1.539(4) . ? C67 C73 1.548(4) . ? C68 C69 1.539(4) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.524(5) . ? C69 C75 1.530(5) . ? C69 H69 0.9800 . ? C70 C71 1.526(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C76 1.520(5) . ? C71 C72 1.535(5) . ? C71 H71 0.9800 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.532(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.519(5) . ? C74 C76 1.527(5) . ? C74 H74 0.9800 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C82 1.539(4) . ? C77 C78 1.544(4) . ? C77 C83 1.548(4) . ? C78 C79 1.531(4) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C85 1.525(5) . ? C79 C80 1.528(5) . ? C79 H79 0.9800 . ? C80 C81 1.529(5) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C86 1.518(5) . ? C81 C82 1.534(4) . ? C81 H81 0.9800 . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.538(5) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C85 1.520(5) . ? C84 C86 1.520(5) . ? C84 H84 0.9800 . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C24 106.91(13) . . ? C1 P1 C34 107.07(13) . . ? C24 P1 C34 109.79(13) . . ? C2 O1 C3 118.2(2) . . ? C6 O2 C7 117.8(2) . . ? C2 C1 C8 117.2(3) . . ? C2 C1 P1 124.8(2) . . ? C8 C1 P1 117.6(2) . . ? C4 C2 O1 122.0(3) . . ? C4 C2 C1 122.1(3) . . ? O1 C2 C1 116.0(3) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 120.2(3) . . ? C2 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? O2 C6 C5 122.8(3) . . ? O2 C6 C8 116.0(3) . . ? C5 C6 C8 121.2(3) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C1 119.5(3) . . ? C6 C8 C9 114.4(2) . . ? C1 C8 C9 126.0(2) . . ? C20 C9 C10 118.9(3) . . ? C20 C9 C8 121.6(3) . . ? C10 C9 C8 119.0(3) . . ? C14 C10 C9 119.2(3) . . ? C14 C10 C11 117.4(3) . . ? C9 C10 C11 123.2(3) . . ? C10 C11 C12 113.6(3) . . ? C10 C11 C13 111.6(3) . . ? C12 C11 C13 108.6(3) . . ? C10 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C13 C11 H11 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 122.5(3) . . ? C15 C14 H14 118.8 . . ? C10 C14 H14 118.8 . . ? C14 C15 C19 117.7(3) . . ? C14 C15 C16A 115.7(4) . . ? C19 C15 C16A 126.4(4) . . ? C14 C15 C16B 135.3(6) . . ? C19 C15 C16B 106.5(6) . . ? C17A C16A C15 111.1(6) . . ? C17A C16A C18A 106.4(6) . . ? C15 C16A C18A 112.1(5) . . ? C17A C16A H16A 109.1 . . ? C15 C16A H16A 109.1 . . ? C18A C16A H16A 109.1 . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C16A C18A H18A 109.5 . . ? C16A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C16A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C18B C16B C17B 99.1(12) . . ? C18B C16B C15 102.2(13) . . ? C17B C16B C15 104.3(15) . . ? C18B C16B H16B 116.3 . . ? C17B C16B H16B 116.3 . . ? C15 C16B H16B 116.3 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C16B C18B H18D 109.5 . . ? C16B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C16B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C15 C19 C20 122.2(3) . . ? C15 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C9 119.5(3) . . ? C19 C20 C21 119.4(3) . . ? C9 C20 C21 121.0(3) . . ? C20 C21 C22 114.7(3) . . ? C20 C21 C23 110.7(3) . . ? C22 C21 C23 110.2(3) . . ? C20 C21 H21 107.0 . . ? C22 C21 H21 107.0 . . ? C23 C21 H21 107.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 107.3(3) . . ? C29 C24 C30 109.0(2) . . ? C25 C24 C30 107.1(2) . . ? C29 C24 P1 120.8(2) . . ? C25 C24 P1 104.6(2) . . ? C30 C24 P1 107.2(2) . . ? C24 C25 C26 111.2(3) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C32 C26 C27 109.7(3) . . ? C32 C26 C25 109.8(3) . . ? C27 C26 C25 109.2(3) . . ? C32 C26 H26 109.4 . . ? C27 C26 H26 109.4 . . ? C25 C26 H26 109.4 . . ? C28 C27 C26 109.5(3) . . ? C28 C27 H27A 109.8 . . ? C26 C27 H27A 109.8 . . ? C28 C27 H27B 109.8 . . ? C26 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? C27 C28 C33 109.7(3) . . ? C27 C28 C29 109.7(3) . . ? C33 C28 C29 109.9(3) . . ? C27 C28 H28 109.2 . . ? C33 C28 H28 109.2 . . ? C29 C28 H28 109.2 . . ? C24 C29 C28 110.7(3) . . ? C24 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C24 111.1(3) . . ? C31 C30 H30A 109.4 . . ? C24 C30 H30A 109.4 . . ? C31 C30 H30B 109.4 . . ? C24 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C33 C31 C32 110.3(3) . . ? C33 C31 C30 109.4(3) . . ? C32 C31 C30 108.9(3) . . ? C33 C31 H31 109.4 . . ? C32 C31 H31 109.4 . . ? C30 C31 H31 109.4 . . ? C26 C32 C31 108.7(3) . . ? C26 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? C26 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C28 C33 C31 109.2(3) . . ? C28 C33 H33A 109.8 . . ? C31 C33 H33A 109.8 . . ? C28 C33 H33B 109.8 . . ? C31 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? C39 C34 C40 107.5(2) . . ? C39 C34 C35 107.6(2) . . ? C40 C34 C35 107.6(2) . . ? C39 C34 P1 110.67(19) . . ? C40 C34 P1 119.3(2) . . ? C35 C34 P1 103.62(19) . . ? C36 C35 C34 111.2(3) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C37 C36 C35 109.5(3) . . ? C37 C36 C42 109.0(3) . . ? C35 C36 C42 109.8(3) . . ? C37 C36 H36 109.5 . . ? C35 C36 H36 109.5 . . ? C42 C36 H36 109.5 . . ? C38 C37 C36 109.2(3) . . ? C38 C37 H37A 109.8 . . ? C36 C37 H37A 109.8 . . ? C38 C37 H37B 109.8 . . ? C36 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? C37 C38 C43 109.5(3) . . ? C37 C38 C39 109.9(3) . . ? C43 C38 C39 109.4(3) . . ? C37 C38 H38 109.3 . . ? C43 C38 H38 109.3 . . ? C39 C38 H38 109.3 . . ? C38 C39 C34 111.3(2) . . ? C38 C39 H39A 109.4 . . ? C34 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? C34 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C34 111.1(3) . . ? C41 C40 H40A 109.4 . . ? C34 C40 H40A 109.4 . . ? C41 C40 H40B 109.4 . . ? C34 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C43 109.5(3) . . ? C42 C41 C40 110.1(3) . . ? C43 C41 C40 109.6(3) . . ? C42 C41 H41 109.2 . . ? C43 C41 H41 109.2 . . ? C40 C41 H41 109.2 . . ? C41 C42 C36 109.2(3) . . ? C41 C42 H42A 109.8 . . ? C36 C42 H42A 109.8 . . ? C41 C42 H42B 109.8 . . ? C36 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C41 C43 C38 109.2(3) . . ? C41 C43 H43A 109.8 . . ? C38 C43 H43A 109.8 . . ? C41 C43 H43B 109.8 . . ? C38 C43 H43B 109.8 . . ? H43A C43 H43B 108.3 . . ? C51 P2 C67 104.54(13) . . ? C51 P2 C77 108.30(14) . . ? C67 P2 C77 109.97(13) . . ? C49 O3 C50 118.7(2) . . ? C45 O4 C46 118.1(3) . . ? C45 C44 C51 119.2(3) . . ? C45 C44 C52 114.6(3) . . ? C51 C44 C52 126.0(3) . . ? O4 C45 C47 123.0(3) . . ? O4 C45 C44 115.7(3) . . ? C47 C45 C44 121.3(3) . . ? O4 C46 H46A 109.5 . . ? O4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C45 120.0(3) . . ? C48 C47 H47 120.0 . . ? C45 C47 H47 120.0 . . ? C49 C48 C47 120.2(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 O3 121.2(3) . . ? C48 C49 C51 121.7(3) . . ? O3 C49 C51 117.1(3) . . ? O3 C50 H50A 109.5 . . ? O3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C44 C51 C49 117.5(3) . . ? C44 C51 P2 118.4(2) . . ? C49 C51 P2 123.9(2) . . ? C53 C52 C63 118.7(3) . . ? C53 C52 C44 121.6(3) . . ? C63 C52 C44 119.0(3) . . ? C57 C53 C52 119.2(3) . . ? C57 C53 C54 117.0(3) . . ? C52 C53 C54 123.7(3) . . ? C55 C54 C53 112.6(4) . . ? C55 C54 C56 109.4(4) . . ? C53 C54 C56 110.8(3) . . ? C55 C54 H54 108.0 . . ? C53 C54 H54 108.0 . . ? C56 C54 H54 108.0 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C53 122.6(3) . . ? C58 C57 H57 118.7 . . ? C53 C57 H57 118.7 . . ? C62 C58 C57 116.6(3) . . ? C62 C58 C59B 120.8(13) . . ? C57 C58 C59B 122.6(13) . . ? C62 C58 C59A 123.9(6) . . ? C57 C58 C59A 119.2(6) . . ? C60A C59A C61A 111.8(8) . . ? C60A C59A C58 112.2(8) . . ? C61A C59A C58 107.5(9) . . ? C60A C59A H59A 108.4 . . ? C61A C59A H59A 108.4 . . ? C58 C59A H59A 108.4 . . ? C59A C60A H60A 109.5 . . ? C59A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? C59A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? C59A C61A H61A 109.5 . . ? C59A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C59A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C58 C59B C61B 121(2) . . ? C58 C59B C60B 114(2) . . ? C61B C59B C60B 113.0(18) . . ? C58 C59B H59B 101.7 . . ? C61B C59B H59B 101.7 . . ? C60B C59B H59B 101.7 . . ? C59B C60B H60D 109.5 . . ? C59B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? C59B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? C59B C61B H61D 109.5 . . ? C59B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C59B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? C58 C62 C63 123.6(3) . . ? C58 C62 H62 118.2 . . ? C63 C62 H62 118.2 . . ? C62 C63 C52 119.2(3) . . ? C62 C63 C64 118.8(3) . . ? C52 C63 C64 122.0(3) . . ? C63 C64 C65 112.9(3) . . ? C63 C64 C66 110.9(3) . . ? C65 C64 C66 110.1(3) . . ? C63 C64 H64 107.6 . . ? C65 C64 H64 107.6 . . ? C66 C64 H64 107.6 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C67 C68 107.3(3) . . ? C72 C67 C73 107.0(3) . . ? C68 C67 C73 108.7(2) . . ? C72 C67 P2 104.9(2) . . ? C68 C67 P2 120.5(2) . . ? C73 C67 P2 107.8(2) . . ? C67 C68 C69 110.9(3) . . ? C67 C68 H68A 109.5 . . ? C69 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? C70 C69 C75 109.6(3) . . ? C70 C69 C68 109.7(3) . . ? C75 C69 C68 109.6(3) . . ? C70 C69 H69 109.3 . . ? C75 C69 H69 109.3 . . ? C68 C69 H69 109.3 . . ? C69 C70 C71 109.1(3) . . ? C69 C70 H70A 109.9 . . ? C71 C70 H70A 109.9 . . ? C69 C70 H70B 109.9 . . ? C71 C70 H70B 109.9 . . ? H70A C70 H70B 108.3 . . ? C76 C71 C70 109.3(3) . . ? C76 C71 C72 109.3(3) . . ? C70 C71 C72 109.5(3) . . ? C76 C71 H71 109.6 . . ? C70 C71 H71 109.6 . . ? C72 C71 H71 109.6 . . ? C71 C72 C67 111.7(3) . . ? C71 C72 H72A 109.3 . . ? C67 C72 H72A 109.3 . . ? C71 C72 H72B 109.3 . . ? C67 C72 H72B 109.3 . . ? H72A C72 H72B 107.9 . . ? C74 C73 C67 111.0(3) . . ? C74 C73 H73A 109.4 . . ? C67 C73 H73A 109.4 . . ? C74 C73 H73B 109.4 . . ? C67 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? C75 C74 C76 109.6(3) . . ? C75 C74 C73 109.8(3) . . ? C76 C74 C73 109.2(3) . . ? C75 C74 H74 109.4 . . ? C76 C74 H74 109.4 . . ? C73 C74 H74 109.4 . . ? C74 C75 C69 109.3(3) . . ? C74 C75 H75A 109.8 . . ? C69 C75 H75A 109.8 . . ? C74 C75 H75B 109.8 . . ? C69 C75 H75B 109.8 . . ? H75A C75 H75B 108.3 . . ? C71 C76 C74 109.6(3) . . ? C71 C76 H76A 109.8 . . ? C74 C76 H76A 109.8 . . ? C71 C76 H76B 109.8 . . ? C74 C76 H76B 109.8 . . ? H76A C76 H76B 108.2 . . ? C82 C77 C78 108.5(2) . . ? C82 C77 C83 107.2(3) . . ? C78 C77 C83 107.6(2) . . ? C82 C77 P2 110.1(2) . . ? C78 C77 P2 119.5(2) . . ? C83 C77 P2 103.3(2) . . ? C79 C78 C77 110.6(3) . . ? C79 C78 H78A 109.5 . . ? C77 C78 H78A 109.5 . . ? C79 C78 H78B 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 108.1 . . ? C85 C79 C80 109.7(3) . . ? C85 C79 C78 109.9(3) . . ? C80 C79 C78 109.9(3) . . ? C85 C79 H79 109.1 . . ? C80 C79 H79 109.1 . . ? C78 C79 H79 109.1 . . ? C79 C80 C81 108.7(3) . . ? C79 C80 H80A 110.0 . . ? C81 C80 H80A 110.0 . . ? C79 C80 H80B 110.0 . . ? C81 C80 H80B 110.0 . . ? H80A C80 H80B 108.3 . . ? C86 C81 C80 109.8(3) . . ? C86 C81 C82 109.8(3) . . ? C80 C81 C82 109.7(3) . . ? C86 C81 H81 109.2 . . ? C80 C81 H81 109.2 . . ? C82 C81 H81 109.2 . . ? C81 C82 C77 111.1(3) . . ? C81 C82 H82A 109.4 . . ? C77 C82 H82A 109.4 . . ? C81 C82 H82B 109.4 . . ? C77 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? C84 C83 C77 110.8(3) . . ? C84 C83 H83A 109.5 . . ? C77 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? C77 C83 H83B 109.5 . . ? H83A C83 H83B 108.1 . . ? C85 C84 C86 109.9(3) . . ? C85 C84 C83 109.5(3) . . ? C86 C84 C83 109.8(3) . . ? C85 C84 H84 109.2 . . ? C86 C84 H84 109.2 . . ? C83 C84 H84 109.2 . . ? C84 C85 C79 109.0(3) . . ? C84 C85 H85A 109.9 . . ? C79 C85 H85A 109.9 . . ? C84 C85 H85B 109.9 . . ? C79 C85 H85B 109.9 . . ? H85A C85 H85B 108.3 . . ? C81 C86 C84 109.0(3) . . ? C81 C86 H86A 109.9 . . ? C84 C86 H86A 109.9 . . ? C81 C86 H86B 109.9 . . ? C84 C86 H86B 109.9 . . ? H86A C86 H86B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C24 P1 C1 C2 -69.5(3) . . . . ? C34 P1 C1 C2 48.1(3) . . . . ? C24 P1 C1 C8 117.8(2) . . . . ? C34 P1 C1 C8 -124.6(2) . . . . ? C3 O1 C2 C4 1.2(4) . . . . ? C3 O1 C2 C1 -177.9(3) . . . . ? C8 C1 C2 C4 -0.2(4) . . . . ? P1 C1 C2 C4 -172.9(2) . . . . ? C8 C1 C2 O1 179.0(2) . . . . ? P1 C1 C2 O1 6.3(4) . . . . ? O1 C2 C4 C5 -176.1(3) . . . . ? C1 C2 C4 C5 3.1(5) . . . . ? C2 C4 C5 C6 -1.5(5) . . . . ? C7 O2 C6 C5 -11.0(4) . . . . ? C7 O2 C6 C8 169.3(3) . . . . ? C4 C5 C6 O2 177.4(3) . . . . ? C4 C5 C6 C8 -3.0(5) . . . . ? O2 C6 C8 C1 -174.4(3) . . . . ? C5 C6 C8 C1 5.9(4) . . . . ? O2 C6 C8 C9 8.5(4) . . . . ? C5 C6 C8 C9 -171.2(3) . . . . ? C2 C1 C8 C6 -4.2(4) . . . . ? P1 C1 C8 C6 169.0(2) . . . . ? C2 C1 C8 C9 172.5(3) . . . . ? P1 C1 C8 C9 -14.2(4) . . . . ? C6 C8 C9 C20 -97.4(3) . . . . ? C1 C8 C9 C20 85.7(4) . . . . ? C6 C8 C9 C10 74.6(3) . . . . ? C1 C8 C9 C10 -102.3(3) . . . . ? C20 C9 C10 C14 -2.0(4) . . . . ? C8 C9 C10 C14 -174.3(3) . . . . ? C20 C9 C10 C11 172.9(3) . . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C14 C10 C11 C12 -55.6(4) . . . . ? C9 C10 C11 C12 129.4(3) . . . . ? C14 C10 C11 C13 67.6(4) . . . . ? C9 C10 C11 C13 -107.4(3) . . . . ? C9 C10 C14 C15 1.3(5) . . . . ? C11 C10 C14 C15 -173.9(3) . . . . ? C10 C14 C15 C19 -0.4(5) . . . . ? C10 C14 C15 C16A 174.8(4) . . . . ? C10 C14 C15 C16B -170.8(10) . . . . ? C14 C15 C16A C17A 96.6(7) . . . . ? C19 C15 C16A C17A -88.7(7) . . . . ? C14 C15 C16A C18A -144.5(5) . . . . ? C19 C15 C16A C18A 30.2(8) . . . . ? C14 C15 C16B C18B 11.0(17) . . . . ? C19 C15 C16B C18B -160.1(10) . . . . ? C14 C15 C16B C17B -91.8(14) . . . . ? C19 C15 C16B C17B 97.1(12) . . . . ? C14 C15 C19 C20 0.3(5) . . . . ? C16A C15 C19 C20 -174.3(4) . . . . ? C16B C15 C19 C20 173.2(7) . . . . ? C15 C19 C20 C9 -1.0(5) . . . . ? C15 C19 C20 C21 174.7(3) . . . . ? C10 C9 C20 C19 1.9(4) . . . . ? C8 C9 C20 C19 173.9(3) . . . . ? C10 C9 C20 C21 -173.7(3) . . . . ? C8 C9 C20 C21 -1.7(4) . . . . ? C19 C20 C21 C22 40.2(4) . . . . ? C9 C20 C21 C22 -144.2(3) . . . . ? C19 C20 C21 C23 -85.2(4) . . . . ? C9 C20 C21 C23 90.4(4) . . . . ? C1 P1 C24 C29 55.9(3) . . . . ? C34 P1 C24 C29 -59.9(3) . . . . ? C1 P1 C24 C25 -64.9(2) . . . . ? C34 P1 C24 C25 179.27(19) . . . . ? C1 P1 C24 C30 -178.43(19) . . . . ? C34 P1 C24 C30 65.8(2) . . . . ? C29 C24 C25 C26 58.9(3) . . . . ? C30 C24 C25 C26 -58.1(3) . . . . ? P1 C24 C25 C26 -171.6(2) . . . . ? C24 C25 C26 C32 60.3(4) . . . . ? C24 C25 C26 C27 -59.9(4) . . . . ? C32 C26 C27 C28 -60.8(4) . . . . ? C25 C26 C27 C28 59.5(4) . . . . ? C26 C27 C28 C33 60.6(4) . . . . ? C26 C27 C28 C29 -60.2(4) . . . . ? C25 C24 C29 C28 -58.9(3) . . . . ? C30 C24 C29 C28 56.8(4) . . . . ? P1 C24 C29 C28 -178.5(2) . . . . ? C27 C28 C29 C24 60.9(4) . . . . ? C33 C28 C29 C24 -59.7(4) . . . . ? C29 C24 C30 C31 -56.8(3) . . . . ? C25 C24 C30 C31 59.0(3) . . . . ? P1 C24 C30 C31 170.8(2) . . . . ? C24 C30 C31 C33 59.0(4) . . . . ? C24 C30 C31 C32 -61.5(4) . . . . ? C27 C26 C32 C31 59.6(4) . . . . ? C25 C26 C32 C31 -60.3(4) . . . . ? C33 C31 C32 C26 -59.3(4) . . . . ? C30 C31 C32 C26 60.8(4) . . . . ? C27 C28 C33 C31 -59.8(4) . . . . ? C29 C28 C33 C31 60.9(4) . . . . ? C32 C31 C33 C28 59.4(4) . . . . ? C30 C31 C33 C28 -60.4(4) . . . . ? C39 C34 C35 C36 -57.8(3) . . . . ? C40 C34 C35 C36 57.8(3) . . . . ? P1 C34 C35 C36 -175.0(2) . . . . ? C34 C35 C36 C37 60.0(4) . . . . ? C34 C35 C36 C42 -59.6(3) . . . . ? C35 C36 C37 C38 -59.9(4) . . . . ? C42 C36 C37 C38 60.2(3) . . . . ? C36 C37 C38 C43 -60.3(3) . . . . ? C36 C37 C38 C39 59.9(3) . . . . ? C37 C38 C39 C34 -60.0(3) . . . . ? C43 C38 C39 C34 60.3(3) . . . . ? C40 C34 C39 C38 -58.0(3) . . . . ? C35 C34 C39 C38 57.6(3) . . . . ? P1 C34 C39 C38 170.1(2) . . . . ? C39 C34 C40 C41 57.8(3) . . . . ? C35 C34 C40 C41 -57.8(3) . . . . ? P1 C34 C40 C41 -175.3(2) . . . . ? C34 C40 C41 C42 60.3(3) . . . . ? C34 C40 C41 C43 -60.2(3) . . . . ? C43 C41 C42 C36 60.9(3) . . . . ? C40 C41 C42 C36 -59.7(3) . . . . ? C37 C36 C42 C41 -60.5(3) . . . . ? C35 C36 C42 C41 59.4(4) . . . . ? C42 C41 C43 C38 -60.6(3) . . . . ? C40 C41 C43 C38 60.3(4) . . . . ? C37 C38 C43 C41 60.3(3) . . . . ? C39 C38 C43 C41 -60.3(4) . . . . ? C46 O4 C45 C47 6.0(5) . . . . ? C46 O4 C45 C44 -173.0(4) . . . . ? C51 C44 C45 O4 175.9(3) . . . . ? C52 C44 C45 O4 -0.1(4) . . . . ? C51 C44 C45 C47 -3.2(5) . . . . ? C52 C44 C45 C47 -179.2(3) . . . . ? O4 C45 C47 C48 -177.0(3) . . . . ? C44 C45 C47 C48 2.1(5) . . . . ? C45 C47 C48 C49 0.5(5) . . . . ? C47 C48 C49 O3 177.8(3) . . . . ? C47 C48 C49 C51 -1.9(5) . . . . ? C50 O3 C49 C48 -15.7(4) . . . . ? C50 O3 C49 C51 164.1(3) . . . . ? C45 C44 C51 C49 1.8(4) . . . . ? C52 C44 C51 C49 177.3(3) . . . . ? C45 C44 C51 P2 -174.6(2) . . . . ? C52 C44 C51 P2 0.9(4) . . . . ? C48 C49 C51 C44 0.7(4) . . . . ? O3 C49 C51 C44 -179.0(3) . . . . ? C48 C49 C51 P2 176.9(2) . . . . ? O3 C49 C51 P2 -2.8(4) . . . . ? C67 P2 C51 C44 -113.1(2) . . . . ? C77 P2 C51 C44 129.7(2) . . . . ? C67 P2 C51 C49 70.7(3) . . . . ? C77 P2 C51 C49 -46.5(3) . . . . ? C45 C44 C52 C53 -78.7(4) . . . . ? C51 C44 C52 C53 105.6(4) . . . . ? C45 C44 C52 C63 91.2(4) . . . . ? C51 C44 C52 C63 -84.5(4) . . . . ? C63 C52 C53 C57 2.4(5) . . . . ? C44 C52 C53 C57 172.3(3) . . . . ? C63 C52 C53 C54 -174.2(3) . . . . ? C44 C52 C53 C54 -4.3(5) . . . . ? C57 C53 C54 C55 48.9(5) . . . . ? C52 C53 C54 C55 -134.4(4) . . . . ? C57 C53 C54 C56 -74.1(5) . . . . ? C52 C53 C54 C56 102.7(4) . . . . ? C52 C53 C57 C58 -2.1(6) . . . . ? C54 C53 C57 C58 174.8(4) . . . . ? C53 C57 C58 C62 0.9(6) . . . . ? C53 C57 C58 C59B -178.4(16) . . . . ? C53 C57 C58 C59A -172.5(6) . . . . ? C62 C58 C59A C60A 39.4(10) . . . . ? C57 C58 C59A C60A -147.7(6) . . . . ? C62 C58 C59A C61A -83.9(10) . . . . ? C57 C58 C59A C61A 89.0(8) . . . . ? C62 C58 C59B C61B 159.7(19) . . . . ? C57 C58 C59B C61B -21(3) . . . . ? C62 C58 C59B C60B -60(3) . . . . ? C57 C58 C59B C60B 119(2) . . . . ? C57 C58 C62 C63 -0.2(5) . . . . ? C59B C58 C62 C63 179.2(15) . . . . ? C59A C58 C62 C63 172.9(6) . . . . ? C58 C62 C63 C52 0.6(5) . . . . ? C58 C62 C63 C64 -176.2(3) . . . . ? C53 C52 C63 C62 -1.7(5) . . . . ? C44 C52 C63 C62 -171.9(3) . . . . ? C53 C52 C63 C64 175.0(3) . . . . ? C44 C52 C63 C64 4.8(5) . . . . ? C62 C63 C64 C65 -46.4(4) . . . . ? C52 C63 C64 C65 136.9(3) . . . . ? C62 C63 C64 C66 77.7(4) . . . . ? C52 C63 C64 C66 -99.0(4) . . . . ? C51 P2 C67 C72 64.5(2) . . . . ? C77 P2 C67 C72 -179.5(2) . . . . ? C51 P2 C67 C68 -56.4(3) . . . . ? C77 P2 C67 C68 59.6(3) . . . . ? C51 P2 C67 C73 178.2(2) . . . . ? C77 P2 C67 C73 -65.8(2) . . . . ? C72 C67 C68 C69 58.4(3) . . . . ? C73 C67 C68 C69 -56.9(3) . . . . ? P2 C67 C68 C69 178.1(2) . . . . ? C67 C68 C69 C70 -60.9(4) . . . . ? C67 C68 C69 C75 59.5(4) . . . . ? C75 C69 C70 C71 -60.3(4) . . . . ? C68 C69 C70 C71 60.1(4) . . . . ? C69 C70 C71 C76 60.4(4) . . . . ? C69 C70 C71 C72 -59.3(4) . . . . ? C76 C71 C72 C67 -59.9(4) . . . . ? C70 C71 C72 C67 59.8(4) . . . . ? C68 C67 C72 C71 -58.2(3) . . . . ? C73 C67 C72 C71 58.2(3) . . . . ? P2 C67 C72 C71 172.5(2) . . . . ? C72 C67 C73 C74 -58.6(3) . . . . ? C68 C67 C73 C74 56.9(3) . . . . ? P2 C67 C73 C74 -171.0(2) . . . . ? C67 C73 C74 C75 -59.4(4) . . . . ? C67 C73 C74 C76 60.8(3) . . . . ? C76 C74 C75 C69 -59.5(4) . . . . ? C73 C74 C75 C69 60.5(4) . . . . ? C70 C69 C75 C74 60.0(4) . . . . ? C68 C69 C75 C74 -60.5(4) . . . . ? C70 C71 C76 C74 -60.3(4) . . . . ? C72 C71 C76 C74 59.5(4) . . . . ? C75 C74 C76 C71 60.0(4) . . . . ? C73 C74 C76 C71 -60.3(4) . . . . ? C82 C77 C78 C79 -57.4(3) . . . . ? C83 C77 C78 C79 58.2(3) . . . . ? P2 C77 C78 C79 175.4(2) . . . . ? C77 C78 C79 C85 -60.6(4) . . . . ? C77 C78 C79 C80 60.2(4) . . . . ? C85 C79 C80 C81 60.1(4) . . . . ? C78 C79 C80 C81 -60.8(4) . . . . ? C79 C80 C81 C86 -60.3(4) . . . . ? C79 C80 C81 C82 60.4(4) . . . . ? C86 C81 C82 C77 60.8(4) . . . . ? C80 C81 C82 C77 -59.8(4) . . . . ? C78 C77 C82 C81 57.4(3) . . . . ? C83 C77 C82 C81 -58.5(3) . . . . ? P2 C77 C82 C81 -170.2(2) . . . . ? C82 C77 C83 C84 58.3(3) . . . . ? C78 C77 C83 C84 -58.2(3) . . . . ? P2 C77 C83 C84 174.5(2) . . . . ? C77 C83 C84 C85 60.4(4) . . . . ? C77 C83 C84 C86 -60.4(4) . . . . ? C86 C84 C85 C79 60.3(4) . . . . ? C83 C84 C85 C79 -60.4(4) . . . . ? C80 C79 C85 C84 -60.2(4) . . . . ? C78 C79 C85 C84 60.7(4) . . . . ? C80 C81 C86 C84 60.5(4) . . . . ? C82 C81 C86 C84 -60.2(4) . . . . ? C85 C84 C86 C81 -60.5(4) . . . . ? C83 C84 C86 C81 60.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7B O2 0.96 2.49 3.366(4) 152.0 2_757 C29 H29B O1 0.97 2.41 2.971(4) 116.3 . C39 H39A O1 0.97 2.52 3.243(4) 131.4 . C40 H40B O1 0.97 2.39 3.148(4) 134.2 . C68 H68A O3 0.97 2.41 2.964(4) 115.5 . C78 H78A O3 0.97 2.34 3.099(4) 134.1 . C82 H82B O3 0.97 2.48 3.202(4) 131.1 . _refine_diff_density_max 0.687 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.051 _shelx_res_file ; TITL XRAY5779_0m_a.res in P-1 XRAY5779_0m_a.res created by SHELXL-2016/6 at 19:54:01 on 13-Mar-2019 CELL 0.71073 12.8378 16.3574 19.0289 97.751 102.559 102.096 ZERR 4.000 0.0036 0.0046 0.0053 0.004 0.004 0.004 LATT 1 SFAC C H O P UNIT 172 244 8 4 OMIT 0 0 1 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 SADI C60A C61A C60B C61B SADI C59A C60A C59A C61A C59B C60B C59B C61B SADI C17A C18A C17B C18B SADI C16A C17A C16A C18A C16B C17B C16B C18B EADP C59A C59B EADP C61A C60B EADP C18A C18B EADP C17A C17B EADP C16A C16B SIZE 0.03 0.20 0.20 WPDB CONF EQIV $1 -x+2, -y, -z+2 HTAB C7 O2_$1 HTAB C29 O1 HTAB C39 O1 HTAB C40 O1 HTAB C68 O3 HTAB C78 O3 HTAB C82 O3 ISOR 0.3 O5 TEMP 23.0 WGHT 0.100000 0.559580 FVAR 0.44288 0.72445 0.69773 PART -1 MOLE 3 O5 3 0.974879 0.971997 0.505519 10.12000 0.08336 PART 0 MOLE 1 P1 4 0.737296 0.300544 1.039422 11.00000 0.02930 0.03168 = 0.03094 0.00730 0.00938 0.01086 O1 3 0.662133 0.230226 1.168487 11.00000 0.05074 0.04886 = 0.03663 0.01269 0.02434 0.02121 O2 3 0.896933 0.036726 1.039760 11.00000 0.05881 0.05094 = 0.04675 0.02099 0.02415 0.03564 C1 1 0.748907 0.200297 1.073867 11.00000 0.02686 0.02908 = 0.03074 0.00706 0.00592 0.00627 C2 1 0.715729 0.177480 1.136213 11.00000 0.03074 0.03573 = 0.02689 0.00334 0.00785 0.00803 C3 1 0.630623 0.211985 1.232046 11.00000 0.08891 0.05655 = 0.05175 0.00979 0.04227 0.02621 AFIX 137 H3A 2 0.579066 0.157340 1.220754 11.00000 -1.50000 H3B 2 0.596842 0.254877 1.249790 11.00000 -1.50000 H3C 2 0.694434 0.211278 1.269013 11.00000 -1.50000 AFIX 0 C4 1 0.737031 0.107508 1.163390 11.00000 0.03878 0.04471 = 0.03064 0.01266 0.01381 0.01236 AFIX 43 H4 2 0.711028 0.092737 1.203068 11.00000 -1.20000 AFIX 0 C5 1 0.797088 0.058801 1.131973 11.00000 0.05019 0.03871 = 0.03863 0.01647 0.01447 0.01796 AFIX 43 H5 2 0.812952 0.012121 1.151101 11.00000 -1.20000 AFIX 0 C6 1 0.833275 0.079996 1.072049 11.00000 0.03743 0.03763 = 0.03146 0.00800 0.01031 0.01553 C7 1 0.942705 -0.022543 1.077488 11.00000 0.07376 0.05974 = 0.06467 0.03107 0.02973 0.04479 AFIX 137 H7A 2 0.982673 0.005283 1.126563 11.00000 -1.50000 H7B 2 0.991706 -0.043390 1.052166 11.00000 -1.50000 H7C 2 0.884473 -0.069324 1.079072 11.00000 -1.50000 AFIX 0 C8 1 0.805908 0.147768 1.040125 11.00000 0.02642 0.03131 = 0.02802 0.00736 0.00445 0.00986 C9 1 0.837082 0.154164 0.968554 11.00000 0.03296 0.03264 = 0.03419 0.01261 0.01495 0.01630 C10 1 0.773931 0.095505 0.904865 11.00000 0.03987 0.03776 = 0.03504 0.01247 0.00945 0.01642 C11 1 0.674057 0.025657 0.903954 11.00000 0.05179 0.04431 = 0.03553 0.00599 0.00753 0.00557 AFIX 13 H11 2 0.656217 0.036947 0.951287 11.00000 -1.20000 AFIX 0 C12 1 0.571908 0.022747 0.844065 11.00000 0.04966 0.05399 = 0.04969 -0.00266 0.00123 0.00489 AFIX 137 H12A 2 0.582410 0.002196 0.797059 11.00000 -1.50000 H12B 2 0.560061 0.078908 0.845409 11.00000 -1.50000 H12C 2 0.509007 -0.014694 0.852062 11.00000 -1.50000 AFIX 0 C13 1 0.698775 -0.062286 0.895619 11.00000 0.08587 0.05075 = 0.08170 0.01763 0.00166 0.00711 AFIX 137 H13A 2 0.720260 -0.073880 0.850753 11.00000 -1.50000 H13B 2 0.634072 -0.104818 0.894609 11.00000 -1.50000 H13C 2 0.757481 -0.063269 0.936273 11.00000 -1.50000 AFIX 0 C14 1 0.808165 0.096239 0.840117 11.00000 0.05124 0.05656 = 0.02772 0.00788 0.00812 0.02098 AFIX 43 H14 2 0.765271 0.058097 0.797961 11.00000 -1.20000 AFIX 0 C15 1 0.902717 0.151110 0.836309 11.00000 0.05080 0.07234 = 0.03154 0.02206 0.01710 0.02990 PART 1 C16A 1 0.933441 0.138115 0.762972 21.00000 0.05370 0.07448 = 0.04277 0.02299 0.02161 0.01025 AFIX 13 H16A 2 0.899442 0.079273 0.737254 21.00000 -1.20000 AFIX 0 C17A 1 0.894345 0.197358 0.715884 21.00000 0.12057 0.11014 = 0.07249 0.05722 0.05472 0.07451 AFIX 137 H17A 2 0.815473 0.185657 0.704959 21.00000 -1.50000 H17B 2 0.916885 0.189349 0.671057 21.00000 -1.50000 H17C 2 0.925581 0.255100 0.741407 21.00000 -1.50000 AFIX 0 C18A 1 1.059272 0.156006 0.773116 21.00000 0.06946 0.08831 = 0.05430 0.02654 0.03600 0.02736 AFIX 137 H18A 2 1.075197 0.149651 0.725952 21.00000 -1.50000 H18B 2 1.087559 0.116451 0.800123 21.00000 -1.50000 H18C 2 1.093306 0.213039 0.799581 21.00000 -1.50000 PART 2 AFIX 0 C16B 1 0.957943 0.177200 0.770501 -21.00000 0.05370 0.07448 = 0.04277 0.02299 0.02161 0.01025 AFIX 13 H16B 2 0.991742 0.237838 0.774926 -21.00000 -1.20000 AFIX 0 C17B 1 1.034334 0.115079 0.763006 -21.00000 0.12057 0.11014 = 0.07249 0.05722 0.05472 0.07451 AFIX 137 H17D 2 0.990039 0.059202 0.739306 -21.00000 -1.50000 H17E 2 1.075995 0.112769 0.810826 -21.00000 -1.50000 H17F 2 1.083782 0.135196 0.734292 -21.00000 -1.50000 AFIX 0 C18B 1 0.863385 0.135621 0.701642 -21.00000 0.06946 0.08831 = 0.05430 0.02654 0.03600 0.02736 AFIX 137 H18D 2 0.879092 0.159245 0.660467 -21.00000 -1.50000 H18E 2 0.795793 0.146400 0.709646 -21.00000 -1.50000 H18F 2 0.856366 0.075318 0.691918 -21.00000 -1.50000 PART 0 AFIX 0 C19 1 0.964846 0.207685 0.899671 11.00000 0.03737 0.05363 = 0.04803 0.02035 0.01885 0.01385 AFIX 43 H19 2 1.029022 0.245507 0.898063 11.00000 -1.20000 AFIX 0 C20 1 0.934522 0.209860 0.965634 11.00000 0.03204 0.03681 = 0.03712 0.01127 0.01432 0.01384 C21 1 1.011510 0.268061 1.034355 11.00000 0.03369 0.05183 = 0.04766 0.00415 0.01694 0.00652 AFIX 13 H21 2 0.966760 0.277768 1.068856 11.00000 -1.20000 AFIX 0 C22 1 1.067899 0.355373 1.022931 11.00000 0.06241 0.05161 = 0.08087 0.00666 0.02852 0.00277 AFIX 137 H22A 2 1.118995 0.348986 0.993727 11.00000 -1.50000 H22B 2 1.106687 0.390845 1.069627 11.00000 -1.50000 H22C 2 1.013481 0.381201 0.998253 11.00000 -1.50000 AFIX 0 C23 1 1.097398 0.224440 1.070775 11.00000 0.05708 0.07059 = 0.07390 0.00715 -0.01324 0.00793 AFIX 137 H23A 2 1.060889 0.171742 1.081344 11.00000 -1.50000 H23B 2 1.142657 0.260899 1.115549 11.00000 -1.50000 H23C 2 1.142595 0.213280 1.038306 11.00000 -1.50000 AFIX 0 C24 1 0.585286 0.291488 1.001650 11.00000 0.03044 0.04042 = 0.03020 0.00924 0.00789 0.01090 C25 1 0.548927 0.217098 0.935723 11.00000 0.03931 0.04362 = 0.04107 0.00162 0.00278 0.00981 AFIX 23 H25A 2 0.552972 0.164438 0.953027 11.00000 -1.20000 H25B 2 0.598641 0.225947 0.904144 11.00000 -1.20000 AFIX 0 C26 1 0.430562 0.209535 0.891570 11.00000 0.04312 0.06447 = 0.04425 0.00180 -0.00518 0.00782 AFIX 13 H26 2 0.409453 0.161524 0.850232 11.00000 -1.20000 AFIX 0 C27 1 0.352574 0.194305 0.941195 11.00000 0.03760 0.08521 = 0.06123 0.01453 -0.00293 0.00176 AFIX 23 H27A 2 0.277679 0.189408 0.913817 11.00000 -1.20000 H27B 2 0.355292 0.141549 0.958636 11.00000 -1.20000 AFIX 0 C28 1 0.385983 0.267634 1.005611 11.00000 0.03536 0.08546 = 0.05247 0.01756 0.01412 0.01299 AFIX 13 H28 2 0.335810 0.257417 1.037403 11.00000 -1.20000 AFIX 0 C29 1 0.504162 0.274597 1.049530 11.00000 0.03261 0.05391 = 0.03872 0.00959 0.00912 0.00809 AFIX 23 H29A 2 0.524541 0.320584 1.091671 11.00000 -1.20000 H29B 2 0.507774 0.222116 1.067258 11.00000 -1.20000 AFIX 0 C30 1 0.575265 0.372874 0.971151 11.00000 0.03773 0.04570 = 0.04525 0.01382 0.00991 0.01680 AFIX 23 H30A 2 0.597563 0.421281 1.011370 11.00000 -1.20000 H30B 2 0.624278 0.382621 0.939219 11.00000 -1.20000 AFIX 0 C31 1 0.456343 0.365361 0.928025 11.00000 0.04535 0.06161 = 0.05193 0.01959 0.00625 0.02604 AFIX 13 H31 2 0.451976 0.418268 0.910080 11.00000 -1.20000 AFIX 0 C32 1 0.423969 0.291131 0.862762 11.00000 0.04286 0.08203 = 0.04618 0.01667 0.00007 0.01773 AFIX 23 H32A 2 0.349646 0.286234 0.834363 11.00000 -1.20000 H32B 2 0.473467 0.301085 0.831169 11.00000 -1.20000 AFIX 0 C33 1 0.379261 0.349953 0.978200 11.00000 0.04042 0.09033 = 0.06406 0.01497 0.01029 0.03200 AFIX 23 H33A 2 0.400310 0.397097 1.019447 11.00000 -1.20000 H33B 2 0.304282 0.346024 0.951544 11.00000 -1.20000 AFIX 0 C34 1 0.796470 0.392784 1.122428 11.00000 0.03122 0.03101 = 0.03158 0.00640 0.00806 0.00821 C35 1 0.852633 0.466803 1.090014 11.00000 0.04415 0.03632 = 0.04042 0.00902 0.01077 0.00686 AFIX 23 H35A 2 0.904169 0.448230 1.064905 11.00000 -1.20000 H35B 2 0.797327 0.482316 1.054377 11.00000 -1.20000 AFIX 0 C36 1 0.913926 0.544692 1.150103 11.00000 0.05625 0.03382 = 0.04708 0.00641 0.01060 -0.00082 AFIX 13 H36 2 0.948513 0.590520 1.128100 11.00000 -1.20000 AFIX 0 C37 1 1.002513 0.520776 1.205639 11.00000 0.03783 0.05150 = 0.05475 -0.00381 0.00911 0.00200 AFIX 23 H37A 2 1.054877 0.502101 1.181399 11.00000 -1.20000 H37B 2 1.041988 0.570011 1.243644 11.00000 -1.20000 AFIX 0 C38 1 0.948280 0.449610 1.239553 11.00000 0.04046 0.04674 = 0.03461 0.00149 -0.00077 0.01129 AFIX 13 H38 2 1.004964 0.434186 1.275135 11.00000 -1.20000 AFIX 0 C39 1 0.886797 0.371694 1.179862 11.00000 0.03489 0.03889 = 0.03954 0.00602 0.00521 0.01224 AFIX 23 H39A 2 0.853559 0.326351 1.202062 11.00000 -1.20000 H39B 2 0.938589 0.351702 1.155843 11.00000 -1.20000 AFIX 0 C40 1 0.717542 0.425745 1.163222 11.00000 0.03510 0.04369 = 0.03478 0.00192 0.00930 0.01262 AFIX 23 H40A 2 0.660575 0.440837 1.128547 11.00000 -1.20000 H40B 2 0.682254 0.380934 1.185097 11.00000 -1.20000 AFIX 0 C41 1 0.779351 0.503640 1.223188 11.00000 0.04321 0.04361 = 0.04426 -0.00402 0.00860 0.01465 AFIX 13 H41 2 0.727192 0.522929 1.248168 11.00000 -1.20000 AFIX 0 C42 1 0.832990 0.575124 1.189648 11.00000 0.05950 0.03856 = 0.05348 -0.00319 -0.00159 0.01488 AFIX 23 H42A 2 0.871798 0.624403 1.227765 11.00000 -1.20000 H42B 2 0.777060 0.591490 1.155162 11.00000 -1.20000 AFIX 0 C43 1 0.867177 0.479880 1.278513 11.00000 0.05437 0.04838 = 0.03503 -0.00229 0.00553 0.00581 AFIX 23 H43A 2 0.833144 0.434978 1.300825 11.00000 -1.20000 H43B 2 0.905811 0.528886 1.316945 11.00000 -1.20000 AFIX 0 MOLE 2 P2 4 0.559680 0.357330 0.579359 11.00000 0.02919 0.03486 = 0.03528 0.00925 0.00408 0.01022 O3 3 0.681673 0.312503 0.722952 11.00000 0.03735 0.04977 = 0.03399 0.01412 0.00440 0.00781 O4 3 0.294373 0.074493 0.584425 11.00000 0.05456 0.04881 = 0.09042 0.01904 0.00536 -0.00867 C44 1 0.426482 0.198599 0.585864 11.00000 0.03350 0.03321 = 0.04083 0.00496 0.01010 0.01373 C45 1 0.394194 0.129984 0.619658 11.00000 0.03790 0.03311 = 0.05955 0.00658 0.00947 0.00400 C46 1 0.251770 0.009391 0.620214 11.00000 0.07497 0.07496 = 0.15896 0.05235 0.01671 -0.01871 AFIX 137 H46A 2 0.302391 -0.025992 0.628969 11.00000 -1.50000 H46B 2 0.182183 -0.024528 0.589805 11.00000 -1.50000 H46C 2 0.241893 0.034614 0.666099 11.00000 -1.50000 AFIX 0 C47 1 0.458882 0.120563 0.684650 11.00000 0.06000 0.03437 = 0.06109 0.01942 0.01711 0.00900 AFIX 43 H47 2 0.437178 0.073577 0.705433 11.00000 -1.20000 AFIX 0 C48 1 0.555441 0.180588 0.718742 11.00000 0.05305 0.04334 = 0.04359 0.01427 0.01380 0.01431 AFIX 43 H48 2 0.599238 0.173878 0.762372 11.00000 -1.20000 AFIX 0 C49 1 0.587401 0.250363 0.688605 11.00000 0.03250 0.03591 = 0.04154 0.00663 0.01230 0.01004 C50 1 0.731002 0.315389 0.797825 11.00000 0.04828 0.06994 = 0.03786 0.01385 0.00311 0.01021 AFIX 137 H50A 2 0.677028 0.316597 0.825583 11.00000 -1.50000 H50B 2 0.790315 0.365642 0.816009 11.00000 -1.50000 H50C 2 0.759065 0.265883 0.802580 11.00000 -1.50000 AFIX 0 C51 1 0.524766 0.261703 0.621125 11.00000 0.02901 0.03301 = 0.03648 0.00737 0.00914 0.01127 C52 1 0.345161 0.200224 0.515075 11.00000 0.03085 0.03238 = 0.04659 0.00324 0.00667 0.00554 C53 1 0.338730 0.148095 0.448900 11.00000 0.03538 0.04422 = 0.04929 -0.00303 0.00452 0.00946 C54 1 0.416312 0.090145 0.440122 11.00000 0.04777 0.06447 = 0.06908 -0.01932 0.00048 0.02212 AFIX 13 H54 2 0.479731 0.107999 0.482971 11.00000 -1.20000 AFIX 0 C55 1 0.459193 0.096253 0.371785 11.00000 0.06170 0.12146 = 0.09116 -0.04746 0.01642 0.02457 AFIX 137 H55A 2 0.401922 0.066325 0.329125 11.00000 -1.50000 H55B 2 0.521028 0.071301 0.375135 11.00000 -1.50000 H55C 2 0.481614 0.154977 0.368092 11.00000 -1.50000 AFIX 0 C56 1 0.359429 -0.002702 0.437935 11.00000 0.09416 0.05999 = 0.12889 -0.01242 0.00998 0.03744 AFIX 137 H56A 2 0.338440 -0.007460 0.482940 11.00000 -1.50000 H56B 2 0.409177 -0.037952 0.431944 11.00000 -1.50000 H56C 2 0.295023 -0.020883 0.397552 11.00000 -1.50000 AFIX 0 C57 1 0.254296 0.144453 0.387737 11.00000 0.04942 0.05813 = 0.04292 -0.00988 0.00404 0.01112 AFIX 43 H57 2 0.251972 0.111090 0.343525 11.00000 -1.20000 AFIX 0 C58 1 0.173338 0.188677 0.390098 11.00000 0.03972 0.06240 = 0.04531 0.01311 0.00500 0.01174 PART 1 C59A 1 0.072201 0.172010 0.320573 31.00000 0.05097 0.10776 = 0.04605 0.00943 -0.01085 0.01898 AFIX 13 H59A 2 0.096280 0.154259 0.276728 31.00000 -1.20000 AFIX 0 C60A 1 0.030613 0.250159 0.312028 31.00000 0.06365 0.11852 = 0.13707 0.05903 -0.03223 0.02446 AFIX 137 H60A 2 -0.018858 0.241275 0.264391 31.00000 -1.50000 H60B 2 0.091625 0.297862 0.317211 31.00000 -1.50000 H60C 2 -0.007546 0.261355 0.349014 31.00000 -1.50000 AFIX 0 C61A 1 -0.016739 0.098984 0.328508 31.00000 0.09255 0.10797 = 0.13271 0.03917 -0.05472 -0.03312 AFIX 137 H61A 2 -0.031491 0.111015 0.375662 31.00000 -1.50000 H61B 2 0.007764 0.047398 0.324137 31.00000 -1.50000 H61C 2 -0.082724 0.092369 0.290742 31.00000 -1.50000 PART 2 AFIX 0 C59B 1 0.086309 0.183304 0.328530 -31.00000 0.05097 0.10776 = 0.04605 0.00943 -0.01085 0.01898 AFIX 13 H59B 2 0.087135 0.243432 0.329078 -31.00000 -1.20000 AFIX 0 C60B 1 -0.026100 0.148411 0.339368 -31.00000 0.09255 0.10797 = 0.13271 0.03917 -0.05472 -0.03312 AFIX 137 H60D 2 -0.035718 0.089099 0.341612 -31.00000 -1.50000 H60E 2 -0.081409 0.155074 0.299098 -31.00000 -1.50000 H60F 2 -0.032849 0.178812 0.384307 -31.00000 -1.50000 AFIX 0 C61B 1 0.094995 0.154759 0.252148 -31.00000 0.07825 0.19804 = 0.02611 0.01087 -0.01216 -0.00029 AFIX 137 H61D 2 0.167794 0.179240 0.248171 -31.00000 -1.50000 H61E 2 0.042099 0.172982 0.217797 -31.00000 -1.50000 H61F 2 0.080648 0.093794 0.241614 -31.00000 -1.50000 PART 0 AFIX 0 C62 1 0.181013 0.237953 0.456047 11.00000 0.04120 0.04879 = 0.05337 0.00999 0.01040 0.02013 AFIX 43 H62 2 0.127921 0.268306 0.458942 11.00000 -1.20000 AFIX 0 C63 1 0.263105 0.245031 0.518367 11.00000 0.03113 0.03777 = 0.04355 0.00665 0.00824 0.00973 C64 1 0.258944 0.296898 0.589019 11.00000 0.03714 0.05406 = 0.05216 -0.00072 0.00671 0.02074 AFIX 13 H64 2 0.331521 0.307985 0.623356 11.00000 -1.20000 AFIX 0 C65 1 0.234913 0.382569 0.579678 11.00000 0.05917 0.05839 = 0.08214 -0.00549 0.01021 0.03144 AFIX 137 H65A 2 0.285639 0.411987 0.555673 11.00000 -1.50000 H65B 2 0.242960 0.415993 0.626936 11.00000 -1.50000 H65C 2 0.160977 0.373781 0.550529 11.00000 -1.50000 AFIX 0 C66 1 0.174715 0.247091 0.623176 11.00000 0.10607 0.09387 = 0.08824 0.01830 0.06059 0.03747 AFIX 137 H66A 2 0.103256 0.232332 0.589416 11.00000 -1.50000 H66B 2 0.172675 0.281531 0.667654 11.00000 -1.50000 H66C 2 0.195292 0.196117 0.633918 11.00000 -1.50000 AFIX 0 C67 1 0.687594 0.347616 0.548171 11.00000 0.03608 0.03597 = 0.03368 0.01169 0.01067 0.01201 C68 1 0.791002 0.340047 0.603005 11.00000 0.04081 0.05804 = 0.03748 0.01618 0.01101 0.02721 AFIX 23 H68A 2 0.772340 0.291206 0.625739 11.00000 -1.20000 H68B 2 0.817527 0.390542 0.641292 11.00000 -1.20000 AFIX 0 C69 1 0.882367 0.329944 0.564344 11.00000 0.04251 0.07262 = 0.04601 0.01983 0.01427 0.03147 AFIX 13 H69 2 0.947503 0.325965 0.600443 11.00000 -1.20000 AFIX 0 C70 1 0.842333 0.249211 0.505701 11.00000 0.06953 0.06325 = 0.05933 0.02021 0.03190 0.03701 AFIX 23 H70A 2 0.824056 0.200009 0.528081 11.00000 -1.20000 H70B 2 0.900053 0.242368 0.481589 11.00000 -1.20000 AFIX 0 C71 1 0.740837 0.255615 0.449672 11.00000 0.06299 0.05155 = 0.04192 0.00179 0.01990 0.01639 AFIX 13 H71 2 0.714249 0.203638 0.412020 11.00000 -1.20000 AFIX 0 C72 1 0.650100 0.266742 0.488330 11.00000 0.05036 0.04227 = 0.04736 0.00674 0.01450 0.01175 AFIX 23 H72A 2 0.629967 0.217477 0.510271 11.00000 -1.20000 H72B 2 0.585348 0.269925 0.452443 11.00000 -1.20000 AFIX 0 C73 1 0.720006 0.423687 0.510296 11.00000 0.03705 0.04328 = 0.04026 0.01265 0.00790 0.01462 AFIX 23 H73A 2 0.656021 0.427731 0.474183 11.00000 -1.20000 H73B 2 0.744793 0.476058 0.546496 11.00000 -1.20000 AFIX 0 C74 1 0.811698 0.413136 0.472687 11.00000 0.04926 0.05343 = 0.05053 0.02237 0.02252 0.01759 AFIX 13 H74 2 0.831104 0.462281 0.449592 11.00000 -1.20000 AFIX 0 C75 1 0.912577 0.407202 0.528894 11.00000 0.04062 0.06493 = 0.05663 0.01223 0.01865 0.01743 AFIX 23 H75A 2 0.938701 0.458652 0.566159 11.00000 -1.20000 H75B 2 0.971072 0.401521 0.505205 11.00000 -1.20000 AFIX 0 C76 1 0.771004 0.332039 0.414124 11.00000 0.05753 0.07061 = 0.04081 0.01389 0.01993 0.02265 AFIX 23 H76A 2 0.707096 0.335947 0.377869 11.00000 -1.20000 H76B 2 0.828208 0.325355 0.389474 11.00000 -1.20000 AFIX 0 C77 1 0.593121 0.457198 0.654445 11.00000 0.02979 0.03249 = 0.03952 0.00635 0.00314 0.00796 C78 1 0.713958 0.498147 0.697050 11.00000 0.03048 0.04509 = 0.04221 0.00346 0.00815 0.00816 AFIX 23 H78A 2 0.742416 0.458469 0.724772 11.00000 -1.20000 H78B 2 0.758288 0.510596 0.662726 11.00000 -1.20000 AFIX 0 C79 1 0.722471 0.580420 0.749411 11.00000 0.04089 0.04261 = 0.05643 -0.00454 0.00767 0.00437 AFIX 13 H79 2 0.799728 0.605071 0.775887 11.00000 -1.20000 AFIX 0 C80 1 0.654525 0.561169 0.804596 11.00000 0.05344 0.05198 = 0.05546 -0.00612 0.01257 0.01495 AFIX 23 H80A 2 0.661096 0.613056 0.838427 11.00000 -1.20000 H80B 2 0.681364 0.521102 0.832585 11.00000 -1.20000 AFIX 0 C81 1 0.534065 0.523341 0.762752 11.00000 0.04806 0.05123 = 0.06138 0.00158 0.02497 0.01595 AFIX 13 H81 2 0.489884 0.510794 0.797773 11.00000 -1.20000 AFIX 0 C82 1 0.524068 0.440716 0.710140 11.00000 0.03734 0.04265 = 0.05097 0.00662 0.01405 0.01070 AFIX 23 H82A 2 0.447447 0.416530 0.684190 11.00000 -1.20000 H82B 2 0.548930 0.399857 0.737996 11.00000 -1.20000 AFIX 0 C83 1 0.550778 0.523243 0.612296 11.00000 0.03967 0.04056 = 0.05942 0.01437 0.00660 0.01376 AFIX 23 H83A 2 0.593343 0.535908 0.577046 11.00000 -1.20000 H83B 2 0.474398 0.499546 0.585585 11.00000 -1.20000 AFIX 0 C84 1 0.560543 0.605771 0.665402 11.00000 0.05819 0.03807 = 0.07649 0.00882 0.00885 0.02212 AFIX 13 H84 2 0.533334 0.646457 0.637428 11.00000 -1.20000 AFIX 0 C85 1 0.680534 0.644044 0.706059 11.00000 0.05967 0.03700 = 0.07646 -0.00246 0.01546 0.00479 AFIX 23 H85A 2 0.687306 0.696587 0.739110 11.00000 -1.20000 H85B 2 0.724072 0.656906 0.671374 11.00000 -1.20000 AFIX 0 C86 1 0.491969 0.586683 0.719789 11.00000 0.05334 0.05143 = 0.08772 -0.00006 0.02268 0.02516 AFIX 23 H86A 2 0.497457 0.638758 0.753037 11.00000 -1.20000 H86B 2 0.415219 0.563148 0.693852 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5779_0m_a.res in P-1 REM R1 = 0.0655 for 8030 Fo > 4sig(Fo) and 0.1590 for all 16418 data REM 879 parameters refined using 14 restraints END WGHT 0.0755 0.0000 REM Highest difference peak 0.687, deepest hole -0.280, 1-sigma level 0.051 Q1 1 1.0242 0.9650 0.4670 11.00000 0.05 0.69 Q2 1 0.9550 0.0705 0.7337 11.00000 0.05 0.32 Q3 1 0.9649 0.9588 0.5572 11.00000 0.05 0.30 Q4 1 0.7246 0.2468 1.0451 11.00000 0.05 0.25 Q5 1 0.6609 0.3002 1.0328 11.00000 0.05 0.24 Q6 1 0.0807 0.2192 0.2791 11.00000 0.05 0.23 Q7 1 0.0417 0.0995 0.2911 11.00000 0.05 0.23 Q8 1 0.5146 0.3471 0.5200 11.00000 0.05 0.23 Q9 1 0.9012 0.1586 0.9662 11.00000 0.05 0.22 Q10 1 -0.0231 0.2084 0.3327 11.00000 0.05 0.21 Q11 1 0.3891 0.1979 0.5502 11.00000 0.05 0.21 Q12 1 0.7767 0.0569 1.0788 11.00000 0.05 0.21 Q13 1 0.4006 0.1385 0.6718 11.00000 0.05 0.21 Q14 1 0.8196 0.4637 1.0301 11.00000 0.05 0.20 Q15 1 0.5183 0.3010 0.5846 11.00000 0.05 0.20 Q16 1 0.7039 0.1590 1.0842 11.00000 0.05 0.19 Q17 1 0.6254 0.3570 0.5706 11.00000 0.05 0.19 Q18 1 0.7725 0.2062 1.1279 11.00000 0.05 0.19 Q19 1 0.7084 0.2935 0.9764 11.00000 0.05 0.18 Q20 1 0.6180 0.1561 1.2491 11.00000 0.05 0.18 ; _shelx_res_checksum 24608 _shelx_hkl_file ; -1 0 0 1307.07 25.90 1 0 0 1283.07 25.70 -2 0 0 400.86 11.00 -2 0 0 406.56 10.20 2 0 0 404.16 10.70 -3 0 0 2.80 3.70 -3 0 0 -1.10 4.60 3 0 0 2.30 4.20 -4 0 0 400.16 13.40 -4 0 0 403.66 12.40 4 0 0 400.36 12.50 -5 0 0 75.99 6.40 -5 0 0 66.29 7.00 5 0 0 69.49 6.60 -6 0 0 651.53 18.50 -6 0 0 647.34 20.00 6 0 0 659.23 18.80 -7 0 0 233.28 12.00 -7 0 0 269.87 14.40 7 0 0 223.58 12.20 -8 0 0 248.18 13.30 -8 0 0 261.97 15.30 8 0 0 257.67 14.30 -9 0 0 9.10 8.60 -9 0 0 2.20 7.00 9 0 0 -2.20 7.50 -10 0 0 67.29 11.20 -10 0 0 53.39 9.60 10 0 0 68.29 10.20 -11 0 0 140.19 12.60 -11 0 0 123.19 13.90 11 0 0 150.58 13.10 -12 0 0 52.39 10.80 -12 0 0 52.09 12.00 12 0 0 35.40 10.40 -13 0 0 82.19 12.30 -13 0 0 78.29 13.70 13 0 0 94.79 12.70 13 0 0 86.59 12.70 -14 0 0 -11.30 10.90 14 0 0 11.60 10.00 14 0 0 2.70 10.20 -15 0 0 13.90 12.30 15 0 0 8.50 10.50 15 0 0 13.00 11.30 15 -1 0 -8.10 10.20 15 -1 0 -16.40 10.30 -15 1 0 -10.30 11.50 14 -1 0 20.00 10.00 14 -1 0 4.20 10.20 -14 1 0 0.00 11.10 13 -1 0 3.70 9.00 13 -1 0 6.90 9.40 -13 1 0 -13.60 10.50 12 -1 0 -8.20 7.90 12 -1 0 -8.10 8.70 -12 1 0 10.80 10.30 11 -1 0 -0.20 8.10 11 -1 0 7.30 8.10 -11 1 0 10.30 9.70 -11 1 0 -4.10 8.00 10 -1 0 3.20 7.90 -10 1 0 3.00 7.60 -10 1 0 -12.00 8.50 9 -1 0 0.20 7.30 -9 1 0 2.20 8.20 -9 1 0 1.80 7.20 8 -1 0 10.70 6.50 -8 1 0 12.30 7.90 -8 1 0 -1.80 6.10 7 -1 0 101.19 8.30 -7 1 0 105.39 8.60 -7 1 0 94.59 9.40 6 -1 0 139.39 9.10 -6 1 0 130.39 9.00 -6 1 0 112.59 9.00 5 -1 0 75.89 6.30 -5 1 0 68.59 7.20 -5 1 0 61.19 6.10 4 -1 0 81.19 5.90 -4 1 0 75.69 4.30 -4 1 0 70.09 6.50 -4 1 0 74.19 5.80 3 -1 0 1347.87 26.90 -3 1 0 1233.18 27.00 -3 1 0 1230.08 27.80 -3 1 0 1208.18 25.30 2 -1 0 349.07 8.60 2 -1 0 295.97 8.60 -2 1 0 306.27 7.80 1 -1 0 599.54 13.20 1 -1 0 624.84 13.60 -1 1 0 686.33 13.60 -1 1 0 700.03 13.70 0 -1 0 623.84 13.50 0 1 0 717.53 13.80 -1 -1 0 3944.41 74.49 1 1 0 3755.92 74.09 1 1 0 3807.52 74.69 -2 -1 0 48.10 4.40 -2 -1 0 42.70 3.90 2 1 0 51.89 3.30 2 1 0 53.29 4.40 -3 -1 0 5.90 4.60 -3 -1 0 13.50 4.40 3 1 0 16.80 4.60 -4 -1 0 290.07 10.30 -4 -1 0 279.57 11.40 4 1 0 285.77 11.00 -5 -1 0 547.05 17.10 -5 -1 0 507.85 15.60 5 1 0 543.25 16.30 -6 -1 0 60.29 7.70 -6 -1 0 65.39 6.90 6 1 0 64.99 7.30 -7 -1 0 65.29 7.80 -7 -1 0 68.99 8.70 7 1 0 56.79 8.20 -8 -1 0 14.10 7.90 -8 -1 0 1.30 6.40 8 1 0 -6.10 6.80 -9 -1 0 -1.10 7.40 -9 -1 0 4.80 8.60 9 1 0 -2.70 7.40 -10 -1 0 18.90 8.30 -10 -1 0 -12.00 8.80 10 1 0 -6.90 8.30 -11 -1 0 -2.40 9.20 -11 -1 0 3.80 8.10 11 1 0 7.70 9.00 -12 -1 0 31.40 10.10 -12 -1 0 22.40 10.60 12 1 0 23.70 10.50 -13 -1 0 11.00 11.10 -13 -1 0 5.10 9.80 13 1 0 -4.60 9.90 -14 -1 0 54.59 12.30 -14 -1 0 57.79 13.20 14 1 0 32.80 11.60 -15 -1 0 -5.40 11.70 15 1 0 -1.40 10.60 15 1 0 -15.00 10.60 15 -2 0 5.80 10.70 15 -2 0 -13.70 9.50 -15 2 0 13.10 12.50 14 -2 0 2.20 9.60 14 -2 0 -1.20 9.50 -14 2 0 -7.10 11.40 13 -2 0 37.80 10.60 13 -2 0 34.70 10.60 -13 2 0 43.50 12.20 12 -2 0 38.30 9.70 12 -2 0 40.50 9.90 -12 2 0 47.70 11.90 11 -2 0 15.30 8.10 11 -2 0 11.30 8.40 -11 2 0 15.20 10.10 10 -2 0 188.78 14.80 10 -2 0 188.68 14.00 -10 2 0 202.08 15.50 9 -2 0 -9.30 6.40 9 -2 0 13.80 7.00 -9 2 0 2.90 7.90 8 -2 0 7.20 6.80 8 -2 0 -0.90 6.00 -8 2 0 5.10 7.10 7 -2 0 1.40 5.20 7 -2 0 1.80 5.40 -7 2 0 1.20 6.30 -7 2 0 3.10 2.90 6 -2 0 70.29 6.50 6 -2 0 76.49 7.10 -6 2 0 77.29 5.40 -6 2 0 73.79 7.80 5 -2 0 24.30 5.20 5 -2 0 28.20 4.80 -5 2 0 15.50 3.60 -5 2 0 5.70 5.20 4 -2 0 149.39 7.40 4 -2 0 126.39 7.90 -4 2 0 128.79 8.90 -4 2 0 111.79 6.80 3 -2 0 0.50 3.60 3 -2 0 4.20 4.00 -3 2 0 5.80 3.80 -3 2 0 3.20 4.10 2 -2 0 725.83 16.90 2 -2 0 691.53 15.90 -2 2 0 780.12 17.00 -2 2 0 783.92 16.90 1 -2 0 1479.75 29.10 1 -2 0 1448.66 29.80 -1 2 0 1490.65 29.50 -1 2 0 1459.05 30.20 0 -2 0 1998.40 38.90 0 -2 0 1983.70 39.50 0 -2 0 2029.00 39.90 0 2 0 1993.00 40.10 -1 -2 0 29.30 3.10 -1 -2 0 26.90 3.60 1 2 0 29.70 3.60 1 2 0 23.30 3.40 -2 -2 0 878.01 20.00 -2 -2 0 871.51 19.80 2 2 0 906.01 19.10 2 2 0 887.11 20.40 -3 -2 0 426.86 12.70 -3 -2 0 412.86 12.20 3 2 0 407.66 12.90 3 2 0 424.26 10.20 -4 -2 0 36.30 5.70 -4 -2 0 58.09 5.90 4 2 0 43.40 6.10 4 2 0 49.50 3.70 -5 -2 0 206.58 10.90 -5 -2 0 198.98 9.90 5 2 0 179.08 10.70 -6 -2 0 334.77 14.70 -6 -2 0 328.07 13.40 6 2 0 313.27 14.00 -7 -2 0 9.60 7.00 -7 -2 0 5.80 5.90 7 2 0 9.40 6.50 -8 -2 0 13.30 7.20 -8 -2 0 23.50 8.00 8 2 0 13.70 8.10 -9 -2 0 32.00 9.70 -9 -2 0 48.80 9.00 9 2 0 39.10 9.60 -10 -2 0 17.10 8.70 -10 -2 0 26.90 9.60 10 2 0 26.50 9.30 -11 -2 0 -8.10 8.80 -11 -2 0 9.60 8.60 11 2 0 3.80 9.50 -12 -2 0 118.89 13.50 -12 -2 0 116.59 14.10 12 2 0 116.89 13.50 -13 -2 0 55.09 12.90 -13 -2 0 64.99 12.10 13 2 0 35.60 11.60 -14 -2 0 45.60 12.00 -14 -2 0 30.40 12.70 14 2 0 23.10 12.10 -15 -2 0 1.00 12.20 -15 -2 0 -7.60 10.90 15 2 0 6.00 11.50 15 -3 0 5.10 10.60 15 -3 0 11.00 10.80 -15 3 0 10.90 12.80 14 -3 0 3.40 9.60 14 -3 0 10.10 9.60 -14 3 0 6.60 11.70 13 -3 0 19.00 9.30 13 -3 0 1.60 9.20 -13 3 0 8.00 11.10 12 -3 0 47.20 9.70 12 -3 0 39.50 10.10 -12 3 0 51.99 12.20 11 -3 0 99.29 11.50 11 -3 0 65.79 9.90 -11 3 0 68.39 12.00 10 -3 0 2.70 7.70 10 -3 0 1.00 7.20 -10 3 0 8.20 9.20 9 -3 0 415.56 16.70 9 -3 0 403.26 17.20 -9 3 0 441.96 19.60 8 -3 0 -2.50 6.40 8 -3 0 1.20 5.70 -8 3 0 -0.80 3.90 -8 3 0 5.70 7.50 7 -3 0 37.90 6.60 7 -3 0 28.20 5.80 -7 3 0 28.70 7.20 -7 3 0 31.20 4.50 6 -3 0 458.35 15.00 6 -3 0 450.95 14.00 -6 3 0 463.75 12.80 -6 3 0 438.66 15.90 5 -3 0 71.49 6.40 5 -3 0 75.59 5.80 -5 3 0 71.69 5.60 -5 3 0 90.39 7.60 4 -3 0 966.80 23.70 4 -3 0 984.30 22.50 -4 3 0 1005.10 24.40 -4 3 0 1079.59 23.10 3 -3 0 181.08 7.40 3 -3 0 207.38 9.20 -3 3 0 202.18 9.10 -3 3 0 220.08 9.20 2 -3 0 6266.87 123.69 2 -3 0 6278.37 124.79 -2 3 0 6849.42 124.69 -2 3 0 6221.58 125.09 1 -3 0 1050.49 23.40 1 -3 0 1134.69 22.40 -1 3 0 1071.49 22.40 0 -3 0 157.78 4.70 0 -3 0 144.09 5.80 0 -3 0 141.49 7.40 0 3 0 159.18 7.90 -1 -3 0 439.76 10.70 1 3 0 438.16 12.50 1 3 0 426.66 12.10 -2 -3 0 644.34 16.40 -2 -3 0 666.83 15.80 2 3 0 674.03 16.00 2 3 0 639.54 16.90 -3 -3 0 107.29 7.50 -3 -3 0 92.89 7.70 3 3 0 87.49 6.70 3 3 0 120.49 6.60 -4 -3 0 54.69 5.90 -4 -3 0 58.19 6.10 4 3 0 42.30 6.20 4 3 0 55.79 4.20 -5 -3 0 235.08 11.80 -5 -3 0 214.78 11.10 5 3 0 196.18 12.20 5 3 0 230.08 7.10 -6 -3 0 18.30 6.70 -6 -3 0 31.90 6.60 6 3 0 23.20 6.90 -7 -3 0 53.19 7.90 -7 -3 0 56.99 8.70 7 3 0 35.30 8.00 -8 -3 0 8.70 8.40 -8 -3 0 7.90 7.10 8 3 0 2.00 7.80 -9 -3 0 -6.60 7.60 -9 -3 0 -1.70 8.50 9 3 0 -2.10 8.40 -10 -3 0 8.40 7.90 -10 -3 0 23.40 9.50 10 3 0 6.40 9.20 -11 -3 0 4.20 9.60 -11 -3 0 -10.30 8.20 11 3 0 -6.50 8.90 -12 -3 0 20.20 11.10 -12 -3 0 26.70 10.10 12 3 0 44.00 11.50 -13 -3 0 28.80 11.40 -13 -3 0 5.50 10.30 13 3 0 8.90 11.60 -14 -3 0 4.80 11.50 -14 -3 0 9.80 10.30 14 3 0 2.80 11.70 16 -4 0 3.80 10.70 -16 4 0 -7.20 13.10 15 -4 0 31.50 11.60 -15 4 0 16.10 12.70 14 -4 0 6.50 9.50 14 -4 0 -5.00 9.30 -14 4 0 -1.10 11.80 13 -4 0 41.00 10.80 13 -4 0 22.80 9.40 -13 4 0 18.20 12.30 12 -4 0 0.20 8.00 12 -4 0 3.90 8.40 -12 4 0 -22.10 9.30 11 -4 0 54.39 9.20 11 -4 0 40.70 9.90 -11 4 0 63.89 11.60 10 -4 0 89.19 9.50 10 -4 0 73.59 10.30 -10 4 0 86.19 11.70 9 -4 0 33.10 7.40 9 -4 0 40.20 8.70 -9 4 0 46.70 9.40 8 -4 0 832.92 22.60 8 -4 0 841.72 24.40 -8 4 0 813.92 20.40 -8 4 0 825.62 25.80 7 -4 0 31.00 5.50 7 -4 0 30.50 6.70 -7 4 0 32.60 5.30 -7 4 0 24.30 7.00 6 -4 0 140.79 9.70 6 -4 0 143.89 8.30 -6 4 0 138.89 10.50 -6 4 0 148.59 9.10 5 -4 0 57.39 6.60 5 -4 0 64.89 5.50 -5 4 0 67.19 7.00 -5 4 0 60.99 6.30 4 -4 0 93.79 7.10 4 -4 0 99.29 6.60 -4 4 0 119.59 8.70 -4 4 0 113.29 8.50 3 -4 0 1340.87 30.00 3 -4 0 1327.17 28.20 -3 4 0 1314.97 30.30 -3 4 0 1433.66 29.80 2 -4 0 18.80 4.80 2 -4 0 22.20 3.50 -2 4 0 30.10 6.00 -2 4 0 26.20 4.10 1 -4 0 328.97 9.20 -1 4 0 352.26 12.20 -1 4 0 335.77 9.00 0 -4 0 115.09 4.80 0 -4 0 107.49 6.40 0 -4 0 104.79 8.00 0 4 0 111.59 8.80 -1 -4 0 567.04 13.00 -1 -4 0 534.75 14.70 1 4 0 540.25 14.80 1 4 0 549.15 15.50 -2 -4 0 47.80 4.50 -2 -4 0 45.90 5.60 2 4 0 38.20 5.30 2 4 0 36.10 5.40 -3 -4 0 54.09 5.30 -3 -4 0 48.20 5.50 3 4 0 67.89 5.50 3 4 0 53.49 6.10 -4 -4 0 79.09 7.20 -4 -4 0 99.09 8.20 4 4 0 89.49 7.60 4 4 0 95.19 7.00 -5 -4 0 30.00 6.20 -5 -4 0 22.70 6.00 5 4 0 33.40 7.10 5 4 0 33.30 4.30 -6 -4 0 42.60 7.30 -6 -4 0 26.10 6.90 6 4 0 31.90 7.90 6 4 0 39.80 3.80 -7 -4 0 4.70 6.90 -7 -4 0 -1.90 6.80 7 4 0 8.60 8.00 -8 -4 0 28.00 8.40 -8 -4 0 27.90 8.90 8 4 0 23.80 8.70 -9 -4 0 31.10 9.70 -9 -4 0 36.10 9.20 9 4 0 35.90 9.90 -10 -4 0 16.50 9.50 -10 -4 0 -0.70 8.60 10 4 0 -3.30 9.50 -11 -4 0 108.89 13.00 -11 -4 0 100.89 12.80 11 4 0 78.29 12.60 -12 -4 0 152.18 15.10 -12 -4 0 121.49 14.70 12 4 0 117.99 14.60 -13 -4 0 3.70 10.10 -13 -4 0 18.10 11.10 13 4 0 -5.90 11.00 -14 -4 0 0.10 11.00 -14 -4 0 11.30 12.10 14 4 0 11.60 12.90 16 -5 0 5.70 10.60 -16 5 0 22.20 14.20 15 -5 0 102.79 14.50 -15 5 0 107.69 16.40 14 -5 0 72.39 12.70 -14 5 0 99.29 15.10 13 -5 0 53.69 10.30 13 -5 0 69.99 12.10 -13 5 0 68.09 13.80 12 -5 0 90.29 12.20 12 -5 0 91.79 10.70 -12 5 0 94.29 13.90 11 -5 0 21.10 8.10 11 -5 0 24.40 9.20 -11 5 0 30.30 11.00 10 -5 0 4.20 6.80 10 -5 0 -6.90 7.40 -10 5 0 14.00 9.60 9 -5 0 28.20 7.00 9 -5 0 3.00 7.70 -9 5 0 24.30 9.20 8 -5 0 150.18 11.70 8 -5 0 138.89 9.90 -8 5 0 126.19 11.20 -8 5 0 142.89 9.90 7 -5 0 92.09 7.30 7 -5 0 100.19 8.80 -7 5 0 85.89 8.80 -7 5 0 99.19 7.70 6 -5 0 71.69 7.60 6 -5 0 65.09 5.90 -6 5 0 76.29 7.20 -6 5 0 70.69 8.00 5 -5 0 69.29 5.50 5 -5 0 58.09 6.70 -5 5 0 55.29 6.60 -5 5 0 52.19 6.80 4 -5 0 1348.27 31.40 4 -5 0 1378.86 29.30 -4 5 0 1339.77 31.60 -4 5 0 1407.46 31.00 3 -5 0 107.29 8.10 3 -5 0 118.59 6.10 -3 5 0 113.99 9.40 -3 5 0 110.39 7.30 2 -5 0 1230.68 28.50 2 -5 0 1301.37 27.00 -2 5 0 1274.37 27.30 -2 5 0 1312.57 30.00 1 -5 0 11.60 3.70 1 -5 0 21.00 5.30 -1 5 0 17.80 3.20 -1 5 0 25.80 6.10 0 -5 0 286.07 9.60 0 -5 0 272.97 10.80 0 -5 0 283.47 7.80 0 5 0 260.67 12.30 -1 -5 0 18.30 4.90 -1 -5 0 17.00 3.30 1 5 0 18.30 5.60 1 5 0 20.90 4.80 -2 -5 0 8.20 3.80 -2 -5 0 10.30 4.80 2 5 0 20.10 5.40 2 5 0 2.20 5.20 -3 -5 0 110.99 7.50 -3 -5 0 122.39 8.70 3 5 0 125.59 8.70 3 5 0 120.29 8.70 -4 -5 0 216.98 11.10 -4 -5 0 212.08 10.50 4 5 0 219.18 11.90 4 5 0 228.58 10.00 -5 -5 0 51.59 7.40 -5 -5 0 45.90 6.70 5 5 0 60.59 8.30 5 5 0 62.09 5.60 -6 -5 0 77.69 8.70 -6 -5 0 78.79 8.60 6 5 0 87.19 6.70 6 5 0 64.99 9.10 -7 -5 0 126.59 10.70 -7 -5 0 101.79 10.20 7 5 0 125.09 11.70 -8 -5 0 195.88 15.40 -8 -5 0 179.08 13.10 8 5 0 181.68 14.20 -9 -5 0 99.59 11.40 -9 -5 0 99.39 11.60 9 5 0 83.49 11.50 -10 -5 0 31.60 9.70 -10 -5 0 47.10 10.40 10 5 0 16.10 10.20 -11 -5 0 9.10 9.40 -11 -5 0 14.80 9.80 11 5 0 -1.90 10.40 -12 -5 0 56.09 12.30 -12 -5 0 33.30 10.80 12 5 0 58.69 12.80 -13 -5 0 18.20 11.70 -13 -5 0 8.20 11.00 13 5 0 11.90 12.20 -14 -5 0 27.20 12.50 -14 -5 0 18.80 12.10 14 5 0 3.20 13.10 16 -6 0 14.80 12.00 -16 6 0 0.40 14.00 15 -6 0 7.80 10.50 -15 6 0 10.20 12.70 14 -6 0 28.30 10.80 -14 6 0 37.50 13.30 13 -6 0 46.80 10.90 -13 6 0 43.90 12.30 12 -6 0 67.89 10.00 12 -6 0 53.29 10.70 -12 6 0 57.69 12.30 11 -6 0 21.50 8.90 11 -6 0 14.70 7.90 -11 6 0 11.50 10.20 10 -6 0 187.68 13.10 10 -6 0 187.08 14.60 -10 6 0 206.48 15.50 9 -6 0 274.87 13.30 9 -6 0 243.68 16.00 -9 6 0 298.47 17.30 -9 6 0 270.27 13.50 8 -6 0 74.29 9.20 8 -6 0 78.19 7.50 -8 6 0 77.59 10.00 -8 6 0 69.19 8.00 7 -6 0 14.90 6.60 7 -6 0 22.20 5.40 -7 6 0 11.10 6.70 -7 6 0 16.50 6.50 6 -6 0 138.39 8.30 6 -6 0 141.59 10.90 -6 6 0 122.59 10.20 -6 6 0 142.39 10.80 5 -6 0 183.38 10.70 5 -6 0 195.18 8.40 -5 6 0 203.18 10.70 -5 6 0 190.58 12.10 4 -6 0 4.70 5.20 4 -6 0 16.70 3.80 -4 6 0 15.80 4.80 -4 6 0 16.40 6.30 3 -6 0 165.68 9.90 3 -6 0 156.08 6.80 -3 6 0 190.08 11.10 -3 6 0 173.38 8.20 2 -6 0 169.28 7.20 2 -6 0 171.18 9.50 -2 6 0 176.58 7.20 -2 6 0 161.98 11.00 1 -6 0 169.18 9.40 1 -6 0 172.48 7.50 -1 6 0 152.18 10.60 -1 6 0 172.68 6.40 0 -6 0 9.70 5.40 0 -6 0 8.80 2.90 0 -6 0 12.30 4.10 0 6 0 8.80 5.90 -1 -6 0 23.50 3.50 -1 -6 0 23.40 5.70 1 6 0 22.90 5.20 1 6 0 24.40 6.30 -2 -6 0 91.29 6.50 -2 -6 0 107.89 7.80 2 6 0 95.79 7.90 2 6 0 78.59 7.20 -3 -6 0 658.23 18.90 -3 -6 0 623.24 16.70 3 6 0 634.04 18.20 3 6 0 652.53 19.30 -4 -6 0 166.58 11.40 -4 -6 0 187.18 9.90 4 6 0 180.98 10.30 4 6 0 199.78 12.10 -5 -6 0 -12.70 6.10 -5 -6 0 5.30 5.60 5 6 0 1.90 6.70 5 6 0 7.10 5.10 -6 -6 0 77.49 8.70 -6 -6 0 74.79 9.10 6 6 0 54.19 9.70 -7 -6 0 5.70 7.40 -7 -6 0 7.80 8.00 7 6 0 11.50 8.60 -8 -6 0 120.79 11.60 -8 -6 0 119.29 11.70 8 6 0 143.69 13.80 -9 -6 0 28.70 9.40 -9 -6 0 22.40 8.90 9 6 0 25.60 10.20 -10 -6 0 -7.10 8.70 -10 -6 0 2.10 9.30 10 6 0 6.90 10.30 -11 -6 0 13.80 9.90 -11 -6 0 5.90 9.80 11 6 0 -10.70 10.70 -12 -6 0 5.00 10.70 -12 -6 0 5.40 10.10 12 6 0 -3.70 11.10 -13 -6 0 0.50 10.50 13 6 0 13.00 13.00 15 -7 0 122.29 15.60 -15 7 0 132.49 18.20 14 -7 0 1.80 10.30 -14 7 0 -3.00 11.80 13 -7 0 62.39 12.10 -13 7 0 92.19 14.30 12 -7 0 49.90 11.20 -12 7 0 68.29 13.10 11 -7 0 16.60 9.00 11 -7 0 2.30 8.00 -11 7 0 0.60 9.40 10 -7 0 0.90 8.10 10 -7 0 5.10 7.00 -10 7 0 -6.70 8.80 9 -7 0 578.44 18.80 9 -7 0 538.35 21.20 -9 7 0 566.74 22.20 -9 7 0 569.54 19.50 8 -7 0 46.80 7.00 8 -7 0 39.70 8.30 -8 7 0 35.90 8.10 -8 7 0 46.00 8.80 7 -7 0 -6.90 4.70 7 -7 0 -1.40 6.50 -7 7 0 3.90 6.50 -7 7 0 7.10 7.00 6 -7 0 144.09 11.00 6 -7 0 135.19 8.10 -6 7 0 141.79 10.50 -6 7 0 148.39 11.20 5 -7 0 171.08 8.10 5 -7 0 178.68 10.80 -5 7 0 179.38 10.30 -5 7 0 188.88 12.90 4 -7 0 96.99 8.00 4 -7 0 78.09 6.30 -4 7 0 94.79 9.20 -4 7 0 83.99 6.40 3 -7 0 89.29 7.80 3 -7 0 91.69 6.20 -3 7 0 74.49 8.20 -3 7 0 75.49 5.70 2 -7 0 72.29 5.20 2 -7 0 72.59 7.20 -2 7 0 64.09 4.70 -2 7 0 80.69 8.40 1 -7 0 203.98 8.60 1 -7 0 188.18 10.40 -1 7 0 186.08 12.10 0 -7 0 104.99 5.60 0 -7 0 83.69 6.30 0 -7 0 88.39 7.40 0 7 0 108.99 9.10 -1 -7 0 349.77 9.90 -1 -7 0 330.57 13.20 1 7 0 331.37 12.80 1 7 0 346.47 14.10 -2 -7 0 20.00 4.20 -2 -7 0 5.00 5.20 2 7 0 17.50 6.50 2 7 0 11.20 5.70 -3 -7 0 11.90 6.00 -3 -7 0 15.50 4.50 3 7 0 6.30 6.20 3 7 0 2.80 6.00 -4 -7 0 31.80 7.30 -4 -7 0 36.40 5.60 4 7 0 27.20 7.70 4 7 0 16.40 6.30 -5 -7 0 6.80 7.00 -5 -7 0 1.80 5.60 5 7 0 -3.40 7.30 5 7 0 3.60 5.80 -6 -7 0 52.19 9.20 -6 -7 0 72.79 8.60 6 7 0 53.69 9.80 -7 -7 0 52.59 9.00 -7 -7 0 43.20 9.60 7 7 0 21.70 10.10 -8 -7 0 396.56 19.10 -8 -7 0 413.46 18.80 8 7 0 383.46 20.40 -9 -7 0 130.99 13.30 -9 -7 0 142.39 12.90 9 7 0 130.69 14.50 -10 -7 0 7.00 9.60 -10 -7 0 10.30 10.50 10 7 0 7.20 10.30 -11 -7 0 21.30 10.80 11 7 0 -36.90 9.80 -12 -7 0 20.00 11.30 12 7 0 38.60 13.10 -13 -7 0 -4.40 11.30 13 7 0 -3.50 12.20 15 -8 0 5.00 11.40 -15 8 0 14.60 13.90 14 -8 0 2.90 10.10 -14 8 0 -5.70 12.50 13 -8 0 -2.90 9.70 -13 8 0 7.90 11.60 12 -8 0 51.09 11.20 -12 8 0 49.99 12.00 11 -8 0 53.29 10.40 -11 8 0 58.59 11.80 10 -8 0 69.09 10.60 -10 8 0 72.09 11.40 9 -8 0 314.47 14.10 9 -8 0 292.47 16.80 -9 8 0 323.97 18.70 -9 8 0 327.67 16.20 8 -8 0 39.40 6.40 8 -8 0 22.60 8.70 -8 8 0 38.00 8.70 -8 8 0 45.80 9.00 7 -8 0 -8.80 6.60 7 -8 0 -7.00 4.50 -7 8 0 4.80 6.70 -7 8 0 -6.10 7.40 6 -8 0 190.98 9.30 6 -8 0 168.78 11.80 -6 8 0 193.88 13.50 -6 8 0 221.58 12.00 5 -8 0 334.27 11.10 5 -8 0 334.87 14.20 -5 8 0 319.77 13.00 -5 8 0 353.16 16.60 4 -8 0 19.10 6.30 4 -8 0 9.40 3.90 -4 8 0 8.30 4.40 -4 8 0 -0.20 6.80 3 -8 0 268.97 9.60 3 -8 0 272.07 12.50 -3 8 0 269.47 10.00 -3 8 0 265.27 14.60 2 -8 0 551.04 14.80 2 -8 0 548.15 17.10 -2 8 0 540.35 19.10 -2 8 0 525.05 13.80 1 -8 0 13.50 4.60 1 -8 0 16.90 3.50 1 -8 0 11.90 6.20 -1 8 0 5.40 7.30 0 -8 0 11.90 6.00 0 -8 0 7.80 3.30 0 -8 0 13.70 5.10 0 8 0 2.20 6.70 -1 -8 0 24.80 3.90 -1 -8 0 23.90 6.60 1 8 0 22.70 5.80 1 8 0 24.70 7.40 -2 -8 0 141.29 10.70 -2 -8 0 162.38 7.90 2 8 0 163.68 11.50 2 8 0 147.49 12.20 -3 -8 0 35.80 5.30 -3 -8 0 33.40 7.30 3 8 0 38.00 7.50 3 8 0 30.30 7.50 -4 -8 0 4.90 5.10 -4 -8 0 -2.60 6.70 4 8 0 -2.80 6.90 4 8 0 4.50 6.60 -5 -8 0 80.09 8.10 -5 -8 0 92.29 10.20 5 8 0 72.39 8.50 5 8 0 83.19 10.50 -6 -8 0 29.00 8.90 -6 -8 0 29.50 7.60 6 8 0 24.50 9.40 -7 -8 0 13.30 8.60 -7 -8 0 3.50 7.40 7 8 0 15.50 9.40 -8 -8 0 1.00 8.70 8 8 0 5.40 10.10 -9 -8 0 7.20 9.40 9 8 0 2.20 10.20 -10 -8 0 33.40 11.10 10 8 0 30.90 11.50 -11 -8 0 7.80 10.40 11 8 0 5.70 11.80 -12 -8 0 -4.30 10.60 12 8 0 -3.90 12.50 15 -9 0 -3.80 11.10 -15 9 0 7.50 13.20 14 -9 0 -0.70 10.60 -14 9 0 28.70 13.40 13 -9 0 12.60 10.30 -13 9 0 34.40 12.20 12 -9 0 39.30 10.80 -12 9 0 0.70 10.90 11 -9 0 13.70 9.40 -11 9 0 1.60 9.90 10 -9 0 452.45 20.60 -10 9 0 438.46 21.50 9 -9 0 78.39 10.80 -9 9 0 82.29 10.80 -9 9 0 97.99 11.70 8 -9 0 1.50 5.40 8 -9 0 7.60 8.00 -8 9 0 2.90 7.30 -8 9 0 -2.10 8.20 7 -9 0 52.09 6.50 7 -9 0 58.19 9.30 -7 9 0 67.49 10.00 -7 9 0 64.39 8.60 6 -9 0 162.48 11.60 6 -9 0 123.09 8.30 -6 9 0 127.69 10.70 -6 9 0 125.19 11.50 5 -9 0 200.48 12.70 5 -9 0 212.58 9.00 -5 9 0 203.88 11.10 -5 9 0 183.38 14.30 4 -9 0 36.20 7.40 4 -9 0 40.30 4.90 -4 9 0 41.30 8.90 -4 9 0 48.40 5.90 3 -9 0 119.89 9.20 3 -9 0 115.99 7.40 -3 9 0 128.59 7.60 -3 9 0 124.89 11.20 2 -9 0 94.49 9.10 2 -9 0 79.89 6.30 -2 9 0 72.39 10.00 -2 9 0 92.79 6.30 1 -9 0 2.50 3.30 1 -9 0 3.90 4.50 1 -9 0 1.30 6.60 -1 9 0 4.70 7.40 0 -9 0 13.60 6.50 0 -9 0 7.90 5.20 0 -9 0 20.40 3.70 0 9 0 24.30 7.80 0 9 0 14.40 5.70 -1 -9 0 50.29 7.70 -1 -9 0 43.00 4.60 1 9 0 36.00 8.30 1 9 0 37.80 6.80 -2 -9 0 15.10 4.40 -2 -9 0 16.40 6.70 2 9 0 9.00 6.60 2 9 0 26.70 7.90 -3 -9 0 534.15 15.00 -3 -9 0 520.85 19.00 3 9 0 528.75 19.60 3 9 0 491.15 18.90 -4 -9 0 218.58 12.90 -4 -9 0 215.78 14.00 4 9 0 227.28 14.60 4 9 0 226.78 14.90 -5 -9 0 137.69 12.40 5 9 0 129.39 12.40 5 9 0 166.18 13.40 -6 -9 0 43.40 10.00 6 9 0 22.20 9.90 -7 -9 0 4.10 8.30 7 9 0 3.10 9.80 -8 -9 0 10.80 9.30 8 9 0 -13.00 9.70 -9 -9 0 26.00 11.20 9 9 0 17.00 11.80 -10 -9 0 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7 10 -3 28.10 10.60 -7 -10 3 24.70 9.30 6 10 -3 40.60 10.00 -6 -10 3 18.20 9.50 -6 -10 3 21.30 8.80 5 10 -3 526.85 21.40 5 10 -3 546.25 20.50 -5 -10 3 535.15 19.70 -5 -10 3 534.15 20.60 4 10 -3 28.40 8.80 4 10 -3 20.40 8.60 -4 -10 3 28.50 7.40 -4 -10 3 40.80 8.90 3 10 -3 19.80 8.40 3 10 -3 10.00 7.30 -3 -10 3 7.40 7.10 -3 -10 3 7.90 6.20 2 10 -3 95.89 8.90 2 10 -3 99.39 10.30 -2 -10 3 79.79 9.30 -2 -10 3 81.89 7.60 1 10 -3 169.38 10.70 1 10 -3 177.98 13.70 -1 -10 3 193.48 10.50 -1 -10 3 187.78 12.60 0 10 -3 26.20 8.10 0 10 -3 27.60 5.50 0 -10 3 34.30 7.90 0 -10 3 34.40 5.60 -1 10 -3 100.89 10.40 -1 10 -3 101.59 7.80 1 -10 3 116.29 8.60 1 -10 3 107.79 9.60 -2 10 -3 708.63 17.60 -2 10 -3 696.93 23.20 -2 10 -3 720.23 19.50 2 -10 3 674.83 21.50 -3 10 -3 42.00 6.20 -3 10 -3 20.50 8.10 3 -10 3 43.20 4.20 3 -10 3 43.00 8.10 -4 10 -3 1.00 7.50 -4 10 -3 7.70 5.60 4 -10 3 4.00 6.80 -5 10 -3 10.70 8.20 -5 10 -3 5.00 5.90 5 -10 3 7.80 7.20 -6 10 -3 468.65 18.50 -6 10 -3 446.76 20.10 6 -10 3 505.45 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11.70 2 9 -3 255.37 14.30 -2 -9 3 214.48 11.00 1 9 -3 295.57 14.70 1 9 -3 304.37 12.20 -1 -9 3 303.37 11.90 -1 -9 3 303.17 13.80 0 9 -3 362.26 12.30 0 9 -3 362.56 16.10 0 -9 3 347.57 15.30 0 -9 3 360.56 12.60 -1 9 -3 123.69 10.10 -1 9 -3 115.59 7.40 1 -9 3 131.99 8.80 1 -9 3 134.59 9.60 -2 9 -3 75.09 9.00 -2 9 -3 64.29 6.50 -2 9 -3 72.79 5.00 2 -9 3 69.29 8.00 -3 9 -3 56.49 6.60 -3 9 -3 64.39 8.80 3 -9 3 58.39 8.00 3 -9 3 63.39 4.10 -4 9 -3 48.10 6.70 -4 9 -3 54.89 8.30 4 -9 3 66.29 8.40 4 -9 3 59.99 3.90 -5 9 -3 38.60 6.70 -5 9 -3 36.00 8.30 5 -9 3 33.80 7.70 -6 9 -3 7.30 6.90 -6 9 -3 34.60 8.70 6 -9 3 30.20 7.70 -7 9 -3 219.78 14.30 -7 9 -3 218.38 15.10 7 -9 3 232.18 15.00 -8 9 -3 37.30 8.90 -8 9 -3 42.50 9.50 8 -9 3 52.89 10.10 -9 9 -3 94.09 11.60 -9 9 -3 114.49 10.90 9 -9 3 102.29 11.90 -10 9 -3 140.59 14.00 10 -9 3 152.88 14.30 -11 9 -3 154.68 15.40 11 -9 3 128.89 13.60 -12 9 -3 80.79 14.60 12 -9 3 79.29 13.20 -13 9 -3 64.49 15.20 13 -9 3 33.70 12.20 -14 9 -3 49.90 16.50 14 -9 3 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139.89 11.20 -6 5 -3 138.49 9.30 6 -5 3 147.69 10.70 6 -5 3 137.59 7.40 -7 5 -3 149.69 12.30 -7 5 -3 157.98 9.60 7 -5 3 158.68 12.00 7 -5 3 163.08 8.90 -8 5 -3 72.49 7.00 -8 5 -3 59.69 9.90 8 -5 3 62.09 9.00 8 -5 3 62.49 6.90 -9 5 -3 200.58 16.50 9 -5 3 227.28 15.80 9 -5 3 198.78 11.70 -10 5 -3 216.28 17.60 10 -5 3 206.08 12.90 10 -5 3 197.88 15.40 -11 5 -3 -4.70 9.30 11 -5 3 -2.70 8.80 -12 5 -3 12.70 10.80 12 -5 3 2.50 9.80 -13 5 -3 25.70 11.70 13 -5 3 24.10 11.00 -14 5 -3 -2.50 11.30 14 -5 3 6.30 10.40 -15 5 -3 7.80 12.50 15 -5 3 17.00 11.70 14 4 -3 10.90 12.40 -14 -4 3 0.20 11.30 -14 -4 3 4.30 10.70 13 4 -3 22.40 11.70 -13 -4 3 5.60 9.90 -13 -4 3 19.60 11.50 12 4 -3 2.50 10.90 -12 -4 3 7.50 9.40 -12 -4 3 2.10 10.60 11 4 -3 69.29 12.00 -11 -4 3 61.49 12.20 -11 -4 3 57.49 10.50 10 4 -3 -10.00 9.00 -10 -4 3 -4.20 7.60 -10 -4 3 14.90 9.70 9 4 -3 128.19 12.50 -9 -4 3 117.49 10.80 -9 -4 3 101.89 11.90 8 4 -3 110.99 11.20 -8 -4 3 108.49 9.50 -8 -4 3 116.09 11.40 7 4 -3 3.20 7.10 -7 -4 3 7.50 7.10 -7 -4 3 2.40 6.00 6 4 -3 36.30 4.40 6 4 -3 33.10 8.00 -6 -4 3 34.50 7.30 -6 -4 3 55.09 6.80 5 4 -3 315.07 10.30 5 4 -3 322.97 13.70 -5 -4 3 308.17 13.80 -5 -4 3 319.87 12.10 4 4 -3 344.87 12.80 4 4 -3 323.77 10.70 -4 -4 3 322.57 13.10 -4 -4 3 334.27 11.70 3 4 -3 64.59 5.60 3 4 -3 63.49 6.30 -3 -4 3 65.59 6.40 -3 -4 3 69.49 5.60 2 4 -3 4.40 4.60 2 4 -3 6.00 4.50 -2 -4 3 9.60 4.70 -2 -4 3 4.20 4.30 1 4 -3 8.10 5.00 1 4 -3 15.80 4.00 -1 -4 3 7.20 4.60 -1 -4 3 14.50 4.60 0 4 -3 -5.50 4.90 0 4 -3 12.50 3.10 0 -4 3 7.10 4.30 0 -4 3 14.50 4.70 -1 4 -3 268.87 9.90 -1 4 -3 236.78 10.60 1 -4 3 267.57 9.60 -2 4 -3 9.60 4.40 -2 4 -3 6.70 5.10 2 -4 3 -0.30 4.40 -3 4 -3 506.45 14.60 -3 4 -3 503.25 15.20 3 -4 3 497.35 15.10 3 -4 3 516.25 11.20 -4 4 -3 114.49 8.00 -4 4 -3 113.59 8.90 4 -4 3 111.19 8.60 4 -4 3 122.29 5.30 -5 4 -3 41.70 5.70 -5 4 -3 38.40 6.60 5 -4 3 44.10 4.30 5 -4 3 32.30 6.00 -6 4 -3 242.98 13.70 -6 4 -3 237.38 10.10 6 -4 3 249.88 9.50 6 -4 3 229.68 12.20 -7 4 -3 -14.90 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23.60 6.70 6 3 -3 44.10 4.00 -6 -3 3 33.00 7.30 -6 -3 3 40.20 6.10 5 3 -3 763.62 21.00 5 3 -3 730.33 17.10 -5 -3 3 727.23 18.90 -5 -3 3 718.33 20.80 4 3 -3 40.30 4.30 4 3 -3 35.10 6.00 -4 -3 3 45.30 5.10 -4 -3 3 33.40 6.10 3 3 -3 1874.81 38.90 3 3 -3 1921.41 40.30 -3 -3 3 1889.11 39.00 -3 -3 3 1813.12 40.30 2 3 -3 24.00 4.70 2 3 -3 23.60 4.70 -2 -3 3 25.10 4.10 -2 -3 3 20.80 4.90 1 3 -3 846.52 19.00 1 3 -3 853.41 20.00 -1 -3 3 827.92 19.90 -1 -3 3 859.01 19.10 0 3 -3 23.10 2.90 0 3 -3 23.20 5.00 0 -3 3 33.20 4.60 0 -3 3 30.70 4.10 -1 3 -3 959.50 22.20 -1 3 -3 974.00 22.70 1 -3 3 1002.80 21.90 -2 3 -3 244.68 10.10 -2 3 -3 235.88 10.20 2 -3 3 254.27 9.70 2 -3 3 239.28 5.90 -3 3 -3 527.65 14.50 -3 3 -3 530.95 15.70 3 -3 3 537.25 15.10 3 -3 3 532.15 12.30 -4 3 -3 98.89 7.10 -4 3 -3 65.19 6.60 4 -3 3 86.09 5.60 4 -3 3 70.29 6.50 -5 3 -3 2160.98 48.00 -5 3 -3 2143.19 45.00 5 -3 3 2175.58 47.50 5 -3 3 2192.68 45.00 -6 3 -3 -2.60 6.20 -6 3 -3 13.20 4.10 6 -3 3 13.70 4.60 6 -3 3 9.60 5.60 -7 3 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33.30 11.00 -9 15 -4 51.99 11.60 -9 15 -4 41.10 12.20 9 -15 4 55.59 12.00 -10 15 -4 29.30 11.20 -10 15 -4 38.60 11.60 10 -15 4 7.80 10.50 -11 15 -4 -0.60 10.90 11 -15 4 -5.90 10.20 -12 15 -4 10.60 11.90 12 -15 4 -3.40 10.80 9 14 -4 14.50 12.40 -9 -14 4 15.20 11.50 8 14 -4 -16.40 10.60 -8 -14 4 0.20 10.90 7 14 -4 -5.30 10.80 -7 -14 4 10.30 10.40 6 14 -4 15.20 10.50 -6 -14 4 10.10 10.50 5 14 -4 -2.60 9.40 -5 -14 4 16.10 9.70 4 14 -4 47.80 10.90 4 14 -4 75.69 12.70 -4 -14 4 51.09 11.00 3 14 -4 24.00 9.60 3 14 -4 58.49 12.40 -3 -14 4 38.00 9.70 2 14 -4 -14.50 10.20 2 14 -4 -0.70 8.00 -2 -14 4 -7.00 8.20 1 14 -4 1.60 10.80 1 14 -4 17.90 8.60 -1 -14 4 6.50 8.40 0 14 -4 0.40 10.20 0 -14 4 -1.00 8.80 -1 14 -4 5.20 9.90 1 -14 4 5.10 9.30 -2 14 -4 257.27 19.00 2 -14 4 264.97 17.20 -3 14 -4 2.50 9.90 3 -14 4 -1.50 9.30 -4 14 -4 -1.00 9.40 -4 14 -4 3.40 8.60 4 -14 4 -9.90 8.40 -5 14 -4 8.40 7.30 -5 14 -4 11.60 10.00 5 -14 4 4.60 9.20 -6 14 -4 27.20 8.50 -6 14 -4 46.50 11.20 6 -14 4 17.10 10.10 -7 14 -4 31.50 10.80 -7 14 -4 20.20 8.60 7 -14 4 5.90 9.20 -8 14 -4 0.50 8.80 -8 14 -4 -1.60 9.80 8 -14 4 -9.50 9.20 -9 14 -4 121.59 13.90 -9 14 -4 117.89 13.50 9 -14 4 123.39 14.70 -10 14 -4 2.00 10.10 -10 14 -4 27.50 11.20 10 -14 4 7.40 10.20 -11 14 -4 -3.20 10.50 11 -14 4 -1.80 9.70 -12 14 -4 29.30 12.30 12 -14 4 3.40 10.40 -13 14 -4 -3.70 12.90 13 -14 4 -4.20 10.70 10 13 -4 28.70 13.20 -10 -13 4 3.40 11.90 9 13 -4 -17.30 11.00 -9 -13 4 2.80 10.40 8 13 -4 27.90 11.80 -8 -13 4 36.20 11.50 7 13 -4 19.50 10.90 -7 -13 4 24.80 10.90 6 13 -4 -3.50 9.40 -6 -13 4 -7.60 8.70 5 13 -4 12.20 10.80 5 13 -4 5.80 9.70 -5 -13 4 9.60 9.40 4 13 -4 0.80 8.50 4 13 -4 0.80 9.40 -4 -13 4 12.20 9.00 3 13 -4 38.60 11.10 3 13 -4 37.40 9.50 -3 -13 4 46.30 9.60 2 13 -4 36.80 8.90 2 13 -4 51.19 11.30 -2 -13 4 55.39 10.20 1 13 -4 9.00 10.10 1 13 -4 14.30 7.50 -1 -13 4 6.50 8.20 0 13 -4 48.40 8.00 0 13 -4 43.70 11.10 0 -13 4 24.50 9.00 -1 13 -4 121.89 13.30 1 -13 4 126.69 12.20 -2 13 -4 39.60 10.80 2 -13 4 48.50 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6.70 1 -10 5 2.70 5.60 -2 10 -5 292.27 15.90 -2 10 -5 265.67 13.00 -2 10 -5 285.67 12.40 2 -10 5 280.67 14.40 -3 10 -5 72.79 9.80 -3 10 -5 80.19 8.50 3 -10 5 81.59 9.30 -4 10 -5 6.80 6.40 -4 10 -5 -1.50 7.80 4 -10 5 9.80 7.50 -5 10 -5 4.10 8.20 -5 10 -5 -0.50 6.80 5 -10 5 2.80 7.50 -6 10 -5 136.09 11.20 -6 10 -5 141.89 12.30 6 -10 5 130.59 11.80 -7 10 -5 186.38 13.70 -7 10 -5 232.18 16.00 7 -10 5 207.38 15.20 -8 10 -5 24.10 9.40 -8 10 -5 15.70 8.70 8 -10 5 18.20 9.10 -9 10 -5 13.90 9.90 -9 10 -5 11.20 8.30 9 -10 5 12.70 9.60 -10 10 -5 24.00 11.30 10 -10 5 -7.40 9.00 -11 10 -5 13.50 12.10 11 -10 5 4.10 9.80 -12 10 -5 21.30 13.90 12 -10 5 35.70 11.80 -13 10 -5 21.20 14.90 13 -10 5 12.60 11.60 -14 10 -5 1.80 15.50 14 -10 5 0.50 11.60 12 9 -5 -5.10 11.80 -12 -9 5 13.50 10.50 11 9 -5 -0.10 10.80 -11 -9 5 12.80 9.80 -11 -9 5 -5.20 12.60 10 9 -5 4.50 11.10 -10 -9 5 7.50 9.50 -10 -9 5 26.90 10.70 9 9 -5 0.90 10.30 -9 -9 5 1.90 9.00 -9 -9 5 8.00 9.70 8 9 -5 81.79 12.30 -8 -9 5 77.29 11.50 -8 -9 5 90.79 11.30 7 9 -5 -10.20 8.40 -7 -9 5 0.40 7.70 -7 -9 5 -2.30 8.70 6 9 -5 78.09 11.20 6 9 -5 93.79 9.80 -6 -9 5 70.69 10.00 -6 -9 5 82.79 10.50 5 9 -5 66.79 8.80 5 9 -5 47.60 9.00 -5 -9 5 46.40 9.00 -5 -9 5 62.49 9.00 4 9 -5 91.09 9.70 4 9 -5 89.49 9.80 -4 -9 5 92.39 9.40 -4 -9 5 103.09 9.90 3 9 -5 9.00 6.20 3 9 -5 11.80 7.30 -3 -9 5 6.80 6.20 -3 -9 5 14.20 6.80 2 9 -5 13.90 5.90 2 9 -5 9.90 7.00 -2 -9 5 11.10 6.50 -2 -9 5 5.30 5.80 1 9 -5 404.76 13.50 1 9 -5 396.46 16.80 -1 -9 5 398.96 15.00 -1 -9 5 399.86 15.50 0 9 -5 10.20 7.00 0 9 -5 9.00 4.40 0 -9 5 14.90 6.80 0 -9 5 7.30 5.30 -1 9 -5 145.49 12.50 -1 9 -5 158.48 7.40 1 -9 5 135.09 10.10 1 -9 5 147.59 11.50 -2 9 -5 149.79 10.20 -2 9 -5 138.19 5.80 -2 9 -5 122.69 10.60 2 -9 5 162.38 11.30 -3 9 -5 7.60 7.30 -3 9 -5 18.50 6.10 3 -9 5 6.50 6.60 -4 9 -5 359.26 15.20 -4 9 -5 330.97 16.70 4 -9 5 330.67 15.20 -5 9 -5 392.46 17.30 -5 9 -5 392.26 17.00 5 -9 5 395.26 16.80 -6 9 -5 326.67 16.10 -6 9 -5 322.97 16.70 6 -9 5 339.77 16.70 -7 9 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6 -5 2.50 8.90 -9 -6 5 0.20 8.70 -9 -6 5 -1.80 7.40 8 6 -5 -0.20 8.90 -8 -6 5 3.20 8.50 -8 -6 5 -3.50 7.20 7 6 -5 37.40 9.20 -7 -6 5 30.60 9.00 -7 -6 5 37.10 7.50 6 6 -5 300.47 16.00 6 6 -5 305.87 12.60 -6 -6 5 335.17 16.60 -6 -6 5 315.27 13.70 5 6 -5 14.20 6.40 5 6 -5 8.30 5.40 -5 -6 5 10.70 5.40 -5 -6 5 5.60 6.50 4 6 -5 112.19 9.40 4 6 -5 114.29 8.90 -4 -6 5 121.39 9.40 -4 -6 5 117.99 8.70 3 6 -5 1.00 5.20 3 6 -5 -4.30 5.10 -3 -6 5 -4.10 4.60 -3 -6 5 -7.00 5.50 2 6 -5 971.90 25.20 2 6 -5 964.10 23.40 -2 -6 5 992.50 23.70 -2 -6 5 962.90 24.60 1 6 -5 691.33 20.30 1 6 -5 733.43 17.70 -1 -6 5 735.63 19.80 -1 -6 5 725.83 18.90 0 6 -5 204.38 11.60 0 6 -5 202.18 7.40 0 -6 5 209.18 10.60 0 -6 5 214.78 9.50 -1 6 -5 275.27 7.00 -1 6 -5 284.17 11.60 -1 6 -5 261.17 12.80 1 -6 5 263.97 10.80 -2 6 -5 281.27 13.10 -2 6 -5 275.67 12.20 2 -6 5 294.27 11.50 -3 6 -5 1239.58 30.10 -3 6 -5 1226.98 29.90 3 -6 5 1179.18 29.50 -4 6 -5 70.39 8.00 -4 6 -5 53.99 7.20 4 -6 5 66.49 7.60 -5 6 -5 354.66 15.10 -5 6 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5 -5 13.80 5.00 -6 -5 5 22.70 5.80 -6 -5 5 9.80 7.20 5 5 -5 169.68 12.00 5 5 -5 174.58 9.70 -5 -5 5 178.58 12.70 -5 -5 5 193.78 9.80 4 5 -5 4.40 5.40 4 5 -5 -1.00 4.70 -4 -5 5 12.00 4.60 -4 -5 5 6.80 6.00 3 5 -5 1424.96 32.90 3 5 -5 1390.56 32.50 -3 -5 5 1473.85 33.80 -3 -5 5 1470.55 31.80 2 5 -5 313.37 11.00 2 5 -5 330.07 12.40 -2 -5 5 302.97 10.80 -2 -5 5 306.37 12.20 1 5 -5 4.10 3.70 1 5 -5 5.20 5.40 -1 -5 5 1.40 4.30 -1 -5 5 6.00 4.90 0 5 -5 306.07 8.40 0 5 -5 305.87 12.50 0 -5 5 283.77 10.30 0 -5 5 301.67 12.00 -1 5 -5 49.40 3.20 -1 5 -5 52.29 6.70 -1 5 -5 45.50 5.80 1 -5 5 56.39 5.70 -2 5 -5 12.30 5.40 -2 5 -5 15.80 5.90 2 -5 5 19.40 5.20 -3 5 -5 3.40 5.70 -3 5 -5 29.40 6.00 3 -5 5 21.90 5.60 -4 5 -5 2012.50 45.70 -4 5 -5 2029.80 44.80 4 -5 5 2014.50 40.50 4 -5 5 2090.09 45.40 -5 5 -5 87.49 8.30 -5 5 -5 104.59 8.00 5 -5 5 101.49 6.00 5 -5 5 103.69 8.60 -6 5 -5 8.10 6.40 -6 5 -5 3.30 5.30 6 -5 5 -2.60 3.70 6 -5 5 0.70 6.30 -7 5 -5 434.76 17.90 -7 5 -5 413.96 14.90 7 -5 5 404.76 13.20 7 -5 5 397.46 17.10 -8 5 -5 116.89 11.60 8 -5 5 121.59 8.30 8 -5 5 108.99 11.00 -9 5 -5 3.60 9.00 9 -5 5 0.40 7.90 -10 5 -5 64.09 12.10 10 -5 5 72.99 11.30 -11 5 -5 41.00 12.70 11 -5 5 47.30 10.70 -12 5 -5 20.10 13.70 12 -5 5 -7.20 9.30 -13 5 -5 6.40 14.50 13 -5 5 2.30 10.20 -14 5 -5 9.70 16.60 14 -5 5 14.80 11.50 15 4 -5 28.10 14.50 -15 -4 5 20.90 13.20 14 4 -5 -0.60 12.70 -14 -4 5 -2.90 11.10 13 4 -5 -15.70 10.80 -13 -4 5 9.50 11.50 -13 -4 5 5.60 9.40 12 4 -5 32.80 12.00 -12 -4 5 37.40 9.60 -12 -4 5 34.10 11.90 11 4 -5 54.69 12.20 -11 -4 5 91.59 13.00 -11 -4 5 79.19 10.60 10 4 -5 16.80 10.00 -10 -4 5 7.70 9.30 -10 -4 5 30.00 8.20 9 4 -5 2.80 8.80 -9 -4 5 -9.40 6.60 -9 -4 5 -4.70 8.80 8 4 -5 11.70 8.40 -8 -4 5 2.20 6.00 -8 -4 5 8.20 8.50 7 4 -5 5.80 7.20 7 4 -5 17.90 4.50 -7 -4 5 21.70 8.30 -7 -4 5 12.90 5.80 6 4 -5 3.90 4.20 6 4 -5 6.20 6.50 -6 -4 5 7.20 7.00 -6 -4 5 13.30 5.10 5 4 -5 7.30 6.20 5 4 -5 -1.90 4.00 -5 -4 5 -11.80 6.30 -5 -4 5 1.10 4.30 4 4 -5 42.80 5.60 4 4 -5 40.20 6.20 -4 -4 5 46.70 5.20 -4 -4 5 39.70 6.80 3 4 -5 53.49 6.10 3 4 -5 49.10 5.90 -3 -4 5 52.19 4.90 -3 -4 5 40.00 6.60 2 4 -5 611.94 16.00 2 4 -5 616.94 17.10 -2 -4 5 603.44 15.20 -2 -4 5 615.94 17.70 1 4 -5 56.29 6.20 1 4 -5 66.39 4.90 -1 -4 5 72.49 5.50 -1 -4 5 65.59 6.40 0 4 -5 167.98 9.10 0 4 -5 168.28 6.20 0 -4 5 177.88 8.00 0 -4 5 164.48 9.30 -1 4 -5 833.82 21.40 -1 4 -5 849.81 17.40 -1 4 -5 850.21 21.80 1 -4 5 874.51 20.50 -2 4 -5 67.59 6.50 -2 4 -5 68.59 6.50 2 -4 5 80.09 6.40 -3 4 -5 10.80 5.20 -3 4 -5 5.90 5.10 3 -4 5 6.70 4.80 3 -4 5 9.30 2.60 -4 4 -5 2035.10 44.60 -4 4 -5 2100.29 46.20 4 -4 5 2066.39 41.70 4 -4 5 2049.59 45.30 -5 4 -5 4.90 6.00 -5 4 -5 -3.90 4.60 5 -4 5 8.20 3.60 5 -4 5 6.50 6.00 -6 4 -5 14.10 5.20 -6 4 -5 13.90 6.50 6 -4 5 22.40 4.60 6 -4 5 8.20 6.40 -7 4 -5 206.58 10.40 -7 4 -5 183.28 13.70 7 -4 5 191.68 10.20 7 -4 5 192.58 13.10 -8 4 -5 40.70 9.30 8 -4 5 50.79 8.70 8 -4 5 55.59 7.30 -9 4 -5 20.90 9.40 9 -4 5 13.60 6.80 9 -4 5 11.70 8.00 -10 4 -5 23.80 10.50 10 -4 5 5.20 8.70 10 -4 5 2.30 9.30 -11 4 -5 2.10 10.80 11 -4 5 11.40 9.30 -12 4 -5 17.00 13.90 12 -4 5 -0.60 9.40 -13 4 -5 14.70 15.40 13 -4 5 2.40 10.30 -14 4 -5 26.70 15.70 14 -4 5 -10.80 10.10 15 3 -5 24.80 13.40 -15 -3 5 21.00 13.20 14 3 -5 32.70 13.00 -14 -3 5 36.70 12.90 13 3 -5 32.90 12.30 -13 -3 5 35.80 12.30 -13 -3 5 28.10 10.00 12 3 -5 3.30 10.50 -12 -3 5 7.30 11.00 -12 -3 5 -10.50 7.90 11 3 -5 13.40 10.10 -11 -3 5 1.70 7.30 -11 -3 5 -0.60 9.50 10 3 -5 97.09 12.20 -10 -3 5 68.59 9.20 -10 -3 5 93.19 12.40 9 3 -5 46.90 10.40 -9 -3 5 49.90 10.40 -9 -3 5 57.29 8.40 8 3 -5 7.40 7.80 -8 -3 5 -0.30 8.00 -8 -3 5 -0.80 5.70 7 3 -5 33.80 4.70 7 3 -5 36.30 8.10 -7 -3 5 24.30 7.80 -7 -3 5 20.20 5.60 6 3 -5 84.69 6.90 6 3 -5 81.99 8.70 -6 -3 5 97.59 7.10 -6 -3 5 77.89 9.00 5 3 -5 173.78 11.10 5 3 -5 178.88 8.50 -5 -3 5 166.68 8.20 -5 -3 5 162.28 12.30 4 3 -5 449.76 13.50 4 3 -5 449.16 14.80 -4 -3 5 466.75 12.40 -4 -3 5 449.76 15.60 3 3 -5 2.80 4.40 3 3 -5 5.20 4.70 -3 -3 5 4.40 3.30 -3 -3 5 -0.20 5.30 2 3 -5 76.69 6.40 2 3 -5 66.19 5.70 -2 -3 5 83.69 7.00 -2 -3 5 75.99 4.80 1 3 -5 20.90 4.00 1 3 -5 24.50 5.60 -1 -3 5 23.60 5.30 -1 -3 5 31.80 4.00 0 3 -5 19.50 5.60 0 3 -5 29.80 3.40 0 -3 5 32.50 5.50 0 -3 5 36.30 4.20 -1 3 -5 304.77 11.50 -1 3 -5 309.57 11.40 -1 3 -5 302.77 7.90 1 -3 5 318.67 10.30 -2 3 -5 7.50 4.90 -2 3 -5 5.00 5.00 -2 3 -5 7.10 2.60 2 -3 5 8.10 4.30 -3 3 -5 803.62 21.60 -3 3 -5 838.32 20.70 3 -3 5 813.52 21.00 3 -3 5 830.02 18.20 -4 3 -5 252.77 12.10 -4 3 -5 249.58 10.40 4 -3 5 248.78 11.70 4 -3 5 255.97 8.90 -5 3 -5 85.59 8.20 -5 3 -5 88.59 7.70 5 -3 5 102.19 7.20 5 -3 5 72.09 7.50 -6 3 -5 248.88 13.40 -6 3 -5 236.98 10.00 6 -3 5 264.67 12.90 6 -3 5 252.27 10.40 -7 3 -5 0.80 6.90 -7 3 -5 5.10 4.60 7 -3 5 1.00 5.10 7 -3 5 2.00 6.30 -8 3 -5 5.30 8.30 8 -3 5 14.00 6.60 8 -3 5 -5.90 6.80 -9 3 -5 105.49 12.40 9 -3 5 101.79 11.00 9 -3 5 88.99 9.50 -10 3 -5 268.77 20.80 10 -3 5 238.28 16.20 10 -3 5 226.38 14.80 -11 3 -5 13.90 11.50 11 -3 5 3.50 8.50 11 -3 5 -5.10 8.00 -12 3 -5 45.50 14.70 12 -3 5 22.70 9.90 -13 3 -5 1.60 13.40 13 -3 5 6.60 9.80 -14 3 -5 -2.10 15.60 14 -3 5 14.30 10.60 15 2 -5 10.30 12.60 -15 -2 5 -5.20 12.20 14 2 -5 66.29 13.60 -14 -2 5 68.19 13.90 13 2 -5 29.70 11.60 -13 -2 5 44.00 10.30 -13 -2 5 36.80 12.50 12 2 -5 -5.40 9.70 -12 -2 5 12.80 10.80 -12 -2 5 -4.30 7.80 11 2 -5 -4.80 8.80 -11 -2 5 7.70 7.30 -11 -2 5 7.40 10.20 10 2 -5 264.37 17.60 -10 -2 5 264.07 19.10 -10 -2 5 217.18 13.80 9 2 -5 1099.19 31.40 -9 -2 5 1081.69 32.60 -9 -2 5 1101.29 28.40 8 2 -5 173.68 13.70 -8 -2 5 184.38 10.90 -8 -2 5 209.18 15.50 7 2 -5 46.50 8.10 7 2 -5 43.70 4.80 -7 -2 5 40.90 5.70 -7 -2 5 50.69 7.90 6 2 -5 79.09 6.70 6 2 -5 98.49 8.80 -6 -2 5 91.79 6.40 -6 -2 5 72.49 8.60 5 2 -5 10.30 5.90 5 2 -5 -5.40 3.70 -5 -2 5 7.60 3.70 -5 -2 5 0.10 6.20 4 2 -5 12.70 5.50 4 2 -5 4.00 4.10 -4 -2 5 12.20 5.90 -4 -2 5 10.90 3.40 3 2 -5 756.32 19.30 3 2 -5 768.72 19.20 -3 -2 5 787.62 16.80 -3 -2 5 756.02 20.40 2 2 -5 7.60 4.70 2 2 -5 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89.09 13.20 -8 14 -6 95.59 12.70 8 -14 6 101.89 13.30 -9 14 -6 -14.40 9.60 -9 14 -6 14.60 10.30 9 -14 6 -6.40 9.70 -10 14 -6 1.40 10.90 -10 14 -6 4.60 13.20 10 -14 6 22.40 10.20 -11 14 -6 3.70 11.30 11 -14 6 -16.10 9.70 -12 14 -6 -16.90 11.70 12 -14 6 7.90 10.50 10 13 -6 -3.20 10.80 -10 -13 6 22.90 12.30 9 13 -6 -1.20 11.20 -9 -13 6 15.80 11.20 8 13 -6 31.90 11.80 -8 -13 6 47.50 11.50 7 13 -6 -12.30 10.10 -7 -13 6 11.20 9.80 6 13 -6 22.50 10.60 -6 -13 6 41.20 10.50 5 13 -6 29.20 10.60 5 13 -6 24.00 9.90 -5 -13 6 25.60 9.70 4 13 -6 74.69 12.20 4 13 -6 82.29 10.80 -4 -13 6 93.69 11.40 3 13 -6 38.80 9.10 3 13 -6 69.79 12.20 -3 -13 6 58.39 9.80 2 13 -6 51.79 11.30 2 13 -6 44.40 8.40 -2 -13 6 43.60 9.80 1 13 -6 77.19 12.10 -1 -13 6 95.99 11.20 -1 -13 6 66.29 8.90 0 13 -6 38.90 11.00 0 -13 6 38.30 8.30 0 -13 6 35.50 9.70 -1 13 -6 5.80 9.70 1 -13 6 0.40 7.10 1 -13 6 6.90 8.70 -2 13 -6 60.79 11.20 2 -13 6 65.69 10.50 2 -13 6 58.99 9.10 -3 13 -6 186.98 14.60 -3 13 -6 225.68 17.50 3 -13 6 205.48 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21.90 -7 9 -7 119.59 12.40 -7 9 -7 106.99 11.60 7 -9 7 110.99 12.10 -8 9 -7 117.69 11.60 -8 9 -7 137.09 13.50 8 -9 7 103.09 12.20 -9 9 -7 7.50 10.40 9 -9 7 36.30 10.60 -10 9 -7 1.70 10.80 10 -9 7 39.40 10.90 -11 9 -7 49.99 13.80 11 -9 7 47.30 12.20 -12 9 -7 46.20 15.60 12 -9 7 18.40 10.80 -13 9 -7 19.90 16.10 13 -9 7 7.30 10.50 -14 9 -7 37.80 18.10 14 -9 7 11.40 12.50 13 8 -7 -8.90 12.60 -13 -8 7 13.10 12.30 12 8 -7 9.40 12.10 -12 -8 7 11.60 11.00 11 8 -7 1.60 11.50 -11 -8 7 -0.90 9.80 10 8 -7 61.89 12.90 -10 -8 7 51.09 10.30 -10 -8 7 62.79 12.40 9 8 -7 35.10 11.20 -9 -8 7 56.89 11.50 -9 -8 7 24.80 8.80 8 8 -7 297.77 18.50 -8 -8 7 296.97 15.90 -8 -8 7 306.77 19.40 7 8 -7 26.60 9.80 -7 -8 7 19.30 9.50 -7 -8 7 12.70 7.50 6 8 -7 61.19 9.00 6 8 -7 59.49 9.90 -6 -8 7 60.69 10.60 -6 -8 7 46.50 8.20 5 8 -7 -0.50 7.20 5 8 -7 0.30 6.90 -5 -8 7 -2.70 7.80 -5 -8 7 2.30 6.00 4 8 -7 24.40 7.00 4 8 -7 19.00 7.20 -4 -8 7 20.40 6.30 -4 -8 7 24.00 8.10 3 8 -7 21.40 7.70 3 8 -7 22.50 6.40 -3 -8 7 17.30 6.30 -3 -8 7 34.80 7.40 2 8 -7 15.30 5.50 2 8 -7 33.60 7.80 -2 -8 7 21.10 6.30 -2 -8 7 4.60 6.10 1 8 -7 3.40 4.40 1 8 -7 8.90 7.20 -1 -8 7 12.20 6.10 -1 -8 7 21.50 6.40 0 8 -7 78.79 5.20 0 8 -7 84.59 9.60 0 -8 7 77.69 7.80 0 -8 7 63.59 7.60 -1 8 -7 93.89 9.70 -1 8 -7 104.49 5.00 1 -8 7 103.19 8.90 1 -8 7 121.19 9.00 -2 8 -7 21.70 7.30 -2 8 -7 28.70 6.60 2 -8 7 21.20 6.50 -3 8 -7 99.69 9.80 -3 8 -7 124.89 10.10 3 -8 7 104.59 9.30 -4 8 -7 1.70 6.70 -4 8 -7 5.20 7.60 4 -8 7 14.20 7.10 -5 8 -7 3.40 7.10 -5 8 -7 1.30 7.50 5 -8 7 8.80 7.30 -6 8 -7 79.49 10.10 -6 8 -7 91.29 10.30 6 -8 7 95.59 10.40 -7 8 -7 -3.70 7.60 -7 8 -7 -0.20 7.90 7 -8 7 -5.60 7.90 -8 8 -7 136.39 11.70 -8 8 -7 148.99 13.90 8 -8 7 138.19 13.00 -9 8 -7 -10.00 9.00 9 -8 7 -9.30 8.10 -10 8 -7 12.10 11.80 10 -8 7 32.80 10.40 -11 8 -7 0.50 12.30 11 -8 7 15.70 10.30 -12 8 -7 21.60 15.20 12 -8 7 9.50 10.30 -13 8 -7 26.30 17.50 13 -8 7 22.50 11.40 -14 8 -7 19.10 17.00 14 -8 7 5.80 11.40 14 7 -7 31.00 14.90 -14 -7 7 39.60 14.20 13 7 -7 -17.40 11.50 -13 -7 7 17.60 12.20 12 7 -7 3.10 12.20 -12 -7 7 6.80 10.70 11 7 -7 6.90 11.50 -11 -7 7 1.80 10.40 10 7 -7 57.29 12.70 -10 -7 7 65.59 9.90 -10 -7 7 38.70 11.10 9 7 -7 21.50 10.30 -9 -7 7 27.80 8.60 -9 -7 7 42.20 10.60 8 7 -7 -1.20 9.00 -8 -7 7 10.70 9.50 -8 -7 7 7.70 7.10 7 7 -7 14.30 7.00 7 7 -7 16.20 9.30 -7 -7 7 11.00 8.90 -7 -7 7 4.80 6.70 6 7 -7 1.90 6.50 6 7 -7 0.50 7.60 -6 -7 7 -7.70 6.00 -6 -7 7 1.20 8.20 5 7 -7 156.68 12.00 5 7 -7 137.29 10.70 -5 -7 7 166.38 10.60 -5 -7 7 156.18 12.00 4 7 -7 4.30 6.30 4 7 -7 13.10 6.80 -4 -7 7 15.60 7.40 -4 -7 7 11.30 5.60 3 7 -7 160.88 10.30 3 7 -7 170.68 11.60 -3 -7 7 157.78 12.10 -3 -7 7 158.08 9.70 2 7 -7 -6.20 6.10 2 7 -7 -5.40 4.60 -2 -7 7 0.70 5.90 -2 -7 7 3.80 5.30 1 7 -7 52.99 5.20 1 7 -7 39.40 7.40 -1 -7 7 45.50 7.10 -1 -7 7 51.79 6.70 0 7 -7 264.27 13.90 0 7 -7 266.67 8.70 0 -7 7 286.07 13.40 0 -7 7 286.67 12.00 -1 7 -7 3.00 2.50 -1 7 -7 5.70 5.60 -1 7 -7 3.90 6.50 1 -7 7 4.10 5.60 1 -7 7 -2.80 5.80 -2 7 -7 -4.10 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49.20 9.80 4 -10 9 59.09 9.60 -5 10 -9 11.20 9.10 -5 10 -9 21.60 9.30 5 -10 9 8.80 8.00 -6 10 -9 -13.30 8.10 -6 10 -9 -10.90 8.40 6 -10 9 -8.40 8.10 -7 10 -9 -4.50 8.60 -7 10 -9 1.00 8.90 7 -10 9 2.40 8.80 -8 10 -9 22.20 9.50 -8 10 -9 2.30 9.80 8 -10 9 -4.10 9.20 -9 10 -9 4.10 10.90 9 -10 9 18.20 10.40 -10 10 -9 2.40 11.70 10 -10 9 -6.90 9.70 -11 10 -9 2.60 14.10 11 -10 9 -2.60 10.90 -12 10 -9 -4.10 14.80 12 -10 9 -15.20 10.60 -13 10 -9 3.00 16.70 13 -10 9 -8.60 12.50 12 9 -9 17.30 13.70 -12 -9 9 -1.80 12.30 11 9 -9 17.50 12.90 -11 -9 9 6.20 11.60 10 9 -9 4.90 11.90 -10 -9 9 20.70 11.50 9 9 -9 -4.80 10.80 -9 -9 9 21.40 10.80 8 9 -9 11.00 10.00 -8 -9 9 -1.90 9.50 7 9 -9 9.20 9.70 7 9 -9 5.80 9.20 -7 -9 9 11.80 7.50 -7 -9 9 23.10 10.10 6 9 -9 9.90 8.70 6 9 -9 -0.30 8.00 -6 -9 9 -2.90 9.20 -6 -9 9 -5.00 6.60 5 9 -9 189.88 15.90 5 9 -9 196.58 14.50 -5 -9 9 166.38 13.70 -5 -9 9 174.68 12.00 4 9 -9 29.30 8.90 4 9 -9 37.60 8.00 -4 -9 9 19.90 8.80 -4 -9 9 31.80 7.20 3 9 -9 270.77 13.30 3 9 -9 265.27 17.30 -3 -9 9 283.07 13.50 -3 -9 9 283.07 16.50 2 9 -9 269.87 12.00 2 9 -9 255.87 16.30 -2 -9 9 268.27 15.70 -2 -9 9 290.27 14.00 1 9 -9 57.49 6.10 1 9 -9 39.60 9.20 -1 -9 9 53.09 8.80 -1 -9 9 50.79 8.00 0 9 -9 26.70 8.60 0 -9 9 27.60 7.40 0 -9 9 21.20 7.60 -1 9 -9 35.70 8.80 1 -9 9 44.10 8.60 1 -9 9 37.00 7.80 -2 9 -9 927.81 28.60 -2 9 -9 914.51 27.90 2 -9 9 912.61 25.50 -3 9 -9 57.59 10.00 -3 9 -9 72.19 9.60 3 -9 9 56.99 8.60 -4 9 -9 83.29 10.70 -4 9 -9 93.89 11.20 4 -9 9 72.49 9.60 -5 9 -9 131.89 12.50 -5 9 -9 149.99 13.00 5 -9 9 157.08 12.60 -6 9 -9 122.69 12.10 -6 9 -9 131.39 13.10 6 -9 9 129.39 12.50 -7 9 -9 9.20 8.20 -7 9 -9 -11.90 8.80 7 -9 9 -6.20 8.40 -8 9 -9 132.39 14.40 -8 9 -9 133.79 12.70 8 -9 9 141.09 13.70 -9 9 -9 175.98 17.00 9 -9 9 168.28 15.60 -10 9 -9 20.60 13.00 10 -9 9 -6.10 9.50 -11 9 -9 40.80 15.40 11 -9 9 18.00 11.50 -12 9 -9 -17.90 14.40 12 -9 9 -2.40 10.60 -13 9 -9 -21.20 16.30 13 -9 9 7.00 11.70 13 8 -9 -2.00 12.80 -13 -8 9 -13.30 11.00 12 8 -9 -12.80 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170.68 16.30 -12 -3 9 159.98 17.10 11 3 -9 78.39 12.90 -11 -3 9 90.39 13.70 10 3 -9 1.20 9.50 -10 -3 9 5.60 9.00 9 3 -9 27.20 9.90 -9 -3 9 14.20 9.20 8 3 -9 199.78 12.40 8 3 -9 206.58 16.20 -8 -3 9 159.78 13.80 7 3 -9 24.20 6.80 7 3 -9 26.50 8.60 -7 -3 9 25.70 4.80 -7 -3 9 27.30 9.50 6 3 -9 221.58 13.20 6 3 -9 200.88 12.00 -6 -3 9 209.48 8.00 -6 -3 9 216.08 15.10 5 3 -9 43.70 7.00 5 3 -9 51.89 7.70 -5 -3 9 36.50 8.20 -5 -3 9 44.10 3.90 4 3 -9 140.49 10.40 4 3 -9 152.48 10.40 -4 -3 9 143.09 5.60 -4 -3 9 176.88 12.20 3 3 -9 423.36 15.60 3 3 -9 435.96 14.80 -3 -3 9 470.25 16.90 -3 -3 9 435.46 10.60 2 3 -9 22.10 6.50 2 3 -9 15.90 5.10 -2 -3 9 17.00 6.30 -2 -3 9 24.10 3.40 1 3 -9 241.08 12.40 1 3 -9 234.18 9.90 -1 -3 9 238.68 12.20 -1 -3 9 243.38 8.10 0 3 -9 49.40 5.20 0 3 -9 53.59 7.20 0 -3 9 55.69 7.40 0 -3 9 52.79 5.00 -1 3 -9 19.00 6.30 -1 3 -9 18.50 4.20 -1 3 -9 11.00 6.00 1 -3 9 16.60 4.50 -2 3 -9 39.60 4.80 -2 3 -9 46.10 7.10 -2 3 -9 36.60 7.10 2 -3 9 41.30 5.80 -3 3 -9 268.37 14.40 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22.10 9.60 -4 -10 10 0.40 7.00 -4 -10 10 6.70 8.90 3 10 -10 145.29 11.60 3 10 -10 173.68 14.70 -3 -10 10 153.68 11.20 -3 -10 10 139.09 12.70 2 10 -10 24.80 9.80 2 10 -10 21.20 7.60 -2 -10 10 26.70 8.90 -2 -10 10 12.80 7.50 1 10 -10 -11.00 8.60 -1 -10 10 14.10 8.20 -1 -10 10 -6.20 6.70 0 10 -10 39.60 10.40 0 -10 10 55.39 9.50 0 -10 10 57.49 8.80 -1 10 -10 132.09 13.20 1 -10 10 117.59 12.10 1 -10 10 118.89 10.70 -2 10 -10 7.50 9.30 2 -10 10 25.70 9.10 2 -10 10 -0.60 7.30 -3 10 -10 178.88 13.80 -3 10 -10 139.39 13.10 3 -10 10 173.18 12.50 -4 10 -10 261.07 17.90 -4 10 -10 262.87 17.40 4 -10 10 289.57 16.80 -5 10 -10 60.79 10.90 -5 10 -10 39.20 10.40 5 -10 10 53.09 10.30 -6 10 -10 68.89 11.40 -6 10 -10 48.90 11.10 6 -10 10 72.79 11.00 -7 10 -10 17.60 10.80 -7 10 -10 -6.90 8.30 7 -10 10 21.30 9.70 -8 10 -10 23.10 11.40 -8 10 -10 7.50 9.30 8 -10 10 12.50 9.90 -9 10 -10 20.30 12.70 9 -10 10 -22.10 9.50 -10 10 -10 77.69 15.90 10 -10 10 74.79 13.50 -11 10 -10 106.39 18.20 11 -10 10 137.19 16.00 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12.50 9.00 -3 9 -10 3.90 7.70 3 -9 10 -2.30 7.00 -4 9 -10 105.39 12.10 -4 9 -10 78.49 11.20 4 -9 10 120.09 10.90 -5 9 -10 9.70 9.00 -5 9 -10 -6.10 8.80 5 -9 10 -1.60 8.40 -6 9 -10 20.40 9.90 -6 9 -10 50.09 10.20 6 -9 10 46.70 10.00 -7 9 -10 33.20 9.60 -7 9 -10 33.60 10.60 7 -9 10 21.60 9.60 -8 9 -10 7.70 8.90 -8 9 -10 -17.00 10.30 8 -9 10 17.70 10.10 -9 9 -10 44.60 13.40 9 -9 10 45.10 11.80 -10 9 -10 6.90 14.20 10 -9 10 31.30 11.70 -11 9 -10 15.10 15.20 11 -9 10 17.60 11.40 -12 9 -10 6.70 14.90 12 -9 10 0.00 10.70 13 8 -10 9.30 14.00 -13 -8 10 22.40 13.20 12 8 -10 0.40 12.70 -12 -8 10 12.20 12.00 11 8 -10 -1.70 11.50 -11 -8 10 20.90 12.40 10 8 -10 2.00 11.40 -10 -8 10 -6.90 10.90 9 8 -10 -12.00 10.00 -9 -8 10 12.30 10.90 8 8 -10 36.50 10.90 -8 -8 10 27.70 11.00 7 8 -10 130.49 11.80 7 8 -10 147.79 13.10 -7 -8 10 119.49 13.50 6 8 -10 377.86 17.90 6 8 -10 395.16 18.50 -6 -8 10 378.86 21.10 -6 -8 10 379.56 16.10 5 8 -10 -2.60 7.70 5 8 -10 0.30 8.10 -5 -8 10 1.50 6.00 -5 -8 10 -12.00 8.70 4 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16.60 12 -8 10 27.20 12.20 -13 8 -10 16.00 17.40 13 -8 10 6.40 12.00 13 7 -10 -13.00 11.80 -13 -7 10 -10.20 11.20 12 7 -10 16.20 13.00 -12 -7 10 1.30 11.40 11 7 -10 24.70 12.70 -11 -7 10 41.40 12.90 10 7 -10 10.90 11.20 -10 -7 10 11.50 10.80 9 7 -10 -10.00 10.40 -9 -7 10 12.60 11.00 8 7 -10 13.00 9.50 -8 -7 10 12.00 10.60 7 7 -10 28.90 9.50 7 7 -10 18.70 8.10 -7 -7 10 22.80 10.60 6 7 -10 191.98 13.40 6 7 -10 224.18 15.00 -6 -7 10 188.18 14.90 -6 -7 10 214.08 13.20 5 7 -10 233.98 14.90 5 7 -10 251.67 15.50 -5 -7 10 210.88 17.30 -5 -7 10 249.58 11.40 4 7 -10 33.10 8.70 4 7 -10 40.80 7.70 -4 -7 10 50.79 6.40 -4 -7 10 32.60 8.90 3 7 -10 27.60 8.30 3 7 -10 25.40 6.40 -3 -7 10 25.00 5.70 -3 -7 10 12.20 7.40 2 7 -10 5.20 5.10 2 7 -10 4.20 7.50 -2 -7 10 0.30 5.20 -2 -7 10 -0.20 7.00 1 7 -10 281.97 10.80 1 7 -10 283.97 15.80 -1 -7 10 266.87 11.60 -1 -7 10 275.17 15.00 0 7 -10 31.10 4.60 0 7 -10 2.80 7.70 0 -7 10 28.00 6.20 0 -7 10 42.60 8.30 -1 7 -10 -8.00 7.40 1 -7 10 8.20 5.80 1 -7 10 -5.90 7.00 -2 7 -10 24.50 7.80 -2 7 -10 27.70 8.70 2 -7 10 24.00 6.50 -3 7 -10 211.28 14.60 -3 7 -10 160.38 12.70 3 -7 10 196.88 12.80 -4 7 -10 43.80 9.50 -4 7 -10 39.90 9.30 4 -7 10 47.70 8.50 -5 7 -10 5.20 8.40 -5 7 -10 -0.30 8.30 5 -7 10 4.10 7.80 -6 7 -10 84.39 10.90 -6 7 -10 112.99 12.70 6 -7 10 79.79 10.90 -7 7 -10 86.09 12.10 -7 7 -10 54.09 9.90 7 -7 10 44.90 10.30 -8 7 -10 -12.40 9.10 8 -7 10 0.60 8.80 -9 7 -10 -10.60 10.80 9 -7 10 6.20 9.80 -10 7 -10 5.80 13.30 10 -7 10 -5.40 9.90 -11 7 -10 114.39 17.90 11 -7 10 69.19 13.10 -12 7 -10 59.79 17.40 12 -7 10 60.29 13.70 -13 7 -10 17.40 17.00 13 -7 10 -6.90 11.20 14 6 -10 9.20 12.90 -14 -6 10 15.90 12.80 13 6 -10 -3.30 12.50 -13 -6 10 1.30 11.40 12 6 -10 -13.50 11.50 -12 -6 10 2.20 11.40 11 6 -10 0.50 11.30 -11 -6 10 -1.10 10.50 10 6 -10 21.90 11.40 -10 -6 10 22.70 11.80 9 6 -10 62.59 11.70 -9 -6 10 44.70 11.70 8 6 -10 6.80 9.40 -8 -6 10 -5.20 10.00 7 6 -10 18.20 7.70 7 6 -10 18.80 9.30 -7 -6 10 8.90 10.10 6 6 -10 12.00 8.60 6 6 -10 7.50 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9.30 12.00 12 6 -12 -11.50 11.50 -12 -6 12 15.20 12.30 11 6 -12 34.00 12.90 -11 -6 12 30.50 12.60 10 6 -12 -5.70 10.90 -10 -6 12 -1.30 10.80 9 6 -12 140.49 14.70 -9 -6 12 140.79 15.50 8 6 -12 1.80 8.10 8 6 -12 4.30 9.30 -8 -6 12 7.60 10.60 7 6 -12 62.59 10.50 7 6 -12 50.69 9.40 -7 -6 12 62.39 12.30 6 6 -12 62.29 10.30 6 6 -12 42.50 9.50 -6 -6 12 65.99 12.30 5 6 -12 14.20 8.70 5 6 -12 4.60 7.80 -5 -6 12 2.40 8.50 4 6 -12 7.90 7.00 4 6 -12 5.50 8.00 -4 -6 12 4.90 8.30 3 6 -12 343.87 14.30 3 6 -12 330.57 17.30 -3 -6 12 323.27 17.30 2 6 -12 65.79 7.40 2 6 -12 69.19 10.40 -2 -6 12 58.59 6.40 -2 -6 12 62.19 9.60 1 6 -12 2.30 5.10 1 6 -12 -9.50 7.40 -1 -6 12 -0.20 7.70 -1 -6 12 2.10 5.10 0 6 -12 191.78 9.60 0 6 -12 187.68 14.50 0 -6 12 189.78 14.50 0 -6 12 189.08 10.60 -1 6 -12 14.40 8.30 1 -6 12 33.60 9.10 1 -6 12 36.90 6.70 -2 6 -12 457.45 20.10 -2 6 -12 494.95 20.60 2 -6 12 464.45 17.00 -3 6 -12 9.60 8.30 -3 6 -12 -1.20 8.10 3 -6 12 13.00 7.30 -4 6 -12 0.30 9.00 -4 6 -12 3.80 8.40 4 -6 12 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6.60 -3 -5 12 12.90 7.70 2 5 -12 86.99 10.30 2 5 -12 85.39 8.00 -2 -5 12 84.59 6.30 -2 -5 12 95.49 10.10 1 5 -12 112.89 11.40 1 5 -12 136.69 9.40 -1 -5 12 124.49 11.20 -1 -5 12 103.09 8.30 0 5 -12 131.79 12.00 0 5 -12 119.09 8.70 0 -5 12 119.69 11.00 0 -5 12 138.49 9.20 -1 5 -12 126.89 8.30 -1 5 -12 125.39 11.80 1 -5 12 135.09 10.00 1 -5 12 128.09 11.80 -2 5 -12 9.00 8.20 -2 5 -12 10.60 8.30 2 -5 12 17.80 6.30 -3 5 -12 257.67 16.00 -3 5 -12 246.98 17.00 3 -5 12 261.97 13.90 -4 5 -12 18.50 9.00 -4 5 -12 23.40 8.90 4 -5 12 23.40 7.70 -5 5 -12 -6.40 7.70 -5 5 -12 3.30 9.00 5 -5 12 1.40 7.50 -6 5 -12 168.58 13.10 -6 5 -12 190.28 15.80 6 -5 12 159.88 13.30 -7 5 -12 44.20 11.80 7 -5 12 55.29 10.60 -8 5 -12 -2.40 11.40 8 -5 12 3.10 9.40 -9 5 -12 6.50 13.10 9 -5 12 -17.60 9.00 -10 5 -12 32.20 15.20 10 -5 12 1.80 10.40 -11 5 -12 38.60 15.50 11 -5 12 25.20 12.30 -12 5 -12 17.60 16.10 12 -5 12 1.50 12.20 14 4 -12 0.60 13.10 -14 -4 12 -3.10 12.30 13 4 -12 -13.80 11.90 -13 -4 12 11.80 12.30 12 4 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5 8 -14 -0.50 7.90 5 8 -14 17.30 10.30 -5 -8 14 -3.90 9.00 4 8 -14 225.38 14.10 4 8 -14 203.58 16.20 -4 -8 14 177.18 15.00 3 8 -14 4.50 10.00 -3 -8 14 -11.90 8.80 2 8 -14 121.49 13.60 -2 -8 14 95.99 12.60 1 8 -14 14.50 9.90 -1 -8 14 14.30 8.90 0 8 -14 273.97 18.80 0 -8 14 236.58 17.80 0 -8 14 227.08 18.30 -1 8 -14 185.78 15.60 1 -8 14 152.78 11.00 1 -8 14 168.88 15.00 -2 8 -14 5.60 9.40 2 -8 14 -8.60 9.30 2 -8 14 14.80 7.50 -3 8 -14 30.90 11.10 -3 8 -14 14.50 9.40 3 -8 14 19.30 8.20 -4 8 -14 54.09 11.10 -4 8 -14 77.29 12.90 4 -8 14 87.39 10.90 -5 8 -14 11.50 11.10 -5 8 -14 4.60 9.40 5 -8 14 16.60 9.60 -6 8 -14 38.20 10.70 -6 8 -14 55.59 13.40 6 -8 14 22.70 10.00 -7 8 -14 21.80 10.70 -7 8 -14 5.30 12.20 7 -8 14 18.50 10.10 -8 8 -14 -5.40 13.30 8 -8 14 -3.00 10.20 -9 8 -14 19.70 15.00 9 -8 14 8.20 11.00 -10 8 -14 -4.20 14.70 10 -8 14 -3.70 11.40 13 7 -14 -6.50 13.70 -13 -7 14 -4.30 13.10 12 7 -14 -2.20 12.20 -12 -7 14 2.10 12.50 11 7 -14 67.99 14.40 -11 -7 14 59.59 14.30 10 7 -14 46.10 12.70 -10 -7 14 45.10 13.80 9 7 -14 11.80 10.50 -9 -7 14 -10.90 11.30 8 7 -14 122.89 13.80 8 7 -14 87.59 12.50 -8 -7 14 122.49 15.70 7 7 -14 64.49 11.30 7 7 -14 45.30 10.80 -7 -7 14 55.19 12.50 6 7 -14 23.00 10.10 6 7 -14 34.60 9.70 -6 -7 14 9.70 10.40 5 7 -14 8.60 9.60 5 7 -14 29.30 8.80 -5 -7 14 33.40 10.60 4 7 -14 231.08 14.40 4 7 -14 262.77 19.20 -4 -7 14 250.07 18.90 3 7 -14 66.69 8.90 3 7 -14 53.29 11.20 -3 -7 14 57.29 11.20 2 7 -14 31.10 10.30 2 7 -14 51.39 10.90 -2 -7 14 49.50 9.90 1 7 -14 13.80 9.90 -1 -7 14 30.30 9.40 0 7 -14 32.10 10.10 0 -7 14 22.60 10.00 -1 7 -14 52.29 10.60 1 -7 14 49.10 8.10 1 -7 14 40.90 10.50 -2 7 -14 181.98 15.00 2 -7 14 184.48 15.10 2 -7 14 188.28 13.00 -3 7 -14 22.10 9.40 -3 7 -14 10.90 10.00 3 -7 14 20.10 8.30 -4 7 -14 3.40 10.00 -4 7 -14 4.20 8.80 4 -7 14 5.90 8.30 -5 7 -14 21.30 9.70 -5 7 -14 24.80 11.30 5 -7 14 2.40 8.70 -6 7 -14 62.59 13.70 -6 7 -14 50.39 11.20 6 -7 14 72.79 11.70 -7 7 -14 10.20 13.10 7 -7 14 -5.20 9.40 -8 7 -14 -5.30 13.00 8 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9.20 2 5 -14 -3.30 8.50 2 5 -14 -1.40 6.50 -2 -5 14 -19.70 7.50 1 5 -14 7.90 8.70 1 5 -14 7.90 6.30 -1 -5 14 -0.50 8.10 0 5 -14 11.20 6.20 0 5 -14 6.20 8.60 0 -5 14 19.60 9.30 -1 5 -14 -2.20 8.30 1 -5 14 4.00 9.20 1 -5 14 -11.10 5.90 -2 5 -14 109.19 12.40 2 -5 14 113.09 12.60 2 -5 14 91.69 9.20 -3 5 -14 58.39 10.40 -3 5 -14 65.59 11.60 3 -5 14 70.69 9.30 -4 5 -14 207.98 16.00 -4 5 -14 210.48 17.10 4 -5 14 189.38 14.30 -5 5 -14 50.49 10.40 -5 5 -14 26.10 11.50 5 -5 14 13.40 8.30 -6 5 -14 94.69 11.90 -6 5 -14 122.89 14.60 6 -5 14 99.79 11.80 -7 5 -14 15.60 12.40 7 -5 14 -8.00 9.00 -8 5 -14 22.50 13.80 8 -5 14 26.50 11.00 -9 5 -14 16.00 14.10 9 -5 14 8.00 10.70 -10 5 -14 12.60 14.30 10 -5 14 33.10 12.30 -11 5 -14 23.70 16.00 11 -5 14 21.70 12.80 14 4 -14 6.70 13.40 -14 -4 14 24.20 14.00 13 4 -14 20.70 12.80 -13 -4 14 4.00 12.90 12 4 -14 2.40 12.00 -12 -4 14 3.10 12.00 11 4 -14 -27.40 10.40 -11 -4 14 -8.60 11.70 10 4 -14 37.80 12.60 -10 -4 14 31.00 13.00 9 4 -14 24.20 11.10 9 4 -14 28.30 9.60 -9 -4 14 26.30 11.90 8 4 -14 15.90 9.00 8 4 -14 -1.20 9.70 -8 -4 14 7.40 11.40 7 4 -14 14.00 9.00 7 4 -14 -1.80 8.80 -7 -4 14 21.60 11.30 6 4 -14 5.80 9.20 6 4 -14 10.50 9.00 -6 -4 14 -7.30 9.30 5 4 -14 -3.70 8.00 5 4 -14 7.40 8.90 -5 -4 14 -8.70 8.00 4 4 -14 11.60 9.40 4 4 -14 6.30 7.20 -4 -4 14 17.50 8.50 3 4 -14 124.19 12.90 3 4 -14 109.59 10.00 -3 -4 14 105.09 12.00 2 4 -14 55.09 8.10 2 4 -14 59.69 10.70 -2 -4 14 68.69 10.30 1 4 -14 -0.20 8.40 1 4 -14 2.50 6.20 -1 -4 14 -2.00 8.00 0 4 -14 25.20 9.30 0 4 -14 17.20 6.40 0 -4 14 28.40 9.20 -1 4 -14 226.18 11.90 -1 4 -14 206.28 17.00 1 -4 14 220.98 12.20 1 -4 14 251.97 17.20 -2 4 -14 17.90 8.90 2 -4 14 14.30 6.60 2 -4 14 30.20 9.80 -3 4 -14 103.29 12.00 -3 4 -14 110.79 12.70 3 -4 14 121.49 10.50 -4 4 -14 9.70 9.30 -4 4 -14 5.50 8.80 4 -4 14 4.40 7.50 -5 4 -14 9.20 10.30 -5 4 -14 13.40 8.90 5 -4 14 2.60 8.20 -6 4 -14 2.10 9.40 -6 4 -14 18.40 10.90 6 -4 14 -2.80 8.50 -7 4 -14 38.50 13.40 7 -4 14 55.09 11.30 -8 4 -14 22.30 13.50 8 -4 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6 -23 42.70 16.20 -7 -6 23 20.40 17.10 6 6 -23 -19.50 14.40 -6 -6 23 -35.70 14.00 5 6 -23 -2.10 15.10 -5 -6 23 11.90 16.00 4 6 -23 34.40 16.10 -4 -6 23 25.70 15.60 3 6 -23 3.40 13.70 -3 -6 23 2.60 14.20 2 6 -23 -1.80 11.80 -2 -6 23 -10.70 13.60 1 6 -23 10.30 12.50 -1 -6 23 5.30 14.20 0 6 -23 -0.10 11.90 0 -6 23 -18.00 13.10 -1 6 -23 2.60 12.40 1 -6 23 23.40 15.10 7 5 -23 21.00 15.60 -7 -5 23 -5.80 16.30 6 5 -23 45.90 16.80 -6 -5 23 28.60 17.00 5 5 -23 8.90 15.10 -5 -5 23 -36.30 12.80 4 5 -23 16.50 14.70 -4 -5 23 -27.20 12.90 3 5 -23 -1.30 13.90 -3 -5 23 -8.20 14.60 2 5 -23 -3.50 12.50 -2 -5 23 -16.80 13.20 1 5 -23 18.80 12.90 -1 -5 23 4.20 14.00 0 5 -23 30.00 14.10 0 -5 23 39.80 15.70 -1 5 -23 -5.10 12.60 1 -5 23 8.90 14.00 8 4 -23 -12.00 14.00 8 4 -23 -6.50 14.50 -8 -4 23 -1.80 16.10 7 4 -23 12.10 14.90 -7 -4 23 -26.10 15.00 6 4 -23 20.20 15.70 -6 -4 23 -10.30 15.80 5 4 -23 13.50 15.10 -5 -4 23 -25.70 14.00 4 4 -23 1.70 14.00 -4 -4 23 13.30 14.50 3 4 -23 19.80 13.90 -3 -4 23 9.90 14.60 2 4 -23 16.90 13.40 -2 -4 23 5.00 13.60 1 4 -23 -1.00 12.90 -1 -4 23 30.80 14.80 0 4 -23 1.40 12.70 0 -4 23 8.70 13.90 -1 4 -23 -4.90 13.20 1 -4 23 31.20 15.10 8 3 -23 -12.10 14.30 8 3 -23 -1.90 12.70 -8 -3 23 -41.50 14.20 7 3 -23 -8.00 11.90 7 3 -23 -8.60 14.50 -7 -3 23 -43.00 14.50 6 3 -23 16.90 15.00 -6 -3 23 -26.80 15.00 5 3 -23 21.60 14.90 -5 -3 23 -1.60 14.30 4 3 -23 -3.60 13.10 -4 -3 23 -30.00 12.40 3 3 -23 -3.00 12.90 -3 -3 23 -2.00 13.90 2 3 -23 81.19 15.60 -2 -3 23 71.09 16.00 1 3 -23 27.70 13.50 -1 -3 23 16.30 14.20 0 3 -23 -7.30 11.90 0 -3 23 13.30 14.00 -1 3 -23 -5.50 12.00 1 -3 23 -0.80 13.30 8 2 -23 25.10 16.00 8 2 -23 44.80 13.80 -8 -2 23 6.00 16.70 7 2 -23 -6.20 14.90 7 2 -23 -2.20 12.30 -7 -2 23 -1.10 14.80 6 2 -23 2.10 14.80 6 2 -23 -17.40 11.50 -6 -2 23 -21.20 13.90 5 2 -23 2.40 14.20 -5 -2 23 -5.20 14.10 4 2 -23 -8.10 13.50 -4 -2 23 -3.10 14.00 3 2 -23 -2.80 12.10 -3 -2 23 6.10 14.10 2 2 -23 22.50 13.30 -2 -2 23 17.20 14.30 1 2 -23 1.70 12.60 -1 -2 23 -3.30 12.70 0 2 -23 -17.40 12.30 0 -2 23 15.50 13.70 -1 2 -23 11.60 13.80 1 -2 23 16.70 13.80 8 1 -23 -16.00 14.60 8 1 -23 -10.60 12.10 -8 -1 23 -36.80 15.10 7 1 -23 36.70 15.90 7 1 -23 9.20 13.10 -7 -1 23 20.00 15.50 6 1 -23 -13.40 13.10 6 1 -23 -6.90 12.30 -6 -1 23 -24.50 13.50 5 1 -23 8.00 14.40 5 1 -23 0.20 12.10 -5 -1 23 -20.20 13.30 4 1 -23 8.90 13.60 4 1 -23 -4.90 16.30 -4 -1 23 6.20 14.40 3 1 -23 -3.80 12.20 -3 -1 23 -19.80 12.30 2 1 -23 28.20 13.40 -2 -1 23 23.70 13.80 1 1 -23 31.90 14.00 -1 -1 23 7.50 14.30 0 1 -23 6.60 12.70 -1 1 -23 8.20 13.20 8 0 -23 34.40 16.50 8 0 -23 42.30 14.10 -8 0 23 64.69 14.70 -8 0 23 23.00 16.20 7 0 -23 -1.10 14.70 7 0 -23 -3.90 12.10 -7 0 23 -38.00 13.10 6 0 -23 -13.60 14.40 6 0 -23 -8.00 11.70 -6 0 23 -22.20 14.40 5 0 -23 -9.90 13.80 5 0 -23 2.60 12.00 -5 0 23 -18.10 13.90 4 0 -23 -1.60 12.20 4 0 -23 12.60 12.50 -4 0 23 -20.30 12.70 3 0 -23 48.70 14.20 3 0 -23 59.89 15.00 2 0 -23 11.10 12.90 1 0 -23 13.70 13.60 0 0 -23 -15.20 12.30 8 -1 -23 3.90 13.00 -8 1 23 -9.70 15.00 -8 1 23 24.30 13.80 7 -1 -23 -0.60 12.50 -7 1 23 -38.30 14.00 -7 1 23 16.80 13.00 6 -1 -23 -2.50 12.10 -6 1 23 6.90 13.40 5 -1 -23 -7.60 11.40 5 -1 -23 -6.30 13.20 -5 1 23 -19.60 13.80 4 -1 -23 11.30 12.30 4 -1 -23 -25.40 11.60 -4 1 23 30.90 15.40 3 -1 -23 37.60 14.70 3 -1 -23 54.19 13.80 -3 1 23 89.19 18.00 2 -1 -23 25.70 13.80 2 -1 -23 38.50 14.30 -2 1 23 33.70 16.20 1 -1 -23 -10.70 12.20 -1 1 23 15.40 16.00 0 1 23 -8.70 15.90 8 -2 -23 4.60 13.20 7 -2 -23 26.10 13.40 -7 2 23 8.40 14.00 6 -2 -23 -14.80 11.80 -6 2 23 15.90 15.20 5 -2 -23 10.10 12.60 -5 2 23 -9.60 14.20 4 -2 -23 10.00 11.90 -4 2 23 10.40 16.20 3 -2 -23 -7.40 12.30 -3 2 23 31.30 16.90 2 -2 -23 45.80 14.10 -2 2 23 20.80 17.60 1 -2 -23 -5.90 12.90 -1 2 23 -5.50 16.80 7 -3 -23 -8.50 12.60 -7 3 23 23.50 15.10 6 -3 -23 -9.20 11.70 -6 3 23 -12.30 15.10 5 -3 -23 24.90 13.20 -5 3 23 -27.40 15.70 4 -3 -23 37.70 13.80 -4 3 23 22.60 17.10 3 -3 -23 -11.90 12.30 -3 3 23 16.00 17.30 2 -3 -23 6.20 13.50 -2 3 23 -26.40 15.60 5 -4 -23 35.70 14.10 -5 4 23 25.10 18.40 4 -4 -23 8.70 12.60 -4 4 23 -6.60 17.00 4 6 -24 -11.40 15.30 3 6 -24 -16.50 14.20 -3 -6 24 7.80 14.90 2 6 -24 -12.00 13.00 -2 -6 24 -23.30 14.70 5 5 -24 15.50 16.30 -5 -5 24 -15.60 14.70 4 5 -24 11.20 15.00 -4 -5 24 -23.50 14.90 3 5 -24 -14.00 13.70 -3 -5 24 -7.40 14.40 2 5 -24 15.50 14.10 -2 -5 24 0.00 14.90 5 4 -24 -6.40 15.30 -5 -4 24 -9.30 15.10 4 4 -24 11.00 15.20 -4 -4 24 -29.50 14.00 3 4 -24 -9.90 12.80 -3 -4 24 -16.00 13.60 2 4 -24 11.10 13.80 -2 -4 24 1.50 14.60 1 4 -24 4.40 13.60 -1 -4 24 16.80 14.80 6 3 -24 -8.10 15.50 -6 -3 24 -3.00 15.90 5 3 -24 1.60 14.20 -5 -3 24 -27.20 13.60 4 3 -24 4.80 14.50 -4 -3 24 -35.40 14.00 3 3 -24 24.30 14.70 -3 -3 24 28.20 15.10 2 3 -24 -22.30 12.40 -2 -3 24 1.90 14.10 1 3 -24 -28.00 12.40 -1 -3 24 -34.30 13.20 6 2 -24 -6.90 15.20 -6 -2 24 -25.90 14.10 5 2 -24 4.90 15.10 -5 -2 24 -1.20 15.40 4 2 -24 -4.30 14.00 -4 -2 24 -29.40 13.60 3 2 -24 -8.60 12.90 -3 -2 24 12.50 15.00 2 2 -24 27.60 14.70 -2 -2 24 76.89 17.00 6 1 -24 -4.30 12.60 6 1 -24 -11.60 14.60 -6 -1 24 -17.40 14.50 5 1 -24 -21.10 14.40 -5 -1 24 -32.90 14.60 4 1 -24 -8.90 13.10 -4 -1 24 -13.10 14.00 3 1 -24 14.50 14.30 -3 -1 24 15.80 15.20 2 1 -24 6.10 14.10 5 0 -24 -8.30 13.70 5 0 -24 -2.80 12.70 4 0 -24 13.20 14.40 3 0 -24 -6.00 12.90 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 57988 #===END data_Ox_5c _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Ox_5c' _chemical_melting_point ? _chemical_formula_moiety 'C41 H55 Br N O4 P Pd, 1.5(C H2 Cl2)' _chemical_formula_sum 'C42.50 H58 Br Cl3 N O4 P Pd' _chemical_formula_weight 970.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.542(2) _cell_length_b 11.548(2) _cell_length_c 17.998(3) _cell_angle_alpha 81.507(2) _cell_angle_beta 77.635(2) _cell_angle_gamma 72.621(2) _cell_volume 2227.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7336 _cell_measurement_theta_min 2.247 _cell_measurement_theta_max 27.300 _exptl_crystal_description Blade _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_F_000 998 _exptl_transmission_factor_min 0.918 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 1.570 _shelx_estimated_absorpt_T_min 0.799 _shelx_estimated_absorpt_T_max 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26553 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.855 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 10062 _reflns_number_gt 7443 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10062 _refine_ls_number_parameters 518 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1A Cl 0.1760(2) 0.2141(2) 0.50662(13) 0.0751(6) Uani 0.869(2) 1 d D . P A 1 Cl2A Cl 0.4275(2) 0.1658(3) 0.52987(19) 0.1043(10) Uani 0.869(2) 1 d D . P A 1 C42A C 0.3067(6) 0.1030(8) 0.5359(5) 0.065(2) Uani 0.869(2) 1 d D . P A 1 H42A H 0.283396 0.069926 0.589138 0.077 Uiso 0.869(2) 1 calc R U P A 1 H42B H 0.333575 0.034769 0.502951 0.077 Uiso 0.869(2) 1 calc R U P A 1 Cl1B Cl 0.2844(14) 0.2412(13) 0.4933(8) 0.0751(6) Uani 0.131(2) 1 d D . P A 2 Cl2B Cl 0.4792(13) 0.0332(15) 0.4686(11) 0.1043(10) Uani 0.131(2) 1 d D . P A 2 C42B C 0.338(3) 0.113(3) 0.441(2) 0.065(2) Uani 0.131(2) 1 d D . P A 2 H42C H 0.279588 0.063019 0.453096 0.077 Uiso 0.131(2) 1 calc R U P A 2 H42D H 0.350282 0.138191 0.385219 0.077 Uiso 0.131(2) 1 calc R U P A 2 Cl3 Cl 1.0269(4) 0.9901(6) -0.0079(4) 0.0579(11) Uani 0.5 1 d . . P B -1 Cl4 Cl 0.9041(2) 0.8268(2) 0.09864(15) 0.0404(6) Uani 0.5 1 d . . P B -1 C43 C 0.8869(10) 0.9701(10) 0.0512(6) 0.043(3) Uani 0.5 1 d . . P B -1 H43A H 0.857190 1.031222 0.089214 0.052 Uiso 0.5 1 calc R U P B -1 H43B H 0.823286 0.985427 0.019093 0.052 Uiso 0.5 1 calc R U P B -1 Pd1 Pd 0.27555(3) 0.70611(2) 0.76614(2) 0.01505(10) Uani 1 1 d . . . . . Br1 Br 0.20555(4) 0.92863(4) 0.73718(3) 0.03467(14) Uani 1 1 d . . . . . P1 P 0.36402(9) 0.49704(9) 0.78087(5) 0.0135(2) Uani 1 1 d . . . . . O1 O 0.3811(3) 0.2290(2) 0.77583(18) 0.0282(7) Uani 1 1 d . . . . . O2 O -0.0205(3) 0.5436(3) 0.66713(16) 0.0218(6) Uani 1 1 d . . . . . O3 O 0.6849(3) 0.3972(3) 0.88434(17) 0.0269(7) Uani 1 1 d . . . . . O4 O 0.7218(3) 0.2473(3) 0.80503(17) 0.0285(7) Uani 1 1 d . . . . . N1 N 0.6797(4) 0.9426(4) 0.9385(3) 0.0428(11) Uani 1 1 d . . . . . C1 C 0.2626(4) 0.4286(3) 0.7466(2) 0.0156(8) Uani 1 1 d . . . . . C2 C 0.2831(4) 0.3022(4) 0.7453(2) 0.0219(9) Uani 1 1 d . . . . . C3 C 0.4236(5) 0.1022(4) 0.7606(4) 0.0430(13) Uani 1 1 d . . . . . H3A H 0.368583 0.057756 0.793407 0.064 Uiso 1 1 calc R U . . . H3B H 0.507579 0.067053 0.771038 0.064 Uiso 1 1 calc R U . . . H3C H 0.423430 0.095853 0.706884 0.064 Uiso 1 1 calc R U . . . C4 C 0.2070(4) 0.2568(4) 0.7159(3) 0.0275(10) Uani 1 1 d . . . . . H4 H 0.223787 0.171349 0.714465 0.033 Uiso 1 1 calc R U . . . C5 C 0.1052(4) 0.3358(4) 0.6883(2) 0.0243(9) Uani 1 1 d . . . . . H5 H 0.052517 0.304448 0.667838 0.029 Uiso 1 1 calc R U . . . C6 C 0.0809(4) 0.4602(3) 0.6906(2) 0.0179(8) Uani 1 1 d . . . . . C7 C -0.0889(4) 0.4991(4) 0.6260(3) 0.0335(11) Uani 1 1 d . . . . . H7A H -0.033530 0.460141 0.581797 0.050 Uiso 1 1 calc R U . . . H7B H -0.154351 0.567053 0.608603 0.050 Uiso 1 1 calc R U . . . H7C H -0.125669 0.439428 0.659522 0.050 Uiso 1 1 calc R U . . . C8 C 0.1590(4) 0.5080(3) 0.7192(2) 0.0135(7) Uani 1 1 d . . . . . C9 C 0.1189(3) 0.6458(3) 0.7188(2) 0.0156(8) Uani 1 1 d . . . . . C10 C 0.1278(4) 0.7152(3) 0.6467(2) 0.0167(8) Uani 1 1 d . . . . . C11 C 0.2226(4) 0.6655(4) 0.5778(2) 0.0187(8) Uani 1 1 d . . . . . H11 H 0.279685 0.587906 0.596185 0.022 Uiso 1 1 calc R U . . . C12 C 0.3004(4) 0.7534(4) 0.5424(2) 0.0222(9) Uani 1 1 d . . . . . H12A H 0.248084 0.828161 0.520195 0.033 Uiso 1 1 calc R U . . . H12B H 0.366974 0.714838 0.502399 0.033 Uiso 1 1 calc R U . . . H12C H 0.335976 0.773326 0.582048 0.033 Uiso 1 1 calc R U . . . C13 C 0.1638(4) 0.6357(4) 0.5177(2) 0.0266(9) Uani 1 1 d . . . . . H13A H 0.120577 0.573963 0.540005 0.040 Uiso 1 1 calc R U . . . H13B H 0.228132 0.604229 0.474592 0.040 Uiso 1 1 calc R U . . . H13C H 0.104948 0.709581 0.499807 0.040 Uiso 1 1 calc R U . . . C14 C 0.0451(4) 0.8302(3) 0.6385(2) 0.0191(8) Uani 1 1 d . . . . . H14 H 0.049755 0.876040 0.590125 0.023 Uiso 1 1 calc R U . . . C15 C -0.0448(4) 0.8799(3) 0.6997(2) 0.0202(8) Uani 1 1 d . . . . . C16 C -0.1379(4) 1.0041(4) 0.6883(2) 0.0250(9) Uani 1 1 d . . . . . H16 H -0.188678 1.025702 0.739304 0.030 Uiso 1 1 calc R U . . . C17 C -0.0737(4) 1.1045(4) 0.6561(3) 0.0338(11) Uani 1 1 d . . . . . H17A H -0.025140 1.086779 0.605318 0.051 Uiso 1 1 calc R U . . . H17B H -0.019085 1.107618 0.690202 0.051 Uiso 1 1 calc R U . . . H17C H -0.136059 1.183243 0.652431 0.051 Uiso 1 1 calc R U . . . C18 C -0.2243(4) 0.9984(4) 0.6371(3) 0.0328(11) Uani 1 1 d . . . . . H18A H -0.177668 0.983712 0.585412 0.049 Uiso 1 1 calc R U . . . H18B H -0.288981 1.075794 0.635358 0.049 Uiso 1 1 calc R U . . . H18C H -0.262072 0.931994 0.657349 0.049 Uiso 1 1 calc R U . . . C19 C -0.0482(4) 0.8144(3) 0.7703(2) 0.0174(8) Uani 1 1 d . . . . . H19 H -0.105436 0.850115 0.812661 0.021 Uiso 1 1 calc R U . . . C20 C 0.0289(4) 0.6982(3) 0.7815(2) 0.0159(8) Uani 1 1 d . . . . . C21 C 0.0086(4) 0.6235(3) 0.8576(2) 0.0186(8) Uani 1 1 d . . . . . H21 H 0.078991 0.547676 0.856775 0.022 Uiso 1 1 calc R U . . . C22 C 0.0073(4) 0.6909(4) 0.9254(2) 0.0279(10) Uani 1 1 d . . . . . H22A H 0.083982 0.714731 0.917656 0.042 Uiso 1 1 calc R U . . . H22B H 0.000281 0.637141 0.972633 0.042 Uiso 1 1 calc R U . . . H22C H -0.063248 0.763836 0.929009 0.042 Uiso 1 1 calc R U . . . C23 C -0.1106(4) 0.5849(4) 0.8682(2) 0.0290(10) Uani 1 1 d . . . . . H23A H -0.117755 0.530206 0.915059 0.043 Uiso 1 1 calc R U . . . H23B H -0.108417 0.542529 0.824371 0.043 Uiso 1 1 calc R U . . . H23C H -0.181735 0.657265 0.871987 0.043 Uiso 1 1 calc R U . . . C24 C 0.5212(4) 0.4537(4) 0.7170(2) 0.0182(8) Uani 1 1 d . . . . . C25 C 0.5225(4) 0.5521(4) 0.6492(2) 0.0229(9) Uani 1 1 d . . . . . H25A H 0.477420 0.632283 0.667061 0.034 Uiso 1 1 calc R U . . . H25B H 0.482985 0.535348 0.610452 0.034 Uiso 1 1 calc R U . . . H25C H 0.608015 0.551227 0.626903 0.034 Uiso 1 1 calc R U . . . C26 C 0.5623(4) 0.3317(4) 0.6808(2) 0.0268(10) Uani 1 1 d . . . . . H26A H 0.640608 0.325611 0.645196 0.040 Uiso 1 1 calc R U . . . H26B H 0.499259 0.327571 0.653236 0.040 Uiso 1 1 calc R U . . . H26C H 0.573144 0.264217 0.721042 0.040 Uiso 1 1 calc R U . . . C27 C 0.6121(4) 0.4574(4) 0.7678(2) 0.0217(9) Uani 1 1 d . . . . . H27A H 0.693172 0.454792 0.734729 0.026 Uiso 1 1 calc R U . . . H27B H 0.582072 0.536293 0.790585 0.026 Uiso 1 1 calc R U . . . C28 C 0.6314(4) 0.3546(4) 0.8325(2) 0.0214(9) Uani 1 1 d . . . . . C29 C 0.7800(5) 0.2953(4) 0.9078(3) 0.0340(11) Uani 1 1 d . . . . . H29A H 0.746374 0.245530 0.951982 0.041 Uiso 1 1 calc R U . . . H29B H 0.846020 0.322146 0.921351 0.041 Uiso 1 1 calc R U . . . C30 C 0.8262(5) 0.2269(5) 0.8394(3) 0.0403(12) Uani 1 1 d . . . . . H30A H 0.891389 0.257493 0.804287 0.048 Uiso 1 1 calc R U . . . H30B H 0.860216 0.138986 0.853845 0.048 Uiso 1 1 calc R U . . . C31 C 0.5158(4) 0.3192(4) 0.8725(2) 0.0214(9) Uani 1 1 d . . . . . H31A H 0.527588 0.283456 0.924736 0.026 Uiso 1 1 calc R U . . . H31B H 0.507891 0.254182 0.845251 0.026 Uiso 1 1 calc R U . . . C32 C 0.3929(4) 0.4202(4) 0.8790(2) 0.0202(8) Uani 1 1 d . . . . . C33 C 0.3944(4) 0.5152(4) 0.9296(2) 0.0276(10) Uani 1 1 d . . . . . H33A H 0.405775 0.475901 0.980678 0.041 Uiso 1 1 calc R U . . . H33B H 0.315920 0.579247 0.933446 0.041 Uiso 1 1 calc R U . . . H33C H 0.462353 0.551065 0.907131 0.041 Uiso 1 1 calc R U . . . C34 C 0.2871(4) 0.3657(4) 0.9201(2) 0.0289(10) Uani 1 1 d . . . . . H34A H 0.283902 0.301443 0.891145 0.043 Uiso 1 1 calc R U . . . H34B H 0.208599 0.429717 0.923653 0.043 Uiso 1 1 calc R U . . . H34C H 0.301348 0.331101 0.971491 0.043 Uiso 1 1 calc R U . . . C35 C 0.3978(4) 0.7565(4) 0.8109(2) 0.0205(8) Uani 1 1 d . . . . . C36 C 0.3548(5) 0.7999(4) 0.8832(3) 0.0321(11) Uani 1 1 d . . . . . H36 H 0.274788 0.797701 0.909578 0.038 Uiso 1 1 calc R U . . . C37 C 0.4270(5) 0.8465(4) 0.9174(2) 0.0297(10) Uani 1 1 d . . . . . H37 H 0.396056 0.876178 0.966337 0.036 Uiso 1 1 calc R U . . . C38 C 0.5447(4) 0.8493(4) 0.8792(2) 0.0239(9) Uani 1 1 d . . . . . C39 C 0.6192(4) 0.9014(4) 0.9130(3) 0.0290(10) Uani 1 1 d . . . . . C40 C 0.5877(4) 0.8089(4) 0.8069(2) 0.0215(8) Uani 1 1 d . . . . . H40 H 0.667786 0.811110 0.780706 0.026 Uiso 1 1 calc R U . . . C41 C 0.5143(4) 0.7652(3) 0.7728(2) 0.0198(8) Uani 1 1 d . . . . . H41 H 0.543733 0.740651 0.722510 0.024 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1A 0.0755(14) 0.0771(14) 0.0698(13) -0.0235(11) -0.0078(11) -0.0120(11) Cl2A 0.0682(15) 0.115(2) 0.144(3) -0.0479(19) 0.0123(15) -0.0508(15) C42A 0.062(5) 0.080(6) 0.061(5) -0.003(4) -0.018(4) -0.031(4) Cl1B 0.0755(14) 0.0771(14) 0.0698(13) -0.0235(11) -0.0078(11) -0.0120(11) Cl2B 0.0682(15) 0.115(2) 0.144(3) -0.0479(19) 0.0123(15) -0.0508(15) C42B 0.062(5) 0.080(6) 0.061(5) -0.003(4) -0.018(4) -0.031(4) Cl3 0.053(4) 0.041(2) 0.073(3) -0.0001(19) 0.002(3) -0.014(3) Cl4 0.0351(13) 0.0520(15) 0.0400(13) -0.0153(11) -0.0011(10) -0.0193(12) C43 0.034(6) 0.046(6) 0.048(6) -0.008(5) -0.013(5) -0.001(5) Pd1 0.01961(17) 0.01101(15) 0.01635(15) -0.00393(10) -0.00037(11) -0.00767(11) Br1 0.0370(3) 0.0117(2) 0.0613(3) -0.0042(2) -0.0174(2) -0.00949(19) P1 0.0181(5) 0.0129(5) 0.0103(4) -0.0016(3) -0.0016(4) -0.0061(4) O1 0.0360(18) 0.0081(13) 0.0428(18) 0.0008(12) -0.0172(15) -0.0039(12) O2 0.0196(15) 0.0212(15) 0.0266(15) -0.0021(12) -0.0077(12) -0.0063(12) O3 0.0291(17) 0.0257(16) 0.0299(16) -0.0069(13) -0.0133(13) -0.0058(13) O4 0.0270(17) 0.0283(16) 0.0288(16) -0.0111(13) -0.0101(13) 0.0018(13) N1 0.041(3) 0.045(3) 0.052(3) -0.019(2) -0.022(2) -0.009(2) C1 0.025(2) 0.0119(17) 0.0116(17) -0.0001(14) -0.0019(15) -0.0098(16) C2 0.029(2) 0.0129(19) 0.024(2) 0.0015(15) -0.0095(17) -0.0030(17) C3 0.042(3) 0.015(2) 0.073(4) 0.000(2) -0.024(3) -0.002(2) C4 0.038(3) 0.013(2) 0.036(2) -0.0014(17) -0.013(2) -0.0115(19) C5 0.032(2) 0.018(2) 0.029(2) -0.0042(17) -0.0090(18) -0.0125(18) C6 0.023(2) 0.0141(18) 0.0163(18) 0.0006(14) -0.0004(15) -0.0071(16) C7 0.024(2) 0.037(3) 0.047(3) -0.001(2) -0.015(2) -0.015(2) C8 0.0208(19) 0.0096(17) 0.0113(16) -0.0027(13) 0.0012(14) -0.0080(15) C9 0.0171(19) 0.0119(17) 0.0179(18) -0.0023(14) -0.0013(15) -0.0050(15) C10 0.021(2) 0.0134(18) 0.0152(18) -0.0010(14) -0.0002(15) -0.0066(15) C11 0.020(2) 0.0174(19) 0.0160(18) -0.0012(15) 0.0024(15) -0.0046(16) C12 0.029(2) 0.022(2) 0.0157(19) -0.0018(16) 0.0042(16) -0.0135(18) C13 0.029(2) 0.036(2) 0.019(2) -0.0094(18) 0.0029(17) -0.016(2) C14 0.025(2) 0.0142(18) 0.0174(19) 0.0033(15) -0.0038(16) -0.0072(16) C15 0.021(2) 0.0129(18) 0.025(2) -0.0031(15) -0.0011(16) -0.0027(16) C16 0.027(2) 0.0154(19) 0.026(2) -0.0018(16) -0.0002(18) 0.0012(17) C17 0.035(3) 0.013(2) 0.047(3) 0.0009(19) -0.001(2) -0.0031(19) C18 0.032(3) 0.022(2) 0.038(3) 0.0019(19) -0.013(2) 0.0047(19) C19 0.019(2) 0.0135(18) 0.0181(18) -0.0056(14) 0.0018(15) -0.0035(15) C20 0.020(2) 0.0140(18) 0.0148(18) -0.0037(14) -0.0019(15) -0.0059(15) C21 0.020(2) 0.0143(18) 0.0175(19) -0.0023(15) 0.0014(15) -0.0023(15) C22 0.033(2) 0.034(2) 0.0146(19) -0.0017(17) 0.0013(17) -0.009(2) C23 0.032(2) 0.035(3) 0.020(2) 0.0018(18) 0.0043(18) -0.019(2) C24 0.021(2) 0.0189(19) 0.0127(17) -0.0044(15) 0.0026(15) -0.0049(16) C25 0.026(2) 0.025(2) 0.0167(19) -0.0019(16) 0.0005(16) -0.0083(18) C26 0.033(2) 0.021(2) 0.022(2) -0.0076(17) -0.0030(18) -0.0015(19) C27 0.022(2) 0.021(2) 0.021(2) -0.0013(16) -0.0017(16) -0.0064(17) C28 0.022(2) 0.021(2) 0.021(2) -0.0056(16) -0.0077(17) -0.0030(17) C29 0.041(3) 0.030(2) 0.033(2) 0.002(2) -0.019(2) -0.007(2) C30 0.038(3) 0.044(3) 0.039(3) -0.008(2) -0.022(2) 0.001(2) C31 0.028(2) 0.019(2) 0.0181(19) 0.0023(15) -0.0103(17) -0.0048(17) C32 0.024(2) 0.024(2) 0.0137(18) 0.0013(15) -0.0058(16) -0.0075(17) C33 0.031(2) 0.034(2) 0.018(2) -0.0069(18) -0.0076(18) -0.003(2) C34 0.028(2) 0.036(3) 0.021(2) 0.0107(18) -0.0055(18) -0.012(2) C35 0.031(2) 0.0174(19) 0.0193(19) -0.0034(15) -0.0056(17) -0.0137(17) C36 0.044(3) 0.036(3) 0.025(2) -0.0114(19) 0.005(2) -0.028(2) C37 0.047(3) 0.026(2) 0.022(2) -0.0054(18) -0.006(2) -0.019(2) C38 0.034(2) 0.0148(19) 0.026(2) -0.0007(16) -0.0154(19) -0.0063(18) C39 0.035(3) 0.021(2) 0.034(2) -0.0058(18) -0.015(2) -0.0027(19) C40 0.023(2) 0.0163(19) 0.027(2) -0.0007(16) -0.0076(17) -0.0062(16) C41 0.026(2) 0.0167(19) 0.0170(19) -0.0020(15) -0.0063(16) -0.0052(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1A C42A 1.784(7) . ? Cl2A C42A 1.732(7) . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? Cl1B C42B 1.753(17) . ? Cl2B Cl2B 1.36(4) 2_656 ? Cl2B C42B 1.751(17) . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? Cl3 C43 1.791(12) . ? Cl4 C43 1.722(11) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? Pd1 C35 2.024(4) . ? Pd1 P1 2.3230(10) . ? Pd1 C9 2.464(4) . ? Pd1 Br1 2.4641(6) . ? P1 C1 1.838(4) . ? P1 C24 1.897(4) . ? P1 C32 1.905(4) . ? O1 C2 1.362(5) . ? O1 C3 1.446(5) . ? O2 C6 1.376(5) . ? O2 C7 1.429(5) . ? O3 C29 1.431(5) . ? O3 C28 1.434(5) . ? O4 C30 1.414(5) . ? O4 C28 1.434(5) . ? N1 C39 1.150(6) . ? C1 C8 1.406(5) . ? C1 C2 1.410(5) . ? C2 C4 1.373(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C8 1.402(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.518(5) . ? C9 C10 1.421(5) . ? C9 C20 1.430(5) . ? C10 C14 1.393(5) . ? C10 C11 1.523(5) . ? C11 C13 1.520(6) . ? C11 C12 1.534(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.401(5) . ? C14 H14 0.9500 . ? C15 C19 1.378(5) . ? C15 C16 1.530(5) . ? C16 C18 1.516(6) . ? C16 C17 1.535(6) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 C21 1.520(5) . ? C21 C23 1.535(6) . ? C21 C22 1.536(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.540(5) . ? C24 C26 1.541(5) . ? C24 C27 1.545(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.537(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C31 1.515(6) . ? C29 C30 1.475(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.539(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.531(6) . ? C32 C34 1.540(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C41 1.398(6) . ? C35 C36 1.399(6) . ? C36 C37 1.395(6) . ? C36 H36 0.9500 . ? C37 C38 1.392(6) . ? C37 H37 0.9500 . ? C38 C40 1.386(6) . ? C38 C39 1.454(6) . ? C40 C41 1.385(6) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2A C42A Cl1A 111.0(5) . . ? Cl2A C42A H42A 109.4 . . ? Cl1A C42A H42A 109.4 . . ? Cl2A C42A H42B 109.4 . . ? Cl1A C42A H42B 109.4 . . ? H42A C42A H42B 108.0 . . ? Cl2B Cl2B C42B 139(2) 2_656 . ? Cl2B C42B Cl1B 104.6(14) . . ? Cl2B C42B H42C 110.8 . . ? Cl1B C42B H42C 110.8 . . ? Cl2B C42B H42D 110.8 . . ? Cl1B C42B H42D 110.8 . . ? H42C C42B H42D 108.9 . . ? Cl4 C43 Cl3 113.2(6) . . ? Cl4 C43 H43A 108.9 . . ? Cl3 C43 H43A 108.9 . . ? Cl4 C43 H43B 108.9 . . ? Cl3 C43 H43B 108.9 . . ? H43A C43 H43B 107.8 . . ? C35 Pd1 P1 97.30(12) . . ? C35 Pd1 C9 176.74(14) . . ? P1 Pd1 C9 83.09(9) . . ? C35 Pd1 Br1 80.29(11) . . ? P1 Pd1 Br1 172.43(3) . . ? C9 Pd1 Br1 99.72(9) . . ? C1 P1 C24 107.45(17) . . ? C1 P1 C32 109.31(17) . . ? C24 P1 C32 104.24(17) . . ? C1 P1 Pd1 105.47(12) . . ? C24 P1 Pd1 110.41(12) . . ? C32 P1 Pd1 119.50(13) . . ? C2 O1 C3 118.2(4) . . ? C6 O2 C7 116.5(3) . . ? C29 O3 C28 106.4(3) . . ? C30 O4 C28 108.3(3) . . ? C8 C1 C2 118.3(3) . . ? C8 C1 P1 117.6(3) . . ? C2 C1 P1 124.1(3) . . ? O1 C2 C4 122.5(4) . . ? O1 C2 C1 116.1(4) . . ? C4 C2 C1 121.5(4) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 120.0(4) . . ? C2 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? O2 C6 C5 123.2(4) . . ? O2 C6 C8 116.0(3) . . ? C5 C6 C8 120.7(4) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C1 119.6(3) . . ? C6 C8 C9 114.3(3) . . ? C1 C8 C9 126.0(3) . . ? C10 C9 C20 119.0(3) . . ? C10 C9 C8 117.6(3) . . ? C20 C9 C8 117.8(3) . . ? C10 C9 Pd1 96.9(2) . . ? C20 C9 Pd1 89.1(2) . . ? C8 C9 Pd1 107.7(2) . . ? C14 C10 C9 119.0(3) . . ? C14 C10 C11 119.3(3) . . ? C9 C10 C11 121.7(3) . . ? C13 C11 C10 112.4(3) . . ? C13 C11 C12 110.4(3) . . ? C10 C11 C12 111.3(3) . . ? C13 C11 H11 107.5 . . ? C10 C11 H11 107.5 . . ? C12 C11 H11 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 121.7(3) . . ? C10 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C19 C15 C14 118.7(4) . . ? C19 C15 C16 120.8(4) . . ? C14 C15 C16 120.6(4) . . ? C18 C16 C15 110.8(4) . . ? C18 C16 C17 110.6(4) . . ? C15 C16 C17 111.9(4) . . ? C18 C16 H16 107.8 . . ? C15 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 122.2(3) . . ? C15 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C9 119.3(3) . . ? C19 C20 C21 119.7(3) . . ? C9 C20 C21 120.7(3) . . ? C20 C21 C23 110.8(3) . . ? C20 C21 C22 112.3(3) . . ? C23 C21 C22 110.6(3) . . ? C20 C21 H21 107.6 . . ? C23 C21 H21 107.6 . . ? C22 C21 H21 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 105.3(3) . . ? C25 C24 C27 110.2(3) . . ? C26 C24 C27 110.7(3) . . ? C25 C24 P1 107.8(3) . . ? C26 C24 P1 118.6(3) . . ? C27 C24 P1 104.2(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C24 115.8(3) . . ? C28 C27 H27A 108.3 . . ? C24 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? C24 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? O4 C28 O3 106.0(3) . . ? O4 C28 C31 108.1(3) . . ? O3 C28 C31 111.7(3) . . ? O4 C28 C27 110.8(3) . . ? O3 C28 C27 105.1(3) . . ? C31 C28 C27 114.8(3) . . ? O3 C29 C30 103.0(4) . . ? O3 C29 H29A 111.2 . . ? C30 C29 H29A 111.2 . . ? O3 C29 H29B 111.2 . . ? C30 C29 H29B 111.2 . . ? H29A C29 H29B 109.1 . . ? O4 C30 C29 104.8(4) . . ? O4 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? O4 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? H30A C30 H30B 108.9 . . ? C28 C31 C32 117.4(3) . . ? C28 C31 H31A 107.9 . . ? C32 C31 H31A 107.9 . . ? C28 C31 H31B 107.9 . . ? C32 C31 H31B 107.9 . . ? H31A C31 H31B 107.2 . . ? C33 C32 C31 109.9(3) . . ? C33 C32 C34 105.8(3) . . ? C31 C32 C34 109.4(3) . . ? C33 C32 P1 109.7(3) . . ? C31 C32 P1 110.9(3) . . ? C34 C32 P1 110.9(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 C35 C36 117.6(4) . . ? C41 C35 Pd1 125.8(3) . . ? C36 C35 Pd1 116.1(3) . . ? C37 C36 C35 121.4(4) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 119.6(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C40 C38 C37 119.7(4) . . ? C40 C38 C39 120.1(4) . . ? C37 C38 C39 120.1(4) . . ? N1 C39 C38 178.7(5) . . ? C41 C40 C38 120.3(4) . . ? C41 C40 H40 119.9 . . ? C38 C40 H40 119.9 . . ? C40 C41 C35 121.3(4) . . ? C40 C41 H41 119.3 . . ? C35 C41 H41 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2B Cl2B C42B Cl1B 70(4) 2_656 . . . ? C24 P1 C1 C8 -117.2(3) . . . . ? C32 P1 C1 C8 130.3(3) . . . . ? Pd1 P1 C1 C8 0.6(3) . . . . ? C24 P1 C1 C2 61.9(4) . . . . ? C32 P1 C1 C2 -50.6(4) . . . . ? Pd1 P1 C1 C2 179.7(3) . . . . ? C3 O1 C2 C4 15.0(6) . . . . ? C3 O1 C2 C1 -166.1(4) . . . . ? C8 C1 C2 O1 -176.9(3) . . . . ? P1 C1 C2 O1 3.9(5) . . . . ? C8 C1 C2 C4 2.0(6) . . . . ? P1 C1 C2 C4 -177.1(3) . . . . ? O1 C2 C4 C5 177.4(4) . . . . ? C1 C2 C4 C5 -1.5(7) . . . . ? C2 C4 C5 C6 -0.1(7) . . . . ? C7 O2 C6 C5 -11.7(5) . . . . ? C7 O2 C6 C8 169.6(3) . . . . ? C4 C5 C6 O2 -177.4(4) . . . . ? C4 C5 C6 C8 1.2(6) . . . . ? O2 C6 C8 C1 178.0(3) . . . . ? C5 C6 C8 C1 -0.6(6) . . . . ? O2 C6 C8 C9 -0.7(5) . . . . ? C5 C6 C8 C9 -179.3(3) . . . . ? C2 C1 C8 C6 -0.9(5) . . . . ? P1 C1 C8 C6 178.2(3) . . . . ? C2 C1 C8 C9 177.6(3) . . . . ? P1 C1 C8 C9 -3.3(5) . . . . ? C6 C8 C9 C10 -69.5(4) . . . . ? C1 C8 C9 C10 112.0(4) . . . . ? C6 C8 C9 C20 83.9(4) . . . . ? C1 C8 C9 C20 -94.7(5) . . . . ? C6 C8 C9 Pd1 -177.5(2) . . . . ? C1 C8 C9 Pd1 3.9(4) . . . . ? C20 C9 C10 C14 -2.8(6) . . . . ? C8 C9 C10 C14 150.2(4) . . . . ? Pd1 C9 C10 C14 -95.6(4) . . . . ? C20 C9 C10 C11 179.3(4) . . . . ? C8 C9 C10 C11 -27.7(5) . . . . ? Pd1 C9 C10 C11 86.5(4) . . . . ? C14 C10 C11 C13 -69.0(5) . . . . ? C9 C10 C11 C13 109.0(4) . . . . ? C14 C10 C11 C12 55.5(5) . . . . ? C9 C10 C11 C12 -126.6(4) . . . . ? C9 C10 C14 C15 1.3(6) . . . . ? C11 C10 C14 C15 179.3(4) . . . . ? C10 C14 C15 C19 2.1(6) . . . . ? C10 C14 C15 C16 -177.4(4) . . . . ? C19 C15 C16 C18 -112.7(5) . . . . ? C14 C15 C16 C18 66.8(5) . . . . ? C19 C15 C16 C17 123.5(4) . . . . ? C14 C15 C16 C17 -57.0(6) . . . . ? C14 C15 C19 C20 -4.1(6) . . . . ? C16 C15 C19 C20 175.4(4) . . . . ? C15 C19 C20 C9 2.6(6) . . . . ? C15 C19 C20 C21 -171.2(4) . . . . ? C10 C9 C20 C19 0.9(6) . . . . ? C8 C9 C20 C19 -152.1(4) . . . . ? Pd1 C9 C20 C19 98.3(3) . . . . ? C10 C9 C20 C21 174.7(4) . . . . ? C8 C9 C20 C21 21.7(5) . . . . ? Pd1 C9 C20 C21 -88.0(3) . . . . ? C19 C20 C21 C23 69.5(5) . . . . ? C9 C20 C21 C23 -104.2(4) . . . . ? C19 C20 C21 C22 -54.7(5) . . . . ? C9 C20 C21 C22 131.5(4) . . . . ? C1 P1 C24 C25 89.1(3) . . . . ? C32 P1 C24 C25 -154.9(3) . . . . ? Pd1 P1 C24 C25 -25.4(3) . . . . ? C1 P1 C24 C26 -30.2(3) . . . . ? C32 P1 C24 C26 85.7(3) . . . . ? Pd1 P1 C24 C26 -144.8(3) . . . . ? C1 P1 C24 C27 -153.8(2) . . . . ? C32 P1 C24 C27 -37.8(3) . . . . ? Pd1 P1 C24 C27 91.7(2) . . . . ? C25 C24 C27 C28 -173.3(3) . . . . ? C26 C24 C27 C28 -57.2(4) . . . . ? P1 C24 C27 C28 71.3(4) . . . . ? C30 O4 C28 O3 -0.1(5) . . . . ? C30 O4 C28 C31 -120.0(4) . . . . ? C30 O4 C28 C27 113.4(4) . . . . ? C29 O3 C28 O4 -20.9(4) . . . . ? C29 O3 C28 C31 96.6(4) . . . . ? C29 O3 C28 C27 -138.3(3) . . . . ? C24 C27 C28 O4 83.7(4) . . . . ? C24 C27 C28 O3 -162.3(3) . . . . ? C24 C27 C28 C31 -39.2(5) . . . . ? C28 O3 C29 C30 32.8(5) . . . . ? C28 O4 C30 C29 20.3(5) . . . . ? O3 C29 C30 O4 -32.5(5) . . . . ? O4 C28 C31 C32 -156.7(3) . . . . ? O3 C28 C31 C32 87.1(4) . . . . ? C27 C28 C31 C32 -32.4(5) . . . . ? C28 C31 C32 C33 -65.1(4) . . . . ? C28 C31 C32 C34 179.1(3) . . . . ? C28 C31 C32 P1 56.5(4) . . . . ? C41 C35 C36 C37 -2.2(7) . . . . ? Pd1 C35 C36 C37 -174.8(4) . . . . ? C35 C36 C37 C38 -0.4(7) . . . . ? C36 C37 C38 C40 1.7(6) . . . . ? C36 C37 C38 C39 177.9(4) . . . . ? C37 C38 C40 C41 -0.4(6) . . . . ? C39 C38 C40 C41 -176.5(4) . . . . ? C38 C40 C41 C35 -2.4(6) . . . . ? C36 C35 C41 C40 3.6(6) . . . . ? Pd1 C35 C41 C40 175.4(3) . . . . ? _refine_diff_density_max 1.361 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.115 _shelx_res_file ; TITL XRAY5702_0m_a.res in P-1 XRAY5702_0m_a.res created by SHELXL-2016/6 at 14:44:16 on 11-Mar-2019 CELL 0.71073 11.5424 11.5479 17.9977 81.507 77.635 72.621 ZERR 2.000 0.0020 0.0020 0.0031 0.002 0.002 0.002 LATT 1 SFAC C H N O P Br Pd Cl UNIT 85 116 2 8 2 2 2 6 OMIT -1 -1 7 OMIT 0 0 1 OMIT 1 1 1 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 CONF WPDB EADP CL2A CL2B EADP Cl1A Cl1B EADP C42A C42B SADI CL1A CL2A CL1B CL2B SADI CL1A C42A CL2A C42A CL1B C42B CL2B C42B SIZE 0.030 0.100 0.150 TEMP -173.0 WGHT 0.100000 0.205470 FVAR 0.35106 0.86877 PART 1 MOLE 2 CL1A 8 0.176045 0.214074 0.506618 21.00000 0.07547 0.07707 = 0.06976 -0.02350 -0.00780 -0.01204 CL2A 8 0.427480 0.165829 0.529873 21.00000 0.06819 0.11457 = 0.14412 -0.04789 0.01230 -0.05084 C42A 1 0.306689 0.102953 0.535858 21.00000 0.06211 0.07993 = 0.06132 -0.00273 -0.01782 -0.03110 AFIX 23 H42A 2 0.283396 0.069926 0.589138 21.00000 -1.20000 H42B 2 0.333575 0.034769 0.502951 21.00000 -1.20000 PART 2 AFIX 0 CL1B 8 0.284440 0.241194 0.493287 -21.00000 0.07547 0.07707 = 0.06976 -0.02350 -0.00780 -0.01204 CL2B 8 0.479217 0.033195 0.468621 -21.00000 0.06819 0.11457 = 0.14412 -0.04789 0.01230 -0.05084 C42B 1 0.338329 0.113377 0.440753 -21.00000 0.06211 0.07993 = 0.06132 -0.00273 -0.01782 -0.03110 AFIX 23 H42C 2 0.279588 0.063019 0.453096 -21.00000 -1.20000 H42D 2 0.350282 0.138191 0.385219 -21.00000 -1.20000 PART -1 AFIX 0 MOLE 3 CL3 8 1.026877 0.990081 -0.007898 10.50000 0.05281 0.04064 = 0.07291 -0.00015 0.00183 -0.01357 CL4 8 0.904094 0.826811 0.098643 10.50000 0.03505 0.05205 = 0.03999 -0.01535 -0.00106 -0.01933 C43 1 0.886937 0.970113 0.051243 10.50000 0.03407 0.04563 = 0.04757 -0.00757 -0.01285 -0.00142 AFIX 23 H43A 2 0.857190 1.031222 0.089214 10.50000 -1.20000 H43B 2 0.823286 0.985427 0.019093 10.50000 -1.20000 PART 0 AFIX 0 MOLE 1 PD1 7 0.275548 0.706108 0.766138 11.00000 0.01961 0.01101 = 0.01635 -0.00393 -0.00037 -0.00767 BR1 6 0.205552 0.928629 0.737179 11.00000 0.03705 0.01172 = 0.06134 -0.00417 -0.01735 -0.00949 P1 5 0.364016 0.497037 0.780871 11.00000 0.01814 0.01290 = 0.01030 -0.00158 -0.00163 -0.00609 O1 4 0.381144 0.228959 0.775833 11.00000 0.03598 0.00806 = 0.04282 0.00080 -0.01722 -0.00390 O2 4 -0.020455 0.543633 0.667128 11.00000 0.01957 0.02125 = 0.02658 -0.00205 -0.00769 -0.00628 O3 4 0.684884 0.397205 0.884343 11.00000 0.02910 0.02567 = 0.02994 -0.00690 -0.01325 -0.00579 O4 4 0.721766 0.247313 0.805025 11.00000 0.02703 0.02833 = 0.02882 -0.01110 -0.01010 0.00180 N1 3 0.679658 0.942621 0.938525 11.00000 0.04088 0.04517 = 0.05192 -0.01883 -0.02236 -0.00925 C1 1 0.262564 0.428626 0.746649 11.00000 0.02548 0.01187 = 0.01162 -0.00007 -0.00191 -0.00983 C2 1 0.283119 0.302244 0.745306 11.00000 0.02869 0.01286 = 0.02360 0.00150 -0.00951 -0.00298 C3 1 0.423606 0.102190 0.760559 11.00000 0.04224 0.01477 = 0.07270 0.00032 -0.02355 -0.00174 AFIX 137 H3A 2 0.368583 0.057756 0.793407 11.00000 -1.50000 H3B 2 0.507579 0.067053 0.771038 11.00000 -1.50000 H3C 2 0.423430 0.095853 0.706884 11.00000 -1.50000 AFIX 0 C4 1 0.206991 0.256768 0.715921 11.00000 0.03844 0.01342 = 0.03622 -0.00142 -0.01293 -0.01145 AFIX 43 H4 2 0.223787 0.171349 0.714465 11.00000 -1.20000 AFIX 0 C5 1 0.105194 0.335810 0.688259 11.00000 0.03237 0.01786 = 0.02867 -0.00415 -0.00897 -0.01255 AFIX 43 H5 2 0.052517 0.304448 0.667838 11.00000 -1.20000 AFIX 0 C6 1 0.080874 0.460212 0.690566 11.00000 0.02250 0.01406 = 0.01629 0.00057 -0.00043 -0.00706 C7 1 -0.088872 0.499066 0.626037 11.00000 0.02368 0.03736 = 0.04704 -0.00076 -0.01531 -0.01508 AFIX 137 H7A 2 -0.033530 0.460141 0.581797 11.00000 -1.50000 H7B 2 -0.154351 0.567053 0.608603 11.00000 -1.50000 H7C 2 -0.125669 0.439428 0.659522 11.00000 -1.50000 AFIX 0 C8 1 0.159010 0.508023 0.719229 11.00000 0.02083 0.00957 = 0.01133 -0.00270 0.00124 -0.00800 C9 1 0.118917 0.645786 0.718754 11.00000 0.01705 0.01188 = 0.01794 -0.00228 -0.00127 -0.00504 C10 1 0.127848 0.715236 0.646712 11.00000 0.02100 0.01343 = 0.01525 -0.00099 -0.00017 -0.00662 C11 1 0.222577 0.665503 0.577794 11.00000 0.01955 0.01744 = 0.01601 -0.00118 0.00243 -0.00463 AFIX 13 H11 2 0.279685 0.587906 0.596185 11.00000 -1.20000 AFIX 0 C12 1 0.300428 0.753388 0.542417 11.00000 0.02901 0.02227 = 0.01574 -0.00177 0.00418 -0.01351 AFIX 137 H12A 2 0.248084 0.828161 0.520195 11.00000 -1.50000 H12B 2 0.366974 0.714838 0.502399 11.00000 -1.50000 H12C 2 0.335976 0.773326 0.582048 11.00000 -1.50000 AFIX 0 C13 1 0.163840 0.635669 0.517712 11.00000 0.02908 0.03564 = 0.01881 -0.00943 0.00286 -0.01635 AFIX 137 H13A 2 0.120577 0.573963 0.540005 11.00000 -1.50000 H13B 2 0.228132 0.604229 0.474592 11.00000 -1.50000 H13C 2 0.104948 0.709581 0.499807 11.00000 -1.50000 AFIX 0 C14 1 0.045095 0.830190 0.638516 11.00000 0.02536 0.01424 = 0.01745 0.00328 -0.00381 -0.00716 AFIX 43 H14 2 0.049755 0.876040 0.590125 11.00000 -1.20000 AFIX 0 C15 1 -0.044790 0.879935 0.699749 11.00000 0.02052 0.01286 = 0.02500 -0.00313 -0.00112 -0.00271 C16 1 -0.137854 1.004107 0.688252 11.00000 0.02674 0.01535 = 0.02620 -0.00185 -0.00022 0.00120 AFIX 13 H16 2 -0.188678 1.025702 0.739304 11.00000 -1.20000 AFIX 0 C17 1 -0.073736 1.104518 0.656147 11.00000 0.03504 0.01342 = 0.04668 0.00088 -0.00139 -0.00310 AFIX 137 H17A 2 -0.025140 1.086779 0.605318 11.00000 -1.50000 H17B 2 -0.019085 1.107618 0.690202 11.00000 -1.50000 H17C 2 -0.136059 1.183243 0.652431 11.00000 -1.50000 AFIX 0 C18 1 -0.224286 0.998397 0.637067 11.00000 0.03186 0.02211 = 0.03781 0.00191 -0.01287 0.00474 AFIX 137 H18A 2 -0.177668 0.983712 0.585412 11.00000 -1.50000 H18B 2 -0.288981 1.075794 0.635358 11.00000 -1.50000 H18C 2 -0.262072 0.931994 0.657349 11.00000 -1.50000 AFIX 0 C19 1 -0.048206 0.814389 0.770289 11.00000 0.01902 0.01350 = 0.01807 -0.00560 0.00179 -0.00353 AFIX 43 H19 2 -0.105436 0.850115 0.812661 11.00000 -1.20000 AFIX 0 C20 1 0.028941 0.698247 0.781489 11.00000 0.01996 0.01399 = 0.01482 -0.00368 -0.00189 -0.00594 C21 1 0.008607 0.623456 0.857583 11.00000 0.02039 0.01431 = 0.01748 -0.00234 0.00139 -0.00229 AFIX 13 H21 2 0.078991 0.547676 0.856775 11.00000 -1.20000 AFIX 0 C22 1 0.007286 0.690896 0.925355 11.00000 0.03273 0.03356 = 0.01462 -0.00174 0.00133 -0.00893 AFIX 137 H22A 2 0.083982 0.714731 0.917656 11.00000 -1.50000 H22B 2 0.000281 0.637141 0.972633 11.00000 -1.50000 H22C 2 -0.063248 0.763836 0.929009 11.00000 -1.50000 AFIX 0 C23 1 -0.110602 0.584876 0.868210 11.00000 0.03240 0.03534 = 0.01983 0.00178 0.00431 -0.01866 AFIX 137 H23A 2 -0.117755 0.530206 0.915059 11.00000 -1.50000 H23B 2 -0.108417 0.542529 0.824371 11.00000 -1.50000 H23C 2 -0.181735 0.657265 0.871987 11.00000 -1.50000 AFIX 0 C24 1 0.521207 0.453716 0.716988 11.00000 0.02103 0.01892 = 0.01267 -0.00445 0.00256 -0.00494 C25 1 0.522527 0.552091 0.649184 11.00000 0.02600 0.02486 = 0.01674 -0.00191 0.00048 -0.00828 AFIX 137 H25A 2 0.477420 0.632283 0.667061 11.00000 -1.50000 H25B 2 0.482985 0.535348 0.610452 11.00000 -1.50000 H25C 2 0.608015 0.551227 0.626903 11.00000 -1.50000 AFIX 0 C26 1 0.562293 0.331673 0.680825 11.00000 0.03336 0.02146 = 0.02227 -0.00757 -0.00300 -0.00152 AFIX 137 H26A 2 0.640608 0.325611 0.645196 11.00000 -1.50000 H26B 2 0.499259 0.327571 0.653236 11.00000 -1.50000 H26C 2 0.573144 0.264217 0.721042 11.00000 -1.50000 AFIX 0 C27 1 0.612113 0.457382 0.767766 11.00000 0.02233 0.02123 = 0.02065 -0.00130 -0.00171 -0.00637 AFIX 23 H27A 2 0.693172 0.454792 0.734729 11.00000 -1.20000 H27B 2 0.582072 0.536293 0.790585 11.00000 -1.20000 AFIX 0 C28 1 0.631392 0.354592 0.832527 11.00000 0.02248 0.02140 = 0.02116 -0.00559 -0.00765 -0.00295 C29 1 0.779998 0.295292 0.907761 11.00000 0.04149 0.03021 = 0.03285 0.00169 -0.01936 -0.00683 AFIX 23 H29A 2 0.746374 0.245530 0.951982 11.00000 -1.20000 H29B 2 0.846020 0.322146 0.921351 11.00000 -1.20000 AFIX 0 C30 1 0.826193 0.226914 0.839439 11.00000 0.03803 0.04381 = 0.03888 -0.00758 -0.02161 0.00110 AFIX 23 H30A 2 0.891389 0.257493 0.804287 11.00000 -1.20000 H30B 2 0.860216 0.138986 0.853845 11.00000 -1.20000 AFIX 0 C31 1 0.515758 0.319175 0.872479 11.00000 0.02798 0.01881 = 0.01808 0.00234 -0.01032 -0.00482 AFIX 23 H31A 2 0.527588 0.283456 0.924736 11.00000 -1.20000 H31B 2 0.507891 0.254182 0.845251 11.00000 -1.20000 AFIX 0 C32 1 0.392881 0.420250 0.879008 11.00000 0.02375 0.02395 = 0.01369 0.00132 -0.00583 -0.00750 C33 1 0.394366 0.515154 0.929619 11.00000 0.03054 0.03366 = 0.01783 -0.00694 -0.00758 -0.00310 AFIX 137 H33A 2 0.405775 0.475901 0.980678 11.00000 -1.50000 H33B 2 0.315920 0.579247 0.933446 11.00000 -1.50000 H33C 2 0.462353 0.551065 0.907131 11.00000 -1.50000 AFIX 0 C34 1 0.287066 0.365667 0.920054 11.00000 0.02763 0.03634 = 0.02106 0.01066 -0.00551 -0.01177 AFIX 137 H34A 2 0.283902 0.301443 0.891145 11.00000 -1.50000 H34B 2 0.208599 0.429717 0.923653 11.00000 -1.50000 H34C 2 0.301348 0.331101 0.971491 11.00000 -1.50000 AFIX 0 C35 1 0.397819 0.756460 0.810944 11.00000 0.03063 0.01743 = 0.01930 -0.00341 -0.00562 -0.01373 C36 1 0.354838 0.799948 0.883208 11.00000 0.04400 0.03610 = 0.02485 -0.01143 0.00520 -0.02794 AFIX 43 H36 2 0.274788 0.797701 0.909578 11.00000 -1.20000 AFIX 0 C37 1 0.427020 0.846544 0.917374 11.00000 0.04744 0.02648 = 0.02204 -0.00538 -0.00562 -0.01920 AFIX 43 H37 2 0.396056 0.876178 0.966337 11.00000 -1.20000 AFIX 0 C38 1 0.544676 0.849316 0.879244 11.00000 0.03426 0.01477 = 0.02650 -0.00070 -0.01542 -0.00630 C39 1 0.619173 0.901449 0.913042 11.00000 0.03462 0.02062 = 0.03377 -0.00578 -0.01497 -0.00270 C40 1 0.587672 0.808861 0.806949 11.00000 0.02292 0.01625 = 0.02684 -0.00068 -0.00757 -0.00620 AFIX 43 H40 2 0.667786 0.811110 0.780706 11.00000 -1.20000 AFIX 0 C41 1 0.514300 0.765182 0.772834 11.00000 0.02646 0.01669 = 0.01699 -0.00199 -0.00630 -0.00519 AFIX 43 H41 2 0.543733 0.740651 0.722510 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5702_0m_a.res in P-1 REM R1 = 0.0475 for 7443 Fo > 4sig(Fo) and 0.0754 for all 10062 data REM 518 parameters refined using 7 restraints END WGHT 0.0613 3.7219 REM Highest difference peak 1.361, deepest hole -1.466, 1-sigma level 0.115 Q1 1 0.2591 0.9219 0.6923 11.00000 0.05 1.36 Q2 1 0.2204 0.6943 0.7942 11.00000 0.05 1.11 Q3 1 0.3372 0.7039 0.7336 11.00000 0.05 1.04 Q4 1 0.1407 0.9212 0.7832 11.00000 0.05 0.74 Q5 1 0.2807 0.7550 0.7847 11.00000 0.05 0.64 Q6 1 0.3596 0.1447 0.5132 11.00000 0.05 0.63 Q7 1 0.2613 0.6959 0.7284 11.00000 0.05 0.58 Q8 1 -0.1150 0.5210 0.8569 11.00000 0.05 0.56 Q9 1 -0.2800 1.1730 0.6962 11.00000 0.05 0.55 Q10 1 0.3763 0.7122 0.7811 11.00000 0.05 0.55 Q11 1 0.1247 0.7041 0.8122 11.00000 0.05 0.52 Q12 1 0.1708 0.6945 0.7523 11.00000 0.05 0.51 Q13 1 -0.1129 0.5825 0.6281 11.00000 0.05 0.50 Q14 1 0.4344 0.4770 0.7565 11.00000 0.05 0.49 Q15 1 0.2129 0.9452 0.7481 11.00000 0.05 0.49 Q16 1 0.2803 0.6426 0.9956 11.00000 0.05 0.48 Q17 1 0.2015 0.8027 0.8060 11.00000 0.05 0.48 Q18 1 0.3017 0.4637 0.7529 11.00000 0.05 0.48 Q19 1 0.3609 0.7202 0.7994 11.00000 0.05 0.48 Q20 1 0.2383 0.7324 0.8420 11.00000 0.05 0.47 ; _shelx_res_checksum 53603 _shelx_hkl_file ; -1 0 0 27.70 2.30 -1 0 0 23.90 1.90 1 0 0 22.70 2.00 -2 0 0 670.93 13.50 -2 0 0 708.83 11.70 2 0 0 726.63 14.40 -3 0 0 134.69 3.50 -3 0 0 136.69 7.90 -3 0 0 123.29 7.50 3 0 0 163.08 8.90 -4 0 0 184.48 9.30 -4 0 0 190.08 8.50 4 0 0 210.68 10.10 -5 0 0 34.70 5.50 -5 0 0 27.90 6.10 5 0 0 33.00 6.70 -6 0 0 118.69 9.70 -6 0 0 104.29 8.60 6 0 0 101.59 9.10 -7 0 0 70.19 7.80 -7 0 0 58.09 8.50 7 0 0 54.19 9.50 -8 0 0 14.60 7.50 8 0 0 37.80 10.20 -9 0 0 182.68 15.00 9 0 0 175.98 18.00 9 0 0 163.48 12.50 -10 0 0 177.88 16.00 10 0 0 163.68 15.30 10 0 0 194.18 13.70 -11 0 0 174.08 14.80 11 0 0 159.68 14.70 11 0 0 112.69 15.40 -12 0 0 144.09 15.40 12 0 0 121.69 17.30 12 0 0 138.49 13.00 -13 0 0 98.29 15.00 13 0 0 74.49 16.80 13 0 0 97.29 13.20 -14 0 0 53.49 16.00 14 0 0 36.00 17.50 14 0 0 58.89 14.40 13 -1 0 8.90 11.40 13 -1 0 -10.70 15.20 -13 1 0 5.50 12.60 12 -1 0 81.59 16.60 12 -1 0 74.19 12.30 -12 1 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-3.60 12.20 -6 -6 -21 54.89 13.60 6 6 21 59.19 13.30 6 6 21 56.09 13.80 -7 -6 -21 15.90 12.40 7 6 21 -9.90 12.00 7 6 21 7.50 12.10 -8 -6 -21 71.49 14.00 8 6 21 92.39 16.00 -1 -7 -21 20.40 13.00 1 7 21 4.40 13.80 -2 -7 -21 181.68 16.80 2 7 21 154.08 17.30 -3 -7 -21 24.70 13.00 3 7 21 -2.40 12.90 -4 -7 -21 38.80 13.60 4 7 21 33.40 13.70 -5 -7 -21 44.20 13.60 5 7 21 39.50 13.70 -6 -7 -21 40.40 13.40 6 7 21 22.80 12.90 -7 -7 -21 24.30 13.20 7 7 21 -5.00 12.00 8 7 21 14.20 13.20 -3 -8 -21 145.39 17.20 3 8 21 110.09 18.70 -4 -8 -21 41.40 13.90 4 8 21 19.40 14.10 -5 -8 -21 106.79 15.50 5 8 21 74.29 15.90 -6 -8 -21 35.30 14.90 6 8 21 10.90 13.10 0 2 -22 178.68 20.50 0 -2 22 189.18 19.60 -1 2 -22 4.60 14.10 1 -2 22 -6.30 12.80 -2 2 -22 123.09 17.80 2 -2 22 85.39 14.40 -3 2 -22 8.90 14.00 3 -2 22 -2.00 12.00 -4 2 -22 86.79 19.70 4 -2 22 85.59 14.40 1 1 -22 11.40 13.80 -1 -1 22 0.20 15.20 0 1 -22 30.30 14.60 0 -1 22 32.10 14.10 -1 1 -22 41.50 14.70 1 -1 22 28.20 13.60 -2 1 -22 28.20 14.00 2 -1 22 36.40 13.80 -3 1 -22 229.18 21.00 3 -1 22 199.78 17.80 -4 1 -22 -3.00 13.70 4 -1 22 21.50 12.30 -5 1 -22 112.89 17.90 5 -1 22 133.79 15.00 1 0 -22 11.60 13.50 -1 0 22 15.30 13.60 0 0 -22 95.19 16.20 0 0 22 66.69 15.20 -1 0 -22 3.90 12.90 1 0 22 -16.80 12.10 -2 0 -22 2.90 12.60 2 0 22 -4.80 12.00 -3 0 -22 22.20 13.90 3 0 22 17.00 12.80 -4 0 -22 7.70 13.50 4 0 22 20.70 12.60 -5 0 -22 0.70 13.50 5 0 22 6.20 11.40 -6 0 -22 169.88 19.50 -6 0 -22 167.58 16.00 6 0 22 149.59 15.50 1 -1 -22 4.30 12.80 -1 1 22 -3.10 13.10 0 -1 -22 57.99 14.80 0 1 22 42.90 14.60 -1 -1 -22 54.39 14.80 1 1 22 47.90 14.30 -2 -1 -22 9.90 12.70 2 1 22 0.30 13.30 -3 -1 -22 3.80 13.30 3 1 22 -11.90 11.90 -4 -1 -22 10.40 13.30 -4 -1 -22 22.60 11.20 4 1 22 8.40 12.20 -5 -1 -22 137.09 17.50 -5 -1 -22 134.09 14.80 5 1 22 108.19 14.80 -6 -1 -22 5.80 11.80 -6 -1 -22 6.70 14.40 6 1 22 -3.50 12.00 -7 -1 -22 84.29 14.80 7 1 22 78.19 15.70 1 -2 -22 138.39 17.10 -1 2 22 128.69 16.60 0 -2 -22 10.60 12.70 0 2 22 6.70 13.10 -1 -2 -22 127.09 16.30 1 2 22 109.99 15.50 -2 -2 -22 34.20 12.90 2 2 22 45.50 13.70 -3 -2 -22 49.60 12.20 -3 -2 -22 38.40 13.90 3 2 22 27.20 13.20 -4 -2 -22 32.60 14.10 -4 -2 -22 34.90 12.00 4 2 22 40.10 13.40 -5 -2 -22 5.00 13.50 -5 -2 -22 28.30 11.40 5 2 22 7.20 12.50 -6 -2 -22 -9.40 13.50 -6 -2 -22 -14.10 10.90 6 2 22 6.80 11.90 6 2 22 -19.10 11.40 -7 -2 -22 11.70 11.80 7 2 22 20.80 13.40 -1 3 22 29.00 14.80 0 -3 -22 70.19 14.60 0 3 22 59.19 14.40 -1 -3 -22 7.90 12.20 1 3 22 -21.70 11.50 -2 -3 -22 168.18 15.20 -2 -3 -22 146.49 16.80 2 3 22 137.49 15.90 -3 -3 -22 6.90 12.70 -3 -3 -22 17.30 10.90 3 3 22 2.60 12.30 -4 -3 -22 75.79 12.60 -4 -3 -22 74.29 15.50 4 3 22 59.29 13.70 -5 -3 -22 18.30 11.80 -5 -3 -22 14.00 13.50 5 3 22 2.10 12.00 -6 -3 -22 13.10 11.40 6 3 22 14.40 12.10 6 3 22 -8.70 11.40 -7 -3 -22 5.70 11.70 7 3 22 0.70 12.60 7 3 22 -6.70 13.70 0 -4 -22 -1.20 14.40 0 4 22 -11.50 12.60 -1 -4 -22 114.39 14.00 1 4 22 85.29 15.30 -2 -4 -22 9.20 11.50 -2 -4 -22 -19.30 11.80 2 4 22 -10.00 12.40 -3 -4 -22 137.89 15.00 -3 -4 -22 123.99 16.20 3 4 22 87.19 14.70 -4 -4 -22 12.20 12.90 -4 -4 -22 15.00 11.20 4 4 22 -4.70 11.60 -5 -4 -22 242.98 22.40 -5 -4 -22 238.98 20.30 5 4 22 192.88 16.60 -6 -4 -22 37.50 12.80 6 4 22 1.30 12.40 6 4 22 13.80 12.80 -7 -4 -22 36.80 12.70 7 4 22 33.30 13.90 7 4 22 30.20 12.10 -1 -5 -22 25.20 12.00 1 5 22 -6.30 12.90 -2 -5 -22 86.59 13.70 2 5 22 55.29 14.90 -3 -5 -22 17.30 12.00 3 5 22 -13.10 12.50 -4 -5 -22 2.30 11.60 -4 -5 -22 -5.50 11.50 4 5 22 -15.50 12.20 -5 -5 -22 31.00 12.80 5 5 22 0.80 12.50 5 5 22 33.30 12.70 -6 -5 -22 112.59 15.00 6 5 22 98.69 15.20 6 5 22 69.39 14.10 -7 -5 -22 83.19 14.70 7 5 22 47.80 14.60 7 5 22 46.20 12.90 -2 -6 -22 21.30 12.40 2 6 22 -7.50 15.20 -3 -6 -22 23.00 12.90 3 6 22 4.10 13.50 -4 -6 -22 -2.50 12.50 4 6 22 -14.90 12.80 -5 -6 -22 66.39 14.00 5 6 22 71.09 14.90 -6 -6 -22 31.40 13.40 6 6 22 2.20 11.90 7 6 22 4.90 12.40 -4 -7 -22 31.50 13.70 4 7 22 2.90 14.30 5 7 22 6.70 13.10 -2 0 -23 68.39 16.10 2 0 23 79.39 15.40 -3 0 -23 -8.30 14.70 3 0 23 -9.40 12.80 -1 -1 -23 17.90 13.70 -2 -1 -23 43.20 14.50 2 1 23 33.00 14.10 -3 -1 -23 7.60 13.90 3 1 23 -31.90 11.70 -4 -1 -23 91.39 17.10 4 1 23 100.49 15.40 5 1 23 -6.20 13.00 -1 -2 -23 19.10 13.00 1 2 23 25.50 22.30 -2 -2 -23 131.19 17.20 2 2 23 98.39 15.90 -3 -2 -23 32.20 14.20 3 2 23 32.20 13.80 -4 -2 -23 3.40 14.10 -4 -2 -23 14.10 11.30 4 2 23 -15.50 12.50 -5 -2 -23 10.90 13.90 -5 -2 -23 13.80 11.30 5 2 23 1.80 12.30 -2 -3 -23 -15.00 12.00 2 3 23 -9.20 13.10 -3 -3 -23 236.48 19.90 -3 -3 -23 192.38 18.60 3 3 23 153.78 17.20 -4 -3 -23 24.10 14.50 -4 -3 -23 45.80 12.40 4 3 23 26.70 13.10 -5 -3 -23 -5.20 13.10 -5 -3 -23 27.50 12.00 5 3 23 3.10 12.60 -3 -4 -23 19.80 11.70 -3 -4 -23 3.30 12.90 3 4 23 7.00 13.10 -4 -4 -23 58.99 13.60 -4 -4 -23 76.89 15.30 4 4 23 59.19 13.90 -5 -4 -23 21.80 14.40 -5 -4 -23 18.00 12.70 5 4 23 2.90 13.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30211 #===END data_Ox_5f _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common 'Ox_5f' _chemical_melting_point ? _chemical_formula_moiety 'C43 H57 Br N O3 P Pd, 1.5(C7H8)' _chemical_formula_sum 'C53.50 H69 Br N O3 P Pd' _chemical_formula_weight 991.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.7459(8) _cell_length_b 19.0935(8) _cell_length_c 53.801(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18229.6(14) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9594 _cell_measurement_theta_min 2.983 _cell_measurement_theta_max 66.567 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_F_000 8272 _exptl_transmission_factor_min 0.543 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.900 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 4.987 _shelx_estimated_absorpt_T_min 0.094 _shelx_estimated_absorpt_T_max 0.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CPAD _diffrn_measurement_method 'Mixed Phi and Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16123 _diffrn_reflns_av_unetI/netI 0.1056 _diffrn_reflns_av_R_equivalents 0.1746 _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 1.642 _diffrn_reflns_theta_max 66.751 _diffrn_reflns_theta_full 66.751 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 16123 _reflns_number_gt 12903 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.250 -0.033 0.159 793 57 ' ' 2 0.250 0.501 0.341 793 50 ' ' 3 -0.250 0.532 0.659 793 57 ' ' 4 0.250 0.991 0.841 793 52 ' ' _platon_squeeze_details ; The structure is a channel solvate, containing a mixture of toluene and pentane (confirmed by single-crystal NMR analysis, but not possible to quantitate due to sample stability). Using an approximation of 24 molecules of toluene (1.5:1 ratio to Pd complex), the disordered solvent in the unit cell was treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+91.5852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 16123 _refine_ls_number_parameters 934 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.1899 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.34115(2) 0.29142(2) 0.47704(2) 0.02904(13) Uani 1 1 d . . . . . Br1 Br 0.45004(4) 0.36324(4) 0.46473(2) 0.03686(17) Uani 1 1 d . . . . . P1 P 0.25187(8) 0.20970(8) 0.49095(3) 0.0276(3) Uani 1 1 d . . . . . O1 O 0.1305(3) 0.0984(2) 0.48569(9) 0.0383(10) Uani 1 1 d . . . . . O2 O 0.2288(3) 0.2242(2) 0.56848(8) 0.0346(9) Uani 1 1 d . . . . . O3 O 0.2039(2) 0.1082(2) 0.56138(8) 0.0341(9) Uani 1 1 d . . . . . N1 N 0.4539(5) 0.4380(7) 0.59918(15) 0.085(3) Uani 1 1 d . . . . . C1 C 0.2140(3) 0.1682(4) 0.46294(12) 0.0345(14) Uani 1 1 d . . . . . C2 C 0.1593(4) 0.1145(4) 0.46311(14) 0.0382(15) Uani 1 1 d . . . . . C3 C 0.0722(4) 0.0469(3) 0.48747(15) 0.0396(15) Uani 1 1 d . . . . . H3A H 0.0922 0.0011 0.4825 0.059 Uiso 1 1 calc R U . . . H3B H 0.0304 0.0598 0.4765 0.059 Uiso 1 1 calc R U . . . H3C H 0.0542 0.0443 0.5047 0.059 Uiso 1 1 calc R U . . . C4 C 0.1332(5) 0.0833(5) 0.44126(16) 0.0528(19) Uani 1 1 d . . . . . H4 H 0.0954 0.0480 0.4418 0.063 Uiso 1 1 calc R U . . . C5 C 0.1633(5) 0.1046(6) 0.41914(18) 0.066(3) Uani 1 1 d . . . . . H5 H 0.1465 0.0837 0.4041 0.079 Uiso 1 1 calc R U . . . C6 C 0.2181(5) 0.1566(6) 0.41841(16) 0.062(2) Uani 1 1 d . . . . . H6 H 0.2387 0.1702 0.4028 0.074 Uiso 1 1 calc R U . . . C7 C 0.2434(4) 0.1891(4) 0.43983(14) 0.0444(16) Uani 1 1 d . . . . . C8 C 0.2985(4) 0.2482(4) 0.43559(12) 0.0432(16) Uani 1 1 d . . . . . C9 C 0.2718(4) 0.3181(5) 0.43178(13) 0.0474(18) Uani 1 1 d . . . . . C10 C 0.1918(5) 0.3393(5) 0.43949(16) 0.055(2) Uani 1 1 d . . . . . H10 H 0.1718 0.3027 0.4510 0.066 Uiso 1 1 calc R U . . . C11 C 0.1910(5) 0.4107(5) 0.45327(17) 0.061(2) Uani 1 1 d . . . . . H11A H 0.2063 0.4479 0.4418 0.091 Uiso 1 1 calc R U . . . H11B H 0.2262 0.4090 0.4673 0.091 Uiso 1 1 calc R U . . . H11C H 0.1401 0.4202 0.4594 0.091 Uiso 1 1 calc R U . . . C12 C 0.1421(6) 0.3413(10) 0.4168(2) 0.095(4) Uani 1 1 d . . . . . H12A H 0.1691 0.3641 0.4031 0.143 Uiso 1 1 calc R U . . . H12B H 0.0961 0.3678 0.4205 0.143 Uiso 1 1 calc R U . . . H12C H 0.1287 0.2935 0.4119 0.143 Uiso 1 1 calc R U . . . C13 C 0.3159(5) 0.3664(4) 0.41926(14) 0.0478(17) Uani 1 1 d . . . . . H13 H 0.2978 0.4129 0.4174 0.057 Uiso 1 1 calc R U . . . C14 C 0.3862(4) 0.3489(5) 0.40927(15) 0.0509(19) Uani 1 1 d . . . . . C15 C 0.4314(5) 0.4046(6) 0.39575(19) 0.064(2) Uani 1 1 d . . . . . H15 H 0.4265 0.4478 0.4061 0.077 Uiso 1 1 calc R U . . . C16 C 0.3954(8) 0.4226(8) 0.3712(2) 0.089(4) Uani 1 1 d . . . . . H16A H 0.3937 0.3808 0.3607 0.134 Uiso 1 1 calc R U . . . H16B H 0.4251 0.4591 0.3629 0.134 Uiso 1 1 calc R U . . . H16C H 0.3441 0.4398 0.3740 0.134 Uiso 1 1 calc R U . . . C17 C 0.5146(7) 0.3893(7) 0.3949(2) 0.078(3) Uani 1 1 d . . . . . H17A H 0.5311 0.3713 0.4111 0.117 Uiso 1 1 calc R U . . . H17B H 0.5422 0.4324 0.3910 0.117 Uiso 1 1 calc R U . . . H17C H 0.5247 0.3542 0.3820 0.117 Uiso 1 1 calc R U . . . C18 C 0.4129(4) 0.2801(5) 0.41264(14) 0.0513(19) Uani 1 1 d . . . . . H18 H 0.4601 0.2675 0.4056 0.062 Uiso 1 1 calc R U . . . C19 C 0.3723(4) 0.2293(5) 0.42599(13) 0.0460(17) Uani 1 1 d . . . . . C20 C 0.4040(5) 0.1563(5) 0.42917(15) 0.0512(18) Uani 1 1 d . . . . . H20 H 0.3688 0.1286 0.4398 0.061 Uiso 1 1 calc R U . . . C21 C 0.4131(7) 0.1188(6) 0.40449(19) 0.075(3) Uani 1 1 d . . . . . H21A H 0.3684 0.1270 0.3942 0.113 Uiso 1 1 calc R U . . . H21B H 0.4189 0.0685 0.4074 0.113 Uiso 1 1 calc R U . . . H21C H 0.4578 0.1368 0.3959 0.113 Uiso 1 1 calc R U . . . C22 C 0.4812(5) 0.1607(5) 0.44238(16) 0.0528(19) Uani 1 1 d . . . . . H22A H 0.5188 0.1797 0.4309 0.079 Uiso 1 1 calc R U . . . H22B H 0.4966 0.1137 0.4477 0.079 Uiso 1 1 calc R U . . . H22C H 0.4770 0.1913 0.4569 0.079 Uiso 1 1 calc R U . . . C23 C 0.3008(4) 0.1404(3) 0.51000(12) 0.0320(13) Uani 1 1 d . . . . . C24 C 0.3815(4) 0.1349(3) 0.49910(11) 0.0314(13) Uani 1 1 d . . . . . H24A H 0.3781 0.1173 0.4818 0.038 Uiso 1 1 calc R U . . . H24B H 0.4039 0.1824 0.4985 0.038 Uiso 1 1 calc R U . . . C25 C 0.4337(4) 0.0870(4) 0.51388(13) 0.0381(14) Uani 1 1 d . . . . . H25A H 0.4839 0.0857 0.5058 0.046 Uiso 1 1 calc R U . . . H25B H 0.4401 0.1058 0.5309 0.046 Uiso 1 1 calc R U . . . C26 C 0.4016(4) 0.0133(4) 0.51521(16) 0.0480(17) Uani 1 1 d . . . . . H26A H 0.4026 -0.0083 0.4985 0.058 Uiso 1 1 calc R U . . . H26B H 0.4330 -0.0157 0.5264 0.058 Uiso 1 1 calc R U . . . C27 C 0.3214(4) 0.0149(3) 0.52479(13) 0.0384(14) Uani 1 1 d . . . . . H27A H 0.3217 0.0302 0.5424 0.046 Uiso 1 1 calc R U . . . H27B H 0.3004 -0.0332 0.5242 0.046 Uiso 1 1 calc R U . . . C28 C 0.2700(4) 0.0638(3) 0.50989(12) 0.0310(13) Uani 1 1 d . . . . . H28A H 0.2187 0.0631 0.5172 0.037 Uiso 1 1 calc R U . . . H28B H 0.2664 0.0468 0.4925 0.037 Uiso 1 1 calc R U . . . C29 C 0.2992(3) 0.1711(3) 0.53654(11) 0.0276(12) Uani 1 1 d . . . . . H29A H 0.3339 0.1434 0.5471 0.033 Uiso 1 1 calc R U . . . H29B H 0.3189 0.2196 0.5359 0.033 Uiso 1 1 calc R U . . . C30 C 0.2218(3) 0.1727(3) 0.54913(11) 0.0286(12) Uani 1 1 d . . . . . C31 C 0.1984(6) 0.1951(4) 0.59042(15) 0.057(2) Uani 1 1 d . . . . . H31A H 0.1435 0.2037 0.5916 0.069 Uiso 1 1 calc R U . . . H31B H 0.2236 0.2140 0.6054 0.069 Uiso 1 1 calc R U . . . C32 C 0.2152(5) 0.1180(4) 0.58698(14) 0.0502(18) Uani 1 1 d . . . . . H32A H 0.2678 0.1070 0.5918 0.060 Uiso 1 1 calc R U . . . H32B H 0.1804 0.0887 0.5969 0.060 Uiso 1 1 calc R U . . . C33 C 0.1558(3) 0.1891(3) 0.53203(12) 0.0299(12) Uani 1 1 d . . . . . H33A H 0.1140 0.2074 0.5423 0.036 Uiso 1 1 calc R U . . . H33B H 0.1384 0.1447 0.5245 0.036 Uiso 1 1 calc R U . . . C34 C 0.1706(3) 0.2419(3) 0.51091(12) 0.0319(13) Uani 1 1 d . . . . . C35 C 0.1900(4) 0.3141(3) 0.52192(13) 0.0338(13) Uani 1 1 d . . . . . H35A H 0.1488 0.3297 0.5327 0.051 Uiso 1 1 calc R U . . . H35B H 0.1969 0.3480 0.5084 0.051 Uiso 1 1 calc R U . . . H35C H 0.2365 0.3107 0.5316 0.051 Uiso 1 1 calc R U . . . C36 C 0.0982(4) 0.2524(4) 0.49578(13) 0.0379(14) Uani 1 1 d . . . . . H36A H 0.0851 0.2087 0.4873 0.057 Uiso 1 1 calc R U . . . H36B H 0.1061 0.2894 0.4834 0.057 Uiso 1 1 calc R U . . . H36C H 0.0570 0.2659 0.5070 0.057 Uiso 1 1 calc R U . . . C37 C 0.3727(3) 0.3285(3) 0.51068(12) 0.0327(13) Uani 1 1 d . . . . . C38 C 0.4236(3) 0.2962(4) 0.52643(12) 0.0355(14) Uani 1 1 d . . . . . H38 H 0.4455 0.2529 0.5215 0.043 Uiso 1 1 calc R U . . . C39 C 0.4436(4) 0.3247(4) 0.54897(13) 0.0422(16) Uani 1 1 d . . . . . H39 H 0.4776 0.3004 0.5595 0.051 Uiso 1 1 calc R U . . . C40 C 0.4148(4) 0.3882(4) 0.55627(13) 0.0456(17) Uani 1 1 d . . . . . C41 C 0.4354(5) 0.4179(5) 0.58009(16) 0.061(2) Uani 1 1 d . . . . . C42 C 0.3666(4) 0.4253(4) 0.54023(14) 0.0430(17) Uani 1 1 d . . . . . H42 H 0.3479 0.4701 0.5448 0.052 Uiso 1 1 calc R U . . . C43 C 0.3467(4) 0.3955(3) 0.51745(12) 0.0339(13) Uani 1 1 d . . . . . H43 H 0.3151 0.4209 0.5064 0.041 Uiso 1 1 calc R U . . . Pd2 Pd 0.35642(3) 0.27382(2) 0.69888(2) 0.03582(14) Uani 1 1 d . . . . . Br2 Br 0.46861(4) 0.20165(4) 0.70689(2) 0.0462(2) Uani 1 1 d . . . . . P2 P 0.26627(10) 0.35796(9) 0.68856(3) 0.0385(4) Uani 1 1 d . . . . . O4 O 0.1517(4) 0.4746(3) 0.69995(10) 0.0574(15) Uani 1 1 d . . . . . O5 O 0.2051(3) 0.4672(3) 0.62019(9) 0.0455(12) Uani 1 1 d . . . . . O6 O 0.2219(3) 0.3504(3) 0.61234(9) 0.0424(11) Uani 1 1 d . . . . . N2 N 0.4417(4) 0.0947(5) 0.58039(13) 0.0579(18) Uani 1 1 d . . . . . C44 C 0.2386(4) 0.3982(4) 0.71835(13) 0.0421(15) Uani 1 1 d . . . . . C45 C 0.1877(5) 0.4541(4) 0.72093(14) 0.0474(17) Uani 1 1 d . . . . . C46 C 0.1104(5) 0.5388(4) 0.70104(17) 0.0520(19) Uani 1 1 d . . . . . H46A H 0.0609 0.5302 0.7086 0.078 Uiso 1 1 calc R U . . . H46B H 0.1037 0.5573 0.6842 0.078 Uiso 1 1 calc R U . . . H46C H 0.1382 0.5728 0.7111 0.078 Uiso 1 1 calc R U . . . C47 C 0.1753(5) 0.4848(4) 0.74408(16) 0.054(2) Uani 1 1 d . . . . . H47 H 0.1443 0.5252 0.7453 0.064 Uiso 1 1 calc R U . . . C48 C 0.2065(5) 0.4581(5) 0.76453(16) 0.057(2) Uani 1 1 d . . . . . H48 H 0.1949 0.4780 0.7803 0.069 Uiso 1 1 calc R U . . . C49 C 0.2554(5) 0.4018(4) 0.76319(14) 0.0501(18) Uani 1 1 d . . . . . H49 H 0.2772 0.3832 0.7779 0.060 Uiso 1 1 calc R U . . . C50 C 0.2730(5) 0.3719(4) 0.73995(14) 0.0465(17) Uani 1 1 d . . . . . C51 C 0.3267(5) 0.3117(4) 0.74185(13) 0.0419(15) Uani 1 1 d . . . . . C52 C 0.2984(5) 0.2435(4) 0.74616(13) 0.0447(16) Uani 1 1 d . . . . . C53 C 0.2167(5) 0.2251(4) 0.74040(14) 0.0475(17) Uani 1 1 d . . . . . H53 H 0.1962 0.2632 0.7296 0.057 Uiso 1 1 calc R U . . . C54 C 0.2090(5) 0.1570(4) 0.72618(16) 0.0508(18) Uani 1 1 d . . . . . H54A H 0.2236 0.1178 0.7369 0.076 Uiso 1 1 calc R U . . . H54B H 0.2418 0.1581 0.7115 0.076 Uiso 1 1 calc R U . . . H54C H 0.1565 0.1510 0.7209 0.076 Uiso 1 1 calc R U . . . C55 C 0.1705(6) 0.2254(6) 0.76457(19) 0.066(2) Uani 1 1 d . . . . . H55A H 0.1885 0.1879 0.7755 0.099 Uiso 1 1 calc R U . . . H55B H 0.1172 0.2177 0.7607 0.099 Uiso 1 1 calc R U . . . H55C H 0.1765 0.2707 0.7729 0.099 Uiso 1 1 calc R U . . . C56 C 0.3433(5) 0.1944(4) 0.75876(14) 0.0480(18) Uani 1 1 d . . . . . H56 H 0.3242 0.1486 0.7615 0.058 Uiso 1 1 calc R U . . . C57 C 0.4143(5) 0.2109(4) 0.76721(14) 0.053(2) Uani 1 1 d . . . . . C58 C 0.4608(7) 0.1585(6) 0.78239(17) 0.070(3) Uani 1 1 d . . . . . H58 H 0.5010 0.1848 0.7914 0.085 Uiso 1 1 calc R U . . . C59 C 0.4115(8) 0.1196(7) 0.8019(2) 0.085(2) Uani 1 1 d . . . . . H59A H 0.3937 0.1530 0.8144 0.127 Uiso 1 1 calc R U . . . H59B H 0.4415 0.0831 0.8100 0.127 Uiso 1 1 calc R U . . . H59C H 0.3681 0.0982 0.7935 0.127 Uiso 1 1 calc R U . . . C60 C 0.4984(8) 0.1039(7) 0.7660(2) 0.085(2) Uani 1 1 d . . . . . H60A H 0.4599 0.0786 0.7565 0.127 Uiso 1 1 calc R U . . . H60B H 0.5264 0.0708 0.7764 0.127 Uiso 1 1 calc R U . . . H60C H 0.5332 0.1270 0.7545 0.127 Uiso 1 1 calc R U . . . C61 C 0.4435(5) 0.2763(5) 0.76192(15) 0.0526(19) Uani 1 1 d . . . . . H61 H 0.4935 0.2868 0.7670 0.063 Uiso 1 1 calc R U . . . C62 C 0.4019(5) 0.3278(4) 0.74939(15) 0.0521(19) Uani 1 1 d . . . . . C63 C 0.4375(5) 0.3988(4) 0.74525(15) 0.0525(19) Uani 1 1 d . . . . . H63 H 0.4016 0.4269 0.7349 0.063 Uiso 1 1 calc R U . . . C64 C 0.4484(6) 0.4378(5) 0.76979(18) 0.065(2) Uani 1 1 d . . . . . H64A H 0.4852 0.4128 0.7800 0.097 Uiso 1 1 calc R U . . . H64B H 0.4002 0.4404 0.7786 0.097 Uiso 1 1 calc R U . . . H64C H 0.4667 0.4853 0.7664 0.097 Uiso 1 1 calc R U . . . C65 C 0.5111(5) 0.3937(5) 0.73083(19) 0.062(2) Uani 1 1 d . . . . . H65A H 0.5494 0.3711 0.7412 0.093 Uiso 1 1 calc R U . . . H65B H 0.5281 0.4408 0.7263 0.093 Uiso 1 1 calc R U . . . H65C H 0.5032 0.3659 0.7157 0.093 Uiso 1 1 calc R U . . . C66 C 0.3123(4) 0.4285(4) 0.66904(13) 0.0406(15) Uani 1 1 d . . . . . C67A C 0.3959(5) 0.4298(4) 0.67739(15) 0.0467(17) Uani 0.754(10) 1 d . . P A 1 H67A H 0.3976 0.4401 0.6954 0.056 Uiso 0.754(10) 1 calc R U P A 1 H67B H 0.4174 0.3824 0.6750 0.056 Uiso 0.754(10) 1 calc R U P A 1 C68A C 0.4443(5) 0.4804(5) 0.66451(16) 0.038(2) Uani 0.754(10) 1 d . . P A 1 H68A H 0.4494 0.4670 0.6468 0.045 Uiso 0.754(10) 1 calc R U P A 1 H68B H 0.4951 0.4804 0.6721 0.045 Uiso 0.754(10) 1 calc R U P A 1 C69A C 0.4091(5) 0.5553(5) 0.66645(17) 0.0388(19) Uani 0.754(10) 1 d . . P A 1 H69A H 0.4100 0.5712 0.6840 0.047 Uiso 0.754(10) 1 calc R U P A 1 H69B H 0.4390 0.5886 0.6564 0.047 Uiso 0.754(10) 1 calc R U P A 1 C70A C 0.3275(6) 0.5538(5) 0.65701(17) 0.041(2) Uani 0.754(10) 1 d . . P A 1 H70A H 0.3051 0.6011 0.6585 0.049 Uiso 0.754(10) 1 calc R U P A 1 H70B H 0.3268 0.5402 0.6393 0.049 Uiso 0.754(10) 1 calc R U P A 1 C71A C 0.2831(5) 0.5042(4) 0.67133(14) 0.0483(17) Uani 0.754(10) 1 d . . P A 1 H71A H 0.2301 0.5059 0.6656 0.058 Uiso 0.754(10) 1 calc R U P A 1 H71B H 0.2839 0.5182 0.6890 0.058 Uiso 0.754(10) 1 calc R U P A 1 C67B C 0.1902(4) 0.2605(4) 0.65834(15) 0.0471(17) Uani 0.246(10) 1 d . . P A 2 H67C H 0.2345 0.2628 0.6472 0.057 Uiso 0.246(10) 1 calc R U P A 2 H67D H 0.2001 0.2247 0.6713 0.057 Uiso 0.246(10) 1 calc R U P A 2 C68B C 0.1234(14) 0.2417(12) 0.6442(4) 0.026(5) Uani 0.246(10) 1 d . . P A 2 H68C H 0.1299 0.1948 0.6367 0.031 Uiso 0.246(10) 1 calc R U P A 2 H68D H 0.1150 0.2761 0.6307 0.031 Uiso 0.246(10) 1 calc R U P A 2 C69B C 0.0561(16) 0.2414(14) 0.6620(5) 0.0388(19) Uani 0.246(10) 1 d . . P A 2 H69C H 0.0101 0.2285 0.6526 0.047 Uiso 0.246(10) 1 calc R U P A 2 H69D H 0.0643 0.2051 0.6749 0.047 Uiso 0.246(10) 1 calc R U P A 2 C70B C 0.0435(18) 0.3105(19) 0.6745(5) 0.048(8) Uani 0.246(10) 1 d . . P A 2 H70C H 0.0346 0.3477 0.6620 0.058 Uiso 0.246(10) 1 calc R U P A 2 H70D H -0.0007 0.3081 0.6857 0.058 Uiso 0.246(10) 1 calc R U P A 2 C71B C 0.1092(5) 0.3246(5) 0.68811(16) 0.0527(19) Uani 0.246(10) 1 d . . P A 2 H71C H 0.1186 0.2861 0.7000 0.063 Uiso 0.246(10) 1 calc R U P A 2 H71D H 0.1025 0.3684 0.6977 0.063 Uiso 0.246(10) 1 calc R U P A 2 C72 C 0.3034(4) 0.4007(4) 0.64216(13) 0.0409(15) Uani 1 1 d . . . . . H72A H 0.3357 0.4292 0.6311 0.049 Uiso 1 1 calc R U . . . H72B H 0.3226 0.3520 0.6416 0.049 Uiso 1 1 calc R U . . . C73 C 0.2235(4) 0.4013(4) 0.63185(13) 0.0423(15) Uani 1 1 d . . . . . C74 C 0.2044(6) 0.4561(4) 0.59375(14) 0.054(2) Uani 1 1 d . . . . . H74A H 0.2546 0.4650 0.5864 0.065 Uiso 1 1 calc R U . . . H74B H 0.1667 0.4865 0.5855 0.065 Uiso 1 1 calc R U . . . C75 C 0.1833(6) 0.3808(4) 0.59179(15) 0.054(2) Uani 1 1 d . . . . . H75A H 0.1281 0.3743 0.5933 0.064 Uiso 1 1 calc R U . . . H75B H 0.2006 0.3604 0.5759 0.064 Uiso 1 1 calc R U . . . C76 C 0.1606(5) 0.3880(5) 0.65059(14) 0.0493(18) Uani 1 1 d . . . . . H76A H 0.1149 0.3738 0.6413 0.059 Uiso 1 1 calc R U . . . H76B H 0.1490 0.4328 0.6591 0.059 Uiso 1 1 calc R U . . . C77 C 0.1768(4) 0.3322(4) 0.67058(14) 0.0440(16) Uani 1 1 d . . . . . C78A C 0.1902(4) 0.2605(4) 0.65834(15) 0.0471(17) Uani 0.754(10) 1 d . . P A 1 H78A H 0.2332 0.2635 0.6470 0.071 Uiso 0.754(10) 1 calc R U P A 1 H78B H 0.2007 0.2255 0.6712 0.071 Uiso 0.754(10) 1 calc R U P A 1 H78C H 0.1451 0.2466 0.6490 0.071 Uiso 0.754(10) 1 calc R U P A 1 C79A C 0.1092(5) 0.3246(5) 0.68811(16) 0.0527(19) Uani 0.754(10) 1 d . . P A 1 H79A H 0.0992 0.3696 0.6962 0.079 Uiso 0.754(10) 1 calc R U P A 1 H79B H 0.0647 0.3103 0.6786 0.079 Uiso 0.754(10) 1 calc R U P A 1 H79C H 0.1203 0.2892 0.7007 0.079 Uiso 0.754(10) 1 calc R U P A 1 C78B C 0.3959(5) 0.4298(4) 0.67739(15) 0.0467(17) Uani 0.246(10) 1 d . . P A 2 H78D H 0.4171 0.3825 0.6762 0.070 Uiso 0.246(10) 1 calc R U P A 2 H78E H 0.4245 0.4615 0.6666 0.070 Uiso 0.246(10) 1 calc R U P A 2 H78F H 0.3991 0.4463 0.6946 0.070 Uiso 0.246(10) 1 calc R U P A 2 C79B C 0.2831(5) 0.5042(4) 0.67133(14) 0.0483(17) Uani 0.246(10) 1 d . . P A 2 H79D H 0.2894 0.5204 0.6885 0.073 Uiso 0.246(10) 1 calc R U P A 2 H79E H 0.3117 0.5347 0.6601 0.073 Uiso 0.246(10) 1 calc R U P A 2 H79F H 0.2296 0.5056 0.6669 0.073 Uiso 0.246(10) 1 calc R U P A 2 C80 C 0.3746(4) 0.2353(3) 0.66448(12) 0.0359(14) Uani 1 1 d . . . . . C81 C 0.4266(4) 0.2637(4) 0.64722(14) 0.0407(15) Uani 1 1 d . . . . . H81 H 0.4512 0.3068 0.6507 0.049 Uiso 1 1 calc R U . . . C82 C 0.4417(4) 0.2283(4) 0.62510(14) 0.0442(16) Uani 1 1 d . . . . . H82 H 0.4746 0.2487 0.6132 0.053 Uiso 1 1 calc R U . . . C83 C 0.4093(4) 0.1640(4) 0.62041(13) 0.0398(15) Uani 1 1 d . . . . . C84 C 0.4281(4) 0.1255(4) 0.59811(15) 0.0473(17) Uani 1 1 d . . . . . C85 C 0.3584(4) 0.1342(4) 0.63725(13) 0.0405(15) Uani 1 1 d . . . . . H85 H 0.3355 0.0903 0.6339 0.049 Uiso 1 1 calc R U . . . C86 C 0.3424(4) 0.1705(4) 0.65890(12) 0.0353(14) Uani 1 1 d . . . . . H86 H 0.3081 0.1504 0.6704 0.042 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0222(2) 0.0297(2) 0.0352(2) 0.00108(17) 0.00204(16) -0.00042(16) Br1 0.0274(3) 0.0366(3) 0.0466(4) 0.0017(3) 0.0075(3) -0.0041(3) P1 0.0211(7) 0.0256(7) 0.0362(7) -0.0021(6) 0.0022(6) -0.0013(5) O1 0.031(2) 0.035(2) 0.050(3) -0.009(2) 0.0023(19) -0.0060(19) O2 0.035(2) 0.029(2) 0.040(2) -0.0090(18) 0.0067(18) -0.0055(18) O3 0.031(2) 0.029(2) 0.042(2) 0.0001(18) 0.0079(18) -0.0082(17) N1 0.074(5) 0.132(9) 0.049(4) -0.026(5) 0.006(4) -0.045(6) C1 0.022(3) 0.041(3) 0.040(3) -0.010(3) -0.005(2) 0.003(3) C2 0.024(3) 0.041(4) 0.050(4) -0.009(3) 0.003(3) 0.003(3) C3 0.026(3) 0.028(3) 0.064(4) 0.002(3) -0.007(3) -0.009(3) C4 0.041(4) 0.059(5) 0.058(5) -0.023(4) -0.003(3) -0.011(4) C5 0.054(5) 0.091(7) 0.054(5) -0.026(5) -0.007(4) -0.011(5) C6 0.056(5) 0.089(7) 0.041(4) -0.018(4) 0.000(4) -0.016(5) C7 0.032(3) 0.054(4) 0.047(4) -0.007(3) -0.002(3) -0.010(3) C8 0.041(4) 0.059(4) 0.030(3) 0.004(3) -0.001(3) -0.002(3) C9 0.031(4) 0.076(5) 0.036(3) 0.002(3) -0.004(3) 0.003(3) C10 0.039(4) 0.074(6) 0.052(4) 0.009(4) -0.002(3) 0.006(4) C11 0.053(5) 0.067(5) 0.062(5) 0.013(4) 0.003(4) 0.018(4) C12 0.042(5) 0.155(13) 0.088(7) -0.006(8) -0.017(5) 0.030(7) C13 0.041(4) 0.054(4) 0.049(4) 0.005(3) -0.001(3) 0.007(3) C14 0.034(4) 0.068(5) 0.050(4) 0.012(4) 0.005(3) -0.001(4) C15 0.052(5) 0.072(6) 0.068(5) 0.024(5) 0.010(4) -0.001(4) C16 0.089(8) 0.119(10) 0.060(6) 0.017(6) 0.009(5) -0.015(7) C17 0.071(6) 0.082(7) 0.082(7) 0.026(6) 0.017(5) -0.007(5) C18 0.035(4) 0.077(6) 0.042(4) 0.005(4) 0.008(3) 0.001(4) C19 0.038(4) 0.062(5) 0.038(4) -0.010(3) -0.003(3) -0.003(3) C20 0.045(4) 0.063(5) 0.046(4) -0.015(4) 0.005(3) -0.002(4) C21 0.097(8) 0.068(6) 0.061(5) -0.021(5) 0.012(5) 0.002(5) C22 0.044(4) 0.057(5) 0.057(4) -0.001(4) 0.011(3) 0.004(4) C23 0.029(3) 0.025(3) 0.041(3) -0.006(2) 0.001(3) 0.003(2) C24 0.031(3) 0.030(3) 0.032(3) 0.001(2) 0.001(2) 0.007(2) C25 0.028(3) 0.042(4) 0.044(3) -0.005(3) 0.008(3) 0.008(3) C26 0.045(4) 0.039(4) 0.060(4) -0.007(3) -0.005(3) 0.015(3) C27 0.043(4) 0.023(3) 0.049(4) -0.002(3) -0.003(3) 0.002(3) C28 0.036(3) 0.019(3) 0.038(3) -0.007(2) 0.002(2) 0.000(2) C29 0.021(3) 0.023(3) 0.039(3) -0.002(2) 0.000(2) 0.001(2) C30 0.029(3) 0.021(3) 0.036(3) -0.006(2) 0.003(2) -0.002(2) C31 0.083(6) 0.044(4) 0.045(4) -0.010(3) 0.014(4) -0.004(4) C32 0.066(5) 0.037(4) 0.047(4) 0.004(3) 0.001(4) -0.002(4) C33 0.021(3) 0.025(3) 0.045(3) -0.003(3) 0.005(2) -0.005(2) C34 0.021(3) 0.032(3) 0.043(3) -0.003(3) 0.006(2) 0.001(2) C35 0.028(3) 0.025(3) 0.048(4) 0.001(3) 0.005(3) 0.000(2) C36 0.024(3) 0.041(3) 0.049(4) -0.001(3) 0.003(3) 0.009(3) C37 0.025(3) 0.034(3) 0.039(3) 0.002(3) 0.003(2) -0.009(2) C38 0.021(3) 0.045(4) 0.041(3) 0.009(3) -0.002(2) -0.005(3) C39 0.030(3) 0.053(4) 0.044(4) 0.008(3) 0.000(3) -0.016(3) C40 0.037(4) 0.059(5) 0.042(4) -0.002(3) 0.003(3) -0.024(3) C41 0.057(5) 0.074(6) 0.051(5) -0.009(4) 0.013(4) -0.030(5) C42 0.036(4) 0.042(4) 0.051(4) -0.007(3) 0.015(3) -0.022(3) C43 0.030(3) 0.031(3) 0.040(3) -0.005(3) 0.005(3) -0.005(3) Pd2 0.0392(3) 0.0313(2) 0.0369(3) -0.00378(18) -0.00204(19) -0.00024(19) Br2 0.0438(4) 0.0444(4) 0.0503(4) -0.0045(3) -0.0091(3) 0.0028(3) P2 0.0423(9) 0.0377(8) 0.0355(8) -0.0049(7) -0.0009(7) 0.0039(7) O4 0.073(4) 0.054(3) 0.045(3) -0.003(2) 0.007(3) 0.029(3) O5 0.057(3) 0.041(3) 0.039(2) -0.006(2) -0.004(2) 0.013(2) O6 0.049(3) 0.039(2) 0.039(2) -0.008(2) -0.001(2) 0.000(2) N2 0.049(4) 0.080(5) 0.045(3) -0.020(4) 0.006(3) -0.003(4) C44 0.050(4) 0.039(4) 0.037(3) -0.008(3) -0.002(3) 0.006(3) C45 0.055(4) 0.043(4) 0.044(4) -0.002(3) 0.006(3) 0.006(3) C46 0.047(4) 0.043(4) 0.065(5) 0.008(4) 0.011(4) 0.012(3) C47 0.058(5) 0.038(4) 0.064(5) -0.010(4) 0.016(4) 0.001(4) C48 0.065(5) 0.057(5) 0.049(4) -0.016(4) 0.008(4) -0.001(4) C49 0.069(5) 0.041(4) 0.040(4) -0.007(3) -0.002(3) 0.001(4) C50 0.062(5) 0.038(4) 0.039(4) -0.004(3) -0.003(3) -0.006(3) C51 0.052(4) 0.035(3) 0.039(3) 0.000(3) -0.008(3) -0.003(3) C52 0.059(5) 0.041(4) 0.033(3) 0.002(3) -0.001(3) 0.001(3) C53 0.057(5) 0.040(4) 0.045(4) -0.002(3) 0.010(3) 0.000(3) C54 0.047(4) 0.050(4) 0.055(4) -0.001(4) 0.001(3) -0.013(3) C55 0.068(6) 0.064(5) 0.066(5) -0.012(4) 0.015(5) -0.001(5) C56 0.060(5) 0.039(4) 0.046(4) 0.007(3) 0.004(3) 0.001(3) C57 0.072(6) 0.048(4) 0.039(4) -0.001(3) -0.007(4) 0.010(4) C58 0.095(7) 0.068(6) 0.049(5) 0.014(4) -0.020(5) 0.024(5) C59 0.087(6) 0.075(5) 0.092(5) 0.015(4) -0.021(4) 0.014(4) C60 0.087(6) 0.075(5) 0.092(5) 0.015(4) -0.021(4) 0.014(4) C61 0.056(5) 0.053(5) 0.049(4) -0.001(4) -0.012(4) 0.000(4) C62 0.068(5) 0.044(4) 0.045(4) -0.007(3) -0.010(4) -0.007(4) C63 0.064(5) 0.042(4) 0.052(4) -0.005(3) -0.018(4) -0.008(4) C64 0.079(6) 0.053(5) 0.062(5) -0.014(4) -0.020(5) -0.010(4) C65 0.054(5) 0.059(5) 0.073(6) -0.008(4) -0.004(4) -0.010(4) C66 0.048(4) 0.035(3) 0.039(3) -0.008(3) 0.001(3) 0.001(3) C67A 0.053(4) 0.037(4) 0.050(4) -0.004(3) -0.010(3) -0.003(3) C68A 0.039(5) 0.040(5) 0.035(4) 0.004(4) 0.001(4) -0.011(4) C69A 0.040(5) 0.033(4) 0.044(4) 0.004(3) 0.008(4) -0.010(3) C70A 0.048(5) 0.035(5) 0.039(5) 0.006(4) 0.006(4) -0.001(4) C71A 0.065(5) 0.042(4) 0.039(4) -0.008(3) -0.001(3) 0.006(4) C67B 0.042(4) 0.051(4) 0.049(4) -0.002(3) -0.003(3) -0.003(3) C68B 0.033(12) 0.025(11) 0.020(10) -0.003(9) 0.012(9) -0.003(9) C69B 0.040(5) 0.033(4) 0.044(4) 0.004(3) 0.008(4) -0.010(3) C70B 0.050(17) 0.07(2) 0.025(13) -0.029(13) 0.007(11) -0.018(15) C71B 0.039(4) 0.064(5) 0.055(4) 0.004(4) 0.003(3) 0.003(4) C72 0.047(4) 0.039(4) 0.037(3) -0.005(3) 0.003(3) 0.004(3) C73 0.051(4) 0.035(3) 0.041(4) -0.006(3) -0.005(3) 0.007(3) C74 0.077(6) 0.047(4) 0.038(4) -0.005(3) -0.005(4) 0.012(4) C75 0.072(5) 0.049(4) 0.041(4) -0.013(3) -0.014(4) 0.009(4) C76 0.044(4) 0.058(5) 0.046(4) -0.011(3) -0.004(3) 0.008(3) C77 0.038(4) 0.050(4) 0.043(4) -0.006(3) -0.001(3) 0.008(3) C78A 0.042(4) 0.051(4) 0.049(4) -0.002(3) -0.003(3) -0.003(3) C79A 0.039(4) 0.064(5) 0.055(4) 0.004(4) 0.003(3) 0.003(4) C78B 0.053(4) 0.037(4) 0.050(4) -0.004(3) -0.010(3) -0.003(3) C79B 0.065(5) 0.042(4) 0.039(4) -0.008(3) -0.001(3) 0.006(4) C80 0.036(3) 0.033(3) 0.039(3) -0.002(3) 0.001(3) 0.000(3) C81 0.031(3) 0.040(4) 0.051(4) -0.007(3) 0.005(3) -0.001(3) C82 0.045(4) 0.043(4) 0.044(4) 0.001(3) 0.008(3) -0.007(3) C83 0.034(3) 0.047(4) 0.039(3) -0.001(3) 0.003(3) -0.001(3) C84 0.037(4) 0.056(4) 0.049(4) -0.004(4) 0.009(3) -0.001(3) C85 0.042(4) 0.041(4) 0.038(3) -0.002(3) -0.001(3) -0.006(3) C86 0.034(3) 0.035(3) 0.037(3) -0.001(3) 0.005(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C37 2.022(6) . ? Pd1 P1 2.3462(15) . ? Pd1 Br1 2.4605(7) . ? Pd1 C8 2.495(7) . ? P1 C1 1.831(6) . ? P1 C23 1.885(6) . ? P1 C34 1.899(6) . ? O1 C2 1.353(9) . ? O1 C3 1.431(8) . ? O2 C31 1.412(10) . ? O2 C30 1.437(7) . ? O3 C32 1.405(9) . ? O3 C30 1.433(8) . ? N1 C41 1.145(12) . ? C1 C7 1.405(11) . ? C1 C2 1.412(10) . ? C2 C4 1.397(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.367(14) . ? C4 H4 0.9500 . ? C5 C6 1.391(15) . ? C5 H5 0.9500 . ? C6 C7 1.384(11) . ? C6 H6 0.9500 . ? C7 C8 1.512(11) . ? C8 C9 1.431(13) . ? C8 C19 1.453(11) . ? C9 C13 1.384(12) . ? C9 C10 1.533(11) . ? C10 C12 1.508(14) . ? C10 C11 1.551(15) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.400(12) . ? C13 H13 0.9500 . ? C14 C18 1.408(14) . ? C14 C15 1.518(13) . ? C15 C17 1.505(16) . ? C15 C16 1.508(16) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.405(13) . ? C18 H18 0.9500 . ? C19 C20 1.513(13) . ? C20 C21 1.517(12) . ? C20 C22 1.545(12) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C29 1.543(9) . ? C23 C24 1.550(9) . ? C23 C28 1.563(8) . ? C24 C25 1.526(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.521(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.514(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.532(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.530(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.522(9) . ? C31 C32 1.512(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.541(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C36 1.536(9) . ? C34 C35 1.540(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.385(10) . ? C37 C43 1.408(10) . ? C38 C39 1.376(11) . ? C38 H38 0.9500 . ? C39 C40 1.372(12) . ? C39 H39 0.9500 . ? C40 C42 1.407(12) . ? C40 C41 1.448(12) . ? C42 C43 1.397(10) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? Pd2 C80 2.017(7) . ? Pd2 P2 2.3341(18) . ? Pd2 Br2 2.4596(9) . ? Pd2 C51 2.480(7) . ? P2 C44 1.844(7) . ? P2 C66 1.893(8) . ? P2 C77 1.922(8) . ? O4 C45 1.354(10) . ? O4 C46 1.430(10) . ? O5 C74 1.438(9) . ? O5 C73 1.442(9) . ? O6 C75 1.424(10) . ? O6 C73 1.431(9) . ? N2 C84 1.146(11) . ? C44 C50 1.405(11) . ? C44 C45 1.406(11) . ? C45 C47 1.393(12) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.333(14) . ? C47 H47 0.9500 . ? C48 C49 1.385(13) . ? C48 H48 0.9500 . ? C49 C50 1.409(11) . ? C49 H49 0.9500 . ? C50 C51 1.497(12) . ? C51 C52 1.414(11) . ? C51 C62 1.429(12) . ? C52 C56 1.405(12) . ? C52 C53 1.524(12) . ? C53 C54 1.515(12) . ? C53 C55 1.537(12) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.376(13) . ? C56 H56 0.9500 . ? C57 C61 1.381(13) . ? C57 C58 1.533(12) . ? C58 C60 1.519(18) . ? C58 C59 1.555(18) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.401(13) . ? C61 H61 0.9500 . ? C62 C63 1.511(12) . ? C63 C65 1.522(14) . ? C63 C64 1.528(12) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C79B 1.540(11) . ? C66 C71A 1.540(11) . ? C66 C72 1.549(10) . ? C66 C78B 1.550(11) . ? C66 C67A 1.550(11) . ? C67A C68A 1.466(12) . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? C68A C69A 1.563(14) . ? C68A H68A 0.9900 . ? C68A H68B 0.9900 . ? C69A C70A 1.535(14) . ? C69A H69A 0.9900 . ? C69A H69B 0.9900 . ? C70A C71A 1.453(13) . ? C70A H70A 0.9900 . ? C70A H70B 0.9900 . ? C71A H71A 0.9900 . ? C71A H71B 0.9900 . ? C67B C68B 1.45(3) . ? C67B C77 1.538(11) . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? C68B C69B 1.53(3) . ? C68B H68C 0.9900 . ? C68B H68D 0.9900 . ? C69B C70B 1.50(4) . ? C69B H69C 0.9900 . ? C69B H69D 0.9900 . ? C70B C71B 1.40(3) . ? C70B H70C 0.9900 . ? C70B H70D 0.9900 . ? C71B C77 1.534(11) . ? C71B H71C 0.9900 . ? C71B H71D 0.9900 . ? C72 C73 1.523(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C76 1.525(12) . ? C74 C75 1.490(13) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.542(12) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C79A 1.534(11) . ? C77 C78A 1.538(11) . ? C78A H78A 0.9800 . ? C78A H78B 0.9800 . ? C78A H78C 0.9800 . ? C79A H79A 0.9800 . ? C79A H79B 0.9800 . ? C79A H79C 0.9800 . ? C78B H78D 0.9800 . ? C78B H78E 0.9800 . ? C78B H78F 0.9800 . ? C79B H79D 0.9800 . ? C79B H79E 0.9800 . ? C79B H79F 0.9800 . ? C80 C86 1.396(10) . ? C80 C81 1.418(10) . ? C81 C82 1.394(11) . ? C81 H81 0.9500 . ? C82 C83 1.380(11) . ? C82 H82 0.9500 . ? C83 C85 1.399(10) . ? C83 C84 1.446(11) . ? C85 C86 1.384(10) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 Pd1 P1 97.72(17) . . ? C37 Pd1 Br1 80.12(17) . . ? P1 Pd1 Br1 170.72(4) . . ? C37 Pd1 C8 178.1(3) . . ? P1 Pd1 C8 82.00(18) . . ? Br1 Pd1 C8 100.46(17) . . ? C1 P1 C23 108.2(3) . . ? C1 P1 C34 109.1(3) . . ? C23 P1 C34 105.6(3) . . ? C1 P1 Pd1 105.8(2) . . ? C23 P1 Pd1 109.2(2) . . ? C34 P1 Pd1 118.5(2) . . ? C2 O1 C3 119.3(5) . . ? C31 O2 C30 107.7(5) . . ? C32 O3 C30 107.7(5) . . ? C7 C1 C2 117.8(6) . . ? C7 C1 P1 118.0(5) . . ? C2 C1 P1 124.1(5) . . ? O1 C2 C4 122.2(7) . . ? O1 C2 C1 115.5(6) . . ? C4 C2 C1 122.2(7) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 118.4(8) . . ? C5 C4 H4 120.8 . . ? C2 C4 H4 120.8 . . ? C4 C5 C6 120.7(8) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 121.5(8) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C1 119.3(7) . . ? C6 C7 C8 114.7(7) . . ? C1 C7 C8 125.8(6) . . ? C9 C8 C19 118.7(7) . . ? C9 C8 C7 120.3(7) . . ? C19 C8 C7 116.8(7) . . ? C9 C8 Pd1 85.4(4) . . ? C19 C8 Pd1 97.3(4) . . ? C7 C8 Pd1 107.9(4) . . ? C13 C9 C8 120.2(7) . . ? C13 C9 C10 118.6(8) . . ? C8 C9 C10 121.0(7) . . ? C12 C10 C9 109.2(8) . . ? C12 C10 C11 111.0(9) . . ? C9 C10 C11 111.7(8) . . ? C12 C10 H10 108.3 . . ? C9 C10 H10 108.3 . . ? C11 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 122.1(8) . . ? C9 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C18 118.2(7) . . ? C13 C14 C15 119.2(8) . . ? C18 C14 C15 122.6(7) . . ? C17 C15 C16 115.7(9) . . ? C17 C15 C14 113.4(8) . . ? C16 C15 C14 110.8(9) . . ? C17 C15 H15 105.3 . . ? C16 C15 H15 105.3 . . ? C14 C15 H15 105.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C14 122.5(7) . . ? C19 C18 H18 118.8 . . ? C14 C18 H18 118.8 . . ? C18 C19 C8 118.2(8) . . ? C18 C19 C20 120.1(7) . . ? C8 C19 C20 121.7(7) . . ? C19 C20 C21 112.0(8) . . ? C19 C20 C22 109.4(7) . . ? C21 C20 C22 109.5(8) . . ? C19 C20 H20 108.6 . . ? C21 C20 H20 108.6 . . ? C22 C20 H20 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C29 C23 C24 113.2(5) . . ? C29 C23 C28 110.6(5) . . ? C24 C23 C28 105.0(5) . . ? C29 C23 P1 103.2(4) . . ? C24 C23 P1 105.5(4) . . ? C28 C23 P1 119.5(4) . . ? C25 C24 C23 113.9(5) . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 110.6(6) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 110.5(6) . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 113.2(6) . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C23 111.1(5) . . ? C27 C28 H28A 109.4 . . ? C23 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C23 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C23 115.7(5) . . ? C30 C29 H29A 108.3 . . ? C23 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? C23 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? O3 C30 O2 105.9(5) . . ? O3 C30 C33 106.5(5) . . ? O2 C30 C33 111.2(5) . . ? O3 C30 C29 112.7(5) . . ? O2 C30 C29 104.9(5) . . ? C33 C30 C29 115.2(5) . . ? O2 C31 C32 101.8(6) . . ? O2 C31 H31A 111.4 . . ? C32 C31 H31A 111.4 . . ? O2 C31 H31B 111.4 . . ? C32 C31 H31B 111.4 . . ? H31A C31 H31B 109.3 . . ? O3 C32 C31 102.8(6) . . ? O3 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? O3 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C30 C33 C34 116.7(5) . . ? C30 C33 H33A 108.1 . . ? C34 C33 H33A 108.1 . . ? C30 C33 H33B 108.1 . . ? C34 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C36 C34 C35 105.8(5) . . ? C36 C34 C33 109.5(5) . . ? C35 C34 C33 109.9(5) . . ? C36 C34 P1 112.2(4) . . ? C35 C34 P1 109.8(4) . . ? C33 C34 P1 109.6(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C43 117.5(6) . . ? C38 C37 Pd1 124.9(5) . . ? C43 C37 Pd1 117.3(5) . . ? C39 C38 C37 122.0(7) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C40 C39 C38 120.4(7) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C42 119.7(7) . . ? C39 C40 C41 120.4(8) . . ? C42 C40 C41 119.9(8) . . ? N1 C41 C40 176.2(13) . . ? C43 C42 C40 119.2(7) . . ? C43 C42 H42 120.4 . . ? C40 C42 H42 120.4 . . ? C42 C43 C37 120.9(7) . . ? C42 C43 H43 119.5 . . ? C37 C43 H43 119.5 . . ? C80 Pd2 P2 98.2(2) . . ? C80 Pd2 Br2 80.06(19) . . ? P2 Pd2 Br2 169.16(6) . . ? C80 Pd2 C51 174.8(3) . . ? P2 Pd2 C51 82.82(18) . . ? Br2 Pd2 C51 99.92(18) . . ? C44 P2 C66 107.5(3) . . ? C44 P2 C77 108.9(3) . . ? C66 P2 C77 105.0(3) . . ? C44 P2 Pd2 105.2(2) . . ? C66 P2 Pd2 109.0(2) . . ? C77 P2 Pd2 120.6(2) . . ? C45 O4 C46 117.0(6) . . ? C74 O5 C73 107.7(5) . . ? C75 O6 C73 107.6(5) . . ? C50 C44 C45 117.9(6) . . ? C50 C44 P2 117.1(6) . . ? C45 C44 P2 125.0(6) . . ? O4 C45 C47 123.3(7) . . ? O4 C45 C44 116.1(6) . . ? C47 C45 C44 120.6(7) . . ? O4 C46 H46A 109.5 . . ? O4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C45 120.8(8) . . ? C48 C47 H47 119.6 . . ? C45 C47 H47 119.6 . . ? C47 C48 C49 120.9(7) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C50 119.9(8) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C44 C50 C49 119.6(7) . . ? C44 C50 C51 127.4(7) . . ? C49 C50 C51 113.0(7) . . ? C52 C51 C62 118.8(7) . . ? C52 C51 C50 119.5(7) . . ? C62 C51 C50 116.7(7) . . ? C52 C51 Pd2 87.7(4) . . ? C62 C51 Pd2 97.4(5) . . ? C50 C51 Pd2 107.2(4) . . ? C56 C52 C51 119.5(8) . . ? C56 C52 C53 118.9(7) . . ? C51 C52 C53 121.1(7) . . ? C54 C53 C52 112.8(7) . . ? C54 C53 C55 112.4(7) . . ? C52 C53 C55 109.5(7) . . ? C54 C53 H53 107.3 . . ? C52 C53 H53 107.3 . . ? C55 C53 H53 107.3 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C52 121.7(8) . . ? C57 C56 H56 119.1 . . ? C52 C56 H56 119.1 . . ? C56 C57 C61 118.8(8) . . ? C56 C57 C58 121.3(9) . . ? C61 C57 C58 119.9(9) . . ? C60 C58 C57 112.1(8) . . ? C60 C58 C59 108.1(10) . . ? C57 C58 C59 111.6(9) . . ? C60 C58 H58 108.3 . . ? C57 C58 H58 108.3 . . ? C59 C58 H58 108.3 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C61 C62 122.5(8) . . ? C57 C61 H61 118.8 . . ? C62 C61 H61 118.8 . . ? C61 C62 C51 118.5(8) . . ? C61 C62 C63 118.7(8) . . ? C51 C62 C63 122.7(7) . . ? C62 C63 C65 112.1(8) . . ? C62 C63 C64 111.3(7) . . ? C65 C63 C64 111.2(8) . . ? C62 C63 H63 107.3 . . ? C65 C63 H63 107.3 . . ? C64 C63 H63 107.3 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C79B C66 C72 111.2(6) . . ? C71A C66 C72 111.2(6) . . ? C79B C66 C78B 106.5(6) . . ? C72 C66 C78B 112.0(6) . . ? C71A C66 C67A 106.5(6) . . ? C72 C66 C67A 112.0(6) . . ? C79B C66 P2 118.5(5) . . ? C71A C66 P2 118.5(5) . . ? C72 C66 P2 103.3(5) . . ? C78B C66 P2 105.3(5) . . ? C67A C66 P2 105.3(5) . . ? C68A C67A C66 115.7(7) . . ? C68A C67A H67A 108.4 . . ? C66 C67A H67A 108.4 . . ? C68A C67A H67B 108.4 . . ? C66 C67A H67B 108.4 . . ? H67A C67A H67B 107.4 . . ? C67A C68A C69A 109.7(7) . . ? C67A C68A H68A 109.7 . . ? C69A C68A H68A 109.7 . . ? C67A C68A H68B 109.7 . . ? C69A C68A H68B 109.7 . . ? H68A C68A H68B 108.2 . . ? C70A C69A C68A 109.8(7) . . ? C70A C69A H69A 109.7 . . ? C68A C69A H69A 109.7 . . ? C70A C69A H69B 109.7 . . ? C68A C69A H69B 109.7 . . ? H69A C69A H69B 108.2 . . ? C71A C70A C69A 110.4(8) . . ? C71A C70A H70A 109.6 . . ? C69A C70A H70A 109.6 . . ? C71A C70A H70B 109.6 . . ? C69A C70A H70B 109.6 . . ? H70A C70A H70B 108.1 . . ? C70A C71A C66 112.7(7) . . ? C70A C71A H71A 109.0 . . ? C66 C71A H71A 109.0 . . ? C70A C71A H71B 109.0 . . ? C66 C71A H71B 109.0 . . ? H71A C71A H71B 107.8 . . ? C68B C67B C77 108.6(11) . . ? C68B C67B H67C 110.0 . . ? C77 C67B H67C 110.0 . . ? C68B C67B H67D 110.0 . . ? C77 C67B H67D 110.0 . . ? H67C C67B H67D 108.4 . . ? C67B C68B C69B 108.1(18) . . ? C67B C68B H68C 110.1 . . ? C69B C68B H68C 110.1 . . ? C67B C68B H68D 110.1 . . ? C69B C68B H68D 110.1 . . ? H68C C68B H68D 108.4 . . ? C70B C69B C68B 113(2) . . ? C70B C69B H69C 109.0 . . ? C68B C69B H69C 109.0 . . ? C70B C69B H69D 109.0 . . ? C68B C69B H69D 109.0 . . ? H69C C69B H69D 107.8 . . ? C71B C70B C69B 106(3) . . ? C71B C70B H70C 110.5 . . ? C69B C70B H70C 110.5 . . ? C71B C70B H70D 110.5 . . ? C69B C70B H70D 110.5 . . ? H70C C70B H70D 108.7 . . ? C70B C71B C77 110.3(13) . . ? C70B C71B H71C 109.6 . . ? C77 C71B H71C 109.6 . . ? C70B C71B H71D 109.6 . . ? C77 C71B H71D 109.6 . . ? H71C C71B H71D 108.1 . . ? C73 C72 C66 115.6(6) . . ? C73 C72 H72A 108.4 . . ? C66 C72 H72A 108.4 . . ? C73 C72 H72B 108.4 . . ? C66 C72 H72B 108.4 . . ? H72A C72 H72B 107.4 . . ? O6 C73 O5 105.6(5) . . ? O6 C73 C72 106.3(6) . . ? O5 C73 C72 112.0(6) . . ? O6 C73 C76 111.0(6) . . ? O5 C73 C76 105.5(6) . . ? C72 C73 C76 116.1(6) . . ? O5 C74 C75 102.3(7) . . ? O5 C74 H74A 111.3 . . ? C75 C74 H74A 111.3 . . ? O5 C74 H74B 111.3 . . ? C75 C74 H74B 111.3 . . ? H74A C74 H74B 109.2 . . ? O6 C75 C74 102.5(6) . . ? O6 C75 H75A 111.3 . . ? C74 C75 H75A 111.3 . . ? O6 C75 H75B 111.3 . . ? C74 C75 H75B 111.3 . . ? H75A C75 H75B 109.2 . . ? C73 C76 C77 116.1(6) . . ? C73 C76 H76A 108.3 . . ? C77 C76 H76A 108.3 . . ? C73 C76 H76B 108.3 . . ? C77 C76 H76B 108.3 . . ? H76A C76 H76B 107.4 . . ? C79A C77 C78A 107.4(7) . . ? C71B C77 C67B 107.4(7) . . ? C79A C77 C76 110.3(6) . . ? C71B C77 C76 110.3(6) . . ? C78A C77 C76 110.2(6) . . ? C67B C77 C76 110.2(6) . . ? C79A C77 P2 111.2(5) . . ? C71B C77 P2 111.2(5) . . ? C78A C77 P2 108.4(5) . . ? C67B C77 P2 108.4(5) . . ? C76 C77 P2 109.2(6) . . ? C77 C78A H78A 109.5 . . ? C77 C78A H78B 109.5 . . ? H78A C78A H78B 109.5 . . ? C77 C78A H78C 109.5 . . ? H78A C78A H78C 109.5 . . ? H78B C78A H78C 109.5 . . ? C77 C79A H79A 109.5 . . ? C77 C79A H79B 109.5 . . ? H79A C79A H79B 109.5 . . ? C77 C79A H79C 109.5 . . ? H79A C79A H79C 109.5 . . ? H79B C79A H79C 109.5 . . ? C66 C78B H78D 109.5 . . ? C66 C78B H78E 109.5 . . ? H78D C78B H78E 109.5 . . ? C66 C78B H78F 109.5 . . ? H78D C78B H78F 109.5 . . ? H78E C78B H78F 109.5 . . ? C66 C79B H79D 109.5 . . ? C66 C79B H79E 109.5 . . ? H79D C79B H79E 109.5 . . ? C66 C79B H79F 109.5 . . ? H79D C79B H79F 109.5 . . ? H79E C79B H79F 109.5 . . ? C86 C80 C81 117.7(6) . . ? C86 C80 Pd2 117.1(5) . . ? C81 C80 Pd2 124.5(5) . . ? C82 C81 C80 120.0(7) . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C83 C82 C81 120.5(7) . . ? C83 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C82 C83 C85 120.8(7) . . ? C82 C83 C84 120.5(7) . . ? C85 C83 C84 118.7(7) . . ? N2 C84 C83 178.8(9) . . ? C86 C85 C83 118.3(7) . . ? C86 C85 H85 120.9 . . ? C83 C85 H85 120.9 . . ? C85 C86 C80 122.7(6) . . ? C85 C86 H86 118.6 . . ? C80 C86 H86 118.6 . . ? _refine_diff_density_max 1.649 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.157 _shelx_res_file ; XRAY5803_0m_a.res created by SHELXL-2014/7 TITL XRAY5803_0m_a.res in Pbca CELL 1.54178 17.7459 19.0935 53.8014 90.000 90.000 90.000 ZERR 16.000 0.0008 0.0008 0.0025 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H Br N O P Pd UNIT 856 1104 16 16 48 16 16 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.10 0.10 0.90 EADP C69A C69B EADP C60 C59 EXYZ C78B C67A EXYZ C79B C71A EADP C78B C67A EADP C79B C71A EXYZ C78A C67B EXYZ C79A C71B EADP C78A C67B EADP C79A C71B TEMP -173.000 WGHT 0.093700 91.585190 FVAR 5.64167 0.75415 0.88991 MOLE 2 PD1 7 0.341145 0.291417 0.477043 11.00000 0.02223 0.02971 = 0.03517 0.00108 0.00204 -0.00042 BR1 3 0.450038 0.363242 0.464728 11.00000 0.02739 0.03662 = 0.04658 0.00170 0.00748 -0.00411 P1 6 0.251867 0.209700 0.490954 11.00000 0.02112 0.02559 = 0.03618 -0.00215 0.00221 -0.00130 O1 5 0.130529 0.098390 0.485693 11.00000 0.03075 0.03452 = 0.04956 -0.00927 0.00234 -0.00603 O2 5 0.228787 0.224168 0.568478 11.00000 0.03513 0.02851 = 0.04018 -0.00900 0.00669 -0.00545 O3 5 0.203930 0.108172 0.561382 11.00000 0.03118 0.02911 = 0.04215 0.00013 0.00794 -0.00820 N1 4 0.453915 0.438026 0.599181 11.00000 0.07371 0.13166 = 0.04896 -0.02563 0.00606 -0.04450 C1 1 0.214044 0.168193 0.462935 11.00000 0.02226 0.04098 = 0.04034 -0.01048 -0.00526 0.00298 C2 1 0.159262 0.114548 0.463106 11.00000 0.02380 0.04072 = 0.05001 -0.00908 0.00265 0.00290 C3 1 0.072213 0.046854 0.487466 11.00000 0.02589 0.02828 = 0.06448 0.00226 -0.00740 -0.00860 AFIX 137 H3A 2 0.092151 0.001113 0.482462 11.00000 -1.50000 H3B 2 0.030403 0.059840 0.476495 11.00000 -1.50000 H3C 2 0.054153 0.044319 0.504656 11.00000 -1.50000 AFIX 0 C4 1 0.133185 0.083283 0.441262 11.00000 0.04133 0.05913 = 0.05800 -0.02313 -0.00342 -0.01101 AFIX 43 H4 2 0.095444 0.048025 0.441773 11.00000 -1.20000 AFIX 0 C5 1 0.163271 0.104636 0.419138 11.00000 0.05376 0.09123 = 0.05357 -0.02643 -0.00674 -0.01091 AFIX 43 H5 2 0.146545 0.083727 0.404095 11.00000 -1.20000 AFIX 0 C6 1 0.218094 0.156628 0.418407 11.00000 0.05586 0.08919 = 0.04089 -0.01751 0.00013 -0.01565 AFIX 43 H6 2 0.238654 0.170192 0.402830 11.00000 -1.20000 AFIX 0 C7 1 0.243401 0.189070 0.439834 11.00000 0.03207 0.05416 = 0.04697 -0.00711 -0.00154 -0.00974 C8 1 0.298522 0.248243 0.435587 11.00000 0.04120 0.05876 = 0.02952 0.00385 -0.00135 -0.00159 C9 1 0.271778 0.318103 0.431778 11.00000 0.03101 0.07550 = 0.03568 0.00167 -0.00439 0.00256 C10 1 0.191807 0.339297 0.439490 11.00000 0.03884 0.07445 = 0.05212 0.00896 -0.00210 0.00619 AFIX 13 H10 2 0.171756 0.302730 0.451037 11.00000 -1.20000 AFIX 0 C11 1 0.191022 0.410664 0.453268 11.00000 0.05307 0.06685 = 0.06224 0.01287 0.00293 0.01805 AFIX 137 H11A 2 0.206345 0.447883 0.441789 11.00000 -1.50000 H11B 2 0.226160 0.408954 0.467307 11.00000 -1.50000 H11C 2 0.140066 0.420238 0.459413 11.00000 -1.50000 AFIX 0 C12 1 0.142062 0.341346 0.416778 11.00000 0.04218 0.15535 = 0.08781 -0.00583 -0.01703 0.02951 AFIX 137 H12A 2 0.169088 0.364126 0.403104 11.00000 -1.50000 H12B 2 0.096117 0.367782 0.420533 11.00000 -1.50000 H12C 2 0.128654 0.293461 0.411936 11.00000 -1.50000 AFIX 0 C13 1 0.315854 0.366411 0.419260 11.00000 0.04070 0.05431 = 0.04850 0.00451 -0.00086 0.00666 AFIX 43 H13 2 0.297782 0.412948 0.417390 11.00000 -1.20000 AFIX 0 C14 1 0.386225 0.348876 0.409265 11.00000 0.03408 0.06840 = 0.05034 0.01195 0.00538 -0.00125 C15 1 0.431438 0.404614 0.395753 11.00000 0.05242 0.07249 = 0.06811 0.02367 0.01049 -0.00075 AFIX 13 H15 2 0.426475 0.447809 0.406136 11.00000 -1.20000 AFIX 0 C16 1 0.395423 0.422638 0.371185 11.00000 0.08888 0.11887 = 0.05982 0.01726 0.00907 -0.01531 AFIX 137 H16A 2 0.393701 0.380769 0.360664 11.00000 -1.50000 H16B 2 0.425080 0.459095 0.362897 11.00000 -1.50000 H16C 2 0.344081 0.439761 0.374029 11.00000 -1.50000 AFIX 0 C17 1 0.514610 0.389263 0.394892 11.00000 0.07059 0.08200 = 0.08216 0.02630 0.01715 -0.00662 AFIX 137 H17A 2 0.531076 0.371256 0.411062 11.00000 -1.50000 H17B 2 0.542229 0.432361 0.391037 11.00000 -1.50000 H17C 2 0.524665 0.354177 0.382018 11.00000 -1.50000 AFIX 0 C18 1 0.412889 0.280054 0.412641 11.00000 0.03499 0.07666 = 0.04225 0.00502 0.00774 0.00128 AFIX 43 H18 2 0.460119 0.267475 0.405629 11.00000 -1.20000 AFIX 0 C19 1 0.372268 0.229283 0.425992 11.00000 0.03850 0.06176 = 0.03787 -0.01029 -0.00257 -0.00330 C20 1 0.404031 0.156284 0.429168 11.00000 0.04481 0.06299 = 0.04568 -0.01473 0.00517 -0.00152 AFIX 13 H20 2 0.368785 0.128578 0.439828 11.00000 -1.20000 AFIX 0 C21 1 0.413078 0.118845 0.404485 11.00000 0.09713 0.06774 = 0.06080 -0.02095 0.01174 0.00194 AFIX 137 H21A 2 0.368357 0.127040 0.394202 11.00000 -1.50000 H21B 2 0.418949 0.068478 0.407407 11.00000 -1.50000 H21C 2 0.457773 0.136825 0.395898 11.00000 -1.50000 AFIX 0 C22 1 0.481170 0.160659 0.442376 11.00000 0.04387 0.05742 = 0.05701 -0.00065 0.01121 0.00441 AFIX 137 H22A 2 0.518783 0.179713 0.430881 11.00000 -1.50000 H22B 2 0.496634 0.113730 0.447705 11.00000 -1.50000 H22C 2 0.477033 0.191309 0.456923 11.00000 -1.50000 AFIX 0 C23 1 0.300835 0.140442 0.510005 11.00000 0.02944 0.02523 = 0.04143 -0.00595 0.00099 0.00300 C24 1 0.381464 0.134947 0.499101 11.00000 0.03147 0.03047 = 0.03223 0.00075 0.00087 0.00716 AFIX 23 H24A 2 0.378071 0.117319 0.481832 11.00000 -1.20000 H24B 2 0.403889 0.182390 0.498473 11.00000 -1.20000 AFIX 0 C25 1 0.433733 0.087023 0.513881 11.00000 0.02832 0.04208 = 0.04385 -0.00518 0.00802 0.00798 AFIX 23 H25A 2 0.483902 0.085699 0.505847 11.00000 -1.20000 H25B 2 0.440103 0.105793 0.530905 11.00000 -1.20000 AFIX 0 C26 1 0.401570 0.013258 0.515215 11.00000 0.04483 0.03903 = 0.06000 -0.00710 -0.00520 0.01464 AFIX 23 H26A 2 0.402559 -0.008261 0.498477 11.00000 -1.20000 H26B 2 0.433036 -0.015732 0.526396 11.00000 -1.20000 AFIX 0 C27 1 0.321358 0.014859 0.524795 11.00000 0.04253 0.02329 = 0.04948 -0.00209 -0.00260 0.00215 AFIX 23 H27A 2 0.321750 0.030162 0.542375 11.00000 -1.20000 H27B 2 0.300375 -0.033158 0.524237 11.00000 -1.20000 AFIX 0 C28 1 0.269960 0.063753 0.509886 11.00000 0.03632 0.01872 = 0.03810 -0.00688 0.00229 0.00012 AFIX 23 H28A 2 0.218709 0.063084 0.517151 11.00000 -1.20000 H28B 2 0.266400 0.046800 0.492536 11.00000 -1.20000 AFIX 0 C29 1 0.299154 0.171127 0.536538 11.00000 0.02131 0.02269 = 0.03884 -0.00228 0.00039 0.00116 AFIX 23 H29A 2 0.333876 0.143448 0.547071 11.00000 -1.20000 H29B 2 0.318877 0.219593 0.535877 11.00000 -1.20000 AFIX 0 C30 1 0.221849 0.172675 0.549133 11.00000 0.02909 0.02100 = 0.03582 -0.00624 0.00283 -0.00192 C31 1 0.198402 0.195071 0.590419 11.00000 0.08302 0.04398 = 0.04472 -0.00977 0.01443 -0.00358 AFIX 23 H31A 2 0.143520 0.203735 0.591628 11.00000 -1.20000 H31B 2 0.223597 0.213976 0.605403 11.00000 -1.20000 AFIX 0 C32 1 0.215242 0.118027 0.586983 11.00000 0.06596 0.03720 = 0.04737 0.00404 0.00062 -0.00179 AFIX 23 H32A 2 0.267769 0.106967 0.591780 11.00000 -1.20000 H32B 2 0.180373 0.088663 0.596868 11.00000 -1.20000 AFIX 0 C33 1 0.155828 0.189132 0.532033 11.00000 0.02052 0.02454 = 0.04477 -0.00283 0.00463 -0.00464 AFIX 23 H33A 2 0.114006 0.207394 0.542343 11.00000 -1.20000 H33B 2 0.138415 0.144692 0.524491 11.00000 -1.20000 AFIX 0 C34 1 0.170642 0.241864 0.510910 11.00000 0.02059 0.03179 = 0.04339 -0.00332 0.00568 0.00071 C35 1 0.189978 0.314122 0.521924 11.00000 0.02816 0.02534 = 0.04784 0.00079 0.00513 -0.00015 AFIX 137 H35A 2 0.148772 0.329681 0.532721 11.00000 -1.50000 H35B 2 0.196917 0.347960 0.508420 11.00000 -1.50000 H35C 2 0.236548 0.310701 0.531638 11.00000 -1.50000 AFIX 0 C36 1 0.098158 0.252428 0.495780 11.00000 0.02406 0.04057 = 0.04916 -0.00137 0.00271 0.00879 AFIX 137 H36A 2 0.085079 0.208667 0.487295 11.00000 -1.50000 H36B 2 0.106109 0.289444 0.483438 11.00000 -1.50000 H36C 2 0.057024 0.265914 0.506952 11.00000 -1.50000 AFIX 0 C37 1 0.372667 0.328533 0.510679 11.00000 0.02462 0.03416 = 0.03919 0.00161 0.00256 -0.00867 C38 1 0.423635 0.296155 0.526426 11.00000 0.02112 0.04479 = 0.04072 0.00852 -0.00166 -0.00546 AFIX 43 H38 2 0.445473 0.252884 0.521519 11.00000 -1.20000 AFIX 0 C39 1 0.443622 0.324749 0.548968 11.00000 0.03017 0.05258 = 0.04373 0.00842 -0.00023 -0.01614 AFIX 43 H39 2 0.477566 0.300393 0.559538 11.00000 -1.20000 AFIX 0 C40 1 0.414848 0.388189 0.556274 11.00000 0.03666 0.05867 = 0.04150 -0.00157 0.00299 -0.02377 C41 1 0.435398 0.417874 0.580088 11.00000 0.05726 0.07435 = 0.05059 -0.00856 0.01280 -0.02980 C42 1 0.366641 0.425305 0.540230 11.00000 0.03626 0.04215 = 0.05067 -0.00673 0.01528 -0.02152 AFIX 43 H42 2 0.347891 0.470065 0.544836 11.00000 -1.20000 AFIX 0 C43 1 0.346687 0.395546 0.517451 11.00000 0.03013 0.03127 = 0.04026 -0.00454 0.00461 -0.00488 AFIX 43 H43 2 0.315145 0.420868 0.506370 11.00000 -1.20000 AFIX 0 PD2 7 0.356416 0.273825 0.698877 11.00000 0.03921 0.03132 = 0.03692 -0.00378 -0.00204 -0.00024 BR2 3 0.468613 0.201646 0.706895 11.00000 0.04385 0.04439 = 0.05030 -0.00455 -0.00912 0.00282 P2 6 0.266266 0.357957 0.688559 11.00000 0.04233 0.03768 = 0.03546 -0.00487 -0.00093 0.00386 O4 5 0.151737 0.474558 0.699950 11.00000 0.07330 0.05360 = 0.04525 -0.00252 0.00704 0.02882 O5 5 0.205129 0.467172 0.620193 11.00000 0.05723 0.04081 = 0.03850 -0.00601 -0.00445 0.01291 O6 5 0.221935 0.350426 0.612335 11.00000 0.04936 0.03922 = 0.03854 -0.00777 -0.00078 -0.00018 N2 4 0.441726 0.094653 0.580393 11.00000 0.04896 0.08002 = 0.04460 -0.02016 0.00599 -0.00318 C44 1 0.238587 0.398173 0.718349 11.00000 0.05048 0.03918 = 0.03663 -0.00820 -0.00165 0.00592 C45 1 0.187727 0.454132 0.720930 11.00000 0.05503 0.04349 = 0.04367 -0.00227 0.00640 0.00576 C46 1 0.110402 0.538774 0.701036 11.00000 0.04728 0.04335 = 0.06536 0.00766 0.01115 0.01203 AFIX 137 H46A 2 0.060949 0.530221 0.708553 11.00000 -1.50000 H46B 2 0.103715 0.557273 0.684189 11.00000 -1.50000 H46C 2 0.138213 0.572839 0.711111 11.00000 -1.50000 AFIX 0 C47 1 0.175348 0.484786 0.744075 11.00000 0.05833 0.03820 = 0.06398 -0.01032 0.01565 0.00052 AFIX 43 H47 2 0.144346 0.525204 0.745289 11.00000 -1.20000 AFIX 0 C48 1 0.206473 0.458091 0.764533 11.00000 0.06544 0.05711 = 0.04920 -0.01571 0.00762 -0.00055 AFIX 43 H48 2 0.194893 0.477996 0.780259 11.00000 -1.20000 AFIX 0 C49 1 0.255444 0.401762 0.763194 11.00000 0.06913 0.04112 = 0.04016 -0.00664 -0.00238 0.00060 AFIX 43 H49 2 0.277191 0.383243 0.777930 11.00000 -1.20000 AFIX 0 C50 1 0.272979 0.371948 0.739950 11.00000 0.06194 0.03817 = 0.03933 -0.00432 -0.00340 -0.00642 C51 1 0.326667 0.311733 0.741854 11.00000 0.05166 0.03508 = 0.03886 -0.00037 -0.00826 -0.00344 C52 1 0.298415 0.243540 0.746164 11.00000 0.05940 0.04143 = 0.03342 0.00178 -0.00058 0.00058 C53 1 0.216704 0.225104 0.740405 11.00000 0.05687 0.04025 = 0.04525 -0.00244 0.01041 0.00014 AFIX 13 H53 2 0.196214 0.263170 0.729575 11.00000 -1.20000 AFIX 0 C54 1 0.208952 0.156985 0.726181 11.00000 0.04690 0.05004 = 0.05540 -0.00055 0.00089 -0.01320 AFIX 137 H54A 2 0.223564 0.117813 0.736919 11.00000 -1.50000 H54B 2 0.241772 0.158105 0.711537 11.00000 -1.50000 H54C 2 0.156507 0.150983 0.720888 11.00000 -1.50000 AFIX 0 C55 1 0.170532 0.225381 0.764569 11.00000 0.06849 0.06371 = 0.06592 -0.01156 0.01528 -0.00078 AFIX 137 H55A 2 0.188460 0.187919 0.775527 11.00000 -1.50000 H55B 2 0.117217 0.217734 0.760673 11.00000 -1.50000 H55C 2 0.176475 0.270665 0.772916 11.00000 -1.50000 AFIX 0 C56 1 0.343339 0.194393 0.758757 11.00000 0.05957 0.03888 = 0.04556 0.00690 0.00359 0.00100 AFIX 43 H56 2 0.324202 0.148574 0.761502 11.00000 -1.20000 AFIX 0 C57 1 0.414316 0.210916 0.767214 11.00000 0.07170 0.04772 = 0.03946 -0.00070 -0.00711 0.01006 C58 1 0.460824 0.158464 0.782389 11.00000 0.09464 0.06811 = 0.04852 0.01383 -0.01962 0.02365 AFIX 13 H58 2 0.501039 0.184841 0.791438 11.00000 -1.20000 AFIX 0 C59 1 0.411461 0.119580 0.801867 11.00000 0.08671 0.07461 = 0.09246 0.01522 -0.02054 0.01353 AFIX 137 H59A 2 0.393673 0.153021 0.814377 11.00000 -1.50000 H59B 2 0.441490 0.083052 0.809969 11.00000 -1.50000 H59C 2 0.368104 0.098154 0.793533 11.00000 -1.50000 AFIX 0 C60 1 0.498429 0.103864 0.766012 11.00000 0.08671 0.07461 = 0.09246 0.01522 -0.02054 0.01353 AFIX 137 H60A 2 0.459904 0.078560 0.756542 11.00000 -1.50000 H60B 2 0.526432 0.070775 0.776432 11.00000 -1.50000 H60C 2 0.533207 0.127039 0.754499 11.00000 -1.50000 AFIX 0 C61 1 0.443456 0.276316 0.761917 11.00000 0.05564 0.05287 = 0.04940 -0.00060 -0.01177 0.00045 AFIX 43 H61 2 0.493513 0.286782 0.766956 11.00000 -1.20000 AFIX 0 C62 1 0.401940 0.327796 0.749390 11.00000 0.06769 0.04421 = 0.04455 -0.00677 -0.01010 -0.00655 C63 1 0.437477 0.398760 0.745250 11.00000 0.06351 0.04225 = 0.05174 -0.00471 -0.01759 -0.00815 AFIX 13 H63 2 0.401632 0.426871 0.734946 11.00000 -1.20000 AFIX 0 C64 1 0.448386 0.437808 0.769787 11.00000 0.07873 0.05295 = 0.06214 -0.01379 -0.01996 -0.00957 AFIX 137 H64A 2 0.485226 0.412790 0.780049 11.00000 -1.50000 H64B 2 0.400186 0.440396 0.778629 11.00000 -1.50000 H64C 2 0.466742 0.485275 0.766415 11.00000 -1.50000 AFIX 0 C65 1 0.511098 0.393688 0.730831 11.00000 0.05422 0.05940 = 0.07319 -0.00750 -0.00359 -0.00956 AFIX 137 H65A 2 0.549438 0.371128 0.741212 11.00000 -1.50000 H65B 2 0.528066 0.440798 0.726254 11.00000 -1.50000 H65C 2 0.503178 0.365874 0.715747 11.00000 -1.50000 AFIX 0 C66 1 0.312344 0.428499 0.669044 11.00000 0.04794 0.03463 = 0.03930 -0.00813 0.00145 0.00092 PART 1 C67A 1 0.395936 0.429814 0.677391 21.00000 0.05334 0.03711 = 0.04963 -0.00374 -0.01042 -0.00271 AFIX 23 H67A 2 0.397564 0.440115 0.695417 21.00000 -1.20000 H67B 2 0.417388 0.382443 0.674962 21.00000 -1.20000 AFIX 0 C68A 1 0.444273 0.480444 0.664510 21.00000 0.03857 0.03998 = 0.03473 0.00389 0.00105 -0.01085 AFIX 23 H68A 2 0.449397 0.467026 0.646816 21.00000 -1.20000 H68B 2 0.495101 0.480398 0.672094 21.00000 -1.20000 AFIX 0 C69A 1 0.409063 0.555257 0.666451 21.00000 0.03988 0.03262 = 0.04381 0.00368 0.00761 -0.01029 AFIX 23 H69A 2 0.410050 0.571183 0.683960 21.00000 -1.20000 H69B 2 0.438991 0.588627 0.656406 21.00000 -1.20000 AFIX 0 C70A 1 0.327469 0.553771 0.657009 21.00000 0.04848 0.03519 = 0.03905 0.00640 0.00617 -0.00131 AFIX 23 H70A 2 0.305098 0.601090 0.658472 21.00000 -1.20000 H70B 2 0.326828 0.540201 0.639251 21.00000 -1.20000 AFIX 0 C71A 1 0.283081 0.504184 0.671333 21.00000 0.06458 0.04191 = 0.03854 -0.00806 -0.00108 0.00630 AFIX 23 H71A 2 0.230138 0.505926 0.665565 21.00000 -1.20000 H71B 2 0.283864 0.518232 0.689044 21.00000 -1.20000 PART 2 AFIX 0 C67B 1 0.190166 0.260470 0.658344 -21.00000 0.04160 0.05078 = 0.04897 -0.00174 -0.00335 -0.00261 AFIX 23 H67C 2 0.234471 0.262782 0.647193 -21.00000 -1.20000 H67D 2 0.200070 0.224684 0.671253 -21.00000 -1.20000 AFIX 0 C68B 1 0.123398 0.241714 0.644218 -21.00000 0.03320 0.02455 = 0.02041 -0.00288 0.01213 -0.00308 AFIX 23 H68C 2 0.129865 0.194826 0.636658 -21.00000 -1.20000 H68D 2 0.114967 0.276095 0.630728 -21.00000 -1.20000 AFIX 0 C69B 1 0.056054 0.241360 0.662015 -21.00000 0.03988 0.03262 = 0.04381 0.00368 0.00761 -0.01029 AFIX 23 H69C 2 0.010108 0.228501 0.652629 -21.00000 -1.20000 H69D 2 0.064306 0.205099 0.674883 -21.00000 -1.20000 AFIX 0 C70B 1 0.043505 0.310534 0.674502 -21.00000 0.04983 0.06868 = 0.02534 -0.02910 0.00679 -0.01767 AFIX 23 H70C 2 0.034614 0.347650 0.661992 -21.00000 -1.20000 H70D 2 -0.000710 0.308149 0.685691 -21.00000 -1.20000 AFIX 0 C71B 1 0.109151 0.324646 0.688110 -21.00000 0.03916 0.06368 = 0.05528 0.00410 0.00330 0.00298 AFIX 23 H71C 2 0.118583 0.286078 0.700009 -21.00000 -1.20000 H71D 2 0.102463 0.368437 0.697712 -21.00000 -1.20000 PART 0 AFIX 0 C72 1 0.303430 0.400721 0.642157 11.00000 0.04663 0.03917 = 0.03688 -0.00531 0.00262 0.00416 AFIX 23 H72A 2 0.335689 0.429248 0.631071 11.00000 -1.20000 H72B 2 0.322559 0.352040 0.641591 11.00000 -1.20000 AFIX 0 C73 1 0.223482 0.401318 0.631853 11.00000 0.05106 0.03533 = 0.04063 -0.00550 -0.00483 0.00736 C74 1 0.204383 0.456142 0.593754 11.00000 0.07734 0.04748 = 0.03786 -0.00540 -0.00500 0.01176 AFIX 23 H74A 2 0.254585 0.465039 0.586376 11.00000 -1.20000 H74B 2 0.166656 0.486481 0.585519 11.00000 -1.20000 AFIX 0 C75 1 0.183288 0.380789 0.591789 11.00000 0.07164 0.04858 = 0.04077 -0.01297 -0.01431 0.00885 AFIX 23 H75A 2 0.128118 0.374345 0.593282 11.00000 -1.20000 H75B 2 0.200599 0.360425 0.575859 11.00000 -1.20000 AFIX 0 C76 1 0.160595 0.388044 0.650589 11.00000 0.04445 0.05792 = 0.04565 -0.01061 -0.00422 0.00808 AFIX 23 H76A 2 0.114864 0.373779 0.641346 11.00000 -1.20000 H76B 2 0.149011 0.432770 0.659078 11.00000 -1.20000 AFIX 0 C77 1 0.176844 0.332211 0.670579 11.00000 0.03823 0.05019 = 0.04350 -0.00630 -0.00051 0.00830 PART 1 C78A 1 0.190166 0.260470 0.658344 21.00000 0.04160 0.05078 = 0.04897 -0.00174 -0.00335 -0.00261 AFIX 33 H78A 2 0.233215 0.263543 0.646987 21.00000 -1.50000 H78B 2 0.200669 0.225507 0.671222 21.00000 -1.50000 H78C 2 0.145103 0.246646 0.649028 21.00000 -1.50000 AFIX 0 C79A 1 0.109151 0.324646 0.688110 21.00000 0.03916 0.06368 = 0.05528 0.00410 0.00330 0.00298 AFIX 33 H79A 2 0.099152 0.369639 0.696230 21.00000 -1.50000 H79B 2 0.064746 0.310302 0.678552 21.00000 -1.50000 H79C 2 0.120312 0.289163 0.700746 21.00000 -1.50000 PART 2 AFIX 0 C78B 1 0.395936 0.429814 0.677391 -21.00000 0.05334 0.03711 = 0.04963 -0.00374 -0.01042 -0.00271 AFIX 33 H78D 2 0.417087 0.382512 0.676243 -21.00000 -1.50000 H78E 2 0.424505 0.461493 0.666593 -21.00000 -1.50000 H78F 2 0.399065 0.446269 0.694614 -21.00000 -1.50000 AFIX 0 C79B 1 0.283081 0.504184 0.671333 -21.00000 0.06458 0.04191 = 0.03854 -0.00806 -0.00108 0.00630 AFIX 33 H79D 2 0.289383 0.520407 0.688489 -21.00000 -1.50000 H79E 2 0.311669 0.534663 0.660114 -21.00000 -1.50000 H79F 2 0.229577 0.505628 0.666852 -21.00000 -1.50000 PART 0 AFIX 0 C80 1 0.374578 0.235322 0.664485 11.00000 0.03592 0.03278 = 0.03888 -0.00205 0.00103 -0.00040 C81 1 0.426621 0.263700 0.647219 11.00000 0.03127 0.04017 = 0.05052 -0.00653 0.00531 -0.00146 AFIX 43 H81 2 0.451199 0.306788 0.650718 11.00000 -1.20000 AFIX 0 C82 1 0.441714 0.228344 0.625103 11.00000 0.04523 0.04326 = 0.04405 0.00104 0.00784 -0.00724 AFIX 43 H82 2 0.474558 0.248690 0.613174 11.00000 -1.20000 AFIX 0 C83 1 0.409274 0.163979 0.620414 11.00000 0.03374 0.04693 = 0.03867 -0.00102 0.00251 -0.00134 C84 1 0.428113 0.125488 0.598111 11.00000 0.03685 0.05578 = 0.04924 -0.00355 0.00908 -0.00147 C85 1 0.358422 0.134242 0.637250 11.00000 0.04173 0.04119 = 0.03848 -0.00171 -0.00131 -0.00624 AFIX 43 H85 2 0.335456 0.090293 0.633912 11.00000 -1.20000 AFIX 0 C86 1 0.342427 0.170502 0.658897 11.00000 0.03381 0.03548 = 0.03673 -0.00100 0.00503 -0.00735 AFIX 43 H86 2 0.308131 0.150422 0.670431 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5803_0m_a.res in Pbca REM R1 = 0.0777 for 12903 Fo > 4sig(Fo) and 0.1074 for all 16123 data REM 934 parameters refined using 0 restraints END WGHT 0.0923 96.4980 REM Highest difference peak 1.649, deepest hole -1.043, 1-sigma level 0.157 Q1 1 0.4233 0.3621 0.4512 11.00000 0.05 1.65 Q2 1 0.3288 0.2708 0.4666 11.00000 0.05 1.52 Q3 1 0.4043 0.2616 0.7057 11.00000 0.05 1.02 Q4 1 0.2967 0.2885 0.4745 11.00000 0.05 0.98 Q5 1 0.4396 0.1607 0.8097 11.00000 0.05 0.94 Q6 1 0.4401 0.2375 0.7164 11.00000 0.05 0.84 Q7 1 0.4374 0.1678 0.7159 11.00000 0.05 0.81 Q8 1 0.5223 0.1983 0.7097 11.00000 0.05 0.81 Q9 1 0.3395 0.2921 0.4940 11.00000 0.05 0.78 Q10 1 0.2992 0.2839 0.7005 11.00000 0.05 0.73 Q11 1 0.3514 0.3202 0.4690 11.00000 0.05 0.71 Q12 1 0.3966 0.2989 0.4756 11.00000 0.05 0.68 Q13 1 0.1564 0.6059 0.6983 11.00000 0.05 0.66 Q14 1 0.4581 0.2015 0.7295 11.00000 0.05 0.62 Q15 1 0.5052 0.3591 0.4644 11.00000 0.05 0.62 Q16 1 0.3606 0.4025 0.6975 11.00000 0.05 0.59 Q17 1 0.3555 0.2754 0.7193 11.00000 0.05 0.57 Q18 1 0.3568 0.2529 0.7521 11.00000 0.05 0.57 Q19 1 0.4853 0.3845 0.4592 11.00000 0.05 0.56 Q20 1 0.4983 0.2076 0.6853 11.00000 0.05 0.55 ; _shelx_res_checksum 13379 _shelx_hkl_file ; 2 0 014076994 1109501 25738340 -228.10 0.59 1.0000 4 0 0 4684833 287367 6124448 -53.72 0.03 1.0000 6 0 0 1914554 79932 1387171 -36.67 1.59 1.0000 8 0 0 3578469 591586 3500641 3.58 0.15 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1.0000 1 4 60 77324 6713 68297 -2.59 -2.87 1.0000 2 4 60 42729 6405 36619 2.66 0.00 1.0000 3 4 60 81 4950 -4950 0.96 -1.22 1.0000 4 4 60 62532 8183 63266 -0.21 -0.30 1.0000 5 4 60 230084 10257 227070 0.67 -1.02 1.0000 6 4 60 5381 5508 5828 -0.76 2.57 1.0000 1 5 60 3516 6356 5032 -1.38 -1.50 1.0000 2 5 60 30586 6915 28401 -0.75 -3.33 1.0000 3 5 60 68776 7539 64619 -1.64 1.54 1.0000 4 5 60 84191 9982 88874 -1.44 0.95 1.0000 5 5 60 82 5688 -5688 1.46 0.54 1.0000 0 6 60 75089 12687 79325 -1.43 0.67 1.0000 1 6 60 26445 6887 25907 0.27 0.18 1.0000 2 6 60 13311 5106 14103 0.61 -0.22 1.0000 3 6 60 8037 9361 14644 3.60 4.16 1.0000 4 6 60 8566 5751 11795 2.32 1.88 1.0000 1 7 60 1968 7174 1887 -0.11 -0.90 1.0000 2 7 60 116483 8344 114850 0.61 -1.33 1.0000 3 7 60 29780 6729 38230 3.91 0.96 1.0000 1 1 61 23354 5607 26946 -1.98 1.02 1.0000 2 1 61 16328 5617 16603 0.02 4.06 1.0000 3 1 61 21836 5098 20443 0.95 -0.87 1.0000 4 1 61 10267 4387 12564 1.50 -2.03 1.0000 5 1 61 8118 4164 9617 -0.96 -2.85 1.0000 6 1 61 19441 4359 19706 -0.16 0.00 1.0000 0 2 61 25718 11962 27087 0.33 2.12 1.0000 1 2 61 15784 5531 17895 1.51 -2.95 1.0000 2 2 61 12162 5010 14824 1.98 -0.06 1.0000 3 2 61 11818 6266 12259 -0.26 -0.68 1.0000 4 2 61 5173 4589 9500 1.92 -4.20 1.0000 5 2 61 70911 5814 71247 -0.19 0.88 1.0000 6 2 61 23682 4716 23411 0.15 0.04 1.0000 1 3 61 40340 5998 39751 -0.27 0.33 1.0000 2 3 61 42535 5638 43752 0.54 -2.58 1.0000 3 3 61 50278 5557 51152 -0.18 2.77 1.0000 4 3 61 3792 4714 3933 0.56 4.10 1.0000 5 3 61 71 4576 -4576 -1.44 0.20 1.0000 0 4 61 16770 11693 17114 -0.25 1.82 1.0000 1 4 61 180 6509 -6509 2.30 -0.25 1.0000 2 4 61 59137 7558 60905 0.61 0.18 1.0000 3 4 61 6245 4824 5686 -0.52 -1.82 1.0000 4 4 61 6461 6155 4212 2.89 1.55 1.0000 5 4 61 111563 8082 111636 0.16 -1.58 1.0000 1 5 61 6536 7134 4557 2.32 -2.51 1.0000 2 5 61 238 6635 -5333 -0.58 2.60 1.0000 3 5 61 50315 8493 50549 -0.36 2.58 1.0000 4 5 61 45240 6480 45249 0.09 -0.80 1.0000 0 6 61 41821 16177 45795 -1.54 -0.89 1.0000 1 6 61 10217 7988 12232 -1.48 1.60 1.0000 2 6 61 73635 6802 73575 -0.13 1.77 1.0000 3 6 61 277 5658 -4607 -1.77 2.26 1.0000 0 0 62 280947 19249 268768 1.67 2.20 1.0000 1 0 62 13630 8421 19336 3.80 3.80 1.0000 2 0 62 248448 13246 236215 -1.98 -1.56 1.0000 3 0 62 210 10023 -10023 1.36 -2.10 1.0000 4 0 62 114822 8435 111649 -0.57 -1.48 1.0000 5 0 62 163463 19513 172776 1.72 1.98 1.0000 1 1 62 15149 5678 11037 3.09 0.81 1.0000 2 1 62 206558 8467 195558 2.24 -0.47 1.0000 3 1 62 115556 6834 124252 -2.26 0.83 1.0000 4 1 62 147098 7015 147394 -0.32 1.97 1.0000 5 1 62 31765 4509 29565 1.31 -1.11 1.0000 0 2 62 169208 15460 176410 1.35 0.84 1.0000 1 2 62 9615 5472 10752 0.81 0.88 1.0000 2 2 62 26931 5413 29317 -0.49 -2.08 1.0000 3 2 62 7863 5570 4942 3.13 -0.85 1.0000 4 2 62 140232 6950 140309 -0.12 0.73 1.0000 5 2 62 56474 11457 55842 0.06 1.35 1.0000 1 3 62 17251 6004 12454 3.32 0.98 1.0000 2 3 62 221782 9374 201874 -3.84 0.35 1.0000 3 3 62 74515 6603 74178 -0.16 0.51 1.0000 4 3 62 7921 6236 7958 -0.44 0.98 1.0000 0 4 62 229751 18864 212078 3.06 1.59 1.0000 1 4 62 128114 10164 127854 -0.12 2.18 1.0000 2 4 62 19088 8189 16018 -1.99 -0.21 1.0000 3 4 62 144 5787 -5787 1.72 1.16 1.0000 1 5 62 70771 8215 77980 1.78 3.69 1.0000 2 5 62 25716 7356 26129 -0.04 -0.77 1.0000 1 1 63 12908 5754 11852 -0.61 -2.54 1.0000 2 1 63 9276 5159 9752 -0.66 0.93 1.0000 3 1 63 5086 5219 2919 -2.22 2.85 1.0000 0 2 63 170551 18339 167105 -1.06 2.63 1.0000 1 2 63 10656 5783 10039 -1.78 3.79 1.0000 2 2 63 6 6963 -1994 0.29 -0.30 1.0000 3 2 63 100276 8342 101482 0.22 1.34 1.0000 1 3 63 108410 8909 107499 0.08 1.30 1.0000 2 3 63 86378 8527 87393 0.32 -0.18 1.0000 0 4 63 93003 12994 94197 -0.46 1.30 1.0000 1 4 63 69018 14279 70588 -0.92 1.91 1.0000 0 0 64 88729 27124 106634 -4.71 -1.54 1.0000 1 0 64 192709 15067 194309 0.07 1.67 1.0000 ; _shelx_hkl_checksum 21039 #===END data_Ox_5j _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Ox_5j' _chemical_melting_point ? _chemical_formula_moiety 'C46 H61 Br N O3 P Pd, 0.5(C5 H12), C H2 Cl2' _chemical_formula_sum 'C49.50 H69 Br Cl2 N O3 P Pd' _chemical_formula_weight 1014.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.660(13) _cell_length_b 21.676(10) _cell_length_c 19.545(9) _cell_angle_alpha 90 _cell_angle_beta 123.911(5) _cell_angle_gamma 90 _cell_volume 9725(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9853 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 27.279 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_F_000 4216 _exptl_transmission_factor_min 0.869 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 1.387 _shelx_estimated_absorpt_T_min 0.607 _shelx_estimated_absorpt_T_max 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56993 _diffrn_reflns_av_unetI/netI 0.0604 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.415 _diffrn_reflns_theta_max 27.497 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 11093 _reflns_number_gt 8522 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+16.5434P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11093 _refine_ls_number_parameters 557 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1A Cl 0.6722(12) 0.8142(8) 0.2010(14) 0.0959(12) Uani 0.274(6) 1 d D . P A 1 Cl2A Cl 0.6537(3) 0.7306(4) 0.0787(4) 0.0628(8) Uani 0.274(6) 1 d D . P A 1 C47A C 0.6618(7) 0.7384(8) 0.1722(8) 0.0278(12) Uani 0.274(6) 1 d D . P A 1 H47A H 0.626560 0.722617 0.167813 0.033 Uiso 0.274(6) 1 calc R U P A 1 H47B H 0.695589 0.713758 0.214449 0.033 Uiso 0.274(6) 1 calc R U P A 1 Cl1B Cl 0.6698(4) 0.8043(3) 0.1850(5) 0.0959(12) Uani 0.726(6) 1 d D . P A 2 Cl2B Cl 0.63524(12) 0.70038(16) 0.07050(12) 0.0628(8) Uani 0.726(6) 1 d D . P A 2 C47B C 0.6445(2) 0.7295(3) 0.1610(3) 0.0278(12) Uani 0.726(6) 1 d D . P A 2 H47C H 0.606680 0.727322 0.155327 0.033 Uiso 0.726(6) 1 calc R U P A 2 H47D H 0.672177 0.702459 0.207644 0.033 Uiso 0.726(6) 1 calc R U P A 2 C48 C 0.1063(9) 0.3160(10) 0.8902(15) 0.074(2) Uani 0.5 1 d D . P B -1 H48A H 0.125219 0.307676 0.861155 0.111 Uiso 0.5 1 calc R U P B -1 H48B H 0.130915 0.300641 0.946886 0.111 Uiso 0.5 1 calc R U P B -1 H48C H 0.100680 0.360602 0.891058 0.111 Uiso 0.5 1 calc R U P B -1 C49 C 0.0496(5) 0.2849(6) 0.8476(7) 0.090(3) Uani 0.5 1 d D . P B -1 H49A H 0.031368 0.291782 0.878467 0.108 Uiso 0.5 1 calc R U P B -1 H49B H 0.055305 0.239974 0.846112 0.108 Uiso 0.5 1 calc R U P B -1 C50 C 0.0095(10) 0.3089(4) 0.7603(16) 0.063(4) Uani 0.5 1 d D . P B -1 H50A H 0.006912 0.354310 0.762646 0.076 Uiso 0.5 1 calc R U P B -1 H50B H 0.027468 0.299800 0.729551 0.076 Uiso 0.5 1 calc R U P B -1 C51 C -0.0516(5) 0.2828(6) 0.7124(7) 0.090(3) Uani 0.5 1 d D . P B -1 H51A H -0.048197 0.237585 0.708774 0.108 Uiso 0.5 1 calc R U P B -1 H51B H -0.067730 0.289455 0.746111 0.108 Uiso 0.5 1 calc R U P B -1 C52 C -0.0950(8) 0.3049(11) 0.6292(13) 0.074(2) Uani 0.5 1 d D . P B -1 H52A H -0.098734 0.349775 0.630259 0.111 Uiso 0.5 1 calc R U P B -1 H52B H -0.132701 0.285518 0.609278 0.111 Uiso 0.5 1 calc R U P B -1 H52C H -0.082760 0.294164 0.592388 0.111 Uiso 0.5 1 calc R U P B -1 Pd1 Pd 0.26070(2) 0.08198(2) 0.42556(2) 0.01420(6) Uani 1 1 d . . . . . Br1 Br 0.27469(2) 0.17301(2) 0.36246(2) 0.01863(7) Uani 1 1 d . . . . . P1 P 0.24031(3) 0.00863(3) 0.49454(4) 0.01448(15) Uani 1 1 d . . . . . O1 O 0.27356(8) -0.08106(9) 0.63650(12) 0.0210(4) Uani 1 1 d . . . . . O2 O 0.06236(8) -0.03699(10) 0.35356(11) 0.0194(4) Uani 1 1 d . . . . . O3 O 0.08501(8) -0.04671(10) 0.48538(12) 0.0210(4) Uani 1 1 d . . . . . N1 N -0.02526(12) 0.13557(14) 0.03510(17) 0.0348(7) Uani 1 1 d . . . . . C1 C 0.31200(11) -0.00827(13) 0.58945(16) 0.0165(6) Uani 1 1 d . . . . . C2 C 0.32115(12) -0.04948(13) 0.65203(17) 0.0185(6) Uani 1 1 d . . . . . C3 C 0.27809(15) -0.11696(17) 0.70090(19) 0.0327(8) Uani 1 1 d . . . . . H3A H 0.303017 -0.152841 0.712000 0.049 Uiso 1 1 calc R U . . . H3B H 0.239248 -0.130929 0.684106 0.049 Uiso 1 1 calc R U . . . H3C H 0.295130 -0.091801 0.750891 0.049 Uiso 1 1 calc R U . . . C4 C 0.37593(13) -0.05722(15) 0.72464(18) 0.0247(7) Uani 1 1 d . . . . . H4 H 0.380885 -0.084368 0.766266 0.030 Uiso 1 1 calc R U . . . C5 C 0.42313(13) -0.02515(15) 0.73586(18) 0.0273(7) Uani 1 1 d . . . . . H5 H 0.460586 -0.030317 0.785292 0.033 Uiso 1 1 calc R U . . . C6 C 0.41587(12) 0.01423(15) 0.67549(18) 0.0236(6) Uani 1 1 d . . . . . H6 H 0.448630 0.035639 0.683524 0.028 Uiso 1 1 calc R U . . . C7 C 0.36099(12) 0.02324(13) 0.60245(16) 0.0172(6) Uani 1 1 d . . . . . C8 C 0.36206(11) 0.06737(13) 0.54331(17) 0.0183(6) Uani 1 1 d . . . . . C9 C 0.37740(12) 0.13001(14) 0.56909(18) 0.0211(6) Uani 1 1 d . . . . . C10 C 0.36575(13) 0.15991(15) 0.62887(19) 0.0258(7) Uani 1 1 d . . . . . H10 H 0.345596 0.128853 0.642476 0.031 Uiso 1 1 calc R U . . . C11 C 0.32504(14) 0.21536(15) 0.5886(2) 0.0334(8) Uani 1 1 d . . . . . H11A H 0.345619 0.248667 0.581089 0.050 Uiso 1 1 calc R U . . . H11B H 0.312660 0.229743 0.624098 0.050 Uiso 1 1 calc R U . . . H11C H 0.290776 0.203162 0.534882 0.050 Uiso 1 1 calc R U . . . C12 C 0.42235(15) 0.17896(18) 0.7098(2) 0.0415(9) Uani 1 1 d . . . . . H12A H 0.446870 0.142490 0.736170 0.062 Uiso 1 1 calc R U . . . H12B H 0.412995 0.197502 0.746828 0.062 Uiso 1 1 calc R U . . . H12C H 0.443273 0.209024 0.698094 0.062 Uiso 1 1 calc R U . . . C13 C 0.40456(12) 0.16425(15) 0.53900(19) 0.0267(7) Uani 1 1 d . . . . . H13 H 0.414516 0.206026 0.555765 0.032 Uiso 1 1 calc R U . . . C14 C 0.41764(13) 0.13921(16) 0.48495(19) 0.0275(7) Uani 1 1 d . . . . . C15 C 0.45160(15) 0.17517(18) 0.4576(2) 0.0380(9) Uani 1 1 d . . . . . H15 H 0.461353 0.145752 0.427639 0.046 Uiso 1 1 calc R U . . . C16 C 0.41632(17) 0.22595(19) 0.3994(3) 0.0475(10) Uani 1 1 d . . . . . H16A H 0.379970 0.209048 0.352266 0.071 Uiso 1 1 calc R U . . . H16B H 0.438447 0.245634 0.379972 0.071 Uiso 1 1 calc R U . . . H16C H 0.407341 0.256554 0.427684 0.071 Uiso 1 1 calc R U . . . C17 C 0.50914(14) 0.19881(17) 0.5327(2) 0.0342(8) Uani 1 1 d . . . . . H17A H 0.531717 0.219023 0.514340 0.051 Uiso 1 1 calc R U . . . H17B H 0.531456 0.164062 0.568805 0.051 Uiso 1 1 calc R U . . . H17C H 0.501095 0.228478 0.562971 0.051 Uiso 1 1 calc R U . . . C18 C 0.40038(12) 0.08004(15) 0.45812(19) 0.0252(7) Uani 1 1 d . . . . . H18 H 0.406922 0.063502 0.418931 0.030 Uiso 1 1 calc R U . . . C19 C 0.37360(12) 0.04310(14) 0.48595(17) 0.0199(6) Uani 1 1 d . . . . . C20 C 0.36328(13) -0.02460(15) 0.46088(19) 0.0251(7) Uani 1 1 d . . . . . H20 H 0.340772 -0.043157 0.481778 0.030 Uiso 1 1 calc R U . . . C21 C 0.32675(15) -0.03231(17) 0.3665(2) 0.0330(8) Uani 1 1 d . . . . . H21A H 0.291002 -0.007837 0.342110 0.050 Uiso 1 1 calc R U . . . H21B H 0.316668 -0.075898 0.352481 0.050 Uiso 1 1 calc R U . . . H21C H 0.349339 -0.018082 0.344804 0.050 Uiso 1 1 calc R U . . . C22 C 0.42133(16) -0.05953(18) 0.5011(2) 0.0422(9) Uani 1 1 d . . . . . H22A H 0.444679 -0.041774 0.482488 0.063 Uiso 1 1 calc R U . . . H22B H 0.413666 -0.103132 0.485330 0.063 Uiso 1 1 calc R U . . . H22C H 0.442671 -0.055969 0.561222 0.063 Uiso 1 1 calc R U . . . C23 C 0.19364(11) 0.04621(13) 0.52669(16) 0.0161(6) Uani 1 1 d . . . . . C24 C 0.21054(12) 0.11553(13) 0.53791(17) 0.0180(6) Uani 1 1 d . . . . . H24A H 0.252195 0.119598 0.583132 0.022 Uiso 1 1 calc R U . . . H24B H 0.205864 0.130779 0.486790 0.022 Uiso 1 1 calc R U . . . C25 C 0.17453(13) 0.15636(14) 0.55739(18) 0.0230(6) Uani 1 1 d . . . . . H25A H 0.188324 0.199538 0.565029 0.028 Uiso 1 1 calc R U . . . H25B H 0.133127 0.155317 0.510580 0.028 Uiso 1 1 calc R U . . . C26 C 0.18000(14) 0.13394(15) 0.63561(19) 0.0263(7) Uani 1 1 d . . . . . H26A H 0.220224 0.141073 0.683850 0.032 Uiso 1 1 calc R U . . . H26B H 0.153107 0.157708 0.643918 0.032 Uiso 1 1 calc R U . . . C27 C 0.16556(14) 0.06541(14) 0.62914(18) 0.0231(6) Uani 1 1 d . . . . . H27A H 0.123735 0.059387 0.585700 0.028 Uiso 1 1 calc R U . . . H27B H 0.172402 0.051271 0.682031 0.028 Uiso 1 1 calc R U . . . C28 C 0.20200(12) 0.02583(14) 0.60883(16) 0.0183(6) Uani 1 1 d . . . . . H28A H 0.190488 -0.017964 0.604583 0.022 Uiso 1 1 calc R U . . . H28B H 0.243685 0.029344 0.654157 0.022 Uiso 1 1 calc R U . . . C29 C 0.13083(11) 0.03434(13) 0.45190(16) 0.0162(6) Uani 1 1 d . . . . . H29A H 0.103998 0.060255 0.458033 0.019 Uiso 1 1 calc R U . . . H29B H 0.127973 0.048198 0.401496 0.019 Uiso 1 1 calc R U . . . C30 C 0.10987(12) -0.03222(14) 0.43924(16) 0.0176(6) Uani 1 1 d . . . . . C31 C 0.01442(14) -0.06498(18) 0.34992(19) 0.0329(8) Uani 1 1 d . . . . . H31A H 0.015914 -0.110493 0.347280 0.039 Uiso 1 1 calc R U . . . H31B H -0.023162 -0.050057 0.301708 0.039 Uiso 1 1 calc R U . . . C32 C 0.02292(13) -0.04439(17) 0.42949(19) 0.0284(7) Uani 1 1 d . . . . . H32A H 0.007964 -0.002044 0.424881 0.034 Uiso 1 1 calc R U . . . H32B H 0.003569 -0.072788 0.446716 0.034 Uiso 1 1 calc R U . . . C33 C 0.15642(12) -0.08107(13) 0.46231(17) 0.0178(6) Uani 1 1 d . . . . . H33A H 0.136546 -0.120167 0.434743 0.021 Uiso 1 1 calc R U . . . H33B H 0.178163 -0.088193 0.522503 0.021 Uiso 1 1 calc R U . . . C34 C 0.20098(12) -0.06634(13) 0.44034(16) 0.0167(6) Uani 1 1 d . . . . . C35 C 0.17039(12) -0.05753(13) 0.34627(16) 0.0175(6) Uani 1 1 d . . . . . H35A H 0.140488 -0.024859 0.327059 0.021 Uiso 1 1 calc R U . . . H35B H 0.199435 -0.043504 0.335138 0.021 Uiso 1 1 calc R U . . . C36 C 0.14128(13) -0.11685(13) 0.29711(17) 0.0205(6) Uani 1 1 d . . . . . H36A H 0.110039 -0.129280 0.304524 0.025 Uiso 1 1 calc R U . . . H36B H 0.123244 -0.108849 0.237725 0.025 Uiso 1 1 calc R U . . . C37 C 0.18538(14) -0.16920(14) 0.32530(18) 0.0255(7) Uani 1 1 d . . . . . H37A H 0.214010 -0.158955 0.311762 0.031 Uiso 1 1 calc R U . . . H37B H 0.165027 -0.207556 0.295646 0.031 Uiso 1 1 calc R U . . . C38 C 0.21722(14) -0.17959(14) 0.41826(19) 0.0254(7) Uani 1 1 d . . . . . H38A H 0.247812 -0.211264 0.435997 0.031 Uiso 1 1 calc R U . . . H38B H 0.189297 -0.195201 0.430716 0.031 Uiso 1 1 calc R U . . . C39 C 0.24517(13) -0.11988(13) 0.46663(18) 0.0215(6) Uani 1 1 d . . . . . H39A H 0.275992 -0.106909 0.458582 0.026 Uiso 1 1 calc R U . . . H39B H 0.263915 -0.128159 0.526111 0.026 Uiso 1 1 calc R U . . . C40 C 0.17880(12) 0.09220(13) 0.32469(17) 0.0165(6) Uani 1 1 d . . . . . C41 C 0.16715(12) 0.06696(13) 0.25120(17) 0.0177(6) Uani 1 1 d . . . . . H41 H 0.196172 0.042599 0.252416 0.021 Uiso 1 1 calc R U . . . C42 C 0.11442(12) 0.07643(13) 0.17642(17) 0.0201(6) Uani 1 1 d . . . . . H42 H 0.107448 0.058588 0.127275 0.024 Uiso 1 1 calc R U . . . C43 C 0.07182(12) 0.11240(14) 0.17425(17) 0.0207(6) Uani 1 1 d . . . . . C44 C 0.01749(13) 0.12503(14) 0.09680(18) 0.0240(7) Uani 1 1 d . . . . . C45 C 0.08277(12) 0.13900(14) 0.24660(18) 0.0216(6) Uani 1 1 d . . . . . H45 H 0.053842 0.163643 0.245228 0.026 Uiso 1 1 calc R U . . . C46 C 0.13615(12) 0.12938(13) 0.32082(17) 0.0186(6) Uani 1 1 d . . . . . H46 H 0.143663 0.148429 0.369630 0.022 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1A 0.0640(12) 0.042(2) 0.098(3) 0.0064(13) -0.006(2) -0.0308(17) Cl2A 0.0767(15) 0.0737(19) 0.0375(7) 0.0145(11) 0.0315(9) 0.0439(14) C47A 0.014(3) 0.032(3) 0.032(2) 0.0010(18) 0.009(2) -0.008(2) Cl1B 0.0640(12) 0.042(2) 0.098(3) 0.0064(13) -0.006(2) -0.0308(17) Cl2B 0.0767(15) 0.0737(19) 0.0375(7) 0.0145(11) 0.0315(9) 0.0439(14) C47B 0.014(3) 0.032(3) 0.032(2) 0.0010(18) 0.009(2) -0.008(2) C48 0.084(8) 0.051(7) 0.069(9) -0.006(5) 0.032(7) -0.016(6) C49 0.087(6) 0.097(6) 0.076(6) 0.002(5) 0.040(5) -0.040(6) C50 0.068(17) 0.056(5) 0.072(12) -0.013(7) 0.043(10) 0.000(6) C51 0.087(6) 0.097(6) 0.076(6) 0.002(5) 0.040(5) -0.040(6) C52 0.084(8) 0.051(7) 0.069(9) -0.006(5) 0.032(7) -0.016(6) Pd1 0.01154(10) 0.01781(11) 0.01104(10) 0.00002(8) 0.00493(8) -0.00072(8) Br1 0.01727(14) 0.01994(15) 0.01676(14) 0.00075(11) 0.00832(11) -0.00214(11) P1 0.0118(3) 0.0189(4) 0.0103(3) -0.0001(3) 0.0046(3) -0.0011(3) O1 0.0179(10) 0.0269(11) 0.0149(10) 0.0049(8) 0.0071(8) -0.0022(9) O2 0.0124(9) 0.0313(12) 0.0094(9) -0.0007(8) 0.0029(8) -0.0055(8) O3 0.0163(10) 0.0327(12) 0.0143(10) 0.0006(8) 0.0088(8) -0.0053(9) N1 0.0216(14) 0.0420(18) 0.0263(15) 0.0023(13) 0.0043(12) 0.0040(13) C1 0.0139(13) 0.0200(15) 0.0134(13) -0.0015(11) 0.0063(11) 0.0015(11) C2 0.0163(14) 0.0220(15) 0.0168(14) -0.0009(11) 0.0090(12) 0.0003(12) C3 0.0301(18) 0.042(2) 0.0216(16) 0.0118(15) 0.0116(14) -0.0061(15) C4 0.0214(15) 0.0334(18) 0.0152(14) 0.0080(13) 0.0076(12) 0.0037(13) C5 0.0142(14) 0.0383(19) 0.0177(15) 0.0066(13) 0.0018(12) 0.0048(13) C6 0.0134(14) 0.0309(17) 0.0206(15) 0.0027(13) 0.0059(12) -0.0010(12) C7 0.0149(13) 0.0218(15) 0.0131(13) -0.0001(11) 0.0066(11) 0.0019(11) C8 0.0109(12) 0.0223(15) 0.0180(14) 0.0009(11) 0.0058(11) 0.0004(11) C9 0.0110(13) 0.0243(16) 0.0190(14) -0.0005(12) 0.0028(11) 0.0006(11) C10 0.0200(15) 0.0258(17) 0.0224(16) -0.0057(13) 0.0061(13) -0.0014(13) C11 0.0273(17) 0.0260(18) 0.0372(19) -0.0068(15) 0.0120(15) -0.0015(14) C12 0.0247(18) 0.049(2) 0.033(2) -0.0155(17) 0.0049(15) -0.0017(16) C13 0.0144(14) 0.0224(16) 0.0276(16) 0.0023(13) 0.0021(13) -0.0052(12) C14 0.0173(15) 0.039(2) 0.0215(16) 0.0081(14) 0.0079(13) -0.0041(13) C15 0.0250(17) 0.049(2) 0.039(2) 0.0063(17) 0.0168(16) -0.0057(16) C16 0.035(2) 0.056(3) 0.049(2) 0.013(2) 0.0221(19) -0.0084(19) C17 0.0204(16) 0.041(2) 0.039(2) -0.0001(16) 0.0158(15) -0.0086(15) C18 0.0162(14) 0.0374(18) 0.0223(15) 0.0029(14) 0.0110(12) -0.0014(13) C19 0.0117(13) 0.0268(16) 0.0177(14) 0.0029(12) 0.0061(12) 0.0040(12) C20 0.0239(16) 0.0288(17) 0.0248(16) 0.0001(13) 0.0150(14) 0.0057(13) C21 0.0352(19) 0.037(2) 0.0287(18) -0.0058(15) 0.0192(16) 0.0017(15) C22 0.039(2) 0.040(2) 0.043(2) 0.0010(17) 0.0203(18) 0.0153(17) C23 0.0129(13) 0.0204(15) 0.0134(13) -0.0016(11) 0.0064(11) -0.0005(11) C24 0.0164(14) 0.0222(15) 0.0155(14) -0.0016(11) 0.0089(12) -0.0006(11) C25 0.0248(15) 0.0219(15) 0.0247(15) -0.0028(12) 0.0154(13) -0.0021(12) C26 0.0320(17) 0.0294(17) 0.0231(16) -0.0045(13) 0.0189(14) 0.0005(14) C27 0.0290(16) 0.0278(17) 0.0182(14) 0.0012(12) 0.0167(13) 0.0019(13) C28 0.0163(13) 0.0258(16) 0.0128(13) -0.0015(11) 0.0082(11) -0.0012(12) C29 0.0131(13) 0.0230(15) 0.0123(13) 0.0007(11) 0.0071(11) 0.0004(11) C30 0.0142(13) 0.0282(16) 0.0085(12) -0.0010(11) 0.0052(11) -0.0039(11) C31 0.0215(16) 0.052(2) 0.0197(16) -0.0003(15) 0.0082(13) -0.0115(15) C32 0.0150(14) 0.046(2) 0.0232(16) 0.0014(14) 0.0100(13) -0.0032(14) C33 0.0189(14) 0.0197(14) 0.0137(13) -0.0003(11) 0.0085(11) -0.0033(12) C34 0.0160(13) 0.0202(15) 0.0112(13) 0.0000(11) 0.0060(11) -0.0033(11) C35 0.0186(14) 0.0195(14) 0.0144(13) -0.0003(11) 0.0093(12) -0.0029(11) C36 0.0223(15) 0.0238(16) 0.0150(14) -0.0032(12) 0.0102(12) -0.0049(12) C37 0.0292(16) 0.0221(16) 0.0232(15) -0.0066(13) 0.0133(14) -0.0032(13) C38 0.0257(16) 0.0209(16) 0.0254(16) 0.0010(13) 0.0116(14) 0.0016(13) C39 0.0200(14) 0.0202(15) 0.0205(15) -0.0002(12) 0.0089(12) -0.0009(12) C40 0.0145(13) 0.0181(15) 0.0135(13) 0.0010(10) 0.0057(11) -0.0009(11) C41 0.0175(13) 0.0175(14) 0.0190(14) 0.0014(11) 0.0108(12) -0.0002(11) C42 0.0186(14) 0.0218(15) 0.0152(13) -0.0003(12) 0.0066(12) -0.0018(12) C43 0.0160(14) 0.0212(15) 0.0185(14) 0.0034(12) 0.0058(12) -0.0011(12) C44 0.0196(15) 0.0259(17) 0.0219(16) 0.0001(13) 0.0088(13) 0.0003(12) C45 0.0164(14) 0.0222(16) 0.0240(15) 0.0030(12) 0.0099(12) 0.0020(12) C46 0.0183(14) 0.0208(15) 0.0169(14) -0.0014(11) 0.0099(12) -0.0017(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1A C47A 1.710(11) . ? Cl2A C47A 1.720(11) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? Cl1B C47B 1.726(6) . ? Cl2B C47B 1.757(5) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48 C49 1.466(15) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.52(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.51(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.462(15) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? Pd1 C40 2.021(3) . ? Pd1 P1 2.3478(10) . ? Pd1 C8 2.461(3) . ? Pd1 Br1 2.4690(9) . ? P1 C1 1.845(3) . ? P1 C23 1.905(3) . ? P1 C34 1.913(3) . ? O1 C2 1.359(3) . ? O1 C3 1.425(3) . ? O2 C31 1.423(4) . ? O2 C30 1.444(3) . ? O3 C32 1.432(3) . ? O3 C30 1.441(3) . ? N1 C44 1.146(4) . ? C1 C7 1.408(4) . ? C1 C2 1.419(4) . ? C2 C4 1.392(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.377(4) . ? C5 H5 0.9500 . ? C6 C7 1.401(4) . ? C6 H6 0.9500 . ? C7 C8 1.513(4) . ? C8 C19 1.426(4) . ? C8 C9 1.428(4) . ? C9 C13 1.398(4) . ? C9 C10 1.520(4) . ? C10 C11 1.531(4) . ? C10 C12 1.536(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.403(5) . ? C13 H13 0.9500 . ? C14 C18 1.367(5) . ? C14 C15 1.528(5) . ? C15 C16 1.490(5) . ? C15 C17 1.530(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.391(4) . ? C18 H18 0.9500 . ? C19 C20 1.523(4) . ? C20 C22 1.536(4) . ? C20 C21 1.540(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C29 1.545(4) . ? C23 C24 1.552(4) . ? C23 C28 1.553(4) . ? C24 C25 1.531(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.529(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.525(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.535(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.523(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.528(4) . ? C31 C32 1.505(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.548(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.548(4) . ? C34 C39 1.550(4) . ? C35 C36 1.537(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.526(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.530(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.533(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C46 1.396(4) . ? C40 C41 1.396(4) . ? C41 C42 1.388(4) . ? C41 H41 0.9500 . ? C42 C43 1.394(4) . ? C42 H42 0.9500 . ? C43 C45 1.395(4) . ? C43 C44 1.444(4) . ? C45 C46 1.392(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1A C47A Cl2A 110.0(11) . . ? Cl1A C47A H47A 109.7 . . ? Cl2A C47A H47A 109.7 . . ? Cl1A C47A H47B 109.7 . . ? Cl2A C47A H47B 109.7 . . ? H47A C47A H47B 108.2 . . ? Cl1B C47B Cl2B 114.8(4) . . ? Cl1B C47B H47C 108.6 . . ? Cl2B C47B H47C 108.6 . . ? Cl1B C47B H47D 108.6 . . ? Cl2B C47B H47D 108.6 . . ? H47C C47B H47D 107.5 . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C48 C49 C50 111.1(18) . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? C50 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C51 C50 C49 116(2) . . ? C51 C50 H50A 108.4 . . ? C49 C50 H50A 108.4 . . ? C51 C50 H50B 108.4 . . ? C49 C50 H50B 108.4 . . ? H50A C50 H50B 107.5 . . ? C52 C51 C50 120.4(16) . . ? C52 C51 H51A 107.2 . . ? C50 C51 H51A 107.2 . . ? C52 C51 H51B 107.2 . . ? C50 C51 H51B 107.2 . . ? H51A C51 H51B 106.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C40 Pd1 P1 97.86(9) . . ? C40 Pd1 C8 176.79(10) . . ? P1 Pd1 C8 83.64(8) . . ? C40 Pd1 Br1 80.09(8) . . ? P1 Pd1 Br1 169.35(2) . . ? C8 Pd1 Br1 98.96(7) . . ? C1 P1 C23 107.41(13) . . ? C1 P1 C34 110.38(13) . . ? C23 P1 C34 105.37(13) . . ? C1 P1 Pd1 104.13(10) . . ? C23 P1 Pd1 108.90(9) . . ? C34 P1 Pd1 120.12(9) . . ? C2 O1 C3 118.7(2) . . ? C31 O2 C30 107.9(2) . . ? C32 O3 C30 107.6(2) . . ? C7 C1 C2 117.3(2) . . ? C7 C1 P1 118.1(2) . . ? C2 C1 P1 124.5(2) . . ? O1 C2 C4 122.3(3) . . ? O1 C2 C1 116.1(2) . . ? C4 C2 C1 121.6(3) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 119.7(3) . . ? C5 C4 H4 120.2 . . ? C2 C4 H4 120.2 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 121.1(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C1 120.2(3) . . ? C6 C7 C8 113.3(2) . . ? C1 C7 C8 126.6(2) . . ? C19 C8 C9 118.4(3) . . ? C19 C8 C7 118.4(3) . . ? C9 C8 C7 117.4(3) . . ? C19 C8 Pd1 87.14(17) . . ? C9 C8 Pd1 99.60(18) . . ? C7 C8 Pd1 107.34(17) . . ? C13 C9 C8 118.7(3) . . ? C13 C9 C10 119.4(3) . . ? C8 C9 C10 121.9(3) . . ? C9 C10 C11 110.5(3) . . ? C9 C10 C12 112.0(3) . . ? C11 C10 C12 110.7(3) . . ? C9 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 122.4(3) . . ? C9 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C18 C14 C13 118.0(3) . . ? C18 C14 C15 119.7(3) . . ? C13 C14 C15 122.2(3) . . ? C16 C15 C14 112.1(3) . . ? C16 C15 C17 111.9(3) . . ? C14 C15 C17 110.5(3) . . ? C16 C15 H15 107.4 . . ? C14 C15 H15 107.4 . . ? C17 C15 H15 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 122.6(3) . . ? C14 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C18 C19 C8 119.8(3) . . ? C18 C19 C20 118.3(3) . . ? C8 C19 C20 121.6(3) . . ? C19 C20 C22 110.8(3) . . ? C19 C20 C21 111.7(3) . . ? C22 C20 C21 111.1(3) . . ? C19 C20 H20 107.7 . . ? C22 C20 H20 107.7 . . ? C21 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C29 C23 C24 112.7(2) . . ? C29 C23 C28 111.8(2) . . ? C24 C23 C28 105.6(2) . . ? C29 C23 P1 103.18(18) . . ? C24 C23 P1 104.74(18) . . ? C28 C23 P1 118.80(19) . . ? C25 C24 C23 114.1(2) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C26 C25 C24 110.5(2) . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 110.6(2) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 112.7(2) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C23 111.6(2) . . ? C27 C28 H28A 109.3 . . ? C23 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C23 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C23 115.9(2) . . ? C30 C29 H29A 108.3 . . ? C23 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? C23 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? O3 C30 O2 105.5(2) . . ? O3 C30 C29 112.1(2) . . ? O2 C30 C29 105.9(2) . . ? O3 C30 C33 106.4(2) . . ? O2 C30 C33 111.4(2) . . ? C29 C30 C33 115.3(2) . . ? O2 C31 C32 102.6(2) . . ? O2 C31 H31A 111.3 . . ? C32 C31 H31A 111.3 . . ? O2 C31 H31B 111.3 . . ? C32 C31 H31B 111.3 . . ? H31A C31 H31B 109.2 . . ? O3 C32 C31 102.0(2) . . ? O3 C32 H32A 111.4 . . ? C31 C32 H32A 111.4 . . ? O3 C32 H32B 111.4 . . ? C31 C32 H32B 111.4 . . ? H32A C32 H32B 109.2 . . ? C30 C33 C34 116.5(2) . . ? C30 C33 H33A 108.2 . . ? C34 C33 H33A 108.2 . . ? C30 C33 H33B 108.2 . . ? C34 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? C33 C34 C35 111.3(2) . . ? C33 C34 C39 110.9(2) . . ? C35 C34 C39 107.1(2) . . ? C33 C34 P1 108.45(19) . . ? C35 C34 P1 108.54(18) . . ? C39 C34 P1 110.64(19) . . ? C36 C35 C34 112.8(2) . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? C34 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 111.2(2) . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C38 110.6(2) . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 111.5(3) . . ? C37 C38 H38A 109.3 . . ? C39 C38 H38A 109.3 . . ? C37 C38 H38B 109.3 . . ? C39 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C34 113.2(2) . . ? C38 C39 H39A 108.9 . . ? C34 C39 H39A 108.9 . . ? C38 C39 H39B 108.9 . . ? C34 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C46 C40 C41 117.9(2) . . ? C46 C40 Pd1 124.7(2) . . ? C41 C40 Pd1 116.8(2) . . ? C42 C41 C40 121.9(3) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C41 C42 C43 119.2(3) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C45 119.9(3) . . ? C42 C43 C44 120.4(3) . . ? C45 C43 C44 119.7(3) . . ? N1 C44 C43 179.1(4) . . ? C46 C45 C43 119.9(3) . . ? C46 C45 H45 120.0 . . ? C43 C45 H45 120.0 . . ? C45 C46 C40 121.1(3) . . ? C45 C46 H46 119.5 . . ? C40 C46 H46 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C48 C49 C50 C51 -176.3(19) . . . . ? C49 C50 C51 C52 177(2) . . . . ? C23 P1 C1 C7 -114.8(2) . . . . ? C34 P1 C1 C7 130.8(2) . . . . ? Pd1 P1 C1 C7 0.6(2) . . . . ? C23 P1 C1 C2 63.0(3) . . . . ? C34 P1 C1 C2 -51.4(3) . . . . ? Pd1 P1 C1 C2 178.4(2) . . . . ? C3 O1 C2 C4 8.6(4) . . . . ? C3 O1 C2 C1 -171.9(3) . . . . ? C7 C1 C2 O1 -177.5(2) . . . . ? P1 C1 C2 O1 4.6(4) . . . . ? C7 C1 C2 C4 2.0(4) . . . . ? P1 C1 C2 C4 -175.9(2) . . . . ? O1 C2 C4 C5 178.0(3) . . . . ? C1 C2 C4 C5 -1.4(5) . . . . ? C2 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C7 0.8(5) . . . . ? C5 C6 C7 C1 -0.2(5) . . . . ? C5 C6 C7 C8 -179.1(3) . . . . ? C2 C1 C7 C6 -1.1(4) . . . . ? P1 C1 C7 C6 176.8(2) . . . . ? C2 C1 C7 C8 177.6(3) . . . . ? P1 C1 C7 C8 -4.4(4) . . . . ? C6 C7 C8 C19 88.0(3) . . . . ? C1 C7 C8 C19 -90.9(4) . . . . ? C6 C7 C8 C9 -64.7(3) . . . . ? C1 C7 C8 C9 116.4(3) . . . . ? C6 C7 C8 Pd1 -175.7(2) . . . . ? C1 C7 C8 Pd1 5.4(3) . . . . ? C19 C8 C9 C13 -1.9(4) . . . . ? C7 C8 C9 C13 150.9(3) . . . . ? Pd1 C8 C9 C13 -93.8(3) . . . . ? C19 C8 C9 C10 179.0(2) . . . . ? C7 C8 C9 C10 -28.3(4) . . . . ? Pd1 C8 C9 C10 87.0(3) . . . . ? C13 C9 C10 C11 61.3(3) . . . . ? C8 C9 C10 C11 -119.5(3) . . . . ? C13 C9 C10 C12 -62.6(4) . . . . ? C8 C9 C10 C12 116.6(3) . . . . ? C8 C9 C13 C14 -0.5(4) . . . . ? C10 C9 C13 C14 178.7(3) . . . . ? C9 C13 C14 C18 3.3(4) . . . . ? C9 C13 C14 C15 -175.0(3) . . . . ? C18 C14 C15 C16 109.9(4) . . . . ? C13 C14 C15 C16 -71.8(4) . . . . ? C18 C14 C15 C17 -124.6(3) . . . . ? C13 C14 C15 C17 53.6(4) . . . . ? C13 C14 C18 C19 -3.8(5) . . . . ? C15 C14 C18 C19 174.6(3) . . . . ? C14 C18 C19 C8 1.5(4) . . . . ? C14 C18 C19 C20 -172.1(3) . . . . ? C9 C8 C19 C18 1.4(4) . . . . ? C7 C8 C19 C18 -151.0(3) . . . . ? Pd1 C8 C19 C18 100.8(3) . . . . ? C9 C8 C19 C20 174.8(2) . . . . ? C7 C8 C19 C20 22.4(4) . . . . ? Pd1 C8 C19 C20 -85.8(2) . . . . ? C18 C19 C20 C22 67.3(4) . . . . ? C8 C19 C20 C22 -106.1(3) . . . . ? C18 C19 C20 C21 -57.1(4) . . . . ? C8 C19 C20 C21 129.4(3) . . . . ? C29 C23 C24 C25 63.9(3) . . . . ? C28 C23 C24 C25 -58.4(3) . . . . ? P1 C23 C24 C25 175.36(19) . . . . ? C23 C24 C25 C26 57.8(3) . . . . ? C24 C25 C26 C27 -52.8(3) . . . . ? C25 C26 C27 C28 54.3(3) . . . . ? C26 C27 C28 C23 -58.2(3) . . . . ? C29 C23 C28 C27 -65.9(3) . . . . ? C24 C23 C28 C27 57.0(3) . . . . ? P1 C23 C28 C27 174.1(2) . . . . ? C24 C23 C29 C30 -177.0(2) . . . . ? C28 C23 C29 C30 -58.2(3) . . . . ? P1 C23 C29 C30 70.6(2) . . . . ? C32 O3 C30 O2 -14.2(3) . . . . ? C32 O3 C30 C29 100.6(3) . . . . ? C32 O3 C30 C33 -132.6(2) . . . . ? C31 O2 C30 O3 -10.9(3) . . . . ? C31 O2 C30 C29 -129.9(3) . . . . ? C31 O2 C30 C33 104.1(3) . . . . ? C23 C29 C30 O3 87.1(3) . . . . ? C23 C29 C30 O2 -158.4(2) . . . . ? C23 C29 C30 C33 -34.8(3) . . . . ? C30 O2 C31 C32 30.2(3) . . . . ? C30 O3 C32 C31 32.0(3) . . . . ? O2 C31 C32 O3 -37.7(3) . . . . ? O3 C30 C33 C34 -163.8(2) . . . . ? O2 C30 C33 C34 81.8(3) . . . . ? C29 C30 C33 C34 -38.9(3) . . . . ? C30 C33 C34 C35 -60.6(3) . . . . ? C30 C33 C34 C39 -179.6(2) . . . . ? C30 C33 C34 P1 58.7(3) . . . . ? C33 C34 C35 C36 -65.2(3) . . . . ? C39 C34 C35 C36 56.1(3) . . . . ? P1 C34 C35 C36 175.55(19) . . . . ? C34 C35 C36 C37 -57.8(3) . . . . ? C35 C36 C37 C38 55.0(3) . . . . ? C36 C37 C38 C39 -54.3(3) . . . . ? C37 C38 C39 C34 56.4(3) . . . . ? C33 C34 C39 C38 66.0(3) . . . . ? C35 C34 C39 C38 -55.5(3) . . . . ? P1 C34 C39 C38 -173.6(2) . . . . ? C46 C40 C41 C42 -2.0(4) . . . . ? Pd1 C40 C41 C42 -173.3(2) . . . . ? C40 C41 C42 C43 0.3(4) . . . . ? C41 C42 C43 C45 0.8(4) . . . . ? C41 C42 C43 C44 177.5(3) . . . . ? C42 C43 C45 C46 -0.2(4) . . . . ? C44 C43 C45 C46 -177.0(3) . . . . ? C43 C45 C46 C40 -1.5(4) . . . . ? C41 C40 C46 C45 2.5(4) . . . . ? Pd1 C40 C46 C45 173.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C47A H47B Br1 0.99 2.62 3.555(17) 157.1 3 C47B H47D Br1 0.99 2.83 3.761(6) 156.2 3 C3 H3B Cl2B 0.98 2.89 3.761(4) 148.7 8_456 C28 H28A O3 0.99 2.60 3.171(4) 117.0 . C31 H31B O2 0.99 2.61 3.357(4) 132.6 2 C32 H32B N1 0.99 2.65 3.607(4) 163.4 6_556 C33 H33B O1 0.99 2.32 3.127(3) 137.9 . C35 H35A O2 0.99 2.50 3.102(4) 118.8 . C39 H39B O1 0.99 2.26 3.072(4) 138.0 . _refine_diff_density_max 1.078 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.092 _shelx_res_file ; TITL XRAY5707_0m_a.res in C2/c XRAY5707_0m_a.res created by SHELXL-2016/6 at 16:27:06 on 11-Mar-2019 CELL 0.71073 27.6601 21.6763 19.5445 90.000 123.911 90.000 ZERR 8.000 0.0128 0.0100 0.0090 0.000 0.005 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O P Br Pd Cl UNIT 396 552 8 24 8 8 8 16 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 SADI C49 C50 C50 C51 SADI C48 C49 C52 C51 EADP C48 C52 EADP C49 C51 EADP C47A C47B EADP Cl1A Cl1B EADP Cl2A Cl2B SADI Cl1A C47A Cl2A C47A Cl1B C47B Cl2B C47B SIZE 0.02 0.04 0.40 EQIV $1 x+1/2, y+1/2, z HTAB C47A Br1_$1 HTAB C47B Br1_$1 EQIV $2 x-1/2, -y+1/2, z+1/2 HTAB C3 Cl2B_$2 HTAB C28 O3 EQIV $3 -x, y, -z+1/2 HTAB C31 O2_$3 EQIV $4 x, -y, z+1/2 HTAB C32 N1_$4 HTAB C33 O1 HTAB C35 O2 HTAB C39 O1 WPDB CONF DFIX 1.729 C47A CL1A C47A CL2A C47B CL1B C47B CL2B DFIX 2.90 CL1A CL2A CL1B CL2B SIMU CL1A CL2A SIMU CL1B CL2B TEMP -173.0 WGHT 0.038200 16.543402 FVAR 0.10653 0.27366 PART 1 MOLE 1 CL1A 8 0.672155 0.814241 0.200951 21.00000 0.06401 0.04191 = 0.09797 0.00636 -0.00646 -0.03076 CL2A 8 0.653693 0.730628 0.078727 21.00000 0.07671 0.07370 = 0.03750 0.01447 0.03152 0.04392 C47A 1 0.661771 0.738369 0.172155 21.00000 0.01381 0.03199 = 0.03161 0.00097 0.00891 -0.00785 AFIX 23 H47A 2 0.626560 0.722617 0.167813 21.00000 -1.20000 H47B 2 0.695589 0.713758 0.214449 21.00000 -1.20000 PART 2 AFIX 0 CL1B 8 0.669846 0.804350 0.184963 -21.00000 0.06401 0.04191 = 0.09797 0.00636 -0.00646 -0.03076 CL2B 8 0.635235 0.700384 0.070496 -21.00000 0.07671 0.07370 = 0.03750 0.01447 0.03152 0.04392 C47B 1 0.644525 0.729464 0.161034 -21.00000 0.01381 0.03199 = 0.03161 0.00097 0.00891 -0.00785 AFIX 23 H47C 2 0.606680 0.727322 0.155327 -21.00000 -1.20000 H47D 2 0.672177 0.702459 0.207644 -21.00000 -1.20000 PART -1 AFIX 0 MOLE 2 C48 1 0.106309 0.316041 0.890212 10.50000 0.08351 0.05109 = 0.06927 -0.00576 0.03171 -0.01611 AFIX 137 H48A 2 0.125219 0.307676 0.861155 10.50000 -1.50000 H48B 2 0.130915 0.300641 0.946886 10.50000 -1.50000 H48C 2 0.100680 0.360602 0.891058 10.50000 -1.50000 AFIX 0 C49 1 0.049621 0.284923 0.847621 10.50000 0.08711 0.09715 = 0.07573 0.00218 0.03964 -0.03963 AFIX 23 H49A 2 0.031368 0.291782 0.878467 10.50000 -1.20000 H49B 2 0.055305 0.239974 0.846112 10.50000 -1.20000 AFIX 0 C50 1 0.009530 0.308894 0.760333 10.50000 0.06816 0.05587 = 0.07216 -0.01263 0.04285 0.00033 AFIX 23 H50A 2 0.006912 0.354310 0.762646 10.50000 -1.20000 H50B 2 0.027468 0.299800 0.729551 10.50000 -1.20000 AFIX 0 C51 1 -0.051614 0.282750 0.712444 10.50000 0.08711 0.09715 = 0.07573 0.00218 0.03964 -0.03963 AFIX 23 H51A 2 -0.048197 0.237585 0.708774 10.50000 -1.20000 H51B 2 -0.067730 0.289455 0.746111 10.50000 -1.20000 AFIX 0 C52 1 -0.095032 0.304876 0.629232 10.50000 0.08351 0.05109 = 0.06927 -0.00576 0.03171 -0.01611 AFIX 137 H52A 2 -0.098734 0.349775 0.630259 10.50000 -1.50000 H52B 2 -0.132701 0.285518 0.609278 10.50000 -1.50000 H52C 2 -0.082760 0.294164 0.592388 10.50000 -1.50000 PART 0 AFIX 0 MOLE 1 PD1 7 0.260705 0.081976 0.425559 11.00000 0.01154 0.01781 = 0.01104 0.00002 0.00493 -0.00072 BR1 6 0.274692 0.173005 0.362465 11.00000 0.01727 0.01994 = 0.01676 0.00075 0.00832 -0.00214 P1 5 0.240313 0.008628 0.494538 11.00000 0.01183 0.01886 = 0.01026 -0.00013 0.00463 -0.00111 O1 4 0.273563 -0.081065 0.636499 11.00000 0.01791 0.02686 = 0.01491 0.00493 0.00715 -0.00223 O2 4 0.062357 -0.036991 0.353559 11.00000 0.01238 0.03127 = 0.00944 -0.00072 0.00288 -0.00545 O3 4 0.085007 -0.046713 0.485375 11.00000 0.01630 0.03270 = 0.01430 0.00063 0.00876 -0.00532 N1 3 -0.025264 0.135567 0.035102 11.00000 0.02159 0.04199 = 0.02625 0.00227 0.00434 0.00399 C1 1 0.311999 -0.008271 0.589453 11.00000 0.01387 0.01999 = 0.01341 -0.00146 0.00628 0.00151 C2 1 0.321153 -0.049479 0.652031 11.00000 0.01634 0.02205 = 0.01684 -0.00090 0.00904 0.00030 C3 1 0.278093 -0.116959 0.700898 11.00000 0.03007 0.04192 = 0.02164 0.01177 0.01160 -0.00609 AFIX 137 H3A 2 0.303017 -0.152841 0.712000 11.00000 -1.50000 H3B 2 0.239248 -0.130929 0.684106 11.00000 -1.50000 H3C 2 0.295130 -0.091801 0.750891 11.00000 -1.50000 AFIX 0 C4 1 0.375928 -0.057219 0.724641 11.00000 0.02137 0.03335 = 0.01519 0.00798 0.00765 0.00367 AFIX 43 H4 2 0.380885 -0.084368 0.766266 11.00000 -1.20000 AFIX 0 C5 1 0.423125 -0.025153 0.735864 11.00000 0.01419 0.03830 = 0.01774 0.00661 0.00179 0.00477 AFIX 43 H5 2 0.460586 -0.030317 0.785292 11.00000 -1.20000 AFIX 0 C6 1 0.415868 0.014228 0.675493 11.00000 0.01340 0.03091 = 0.02058 0.00272 0.00590 -0.00102 AFIX 43 H6 2 0.448630 0.035639 0.683524 11.00000 -1.20000 AFIX 0 C7 1 0.360993 0.023242 0.602446 11.00000 0.01491 0.02178 = 0.01308 -0.00014 0.00660 0.00186 C8 1 0.362064 0.067367 0.543305 11.00000 0.01091 0.02229 = 0.01799 0.00092 0.00583 0.00043 C9 1 0.377404 0.130007 0.569094 11.00000 0.01100 0.02434 = 0.01901 -0.00048 0.00277 0.00060 C10 1 0.365748 0.159913 0.628873 11.00000 0.02000 0.02580 = 0.02241 -0.00566 0.00608 -0.00143 AFIX 13 H10 2 0.345596 0.128853 0.642476 11.00000 -1.20000 AFIX 0 C11 1 0.325040 0.215358 0.588615 11.00000 0.02731 0.02601 = 0.03721 -0.00684 0.01200 -0.00146 AFIX 137 H11A 2 0.345619 0.248667 0.581089 11.00000 -1.50000 H11B 2 0.312660 0.229743 0.624098 11.00000 -1.50000 H11C 2 0.290776 0.203162 0.534882 11.00000 -1.50000 AFIX 0 C12 1 0.422346 0.178956 0.709820 11.00000 0.02467 0.04900 = 0.03281 -0.01546 0.00491 -0.00173 AFIX 137 H12A 2 0.446870 0.142490 0.736170 11.00000 -1.50000 H12B 2 0.412995 0.197502 0.746828 11.00000 -1.50000 H12C 2 0.443273 0.209024 0.698094 11.00000 -1.50000 AFIX 0 C13 1 0.404556 0.164252 0.539001 11.00000 0.01439 0.02240 = 0.02757 0.00228 0.00208 -0.00521 AFIX 43 H13 2 0.414516 0.206026 0.555765 11.00000 -1.20000 AFIX 0 C14 1 0.417645 0.139206 0.484949 11.00000 0.01726 0.03889 = 0.02154 0.00815 0.00793 -0.00406 C15 1 0.451602 0.175172 0.457649 11.00000 0.02502 0.04872 = 0.03859 0.00627 0.01676 -0.00574 AFIX 13 H15 2 0.461353 0.145752 0.427639 11.00000 -1.20000 AFIX 0 C16 1 0.416321 0.225946 0.399410 11.00000 0.03540 0.05590 = 0.04888 0.01300 0.02213 -0.00839 AFIX 137 H16A 2 0.379970 0.209048 0.352266 11.00000 -1.50000 H16B 2 0.438447 0.245634 0.379972 11.00000 -1.50000 H16C 2 0.407341 0.256554 0.427684 11.00000 -1.50000 AFIX 0 C17 1 0.509140 0.198809 0.532688 11.00000 0.02043 0.04136 = 0.03934 -0.00010 0.01582 -0.00855 AFIX 137 H17A 2 0.531717 0.219023 0.514340 11.00000 -1.50000 H17B 2 0.531456 0.164062 0.568805 11.00000 -1.50000 H17C 2 0.501095 0.228478 0.562971 11.00000 -1.50000 AFIX 0 C18 1 0.400379 0.080042 0.458116 11.00000 0.01623 0.03738 = 0.02232 0.00286 0.01099 -0.00141 AFIX 43 H18 2 0.406922 0.063502 0.418931 11.00000 -1.20000 AFIX 0 C19 1 0.373595 0.043098 0.485951 11.00000 0.01171 0.02678 = 0.01769 0.00290 0.00610 0.00401 C20 1 0.363283 -0.024603 0.460882 11.00000 0.02387 0.02875 = 0.02480 0.00014 0.01498 0.00566 AFIX 13 H20 2 0.340772 -0.043157 0.481778 11.00000 -1.20000 AFIX 0 C21 1 0.326751 -0.032306 0.366484 11.00000 0.03519 0.03743 = 0.02867 -0.00584 0.01918 0.00173 AFIX 137 H21A 2 0.291002 -0.007837 0.342110 11.00000 -1.50000 H21B 2 0.316668 -0.075898 0.352481 11.00000 -1.50000 H21C 2 0.349339 -0.018082 0.344804 11.00000 -1.50000 AFIX 0 C22 1 0.421331 -0.059532 0.501124 11.00000 0.03914 0.03983 = 0.04330 0.00103 0.02035 0.01530 AFIX 137 H22A 2 0.444679 -0.041774 0.482488 11.00000 -1.50000 H22B 2 0.413666 -0.103132 0.485330 11.00000 -1.50000 H22C 2 0.442671 -0.055969 0.561222 11.00000 -1.50000 AFIX 0 C23 1 0.193642 0.046208 0.526689 11.00000 0.01290 0.02039 = 0.01341 -0.00164 0.00637 -0.00055 C24 1 0.210542 0.115529 0.537912 11.00000 0.01640 0.02216 = 0.01548 -0.00157 0.00885 -0.00058 AFIX 23 H24A 2 0.252195 0.119598 0.583132 11.00000 -1.20000 H24B 2 0.205864 0.130779 0.486790 11.00000 -1.20000 AFIX 0 C25 1 0.174534 0.156363 0.557388 11.00000 0.02480 0.02192 = 0.02475 -0.00282 0.01536 -0.00208 AFIX 23 H25A 2 0.188324 0.199538 0.565029 11.00000 -1.20000 H25B 2 0.133127 0.155317 0.510580 11.00000 -1.20000 AFIX 0 C26 1 0.180004 0.133940 0.635609 11.00000 0.03201 0.02944 = 0.02312 -0.00451 0.01894 0.00055 AFIX 23 H26A 2 0.220224 0.141073 0.683850 11.00000 -1.20000 H26B 2 0.153107 0.157708 0.643918 11.00000 -1.20000 AFIX 0 C27 1 0.165555 0.065411 0.629137 11.00000 0.02898 0.02784 = 0.01823 0.00118 0.01673 0.00192 AFIX 23 H27A 2 0.123735 0.059387 0.585700 11.00000 -1.20000 H27B 2 0.172402 0.051271 0.682031 11.00000 -1.20000 AFIX 0 C28 1 0.202004 0.025833 0.608832 11.00000 0.01630 0.02584 = 0.01282 -0.00154 0.00815 -0.00124 AFIX 23 H28A 2 0.190488 -0.017964 0.604583 11.00000 -1.20000 H28B 2 0.243685 0.029344 0.654157 11.00000 -1.20000 AFIX 0 C29 1 0.130829 0.034335 0.451898 11.00000 0.01313 0.02303 = 0.01234 0.00074 0.00710 0.00036 AFIX 23 H29A 2 0.103998 0.060255 0.458033 11.00000 -1.20000 H29B 2 0.127973 0.048198 0.401496 11.00000 -1.20000 AFIX 0 C30 1 0.109865 -0.032225 0.439239 11.00000 0.01425 0.02823 = 0.00849 -0.00105 0.00523 -0.00387 C31 1 0.014418 -0.064979 0.349920 11.00000 0.02153 0.05209 = 0.01973 -0.00031 0.00825 -0.01145 AFIX 23 H31A 2 0.015914 -0.110493 0.347280 11.00000 -1.20000 H31B 2 -0.023162 -0.050057 0.301708 11.00000 -1.20000 AFIX 0 C32 1 0.022925 -0.044385 0.429491 11.00000 0.01505 0.04585 = 0.02323 0.00143 0.00998 -0.00320 AFIX 23 H32A 2 0.007964 -0.002044 0.424881 11.00000 -1.20000 H32B 2 0.003569 -0.072788 0.446716 11.00000 -1.20000 AFIX 0 C33 1 0.156419 -0.081073 0.462308 11.00000 0.01893 0.01971 = 0.01366 -0.00034 0.00847 -0.00334 AFIX 23 H33A 2 0.136546 -0.120167 0.434743 11.00000 -1.20000 H33B 2 0.178163 -0.088193 0.522503 11.00000 -1.20000 AFIX 0 C34 1 0.200979 -0.066339 0.440339 11.00000 0.01602 0.02020 = 0.01116 0.00003 0.00597 -0.00329 C35 1 0.170391 -0.057530 0.346267 11.00000 0.01860 0.01955 = 0.01444 -0.00033 0.00932 -0.00291 AFIX 23 H35A 2 0.140488 -0.024859 0.327059 11.00000 -1.20000 H35B 2 0.199435 -0.043504 0.335138 11.00000 -1.20000 AFIX 0 C36 1 0.141282 -0.116849 0.297114 11.00000 0.02229 0.02377 = 0.01504 -0.00321 0.01023 -0.00493 AFIX 23 H36A 2 0.110039 -0.129280 0.304524 11.00000 -1.20000 H36B 2 0.123244 -0.108849 0.237725 11.00000 -1.20000 AFIX 0 C37 1 0.185385 -0.169201 0.325303 11.00000 0.02920 0.02213 = 0.02318 -0.00657 0.01332 -0.00324 AFIX 23 H37A 2 0.214010 -0.158955 0.311762 11.00000 -1.20000 H37B 2 0.165027 -0.207556 0.295646 11.00000 -1.20000 AFIX 0 C38 1 0.217222 -0.179594 0.418262 11.00000 0.02574 0.02087 = 0.02540 0.00103 0.01159 0.00159 AFIX 23 H38A 2 0.247812 -0.211264 0.435997 11.00000 -1.20000 H38B 2 0.189297 -0.195201 0.430716 11.00000 -1.20000 AFIX 0 C39 1 0.245171 -0.119876 0.466626 11.00000 0.01995 0.02024 = 0.02046 -0.00016 0.00894 -0.00094 AFIX 23 H39A 2 0.275992 -0.106909 0.458582 11.00000 -1.20000 H39B 2 0.263915 -0.128159 0.526111 11.00000 -1.20000 AFIX 0 C40 1 0.178802 0.092200 0.324690 11.00000 0.01453 0.01812 = 0.01351 0.00096 0.00574 -0.00092 C41 1 0.167154 0.066964 0.251202 11.00000 0.01754 0.01745 = 0.01900 0.00137 0.01078 -0.00015 AFIX 43 H41 2 0.196172 0.042599 0.252416 11.00000 -1.20000 AFIX 0 C42 1 0.114419 0.076427 0.176416 11.00000 0.01859 0.02175 = 0.01523 -0.00028 0.00655 -0.00176 AFIX 43 H42 2 0.107448 0.058588 0.127275 11.00000 -1.20000 AFIX 0 C43 1 0.071817 0.112401 0.174250 11.00000 0.01600 0.02124 = 0.01854 0.00335 0.00581 -0.00114 C44 1 0.017487 0.125026 0.096796 11.00000 0.01960 0.02593 = 0.02192 0.00011 0.00884 0.00032 C45 1 0.082772 0.138996 0.246601 11.00000 0.01636 0.02225 = 0.02397 0.00299 0.00994 0.00203 AFIX 43 H45 2 0.053842 0.163643 0.245228 11.00000 -1.20000 AFIX 0 C46 1 0.136150 0.129377 0.320822 11.00000 0.01829 0.02083 = 0.01691 -0.00142 0.00992 -0.00171 AFIX 43 H46 2 0.143663 0.148429 0.369630 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5707_0m_a.res in C2/c REM R1 = 0.0384 for 8522 Fo > 4sig(Fo) and 0.0612 for all 11093 data REM 557 parameters refined using 14 restraints END WGHT 0.0355 17.9314 REM Highest difference peak 1.078, deepest hole -0.951, 1-sigma level 0.092 Q1 1 0.4387 0.2107 0.4715 11.00000 0.05 1.08 Q2 1 0.4360 0.1868 0.3862 11.00000 0.05 1.03 Q3 1 0.2748 0.0777 0.4708 11.00000 0.05 0.66 Q4 1 0.2447 0.0799 0.3814 11.00000 0.05 0.60 Q5 1 0.6987 0.7783 0.1800 11.00000 0.05 0.60 Q6 1 0.0000 0.2575 0.7500 10.50000 0.05 0.59 Q7 1 0.2944 0.0839 0.4281 11.00000 0.05 0.56 Q8 1 0.2512 0.1168 0.4266 11.00000 0.05 0.55 Q9 1 0.4042 0.1698 0.4928 11.00000 0.05 0.53 Q10 1 0.2739 0.0401 0.4313 11.00000 0.05 0.53 Q11 1 0.6554 0.7638 0.0876 11.00000 0.05 0.52 Q12 1 0.3101 0.1748 0.3705 11.00000 0.05 0.51 Q13 1 0.2711 0.1269 0.3922 11.00000 0.05 0.51 Q14 1 0.6905 0.7377 0.1822 11.00000 0.05 0.49 Q15 1 0.6317 0.8025 0.1814 11.00000 0.05 0.48 Q16 1 0.6672 0.7107 0.0775 11.00000 0.05 0.46 Q17 1 0.2899 0.1716 0.4122 11.00000 0.05 0.46 Q18 1 0.2194 0.0826 0.4118 11.00000 0.05 0.45 Q19 1 0.2299 0.1186 0.3692 11.00000 0.05 0.45 Q20 1 0.2619 0.2101 0.3658 11.00000 0.05 0.44 ; _shelx_res_checksum 13342 _shelx_hkl_file ; 2 0 0 9999.00 743.33 -2 0 0 8815.32 742.93 -2 0 0 9860.51 743.13 -4 0 0 14.70 2.90 4 0 0 17.80 3.30 -4 0 0 12.10 2.90 4 0 0 16.30 3.00 -6 0 0 828.32 56.69 6 0 0 631.34 56.69 -6 0 0 699.33 56.79 -8 0 0 806.72 58.49 -8 0 0 689.43 58.29 8 0 0 735.93 58.59 -10 0 0 546.35 46.30 10 0 0 566.74 46.50 10 0 0 640.74 46.40 -12 0 0 998.10 79.19 12 0 0 1118.79 79.29 12 0 0 912.31 79.29 14 0 0 -3.30 4.50 -14 0 0 -3.30 4.50 14 0 0 4.40 5.40 -14 0 0 6.80 4.80 -16 0 0 52.59 7.70 16 0 0 52.39 8.30 -16 0 0 57.39 7.70 16 0 0 55.99 7.70 -18 0 0 22.80 6.60 -18 0 0 27.60 6.40 18 0 0 35.50 6.60 -20 0 0 541.45 44.60 20 0 0 537.65 44.40 22 0 0 278.67 24.80 -22 0 0 252.67 24.90 -24 0 0 31.70 8.80 24 0 0 0.80 8.20 -26 0 0 -10.80 8.20 26 0 0 -17.80 8.40 -28 0 0 55.69 11.80 28 0 0 67.99 12.40 3 -1 0 37.10 3.80 -3 -1 0 29.40 3.50 3 -1 0 23.10 3.90 3 1 0 28.70 3.70 -3 1 0 45.90 4.20 3 1 0 26.30 3.30 -3 1 0 28.40 3.40 5 -1 0 482.25 35.00 5 -1 0 407.66 34.50 -5 -1 0 439.66 34.60 -5 -1 0 429.06 34.60 5 1 0 411.96 34.50 -5 1 0 476.15 34.60 -5 1 0 462.35 34.60 5 1 0 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314.87 26.00 -11 13 0 332.07 25.90 -11 13 0 302.07 25.40 11 13 0 293.27 24.60 -13 -13 0 84.09 9.90 13 -13 0 50.99 12.60 -13 -13 0 53.69 9.20 13 13 0 54.39 7.90 -13 13 0 66.19 10.10 -13 13 0 62.09 8.80 15 -13 0 -7.30 10.40 -15 -13 0 -0.60 6.70 -15 -13 0 0.10 6.60 -15 13 0 -1.70 6.40 15 13 0 -0.60 5.40 -15 13 0 -5.70 6.70 -17 -13 0 7.10 7.20 -17 -13 0 5.60 7.70 17 -13 0 22.90 12.40 -17 13 0 6.70 7.60 -17 13 0 -0.30 6.60 17 13 0 0.30 6.00 -19 -13 0 253.37 23.80 19 -13 0 232.68 27.90 -19 -13 0 240.28 23.80 -19 13 0 252.47 23.70 19 13 0 221.08 22.50 -21 -13 0 218.18 23.20 21 -13 0 177.58 23.80 -21 13 0 216.28 22.40 21 13 0 232.58 21.90 -23 -13 0 79.99 13.00 23 -13 0 98.49 18.30 23 13 0 55.29 12.10 -23 13 0 121.89 13.10 -25 -13 0 27.00 10.60 -25 13 0 32.10 10.20 25 13 0 20.40 10.20 0 -14 0 1.90 7.30 0 -14 0 10.10 6.60 0 14 0 10.40 4.80 2 -14 0 16.70 6.20 -2 -14 0 19.20 7.70 2 -14 0 8.50 7.80 -2 -14 0 10.20 6.50 2 14 0 19.50 5.00 -2 14 0 13.70 5.00 4 -14 0 6.80 8.40 -4 -14 0 12.20 7.20 -4 -14 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321.67 26.20 -1 19 -4 261.77 27.00 3 -19 4 178.68 21.00 -3 -19 -4 160.38 17.70 -3 19 -4 137.59 17.00 3 19 4 164.18 18.10 -5 -19 -4 129.19 15.10 5 -19 4 120.49 18.50 5 19 4 131.19 14.00 -5 19 -4 85.59 14.20 7 -19 4 158.28 20.60 -7 -19 -4 124.39 16.50 -7 19 -4 192.48 20.70 7 19 4 125.29 15.30 9 -19 4 140.19 20.50 -9 -19 -4 121.09 15.80 9 19 4 126.59 14.40 -9 19 -4 83.39 16.10 -11 -19 -4 163.48 19.90 11 -19 4 199.68 25.20 -11 19 -4 195.18 20.90 11 19 4 198.08 21.90 13 -19 4 263.37 33.20 -13 -19 -4 228.78 25.50 13 19 4 218.98 24.10 -13 19 -4 219.18 27.00 15 -19 4 107.69 21.00 -15 -19 -4 84.99 14.60 15 19 4 98.29 13.80 -15 19 -4 81.29 15.20 -17 -19 -4 56.09 13.00 17 -19 4 47.40 18.10 -17 19 -4 5.90 12.40 17 19 4 51.89 11.50 22 -20 -4 28.00 17.90 -22 20 4 8.20 9.90 22 20 -4 7.60 8.80 20 -20 -4 21.50 16.60 20 20 -4 10.40 8.90 -20 20 4 6.70 9.50 -18 -20 4 5.00 9.50 18 -20 -4 18.70 15.10 18 20 -4 -12.90 7.40 -18 20 4 -3.50 9.20 -16 -20 4 1.20 9.90 16 -20 -4 5.50 14.70 -16 20 4 -1.80 13.10 -16 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142.59 20.30 27 11 -9 86.69 13.00 -27 11 9 125.89 14.40 -25 -11 9 81.89 12.60 -25 -11 9 65.99 11.20 25 -11 -9 97.99 17.60 -25 11 9 110.59 13.10 -23 -11 9 86.29 10.70 -23 -11 9 91.69 11.70 23 -11 -9 84.99 16.30 23 11 -9 83.09 13.60 -23 11 9 73.49 11.80 -21 -11 9 52.39 9.10 -21 -11 9 44.40 7.60 21 -11 -9 39.90 13.60 -21 11 9 35.40 8.80 21 11 -9 33.20 10.80 19 -11 -9 18.80 12.40 -19 -11 9 29.20 7.50 -19 -11 9 36.40 6.50 -19 11 9 30.40 8.00 19 11 -9 21.80 9.80 -17 -11 9 0.90 5.00 17 -11 -9 -1.10 10.50 -17 -11 9 -2.30 5.90 -17 11 9 -0.20 6.90 17 11 -9 -6.20 8.50 17 11 -9 -8.10 5.40 -15 -11 9 118.49 14.90 -15 -11 9 104.69 11.30 -15 -11 9 99.19 11.40 15 -11 -9 115.29 15.00 15 -11 -9 108.39 12.10 15 11 -9 111.19 12.70 -15 11 9 103.19 11.60 -13 -11 9 17.20 4.60 -13 -11 9 21.50 9.80 -13 -11 9 15.10 6.10 13 -11 -9 12.80 5.90 13 -11 -9 22.60 10.00 -13 11 9 24.00 7.00 13 11 -9 20.70 6.20 11 -11 -9 106.69 12.00 -11 -11 9 108.99 14.10 11 -11 -9 93.09 13.60 -11 -11 9 108.79 10.80 11 11 -9 112.59 12.40 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6.80 8.90 8 -12 -9 14.50 6.90 -8 -12 9 15.60 5.50 8 -12 -9 9.00 8.50 -8 12 9 21.60 6.40 8 12 -9 15.50 7.10 -6 -12 9 5.90 8.80 6 -12 -9 2.50 7.60 6 -12 -9 0.20 6.30 -6 -12 9 4.40 5.20 6 12 -9 3.60 7.50 -6 12 9 -1.20 5.80 4 -12 -9 99.19 12.00 -4 -12 9 125.19 14.40 -4 -12 9 94.89 10.70 4 -12 -9 109.59 14.00 4 12 -9 99.09 12.20 -4 12 9 102.19 10.90 -2 -12 9 105.39 11.80 2 -12 -9 129.99 15.10 -2 -12 9 131.19 15.60 2 -12 -9 128.69 14.10 -2 12 9 123.39 13.80 2 12 -9 115.79 13.60 -2 12 9 116.19 11.60 0 -12 9 137.49 13.60 0 -12 9 134.49 16.00 0 -12 -9 127.39 14.40 0 12 9 138.09 12.50 0 12 9 129.29 13.40 0 12 -9 107.59 14.60 2 -12 9 40.60 11.20 2 -12 9 54.09 7.70 -2 -12 -9 44.00 9.60 2 12 9 42.30 8.10 2 12 9 48.20 6.70 -2 12 -9 52.49 10.70 4 -12 9 7.20 9.50 4 -12 9 21.30 6.50 -4 -12 -9 8.00 8.00 4 12 9 16.70 5.50 4 12 9 9.50 6.50 -4 12 -9 6.60 9.00 6 -12 9 55.59 12.30 -6 -12 -9 45.10 10.40 6 -12 9 61.29 8.70 6 12 9 35.00 8.50 6 12 9 55.49 7.80 -6 12 -9 32.00 11.40 8 -12 9 89.59 14.30 8 -12 9 78.39 10.60 -8 -12 -9 59.09 11.80 -8 12 -9 74.59 13.00 8 12 9 91.29 11.10 8 12 9 93.49 10.60 10 -12 9 -1.50 10.60 -10 -12 -9 1.20 9.20 10 -12 9 -1.30 7.40 10 12 9 10.50 7.20 10 12 9 -7.50 7.00 -10 12 -9 -19.40 10.90 12 -12 9 8.50 8.10 -12 -12 -9 0.00 10.00 12 12 9 2.60 7.90 12 12 9 4.80 7.60 -12 12 -9 -16.50 10.60 14 -12 9 0.00 8.70 -14 -12 -9 8.40 9.00 -14 -12 -9 3.30 10.60 14 12 9 -6.20 8.20 14 12 9 -10.00 8.10 -14 12 -9 -8.30 10.70 -16 -12 -9 21.20 10.20 -16 -12 -9 -1.60 10.70 16 -12 9 7.10 9.40 16 12 9 -9.00 8.80 -16 12 -9 -2.10 11.60 -31 -13 9 130.59 16.50 31 13 -9 119.69 16.40 -31 13 9 162.58 18.50 29 -13 -9 186.68 23.80 -29 -13 9 108.49 15.60 29 13 -9 130.89 15.70 -29 13 9 141.59 16.90 -27 -13 9 160.58 18.30 27 -13 -9 213.88 25.50 27 13 -9 168.18 18.60 -27 13 9 218.78 22.10 25 -13 -9 41.50 16.30 -25 -13 9 29.60 8.90 -25 -13 9 45.50 10.70 -25 13 9 33.70 10.20 -23 -13 9 57.59 9.30 -23 -13 9 56.09 10.30 23 -13 -9 81.49 16.30 23 13 -9 48.10 12.10 -23 13 9 54.39 10.50 -21 -13 9 97.29 10.90 21 -13 -9 82.19 16.70 -21 -13 9 112.19 12.10 21 13 -9 77.89 13.80 -21 13 9 84.79 12.10 19 -13 -9 82.59 15.20 -19 -13 9 54.49 8.80 -19 -13 9 86.99 10.30 19 13 -9 75.89 12.60 -19 13 9 57.29 10.40 17 -13 -9 49.30 13.20 -17 -13 9 52.79 7.70 -17 -13 9 47.60 11.90 -17 -13 9 51.19 8.50 -17 13 9 45.80 9.50 17 13 -9 70.89 8.70 17 13 -9 53.39 11.10 15 -13 -9 96.29 14.80 -15 -13 9 81.39 9.80 15 -13 -9 80.99 10.10 -15 -13 9 89.59 13.60 -15 13 9 85.99 10.90 15 13 -9 56.69 9.70 13 -13 -9 288.57 32.60 -13 -13 9 375.76 29.80 -13 -13 9 329.57 32.70 13 -13 -9 362.56 30.10 13 13 -9 391.76 30.50 -13 13 9 344.67 30.90 -11 -13 9 243.78 21.80 -11 -13 9 266.87 25.80 11 -13 -9 220.08 24.90 11 -13 -9 243.58 22.80 11 13 -9 278.67 23.00 -11 13 9 237.98 22.90 9 -13 -9 20.40 9.50 9 -13 -9 29.30 7.70 -9 -13 9 45.60 6.80 -9 -13 9 22.60 9.50 -9 13 9 23.00 6.60 9 13 -9 28.60 7.80 -7 -13 9 35.90 6.80 7 -13 -9 45.20 8.50 7 -13 -9 39.30 9.40 -7 -13 9 48.00 10.90 7 13 -9 45.50 8.80 -7 13 9 39.40 7.40 -5 -13 9 34.50 6.50 5 -13 -9 20.30 7.80 5 -13 -9 28.30 8.60 -5 -13 9 44.20 10.20 -5 13 9 31.50 7.10 5 13 -9 46.10 9.30 -3 -13 9 -5.10 5.50 3 -13 -9 11.40 7.40 3 -13 -9 -8.10 7.10 -3 -13 9 5.70 9.40 -3 13 9 -1.70 6.10 3 13 -9 -5.00 8.40 1 -13 -9 -4.30 7.20 -1 -13 9 -6.10 9.20 -1 -13 9 4.40 5.80 -1 13 9 4.90 6.30 1 13 -9 -3.10 8.60 -1 -13 -9 9.00 8.10 1 -13 9 -7.00 5.80 1 -13 9 -2.60 9.70 -1 13 -9 -2.20 7.80 1 13 9 2.40 6.20 3 -13 9 31.20 7.40 3 -13 9 36.50 11.20 -3 -13 -9 45.10 9.20 3 13 9 38.20 7.90 3 13 9 39.60 6.50 -3 13 -9 29.50 10.20 -5 -13 -9 17.30 8.90 5 -13 9 26.70 11.00 5 -13 9 18.60 6.60 -5 13 -9 9.90 10.20 5 13 9 2.30 5.70 5 13 9 11.10 7.10 7 -13 9 181.58 18.60 -7 -13 -9 155.28 18.80 7 -13 9 185.18 22.70 7 13 9 203.98 19.30 -7 13 -9 156.18 19.30 7 13 9 207.08 18.10 9 -13 9 125.19 17.10 9 -13 9 95.79 12.40 -9 -13 -9 96.99 14.70 9 13 9 120.79 12.60 9 13 9 111.89 13.40 -9 13 -9 110.29 15.80 11 -13 9 20.40 8.40 -11 -13 -9 26.70 10.70 -11 13 -9 31.40 13.20 11 13 9 22.30 8.80 11 13 9 25.70 8.50 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24.70 10.40 2 6 14 29.30 7.80 4 -6 14 211.18 22.20 -4 -6 -14 233.78 24.40 4 6 14 215.78 21.90 4 6 14 222.88 21.20 -4 6 -14 237.88 25.00 -6 -6 -14 242.48 24.70 6 -6 14 223.18 21.90 -6 6 -14 202.28 22.90 6 6 14 205.68 21.50 6 6 14 186.58 20.70 -8 -6 -14 160.08 18.60 8 -6 14 107.19 15.90 8 6 14 135.29 16.10 8 6 14 132.99 15.20 -8 6 -14 198.78 19.60 10 -6 14 143.69 17.40 -10 -6 -14 169.98 19.90 10 6 14 140.79 17.30 -10 6 -14 171.68 20.00 12 -6 14 246.78 25.80 -12 -6 -14 245.68 28.20 -12 6 -14 279.87 29.70 12 6 14 222.08 25.80 33 -7 -14 132.59 24.50 -33 -7 14 210.38 21.30 -33 -7 14 155.28 19.50 -33 7 14 182.68 19.20 -31 -7 14 152.38 15.70 -31 -7 14 154.68 16.90 31 -7 -14 96.69 21.90 -31 7 14 145.39 16.50 31 7 -14 134.99 19.80 -29 -7 14 121.79 15.50 -29 -7 14 168.78 17.40 29 -7 -14 119.89 21.50 -29 7 14 116.29 14.70 -29 7 14 162.48 16.00 29 7 -14 118.99 18.70 27 -7 -14 92.99 18.40 -27 -7 14 88.59 11.50 -27 -7 14 81.79 12.00 -27 7 14 84.59 12.10 -27 7 14 83.59 11.10 27 7 -14 82.29 15.50 -25 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18.10 -9 -7 14 70.49 10.10 9 -7 -14 86.49 12.10 -9 -7 14 81.69 12.90 9 -7 -14 87.79 10.70 -9 7 14 74.09 9.30 -9 7 14 83.49 9.20 9 7 -14 88.39 12.00 7 -7 -14 179.88 18.60 7 -7 -14 171.98 18.20 -7 -7 14 166.68 20.30 -7 -7 14 176.68 17.30 7 7 -14 158.38 19.00 -7 7 14 168.68 16.70 -7 7 14 163.18 16.30 -5 -7 14 49.99 9.50 5 -7 -14 84.89 11.30 -5 -7 14 67.89 11.90 5 7 -14 59.49 11.20 -5 7 14 71.39 8.70 -5 7 14 79.59 9.10 -3 -7 14 31.00 7.80 3 -7 -14 23.50 9.00 -3 -7 14 35.30 9.90 -3 7 14 25.10 6.50 -3 7 14 44.30 7.30 3 7 -14 24.10 10.00 -1 -7 14 13.60 7.30 1 -7 -14 -1.60 8.70 -1 -7 14 14.30 8.80 1 7 -14 -13.10 9.50 -1 7 14 14.20 6.20 -1 7 14 -0.10 5.80 1 -7 14 27.30 8.10 -1 -7 -14 24.00 9.60 1 -7 14 16.90 9.70 1 7 14 16.20 7.20 -1 7 -14 24.80 10.30 1 7 14 18.00 6.70 -3 -7 -14 11.50 10.20 3 -7 14 21.30 8.70 -3 7 -14 19.50 10.80 3 7 14 8.50 6.80 3 7 14 18.90 7.70 -5 -7 -14 7.10 10.10 5 -7 14 8.60 8.40 5 7 14 13.50 8.00 -5 7 -14 -12.20 10.60 5 7 14 12.50 7.20 7 -7 14 42.30 10.20 -7 -7 -14 49.50 12.70 7 7 14 33.80 8.60 -7 7 -14 27.00 12.00 7 7 14 24.40 9.30 9 -7 14 -3.10 8.80 -9 -7 -14 10.10 11.30 9 7 14 -6.90 7.50 -9 7 -14 -5.40 11.70 9 7 14 0.90 8.60 -11 -7 -14 25.40 12.60 11 -7 14 24.90 10.40 -11 7 -14 33.30 12.70 11 7 14 29.60 10.60 -34 -8 14 16.80 14.10 -34 -8 14 36.10 10.90 34 -8 -14 14.50 18.50 -34 8 14 44.50 11.80 32 -8 -14 33.10 18.70 -32 -8 14 52.29 12.30 -32 -8 14 55.89 13.40 -32 8 14 69.29 12.20 32 8 -14 47.10 15.90 30 -8 -14 42.80 17.90 -30 -8 14 66.59 11.80 30 8 -14 47.30 14.20 -30 8 14 56.19 11.00 -28 -8 14 141.79 15.90 28 -8 -14 94.89 20.80 28 8 -14 155.58 19.50 -28 8 14 139.09 15.70 26 -8 -14 30.10 16.20 -26 -8 14 61.59 10.30 26 8 -14 36.10 12.70 -26 8 14 51.09 10.30 24 -8 -14 167.18 21.80 -24 -8 14 136.29 16.40 -24 8 14 201.58 19.50 -24 8 14 176.78 16.70 24 8 -14 151.18 19.70 -22 -8 14 272.77 24.10 22 -8 -14 249.48 29.40 -22 8 14 282.47 23.00 22 8 -14 248.28 27.80 -22 8 14 236.88 24.80 -20 -8 14 516.45 43.90 20 -8 -14 510.35 47.40 20 8 -14 590.94 46.80 -20 8 14 538.95 43.10 -20 8 14 503.25 44.10 18 -8 -14 -11.20 11.40 -18 -8 14 -1.50 6.60 18 8 -14 -4.90 9.80 -18 8 14 -0.70 6.50 -18 8 14 1.50 5.10 16 -8 -14 20.00 11.70 -16 -8 14 31.80 7.60 16 8 -14 27.70 7.80 16 8 -14 31.50 11.10 -16 8 14 19.20 7.10 -16 8 14 30.20 5.90 -14 -8 14 -2.20 6.10 14 -8 -14 -17.80 10.20 -14 8 14 9.00 4.90 14 8 -14 3.00 7.50 -14 8 14 0.60 6.50 14 8 -14 -0.80 9.30 12 -8 -14 10.50 9.70 12 -8 -14 14.50 6.70 -12 -8 14 1.40 6.50 12 8 -14 11.70 9.50 -12 8 14 4.50 6.40 12 8 -14 6.70 7.90 -12 8 14 19.90 5.20 -10 -8 14 24.00 7.00 -10 -8 14 21.50 9.90 10 -8 -14 7.70 9.60 10 -8 -14 20.10 7.30 10 8 -14 24.50 8.30 -10 8 14 17.00 6.30 -10 8 14 18.30 5.60 8 -8 -14 59.59 10.80 -8 -8 14 47.70 11.70 -8 -8 14 64.89 9.20 8 -8 -14 53.09 9.70 8 8 -14 51.59 10.50 -8 8 14 53.19 8.10 -8 8 14 51.09 7.40 -6 -8 14 278.47 24.90 -6 -8 14 270.87 27.40 6 -8 -14 274.37 27.50 6 -8 -14 283.07 25.90 -6 8 14 295.07 24.50 -6 8 14 276.47 24.20 6 8 -14 263.57 27.30 -4 -8 14 267.57 23.90 4 -8 -14 247.58 25.70 -4 -8 14 234.08 25.60 -4 8 14 252.77 23.20 4 8 -14 295.77 26.10 -4 8 14 280.57 23.10 2 -8 -14 315.87 27.70 -2 -8 14 257.47 26.30 -2 -8 14 294.57 28.30 2 8 -14 258.37 28.30 -2 8 14 298.17 25.70 -2 8 14 310.27 25.80 0 -8 14 390.96 36.40 0 -8 14 407.56 35.30 0 -8 -14 430.56 36.40 0 8 14 422.46 34.50 0 8 -14 380.66 36.80 0 8 14 408.96 34.20 2 -8 14 45.70 9.10 -2 -8 -14 36.50 10.70 2 8 14 28.30 7.50 -2 8 -14 16.60 10.80 2 8 14 27.30 7.60 4 -8 14 152.78 16.10 -4 -8 -14 159.58 17.50 4 8 14 140.29 15.30 -4 8 -14 128.59 17.70 4 8 14 150.38 15.30 -6 -8 -14 107.59 16.00 6 -8 14 109.49 14.10 6 8 14 121.69 13.70 -6 8 -14 126.49 16.90 6 8 14 116.49 13.90 8 -8 14 50.99 10.20 -8 -8 -14 53.09 12.90 8 8 14 37.50 9.20 -8 8 -14 30.70 13.10 8 8 14 39.90 10.10 -10 -8 -14 24.90 11.90 10 -8 14 -10.10 9.50 10 8 14 6.00 9.30 10 8 14 5.40 8.60 -10 8 -14 16.40 12.70 -12 -8 -14 16.40 12.30 12 -8 14 -0.70 9.80 12 8 14 6.20 10.30 -12 8 -14 8.70 12.00 33 -9 -14 37.20 19.00 -33 -9 14 26.40 12.20 -33 9 14 43.30 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22 55.79 10.30 -10 -4 22 18.20 9.90 10 -4 -22 26.90 11.90 -10 4 22 27.10 9.50 10 4 -22 37.70 12.30 8 -4 -22 9.40 11.90 -8 -4 22 12.00 10.00 8 4 -22 17.30 12.00 -8 4 22 2.00 9.20 6 -4 -22 28.40 12.60 -6 -4 22 4.60 10.10 6 4 -22 50.49 12.90 -6 4 22 17.40 9.60 4 -4 -22 14.80 13.40 -4 -4 22 1.50 10.60 -4 4 22 22.60 10.80 4 4 -22 0.60 12.50 -29 -5 22 34.40 10.50 29 -5 -22 3.00 17.50 -29 5 22 36.00 9.60 29 5 -22 37.10 17.20 27 -5 -22 -17.90 15.30 -27 -5 22 -3.80 9.30 27 5 -22 -11.70 15.50 -27 5 22 23.50 8.50 25 -5 -22 -26.20 15.00 -25 -5 22 4.20 9.00 -25 5 22 4.40 7.70 25 5 -22 -11.30 14.10 -23 -5 22 -3.40 8.60 23 -5 -22 -23.80 13.90 23 5 -22 -15.00 13.70 -23 5 22 -1.10 7.90 -21 -5 22 15.30 9.00 21 -5 -22 -11.80 13.60 21 5 -22 -12.30 13.20 -21 5 22 3.70 8.10 19 -5 -22 95.09 18.40 -19 -5 22 139.89 15.10 -19 5 22 119.79 14.00 19 5 -22 128.59 18.70 17 -5 -22 74.69 15.80 -17 -5 22 98.59 13.50 17 5 -22 85.49 17.00 -17 5 22 123.29 13.00 -15 -5 22 155.88 18.00 -15 5 22 157.48 17.20 15 5 -22 189.68 21.70 13 -5 -22 257.87 26.00 -13 -5 22 184.28 22.20 -13 5 22 251.57 24.10 13 5 -22 245.98 25.40 13 5 -22 237.48 28.00 11 -5 -22 358.96 33.30 -11 -5 22 335.27 31.20 11 5 -22 324.97 33.40 -11 5 22 316.87 30.60 9 -5 -22 290.57 29.80 -9 -5 22 276.37 29.10 9 5 -22 319.57 31.30 -9 5 22 267.87 27.90 7 -5 -22 295.37 30.40 -7 -5 22 283.87 28.30 7 5 -22 294.57 30.60 -7 5 22 267.37 28.20 -5 -5 22 161.88 22.00 5 -5 -22 242.08 27.30 5 5 -22 274.07 27.70 -5 5 22 245.58 24.20 -30 -6 22 50.59 12.60 30 -6 -22 23.80 20.70 30 6 -22 51.39 19.40 28 -6 -22 104.79 21.20 -28 -6 22 117.79 15.00 28 6 -22 120.59 21.30 26 -6 -22 64.99 19.80 -26 -6 22 117.39 14.30 26 6 -22 106.29 19.70 -24 -6 22 171.48 17.90 24 -6 -22 152.78 23.10 -24 6 22 139.69 16.30 24 6 -22 183.08 22.70 22 -6 -22 179.08 24.40 -22 -6 22 186.78 20.10 22 6 -22 221.78 27.00 -22 6 22 190.88 20.70 -20 -6 22 115.59 13.80 20 -6 -22 79.49 18.50 -20 6 22 97.59 12.60 20 6 -22 114.59 18.30 18 -6 -22 46.40 16.30 -18 -6 22 56.39 11.40 18 6 -22 68.69 15.80 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23 92.59 12.00 21 5 -23 71.89 16.60 -19 -5 23 75.69 11.80 19 -5 -23 37.40 16.00 -19 5 23 76.59 11.10 19 5 -23 56.19 15.40 -17 -5 23 124.49 15.60 -17 5 23 136.39 14.80 17 5 -23 108.69 18.60 -15 -5 23 175.58 19.10 -15 5 23 181.88 18.60 15 5 -23 176.88 22.50 13 -5 -23 219.08 26.60 -13 -5 23 139.99 18.70 13 5 -23 196.48 22.70 13 5 -23 153.08 22.80 -13 5 23 218.28 21.50 11 -5 -23 65.69 13.60 -11 -5 23 55.69 12.30 -11 5 23 50.99 11.50 11 5 -23 75.39 14.40 9 -5 -23 43.70 13.40 -9 -5 23 8.30 10.60 -9 5 23 13.30 10.10 9 5 -23 29.80 12.90 7 -5 -23 10.10 12.20 -7 5 23 20.70 10.00 7 5 -23 26.30 13.10 28 -6 -23 28.60 18.50 -28 -6 23 44.40 12.30 28 6 -23 51.19 19.00 26 -6 -23 -12.80 16.60 -26 -6 23 32.60 10.40 26 6 -23 19.50 16.10 24 -6 -23 -10.20 15.10 -24 -6 23 -1.10 9.30 -24 6 23 26.40 13.40 24 6 -23 -4.60 13.70 22 -6 -23 -0.30 15.70 -22 -6 23 15.60 9.90 22 6 -23 17.50 13.60 -22 6 23 6.60 8.20 -20 -6 23 12.40 9.50 20 -6 -23 -9.10 14.80 -20 6 23 13.20 8.40 20 6 -23 -0.40 14.30 -18 -6 23 39.90 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-5.40 9.20 -14 0 24 3.50 9.50 12 0 -24 189.48 21.60 -12 0 24 186.08 20.20 -10 0 24 125.79 16.50 10 0 -24 128.19 17.80 27 -1 -24 -18.70 15.50 -27 -1 24 -6.00 8.90 -27 1 24 -1.80 9.20 27 1 -24 -12.90 16.30 -25 -1 24 0.60 9.30 25 -1 -24 -9.80 15.10 25 1 -24 -7.70 14.40 -25 1 24 -3.10 9.00 23 -1 -24 -14.10 13.80 -23 -1 24 5.90 9.30 -23 1 24 15.00 9.20 23 1 -24 -14.60 13.60 -21 -1 24 12.70 9.50 21 -1 -24 -12.50 14.30 21 1 -24 -7.30 14.40 -21 1 24 13.40 9.20 -19 -1 24 9.80 9.50 19 -1 -24 -8.10 13.90 19 1 -24 -3.20 12.70 -19 1 24 13.70 9.50 -17 -1 24 40.30 10.10 -17 1 24 22.30 9.50 17 1 -24 7.50 14.20 -15 -1 24 54.09 11.30 -15 1 24 47.20 10.90 -13 -1 24 161.48 18.60 -13 1 24 179.58 18.70 13 1 -24 152.28 26.00 -11 -1 24 119.99 16.00 11 -1 -24 141.39 17.90 -11 1 24 116.19 15.90 11 1 -24 116.19 17.70 -28 -2 24 2.20 9.60 28 -2 -24 -18.90 17.30 -28 2 24 2.90 9.40 28 2 -24 -48.90 20.60 26 -2 -24 19.40 16.30 -26 -2 24 17.70 10.20 -26 2 24 29.00 9.80 26 2 -24 24.40 16.20 24 -2 -24 53.69 17.00 -24 -2 24 35.80 10.70 24 2 -24 24.60 16.50 -24 2 24 31.90 9.80 22 -2 -24 12.20 15.20 -22 -2 24 18.90 9.80 -22 2 24 35.50 9.70 22 2 -24 2.60 14.80 -20 -2 24 112.89 14.60 20 -2 -24 102.29 19.30 20 2 -24 92.19 18.70 -20 2 24 131.49 14.40 -18 -2 24 71.49 11.80 18 -2 -24 27.10 14.40 -18 2 24 60.39 11.20 18 2 -24 39.20 16.00 -16 -2 24 52.69 11.40 16 2 -24 48.80 15.40 -16 2 24 60.59 11.40 -14 -2 24 107.59 14.70 -14 2 24 105.39 14.30 12 -2 -24 176.58 20.60 -12 -2 24 163.68 19.20 -12 2 24 173.58 19.10 -10 -2 24 212.28 25.20 10 -2 -24 272.37 27.50 -10 2 24 170.18 21.20 -27 -3 24 6.90 9.80 27 -3 -24 -14.60 15.90 -27 3 24 2.50 8.60 27 3 -24 -19.70 15.20 -25 -3 24 14.10 9.50 25 -3 -24 -9.10 15.20 -25 3 24 0.90 9.10 25 3 -24 -8.50 15.30 -23 -3 24 71.39 12.20 23 -3 -24 43.00 16.00 -23 3 24 77.69 11.60 23 3 -24 77.29 17.60 -21 -3 24 34.00 10.30 21 -3 -24 29.00 15.30 21 3 -24 15.40 14.80 -21 3 24 33.20 9.60 -19 -3 24 8.50 9.50 19 -3 -24 15.40 14.20 19 3 -24 -1.70 13.90 -19 3 24 8.50 8.90 -17 -3 24 15.10 9.80 17 3 -24 20.90 13.70 -17 3 24 22.20 9.70 -15 -3 24 41.20 10.90 -15 3 24 31.60 10.00 -13 -3 24 48.90 12.00 -13 3 24 43.40 11.40 13 3 -24 48.80 13.30 -11 -3 24 -1.00 10.70 11 -3 -24 20.00 12.40 -11 3 24 -1.10 10.20 11 3 -24 31.30 12.50 26 -4 -24 -10.10 16.80 -26 -4 24 24.90 10.10 -26 4 24 31.50 9.30 26 4 -24 2.60 16.20 -24 -4 24 6.20 9.40 24 -4 -24 -5.40 14.80 -24 4 24 -3.20 8.80 24 4 -24 3.70 15.50 -22 -4 24 15.80 9.90 22 -4 -24 -12.10 14.00 22 4 -24 -6.20 14.80 -22 4 24 21.70 9.00 20 -4 -24 -27.70 14.00 -20 -4 24 15.70 9.80 -20 4 24 24.20 9.00 20 4 -24 -11.40 13.90 -18 -4 24 6.40 10.00 18 4 -24 6.10 13.60 -18 4 24 6.40 8.80 -16 -4 24 12.20 9.90 -16 4 24 18.30 9.40 16 4 -24 0.80 13.30 -14 -4 24 8.10 10.20 -14 4 24 14.90 9.90 12 -4 -24 15.20 11.80 -12 -4 24 9.30 10.70 12 4 -24 12.30 11.80 -12 4 24 6.00 9.80 -25 -5 24 40.90 11.00 25 -5 -24 8.10 16.80 25 5 -24 18.30 16.30 -25 5 24 43.40 9.80 -23 -5 24 41.10 11.10 23 -5 -24 27.20 17.00 23 5 -24 30.00 16.20 -23 5 24 59.09 10.40 -21 -5 24 38.80 10.60 21 -5 -24 4.20 16.50 21 5 -24 54.69 15.90 -21 5 24 59.39 10.30 -19 -5 24 37.60 10.80 -19 5 24 29.50 9.40 19 5 -24 34.00 14.30 -17 -5 24 2.00 9.90 -17 5 24 -2.00 8.60 17 5 -24 -8.10 13.70 -15 -5 24 6.90 10.20 15 5 -24 -8.40 13.40 -15 5 24 9.50 8.70 -13 -5 24 -0.40 10.10 -13 5 24 8.90 9.40 13 5 -24 29.30 12.20 11 -5 -24 14.80 12.50 -24 -6 24 8.10 10.20 24 -6 -24 -27.30 16.30 24 6 -24 7.30 15.80 -22 -6 24 29.60 10.40 22 -6 -24 2.70 16.00 22 6 -24 7.90 14.60 -22 6 24 26.40 14.70 -20 -6 24 42.50 11.20 20 -6 -24 15.50 17.30 20 6 -24 46.30 15.80 -20 6 24 46.30 10.30 -18 -6 24 27.20 10.60 18 6 -24 26.30 14.60 -18 6 24 47.10 10.30 -16 -6 24 91.69 13.80 16 6 -24 87.69 17.80 -16 6 24 84.89 12.80 -14 -6 24 161.18 18.80 -14 6 24 164.98 18.00 12 -6 -24 252.87 28.10 -12 6 24 236.38 26.50 12 6 -24 263.17 28.40 -23 -7 24 1.70 11.40 23 -7 -24 -26.00 16.00 23 7 -24 -6.20 14.60 -21 -7 24 12.30 10.00 21 -7 -24 -3.80 15.80 21 7 -24 -6.90 14.10 -19 -7 24 86.69 12.80 19 7 -24 46.10 16.60 -17 -7 24 14.00 10.10 17 7 -24 -9.80 13.40 -15 -7 24 7.20 10.50 15 7 -24 -2.90 13.90 22 -8 -24 -3.60 17.50 -22 -8 24 30.70 17.40 22 8 -24 15.20 16.10 -20 -8 24 43.10 12.60 20 8 -24 39.50 16.30 -18 -8 24 11.20 10.40 18 8 -24 2.50 14.70 -16 -8 24 28.10 17.60 16 8 -24 11.50 15.10 -24 0 25 -6.00 9.20 24 0 -25 -20.20 14.70 22 0 -25 -6.10 15.50 -22 0 25 3.70 9.30 -20 0 25 -3.90 9.50 20 0 -25 -13.50 14.60 -18 0 25 8.80 9.80 -16 0 25 8.50 9.80 -23 -1 25 142.19 16.60 23 -1 -25 112.29 20.50 -23 1 25 157.68 16.80 23 1 -25 132.39 22.20 21 -1 -25 86.69 19.40 -21 -1 25 129.59 14.90 21 1 -25 94.49 19.50 -21 1 25 120.59 14.70 19 -1 -25 83.69 19.40 -19 -1 25 100.99 14.10 -19 1 25 88.79 13.70 19 1 -25 98.09 18.50 -17 -1 25 84.99 13.40 -17 1 25 84.39 13.30 -22 -2 25 77.99 12.80 22 -2 -25 44.20 17.50 -22 2 25 92.79 12.80 22 2 -25 67.19 16.70 -20 -2 25 36.70 10.80 20 -2 -25 1.80 14.80 20 2 -25 16.90 15.00 -20 2 25 34.10 10.20 -18 -2 25 15.60 10.40 -18 2 25 -6.80 9.10 18 2 -25 -13.70 13.50 -16 -2 25 13.10 11.70 -16 2 25 3.40 9.50 -23 -3 25 82.89 14.20 23 -3 -25 42.00 17.30 -23 3 25 89.09 12.90 23 3 -25 75.49 18.90 21 -3 -25 101.49 19.60 -21 -3 25 120.59 15.20 -21 3 25 109.59 14.30 21 3 -25 104.99 19.90 -19 -3 25 126.99 15.90 19 3 -25 105.79 20.20 -19 3 25 112.39 14.80 -17 -3 25 93.79 17.40 17 3 -25 89.19 23.30 -17 3 25 97.39 13.70 -20 -4 25 10.50 16.90 20 4 -25 26.80 16.00 -20 4 25 23.80 9.80 18 4 -25 64.59 17.50 -18 4 25 84.19 12.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 33135 #===END data_Ox_5k _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Ox_5k' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H63 Br N O4 P Pd' _chemical_formula_weight 923.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.126(9) _cell_length_b 11.472(8) _cell_length_c 28.93(2) _cell_angle_alpha 90 _cell_angle_beta 91.981(10) _cell_angle_gamma 90 _cell_volume 4354(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5577 _cell_measurement_theta_min 2.267 _cell_measurement_theta_max 25.834 _exptl_crystal_description Blade _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_F_000 1920 _exptl_transmission_factor_min 0.712 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 1.424 _shelx_estimated_absorpt_T_min 0.764 _shelx_estimated_absorpt_T_max 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48392 _diffrn_reflns_av_unetI/netI 0.1311 _diffrn_reflns_av_R_equivalents 0.1486 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.409 _diffrn_reflns_theta_max 27.065 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 9496 _reflns_number_gt 5928 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9496 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.37156(3) 0.33906(3) 0.37577(2) 0.01828(10) Uani 1 1 d . . . . . Br1 Br 0.45428(4) 0.53085(4) 0.37508(2) 0.03988(17) Uani 1 1 d . . . . . P1 P 0.28683(9) 0.16230(9) 0.36409(4) 0.0174(3) Uani 1 1 d . . . . . O1 O 0.2725(3) -0.1032(2) 0.35361(12) 0.0292(8) Uani 1 1 d . . . . . O2 O 0.6648(2) 0.0530(3) 0.38466(11) 0.0255(8) Uani 1 1 d . . . . . O3 O -0.0372(2) 0.1902(3) 0.36036(11) 0.0306(8) Uani 1 1 d . . . . . O4 O -0.0085(3) 0.0450(3) 0.30968(12) 0.0347(9) Uani 1 1 d . . . . . N1 N -0.0632(4) 0.7437(4) 0.39606(17) 0.0481(13) Uani 1 1 d . . . . . C1 C 0.3888(3) 0.0522(4) 0.36541(14) 0.0184(10) Uani 1 1 d . . . . . C2 C 0.3707(4) -0.0707(4) 0.36069(16) 0.0219(11) Uani 1 1 d . . . . . C3 C 0.2510(4) -0.2217(4) 0.3447(2) 0.0389(14) Uani 1 1 d . . . . . H3A H 0.293207 -0.249341 0.319610 0.058 Uiso 1 1 calc R U . . . H3B H 0.178826 -0.230368 0.335522 0.058 Uiso 1 1 calc R U . . . H3C H 0.266064 -0.267607 0.372629 0.058 Uiso 1 1 calc R U . . . C4 C 0.4494(4) -0.1478(4) 0.36483(15) 0.0217(11) Uani 1 1 d . . . . . H4 H 0.435814 -0.228923 0.362208 0.026 Uiso 1 1 calc R U . . . C5 C 0.5494(4) -0.1104(4) 0.37283(15) 0.0221(11) Uani 1 1 d . . . . . H5 H 0.603481 -0.165294 0.375358 0.026 Uiso 1 1 calc R U . . . C6 C 0.5688(4) 0.0076(4) 0.37703(15) 0.0205(11) Uani 1 1 d . . . . . C7 C 0.7465(4) -0.0276(4) 0.39186(18) 0.0349(13) Uani 1 1 d . . . . . H7A H 0.729933 -0.081686 0.416719 0.052 Uiso 1 1 calc R U . . . H7B H 0.809019 0.014968 0.400497 0.052 Uiso 1 1 calc R U . . . H7C H 0.756638 -0.071426 0.363313 0.052 Uiso 1 1 calc R U . . . C8 C 0.4891(4) 0.0893(4) 0.37349(14) 0.0180(10) Uani 1 1 d . . . . . C9 C 0.5236(3) 0.2130(3) 0.37981(15) 0.0153(10) Uani 1 1 d . . . . . C10 C 0.5471(3) 0.2515(3) 0.42594(15) 0.0170(10) Uani 1 1 d . . . . . C11 C 0.5005(3) 0.1934(4) 0.46750(14) 0.0190(10) Uani 1 1 d . . . . . H11 H 0.450575 0.134017 0.455468 0.023 Uiso 1 1 calc R U . . . C12 C 0.4427(4) 0.2790(4) 0.49660(16) 0.0308(12) Uani 1 1 d . . . . . H12A H 0.490554 0.334807 0.511002 0.046 Uiso 1 1 calc R U . . . H12B H 0.407339 0.236664 0.520721 0.046 Uiso 1 1 calc R U . . . H12C H 0.392696 0.320895 0.476898 0.046 Uiso 1 1 calc R U . . . C13 C 0.5814(4) 0.1291(4) 0.49687(16) 0.0274(12) Uani 1 1 d . . . . . H13A H 0.615056 0.071031 0.477796 0.041 Uiso 1 1 calc R U . . . H13B H 0.549062 0.090069 0.522672 0.041 Uiso 1 1 calc R U . . . H13C H 0.632096 0.185029 0.508995 0.041 Uiso 1 1 calc R U . . . C14 C 0.6203(4) 0.3366(4) 0.43317(15) 0.0209(10) Uani 1 1 d . . . . . H14 H 0.634742 0.363120 0.463807 0.025 Uiso 1 1 calc R U . . . C15 C 0.6740(3) 0.3849(4) 0.39695(16) 0.0191(10) Uani 1 1 d . . . . . C16 C 0.7608(4) 0.4684(4) 0.40732(16) 0.0258(11) Uani 1 1 d . . . . . H16 H 0.787875 0.493911 0.377054 0.031 Uiso 1 1 calc R U . . . C17 C 0.7261(4) 0.5764(4) 0.43229(19) 0.0394(14) Uani 1 1 d . . . . . H17A H 0.671351 0.614294 0.413978 0.059 Uiso 1 1 calc R U . . . H17B H 0.783574 0.630324 0.436480 0.059 Uiso 1 1 calc R U . . . H17C H 0.700933 0.554442 0.462577 0.059 Uiso 1 1 calc R U . . . C18 C 0.8474(4) 0.4079(4) 0.43420(17) 0.0330(13) Uani 1 1 d . . . . . H18A H 0.821700 0.375411 0.462879 0.050 Uiso 1 1 calc R U . . . H18B H 0.901488 0.464418 0.441653 0.050 Uiso 1 1 calc R U . . . H18C H 0.874735 0.344951 0.415379 0.050 Uiso 1 1 calc R U . . . C19 C 0.6474(3) 0.3510(3) 0.35224(14) 0.0186(10) Uani 1 1 d . . . . . H19 H 0.680433 0.387090 0.327274 0.022 Uiso 1 1 calc R U . . . C20 C 0.5747(3) 0.2664(4) 0.34252(15) 0.0164(10) Uani 1 1 d . . . . . C21 C 0.5540(4) 0.2280(4) 0.29293(15) 0.0232(11) Uani 1 1 d . . . . . H21 H 0.492566 0.176446 0.292723 0.028 Uiso 1 1 calc R U . . . C22 C 0.5285(4) 0.3316(4) 0.26105(16) 0.0343(13) Uani 1 1 d . . . . . H22A H 0.474052 0.378008 0.274273 0.051 Uiso 1 1 calc R U . . . H22B H 0.505958 0.302733 0.230504 0.051 Uiso 1 1 calc R U . . . H22C H 0.589349 0.380181 0.258023 0.051 Uiso 1 1 calc R U . . . C23 C 0.6412(4) 0.1568(5) 0.27358(16) 0.0348(13) Uani 1 1 d . . . . . H23A H 0.702344 0.205531 0.272341 0.052 Uiso 1 1 calc R U . . . H23B H 0.621825 0.129787 0.242358 0.052 Uiso 1 1 calc R U . . . H23C H 0.655267 0.089434 0.293620 0.052 Uiso 1 1 calc R U . . . C24 C 0.1840(4) 0.1160(4) 0.40572(16) 0.0210(11) Uani 1 1 d . . . . . C25 C 0.1444(4) 0.2254(4) 0.43079(16) 0.0235(11) Uani 1 1 d . . . . . H25A H 0.203351 0.268635 0.444470 0.028 Uiso 1 1 calc R U . . . H25B H 0.109820 0.276983 0.407732 0.028 Uiso 1 1 calc R U . . . C26 C 0.0706(4) 0.1979(4) 0.46886(17) 0.0324(13) Uani 1 1 d . . . . . H26A H 0.049820 0.271124 0.483986 0.039 Uiso 1 1 calc R U . . . H26B H 0.008671 0.160345 0.455191 0.039 Uiso 1 1 calc R U . . . C27 C 0.1202(4) 0.1176(4) 0.50442(17) 0.0326(13) Uani 1 1 d . . . . . H27A H 0.178419 0.157999 0.520094 0.039 Uiso 1 1 calc R U . . . H27B H 0.070435 0.097418 0.528085 0.039 Uiso 1 1 calc R U . . . C28 C 0.1575(4) 0.0070(4) 0.48183(17) 0.0324(13) Uani 1 1 d . . . . . H28A H 0.098469 -0.037459 0.468981 0.039 Uiso 1 1 calc R U . . . H28B H 0.193186 -0.042201 0.505381 0.039 Uiso 1 1 calc R U . . . C29 C 0.2299(4) 0.0349(4) 0.44322(16) 0.0256(11) Uani 1 1 d . . . . . H29A H 0.250547 -0.038933 0.428540 0.031 Uiso 1 1 calc R U . . . H29B H 0.292032 0.071813 0.456936 0.031 Uiso 1 1 calc R U . . . C30 C 0.0960(3) 0.0542(4) 0.37799(17) 0.0256(11) Uani 1 1 d . . . . . H30A H 0.123738 -0.016920 0.363696 0.031 Uiso 1 1 calc R U . . . H30B H 0.044351 0.029063 0.400053 0.031 Uiso 1 1 calc R U . . . C31 C 0.0432(4) 0.1255(4) 0.34053(17) 0.0266(12) Uani 1 1 d . . . . . C32 C -0.1157(4) 0.1998(5) 0.32621(18) 0.0356(13) Uani 1 1 d . . . . . H32A H -0.110654 0.274418 0.309236 0.043 Uiso 1 1 calc R U . . . H32B H -0.183414 0.195232 0.340138 0.043 Uiso 1 1 calc R U . . . C33 C -0.0991(4) 0.0971(5) 0.2943(2) 0.0446(15) Uani 1 1 d . . . . . H33A H -0.156353 0.041309 0.295852 0.053 Uiso 1 1 calc R U . . . H33B H -0.093888 0.123939 0.261964 0.053 Uiso 1 1 calc R U . . . C34 C 0.1121(4) 0.2068(4) 0.31450(16) 0.0238(11) Uani 1 1 d . . . . . H34A H 0.119322 0.280027 0.332412 0.029 Uiso 1 1 calc R U . . . H34B H 0.077415 0.226448 0.284585 0.029 Uiso 1 1 calc R U . . . C35 C 0.2195(4) 0.1621(4) 0.30456(15) 0.0218(10) Uani 1 1 d . . . . . C36 C 0.2812(4) 0.2482(4) 0.27509(15) 0.0225(11) Uani 1 1 d . . . . . H36A H 0.284365 0.324417 0.291102 0.027 Uiso 1 1 calc R U . . . H36B H 0.351858 0.218717 0.273280 0.027 Uiso 1 1 calc R U . . . C37 C 0.2377(4) 0.2667(4) 0.22614(16) 0.0326(13) Uani 1 1 d . . . . . H37A H 0.168749 0.301204 0.227380 0.039 Uiso 1 1 calc R U . . . H37B H 0.281611 0.321603 0.209478 0.039 Uiso 1 1 calc R U . . . C38 C 0.2319(4) 0.1517(4) 0.20047(16) 0.0366(13) Uani 1 1 d . . . . . H38A H 0.301706 0.122469 0.195544 0.044 Uiso 1 1 calc R U . . . H38B H 0.197705 0.163425 0.169790 0.044 Uiso 1 1 calc R U . . . C39 C 0.1733(4) 0.0625(4) 0.22770(17) 0.0323(13) Uani 1 1 d . . . . . H39A H 0.174883 -0.013385 0.211408 0.039 Uiso 1 1 calc R U . . . H39B H 0.101238 0.087330 0.228923 0.039 Uiso 1 1 calc R U . . . C40 C 0.2166(4) 0.0466(4) 0.27693(16) 0.0267(11) Uani 1 1 d . . . . . H40A H 0.286642 0.014905 0.275731 0.032 Uiso 1 1 calc R U . . . H40B H 0.174509 -0.010756 0.293235 0.032 Uiso 1 1 calc R U . . . C41 C 0.2477(3) 0.4420(3) 0.37900(15) 0.0161(10) Uani 1 1 d . . . . . C42 C 0.1882(4) 0.4799(4) 0.34088(16) 0.0219(11) Uani 1 1 d . . . . . H42 H 0.205302 0.455856 0.310697 0.026 Uiso 1 1 calc R U . . . C43 C 0.1046(4) 0.5519(4) 0.34636(17) 0.0251(11) Uani 1 1 d . . . . . H43 H 0.063153 0.573334 0.320171 0.030 Uiso 1 1 calc R U . . . C44 C 0.0813(4) 0.5929(4) 0.38979(17) 0.0260(11) Uani 1 1 d . . . . . C45 C -0.0010(4) 0.6757(4) 0.39404(18) 0.0338(13) Uani 1 1 d . . . . . C46 C 0.1414(4) 0.5604(4) 0.42750(17) 0.0314(13) Uani 1 1 d . . . . . H46 H 0.126602 0.588988 0.457338 0.038 Uiso 1 1 calc R U . . . C47 C 0.2231(4) 0.4865(4) 0.42226(16) 0.0297(12) Uani 1 1 d . . . . . H47 H 0.263808 0.465287 0.448726 0.036 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0215(2) 0.01147(16) 0.02176(19) 0.00088(15) -0.00024(14) 0.00181(15) Br1 0.0272(3) 0.0119(2) 0.0799(5) 0.0026(2) -0.0079(3) 0.0010(2) P1 0.0185(7) 0.0118(5) 0.0219(6) -0.0003(5) 0.0010(5) 0.0029(5) O1 0.028(2) 0.0098(16) 0.050(2) -0.0023(14) 0.0043(17) -0.0056(14) O2 0.0195(19) 0.0227(17) 0.034(2) -0.0016(14) -0.0023(15) 0.0097(15) O3 0.019(2) 0.033(2) 0.040(2) -0.0120(15) -0.0003(16) 0.0055(15) O4 0.021(2) 0.032(2) 0.050(2) -0.0178(17) -0.0105(17) 0.0040(16) N1 0.042(3) 0.041(3) 0.062(4) -0.008(2) 0.011(3) 0.012(3) C1 0.017(3) 0.020(2) 0.019(3) 0.0045(18) 0.004(2) 0.0012(19) C2 0.032(3) 0.008(2) 0.026(3) -0.0020(18) 0.007(2) -0.003(2) C3 0.041(4) 0.015(3) 0.061(4) -0.006(2) 0.001(3) -0.009(2) C4 0.028(3) 0.014(2) 0.024(2) 0.0044(19) 0.005(2) 0.008(2) C5 0.026(3) 0.023(2) 0.017(2) 0.0028(19) 0.004(2) 0.014(2) C6 0.019(3) 0.021(2) 0.022(3) -0.0017(19) 0.005(2) 0.003(2) C7 0.021(3) 0.040(3) 0.044(3) -0.005(3) -0.003(2) 0.014(2) C8 0.025(3) 0.013(2) 0.016(2) -0.0002(18) 0.007(2) 0.000(2) C9 0.012(2) 0.011(2) 0.023(3) 0.0060(18) 0.0014(19) 0.0059(18) C10 0.016(3) 0.012(2) 0.023(3) 0.0029(18) 0.004(2) 0.0041(18) C11 0.022(3) 0.018(2) 0.017(2) 0.0021(18) 0.006(2) -0.0002(19) C12 0.034(3) 0.039(3) 0.019(3) 0.005(2) 0.009(2) 0.005(2) C13 0.032(3) 0.026(3) 0.025(3) 0.009(2) 0.004(2) 0.006(2) C14 0.027(3) 0.021(2) 0.015(2) 0.000(2) -0.001(2) 0.007(2) C15 0.017(3) 0.014(2) 0.027(3) 0.0004(19) 0.001(2) 0.0011(19) C16 0.025(3) 0.027(3) 0.026(3) 0.001(2) 0.007(2) 0.002(2) C17 0.040(4) 0.031(3) 0.048(4) -0.015(3) 0.008(3) -0.005(3) C18 0.030(3) 0.037(3) 0.032(3) 0.000(2) -0.002(2) -0.001(2) C19 0.022(3) 0.015(2) 0.019(2) 0.0077(19) 0.004(2) 0.001(2) C20 0.014(3) 0.016(2) 0.020(2) 0.0048(18) 0.0019(19) 0.0036(18) C21 0.023(3) 0.029(3) 0.017(3) 0.002(2) 0.001(2) -0.004(2) C22 0.038(3) 0.045(3) 0.020(3) 0.014(2) -0.001(2) -0.013(3) C23 0.032(3) 0.049(3) 0.023(3) -0.001(3) 0.005(2) -0.001(3) C24 0.017(3) 0.020(2) 0.026(3) 0.0012(19) 0.003(2) -0.001(2) C25 0.022(3) 0.021(2) 0.027(3) -0.001(2) -0.001(2) 0.005(2) C26 0.025(3) 0.035(3) 0.038(3) -0.003(2) 0.012(2) 0.002(2) C27 0.026(3) 0.044(3) 0.029(3) 0.006(2) 0.012(2) -0.001(2) C28 0.025(3) 0.029(3) 0.044(3) 0.014(2) 0.008(3) -0.001(2) C29 0.022(3) 0.025(3) 0.030(3) 0.006(2) 0.002(2) 0.002(2) C30 0.014(3) 0.023(3) 0.040(3) 0.000(2) 0.002(2) -0.005(2) C31 0.017(3) 0.026(3) 0.037(3) -0.012(2) 0.001(2) 0.000(2) C32 0.021(3) 0.047(3) 0.039(3) -0.004(3) -0.002(3) 0.008(2) C33 0.035(4) 0.055(4) 0.044(4) -0.018(3) 0.002(3) 0.006(3) C34 0.025(3) 0.016(2) 0.030(3) -0.005(2) -0.004(2) 0.003(2) C35 0.028(3) 0.015(2) 0.022(2) -0.007(2) 0.001(2) 0.003(2) C36 0.024(3) 0.023(2) 0.020(3) -0.0025(19) -0.004(2) 0.004(2) C37 0.043(4) 0.031(3) 0.024(3) 0.001(2) 0.001(2) 0.010(3) C38 0.049(4) 0.038(3) 0.023(3) -0.013(2) -0.006(2) 0.013(3) C39 0.033(3) 0.027(3) 0.036(3) -0.014(2) -0.007(3) 0.010(2) C40 0.027(3) 0.020(2) 0.033(3) -0.007(2) -0.002(2) 0.004(2) C41 0.018(3) 0.008(2) 0.022(2) 0.0007(17) 0.002(2) -0.0004(18) C42 0.024(3) 0.016(2) 0.025(3) -0.005(2) 0.002(2) 0.001(2) C43 0.026(3) 0.019(2) 0.031(3) 0.002(2) -0.007(2) -0.003(2) C44 0.025(3) 0.019(2) 0.035(3) -0.001(2) 0.007(2) 0.004(2) C45 0.031(3) 0.030(3) 0.041(3) 0.002(2) 0.011(3) 0.004(3) C46 0.045(4) 0.029(3) 0.020(3) -0.002(2) 0.008(3) 0.006(2) C47 0.044(4) 0.024(3) 0.021(3) -0.001(2) 0.000(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C41 2.015(4) . ? Pd1 P1 2.3318(17) . ? Pd1 Br1 2.4541(15) . ? Pd1 C9 2.464(4) . ? P1 C1 1.840(4) . ? P1 C35 1.908(5) . ? P1 C24 1.915(5) . ? O1 C2 1.350(6) . ? O1 C3 1.411(5) . ? O2 C6 1.374(5) . ? O2 C7 1.425(5) . ? O3 C32 1.407(6) . ? O3 C31 1.426(5) . ? O4 C33 1.390(6) . ? O4 C31 1.438(5) . ? N1 C45 1.132(6) . ? C1 C8 1.396(6) . ? C1 C2 1.435(6) . ? C2 C4 1.363(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? C5 C6 1.383(6) . ? C5 H5 0.9500 . ? C6 C8 1.406(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.498(6) . ? C9 C20 1.428(6) . ? C9 C10 1.429(6) . ? C10 C14 1.381(6) . ? C10 C11 1.521(6) . ? C11 C12 1.514(6) . ? C11 C13 1.527(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.397(6) . ? C14 H14 0.9500 . ? C15 C19 1.384(6) . ? C15 C16 1.511(6) . ? C16 C17 1.512(6) . ? C16 C18 1.522(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.383(6) . ? C19 H19 0.9500 . ? C20 C21 1.516(6) . ? C21 C23 1.528(7) . ? C21 C22 1.534(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.535(6) . ? C24 C30 1.555(6) . ? C24 C25 1.549(6) . ? C25 C26 1.525(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.512(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.516(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.524(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.507(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C34 1.517(7) . ? C32 C33 1.517(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.536(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.546(6) . ? C35 C36 1.551(6) . ? C36 C37 1.523(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.515(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.517(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.526(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C47 1.400(6) . ? C41 C42 1.398(6) . ? C42 C43 1.387(6) . ? C42 H42 0.9500 . ? C43 C44 1.385(6) . ? C43 H43 0.9500 . ? C44 C46 1.376(7) . ? C44 C45 1.447(7) . ? C46 C47 1.379(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Pd1 P1 97.76(13) . . ? C41 Pd1 Br1 80.37(12) . . ? P1 Pd1 Br1 170.93(3) . . ? C41 Pd1 C9 174.63(16) . . ? P1 Pd1 C9 82.98(11) . . ? Br1 Pd1 C9 99.72(11) . . ? C1 P1 C35 109.37(19) . . ? C1 P1 C24 108.9(2) . . ? C35 P1 C24 104.6(2) . . ? C1 P1 Pd1 104.54(16) . . ? C35 P1 Pd1 109.61(14) . . ? C24 P1 Pd1 119.56(14) . . ? C2 O1 C3 118.6(4) . . ? C6 O2 C7 117.3(4) . . ? C32 O3 C31 107.0(4) . . ? C33 O4 C31 107.5(4) . . ? C8 C1 C2 118.0(4) . . ? C8 C1 P1 118.4(3) . . ? C2 C1 P1 123.6(3) . . ? O1 C2 C4 123.4(4) . . ? O1 C2 C1 116.1(4) . . ? C4 C2 C1 120.4(4) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 121.5(4) . . ? C2 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 119.1(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? O2 C6 C5 123.4(4) . . ? O2 C6 C8 115.8(4) . . ? C5 C6 C8 120.8(4) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 C6 120.2(4) . . ? C1 C8 C9 126.1(4) . . ? C6 C8 C9 113.7(4) . . ? C20 C9 C10 118.7(4) . . ? C20 C9 C8 117.5(4) . . ? C10 C9 C8 117.4(4) . . ? C20 C9 Pd1 96.5(3) . . ? C10 C9 Pd1 90.6(3) . . ? C8 C9 Pd1 108.0(3) . . ? C14 C10 C9 119.1(4) . . ? C14 C10 C11 119.1(4) . . ? C9 C10 C11 121.6(4) . . ? C12 C11 C10 112.2(4) . . ? C12 C11 C13 110.9(4) . . ? C10 C11 C13 111.2(4) . . ? C12 C11 H11 107.4 . . ? C10 C11 H11 107.4 . . ? C13 C11 H11 107.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 122.2(4) . . ? C10 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C19 C15 C14 118.2(4) . . ? C19 C15 C16 121.9(4) . . ? C14 C15 C16 119.9(4) . . ? C15 C16 C17 112.1(4) . . ? C15 C16 C18 111.0(4) . . ? C17 C16 C18 111.2(4) . . ? C15 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C15 122.5(4) . . ? C20 C19 H19 118.8 . . ? C15 C19 H19 118.8 . . ? C19 C20 C9 119.1(4) . . ? C19 C20 C21 119.7(4) . . ? C9 C20 C21 121.1(4) . . ? C20 C21 C23 113.0(4) . . ? C20 C21 C22 111.8(4) . . ? C23 C21 C22 110.1(4) . . ? C20 C21 H21 107.2 . . ? C23 C21 H21 107.2 . . ? C22 C21 H21 107.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C30 110.8(4) . . ? C29 C24 C25 106.8(4) . . ? C30 C24 C25 110.8(4) . . ? C29 C24 P1 110.2(3) . . ? C30 C24 P1 109.2(3) . . ? C25 C24 P1 109.0(3) . . ? C26 C25 C24 113.7(4) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 110.4(4) . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 110.8(4) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 111.0(4) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C24 114.0(4) . . ? C28 C29 H29A 108.8 . . ? C24 C29 H29A 108.8 . . ? C28 C29 H29B 108.8 . . ? C24 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C24 116.0(4) . . ? C31 C30 H30A 108.3 . . ? C24 C30 H30A 108.3 . . ? C31 C30 H30B 108.3 . . ? C24 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? O3 C31 O4 104.1(4) . . ? O3 C31 C30 108.7(4) . . ? O4 C31 C30 107.0(4) . . ? O3 C31 C34 110.0(4) . . ? O4 C31 C34 111.3(4) . . ? C30 C31 C34 115.0(4) . . ? O3 C32 C33 104.4(4) . . ? O3 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? O3 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? O4 C33 C32 106.2(4) . . ? O4 C33 H33A 110.5 . . ? C32 C33 H33A 110.5 . . ? O4 C33 H33B 110.5 . . ? C32 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C31 C34 C35 117.0(4) . . ? C31 C34 H34A 108.0 . . ? C35 C34 H34A 108.0 . . ? C31 C34 H34B 108.0 . . ? C35 C34 H34B 108.0 . . ? H34A C34 H34B 107.3 . . ? C34 C35 C40 112.1(4) . . ? C34 C35 C36 113.0(4) . . ? C40 C35 C36 105.4(4) . . ? C34 C35 P1 103.3(3) . . ? C40 C35 P1 118.0(3) . . ? C36 C35 P1 105.1(3) . . ? C37 C36 C35 114.4(4) . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C36 110.2(4) . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 110.5(4) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C38 C39 C40 112.7(4) . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C39 C40 C35 112.5(4) . . ? C39 C40 H40A 109.1 . . ? C35 C40 H40A 109.1 . . ? C39 C40 H40B 109.1 . . ? C35 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C47 C41 C42 116.9(4) . . ? C47 C41 Pd1 117.8(3) . . ? C42 C41 Pd1 125.1(3) . . ? C43 C42 C41 121.2(4) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C46 C44 C43 119.2(5) . . ? C46 C44 C45 121.3(4) . . ? C43 C44 C45 119.3(5) . . ? N1 C45 C44 176.9(6) . . ? C47 C46 C44 120.4(4) . . ? C47 C46 H46 119.8 . . ? C44 C46 H46 119.8 . . ? C46 C47 C41 121.8(5) . . ? C46 C47 H47 119.1 . . ? C41 C47 H47 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 P1 C1 C8 118.7(4) . . . . ? C24 P1 C1 C8 -127.5(3) . . . . ? Pd1 P1 C1 C8 1.4(4) . . . . ? C35 P1 C1 C2 -64.3(4) . . . . ? C24 P1 C1 C2 49.6(4) . . . . ? Pd1 P1 C1 C2 178.4(3) . . . . ? C3 O1 C2 C4 -7.7(7) . . . . ? C3 O1 C2 C1 174.5(4) . . . . ? C8 C1 C2 O1 179.0(4) . . . . ? P1 C1 C2 O1 2.0(6) . . . . ? C8 C1 C2 C4 1.1(6) . . . . ? P1 C1 C2 C4 -176.0(3) . . . . ? O1 C2 C4 C5 -179.0(4) . . . . ? C1 C2 C4 C5 -1.2(7) . . . . ? C2 C4 C5 C6 0.6(7) . . . . ? C7 O2 C6 C5 -4.7(6) . . . . ? C7 O2 C6 C8 175.5(4) . . . . ? C4 C5 C6 O2 -179.6(4) . . . . ? C4 C5 C6 C8 0.2(6) . . . . ? C2 C1 C8 C6 -0.3(6) . . . . ? P1 C1 C8 C6 176.9(3) . . . . ? C2 C1 C8 C9 -179.4(4) . . . . ? P1 C1 C8 C9 -2.2(6) . . . . ? O2 C6 C8 C1 179.5(4) . . . . ? C5 C6 C8 C1 -0.3(6) . . . . ? O2 C6 C8 C9 -1.3(5) . . . . ? C5 C6 C8 C9 178.9(4) . . . . ? C1 C8 C9 C20 -106.0(5) . . . . ? C6 C8 C9 C20 74.8(5) . . . . ? C1 C8 C9 C10 102.2(5) . . . . ? C6 C8 C9 C10 -77.0(5) . . . . ? C1 C8 C9 Pd1 1.7(5) . . . . ? C6 C8 C9 Pd1 -177.5(3) . . . . ? C20 C9 C10 C14 -1.8(6) . . . . ? C8 C9 C10 C14 149.7(4) . . . . ? Pd1 C9 C10 C14 -99.6(4) . . . . ? C20 C9 C10 C11 -176.1(4) . . . . ? C8 C9 C10 C11 -24.6(6) . . . . ? Pd1 C9 C10 C11 86.1(4) . . . . ? C14 C10 C11 C12 63.1(5) . . . . ? C9 C10 C11 C12 -122.6(4) . . . . ? C14 C10 C11 C13 -61.7(5) . . . . ? C9 C10 C11 C13 112.6(5) . . . . ? C9 C10 C14 C15 -1.3(6) . . . . ? C11 C10 C14 C15 173.2(4) . . . . ? C10 C14 C15 C19 4.2(6) . . . . ? C10 C14 C15 C16 -173.6(4) . . . . ? C19 C15 C16 C17 121.3(5) . . . . ? C14 C15 C16 C17 -61.1(6) . . . . ? C19 C15 C16 C18 -113.8(5) . . . . ? C14 C15 C16 C18 63.9(5) . . . . ? C14 C15 C19 C20 -4.0(6) . . . . ? C16 C15 C19 C20 173.7(4) . . . . ? C15 C19 C20 C9 1.0(6) . . . . ? C15 C19 C20 C21 -176.2(4) . . . . ? C10 C9 C20 C19 2.0(6) . . . . ? C8 C9 C20 C19 -149.5(4) . . . . ? Pd1 C9 C20 C19 96.3(4) . . . . ? C10 C9 C20 C21 179.1(4) . . . . ? C8 C9 C20 C21 27.7(6) . . . . ? Pd1 C9 C20 C21 -86.6(4) . . . . ? C19 C20 C21 C23 70.7(5) . . . . ? C9 C20 C21 C23 -106.5(5) . . . . ? C19 C20 C21 C22 -54.2(6) . . . . ? C9 C20 C21 C22 128.6(4) . . . . ? C29 C24 C25 C26 -54.5(5) . . . . ? C30 C24 C25 C26 66.3(5) . . . . ? P1 C24 C25 C26 -173.5(3) . . . . ? C24 C25 C26 C27 57.6(6) . . . . ? C25 C26 C27 C28 -56.4(6) . . . . ? C26 C27 C28 C29 55.9(6) . . . . ? C27 C28 C29 C24 -56.4(6) . . . . ? C30 C24 C29 C28 -67.1(5) . . . . ? C25 C24 C29 C28 53.7(5) . . . . ? P1 C24 C29 C28 171.9(3) . . . . ? C29 C24 C30 C31 179.0(4) . . . . ? C25 C24 C30 C31 60.6(5) . . . . ? P1 C24 C30 C31 -59.5(5) . . . . ? C32 O3 C31 O4 -33.3(5) . . . . ? C32 O3 C31 C30 -147.2(4) . . . . ? C32 O3 C31 C34 86.1(5) . . . . ? C33 O4 C31 O3 29.4(5) . . . . ? C33 O4 C31 C30 144.5(4) . . . . ? C33 O4 C31 C34 -89.1(5) . . . . ? C24 C30 C31 O3 -87.4(5) . . . . ? C24 C30 C31 O4 160.6(4) . . . . ? C24 C30 C31 C34 36.4(6) . . . . ? C31 O3 C32 C33 24.1(5) . . . . ? C31 O4 C33 C32 -14.6(6) . . . . ? O3 C32 C33 O4 -5.8(6) . . . . ? O3 C31 C34 C35 160.6(4) . . . . ? O4 C31 C34 C35 -84.5(5) . . . . ? C30 C31 C34 C35 37.5(6) . . . . ? C31 C34 C35 C40 57.4(5) . . . . ? C31 C34 C35 C36 176.2(4) . . . . ? C31 C34 C35 P1 -70.7(4) . . . . ? C34 C35 C36 C37 -65.3(5) . . . . ? C40 C35 C36 C37 57.5(5) . . . . ? P1 C35 C36 C37 -177.2(3) . . . . ? C35 C36 C37 C38 -58.5(5) . . . . ? C36 C37 C38 C39 53.9(6) . . . . ? C37 C38 C39 C40 -54.6(6) . . . . ? C38 C39 C40 C35 57.3(5) . . . . ? C34 C35 C40 C39 67.8(5) . . . . ? C36 C35 C40 C39 -55.5(5) . . . . ? P1 C35 C40 C39 -172.4(3) . . . . ? C47 C41 C42 C43 -4.2(6) . . . . ? Pd1 C41 C42 C43 -179.3(3) . . . . ? C41 C42 C43 C44 3.3(7) . . . . ? C42 C43 C44 C46 -0.6(7) . . . . ? C42 C43 C44 C45 174.8(4) . . . . ? C43 C44 C46 C47 -1.0(7) . . . . ? C45 C44 C46 C47 -176.3(5) . . . . ? C44 C46 C47 C41 -0.2(8) . . . . ? C42 C41 C47 C46 2.7(7) . . . . ? Pd1 C41 C47 C46 178.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 Br1 0.95 2.79 3.699(5) 160.3 1_545 C25 H25B O3 0.99 2.53 3.108(6) 116.9 . C29 H29A O1 0.99 2.32 3.105(6) 135.9 . C30 H30A O1 0.99 2.22 3.040(6) 139.6 . C40 H40B O1 0.99 2.38 2.881(6) 110.4 . C40 H40B O4 0.99 2.55 3.134(6) 117.9 . _refine_diff_density_max 0.935 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.121 _shelx_res_file ; TITL XRAY5726_0m_a.res in P2(1)/c XRAY5726_0m_a.res created by SHELXL-2016/6 at 11:57:41 on 10-Oct-2018 CELL 0.71073 13.1258 11.4725 28.9287 90.000 91.981 90.000 ZERR 4.000 0.0091 0.0080 0.0202 0.000 0.010 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O P Br Pd UNIT 188 252 4 16 4 4 4 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.020 0.050 0.200 EQIV $1 x, y-1, z HTAB C4 Br1_$1 HTAB C25 O3 HTAB C29 O1 HTAB C30 O1 HTAB C40 O1 HTAB C40 O4 WPDB CONF TEMP -173.0 WGHT 0.000000 FVAR 0.16073 PD1 7 0.371556 0.339063 0.375772 11.00000 0.02153 0.01147 = 0.02176 0.00088 -0.00024 0.00181 BR1 6 0.454282 0.530854 0.375075 11.00000 0.02718 0.01186 = 0.07991 0.00260 -0.00792 0.00104 P1 5 0.286826 0.162303 0.364092 11.00000 0.01845 0.01181 = 0.02187 -0.00027 0.00104 0.00290 O1 4 0.272536 -0.103173 0.353615 11.00000 0.02774 0.00978 = 0.05029 -0.00226 0.00426 -0.00556 O2 4 0.664815 0.052985 0.384663 11.00000 0.01949 0.02268 = 0.03424 -0.00159 -0.00228 0.00968 O3 4 -0.037184 0.190205 0.360358 11.00000 0.01927 0.03288 = 0.03956 -0.01195 -0.00031 0.00546 O4 4 -0.008460 0.044976 0.309680 11.00000 0.02087 0.03213 = 0.05028 -0.01784 -0.01047 0.00398 N1 3 -0.063243 0.743676 0.396060 11.00000 0.04194 0.04076 = 0.06227 -0.00779 0.01150 0.01242 C1 1 0.388842 0.052168 0.365411 11.00000 0.01650 0.01973 = 0.01908 0.00453 0.00381 0.00117 C2 1 0.370683 -0.070673 0.360691 11.00000 0.03211 0.00798 = 0.02592 -0.00200 0.00743 -0.00255 C3 1 0.251016 -0.221665 0.344661 11.00000 0.04090 0.01471 = 0.06112 -0.00619 0.00119 -0.00890 AFIX 137 H3A 2 0.293207 -0.249341 0.319610 11.00000 -1.50000 H3B 2 0.178826 -0.230368 0.335522 11.00000 -1.50000 H3C 2 0.266064 -0.267607 0.372629 11.00000 -1.50000 AFIX 0 C4 1 0.449438 -0.147823 0.364834 11.00000 0.02773 0.01392 = 0.02369 0.00441 0.00463 0.00777 AFIX 43 H4 2 0.435814 -0.228923 0.362208 11.00000 -1.20000 AFIX 0 C5 1 0.549359 -0.110438 0.372826 11.00000 0.02579 0.02328 = 0.01737 0.00277 0.00357 0.01444 AFIX 43 H5 2 0.603481 -0.165294 0.375358 11.00000 -1.20000 AFIX 0 C6 1 0.568828 0.007601 0.377032 11.00000 0.01890 0.02118 = 0.02162 -0.00172 0.00484 0.00318 C7 1 0.746479 -0.027582 0.391860 11.00000 0.02056 0.04024 = 0.04366 -0.00509 -0.00306 0.01397 AFIX 137 H7A 2 0.729933 -0.081686 0.416719 11.00000 -1.50000 H7B 2 0.809019 0.014968 0.400497 11.00000 -1.50000 H7C 2 0.756638 -0.071426 0.363313 11.00000 -1.50000 AFIX 0 C8 1 0.489111 0.089349 0.373493 11.00000 0.02527 0.01322 = 0.01594 -0.00016 0.00715 0.00019 C9 1 0.523571 0.212990 0.379807 11.00000 0.01193 0.01098 = 0.02298 0.00600 0.00141 0.00587 C10 1 0.547057 0.251484 0.425942 11.00000 0.01610 0.01236 = 0.02272 0.00291 0.00428 0.00408 C11 1 0.500548 0.193415 0.467502 11.00000 0.02211 0.01843 = 0.01687 0.00207 0.00633 -0.00021 AFIX 13 H11 2 0.450575 0.134017 0.455468 11.00000 -1.20000 AFIX 0 C12 1 0.442679 0.278996 0.496598 11.00000 0.03434 0.03944 = 0.01929 0.00541 0.00884 0.00460 AFIX 137 H12A 2 0.490554 0.334807 0.511002 11.00000 -1.50000 H12B 2 0.407339 0.236664 0.520721 11.00000 -1.50000 H12C 2 0.392696 0.320895 0.476898 11.00000 -1.50000 AFIX 0 C13 1 0.581430 0.129132 0.496870 11.00000 0.03236 0.02562 = 0.02453 0.00862 0.00398 0.00603 AFIX 137 H13A 2 0.615056 0.071031 0.477796 11.00000 -1.50000 H13B 2 0.549062 0.090069 0.522672 11.00000 -1.50000 H13C 2 0.632096 0.185029 0.508995 11.00000 -1.50000 AFIX 0 C14 1 0.620325 0.336576 0.433170 11.00000 0.02678 0.02078 = 0.01518 0.00012 -0.00053 0.00677 AFIX 43 H14 2 0.634742 0.363120 0.463807 11.00000 -1.20000 AFIX 0 C15 1 0.673969 0.384949 0.396947 11.00000 0.01688 0.01373 = 0.02680 0.00043 0.00125 0.00110 C16 1 0.760847 0.468361 0.407323 11.00000 0.02481 0.02660 = 0.02634 0.00060 0.00658 0.00243 AFIX 13 H16 2 0.787875 0.493911 0.377054 11.00000 -1.20000 AFIX 0 C17 1 0.726120 0.576359 0.432286 11.00000 0.04008 0.03066 = 0.04790 -0.01507 0.00806 -0.00458 AFIX 137 H17A 2 0.671351 0.614294 0.413978 11.00000 -1.50000 H17B 2 0.783574 0.630324 0.436480 11.00000 -1.50000 H17C 2 0.700933 0.554442 0.462577 11.00000 -1.50000 AFIX 0 C18 1 0.847393 0.407906 0.434200 11.00000 0.02965 0.03687 = 0.03239 0.00024 -0.00191 -0.00131 AFIX 137 H18A 2 0.821700 0.375411 0.462879 11.00000 -1.50000 H18B 2 0.901488 0.464418 0.441653 11.00000 -1.50000 H18C 2 0.874735 0.344951 0.415379 11.00000 -1.50000 AFIX 0 C19 1 0.647437 0.350969 0.352239 11.00000 0.02193 0.01495 = 0.01930 0.00769 0.00443 0.00146 AFIX 43 H19 2 0.680433 0.387090 0.327274 11.00000 -1.20000 AFIX 0 C20 1 0.574710 0.266422 0.342520 11.00000 0.01374 0.01580 = 0.01979 0.00476 0.00187 0.00356 C21 1 0.554011 0.228000 0.292929 11.00000 0.02287 0.02933 = 0.01744 0.00215 0.00059 -0.00359 AFIX 13 H21 2 0.492566 0.176446 0.292723 11.00000 -1.20000 AFIX 0 C22 1 0.528543 0.331582 0.261055 11.00000 0.03761 0.04549 = 0.01966 0.01406 -0.00135 -0.01320 AFIX 137 H22A 2 0.474052 0.378008 0.274273 11.00000 -1.50000 H22B 2 0.505958 0.302733 0.230504 11.00000 -1.50000 H22C 2 0.589349 0.380181 0.258023 11.00000 -1.50000 AFIX 0 C23 1 0.641173 0.156808 0.273578 11.00000 0.03237 0.04930 = 0.02290 -0.00094 0.00470 -0.00068 AFIX 137 H23A 2 0.702344 0.205531 0.272341 11.00000 -1.50000 H23B 2 0.621825 0.129787 0.242358 11.00000 -1.50000 H23C 2 0.655267 0.089434 0.293620 11.00000 -1.50000 AFIX 0 C24 1 0.184044 0.115957 0.405721 11.00000 0.01743 0.01999 = 0.02585 0.00119 0.00294 -0.00110 C25 1 0.144395 0.225413 0.430793 11.00000 0.02181 0.02143 = 0.02725 -0.00059 -0.00095 0.00535 AFIX 23 H25A 2 0.203351 0.268635 0.444470 11.00000 -1.20000 H25B 2 0.109820 0.276983 0.407732 11.00000 -1.20000 AFIX 0 C26 1 0.070590 0.197888 0.468856 11.00000 0.02530 0.03497 = 0.03768 -0.00265 0.01225 0.00204 AFIX 23 H26A 2 0.049820 0.271124 0.483986 11.00000 -1.20000 H26B 2 0.008671 0.160345 0.455191 11.00000 -1.20000 AFIX 0 C27 1 0.120226 0.117574 0.504423 11.00000 0.02609 0.04351 = 0.02910 0.00559 0.01233 -0.00111 AFIX 23 H27A 2 0.178419 0.157999 0.520094 11.00000 -1.20000 H27B 2 0.070435 0.097418 0.528085 11.00000 -1.20000 AFIX 0 C28 1 0.157547 0.007035 0.481828 11.00000 0.02493 0.02886 = 0.04390 0.01404 0.00785 -0.00129 AFIX 23 H28A 2 0.098469 -0.037459 0.468981 11.00000 -1.20000 H28B 2 0.193186 -0.042201 0.505381 11.00000 -1.20000 AFIX 0 C29 1 0.229858 0.034926 0.443222 11.00000 0.02205 0.02490 = 0.02979 0.00551 0.00209 0.00180 AFIX 23 H29A 2 0.250547 -0.038933 0.428540 11.00000 -1.20000 H29B 2 0.292032 0.071813 0.456936 11.00000 -1.20000 AFIX 0 C30 1 0.095999 0.054220 0.377992 11.00000 0.01371 0.02299 = 0.04012 -0.00038 0.00191 -0.00542 AFIX 23 H30A 2 0.123738 -0.016920 0.363696 11.00000 -1.20000 H30B 2 0.044351 0.029063 0.400053 11.00000 -1.20000 AFIX 0 C31 1 0.043195 0.125511 0.340530 11.00000 0.01703 0.02606 = 0.03664 -0.01168 0.00064 0.00044 C32 1 -0.115687 0.199825 0.326212 11.00000 0.02080 0.04673 = 0.03893 -0.00410 -0.00249 0.00820 AFIX 23 H32A 2 -0.110654 0.274418 0.309236 11.00000 -1.20000 H32B 2 -0.183414 0.195232 0.340138 11.00000 -1.20000 AFIX 0 C33 1 -0.099057 0.097141 0.294328 11.00000 0.03491 0.05500 = 0.04385 -0.01769 0.00177 0.00614 AFIX 23 H33A 2 -0.156353 0.041309 0.295852 11.00000 -1.20000 H33B 2 -0.093888 0.123939 0.261964 11.00000 -1.20000 AFIX 0 C34 1 0.112115 0.206783 0.314502 11.00000 0.02528 0.01617 = 0.02968 -0.00549 -0.00437 0.00299 AFIX 23 H34A 2 0.119322 0.280027 0.332412 11.00000 -1.20000 H34B 2 0.077415 0.226448 0.284585 11.00000 -1.20000 AFIX 0 C35 1 0.219487 0.162072 0.304558 11.00000 0.02784 0.01513 = 0.02245 -0.00720 0.00106 0.00250 C36 1 0.281212 0.248164 0.275095 11.00000 0.02448 0.02262 = 0.02001 -0.00250 -0.00383 0.00409 AFIX 23 H36A 2 0.284365 0.324417 0.291102 11.00000 -1.20000 H36B 2 0.351858 0.218717 0.273280 11.00000 -1.20000 AFIX 0 C37 1 0.237729 0.266691 0.226138 11.00000 0.04320 0.03074 = 0.02376 0.00083 0.00144 0.01039 AFIX 23 H37A 2 0.168749 0.301204 0.227380 11.00000 -1.20000 H37B 2 0.281611 0.321603 0.209478 11.00000 -1.20000 AFIX 0 C38 1 0.231944 0.151683 0.200466 11.00000 0.04933 0.03754 = 0.02253 -0.01276 -0.00610 0.01293 AFIX 23 H38A 2 0.301706 0.122469 0.195544 11.00000 -1.20000 H38B 2 0.197705 0.163425 0.169790 11.00000 -1.20000 AFIX 0 C39 1 0.173316 0.062454 0.227696 11.00000 0.03275 0.02742 = 0.03619 -0.01410 -0.00705 0.00956 AFIX 23 H39A 2 0.174883 -0.013385 0.211408 11.00000 -1.20000 H39B 2 0.101238 0.087330 0.228923 11.00000 -1.20000 AFIX 0 C40 1 0.216648 0.046648 0.276933 11.00000 0.02674 0.01985 = 0.03341 -0.00744 -0.00170 0.00394 AFIX 23 H40A 2 0.286642 0.014905 0.275731 11.00000 -1.20000 H40B 2 0.174509 -0.010756 0.293235 11.00000 -1.20000 AFIX 0 C41 1 0.247678 0.442029 0.378996 11.00000 0.01776 0.00821 = 0.02237 0.00074 0.00201 -0.00041 C42 1 0.188186 0.479898 0.340880 11.00000 0.02411 0.01645 = 0.02537 -0.00521 0.00223 0.00116 AFIX 43 H42 2 0.205302 0.455856 0.310697 11.00000 -1.20000 AFIX 0 C43 1 0.104646 0.551926 0.346362 11.00000 0.02556 0.01857 = 0.03055 0.00232 -0.00715 -0.00336 AFIX 43 H43 2 0.063153 0.573334 0.320171 11.00000 -1.20000 AFIX 0 C44 1 0.081282 0.592884 0.389787 11.00000 0.02473 0.01900 = 0.03468 -0.00111 0.00737 0.00387 C45 1 -0.001045 0.675717 0.394038 11.00000 0.03073 0.03013 = 0.04123 0.00170 0.01133 0.00377 C46 1 0.141438 0.560372 0.427498 11.00000 0.04548 0.02859 = 0.02049 -0.00161 0.00774 0.00584 AFIX 43 H46 2 0.126602 0.588988 0.457338 11.00000 -1.20000 AFIX 0 C47 1 0.223118 0.486527 0.422261 11.00000 0.04359 0.02429 = 0.02107 -0.00143 -0.00013 0.00698 AFIX 43 H47 2 0.263808 0.465287 0.448726 11.00000 -1.20000 AFIX 0 HKLF 4 REM XRAY5726_0m_a.res in P2(1)/c REM R1 = 0.0553 for 5928 Fo > 4sig(Fo) and 0.1130 for all 9496 data REM 504 parameters refined using 0 restraints END WGHT 0.0259 0.0000 REM Highest difference peak 0.935, deepest hole -1.196, 1-sigma level 0.121 Q1 1 0.4280 0.5329 0.4067 11.00000 0.05 0.94 Q2 1 -0.0074 0.2979 0.1996 11.00000 0.05 0.84 Q3 1 0.3582 0.5230 0.3856 11.00000 0.05 0.81 Q4 1 0.4656 0.3397 0.3610 11.00000 0.05 0.80 Q5 1 0.3520 0.3463 0.4030 11.00000 0.05 0.79 Q6 1 0.4010 0.3505 0.3502 11.00000 0.05 0.75 Q7 1 0.3260 0.2325 0.3673 11.00000 0.05 0.73 Q8 1 0.3385 0.4529 0.3654 11.00000 0.05 0.71 Q9 1 0.4123 0.2267 0.3811 11.00000 0.05 0.70 Q10 1 0.2762 0.3476 0.3908 11.00000 0.05 0.64 Q11 1 0.2992 0.3344 0.3425 11.00000 0.05 0.59 Q12 1 0.4176 0.4369 0.3863 11.00000 0.05 0.59 Q13 1 0.4405 0.3440 0.4105 11.00000 0.05 0.59 Q14 1 0.4839 0.4154 0.3717 11.00000 0.05 0.55 Q15 1 0.3407 0.0772 0.3562 11.00000 0.05 0.55 Q16 1 0.3791 0.2384 0.3489 11.00000 0.05 0.55 Q17 1 0.8404 0.4563 0.3931 11.00000 0.05 0.55 Q18 1 -0.1070 0.0372 0.3234 11.00000 0.05 0.54 Q19 1 0.3831 0.1447 0.3653 11.00000 0.05 0.54 Q20 1 0.1998 0.1717 0.3821 11.00000 0.05 0.50 ; _shelx_res_checksum 45867 _shelx_hkl_file ; 1 0 0 1042.70 141.39 1 0 0 1014.20 141.29 -2 0 0 7.80 2.10 -2 0 0 8.80 3.60 2 0 0 16.20 5.00 2 0 0 13.20 3.20 -3 0 0 84.89 13.00 -3 0 0 89.89 14.70 3 0 0 92.59 15.30 3 0 0 101.89 13.80 4 0 0 9.50 4.90 -4 0 0 28.60 6.10 4 0 0 9.20 7.80 -4 0 0 11.50 3.20 -5 0 0 14.90 3.50 5 0 0 18.70 9.00 5 0 0 19.30 5.50 -5 0 0 16.80 6.60 6 0 0 101.69 19.70 -6 0 0 117.19 16.50 -6 0 0 111.99 19.40 6 0 0 121.09 18.10 -7 0 0 23.30 4.50 7 0 0 22.40 12.30 -7 0 0 20.60 8.20 7 0 0 21.60 7.20 -8 0 0 192.28 27.70 -8 0 0 214.08 31.60 8 0 0 232.68 33.70 8 0 0 176.88 29.40 -9 0 0 20.80 11.00 9 0 0 13.90 14.90 9 0 0 17.40 7.90 10 0 0 213.38 38.00 -10 0 0 226.88 36.70 -11 0 0 586.44 84.49 12 0 0 344.57 55.09 -12 0 0 332.67 53.09 -13 0 0 60.59 19.50 13 0 0 83.49 22.70 13 0 0 76.79 17.30 -14 0 0 -6.10 16.00 14 0 0 10.40 20.00 -15 0 0 66.79 21.00 15 0 0 58.59 23.20 -16 0 0 -4.00 16.60 16 0 0 36.90 20.70 0 -1 0 2.80 1.40 0 -1 0 2.10 1.70 0 1 0 -1.20 1.20 1 -1 0 724.53 103.09 1 -1 0 817.52 102.99 -1 -1 0 744.83 102.89 -1 -1 0 765.12 102.99 1 -1 0 688.03 102.99 -1 -1 0 766.12 103.09 -1 1 0 731.03 102.89 2 -1 0 56.79 7.20 2 -1 0 46.00 7.60 -2 -1 0 37.50 6.40 -2 -1 0 39.90 8.00 2 1 0 45.20 6.50 -2 1 0 33.60 7.00 2 1 0 45.30 8.50 -2 1 0 42.50 6.60 -3 -1 0 199.28 27.30 -3 -1 0 237.58 29.60 3 -1 0 154.58 28.40 3 1 0 172.18 27.60 -3 1 0 215.78 28.10 -3 1 0 204.88 27.30 -4 -1 0 120.89 21.80 4 -1 0 129.19 20.30 4 -1 0 169.78 21.70 -4 -1 0 134.09 18.90 -4 1 0 111.69 18.80 -4 1 0 131.89 20.20 4 1 0 171.88 21.80 5 -1 0 108.09 19.00 -5 -1 0 106.39 16.70 5 -1 0 125.59 18.50 -5 1 0 126.09 16.60 -5 1 0 101.89 18.30 5 1 0 134.89 19.80 6 -1 0 411.46 60.09 6 -1 0 456.45 59.09 -6 -1 0 425.76 58.19 -6 -1 0 440.76 60.49 -6 1 0 392.36 58.09 -6 1 0 415.16 59.39 7 -1 0 276.17 37.50 -7 -1 0 274.17 39.30 -7 -1 0 273.87 36.30 7 -1 0 248.48 39.60 7 1 0 233.28 40.30 -7 1 0 263.67 38.40 -7 1 0 243.68 36.10 8 -1 0 35.10 14.20 -8 -1 0 18.60 4.70 8 -1 0 9.90 7.30 -8 -1 0 26.90 11.20 8 1 0 32.50 7.80 -8 1 0 27.70 4.80 -8 1 0 25.20 8.80 8 1 0 30.20 14.00 -9 -1 0 7.50 10.90 9 -1 0 -5.30 14.70 9 -1 0 0.40 7.80 -9 1 0 14.60 9.50 9 1 0 -12.90 14.20 9 1 0 1.40 7.80 -10 -1 0 197.48 29.70 10 -1 0 181.08 28.60 10 1 0 136.29 32.60 -10 1 0 186.98 28.80 10 1 0 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-2 0 536.05 72.69 -3 2 0 523.85 71.89 -3 2 0 534.75 72.49 4 -2 0 101.89 17.30 -4 -2 0 110.79 18.30 -4 -2 0 98.49 15.70 4 -2 0 119.09 17.20 4 2 0 120.59 18.10 -4 2 0 97.99 15.40 -4 2 0 109.89 16.90 -5 -2 0 31.00 9.20 5 -2 0 0.90 8.60 -5 -2 0 39.70 5.70 5 -2 0 22.80 7.70 5 2 0 32.00 10.80 5 2 0 43.30 6.10 -5 2 0 25.10 7.10 -6 -2 0 -12.40 9.10 6 -2 0 -1.60 6.20 6 -2 0 3.70 9.10 -6 -2 0 4.40 3.30 6 2 0 -19.10 9.70 -6 2 0 -4.50 5.00 6 2 0 2.00 4.10 -6 2 0 -3.70 3.60 7 -2 0 49.99 9.80 -7 -2 0 36.20 11.60 -7 -2 0 41.00 6.90 7 -2 0 40.50 12.10 -7 2 0 35.50 6.70 7 2 0 47.30 8.00 7 2 0 22.20 13.00 -7 2 0 39.20 9.20 -8 -2 0 118.09 18.00 -8 -2 0 94.29 14.20 8 -2 0 81.49 15.60 8 2 0 57.09 19.30 -8 2 0 91.49 13.90 -8 2 0 86.39 16.10 8 2 0 104.99 14.90 9 -2 0 287.07 35.50 -9 -2 0 260.17 37.60 9 -2 0 198.48 37.40 9 2 0 212.88 33.90 -9 2 0 245.88 36.40 9 2 0 204.48 38.30 10 -2 0 43.40 16.40 10 -2 0 59.39 11.20 -10 -2 0 15.40 13.20 10 2 0 37.80 19.50 10 2 0 35.80 8.90 -10 2 0 15.40 11.30 11 -2 0 4.40 14.90 11 -2 0 9.00 10.30 -11 -2 0 3.60 14.40 11 2 0 6.20 7.80 11 2 0 5.50 19.00 -11 2 0 9.20 10.90 12 -2 0 20.10 12.40 12 -2 0 20.80 16.50 -12 -2 0 21.30 17.20 12 2 0 9.50 20.40 -12 2 0 40.30 13.90 13 -2 0 22.30 17.80 -13 -2 0 24.60 18.50 13 -2 0 13.70 13.10 -13 2 0 8.70 14.20 13 2 0 18.90 23.00 14 -2 0 23.40 16.30 14 -2 0 42.00 21.00 -14 -2 0 58.79 20.60 14 2 0 69.99 23.90 -14 2 0 47.50 18.60 15 -2 0 40.60 17.20 15 -2 0 25.30 22.20 -15 -2 0 16.60 19.60 15 2 0 25.30 20.00 -15 2 0 -5.30 18.50 16 -2 0 26.30 23.10 -16 -2 0 1.70 19.20 16 2 0 10.40 22.70 -16 2 0 20.10 19.00 0 -3 0 2.30 5.00 0 -3 0 3.30 4.20 0 3 0 11.30 4.10 0 3 0 5.50 3.70 1 -3 0 35.00 7.60 -1 -3 0 46.80 7.00 1 -3 0 41.50 7.80 -1 -3 0 26.90 7.40 1 3 0 37.20 6.70 1 3 0 47.90 8.40 -1 3 0 33.90 6.50 -2 -3 0 2.10 3.50 2 -3 0 -1.50 5.30 2 -3 0 5.20 5.10 -2 -3 0 -1.30 4.90 2 3 0 -1.90 3.60 -2 3 0 9.30 3.50 2 3 0 14.70 7.30 3 -3 0 261.97 44.20 3 -3 0 397.96 45.10 -3 -3 0 324.47 45.20 3 -3 0 327.87 45.20 -3 -3 0 336.57 44.10 -3 3 0 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0 38.10 12.00 -11 -3 0 20.00 15.40 11 -3 0 43.20 16.10 11 3 0 24.20 20.20 -11 3 0 29.30 12.00 12 -3 0 30.20 16.20 -12 -3 0 -0.30 15.40 12 -3 0 4.00 12.30 12 3 0 0.70 22.20 -12 3 0 -14.70 11.40 13 -3 0 18.40 17.20 -13 -3 0 -4.70 16.80 13 -3 0 10.50 14.00 -13 3 0 15.90 14.30 13 3 0 -7.90 23.00 -14 -3 0 7.80 16.80 14 -3 0 -3.60 14.60 14 -3 0 50.99 19.80 -14 3 0 -11.50 16.30 14 3 0 6.50 20.60 -15 -3 0 11.70 18.40 15 -3 0 16.10 17.40 15 3 0 16.00 23.50 -15 3 0 -3.80 17.30 -16 -3 0 41.80 20.00 16 -3 0 39.20 19.50 16 3 0 41.40 24.10 -16 3 0 -7.30 19.10 0 -4 0 1.70 4.60 0 -4 0 -1.40 5.20 0 4 0 4.00 3.90 0 4 0 7.20 4.80 1 -4 0 19.00 6.50 -1 -4 0 19.80 6.50 1 -4 0 27.90 7.00 -1 -4 0 23.90 6.00 1 4 0 19.40 5.40 -1 4 0 22.50 5.50 1 4 0 48.40 7.70 2 -4 0 99.49 15.20 -2 -4 0 84.49 13.80 -2 -4 0 62.59 12.70 2 -4 0 86.79 13.80 -2 4 0 94.19 13.20 2 4 0 99.99 15.60 2 4 0 93.69 13.50 3 -4 0 824.82 116.39 3 -4 0 764.12 116.99 3 -4 0 895.11 117.49 -3 -4 0 860.81 117.29 -3 -4 0 783.32 116.49 -3 4 0 886.21 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1.70 8.00 3 9 -4 1.60 7.20 -2 -9 4 46.50 12.60 2 -9 -4 36.80 12.30 2 -9 -4 27.40 12.80 -2 9 4 45.40 10.50 2 9 -4 39.80 9.80 1 -9 -4 2.90 8.80 -1 -9 4 9.00 9.60 1 -9 -4 4.50 9.90 -1 -9 4 -3.30 8.00 1 9 -4 2.00 6.90 -1 9 4 7.60 7.60 0 -9 -4 -8.40 8.90 0 -9 4 -7.60 8.70 0 -9 4 1.60 8.20 0 -9 -4 3.60 8.60 0 9 4 3.00 7.50 0 9 -4 2.80 7.00 -1 -9 -4 4.60 8.20 1 -9 4 1.80 8.40 1 -9 4 7.20 9.30 -1 -9 -4 1.30 9.70 -1 9 -4 -1.10 6.90 1 9 4 12.00 7.90 -2 -9 -4 -1.60 10.30 2 -9 4 -6.00 9.00 -2 -9 -4 12.40 7.60 2 -9 4 2.70 9.60 -2 9 -4 -6.20 6.70 2 9 4 -5.20 7.30 -3 -9 -4 33.70 12.20 3 -9 4 24.30 10.90 3 -9 4 45.10 12.10 -3 -9 -4 22.50 8.70 -3 9 -4 22.00 8.90 3 9 4 21.50 9.10 4 -9 4 159.38 27.90 -4 -9 -4 177.68 28.60 4 -9 4 151.98 27.60 -4 -9 -4 208.28 29.20 4 9 4 165.38 26.20 -4 9 -4 167.48 25.90 -5 -9 -4 173.28 28.80 5 -9 4 156.98 28.70 5 -9 4 195.18 29.20 5 9 4 157.38 26.40 -5 9 -4 170.08 26.20 5 9 4 180.08 30.30 -6 -9 -4 200.08 31.70 6 -9 4 148.59 30.60 6 -9 4 246.28 32.00 6 9 4 168.58 28.40 6 9 4 221.08 33.40 -6 9 -4 173.18 28.10 7 -9 4 132.89 22.30 -7 -9 -4 122.29 21.90 7 9 4 109.39 24.10 7 9 4 85.59 17.10 -7 9 -4 77.69 16.50 -7 9 -4 92.49 18.70 8 -9 4 160.38 25.40 -8 -9 -4 149.69 25.10 -8 9 -4 100.99 22.10 8 9 4 111.79 20.50 8 9 4 119.79 27.40 9 -9 4 5.40 14.30 -9 -9 -4 4.50 16.10 -9 9 -4 12.20 10.90 9 9 4 -3.20 19.00 10 -9 4 49.90 16.50 -10 -9 -4 42.00 18.80 -10 9 -4 23.30 13.40 10 9 4 38.40 21.60 -11 -9 -4 6.70 18.70 11 -9 4 -18.30 14.90 -11 9 -4 11.10 12.00 11 9 4 34.70 21.60 -12 -9 -4 8.50 19.40 12 -9 4 25.20 17.50 12 9 4 40.00 21.90 -12 9 -4 12.80 13.10 13 -9 4 20.50 20.20 13 9 4 24.90 22.10 12 -10 -4 60.29 21.60 -12 -10 4 58.99 19.80 12 10 -4 -5.10 22.30 -12 10 4 49.80 16.40 11 -10 -4 100.39 20.80 -11 -10 4 54.79 19.20 11 10 -4 -12.00 20.10 -11 10 4 39.50 15.40 -10 -10 4 12.00 16.10 10 -10 -4 25.40 16.60 10 10 -4 4.20 9.20 -10 10 4 7.30 12.10 10 10 -4 -19.70 20.50 9 -10 -4 -14.70 14.50 -9 -10 4 8.70 15.60 9 10 -4 -13.70 20.30 -9 10 4 4.30 11.00 9 10 -4 10.10 9.20 -8 -10 4 71.79 18.70 8 -10 -4 52.69 17.80 -8 10 4 60.89 14.80 -8 10 4 61.99 15.40 8 10 -4 29.90 21.20 8 10 -4 58.09 13.10 7 -10 -4 39.50 15.30 -7 -10 4 36.00 15.30 -7 10 4 10.90 10.40 -7 10 4 32.40 10.80 7 10 -4 17.80 9.70 7 10 -4 5.60 18.00 6 -10 -4 -4.40 12.70 -6 -10 4 6.70 13.10 6 -10 -4 -3.10 11.80 -6 10 4 -25.70 8.90 6 10 -4 2.50 8.30 -5 -10 4 7.90 12.80 5 -10 -4 -12.20 11.70 5 -10 -4 5.90 12.60 -5 10 4 -21.90 8.70 5 10 -4 8.20 8.40 -4 -10 4 158.38 28.90 4 -10 -4 149.29 28.80 4 -10 -4 228.38 29.20 -4 10 4 149.29 26.50 4 10 -4 180.38 26.80 3 -10 -4 37.70 14.20 3 -10 -4 45.80 13.40 -3 -10 4 30.50 14.10 -3 10 4 42.40 11.90 3 10 -4 53.39 11.30 -2 -10 4 10.90 11.20 2 -10 -4 -6.60 10.60 2 -10 -4 4.70 11.50 2 10 -4 -5.90 7.60 -2 10 4 9.30 9.10 -1 -10 4 131.49 25.70 1 -10 -4 202.98 26.10 1 -10 -4 135.39 26.00 1 10 -4 136.09 23.50 -1 10 4 165.28 24.30 0 -10 4 243.58 41.70 0 -10 4 262.37 43.00 0 -10 -4 257.37 41.80 0 10 -4 270.17 40.10 0 10 4 297.27 40.20 1 -10 4 144.39 19.70 -1 -10 -4 81.79 20.90 1 -10 4 100.49 20.90 -1 -10 -4 107.69 18.60 1 10 4 117.69 18.90 -1 10 -4 99.49 18.30 2 -10 4 17.10 11.90 -2 -10 -4 6.10 11.90 2 -10 4 12.30 10.60 -2 -10 -4 8.00 8.40 -2 10 -4 2.50 8.00 2 10 4 7.20 8.80 3 -10 4 135.49 19.20 -3 -10 -4 78.19 19.80 3 -10 4 79.39 18.80 3 10 4 71.79 16.50 -3 10 -4 95.29 16.40 -4 -10 -4 135.69 23.10 4 -10 4 85.59 21.10 4 -10 4 116.49 22.20 -4 10 -4 120.59 19.30 4 10 4 103.59 19.40 5 -10 4 14.60 13.70 5 -10 4 35.90 14.10 -5 -10 -4 5.20 14.00 5 10 4 20.30 9.40 -5 10 -4 -0.10 8.80 -6 -10 -4 -4.40 14.40 6 -10 4 31.60 15.10 6 -10 4 -13.10 13.10 6 10 4 1.30 9.20 -6 10 -4 -0.30 8.50 -7 -10 -4 36.10 16.60 7 -10 4 30.30 16.90 7 10 4 17.50 10.30 -7 10 -4 8.20 9.70 -7 10 -4 30.90 11.60 8 -10 4 47.60 17.40 -8 -10 -4 26.60 17.00 8 10 4 72.79 22.70 -8 10 -4 20.20 11.60 8 10 4 12.60 10.60 9 -10 4 6.90 16.20 -9 -10 -4 42.30 18.90 9 10 4 33.10 21.40 -9 10 -4 21.40 12.20 10 -10 4 42.00 17.00 -10 -10 -4 32.60 19.60 -10 10 -4 14.20 13.20 10 10 4 26.90 21.60 -11 -10 -4 135.79 28.10 11 -10 4 136.69 26.80 11 10 4 87.79 28.90 -11 10 -4 117.09 24.20 12 -10 4 17.70 18.60 12 10 4 39.60 22.80 11 -11 -4 18.80 19.40 -10 -11 4 132.29 25.70 10 -11 -4 101.29 25.30 10 11 -4 105.49 19.90 -10 11 4 94.39 22.30 -9 -11 4 61.19 20.70 9 -11 -4 114.19 21.50 9 11 -4 48.50 14.40 -9 11 4 65.39 17.10 8 -11 -4 39.30 16.40 -8 -11 4 17.80 16.40 -8 11 4 4.80 11.50 8 11 -4 13.80 9.70 -8 11 4 -5.70 12.30 -7 -11 4 10.70 15.50 7 -11 -4 -6.10 15.30 -7 11 4 7.90 11.10 -7 11 4 -11.10 11.30 7 11 -4 -13.20 8.50 6 -11 -4 25.10 15.50 -6 -11 4 5.90 15.50 6 -11 -4 -3.20 13.40 -6 11 4 -6.60 10.30 6 11 -4 3.80 9.00 5 -11 -4 -20.20 12.10 5 -11 -4 1.40 13.70 -5 -11 4 -14.70 14.10 -5 11 4 -2.40 9.70 5 11 -4 8.50 8.60 -4 -11 4 26.80 15.40 4 -11 -4 11.80 13.60 4 -11 -4 24.50 13.40 -4 11 4 -4.50 10.40 4 11 -4 30.80 10.10 3 -11 -4 136.49 25.00 3 -11 -4 161.38 25.50 -3 -11 4 153.78 26.80 -3 11 4 117.29 23.10 3 11 -4 125.39 22.80 2 -11 -4 380.16 58.29 -2 -11 4 410.66 59.89 2 -11 -4 393.76 59.59 2 11 -4 396.76 57.39 -2 11 4 391.66 58.19 -1 -11 4 196.78 30.90 1 -11 -4 198.48 29.20 1 -11 -4 184.88 30.30 1 11 -4 142.59 27.10 -1 11 4 152.88 27.60 0 -11 4 28.00 14.30 0 -11 -4 -1.10 12.40 0 -11 -4 -2.70 10.80 0 11 4 4.70 9.90 0 11 -4 -2.60 8.70 -1 -11 -4 217.58 33.90 1 -11 4 205.88 33.50 -1 11 -4 165.18 30.10 1 11 4 206.08 31.00 -2 -11 -4 172.38 28.90 2 -11 4 135.99 27.80 2 -11 4 184.18 26.70 2 11 4 137.19 24.90 -2 11 -4 151.38 25.10 3 -11 4 70.69 20.20 -3 -11 -4 149.79 23.90 3 -11 4 99.09 21.50 -3 11 -4 110.39 19.00 3 11 4 99.09 19.30 4 -11 4 48.20 15.00 -4 -11 -4 26.40 16.40 4 -11 4 15.50 13.80 4 11 4 11.10 10.20 -4 11 -4 20.00 10.30 5 -11 4 2.50 13.80 -5 -11 -4 23.80 15.20 5 -11 4 9.80 15.10 5 11 4 -4.30 9.80 -5 11 -4 7.80 10.30 6 -11 4 3.80 15.40 -6 -11 -4 1.40 16.50 6 -11 4 14.70 16.00 -6 11 -4 -9.60 9.70 6 11 4 1.70 9.70 -7 -11 -4 14.10 17.80 7 -11 4 -19.60 16.20 7 11 4 3.10 10.40 -7 11 -4 6.90 10.40 -7 11 -4 -10.30 9.70 -8 -11 -4 30.30 18.30 8 -11 4 7.10 17.10 -8 11 -4 -2.60 10.90 8 11 4 -2.00 10.60 -9 -11 -4 160.98 30.70 9 -11 4 171.28 29.70 -9 11 -4 128.99 27.00 10 -11 4 120.49 25.50 -10 -11 -4 103.19 26.40 -10 11 -4 95.59 21.50 9 -12 -4 89.99 22.40 -9 -12 4 61.39 22.40 9 12 -4 78.39 16.90 -9 12 4 72.89 18.50 8 -12 -4 90.09 20.00 -8 -12 4 62.59 20.70 -8 12 4 31.40 14.40 8 12 -4 29.00 12.50 -8 12 4 42.40 15.30 -7 -12 4 50.49 19.40 7 -12 -4 2.50 16.80 7 12 -4 33.00 12.40 -7 12 4 46.00 14.20 -7 12 4 37.00 14.90 6 -12 -4 -10.00 15.80 6 -12 -4 23.30 17.30 -6 -12 4 24.00 17.30 -6 12 4 -13.50 12.40 6 12 -4 3.20 10.10 5 -12 -4 26.50 16.10 -5 -12 4 53.29 18.90 5 -12 -4 38.50 16.50 -5 12 4 3.30 12.20 5 12 -4 13.60 10.80 4 -12 -4 125.09 21.00 -4 -12 4 84.69 22.70 4 -12 -4 93.89 22.00 4 12 -4 82.29 17.50 -4 12 4 73.99 18.80 3 -12 -4 152.68 28.00 3 -12 -4 179.68 29.60 -3 -12 4 142.59 29.70 -3 12 4 150.08 26.30 3 12 -4 162.78 25.80 2 -12 -4 43.70 15.90 2 -12 -4 40.90 14.10 -2 -12 4 -4.40 15.00 -2 12 4 -1.20 11.70 2 12 -4 -7.00 9.20 1 -12 -4 -7.30 14.30 1 -12 -4 6.30 12.80 -1 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52.99 17.50 -7 -13 4 22.60 19.20 7 -13 -4 19.10 17.50 -7 13 4 -7.60 13.40 -7 13 4 10.60 12.20 7 13 -4 10.90 11.50 6 -13 -4 21.20 17.80 6 -13 -4 31.30 18.00 -6 -13 4 33.80 20.50 -6 13 4 36.60 16.00 6 13 -4 47.10 13.20 5 -13 -4 84.49 22.80 5 -13 -4 98.69 22.60 -5 -13 4 103.09 24.40 -5 13 4 108.99 20.50 5 13 -4 72.39 18.50 4 -13 -4 28.40 18.00 -4 -13 4 35.80 18.80 4 -13 -4 23.70 17.00 -4 13 4 14.40 13.40 4 13 -4 32.90 12.50 3 -13 -4 8.80 14.00 3 -13 -4 6.80 15.60 -3 -13 4 -9.20 17.10 3 13 -4 -13.90 9.70 -3 13 4 -6.90 11.70 2 -13 -4 20.60 15.30 -2 -13 4 37.90 18.20 2 -13 -4 -10.80 13.00 -2 13 4 -1.90 11.80 2 13 -4 -11.50 10.20 1 -13 -4 42.30 18.60 -1 -13 4 49.70 19.20 1 13 -4 15.10 11.60 -1 13 4 14.80 13.30 0 -13 -4 5.90 17.30 0 -13 4 17.80 16.20 0 13 -4 6.90 11.20 0 13 4 -6.30 12.00 -1 -13 -4 34.60 17.40 1 -13 4 4.00 16.60 -1 13 -4 26.40 12.20 1 13 4 -22.90 10.70 -2 -13 -4 8.30 18.00 2 -13 4 27.10 17.40 2 13 4 -10.10 11.00 -2 13 -4 11.70 12.00 -3 -13 -4 -12.00 17.30 3 -13 4 -8.00 15.90 -3 13 -4 -5.70 12.00 3 13 4 -16.70 11.20 4 -13 4 -1.20 17.00 -4 -13 -4 36.30 20.00 -4 13 -4 -2.30 12.10 4 13 4 -5.80 11.60 -5 -13 -4 75.79 22.60 5 -13 4 63.69 21.60 5 -13 4 87.49 21.90 -5 13 -4 58.89 16.70 5 13 4 55.69 16.60 6 -13 4 75.69 21.70 6 -13 4 114.39 23.40 -6 -13 -4 67.89 23.20 -6 13 -4 21.50 15.20 6 13 4 30.10 15.00 -7 -13 -4 -3.20 19.40 7 -13 4 38.00 19.40 7 -13 4 -5.50 17.00 -7 13 -4 8.50 11.80 7 13 4 5.50 12.10 -4 -14 4 9.80 19.90 4 -14 -4 -8.70 16.30 4 -14 -4 17.90 18.20 4 14 -4 -14.40 11.30 -4 14 4 10.60 13.80 3 -14 -4 -7.50 16.40 3 -14 -4 -5.90 17.10 -3 -14 4 10.30 19.10 3 14 -4 -7.60 12.40 -3 14 4 -1.10 13.50 -2 -14 4 9.00 18.90 2 -14 -4 5.20 16.30 -2 14 4 11.30 13.90 2 14 -4 9.30 12.50 -1 -14 4 39.40 19.10 1 -14 -4 60.59 20.00 -1 14 4 -2.10 13.60 1 14 -4 9.90 12.20 0 -14 -4 56.79 21.40 0 -14 4 35.20 20.50 0 14 4 52.59 16.40 0 14 -4 37.30 15.20 -1 -14 -4 24.10 19.50 1 -14 4 -0.60 16.80 -1 14 -4 4.40 12.30 1 14 4 -3.90 13.60 2 -14 4 35.10 19.00 -2 -14 -4 14.60 20.10 -2 14 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-28 93.59 18.50 -10 -1 -28 8.50 16.80 10 -1 28 39.70 22.60 10 1 28 20.80 22.90 -10 1 -28 55.79 17.40 11 -2 -28 -21.40 13.80 -11 -2 28 13.40 14.00 11 2 -28 14.70 16.30 -10 -2 28 25.60 14.20 10 -2 -28 7.90 14.00 -10 2 28 5.80 13.40 10 2 -28 6.40 14.20 9 -2 -28 12.30 13.40 -9 -2 28 9.10 13.30 9 2 -28 -9.90 13.50 -9 2 28 28.30 14.60 8 -2 -28 31.30 14.60 -8 -2 28 41.30 15.70 -8 2 28 41.80 15.20 8 2 -28 26.10 15.70 -7 -2 28 21.10 13.80 7 -2 -28 12.80 12.70 7 2 -28 -1.00 12.80 -7 2 28 21.50 13.90 6 -2 -28 10.50 10.00 -6 -2 28 12.80 13.10 6 -2 -28 -4.30 11.50 -6 2 28 15.50 12.30 6 2 -28 5.20 12.60 5 -2 -28 6.50 11.50 5 -2 -28 -3.30 9.80 -5 -2 28 12.60 11.80 5 2 -28 2.20 11.00 -5 2 28 12.10 12.60 4 -2 -28 32.90 13.30 4 -2 -28 45.50 13.40 -4 -2 28 37.20 13.50 -4 2 28 42.20 13.60 4 2 -28 49.30 14.70 3 -2 -28 82.89 19.40 3 -2 -28 122.69 19.70 -3 -2 28 109.79 19.30 -3 2 28 117.49 19.40 3 2 -28 81.29 19.90 -2 -2 28 60.29 14.40 2 -2 -28 43.20 14.00 -2 2 28 87.99 15.00 2 2 -28 39.90 14.40 -2 2 28 44.80 20.10 -1 -2 28 15.50 10.40 1 -2 -28 23.80 10.90 -1 -2 28 -2.20 17.10 1 2 -28 11.90 11.60 -1 2 28 14.30 10.30 1 2 -28 11.00 8.90 -1 2 28 -4.80 17.30 0 -2 -28 18.90 10.40 0 -2 28 5.70 16.80 0 -2 28 16.90 9.60 0 2 28 -25.30 16.60 0 2 28 2.30 9.50 0 2 -28 2.70 9.10 -1 -2 -28 4.20 10.10 1 -2 28 2.00 9.20 1 -2 28 0.90 15.70 1 2 28 -2.50 9.30 1 2 28 -7.40 16.30 -1 2 -28 8.30 9.50 -2 -2 -28 8.40 10.90 2 -2 28 20.90 9.40 2 -2 28 14.20 17.90 2 2 28 1.80 9.00 -2 2 -28 2.80 9.70 2 2 28 -6.90 17.20 3 -2 28 26.50 10.10 -3 -2 -28 16.40 11.40 3 -2 28 16.80 18.20 3 2 28 9.90 17.80 3 2 28 21.30 9.80 -3 2 -28 5.80 10.50 -4 -2 -28 23.30 12.10 4 -2 28 15.40 17.80 -4 2 -28 29.10 12.30 4 2 28 12.50 19.40 5 -2 28 10.10 18.20 -5 -2 -28 9.50 11.60 5 2 28 23.10 19.60 -5 2 -28 1.90 12.00 -6 -2 -28 -19.20 11.30 6 -2 28 -18.70 18.30 6 2 28 -5.50 19.40 -6 2 -28 17.10 12.60 -7 -2 -28 27.00 13.60 7 -2 28 -5.90 18.40 -7 2 -28 27.00 13.80 7 2 28 21.60 18.70 -8 -2 -28 15.70 14.40 8 -2 28 13.10 18.70 -8 2 -28 25.00 14.40 8 2 28 28.60 20.10 -9 -2 -28 31.50 16.10 9 -2 28 23.80 21.10 -9 2 -28 34.10 15.00 9 2 28 3.20 18.90 -10 -2 -28 22.00 15.40 10 -2 28 9.40 21.40 -10 2 -28 -9.50 14.10 10 2 28 25.00 22.00 -10 -3 28 -4.80 13.40 -10 3 28 24.70 14.20 10 3 -28 -2.20 13.70 -9 -3 28 33.00 14.70 9 -3 -28 -11.40 14.20 9 3 -28 1.10 14.20 -9 3 28 -1.10 12.70 -8 -3 28 -3.60 13.80 8 -3 -28 -2.40 11.80 8 3 -28 18.90 15.00 -8 3 28 0.90 14.60 -7 -3 28 -6.10 13.40 7 -3 -28 -13.90 11.30 7 -3 -28 -1.70 10.90 7 3 -28 7.60 13.70 -7 3 28 18.40 14.30 6 -3 -28 -11.30 11.40 6 -3 -28 4.40 10.50 -6 -3 28 3.20 12.20 -6 3 28 9.10 14.10 6 3 -28 -14.20 12.00 -5 -3 28 24.20 12.80 5 -3 -28 2.80 11.60 5 -3 -28 21.90 11.90 5 3 -28 25.60 13.10 -5 3 28 41.40 13.90 4 -3 -28 -5.40 10.70 4 -3 -28 16.00 11.60 -4 -3 28 11.50 12.00 -4 3 28 9.50 12.20 4 3 -28 8.50 12.30 3 -3 -28 -18.10 11.30 -3 -3 28 14.00 10.80 3 -3 -28 -7.30 10.30 -3 3 28 12.30 12.20 3 3 -28 4.50 12.10 2 -3 -28 14.90 11.60 -2 -3 28 0.10 10.50 -2 3 28 5.60 16.70 -2 3 28 -6.00 10.50 2 3 -28 3.10 11.50 -1 -3 28 40.80 12.00 1 -3 -28 8.90 12.30 1 3 -28 23.20 13.10 -1 3 28 55.99 20.40 -1 3 28 25.30 12.10 0 -3 28 41.30 18.90 0 -3 -28 -3.70 10.40 0 -3 28 2.70 10.20 0 3 28 -2.40 9.50 0 3 28 28.30 18.80 0 3 -28 3.70 8.80 -1 -3 -28 10.50 11.20 1 -3 28 -1.20 9.60 1 -3 28 1.50 17.20 1 3 28 7.40 10.40 -1 3 -28 21.50 9.70 1 3 28 -0.10 17.00 2 -3 28 7.30 9.30 2 -3 28 25.90 18.50 -2 -3 -28 -12.30 10.40 2 3 28 -8.20 17.30 2 3 28 11.10 10.10 -2 3 -28 3.30 9.80 3 -3 28 2.90 18.60 -3 -3 -28 3.40 11.00 3 -3 28 24.00 11.20 3 3 28 18.30 18.00 3 3 28 26.90 10.10 -3 3 -28 -3.50 10.60 -4 -3 -28 3.30 11.30 4 -3 28 1.60 17.20 -4 3 -28 9.10 11.50 4 3 28 27.50 19.80 -5 -3 -28 13.70 12.30 5 -3 28 1.90 18.40 5 3 28 13.20 19.80 -5 3 -28 6.20 11.80 6 -3 28 8.10 18.20 -6 -3 -28 0.90 12.10 -6 3 -28 14.90 12.30 6 3 28 15.80 17.90 7 -3 28 30.00 19.50 -7 -3 -28 16.10 13.10 7 3 28 -1.90 17.40 -7 3 -28 9.50 13.00 -8 -3 -28 20.00 14.00 8 -3 28 8.90 18.60 8 3 28 18.40 19.10 -8 3 -28 -6.00 13.10 9 -3 28 -23.20 19.00 -9 -3 -28 -7.60 15.10 9 3 28 8.30 19.00 -9 3 -28 -3.50 13.70 -10 -4 28 10.20 13.20 -10 4 28 4.50 15.10 10 4 -28 12.40 15.40 -9 -4 28 22.10 14.50 -9 4 28 22.70 15.00 9 4 -28 7.40 15.50 8 -4 -28 19.90 11.90 -8 -4 28 21.50 14.10 -8 4 28 29.10 15.10 8 4 -28 -3.20 14.20 7 -4 -28 29.20 14.00 -7 -4 28 71.29 16.90 7 4 -28 21.00 16.20 -7 4 28 57.99 16.80 6 -4 -28 11.80 12.40 -6 -4 28 19.80 14.50 6 -4 -28 14.60 11.80 -6 4 28 26.40 15.40 6 4 -28 21.60 15.50 5 -4 -28 13.60 12.00 -5 -4 28 17.20 12.80 5 -4 -28 -2.40 11.70 -5 4 28 19.00 14.00 5 4 -28 1.30 12.70 -4 -4 28 43.70 13.30 4 -4 -28 19.40 13.10 4 -4 -28 24.40 12.10 -4 4 28 32.60 13.90 4 4 -28 9.60 12.50 3 -4 -28 69.39 14.70 -3 -4 28 17.30 12.70 3 -4 -28 31.10 12.40 3 4 -28 29.00 14.00 -3 4 28 33.30 13.80 -2 -4 28 2.60 10.60 2 -4 -28 -17.00 11.80 -2 4 28 -1.00 17.50 2 4 -28 6.60 12.20 -2 4 28 18.60 11.50 1 -4 -28 16.80 13.10 -1 -4 28 16.00 11.10 1 4 -28 25.00 13.30 -1 4 28 21.80 11.30 -1 4 28 23.90 19.00 0 -4 28 10.20 18.60 0 -4 -28 16.30 11.90 0 -4 28 11.70 9.90 0 4 28 -6.20 17.50 0 4 28 12.20 10.30 0 4 -28 1.20 11.40 1 -4 28 -0.60 17.40 -1 -4 -28 -0.90 10.70 1 -4 28 11.30 9.80 1 4 28 2.20 10.20 -1 4 -28 3.70 9.10 1 4 28 1.70 18.20 -2 -4 -28 -15.40 10.80 2 -4 28 18.70 9.90 2 -4 28 4.30 17.30 2 4 28 20.90 10.00 2 4 28 -21.40 18.30 -2 4 -28 4.30 9.70 -3 -4 -28 3.40 11.10 3 -4 28 19.00 18.10 3 4 28 -5.40 18.20 -3 4 -28 -13.50 10.00 3 4 28 18.50 9.90 4 -4 28 9.00 19.50 -4 -4 -28 14.40 12.60 4 4 28 33.70 19.30 -4 4 -28 16.20 12.00 -5 -4 -28 17.60 12.70 5 -4 28 37.90 19.20 5 4 28 20.10 19.20 -5 4 -28 11.30 11.80 6 -4 28 -2.60 20.00 -6 -4 -28 -10.10 12.20 6 4 28 6.60 16.90 -6 4 -28 -5.70 12.20 7 -4 28 38.50 22.40 -7 -4 -28 41.10 16.20 -7 4 -28 45.40 15.20 7 4 28 27.90 20.40 -8 -4 -28 9.30 15.90 8 -4 28 59.19 23.00 8 4 28 35.40 22.20 -8 4 -28 51.19 15.90 -9 -4 -28 51.29 16.40 9 -4 28 4.80 21.10 9 4 28 26.40 21.20 -9 4 -28 5.80 15.80 9 -5 -28 5.10 14.20 -9 -5 28 39.20 16.20 9 5 -28 24.40 16.50 -9 5 28 -16.10 14.50 8 -5 -28 20.40 13.30 -8 -5 28 44.50 16.30 8 5 -28 36.30 17.20 -8 5 28 26.20 16.90 7 -5 -28 -4.70 12.10 -7 -5 28 -3.50 13.90 -7 5 28 -1.30 14.40 7 5 -28 -5.40 13.80 6 -5 -28 63.79 17.10 -6 -5 28 94.79 19.00 -6 5 28 54.09 19.10 6 5 -28 66.09 19.80 -5 -5 28 34.40 14.80 5 -5 -28 40.40 14.60 5 5 -28 26.80 15.60 -5 5 28 78.99 16.80 -4 -5 28 1.10 12.30 4 -5 -28 0.80 12.40 -4 5 28 -5.40 12.50 4 5 -28 -15.70 12.00 3 -5 -28 78.19 17.50 -3 -5 28 105.09 18.30 3 -5 -28 89.39 18.60 3 5 -28 51.39 18.70 -3 5 28 84.79 17.90 2 -5 -28 142.89 24.10 -2 -5 28 136.59 22.40 2 5 -28 118.29 24.20 -2 5 28 111.99 22.40 -2 5 28 111.59 27.30 -1 -5 28 64.69 14.30 1 -5 -28 57.89 15.70 1 5 -28 40.60 15.30 -1 5 28 47.50 14.00 -1 5 28 22.30 19.60 0 -5 -28 -6.40 12.60 0 -5 28 19.90 10.60 0 5 -28 -13.10 12.00 0 5 28 12.60 17.10 0 5 28 11.60 10.50 1 -5 28 60.79 22.30 -1 -5 -28 39.30 14.80 1 -5 28 58.99 12.80 1 5 28 41.80 20.10 -1 5 -28 29.10 14.60 1 5 28 37.40 12.50 -2 -5 -28 86.89 17.80 2 -5 28 69.09 16.10 2 -5 28 54.99 22.70 2 5 28 71.59 23.60 2 5 28 111.99 17.10 -3 -5 -28 31.70 14.30 3 -5 28 39.10 21.20 3 5 28 51.89 13.20 -3 5 -28 70.89 14.20 3 5 28 44.40 21.60 4 -5 28 19.30 18.50 -4 -5 -28 36.60 13.30 -4 5 -28 41.70 12.70 4 5 28 9.80 19.10 5 -5 28 17.00 18.70 -5 -5 -28 -2.20 13.10 -5 5 -28 -5.60 11.10 5 5 28 10.00 20.30 -6 -5 -28 42.90 16.30 6 -5 28 75.59 23.70 -6 5 -28 37.80 15.00 6 5 28 17.10 19.00 7 -5 28 33.40 20.50 -7 -5 -28 41.00 15.80 7 5 28 0.00 19.50 -7 5 -28 36.10 15.30 -8 -5 -28 -7.70 14.50 8 -5 28 -11.30 20.30 8 5 28 6.70 20.90 -8 5 -28 -9.30 14.50 8 -6 -28 0.80 13.10 -8 -6 28 -5.50 15.30 8 6 -28 -1.90 16.10 -8 6 28 33.00 16.80 7 -6 -28 40.60 14.70 -7 -6 28 45.10 16.90 7 6 -28 -7.70 16.30 -7 6 28 48.30 16.80 -6 -6 28 55.19 17.00 6 -6 -28 35.10 15.20 -6 6 28 37.40 15.90 6 6 -28 36.80 17.60 -5 -6 28 10.70 14.60 5 -6 -28 15.80 12.90 5 6 -28 -4.30 13.80 -5 6 28 21.10 14.50 4 -6 -28 200.98 32.60 -4 -6 28 213.78 32.50 -4 6 28 240.48 33.70 4 6 -28 155.58 33.30 -3 -6 28 42.60 14.80 3 -6 -28 38.10 14.80 3 6 -28 23.50 14.90 -3 6 28 23.10 14.80 2 -6 -28 19.40 13.20 -2 -6 28 -8.10 11.80 2 6 -28 -3.80 12.60 -2 6 28 14.80 13.40 1 -6 -28 62.39 17.90 -1 -6 28 84.39 16.00 -1 6 28 55.09 15.90 1 6 -28 59.79 17.80 0 -6 -28 105.99 20.50 0 -6 28 98.19 18.30 0 6 28 67.39 23.80 0 6 -28 77.39 20.40 0 6 28 89.49 17.90 1 -6 28 16.20 11.30 -1 -6 -28 8.30 13.50 1 6 28 19.20 11.80 1 6 28 8.40 18.60 -1 6 -28 9.00 12.90 2 -6 28 10.70 19.20 -2 -6 -28 16.10 13.30 2 -6 28 3.70 10.70 2 6 28 9.70 11.30 -2 6 -28 -7.50 11.70 2 6 28 5.20 18.50 3 -6 28 -6.30 19.90 -3 -6 -28 -4.80 12.30 3 6 28 8.50 11.30 3 6 28 24.80 20.60 -4 -6 -28 20.60 13.80 4 -6 28 41.30 21.20 4 6 28 44.00 23.00 -4 6 -28 22.40 12.30 5 -6 28 45.50 23.20 -5 -6 -28 51.19 16.30 5 6 28 54.49 22.80 -5 6 -28 62.69 15.70 -6 -6 -28 16.50 13.40 6 -6 28 4.00 20.00 6 6 28 -8.90 19.30 -6 6 -28 7.10 13.10 7 -6 28 19.40 22.50 -7 -6 -28 20.60 16.20 7 6 28 24.50 20.60 -7 6 -28 26.10 15.20 -8 -6 -28 60.99 19.70 -7 -7 28 17.50 16.30 7 -7 -28 30.70 14.90 -7 7 28 22.70 17.10 7 7 -28 4.90 17.20 -6 -7 28 19.50 14.90 6 -7 -28 46.60 15.30 -6 7 28 60.79 18.30 6 7 -28 6.50 15.40 5 -7 -28 119.29 23.30 -5 -7 28 136.69 24.00 -5 7 28 176.38 26.00 5 7 -28 79.79 23.90 4 -7 -28 24.50 14.20 -4 -7 28 23.60 15.10 -4 7 28 44.30 15.90 4 7 -28 8.60 15.50 3 -7 -28 22.40 14.30 -3 -7 28 39.60 15.30 -3 7 28 19.10 15.50 3 7 -28 19.40 15.10 -2 -7 28 -2.40 12.20 2 -7 -28 -23.40 13.00 -2 7 28 20.80 13.50 2 7 -28 3.40 13.50 -1 -7 28 19.30 11.90 1 -7 -28 -12.30 13.10 1 7 -28 4.20 13.30 -1 7 28 -1.90 12.20 0 -7 -28 -22.10 13.50 0 -7 28 10.90 11.60 0 7 28 6.30 11.90 0 7 -28 -2.00 12.60 1 -7 28 25.00 11.50 -1 -7 -28 42.20 15.30 -1 7 -28 17.30 14.20 1 7 28 28.10 13.80 2 -7 28 25.00 11.80 -2 -7 -28 39.60 15.20 2 7 28 4.50 12.60 -2 7 -28 11.00 12.90 3 -7 28 1.00 18.30 -3 -7 -28 19.00 14.70 3 7 28 -2.40 11.90 -3 7 -28 11.40 13.20 3 7 28 -6.40 19.70 -4 -7 -28 -9.30 13.20 4 -7 28 -33.60 18.00 4 7 28 -2.60 20.40 -5 -7 -28 73.99 17.20 5 -7 28 25.90 22.20 5 7 28 52.29 23.70 -5 7 -28 25.80 20.60 -6 -7 -28 96.19 22.30 -6 7 -28 158.98 22.80 6 7 28 52.59 25.00 6 -8 -28 13.70 14.80 -6 -8 28 1.60 15.50 -6 8 28 39.50 18.10 6 8 -28 8.60 17.30 5 -8 -28 -1.60 13.60 -5 -8 28 -14.00 13.80 5 8 -28 13.70 15.10 -5 8 28 9.40 14.50 -4 -8 28 28.70 15.60 4 -8 -28 15.80 14.40 -4 8 28 27.50 16.10 4 8 -28 -11.90 14.50 3 -8 -28 27.10 14.60 -3 -8 28 18.80 14.40 3 8 -28 0.90 14.90 -3 8 28 12.30 14.80 -2 -8 28 -6.00 12.80 2 -8 -28 3.10 13.40 2 8 -28 4.40 14.30 -2 8 28 15.20 13.80 -1 -8 28 -23.60 12.10 1 -8 -28 -15.60 14.10 1 8 -28 2.70 13.30 -1 8 28 -3.60 13.30 0 -8 -28 0.90 14.00 0 -8 28 -1.50 12.20 0 8 -28 9.50 13.80 0 8 28 19.30 13.20 -1 -8 -28 -0.50 15.00 1 -8 28 24.70 12.40 1 8 28 1.90 12.90 -1 8 -28 12.40 13.10 -2 -8 -28 -3.10 15.20 2 -8 28 27.80 12.80 -2 8 -28 22.80 14.00 2 8 28 8.70 12.60 -3 -8 -28 -15.70 14.90 -3 8 -28 -15.40 12.20 3 8 28 -4.60 12.50 -4 -8 -28 11.40 15.70 -5 -8 -28 21.50 16.40 4 -9 -28 -11.00 14.30 -3 -9 28 25.60 16.00 3 -9 -28 -22.40 13.90 -3 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-1 34 52.99 15.70 1 -1 -34 67.19 16.50 -1 1 34 79.89 26.90 -1 1 34 59.49 15.70 1 1 -34 50.69 17.20 0 -1 34 36.00 24.30 0 -1 34 101.09 17.10 0 -1 -34 81.79 17.70 0 1 34 55.79 16.00 0 1 34 58.29 26.70 0 1 -34 83.39 17.30 1 -1 34 15.20 22.20 1 -1 34 21.30 11.80 -1 -1 -34 -0.40 12.80 -1 1 -34 9.90 12.50 1 1 34 20.20 21.10 1 1 34 -3.40 11.10 2 -1 34 22.50 22.20 -2 -1 -34 27.90 13.70 2 1 34 11.70 22.30 -2 1 -34 5.10 13.00 -3 -1 -34 -3.80 12.90 3 -1 34 -11.40 20.80 3 1 34 49.30 23.80 -3 1 -34 4.10 12.90 -4 -1 -34 18.20 14.60 4 -1 34 42.60 22.20 4 1 34 4.50 20.90 -4 1 -34 38.20 15.00 5 -1 34 28.70 22.30 -5 -1 -34 70.59 16.80 5 1 34 10.70 22.20 -5 1 -34 26.00 15.60 6 -2 -34 20.50 15.40 -6 -2 34 -0.30 16.00 6 2 -34 2.20 14.50 -6 2 34 7.70 16.40 5 -2 -34 25.30 15.00 -5 -2 34 36.00 16.60 5 2 -34 -4.80 13.40 -5 2 34 35.20 16.00 4 -2 -34 -17.20 11.60 4 -2 -34 -9.30 14.20 -4 -2 34 8.40 14.00 -4 2 34 11.00 13.60 4 2 -34 5.00 13.50 3 -2 -34 16.80 14.60 -3 -2 34 7.30 12.60 3 -2 -34 10.10 12.80 3 2 -34 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14.90 3 -3 -34 -1.10 12.20 3 -3 -34 -9.80 14.20 -3 -3 34 30.30 13.80 -3 3 34 23.40 14.80 3 3 -34 5.80 14.00 -2 -3 34 0.60 12.00 2 -3 -34 8.20 12.70 2 -3 -34 -18.80 13.40 2 3 -34 4.90 13.60 -2 3 34 -4.30 13.10 -1 -3 34 15.70 12.20 1 -3 -34 14.80 13.70 -1 3 34 -6.50 22.40 -1 3 34 5.90 12.60 1 3 -34 8.10 14.00 0 -3 -34 -3.00 13.30 0 -3 34 11.70 11.20 0 3 34 -1.90 11.90 0 3 -34 -3.80 13.80 0 3 34 28.80 23.70 1 -3 34 -0.50 11.40 -1 -3 -34 9.00 13.20 1 -3 34 24.20 20.40 1 3 34 4.20 21.80 1 3 34 6.60 12.00 -2 -3 -34 10.00 13.60 2 -3 34 10.90 20.70 2 3 34 19.20 21.50 3 -3 34 26.00 21.20 -3 -3 -34 7.40 13.80 3 3 34 -22.20 22.60 -3 3 -34 7.30 13.20 4 -3 34 7.10 20.80 -4 -3 -34 -10.80 13.60 4 3 34 -1.80 22.20 -4 3 -34 -11.00 13.30 4 -4 -34 4.40 13.00 -4 -4 34 18.50 14.50 4 -4 -34 8.10 14.70 -4 4 34 41.50 17.10 4 4 -34 2.90 14.40 -3 -4 34 37.50 15.00 3 -4 -34 21.10 14.70 3 -4 -34 7.10 12.80 -3 4 34 32.80 15.00 3 4 -34 17.40 15.20 2 -4 -34 -17.10 14.20 -2 -4 34 9.70 12.90 2 -4 -34 18.90 13.60 2 4 -34 2.30 14.50 -2 4 34 25.30 14.50 -1 -4 34 12.20 12.00 1 -4 -34 14.90 14.60 1 4 -34 1.50 14.50 -1 4 34 37.30 22.50 -1 4 34 15.00 12.70 0 -4 34 -3.40 11.20 0 -4 -34 -25.10 13.80 0 4 34 8.70 23.60 0 4 34 31.90 12.50 0 4 -34 15.10 14.40 -1 -4 -34 -9.70 13.80 1 -4 34 2.60 11.90 1 -4 34 49.90 23.80 1 4 34 -0.10 12.40 1 4 34 12.60 23.00 -1 4 -34 0.10 14.30 2 -4 34 44.70 24.00 -2 -4 -34 -2.80 13.30 2 4 34 25.10 21.90 -3 -4 -34 -15.60 12.70 3 -4 34 -0.90 20.40 3 4 34 28.60 23.70 3 -5 -34 15.20 15.70 -3 -5 34 31.40 15.60 -3 5 34 46.40 16.40 3 5 -34 18.90 16.00 -2 -5 34 12.60 13.70 2 -5 -34 1.20 14.60 -2 5 34 17.70 14.00 2 5 -34 -6.70 14.30 1 -5 -34 28.20 16.20 -1 -5 34 30.80 13.90 -1 5 34 -0.40 13.90 1 5 -34 27.60 15.50 -1 5 34 13.00 22.70 0 -5 -34 20.60 15.40 0 -5 34 36.90 13.50 0 5 34 24.20 24.30 0 5 -34 9.60 15.70 0 5 34 16.50 12.70 1 -5 34 38.00 13.80 -1 -5 -34 -3.60 15.20 1 5 34 10.30 23.30 -1 5 -34 26.70 16.50 1 5 34 60.29 14.50 -2 -5 -34 -13.20 13.70 2 -5 34 -8.20 21.30 -2 5 -34 -2.90 14.60 2 5 34 -3.50 22.70 5 0 -35 1.70 13.90 -5 0 35 -1.40 14.90 -4 0 35 12.80 15.30 4 0 -35 -4.10 13.40 -3 0 35 35.30 14.00 3 0 -35 -0.90 13.10 2 0 -35 17.60 13.60 -2 0 35 0.20 11.80 1 0 -35 -2.20 12.70 1 0 -35 -5.00 12.70 -1 0 35 -6.70 22.90 -1 0 35 2.90 11.60 0 0 35 32.30 23.90 0 0 35 1.60 11.10 0 0 -35 -11.10 12.50 1 0 35 6.40 22.20 1 0 35 19.50 11.90 -1 0 -35 8.40 12.90 2 0 35 2.50 21.40 -2 0 -35 -21.70 12.90 3 0 35 27.10 24.00 -3 0 -35 -17.00 13.00 4 0 35 16.00 22.30 -4 0 -35 -15.70 13.60 5 -1 -35 -7.00 13.30 -5 -1 35 14.30 15.70 -5 1 35 1.10 15.90 5 1 -35 -10.10 13.10 -4 -1 35 7.50 13.80 4 -1 -35 15.30 13.80 -4 1 35 7.20 15.70 4 1 -35 -5.50 13.50 3 -1 -35 21.60 14.70 -3 -1 35 45.90 15.20 -3 1 35 30.30 14.90 3 1 -35 37.50 15.60 2 -1 -35 30.80 15.40 2 -1 -35 52.69 16.10 -2 -1 35 29.80 13.50 2 1 -35 24.20 15.40 -2 1 35 39.60 14.90 1 -1 -35 12.90 13.30 1 -1 -35 -2.30 13.10 -1 -1 35 13.00 12.10 -1 1 35 4.20 22.10 -1 1 35 -1.30 11.60 1 1 -35 7.30 13.90 0 -1 35 41.70 12.70 0 -1 35 8.90 23.50 0 -1 -35 26.80 14.40 0 1 -35 30.10 17.70 0 1 35 35.30 13.20 0 1 35 23.80 24.40 1 -1 35 33.80 23.10 -1 -1 -35 24.00 14.40 1 -1 35 33.70 12.30 1 1 35 9.00 24.50 -1 1 -35 26.70 14.10 1 1 35 41.60 13.00 -2 -1 -35 3.20 13.40 2 -1 35 5.90 21.30 2 1 35 2.30 22.60 -2 1 -35 -4.40 12.70 -3 -1 -35 -4.90 13.60 3 -1 35 21.10 22.80 3 1 35 26.20 24.50 -3 1 -35 6.70 13.80 -4 -1 -35 21.80 15.00 4 -1 35 -9.30 20.30 -4 1 -35 -24.10 13.30 4 1 35 6.20 23.00 5 -2 -35 17.50 14.70 -5 -2 35 44.40 16.80 5 2 -35 6.80 13.90 -5 2 35 29.60 16.10 -4 -2 35 59.19 16.20 4 -2 -35 38.80 15.90 -4 2 35 42.90 16.00 4 2 -35 13.90 15.60 -3 -2 35 43.30 15.70 3 -2 -35 31.40 16.40 3 -2 -35 37.30 16.00 3 2 -35 47.40 17.00 -3 2 35 59.59 16.40 2 -2 -35 -1.30 12.80 2 -2 -35 9.70 13.90 -2 -2 35 11.00 12.00 -2 2 35 -2.10 12.60 2 2 -35 5.60 13.50 1 -2 -35 9.20 13.30 -1 -2 35 2.10 11.20 1 -2 -35 2.50 13.80 -1 2 35 64.79 25.20 1 2 -35 33.00 14.60 -1 2 35 -5.80 12.10 0 -2 35 60.09 15.10 0 -2 35 50.89 24.60 0 -2 -35 34.90 16.10 0 2 35 21.00 24.80 0 2 35 57.69 14.80 0 2 -35 55.29 17.40 1 -2 35 12.50 12.00 -1 -2 -35 24.40 14.00 1 -2 35 -5.20 21.90 1 2 35 5.70 11.90 1 2 35 4.10 20.90 -2 -2 -35 24.10 14.50 2 -2 35 30.40 23.80 -2 2 -35 13.20 13.90 2 2 35 29.30 24.30 -3 -2 -35 26.00 14.70 3 -2 35 42.50 22.70 -3 2 -35 14.80 13.90 3 2 35 10.90 24.10 4 -2 35 0.80 22.40 -4 -2 -35 -16.00 13.50 -4 2 -35 4.90 13.70 4 2 35 17.80 23.30 -4 -3 35 6.00 14.40 4 -3 -35 18.10 14.80 4 -3 -35 7.20 13.90 4 3 -35 6.90 15.00 -4 3 35 10.30 15.70 3 -3 -35 0.90 12.90 -3 -3 35 20.80 13.60 3 -3 -35 2.80 14.20 -3 3 35 60.29 15.70 3 3 -35 4.40 14.60 2 -3 -35 9.50 13.20 -2 -3 35 7.70 12.60 2 -3 -35 8.00 14.70 -2 3 35 36.30 13.60 2 3 -35 43.50 16.30 1 -3 -35 23.00 14.70 -1 -3 35 20.60 13.00 -1 3 35 7.90 12.00 1 3 -35 11.60 14.80 -1 3 35 10.50 23.30 0 -3 -35 8.90 14.70 0 -3 35 19.00 12.00 0 3 35 14.30 23.30 0 3 35 14.50 12.30 0 3 -35 28.90 15.60 -1 -3 -35 30.50 17.40 1 -3 35 112.29 17.40 1 -3 35 68.69 26.70 1 3 35 78.19 16.30 1 3 35 60.29 27.10 -1 3 -35 68.39 19.20 -2 -3 -35 51.99 15.60 2 -3 35 14.70 23.40 2 3 35 -16.30 21.40 3 -3 35 -25.90 19.90 -3 -3 -35 0.60 13.90 3 3 35 39.50 23.40 -3 3 -35 9.20 13.80 2 -4 -35 -4.00 12.70 -2 -4 35 -17.50 11.80 2 -4 -35 2.00 15.40 2 4 -35 2.20 14.80 -2 4 35 17.70 13.60 -1 -4 35 47.40 14.70 1 -4 -35 33.90 16.50 -1 4 35 40.00 15.20 -1 4 35 35.70 25.70 1 4 -35 27.90 16.50 0 -4 -35 17.80 15.90 0 -4 35 47.80 14.10 0 4 -35 14.30 15.50 0 4 35 49.60 14.20 0 4 35 12.50 24.50 -1 -4 -35 3.50 14.80 1 -4 35 -9.30 13.40 -1 4 -35 13.80 14.90 1 4 35 18.70 24.00 1 4 35 4.00 12.40 -4 0 36 101.99 22.30 3 0 -36 15.40 14.60 -3 0 36 -0.90 13.70 2 0 -36 10.90 13.80 -2 0 36 11.30 12.60 1 0 -36 88.29 22.30 -1 0 36 117.49 20.60 0 0 -36 51.09 16.80 0 0 36 6.00 23.80 0 0 36 94.39 16.00 1 0 36 7.30 11.70 -1 0 -36 -1.50 13.00 1 0 36 5.80 22.00 -2 0 -36 9.00 14.00 2 0 36 26.70 23.40 3 -1 -36 12.60 14.00 -3 -1 36 25.50 14.20 3 1 -36 8.00 14.50 -3 1 36 23.30 14.80 -2 -1 36 38.50 14.40 2 -1 -36 50.79 20.80 2 -1 -36 11.10 14.50 2 1 -36 16.30 15.00 -2 1 36 45.00 14.80 -1 -1 36 0.20 12.30 1 -1 -36 7.10 13.40 1 -1 -36 14.80 14.00 -1 1 36 5.60 23.70 1 1 -36 -9.40 12.90 -1 1 36 -1.80 11.60 0 -1 -36 -1.00 12.80 0 -1 36 29.50 12.60 0 -1 36 8.90 22.40 0 1 36 24.10 11.90 0 1 36 -24.60 21.10 0 1 -36 -1.50 12.90 1 -1 36 6.00 11.80 -1 -1 -36 -3.10 13.60 1 -1 36 6.80 24.90 1 1 36 21.80 11.90 -1 1 -36 -11.40 13.00 1 1 36 -2.80 23.00 -2 -1 -36 -17.40 13.10 2 -1 36 4.90 22.00 2 1 36 7.90 23.80 -2 1 -36 3.70 13.80 -3 -2 36 16.10 14.60 -3 2 36 28.60 15.10 -2 -2 36 -4.50 11.80 2 -2 -36 0.40 13.00 2 -2 -36 3.30 14.40 -2 2 36 -5.30 12.80 2 2 -36 7.40 13.80 -1 -2 36 2.50 12.30 1 -2 -36 14.80 13.20 1 -2 -36 2.30 14.50 -1 2 36 3.50 22.60 1 2 -36 -3.00 13.80 -1 2 36 -10.80 11.20 0 -2 -36 0.10 13.60 0 -2 36 11.70 11.90 0 2 36 26.10 12.90 0 2 36 -3.50 23.10 0 2 -36 17.70 15.10 1 -2 36 52.69 17.20 1 -2 36 -7.70 21.00 -1 -2 -36 9.80 14.10 1 2 36 32.10 13.00 1 2 36 -14.80 23.50 2 2 36 -5.50 23.60 -1 -3 36 10.30 12.80 -1 3 36 10.30 22.80 0 -3 36 1.50 11.40 0 3 36 4.40 11.70 0 3 36 9.40 22.70 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 66780 #===END data_Cpx_5c _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Cpx_5c' _chemical_melting_point ? _chemical_formula_moiety 'C46 H69 F3 N O7 P Pd S, C7 H8' _chemical_formula_sum 'C53 H77 F3 N O7 P Pd S' _chemical_formula_weight 1066.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.4741(4) _cell_length_b 16.7555(6) _cell_length_c 14.1454(5) _cell_angle_alpha 90 _cell_angle_beta 115.680(2) _cell_angle_gamma 90 _cell_volume 2664.50(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.637 _cell_measurement_theta_max 65.030 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_F_000 1124 _exptl_transmission_factor_min 0.552 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 3.953 _shelx_estimated_absorpt_T_min 0.144 _shelx_estimated_absorpt_T_max 0.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Mixed Phi and Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25547 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.467 _diffrn_reflns_theta_max 65.094 _diffrn_reflns_theta_full 65.094 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.897 _diffrn_reflns_point_group_measured_fraction_full 0.898 _reflns_number_total 8167 _reflns_number_gt 7852 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.760 _reflns_Friedel_fraction_max 0.806 _reflns_Friedel_fraction_full 0.806 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3210 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _chemical_absolute_configuration unk _refine_ls_number_reflns 8167 _refine_ls_number_parameters 727 _refine_ls_number_restraints 153 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C47A C 0.964(2) 0.1674(16) -0.0030(18) 0.111(8) Uani 0.60(2) 1 d D U P A 1 H47A H 1.040154 0.171041 -0.007372 0.167 Uiso 0.60(2) 1 calc R U P A 1 H47B H 0.939178 0.220817 0.007734 0.167 Uiso 0.60(2) 1 calc R U P A 1 H47C H 0.903710 0.144841 -0.068317 0.167 Uiso 0.60(2) 1 calc R U P A 1 C48A C 0.9777(14) 0.1151(11) 0.0866(12) 0.069(4) Uani 0.60(2) 1 d D U P A 1 C49A C 1.026(2) 0.0413(12) 0.1014(14) 0.071(5) Uani 0.60(2) 1 d D . P A 1 H49A H 1.052593 0.020815 0.052624 0.085 Uiso 0.60(2) 1 calc R U P A 1 C50A C 1.0373(17) -0.0047(13) 0.1855(13) 0.078(6) Uani 0.60(2) 1 d D . P A 1 H50A H 1.073124 -0.055938 0.195521 0.094 Uiso 0.60(2) 1 calc R U P A 1 C51A C 0.9969(15) 0.0234(11) 0.2549(13) 0.069(4) Uani 0.60(2) 1 d D . P A 1 H51A H 1.003711 -0.008172 0.313086 0.083 Uiso 0.60(2) 1 calc R U P A 1 C52A C 0.9466(16) 0.0973(11) 0.2393(13) 0.071(5) Uani 0.60(2) 1 d D . P A 1 H52A H 0.918636 0.117081 0.287499 0.085 Uiso 0.60(2) 1 calc R U P A 1 C53A C 0.935(2) 0.1438(13) 0.1557(14) 0.078(6) Uani 0.60(2) 1 d D . P A 1 H53A H 0.899253 0.194957 0.145446 0.094 Uiso 0.60(2) 1 calc R U P A 1 C47B C 1.086(3) -0.041(2) 0.254(3) 0.111(8) Uani 0.40(2) 1 d D U P A 2 H47D H 1.147932 -0.025839 0.322886 0.167 Uiso 0.40(2) 1 calc R U P A 2 H47E H 1.118472 -0.078008 0.219798 0.167 Uiso 0.40(2) 1 calc R U P A 2 H47F H 1.019807 -0.066320 0.262462 0.167 Uiso 0.40(2) 1 calc R U P A 2 C48B C 1.042(2) 0.0315(19) 0.188(3) 0.097(12) Uani 0.40(2) 1 d D U P A 2 C49B C 1.051(3) 0.040(2) 0.097(3) 0.100(14) Uani 0.40(2) 1 d D U P A 2 H49B H 1.088713 -0.001190 0.076417 0.120 Uiso 0.40(2) 1 calc R U P A 2 C50B C 1.007(3) 0.105(2) 0.033(3) 0.131(17) Uani 0.40(2) 1 d D U P A 2 H50B H 1.014295 0.109529 -0.031184 0.157 Uiso 0.40(2) 1 calc R U P A 2 C51B C 0.953(3) 0.162(2) 0.065(3) 0.097(12) Uani 0.40(2) 1 d D U P A 2 H51B H 0.915762 0.204192 0.018035 0.117 Uiso 0.40(2) 1 calc R U P A 2 C52B C 0.949(4) 0.163(2) 0.160(3) 0.100(14) Uani 0.40(2) 1 d D U P A 2 H52B H 0.916691 0.206131 0.182556 0.120 Uiso 0.40(2) 1 calc R U P A 2 C53B C 0.996(4) 0.095(2) 0.220(3) 0.131(17) Uani 0.40(2) 1 d D U P A 2 H53B H 0.997328 0.092248 0.287352 0.157 Uiso 0.40(2) 1 calc R U P A 2 S1A S 0.7028(4) 0.3576(3) 0.9772(3) 0.0494(10) Uani 0.663(6) 1 d D . P B 1 F1A F 0.8283(11) 0.4860(9) 1.0480(11) 0.091(3) Uani 0.663(6) 1 d D . P B 1 F2A F 0.6841(15) 0.4724(9) 1.0908(11) 0.111(5) Uani 0.663(6) 1 d D . P B 1 F3A F 0.6462(10) 0.5086(8) 0.9372(10) 0.091(3) Uani 0.663(6) 1 d D . P B 1 O5A O 0.7787(13) 0.3130(8) 1.0704(10) 0.064(4) Uani 0.663(6) 1 d D . P B 1 O6A O 0.7308(14) 0.3518(9) 0.8905(11) 0.090(4) Uani 0.663(6) 1 d D . P B 1 O7A O 0.5774(8) 0.3417(8) 0.9454(9) 0.074(3) Uani 0.663(6) 1 d D . P B 1 C46A C 0.7139(15) 0.4602(10) 1.0137(12) 0.069(4) Uani 0.663(6) 1 d D . P B 1 O3A O 0.3472(10) 0.7642(9) 0.6882(9) 0.037(3) Uani 0.577(13) 1 d D . P C 1 O4A O 0.5171(8) 0.7521(9) 0.8395(8) 0.040(2) Uani 0.577(13) 1 d D . P C 1 C28A C 0.4748(13) 0.7634(14) 0.7258(15) 0.039(5) Uani 0.577(13) 1 d D . P C 1 C29A C 0.316(2) 0.7664(16) 0.7709(15) 0.057(4) Uani 0.577(13) 1 d D . P C 1 H29A H 0.240395 0.737600 0.753839 0.069 Uiso 0.577(13) 1 calc R U P C 1 H29B H 0.308716 0.821873 0.791537 0.069 Uiso 0.577(13) 1 calc R U P C 1 C30A C 0.4204(12) 0.7239(12) 0.8551(12) 0.057(4) Uani 0.577(13) 1 d D . P C 1 H30A H 0.428574 0.737992 0.925887 0.069 Uiso 0.577(13) 1 calc R U P C 1 H30B H 0.412259 0.665287 0.846054 0.069 Uiso 0.577(13) 1 calc R U P C 1 C31A C 0.5206(11) 0.8449(8) 0.7154(10) 0.033(3) Uani 0.577(13) 1 d D . P C 1 H31A H 0.602563 0.850959 0.771269 0.039 Uiso 0.577(13) 1 calc R U P C 1 H31B H 0.470618 0.885893 0.727354 0.039 Uiso 0.577(13) 1 calc R U P C 1 C32A C 0.5217(18) 0.8611(12) 0.6085(14) 0.030(2) Uani 0.577(13) 1 d D . P C 1 C33A C 0.3933(11) 0.8607(9) 0.5225(9) 0.035(3) Uani 0.577(13) 1 d D . P C 1 H33A H 0.346950 0.901549 0.538035 0.053 Uiso 0.577(13) 1 calc R U P C 1 H33B H 0.357657 0.808139 0.520115 0.053 Uiso 0.577(13) 1 calc R U P C 1 H33C H 0.393163 0.872094 0.454536 0.053 Uiso 0.577(13) 1 calc R U P C 1 C34A C 0.5676(12) 0.9453(8) 0.6063(12) 0.038(3) Uani 0.577(13) 1 d D . P C 1 H34A H 0.518810 0.984096 0.622065 0.057 Uiso 0.577(13) 1 calc R U P C 1 H34B H 0.562870 0.956180 0.536531 0.057 Uiso 0.577(13) 1 calc R U P C 1 H34C H 0.650442 0.949570 0.658846 0.057 Uiso 0.577(13) 1 calc R U P C 1 S1B S 0.7497(8) 0.3628(7) 0.9756(8) 0.0494(10) Uani 0.337(6) 1 d D . P B 2 F1B F 0.813(2) 0.5014(19) 1.072(2) 0.091(3) Uani 0.337(6) 1 d D . P B 2 F2B F 0.626(3) 0.4723(18) 1.017(2) 0.111(5) Uani 0.337(6) 1 d D . P B 2 F3B F 0.6943(19) 0.5092(15) 0.9116(16) 0.091(3) Uani 0.337(6) 1 d D . P B 2 O5B O 0.765(3) 0.339(2) 1.0780(16) 0.064(4) Uani 0.337(6) 1 d D . P B 2 O6B O 0.8504(19) 0.3689(17) 0.957(2) 0.090(4) Uani 0.337(6) 1 d D . P B 2 O7B O 0.6398(16) 0.3404(17) 0.8909(15) 0.074(3) Uani 0.337(6) 1 d D . P B 2 C46B C 0.719(3) 0.4643(14) 0.997(2) 0.069(4) Uani 0.337(6) 1 d D . P B 2 O3B O 0.3176(14) 0.7250(14) 0.6585(12) 0.043(4) Uani 0.423(13) 1 d D . P C 2 O4B O 0.4894(15) 0.7822(11) 0.7847(18) 0.044(4) Uani 0.423(13) 1 d D . P C 2 C28B C 0.4355(17) 0.7519(19) 0.677(2) 0.041(5) Uani 0.423(13) 1 d D . P C 2 C29B C 0.311(3) 0.727(3) 0.755(2) 0.075(8) Uani 0.423(13) 1 d D . P C 2 H29C H 0.333922 0.674491 0.790704 0.090 Uiso 0.423(13) 1 calc R U P C 2 H29D H 0.229936 0.740467 0.745116 0.090 Uiso 0.423(13) 1 calc R U P C 2 C30B C 0.402(2) 0.793(2) 0.819(2) 0.075(8) Uani 0.423(13) 1 d D . P C 2 H30C H 0.366661 0.847141 0.801849 0.090 Uiso 0.423(13) 1 calc R U P C 2 H30D H 0.433442 0.784186 0.895790 0.090 Uiso 0.423(13) 1 calc R U P C 2 C31B C 0.4140(17) 0.8199(12) 0.5967(15) 0.037(5) Uani 0.423(13) 1 d D . P C 2 H31C H 0.363999 0.860648 0.608975 0.044 Uiso 0.423(13) 1 calc R U P C 2 H31D H 0.366567 0.797575 0.525819 0.044 Uiso 0.423(13) 1 calc R U P C 2 C32B C 0.522(3) 0.8633(17) 0.5946(17) 0.030(2) Uani 0.423(13) 1 d D . P C 2 C33B C 0.4774(16) 0.9151(11) 0.4957(14) 0.034(4) Uani 0.423(13) 1 d D . P C 2 H33D H 0.455469 0.880961 0.433881 0.052 Uiso 0.423(13) 1 calc R U P C 2 H33E H 0.540237 0.952148 0.500194 0.052 Uiso 0.423(13) 1 calc R U P C 2 H33F H 0.407596 0.945488 0.489814 0.052 Uiso 0.423(13) 1 calc R U P C 2 C34B C 0.5756(19) 0.9173(12) 0.6907(15) 0.043(5) Uani 0.423(13) 1 d D . P C 2 H34D H 0.511522 0.945679 0.699017 0.065 Uiso 0.423(13) 1 calc R U P C 2 H34E H 0.629160 0.956066 0.681464 0.065 Uiso 0.423(13) 1 calc R U P C 2 H34F H 0.620217 0.884938 0.753216 0.065 Uiso 0.423(13) 1 calc R U P C 2 Pd1 Pd 0.55010(3) 0.74691(4) 0.40545(3) 0.02485(17) Uani 1 1 d . . . . . P1 P 0.61770(14) 0.78415(11) 0.57979(13) 0.0260(4) Uani 1 1 d . . . . . O1 O 0.7997(6) 0.8692(4) 0.7821(4) 0.0483(15) Uani 1 1 d . . . . . O2 O 0.9644(5) 0.8251(5) 0.4825(5) 0.0554(19) Uani 1 1 d . . . . . N1 N 0.4778(5) 0.7178(4) 0.2434(5) 0.0317(13) Uani 1 1 d . . . . . H1A H 0.409959 0.746812 0.210200 0.038 Uiso 1 1 calc R U . . . H1B H 0.530051 0.735196 0.218802 0.038 Uiso 1 1 calc R U . . . C1 C 0.7705(6) 0.8215(5) 0.6149(6) 0.0321(15) Uani 1 1 d . . . . . C2 C 0.8467(8) 0.8552(5) 0.7142(6) 0.0405(18) Uani 1 1 d . . . . . C3 C 0.8763(12) 0.9026(8) 0.8821(7) 0.074(3) Uani 1 1 d . . . . . H3A H 0.943664 0.866570 0.918671 0.110 Uiso 1 1 calc R U . . . H3B H 0.831828 0.909453 0.924092 0.110 Uiso 1 1 calc R U . . . H3C H 0.905883 0.954503 0.871845 0.110 Uiso 1 1 calc R U . . . C4 C 0.9658(8) 0.8735(6) 0.7368(7) 0.053(2) Uani 1 1 d . . . . . H4 H 1.017409 0.894074 0.803831 0.063 Uiso 1 1 calc R U . . . C5 C 1.0077(8) 0.8617(6) 0.6619(8) 0.055(2) Uani 1 1 d . . . . . H5 H 1.088450 0.872986 0.677991 0.066 Uiso 1 1 calc R U . . . C6 C 0.9322(7) 0.8334(6) 0.5638(7) 0.0429(19) Uani 1 1 d . . . . . C7 C 1.0838(8) 0.8453(9) 0.5026(10) 0.078(4) Uani 1 1 d . . . . . H7A H 1.103604 0.898014 0.535725 0.117 Uiso 1 1 calc R U . . . H7B H 1.091149 0.846243 0.436409 0.117 Uiso 1 1 calc R U . . . H7C H 1.138556 0.805428 0.549618 0.117 Uiso 1 1 calc R U . . . C8 C 0.8142(6) 0.8122(5) 0.5393(6) 0.0337(15) Uani 1 1 d . . . . . C9 C 0.7446(6) 0.7867(5) 0.4274(6) 0.0314(15) Uani 1 1 d . . . . . C10 C 0.7680(6) 0.7118(5) 0.3929(6) 0.0374(17) Uani 1 1 d . . . . . C11 C 0.8240(7) 0.6438(5) 0.4721(7) 0.0416(18) Uani 1 1 d . . . . . H11 H 0.828645 0.661118 0.541384 0.050 Uiso 1 1 calc R U . . . C12 C 0.7480(10) 0.5681(5) 0.4379(8) 0.054(2) Uani 1 1 d . . . . . H12A H 0.760176 0.541991 0.381310 0.081 Uiso 1 1 calc R U . . . H12B H 0.663903 0.582209 0.412899 0.081 Uiso 1 1 calc R U . . . H12C H 0.771328 0.531569 0.497681 0.081 Uiso 1 1 calc R U . . . C13 C 0.9504(11) 0.6262(9) 0.4856(11) 0.079(5) Uani 1 1 d . . . . . H13A H 0.947196 0.605748 0.419522 0.118 Uiso 1 1 calc R U . . . H13B H 0.987293 0.586183 0.540896 0.118 Uiso 1 1 calc R U . . . H13C H 0.997618 0.675341 0.505109 0.118 Uiso 1 1 calc R U . . . C14 C 0.7494(7) 0.7011(5) 0.2904(6) 0.0372(16) Uani 1 1 d . . . . . H14 H 0.763167 0.650010 0.268549 0.045 Uiso 1 1 calc R U . . . C15 C 0.7110(6) 0.7632(4) 0.2181(6) 0.0351(18) Uani 1 1 d . . . . . C16 C 0.7034(7) 0.7552(8) 0.1081(6) 0.047(2) Uani 1 1 d . . . . . H16 H 0.630956 0.784975 0.059432 0.057 Uiso 1 1 calc R U . . . C17 C 0.6923(10) 0.6716(7) 0.0674(8) 0.060(2) Uani 1 1 d . . . . . H17A H 0.762821 0.640890 0.112475 0.091 Uiso 1 1 calc R U . . . H17B H 0.685489 0.672652 -0.004294 0.091 Uiso 1 1 calc R U . . . H17C H 0.621164 0.646619 0.067224 0.091 Uiso 1 1 calc R U . . . C18 C 0.8127(10) 0.7975(7) 0.1054(8) 0.060(3) Uani 1 1 d . . . . . H18A H 0.885243 0.768404 0.150067 0.090 Uiso 1 1 calc R U . . . H18B H 0.817671 0.852259 0.131279 0.090 Uiso 1 1 calc R U . . . H18C H 0.804115 0.798501 0.033208 0.090 Uiso 1 1 calc R U . . . C19 C 0.6812(7) 0.8354(5) 0.2487(6) 0.0351(16) Uani 1 1 d . . . . . H19 H 0.648298 0.876293 0.197685 0.042 Uiso 1 1 calc R U . . . C20 C 0.6974(6) 0.8506(5) 0.3503(6) 0.0312(15) Uani 1 1 d . . . . . C21 C 0.6748(7) 0.9317(5) 0.3809(6) 0.0374(16) Uani 1 1 d . . . . . H21 H 0.682681 0.928532 0.454213 0.045 Uiso 1 1 calc R U . . . C22 C 0.5493(10) 0.9605(6) 0.3103(8) 0.062(3) Uani 1 1 d . . . . . H22A H 0.539039 0.963569 0.237673 0.093 Uiso 1 1 calc R U . . . H22B H 0.536874 1.013383 0.333359 0.093 Uiso 1 1 calc R U . . . H22C H 0.491222 0.922925 0.314465 0.093 Uiso 1 1 calc R U . . . C23 C 0.7688(10) 0.9920(6) 0.3801(8) 0.061(3) Uani 1 1 d . . . . . H23A H 0.848543 0.973558 0.428022 0.091 Uiso 1 1 calc R U . . . H23B H 0.754158 1.044461 0.402862 0.091 Uiso 1 1 calc R U . . . H23C H 0.762987 0.996092 0.308935 0.091 Uiso 1 1 calc R U . . . C24 C 0.6309(6) 0.7015(5) 0.6751(6) 0.0330(15) Uani 1 1 d . . . . . C25 C 0.6636(8) 0.6256(5) 0.6336(7) 0.0430(19) Uani 1 1 d . . . . . H25A H 0.654013 0.579263 0.671513 0.065 Uiso 1 1 calc R U . . . H25B H 0.746446 0.628993 0.644122 0.065 Uiso 1 1 calc R U . . . H25C H 0.611283 0.619947 0.558625 0.065 Uiso 1 1 calc R U . . . C26 C 0.7257(7) 0.7108(6) 0.7888(6) 0.0465(19) Uani 1 1 d . . . . . H26A H 0.705522 0.756416 0.821363 0.070 Uiso 1 1 calc R U . . . H26B H 0.803548 0.719659 0.789293 0.070 Uiso 1 1 calc R U . . . H26C H 0.728359 0.662154 0.828302 0.070 Uiso 1 1 calc R U . . . C27 C 0.5067(7) 0.6931(5) 0.6717(6) 0.0375(18) Uani 1 1 d . . . . . H27A H 0.503037 0.642605 0.706622 0.045 Uiso 1 1 calc R U . C 1 H27B H 0.446790 0.689900 0.597625 0.045 Uiso 1 1 calc R U . C 1 C35 C 0.3864(6) 0.7103(5) 0.3844(5) 0.0289(14) Uani 1 1 d . . . . . C36 C 0.3649(7) 0.6347(5) 0.4108(6) 0.0387(17) Uani 1 1 d . . . . . H36 H 0.430554 0.603425 0.456234 0.046 Uiso 1 1 calc R U . . . C37 C 0.2514(8) 0.6022(6) 0.3739(7) 0.049(2) Uani 1 1 d . . . . . H37 H 0.240804 0.550045 0.394771 0.059 Uiso 1 1 calc R U . . . C38 C 0.1545(8) 0.6455(7) 0.3075(8) 0.054(3) Uani 1 1 d . . . . . C39 C 0.0310(8) 0.6089(9) 0.2623(10) 0.075(4) Uani 1 1 d . . . . . H39A H 0.004996 0.597533 0.187617 0.112 Uiso 1 1 calc R U . . . H39B H -0.024659 0.646446 0.270556 0.112 Uiso 1 1 calc R U . . . H39C H 0.032791 0.559259 0.299512 0.112 Uiso 1 1 calc R U . . . C40 C 0.1734(7) 0.7227(6) 0.2784(9) 0.058(3) Uani 1 1 d . . . . . H40 H 0.107577 0.753300 0.231983 0.069 Uiso 1 1 calc R U . . . C41 C 0.2883(6) 0.7548(6) 0.3173(6) 0.0410(17) Uani 1 1 d . . . . . H41 H 0.299517 0.807292 0.297808 0.049 Uiso 1 1 calc R U . . . C42 C 0.4487(8) 0.6337(5) 0.2098(7) 0.0439(18) Uani 1 1 d . . . . . H42A H 0.393401 0.613468 0.237635 0.053 Uiso 1 1 calc R U . . . H42B H 0.522610 0.601834 0.242344 0.053 Uiso 1 1 calc R U . . . C43 C 0.3943(9) 0.6196(6) 0.0949(7) 0.052(2) Uani 1 1 d . . . . . H43A H 0.316586 0.647300 0.062448 0.062 Uiso 1 1 calc R U . . . H43B H 0.446162 0.643272 0.065567 0.062 Uiso 1 1 calc R U . . . C44 C 0.376(2) 0.5340(9) 0.0663(12) 0.107(6) Uani 1 1 d . . . . . H44A H 0.315329 0.512426 0.086798 0.128 Uiso 1 1 calc R U . . . H44B H 0.451392 0.505091 0.107333 0.128 Uiso 1 1 calc R U . . . C45 C 0.3367(17) 0.5170(12) -0.0510(15) 0.118(7) Uani 1 1 d . . . . . H45A H 0.262916 0.546045 -0.092521 0.177 Uiso 1 1 calc R U . . . H45B H 0.323097 0.459614 -0.064034 0.177 Uiso 1 1 calc R U . . . H45C H 0.398929 0.534527 -0.071017 0.177 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C47A 0.101(16) 0.113(18) 0.085(15) 0.010(13) 0.008(13) -0.022(14) C48A 0.058(7) 0.086(12) 0.070(9) -0.017(7) 0.034(7) -0.010(7) C49A 0.049(7) 0.111(14) 0.052(8) -0.017(8) 0.021(6) -0.002(8) C50A 0.048(7) 0.127(19) 0.047(9) -0.034(10) 0.010(7) -0.008(11) C51A 0.058(7) 0.086(12) 0.070(9) -0.017(7) 0.034(7) -0.010(7) C52A 0.049(7) 0.111(14) 0.052(8) -0.017(8) 0.021(6) -0.002(8) C53A 0.048(7) 0.127(19) 0.047(9) -0.034(10) 0.010(7) -0.008(11) C47B 0.101(16) 0.113(18) 0.085(15) 0.010(13) 0.008(13) -0.022(14) C48B 0.063(14) 0.09(2) 0.10(2) -0.045(19) 0.000(14) -0.010(13) C49B 0.07(2) 0.065(17) 0.16(3) -0.066(19) 0.05(2) -0.010(13) C50B 0.14(3) 0.19(4) 0.12(3) -0.10(3) 0.10(3) -0.09(3) C51B 0.063(14) 0.09(2) 0.10(2) -0.045(19) 0.000(14) -0.010(13) C52B 0.07(2) 0.065(17) 0.16(3) -0.066(19) 0.05(2) -0.010(13) C53B 0.14(3) 0.19(4) 0.12(3) -0.10(3) 0.10(3) -0.09(3) S1A 0.047(3) 0.0529(17) 0.0397(13) -0.0048(11) 0.011(2) 0.002(2) F1A 0.069(4) 0.067(5) 0.090(6) -0.007(4) -0.008(4) -0.005(4) F2A 0.159(14) 0.098(8) 0.103(10) -0.048(9) 0.082(11) -0.020(9) F3A 0.069(4) 0.067(5) 0.090(6) -0.007(4) -0.008(4) -0.005(4) O5A 0.056(6) 0.053(10) 0.071(6) 0.012(6) 0.016(4) 0.022(6) O6A 0.115(10) 0.087(9) 0.101(10) -0.013(7) 0.076(9) -0.001(8) O7A 0.050(6) 0.089(8) 0.047(6) -0.010(5) -0.011(4) -0.011(5) C46A 0.059(6) 0.082(9) 0.061(8) -0.009(6) 0.020(6) 0.004(6) O3A 0.015(5) 0.055(9) 0.035(6) 0.000(5) 0.005(4) -0.001(4) O4A 0.046(5) 0.053(6) 0.022(5) 0.017(6) 0.016(4) 0.007(6) C28A 0.034(9) 0.064(15) 0.019(10) 0.000(10) 0.012(8) -0.005(8) C29A 0.044(6) 0.099(13) 0.039(6) 0.007(6) 0.028(5) -0.001(6) C30A 0.044(6) 0.099(13) 0.039(6) 0.007(6) 0.028(5) -0.001(6) C31A 0.030(6) 0.044(8) 0.027(7) 0.003(5) 0.015(5) 0.011(5) C32A 0.039(4) 0.027(4) 0.026(5) 0.004(4) 0.016(4) 0.000(3) C33A 0.037(7) 0.050(8) 0.019(6) 0.002(5) 0.013(5) 0.006(6) C34A 0.040(7) 0.026(7) 0.050(8) -0.010(6) 0.021(6) -0.003(5) S1B 0.047(3) 0.0529(17) 0.0397(13) -0.0048(11) 0.011(2) 0.002(2) F1B 0.069(4) 0.067(5) 0.090(6) -0.007(4) -0.008(4) -0.005(4) F2B 0.159(14) 0.098(8) 0.103(10) -0.048(9) 0.082(11) -0.020(9) F3B 0.069(4) 0.067(5) 0.090(6) -0.007(4) -0.008(4) -0.005(4) O5B 0.056(6) 0.053(10) 0.071(6) 0.012(6) 0.016(4) 0.022(6) O6B 0.115(10) 0.087(9) 0.101(10) -0.013(7) 0.076(9) -0.001(8) O7B 0.050(6) 0.089(8) 0.047(6) -0.010(5) -0.011(4) -0.011(5) C46B 0.059(6) 0.082(9) 0.061(8) -0.009(6) 0.020(6) 0.004(6) O3B 0.040(9) 0.069(13) 0.026(8) 0.004(7) 0.021(7) -0.019(8) O4B 0.053(9) 0.054(10) 0.045(13) -0.005(10) 0.040(10) -0.015(8) C28B 0.035(12) 0.057(13) 0.039(15) -0.007(16) 0.025(11) -0.004(14) C29B 0.066(13) 0.12(2) 0.055(12) -0.023(11) 0.044(11) -0.048(13) C30B 0.066(13) 0.12(2) 0.055(12) -0.023(11) 0.044(11) -0.048(13) C31B 0.045(10) 0.043(11) 0.036(11) -0.016(8) 0.031(9) -0.003(9) C32B 0.039(4) 0.027(4) 0.026(5) 0.004(4) 0.016(4) 0.000(3) C33B 0.041(9) 0.036(10) 0.039(10) -0.007(7) 0.029(8) 0.000(7) C34B 0.058(12) 0.039(11) 0.048(11) -0.005(8) 0.036(10) -0.004(9) Pd1 0.0199(2) 0.0288(3) 0.0263(3) 0.0001(2) 0.01038(18) -0.0018(2) P1 0.0249(8) 0.0281(8) 0.0256(9) 0.0004(7) 0.0116(7) -0.0021(6) O1 0.057(4) 0.051(4) 0.028(3) -0.011(2) 0.009(3) -0.013(3) O2 0.022(3) 0.099(6) 0.043(3) 0.019(3) 0.012(3) -0.009(3) N1 0.027(3) 0.038(3) 0.032(3) -0.003(2) 0.015(3) -0.010(2) C1 0.025(3) 0.036(4) 0.028(4) 0.001(3) 0.004(3) -0.007(3) C2 0.045(4) 0.039(4) 0.029(4) 0.004(3) 0.008(4) -0.006(3) C3 0.093(8) 0.080(8) 0.028(5) -0.017(5) 0.008(5) -0.027(7) C4 0.046(5) 0.054(6) 0.036(5) 0.002(4) -0.003(4) -0.017(4) C5 0.032(4) 0.066(6) 0.047(5) 0.016(4) -0.002(4) -0.013(4) C6 0.026(4) 0.060(6) 0.037(4) 0.013(4) 0.008(3) -0.009(3) C7 0.031(4) 0.129(11) 0.071(7) 0.031(7) 0.019(5) -0.023(6) C8 0.022(3) 0.041(4) 0.037(4) 0.007(3) 0.012(3) -0.003(3) C9 0.022(3) 0.037(4) 0.032(4) 0.007(3) 0.009(3) 0.004(3) C10 0.025(3) 0.045(4) 0.046(5) 0.015(4) 0.020(3) 0.008(3) C11 0.037(4) 0.042(5) 0.052(5) 0.019(4) 0.025(4) 0.018(3) C12 0.080(7) 0.038(5) 0.056(6) 0.010(4) 0.041(5) 0.014(4) C13 0.059(6) 0.112(11) 0.085(8) 0.061(8) 0.048(6) 0.050(7) C14 0.039(4) 0.039(4) 0.044(4) 0.004(3) 0.028(4) 0.007(3) C15 0.032(3) 0.039(6) 0.040(4) 0.000(3) 0.021(3) -0.001(3) C16 0.051(4) 0.060(6) 0.037(4) 0.008(5) 0.025(3) 0.003(5) C17 0.072(6) 0.065(7) 0.055(6) -0.001(5) 0.038(5) -0.004(5) C18 0.071(6) 0.073(7) 0.058(6) 0.005(5) 0.050(5) -0.006(5) C19 0.034(4) 0.034(4) 0.039(4) 0.009(3) 0.017(3) -0.002(3) C20 0.025(3) 0.034(4) 0.034(4) 0.006(3) 0.012(3) 0.000(3) C21 0.041(4) 0.033(4) 0.036(4) -0.002(3) 0.014(4) -0.009(3) C22 0.073(6) 0.041(5) 0.049(5) 0.000(4) 0.006(5) 0.028(5) C23 0.094(7) 0.045(5) 0.059(6) -0.008(4) 0.047(6) -0.039(5) C24 0.035(4) 0.030(4) 0.038(4) 0.002(3) 0.019(3) -0.002(3) C25 0.049(4) 0.029(4) 0.059(5) 0.003(3) 0.031(4) 0.001(3) C26 0.039(4) 0.065(5) 0.030(4) 0.011(4) 0.010(4) -0.003(4) C27 0.039(4) 0.047(5) 0.029(4) 0.011(3) 0.018(3) -0.006(3) C35 0.022(3) 0.037(3) 0.029(4) -0.011(3) 0.012(3) -0.004(3) C36 0.036(4) 0.046(5) 0.034(4) -0.007(3) 0.015(3) -0.017(3) C37 0.050(5) 0.061(6) 0.050(5) -0.010(4) 0.034(4) -0.021(4) C38 0.032(4) 0.083(7) 0.054(5) -0.032(5) 0.026(4) -0.017(4) C39 0.034(4) 0.115(10) 0.084(8) -0.030(7) 0.032(5) -0.023(5) C40 0.029(4) 0.056(7) 0.084(7) -0.020(4) 0.020(4) 0.001(3) C41 0.026(3) 0.040(5) 0.053(4) -0.006(4) 0.015(3) 0.000(4) C42 0.053(5) 0.036(4) 0.052(5) -0.002(3) 0.031(4) 0.006(4) C43 0.063(6) 0.052(6) 0.042(5) -0.003(4) 0.025(5) -0.008(4) C44 0.204(19) 0.063(9) 0.076(8) -0.029(7) 0.082(11) -0.047(10) C45 0.116(12) 0.105(14) 0.126(15) -0.072(12) 0.047(12) -0.012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C47A C48A 1.489(19) . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A C49A 1.35(2) . ? C48A C53A 1.382(19) . ? C49A C50A 1.37(2) . ? C49A H49A 0.9500 . ? C50A C51A 1.366(19) . ? C50A H50A 0.9500 . ? C51A C52A 1.362(19) . ? C51A H51A 0.9500 . ? C52A C53A 1.37(2) . ? C52A H52A 0.9500 . ? C53A H53A 0.9500 . ? C47B C48B 1.48(2) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B C49B 1.35(2) . ? C48B C53B 1.36(2) . ? C49B C50B 1.37(3) . ? C49B H49B 0.9500 . ? C50B C51B 1.35(3) . ? C50B H50B 0.9500 . ? C51B C52B 1.36(3) . ? C51B H51B 0.9500 . ? C52B C53B 1.39(3) . ? C52B H52B 0.9500 . ? C53B H53B 0.9500 . ? S1A O6A 1.417(11) . ? S1A O5A 1.452(11) . ? S1A O7A 1.453(10) . ? S1A C46A 1.783(17) . ? F1A C46A 1.364(16) . ? F2A C46A 1.312(15) . ? F3A C46A 1.323(15) . ? O3A C29A 1.385(15) . ? O3A C28A 1.443(15) . ? O4A C30A 1.400(15) . ? O4A C28A 1.471(16) . ? C28A C31A 1.51(3) . ? C28A C27 1.55(2) . ? C29A C30A 1.51(2) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C31A C32A 1.543(18) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A C34A 1.527(17) . ? C32A C33A 1.536(19) . ? C32A P1 1.92(3) . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? S1B O6B 1.393(15) . ? S1B O7B 1.426(14) . ? S1B O5B 1.432(16) . ? S1B C46B 1.79(2) . ? F1B C46B 1.345(19) . ? F2B C46B 1.323(19) . ? F3B C46B 1.34(2) . ? O3B C29B 1.399(19) . ? O3B C28B 1.450(17) . ? O4B C30B 1.384(19) . ? O4B C28B 1.466(18) . ? C28B C27 1.35(3) . ? C28B C31B 1.55(4) . ? C29B C30B 1.57(3) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B C32B 1.55(2) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B C34B 1.53(2) . ? C32B C33B 1.532(19) . ? C32B P1 1.85(3) . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? Pd1 C35 2.027(6) . ? Pd1 N1 2.125(6) . ? Pd1 P1 2.3194(17) . ? Pd1 C9 2.403(7) . ? P1 C1 1.858(7) . ? P1 C24 1.890(7) . ? O1 C2 1.346(11) . ? O1 C3 1.433(11) . ? O2 C6 1.380(11) . ? O2 C7 1.430(10) . ? N1 C42 1.481(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? C1 C8 1.405(11) . ? C1 C2 1.427(11) . ? C2 C4 1.410(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.385(15) . ? C4 H4 0.9500 . ? C5 C6 1.380(14) . ? C5 H5 0.9500 . ? C6 C8 1.405(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.499(11) . ? C9 C10 1.422(11) . ? C9 C20 1.457(10) . ? C10 C14 1.377(11) . ? C10 C11 1.537(10) . ? C11 C12 1.532(14) . ? C11 C13 1.532(12) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.391(11) . ? C14 H14 0.9500 . ? C15 C19 1.389(12) . ? C15 C16 1.523(10) . ? C16 C17 1.497(16) . ? C16 C18 1.551(13) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.385(11) . ? C19 H19 0.9500 . ? C20 C21 1.489(11) . ? C21 C22 1.526(13) . ? C21 C23 1.551(11) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.528(11) . ? C24 C27 1.536(10) . ? C24 C26 1.536(11) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C35 C36 1.379(12) . ? C35 C41 1.396(11) . ? C36 C37 1.390(11) . ? C36 H36 0.9500 . ? C37 C38 1.373(15) . ? C37 H37 0.9500 . ? C38 C40 1.407(16) . ? C38 C39 1.518(12) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.401(11) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.484(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.481(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.54(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C48A C47A H47A 109.5 . . ? C48A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C48A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C49A C48A C53A 119.4(13) . . ? C49A C48A C47A 123.4(17) . . ? C53A C48A C47A 117.3(17) . . ? C48A C49A C50A 121.3(13) . . ? C48A C49A H49A 119.4 . . ? C50A C49A H49A 119.4 . . ? C51A C50A C49A 119.9(14) . . ? C51A C50A H50A 120.0 . . ? C49A C50A H50A 120.0 . . ? C52A C51A C50A 118.9(13) . . ? C52A C51A H51A 120.5 . . ? C50A C51A H51A 120.5 . . ? C51A C52A C53A 121.6(13) . . ? C51A C52A H52A 119.2 . . ? C53A C52A H52A 119.2 . . ? C52A C53A C48A 118.9(14) . . ? C52A C53A H53A 120.5 . . ? C48A C53A H53A 120.5 . . ? C48B C47B H47D 109.5 . . ? C48B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C48B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C49B C48B C53B 117(3) . . ? C49B C48B C47B 122(2) . . ? C53B C48B C47B 122(3) . . ? C48B C49B C50B 123(3) . . ? C48B C49B H49B 118.5 . . ? C50B C49B H49B 118.5 . . ? C51B C50B C49B 117(4) . . ? C51B C50B H50B 121.7 . . ? C49B C50B H50B 121.7 . . ? C50B C51B C52B 125(4) . . ? C50B C51B H51B 117.3 . . ? C52B C51B H51B 117.3 . . ? C51B C52B C53B 114(4) . . ? C51B C52B H52B 123.2 . . ? C53B C52B H52B 123.2 . . ? C48B C53B C52B 124(3) . . ? C48B C53B H53B 117.8 . . ? C52B C53B H53B 117.8 . . ? O6A S1A O5A 116.3(9) . . ? O6A S1A O7A 110.8(8) . . ? O5A S1A O7A 112.2(9) . . ? O6A S1A C46A 107.4(9) . . ? O5A S1A C46A 107.2(8) . . ? O7A S1A C46A 101.8(8) . . ? F2A C46A F3A 105.9(14) . . ? F2A C46A F1A 106.6(14) . . ? F3A C46A F1A 107.2(13) . . ? F2A C46A S1A 112.2(12) . . ? F3A C46A S1A 114.3(12) . . ? F1A C46A S1A 110.2(11) . . ? C29A O3A C28A 111.1(14) . . ? C30A O4A C28A 106.9(11) . . ? O3A C28A O4A 102.7(11) . . ? O3A C28A C31A 111.0(14) . . ? O4A C28A C31A 104.5(16) . . ? O3A C28A C27 107.7(14) . . ? O4A C28A C27 113.3(13) . . ? C31A C28A C27 116.8(11) . . ? O3A C29A C30A 101.0(12) . . ? O3A C29A H29A 111.6 . . ? C30A C29A H29A 111.6 . . ? O3A C29A H29B 111.6 . . ? C30A C29A H29B 111.6 . . ? H29A C29A H29B 109.4 . . ? O4A C30A C29A 103.0(13) . . ? O4A C30A H30A 111.2 . . ? C29A C30A H30A 111.2 . . ? O4A C30A H30B 111.2 . . ? C29A C30A H30B 111.2 . . ? H30A C30A H30B 109.1 . . ? C28A C31A C32A 114.8(14) . . ? C28A C31A H31A 108.6 . . ? C32A C31A H31A 108.6 . . ? C28A C31A H31B 108.6 . . ? C32A C31A H31B 108.6 . . ? H31A C31A H31B 107.6 . . ? C34A C32A C33A 105.0(15) . . ? C34A C32A C31A 110.2(15) . . ? C33A C32A C31A 109.0(14) . . ? C34A C32A P1 110.0(12) . . ? C33A C32A P1 111.2(12) . . ? C31A C32A P1 111.1(13) . . ? C32A C33A H33A 109.5 . . ? C32A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C32A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C32A C34A H34A 109.5 . . ? C32A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C32A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? O6B S1B O7B 118.6(15) . . ? O6B S1B O5B 118.5(16) . . ? O7B S1B O5B 115.7(16) . . ? O6B S1B C46B 103.4(16) . . ? O7B S1B C46B 101.2(15) . . ? O5B S1B C46B 92.1(16) . . ? F2B C46B F3B 105(2) . . ? F2B C46B F1B 109(2) . . ? F3B C46B F1B 104(2) . . ? F2B C46B S1B 114(2) . . ? F3B C46B S1B 112(2) . . ? F1B C46B S1B 113(2) . . ? C29B O3B C28B 107.5(18) . . ? C30B O4B C28B 109.8(17) . . ? C27 C28B O3B 114(2) . . ? C27 C28B O4B 107.0(19) . . ? O3B C28B O4B 105.3(15) . . ? C27 C28B C31B 114.1(15) . . ? O3B C28B C31B 105.0(19) . . ? O4B C28B C31B 111(2) . . ? O3B C29B C30B 104.4(19) . . ? O3B C29B H29C 110.9 . . ? C30B C29B H29C 110.9 . . ? O3B C29B H29D 110.9 . . ? C30B C29B H29D 110.9 . . ? H29C C29B H29D 108.9 . . ? O4B C30B C29B 100(2) . . ? O4B C30B H30C 111.7 . . ? C29B C30B H30C 111.7 . . ? O4B C30B H30D 111.7 . . ? C29B C30B H30D 111.7 . . ? H30C C30B H30D 109.5 . . ? C28B C31B C32B 119.0(17) . . ? C28B C31B H31C 107.6 . . ? C32B C31B H31C 107.6 . . ? C28B C31B H31D 107.6 . . ? C32B C31B H31D 107.6 . . ? H31C C31B H31D 107.0 . . ? C34B C32B C33B 108.8(19) . . ? C34B C32B C31B 108(2) . . ? C33B C32B C31B 107.8(19) . . ? C34B C32B P1 118.3(19) . . ? C33B C32B P1 107.6(16) . . ? C31B C32B P1 106.0(17) . . ? C32B C33B H33D 109.5 . . ? C32B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C32B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C32B C34B H34D 109.5 . . ? C32B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C32B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C35 Pd1 N1 80.9(2) . . ? C35 Pd1 P1 96.68(19) . . ? N1 Pd1 P1 176.07(18) . . ? C35 Pd1 C9 178.2(3) . . ? N1 Pd1 C9 97.8(2) . . ? P1 Pd1 C9 84.62(19) . . ? C32B P1 C1 111.3(8) . . ? C32B P1 C24 107.8(7) . . ? C1 P1 C24 107.1(3) . . ? C1 P1 C32A 112.3(6) . . ? C24 P1 C32A 102.2(5) . . ? C32B P1 Pd1 110.9(7) . . ? C1 P1 Pd1 103.5(2) . . ? C24 P1 Pd1 116.1(2) . . ? C32A P1 Pd1 115.7(5) . . ? C2 O1 C3 117.5(8) . . ? C6 O2 C7 117.6(8) . . ? C42 N1 Pd1 119.7(5) . . ? C42 N1 H1A 107.4 . . ? Pd1 N1 H1A 107.4 . . ? C42 N1 H1B 107.4 . . ? Pd1 N1 H1B 107.4 . . ? H1A N1 H1B 106.9 . . ? C8 C1 C2 118.7(7) . . ? C8 C1 P1 116.8(5) . . ? C2 C1 P1 124.4(6) . . ? O1 C2 C4 122.8(8) . . ? O1 C2 C1 117.4(7) . . ? C4 C2 C1 119.8(8) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 120.3(8) . . ? C5 C4 H4 119.8 . . ? C2 C4 H4 119.8 . . ? C6 C5 C4 119.9(8) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 O2 123.7(7) . . ? C5 C6 C8 121.4(8) . . ? O2 C6 C8 114.9(8) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 C6 119.7(7) . . ? C1 C8 C9 126.7(6) . . ? C6 C8 C9 113.5(7) . . ? C10 C9 C20 117.9(6) . . ? C10 C9 C8 120.1(6) . . ? C20 C9 C8 116.2(7) . . ? C10 C9 Pd1 93.3(5) . . ? C20 C9 Pd1 92.8(4) . . ? C8 C9 Pd1 107.8(4) . . ? C14 C10 C9 120.7(7) . . ? C14 C10 C11 119.1(7) . . ? C9 C10 C11 120.0(7) . . ? C12 C11 C13 110.0(9) . . ? C12 C11 C10 111.1(7) . . ? C13 C11 C10 110.6(7) . . ? C12 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? C10 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 121.6(7) . . ? C10 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C19 C15 C14 118.4(7) . . ? C19 C15 C16 119.3(7) . . ? C14 C15 C16 122.3(7) . . ? C17 C16 C15 115.4(8) . . ? C17 C16 C18 110.7(8) . . ? C15 C16 C18 108.6(7) . . ? C17 C16 H16 107.3 . . ? C15 C16 H16 107.3 . . ? C18 C16 H16 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C15 123.0(7) . . ? C20 C19 H19 118.5 . . ? C15 C19 H19 118.5 . . ? C19 C20 C9 118.1(7) . . ? C19 C20 C21 120.5(7) . . ? C9 C20 C21 121.2(7) . . ? C20 C21 C22 111.6(7) . . ? C20 C21 C23 110.7(7) . . ? C22 C21 C23 110.7(8) . . ? C20 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? C23 C21 H21 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C27 110.2(6) . . ? C25 C24 C26 105.9(7) . . ? C27 C24 C26 110.5(6) . . ? C25 C24 P1 106.9(5) . . ? C27 C24 P1 105.7(5) . . ? C26 C24 P1 117.5(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28B C27 C24 127.5(11) . . ? C24 C27 C28A 112.7(8) . . ? C24 C27 H27A 109.1 . . ? C28A C27 H27A 109.1 . . ? C24 C27 H27B 109.1 . . ? C28A C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C36 C35 C41 117.3(7) . . ? C36 C35 Pd1 122.7(6) . . ? C41 C35 Pd1 117.9(6) . . ? C35 C36 C37 122.9(8) . . ? C35 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C38 C37 C36 120.1(9) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C40 118.4(8) . . ? C37 C38 C39 120.5(11) . . ? C40 C38 C39 121.0(10) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C38 120.7(9) . . ? C41 C40 H40 119.6 . . ? C38 C40 H40 119.6 . . ? C35 C41 C40 120.5(9) . . ? C35 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? N1 C42 C43 115.8(8) . . ? N1 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? N1 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 113.3(10) . . ? C44 C43 H43A 108.9 . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 C45 114.4(13) . . ? C43 C44 H44A 108.7 . . ? C45 C44 H44A 108.7 . . ? C43 C44 H44B 108.7 . . ? C45 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _refine_diff_density_max 1.608 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.093 _shelx_res_file ; TITL XRAY5754_0m_b.res in P2(1) XRAY5754_0m_b.res created by SHELXL-2016/6 at 17:58:04 on 12-Mar-2019 CELL 1.54178 12.4741 16.7555 14.1454 90.000 115.680 90.000 ZERR 2.000 0.0004 0.0006 0.0005 0.000 0.002 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H F N O P Pd S UNIT 106 154 6 2 14 2 2 2 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 EADP F1B F3B EADP F1A F3A EADP C49B C52B EADP C50B C53B EADP C48B C51B EADP C49A C52A EADP C50A C53A EADP C48A C51A SIZE 0.20 0.60 0.80 SADI C49A C51A C51A C53A C53A C49A C48A C50A C50A C52A C52A C48A EADP C32A C32B EADP O7A O7B EADP O6A O6B EADP O5A O5B EADP C46A C46B EADP F2A F2B EADP F1A F1B EADP S1A S1B EADP C29B C30B EADP C29A C30A SADI S1A O5A S1A O6A S1A O7A S1B O5B S1B O6B S1B O7B SADI C46A F1A C46A F2A C46A F3A C46B F1B C46B F2B C46B F3B SADI C29A C30A C29B C30B SADI O3A C29A O4A C30A O3B C29B O4B C30B SADI C28A O3A C28A O4A C28B O3B C28B O4B SADI C32A C33A C32A C34A C32B C33B C32B C34B SADI C31A C32A C31B C32B SADI S1A C46A S1B C46B EADP C47A C47B DFIX 2.474 C47A C49A C47A C53A C47B C49B C47B C53B DFIX 1.507 C47A C48A C47B C48B DFIX 1.383 C48A C49A C48A C53A C48B C49B C48B C53B DFIX 1.385 C49A C50A C53A C52A C49B C50B C53B C52B DFIX 1.375 C50A C51A C51A C52A C50B C51B C51B C52B DFIX 2.421 O5A O6A O6A O7A O7A O5A O5B O6B O6B O7B O7B O5B DFIX 2.151 F1A F2A F2A F3A F3A F1A F1B F2B F2B F3B F3B F1B FLAT C47A C48A C49A C50A C51A C52A C53A FLAT C47B C48B C49B C50B C51B C52B C53B SIMU C47A C48A ISOR C47B C48B C49B C50B C51B C52B C53B TEMP -173.0 WGHT 0.100000 0.616960 FVAR 0.41369 0.57677 0.66257 0.59639 PART 1 MOLE 1 C47A 1 0.964022 0.167417 -0.002993 41.00000 0.10134 0.11261 = 0.08458 0.00985 0.00752 -0.02232 AFIX 137 H47A 2 1.040154 0.171041 -0.007372 41.00000 -1.50000 H47B 2 0.939178 0.220817 0.007734 41.00000 -1.50000 H47C 2 0.903710 0.144841 -0.068317 41.00000 -1.50000 AFIX 0 C48A 1 0.977735 0.115059 0.086638 41.00000 0.05795 0.08602 = 0.07034 -0.01668 0.03374 -0.01018 C49A 1 1.025975 0.041277 0.101405 41.00000 0.04941 0.11052 = 0.05229 -0.01744 0.02091 -0.00170 AFIX 43 H49A 2 1.052593 0.020815 0.052624 41.00000 -1.20000 AFIX 0 C50A 1 1.037269 -0.004693 0.185546 41.00000 0.04817 0.12678 = 0.04742 -0.03405 0.00980 -0.00793 AFIX 43 H50A 2 1.073124 -0.055938 0.195521 41.00000 -1.20000 AFIX 0 C51A 1 0.996870 0.023358 0.254920 41.00000 0.05795 0.08602 = 0.07034 -0.01668 0.03374 -0.01018 AFIX 43 H51A 2 1.003711 -0.008172 0.313086 41.00000 -1.20000 AFIX 0 C52A 1 0.946623 0.097268 0.239331 41.00000 0.04941 0.11052 = 0.05229 -0.01744 0.02091 -0.00170 AFIX 43 H52A 2 0.918636 0.117081 0.287499 41.00000 -1.20000 AFIX 0 C53A 1 0.935452 0.143813 0.155701 41.00000 0.04817 0.12678 = 0.04742 -0.03405 0.00980 -0.00793 AFIX 43 H53A 2 0.899253 0.194957 0.145446 41.00000 -1.20000 PART 2 AFIX 0 C47B 1 1.085717 -0.040748 0.253910 -41.00000 0.10134 0.11261 = 0.08458 0.00985 0.00752 -0.02232 AFIX 137 H47D 2 1.147932 -0.025839 0.322886 -41.00000 -1.50000 H47E 2 1.118472 -0.078008 0.219798 -41.00000 -1.50000 H47F 2 1.019807 -0.066320 0.262462 -41.00000 -1.50000 AFIX 0 C48B 1 1.041895 0.031521 0.188438 -41.00000 0.06264 0.08600 = 0.10459 -0.04547 0.00043 -0.00984 C49B 1 1.050664 0.039827 0.097026 -41.00000 0.07420 0.06478 = 0.16108 -0.06649 0.05029 -0.01042 AFIX 43 H49B 2 1.088713 -0.001190 0.076417 -41.00000 -1.20000 AFIX 0 C50B 1 1.007176 0.104699 0.032771 -41.00000 0.13748 0.18713 = 0.11765 -0.09519 0.10126 -0.09167 AFIX 43 H50B 2 1.014295 0.109529 -0.031184 -41.00000 -1.20000 AFIX 0 C51B 1 0.953474 0.161629 0.065162 -41.00000 0.06264 0.08600 = 0.10459 -0.04547 0.00043 -0.00984 AFIX 43 H51B 2 0.915762 0.204192 0.018035 -41.00000 -1.20000 AFIX 0 C52B 1 0.949036 0.162931 0.159830 -41.00000 0.07420 0.06478 = 0.16108 -0.06649 0.05029 -0.01042 AFIX 43 H52B 2 0.916691 0.206131 0.182556 -41.00000 -1.20000 AFIX 0 C53B 1 0.996497 0.094820 0.219947 -41.00000 0.13748 0.18713 = 0.11765 -0.09519 0.10126 -0.09167 AFIX 43 H53B 2 0.997328 0.092248 0.287352 -41.00000 -1.20000 PART 1 AFIX 0 S1A 8 0.702827 0.357581 0.977225 31.00000 0.04732 0.05291 = 0.03970 -0.00484 0.01113 0.00248 F1A 3 0.828268 0.486000 1.047981 31.00000 0.06901 0.06712 = 0.09019 -0.00741 -0.00801 -0.00490 F2A 3 0.684066 0.472441 1.090840 31.00000 0.15884 0.09810 = 0.10281 -0.04829 0.08216 -0.01955 F3A 3 0.646154 0.508580 0.937158 31.00000 0.06901 0.06712 = 0.09019 -0.00741 -0.00801 -0.00490 O5A 5 0.778701 0.312978 1.070357 31.00000 0.05597 0.05297 = 0.07060 0.01224 0.01585 0.02206 O6A 5 0.730783 0.351823 0.890473 31.00000 0.11512 0.08656 = 0.10063 -0.01305 0.07643 -0.00136 O7A 5 0.577427 0.341699 0.945417 31.00000 0.04977 0.08948 = 0.04723 -0.01046 -0.01122 -0.01105 C46A 1 0.713853 0.460205 1.013733 31.00000 0.05872 0.08204 = 0.06112 -0.00950 0.01977 0.00422 O3A 5 0.347221 0.764216 0.688241 21.00000 0.01523 0.05489 = 0.03495 -0.00018 0.00469 -0.00122 O4A 5 0.517146 0.752075 0.839484 21.00000 0.04574 0.05329 = 0.02164 0.01667 0.01576 0.00652 C28A 1 0.474820 0.763389 0.725791 21.00000 0.03429 0.06413 = 0.01909 0.00037 0.01160 -0.00463 C29A 1 0.315869 0.766380 0.770923 21.00000 0.04409 0.09914 = 0.03902 0.00714 0.02829 -0.00131 AFIX 23 H29A 2 0.240395 0.737600 0.753839 21.00000 -1.20000 H29B 2 0.308716 0.821873 0.791537 21.00000 -1.20000 AFIX 0 C30A 1 0.420367 0.723906 0.855095 21.00000 0.04409 0.09914 = 0.03902 0.00714 0.02829 -0.00131 AFIX 23 H30A 2 0.428574 0.737992 0.925887 21.00000 -1.20000 H30B 2 0.412259 0.665287 0.846054 21.00000 -1.20000 AFIX 0 C31A 1 0.520575 0.844880 0.715432 21.00000 0.03014 0.04389 = 0.02721 0.00284 0.01491 0.01068 AFIX 23 H31A 2 0.602563 0.850959 0.771269 21.00000 -1.20000 H31B 2 0.470618 0.885893 0.727354 21.00000 -1.20000 AFIX 0 C32A 1 0.521744 0.861120 0.608522 21.00000 0.03903 0.02728 = 0.02603 0.00379 0.01630 0.00034 C33A 1 0.393251 0.860686 0.522520 21.00000 0.03694 0.05033 = 0.01949 0.00169 0.01275 0.00623 AFIX 137 H33A 2 0.346950 0.901549 0.538035 21.00000 -1.50000 H33B 2 0.357657 0.808139 0.520115 21.00000 -1.50000 H33C 2 0.393163 0.872094 0.454536 21.00000 -1.50000 AFIX 0 C34A 1 0.567571 0.945279 0.606291 21.00000 0.03961 0.02644 = 0.04997 -0.01022 0.02100 -0.00275 AFIX 137 H34A 2 0.518810 0.984096 0.622065 21.00000 -1.50000 H34B 2 0.562870 0.956180 0.536531 21.00000 -1.50000 H34C 2 0.650442 0.949570 0.658846 21.00000 -1.50000 PART 2 AFIX 0 S1B 8 0.749729 0.362783 0.975645 -31.00000 0.04732 0.05291 = 0.03970 -0.00484 0.01113 0.00248 F1B 3 0.813491 0.501391 1.071613 -31.00000 0.06901 0.06712 = 0.09019 -0.00741 -0.00801 -0.00490 F2B 3 0.625887 0.472280 1.016708 -31.00000 0.15884 0.09810 = 0.10281 -0.04829 0.08216 -0.01955 F3B 3 0.694284 0.509160 0.911626 -31.00000 0.06901 0.06712 = 0.09019 -0.00741 -0.00801 -0.00490 O5B 5 0.764624 0.339329 1.077955 -31.00000 0.05597 0.05297 = 0.07060 0.01224 0.01585 0.02206 O6B 5 0.850392 0.368935 0.957146 -31.00000 0.11512 0.08656 = 0.10063 -0.01305 0.07643 -0.00136 O7B 5 0.639763 0.340364 0.890891 -31.00000 0.04977 0.08948 = 0.04723 -0.01046 -0.01122 -0.01105 C46B 1 0.719496 0.464253 0.996634 -31.00000 0.05872 0.08204 = 0.06112 -0.00950 0.01977 0.00422 O3B 5 0.317610 0.725019 0.658505 -21.00000 0.04046 0.06901 = 0.02625 0.00353 0.02124 -0.01882 O4B 5 0.489356 0.782193 0.784682 -21.00000 0.05251 0.05438 = 0.04497 -0.00540 0.04034 -0.01527 C28B 1 0.435505 0.751945 0.676751 -21.00000 0.03538 0.05696 = 0.03896 -0.00685 0.02517 -0.00404 C29B 1 0.311284 0.726773 0.754863 -21.00000 0.06622 0.12133 = 0.05491 -0.02321 0.04355 -0.04820 AFIX 23 H29C 2 0.333922 0.674491 0.790704 -21.00000 -1.20000 H29D 2 0.229936 0.740467 0.745116 -21.00000 -1.20000 AFIX 0 C30B 1 0.402259 0.793196 0.819297 -21.00000 0.06622 0.12133 = 0.05491 -0.02321 0.04355 -0.04820 AFIX 23 H30C 2 0.366661 0.847141 0.801849 -21.00000 -1.20000 H30D 2 0.433442 0.784186 0.895790 -21.00000 -1.20000 AFIX 0 C31B 1 0.413995 0.819875 0.596667 -21.00000 0.04529 0.04267 = 0.03633 -0.01575 0.03057 -0.00307 AFIX 23 H31C 2 0.363999 0.860648 0.608975 -21.00000 -1.20000 H31D 2 0.366567 0.797575 0.525819 -21.00000 -1.20000 AFIX 0 C32B 1 0.522446 0.863251 0.594578 -21.00000 0.03903 0.02728 = 0.02603 0.00379 0.01630 0.00034 C33B 1 0.477379 0.915134 0.495714 -21.00000 0.04063 0.03617 = 0.03906 -0.00656 0.02930 0.00029 AFIX 137 H33D 2 0.455469 0.880961 0.433881 -21.00000 -1.50000 H33E 2 0.540237 0.952148 0.500194 -21.00000 -1.50000 H33F 2 0.407596 0.945488 0.489814 -21.00000 -1.50000 AFIX 0 C34B 1 0.575585 0.917315 0.690655 -21.00000 0.05776 0.03894 = 0.04756 -0.00518 0.03616 -0.00421 AFIX 137 H34D 2 0.511522 0.945679 0.699017 -21.00000 -1.50000 H34E 2 0.629160 0.956066 0.681464 -21.00000 -1.50000 H34F 2 0.620217 0.884938 0.753216 -21.00000 -1.50000 PART 0 AFIX 0 PD1 7 0.550100 0.746907 0.405447 11.00000 0.01986 0.02879 = 0.02631 0.00007 0.01038 -0.00179 P1 6 0.617701 0.784154 0.579786 11.00000 0.02490 0.02811 = 0.02558 0.00040 0.01162 -0.00208 O1 5 0.799717 0.869196 0.782131 11.00000 0.05670 0.05057 = 0.02777 -0.01071 0.00901 -0.01341 O2 5 0.964442 0.825100 0.482454 11.00000 0.02189 0.09902 = 0.04329 0.01893 0.01217 -0.00926 N1 4 0.477761 0.717788 0.243388 11.00000 0.02744 0.03788 = 0.03180 -0.00291 0.01462 -0.00973 AFIX 23 H1A 2 0.409959 0.746812 0.210200 11.00000 -1.20000 H1B 2 0.530051 0.735196 0.218802 11.00000 -1.20000 AFIX 0 C1 1 0.770501 0.821509 0.614943 11.00000 0.02463 0.03591 = 0.02777 0.00100 0.00374 -0.00697 C2 1 0.846746 0.855154 0.714201 11.00000 0.04515 0.03903 = 0.02897 0.00363 0.00821 -0.00586 C3 1 0.876329 0.902569 0.882087 11.00000 0.09334 0.07992 = 0.02810 -0.01659 0.00798 -0.02658 AFIX 137 H3A 2 0.943664 0.866570 0.918671 11.00000 -1.50000 H3B 2 0.831828 0.909453 0.924092 11.00000 -1.50000 H3C 2 0.905883 0.954503 0.871845 11.00000 -1.50000 AFIX 0 C4 1 0.965774 0.873502 0.736848 11.00000 0.04612 0.05380 = 0.03627 0.00169 -0.00288 -0.01688 AFIX 43 H4 2 1.017409 0.894074 0.803831 11.00000 -1.20000 AFIX 0 C5 1 1.007745 0.861668 0.661873 11.00000 0.03153 0.06589 = 0.04654 0.01590 -0.00171 -0.01268 AFIX 43 H5 2 1.088450 0.872986 0.677991 11.00000 -1.20000 AFIX 0 C6 1 0.932233 0.833428 0.563771 11.00000 0.02567 0.06041 = 0.03678 0.01259 0.00802 -0.00912 C7 1 1.083833 0.845284 0.502640 11.00000 0.03136 0.12882 = 0.07085 0.03061 0.01944 -0.02273 AFIX 137 H7A 2 1.103604 0.898014 0.535725 11.00000 -1.50000 H7B 2 1.091149 0.846243 0.436409 11.00000 -1.50000 H7C 2 1.138556 0.805428 0.549618 11.00000 -1.50000 AFIX 0 C8 1 0.814168 0.812162 0.539263 11.00000 0.02178 0.04144 = 0.03694 0.00696 0.01185 -0.00278 C9 1 0.744582 0.786708 0.427417 11.00000 0.02183 0.03666 = 0.03233 0.00726 0.00857 0.00403 C10 1 0.768045 0.711813 0.392893 11.00000 0.02535 0.04518 = 0.04628 0.01483 0.01994 0.00847 C11 1 0.824029 0.643806 0.472065 11.00000 0.03708 0.04191 = 0.05180 0.01884 0.02494 0.01770 AFIX 13 H11 2 0.828645 0.661118 0.541384 11.00000 -1.20000 AFIX 0 C12 1 0.748016 0.568076 0.437914 11.00000 0.08003 0.03835 = 0.05640 0.00968 0.04077 0.01417 AFIX 137 H12A 2 0.760176 0.541991 0.381310 11.00000 -1.50000 H12B 2 0.663903 0.582209 0.412899 11.00000 -1.50000 H12C 2 0.771328 0.531569 0.497681 11.00000 -1.50000 AFIX 0 C13 1 0.950423 0.626181 0.485619 11.00000 0.05851 0.11154 = 0.08498 0.06083 0.04804 0.04968 AFIX 137 H13A 2 0.947196 0.605748 0.419522 11.00000 -1.50000 H13B 2 0.987293 0.586183 0.540896 11.00000 -1.50000 H13C 2 0.997618 0.675341 0.505109 11.00000 -1.50000 AFIX 0 C14 1 0.749416 0.701068 0.290374 11.00000 0.03901 0.03896 = 0.04406 0.00408 0.02779 0.00670 AFIX 43 H14 2 0.763167 0.650010 0.268549 11.00000 -1.20000 AFIX 0 C15 1 0.710962 0.763167 0.218051 11.00000 0.03218 0.03862 = 0.04002 0.00038 0.02086 -0.00117 C16 1 0.703379 0.755182 0.108069 11.00000 0.05101 0.05976 = 0.03727 0.00802 0.02475 0.00277 AFIX 13 H16 2 0.630956 0.784975 0.059432 11.00000 -1.20000 AFIX 0 C17 1 0.692252 0.671617 0.067351 11.00000 0.07198 0.06473 = 0.05547 -0.00112 0.03782 -0.00378 AFIX 137 H17A 2 0.762821 0.640890 0.112475 11.00000 -1.50000 H17B 2 0.685489 0.672652 -0.004294 11.00000 -1.50000 H17C 2 0.621164 0.646619 0.067224 11.00000 -1.50000 AFIX 0 C18 1 0.812664 0.797481 0.105411 11.00000 0.07147 0.07258 = 0.05839 0.00548 0.04971 -0.00612 AFIX 137 H18A 2 0.885243 0.768404 0.150067 11.00000 -1.50000 H18B 2 0.817671 0.852259 0.131279 11.00000 -1.50000 H18C 2 0.804115 0.798501 0.033208 11.00000 -1.50000 AFIX 0 C19 1 0.681235 0.835405 0.248735 11.00000 0.03389 0.03440 = 0.03873 0.00854 0.01745 -0.00249 AFIX 43 H19 2 0.648298 0.876293 0.197685 11.00000 -1.20000 AFIX 0 C20 1 0.697400 0.850569 0.350337 11.00000 0.02478 0.03413 = 0.03368 0.00605 0.01160 0.00015 C21 1 0.674828 0.931678 0.380892 11.00000 0.04106 0.03271 = 0.03581 -0.00216 0.01423 -0.00850 AFIX 13 H21 2 0.682681 0.928532 0.454213 11.00000 -1.20000 AFIX 0 C22 1 0.549264 0.960463 0.310284 11.00000 0.07324 0.04081 = 0.04918 -0.00028 0.00582 0.02829 AFIX 137 H22A 2 0.539039 0.963569 0.237673 11.00000 -1.50000 H22B 2 0.536874 1.013383 0.333359 11.00000 -1.50000 H22C 2 0.491222 0.922925 0.314465 11.00000 -1.50000 AFIX 0 C23 1 0.768779 0.992001 0.380105 11.00000 0.09357 0.04461 = 0.05931 -0.00794 0.04722 -0.03931 AFIX 137 H23A 2 0.848543 0.973558 0.428022 11.00000 -1.50000 H23B 2 0.754158 1.044461 0.402862 11.00000 -1.50000 H23C 2 0.762987 0.996092 0.308935 11.00000 -1.50000 AFIX 0 C24 1 0.630914 0.701482 0.675119 11.00000 0.03509 0.03009 = 0.03751 0.00173 0.01921 -0.00198 C25 1 0.663593 0.625623 0.633626 11.00000 0.04852 0.02924 = 0.05943 0.00343 0.03095 0.00051 AFIX 137 H25A 2 0.654013 0.579263 0.671513 11.00000 -1.50000 H25B 2 0.746446 0.628993 0.644122 11.00000 -1.50000 H25C 2 0.611283 0.619947 0.558625 11.00000 -1.50000 AFIX 0 C26 1 0.725663 0.710768 0.788811 11.00000 0.03883 0.06534 = 0.03017 0.01137 0.01011 -0.00290 AFIX 137 H26A 2 0.705522 0.756416 0.821363 11.00000 -1.50000 H26B 2 0.803548 0.719659 0.789293 11.00000 -1.50000 H26C 2 0.728359 0.662154 0.828302 11.00000 -1.50000 AFIX 0 C27 1 0.506659 0.693056 0.671693 11.00000 0.03907 0.04695 = 0.02946 0.01129 0.01754 -0.00551 AFIX 23 H27A 2 0.503037 0.642605 0.706622 11.00000 -1.20000 H27B 2 0.446790 0.689900 0.597625 11.00000 -1.20000 AFIX 0 C35 1 0.386354 0.710283 0.384424 11.00000 0.02166 0.03729 = 0.02908 -0.01083 0.01222 -0.00410 C36 1 0.364864 0.634699 0.410820 11.00000 0.03570 0.04622 = 0.03431 -0.00693 0.01524 -0.01668 AFIX 43 H36 2 0.430554 0.603425 0.456234 11.00000 -1.20000 AFIX 0 C37 1 0.251360 0.602233 0.373935 11.00000 0.05038 0.06066 = 0.05008 -0.00993 0.03402 -0.02111 AFIX 43 H37 2 0.240804 0.550045 0.394771 11.00000 -1.20000 AFIX 0 C38 1 0.154524 0.645475 0.307452 11.00000 0.03242 0.08305 = 0.05402 -0.03216 0.02641 -0.01714 C39 1 0.030961 0.608940 0.262281 11.00000 0.03356 0.11497 = 0.08391 -0.02977 0.03246 -0.02296 AFIX 137 H39A 2 0.004996 0.597533 0.187617 11.00000 -1.50000 H39B 2 -0.024659 0.646446 0.270556 11.00000 -1.50000 H39C 2 0.032791 0.559259 0.299512 11.00000 -1.50000 AFIX 0 C40 1 0.173436 0.722655 0.278439 11.00000 0.02922 0.05583 = 0.08366 -0.02013 0.02038 0.00108 AFIX 43 H40 2 0.107577 0.753300 0.231983 11.00000 -1.20000 AFIX 0 C41 1 0.288295 0.754803 0.317296 11.00000 0.02631 0.04041 = 0.05338 -0.00556 0.01453 0.00027 AFIX 43 H41 2 0.299517 0.807292 0.297808 11.00000 -1.20000 AFIX 0 C42 1 0.448657 0.633710 0.209814 11.00000 0.05315 0.03581 = 0.05163 -0.00204 0.03115 0.00628 AFIX 23 H42A 2 0.393401 0.613468 0.237635 11.00000 -1.20000 H42B 2 0.522610 0.601834 0.242344 11.00000 -1.20000 AFIX 0 C43 1 0.394310 0.619619 0.094896 11.00000 0.06333 0.05206 = 0.04195 -0.00303 0.02510 -0.00817 AFIX 23 H43A 2 0.316586 0.647300 0.062448 11.00000 -1.20000 H43B 2 0.446162 0.643272 0.065567 11.00000 -1.20000 AFIX 0 C44 1 0.376145 0.533996 0.066343 11.00000 0.20378 0.06349 = 0.07565 -0.02900 0.08230 -0.04657 AFIX 23 H44A 2 0.315329 0.512426 0.086798 11.00000 -1.20000 H44B 2 0.451392 0.505091 0.107333 11.00000 -1.20000 AFIX 0 C45 1 0.336688 0.517002 -0.050960 11.00000 0.11610 0.10536 = 0.12606 -0.07227 0.04709 -0.01200 AFIX 137 H45A 2 0.262916 0.546045 -0.092521 11.00000 -1.50000 H45B 2 0.323097 0.459614 -0.064034 11.00000 -1.50000 H45C 2 0.398929 0.534527 -0.071017 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY5754_0m_b.res in P2(1) REM R1 = 0.0484 for 7852 Fo > 4sig(Fo) and 0.0501 for all 8167 data REM 727 parameters refined using 153 restraints END WGHT 0.0934 1.7146 REM Highest difference peak 1.608, deepest hole -1.038, 1-sigma level 0.093 Q1 1 0.6164 0.7467 0.3914 11.00000 0.05 1.61 Q2 1 0.4801 0.7494 0.4227 11.00000 0.05 1.56 Q3 1 0.8450 0.4006 0.9990 11.00000 0.05 0.55 Q4 1 0.6985 0.7840 0.5781 11.00000 0.05 0.50 Q5 1 0.4199 0.4902 0.0429 11.00000 0.05 0.44 Q6 1 0.5502 0.7990 0.5913 11.00000 0.05 0.43 Q7 1 0.5382 0.3950 1.0040 11.00000 0.05 0.39 Q8 1 0.5246 0.7485 0.3245 11.00000 0.05 0.38 Q9 1 0.7162 0.7170 0.4179 11.00000 0.05 0.36 Q10 1 0.5906 0.4980 0.9587 11.00000 0.05 0.35 Q11 1 0.8413 0.1014 0.0076 11.00000 0.05 0.34 Q12 1 0.1054 0.5436 0.1999 11.00000 0.05 0.34 Q13 1 0.5534 0.6753 0.6667 11.00000 0.05 0.33 Q14 1 0.6060 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163.28 14.60 7 -12 -7 146.19 13.90 7 -12 -7 177.08 13.00 -7 -12 7 167.18 15.00 7 12 -7 169.88 14.90 7 12 -7 156.28 15.20 7 12 -7 156.68 13.00 6 -12 -7 98.99 9.50 6 -12 -7 108.79 9.30 6 -12 -7 93.69 11.10 6 -12 -7 118.09 12.10 6 12 -7 107.19 9.90 6 12 -7 121.29 11.80 6 12 -7 123.59 13.00 5 -12 -7 142.99 11.00 5 -12 -7 130.19 11.50 5 12 -7 127.69 11.30 5 12 -7 135.99 10.70 4 -12 -7 93.99 7.80 4 -12 -7 80.89 7.90 -4 -12 7 86.99 8.80 4 12 -7 72.99 6.90 4 12 -7 64.69 7.80 -3 -12 7 82.49 8.60 3 -12 -7 78.69 8.10 3 -12 -7 81.79 7.40 3 12 -7 74.89 6.60 3 12 -7 75.59 7.40 -2 -12 7 9.40 3.80 2 -12 -7 8.30 3.20 2 12 -7 3.10 3.80 2 12 -7 6.60 2.60 2 12 -7 9.00 2.10 1 -12 -7 4.60 2.80 -1 -12 7 0.60 3.10 -1 -12 7 3.10 3.20 1 12 -7 1.40 1.70 1 12 -7 -2.90 3.40 1 12 -7 0.20 2.40 0 -12 -7 12.70 3.70 0 -12 7 14.80 3.70 0 -12 7 16.40 4.00 0 12 -7 16.60 2.60 0 12 -7 16.20 3.10 1 -12 7 97.29 9.50 1 -12 7 104.59 9.60 -1 12 -7 109.19 8.50 -1 12 -7 127.69 12.00 -1 12 -7 106.09 11.40 -1 12 -7 106.49 11.70 -1 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23.60 3 8 -8 335.17 24.60 3 8 -8 352.06 24.20 3 8 -8 324.27 24.90 3 8 -8 354.06 23.40 2 -8 -8 91.39 7.90 2 -8 -8 76.69 8.00 2 8 -8 84.19 8.30 2 8 -8 85.79 7.70 2 8 -8 81.89 7.00 2 8 -8 91.09 6.90 2 8 -8 82.99 8.80 2 8 -8 91.49 7.90 -1 -8 8 74.89 6.80 1 -8 -8 76.79 7.30 1 8 -8 61.29 6.80 1 8 -8 59.89 5.30 1 8 -8 60.79 6.20 1 8 -8 56.39 5.70 1 8 -8 61.49 6.40 1 8 -8 62.49 7.30 0 -8 8 121.29 10.10 0 -8 -8 119.09 11.00 0 8 -8 125.29 9.90 0 8 -8 117.19 9.20 0 8 -8 122.59 9.90 0 8 -8 122.09 10.60 0 8 -8 114.09 9.00 0 8 -8 122.19 10.30 -1 8 -8 35.70 5.30 -1 8 -8 33.80 3.90 -1 8 -8 35.50 4.00 -1 8 -8 35.50 4.70 -1 8 -8 34.20 5.00 -1 8 -8 32.50 4.60 2 -8 8 139.99 10.80 2 -8 8 152.38 10.90 -2 8 -8 126.49 10.70 -2 8 -8 118.29 10.60 -2 8 -8 123.79 10.80 -2 8 -8 126.59 9.90 -2 8 -8 124.69 10.50 -2 8 -8 126.59 9.70 3 -8 8 249.88 17.80 3 -8 8 262.97 17.90 -3 8 -8 230.98 17.90 -3 8 -8 221.48 17.80 -3 8 -8 240.88 17.20 -3 8 -8 247.98 18.50 -3 8 -8 247.68 20.00 -3 8 -8 226.78 17.20 -3 8 -8 234.48 17.90 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10.10 7 9 -8 113.19 9.90 6 -9 -8 34.80 5.20 6 -9 -8 32.50 4.70 6 -9 -8 39.70 4.80 6 9 -8 35.20 5.40 6 9 -8 32.50 4.50 6 9 -8 32.20 4.60 5 -9 -8 27.60 5.20 5 -9 -8 31.60 4.50 5 9 -8 28.10 4.90 5 9 -8 32.50 4.60 5 9 -8 34.50 4.10 -4 -9 8 6.70 3.30 4 -9 -8 5.60 2.70 4 -9 -8 3.60 2.60 4 9 -8 5.80 2.90 4 9 -8 5.40 3.60 4 9 -8 10.50 2.10 4 9 -8 9.40 2.60 3 -9 -8 3.90 2.60 -3 -9 8 6.00 3.40 3 -9 -8 3.50 2.70 3 9 -8 4.00 2.20 3 9 -8 1.60 2.40 3 9 -8 4.60 1.70 3 9 -8 1.50 3.60 3 9 -8 -0.30 3.80 2 9 -8 74.09 6.60 2 9 -8 81.19 7.30 2 9 -8 76.69 8.00 2 9 -8 77.69 7.60 2 9 -8 73.39 8.50 2 9 -8 82.39 6.40 -1 -9 8 101.79 8.30 1 -9 -8 88.09 8.50 -1 -9 8 93.49 8.80 1 9 -8 76.09 6.70 1 9 -8 81.39 8.90 1 9 -8 81.09 7.60 1 9 -8 79.99 7.10 1 9 -8 86.29 8.40 1 9 -8 82.79 7.90 0 -9 8 171.88 13.80 0 -9 -8 172.28 14.20 0 -9 8 176.98 13.50 0 9 -8 159.88 12.50 0 9 -8 171.68 13.30 0 9 -8 171.58 13.70 0 9 -8 172.38 13.40 0 9 -8 172.38 14.00 0 9 -8 162.78 12.30 1 -9 8 263.77 19.90 1 -9 8 255.17 19.90 -1 9 -8 269.27 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11.80 3 10 -8 145.49 13.50 2 -10 -8 113.89 9.00 2 10 -8 90.19 8.10 2 10 -8 81.19 8.70 2 10 -8 84.69 7.40 2 10 -8 94.59 7.30 2 10 -8 72.39 9.20 1 -10 -8 110.39 9.30 -1 -10 8 107.99 9.60 -1 -10 8 106.39 8.80 1 10 -8 82.39 9.20 1 10 -8 92.19 9.50 1 10 -8 85.99 7.50 1 10 -8 82.79 8.30 1 10 -8 89.69 7.40 1 10 -8 88.59 8.20 0 -10 -8 50.89 6.80 0 -10 8 44.70 6.00 0 -10 8 46.10 6.60 0 10 -8 39.50 5.30 0 10 -8 43.00 6.40 0 10 -8 45.50 5.20 0 10 -8 42.60 4.60 0 10 -8 45.30 6.90 0 10 -8 46.10 4.40 1 -10 8 28.70 4.60 1 -10 8 28.00 5.00 -1 10 -8 22.70 3.30 -1 10 -8 21.70 3.20 -1 10 -8 27.60 5.00 -1 10 -8 20.90 3.70 -1 10 -8 21.50 4.20 -1 10 -8 21.20 4.20 2 -10 8 147.69 11.10 2 -10 8 144.79 10.90 2 -10 8 148.69 11.10 -2 10 -8 136.79 10.10 -2 10 -8 129.09 11.10 -2 10 -8 134.69 11.40 -2 10 -8 118.89 12.50 -2 10 -8 130.99 12.10 -2 10 -8 123.89 10.20 -2 10 -8 131.89 11.60 -2 10 -8 122.39 12.30 -2 10 -8 129.49 10.20 -2 10 -8 128.39 10.70 -2 10 -8 139.89 13.40 -2 10 -8 133.39 11.10 -2 10 -8 132.79 10.80 3 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382.96 26.00 1 -11 8 384.26 25.70 -1 11 -8 333.97 25.40 -1 11 -8 343.27 25.90 -1 11 -8 384.26 28.20 -1 11 -8 325.57 25.40 -1 11 -8 338.97 27.90 -1 11 -8 332.37 24.90 -1 11 -8 380.56 28.30 -1 11 -8 357.86 27.00 -1 11 -8 359.36 26.50 -1 11 -8 366.16 26.20 -1 11 -8 344.97 24.80 -1 11 -8 332.67 25.10 2 -11 8 329.47 24.30 2 -11 8 297.57 24.00 2 -11 8 303.27 24.10 -2 11 -8 321.97 23.50 -2 11 -8 338.07 24.10 -2 11 -8 364.16 25.80 -2 11 -8 328.77 23.70 -2 11 -8 371.26 26.20 -2 11 -8 332.47 24.00 -2 11 -8 333.17 23.40 -2 11 -8 335.27 24.90 -2 11 -8 378.86 26.70 -2 11 -8 324.87 24.30 -3 11 -8 53.29 7.60 -3 11 -8 40.80 6.40 -3 11 -8 46.70 6.10 -3 11 -8 31.00 7.00 -3 11 -8 41.30 4.40 -3 11 -8 45.70 6.70 -3 11 -8 43.00 5.30 -3 11 -8 42.90 4.70 -4 11 -8 11.30 3.30 -4 11 -8 11.20 2.00 -4 11 -8 10.30 3.80 -4 11 -8 18.10 2.70 -4 11 -8 13.30 5.10 -4 11 -8 17.00 3.00 -4 11 -8 11.30 4.00 -5 11 -8 12.30 2.30 -5 11 -8 12.90 3.10 -5 11 -8 6.80 3.40 -5 11 -8 8.10 2.20 -5 11 -8 15.40 3.90 -5 11 -8 8.10 4.30 11 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16.90 5 8 -9 244.28 17.50 4 -8 -9 109.99 8.70 4 8 -9 83.49 7.90 4 8 -9 95.99 9.30 4 8 -9 86.49 7.30 4 8 -9 76.19 8.30 3 -8 -9 511.05 36.80 3 -8 -9 566.54 36.80 3 8 -9 497.25 37.10 3 8 -9 497.65 35.70 3 8 -9 537.05 36.80 3 8 -9 503.75 37.30 3 8 -9 518.45 36.60 3 8 -9 506.65 36.00 2 -8 -9 509.85 39.10 2 -8 -9 566.44 39.00 2 8 -9 587.74 39.00 2 8 -9 549.25 38.20 2 8 -9 561.54 38.80 2 8 -9 551.14 39.40 2 8 -9 530.55 39.70 2 8 -9 555.74 38.00 1 -8 -9 145.39 12.30 -1 -8 9 151.68 11.80 1 8 -9 134.29 11.50 1 8 -9 133.79 10.40 1 8 -9 146.09 12.00 1 8 -9 145.89 11.60 1 8 -9 128.99 12.30 1 8 -9 134.39 10.60 0 -8 9 66.59 7.40 0 -8 9 71.39 7.10 0 -8 -9 78.89 8.00 0 8 -9 65.09 7.20 0 8 -9 64.39 6.60 0 8 -9 64.49 6.70 0 8 -9 66.09 5.70 0 8 -9 58.09 6.00 0 8 -9 66.69 7.60 1 -8 9 32.80 5.80 1 -8 9 32.10 5.10 -1 8 -9 35.10 4.80 -1 8 -9 40.80 4.30 -1 8 -9 44.60 6.00 -1 8 -9 41.10 5.20 -1 8 -9 41.90 4.10 -1 8 -9 36.90 5.30 2 -8 9 26.00 4.80 2 -8 9 27.10 4.40 -2 8 -9 21.60 3.90 -2 8 -9 25.80 6.40 -2 8 -9 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27.60 4.30 7 -10 -9 24.20 5.90 7 -10 -9 27.60 6.10 7 10 -9 28.70 7.00 7 10 -9 33.00 4.50 7 10 -9 26.00 4.10 7 10 -9 28.10 4.40 6 -10 -9 125.19 10.40 6 -10 -9 110.29 10.70 6 10 -9 134.49 10.70 6 10 -9 128.79 10.70 6 10 -9 145.39 12.30 5 -10 -9 101.39 10.30 5 -10 -9 109.89 9.70 5 10 -9 123.39 9.70 5 10 -9 131.09 9.40 5 10 -9 118.09 10.10 4 -10 -9 169.58 12.30 4 10 -9 132.59 12.20 4 10 -9 137.19 10.70 4 10 -9 130.39 11.50 4 10 -9 124.59 11.00 3 -10 -9 411.56 30.60 -3 -10 9 415.76 31.50 3 -10 -9 383.36 30.80 3 10 -9 441.26 31.70 3 10 -9 445.26 30.80 3 10 -9 455.25 29.90 3 10 -9 448.26 30.20 -2 -10 9 610.14 46.80 -2 -10 9 629.94 47.20 2 -10 -9 594.44 46.70 2 10 -9 709.93 45.70 2 10 -9 693.33 47.60 2 10 -9 708.73 46.00 2 10 -9 664.23 47.10 2 10 -9 706.53 46.60 1 -10 -9 122.69 11.90 -1 -10 9 133.39 12.30 -1 -10 9 123.29 11.80 1 10 -9 149.09 10.70 1 10 -9 139.29 11.30 1 10 -9 147.59 11.80 1 10 -9 152.78 12.80 1 10 -9 144.79 12.40 1 10 -9 137.19 10.40 0 -10 9 110.99 9.40 0 -10 9 111.09 9.00 0 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6.30 5 11 -9 43.20 6.30 5 11 -9 49.99 8.10 5 11 -9 39.30 5.80 4 -11 -9 89.29 8.70 4 -11 -9 91.09 7.90 -4 -11 9 99.09 9.40 4 -11 -9 92.39 11.10 4 11 -9 76.79 8.90 4 11 -9 89.89 8.20 4 11 -9 70.39 7.90 4 11 -9 76.69 7.40 3 -11 -9 3.90 5.10 -3 -11 9 2.90 3.70 3 -11 -9 3.60 3.00 3 11 -9 2.50 2.90 3 11 -9 2.50 4.10 3 11 -9 7.20 4.50 3 11 -9 4.30 2.10 3 11 -9 3.20 7.40 3 11 -9 6.30 2.10 2 -11 -9 32.20 5.70 -2 -11 9 35.60 6.60 2 -11 -9 27.90 6.80 -2 -11 9 32.80 5.60 2 11 -9 45.10 4.50 2 11 -9 53.09 8.40 2 11 -9 39.20 7.10 2 11 -9 48.50 4.40 2 11 -9 44.20 6.90 2 11 -9 38.90 5.70 2 11 -9 52.29 5.10 2 11 -9 35.00 6.10 2 11 -9 41.30 9.40 -1 -11 9 80.39 8.00 1 -11 -9 84.89 8.40 -1 -11 9 93.79 9.10 1 -11 -9 79.99 10.20 1 11 -9 78.59 10.30 1 11 -9 79.09 7.00 1 11 -9 71.39 7.60 1 11 -9 78.59 6.50 1 11 -9 69.59 6.60 1 11 -9 78.29 10.80 1 11 -9 75.49 11.20 1 11 -9 79.69 9.20 1 11 -9 67.69 9.10 0 -11 9 149.99 12.30 0 -11 9 132.29 11.60 0 -11 9 161.88 12.90 0 -11 -9 153.58 12.90 0 11 -9 165.38 15.40 0 11 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20.40 -2 -12 9 253.97 19.50 2 12 -9 222.78 19.50 2 12 -9 242.38 17.70 2 12 -9 234.68 18.30 2 12 -9 234.28 20.40 2 12 -9 233.18 17.50 2 12 -9 246.08 20.10 1 -12 -9 148.89 13.30 -1 -12 9 128.09 11.40 1 -12 -9 126.79 11.10 -1 -12 9 112.89 10.90 1 12 -9 120.09 13.70 1 12 -9 132.39 10.00 1 12 -9 116.99 10.50 1 12 -9 108.29 12.50 1 12 -9 118.19 13.60 1 12 -9 122.89 9.70 1 12 -9 130.39 12.20 1 12 -9 126.29 11.80 0 -12 9 92.99 9.30 0 12 -9 101.39 10.30 0 12 -9 100.59 9.00 0 12 -9 92.39 11.10 0 12 -9 104.09 11.80 0 12 -9 99.59 11.90 0 12 -9 96.69 8.10 0 12 -9 96.49 7.80 1 -12 9 23.60 4.50 -1 12 -9 29.80 4.80 -1 12 -9 30.80 7.60 -1 12 -9 30.30 5.70 -1 12 -9 28.10 4.10 -1 12 -9 25.00 3.50 -1 12 -9 34.20 7.20 -1 12 -9 18.40 4.50 -1 12 -9 33.50 7.30 2 -12 9 12.30 3.30 -2 12 -9 14.50 4.30 -2 12 -9 10.30 2.80 -2 12 -9 22.20 5.10 -2 12 -9 11.60 2.20 -2 12 -9 15.40 2.60 -2 12 -9 9.10 4.90 -2 12 -9 14.90 5.10 -2 12 -9 8.70 3.30 3 -12 9 54.89 6.20 -3 12 -9 52.19 6.40 -3 12 -9 51.19 6.40 -3 12 -9 50.09 7.80 -3 12 -9 40.60 6.90 -3 12 -9 44.10 6.00 -3 12 -9 50.49 5.40 -3 12 -9 50.29 4.90 -4 12 -9 47.70 4.30 -4 12 -9 37.60 5.20 -4 12 -9 39.90 6.50 -4 12 -9 45.10 5.70 -4 12 -9 43.00 4.70 -4 12 -9 40.20 6.00 10 -13 -9 28.70 3.90 10 -13 -9 26.00 4.50 10 13 -9 17.30 4.20 9 13 -9 10.20 3.50 8 -13 -9 54.29 7.00 8 -13 -9 53.99 7.10 8 13 -9 59.49 7.80 7 -13 -9 52.59 6.10 7 -13 -9 43.40 7.00 7 -13 -9 48.20 6.70 7 13 -9 34.20 6.40 7 13 -9 45.90 7.60 6 -13 -9 17.90 5.00 6 13 -9 13.70 4.90 6 13 -9 11.40 4.10 5 -13 -9 25.90 5.70 5 -13 -9 21.30 5.30 5 -13 -9 25.60 4.90 5 13 -9 22.10 5.50 5 13 -9 27.60 6.50 -4 -13 9 28.50 5.40 4 -13 -9 32.00 6.90 4 -13 -9 30.40 5.30 4 13 -9 31.60 5.20 4 13 -9 36.60 7.20 4 13 -9 30.00 6.40 3 -13 -9 18.40 4.00 3 -13 -9 16.60 5.00 -3 -13 9 21.00 5.20 3 13 -9 9.20 4.80 3 13 -9 7.80 5.80 3 13 -9 9.40 3.20 3 13 -9 11.00 4.90 -2 -13 9 9.00 4.40 2 -13 -9 4.60 3.20 2 -13 -9 6.10 4.50 2 13 -9 15.70 2.80 2 13 -9 10.60 6.80 2 13 -9 8.90 4.70 2 13 -9 15.40 4.80 -1 -13 9 87.99 9.00 1 -13 -9 77.49 8.30 1 -13 -9 65.19 9.60 1 13 -9 59.79 9.90 1 13 -9 75.79 10.70 1 13 -9 74.19 10.00 1 13 -9 84.49 7.00 1 13 -9 89.79 9.40 0 13 -9 195.18 13.90 0 13 -9 177.68 17.00 0 13 -9 184.18 15.70 1 -13 9 166.48 12.30 -1 13 -9 123.89 13.60 -1 13 -9 172.08 11.60 -1 13 -9 176.48 14.90 -1 13 -9 135.99 14.10 -1 13 -9 158.78 13.30 -1 13 -9 125.69 12.80 -2 13 -9 96.39 10.00 -2 13 -9 122.89 8.70 -2 13 -9 92.99 10.30 -2 13 -9 119.29 9.20 -2 13 -9 120.29 11.80 -3 13 -9 54.49 7.00 -3 13 -9 50.19 7.10 -3 13 -9 50.69 5.90 -3 13 -9 50.29 5.10 -3 13 -9 48.90 4.70 9 -14 -9 7.50 2.90 8 -14 -9 1.90 3.00 8 -14 -9 7.20 3.20 8 14 -9 1.40 3.20 8 14 -9 1.00 2.50 7 -14 -9 6.60 3.90 7 -14 -9 4.50 2.90 7 -14 -9 7.80 3.40 7 14 -9 9.20 3.70 7 14 -9 5.80 4.10 6 -14 -9 -0.20 2.90 6 -14 -9 0.50 2.80 6 -14 -9 -0.40 3.50 6 14 -9 -1.20 3.80 6 14 -9 0.40 3.30 5 -14 -9 40.20 6.50 5 -14 -9 54.59 7.50 5 -14 -9 56.39 6.40 5 14 -9 40.10 7.00 -4 -14 9 248.18 18.00 4 -14 -9 224.68 17.60 4 14 -9 214.78 19.20 3 -14 -9 205.38 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22.80 3 10 -10 291.07 19.80 3 10 -10 296.87 22.00 3 10 -10 274.67 20.00 2 -10 -10 329.27 23.00 -2 -10 10 343.17 23.70 -2 -10 10 310.37 22.80 2 10 -10 293.67 25.30 2 10 -10 311.97 21.50 2 10 -10 277.07 22.90 2 10 -10 287.17 22.20 2 10 -10 300.27 24.20 2 10 -10 299.27 22.10 2 10 -10 294.47 21.70 2 10 -10 295.77 23.60 2 10 -10 292.97 21.70 -1 -10 10 158.98 13.10 1 -10 -10 170.38 13.80 -1 -10 10 158.68 13.60 1 -10 -10 153.58 14.90 1 10 -10 145.19 11.90 1 10 -10 166.08 12.70 1 10 -10 150.28 13.00 1 10 -10 141.59 13.30 1 10 -10 164.08 14.70 1 10 -10 168.78 13.90 1 10 -10 165.38 16.20 1 10 -10 173.48 16.00 1 10 -10 158.68 13.90 1 10 -10 152.78 12.70 1 10 -10 162.98 11.90 1 10 -10 149.39 12.10 0 -10 10 147.49 13.30 0 -10 10 139.79 12.80 0 10 -10 149.99 11.80 0 10 -10 148.49 12.80 0 10 -10 172.38 14.60 0 10 -10 163.98 13.50 0 10 -10 160.28 15.50 0 10 -10 145.99 13.20 0 10 -10 158.48 15.30 0 10 -10 159.28 12.00 0 10 -10 157.08 12.60 0 10 -10 156.58 11.70 0 10 -10 166.98 13.70 0 10 -10 160.48 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-2 -11 76.59 7.00 6 -2 -11 73.09 7.20 6 -2 -11 80.19 7.00 6 2 -11 60.89 6.30 6 2 -11 64.99 6.80 6 2 -11 72.79 7.00 6 2 -11 62.19 7.20 5 -2 -11 25.60 4.50 5 -2 -11 21.70 4.00 5 -2 -11 22.80 4.50 5 2 -11 28.50 4.90 5 2 -11 30.10 3.80 5 2 -11 28.40 5.10 5 2 -11 31.60 4.90 4 -2 -11 13.40 3.20 4 -2 -11 15.90 3.60 4 -2 -11 14.80 3.60 4 2 -11 8.30 3.10 4 2 -11 8.20 2.40 4 2 -11 7.00 3.40 4 2 -11 9.70 3.50 3 -2 -11 143.49 11.90 3 -2 -11 157.38 11.40 3 -2 -11 145.59 11.70 3 2 -11 126.59 11.20 3 2 -11 127.29 11.70 3 2 -11 123.79 10.40 3 2 -11 130.99 12.00 2 -2 -11 105.89 10.10 2 -2 -11 116.89 9.20 2 -2 -11 101.09 9.50 2 2 -11 97.39 10.20 2 2 -11 97.69 9.60 2 2 -11 107.29 8.40 2 2 -11 106.19 9.20 1 -2 -11 381.26 30.40 1 -2 -11 409.26 29.90 1 2 -11 429.16 29.70 1 2 -11 450.55 29.10 1 2 -11 428.96 30.10 1 2 -11 393.16 30.50 0 -2 -11 474.45 35.80 0 -2 -11 489.75 35.10 0 2 -11 528.75 34.50 0 2 -11 511.35 35.30 0 2 -11 492.75 35.00 0 2 -11 479.65 35.70 -1 2 -11 262.67 20.00 -1 2 -11 271.97 20.60 -1 2 -11 267.47 20.50 -1 2 -11 335.77 24.80 -1 2 -11 277.77 21.20 -2 2 -11 156.38 11.80 -2 2 -11 121.89 13.30 13 -3 -11 223.88 15.00 13 3 -11 163.88 14.50 13 3 -11 205.68 14.80 13 3 -11 209.48 14.80 12 -3 -11 109.09 10.00 12 -3 -11 115.09 10.30 12 -3 -11 101.89 9.20 12 3 -11 132.59 10.00 12 3 -11 137.19 9.50 12 3 -11 140.19 9.90 11 -3 -11 25.00 3.60 11 -3 -11 17.60 3.30 11 -3 -11 12.60 2.80 11 -3 -11 15.50 3.50 10 3 -11 51.29 5.80 10 3 -11 49.10 5.00 10 3 -11 51.59 5.90 10 3 -11 56.69 5.10 9 -3 -11 68.99 6.50 9 3 -11 65.59 6.00 9 3 -11 62.79 5.90 8 -3 -11 65.79 6.60 8 -3 -11 59.79 6.00 8 3 -11 61.99 6.00 8 3 -11 55.29 5.90 8 3 -11 61.49 6.50 7 3 -11 69.99 6.70 7 3 -11 80.99 7.00 7 3 -11 72.09 7.60 6 -3 -11 102.69 8.70 6 -3 -11 106.89 8.70 6 -3 -11 107.39 8.70 6 3 -11 89.69 8.40 6 3 -11 84.19 8.10 6 3 -11 84.09 8.10 6 3 -11 97.29 8.80 6 3 -11 82.79 8.70 5 -3 -11 79.79 7.50 5 -3 -11 85.79 7.60 5 -3 -11 85.19 8.00 5 3 -11 69.79 7.00 5 3 -11 70.49 7.70 5 3 -11 78.79 7.80 5 3 -11 71.09 7.70 5 3 -11 66.79 6.70 4 -3 -11 107.49 10.90 4 -3 -11 113.09 11.10 4 -3 -11 112.69 11.00 4 3 -11 138.79 10.50 4 3 -11 149.49 11.50 4 3 -11 145.29 10.50 4 3 -11 152.08 11.80 4 3 -11 149.09 11.80 3 -3 -11 454.15 28.60 3 -3 -11 425.86 28.90 3 -3 -11 450.05 29.00 3 3 -11 361.56 27.50 3 3 -11 364.16 28.80 3 3 -11 370.76 27.80 3 3 -11 370.06 29.00 3 3 -11 366.46 28.50 2 -3 -11 197.18 15.60 2 -3 -11 188.58 15.90 2 -3 -11 184.88 16.20 2 3 -11 199.18 16.80 2 3 -11 215.38 15.80 2 3 -11 214.48 16.30 2 3 -11 217.18 15.00 2 3 -11 219.68 15.30 1 -3 -11 181.28 14.10 1 -3 -11 184.88 13.30 1 3 -11 157.68 13.30 1 3 -11 157.48 13.00 1 3 -11 160.68 14.00 1 3 -11 158.78 12.20 1 3 -11 138.09 14.30 0 -3 -11 76.99 7.80 0 3 -11 57.69 6.30 0 3 -11 65.09 6.80 0 3 -11 63.59 5.90 0 3 -11 56.99 7.40 -1 3 -11 6.70 3.30 -1 3 -11 7.30 2.90 -1 3 -11 4.50 2.50 -1 3 -11 6.30 2.30 -1 3 -11 7.90 4.20 -1 3 -11 8.00 5.00 -1 3 -11 8.00 2.70 -1 3 -11 6.50 2.50 2 -3 11 39.10 5.00 -2 3 -11 34.70 4.30 -2 3 -11 38.10 6.20 -2 3 -11 37.50 5.00 -2 3 -11 37.50 5.20 -2 3 -11 30.10 4.60 -2 3 -11 32.40 6.10 -3 3 -11 115.99 9.80 -3 3 -11 115.39 10.00 13 -4 -11 15.30 2.90 13 -4 -11 14.00 3.00 13 4 -11 12.30 2.60 13 4 -11 14.20 2.50 12 -4 -11 176.48 12.90 12 -4 -11 159.98 12.40 12 4 -11 145.29 12.10 12 4 -11 158.38 11.70 12 4 -11 159.38 12.20 11 -4 -11 190.98 15.50 11 -4 -11 207.88 16.10 11 4 -11 208.38 15.60 11 4 -11 215.28 15.00 11 4 -11 214.88 15.50 10 -4 -11 224.48 16.60 10 -4 -11 226.38 17.20 10 -4 -11 211.48 16.70 10 4 -11 233.88 16.20 10 4 -11 219.88 16.20 10 4 -11 226.68 16.80 10 4 -11 222.38 16.50 9 -4 -11 317.57 23.10 9 -4 -11 290.67 20.90 9 -4 -11 328.97 21.80 9 -4 -11 310.77 21.10 9 -4 -11 248.48 21.70 9 4 -11 263.97 20.60 9 4 -11 276.47 20.50 9 4 -11 266.87 20.90 8 -4 -11 274.67 18.80 8 -4 -11 265.97 18.60 8 4 -11 236.88 18.20 8 4 -11 228.68 18.20 7 -4 -11 159.68 12.40 7 -4 -11 153.68 12.50 7 -4 -11 154.18 12.50 7 4 -11 161.38 12.80 7 4 -11 157.48 12.10 7 4 -11 157.08 12.20 6 -4 -11 229.68 16.90 6 -4 -11 230.68 16.80 6 -4 -11 249.97 17.10 6 4 -11 213.28 16.40 6 4 -11 206.88 16.50 6 4 -11 222.88 16.90 6 4 -11 198.98 17.00 5 -4 -11 58.29 6.00 5 -4 -11 55.49 6.00 5 4 -11 43.60 6.50 5 4 -11 43.60 6.10 5 4 -11 39.10 5.50 5 4 -11 35.80 5.00 5 4 -11 47.80 6.10 4 -4 -11 17.20 3.50 4 -4 -11 18.40 3.80 4 -4 -11 15.70 3.70 4 4 -11 16.20 3.80 4 4 -11 19.70 4.40 4 4 -11 17.60 4.20 4 4 -11 15.30 2.80 4 4 -11 11.90 3.00 3 -4 -11 345.67 23.00 3 -4 -11 317.77 23.30 3 -4 -11 339.27 23.30 3 4 -11 287.27 22.00 3 4 -11 297.87 22.30 3 4 -11 304.17 23.50 3 4 -11 301.77 23.80 3 4 -11 296.17 22.90 2 4 -11 12.90 3.20 2 4 -11 15.50 2.90 2 4 -11 13.90 2.50 2 4 -11 15.40 4.10 2 4 -11 14.20 4.60 1 -4 -11 55.29 7.90 1 4 -11 73.29 8.90 1 4 -11 77.49 6.70 1 4 -11 77.59 7.20 1 4 -11 76.59 7.80 1 4 -11 77.29 6.50 0 -4 -11 402.06 28.70 0 4 -11 391.96 27.30 0 4 -11 391.46 27.10 0 4 -11 364.06 27.60 0 4 -11 386.06 28.50 0 4 -11 383.86 28.00 -1 4 -11 630.44 45.40 -1 4 -11 631.84 45.30 -1 4 -11 673.93 44.40 -1 4 -11 614.44 44.80 -1 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6 -15 40.20 5.10 4 6 -15 44.30 6.50 4 6 -15 45.90 6.70 4 6 -15 28.50 5.70 4 6 -15 43.00 5.80 3 -6 -15 36.50 6.30 3 6 -15 53.49 6.90 3 6 -15 44.10 5.90 2 6 -15 78.09 8.20 2 6 -15 79.09 8.90 2 6 -15 102.29 8.00 9 7 -15 75.09 7.70 8 -7 -15 95.19 8.50 8 7 -15 83.79 7.20 8 7 -15 81.89 7.50 7 -7 -15 59.09 7.20 7 7 -15 64.29 7.40 7 7 -15 75.79 6.80 7 7 -15 72.69 6.30 6 -7 -15 68.59 7.40 6 7 -15 64.99 6.20 6 7 -15 57.99 6.50 5 -7 -15 87.49 8.30 5 -7 -15 69.59 7.90 5 7 -15 74.99 7.50 5 7 -15 83.19 8.00 5 7 -15 75.19 7.00 5 7 -15 74.79 7.50 4 -7 -15 57.59 7.00 4 7 -15 56.69 5.70 4 7 -15 61.49 6.70 4 7 -15 59.89 7.10 3 -7 -15 32.60 5.20 3 7 -15 30.70 5.50 3 7 -15 26.70 4.10 3 7 -15 24.50 3.80 7 -8 -15 8.60 3.10 7 -8 -15 16.60 3.90 7 8 -15 8.30 2.10 7 8 -15 11.30 2.60 6 -8 -15 28.10 5.00 6 8 -15 34.60 4.20 6 8 -15 23.20 4.40 6 8 -15 36.90 4.60 6 8 -15 23.60 4.20 5 -8 -15 15.20 3.60 5 -8 -15 18.00 3.90 5 8 -15 12.00 3.30 5 8 -15 12.10 2.80 5 8 -15 11.60 3.30 5 8 -15 15.10 2.80 4 -8 -15 17.30 4.20 4 -8 -15 21.90 5.10 4 8 -15 16.40 4.30 4 8 -15 17.20 3.30 4 8 -15 19.50 3.90 4 8 -15 18.80 3.10 4 8 -15 14.60 3.90 9 0 -16 78.19 6.70 9 0 -16 71.39 6.70 8 0 -16 120.39 10.00 8 0 -16 132.59 10.80 7 0 -16 25.20 4.40 7 0 -16 18.70 3.30 7 0 -16 24.00 4.90 6 0 -16 1.80 3.30 6 0 -16 -0.50 2.00 6 0 -16 0.90 2.90 6 0 -16 0.50 2.50 5 0 -16 0.50 3.10 5 0 -16 -0.60 2.70 5 0 -16 4.40 3.50 4 0 -16 -2.00 2.50 4 0 -16 1.50 3.50 4 0 -16 0.30 3.10 3 0 -16 4.60 2.70 3 0 -16 5.70 3.50 3 0 -16 9.70 3.70 9 -1 -16 19.30 3.90 9 -1 -16 20.10 3.50 9 -1 -16 20.00 3.70 9 1 -16 17.60 3.00 9 1 -16 18.70 3.70 8 -1 -16 42.20 5.40 8 -1 -16 40.20 4.60 8 -1 -16 35.90 4.90 8 1 -16 47.30 5.00 8 1 -16 34.20 5.40 8 1 -16 42.10 5.10 7 -1 -16 71.89 7.20 7 -1 -16 82.79 7.80 7 1 -16 83.39 7.40 7 1 -16 78.89 7.10 7 1 -16 55.89 7.40 6 -1 -16 49.30 6.50 6 -1 -16 63.09 6.40 6 1 -16 63.59 6.80 6 1 -16 43.10 6.60 6 1 -16 56.19 6.00 5 -1 -16 80.69 8.40 5 -1 -16 83.79 8.50 5 1 -16 70.29 7.10 5 1 -16 79.39 8.40 4 -1 -16 42.90 5.70 4 -1 -16 50.89 6.70 4 -1 -16 51.09 6.60 4 1 -16 43.10 6.70 4 1 -16 49.50 6.20 4 1 -16 39.90 5.80 3 -1 -16 7.70 2.70 3 -1 -16 8.50 3.60 3 1 -16 5.70 3.20 3 1 -16 6.00 3.50 9 -2 -16 55.59 6.00 9 2 -16 46.70 5.20 8 -2 -16 87.49 7.80 8 -2 -16 94.29 8.50 8 2 -16 77.59 7.60 8 2 -16 80.09 7.60 7 -2 -16 20.00 4.70 7 -2 -16 13.90 3.10 7 -2 -16 12.80 3.50 7 2 -16 12.60 3.50 7 2 -16 20.50 4.30 6 -2 -16 7.50 3.50 6 -2 -16 4.70 3.20 6 -2 -16 6.60 2.90 6 2 -16 4.30 2.40 6 2 -16 7.70 3.30 6 2 -16 9.60 3.70 6 2 -16 3.90 2.60 5 -2 -16 5.80 2.90 5 -2 -16 4.90 3.20 5 -2 -16 4.30 3.30 5 2 -16 3.80 3.50 5 2 -16 2.00 2.60 5 2 -16 -0.70 2.50 5 2 -16 5.10 3.30 4 -2 -16 1.20 3.20 4 -2 -16 1.60 3.00 4 -2 -16 1.90 2.50 4 2 -16 2.20 2.00 4 2 -16 -0.40 2.80 4 2 -16 -1.40 2.60 4 2 -16 1.60 3.20 3 -2 -16 4.40 3.20 3 -2 -16 3.70 2.80 3 2 -16 2.60 3.10 3 2 -16 5.30 2.90 3 2 -16 6.40 3.50 3 2 -16 1.80 3.30 9 -3 -16 14.90 3.70 9 -3 -16 17.90 3.70 9 3 -16 11.70 3.00 9 3 -16 21.90 4.10 8 -3 -16 48.40 5.60 8 -3 -16 69.19 6.70 8 -3 -16 48.10 6.30 8 3 -16 57.79 5.70 7 -3 -16 42.70 5.90 7 -3 -16 42.30 5.20 7 3 -16 40.90 5.40 7 3 -16 34.00 5.50 7 3 -16 40.20 5.00 6 -3 -16 76.79 8.00 6 3 -16 78.49 7.80 6 3 -16 85.79 7.70 6 3 -16 59.79 7.30 6 3 -16 79.79 7.30 5 -3 -16 54.89 5.50 5 -3 -16 49.70 6.20 5 -3 -16 55.39 6.60 5 3 -16 37.50 6.10 5 3 -16 44.20 5.80 5 3 -16 41.00 5.90 5 3 -16 42.70 5.80 4 -3 -16 24.20 5.10 4 3 -16 21.80 5.30 4 3 -16 22.90 3.60 4 3 -16 24.00 4.30 8 -4 -16 67.39 7.00 8 -4 -16 53.59 6.10 8 4 -16 78.79 6.30 7 -4 -16 42.80 6.10 7 -4 -16 50.29 5.60 7 -4 -16 63.29 6.40 7 4 -16 55.19 5.60 7 4 -16 59.59 5.90 7 4 -16 45.00 5.70 6 -4 -16 38.50 5.50 6 4 -16 35.20 5.00 6 4 -16 35.60 5.20 6 4 -16 24.80 4.70 5 -4 -16 2.20 2.80 5 -4 -16 5.30 3.00 5 4 -16 -0.50 2.30 5 4 -16 1.90 2.90 5 4 -16 3.70 3.00 5 4 -16 1.60 2.50 4 -4 -16 8.50 3.60 4 4 -16 2.60 2.50 4 4 -16 3.80 3.40 4 4 -16 -0.40 2.30 4 4 -16 -0.20 3.00 7 -5 -16 43.90 4.80 7 -5 -16 37.90 6.00 7 5 -16 38.10 5.20 6 -5 -16 40.40 5.70 6 -5 -16 30.20 5.60 6 5 -16 44.00 5.20 5 5 -16 52.69 7.70 5 5 -16 38.20 5.80 5 5 -16 47.50 6.30 5 5 -16 50.09 6.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 25806 #===END data_Cpx_5f _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Cpx_5f' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H71 F3 N O6 P Pd S' _chemical_formula_weight 984.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3488(4) _cell_length_b 18.5998(3) _cell_length_c 19.6316(3) _cell_angle_alpha 90 _cell_angle_beta 112.7010(10) _cell_angle_gamma 90 _cell_volume 9549.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9563 _cell_measurement_theta_min 3.358 _cell_measurement_theta_max 65.123 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_F_000 4144 _exptl_transmission_factor_min 0.759 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 4.348 _shelx_estimated_absorpt_T_min 0.337 _shelx_estimated_absorpt_T_max 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'Mixed Phi and Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46045 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.915 _diffrn_reflns_theta_max 65.157 _diffrn_reflns_theta_full 65.157 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 8134 _reflns_number_gt 7341 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8134 _refine_ls_number_parameters 730 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2A O 0.64478(14) 0.3373(2) 0.5286(3) 0.0671(13) Uani 0.632(3) 1 d D . P A 1 O3A O 0.59079(16) 0.4295(2) 0.4745(3) 0.0628(12) Uani 0.632(3) 1 d D . P A 1 C24A C 0.51431(19) 0.1950(3) 0.3832(3) 0.0379(11) Uani 0.632(3) 1 d . . P A 1 H24A H 0.497272 0.152762 0.394419 0.045 Uiso 0.632(3) 1 calc R U P A 1 H24B H 0.487369 0.226697 0.349442 0.045 Uiso 0.632(3) 1 calc R U P A 1 C25A C 0.5482(3) 0.1698(3) 0.3447(3) 0.0462(12) Uani 0.632(3) 1 d . . P A 1 H25A H 0.527716 0.141362 0.300566 0.055 Uiso 0.632(3) 1 calc R U P A 1 H25B H 0.562170 0.212048 0.328064 0.055 Uiso 0.632(3) 1 calc R U P A 1 C26A C 0.5915(3) 0.1246(4) 0.3953(6) 0.056(2) Uani 0.632(3) 1 d . . P A 1 H26A H 0.614506 0.111433 0.369991 0.068 Uiso 0.632(3) 1 calc R U P A 1 H26B H 0.577808 0.079723 0.407632 0.068 Uiso 0.632(3) 1 calc R U P A 1 C27A C 0.6216(3) 0.1657(4) 0.4659(4) 0.0556(16) Uani 0.632(3) 1 d . . P A 1 H27A H 0.638464 0.207607 0.453796 0.067 Uiso 0.632(3) 1 calc R U P A 1 H27B H 0.648713 0.134100 0.499652 0.067 Uiso 0.632(3) 1 calc R U P A 1 C28A C 0.58728(18) 0.1919(3) 0.5055(3) 0.0365(11) Uani 0.632(3) 1 d . . P A 1 H28A H 0.573728 0.149884 0.523049 0.044 Uiso 0.632(3) 1 calc R U P A 1 H28B H 0.607968 0.220871 0.549182 0.044 Uiso 0.632(3) 1 calc R U P A 1 C29A C 0.56082(18) 0.3117(3) 0.4357(3) 0.0389(11) Uani 0.632(3) 1 d . . P A 1 H29A H 0.582060 0.303576 0.406541 0.047 Uiso 0.632(3) 1 calc R U P A 1 H29B H 0.529888 0.338364 0.404029 0.047 Uiso 0.632(3) 1 calc R U P A 1 C31A C 0.6739(3) 0.3968(5) 0.5307(6) 0.086(3) Uani 0.632(3) 1 d D . P A 1 H31A H 0.691908 0.390271 0.496788 0.104 Uiso 0.632(3) 1 calc R U P A 1 H31B H 0.699798 0.403897 0.581247 0.104 Uiso 0.632(3) 1 calc R U P A 1 C32A C 0.6414(3) 0.4574(4) 0.5090(8) 0.085(3) Uani 0.632(3) 1 d D . P A 1 H32A H 0.650087 0.487540 0.473887 0.102 Uiso 0.632(3) 1 calc R U P A 1 H32B H 0.644553 0.487029 0.552440 0.102 Uiso 0.632(3) 1 calc R U P A 1 C33A C 0.5755(2) 0.3556(3) 0.5671(3) 0.0495(14) Uani 0.632(3) 1 d . . P A 1 H33A H 0.586379 0.400515 0.596013 0.059 Uiso 0.632(3) 1 calc R U P A 1 H33B H 0.593097 0.314903 0.599472 0.059 Uiso 0.632(3) 1 calc R U P A 1 C34A C 0.5109(6) 0.3455(10) 0.5397(8) 0.029(3) Uani 0.632(3) 1 d . . P A 1 C35A C 0.5080(3) 0.3475(3) 0.6206(3) 0.0520(14) Uani 0.632(3) 1 d . . P A 1 H35A H 0.521491 0.393485 0.644599 0.078 Uiso 0.632(3) 1 calc R U P A 1 H35B H 0.528339 0.308020 0.650717 0.078 Uiso 0.632(3) 1 calc R U P A 1 H35C H 0.472312 0.342327 0.615257 0.078 Uiso 0.632(3) 1 calc R U P A 1 C36A C 0.4908(2) 0.4157(3) 0.5069(4) 0.0597(16) Uani 0.632(3) 1 d . . P A 1 H36A H 0.453624 0.416556 0.492089 0.090 Uiso 0.632(3) 1 calc R U P A 1 H36B H 0.499192 0.423682 0.463495 0.090 Uiso 0.632(3) 1 calc R U P A 1 H36C H 0.506318 0.453762 0.543248 0.090 Uiso 0.632(3) 1 calc R U P A 1 C44A C 0.3265(4) 0.2450(6) 0.2402(6) 0.062(3) Uani 0.590(11) 1 d D U P B 1 H44A H 0.322307 0.192721 0.245709 0.074 Uiso 0.590(11) 1 calc R U P B 1 H44B H 0.356993 0.251693 0.227973 0.074 Uiso 0.590(11) 1 calc R U P B 1 C45A C 0.2790(6) 0.2733(8) 0.1753(7) 0.120(7) Uani 0.590(11) 1 d D U P B 1 H45A H 0.249225 0.273347 0.189849 0.145 Uiso 0.590(11) 1 calc R U P B 1 H45B H 0.271159 0.240901 0.132358 0.145 Uiso 0.590(11) 1 calc R U P B 1 C46A C 0.2881(4) 0.3510(6) 0.1531(6) 0.088(3) Uani 0.590(11) 1 d D U P B 1 H46A H 0.294645 0.383942 0.195328 0.106 Uiso 0.590(11) 1 calc R U P B 1 H46B H 0.318569 0.351465 0.140046 0.106 Uiso 0.590(11) 1 calc R U P B 1 C47A C 0.2431(5) 0.3757(8) 0.0896(6) 0.138(6) Uani 0.590(11) 1 d D U P B 1 H47A H 0.237187 0.343626 0.047512 0.207 Uiso 0.590(11) 1 calc R U P B 1 H47B H 0.249093 0.424713 0.076318 0.207 Uiso 0.590(11) 1 calc R U P B 1 H47C H 0.213063 0.375379 0.102679 0.207 Uiso 0.590(11) 1 calc R U P B 1 O2B O 0.6270(2) 0.3869(3) 0.5652(3) 0.0434(15) Uani 0.368(3) 1 d D . P A 2 O3B O 0.5972(2) 0.3856(3) 0.4393(3) 0.0384(14) Uani 0.368(3) 1 d D . P A 2 C24B C 0.5308(3) 0.2447(4) 0.3757(4) 0.0303(17) Uani 0.368(3) 1 d . . P A 2 H24C H 0.525073 0.296488 0.363550 0.036 Uiso 0.368(3) 1 calc R U P A 2 H24D H 0.497982 0.219691 0.348991 0.036 Uiso 0.368(3) 1 calc R U P A 2 C25B C 0.5691(3) 0.2176(5) 0.3462(4) 0.0373(19) Uani 0.368(3) 1 d . . P A 2 H25C H 0.555901 0.225977 0.292223 0.045 Uiso 0.368(3) 1 calc R U P A 2 H25D H 0.601302 0.245122 0.369094 0.045 Uiso 0.368(3) 1 calc R U P A 2 C26B C 0.5802(5) 0.1391(7) 0.3612(7) 0.042(3) Uani 0.368(3) 1 d . . P A 2 H26C H 0.606507 0.123945 0.342541 0.050 Uiso 0.368(3) 1 calc R U P A 2 H26D H 0.548785 0.110904 0.334972 0.050 Uiso 0.368(3) 1 calc R U P A 2 C27B C 0.5990(4) 0.1247(6) 0.4430(7) 0.0369(19) Uani 0.368(3) 1 d . . P A 2 H27C H 0.631759 0.150173 0.468765 0.044 Uiso 0.368(3) 1 calc R U P A 2 H27D H 0.605168 0.072552 0.452286 0.044 Uiso 0.368(3) 1 calc R U P A 2 C28B C 0.5595(3) 0.1502(4) 0.4737(4) 0.0301(16) Uani 0.368(3) 1 d . . P A 2 H28C H 0.573477 0.142768 0.527815 0.036 Uiso 0.368(3) 1 calc R U P A 2 H28D H 0.528216 0.120512 0.452003 0.036 Uiso 0.368(3) 1 calc R U P A 2 C29B C 0.5935(3) 0.2767(4) 0.5060(4) 0.0296(17) Uani 0.368(3) 1 d . . P A 2 H29C H 0.601929 0.262092 0.557873 0.036 Uiso 0.368(3) 1 calc R U P A 2 H29D H 0.622020 0.260772 0.492295 0.036 Uiso 0.368(3) 1 calc R U P A 2 C31B C 0.6611(7) 0.4250(12) 0.5450(7) 0.073(3) Uani 0.368(3) 1 d D . P A 2 H31C H 0.692874 0.397096 0.555547 0.088 Uiso 0.368(3) 1 calc R U P A 2 H31D H 0.669938 0.471195 0.572085 0.088 Uiso 0.368(3) 1 calc R U P A 2 C32B C 0.6358(5) 0.4373(8) 0.4679(7) 0.073(3) Uani 0.368(3) 1 d D . P A 2 H32C H 0.620763 0.486171 0.458857 0.088 Uiso 0.368(3) 1 calc R U P A 2 H32D H 0.660406 0.433427 0.443450 0.088 Uiso 0.368(3) 1 calc R U P A 2 C33B C 0.5356(3) 0.3875(4) 0.4958(4) 0.0278(15) Uani 0.368(3) 1 d . . P A 2 H33C H 0.536955 0.440029 0.504408 0.033 Uiso 0.368(3) 1 calc R U P A 2 H33D H 0.509339 0.377562 0.446032 0.033 Uiso 0.368(3) 1 calc R U P A 2 C34B C 0.5226(10) 0.3487(16) 0.5540(16) 0.036(6) Uani 0.368(3) 1 d . . P A 2 C35B C 0.5434(4) 0.3402(4) 0.6214(4) 0.0350(19) Uani 0.368(3) 1 d . . P A 2 H35D H 0.576009 0.315153 0.633255 0.052 Uiso 0.368(3) 1 calc R U P A 2 H35E H 0.521125 0.311572 0.638557 0.052 Uiso 0.368(3) 1 calc R U P A 2 H35F H 0.549586 0.387202 0.645851 0.052 Uiso 0.368(3) 1 calc R U P A 2 C36B C 0.4604(3) 0.3837(4) 0.5343(4) 0.0319(16) Uani 0.368(3) 1 d . . P A 2 H36D H 0.444278 0.357214 0.562767 0.048 Uiso 0.368(3) 1 calc R U P A 2 H36E H 0.439671 0.378542 0.481464 0.048 Uiso 0.368(3) 1 calc R U P A 2 H36F H 0.462927 0.434690 0.547861 0.048 Uiso 0.368(3) 1 calc R U P A 2 C44B C 0.3315(6) 0.2699(10) 0.2324(7) 0.076(6) Uani 0.410(11) 1 d D U P B 2 H44C H 0.363562 0.285260 0.227869 0.091 Uiso 0.410(11) 1 calc R U P B 2 H44D H 0.325998 0.218292 0.219314 0.091 Uiso 0.410(11) 1 calc R U P B 2 C45B C 0.2865(4) 0.3142(15) 0.1801(7) 0.093(7) Uani 0.410(11) 1 d D U P B 2 H45C H 0.254431 0.293112 0.180198 0.111 Uiso 0.410(11) 1 calc R U P B 2 H45D H 0.289290 0.363515 0.200189 0.111 Uiso 0.410(11) 1 calc R U P B 2 C46B C 0.2821(5) 0.3191(11) 0.1020(7) 0.108(6) Uani 0.410(11) 1 d D U P B 2 H46C H 0.257817 0.357279 0.074649 0.129 Uiso 0.410(11) 1 calc R U P B 2 H46D H 0.315731 0.328251 0.099254 0.129 Uiso 0.410(11) 1 calc R U P B 2 C47B C 0.2631(10) 0.2492(11) 0.0746(15) 0.158(11) Uani 0.410(11) 1 d D U P B 2 H47D H 0.283129 0.212717 0.109956 0.237 Uiso 0.410(11) 1 calc R U P B 2 H47E H 0.266096 0.241488 0.027065 0.237 Uiso 0.410(11) 1 calc R U P B 2 H47F H 0.227151 0.245604 0.068117 0.237 Uiso 0.410(11) 1 calc R U P B 2 Pd1 Pd 0.40944(2) 0.26833(2) 0.39639(2) 0.03275(11) Uani 1 1 d . . . . . P1 P 0.49122(3) 0.26170(4) 0.48902(4) 0.02776(17) Uani 1 1 d . . . . . O1 O 0.57126(8) 0.20538(15) 0.63627(12) 0.0516(6) Uani 1 1 d . . . . . N1 N 0.33564(11) 0.28121(19) 0.31221(16) 0.0498(7) Uani 1 1 d D . . . . H1N H 0.3089(16) 0.259(2) 0.328(2) 0.058(11) Uiso 1 1 d D . . . . H2N H 0.321(2) 0.333(2) 0.307(3) 0.109(19) Uiso 1 1 d D . . . . C1 C 0.48611(10) 0.19158(14) 0.55197(14) 0.0295(6) Uani 1 1 d . . . . . C2 C 0.52600(12) 0.17122(15) 0.61904(15) 0.0342(6) Uani 1 1 d . . . . . C3 C 0.61449(14) 0.1844(2) 0.70019(18) 0.0541(9) Uani 1 1 d . . . . . H3A H 0.607509 0.193700 0.744544 0.081 Uiso 1 1 calc R U . . . H3B H 0.644502 0.212122 0.702613 0.081 Uiso 1 1 calc R U . . . H3C H 0.621115 0.133026 0.697244 0.081 Uiso 1 1 calc R U . . . C4 C 0.51823(13) 0.11890(15) 0.66448(15) 0.0388(7) Uani 1 1 d . . . . . H4 H 0.545228 0.106038 0.709521 0.047 Uiso 1 1 calc R U . . . C5 C 0.47169(14) 0.08621(16) 0.64405(16) 0.0435(7) Uani 1 1 d . . . . . H5 H 0.466478 0.050473 0.675013 0.052 Uiso 1 1 calc R U . . . C6 C 0.43184(12) 0.10468(15) 0.57840(16) 0.0372(6) Uani 1 1 d . . . . . H6 H 0.399639 0.081460 0.564653 0.045 Uiso 1 1 calc R U . . . C7 C 0.43904(11) 0.15733(14) 0.53259(14) 0.0297(6) Uani 1 1 d . . . . . C8 C 0.39141(10) 0.17158(14) 0.46453(15) 0.0310(6) Uani 1 1 d . . . . . C9 C 0.35159(12) 0.21271(17) 0.47321(17) 0.0374(6) Uani 1 1 d . . . . . C10 C 0.36309(14) 0.26559(16) 0.53680(18) 0.0407(7) Uani 1 1 d . . . . . H10 H 0.400956 0.272752 0.559867 0.049 Uiso 1 1 calc R U . . . C11 C 0.33804(15) 0.33905(18) 0.51133(19) 0.0500(8) Uani 1 1 d . . . . . H11A H 0.347169 0.356996 0.471093 0.075 Uiso 1 1 calc R U . . . H11B H 0.350109 0.372933 0.552744 0.075 Uiso 1 1 calc R U . . . H11C H 0.300803 0.334216 0.493878 0.075 Uiso 1 1 calc R U . . . C12 C 0.3456(2) 0.23518(19) 0.5958(2) 0.0642(12) Uani 1 1 d . . . . . H12A H 0.308911 0.224873 0.573546 0.096 Uiso 1 1 calc R U . . . H12B H 0.352410 0.270443 0.635511 0.096 Uiso 1 1 calc R U . . . H12C H 0.364423 0.190756 0.615954 0.096 Uiso 1 1 calc R U . . . C13 C 0.30150(12) 0.2007(2) 0.4269(2) 0.0486(8) Uani 1 1 d . . . . . H13 H 0.275344 0.228933 0.432641 0.058 Uiso 1 1 calc R U . . . C14 C 0.28822(13) 0.1491(2) 0.3726(3) 0.0631(11) Uani 1 1 d . . . . . C18 C 0.32699(12) 0.1125(2) 0.3594(2) 0.0533(9) Uani 1 1 d . . . . . H18 H 0.318298 0.080421 0.318768 0.064 Uiso 1 1 calc R U . . . C19 C 0.37835(10) 0.12263(16) 0.40519(16) 0.0366(6) Uani 1 1 d . . . . . C20 C 0.41860(12) 0.07352(17) 0.39606(16) 0.0395(7) Uani 1 1 d . . . . . H20 H 0.453032 0.092129 0.428666 0.047 Uiso 1 1 calc R U . . . C21 C 0.41566(13) 0.0739(2) 0.31656(18) 0.0499(8) Uani 1 1 d . . . . . H21A H 0.384060 0.050131 0.284313 0.075 Uiso 1 1 calc R U . . . H21B H 0.445157 0.048103 0.314249 0.075 Uiso 1 1 calc R U . . . H21C H 0.415868 0.123609 0.300204 0.075 Uiso 1 1 calc R U . . . C22 C 0.41352(16) -0.00324(19) 0.4209(2) 0.0557(9) Uani 1 1 d . . . . . H22A H 0.418019 -0.002791 0.472944 0.084 Uiso 1 1 calc R U . . . H22B H 0.439747 -0.033853 0.414759 0.084 Uiso 1 1 calc R U . . . H22C H 0.379556 -0.022124 0.390811 0.084 Uiso 1 1 calc R U . . . C23 C 0.54383(11) 0.23620(14) 0.45585(16) 0.0311(6) Uani 1 1 d . . . . . C30 C 0.59068(12) 0.35821(17) 0.50184(18) 0.0443(7) Uani 1 1 d D . . . . C37 C 0.42192(10) 0.35412(18) 0.34162(16) 0.0391(7) Uani 1 1 d . . . . . C38 C 0.40113(13) 0.42056(18) 0.34863(18) 0.0456(7) Uani 1 1 d . . . . . H38 H 0.387001 0.426138 0.385032 0.055 Uiso 1 1 calc R U . . . C39 C 0.40057(14) 0.4784(2) 0.30401(19) 0.0532(9) Uani 1 1 d . . . . . H39 H 0.386374 0.522755 0.310747 0.064 Uiso 1 1 calc R U . . . C40 C 0.42009(12) 0.4730(2) 0.2502(2) 0.0553(10) Uani 1 1 d . . . . . C41 C 0.42125(16) 0.5381(3) 0.2033(3) 0.0793(15) Uani 1 1 d . . . . . H41A H 0.389509 0.565551 0.190725 0.119 Uiso 1 1 calc R U . . . H41B H 0.424524 0.521694 0.157866 0.119 Uiso 1 1 calc R U . . . H41C H 0.450465 0.568704 0.231206 0.119 Uiso 1 1 calc R U . . . C42 C 0.43920(13) 0.4074(3) 0.2412(2) 0.0644(12) Uani 1 1 d . . . . . H42 H 0.452032 0.401826 0.203378 0.077 Uiso 1 1 calc R U . . . C43 C 0.44031(13) 0.3490(2) 0.2857(2) 0.0561(10) Uani 1 1 d . . . . . H43 H 0.453928 0.304580 0.277748 0.067 Uiso 1 1 calc R U . . . S1 S 0.76811(3) 0.58007(4) 0.69133(4) 0.03845(19) Uani 1 1 d . . . . . F1 F 0.84470(7) 0.55107(11) 0.65301(12) 0.0557(5) Uani 1 1 d . . . . . F2 F 0.77163(10) 0.55588(15) 0.56175(11) 0.0794(8) Uani 1 1 d . . . . . F3 F 0.79133(9) 0.46458(12) 0.63428(14) 0.0704(6) Uani 1 1 d . . . . . O4 O 0.77640(9) 0.65505(12) 0.68253(13) 0.0483(5) Uani 1 1 d . . . . . O5 O 0.79865(9) 0.55010(13) 0.76244(12) 0.0501(6) Uani 1 1 d . . . . . O6 O 0.71555(8) 0.55881(16) 0.66170(15) 0.0611(7) Uani 1 1 d . . . . . C48 C 0.79530(12) 0.53536(17) 0.63241(18) 0.0433(7) Uani 1 1 d . . . . . C17 C 0.22470(18) 0.0488(4) 0.3511(3) 0.099(2) Uani 1 1 d . . . . . H17A H 0.244616 0.015883 0.333643 0.149 Uiso 1 1 calc R U . . . H17B H 0.188367 0.036279 0.327924 0.149 Uiso 1 1 calc R U . . . H17C H 0.236139 0.044879 0.404833 0.149 Uiso 1 1 calc R U . . . C15 C 0.23275(16) 0.1289(3) 0.3297(3) 0.096(2) Uani 1 1 d . . . . . H15 H 0.210878 0.161337 0.345833 0.115 Uiso 1 1 calc R U . . . C16 C 0.21688(17) 0.1372(3) 0.2476(4) 0.106(2) Uani 1 1 d . . . . . H16A H 0.227769 0.184451 0.236841 0.159 Uiso 1 1 calc R U . . . H16B H 0.179610 0.133253 0.223281 0.159 Uiso 1 1 calc R U . . . H16C H 0.232940 0.099459 0.229069 0.159 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2A 0.030(2) 0.057(3) 0.090(3) 0.008(2) -0.003(2) -0.0136(17) O3A 0.052(2) 0.039(2) 0.085(3) 0.003(2) 0.013(2) -0.0168(18) C24A 0.039(3) 0.032(3) 0.041(3) 0.0004(19) 0.013(2) -0.005(2) C25A 0.055(4) 0.039(3) 0.050(3) 0.006(2) 0.026(3) 0.008(3) C26A 0.074(5) 0.055(4) 0.052(6) 0.018(4) 0.037(5) 0.030(4) C27A 0.042(3) 0.066(4) 0.066(4) 0.021(3) 0.029(3) 0.026(3) C28A 0.027(2) 0.038(3) 0.039(2) 0.006(2) 0.007(2) 0.010(2) C29A 0.027(2) 0.037(3) 0.046(3) 0.002(2) 0.007(2) -0.0006(19) C31A 0.064(5) 0.085(6) 0.114(8) -0.022(5) 0.039(5) -0.046(5) C32A 0.062(5) 0.059(5) 0.103(8) 0.000(4) -0.003(5) -0.034(4) C33A 0.045(3) 0.033(3) 0.052(3) -0.008(2) -0.001(2) -0.004(2) C34A 0.020(6) 0.033(4) 0.025(6) -0.002(4) -0.001(6) 0.001(4) C35A 0.056(4) 0.044(3) 0.048(3) -0.014(2) 0.012(3) 0.009(3) C36A 0.066(4) 0.030(3) 0.068(4) -0.004(2) 0.009(3) 0.012(3) C44A 0.050(5) 0.093(7) 0.042(5) 0.009(4) 0.018(4) -0.024(5) C45A 0.118(12) 0.176(14) 0.049(6) 0.005(7) 0.013(6) -0.060(9) C46A 0.105(8) 0.100(7) 0.050(6) 0.003(5) 0.019(5) -0.010(6) C47A 0.121(10) 0.178(13) 0.074(6) 0.035(7) -0.007(6) 0.029(9) O2B 0.027(3) 0.049(4) 0.047(3) 0.000(3) 0.006(2) -0.011(2) O3B 0.037(3) 0.041(3) 0.040(3) 0.007(3) 0.018(3) -0.012(3) C24B 0.025(4) 0.030(4) 0.033(4) 0.006(3) 0.008(3) 0.005(3) C25B 0.038(5) 0.045(5) 0.034(4) 0.011(3) 0.020(4) 0.013(4) C26B 0.048(7) 0.050(7) 0.033(6) 0.008(5) 0.022(5) 0.012(5) C27B 0.031(5) 0.043(6) 0.035(5) 0.011(4) 0.011(4) 0.012(4) C28B 0.025(4) 0.028(4) 0.038(4) 0.007(3) 0.012(3) 0.008(3) C29B 0.016(3) 0.039(4) 0.030(4) 0.006(3) 0.005(3) 0.004(3) C31B 0.066(7) 0.097(8) 0.055(6) -0.007(6) 0.021(6) -0.051(6) C32B 0.066(7) 0.097(8) 0.055(6) -0.007(6) 0.021(6) -0.051(6) C33B 0.025(3) 0.020(3) 0.030(3) -0.003(3) 0.001(3) -0.008(3) C34B 0.032(13) 0.019(5) 0.031(10) -0.010(5) -0.017(7) 0.005(7) C35B 0.053(6) 0.026(4) 0.020(4) -0.002(3) 0.008(4) -0.009(4) C36B 0.033(4) 0.028(4) 0.039(4) -0.007(3) 0.018(3) 0.001(3) C44B 0.060(7) 0.140(15) 0.019(5) 0.014(6) 0.006(4) -0.060(8) C45B 0.017(4) 0.22(2) 0.035(7) 0.003(11) 0.006(4) 0.006(9) C46B 0.055(7) 0.201(19) 0.062(9) 0.018(10) 0.017(6) 0.007(9) C47B 0.20(3) 0.114(14) 0.22(3) -0.026(15) 0.15(2) -0.031(15) Pd1 0.01962(15) 0.04458(17) 0.03081(16) 0.00954(7) 0.00615(11) 0.00464(7) P1 0.0207(4) 0.0304(4) 0.0285(4) 0.0067(2) 0.0055(3) 0.0033(2) O1 0.0319(12) 0.0697(16) 0.0411(12) 0.0216(11) 0.0006(10) 0.0077(11) N1 0.0276(14) 0.083(2) 0.0332(14) 0.0114(13) 0.0059(11) 0.0007(13) C1 0.0327(14) 0.0276(13) 0.0288(13) 0.0047(10) 0.0127(11) 0.0092(11) C2 0.0390(16) 0.0338(15) 0.0289(13) 0.0026(10) 0.0119(12) 0.0126(12) C3 0.0460(19) 0.059(2) 0.0349(16) 0.0023(14) -0.0095(14) 0.0131(16) C4 0.0555(19) 0.0352(15) 0.0269(13) 0.0063(11) 0.0172(13) 0.0144(14) C5 0.069(2) 0.0337(15) 0.0373(15) 0.0074(12) 0.0305(15) 0.0084(15) C6 0.0476(17) 0.0329(15) 0.0377(15) -0.0015(11) 0.0240(14) 0.0003(13) C7 0.0361(14) 0.0276(13) 0.0294(13) -0.0026(10) 0.0172(12) 0.0038(11) C8 0.0272(13) 0.0312(14) 0.0357(14) -0.0008(10) 0.0134(12) -0.0008(11) C9 0.0403(17) 0.0370(15) 0.0412(16) 0.0063(12) 0.0227(14) 0.0067(13) C10 0.0466(19) 0.0415(18) 0.0365(16) 0.0050(11) 0.0188(15) 0.0158(13) C11 0.065(2) 0.0424(18) 0.0445(17) 0.0053(13) 0.0229(16) 0.0201(16) C12 0.103(4) 0.050(2) 0.066(2) 0.0137(16) 0.062(3) 0.028(2) C13 0.0324(16) 0.054(2) 0.063(2) -0.0091(16) 0.0232(15) 0.0041(15) C14 0.0272(17) 0.074(3) 0.089(3) -0.024(2) 0.0231(18) -0.0042(16) C18 0.0325(16) 0.062(2) 0.063(2) -0.0267(17) 0.0159(15) -0.0113(15) C19 0.0255(13) 0.0397(16) 0.0442(16) -0.0111(12) 0.0130(12) -0.0081(12) C20 0.0321(14) 0.0425(17) 0.0429(17) -0.0152(12) 0.0134(13) -0.0032(13) C21 0.0429(18) 0.063(2) 0.0450(18) -0.0223(15) 0.0179(15) -0.0029(16) C22 0.067(2) 0.0447(19) 0.058(2) -0.0142(16) 0.0275(18) -0.0025(17) C23 0.0264(15) 0.0328(15) 0.0323(15) 0.0010(10) 0.0093(12) -0.0013(11) C30 0.0354(16) 0.0372(17) 0.0522(18) 0.0025(13) 0.0078(14) -0.0075(13) C37 0.0211(13) 0.0534(18) 0.0392(15) 0.0166(13) 0.0076(12) 0.0110(12) C38 0.0441(17) 0.0506(19) 0.0380(16) 0.0160(13) 0.0114(14) 0.0126(15) C39 0.0465(19) 0.054(2) 0.0445(18) 0.0169(15) 0.0012(15) 0.0072(16) C40 0.0290(15) 0.073(2) 0.053(2) 0.0343(17) 0.0038(14) 0.0026(16) C41 0.047(2) 0.099(3) 0.077(3) 0.053(3) 0.007(2) -0.004(2) C42 0.0371(18) 0.102(3) 0.061(2) 0.044(2) 0.0266(17) 0.0254(19) C43 0.0423(18) 0.080(3) 0.053(2) 0.0314(18) 0.0271(16) 0.0282(18) S1 0.0243(3) 0.0507(4) 0.0359(4) 0.0071(3) 0.0067(3) 0.0037(3) F1 0.0411(10) 0.0597(12) 0.0744(13) 0.0066(10) 0.0314(10) 0.0036(9) F2 0.0855(17) 0.108(2) 0.0373(10) -0.0027(11) 0.0155(11) 0.0387(15) F3 0.0585(13) 0.0501(13) 0.0958(17) -0.0169(11) 0.0223(12) -0.0013(10) O4 0.0504(14) 0.0429(13) 0.0460(12) 0.0050(9) 0.0123(11) 0.0089(10) O5 0.0392(12) 0.0660(15) 0.0407(12) 0.0166(10) 0.0105(10) 0.0071(11) O6 0.0246(11) 0.0836(19) 0.0690(16) 0.0104(14) 0.0115(11) -0.0035(11) C48 0.0361(16) 0.0448(18) 0.0449(17) -0.0017(13) 0.0111(14) 0.0029(13) C17 0.057(3) 0.165(6) 0.078(3) -0.040(3) 0.029(2) -0.065(3) C15 0.0282(19) 0.122(4) 0.130(5) -0.073(4) 0.023(2) -0.009(2) C16 0.040(2) 0.096(4) 0.133(5) 0.006(3) -0.021(3) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2A C31A 1.372(8) . ? O2A C30 1.469(5) . ? O3A C32A 1.426(7) . ? O3A C30 1.431(5) . ? C24A C25A 1.508(8) . ? C24A C23 1.549(5) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A C26A 1.504(9) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A C27A 1.524(11) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27A C28A 1.541(7) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A C23 1.489(5) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C29A C30 1.517(6) . ? C29A C23 1.584(5) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C31A C32A 1.414(11) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C30 1.503(7) . ? C33A C34A 1.709(15) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A C36A 1.470(19) . ? C34A C35A 1.621(16) . ? C34A P1 1.818(17) . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C44A N1 1.497(11) . ? C44A C45A 1.545(14) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.560(13) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A C47A 1.472(11) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? O2B C31B 1.374(11) . ? O2B C30 1.380(6) . ? O3B C32B 1.401(11) . ? O3B C30 1.406(6) . ? C24B C23 1.480(8) . ? C24B C25B 1.502(11) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B C26B 1.498(14) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C26B C27B 1.509(13) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27B C28B 1.538(12) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B C23 1.660(7) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B C30 1.519(8) . ? C29B C23 1.566(8) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C31B C32B 1.421(14) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.51(3) . ? C33B C30 1.615(8) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35B 1.23(3) . ? C34B C36B 1.78(3) . ? C34B P1 2.04(3) . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C44B C45B 1.533(17) . ? C44B N1 1.539(14) . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45B C46B 1.493(14) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B C47B 1.430(16) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? Pd1 C37 2.030(3) . ? Pd1 N1 2.121(3) . ? Pd1 P1 2.3329(7) . ? Pd1 C8 2.412(3) . ? P1 C1 1.840(3) . ? P1 C23 1.903(3) . ? O1 C2 1.353(4) . ? O1 C3 1.429(4) . ? N1 H1N 1.02(3) . ? N1 H2N 1.03(4) . ? C1 C7 1.393(4) . ? C1 C2 1.417(4) . ? C2 C4 1.394(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.365(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.397(4) . ? C6 H6 0.9500 . ? C7 C8 1.512(4) . ? C8 C19 1.411(4) . ? C8 C9 1.427(4) . ? C9 C13 1.377(5) . ? C9 C10 1.522(4) . ? C10 C12 1.532(5) . ? C10 C11 1.532(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C18 1.398(5) . ? C14 C15 1.517(5) . ? C18 C19 1.397(4) . ? C18 H18 0.9500 . ? C19 C20 1.525(4) . ? C20 C21 1.530(4) . ? C20 C22 1.533(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C37 C43 1.389(5) . ? C37 C38 1.399(5) . ? C38 C39 1.383(5) . ? C38 H38 0.9500 . ? C39 C40 1.372(5) . ? C39 H39 0.9500 . ? C40 C42 1.374(6) . ? C40 C41 1.529(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.386(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? S1 O6 1.431(2) . ? S1 O4 1.436(2) . ? S1 O5 1.441(2) . ? S1 C48 1.820(3) . ? F1 C48 1.331(4) . ? F2 C48 1.342(4) . ? F3 C48 1.323(4) . ? C17 C15 1.588(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C15 C16 1.505(9) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31A O2A C30 109.3(5) . . ? C32A O3A C30 107.9(5) . . ? C25A C24A C23 113.1(4) . . ? C25A C24A H24A 109.0 . . ? C23 C24A H24A 109.0 . . ? C25A C24A H24B 109.0 . . ? C23 C24A H24B 109.0 . . ? H24A C24A H24B 107.8 . . ? C26A C25A C24A 111.0(5) . . ? C26A C25A H25A 109.4 . . ? C24A C25A H25A 109.4 . . ? C26A C25A H25B 109.4 . . ? C24A C25A H25B 109.4 . . ? H25A C25A H25B 108.0 . . ? C25A C26A C27A 110.4(5) . . ? C25A C26A H26A 109.6 . . ? C27A C26A H26A 109.6 . . ? C25A C26A H26B 109.6 . . ? C27A C26A H26B 109.6 . . ? H26A C26A H26B 108.1 . . ? C26A C27A C28A 112.1(6) . . ? C26A C27A H27A 109.2 . . ? C28A C27A H27A 109.2 . . ? C26A C27A H27B 109.2 . . ? C28A C27A H27B 109.2 . . ? H27A C27A H27B 107.9 . . ? C23 C28A C27A 111.6(4) . . ? C23 C28A H28A 109.3 . . ? C27A C28A H28A 109.3 . . ? C23 C28A H28B 109.3 . . ? C27A C28A H28B 109.3 . . ? H28A C28A H28B 108.0 . . ? C30 C29A C23 114.5(4) . . ? C30 C29A H29A 108.6 . . ? C23 C29A H29A 108.6 . . ? C30 C29A H29B 108.6 . . ? C23 C29A H29B 108.6 . . ? H29A C29A H29B 107.6 . . ? O2A C31A C32A 108.6(7) . . ? O2A C31A H31A 110.0 . . ? C32A C31A H31A 110.0 . . ? O2A C31A H31B 110.0 . . ? C32A C31A H31B 110.0 . . ? H31A C31A H31B 108.3 . . ? C31A C32A O3A 105.8(6) . . ? C31A C32A H32A 110.6 . . ? O3A C32A H32A 110.6 . . ? C31A C32A H32B 110.6 . . ? O3A C32A H32B 110.6 . . ? H32A C32A H32B 108.7 . . ? C30 C33A C34A 111.1(6) . . ? C30 C33A H33A 109.4 . . ? C34A C33A H33A 109.4 . . ? C30 C33A H33B 109.4 . . ? C34A C33A H33B 109.4 . . ? H33A C33A H33B 108.0 . . ? C36A C34A C35A 104.6(10) . . ? C36A C34A C33A 103.1(10) . . ? C35A C34A C33A 98.2(9) . . ? C36A C34A P1 122.5(10) . . ? C35A C34A P1 115.8(10) . . ? C33A C34A P1 109.3(9) . . ? C34A C35A H35A 109.5 . . ? C34A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C34A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C34A C36A H36A 109.5 . . ? C34A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C34A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? N1 C44A C45A 113.8(10) . . ? N1 C44A H44A 108.8 . . ? C45A C44A H44A 108.8 . . ? N1 C44A H44B 108.8 . . ? C45A C44A H44B 108.8 . . ? H44A C44A H44B 107.7 . . ? C44A C45A C46A 111.2(10) . . ? C44A C45A H45A 109.4 . . ? C46A C45A H45A 109.4 . . ? C44A C45A H45B 109.4 . . ? C46A C45A H45B 109.4 . . ? H45A C45A H45B 108.0 . . ? C47A C46A C45A 110.1(10) . . ? C47A C46A H46A 109.6 . . ? C45A C46A H46A 109.6 . . ? C47A C46A H46B 109.6 . . ? C45A C46A H46B 109.6 . . ? H46A C46A H46B 108.2 . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C31B O2B C30 107.7(7) . . ? C32B O3B C30 104.2(6) . . ? C23 C24B C25B 116.9(6) . . ? C23 C24B H24C 108.1 . . ? C25B C24B H24C 108.1 . . ? C23 C24B H24D 108.1 . . ? C25B C24B H24D 108.1 . . ? H24C C24B H24D 107.3 . . ? C26B C25B C24B 112.3(8) . . ? C26B C25B H25C 109.1 . . ? C24B C25B H25C 109.1 . . ? C26B C25B H25D 109.1 . . ? C24B C25B H25D 109.1 . . ? H25C C25B H25D 107.9 . . ? C25B C26B C27B 110.1(9) . . ? C25B C26B H26C 109.6 . . ? C27B C26B H26C 109.6 . . ? C25B C26B H26D 109.6 . . ? C27B C26B H26D 109.6 . . ? H26C C26B H26D 108.2 . . ? C26B C27B C28B 110.5(8) . . ? C26B C27B H27C 109.5 . . ? C28B C27B H27C 109.5 . . ? C26B C27B H27D 109.5 . . ? C28B C27B H27D 109.5 . . ? H27C C27B H27D 108.1 . . ? C27B C28B C23 113.0(6) . . ? C27B C28B H28C 109.0 . . ? C23 C28B H28C 109.0 . . ? C27B C28B H28D 109.0 . . ? C23 C28B H28D 109.0 . . ? H28C C28B H28D 107.8 . . ? C30 C29B C23 115.5(5) . . ? C30 C29B H29C 108.4 . . ? C23 C29B H29C 108.4 . . ? C30 C29B H29D 108.4 . . ? C23 C29B H29D 108.4 . . ? H29C C29B H29D 107.5 . . ? O2B C31B C32B 105.5(10) . . ? O2B C31B H31C 110.6 . . ? C32B C31B H31C 110.6 . . ? O2B C31B H31D 110.6 . . ? C32B C31B H31D 110.6 . . ? H31C C31B H31D 108.8 . . ? O3B C32B C31B 108.2(9) . . ? O3B C32B H32C 110.1 . . ? C31B C32B H32C 110.1 . . ? O3B C32B H32D 110.1 . . ? C31B C32B H32D 110.1 . . ? H32C C32B H32D 108.4 . . ? C34B C33B C30 107.1(11) . . ? C34B C33B H33C 110.3 . . ? C30 C33B H33C 110.3 . . ? C34B C33B H33D 110.3 . . ? C30 C33B H33D 110.3 . . ? H33C C33B H33D 108.5 . . ? C35B C34B C33B 136(2) . . ? C35B C34B C36B 108(2) . . ? C33B C34B C36B 99.9(16) . . ? C35B C34B P1 119(2) . . ? C33B C34B P1 94.6(14) . . ? C36B C34B P1 89.9(11) . . ? C34B C35B H35D 109.5 . . ? C34B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C34B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C34B C36B H36D 109.5 . . ? C34B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C34B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C45B C44B N1 109.0(13) . . ? C45B C44B H44C 109.9 . . ? N1 C44B H44C 109.9 . . ? C45B C44B H44D 109.9 . . ? N1 C44B H44D 109.9 . . ? H44C C44B H44D 108.3 . . ? C46B C45B C44B 116.1(12) . . ? C46B C45B H45C 108.3 . . ? C44B C45B H45C 108.3 . . ? C46B C45B H45D 108.3 . . ? C44B C45B H45D 108.3 . . ? H45C C45B H45D 107.4 . . ? C47B C46B C45B 101.5(18) . . ? C47B C46B H46C 111.5 . . ? C45B C46B H46C 111.5 . . ? C47B C46B H46D 111.5 . . ? C45B C46B H46D 111.5 . . ? H46C C46B H46D 109.3 . . ? C46B C47B H47D 109.5 . . ? C46B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C37 Pd1 N1 79.61(11) . . ? C37 Pd1 P1 97.50(8) . . ? N1 Pd1 P1 176.54(10) . . ? C37 Pd1 C8 176.22(11) . . ? N1 Pd1 C8 99.20(11) . . ? P1 Pd1 C8 83.56(7) . . ? C34A P1 C1 109.1(5) . . ? C34A P1 C23 106.6(5) . . ? C1 P1 C23 109.17(12) . . ? C1 P1 C34B 105.7(9) . . ? C23 P1 C34B 101.6(9) . . ? C34A P1 Pd1 112.6(5) . . ? C1 P1 Pd1 104.41(9) . . ? C23 P1 Pd1 114.87(9) . . ? C34B P1 Pd1 120.5(8) . . ? C2 O1 C3 120.0(3) . . ? C44A N1 Pd1 116.4(5) . . ? C44B N1 Pd1 116.3(7) . . ? C44A N1 H1N 104(3) . . ? C44B N1 H1N 119(3) . . ? Pd1 N1 H1N 110(3) . . ? C44A N1 H2N 114(3) . . ? C44B N1 H2N 99(3) . . ? Pd1 N1 H2N 115(3) . . ? H1N N1 H2N 95(4) . . ? C7 C1 C2 117.9(2) . . ? C7 C1 P1 117.14(19) . . ? C2 C1 P1 124.9(2) . . ? O1 C2 C4 122.5(3) . . ? O1 C2 C1 116.5(2) . . ? C4 C2 C1 121.0(3) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 119.8(3) . . ? C5 C4 H4 120.1 . . ? C2 C4 H4 120.1 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C1 C7 C6 120.5(3) . . ? C1 C7 C8 126.6(2) . . ? C6 C7 C8 112.9(3) . . ? C19 C8 C9 118.5(3) . . ? C19 C8 C7 118.5(2) . . ? C9 C8 C7 117.8(2) . . ? C19 C8 Pd1 93.90(18) . . ? C9 C8 Pd1 90.75(18) . . ? C7 C8 Pd1 108.23(17) . . ? C13 C9 C8 119.7(3) . . ? C13 C9 C10 119.1(3) . . ? C8 C9 C10 121.0(3) . . ? C9 C10 C12 110.6(3) . . ? C9 C10 C11 112.5(3) . . ? C12 C10 C11 109.4(3) . . ? C9 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 121.9(3) . . ? C14 C13 H13 119.0 . . ? C9 C13 H13 119.0 . . ? C13 C14 C18 118.9(3) . . ? C13 C14 C15 121.2(3) . . ? C18 C14 C15 119.9(3) . . ? C19 C18 C14 120.9(3) . . ? C19 C18 H18 119.5 . . ? C14 C18 H18 119.5 . . ? C18 C19 C8 119.6(3) . . ? C18 C19 C20 119.0(3) . . ? C8 C19 C20 120.9(2) . . ? C19 C20 C21 111.6(3) . . ? C19 C20 C22 110.7(3) . . ? C21 C20 C22 110.7(3) . . ? C19 C20 H20 107.9 . . ? C21 C20 H20 107.9 . . ? C22 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28A C23 C24A 110.2(3) . . ? C24B C23 C29B 114.3(5) . . ? C28A C23 C29A 113.5(3) . . ? C24A C23 C29A 108.5(3) . . ? C24B C23 C28B 105.3(4) . . ? C29B C23 C28B 103.2(4) . . ? C24B C23 P1 115.5(3) . . ? C28A C23 P1 118.2(3) . . ? C24A C23 P1 102.8(2) . . ? C29B C23 P1 107.4(3) . . ? C29A C23 P1 102.6(2) . . ? C28B C23 P1 110.4(3) . . ? O2B C30 O3B 110.0(4) . . ? O3A C30 O2A 103.1(3) . . ? O3A C30 C33A 113.1(4) . . ? O2A C30 C33A 106.8(3) . . ? O3A C30 C29A 106.8(3) . . ? O2A C30 C29A 108.4(3) . . ? C33A C30 C29A 117.5(3) . . ? O2B C30 C29B 109.4(4) . . ? O3B C30 C29B 112.7(5) . . ? O2B C30 C33B 107.5(4) . . ? O3B C30 C33B 105.3(4) . . ? C29B C30 C33B 111.7(4) . . ? C43 C37 C38 116.1(3) . . ? C43 C37 Pd1 124.1(3) . . ? C38 C37 Pd1 118.4(2) . . ? C39 C38 C37 121.8(3) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C40 C39 C38 121.4(4) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C42 117.4(3) . . ? C39 C40 C41 121.0(4) . . ? C42 C40 C41 121.6(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 C43 121.9(3) . . ? C40 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C42 C43 C37 121.4(4) . . ? C42 C43 H43 119.3 . . ? C37 C43 H43 119.3 . . ? O6 S1 O4 114.39(16) . . ? O6 S1 O5 115.41(15) . . ? O4 S1 O5 115.30(15) . . ? O6 S1 C48 104.21(16) . . ? O4 S1 C48 103.78(15) . . ? O5 S1 C48 101.27(14) . . ? F3 C48 F1 107.5(3) . . ? F3 C48 F2 107.3(3) . . ? F1 C48 F2 107.4(3) . . ? F3 C48 S1 112.1(2) . . ? F1 C48 S1 111.1(2) . . ? F2 C48 S1 111.2(2) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C15 C14 112.7(5) . . ? C16 C15 C17 111.4(4) . . ? C14 C15 C17 108.0(5) . . ? C16 C15 H15 108.2 . . ? C14 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _refine_diff_density_max 0.921 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.060 _shelx_res_file ; TITL XRAY5748_0m_a.res in C2/c XRAY5748_0m_a.res created by SHELXL-2016/6 at 19:02:34 on 12-Mar-2019 CELL 1.54178 28.3488 18.5998 19.6316 90.000 112.701 90.000 ZERR 8.000 0.0004 0.0003 0.0003 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H F N O P Pd S UNIT 384 568 24 8 48 8 8 8 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.10 0.25 0.32 SADI C31A C32A C31B C32B SADI O2A C31A O3A C32A O2B C31B O3B C32B SADI C30 O2A C30 O3A C30 O2B C30 O3B EADP C31B C32B SADI N1 H1N N1 H2N DFIX 1.485 N1 C44A N1 C44B DFIX 1.506 C44A C45A C44B C45B DFIX 1.511 C45A C46A C45B C46B DFIX 1.492 C46A C47A C46B C47B DFIX 0.04 2.487 N1 C45A N1 C45B DFIX 0.04 2.551 C44A C46A C44B C46B DFIX 0.04 2.503 C45A C47A C45B C47B SIMU C44A C45A SIMU C44B C45B ISOR C45A C45B ISOR C46A C46B ISOR C47A C47B TEMP -173.0 WGHT 0.100000 0.491140 FVAR 0.11362 0.63233 0.59010 PART 1 MOLE 1 O2A 5 0.644782 0.337309 0.528621 21.00000 0.03012 0.05672 = 0.09041 0.00823 -0.00337 -0.01358 O3A 5 0.590786 0.429516 0.474531 21.00000 0.05180 0.03869 = 0.08530 0.00252 0.01254 -0.01677 C24A 1 0.514308 0.194984 0.383229 21.00000 0.03874 0.03151 = 0.04146 0.00043 0.01339 -0.00473 AFIX 23 H24A 2 0.497272 0.152762 0.394419 21.00000 -1.20000 H24B 2 0.487369 0.226697 0.349442 21.00000 -1.20000 AFIX 0 C25A 1 0.548204 0.169827 0.344708 21.00000 0.05452 0.03915 = 0.05024 0.00644 0.02601 0.00771 AFIX 23 H25A 2 0.527716 0.141362 0.300566 21.00000 -1.20000 H25B 2 0.562170 0.212048 0.328064 21.00000 -1.20000 AFIX 0 C26A 1 0.591542 0.124608 0.395290 21.00000 0.07434 0.05486 = 0.05195 0.01771 0.03726 0.02981 AFIX 23 H26A 2 0.614506 0.111433 0.369991 21.00000 -1.20000 H26B 2 0.577808 0.079723 0.407632 21.00000 -1.20000 AFIX 0 C27A 1 0.621641 0.165678 0.465930 21.00000 0.04233 0.06599 = 0.06592 0.02079 0.02901 0.02600 AFIX 23 H27A 2 0.638464 0.207607 0.453796 21.00000 -1.20000 H27B 2 0.648713 0.134100 0.499652 21.00000 -1.20000 AFIX 0 C28A 1 0.587282 0.191943 0.505521 21.00000 0.02737 0.03849 = 0.03868 0.00575 0.00743 0.00963 AFIX 23 H28A 2 0.573728 0.149884 0.523049 21.00000 -1.20000 H28B 2 0.607968 0.220871 0.549182 21.00000 -1.20000 AFIX 0 C29A 1 0.560821 0.311749 0.435725 21.00000 0.02672 0.03750 = 0.04633 0.00245 0.00735 -0.00060 AFIX 23 H29A 2 0.582060 0.303576 0.406541 21.00000 -1.20000 H29B 2 0.529888 0.338364 0.404029 21.00000 -1.20000 AFIX 0 C31A 1 0.673888 0.396828 0.530657 21.00000 0.06358 0.08505 = 0.11439 -0.02184 0.03874 -0.04623 AFIX 23 H31A 2 0.691908 0.390271 0.496788 21.00000 -1.20000 H31B 2 0.699798 0.403897 0.581247 21.00000 -1.20000 AFIX 0 C32A 1 0.641365 0.457439 0.508961 21.00000 0.06185 0.05949 = 0.10329 -0.00034 -0.00258 -0.03439 AFIX 23 H32A 2 0.650087 0.487540 0.473887 21.00000 -1.20000 H32B 2 0.644553 0.487029 0.552440 21.00000 -1.20000 AFIX 0 C33A 1 0.575485 0.355582 0.567135 21.00000 0.04496 0.03280 = 0.05247 -0.00809 -0.00143 -0.00449 AFIX 23 H33A 2 0.586379 0.400515 0.596013 21.00000 -1.20000 H33B 2 0.593097 0.314903 0.599472 21.00000 -1.20000 AFIX 0 C34A 1 0.510852 0.345522 0.539740 21.00000 0.02017 0.03285 = 0.02453 -0.00187 -0.00055 0.00051 C35A 1 0.507963 0.347538 0.620565 21.00000 0.05617 0.04397 = 0.04814 -0.01434 0.01168 0.00917 AFIX 137 H35A 2 0.521491 0.393485 0.644599 21.00000 -1.50000 H35B 2 0.528339 0.308020 0.650717 21.00000 -1.50000 H35C 2 0.472312 0.342327 0.615257 21.00000 -1.50000 AFIX 0 C36A 1 0.490828 0.415730 0.506907 21.00000 0.06561 0.03037 = 0.06791 -0.00426 0.00906 0.01233 AFIX 137 H36A 2 0.453624 0.416556 0.492089 21.00000 -1.50000 H36B 2 0.499192 0.423682 0.463495 21.00000 -1.50000 H36C 2 0.506318 0.453762 0.543248 21.00000 -1.50000 AFIX 0 C44A 1 0.326492 0.244962 0.240152 31.00000 0.04965 0.09252 = 0.04247 0.00867 0.01787 -0.02409 AFIX 23 H44A 2 0.322307 0.192721 0.245709 31.00000 -1.20000 H44B 2 0.356993 0.251693 0.227973 31.00000 -1.20000 AFIX 0 C45A 1 0.279019 0.273313 0.175345 31.00000 0.11843 0.17574 = 0.04933 0.00487 0.01259 -0.05973 AFIX 23 H45A 2 0.249225 0.273347 0.189849 31.00000 -1.20000 H45B 2 0.271159 0.240901 0.132358 31.00000 -1.20000 AFIX 0 C46A 1 0.288133 0.350982 0.153064 31.00000 0.10472 0.09992 = 0.05048 0.00349 0.01936 -0.00965 AFIX 23 H46A 2 0.294645 0.383942 0.195328 31.00000 -1.20000 H46B 2 0.318569 0.351465 0.140046 31.00000 -1.20000 AFIX 0 C47A 1 0.243107 0.375744 0.089590 31.00000 0.12120 0.17819 = 0.07423 0.03467 -0.00726 0.02896 AFIX 137 H47A 2 0.237187 0.343626 0.047512 31.00000 -1.50000 H47B 2 0.249093 0.424713 0.076318 31.00000 -1.50000 H47C 2 0.213063 0.375379 0.102679 31.00000 -1.50000 PART 2 AFIX 0 O2B 5 0.627038 0.386932 0.565153 -21.00000 0.02723 0.04908 = 0.04674 -0.00031 0.00630 -0.01147 O3B 5 0.597214 0.385614 0.439279 -21.00000 0.03714 0.04098 = 0.04014 0.00705 0.01833 -0.01188 C24B 1 0.530792 0.244721 0.375657 -21.00000 0.02489 0.02960 = 0.03349 0.00564 0.00802 0.00511 AFIX 23 H24C 2 0.525073 0.296488 0.363550 -21.00000 -1.20000 H24D 2 0.497982 0.219691 0.348991 -21.00000 -1.20000 AFIX 0 C25B 1 0.569121 0.217593 0.346172 -21.00000 0.03758 0.04506 = 0.03439 0.01062 0.01956 0.01273 AFIX 23 H25C 2 0.555901 0.225977 0.292223 -21.00000 -1.20000 H25D 2 0.601302 0.245122 0.369094 -21.00000 -1.20000 AFIX 0 C26B 1 0.580207 0.139133 0.361177 -21.00000 0.04793 0.04986 = 0.03293 0.00831 0.02240 0.01225 AFIX 23 H26C 2 0.606507 0.123945 0.342541 -21.00000 -1.20000 H26D 2 0.548785 0.110904 0.334972 -21.00000 -1.20000 AFIX 0 C27B 1 0.598996 0.124706 0.443028 -21.00000 0.03146 0.04262 = 0.03480 0.01097 0.01087 0.01220 AFIX 23 H27C 2 0.631759 0.150173 0.468765 -21.00000 -1.20000 H27D 2 0.605168 0.072552 0.452286 -21.00000 -1.20000 AFIX 0 C28B 1 0.559456 0.150230 0.473696 -21.00000 0.02516 0.02800 = 0.03753 0.00660 0.01249 0.00774 AFIX 23 H28C 2 0.573477 0.142768 0.527815 -21.00000 -1.20000 H28D 2 0.528216 0.120512 0.452003 -21.00000 -1.20000 AFIX 0 C29B 1 0.593531 0.276687 0.506005 -21.00000 0.01639 0.03915 = 0.02957 0.00643 0.00473 0.00437 AFIX 23 H29C 2 0.601929 0.262092 0.557873 -21.00000 -1.20000 H29D 2 0.622020 0.260772 0.492295 -21.00000 -1.20000 AFIX 0 C31B 1 0.661104 0.425043 0.544967 -21.00000 0.06594 0.09688 = 0.05488 -0.00718 0.02074 -0.05098 AFIX 23 H31C 2 0.692874 0.397096 0.555547 -21.00000 -1.20000 H31D 2 0.669938 0.471195 0.572085 -21.00000 -1.20000 AFIX 0 C32B 1 0.635785 0.437320 0.467857 -21.00000 0.06594 0.09688 = 0.05488 -0.00718 0.02074 -0.05098 AFIX 23 H32C 2 0.620763 0.486171 0.458857 -21.00000 -1.20000 H32D 2 0.660406 0.433427 0.443450 -21.00000 -1.20000 AFIX 0 C33B 1 0.535568 0.387489 0.495773 -21.00000 0.02512 0.01987 = 0.02954 -0.00316 0.00079 -0.00824 AFIX 23 H33C 2 0.536955 0.440029 0.504408 -21.00000 -1.20000 H33D 2 0.509339 0.377562 0.446032 -21.00000 -1.20000 AFIX 0 C34B 1 0.522558 0.348676 0.553985 -21.00000 0.03183 0.01922 = 0.03120 -0.01006 -0.01711 0.00518 C35B 1 0.543388 0.340217 0.621370 -21.00000 0.05257 0.02640 = 0.02008 -0.00218 0.00756 -0.00864 AFIX 137 H35D 2 0.576009 0.315153 0.633255 -21.00000 -1.50000 H35E 2 0.521125 0.311572 0.638557 -21.00000 -1.50000 H35F 2 0.549586 0.387202 0.645851 -21.00000 -1.50000 AFIX 0 C36B 1 0.460393 0.383705 0.534315 -21.00000 0.03306 0.02753 = 0.03859 -0.00687 0.01753 0.00119 AFIX 137 H36D 2 0.444278 0.357214 0.562767 -21.00000 -1.50000 H36E 2 0.439671 0.378542 0.481464 -21.00000 -1.50000 H36F 2 0.462927 0.434690 0.547861 -21.00000 -1.50000 AFIX 0 C44B 1 0.331476 0.269876 0.232429 -31.00000 0.05996 0.14007 = 0.01911 0.01388 0.00571 -0.06049 AFIX 23 H44C 2 0.363562 0.285260 0.227869 -31.00000 -1.20000 H44D 2 0.325998 0.218292 0.219314 -31.00000 -1.20000 AFIX 0 C45B 1 0.286486 0.314159 0.180120 -31.00000 0.01724 0.22214 = 0.03502 0.00269 0.00610 0.00573 AFIX 23 H45C 2 0.254431 0.293112 0.180198 -31.00000 -1.20000 H45D 2 0.289290 0.363515 0.200189 -31.00000 -1.20000 AFIX 0 C46B 1 0.282098 0.319131 0.101980 -31.00000 0.05479 0.20130 = 0.06237 0.01751 0.01701 0.00668 AFIX 23 H46C 2 0.257817 0.357279 0.074649 -31.00000 -1.20000 H46D 2 0.315731 0.328251 0.099254 -31.00000 -1.20000 AFIX 0 C47B 1 0.263126 0.249237 0.074628 -31.00000 0.19642 0.11385 = 0.22255 -0.02621 0.14671 -0.03096 AFIX 137 H47D 2 0.283129 0.212717 0.109956 -31.00000 -1.50000 H47E 2 0.266096 0.241488 0.027065 -31.00000 -1.50000 H47F 2 0.227151 0.245604 0.068117 -31.00000 -1.50000 PART 0 AFIX 0 PD1 7 0.409444 0.268335 0.396395 11.00000 0.01962 0.04458 = 0.03081 0.00954 0.00615 0.00464 P1 6 0.491220 0.261697 0.489025 11.00000 0.02069 0.03043 = 0.02850 0.00673 0.00547 0.00335 O1 5 0.571263 0.205381 0.636266 11.00000 0.03187 0.06970 = 0.04110 0.02156 0.00064 0.00767 N1 4 0.335639 0.281211 0.312209 11.00000 0.02763 0.08332 = 0.03324 0.01138 0.00593 0.00068 H1N 2 0.308871 0.259247 0.328476 11.00000 0.05812 H2N 2 0.321024 0.332591 0.306663 11.00000 0.10865 C1 1 0.486109 0.191583 0.551973 11.00000 0.03267 0.02764 = 0.02882 0.00473 0.01270 0.00924 C2 1 0.526001 0.171217 0.619043 11.00000 0.03897 0.03380 = 0.02885 0.00258 0.01190 0.01263 C3 1 0.614493 0.184410 0.700187 11.00000 0.04603 0.05870 = 0.03493 0.00229 -0.00952 0.01307 AFIX 137 H3A 2 0.607509 0.193700 0.744544 11.00000 -1.50000 H3B 2 0.644502 0.212122 0.702613 11.00000 -1.50000 H3C 2 0.621115 0.133026 0.697244 11.00000 -1.50000 AFIX 0 C4 1 0.518226 0.118898 0.664484 11.00000 0.05551 0.03520 = 0.02694 0.00628 0.01721 0.01445 AFIX 43 H4 2 0.545228 0.106038 0.709521 11.00000 -1.20000 AFIX 0 C5 1 0.471686 0.086213 0.644048 11.00000 0.06859 0.03369 = 0.03728 0.00739 0.03045 0.00839 AFIX 43 H5 2 0.466478 0.050473 0.675013 11.00000 -1.20000 AFIX 0 C6 1 0.431839 0.104683 0.578399 11.00000 0.04763 0.03288 = 0.03774 -0.00155 0.02395 0.00032 AFIX 43 H6 2 0.399639 0.081460 0.564653 11.00000 -1.20000 AFIX 0 C7 1 0.439044 0.157327 0.532593 11.00000 0.03610 0.02765 = 0.02938 -0.00261 0.01720 0.00378 C8 1 0.391412 0.171583 0.464527 11.00000 0.02716 0.03121 = 0.03568 -0.00078 0.01344 -0.00079 C9 1 0.351585 0.212714 0.473213 11.00000 0.04031 0.03698 = 0.04124 0.00626 0.02270 0.00669 C10 1 0.363089 0.265585 0.536798 11.00000 0.04657 0.04149 = 0.03646 0.00502 0.01884 0.01578 AFIX 13 H10 2 0.400956 0.272752 0.559867 11.00000 -1.20000 AFIX 0 C11 1 0.338035 0.339052 0.511334 11.00000 0.06492 0.04235 = 0.04450 0.00526 0.02290 0.02009 AFIX 137 H11A 2 0.347169 0.356996 0.471093 11.00000 -1.50000 H11B 2 0.350109 0.372933 0.552744 11.00000 -1.50000 H11C 2 0.300803 0.334216 0.493878 11.00000 -1.50000 AFIX 0 C12 1 0.345636 0.235175 0.595763 11.00000 0.10265 0.05021 = 0.06638 0.01368 0.06203 0.02808 AFIX 137 H12A 2 0.308911 0.224873 0.573546 11.00000 -1.50000 H12B 2 0.352410 0.270443 0.635511 11.00000 -1.50000 H12C 2 0.364423 0.190756 0.615954 11.00000 -1.50000 AFIX 0 C13 1 0.301499 0.200710 0.426902 11.00000 0.03239 0.05435 = 0.06330 -0.00907 0.02324 0.00407 AFIX 43 H13 2 0.275344 0.228933 0.432641 11.00000 -1.20000 AFIX 0 C14 1 0.288215 0.149057 0.372571 11.00000 0.02715 0.07371 = 0.08901 -0.02394 0.02308 -0.00419 C18 1 0.326994 0.112541 0.359411 11.00000 0.03254 0.06183 = 0.06320 -0.02672 0.01585 -0.01132 AFIX 43 H18 2 0.318298 0.080421 0.318768 11.00000 -1.20000 AFIX 0 C19 1 0.378346 0.122628 0.405189 11.00000 0.02554 0.03970 = 0.04420 -0.01113 0.01303 -0.00808 C20 1 0.418604 0.073516 0.396055 11.00000 0.03206 0.04248 = 0.04290 -0.01521 0.01341 -0.00317 AFIX 13 H20 2 0.453032 0.092129 0.428666 11.00000 -1.20000 AFIX 0 C21 1 0.415657 0.073872 0.316558 11.00000 0.04287 0.06278 = 0.04497 -0.02234 0.01786 -0.00289 AFIX 137 H21A 2 0.384060 0.050131 0.284313 11.00000 -1.50000 H21B 2 0.445157 0.048103 0.314249 11.00000 -1.50000 H21C 2 0.415868 0.123609 0.300204 11.00000 -1.50000 AFIX 0 C22 1 0.413523 -0.003235 0.420882 11.00000 0.06698 0.04467 = 0.05846 -0.01420 0.02748 -0.00246 AFIX 137 H22A 2 0.418019 -0.002791 0.472944 11.00000 -1.50000 H22B 2 0.439747 -0.033853 0.414759 11.00000 -1.50000 H22C 2 0.379556 -0.022124 0.390811 11.00000 -1.50000 AFIX 0 C23 1 0.543830 0.236197 0.455850 11.00000 0.02644 0.03277 = 0.03226 0.00105 0.00934 -0.00128 C30 1 0.590685 0.358213 0.501838 11.00000 0.03537 0.03717 = 0.05218 0.00248 0.00781 -0.00747 C37 1 0.421924 0.354123 0.341615 11.00000 0.02113 0.05340 = 0.03919 0.01659 0.00757 0.01103 C38 1 0.401126 0.420563 0.348635 11.00000 0.04410 0.05063 = 0.03798 0.01605 0.01142 0.01262 AFIX 43 H38 2 0.387001 0.426138 0.385032 11.00000 -1.20000 AFIX 0 C39 1 0.400574 0.478361 0.304006 11.00000 0.04654 0.05365 = 0.04448 0.01687 0.00125 0.00719 AFIX 43 H39 2 0.386374 0.522755 0.310747 11.00000 -1.20000 AFIX 0 C40 1 0.420092 0.472970 0.250205 11.00000 0.02902 0.07257 = 0.05345 0.03426 0.00381 0.00265 C41 1 0.421252 0.538077 0.203287 11.00000 0.04665 0.09945 = 0.07685 0.05350 0.00735 -0.00439 AFIX 137 H41A 2 0.389509 0.565551 0.190725 11.00000 -1.50000 H41B 2 0.424524 0.521694 0.157866 11.00000 -1.50000 H41C 2 0.450465 0.568704 0.231206 11.00000 -1.50000 AFIX 0 C42 1 0.439204 0.407350 0.241200 11.00000 0.03707 0.10249 = 0.06070 0.04380 0.02659 0.02538 AFIX 43 H42 2 0.452032 0.401826 0.203378 11.00000 -1.20000 AFIX 0 C43 1 0.440309 0.349005 0.285682 11.00000 0.04226 0.08046 = 0.05332 0.03140 0.02707 0.02818 AFIX 43 H43 2 0.453928 0.304580 0.277748 11.00000 -1.20000 AFIX 0 S1 8 0.768113 0.580072 0.691332 11.00000 0.02430 0.05070 = 0.03592 0.00709 0.00674 0.00374 F1 3 0.844696 0.551074 0.653005 11.00000 0.04108 0.05974 = 0.07443 0.00655 0.03139 0.00363 F2 3 0.771631 0.555885 0.561754 11.00000 0.08552 0.10794 = 0.03732 -0.00275 0.01554 0.03874 F3 3 0.791329 0.464578 0.634284 11.00000 0.05852 0.05006 = 0.09575 -0.01690 0.02226 -0.00126 O4 5 0.776403 0.655048 0.682534 11.00000 0.05041 0.04289 = 0.04600 0.00499 0.01227 0.00889 O5 5 0.798649 0.550095 0.762438 11.00000 0.03922 0.06600 = 0.04069 0.01659 0.01054 0.00711 O6 5 0.715547 0.558807 0.661701 11.00000 0.02455 0.08363 = 0.06904 0.01044 0.01146 -0.00347 C48 1 0.795301 0.535361 0.632411 11.00000 0.03608 0.04482 = 0.04487 -0.00172 0.01111 0.00290 C17 1 0.224697 0.048824 0.351068 11.00000 0.05721 0.16457 = 0.07819 -0.03997 0.02907 -0.06549 AFIX 137 H17A 2 0.244616 0.015883 0.333643 11.00000 -1.50000 H17B 2 0.188367 0.036279 0.327924 11.00000 -1.50000 H17C 2 0.236139 0.044879 0.404833 11.00000 -1.50000 AFIX 0 C15 1 0.232747 0.128921 0.329687 11.00000 0.02819 0.12209 = 0.12991 -0.07306 0.02306 -0.00912 AFIX 13 H15 2 0.210878 0.161337 0.345833 11.00000 -1.20000 AFIX 0 C16 1 0.216882 0.137248 0.247552 11.00000 0.04015 0.09610 = 0.13316 0.00618 -0.02108 -0.00654 AFIX 137 H16A 2 0.227769 0.184451 0.236841 11.00000 -1.50000 H16B 2 0.179610 0.133253 0.223281 11.00000 -1.50000 H16C 2 0.232940 0.099459 0.229069 11.00000 -1.50000 AFIX 0 HKLF 4 REM XRAY5748_0m_a.res in C2/c REM R1 = 0.0364 for 7341 Fo > 4sig(Fo) and 0.0416 for all 8134 data REM 730 parameters refined using 76 restraints END WGHT 0.0495 21.9371 REM Highest difference peak 0.921, deepest hole -0.661, 1-sigma level 0.060 Q1 1 0.4196 0.2421 0.3745 11.00000 0.05 0.92 Q2 1 0.2845 0.2200 0.1595 11.00000 0.05 0.56 Q3 1 0.2055 0.1005 0.3368 11.00000 0.05 0.49 Q4 1 0.2417 0.0882 0.3051 11.00000 0.05 0.47 Q5 1 0.2335 0.3095 0.0452 11.00000 0.05 0.43 Q6 1 0.6500 0.3978 0.4573 11.00000 0.05 0.43 Q7 1 0.7176 0.5045 0.6701 11.00000 0.05 0.42 Q8 1 0.4161 0.2382 0.4278 11.00000 0.05 0.40 Q9 1 0.2431 0.2837 0.1485 11.00000 0.05 0.40 Q10 1 0.7881 0.5591 0.6580 11.00000 0.05 0.39 Q11 1 0.4905 0.2245 0.5225 11.00000 0.05 0.38 Q12 1 0.7518 0.6346 0.6871 11.00000 0.05 0.37 Q13 1 0.3368 0.2392 0.2820 11.00000 0.05 0.36 Q14 1 0.4133 0.1607 0.4950 11.00000 0.05 0.33 Q15 1 0.3975 0.1004 0.3935 11.00000 0.05 0.31 Q16 1 0.2976 0.1257 0.3512 11.00000 0.05 0.31 Q17 1 0.1998 0.1599 0.2839 11.00000 0.05 0.30 Q18 1 0.3857 0.3852 0.3280 11.00000 0.05 0.30 Q19 1 0.4150 0.0746 0.3482 11.00000 0.05 0.30 Q20 1 0.3526 0.2394 0.5035 11.00000 0.05 0.30 ; _shelx_res_checksum 43023 _shelx_hkl_file ; 2 0 0 694.23 15.10 4 0 0 134.39 3.40 -4 0 0 135.39 3.40 -6 0 0 5654.23 121.99 6 0 0 5615.24 123.59 -8 0 0 166.08 4.60 8 0 0 173.08 4.50 10 0 0 2068.59 45.00 10 0 0 2091.59 45.10 -10 0 0 2010.50 45.30 12 0 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17.80 12 6 0 745.13 17.10 -12 6 0 727.23 17.50 12 6 0 760.22 17.40 -12 6 0 713.53 17.20 -12 6 0 722.23 17.30 -14 -6 0 23.50 2.80 -14 -6 0 21.60 2.30 14 6 0 23.10 1.80 -14 6 0 19.80 2.10 14 6 0 21.30 1.90 14 6 0 21.90 2.10 -16 -6 0 320.27 9.10 -16 6 0 319.67 9.20 16 6 0 331.57 8.70 16 6 0 327.07 9.00 -18 -6 0 46.10 3.40 18 6 0 48.80 2.80 -18 6 0 47.30 3.70 18 6 0 47.00 3.00 -20 -6 0 33.90 3.40 20 6 0 27.30 2.50 20 6 0 23.10 2.10 -20 6 0 26.60 3.00 -22 -6 0 467.95 13.20 22 6 0 455.75 11.90 -22 6 0 463.35 12.70 -24 -6 0 32.70 3.70 24 -6 0 26.90 2.30 24 6 0 27.20 2.30 24 6 0 29.40 2.60 -24 6 0 30.30 3.00 24 6 0 24.00 2.40 -24 6 0 29.50 3.20 24 6 0 33.30 2.60 -26 -6 0 9.30 2.70 26 -6 0 5.20 1.50 26 6 0 3.60 1.40 -26 6 0 7.30 2.30 26 6 0 5.50 1.50 26 6 0 3.30 1.50 28 -6 0 140.19 4.60 -28 -6 0 152.68 6.20 -28 6 0 146.29 5.50 28 6 0 143.09 4.70 28 6 0 149.39 4.70 28 6 0 140.19 4.70 -1 -7 0 40.50 1.90 1 -7 0 35.60 1.60 1 7 0 36.20 1.80 1 7 0 37.40 1.60 -1 7 0 38.50 1.60 -3 -7 0 4.50 1.10 3 7 0 4.90 0.90 3 7 0 4.20 1.00 -5 -7 0 632.44 15.00 5 7 0 609.34 14.30 5 7 0 618.64 14.80 -7 -7 0 12.30 1.80 7 7 0 10.60 1.20 7 7 0 8.60 1.30 -9 -7 0 195.08 6.40 -9 7 0 190.78 5.40 -9 7 0 191.78 5.70 -9 7 0 189.08 5.60 9 7 0 197.18 5.50 9 7 0 183.48 5.30 9 7 0 196.28 6.00 -11 -7 0 529.95 14.00 11 7 0 551.14 13.60 -11 7 0 522.35 13.10 -11 7 0 536.85 13.00 11 7 0 532.55 12.80 11 7 0 540.85 13.10 -11 7 0 517.15 13.00 -13 -7 0 21.60 2.10 -13 -7 0 17.70 2.40 13 -7 0 20.70 1.70 13 7 0 17.30 2.00 13 7 0 22.30 2.00 -13 7 0 16.50 1.90 13 7 0 21.60 1.80 -13 7 0 17.70 1.80 -13 7 0 22.20 2.10 -15 -7 0 41.30 3.00 15 7 0 40.80 2.60 15 7 0 40.60 2.40 -15 7 0 37.90 3.00 -17 -7 0 98.69 4.60 17 7 0 108.39 4.10 -17 7 0 108.69 4.90 17 7 0 107.19 4.40 -19 -7 0 64.19 4.30 19 7 0 61.99 3.20 -19 7 0 58.99 3.80 19 7 0 55.49 3.40 -21 -7 0 24.10 3.20 21 7 0 23.60 2.20 21 7 0 19.90 2.10 -21 7 0 23.00 2.80 -23 -7 0 260.97 8.90 23 -7 0 247.08 7.40 23 7 0 253.87 7.70 23 7 0 247.98 7.50 23 7 0 251.27 7.60 -23 7 0 238.48 7.90 23 7 0 257.87 7.60 25 -7 0 50.59 3.00 25 7 0 45.00 3.10 25 7 0 46.20 3.20 25 7 0 47.30 3.10 25 7 0 47.70 3.10 27 -7 0 120.69 4.20 -27 -7 0 120.49 5.70 27 7 0 118.79 4.40 27 7 0 120.29 4.30 27 7 0 121.79 4.40 -29 -7 0 15.00 2.30 29 7 0 15.20 1.50 29 7 0 17.50 1.60 29 7 0 17.80 1.50 0 -8 0 72.39 2.60 0 8 0 66.69 2.30 -2 -8 0 504.45 12.00 2 8 0 490.65 11.60 2 8 0 496.35 11.90 -4 -8 0 217.28 6.20 4 8 0 216.18 5.70 4 8 0 211.38 6.10 -6 -8 0 58.49 3.00 6 8 0 53.99 2.30 6 8 0 49.70 2.60 -6 8 0 54.39 2.50 -6 8 0 52.89 2.50 -6 8 0 53.49 2.50 -8 -8 0 17.50 2.20 -8 8 0 7.50 1.30 -8 8 0 8.30 1.40 -8 8 0 7.80 1.20 8 8 0 7.10 1.10 8 8 0 8.60 1.30 8 8 0 12.50 1.60 -10 -8 0 144.19 5.70 10 8 0 137.99 4.40 -10 8 0 146.09 4.80 -10 8 0 150.98 4.70 10 8 0 146.09 5.10 -10 8 0 146.29 4.70 10 8 0 149.19 4.70 -12 -8 0 277.67 8.80 -12 8 0 276.87 7.70 12 8 0 272.87 7.70 -12 8 0 278.97 7.80 -12 8 0 274.37 7.70 12 8 0 264.37 8.10 12 8 0 269.37 7.40 14 -8 0 47.50 2.50 -14 -8 0 48.90 3.10 -14 8 0 45.40 3.20 14 8 0 47.30 2.70 -14 8 0 42.10 3.00 14 8 0 46.30 2.80 -14 8 0 45.20 3.20 -16 -8 0 19.40 2.50 16 8 0 14.50 1.90 -16 8 0 12.60 2.20 16 8 0 17.10 1.80 -18 -8 0 55.79 3.80 -18 8 0 49.99 3.60 18 8 0 55.59 3.40 18 8 0 53.49 3.00 -20 -8 0 26.20 3.10 20 8 0 19.20 2.30 20 8 0 17.40 2.10 -20 8 0 19.20 2.70 22 -8 0 154.88 5.40 -22 -8 0 179.48 7.10 -22 8 0 165.98 6.30 22 8 0 169.58 5.60 22 8 0 156.28 5.50 22 8 0 163.78 5.80 22 8 0 165.58 5.80 22 8 0 162.38 5.90 -22 8 0 162.98 6.70 24 -8 0 62.39 4.60 24 8 0 62.69 3.50 24 8 0 63.89 3.50 -24 8 0 77.39 6.80 24 8 0 65.39 3.60 -24 8 0 57.19 4.50 24 8 0 54.29 3.40 -26 -8 0 68.99 4.70 26 8 0 59.89 3.30 26 8 0 69.19 3.40 26 8 0 64.09 3.40 26 8 0 67.39 3.40 -28 -8 0 11.40 2.30 28 8 0 10.70 1.50 28 8 0 7.10 1.30 28 8 0 8.70 1.40 28 8 0 11.60 1.40 1 9 0 339.57 8.40 -1 9 0 349.07 8.50 -1 9 0 345.27 8.70 -3 -9 0 41.20 2.30 -3 9 0 34.00 2.20 -3 9 0 37.50 2.10 3 9 0 40.30 2.20 3 9 0 38.50 1.90 -5 -9 0 122.79 4.50 -5 9 0 121.49 3.60 -5 9 0 120.29 4.10 -5 9 0 116.39 4.00 5 9 0 120.39 4.30 5 9 0 120.99 3.80 -7 -9 0 219.78 6.90 -7 9 0 208.28 6.10 7 9 0 218.18 6.00 7 9 0 205.08 6.40 7 9 0 202.18 5.70 -7 9 0 212.68 6.20 -7 9 0 218.28 5.80 -9 -9 0 345.37 10.10 9 9 0 338.47 8.80 9 9 0 356.36 9.10 9 9 0 330.87 9.50 -9 9 0 336.97 9.20 -9 9 0 359.66 9.30 -9 9 0 343.87 8.90 -11 -9 0 208.18 7.40 11 9 0 204.28 6.70 -11 9 0 212.08 6.30 -11 9 0 213.68 6.40 11 9 0 203.68 6.00 -11 9 0 210.58 6.50 11 9 0 215.08 6.30 -13 -9 0 16.00 2.20 13 9 0 19.10 1.80 13 9 0 21.40 2.20 -13 9 0 22.20 2.50 -13 9 0 19.20 2.10 -13 9 0 16.40 2.00 15 -9 0 147.79 4.80 -15 -9 0 148.69 5.70 -15 9 0 143.29 5.30 15 9 0 140.99 5.20 -15 9 0 144.09 5.50 15 9 0 147.19 4.90 -15 9 0 138.89 5.60 -17 -9 0 89.99 4.60 17 9 0 90.39 4.10 -17 9 0 89.59 4.40 17 9 0 88.29 3.80 -19 -9 0 0.50 2.20 19 9 0 -0.80 1.30 -19 9 0 -1.80 1.80 19 9 0 -2.10 1.40 -21 -9 0 115.09 5.90 21 9 0 121.09 4.50 21 9 0 122.39 4.90 21 9 0 119.49 4.90 -21 9 0 123.29 5.30 -21 9 0 126.49 6.00 21 9 0 117.29 4.60 21 9 0 122.79 5.00 -23 -9 0 72.99 5.20 23 -9 0 72.29 3.40 23 9 0 72.69 3.80 23 9 0 76.69 3.80 23 9 0 72.29 3.60 -23 9 0 71.59 4.80 23 9 0 75.99 3.90 -23 9 0 67.09 4.20 25 -9 0 4.40 1.30 -25 9 0 2.70 2.00 25 9 0 0.10 1.40 25 9 0 2.90 1.40 25 9 0 1.60 1.40 25 9 0 -0.20 1.30 -27 -9 0 125.49 5.40 27 9 0 115.89 4.10 27 9 0 115.29 4.10 27 9 0 110.89 4.10 27 9 0 114.69 4.00 0 10 0 1213.68 27.60 0 10 0 1231.28 27.40 -2 10 0 41.70 1.90 2 10 0 43.80 2.00 -2 10 0 38.70 2.20 2 10 0 39.70 2.30 -2 10 0 37.80 2.30 -4 -10 0 9.70 1.60 4 10 0 8.70 1.20 -4 10 0 9.40 1.60 -4 10 0 7.80 1.30 -4 10 0 11.70 1.30 -6 -10 0 14.60 1.90 6 10 0 15.80 1.60 -6 10 0 15.80 1.40 -6 10 0 17.00 1.90 -6 10 0 13.60 1.70 6 10 0 17.90 2.00 -8 -10 0 3.60 1.70 8 10 0 2.90 1.20 8 10 0 3.80 1.20 -8 10 0 4.70 1.20 -8 10 0 3.40 1.40 -8 10 0 1.50 1.40 8 10 0 3.70 1.10 -10 10 0 90.19 3.70 10 10 0 92.29 3.70 -10 10 0 92.59 3.90 10 10 0 89.59 3.40 -10 10 0 86.49 3.90 -12 10 0 6.20 1.60 -12 10 0 6.50 1.80 12 10 0 6.20 1.40 12 10 0 10.80 1.80 -12 10 0 5.90 1.80 14 -10 0 125.09 4.40 -14 -10 0 124.39 5.10 14 10 0 126.89 4.60 -14 10 0 126.99 5.20 14 10 0 126.29 5.00 -14 10 0 131.89 5.40 -14 10 0 134.69 5.10 16 -10 0 145.29 5.10 -16 -10 0 153.98 6.00 -16 10 0 146.89 5.60 16 10 0 150.18 5.10 -16 10 0 153.58 6.00 16 10 0 142.59 5.40 -16 10 0 150.38 5.70 -18 -10 0 3.00 2.00 18 10 0 1.00 1.40 -18 10 0 0.80 2.00 18 10 0 2.50 1.50 -20 -10 0 52.79 4.20 20 10 0 43.10 3.30 20 10 0 48.80 3.10 -20 10 0 49.00 4.30 20 10 0 48.10 3.50 20 10 0 43.90 3.40 -20 10 0 38.90 3.40 -22 -10 0 48.90 4.10 22 -10 0 43.70 2.80 22 10 0 37.10 3.20 22 10 0 40.20 3.20 22 10 0 41.40 3.00 -22 10 0 38.70 3.40 -22 10 0 46.30 3.60 22 10 0 39.80 3.10 24 -10 0 16.60 1.70 24 10 0 13.50 1.80 24 10 0 21.60 2.10 24 10 0 16.20 1.80 24 10 0 20.60 2.10 -24 10 0 19.60 2.70 -26 -10 0 9.90 2.30 26 -10 0 8.00 1.30 26 10 0 7.70 1.40 26 10 0 9.30 1.50 26 10 0 10.40 1.50 -26 10 0 13.40 2.10 26 10 0 7.70 1.50 -1 11 0 820.32 19.40 1 11 0 847.12 19.10 1 11 0 819.32 19.30 -1 11 0 819.32 19.20 -3 11 0 68.59 3.30 -3 11 0 65.99 3.10 3 11 0 66.89 3.00 5 11 0 494.95 12.10 -5 11 0 480.45 12.40 -5 11 0 489.65 12.30 -5 11 0 488.45 11.80 -7 -11 0 106.79 4.70 -7 11 0 118.79 4.50 -7 11 0 112.99 4.50 7 11 0 112.39 4.00 -7 11 0 115.59 3.90 -9 11 0 332.47 8.80 9 11 0 330.77 8.80 9 11 0 335.67 9.00 -9 11 0 332.47 9.30 -9 11 0 324.67 9.30 -11 11 0 475.35 12.60 -11 11 0 483.45 12.50 11 11 0 473.95 12.00 11 11 0 477.65 12.40 -11 11 0 468.85 12.20 -13 -11 0 245.78 7.90 -13 11 0 266.57 7.90 -13 11 0 254.97 8.10 13 11 0 256.87 7.90 13 11 0 258.07 7.50 -13 11 0 264.67 8.10 15 -11 0 143.89 5.00 -15 -11 0 144.09 5.80 -15 11 0 147.89 6.10 -15 11 0 140.39 5.50 15 11 0 142.19 5.50 -15 11 0 143.59 5.70 15 11 0 140.79 5.00 -17 -11 0 89.89 4.90 17 11 0 79.39 4.10 -17 11 0 92.19 4.40 17 11 0 89.19 4.00 19 11 0 113.49 4.90 -19 11 0 111.79 6.00 19 11 0 116.89 4.90 -19 11 0 105.29 4.90 19 11 0 105.59 4.90 -21 -11 0 120.09 5.80 21 11 0 115.99 4.90 21 11 0 121.69 4.90 21 11 0 123.09 4.80 -21 11 0 116.59 5.80 21 11 0 118.29 4.50 -21 11 0 116.39 5.10 23 -11 0 174.48 5.40 -23 11 0 165.58 6.60 23 11 0 171.08 5.70 23 11 0 163.58 5.70 23 11 0 171.18 5.80 25 -11 0 1.20 1.10 -25 -11 0 5.40 2.10 25 11 0 -1.10 1.20 -25 11 0 3.80 1.90 25 11 0 0.80 1.20 25 11 0 -0.40 1.20 0 12 0 96.69 4.00 0 12 0 108.79 3.80 -2 12 0 179.88 5.90 -2 12 0 184.88 5.70 2 12 0 183.48 5.80 -4 12 0 23.30 2.30 -4 12 0 26.30 2.30 -6 12 0 19.80 1.80 6 12 0 16.80 1.90 -6 12 0 19.40 2.50 -6 12 0 23.00 2.40 -8 12 0 60.79 3.90 8 12 0 55.19 3.20 -8 12 0 60.99 3.10 -8 12 0 61.59 3.70 -10 12 0 3.60 1.80 -10 12 0 3.10 2.00 -10 12 0 5.50 1.60 10 12 0 2.10 1.50 -12 -12 0 51.99 3.80 12 12 0 42.50 2.90 -12 12 0 51.69 3.40 -12 12 0 45.70 3.70 12 12 0 48.20 3.40 -12 12 0 51.39 3.90 14 -12 0 16.50 2.10 -14 -12 0 17.80 2.60 -14 12 0 19.20 2.90 -14 12 0 15.80 2.30 14 12 0 19.00 2.10 14 12 0 14.80 2.10 -14 12 0 11.90 2.50 16 -12 0 18.10 2.20 -16 -12 0 20.20 2.80 -16 12 0 16.60 2.50 16 12 0 12.60 2.10 -16 12 0 16.20 2.70 -16 12 0 22.70 2.60 16 12 0 24.20 2.30 18 12 0 15.80 2.20 -18 12 0 19.10 2.60 18 12 0 22.00 2.60 18 12 0 15.70 2.10 -18 12 0 17.60 3.30 18 12 0 14.10 1.80 -20 -12 0 0.90 2.30 20 12 0 4.40 1.80 -20 12 0 3.80 1.90 20 12 0 2.40 1.50 20 12 0 1.50 1.60 -20 12 0 1.90 2.40 20 12 0 1.60 1.40 22 -12 0 59.59 3.00 22 12 0 54.59 3.40 22 12 0 53.59 3.40 22 12 0 52.79 3.30 -22 12 0 50.49 4.40 24 -12 0 16.70 1.60 24 12 0 15.20 1.70 -24 12 0 14.40 2.30 24 12 0 16.10 1.80 24 12 0 18.40 1.90 -1 13 0 665.13 16.10 -1 13 0 678.93 16.50 1 13 0 673.83 16.00 1 13 0 652.43 16.30 -3 13 0 0.10 1.40 -3 13 0 1.80 1.60 -5 13 0 72.99 3.90 -5 13 0 70.79 3.60 -7 13 0 5.10 1.90 -7 13 0 6.10 2.50 -7 13 0 6.70 1.90 -9 13 0 144.99 5.70 -9 13 0 141.89 5.60 -9 13 0 138.39 4.90 9 13 0 133.89 5.10 11 13 0 833.72 20.40 -11 13 0 836.62 20.10 13 -13 0 37.80 3.10 -13 13 0 34.00 3.30 -13 13 0 41.10 3.10 -13 13 0 38.20 3.50 13 13 0 37.20 3.20 15 -13 0 5.10 1.70 -15 -13 0 3.20 2.10 -15 13 0 3.20 2.10 -15 13 0 1.60 2.30 15 13 0 1.70 1.50 -15 13 0 1.30 1.80 17 -13 0 224.68 6.90 -17 -13 0 219.08 7.50 17 13 0 213.58 6.60 17 13 0 208.28 7.00 -17 13 0 212.48 8.10 -17 13 0 214.88 7.50 17 13 0 211.98 7.20 -17 13 0 216.88 7.20 -17 13 0 212.98 7.20 -17 13 0 215.18 8.30 19 13 0 26.90 2.50 19 13 0 24.10 2.50 -19 13 0 15.10 3.20 -19 13 0 25.80 3.90 -19 13 0 19.50 3.00 19 13 0 28.10 2.60 21 13 0 56.29 3.50 21 13 0 52.59 3.40 21 13 0 58.29 3.50 -21 13 0 54.99 4.50 23 -13 0 83.99 3.40 -23 13 0 91.39 4.70 23 13 0 81.49 3.60 23 13 0 86.69 3.80 23 13 0 87.89 3.80 0 14 0 3.80 1.40 0 14 0 3.20 1.80 -2 14 0 17.30 2.20 -2 14 0 19.20 2.50 2 14 0 17.90 2.30 -4 14 0 3.50 1.80 -4 14 0 2.10 1.70 -6 14 0 164.68 6.00 -6 14 0 155.58 6.30 -8 14 0 9.70 2.20 -8 14 0 9.90 2.30 -10 14 0 10.00 2.50 -10 14 0 3.70 1.90 -10 14 0 6.80 2.30 12 -14 0 61.89 3.60 -12 14 0 63.19 4.20 -12 14 0 61.59 4.30 12 14 0 50.89 3.60 -12 14 0 57.99 3.60 14 -14 0 19.60 2.20 -14 14 0 23.90 3.30 14 14 0 23.40 2.50 -14 14 0 26.40 3.10 -14 14 0 27.00 3.30 -14 14 0 18.40 3.20 -14 14 0 19.40 3.00 -14 14 0 19.30 2.40 14 14 0 20.30 2.50 -14 14 0 21.80 3.10 16 -14 0 25.50 2.50 -16 14 0 20.00 2.60 16 14 0 20.40 2.40 -16 14 0 26.50 2.80 -16 14 0 20.60 2.90 -16 14 0 24.80 3.60 -16 14 0 26.20 3.50 -16 14 0 26.10 3.40 16 14 0 26.60 2.60 -16 14 0 24.30 3.20 -18 14 0 3.20 2.50 18 14 0 3.60 1.60 18 14 0 5.00 1.70 -18 14 0 4.30 2.70 -20 14 0 7.50 2.40 20 14 0 4.10 1.60 -20 14 0 4.00 3.10 20 14 0 3.60 1.50 20 14 0 6.10 1.80 22 -14 0 19.40 1.70 -22 14 0 21.50 2.70 22 14 0 20.60 2.00 22 14 0 21.90 2.00 22 14 0 21.70 2.00 -1 15 0 299.77 8.50 -1 15 0 304.97 9.20 1 15 0 297.57 9.00 -3 15 0 -2.30 1.60 -3 15 0 0.00 1.90 -5 15 0 154.88 6.40 -5 15 0 154.88 5.70 -7 15 0 2.00 2.20 -7 15 0 1.70 2.00 -9 15 0 88.69 4.80 -9 15 0 86.19 5.00 11 -15 0 362.16 10.00 -11 15 0 361.16 10.50 -11 15 0 353.26 10.70 13 -15 0 141.69 5.30 -13 15 0 134.99 6.10 -13 15 0 142.79 6.10 -13 15 0 146.49 6.80 -13 15 0 134.99 6.20 13 15 0 134.69 5.50 -13 15 0 131.99 6.20 -13 15 0 144.09 6.00 15 -15 0 12.80 2.00 -15 15 0 17.50 2.80 -15 15 0 13.40 2.90 -15 15 0 17.20 2.90 -15 15 0 8.40 3.00 15 15 0 12.40 2.00 -15 15 0 16.60 2.80 15 15 0 12.40 2.10 -15 15 0 14.50 2.80 -15 15 0 17.50 2.80 -17 15 0 58.09 4.90 17 15 0 59.09 3.80 -17 15 0 68.79 5.00 -17 15 0 56.59 4.70 17 15 0 60.09 3.80 -17 15 0 62.89 4.50 19 15 0 25.20 2.20 19 15 0 25.80 2.40 -19 15 0 27.00 3.20 -19 15 0 21.60 2.90 -21 15 0 125.49 5.30 21 15 0 126.29 4.70 21 15 0 123.39 4.50 0 16 0 32.00 3.20 -2 16 0 3.10 1.60 -2 16 0 3.90 2.10 -4 16 0 2.20 1.70 -4 16 0 1.00 2.00 -6 16 0 13.60 2.70 -6 16 0 16.40 2.60 -8 16 0 25.80 3.00 -8 16 0 32.20 5.40 -8 16 0 25.70 2.90 -8 16 0 35.00 5.20 -8 16 0 37.70 3.80 -8 16 0 24.90 4.10 10 -16 0 0.90 1.70 -10 16 0 3.90 2.90 -10 16 0 5.30 2.60 -10 16 0 3.60 2.40 -10 16 0 6.70 2.60 -10 16 0 2.90 2.20 -10 16 0 6.90 2.50 12 -16 0 4.60 1.70 -12 16 0 3.60 2.80 -12 16 0 2.80 2.40 -12 16 0 2.90 2.40 -12 16 0 4.50 2.40 -12 16 0 4.30 2.60 -12 16 0 1.70 2.10 -14 16 0 14.20 2.80 -14 16 0 17.90 2.90 14 16 0 11.90 2.10 -14 16 0 18.70 3.40 -14 16 0 18.40 2.90 -16 16 0 5.30 2.40 16 16 0 6.00 1.70 -16 16 0 8.20 2.70 -16 16 0 9.10 2.90 16 16 0 5.20 1.80 -16 16 0 4.30 2.40 -18 16 0 1.10 2.20 18 16 0 1.20 1.50 -18 16 0 0.50 2.30 18 16 0 -0.90 1.30 -18 16 0 -0.70 2.00 20 16 0 1.60 1.20 -20 16 0 -1.60 1.80 20 16 0 1.30 1.40 -20 16 0 0.60 2.00 -1 17 0 33.70 4.90 -1 17 0 37.60 5.30 -1 17 0 44.50 3.70 -3 17 0 -2.50 2.10 -3 17 0 -1.70 2.00 -3 17 0 -0.10 1.60 -3 17 0 -1.70 2.00 -3 17 0 0.10 2.50 -3 17 0 1.90 2.80 -5 17 0 4.60 2.60 -5 17 0 2.70 2.40 -5 17 0 3.70 2.00 -5 17 0 2.80 2.30 -5 17 0 -0.30 2.20 -5 17 0 5.20 2.50 -7 17 0 50.89 4.20 -7 17 0 49.30 4.50 -7 17 0 53.39 4.20 -7 17 0 63.89 4.80 -7 17 0 49.10 3.90 -7 17 0 43.70 3.80 9 -17 0 78.89 4.00 -9 17 0 69.39 4.90 -9 17 0 75.99 5.10 -9 17 0 72.59 4.70 -9 17 0 75.39 4.50 -9 17 0 82.79 5.50 -9 17 0 72.79 4.90 11 -17 0 35.10 2.90 -11 17 0 27.00 3.30 -11 17 0 32.30 3.80 -11 17 0 32.40 3.60 -11 17 0 38.90 3.60 -11 17 0 34.00 3.20 -11 17 0 29.40 3.30 -13 17 0 48.60 4.30 -13 17 0 43.40 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2.40 21 15 -3 0.80 1.40 -21 15 3 -1.10 2.00 21 15 -3 2.10 1.40 19 15 -3 3.60 1.70 -19 15 3 0.60 2.60 -19 15 3 1.60 2.10 -19 15 3 0.90 2.30 -17 15 3 2.60 2.70 -17 15 3 0.90 2.40 -17 15 3 3.70 2.20 -17 15 3 5.20 2.40 -17 15 3 4.40 2.70 17 15 -3 4.10 1.80 -15 15 3 1.10 2.00 -15 15 3 4.10 2.50 -15 15 3 2.20 2.70 -15 15 3 4.90 2.30 -15 15 3 0.40 1.90 -15 15 3 0.10 2.40 -13 15 3 102.19 6.00 -13 15 3 105.99 5.60 -13 15 3 117.19 5.50 -13 15 3 113.59 5.80 -13 15 3 111.49 6.00 -13 15 3 114.29 5.50 -11 15 3 15.60 2.80 -11 15 3 7.80 2.50 -9 15 3 2.80 2.20 -9 15 3 2.30 2.10 -7 15 3 25.70 2.90 -7 15 3 25.60 2.90 -5 15 3 97.69 4.70 -5 15 3 94.89 4.40 -3 15 3 7.10 1.90 -3 15 3 6.00 2.10 3 15 -3 5.60 2.50 1 15 -3 3.60 2.60 1 15 -3 -1.10 1.30 -1 15 3 4.00 1.90 1 15 3 58.79 3.80 -1 15 -3 68.89 4.30 -1 15 -3 63.19 3.70 -3 15 -3 13.00 2.50 -3 15 -3 13.20 1.80 -3 15 -3 15.80 2.40 5 -15 3 58.79 3.60 -5 15 -3 66.09 4.10 -5 15 -3 61.59 4.50 -5 15 -3 57.09 3.40 -7 -15 -3 5.00 2.20 7 -15 3 5.60 1.90 -7 15 -3 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29.60 2.50 -24 8 4 29.00 3.40 24 8 -4 25.80 2.50 24 8 -4 31.10 2.60 -24 8 4 32.30 3.10 24 8 -4 31.20 2.70 -22 -8 4 111.99 5.40 22 8 -4 110.29 4.50 22 8 -4 102.49 4.70 -22 8 4 113.39 5.20 -20 -8 4 8.70 2.30 -20 -8 4 7.60 2.10 20 8 -4 10.40 1.90 20 8 -4 12.50 2.10 -20 8 4 6.80 2.20 -18 -8 4 136.39 5.20 -18 8 4 132.89 5.10 -18 8 4 129.69 5.30 18 8 -4 133.69 4.90 18 8 -4 131.89 5.10 -16 -8 4 201.58 6.30 16 8 -4 212.48 6.40 -16 8 4 206.08 6.60 16 8 -4 200.08 6.00 -16 8 4 211.08 6.50 16 8 -4 202.58 6.50 -14 -8 4 135.09 4.50 -14 8 4 129.79 4.60 -14 8 4 134.79 4.80 14 8 -4 141.49 4.40 14 8 -4 131.49 4.70 -14 8 4 130.99 4.70 14 8 -4 140.89 4.70 12 -8 -4 1.20 1.20 12 8 -4 2.10 1.10 -12 8 4 2.60 1.30 -12 8 4 3.00 1.30 12 8 -4 3.20 1.00 12 8 -4 5.60 1.20 -12 8 4 2.00 1.20 12 8 -4 2.10 1.20 10 -8 -4 133.09 4.50 10 8 -4 131.39 4.00 10 8 -4 132.49 5.00 -10 8 4 133.09 4.30 -10 8 4 126.79 4.40 10 8 -4 134.89 4.30 10 8 -4 139.29 4.20 8 -8 -4 224.48 6.20 8 8 -4 225.18 6.00 -8 8 4 211.28 6.00 8 8 -4 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20 10 4 15.70 2.00 -20 10 -4 15.40 2.60 22 -10 4 33.20 2.50 -22 10 -4 31.60 2.90 22 10 4 32.30 2.50 -22 10 -4 38.30 3.30 22 10 4 29.10 2.80 22 10 4 31.70 2.80 24 -10 4 32.10 2.30 24 10 4 34.00 2.30 -24 10 -4 36.20 2.80 24 10 4 33.80 2.50 -24 10 -4 26.80 2.30 24 10 4 32.60 2.40 27 -11 -4 133.59 4.50 27 11 -4 148.69 4.90 27 11 -4 138.69 4.60 27 11 -4 139.59 4.70 25 -11 -4 17.80 2.00 25 11 -4 18.70 2.10 25 11 -4 19.20 2.00 25 11 -4 21.30 2.10 -23 -11 4 1.00 3.10 23 -11 -4 4.10 1.60 23 11 -4 2.40 2.10 -23 11 4 1.50 2.30 23 11 -4 4.90 1.80 23 11 -4 6.80 1.70 23 11 -4 1.30 1.50 21 -11 -4 194.08 6.40 -21 -11 4 196.68 7.20 -21 11 4 182.68 6.60 21 11 -4 184.48 6.60 21 11 -4 188.58 6.30 -21 11 4 185.48 7.40 21 11 -4 196.68 6.50 -21 11 4 172.68 7.40 21 11 -4 193.58 6.50 -19 -11 4 1.90 2.30 -19 11 4 2.70 2.00 -19 11 4 3.80 2.00 19 11 -4 1.70 1.50 19 11 -4 3.20 1.80 -17 11 4 49.30 3.80 -17 11 4 51.69 3.40 17 11 -4 45.30 3.40 17 11 -4 51.69 3.20 15 11 -4 274.07 8.40 -15 11 4 287.77 8.60 -15 11 4 289.37 8.70 15 11 -4 292.77 8.30 -13 -11 4 79.09 3.60 -13 11 4 84.79 4.20 13 11 -4 94.19 4.00 -13 11 4 86.29 4.10 -11 11 4 91.29 4.00 11 11 -4 94.49 3.50 11 11 -4 89.49 3.70 -11 11 4 94.59 4.30 9 11 -4 32.40 2.20 -9 11 4 25.20 2.30 -9 11 4 33.30 2.70 9 11 -4 30.20 2.10 7 11 -4 8.70 1.40 -7 11 4 7.00 1.60 7 11 -4 6.30 1.30 -7 11 4 5.90 1.50 5 -11 -4 837.02 19.00 5 11 -4 799.52 18.50 5 11 -4 771.72 18.50 5 11 -4 781.22 18.40 -5 11 4 803.02 18.90 -5 11 4 790.82 18.80 3 -11 -4 25.70 2.20 3 11 -4 23.90 1.80 -3 11 4 22.80 2.00 -3 11 4 21.50 2.00 3 11 -4 25.60 2.00 -3 11 4 26.40 1.90 1 -11 -4 0.30 1.20 1 11 -4 -0.30 1.10 -1 11 4 1.00 1.20 -1 11 4 0.80 1.10 1 11 -4 1.10 0.90 1 11 -4 2.00 1.30 -1 -11 -4 276.57 7.80 -1 11 -4 270.57 7.60 1 11 4 291.47 7.70 1 11 4 273.67 7.60 -1 11 -4 255.37 7.80 -1 11 -4 270.47 7.20 -3 -11 -4 114.79 4.50 3 11 4 113.29 4.30 -3 11 -4 114.29 4.30 3 11 4 109.09 4.00 -3 11 -4 118.69 3.90 -3 11 -4 112.19 4.70 5 -11 4 3.80 1.40 -5 11 -4 1.80 1.20 5 11 4 4.50 1.40 -5 11 -4 5.80 1.60 -5 11 -4 1.00 1.60 7 -11 4 520.55 12.80 -7 11 -4 508.75 13.40 -7 11 -4 510.25 13.20 -7 11 -4 495.25 12.70 7 11 4 502.35 13.00 9 -11 4 110.39 4.30 -9 11 -4 113.49 4.60 9 11 4 112.19 4.70 -9 11 -4 113.69 4.80 -9 11 -4 119.79 5.30 11 -11 4 89.39 3.80 -11 11 -4 89.89 4.90 11 11 4 85.39 4.30 -11 11 -4 87.59 4.50 -11 11 -4 79.79 4.00 13 -11 4 150.58 5.30 -13 11 -4 147.79 5.70 13 11 4 139.39 5.50 -13 11 -4 146.49 6.20 -13 11 -4 161.28 6.30 15 -11 4 8.80 1.70 -15 -11 -4 9.30 2.80 -15 11 -4 9.80 2.30 -17 -11 -4 157.68 6.80 -17 11 -4 154.58 7.10 17 11 4 162.38 5.90 17 11 4 156.08 5.70 17 11 4 147.49 5.70 -17 11 -4 156.28 6.00 -17 11 -4 166.08 6.80 19 -11 4 108.49 4.30 19 11 4 113.29 4.80 19 11 4 114.39 4.80 -19 11 -4 115.79 5.90 -19 11 -4 121.09 5.90 19 11 4 121.79 4.70 21 -11 4 0.70 1.20 -21 11 -4 2.70 2.20 21 11 4 0.20 1.40 21 11 4 0.30 1.40 21 11 4 -0.70 1.30 23 -11 4 152.98 4.60 -23 11 -4 152.18 5.60 23 11 4 146.29 4.80 23 11 4 143.59 4.80 26 -12 -4 4.00 1.30 26 12 -4 4.00 1.40 26 12 -4 4.30 1.50 26 12 -4 5.10 1.30 24 -12 -4 2.10 1.50 24 12 -4 0.00 1.50 24 12 -4 0.40 1.30 24 12 -4 -0.20 1.30 22 -12 -4 3.60 1.70 22 12 -4 3.40 1.50 -22 12 4 5.50 2.50 -22 12 4 6.90 2.60 22 12 -4 3.30 1.50 22 12 -4 3.10 1.70 20 -12 -4 3.30 1.70 -20 -12 4 6.10 2.40 20 12 -4 4.30 1.70 20 12 -4 2.40 1.70 -20 12 4 4.70 2.60 20 12 -4 2.90 1.60 20 12 -4 5.80 1.90 -20 12 4 0.10 2.50 -20 12 4 0.30 1.90 18 12 -4 147.39 5.40 -18 12 4 154.18 6.00 -16 12 4 21.30 2.70 -16 12 4 16.70 2.70 16 12 -4 20.50 2.30 -14 12 4 292.27 8.80 14 12 -4 274.87 8.10 -14 12 4 275.47 8.60 -12 12 4 10.00 2.20 -12 12 4 11.50 2.20 12 12 -4 12.40 1.80 10 12 -4 31.30 2.40 -10 12 4 32.20 2.80 -10 12 4 30.00 2.70 8 12 -4 2.60 1.20 -8 12 4 1.20 1.60 8 12 -4 2.00 1.20 -8 12 4 1.10 1.50 -6 12 4 175.68 5.70 6 12 -4 151.48 5.50 -6 12 4 178.18 5.80 6 12 -4 173.28 5.10 4 -12 -4 30.30 2.60 -4 12 4 33.40 2.30 4 12 -4 32.50 2.00 -4 12 4 30.00 2.50 4 12 -4 29.60 2.30 2 -12 -4 7.60 1.80 2 12 -4 9.30 1.90 2 12 -4 7.20 1.50 -2 12 4 7.10 1.60 -2 12 4 5.60 1.50 2 12 -4 6.90 1.30 0 -12 -4 40.50 3.00 0 12 4 41.30 2.60 0 12 -4 40.80 2.70 0 12 -4 44.80 3.20 0 12 4 43.80 2.90 0 12 -4 43.20 2.50 -2 -12 -4 10.30 2.10 -2 12 -4 10.10 1.80 2 12 4 11.30 1.70 -2 12 -4 9.70 1.90 2 12 4 13.60 1.80 -2 12 -4 12.90 1.70 -4 -12 -4 18.90 2.30 4 -12 4 13.80 1.80 -4 12 -4 15.90 2.10 4 12 4 18.20 2.10 -4 12 -4 18.70 2.50 4 12 4 16.70 2.30 -4 12 -4 15.50 1.80 6 -12 4 3.60 1.60 -6 12 -4 4.80 1.80 -6 12 -4 5.20 2.10 -6 12 -4 6.30 1.60 6 12 4 5.60 1.70 8 -12 4 33.70 2.60 -8 12 -4 32.40 2.90 -8 12 -4 28.40 2.50 8 12 4 28.20 2.70 -8 12 -4 26.50 3.10 10 -12 4 54.09 3.30 10 12 4 53.39 3.60 -10 12 -4 49.30 3.90 -10 12 -4 58.59 4.00 -10 12 -4 52.99 3.30 12 -12 4 3.60 1.70 -12 12 -4 1.20 2.10 -12 12 -4 -0.40 1.70 -12 12 -4 2.00 2.00 12 12 4 1.60 1.50 14 -12 4 6.50 1.60 14 12 4 10.10 2.10 -14 12 -4 9.70 3.00 14 12 4 4.20 1.70 -14 12 -4 10.50 2.70 -14 12 -4 7.50 2.10 14 12 4 7.20 1.80 -14 12 -4 9.30 3.40 16 -12 4 148.39 5.00 16 12 4 144.59 5.50 -16 12 -4 146.59 6.80 -16 12 -4 141.49 5.80 -16 12 -4 144.99 6.50 18 -12 4 17.90 1.90 -18 12 -4 18.90 3.30 18 12 4 13.00 2.00 18 12 4 14.00 2.00 -18 12 -4 22.30 3.10 18 12 4 17.40 2.10 20 -12 4 1.40 1.30 -20 12 -4 1.80 2.20 20 12 4 1.60 1.50 20 12 4 1.00 1.40 20 12 4 1.10 1.40 -20 12 -4 3.00 2.10 22 -12 4 47.50 2.50 22 12 4 51.59 2.90 22 12 4 45.90 3.00 -22 12 -4 33.40 2.80 22 12 4 45.90 2.80 25 -13 -4 76.89 3.20 25 13 -4 75.19 3.70 25 13 -4 72.49 3.30 25 13 -4 72.89 3.10 23 -13 -4 44.10 2.80 23 13 -4 44.40 3.10 -23 13 4 35.00 3.10 23 13 -4 42.20 3.20 -23 13 4 40.40 3.30 23 13 -4 44.50 2.90 21 -13 -4 9.10 2.00 21 13 -4 5.90 2.00 -21 13 4 8.00 2.50 -21 13 4 5.50 2.50 21 13 -4 3.70 1.70 21 13 -4 8.40 1.80 19 -13 -4 42.20 3.70 -19 -13 4 54.69 4.20 -19 13 4 55.79 4.90 19 13 -4 48.90 3.40 -19 13 4 51.09 4.60 19 13 -4 53.59 3.80 -19 13 4 62.19 4.60 19 13 -4 54.19 3.40 17 -13 -4 63.39 3.90 -17 13 4 60.59 4.80 -17 13 4 58.19 4.80 -17 13 4 55.29 4.60 17 13 -4 60.19 3.60 17 13 -4 64.89 4.10 17 13 -4 60.29 4.20 -17 13 4 62.59 4.60 -17 13 4 66.69 4.30 -15 13 4 92.39 4.80 -15 13 4 91.19 4.90 15 13 -4 87.89 4.20 13 13 -4 13.30 2.10 -13 13 4 6.90 2.30 -13 13 4 6.70 2.10 -11 13 4 38.20 3.30 11 13 -4 40.10 2.80 -11 13 4 41.80 3.40 -9 13 4 80.19 4.10 -9 13 4 76.29 4.20 9 13 -4 84.29 3.70 -7 13 4 257.07 7.80 -7 13 4 277.37 8.00 7 13 -4 249.58 7.30 5 13 -4 152.28 5.00 -5 13 4 155.48 5.60 -5 13 4 149.99 5.30 5 13 -4 153.78 4.80 -3 13 4 310.57 8.60 3 13 -4 312.97 8.30 3 13 -4 303.37 8.40 -3 13 4 316.67 9.00 1 -13 -4 120.29 4.90 1 13 -4 113.69 4.10 1 13 -4 120.79 5.00 -1 13 4 119.29 4.60 -1 13 4 120.89 4.80 1 13 -4 122.79 4.60 -1 -13 -4 54.99 3.60 1 13 4 56.69 3.40 1 13 4 55.09 3.30 -1 13 -4 55.39 3.80 -1 13 -4 53.99 3.20 -1 13 -4 55.69 2.80 -3 -13 -4 26.20 2.70 3 -13 4 28.80 2.50 -3 13 -4 26.70 2.30 3 13 4 26.80 2.50 -3 13 -4 29.00 2.80 -3 13 -4 25.10 2.90 3 13 4 26.00 2.40 5 -13 4 268.87 7.90 -5 -13 -4 276.37 8.50 -5 13 -4 286.37 8.40 -5 13 -4 255.87 7.70 5 13 4 263.27 8.10 -5 13 -4 272.47 8.70 7 -13 4 186.58 6.00 -7 -13 -4 178.78 6.70 -7 13 -4 178.28 7.00 7 13 4 187.68 6.40 -7 13 -4 179.28 6.00 -7 13 -4 176.58 6.60 9 -13 4 61.49 3.50 -9 13 -4 58.69 4.20 -9 13 -4 60.49 4.20 -9 13 -4 51.89 3.60 9 13 4 58.09 3.70 11 -13 4 77.19 3.70 -11 13 -4 83.69 4.90 -11 13 -4 74.19 4.20 -11 13 -4 76.49 4.00 11 13 4 75.19 4.20 13 -13 4 11.60 2.00 13 13 4 12.30 2.20 13 13 4 8.00 1.90 -13 13 -4 14.80 2.50 -13 13 -4 12.60 2.80 -13 13 -4 13.60 3.10 -13 13 -4 7.40 2.90 13 13 4 7.70 1.90 -13 13 -4 11.70 2.30 -13 13 -4 4.90 2.50 -13 13 -4 6.20 3.10 15 -13 4 18.50 2.00 15 13 4 15.90 2.20 15 13 4 19.50 2.30 -15 13 -4 20.80 3.50 -15 13 -4 16.10 3.00 -15 13 -4 20.60 4.60 -15 13 -4 21.30 2.70 15 13 4 18.70 2.30 -17 13 -4 110.39 6.00 17 13 4 123.59 5.00 17 13 4 113.99 4.80 17 13 4 124.29 4.90 -17 13 -4 109.59 5.70 19 -13 4 109.69 4.20 19 13 4 115.19 4.60 19 13 4 112.39 4.60 -19 13 -4 105.89 5.30 -19 13 -4 117.69 5.40 19 13 4 109.09 4.60 21 -13 4 36.40 2.40 -21 13 -4 28.70 2.60 21 13 4 34.90 2.70 21 13 4 38.60 2.60 21 13 4 34.80 2.60 24 14 -4 15.20 1.60 24 14 -4 16.40 1.80 -24 14 4 14.70 2.20 24 14 -4 16.90 1.60 22 -14 -4 1.20 1.40 22 14 -4 -2.60 1.30 -22 14 4 1.80 2.20 22 14 -4 0.70 1.40 22 14 -4 3.20 1.40 20 -14 -4 4.00 1.80 20 14 -4 -1.10 1.80 20 14 -4 3.00 1.70 -20 14 4 7.40 3.40 -20 14 4 0.00 2.40 -20 14 4 0.80 2.30 18 -14 -4 20.00 2.30 -18 -14 4 13.20 2.50 -18 14 4 17.60 2.70 18 14 -4 12.90 2.00 -18 14 4 20.50 4.00 -18 14 4 21.00 3.50 -18 14 4 15.90 2.80 -18 14 4 15.30 3.00 18 14 -4 13.60 2.20 -16 14 4 14.50 2.60 -16 14 4 7.90 2.50 -16 14 4 10.70 2.60 16 14 -4 10.10 1.90 -16 14 4 9.40 2.50 -16 14 4 7.40 2.90 -16 14 4 9.60 2.30 -14 14 4 9.60 2.40 14 14 -4 11.10 2.00 -14 14 4 10.20 2.40 12 14 -4 52.79 3.30 -12 14 4 53.89 3.80 -12 14 4 53.29 3.80 -10 14 4 1.40 2.10 -10 14 4 1.80 2.00 -8 14 4 13.70 2.30 -8 14 4 14.40 2.50 -6 14 4 13.80 2.40 -6 14 4 15.10 2.30 -4 14 4 -0.20 1.40 4 14 -4 -0.70 1.30 -4 14 4 3.00 1.90 4 14 -4 1.40 1.10 2 14 -4 13.70 1.80 2 14 -4 11.90 1.60 -2 14 4 10.90 2.00 0 -14 4 0.90 1.50 0 14 -4 1.70 1.50 0 14 -4 -0.50 1.30 0 14 -4 -0.70 1.90 0 14 4 -0.60 1.60 2 -14 4 33.00 2.70 -2 -14 -4 33.90 3.10 2 14 4 27.80 2.60 2 14 4 30.30 2.70 -2 14 -4 26.80 2.20 -2 14 -4 30.50 2.70 -2 14 -4 34.30 3.20 4 -14 4 0.90 1.60 -4 -14 -4 2.40 2.00 -4 14 -4 6.10 2.30 4 14 4 2.70 1.70 -4 14 -4 -2.00 1.60 -4 14 -4 1.00 1.30 -6 -14 -4 3.50 2.10 6 -14 4 0.40 1.60 -6 14 -4 0.30 2.20 6 14 4 1.30 1.60 -6 14 -4 0.60 2.00 -6 14 -4 1.30 1.60 8 -14 4 2.40 1.70 -8 -14 -4 2.30 2.10 8 14 4 -1.00 1.40 -8 14 -4 1.70 1.60 -8 14 -4 0.80 1.90 -8 14 -4 -0.20 2.10 10 -14 4 25.00 2.40 -10 14 -4 26.90 3.00 -10 14 -4 31.00 3.40 -10 14 -4 30.60 2.90 12 -14 4 2.20 1.50 -12 14 -4 1.10 2.30 -12 14 -4 -4.50 2.70 12 14 4 -0.10 1.60 -12 14 -4 1.40 2.40 -12 14 -4 -0.70 2.50 12 14 4 0.30 1.80 -12 14 -4 2.40 1.90 -12 14 -4 -1.50 1.90 12 14 4 2.60 1.70 -12 14 -4 -1.20 2.40 14 -14 4 35.90 2.80 -14 14 -4 35.50 3.00 -14 14 -4 26.20 3.10 -14 14 -4 39.40 3.80 -14 14 -4 27.70 3.20 -14 14 -4 32.60 3.40 -14 14 -4 30.10 3.00 14 14 4 38.60 3.50 14 14 4 37.80 3.30 14 14 4 39.30 3.40 -14 14 -4 31.90 3.70 16 14 4 5.20 1.80 -16 14 -4 3.60 2.50 -16 14 -4 4.40 2.50 16 14 4 4.30 1.80 16 14 4 3.10 1.60 18 -14 4 2.10 1.30 -18 14 -4 1.20 2.30 -18 14 -4 2.40 2.20 18 14 4 1.60 1.50 18 14 4 1.20 1.50 18 14 4 2.90 1.50 20 -14 4 38.70 2.40 20 14 4 36.00 2.70 20 14 4 37.50 2.60 20 14 4 34.10 2.70 -20 14 -4 23.00 2.50 -20 14 -4 29.40 2.70 23 15 -4 20.00 1.90 -23 15 4 20.20 2.40 21 15 -4 95.69 4.30 -21 15 4 88.29 5.00 -19 15 4 3.20 2.20 -19 15 4 3.40 2.50 -19 15 4 4.60 2.80 19 15 -4 3.40 1.80 17 -15 -4 76.19 5.50 -17 15 4 53.19 4.20 -17 15 4 59.59 5.10 -17 15 4 62.49 4.40 -17 15 4 63.99 4.90 -17 15 4 60.89 4.80 -15 15 4 158.58 7.20 -15 15 4 165.58 6.90 -15 15 4 161.78 6.50 -15 15 4 166.18 6.60 -15 15 4 177.58 6.60 -15 15 4 169.48 7.10 -13 15 4 5.60 2.70 -13 15 4 6.20 2.60 -13 15 4 9.50 2.70 -13 15 4 7.10 2.30 -13 15 4 9.70 2.60 -13 15 4 10.50 2.70 -11 15 4 165.58 6.50 -11 15 4 171.88 6.60 -9 15 4 90.39 4.60 -9 15 4 91.29 4.90 -7 15 4 79.29 4.30 -7 15 4 71.69 4.30 -5 15 4 558.34 14.80 -5 15 4 574.94 14.60 -3 15 4 109.69 5.00 3 15 -4 103.79 4.40 -1 -15 4 1.00 1.70 1 15 -4 0.40 1.40 1 15 -4 1.60 1.70 -1 15 4 5.30 2.00 1 -15 4 118.19 4.80 -1 15 -4 110.19 4.80 1 15 4 116.09 5.00 -1 15 -4 112.39 4.40 -1 15 -4 114.59 5.20 3 -15 4 24.90 2.40 -3 15 -4 27.00 2.40 -3 15 -4 29.50 2.90 -3 15 -4 30.20 3.40 -5 -15 -4 195.78 7.00 5 -15 4 197.08 6.40 -5 15 -4 203.28 6.90 -5 15 -4 187.78 6.30 -5 15 -4 199.88 7.40 5 15 4 181.38 6.60 7 -15 4 244.28 7.40 -7 15 -4 224.78 8.00 -7 15 -4 227.58 7.70 -7 15 -4 233.58 7.20 9 -15 4 16.10 2.20 -9 15 -4 11.10 2.50 -9 15 -4 17.80 2.20 9 15 4 13.80 2.30 9 15 4 14.80 2.50 -9 15 -4 13.10 2.90 -9 15 -4 11.30 2.60 -9 15 -4 15.90 3.10 -9 15 -4 12.60 2.60 9 15 4 15.00 2.30 -9 15 -4 13.20 3.20 11 -15 4 27.70 2.50 -11 15 -4 21.50 3.20 -11 15 -4 23.50 3.10 -11 15 -4 19.40 2.80 11 15 4 25.90 2.60 -11 15 -4 18.50 3.00 -11 15 -4 23.80 3.70 11 15 4 18.90 2.40 11 15 4 24.90 2.60 -11 15 -4 21.50 2.80 -11 15 -4 22.60 2.60 -13 15 -4 26.00 3.30 -13 15 -4 22.30 3.10 13 15 4 13.30 2.10 13 15 4 17.40 2.40 -13 15 -4 17.20 3.30 13 15 4 19.10 2.20 -13 15 -4 17.00 2.80 15 15 4 15.40 2.10 -15 15 -4 12.80 2.60 15 15 4 12.90 2.00 -15 15 -4 19.20 3.10 -15 15 -4 17.80 3.20 15 15 4 10.60 2.00 -15 15 -4 16.20 2.80 17 -15 4 56.49 3.00 17 15 4 56.69 3.30 17 15 4 56.49 3.50 -17 15 -4 63.29 4.30 17 15 4 57.89 3.40 -17 15 -4 53.49 4.40 19 -15 4 57.19 2.80 -19 15 -4 55.79 3.70 19 15 4 56.49 3.10 19 15 4 58.79 3.00 -19 15 -4 58.09 3.80 19 15 4 60.69 3.00 22 16 -4 2.50 1.30 -22 16 4 2.80 1.80 -20 16 4 8.10 2.20 20 16 -4 8.00 1.70 -20 16 4 8.60 2.40 -18 16 4 5.20 2.30 -18 16 4 -0.70 2.20 -18 16 4 2.50 2.60 -18 16 4 2.40 2.20 -16 16 4 13.10 3.00 -16 16 4 19.50 3.10 -16 16 4 15.50 2.90 -16 16 4 13.40 2.70 -14 16 4 26.20 3.10 -14 16 4 16.40 2.90 -14 16 4 15.60 3.00 -14 16 4 13.30 2.60 -14 16 4 19.00 2.80 -14 16 4 10.40 2.70 -12 16 4 4.50 2.20 -12 16 4 -0.20 2.30 -12 16 4 1.50 2.40 -12 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20.90 -5 -3 -9 865.21 22.00 5 -3 9 893.41 20.50 5 3 9 863.51 20.50 -5 3 -9 910.01 20.90 7 -3 9 60.19 2.70 -7 -3 -9 61.29 3.60 -7 3 -9 56.19 3.20 7 3 9 55.99 2.70 -9 -3 -9 381.46 10.80 9 -3 9 371.56 9.80 9 3 9 388.26 9.90 -9 3 -9 384.46 10.70 11 -3 9 2.80 1.30 -11 -3 -9 1.30 2.10 -11 3 -9 0.90 1.90 13 -3 9 4.40 1.40 -13 -3 -9 5.30 2.40 -13 3 -9 4.50 2.40 -15 -3 -9 500.25 13.80 -15 3 -9 494.65 13.60 17 -3 9 15.40 1.80 -17 -3 -9 17.20 3.00 -17 3 -9 14.30 2.50 17 3 9 16.10 1.90 -17 3 -9 15.50 2.50 19 -3 9 10.70 1.60 -19 3 -9 13.40 2.50 19 3 9 12.70 1.60 21 -3 9 80.69 3.20 -21 3 -9 74.69 4.30 21 3 9 79.49 3.20 23 -3 9 44.90 2.20 23 3 9 42.70 2.10 -23 3 -9 43.70 3.10 -32 -4 9 2.70 1.80 32 -4 -9 2.10 1.20 32 -4 -9 1.30 1.10 32 4 -9 2.20 1.10 32 4 -9 1.50 1.10 32 4 -9 1.70 1.10 30 -4 -9 117.59 4.30 30 -4 -9 114.99 4.40 30 4 -9 107.39 4.30 30 4 -9 115.39 4.30 30 4 -9 113.69 4.40 28 -4 -9 0.80 1.40 28 -4 -9 4.20 1.60 28 4 -9 2.00 1.40 28 4 -9 2.40 1.40 28 4 -9 3.20 1.60 26 -4 -9 0.40 1.60 26 -4 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1.80 10 -4 -9 17.90 1.70 10 4 -9 16.40 1.90 10 4 -9 18.60 1.70 -10 4 9 18.00 1.50 -10 4 9 14.90 1.60 10 4 -9 16.60 1.50 10 4 -9 12.70 1.30 8 -4 -9 138.19 4.60 -8 -4 9 138.69 4.20 8 -4 -9 139.69 4.70 -8 4 9 142.89 4.50 8 4 -9 142.59 4.30 8 4 -9 148.19 4.20 -8 4 9 138.39 4.10 8 4 -9 141.89 4.10 8 4 -9 151.18 5.00 6 -4 -9 32.10 2.20 -6 -4 9 31.00 1.90 6 -4 -9 34.60 2.50 6 4 -9 32.50 1.70 -6 4 9 33.60 1.80 6 4 -9 32.20 2.00 6 4 -9 34.20 2.40 -6 4 9 31.70 2.00 6 4 -9 34.20 1.90 4 -4 -9 78.29 3.10 4 -4 -9 74.29 3.40 -4 -4 9 75.29 2.70 -4 4 9 76.59 2.80 4 4 -9 74.49 3.00 4 4 -9 74.99 2.60 4 4 -9 72.79 2.80 4 4 -9 77.09 3.30 2 -4 -9 305.87 8.20 2 -4 -9 309.77 8.80 -2 -4 9 316.67 7.80 -2 -4 9 294.97 7.70 -2 4 9 303.67 7.90 2 4 -9 323.57 8.70 2 4 -9 300.67 8.00 -2 4 9 317.77 8.10 2 4 -9 318.07 7.70 2 4 -9 316.77 7.90 0 -4 9 374.26 9.20 0 -4 9 364.36 9.20 0 -4 -9 372.26 9.50 0 -4 -9 373.06 10.30 0 4 -9 371.16 9.00 0 4 -9 380.56 9.30 0 4 -9 379.46 9.40 0 4 9 373.66 9.40 0 4 9 369.66 9.30 0 4 -9 362.16 9.90 -2 -4 -9 1.30 1.70 2 -4 9 0.90 0.90 2 -4 9 1.10 0.90 -2 -4 -9 0.30 1.20 -2 4 -9 2.10 1.10 -2 4 -9 1.50 1.40 2 4 9 0.60 0.90 -2 4 -9 2.20 1.10 -2 4 -9 2.00 0.90 2 4 9 1.60 0.90 -4 -4 -9 873.01 21.00 4 -4 9 911.61 20.80 -4 -4 -9 891.91 21.00 -4 -4 -9 890.21 22.30 -4 4 -9 920.51 21.10 4 4 9 919.81 20.90 4 4 9 893.71 20.80 -6 -4 -9 0.20 2.00 -6 -4 -9 0.90 1.40 6 -4 9 -1.10 0.90 6 4 9 0.70 1.10 6 4 9 0.00 0.90 -6 4 -9 -1.70 1.20 -8 -4 -9 30.50 2.80 8 -4 9 33.40 2.20 8 4 9 28.70 2.20 -8 4 -9 31.10 2.70 10 -4 9 56.79 2.80 -10 -4 -9 59.69 4.00 -10 4 -9 54.49 3.70 12 -4 9 48.70 2.90 -12 -4 -9 55.29 4.20 -12 4 -9 54.49 4.20 -14 -4 -9 56.39 4.30 14 -4 9 52.59 3.10 -14 4 -9 55.39 4.20 16 -4 9 146.69 5.10 -16 -4 -9 151.58 6.30 16 4 9 146.59 5.20 -16 4 -9 145.09 5.80 -16 4 -9 140.59 6.60 -16 4 -9 147.99 6.40 18 -4 9 1.40 1.30 18 4 9 2.10 1.30 -18 4 -9 0.60 2.10 20 -4 9 16.00 1.60 -20 4 -9 17.50 2.50 20 4 9 21.30 1.80 22 -4 9 0.50 1.00 22 4 9 0.80 0.90 -22 4 -9 1.70 1.60 31 -5 -9 8.30 1.40 31 -5 -9 6.40 1.50 31 5 -9 6.30 1.30 31 5 -9 9.00 1.50 31 5 -9 2.60 1.40 29 -5 -9 16.70 1.90 29 -5 -9 16.40 1.90 29 5 -9 19.30 2.00 29 5 -9 15.90 1.90 29 5 -9 15.90 2.00 27 -5 -9 31.50 2.60 -27 -5 9 21.60 2.70 27 -5 -9 26.70 2.40 27 5 -9 27.50 2.50 -27 5 9 29.70 3.10 27 5 -9 20.40 2.10 27 5 -9 28.10 2.60 -25 -5 9 207.68 7.00 25 -5 -9 189.58 6.30 25 -5 -9 182.78 6.20 25 5 -9 188.18 6.50 -25 5 9 192.08 6.90 -25 5 9 180.48 7.50 25 5 -9 185.68 6.50 25 5 -9 193.58 6.30 23 -5 -9 161.78 5.90 -23 -5 9 167.68 6.10 23 5 -9 167.78 6.00 23 5 -9 162.38 5.70 -23 5 9 173.48 6.50 -21 -5 9 55.09 3.60 21 -5 -9 55.09 3.40 -21 5 9 54.29 3.50 -21 5 9 54.69 3.90 21 5 -9 49.99 3.00 21 5 -9 53.89 3.30 -19 -5 9 177.88 5.90 19 -5 -9 185.18 6.30 -19 5 9 171.88 6.00 19 5 -9 173.78 5.60 19 5 -9 179.58 5.70 -19 5 9 175.88 8.20 19 5 -9 167.18 5.90 17 -5 -9 69.39 3.60 -17 -5 9 70.49 3.40 17 5 -9 75.19 3.30 17 5 -9 70.29 3.20 17 5 -9 69.89 3.50 -17 5 9 74.49 3.50 -15 -5 9 101.99 3.80 15 -5 -9 100.99 4.30 -15 -5 9 95.69 3.60 -15 5 9 98.39 4.00 15 5 -9 98.79 3.70 15 5 -9 96.69 3.70 15 5 -9 95.79 3.80 -13 -5 9 441.56 10.90 13 -5 -9 454.75 11.50 13 5 -9 437.76 10.90 -13 5 9 438.76 11.20 13 5 -9 437.56 10.90 13 5 -9 431.26 11.90 13 5 -9 440.36 11.20 -11 -5 9 51.99 2.50 11 -5 -9 43.90 2.80 11 5 -9 48.00 2.90 11 5 -9 49.70 2.30 11 5 -9 46.80 2.40 -11 5 9 44.50 2.40 11 5 -9 49.90 2.40 -11 5 9 44.00 2.50 -9 -5 9 238.88 6.50 9 -5 -9 257.97 8.30 9 -5 -9 237.08 7.00 9 5 -9 243.28 7.40 -9 5 9 234.78 6.70 9 5 -9 255.17 6.60 -9 5 9 245.38 6.50 9 5 -9 240.18 6.40 9 5 -9 245.38 6.50 -7 -5 9 548.85 13.10 7 -5 -9 557.84 13.70 7 -5 -9 566.84 13.60 7 5 -9 544.05 13.90 7 5 -9 553.54 13.20 -7 5 9 542.45 13.30 7 5 -9 570.04 13.10 7 5 -9 546.95 12.90 -7 5 9 551.74 13.10 5 -5 -9 4.60 1.30 -5 -5 9 2.10 1.00 5 -5 -9 3.50 1.20 5 5 -9 3.90 1.00 5 5 -9 3.00 1.20 5 5 -9 4.10 1.00 -5 5 9 3.50 1.10 -5 5 9 3.90 1.00 5 5 -9 3.10 1.10 -3 -5 9 217.28 5.90 -3 -5 9 207.78 5.80 3 -5 -9 221.98 6.40 3 -5 -9 229.38 6.90 3 5 -9 220.88 5.80 3 5 -9 226.48 6.10 -3 5 9 224.58 6.20 -3 5 9 213.08 6.00 3 5 -9 212.58 6.60 3 5 -9 229.28 6.10 -1 -5 9 7.30 1.10 -1 -5 9 6.10 1.10 1 -5 -9 4.30 1.30 1 -5 -9 4.20 1.60 1 5 -9 4.30 1.10 1 5 -9 4.10 1.00 1 5 -9 3.00 1.10 1 5 -9 4.90 1.30 -1 5 9 5.60 1.20 -1 5 9 5.20 1.10 -1 -5 -9 1.30 1.70 1 -5 9 2.40 1.00 -1 -5 -9 2.10 1.20 1 -5 9 1.60 0.90 -1 5 -9 3.30 1.00 1 5 9 2.20 1.00 -1 5 -9 2.60 1.00 -1 5 -9 2.00 1.20 1 5 9 2.70 1.00 3 -5 9 1292.47 29.10 -3 -5 -9 1295.17 29.50 -3 5 -9 1284.67 29.20 3 5 9 1304.87 29.30 -3 5 -9 1291.37 28.90 -3 5 -9 1287.97 29.30 3 5 9 1268.97 29.20 5 -5 9 445.46 11.10 -5 -5 -9 445.06 11.60 -5 -5 -9 440.46 11.50 5 5 9 446.66 11.20 5 5 9 435.96 11.20 -5 5 -9 443.56 11.40 -5 5 -9 444.36 10.90 -7 -5 -9 34.60 2.90 -7 -5 -9 32.10 2.80 7 -5 9 36.00 2.20 7 5 9 32.20 2.30 7 5 9 30.20 2.30 -7 5 -9 35.50 2.70 -7 5 -9 29.70 2.60 9 -5 9 195.48 5.90 -9 -5 -9 197.78 6.90 9 5 9 191.38 6.00 -9 5 -9 195.88 6.60 11 -5 9 34.20 2.40 -11 -5 -9 38.20 3.70 -11 5 -9 30.80 3.20 -13 -5 -9 385.46 11.30 13 -5 9 383.86 10.00 -13 5 -9 369.06 11.00 15 -5 9 173.18 5.70 15 -5 9 167.08 5.90 -15 -5 -9 171.98 6.90 15 5 9 165.08 5.70 -15 5 -9 160.48 6.80 -15 5 -9 174.08 6.70 -15 5 -9 168.68 6.50 -15 5 -9 163.48 7.00 17 -5 9 67.59 3.40 -17 -5 -9 68.89 4.60 17 5 9 69.89 3.40 -17 5 -9 70.09 4.70 -17 5 -9 65.69 4.70 -17 5 -9 65.39 4.10 19 -5 9 76.99 3.40 19 5 9 81.49 3.50 -19 5 -9 73.29 4.70 21 -5 9 23.40 2.10 -21 5 -9 24.50 2.60 21 5 9 24.10 2.00 32 -6 -9 1.50 1.00 32 -6 -9 1.80 1.10 32 6 -9 0.90 1.00 32 6 -9 1.20 1.00 32 6 -9 0.00 1.10 30 -6 -9 34.80 2.70 30 -6 -9 36.90 2.70 30 6 -9 42.30 2.80 30 6 -9 41.50 2.60 30 6 -9 37.40 2.70 28 -6 -9 9.40 1.80 28 -6 -9 10.70 1.80 28 6 -9 7.50 1.80 28 6 -9 5.50 1.60 28 6 -9 6.80 1.70 26 -6 -9 62.69 3.70 -26 -6 9 67.19 4.20 26 -6 -9 70.69 3.60 26 6 -9 64.29 3.60 26 6 -9 63.29 3.70 -26 6 9 63.99 4.20 -26 6 9 64.09 5.00 26 6 -9 64.59 3.80 24 -6 -9 17.40 2.30 -24 -6 9 18.80 2.70 24 -6 -9 20.60 2.40 -24 6 9 19.00 3.60 24 6 -9 18.80 2.10 24 6 -9 15.20 2.10 24 6 -9 18.00 2.40 24 6 -9 17.90 2.20 -24 6 9 15.50 2.50 -22 -6 9 98.09 4.80 22 -6 -9 94.49 4.40 -22 6 9 97.29 5.40 -22 6 9 101.39 4.60 22 6 -9 94.89 4.40 22 6 -9 98.39 4.30 20 -6 -9 40.70 3.30 -20 -6 9 35.80 3.00 20 6 -9 33.50 2.70 -20 6 9 31.90 2.80 20 6 -9 40.60 3.00 20 6 -9 35.70 3.00 18 -6 -9 11.40 1.90 -18 -6 9 10.90 2.00 18 6 -9 11.00 1.80 18 6 -9 14.10 1.90 18 6 -9 11.90 1.70 -18 6 9 10.30 1.90 -16 -6 9 1.50 1.50 16 -6 -9 0.90 1.60 16 6 -9 -0.20 1.20 16 6 -9 0.20 1.10 16 6 -9 0.40 1.20 -16 6 9 -0.70 1.30 -14 -6 9 190.08 5.60 14 -6 -9 191.28 6.20 -14 -6 9 179.98 5.60 -14 6 9 188.78 6.00 14 6 -9 188.88 5.70 14 6 -9 191.38 5.70 12 -6 -9 139.09 5.00 -12 -6 9 133.99 4.30 12 6 -9 135.19 4.40 -12 6 9 139.49 4.80 12 6 -9 130.89 5.20 12 6 -9 132.69 4.30 12 6 -9 137.69 4.40 -10 -6 9 4.00 1.00 10 -6 -9 4.70 1.50 -10 6 9 4.00 1.10 10 6 -9 4.90 1.40 10 6 -9 5.40 1.20 10 6 -9 5.50 1.10 -10 6 9 2.90 1.30 10 6 -9 4.30 1.00 -8 -6 9 6.70 1.10 8 -6 -9 8.10 1.70 -8 6 9 5.60 1.30 8 6 -9 6.70 1.20 8 6 -9 9.70 1.30 8 6 -9 7.20 1.20 8 6 -9 7.10 1.50 -8 6 9 5.10 1.20 -6 -6 9 3.40 1.00 6 -6 -9 4.60 1.40 6 -6 -9 3.30 1.40 6 6 -9 3.50 1.00 -6 6 9 4.60 1.30 6 6 -9 3.80 1.00 -6 6 9 4.30 1.10 6 6 -9 2.90 1.30 6 6 -9 1.50 1.00 -4 -6 9 6.20 1.10 4 -6 -9 6.30 1.60 4 -6 -9 7.40 1.40 -4 -6 9 6.80 1.00 4 6 -9 7.90 1.10 -4 6 9 6.30 1.20 4 6 -9 7.60 1.40 4 6 -9 8.40 1.20 -4 6 9 7.80 1.20 4 6 -9 5.50 1.20 -2 -6 9 241.38 6.40 2 -6 -9 243.88 6.90 -2 -6 9 236.28 6.40 2 -6 -9 239.08 7.40 -2 6 9 233.18 6.50 2 6 -9 248.78 6.40 -2 6 9 242.18 6.80 2 6 -9 236.78 6.50 2 6 -9 228.28 7.10 2 6 -9 244.68 6.70 0 -6 -9 1.40 1.60 0 -6 9 2.60 1.00 0 -6 -9 2.90 1.30 0 6 9 3.50 1.10 0 6 -9 3.20 1.10 0 6 -9 1.70 1.00 0 6 -9 2.80 1.30 0 6 9 3.10 1.10 -2 -6 -9 206.28 6.20 2 -6 9 201.88 5.80 -2 -6 -9 197.48 7.10 -2 6 -9 204.88 6.00 -2 6 -9 196.28 5.60 -2 6 -9 200.78 6.10 2 6 9 191.28 5.90 2 6 9 203.58 5.90 4 -6 9 381.86 9.60 -4 -6 -9 369.96 10.00 4 6 9 352.96 9.60 -4 6 -9 356.36 9.70 -4 6 -9 378.16 9.80 4 6 9 383.66 9.80 -4 6 -9 369.46 9.40 -6 -6 -9 30.80 2.80 6 -6 9 37.20 2.50 6 6 9 37.90 2.40 6 6 9 37.70 2.60 -6 6 -9 37.70 2.70 -6 6 -9 40.00 2.50 8 -6 9 296.47 7.90 -8 -6 -9 276.87 8.70 -8 -6 -9 288.97 8.70 -8 6 -9 280.77 8.40 8 6 9 293.67 8.00 8 6 9 283.07 8.10 -8 6 -9 283.57 8.00 10 -6 9 3.10 1.40 -10 -6 -9 5.30 2.40 -10 6 -9 7.00 2.20 -10 6 -9 7.10 3.00 12 -6 9 57.69 2.90 -12 -6 -9 54.19 4.30 -12 6 -9 54.89 4.10 14 -6 9 248.48 7.40 14 -6 9 243.88 7.60 14 -6 9 263.47 7.20 -14 -6 -9 253.57 8.70 14 6 9 242.58 7.60 -14 6 -9 231.38 8.70 -14 6 -9 252.87 8.20 -14 6 -9 250.57 8.70 14 6 9 254.47 7.90 -14 6 -9 251.67 8.90 16 -6 9 117.19 4.60 -16 -6 -9 109.39 5.50 16 -6 9 106.49 4.30 16 6 9 114.59 4.50 -16 6 -9 109.89 5.60 -16 6 -9 111.69 5.50 -16 6 -9 106.99 5.60 -16 6 -9 106.29 5.80 16 6 9 108.89 4.50 18 -6 9 1.90 1.30 -18 6 -9 3.20 2.20 -18 6 -9 1.40 2.20 18 6 9 2.90 1.30 18 6 9 2.90 1.40 20 -6 9 30.90 2.20 20 6 9 30.50 2.30 20 6 9 33.50 2.40 -20 6 -9 28.60 2.80 22 -6 9 5.40 1.10 -22 6 -9 4.90 1.80 31 -7 -9 45.30 2.70 31 7 -9 46.60 2.70 31 7 -9 45.80 2.70 31 7 -9 46.90 2.50 29 -7 -9 18.00 1.90 29 -7 -9 19.30 1.90 29 7 -9 15.40 1.80 29 7 -9 21.70 2.10 29 7 -9 24.00 2.00 27 -7 -9 35.00 3.00 27 -7 -9 35.10 2.90 27 7 -9 35.50 3.10 27 7 -9 32.10 2.80 27 7 -9 31.90 2.60 25 -7 -9 116.79 4.80 25 -7 -9 121.89 4.90 -25 -7 9 119.99 5.30 -25 -7 9 122.19 5.30 25 7 -9 122.69 4.80 25 7 -9 120.89 5.10 25 7 -9 121.19 4.80 -25 7 9 123.79 6.20 25 7 -9 115.79 4.60 -23 -7 9 270.27 8.30 -23 7 9 238.88 8.20 23 7 -9 267.97 7.80 -21 -7 9 5.60 2.10 21 -7 -9 2.40 1.50 21 7 -9 0.40 1.30 -21 7 9 0.40 1.70 21 7 -9 1.70 1.50 21 7 -9 0.30 1.60 -19 -7 9 103.19 4.60 19 -7 -9 95.79 4.60 19 7 -9 99.89 4.30 19 7 -9 90.09 4.30 -19 7 9 101.19 4.60 19 7 -9 102.09 4.10 17 -7 -9 48.40 3.40 -17 -7 9 46.70 3.00 17 7 -9 50.99 3.00 -17 7 9 52.09 3.30 17 7 -9 46.50 2.80 17 7 -9 51.09 3.10 -15 -7 9 181.08 5.80 15 -7 -9 175.98 6.20 15 7 -9 185.68 5.80 -15 7 9 187.88 6.10 15 7 -9 190.38 5.70 13 -7 -9 127.29 5.10 -13 -7 9 125.99 4.20 -13 7 9 134.89 4.80 13 7 -9 127.19 4.40 13 7 -9 126.39 4.30 11 -7 -9 185.08 6.20 -11 -7 9 173.68 5.30 -11 7 9 180.88 5.80 -11 7 9 184.48 5.50 11 7 -9 185.88 5.50 11 7 -9 182.98 6.40 11 7 -9 180.28 5.50 11 7 -9 181.38 5.30 9 -7 -9 12.60 1.90 -9 -7 9 9.90 1.40 9 7 -9 11.70 1.40 -9 7 9 13.40 1.70 9 7 -9 9.20 1.60 -9 7 9 9.90 1.40 9 7 -9 12.60 1.40 9 7 -9 11.70 1.40 -7 -7 9 233.38 6.50 7 -7 -9 253.17 7.30 -7 7 9 235.18 6.60 7 7 -9 237.38 6.40 7 7 -9 244.18 6.70 7 7 -9 233.58 6.50 7 7 -9 235.68 7.40 -7 7 9 251.57 6.90 5 -7 -9 61.49 3.30 -5 -7 9 64.69 2.70 5 -7 -9 63.39 3.20 -5 7 9 66.49 2.80 -5 7 9 64.69 2.80 5 7 -9 58.19 3.30 5 7 -9 65.59 2.80 5 7 -9 62.49 2.70 5 7 -9 64.89 2.60 3 -7 -9 118.19 4.80 -3 -7 9 119.19 3.90 3 -7 -9 125.39 4.60 3 7 -9 121.19 4.00 -3 7 9 129.29 4.40 -3 7 9 125.69 4.10 3 7 -9 122.59 4.20 3 7 -9 124.19 3.90 1 -7 -9 144.99 5.00 1 -7 -9 135.89 5.40 -1 -7 9 140.39 4.40 -1 7 9 136.09 4.60 1 7 -9 140.69 4.70 -1 7 9 138.09 4.80 1 7 -9 146.89 4.40 1 7 -9 134.69 4.50 1 -7 9 240.08 6.70 -1 -7 -9 233.18 7.20 -1 7 -9 251.37 6.70 -1 7 -9 235.88 6.80 1 7 9 245.98 6.90 1 7 9 248.68 7.00 -1 7 -9 255.67 7.10 3 -7 9 282.07 7.50 -3 -7 -9 275.77 8.00 -3 7 -9 268.37 7.30 3 7 9 272.47 7.70 -3 7 -9 268.57 7.70 3 7 9 259.77 7.60 -3 7 -9 277.17 7.70 -5 -7 -9 317.27 9.10 5 -7 9 310.67 8.40 5 7 9 306.17 8.60 5 7 9 299.77 8.40 -5 7 -9 317.57 8.30 -5 7 -9 307.27 8.70 -5 7 -9 309.77 8.70 7 -7 9 17.50 1.80 -7 -7 -9 15.90 2.40 7 7 9 19.20 2.20 -7 7 -9 21.70 2.30 7 7 9 18.40 2.00 -7 7 -9 16.50 1.90 -9 -7 -9 119.49 5.40 -9 -7 -9 118.99 6.00 9 -7 9 130.29 4.50 9 7 9 113.79 4.70 -9 7 -9 126.19 4.80 -9 7 -9 123.39 5.10 -11 -7 -9 25.10 3.20 11 -7 9 22.60 2.10 -11 7 -9 15.30 2.10 -11 7 -9 27.00 3.00 11 7 9 19.80 2.30 -13 -7 -9 271.37 9.00 13 -7 9 271.47 7.60 -13 7 -9 247.68 8.20 15 -7 9 240.48 7.40 -15 -7 -9 250.57 8.50 15 -7 9 239.28 7.10 15 -7 9 234.88 7.00 15 7 9 239.18 7.40 -15 7 -9 251.37 8.50 -15 7 -9 238.18 8.60 -15 7 -9 248.68 8.40 15 7 9 251.27 7.40 17 -7 9 26.80 2.30 17 -7 9 19.00 1.90 17 7 9 20.10 1.90 -17 7 -9 26.70 3.20 -17 7 -9 25.20 3.20 -17 7 -9 22.00 2.80 17 7 9 19.60 2.10 19 -7 9 9.10 1.50 19 7 9 10.20 1.50 -19 7 -9 16.90 2.60 19 7 9 11.00 1.50 21 -7 9 0.50 1.00 21 7 9 3.20 1.00 -21 7 -9 0.90 1.60 30 -8 -9 5.60 1.40 30 8 -9 7.90 1.40 30 8 -9 3.60 1.20 30 8 -9 7.60 1.40 28 -8 -9 21.60 2.20 28 -8 -9 23.20 2.10 28 8 -9 16.00 1.90 28 8 -9 24.50 2.10 28 8 -9 22.90 2.20 26 -8 -9 137.19 5.10 26 -8 -9 143.79 5.10 26 8 -9 136.89 5.20 26 8 -9 135.59 5.00 26 8 -9 134.39 5.30 -26 8 9 133.99 6.40 -24 -8 9 162.18 6.20 24 -8 -9 164.48 5.80 24 -8 -9 163.08 5.90 24 8 -9 160.48 5.70 -24 8 9 163.18 7.10 24 8 -9 171.58 6.10 24 8 -9 170.78 5.90 24 8 -9 171.78 5.90 -22 -8 9 17.90 2.50 22 8 -9 23.40 2.50 -22 8 9 26.10 2.80 20 -8 -9 170.18 6.10 -20 -8 9 163.38 5.90 20 8 -9 156.08 6.30 20 8 -9 168.98 5.80 -20 8 9 168.18 6.10 20 8 -9 168.78 5.80 -18 -8 9 141.69 5.40 18 -8 -9 132.59 5.50 18 8 -9 141.59 5.10 18 8 -9 138.19 5.10 -18 8 9 139.89 5.60 16 -8 -9 1.00 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64.89 3.30 -1 9 -9 72.49 3.20 -1 9 -9 65.29 3.60 1 9 9 68.39 3.30 1 9 9 66.19 3.40 3 -9 9 341.37 9.10 -3 -9 -9 339.67 9.80 3 9 9 335.47 9.40 -3 9 -9 336.37 9.00 -3 9 -9 342.37 9.50 -3 9 -9 340.27 9.30 3 9 9 335.17 9.30 5 -9 9 100.19 4.00 -5 -9 -9 96.69 4.80 5 9 9 105.69 4.30 -5 9 -9 103.19 4.40 -5 9 -9 99.49 4.60 -5 9 -9 109.69 4.30 5 9 9 107.89 4.50 7 -9 9 11.10 1.80 -7 -9 -9 8.80 2.40 -7 9 -9 10.60 2.00 -7 9 -9 6.70 2.00 -7 9 -9 4.60 3.30 7 9 9 6.30 1.60 -9 -9 -9 94.49 5.10 9 -9 9 101.39 4.10 -9 9 -9 106.59 4.50 9 9 9 87.29 4.30 -9 9 -9 98.09 4.70 11 -9 9 129.59 4.70 -11 9 -9 119.39 4.90 13 -9 9 85.19 3.70 13 -9 9 80.59 3.70 -13 9 -9 85.79 5.30 13 9 9 80.99 4.10 -13 9 -9 86.39 5.10 13 9 9 80.99 4.00 13 9 9 83.99 4.10 -13 9 -9 90.29 5.20 13 9 9 85.79 4.50 -13 9 -9 84.99 4.30 15 -9 9 184.88 6.20 15 -9 9 194.38 6.00 -15 9 -9 208.58 7.70 15 9 9 191.98 6.20 15 9 9 197.88 6.50 -15 9 -9 184.58 7.20 -15 9 -9 204.08 7.40 15 9 9 197.58 6.30 15 9 9 189.28 6.40 17 -9 9 3.90 1.40 17 -9 9 4.80 1.50 -17 9 -9 5.10 2.20 17 9 9 7.00 1.50 17 9 9 3.00 1.50 17 9 9 6.60 1.60 17 9 9 2.70 1.30 -17 9 -9 1.40 2.20 -17 9 -9 3.90 2.20 19 -9 9 13.10 1.40 19 -9 9 9.80 1.40 19 9 9 15.80 1.70 -19 9 -9 13.80 2.10 -19 9 -9 13.90 2.30 28 -10 -9 1.00 1.40 28 10 -9 3.10 1.30 28 10 -9 2.10 1.40 28 10 -9 2.70 1.40 26 -10 -9 -2.90 1.40 -26 10 9 3.40 2.30 26 10 -9 -0.20 1.60 26 10 -9 0.70 1.40 24 -10 -9 257.27 8.80 24 -10 -9 242.28 7.50 24 10 -9 238.78 7.70 -24 10 9 260.67 8.70 24 10 -9 239.68 7.60 22 -10 -9 23.10 2.40 22 -10 -9 19.70 2.30 -22 -10 9 24.20 2.80 22 10 -9 22.90 2.50 -22 10 9 28.70 3.20 -22 10 9 19.90 2.60 -22 10 9 26.80 3.60 22 10 -9 18.00 2.20 22 10 -9 22.00 2.50 -20 -10 9 15.10 2.40 -20 10 9 15.20 2.40 20 10 -9 13.50 2.00 20 10 -9 12.70 2.10 -18 -10 9 351.06 9.90 18 -10 -9 333.67 10.00 18 10 -9 346.97 9.50 18 10 -9 361.76 9.80 -18 10 9 355.56 10.30 -16 -10 9 25.80 2.50 16 -10 -9 24.50 2.70 -16 10 9 23.10 2.70 16 10 -9 29.30 2.60 16 10 -9 27.50 2.50 14 -10 -9 64.09 3.90 -14 10 9 60.89 3.50 -14 10 9 56.79 3.70 14 10 -9 57.39 3.40 14 10 -9 56.89 3.30 12 -10 -9 215.58 7.20 12 10 -9 196.48 6.10 -12 10 9 201.18 6.50 12 10 -9 204.78 6.40 12 10 -9 196.08 6.30 -12 10 9 206.58 6.90 -10 -10 9 57.89 3.10 10 -10 -9 63.69 3.80 10 10 -9 55.29 3.10 -10 10 9 61.39 3.50 -10 10 9 60.29 3.30 10 10 -9 58.39 3.10 10 10 -9 62.79 3.00 -8 -10 9 701.93 16.80 8 -10 -9 718.33 17.60 8 10 -9 689.33 16.90 -8 10 9 720.53 17.10 8 10 -9 699.63 16.70 -8 10 9 684.53 17.20 8 10 -9 710.53 17.00 6 -10 -9 110.79 4.80 -6 -10 9 105.49 4.00 6 10 -9 106.69 4.20 6 10 -9 111.29 4.10 -6 10 9 108.59 4.40 -6 10 9 111.19 4.20 6 10 -9 109.79 4.10 4 -10 -9 -1.00 1.60 4 10 -9 -0.10 1.10 4 10 -9 0.20 1.20 -4 10 9 3.70 1.50 4 10 -9 0.70 1.40 -2 -10 9 187.68 5.80 2 -10 -9 193.28 6.60 2 10 -9 183.38 5.90 -2 10 9 197.48 6.20 -2 10 9 185.38 6.20 2 10 -9 195.68 5.80 2 10 -9 197.18 6.20 0 -10 -9 39.60 3.50 0 -10 9 42.10 2.60 0 10 -9 42.20 2.80 0 10 -9 40.90 2.60 0 10 9 43.50 3.00 0 10 9 41.10 3.00 0 10 -9 40.90 2.90 2 -10 9 2.00 1.30 -2 -10 -9 2.50 1.80 2 10 9 4.60 1.60 2 10 9 9.40 1.80 -2 10 -9 2.40 1.40 -2 10 -9 1.80 1.40 -2 10 -9 2.00 1.60 -4 -10 -9 346.97 10.10 4 -10 9 342.17 9.20 -4 10 -9 331.07 9.50 4 10 9 335.87 9.60 -4 10 -9 330.47 9.60 -4 10 -9 330.07 9.20 4 10 9 341.17 9.40 -6 -10 -9 2.70 2.10 6 -10 9 3.10 1.50 -6 10 -9 1.90 1.70 -6 10 -9 3.90 1.70 6 10 9 1.70 1.60 6 10 9 2.30 1.60 -6 10 -9 -0.40 1.90 8 -10 9 39.20 2.70 -8 -10 -9 45.40 4.10 -8 10 -9 42.40 3.10 8 10 9 42.40 3.20 10 -10 9 141.59 4.90 10 10 9 117.29 7.50 -10 10 -9 128.79 5.30 12 -10 9 2.80 1.40 12 -10 9 3.90 1.40 -12 10 -9 4.50 2.60 12 10 9 3.40 1.70 12 10 9 3.30 1.60 12 10 9 3.60 1.60 -12 10 -9 -0.40 2.10 -12 10 -9 0.80 2.40 -12 10 -9 -0.30 2.30 12 10 9 3.10 1.70 -12 10 -9 3.40 2.00 14 -10 9 125.79 4.60 -14 10 -9 140.39 6.10 14 10 9 133.59 5.00 -14 10 -9 136.79 5.90 -14 10 -9 136.59 6.40 14 10 9 130.39 5.30 14 10 9 127.19 5.00 14 10 9 135.49 5.20 16 -10 9 152.18 5.30 16 -10 9 152.18 5.00 16 10 9 153.88 5.50 -16 10 -9 149.69 6.40 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61.09 3.30 15 11 -9 60.79 3.50 -15 11 9 67.49 3.60 -15 11 9 66.59 4.00 13 -11 -9 49.00 3.90 13 11 -9 45.60 3.20 -13 11 9 46.50 3.80 -13 11 9 42.30 3.10 13 11 -9 45.70 3.00 -11 -11 9 0.60 1.30 11 -11 -9 -0.70 1.90 11 11 -9 1.30 1.40 -11 11 9 1.60 1.70 11 11 -9 0.00 1.30 11 11 -9 0.30 1.40 -11 11 9 -0.50 1.80 -9 -11 9 200.48 6.20 9 -11 -9 204.58 7.20 -9 11 9 220.78 7.00 9 11 -9 198.98 6.40 9 11 -9 202.48 6.40 -9 11 9 203.98 6.60 9 11 -9 207.48 6.20 -7 -11 9 35.90 2.50 7 -11 -9 39.50 3.40 7 11 -9 39.70 2.60 7 11 -9 41.60 2.70 -7 11 9 38.90 3.10 -7 11 9 35.20 2.80 7 11 -9 37.20 2.90 5 -11 -9 5.20 2.20 5 11 -9 2.60 1.30 5 11 -9 4.80 1.40 -5 11 9 4.80 1.70 5 11 -9 3.60 1.50 3 -11 -9 60.29 3.80 3 11 -9 57.39 3.50 3 11 -9 61.59 3.30 -3 11 9 55.99 3.30 3 11 -9 56.99 3.00 -1 -11 9 3.70 1.50 1 -11 -9 4.90 2.10 1 11 -9 6.00 1.90 1 11 -9 3.00 1.50 -1 11 9 4.70 1.80 1 11 -9 1.30 1.70 1 11 -9 2.70 1.40 -1 11 9 3.70 1.60 -1 -11 -9 7.30 2.20 1 -11 9 7.90 1.60 -1 11 -9 8.40 1.60 1 11 9 12.60 2.10 -1 11 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-19 3 10 2.10 1.70 19 3 -10 0.90 1.30 -19 3 10 2.80 1.60 17 -3 -10 2.80 1.40 -17 -3 10 4.90 1.50 -17 -3 10 5.40 1.40 17 3 -10 4.10 1.30 17 3 -10 3.80 1.30 -17 3 10 5.70 1.70 17 3 -10 4.90 1.50 -15 -3 10 113.09 4.10 -15 -3 10 112.89 4.00 15 -3 -10 118.29 4.50 15 3 -10 115.89 3.90 15 3 -10 111.99 4.70 15 3 -10 121.79 4.40 -15 3 10 112.49 4.20 15 3 -10 109.59 3.90 13 -3 -10 16.00 1.90 -13 -3 10 14.90 1.60 -13 -3 10 18.10 1.70 -13 3 10 13.80 1.70 13 3 -10 14.30 1.40 13 3 -10 20.40 2.20 13 3 -10 16.50 1.60 13 3 -10 16.10 1.70 -11 -3 10 175.98 5.20 11 -3 -10 182.48 5.70 11 -3 -10 182.68 5.80 11 3 -10 179.18 5.10 11 3 -10 180.58 6.00 -11 3 10 182.38 5.50 11 3 -10 184.38 5.80 11 3 -10 184.48 5.20 -9 -3 10 1.60 1.00 9 -3 -10 1.10 1.30 9 -3 -10 1.70 1.30 9 3 -10 0.40 0.80 -9 3 10 1.40 0.80 9 3 -10 1.20 0.80 9 3 -10 0.50 1.10 -9 3 10 1.70 1.00 7 -3 -10 45.40 2.70 7 -3 -10 48.00 2.80 -7 -3 10 46.10 2.30 7 3 -10 46.80 2.70 7 3 -10 49.99 2.40 7 3 -10 43.80 2.00 7 3 -10 47.20 2.20 -7 3 10 45.30 2.10 -7 3 10 45.30 2.30 -5 -3 10 16.50 1.50 -5 -3 10 16.60 1.30 5 -3 -10 15.40 1.90 5 -3 -10 14.00 1.70 -5 3 10 15.50 1.40 5 3 -10 18.90 1.70 5 3 -10 16.30 1.40 5 3 -10 21.10 2.10 -5 3 10 16.80 1.60 5 3 -10 16.00 1.40 -3 -3 10 34.30 1.80 3 -3 -10 34.50 2.80 3 -3 -10 33.90 2.30 -3 -3 10 33.10 1.90 3 3 -10 33.80 2.20 -3 3 10 28.70 2.20 -3 3 10 34.00 1.90 3 3 -10 29.80 1.90 3 3 -10 35.20 2.60 -1 -3 10 45.10 2.10 1 -3 -10 45.20 2.50 -1 -3 10 44.60 2.20 1 -3 -10 40.50 2.90 1 3 -10 45.60 3.00 1 3 -10 39.80 2.20 -1 3 10 48.40 2.30 1 3 -10 43.60 2.30 -1 3 10 45.00 2.30 1 -3 10 110.49 3.60 -1 -3 -10 111.39 3.90 -1 -3 -10 109.89 4.90 -1 -3 -10 113.29 3.80 1 -3 10 112.19 3.80 1 3 10 104.49 3.80 -1 3 -10 103.39 3.70 1 3 10 111.09 3.80 -1 3 -10 112.59 4.50 -1 3 -10 106.39 3.80 -3 -3 -10 38.50 3.30 -3 -3 -10 41.80 2.50 3 -3 10 43.10 2.30 -3 3 -10 46.00 2.60 3 3 10 45.70 2.40 -5 -3 -10 84.59 3.70 5 -3 10 83.59 3.30 -5 3 -10 86.39 3.80 5 3 10 83.59 3.40 7 -3 10 20.30 1.90 -7 -3 -10 17.70 2.30 -7 3 -10 22.20 2.40 7 3 10 18.40 1.90 9 -3 10 29.50 2.20 -9 -3 -10 24.30 3.00 -9 3 -10 28.50 2.90 9 3 10 33.60 2.50 -11 -3 -10 49.00 3.90 11 -3 10 43.30 2.70 -11 3 -10 42.10 3.50 13 -3 10 21.00 2.00 -13 -3 -10 26.60 3.30 -13 3 -10 20.00 2.70 15 -3 10 6.00 1.60 -15 -3 -10 6.80 2.50 15 -3 10 7.40 1.60 -15 3 -10 8.30 2.40 15 3 10 5.90 1.50 -15 3 -10 2.20 2.30 -15 3 -10 9.60 2.50 17 -3 10 11.10 1.60 17 3 10 11.60 1.60 -17 3 -10 9.40 2.30 19 -3 10 -1.50 1.10 -19 3 -10 -3.30 1.70 19 3 10 0.50 1.10 21 -3 10 5.50 1.20 -21 3 -10 1.20 1.60 21 3 10 5.30 1.10 32 -4 -10 42.70 2.60 32 -4 -10 44.80 2.60 32 4 -10 46.00 2.50 32 4 -10 46.20 2.60 32 4 -10 41.30 2.40 30 -4 -10 25.50 2.20 30 -4 -10 22.00 2.00 30 4 -10 18.80 1.90 30 4 -10 15.60 1.70 30 4 -10 19.30 2.00 28 -4 -10 17.70 2.00 28 -4 -10 24.00 2.20 28 4 -10 22.00 2.20 28 4 -10 22.70 2.10 28 4 -10 17.40 2.00 26 -4 -10 35.00 3.10 -26 -4 10 38.70 3.30 26 -4 -10 38.50 3.00 26 4 -10 36.80 3.00 -26 4 10 34.50 3.20 26 4 -10 36.20 3.20 26 4 -10 34.90 2.80 -24 -4 10 51.29 3.90 24 -4 -10 49.40 3.60 -24 4 10 49.30 4.00 24 4 -10 51.99 3.70 22 -4 -10 226.68 7.50 -22 -4 10 226.68 7.60 22 4 -10 231.28 7.40 -22 4 10 238.98 7.60 -22 4 10 237.18 7.40 -20 -4 10 60.99 3.60 20 -4 -10 63.59 3.80 -20 4 10 63.59 3.60 20 4 -10 62.89 3.30 -20 4 10 61.09 5.40 20 4 -10 61.59 3.20 20 4 -10 61.19 3.40 -18 -4 10 41.10 3.10 18 -4 -10 38.90 3.20 18 4 -10 41.50 2.80 -18 4 10 40.50 3.10 18 4 -10 42.20 2.90 18 4 -10 42.70 2.70 -16 -4 10 78.89 3.60 16 -4 -10 77.29 3.90 -16 -4 10 76.69 3.30 16 4 -10 78.09 3.20 16 4 -10 75.99 3.30 16 4 -10 86.19 3.70 -16 4 10 78.59 3.80 -14 -4 10 7.10 1.50 -14 -4 10 5.00 1.20 14 -4 -10 4.10 1.60 14 4 -10 6.70 1.30 14 4 -10 6.30 1.50 -14 4 10 7.00 1.50 14 4 -10 5.10 1.30 14 4 -10 6.50 1.20 -12 -4 10 815.72 19.30 12 -4 -10 841.22 19.90 12 4 -10 827.52 19.30 12 4 -10 855.41 19.30 -12 4 10 836.72 19.70 12 4 -10 828.72 20.40 -10 -4 10 377.16 9.70 10 -4 -10 398.76 10.30 10 -4 -10 386.36 10.20 -10 4 10 385.66 10.00 10 4 -10 395.46 10.70 -10 4 10 383.66 9.50 10 4 -10 391.16 9.60 10 4 -10 398.76 9.70 -8 -4 10 1.90 1.00 8 -4 -10 3.10 1.20 8 -4 -10 3.90 1.50 8 4 -10 4.30 1.20 -8 4 10 4.40 1.00 8 4 -10 4.70 1.30 8 4 -10 3.70 1.10 -8 4 10 5.20 1.20 8 4 -10 3.10 0.90 6 -4 -10 330.17 9.00 -6 -4 10 314.77 8.10 6 -4 -10 313.17 8.50 6 4 -10 319.57 7.90 6 4 -10 320.67 8.30 -6 4 10 315.17 8.10 6 4 -10 328.37 8.10 -6 4 10 305.27 8.30 6 4 -10 320.57 9.00 4 -4 -10 -0.30 1.10 -4 -4 10 3.20 0.90 -4 -4 10 2.10 0.80 4 -4 -10 2.10 1.30 -4 4 10 1.30 1.10 -4 4 10 1.40 0.90 4 4 -10 0.30 1.20 4 4 -10 0.20 0.80 4 4 -10 1.30 1.00 4 4 -10 -1.50 0.80 2 -4 -10 352.86 9.20 -2 -4 10 342.37 8.70 -2 -4 10 353.86 8.80 2 -4 -10 345.47 9.80 2 4 -10 353.56 8.60 2 4 -10 343.97 9.70 -2 4 10 346.67 9.00 2 4 -10 339.57 8.80 -2 4 10 359.16 8.90 2 4 -10 349.07 9.00 0 -4 -10 494.05 12.10 0 -4 10 489.35 11.60 0 -4 10 472.45 11.70 0 -4 -10 455.95 12.80 0 4 10 492.15 11.90 0 4 -10 492.75 11.80 0 4 -10 467.25 12.60 0 4 -10 489.05 11.90 0 4 10 467.25 11.70 -2 -4 -10 270.17 7.50 2 -4 10 253.87 7.10 2 -4 10 271.57 7.30 -2 -4 -10 262.87 8.50 -2 4 -10 268.27 7.30 -2 4 -10 251.87 7.20 2 4 10 261.17 7.20 2 4 10 256.47 7.20 4 -4 10 522.55 12.90 -4 -4 -10 533.45 13.20 4 4 10 535.75 13.20 4 4 10 511.05 13.00 -4 4 -10 528.65 13.20 6 -4 10 16.70 1.70 -6 -4 -10 18.80 2.20 -6 4 -10 19.00 2.40 6 4 10 21.20 1.90 -8 -4 -10 -1.30 1.80 8 -4 10 2.80 1.20 -8 4 -10 4.20 2.00 8 4 10 0.00 1.20 10 -4 10 491.05 12.50 -10 -4 -10 511.45 13.80 -10 4 -10 498.45 13.50 -12 -4 -10 187.48 7.20 12 -4 10 183.88 5.80 -12 4 -10 185.08 7.00 14 -4 10 10.10 2.30 14 -4 10 6.90 1.70 -14 -4 -10 8.50 2.60 14 -4 10 11.10 2.00 -14 4 -10 6.90 2.40 -14 4 -10 11.90 2.60 14 4 10 9.50 1.80 -14 4 -10 2.30 2.50 -16 -4 -10 268.97 8.70 16 -4 10 250.27 7.40 16 -4 10 260.77 7.60 -16 4 -10 240.08 8.60 -16 4 -10 248.78 8.30 -16 4 -10 267.17 8.60 16 4 10 262.47 7.50 18 -4 10 55.89 2.90 18 4 10 49.99 2.90 -18 4 -10 53.39 4.20 20 -4 10 36.20 2.40 -20 4 -10 40.40 3.00 20 4 10 38.60 2.30 31 -5 -10 13.00 1.60 31 -5 -10 16.00 1.70 31 5 -10 12.70 1.60 31 5 -10 11.10 1.60 31 5 -10 16.60 1.80 29 -5 -10 44.00 3.00 29 -5 -10 42.30 3.00 29 5 -10 47.70 3.00 29 5 -10 45.20 3.10 29 5 -10 46.20 3.20 27 -5 -10 20.40 2.20 -27 -5 10 28.20 2.90 27 -5 -10 25.20 2.30 -27 5 10 19.10 3.20 27 5 -10 27.40 2.50 27 5 -10 24.40 2.40 27 5 -10 22.90 2.20 25 -5 -10 21.80 2.40 -25 -5 10 27.20 3.10 25 -5 -10 26.30 2.50 25 5 -10 23.60 2.60 25 5 -10 22.00 2.30 -25 5 10 22.20 2.80 25 5 -10 18.70 2.30 -25 5 10 19.40 3.20 -23 -5 10 88.49 4.70 23 -5 -10 93.99 4.50 23 5 -10 86.39 4.20 23 5 -10 91.69 4.10 21 -5 -10 96.49 4.60 -21 -5 10 104.09 4.60 21 5 -10 97.59 4.50 21 5 -10 105.09 4.40 -21 5 10 101.89 4.40 -19 -5 10 3.00 1.60 19 -5 -10 1.20 1.60 -19 5 10 4.80 1.80 19 5 -10 2.60 1.50 19 5 -10 0.90 1.40 19 5 -10 1.30 1.40 -17 -5 10 3.10 1.60 17 -5 -10 6.70 1.80 17 5 -10 4.20 1.50 -17 5 10 4.90 1.60 17 5 -10 6.30 1.50 17 5 -10 5.70 1.50 -15 -5 10 29.70 2.40 -15 -5 10 29.40 2.30 15 -5 -10 37.30 2.90 15 5 -10 36.40 2.60 15 5 -10 31.70 2.20 -15 5 10 33.20 2.60 15 5 -10 30.60 2.30 -13 -5 10 62.99 2.80 13 -5 -10 63.79 3.60 13 5 -10 62.29 2.90 13 5 -10 61.69 2.80 13 5 -10 76.69 5.30 -13 5 10 68.69 3.40 -11 -5 10 146.39 4.60 11 -5 -10 151.48 5.30 11 5 -10 156.78 4.70 11 5 -10 154.18 4.70 11 5 -10 150.98 5.50 -11 5 10 147.99 4.60 -11 5 10 147.79 5.00 9 -5 -10 9.80 1.60 9 -5 -10 10.90 1.90 -9 -5 10 9.60 1.30 9 5 -10 10.30 1.70 9 5 -10 11.20 1.40 -9 5 10 9.30 1.50 -9 5 10 11.60 1.40 9 5 -10 12.50 1.40 9 5 -10 9.60 1.30 7 -5 -10 405.66 10.30 7 -5 -10 386.46 10.40 -7 -5 10 384.16 9.70 -7 5 10 371.86 9.90 7 5 -10 402.46 10.00 7 5 -10 395.76 10.70 7 5 -10 393.46 9.60 -7 5 10 394.86 9.80 7 5 -10 387.26 9.70 5 -5 -10 15.80 2.00 -5 -5 10 14.10 1.30 -5 -5 10 14.20 1.40 5 -5 -10 13.10 1.90 5 5 -10 14.80 1.40 5 5 -10 14.60 1.50 -5 5 10 12.90 1.50 -5 5 10 12.60 1.50 5 5 -10 13.90 1.60 5 5 -10 15.30 1.80 3 -5 -10 47.90 3.10 3 -5 -10 53.69 2.80 -3 -5 10 50.59 2.40 -3 -5 10 49.80 2.30 3 5 -10 52.09 2.50 3 5 -10 52.09 3.10 3 5 -10 52.09 2.40 3 5 -10 56.79 2.70 -3 5 10 49.60 2.40 -1 -5 10 594.54 13.70 1 -5 -10 560.04 14.10 1 -5 -10 558.84 14.80 -1 -5 10 552.54 13.60 1 5 -10 578.94 13.80 -1 5 10 590.14 14.00 1 5 -10 580.64 13.90 1 5 -10 572.54 13.50 -1 5 10 577.64 13.80 1 5 -10 567.54 14.60 -1 -5 -10 164.48 5.50 1 -5 10 173.28 5.00 -1 -5 -10 162.38 6.40 1 -5 10 168.68 5.10 1 5 10 168.98 5.20 -1 5 -10 168.78 4.90 1 5 10 168.88 5.30 -1 5 -10 170.68 5.30 -1 5 -10 171.98 5.30 3 -5 10 16.60 1.70 -3 -5 -10 13.60 2.00 3 5 10 17.00 1.80 -3 5 -10 15.90 1.80 3 5 10 13.80 1.60 -3 5 -10 15.50 1.90 -3 5 -10 14.20 1.80 -5 -5 -10 249.78 8.60 5 -5 10 282.67 7.60 -5 -5 -10 270.37 8.10 5 5 10 276.77 7.70 5 5 10 277.57 7.70 -5 5 -10 286.67 8.00 7 -5 10 150.98 4.90 -7 -5 -10 151.48 5.80 -7 5 -10 145.59 5.50 7 5 10 147.29 5.00 9 -5 10 147.69 5.00 -9 -5 -10 147.29 6.10 -9 5 -10 148.09 6.00 9 5 10 147.19 5.00 11 -5 10 42.20 2.60 -11 -5 -10 36.90 3.50 -11 5 -10 45.10 3.70 -13 -5 -10 155.88 6.40 13 -5 10 115.49 5.60 13 -5 10 130.89 5.30 13 -5 10 144.89 4.90 -13 5 -10 119.89 8.20 13 5 10 152.78 5.70 -13 5 -10 139.59 8.30 -13 5 -10 160.78 8.60 -13 5 -10 144.89 5.80 15 -5 10 54.79 3.20 15 -5 10 49.90 3.20 -15 -5 -10 53.59 4.40 -15 5 -10 51.19 4.40 -15 5 -10 47.90 4.60 15 5 10 48.30 3.20 -15 5 -10 53.49 4.00 17 -5 10 17.00 1.90 17 -5 10 13.90 1.80 17 5 10 15.00 1.80 -17 5 -10 14.90 2.60 -17 5 -10 16.80 2.70 19 -5 10 0.90 1.10 19 5 10 2.10 1.20 -19 5 -10 0.40 1.80 21 -5 10 46.20 2.30 21 5 10 42.50 2.20 -21 5 -10 44.50 3.40 32 -6 -10 10.30 1.40 30 -6 -10 9.50 1.70 30 -6 -10 11.20 1.70 30 6 -10 12.60 1.80 30 6 -10 13.60 1.70 30 6 -10 13.90 1.70 28 -6 -10 111.39 4.50 28 -6 -10 106.89 4.40 28 6 -10 117.59 4.60 28 6 -10 111.89 4.40 28 6 -10 104.09 4.40 26 -6 -10 53.99 3.40 -26 -6 10 51.29 3.90 26 -6 -10 49.90 3.20 26 6 -10 48.60 3.20 -26 6 10 55.59 4.40 26 6 -10 48.90 3.50 26 6 -10 49.80 3.60 24 -6 -10 22.60 2.30 24 -6 -10 25.90 2.70 -24 -6 10 28.50 3.10 24 6 -10 32.70 2.70 24 6 -10 23.80 2.40 24 6 -10 30.70 2.90 24 6 -10 25.10 2.40 -24 6 10 29.40 3.60 22 -6 -10 276.07 8.60 -22 -6 10 296.07 8.80 22 6 -10 280.57 8.60 -22 6 10 289.77 8.70 22 6 -10 285.07 8.30 20 -6 -10 3.60 1.70 -20 -6 10 5.30 2.00 20 6 -10 2.20 1.60 20 6 -10 3.30 1.70 -20 6 10 2.50 1.70 20 6 -10 4.20 1.70 -18 -6 10 22.50 2.40 18 -6 -10 22.40 2.60 18 6 -10 22.50 2.20 18 6 -10 22.00 2.20 -18 6 10 20.00 2.30 18 6 -10 25.40 2.40 16 -6 -10 25.50 2.80 -16 -6 10 22.70 2.20 16 6 -10 17.80 1.90 -16 6 10 21.00 2.40 16 6 -10 21.10 2.20 -14 -6 10 146.79 4.90 14 -6 -10 155.98 5.60 14 6 -10 157.78 5.00 -14 6 10 157.98 5.50 14 6 -10 155.78 5.00 12 -6 -10 434.76 11.60 -12 -6 10 428.46 10.90 12 6 -10 437.36 10.90 12 6 -10 439.06 11.00 -12 6 10 450.15 11.40 10 -6 -10 73.29 3.70 -10 -6 10 70.99 3.00 10 6 -10 71.49 3.20 10 6 -10 71.49 3.70 10 6 -10 69.39 3.00 -10 6 10 67.59 3.00 10 6 -10 74.59 2.90 -10 6 10 71.49 3.30 -8 -6 10 30.50 2.10 8 -6 -10 31.40 2.60 8 6 -10 27.50 2.00 -8 6 10 31.00 2.30 8 6 -10 31.80 1.90 -8 6 10 34.90 2.20 8 6 -10 32.10 2.60 8 6 -10 33.00 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10 486.05 12.30 -1 7 -10 467.25 12.20 -1 7 -10 479.65 12.10 1 7 10 466.95 12.00 -1 7 -10 469.05 11.70 -3 -7 -10 7.30 2.00 3 -7 10 10.80 1.50 3 -7 10 10.00 1.70 -3 7 -10 7.80 1.50 -3 7 -10 7.80 1.60 -3 7 -10 7.00 1.80 3 7 10 10.10 1.80 3 7 10 8.10 1.60 -5 -7 -10 31.00 3.00 5 -7 10 30.20 2.30 5 7 10 29.80 2.40 -5 7 -10 28.10 2.60 -5 7 -10 25.40 2.30 5 7 10 29.60 2.40 -7 -7 -10 14.80 2.30 7 -7 10 10.90 1.80 7 7 10 12.20 1.90 7 7 10 10.70 1.70 -7 7 -10 14.30 2.00 -7 7 -10 9.90 2.10 9 -7 10 52.19 2.90 9 7 10 52.19 3.80 -9 7 -10 48.80 3.60 -11 -7 -10 80.09 5.60 11 -7 10 79.99 3.70 -11 7 -10 80.49 4.50 13 -7 10 2.40 1.50 -13 -7 -10 7.40 2.40 13 -7 10 5.50 1.60 13 -7 10 4.00 1.60 13 7 10 6.30 1.70 -13 7 -10 4.10 2.00 -13 7 -10 7.40 2.60 -13 7 -10 3.70 2.20 -13 7 -10 3.60 2.20 13 7 10 5.70 1.70 15 -7 10 1.40 1.30 15 -7 10 1.60 1.40 -15 7 -10 1.40 2.30 15 7 10 3.50 1.50 -15 7 -10 -1.30 2.00 -15 7 -10 3.10 2.30 15 7 10 2.20 1.40 17 -7 10 93.19 3.70 17 -7 10 93.19 3.90 17 7 10 95.49 3.90 -17 7 -10 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6 -14 71.69 3.50 -16 6 14 69.69 4.00 14 -6 -14 47.90 3.90 -14 -6 14 48.90 3.10 -14 -6 14 51.29 3.10 14 6 -14 56.59 3.20 14 6 -14 47.00 3.20 -14 6 14 48.60 3.70 12 -6 -14 58.59 4.30 -12 -6 14 60.49 3.30 -12 6 14 59.89 3.80 12 6 -14 58.89 3.10 12 6 -14 59.49 3.40 10 -6 -14 30.00 3.10 -10 -6 14 31.60 2.60 -10 6 14 37.30 3.00 -10 6 14 28.30 2.40 10 6 -14 32.10 2.60 10 6 -14 30.40 2.40 8 -6 -14 15.00 2.60 -8 -6 14 15.80 2.10 -8 6 14 22.20 2.60 8 6 -14 15.50 2.00 -8 6 14 13.70 1.90 8 6 -14 19.20 2.80 -6 -6 14 467.05 11.90 6 6 -14 438.86 11.70 6 6 -14 453.95 12.10 -6 6 14 455.75 11.90 -4 -6 14 247.88 7.20 4 -6 -14 223.48 7.80 -4 -6 14 228.08 6.80 4 6 -14 232.68 7.40 -4 6 14 239.18 7.20 4 6 -14 234.78 7.10 -2 -6 14 20.20 2.20 -2 -6 14 21.60 2.20 -2 6 14 25.40 2.40 2 6 -14 16.50 2.20 2 6 -14 21.60 2.60 0 -6 14 81.49 3.80 0 6 -14 73.29 4.30 0 6 -14 82.89 4.00 0 6 14 81.59 4.00 2 -6 14 17.40 2.10 -2 6 -14 11.40 2.10 2 6 14 13.80 2.00 4 -6 14 86.19 4.00 4 6 14 86.79 4.10 -4 6 -14 79.99 4.50 6 -6 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20 8 -14 14.40 2.20 -20 8 14 11.40 2.60 -20 8 14 17.30 2.50 20 8 -14 15.10 2.00 -20 8 14 13.10 2.70 -20 8 14 15.80 3.00 20 8 -14 15.50 2.10 18 -8 -14 20.20 2.50 -18 -8 14 17.00 2.40 18 -8 -14 17.90 2.80 -18 -8 14 16.00 2.10 -18 8 14 18.80 3.00 18 8 -14 19.20 2.30 -18 8 14 21.10 3.00 -18 8 14 18.30 2.60 -18 8 14 15.00 2.70 18 8 -14 15.50 2.10 18 8 -14 19.60 2.30 -16 -8 14 154.68 5.50 16 -8 -14 156.38 6.10 -16 -8 14 149.59 5.50 -16 8 14 154.08 5.90 16 8 -14 148.39 5.50 16 8 -14 149.99 5.50 -14 -8 14 15.60 2.10 14 -8 -14 13.10 2.40 -14 -8 14 12.70 2.00 -14 8 14 13.10 2.40 14 8 -14 16.20 2.10 14 8 -14 14.00 2.10 12 -8 -14 20.10 2.90 -12 -8 14 22.40 2.30 12 8 -14 23.80 2.50 -12 8 14 18.60 2.10 -12 8 14 22.10 2.70 12 8 -14 20.60 2.10 -10 -8 14 28.80 2.50 10 -8 -14 38.00 3.60 10 8 -14 38.70 2.80 10 8 -14 39.20 2.90 -10 8 14 32.30 2.70 -10 8 14 30.70 2.80 8 -8 -14 46.10 4.20 -8 -8 14 48.50 3.30 8 8 -14 48.30 3.30 -8 8 14 46.50 3.20 8 8 -14 43.70 3.20 8 8 -14 44.20 3.00 6 -8 -14 8.20 2.50 -6 -8 14 10.90 2.00 -6 8 14 11.90 2.00 6 8 -14 8.30 1.80 6 8 -14 9.90 1.80 6 8 -14 9.50 2.10 -4 -8 14 198.28 6.40 4 -8 -14 194.28 7.30 -4 8 14 198.18 6.40 4 8 -14 190.58 6.00 4 8 -14 191.08 6.40 4 8 -14 201.58 6.90 2 -8 -14 0.90 2.20 -2 -8 14 1.70 1.40 -2 -8 14 1.10 1.50 2 8 -14 2.70 2.00 2 8 -14 2.90 1.60 -2 8 14 1.30 1.60 0 -8 14 41.50 3.00 0 -8 -14 32.70 3.40 0 -8 14 48.30 3.10 0 8 -14 47.60 3.70 0 8 -14 41.50 3.20 0 8 14 44.90 3.30 2 -8 14 11.80 1.80 2 -8 14 11.90 2.90 2 8 14 11.10 2.90 -2 8 -14 9.50 2.10 2 8 14 9.20 2.70 -2 8 -14 10.50 3.10 2 8 14 10.40 1.90 -2 8 -14 12.10 3.90 -2 8 -14 7.90 3.40 2 8 14 7.90 2.80 -2 8 -14 12.70 3.40 4 -8 14 -0.20 1.30 4 -8 14 0.00 1.60 4 8 14 1.10 1.80 4 8 14 0.60 1.60 4 8 14 0.80 1.70 4 8 14 -1.70 1.50 -4 8 -14 0.40 1.80 -4 8 -14 1.10 2.00 -4 8 -14 -0.90 2.10 -4 8 -14 1.10 1.90 6 -8 14 102.49 4.50 6 -8 14 93.19 4.00 6 8 14 98.79 4.30 -6 8 -14 103.19 5.80 6 8 14 94.29 4.50 6 8 14 95.29 4.80 -6 8 -14 97.39 4.80 -6 8 -14 94.99 4.90 -6 8 -14 97.19 5.30 6 8 14 92.39 4.30 8 -8 14 -0.50 1.50 8 -8 14 2.20 1.40 -8 8 -14 0.80 1.90 -8 8 -14 0.20 2.10 8 8 14 -0.10 1.40 8 8 14 -0.40 1.40 8 8 14 -2.30 1.80 -8 8 -14 -1.20 2.20 10 -8 14 13.00 1.80 10 -8 14 12.60 2.00 -10 8 -14 10.00 2.30 10 8 14 9.10 1.70 10 8 14 14.40 1.90 -10 8 -14 9.70 2.50 -10 8 -14 11.20 2.20 12 -8 14 41.80 2.70 12 -8 14 43.70 2.50 -12 8 -14 45.50 4.10 -12 8 -14 40.20 3.30 12 8 14 39.40 2.60 27 -9 -14 114.39 4.20 27 -9 -14 116.69 4.20 27 9 -14 110.69 4.20 27 9 -14 113.19 4.40 -27 9 14 120.09 5.10 25 -9 -14 48.00 3.30 25 -9 -14 51.89 3.10 25 9 -14 45.60 3.40 -25 9 14 48.60 4.40 25 9 -14 43.50 3.50 23 -9 -14 3.40 1.80 23 -9 -14 6.70 1.90 -23 9 14 7.00 2.60 23 9 -14 7.30 2.00 -23 9 14 7.90 2.30 23 9 -14 7.70 1.90 -23 9 14 5.60 2.60 21 -9 -14 23.40 2.40 21 -9 -14 23.20 2.40 -21 -9 14 24.20 2.80 -21 9 14 26.10 3.30 -21 9 14 25.70 3.00 21 9 -14 26.70 2.70 21 9 -14 22.70 2.30 21 9 -14 32.00 2.70 -21 9 14 26.40 3.40 -21 9 14 22.40 2.60 19 -9 -14 7.30 2.20 -19 -9 14 5.10 2.10 -19 9 14 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-5 -21 0.60 1.90 -13 -5 21 2.20 1.60 13 5 -21 1.10 2.00 -13 5 21 3.80 1.90 -13 5 21 3.10 1.60 -11 -5 21 185.58 5.80 -11 -5 21 193.38 6.40 11 -5 -21 187.88 6.60 11 5 -21 188.78 6.70 -11 5 21 183.38 6.50 -11 5 21 186.38 6.50 -11 5 21 196.58 6.20 9 -5 -21 81.19 4.50 -9 -5 21 79.59 3.60 -9 -5 21 81.09 4.10 9 5 -21 75.99 4.50 -9 5 21 82.69 4.40 -9 5 21 81.09 4.10 -7 -5 21 29.60 2.50 -7 -5 21 23.30 2.20 -7 5 21 23.60 2.70 -7 5 21 32.90 3.60 -7 5 21 29.50 2.50 7 5 -21 29.30 3.00 -5 -5 21 63.39 3.40 -5 -5 21 64.89 3.20 -5 5 21 64.59 3.30 5 5 -21 61.69 4.10 -5 5 21 62.29 3.40 -3 -5 21 10.00 1.50 -3 5 21 5.00 1.50 -3 5 21 6.20 1.50 -1 -5 21 18.00 1.60 -1 5 21 21.10 1.90 -1 5 21 18.50 1.60 -20 -6 21 41.30 2.70 20 -6 -21 34.20 3.20 -20 6 21 30.50 2.50 18 -6 -21 -0.40 1.60 -18 -6 21 0.60 1.40 18 6 -21 0.20 1.50 -18 6 21 -0.80 1.80 -16 -6 21 26.20 2.40 16 -6 -21 23.30 2.40 -16 6 21 24.10 2.10 16 6 -21 23.90 2.40 -16 6 21 29.10 2.70 14 -6 -21 -0.30 1.80 -14 -6 21 1.40 1.50 14 6 -21 1.00 1.80 -14 6 21 -0.50 1.80 -14 6 21 -0.60 1.40 -12 -6 21 10.40 1.90 12 -6 -21 8.50 2.20 -12 6 21 11.10 1.90 -12 6 21 10.60 2.10 -12 6 21 9.90 2.00 12 6 -21 8.50 2.20 10 -6 -21 40.60 3.80 -10 -6 21 41.60 3.30 -10 -6 21 41.50 2.80 -10 6 21 43.50 3.50 -10 6 21 42.10 3.50 -10 6 21 47.80 3.40 10 6 -21 34.70 3.10 -8 -6 21 17.80 2.10 8 -6 -21 19.00 2.40 -8 -6 21 22.40 1.90 8 6 -21 22.40 2.60 -8 6 21 16.50 2.20 -8 6 21 17.20 2.00 -6 -6 21 13.50 1.90 6 -6 -21 15.00 2.30 -6 -6 21 15.30 1.70 -6 6 21 10.60 1.80 -6 6 21 15.50 1.80 -6 6 21 14.90 2.00 6 6 -21 14.90 2.40 -4 -6 21 28.80 2.30 -4 -6 21 30.80 2.60 4 6 -21 35.80 3.10 -4 6 21 30.10 2.60 -4 6 21 30.10 2.60 19 -7 -21 3.40 1.60 -19 -7 21 6.90 1.50 -19 7 21 2.80 1.70 17 -7 -21 17.80 2.20 -17 -7 21 19.00 2.00 -17 7 21 15.90 1.80 -17 7 21 14.10 2.20 17 7 -21 17.70 2.00 15 -7 -21 24.90 2.40 -15 -7 21 24.20 2.20 15 7 -21 20.60 2.30 -15 7 21 30.20 2.70 -15 7 21 26.10 2.20 -13 -7 21 6.70 1.70 13 -7 -21 4.70 1.90 -13 7 21 7.50 2.00 13 7 -21 8.60 2.10 -13 7 21 10.20 1.80 11 -7 -21 55.89 3.90 -11 -7 21 55.89 3.50 11 7 -21 53.59 4.00 -11 7 21 56.39 3.60 -11 7 21 56.49 3.30 -11 7 21 54.09 3.60 -9 -7 21 47.90 3.30 9 -7 -21 44.80 3.90 -9 -7 21 46.70 2.60 -9 7 21 48.30 3.30 -9 7 21 50.29 3.40 9 7 -21 46.30 3.70 -7 -7 21 2.00 1.20 7 -7 -21 0.10 1.80 -7 -7 21 0.90 1.40 -7 7 21 3.00 1.40 -7 7 21 1.10 1.50 -7 7 21 3.50 1.60 7 7 -21 4.90 2.00 -5 -7 21 23.50 1.90 -5 -7 21 20.50 1.90 5 -7 -21 19.70 2.30 5 7 -21 22.80 2.40 -5 7 21 20.40 1.90 -5 7 21 19.30 2.00 -5 7 21 17.70 1.80 16 -8 -21 68.99 3.80 -16 -8 21 67.09 3.40 -16 8 21 71.79 3.90 -16 8 21 63.39 3.30 16 8 -21 67.09 3.40 -14 -8 21 6.60 1.60 14 -8 -21 6.70 1.90 14 8 -21 5.50 1.80 -14 8 21 3.80 1.50 -14 8 21 5.10 1.80 -12 -8 21 1.80 1.50 12 -8 -21 1.00 1.80 12 8 -21 3.80 1.80 -12 8 21 4.30 1.70 -12 8 21 3.50 1.50 -12 8 21 3.80 1.60 -10 -8 21 69.19 3.00 -10 -8 21 76.79 3.70 10 -8 -21 75.29 4.10 10 8 -21 73.59 4.20 -10 8 21 73.09 3.80 -10 8 21 72.69 3.50 -8 -8 21 5.30 1.60 8 -8 -21 3.40 1.80 -8 -8 21 5.30 1.30 -8 8 21 5.80 1.40 -8 8 21 8.50 1.70 8 8 -21 7.30 2.10 -8 8 21 4.20 1.70 -6 -8 21 0.20 1.10 6 -8 -21 1.30 1.80 -6 -8 21 -0.40 1.30 -6 8 21 -0.40 1.40 -6 8 21 3.20 1.40 6 8 -21 1.70 1.60 -6 8 21 -1.00 1.20 13 -9 -21 25.30 2.40 -13 -9 21 23.10 2.00 -13 9 21 21.20 2.10 -13 9 21 25.20 2.10 13 9 -21 20.20 2.10 11 -9 -21 38.50 3.50 -11 -9 21 34.70 2.90 11 9 -21 39.40 3.10 -11 9 21 33.80 2.90 -11 9 21 40.90 3.10 20 0 -22 53.09 3.10 -20 0 22 55.39 3.30 18 0 -22 18.10 2.10 -18 0 22 16.30 2.00 -16 0 22 60.29 3.60 -14 0 22 14.70 2.10 -14 0 22 12.40 1.80 -12 0 22 38.20 3.00 -12 0 22 43.50 3.30 -10 0 22 77.89 3.80 -10 0 22 83.59 3.70 -8 0 22 57.59 3.20 -8 0 22 61.29 3.20 -6 0 22 8.10 1.50 -4 0 22 124.79 4.30 21 -1 -22 5.90 1.50 -21 -1 22 8.20 1.60 -21 1 22 6.20 1.60 21 1 -22 7.30 1.50 19 -1 -22 -0.30 1.40 -19 -1 22 -0.60 1.40 -19 1 22 -1.50 1.50 17 -1 -22 1.20 1.60 -17 -1 22 3.00 1.60 -17 1 22 1.10 1.60 -15 -1 22 3.10 1.70 -15 1 22 2.40 1.50 -15 1 22 2.70 1.60 -13 -1 22 17.20 2.10 -13 -1 22 18.40 2.00 -13 1 22 19.40 2.20 -13 1 22 20.50 2.10 -11 -1 22 0.10 1.50 -11 -1 22 0.40 1.40 -11 1 22 0.40 1.40 -11 1 22 0.40 1.50 -9 -1 22 1.20 1.40 -9 -1 22 1.00 1.50 -9 1 22 0.80 1.40 -9 1 22 2.00 1.40 -7 -1 22 -1.30 1.10 -7 -1 22 0.10 1.30 -7 1 22 -1.10 1.30 -5 -1 22 6.50 1.30 -5 1 22 8.60 1.60 -3 -1 22 1.30 1.20 -3 1 22 0.40 1.00 -3 1 22 0.30 1.20 -20 -2 22 66.09 3.40 20 -2 -22 65.69 3.50 -20 2 22 67.59 3.60 18 -2 -22 -1.80 1.50 -18 -2 22 -1.00 1.40 -18 2 22 -1.70 1.60 16 -2 -22 5.60 1.80 -16 -2 22 6.00 1.80 -16 2 22 5.60 1.90 14 -2 -22 171.68 7.10 -14 -2 22 165.78 5.80 -14 2 22 172.28 5.50 -14 2 22 168.18 5.90 -12 -2 22 10.80 2.00 -12 -2 22 10.30 1.70 -12 2 22 12.30 2.00 -12 2 22 11.30 1.80 -10 -2 22 7.90 1.80 -10 -2 22 5.30 1.50 -10 2 22 6.50 1.60 -10 2 22 6.40 1.70 -8 -2 22 57.39 3.20 -8 -2 22 59.59 3.30 -8 2 22 59.69 3.20 -8 2 22 68.49 5.10 -6 -2 22 -1.00 1.30 -6 -2 22 -0.20 1.20 -6 2 22 -1.30 1.20 -4 -2 22 50.39 2.80 -4 2 22 47.10 2.80 -4 2 22 45.30 2.60 19 -3 -22 12.60 1.90 -19 -3 22 9.30 1.70 -19 3 22 12.00 2.00 -17 -3 22 0.80 1.40 17 -3 -22 -0.80 1.50 -17 3 22 1.10 1.70 15 -3 -22 26.90 2.50 -15 -3 22 26.50 2.50 -15 3 22 23.40 2.10 -15 3 22 30.00 2.70 -13 -3 22 9.60 1.80 13 -3 -22 8.10 1.90 -13 -3 22 12.70 1.80 -13 3 22 13.90 1.90 -13 3 22 9.40 2.00 -11 -3 22 12.60 1.70 -11 -3 22 12.30 1.80 -11 3 22 14.10 2.10 11 3 -22 16.40 2.40 -11 3 22 13.40 1.80 -9 -3 22 3.90 1.50 -9 -3 22 3.30 1.40 9 3 -22 3.80 2.00 -9 3 22 3.70 1.60 -9 3 22 4.40 1.50 -7 -3 22 -1.10 1.20 -7 -3 22 0.40 1.30 -7 3 22 -0.50 1.20 -5 -3 22 4.00 1.30 -5 3 22 0.80 1.30 -5 3 22 2.40 1.40 18 -4 -22 6.60 1.70 -18 -4 22 7.00 1.60 -18 4 22 7.80 1.90 16 -4 -22 23.40 2.30 -16 -4 22 19.80 2.10 -16 4 22 20.80 1.90 -16 4 22 23.50 2.50 -14 -4 22 138.09 5.10 14 -4 -22 140.09 5.20 -14 4 22 137.89 4.80 14 4 -22 145.89 5.40 -14 4 22 142.79 5.30 12 -4 -22 22.10 2.20 -12 -4 22 26.70 2.30 -12 -4 22 22.40 1.90 -12 4 22 24.90 2.20 12 4 -22 25.10 2.60 -12 4 22 23.90 2.30 -10 -4 22 3.50 1.40 -10 -4 22 2.00 1.50 10 4 -22 2.80 1.90 -10 4 22 -1.70 1.30 -10 4 22 1.60 1.60 -8 -4 22 62.39 3.10 -8 -4 22 58.29 3.20 8 4 -22 52.39 3.80 -8 4 22 53.39 3.20 -6 -4 22 5.40 1.40 -6 -4 22 6.80 1.30 -6 4 22 1.50 1.30 6 4 -22 1.30 1.70 -17 -5 22 5.00 1.50 17 -5 -22 3.70 1.60 -17 5 22 4.60 1.50 -17 5 22 5.50 1.80 -15 -5 22 13.10 1.80 15 -5 -22 18.40 2.00 -15 5 22 17.50 1.80 15 5 -22 20.50 2.20 -15 5 22 17.20 2.20 13 -5 -22 16.30 2.10 -13 -5 22 13.00 1.80 13 5 -22 16.40 2.20 -13 5 22 15.00 2.10 -13 5 22 15.80 1.80 -11 -5 22 2.40 1.20 11 -5 -22 1.00 1.50 -11 -5 22 0.60 1.40 -11 5 22 3.70 1.50 11 5 -22 5.80 1.90 -11 5 22 3.30 1.70 -9 -5 22 28.40 2.20 -9 -5 22 21.30 2.00 9 5 -22 26.90 2.50 -9 5 22 25.60 2.20 -7 -5 22 3.40 1.20 -7 -5 22 2.90 1.30 7 5 -22 0.90 1.70 -7 5 22 -1.10 1.30 -16 -6 22 68.89 3.30 16 -6 -22 66.69 3.60 -16 6 22 64.19 3.10 -16 6 22 61.49 3.60 -14 -6 22 18.70 1.90 14 -6 -22 19.40 2.10 -14 6 22 24.70 2.00 -14 6 22 26.40 2.30 14 6 -22 26.10 2.40 -12 -6 22 24.10 2.20 12 -6 -22 19.60 2.10 -12 6 22 27.10 2.30 12 6 -22 24.90 2.40 -12 6 22 30.20 2.60 10 -6 -22 54.09 3.50 -10 -6 22 60.69 2.80 -10 -6 22 63.99 3.20 10 6 -22 62.59 3.70 -10 6 22 62.39 3.20 -14 0 23 -1.10 1.30 -14 0 23 0.60 1.20 -12 0 23 2.20 1.40 -12 0 23 2.70 1.30 -10 0 23 -1.50 1.20 -15 -1 23 37.60 2.80 -15 1 23 31.40 2.40 -15 1 23 36.60 3.10 -13 -1 23 101.69 4.10 -13 -1 23 89.19 3.50 -13 1 23 97.79 3.60 -13 1 23 97.29 4.20 -11 -1 23 55.39 3.20 -11 -1 23 55.29 3.00 -11 1 23 62.29 3.30 -11 1 23 58.49 3.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30681 #===END data_Cpx_5j _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common 'Cpx_5j' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H75 F3 N O6 P Pd S' _chemical_formula_weight 1024.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0843(4) _cell_length_b 17.9837(5) _cell_length_c 19.7605(5) _cell_angle_alpha 90 _cell_angle_beta 108.1210(10) _cell_angle_gamma 90 _cell_volume 5094.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 3.245 _cell_measurement_theta_max 66.555 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_F_000 2160 _exptl_transmission_factor_min 0.685 _exptl_transmission_factor_max 1 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 4.097 _shelx_estimated_absorpt_T_min 0.495 _shelx_estimated_absorpt_T_max 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type CPAD _diffrn_measurement_method 'Mixed Phi and Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 88200 _diffrn_reflns_av_unetI/netI 0.0693 _diffrn_reflns_av_R_equivalents 0.1178 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.245 _diffrn_reflns_theta_max 66.661 _diffrn_reflns_theta_full 66.661 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 8991 _reflns_number_gt 7189 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4349P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8991 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.55938(2) 0.29803(2) 0.22583(2) 0.02439(12) Uani 1 1 d . . . . . P1 P 0.43529(6) 0.29125(5) 0.27306(4) 0.0240(2) Uani 1 1 d . . . . . O1 O 0.24439(17) 0.23166(16) 0.27555(14) 0.0336(6) Uani 1 1 d . . . . . O2 O 0.49652(18) 0.39079(16) 0.47542(14) 0.0371(6) Uani 1 1 d . . . . . O3 O 0.33859(19) 0.40543(18) 0.43045(16) 0.0427(7) Uani 1 1 d . . . . . N1 N 0.6767(2) 0.30613(19) 0.18682(19) 0.0336(7) Uani 1 1 d . . . . . C1 C 0.3471(2) 0.23564(18) 0.20699(18) 0.0248(7) Uani 1 1 d . . . . . C2 C 0.2597(3) 0.21441(19) 0.21303(19) 0.0267(7) Uani 1 1 d . . . . . C3 C 0.1514(3) 0.2262(3) 0.2796(3) 0.0433(10) Uani 1 1 d . . . . . H3A H 0.109092 0.255820 0.241488 0.065 Uiso 1 1 calc R U . . . H3B H 0.150019 0.244834 0.325886 0.065 Uiso 1 1 calc R U . . . H3C H 0.131414 0.174037 0.274297 0.065 Uiso 1 1 calc R U . . . C4 C 0.1929(2) 0.1759(2) 0.15920(19) 0.0290(7) Uani 1 1 d . . . . . H4 H 0.134227 0.163341 0.164362 0.035 Uiso 1 1 calc R U . . . C5 C 0.2143(3) 0.1566(2) 0.0983(2) 0.0322(8) Uani 1 1 d . . . . . H5 H 0.169954 0.130424 0.061215 0.039 Uiso 1 1 calc R U . . . C6 C 0.2997(3) 0.1753(2) 0.09123(19) 0.0300(7) Uani 1 1 d . . . . . H6 H 0.313531 0.161224 0.049274 0.036 Uiso 1 1 calc R U . . . C7 C 0.3664(2) 0.21447(19) 0.14454(19) 0.0253(7) Uani 1 1 d . . . . . C8 C 0.4568(2) 0.2259(2) 0.12853(18) 0.0263(7) Uani 1 1 d . . . . . C9 C 0.4582(2) 0.2758(2) 0.07252(19) 0.0284(7) Uani 1 1 d . . . . . C10 C 0.3895(3) 0.3401(2) 0.0501(2) 0.0312(8) Uani 1 1 d . . . . . H10 H 0.350889 0.340990 0.083027 0.037 Uiso 1 1 calc R U . . . C11 C 0.4409(3) 0.4152(2) 0.0573(2) 0.0414(9) Uani 1 1 d . . . . . H11A H 0.476179 0.417208 0.023225 0.062 Uiso 1 1 calc R U . . . H11B H 0.483812 0.420363 0.105784 0.062 Uiso 1 1 calc R U . . . H11C H 0.395322 0.455825 0.047415 0.062 Uiso 1 1 calc R U . . . C12 C 0.3233(3) 0.3314(2) -0.0257(2) 0.0405(9) Uani 1 1 d . . . . . H12A H 0.359532 0.328503 -0.059041 0.061 Uiso 1 1 calc R U . . . H12B H 0.281227 0.374266 -0.037672 0.061 Uiso 1 1 calc R U . . . H12C H 0.286674 0.285766 -0.028883 0.061 Uiso 1 1 calc R U . . . C13 C 0.5209(3) 0.2630(2) 0.03498(19) 0.0301(7) Uani 1 1 d . . . . . H13 H 0.521695 0.296408 -0.002084 0.036 Uiso 1 1 calc R U . . . C14 C 0.5827(3) 0.2029(2) 0.0498(2) 0.0306(8) Uani 1 1 d . . . . . C15 C 0.6438(3) 0.1854(2) 0.0034(2) 0.0351(8) Uani 1 1 d . . . . . H15 H 0.686969 0.144384 0.027308 0.042 Uiso 1 1 calc R U . . . C16 C 0.7039(3) 0.2502(3) -0.0046(3) 0.0481(11) Uani 1 1 d . . . . . H16A H 0.663836 0.291264 -0.028939 0.072 Uiso 1 1 calc R U . . . H16B H 0.744117 0.234654 -0.032512 0.072 Uiso 1 1 calc R U . . . H16C H 0.742581 0.266755 0.042649 0.072 Uiso 1 1 calc R U . . . C17 C 0.5843(3) 0.1560(2) -0.0694(2) 0.0393(9) Uani 1 1 d . . . . . H17A H 0.544406 0.196056 -0.096066 0.059 Uiso 1 1 calc R U . . . H17B H 0.545334 0.114874 -0.062684 0.059 Uiso 1 1 calc R U . . . H17C H 0.625197 0.138393 -0.096103 0.059 Uiso 1 1 calc R U . . . C18 C 0.5848(2) 0.1579(2) 0.10718(19) 0.0292(7) Uani 1 1 d . . . . . H18 H 0.629632 0.119097 0.120042 0.035 Uiso 1 1 calc R U . . . C19 C 0.5236(2) 0.1675(2) 0.14676(18) 0.0263(7) Uani 1 1 d . . . . . C20 C 0.5244(3) 0.1101(2) 0.2041(2) 0.0318(8) Uani 1 1 d . . . . . H20 H 0.480106 0.127511 0.229226 0.038 Uiso 1 1 calc R U . . . C21 C 0.6211(3) 0.1039(2) 0.2594(2) 0.0367(8) Uani 1 1 d . . . . . H21A H 0.617868 0.070820 0.297983 0.055 Uiso 1 1 calc R U . . . H21B H 0.642007 0.153279 0.278806 0.055 Uiso 1 1 calc R U . . . H21C H 0.665255 0.083617 0.236838 0.055 Uiso 1 1 calc R U . . . C22 C 0.4909(3) 0.0343(2) 0.1717(2) 0.0400(9) Uani 1 1 d . . . . . H22A H 0.532526 0.016124 0.145919 0.060 Uiso 1 1 calc R U . . . H22B H 0.427398 0.038827 0.138704 0.060 Uiso 1 1 calc R U . . . H22C H 0.491108 -0.000816 0.209694 0.060 Uiso 1 1 calc R U . . . C23 C 0.3812(2) 0.3856(2) 0.2775(2) 0.0304(7) Uani 1 1 d . . . . . C24 C 0.4006(3) 0.4320(2) 0.2180(2) 0.0325(8) Uani 1 1 d . . . . . H24A H 0.468804 0.433709 0.226536 0.039 Uiso 1 1 calc R U . . . H24B H 0.372146 0.406466 0.171914 0.039 Uiso 1 1 calc R U . . . C25 C 0.3636(3) 0.5118(2) 0.2118(2) 0.0408(9) Uani 1 1 d . . . . . H25A H 0.396350 0.539771 0.255584 0.049 Uiso 1 1 calc R U . . . H25B H 0.375823 0.536889 0.170997 0.049 Uiso 1 1 calc R U . . . C26 C 0.2588(3) 0.5116(2) 0.2011(3) 0.0506(11) Uani 1 1 d . . . . . H26A H 0.236636 0.563447 0.201350 0.061 Uiso 1 1 calc R U . . . H26B H 0.225381 0.489440 0.154268 0.061 Uiso 1 1 calc R U . . . C27 C 0.2369(3) 0.4678(3) 0.2594(3) 0.0484(11) Uani 1 1 d . . . . . H27A H 0.168470 0.466038 0.249712 0.058 Uiso 1 1 calc R U . . . H27B H 0.264569 0.493290 0.305556 0.058 Uiso 1 1 calc R U . . . C28 C 0.2750(3) 0.3883(2) 0.2644(2) 0.0358(8) Uani 1 1 d . . . . . H28A H 0.243060 0.361582 0.219664 0.043 Uiso 1 1 calc R U . . . H28B H 0.260462 0.362037 0.303762 0.043 Uiso 1 1 calc R U . . . C29 C 0.4361(3) 0.4152(2) 0.3524(2) 0.0321(8) Uani 1 1 d . . . . . H29A H 0.503623 0.411947 0.358267 0.038 Uiso 1 1 calc R U . . . H29B H 0.420720 0.468426 0.354948 0.038 Uiso 1 1 calc R U . . . C30 C 0.4178(3) 0.3749(2) 0.4144(2) 0.0335(8) Uani 1 1 d . . . . . C31 C 0.4614(3) 0.3988(2) 0.5348(2) 0.0398(9) Uani 1 1 d . . . . . H31A H 0.503283 0.429862 0.572807 0.048 Uiso 1 1 calc R U . . . H31B H 0.452536 0.349941 0.554768 0.048 Uiso 1 1 calc R U . . . C32 C 0.3693(3) 0.4372(2) 0.5001(2) 0.0428(9) Uani 1 1 d . . . . . H32A H 0.324333 0.426832 0.526301 0.051 Uiso 1 1 calc R U . . . H32B H 0.377587 0.491624 0.497847 0.051 Uiso 1 1 calc R U . . . C33 C 0.3997(3) 0.2914(2) 0.4042(2) 0.0329(8) Uani 1 1 d . . . . . H33A H 0.333035 0.284133 0.377114 0.039 Uiso 1 1 calc R U . . . H33B H 0.410457 0.268690 0.451712 0.039 Uiso 1 1 calc R U . . . C34 C 0.4583(3) 0.2486(2) 0.36588(18) 0.0286(7) Uani 1 1 d . . . . . C35 C 0.5639(3) 0.2537(2) 0.4084(2) 0.0314(8) Uani 1 1 d . . . . . H35A H 0.600592 0.230514 0.380342 0.038 Uiso 1 1 calc R U . . . H35B H 0.582272 0.306612 0.415889 0.038 Uiso 1 1 calc R U . . . C36 C 0.5866(3) 0.2147(2) 0.4810(2) 0.0382(9) Uani 1 1 d . . . . . H36A H 0.654370 0.218799 0.506048 0.046 Uiso 1 1 calc R U . . . H36B H 0.553124 0.239949 0.510280 0.046 Uiso 1 1 calc R U . . . C37 C 0.5590(3) 0.1326(3) 0.4731(2) 0.0416(9) Uani 1 1 d . . . . . H37A H 0.597539 0.105943 0.448556 0.050 Uiso 1 1 calc R U . . . H37B H 0.570839 0.110204 0.520889 0.050 Uiso 1 1 calc R U . . . C38 C 0.4562(3) 0.1242(2) 0.4307(2) 0.0380(9) Uani 1 1 d . . . . . H38A H 0.417511 0.144768 0.458635 0.046 Uiso 1 1 calc R U . . . H38B H 0.440928 0.070806 0.422341 0.046 Uiso 1 1 calc R U . . . C39 C 0.4328(3) 0.1648(2) 0.3589(2) 0.0331(8) Uani 1 1 d . . . . . H39A H 0.365145 0.159739 0.333856 0.040 Uiso 1 1 calc R U . . . H39B H 0.466606 0.140440 0.329318 0.040 Uiso 1 1 calc R U . . . C40 C 0.6478(2) 0.3557(2) 0.30654(18) 0.0279(7) Uani 1 1 d . . . . . C41 C 0.6479(2) 0.4330(2) 0.31548(19) 0.0284(7) Uani 1 1 d . . . . . H41 H 0.597953 0.461681 0.285813 0.034 Uiso 1 1 calc R U . . . C42 C 0.7200(3) 0.4685(2) 0.3672(2) 0.0307(7) Uani 1 1 d . . . . . H42 H 0.717716 0.520891 0.372530 0.037 Uiso 1 1 calc R U . . . C43 C 0.7951(2) 0.4291(2) 0.41121(19) 0.0294(7) Uani 1 1 d . . . . . C44 C 0.8714(3) 0.4668(2) 0.4699(2) 0.0360(8) Uani 1 1 d . . . . . H44A H 0.917658 0.429674 0.494799 0.054 Uiso 1 1 calc R U . . . H44B H 0.844267 0.490219 0.503599 0.054 Uiso 1 1 calc R U . . . H44C H 0.901718 0.504728 0.449068 0.054 Uiso 1 1 calc R U . . . C45 C 0.7976(3) 0.3528(2) 0.40054(19) 0.0306(7) Uani 1 1 d . . . . . H45 H 0.849417 0.324691 0.428375 0.037 Uiso 1 1 calc R U . . . C46 C 0.7246(3) 0.3169(2) 0.34930(19) 0.0292(7) Uani 1 1 d . . . . . H46 H 0.727619 0.264602 0.343596 0.035 Uiso 1 1 calc R U . . . C47 C 0.6937(3) 0.3757(2) 0.1532(2) 0.0399(9) Uani 1 1 d . . . . . H47A H 0.677125 0.418567 0.178354 0.048 Uiso 1 1 calc R U . . . H47B H 0.652716 0.377030 0.103161 0.048 Uiso 1 1 calc R U . . . C48 C 0.7943(3) 0.3834(3) 0.1546(3) 0.0453(10) Uani 1 1 d . . . . . H48A H 0.831978 0.399744 0.202873 0.054 Uiso 1 1 calc R U . . . H48B H 0.817422 0.333810 0.146350 0.054 Uiso 1 1 calc R U . . . C49 C 0.8107(4) 0.4369(3) 0.1011(3) 0.0549(12) Uani 1 1 d . . . . . H49A H 0.791032 0.487394 0.110448 0.066 Uiso 1 1 calc R U . . . H49B H 0.772212 0.421991 0.052681 0.066 Uiso 1 1 calc R U . . . C50 C 0.9131(4) 0.4386(3) 0.1048(4) 0.0665(15) Uani 1 1 d . . . . . H50A H 0.950018 0.461677 0.149560 0.100 Uiso 1 1 calc R U . . . H50B H 0.919982 0.467389 0.064602 0.100 Uiso 1 1 calc R U . . . H50C H 0.935136 0.387641 0.102411 0.100 Uiso 1 1 calc R U . . . S1 S 0.39784(7) 0.33471(6) 0.69880(6) 0.0421(2) Uani 1 1 d . . . . . F1 F 0.3623(3) 0.2924(3) 0.8132(2) 0.1001(16) Uani 1 1 d . . . . . F2 F 0.3699(2) 0.4108(2) 0.80332(18) 0.0779(10) Uani 1 1 d . . . . . F3 F 0.4948(2) 0.34599(19) 0.83504(15) 0.0609(7) Uani 1 1 d . . . . . O4 O 0.2993(2) 0.33652(19) 0.66370(18) 0.0504(7) Uani 1 1 d . . . . . O5 O 0.4409(3) 0.2650(2) 0.6971(3) 0.0712(11) Uani 1 1 d . . . . . O6 O 0.4483(2) 0.3971(2) 0.68542(17) 0.0543(8) Uani 1 1 d . . . . . C51 C 0.4077(3) 0.3474(3) 0.7922(3) 0.0511(12) Uani 1 1 d . . . . . H1N H 0.728(4) 0.298(3) 0.227(3) 0.039(12) Uiso 1 1 d . . . . . H2N H 0.688(4) 0.261(4) 0.156(3) 0.059(15) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02161(16) 0.02858(16) 0.02420(16) -0.00341(9) 0.00889(11) -0.00128(9) P1 0.0221(4) 0.0265(4) 0.0255(4) -0.0046(3) 0.0105(4) -0.0021(3) O1 0.0254(13) 0.0458(15) 0.0345(14) -0.0132(11) 0.0166(11) -0.0091(11) O2 0.0314(13) 0.0508(15) 0.0316(13) -0.0163(12) 0.0134(11) -0.0090(11) O3 0.0323(14) 0.0592(18) 0.0423(15) -0.0202(13) 0.0199(12) -0.0007(12) N1 0.0296(17) 0.0397(17) 0.0339(18) -0.0030(14) 0.0136(15) -0.0061(13) C1 0.0219(16) 0.0260(16) 0.0271(17) -0.0023(13) 0.0085(13) -0.0012(13) C2 0.0264(17) 0.0282(16) 0.0277(17) -0.0020(14) 0.0114(14) 0.0004(13) C3 0.032(2) 0.054(2) 0.052(3) -0.017(2) 0.0254(19) -0.0147(18) C4 0.0232(17) 0.0326(17) 0.0297(18) 0.0009(15) 0.0060(14) -0.0030(14) C5 0.0289(18) 0.0368(19) 0.0282(18) -0.0029(15) 0.0049(14) -0.0025(14) C6 0.0286(18) 0.0366(18) 0.0254(17) -0.0055(15) 0.0093(14) -0.0019(15) C7 0.0219(16) 0.0287(16) 0.0248(17) 0.0000(13) 0.0065(13) 0.0014(13) C8 0.0235(16) 0.0306(16) 0.0258(17) -0.0059(14) 0.0093(13) -0.0014(13) C9 0.0250(17) 0.0323(17) 0.0275(17) -0.0032(14) 0.0074(14) -0.0029(14) C10 0.0285(18) 0.0341(18) 0.0326(19) 0.0011(15) 0.0119(15) 0.0018(14) C11 0.046(2) 0.0331(19) 0.049(2) 0.0061(17) 0.0200(19) 0.0011(17) C12 0.039(2) 0.045(2) 0.036(2) 0.0035(17) 0.0094(17) 0.0061(17) C13 0.0317(18) 0.0327(18) 0.0275(17) 0.0002(15) 0.0114(14) -0.0041(14) C14 0.0286(18) 0.0358(19) 0.0282(18) -0.0045(15) 0.0098(15) -0.0023(14) C15 0.035(2) 0.043(2) 0.0315(19) -0.0001(16) 0.0157(16) 0.0049(16) C16 0.043(2) 0.061(3) 0.050(3) -0.011(2) 0.030(2) -0.010(2) C17 0.050(2) 0.041(2) 0.033(2) -0.0019(17) 0.0210(18) 0.0005(17) C18 0.0245(17) 0.0352(18) 0.0278(18) -0.0045(15) 0.0082(14) -0.0001(14) C19 0.0236(16) 0.0319(17) 0.0244(16) -0.0057(14) 0.0090(13) -0.0019(13) C20 0.0355(19) 0.0349(19) 0.0293(17) -0.0019(15) 0.0163(15) 0.0040(15) C21 0.0324(19) 0.039(2) 0.036(2) 0.0063(16) 0.0075(16) 0.0040(16) C22 0.052(2) 0.036(2) 0.035(2) -0.0020(16) 0.0170(18) -0.0099(17) C23 0.0286(18) 0.0274(17) 0.0355(19) -0.0089(15) 0.0104(15) 0.0000(14) C24 0.0300(18) 0.0291(17) 0.0348(19) -0.0050(15) 0.0047(15) 0.0017(14) C25 0.037(2) 0.0303(19) 0.050(2) -0.0005(17) 0.0058(18) 0.0049(15) C26 0.036(2) 0.037(2) 0.070(3) -0.008(2) 0.003(2) 0.0089(17) C27 0.029(2) 0.046(2) 0.069(3) -0.017(2) 0.013(2) 0.0079(17) C28 0.0244(18) 0.039(2) 0.043(2) -0.0102(17) 0.0090(15) 0.0017(15) C29 0.0263(17) 0.0331(18) 0.038(2) -0.0128(15) 0.0122(15) -0.0021(14) C30 0.0255(17) 0.045(2) 0.0331(19) -0.0117(16) 0.0145(15) -0.0047(15) C31 0.045(2) 0.047(2) 0.033(2) -0.0101(17) 0.0193(17) -0.0104(18) C32 0.047(2) 0.045(2) 0.046(2) -0.0162(19) 0.0284(19) -0.0100(18) C33 0.0277(18) 0.045(2) 0.0294(18) -0.0090(16) 0.0141(15) -0.0082(15) C34 0.0311(18) 0.0335(18) 0.0237(16) -0.0048(14) 0.0122(14) -0.0044(14) C35 0.0274(18) 0.0378(19) 0.0316(19) -0.0043(15) 0.0130(15) -0.0042(14) C36 0.034(2) 0.052(2) 0.0291(19) -0.0033(17) 0.0105(16) -0.0072(17) C37 0.041(2) 0.049(2) 0.034(2) 0.0061(18) 0.0103(17) -0.0052(18) C38 0.042(2) 0.039(2) 0.035(2) -0.0005(16) 0.0161(17) -0.0105(17) C39 0.0338(19) 0.0365(19) 0.0313(19) -0.0035(15) 0.0133(15) -0.0048(15) C40 0.0256(17) 0.0362(18) 0.0230(16) -0.0043(14) 0.0093(13) -0.0022(14) C41 0.0262(17) 0.0319(17) 0.0287(17) -0.0022(14) 0.0110(14) -0.0006(14) C42 0.0331(19) 0.0312(17) 0.0312(18) -0.0040(15) 0.0146(15) -0.0033(14) C43 0.0296(18) 0.0351(18) 0.0251(16) -0.0002(14) 0.0108(14) -0.0053(14) C44 0.0339(19) 0.040(2) 0.0322(19) 0.0009(16) 0.0074(16) -0.0061(16) C45 0.0273(17) 0.0351(18) 0.0285(18) 0.0034(15) 0.0071(14) -0.0022(14) C46 0.0298(18) 0.0302(17) 0.0286(18) -0.0004(14) 0.0108(15) -0.0025(14) C47 0.035(2) 0.048(2) 0.038(2) 0.0049(18) 0.0141(17) 0.0008(17) C48 0.043(2) 0.050(2) 0.048(2) -0.008(2) 0.0216(19) -0.0106(19) C49 0.062(3) 0.052(3) 0.058(3) -0.006(2) 0.028(2) -0.014(2) C50 0.073(4) 0.063(3) 0.084(4) -0.015(3) 0.054(3) -0.020(3) S1 0.0330(5) 0.0428(5) 0.0463(6) -0.0015(4) 0.0063(4) -0.0023(4) F1 0.085(3) 0.141(4) 0.073(2) 0.034(2) 0.022(2) -0.052(3) F2 0.0629(19) 0.113(3) 0.0591(18) -0.0192(18) 0.0216(15) 0.0138(19) F3 0.0460(15) 0.084(2) 0.0457(15) 0.0117(14) 0.0048(12) -0.0047(14) O4 0.0333(15) 0.0560(18) 0.0559(19) 0.0000(15) 0.0053(13) -0.0028(13) O5 0.0450(19) 0.057(2) 0.098(3) -0.019(2) 0.0027(19) 0.0058(16) O6 0.0537(19) 0.069(2) 0.0422(17) -0.0006(15) 0.0174(14) -0.0169(16) C51 0.034(2) 0.074(3) 0.046(2) 0.016(2) 0.0146(19) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C40 2.019(3) . ? Pd1 N1 2.144(3) . ? Pd1 P1 2.3401(8) . ? Pd1 C8 2.433(3) . ? P1 C1 1.842(3) . ? P1 C23 1.897(4) . ? P1 C34 1.917(4) . ? O1 C2 1.361(4) . ? O1 C3 1.434(5) . ? O2 C30 1.434(5) . ? O2 C31 1.436(5) . ? O3 C32 1.428(5) . ? O3 C30 1.437(5) . ? N1 C47 1.477(6) . ? N1 H1N 0.94(6) . ? N1 H2N 1.06(7) . ? C1 C7 1.406(5) . ? C1 C2 1.413(5) . ? C2 C4 1.399(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.380(5) . ? C5 H5 0.9500 . ? C6 C7 1.400(5) . ? C6 H6 0.9500 . ? C7 C8 1.508(5) . ? C8 C19 1.422(5) . ? C8 C9 1.429(5) . ? C9 C13 1.390(5) . ? C9 C10 1.524(5) . ? C10 C12 1.527(6) . ? C10 C11 1.542(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.398(6) . ? C13 H13 0.9500 . ? C14 C18 1.386(6) . ? C14 C15 1.522(5) . ? C15 C16 1.514(6) . ? C15 C17 1.533(6) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.394(5) . ? C18 H18 0.9500 . ? C19 C20 1.530(5) . ? C20 C22 1.523(6) . ? C20 C21 1.530(6) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.543(5) . ? C23 C24 1.543(6) . ? C23 C29 1.548(5) . ? C24 C25 1.531(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.514(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.533(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.521(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.528(6) . ? C31 C32 1.512(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.538(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.551(5) . ? C34 C35 1.554(5) . ? C35 C36 1.535(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.528(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.524(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.536(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C46 1.391(5) . ? C40 C41 1.400(5) . ? C41 C42 1.395(5) . ? C41 H41 0.9500 . ? C42 C43 1.388(6) . ? C42 H42 0.9500 . ? C43 C45 1.391(6) . ? C43 C44 1.516(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.400(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.516(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.505(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.524(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? S1 O5 1.417(4) . ? S1 O6 1.426(4) . ? S1 O4 1.432(3) . ? S1 C51 1.820(5) . ? F1 C51 1.340(6) . ? F2 C51 1.323(7) . ? F3 C51 1.324(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Pd1 N1 80.35(13) . . ? C40 Pd1 P1 97.23(10) . . ? N1 Pd1 P1 177.56(10) . . ? C40 Pd1 C8 178.20(13) . . ? N1 Pd1 C8 98.34(12) . . ? P1 Pd1 C8 84.06(8) . . ? C1 P1 C23 107.00(16) . . ? C1 P1 C34 109.68(15) . . ? C23 P1 C34 105.43(16) . . ? C1 P1 Pd1 103.69(11) . . ? C23 P1 Pd1 112.38(12) . . ? C34 P1 Pd1 118.21(11) . . ? C2 O1 C3 118.7(3) . . ? C30 O2 C31 106.7(3) . . ? C32 O3 C30 108.9(3) . . ? C47 N1 Pd1 119.8(3) . . ? C47 N1 H1N 108(3) . . ? Pd1 N1 H1N 104(3) . . ? C47 N1 H2N 108(3) . . ? Pd1 N1 H2N 117(3) . . ? H1N N1 H2N 98(4) . . ? C7 C1 C2 117.0(3) . . ? C7 C1 P1 117.9(2) . . ? C2 C1 P1 125.0(3) . . ? O1 C2 C4 121.2(3) . . ? O1 C2 C1 116.2(3) . . ? C4 C2 C1 122.6(3) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 118.6(3) . . ? C5 C4 H4 120.7 . . ? C2 C4 H4 120.7 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C1 120.0(3) . . ? C6 C7 C8 113.4(3) . . ? C1 C7 C8 126.5(3) . . ? C19 C8 C9 118.6(3) . . ? C19 C8 C7 117.5(3) . . ? C9 C8 C7 118.7(3) . . ? C19 C8 Pd1 88.1(2) . . ? C9 C8 Pd1 96.8(2) . . ? C7 C8 Pd1 107.5(2) . . ? C13 C9 C8 119.1(3) . . ? C13 C9 C10 118.9(3) . . ? C8 C9 C10 121.9(3) . . ? C9 C10 C12 112.7(3) . . ? C9 C10 C11 111.2(3) . . ? C12 C10 C11 109.7(3) . . ? C9 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 122.4(3) . . ? C9 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C18 C14 C13 117.8(3) . . ? C18 C14 C15 120.6(3) . . ? C13 C14 C15 121.6(3) . . ? C16 C15 C14 113.4(3) . . ? C16 C15 C17 111.3(3) . . ? C14 C15 C17 110.4(3) . . ? C16 C15 H15 107.1 . . ? C14 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 122.5(3) . . ? C14 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C18 C19 C8 119.3(3) . . ? C18 C19 C20 118.5(3) . . ? C8 C19 C20 121.9(3) . . ? C22 C20 C21 110.7(3) . . ? C22 C20 C19 111.6(3) . . ? C21 C20 C19 111.4(3) . . ? C22 C20 H20 107.6 . . ? C21 C20 H20 107.6 . . ? C19 C20 H20 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 106.8(3) . . ? C28 C23 C29 111.6(3) . . ? C24 C23 C29 111.8(3) . . ? C28 C23 P1 117.3(3) . . ? C24 C23 P1 105.2(2) . . ? C29 C23 P1 104.0(2) . . ? C25 C24 C23 114.6(3) . . ? C25 C24 H24A 108.6 . . ? C23 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C26 C25 C24 110.2(3) . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 110.9(4) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 111.7(4) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C23 112.9(3) . . ? C27 C28 H28A 109.0 . . ? C23 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C23 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C23 115.4(3) . . ? C30 C29 H29A 108.4 . . ? C23 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? C23 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? O2 C30 O3 105.4(3) . . ? O2 C30 C29 105.7(3) . . ? O3 C30 C29 111.6(3) . . ? O2 C30 C33 112.0(3) . . ? O3 C30 C33 106.2(3) . . ? C29 C30 C33 115.6(3) . . ? O2 C31 C32 101.3(3) . . ? O2 C31 H31A 111.5 . . ? C32 C31 H31A 111.5 . . ? O2 C31 H31B 111.5 . . ? C32 C31 H31B 111.5 . . ? H31A C31 H31B 109.3 . . ? O3 C32 C31 103.4(3) . . ? O3 C32 H32A 111.1 . . ? C31 C32 H32A 111.1 . . ? O3 C32 H32B 111.1 . . ? C31 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? C30 C33 C34 116.8(3) . . ? C30 C33 H33A 108.1 . . ? C34 C33 H33A 108.1 . . ? C30 C33 H33B 108.1 . . ? C34 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C33 C34 C39 111.4(3) . . ? C33 C34 C35 110.7(3) . . ? C39 C34 C35 106.8(3) . . ? C33 C34 P1 108.1(3) . . ? C39 C34 P1 109.7(2) . . ? C35 C34 P1 110.2(2) . . ? C36 C35 C34 111.9(3) . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35B 109.2 . . ? C34 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C35 111.8(3) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C36 110.5(4) . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 111.3(3) . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38B 109.4 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C34 113.6(3) . . ? C38 C39 H39A 108.8 . . ? C34 C39 H39A 108.8 . . ? C38 C39 H39B 108.8 . . ? C34 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C46 C40 C41 117.0(3) . . ? C46 C40 Pd1 116.3(3) . . ? C41 C40 Pd1 125.7(3) . . ? C42 C41 C40 121.1(3) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C43 C42 C41 121.6(3) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C45 117.6(3) . . ? C42 C43 C44 121.9(3) . . ? C45 C43 C44 120.4(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 C46 120.8(3) . . ? C43 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C40 C46 C45 121.8(3) . . ? C40 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? N1 C47 C48 112.5(4) . . ? N1 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? N1 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C47 115.3(4) . . ? C49 C48 H48A 108.5 . . ? C47 C48 H48A 108.5 . . ? C49 C48 H48B 108.5 . . ? C47 C48 H48B 108.5 . . ? H48A C48 H48B 107.5 . . ? C48 C49 C50 111.4(5) . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? C50 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O5 S1 O6 114.6(2) . . ? O5 S1 O4 115.0(2) . . ? O6 S1 O4 115.2(2) . . ? O5 S1 C51 104.0(3) . . ? O6 S1 C51 102.1(2) . . ? O4 S1 C51 103.5(2) . . ? F2 C51 F3 107.7(4) . . ? F2 C51 F1 107.3(4) . . ? F3 C51 F1 106.8(4) . . ? F2 C51 S1 111.9(3) . . ? F3 C51 S1 113.4(3) . . ? F1 C51 S1 109.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 P1 C1 C7 114.9(3) . . . . ? C34 P1 C1 C7 -131.2(3) . . . . ? Pd1 P1 C1 C7 -4.1(3) . . . . ? C23 P1 C1 C2 -63.0(3) . . . . ? C34 P1 C1 C2 50.9(3) . . . . ? Pd1 P1 C1 C2 178.1(3) . . . . ? C3 O1 C2 C4 -14.8(5) . . . . ? C3 O1 C2 C1 167.0(3) . . . . ? C7 C1 C2 O1 176.4(3) . . . . ? P1 C1 C2 O1 -5.8(5) . . . . ? C7 C1 C2 C4 -1.8(5) . . . . ? P1 C1 C2 C4 176.0(3) . . . . ? O1 C2 C4 C5 -176.7(3) . . . . ? C1 C2 C4 C5 1.4(5) . . . . ? C2 C4 C5 C6 -0.1(6) . . . . ? C4 C5 C6 C7 -0.6(6) . . . . ? C5 C6 C7 C1 0.1(5) . . . . ? C5 C6 C7 C8 177.0(3) . . . . ? C2 C1 C7 C6 1.1(5) . . . . ? P1 C1 C7 C6 -176.9(3) . . . . ? C2 C1 C7 C8 -175.4(3) . . . . ? P1 C1 C7 C8 6.6(5) . . . . ? C6 C7 C8 C19 -84.5(4) . . . . ? C1 C7 C8 C19 92.2(4) . . . . ? C6 C7 C8 C9 69.8(4) . . . . ? C1 C7 C8 C9 -113.5(4) . . . . ? C6 C7 C8 Pd1 178.2(2) . . . . ? C1 C7 C8 Pd1 -5.1(4) . . . . ? C19 C8 C9 C13 3.8(5) . . . . ? C7 C8 C9 C13 -150.3(3) . . . . ? Pd1 C8 C9 C13 95.4(3) . . . . ? C19 C8 C9 C10 -179.6(3) . . . . ? C7 C8 C9 C10 26.3(5) . . . . ? Pd1 C8 C9 C10 -88.0(3) . . . . ? C13 C9 C10 C12 61.9(4) . . . . ? C8 C9 C10 C12 -114.7(4) . . . . ? C13 C9 C10 C11 -61.7(4) . . . . ? C8 C9 C10 C11 121.6(4) . . . . ? C8 C9 C13 C14 0.2(5) . . . . ? C10 C9 C13 C14 -176.5(3) . . . . ? C9 C13 C14 C18 -4.4(5) . . . . ? C9 C13 C14 C15 173.7(4) . . . . ? C18 C14 C15 C16 -126.5(4) . . . . ? C13 C14 C15 C16 55.4(5) . . . . ? C18 C14 C15 C17 107.9(4) . . . . ? C13 C14 C15 C17 -70.2(5) . . . . ? C13 C14 C18 C19 4.6(5) . . . . ? C15 C14 C18 C19 -173.5(3) . . . . ? C14 C18 C19 C8 -0.7(5) . . . . ? C14 C18 C19 C20 173.6(3) . . . . ? C9 C8 C19 C18 -3.6(5) . . . . ? C7 C8 C19 C18 150.8(3) . . . . ? Pd1 C8 C19 C18 -100.3(3) . . . . ? C9 C8 C19 C20 -177.6(3) . . . . ? C7 C8 C19 C20 -23.2(5) . . . . ? Pd1 C8 C19 C20 85.6(3) . . . . ? C18 C19 C20 C22 -66.1(4) . . . . ? C8 C19 C20 C22 107.9(4) . . . . ? C18 C19 C20 C21 58.2(4) . . . . ? C8 C19 C20 C21 -127.8(4) . . . . ? C1 P1 C23 C28 32.1(3) . . . . ? C34 P1 C23 C28 -84.6(3) . . . . ? Pd1 P1 C23 C28 145.3(3) . . . . ? C1 P1 C23 C24 -86.4(3) . . . . ? C34 P1 C23 C24 156.8(2) . . . . ? Pd1 P1 C23 C24 26.7(3) . . . . ? C1 P1 C23 C29 155.9(2) . . . . ? C34 P1 C23 C29 39.1(3) . . . . ? Pd1 P1 C23 C29 -91.0(2) . . . . ? C28 C23 C24 C25 55.2(4) . . . . ? C29 C23 C24 C25 -67.2(4) . . . . ? P1 C23 C24 C25 -179.4(3) . . . . ? C23 C24 C25 C26 -56.4(5) . . . . ? C24 C25 C26 C27 54.3(5) . . . . ? C25 C26 C27 C28 -55.7(5) . . . . ? C26 C27 C28 C23 57.4(5) . . . . ? C24 C23 C28 C27 -54.6(4) . . . . ? C29 C23 C28 C27 67.8(5) . . . . ? P1 C23 C28 C27 -172.3(3) . . . . ? C28 C23 C29 C30 57.7(4) . . . . ? C24 C23 C29 C30 177.3(3) . . . . ? P1 C23 C29 C30 -69.7(3) . . . . ? C31 O2 C30 O3 24.8(4) . . . . ? C31 O2 C30 C29 143.1(3) . . . . ? C31 O2 C30 C33 -90.2(4) . . . . ? C32 O3 C30 O2 -1.3(4) . . . . ? C32 O3 C30 C29 -115.7(3) . . . . ? C32 O3 C30 C33 117.6(3) . . . . ? C23 C29 C30 O2 159.3(3) . . . . ? C23 C29 C30 O3 -86.6(4) . . . . ? C23 C29 C30 C33 34.8(5) . . . . ? C30 O2 C31 C32 -36.9(4) . . . . ? C30 O3 C32 C31 -21.0(4) . . . . ? O2 C31 C32 O3 35.0(4) . . . . ? O2 C30 C33 C34 -82.6(4) . . . . ? O3 C30 C33 C34 162.9(3) . . . . ? C29 C30 C33 C34 38.6(5) . . . . ? C30 C33 C34 C39 -179.8(3) . . . . ? C30 C33 C34 C35 61.5(4) . . . . ? C30 C33 C34 P1 -59.2(4) . . . . ? C33 C34 C35 C36 65.0(4) . . . . ? C39 C34 C35 C36 -56.4(4) . . . . ? P1 C34 C35 C36 -175.5(3) . . . . ? C34 C35 C36 C37 58.4(4) . . . . ? C35 C36 C37 C38 -55.5(5) . . . . ? C36 C37 C38 C39 53.8(5) . . . . ? C37 C38 C39 C34 -56.4(5) . . . . ? C33 C34 C39 C38 -64.9(4) . . . . ? C35 C34 C39 C38 56.0(4) . . . . ? P1 C34 C39 C38 175.4(3) . . . . ? C46 C40 C41 C42 -2.7(5) . . . . ? Pd1 C40 C41 C42 -170.7(3) . . . . ? C40 C41 C42 C43 0.9(5) . . . . ? C41 C42 C43 C45 1.9(5) . . . . ? C41 C42 C43 C44 -177.1(3) . . . . ? C42 C43 C45 C46 -2.8(5) . . . . ? C44 C43 C45 C46 176.2(3) . . . . ? C41 C40 C46 C45 1.8(5) . . . . ? Pd1 C40 C46 C45 171.0(3) . . . . ? C43 C45 C46 C40 0.9(6) . . . . ? Pd1 N1 C47 C48 158.0(3) . . . . ? N1 C47 C48 C49 159.7(4) . . . . ? C47 C48 C49 C50 -177.8(4) . . . . ? O5 S1 C51 F2 -179.7(3) . . . . ? O6 S1 C51 F2 60.7(4) . . . . ? O4 S1 C51 F2 -59.2(4) . . . . ? O5 S1 C51 F3 58.2(4) . . . . ? O6 S1 C51 F3 -61.3(4) . . . . ? O4 S1 C51 F3 178.7(4) . . . . ? O5 S1 C51 F1 -61.0(4) . . . . ? O6 S1 C51 F1 179.5(4) . . . . ? O4 S1 C51 F1 59.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N O4 1.06(7) 2.40(6) 3.276(5) 139(5) 4_665 C48 H48B O5 0.99 2.54 3.401(6) 144.8 4_665 C39 H39A O1 0.99 2.24 3.053(5) 138.7 . C35 H35B O2 0.99 2.51 3.115(5) 119.2 . C33 H33A O1 0.99 2.24 3.066(5) 139.6 . C28 H28B O3 0.99 2.54 3.134(5) 118.7 . C3 H3A O5 0.98 2.44 3.089(6) 123.2 4_565 _refine_diff_density_max 1.134 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.101 _shelx_res_file ; TITL XRAY5796_0m_a.res in P2(1)/n XRAY5796_0m_a.res created by SHELXL-2016/6 at 19:49:18 on 12-Mar-2019 CELL 1.54178 15.0843 17.9837 19.7605 90.000 108.121 90.000 ZERR 4.000 0.0004 0.0005 0.0005 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H F N O P Pd S UNIT 204 300 12 4 24 4 4 4 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 CONF WPDB HTAB N1 O4_$2 HTAB C48 O5_$2 EQIV $2 x+1/2, -y+1/2, z-1/2 HTAB C39 O1 HTAB C35 O2 HTAB C33 O1 HTAB C28 O3 HTAB C3 O5_$1 EQIV $1 x-1/2, -y+1/2, z-1/2 SIZE 0.05 0.10 0.20 TEMP -173.00 WGHT 0.100000 0.434940 FVAR 0.19286 MOLE 1 PD1 7 0.559380 0.298029 0.225829 11.00000 0.02161 0.02858 = 0.02420 -0.00341 0.00889 -0.00128 P1 6 0.435291 0.291250 0.273055 11.00000 0.02206 0.02651 = 0.02547 -0.00463 0.01050 -0.00213 O1 5 0.244388 0.231662 0.275553 11.00000 0.02544 0.04579 = 0.03451 -0.01318 0.01655 -0.00912 O2 5 0.496517 0.390789 0.475423 11.00000 0.03140 0.05083 = 0.03164 -0.01628 0.01344 -0.00904 O3 5 0.338591 0.405428 0.430452 11.00000 0.03234 0.05924 = 0.04235 -0.02021 0.01990 -0.00066 N1 4 0.676705 0.306128 0.186819 11.00000 0.02965 0.03973 = 0.03393 -0.00304 0.01364 -0.00612 C1 1 0.347085 0.235645 0.206992 11.00000 0.02194 0.02602 = 0.02706 -0.00227 0.00851 -0.00116 C2 1 0.259692 0.214414 0.213026 11.00000 0.02641 0.02816 = 0.02768 -0.00204 0.01136 0.00038 C3 1 0.151370 0.226152 0.279628 11.00000 0.03200 0.05373 = 0.05248 -0.01734 0.02540 -0.01466 AFIX 137 H3A 2 0.109092 0.255820 0.241488 11.00000 -1.50000 H3B 2 0.150019 0.244834 0.325886 11.00000 -1.50000 H3C 2 0.131414 0.174037 0.274297 11.00000 -1.50000 AFIX 0 C4 1 0.192947 0.175937 0.159200 11.00000 0.02323 0.03258 = 0.02971 0.00094 0.00597 -0.00299 AFIX 43 H4 2 0.134227 0.163341 0.164362 11.00000 -1.20000 AFIX 0 C5 1 0.214299 0.156643 0.098331 11.00000 0.02888 0.03676 = 0.02816 -0.00291 0.00485 -0.00251 AFIX 43 H5 2 0.169954 0.130424 0.061215 11.00000 -1.20000 AFIX 0 C6 1 0.299702 0.175284 0.091233 11.00000 0.02859 0.03663 = 0.02537 -0.00554 0.00932 -0.00191 AFIX 43 H6 2 0.313531 0.161224 0.049274 11.00000 -1.20000 AFIX 0 C7 1 0.366383 0.214468 0.144543 11.00000 0.02195 0.02873 = 0.02478 -0.00003 0.00647 0.00141 C8 1 0.456829 0.225950 0.128528 11.00000 0.02351 0.03060 = 0.02576 -0.00589 0.00928 -0.00139 C9 1 0.458238 0.275790 0.072519 11.00000 0.02500 0.03229 = 0.02747 -0.00323 0.00740 -0.00290 C10 1 0.389522 0.340106 0.050072 11.00000 0.02847 0.03409 = 0.03260 0.00111 0.01190 0.00178 AFIX 13 H10 2 0.350889 0.340990 0.083027 11.00000 -1.20000 AFIX 0 C11 1 0.440887 0.415216 0.057281 11.00000 0.04559 0.03305 = 0.04904 0.00605 0.01999 0.00108 AFIX 137 H11A 2 0.476179 0.417208 0.023225 11.00000 -1.50000 H11B 2 0.483812 0.420363 0.105784 11.00000 -1.50000 H11C 2 0.395322 0.455825 0.047415 11.00000 -1.50000 AFIX 0 C12 1 0.323308 0.331379 -0.025665 11.00000 0.03883 0.04510 = 0.03611 0.00346 0.00943 0.00614 AFIX 137 H12A 2 0.359532 0.328503 -0.059041 11.00000 -1.50000 H12B 2 0.281227 0.374266 -0.037672 11.00000 -1.50000 H12C 2 0.286674 0.285766 -0.028883 11.00000 -1.50000 AFIX 0 C13 1 0.520862 0.263038 0.034983 11.00000 0.03167 0.03266 = 0.02746 0.00023 0.01145 -0.00408 AFIX 43 H13 2 0.521695 0.296408 -0.002084 11.00000 -1.20000 AFIX 0 C14 1 0.582694 0.202912 0.049750 11.00000 0.02858 0.03583 = 0.02823 -0.00453 0.00984 -0.00228 C15 1 0.643828 0.185403 0.003363 11.00000 0.03488 0.04272 = 0.03149 -0.00012 0.01572 0.00485 AFIX 13 H15 2 0.686969 0.144384 0.027308 11.00000 -1.20000 AFIX 0 C16 1 0.703888 0.250238 -0.004558 11.00000 0.04347 0.06147 = 0.05016 -0.01129 0.03007 -0.00994 AFIX 137 H16A 2 0.663836 0.291264 -0.028939 11.00000 -1.50000 H16B 2 0.744117 0.234654 -0.032512 11.00000 -1.50000 H16C 2 0.742581 0.266755 0.042649 11.00000 -1.50000 AFIX 0 C17 1 0.584323 0.156032 -0.069440 11.00000 0.04966 0.04099 = 0.03278 -0.00187 0.02103 0.00054 AFIX 137 H17A 2 0.544406 0.196056 -0.096066 11.00000 -1.50000 H17B 2 0.545334 0.114874 -0.062684 11.00000 -1.50000 H17C 2 0.625197 0.138393 -0.096103 11.00000 -1.50000 AFIX 0 C18 1 0.584805 0.157925 0.107179 11.00000 0.02454 0.03522 = 0.02775 -0.00454 0.00815 -0.00011 AFIX 43 H18 2 0.629632 0.119097 0.120042 11.00000 -1.20000 AFIX 0 C19 1 0.523623 0.167521 0.146762 11.00000 0.02360 0.03192 = 0.02438 -0.00566 0.00897 -0.00185 C20 1 0.524440 0.110052 0.204059 11.00000 0.03547 0.03494 = 0.02932 -0.00189 0.01630 0.00400 AFIX 13 H20 2 0.480106 0.127511 0.229226 11.00000 -1.20000 AFIX 0 C21 1 0.621079 0.103888 0.259396 11.00000 0.03242 0.03913 = 0.03627 0.00625 0.00752 0.00403 AFIX 137 H21A 2 0.617868 0.070820 0.297983 11.00000 -1.50000 H21B 2 0.642007 0.153279 0.278806 11.00000 -1.50000 H21C 2 0.665255 0.083617 0.236838 11.00000 -1.50000 AFIX 0 C22 1 0.490876 0.034294 0.171711 11.00000 0.05176 0.03564 = 0.03490 -0.00195 0.01700 -0.00986 AFIX 137 H22A 2 0.532526 0.016124 0.145919 11.00000 -1.50000 H22B 2 0.427398 0.038827 0.138704 11.00000 -1.50000 H22C 2 0.491108 -0.000816 0.209694 11.00000 -1.50000 AFIX 0 C23 1 0.381222 0.385623 0.277509 11.00000 0.02857 0.02739 = 0.03549 -0.00886 0.01036 -0.00004 C24 1 0.400582 0.432027 0.217950 11.00000 0.02999 0.02906 = 0.03476 -0.00498 0.00470 0.00172 AFIX 23 H24A 2 0.468804 0.433709 0.226536 11.00000 -1.20000 H24B 2 0.372146 0.406466 0.171914 11.00000 -1.20000 AFIX 0 C25 1 0.363557 0.511815 0.211789 11.00000 0.03653 0.03028 = 0.05018 -0.00050 0.00577 0.00486 AFIX 23 H25A 2 0.396350 0.539771 0.255584 11.00000 -1.20000 H25B 2 0.375823 0.536889 0.170997 11.00000 -1.20000 AFIX 0 C26 1 0.258759 0.511648 0.201117 11.00000 0.03615 0.03721 = 0.06956 -0.00752 0.00341 0.00889 AFIX 23 H26A 2 0.236636 0.563447 0.201350 11.00000 -1.20000 H26B 2 0.225381 0.489440 0.154268 11.00000 -1.20000 AFIX 0 C27 1 0.236895 0.467782 0.259387 11.00000 0.02927 0.04561 = 0.06874 -0.01660 0.01298 0.00789 AFIX 23 H27A 2 0.168470 0.466038 0.249712 11.00000 -1.20000 H27B 2 0.264569 0.493290 0.305556 11.00000 -1.20000 AFIX 0 C28 1 0.274981 0.388271 0.264442 11.00000 0.02444 0.03852 = 0.04335 -0.01020 0.00895 0.00167 AFIX 23 H28A 2 0.243060 0.361582 0.219664 11.00000 -1.20000 H28B 2 0.260462 0.362037 0.303762 11.00000 -1.20000 AFIX 0 C29 1 0.436130 0.415196 0.352424 11.00000 0.02632 0.03313 = 0.03822 -0.01280 0.01223 -0.00211 AFIX 23 H29A 2 0.503623 0.411947 0.358267 11.00000 -1.20000 H29B 2 0.420720 0.468426 0.354948 11.00000 -1.20000 AFIX 0 C30 1 0.417773 0.374874 0.414379 11.00000 0.02552 0.04545 = 0.03311 -0.01169 0.01447 -0.00470 C31 1 0.461412 0.398830 0.534765 11.00000 0.04468 0.04710 = 0.03250 -0.01009 0.01929 -0.01039 AFIX 23 H31A 2 0.503283 0.429862 0.572807 11.00000 -1.20000 H31B 2 0.452536 0.349941 0.554768 11.00000 -1.20000 AFIX 0 C32 1 0.369253 0.437175 0.500098 11.00000 0.04728 0.04510 = 0.04556 -0.01620 0.02836 -0.01005 AFIX 23 H32A 2 0.324333 0.426832 0.526301 11.00000 -1.20000 H32B 2 0.377587 0.491624 0.497847 11.00000 -1.20000 AFIX 0 C33 1 0.399704 0.291411 0.404197 11.00000 0.02765 0.04516 = 0.02936 -0.00897 0.01411 -0.00816 AFIX 23 H33A 2 0.333035 0.284133 0.377114 11.00000 -1.20000 H33B 2 0.410457 0.268690 0.451712 11.00000 -1.20000 AFIX 0 C34 1 0.458338 0.248607 0.365876 11.00000 0.03108 0.03351 = 0.02366 -0.00479 0.01218 -0.00440 C35 1 0.563853 0.253665 0.408439 11.00000 0.02736 0.03784 = 0.03163 -0.00427 0.01303 -0.00424 AFIX 23 H35A 2 0.600592 0.230514 0.380342 11.00000 -1.20000 H35B 2 0.582272 0.306612 0.415889 11.00000 -1.20000 AFIX 0 C36 1 0.586637 0.214669 0.480960 11.00000 0.03444 0.05160 = 0.02914 -0.00327 0.01054 -0.00719 AFIX 23 H36A 2 0.654370 0.218799 0.506048 11.00000 -1.20000 H36B 2 0.553124 0.239949 0.510280 11.00000 -1.20000 AFIX 0 C37 1 0.559007 0.132642 0.473144 11.00000 0.04056 0.04888 = 0.03449 0.00612 0.01027 -0.00519 AFIX 23 H37A 2 0.597539 0.105943 0.448556 11.00000 -1.20000 H37B 2 0.570839 0.110204 0.520889 11.00000 -1.20000 AFIX 0 C38 1 0.456158 0.124244 0.430730 11.00000 0.04204 0.03932 = 0.03549 -0.00049 0.01607 -0.01052 AFIX 23 H38A 2 0.417511 0.144768 0.458635 11.00000 -1.20000 H38B 2 0.440928 0.070806 0.422341 11.00000 -1.20000 AFIX 0 C39 1 0.432779 0.164814 0.358912 11.00000 0.03384 0.03654 = 0.03126 -0.00347 0.01334 -0.00475 AFIX 23 H39A 2 0.365145 0.159739 0.333856 11.00000 -1.20000 H39B 2 0.466606 0.140440 0.329318 11.00000 -1.20000 AFIX 0 C40 1 0.647847 0.355745 0.306536 11.00000 0.02564 0.03624 = 0.02303 -0.00434 0.00930 -0.00225 C41 1 0.647879 0.432988 0.315483 11.00000 0.02625 0.03186 = 0.02875 -0.00222 0.01098 -0.00058 AFIX 43 H41 2 0.597953 0.461681 0.285813 11.00000 -1.20000 AFIX 0 C42 1 0.720014 0.468487 0.367245 11.00000 0.03306 0.03118 = 0.03118 -0.00403 0.01464 -0.00332 AFIX 43 H42 2 0.717716 0.520891 0.372530 11.00000 -1.20000 AFIX 0 C43 1 0.795059 0.429121 0.411212 11.00000 0.02960 0.03508 = 0.02513 -0.00023 0.01079 -0.00531 C44 1 0.871423 0.466762 0.469851 11.00000 0.03393 0.03976 = 0.03216 0.00089 0.00737 -0.00611 AFIX 137 H44A 2 0.917658 0.429674 0.494799 11.00000 -1.50000 H44B 2 0.844267 0.490219 0.503599 11.00000 -1.50000 H44C 2 0.901718 0.504728 0.449068 11.00000 -1.50000 AFIX 0 C45 1 0.797555 0.352806 0.400542 11.00000 0.02725 0.03506 = 0.02849 0.00345 0.00708 -0.00224 AFIX 43 H45 2 0.849417 0.324691 0.428375 11.00000 -1.20000 AFIX 0 C46 1 0.724607 0.316898 0.349304 11.00000 0.02985 0.03022 = 0.02857 -0.00044 0.01075 -0.00254 AFIX 43 H46 2 0.727619 0.264602 0.343596 11.00000 -1.20000 AFIX 0 C47 1 0.693699 0.375740 0.153198 11.00000 0.03548 0.04765 = 0.03828 0.00494 0.01407 0.00085 AFIX 23 H47A 2 0.677125 0.418567 0.178354 11.00000 -1.20000 H47B 2 0.652716 0.377030 0.103161 11.00000 -1.20000 AFIX 0 C48 1 0.794329 0.383432 0.154646 11.00000 0.04309 0.04970 = 0.04814 -0.00830 0.02156 -0.01058 AFIX 23 H48A 2 0.831978 0.399744 0.202873 11.00000 -1.20000 H48B 2 0.817422 0.333810 0.146350 11.00000 -1.20000 AFIX 0 C49 1 0.810696 0.436907 0.101140 11.00000 0.06192 0.05197 = 0.05764 -0.00590 0.02848 -0.01373 AFIX 23 H49A 2 0.791032 0.487394 0.110448 11.00000 -1.20000 H49B 2 0.772212 0.421991 0.052681 11.00000 -1.20000 AFIX 0 C50 1 0.913099 0.438550 0.104751 11.00000 0.07337 0.06285 = 0.08368 -0.01458 0.05418 -0.02023 AFIX 137 H50A 2 0.950018 0.461677 0.149560 11.00000 -1.50000 H50B 2 0.919982 0.467389 0.064602 11.00000 -1.50000 H50C 2 0.935136 0.387641 0.102411 11.00000 -1.50000 AFIX 0 S1 8 0.397844 0.334706 0.698796 11.00000 0.03299 0.04285 = 0.04629 -0.00152 0.00633 -0.00234 F1 3 0.362286 0.292406 0.813219 11.00000 0.08481 0.14058 = 0.07324 0.03432 0.02224 -0.05165 F2 3 0.369856 0.410809 0.803315 11.00000 0.06294 0.11331 = 0.05913 -0.01923 0.02160 0.01376 F3 3 0.494847 0.345991 0.835042 11.00000 0.04600 0.08445 = 0.04569 0.01165 0.00478 -0.00466 O4 5 0.299264 0.336521 0.663702 11.00000 0.03332 0.05601 = 0.05585 -0.00002 0.00533 -0.00281 O5 5 0.440911 0.264999 0.697067 11.00000 0.04504 0.05658 = 0.09842 -0.01895 0.00271 0.00583 O6 5 0.448255 0.397130 0.685417 11.00000 0.05368 0.06869 = 0.04222 -0.00061 0.01737 -0.01689 C51 1 0.407684 0.347402 0.792241 11.00000 0.03432 0.07448 = 0.04596 0.01562 0.01462 -0.00712 H1N 2 0.727860 0.297637 0.227328 11.00000 0.03853 H2N 2 0.687961 0.260802 0.155794 11.00000 0.05880 HKLF 4 REM XRAY5796_0m_a.res in P2(1)/n REM R1 = 0.0503 for 7189 Fo > 4sig(Fo) and 0.0733 for all 8991 data REM 594 parameters refined using 0 restraints END WGHT 0.0762 3.8211 REM Highest difference peak 1.134, deepest hole -0.927, 1-sigma level 0.101 Q1 1 0.5823 0.2569 0.2608 11.00000 0.05 1.13 Q2 1 0.5571 0.2437 0.2305 11.00000 0.05 1.12 Q3 1 0.5252 0.3369 0.1900 11.00000 0.05 1.04 Q4 1 0.5582 0.3528 0.2270 11.00000 0.05 1.02 Q5 1 0.5877 0.3442 0.2582 11.00000 0.05 1.01 Q6 1 0.3992 0.3308 0.7494 11.00000 0.05 0.80 Q7 1 0.5240 0.1382 0.1781 11.00000 0.05 0.56 Q8 1 0.3945 0.2630 0.2401 11.00000 0.05 0.52 Q9 1 0.4664 0.2631 0.1158 11.00000 0.05 0.48 Q10 1 0.4183 0.3392 0.2566 11.00000 0.05 0.47 Q11 1 0.8616 0.3895 0.1940 11.00000 0.05 0.42 Q12 1 0.4494 0.3838 0.8329 11.00000 0.05 0.41 Q13 1 0.5173 0.2659 0.3780 11.00000 0.05 0.40 Q14 1 0.3617 0.2843 0.6956 11.00000 0.05 0.38 Q15 1 0.5034 0.0795 0.1811 11.00000 0.05 0.38 Q16 1 0.3833 0.4760 0.2195 11.00000 0.05 0.38 Q17 1 0.7227 0.3799 0.3432 11.00000 0.05 0.37 Q18 1 0.3214 0.2650 0.7413 11.00000 0.05 0.37 Q19 1 0.3793 0.3968 0.7069 11.00000 0.05 0.36 Q20 1 0.4665 0.3409 0.6788 11.00000 0.05 0.35 ; _shelx_res_checksum 22283 _shelx_hkl_file ; -1 0 0 2.10 0.80 1 0 0 7.20 6.10 -1 0 0 -2.30 4.30 -2 0 0 1936.91 122.69 -2 0 0 2019.60 152.98 2 0 0 2111.79 154.88 3 0 0 4.90 14.00 -3 0 0 21.00 16.60 -4 0 0 240.98 47.00 4 0 0 148.39 48.60 -4 0 0 166.48 12.10 -5 0 0 1.90 2.80 5 0 0 -21.40 24.10 -5 0 0 -5.70 17.00 -6 0 0 843.82 129.99 6 0 0 1047.50 140.39 -6 0 0 979.60 60.59 7 0 0 -39.30 59.69 -7 0 0 -11.00 39.00 -7 0 0 -0.30 3.20 -8 0 0 655.83 42.60 8 0 0 745.63 181.38 -8 0 0 525.65 167.28 -9 0 0 313.57 187.48 9 0 0 212.38 178.98 10 0 0 301.37 24.60 -10 0 0 307.97 23.10 -10 0 0 326.27 23.50 -10 0 0 276.17 22.60 -10 0 0 330.87 23.40 10 0 0 284.57 24.90 10 0 0 369.76 31.30 -11 0 0 1.70 4.00 -11 0 0 -7.10 4.70 11 0 0 3.50 6.70 11 0 0 1.70 4.60 11 0 0 -9.50 6.10 -11 0 0 1.40 3.70 -12 0 0 31.50 6.50 12 0 0 43.60 9.10 -12 0 0 33.90 6.80 -12 0 0 33.30 6.80 12 0 0 38.70 8.90 13 0 0 -3.00 5.30 -13 0 0 -2.60 5.00 13 0 0 -5.70 5.50 -13 0 0 -8.00 5.00 -13 0 0 -2.90 2.60 -14 0 0 130.79 14.20 -14 0 0 117.19 12.50 14 0 0 126.29 14.90 14 0 0 141.99 16.30 -14 0 0 166.58 13.50 -15 0 0 2.40 3.60 15 0 0 2.30 5.00 15 0 0 1.00 3.60 -15 0 0 2.80 3.50 16 0 0 108.49 12.60 16 0 0 113.29 13.10 -16 0 0 108.59 10.50 17 0 0 0.60 2.80 -17 0 0 3.70 2.70 0 -1 0 12.00 1.00 0 1 0 6.10 4.70 0 1 0 9.50 0.90 -1 -1 0 1759.52 119.79 -1 -1 0 1432.36 100.49 1 -1 0 1608.04 120.19 -1 -1 0 1633.24 100.49 -1 1 0 1841.62 100.99 -1 1 0 1671.53 119.09 1 1 0 1664.33 118.69 -2 -1 0 438.96 27.30 2 -1 0 343.57 47.30 -2 -1 0 542.55 56.99 -2 1 0 480.25 27.80 -2 1 0 389.06 50.59 3 -1 0 185.38 40.90 -3 -1 0 279.67 47.40 -3 -1 0 257.97 17.00 -3 1 0 279.47 17.60 3 1 0 266.17 45.50 -3 1 0 361.26 53.79 -4 -1 0 17.10 3.10 4 -1 0 16.90 25.00 -4 -1 0 49.00 29.20 -4 1 0 18.90 3.80 4 1 0 7.40 20.90 -4 1 0 6.50 19.70 -5 -1 0 77.59 39.70 5 -1 0 49.00 33.20 -5 -1 0 47.80 5.40 -5 1 0 49.40 5.80 -5 1 0 74.19 43.70 5 1 0 29.00 36.30 -6 -1 0 251.97 78.79 6 -1 0 226.88 72.79 -6 -1 0 200.88 14.90 6 1 0 256.87 82.49 -6 1 0 211.68 15.50 -6 1 0 261.67 76.39 -7 -1 0 -22.50 46.10 7 1 0 36.40 53.59 -7 1 0 86.99 73.49 8 -1 0 -21.10 90.79 -8 -1 0 69.59 76.79 -8 1 0 72.69 104.99 8 1 0 197.38 96.09 9 -1 0 52.69 194.28 -9 1 0 218.18 287.27 -10 -1 0 92.19 9.90 -10 -1 0 82.79 10.40 -10 -1 0 92.99 9.60 10 -1 0 101.59 11.90 10 -1 0 96.99 13.70 10 -1 0 109.19 12.60 -10 1 0 90.69 10.90 -10 1 0 112.59 10.50 -10 1 0 90.09 9.50 -10 1 0 97.09 10.40 10 1 0 103.29 12.70 10 1 0 114.69 12.20 11 -1 0 18.10 7.00 -11 -1 0 17.70 5.90 -11 -1 0 2.80 8.70 -11 -1 0 21.70 7.20 -11 -1 0 17.80 5.30 -11 -1 0 19.60 5.30 11 -1 0 19.50 6.60 -11 1 0 21.30 5.70 -11 1 0 16.10 6.50 11 1 0 21.70 8.70 11 1 0 15.40 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0 70.39 5.40 1 2 0 63.89 18.60 -1 2 0 42.40 16.10 -2 -2 0 1250.87 109.09 -2 -2 0 1019.50 74.19 2 2 0 1335.77 109.89 -2 2 0 1289.97 75.09 -2 2 0 1325.27 111.09 3 -2 0 2774.92 226.98 -3 -2 0 2932.51 231.68 -3 -2 0 2938.81 178.38 -3 2 0 2994.50 179.18 -3 2 0 2999.30 230.28 4 -2 0 -6.00 19.10 -4 -2 0 1.60 1.90 -4 -2 0 21.20 23.60 -4 2 0 0.80 3.00 -4 2 0 19.60 15.60 4 2 0 -7.20 17.90 -5 -2 0 21.40 3.30 5 -2 0 7.20 27.30 -5 2 0 20.50 4.10 5 2 0 41.60 29.40 -5 2 0 52.39 32.90 -6 -2 0 498.15 98.59 6 -2 0 615.34 116.89 -6 -2 0 494.65 31.70 -6 2 0 474.95 32.70 6 2 0 538.15 100.19 -7 -2 0 429.86 28.30 -7 -2 0 517.25 110.89 7 -2 0 445.36 128.59 -7 2 0 430.56 29.50 7 2 0 429.66 150.38 -7 2 0 398.26 116.59 -8 -2 0 1091.09 69.89 8 -2 0 1153.68 342.77 -8 -2 0 1047.00 228.48 -8 2 0 1130.69 71.29 -8 2 0 874.11 218.48 8 2 0 1431.66 209.48 9 -2 0 16.50 7.60 -9 -2 0 10.90 3.80 -9 -2 0 15.20 4.30 -9 -2 0 16.30 4.90 9 -2 0 21.80 5.70 9 -2 0 13.30 6.30 -9 2 0 11.40 4.40 -9 2 0 17.20 5.70 9 2 0 23.50 6.40 -9 2 0 21.90 6.00 9 2 0 15.00 5.40 -10 -2 0 309.37 23.20 -10 -2 0 304.27 21.90 10 -2 0 285.67 23.40 -10 -2 0 228.08 21.00 10 -2 0 302.47 27.50 10 -2 0 281.97 23.60 -10 -2 0 286.27 21.70 -10 2 0 327.77 22.10 -10 2 0 304.77 23.00 10 2 0 264.97 23.00 -10 2 0 287.07 21.60 10 2 0 277.27 22.90 -11 -2 0 44.80 13.60 -11 -2 0 73.19 8.90 -11 -2 0 59.19 8.90 11 -2 0 51.29 10.20 11 -2 0 72.29 14.50 11 -2 0 53.79 10.20 11 2 0 62.09 10.40 11 2 0 49.40 9.80 -11 2 0 59.99 8.50 -11 2 0 51.59 8.10 -11 2 0 55.89 8.40 12 -2 0 -2.70 5.40 -12 -2 0 -4.30 3.30 12 -2 0 -6.00 5.10 -12 -2 0 -1.30 3.90 12 -2 0 3.40 5.60 -12 -2 0 0.10 3.70 -12 2 0 -1.00 4.70 -12 2 0 7.60 3.90 -12 2 0 -1.90 5.90 12 2 0 3.70 5.30 -12 2 0 -3.90 3.50 12 2 0 8.70 5.50 13 -2 0 191.98 23.00 -13 -2 0 238.28 21.00 -13 2 0 215.98 20.10 13 2 0 194.98 22.40 14 -2 0 17.10 7.20 14 -2 0 13.00 4.90 -14 -2 0 26.10 6.20 -14 -2 0 25.20 5.70 -14 -2 0 19.10 6.00 14 2 0 30.10 8.90 -14 2 0 23.10 5.70 -14 2 0 32.30 6.70 14 2 0 23.80 7.60 15 -2 0 -1.00 5.10 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255.67 28.70 12 -7 0 282.67 22.50 -12 7 0 226.98 19.80 12 7 0 222.08 20.40 12 7 0 243.28 21.80 -12 7 0 217.18 19.70 13 -7 0 5.40 7.70 13 -7 0 10.20 6.50 -13 -7 0 12.90 4.20 -13 -7 0 3.00 4.10 -13 -7 0 11.70 5.00 13 7 0 1.90 4.60 13 7 0 12.30 6.00 13 7 0 3.70 4.70 -13 7 0 7.50 4.50 -13 7 0 10.10 4.70 -14 -7 0 6.90 4.90 -14 -7 0 9.90 4.70 -14 -7 0 10.20 5.20 14 -7 0 3.30 5.60 14 -7 0 -2.30 6.50 -14 7 0 12.80 5.40 14 7 0 -5.30 3.70 -14 7 0 12.60 5.40 14 7 0 9.50 5.50 14 7 0 6.50 7.00 15 -7 0 118.49 12.70 15 -7 0 103.89 15.10 -15 -7 0 102.29 10.70 -15 -7 0 100.79 17.20 15 7 0 159.48 14.60 -15 7 0 117.69 11.20 15 7 0 114.79 13.00 -15 7 0 95.59 10.70 -16 -7 0 5.90 3.00 16 -7 0 8.30 6.20 16 -7 0 4.50 6.70 -16 7 0 10.50 3.50 16 7 0 15.90 7.60 -16 7 0 9.70 3.70 0 -8 0 299.77 96.49 0 -8 0 280.77 79.79 0 8 0 230.68 15.90 -1 -8 0 45.60 45.80 -1 -8 0 -15.10 42.30 1 -8 0 20.60 42.50 1 -8 0 -14.70 38.10 1 8 0 3.50 1.70 -1 8 0 4.10 2.60 -2 -8 0 29.90 37.90 -2 8 0 26.50 4.60 -2 8 0 13.20 48.60 -3 -8 0 144.59 73.29 3 -8 0 3.50 60.59 -3 -8 0 10.60 53.99 -3 8 0 10.00 3.90 -3 8 0 18.60 56.49 -4 8 0 244.08 18.20 -4 8 0 334.27 106.19 5 -8 0 294.17 120.99 -5 8 0 284.27 118.29 -6 -8 0 88.59 9.80 -6 -8 0 96.09 10.30 6 -8 0 95.59 10.40 -6 -8 0 91.49 9.50 6 -8 0 95.89 13.70 -6 -8 0 91.29 11.10 -6 -8 0 77.69 10.50 6 -8 0 77.49 9.40 -6 8 0 86.99 9.70 7 -8 0 -13.80 5.90 -7 -8 0 -0.70 3.90 7 -8 0 7.50 3.90 7 -8 0 11.10 8.10 7 -8 0 0.20 4.20 7 -8 0 5.10 5.70 -7 -8 0 0.80 3.70 -7 -8 0 4.00 3.00 -7 -8 0 -0.40 3.90 -7 -8 0 11.50 5.00 -7 -8 0 4.50 4.50 -7 8 0 3.40 4.50 7 8 0 2.10 6.00 -7 8 0 7.70 4.50 -8 -8 0 262.07 19.80 8 -8 0 241.28 20.30 -8 -8 0 216.98 20.10 -8 -8 0 267.97 21.50 -8 -8 0 259.87 20.30 8 -8 0 245.68 19.90 8 -8 0 277.87 29.50 8 -8 0 284.27 21.90 -8 -8 0 276.07 23.00 8 -8 0 256.07 20.90 -8 -8 0 232.28 20.70 8 -8 0 267.37 20.30 -8 8 0 228.68 20.30 -8 8 0 253.27 20.30 -8 8 0 262.27 20.60 8 8 0 253.27 21.00 -9 -8 0 0.10 5.10 9 -8 0 4.90 5.40 -9 -8 0 6.20 4.20 9 -8 0 4.40 8.00 -9 -8 0 8.80 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32.70 7.50 -5 -10 0 34.40 6.10 -5 -10 0 27.20 6.50 5 -10 0 26.10 7.00 -5 -10 0 29.80 7.60 5 -10 0 48.40 12.00 -5 -10 0 30.10 7.50 -5 10 0 33.90 6.70 -6 -10 0 78.69 11.90 6 -10 0 76.99 9.20 -6 -10 0 82.89 11.80 6 -10 0 86.39 10.40 -6 -10 0 77.29 10.80 -6 -10 0 87.69 9.70 -6 -10 0 94.19 10.90 6 -10 0 91.79 10.80 6 -10 0 74.59 12.30 6 -10 0 83.89 10.80 -6 -10 0 79.99 10.40 6 -10 0 88.19 14.30 -6 -10 0 93.29 10.40 -6 10 0 94.19 10.00 -6 10 0 92.59 11.20 -7 -10 0 13.20 4.50 7 -10 0 8.00 7.80 7 -10 0 3.10 4.60 -7 -10 0 10.00 5.50 -7 -10 0 6.90 4.40 7 -10 0 9.20 7.20 7 -10 0 14.20 6.00 -7 -10 0 4.70 5.60 7 -10 0 9.80 6.80 -7 -10 0 2.60 4.60 7 -10 0 8.90 5.30 -7 10 0 13.30 5.00 -7 10 0 5.80 4.70 7 10 0 10.60 5.20 -8 -10 0 204.88 19.00 8 -10 0 232.18 25.00 -8 -10 0 248.88 20.10 8 -10 0 219.78 19.90 8 -10 0 225.78 19.20 -8 -10 0 221.08 18.00 -8 -10 0 190.68 19.00 8 -10 0 248.38 26.00 -8 -10 0 220.98 19.60 -8 -10 0 243.48 19.10 -8 10 0 224.68 19.50 8 10 0 202.38 23.30 -8 10 0 214.38 18.40 -9 -10 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4.10 12 -10 0 2.80 4.80 -12 10 0 2.10 4.30 -12 10 0 0.40 4.10 12 10 0 8.60 5.60 12 10 0 5.70 5.20 -13 -10 0 0.50 3.90 -13 -10 0 7.80 5.00 13 -10 0 4.20 7.50 -13 -10 0 12.80 4.90 13 -10 0 3.80 5.90 -13 -10 0 -2.10 5.40 13 -10 0 4.90 6.10 -13 10 0 11.30 4.80 13 10 0 3.40 4.60 13 10 0 15.10 5.90 -13 10 0 6.20 4.10 -14 -10 0 33.60 6.00 14 -10 0 26.40 6.80 -14 -10 0 21.00 6.80 14 -10 0 33.30 10.30 -14 -10 0 45.00 7.30 14 10 0 47.00 8.00 -14 10 0 42.50 6.90 -14 10 0 32.30 6.00 14 10 0 32.20 6.20 15 -10 0 -2.90 4.60 -15 -10 0 -1.70 2.60 -15 10 0 1.90 2.40 -15 10 0 -6.20 3.50 15 10 0 0.10 3.90 15 10 0 0.70 4.50 0 -11 0 -4.90 4.20 0 -11 0 6.40 3.80 0 -11 0 1.00 2.80 0 -11 0 -2.60 3.20 0 11 0 0.30 1.90 1 -11 0 77.99 9.50 -1 -11 0 74.19 11.30 -1 -11 0 73.89 10.10 -1 -11 0 79.69 8.70 -1 -11 0 67.99 8.50 1 -11 0 76.39 9.20 -1 11 0 72.79 7.10 2 -11 0 312.87 23.90 2 -11 0 335.07 30.10 -2 -11 0 298.57 23.50 -2 -11 0 298.47 24.20 2 -11 0 315.77 26.20 -2 11 0 262.57 20.60 -3 -11 0 7.00 5.00 -3 -11 0 11.60 4.40 -3 -11 0 5.00 4.70 3 -11 0 6.80 3.80 3 -11 0 5.00 4.00 -3 -11 0 14.30 4.90 -3 -11 0 4.70 4.10 -3 -11 0 7.20 4.90 3 -11 0 6.80 7.80 3 -11 0 9.30 4.90 3 -11 0 8.70 5.90 -3 -11 0 15.90 5.90 -3 11 0 4.30 3.40 4 -11 0 166.68 20.10 4 -11 0 162.18 15.40 -4 -11 0 160.48 14.30 -4 -11 0 146.39 15.00 4 -11 0 154.38 14.40 4 -11 0 166.78 14.30 4 -11 0 168.68 16.80 -4 -11 0 163.98 14.70 4 -11 0 152.68 14.30 -4 -11 0 165.58 14.90 -4 -11 0 145.89 14.70 -4 -11 0 160.28 13.50 4 -11 0 160.18 15.70 -4 -11 0 144.19 14.80 -4 11 0 148.09 13.30 5 -11 0 -5.00 4.30 5 -11 0 2.90 4.30 5 -11 0 -6.20 3.20 -5 -11 0 3.40 5.30 -5 -11 0 -1.00 2.90 5 -11 0 0.70 4.20 -5 -11 0 2.20 3.70 5 -11 0 -0.50 3.00 -5 -11 0 -5.80 4.50 -5 -11 0 -2.50 4.20 5 -11 0 13.20 8.50 -5 -11 0 -6.80 3.50 -5 -11 0 -0.30 4.40 -5 11 0 -1.30 4.70 -5 11 0 -1.20 3.40 6 -11 0 83.09 11.00 6 -11 0 70.79 10.20 -6 -11 0 82.19 11.90 -6 -11 0 76.49 11.10 -6 -11 0 86.39 10.10 6 -11 0 86.49 13.40 -6 -11 0 77.69 11.80 -6 -11 0 81.39 10.10 6 -11 0 95.89 10.40 -6 -11 0 89.79 11.50 6 -11 0 91.69 15.10 -6 -11 0 83.49 9.80 -6 11 0 96.49 10.30 6 11 0 89.69 11.50 -7 -11 0 5.50 6.30 -7 -11 0 17.10 6.10 7 -11 0 19.30 7.50 -7 -11 0 11.20 4.60 7 -11 0 8.60 6.00 -7 -11 0 8.10 4.70 7 -11 0 4.50 5.60 -7 -11 0 10.40 5.60 7 -11 0 9.50 8.30 7 -11 0 7.90 5.30 -7 11 0 14.50 5.40 7 11 0 12.50 5.20 -8 -11 0 14.50 6.60 8 -11 0 14.50 6.20 -8 -11 0 11.40 5.80 -8 -11 0 13.40 5.90 8 -11 0 12.40 6.30 -8 -11 0 10.20 4.80 8 -11 0 13.60 5.70 8 -11 0 11.10 6.10 -8 -11 0 10.80 5.20 8 -11 0 9.20 8.80 -8 -11 0 20.80 7.40 -8 11 0 8.30 5.10 8 11 0 16.60 5.60 -8 11 0 16.70 5.90 -8 11 0 11.40 4.90 9 -11 0 5.50 5.90 -9 -11 0 1.40 4.20 -9 -11 0 6.70 5.10 9 -11 0 14.20 5.50 9 -11 0 0.50 7.40 -9 -11 0 9.50 6.00 9 -11 0 14.50 5.80 -9 -11 0 2.50 3.90 9 -11 0 0.40 5.70 -9 -11 0 6.20 5.60 -9 11 0 13.70 6.60 -9 11 0 12.10 4.90 9 11 0 7.90 5.10 10 -11 0 57.69 9.90 -10 -11 0 70.89 10.70 -10 -11 0 59.49 10.40 10 -11 0 74.39 17.70 -10 -11 0 68.39 10.30 10 -11 0 70.99 11.70 10 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10.30 -4 -12 0 11.80 5.00 4 -12 0 25.70 9.50 -4 -12 0 15.50 6.20 4 -12 0 22.10 8.60 4 -12 0 15.00 8.10 -4 -12 0 12.10 6.40 4 -12 0 18.00 7.20 -4 12 0 14.70 4.90 -5 -12 0 75.79 9.00 5 -12 0 64.89 13.40 5 -12 0 60.09 8.70 -5 -12 0 67.19 10.40 5 -12 0 66.99 9.10 5 -12 0 73.79 15.40 -5 -12 0 78.49 9.70 5 -12 0 73.69 10.70 5 -12 0 73.59 11.50 -5 -12 0 66.59 10.40 -5 -12 0 80.89 11.90 -5 12 0 75.59 9.20 -5 12 0 81.79 10.50 6 -12 0 150.98 12.90 6 -12 0 102.19 12.50 -6 -12 0 112.59 13.10 -6 -12 0 92.49 12.70 6 -12 0 118.89 13.00 6 -12 0 113.49 14.90 -6 -12 0 111.19 11.40 -6 -12 0 114.49 13.20 -6 -12 0 110.69 12.00 6 -12 0 121.69 17.30 6 -12 0 103.39 13.30 -6 -12 0 107.89 12.40 -6 -12 0 112.69 11.40 -6 12 0 101.69 11.50 -6 12 0 108.19 12.50 7 -12 0 -3.00 5.00 7 -12 0 -4.30 4.10 -7 -12 0 2.40 5.70 -7 -12 0 1.70 4.60 7 -12 0 -4.30 4.30 -7 -12 0 -2.00 3.60 -7 -12 0 -5.10 3.40 -7 -12 0 6.30 5.20 7 -12 0 -2.80 6.80 7 -12 0 0.60 5.70 7 -12 0 -5.80 4.30 -7 -12 0 10.40 6.20 -7 -12 0 -0.90 4.70 7 12 0 0.30 5.10 -7 12 0 4.60 5.00 -7 12 0 -4.30 3.70 8 -12 0 115.19 12.70 8 -12 0 131.29 14.40 -8 -12 0 104.39 12.80 8 -12 0 117.39 13.80 -8 -12 0 116.39 13.70 -8 -12 0 124.59 12.50 -8 -12 0 108.89 12.00 8 -12 0 93.69 17.00 -8 -12 0 117.19 13.60 8 -12 0 123.69 13.50 8 12 0 119.39 12.80 -8 12 0 123.29 13.80 -8 12 0 101.29 11.90 9 -12 0 72.09 16.90 -9 -12 0 79.79 13.60 -9 -12 0 75.09 11.80 9 -12 0 80.79 19.60 9 -12 0 107.79 18.80 9 -12 0 69.19 13.40 9 -12 0 80.79 16.40 -9 -12 0 64.59 13.10 -9 12 0 67.39 16.90 9 12 0 79.29 13.80 -10 -12 0 180.08 17.10 -10 -12 0 175.58 16.30 -10 -12 0 169.18 16.60 -10 -12 0 199.48 16.10 -10 -12 0 167.38 16.90 10 -12 0 193.48 17.10 10 -12 0 147.19 16.80 10 -12 0 201.08 17.60 10 -12 0 194.78 17.30 10 -12 0 191.38 24.20 -10 12 0 177.98 15.60 -10 12 0 164.08 16.70 10 12 0 188.98 16.50 10 12 0 179.08 16.80 -11 -12 0 2.60 5.60 -11 -12 0 0.70 7.10 -11 -12 0 6.30 4.00 11 -12 0 8.10 8.30 11 -12 0 6.80 5.70 -11 -12 0 15.90 5.70 11 -12 0 7.90 8.80 -11 -12 0 6.50 4.40 -11 12 0 1.30 4.70 -11 12 0 0.60 3.60 11 12 0 12.30 5.50 11 12 0 6.90 5.10 -12 -12 0 -4.10 4.30 12 -12 0 -2.70 6.20 -12 -12 0 -1.40 3.20 12 -12 0 -4.90 4.90 -12 -12 0 1.90 3.10 -12 12 0 0.30 3.20 -12 12 0 -0.80 4.30 12 12 0 0.60 3.90 12 12 0 2.40 4.40 -13 -12 0 12.90 6.30 13 -12 0 2.70 6.60 -13 -12 0 0.50 7.00 -13 -12 0 11.80 4.50 13 -12 0 30.30 8.30 -13 12 0 17.00 4.90 13 12 0 2.40 7.90 13 12 0 16.00 5.10 -13 12 0 14.20 4.50 13 12 0 7.60 5.40 -14 -12 0 42.30 5.90 14 12 0 15.20 6.00 14 12 0 38.70 5.80 -14 12 0 35.40 5.80 -14 12 0 31.90 5.30 0 -13 0 -2.60 4.00 0 -13 0 12.30 7.40 0 -13 0 -4.80 4.10 0 -13 0 1.20 5.00 -1 -13 0 15.80 5.70 -1 -13 0 12.50 5.80 1 -13 0 12.30 5.20 1 -13 0 12.30 5.50 1 -13 0 15.10 6.60 1 -13 0 9.80 4.20 -1 -13 0 17.40 5.20 1 -13 0 14.20 6.30 -1 -13 0 12.60 5.60 -1 -13 0 10.60 5.10 2 -13 0 55.09 10.30 -2 -13 0 51.29 8.50 2 -13 0 47.40 8.10 -2 -13 0 57.69 8.90 2 -13 0 57.59 10.90 -2 -13 0 63.59 10.60 2 -13 0 51.19 9.00 -2 -13 0 51.39 8.50 2 -13 0 55.59 8.60 -2 -13 0 61.59 9.90 -2 -13 0 62.99 9.90 -2 13 0 61.99 7.00 2 13 0 46.80 8.20 -2 13 0 51.29 8.60 -3 -13 0 13.90 5.00 3 -13 0 18.60 6.30 -3 -13 0 16.20 5.20 -3 -13 0 19.40 6.20 3 -13 0 17.00 6.20 -3 -13 0 15.20 6.60 -3 -13 0 22.00 7.10 3 -13 0 18.50 7.80 3 -13 0 11.90 10.50 -3 -13 0 16.20 6.00 3 -13 0 10.10 4.60 3 -13 0 24.50 10.00 3 -13 0 13.00 5.30 -3 13 0 13.30 5.30 3 13 0 11.00 5.40 -3 13 0 12.50 5.00 4 -13 0 78.49 12.80 4 -13 0 79.39 10.10 4 -13 0 72.79 10.70 -4 -13 0 77.49 10.10 4 -13 0 108.69 11.80 -4 -13 0 75.69 10.60 -4 -13 0 88.99 11.40 -4 -13 0 69.89 11.70 4 -13 0 51.09 10.70 4 -13 0 68.09 14.20 -4 -13 0 73.99 9.00 -4 -13 0 64.59 9.60 4 -13 0 70.89 11.50 -4 13 0 64.29 8.80 4 13 0 80.79 11.50 5 -13 0 2.70 4.10 -5 -13 0 9.10 5.20 -5 -13 0 -2.70 3.30 5 -13 0 1.70 6.70 -5 -13 0 -3.10 2.90 5 -13 0 -0.30 4.60 5 -13 0 -5.90 3.70 5 -13 0 -5.10 3.90 5 -13 0 -5.20 4.40 -5 -13 0 0.50 4.50 -5 -13 0 0.60 5.00 -5 13 0 3.80 4.90 -5 13 0 -0.70 3.60 5 13 0 0.00 3.80 6 -13 0 15.60 6.20 -6 -13 0 13.00 5.00 -6 -13 0 15.60 5.10 6 -13 0 14.20 7.20 -6 -13 0 20.20 6.20 6 -13 0 12.10 5.10 6 -13 0 10.80 6.30 -6 -13 0 22.20 6.90 6 -13 0 12.60 7.70 -6 -13 0 19.70 6.50 6 -13 0 12.10 6.20 -6 -13 0 21.10 6.90 -6 13 0 8.60 5.70 6 13 0 20.10 5.60 -6 13 0 14.00 5.30 -7 -13 0 179.98 17.30 -7 -13 0 170.18 17.30 -7 -13 0 143.69 16.10 7 -13 0 190.88 17.00 -7 -13 0 167.48 15.40 7 -13 0 191.68 23.00 7 -13 0 170.18 16.30 -7 -13 0 173.28 15.60 7 -13 0 173.98 18.60 -7 -13 0 189.28 16.70 7 -13 0 179.98 17.30 7 -13 0 187.58 17.90 7 13 0 169.78 15.80 -7 13 0 168.38 15.90 8 -13 0 16.50 7.90 -8 -13 0 19.10 8.30 8 -13 0 22.00 16.90 9 -13 0 110.09 12.30 9 -13 0 91.39 12.70 -9 -13 0 121.69 12.70 -9 -13 0 122.19 14.30 9 -13 0 116.89 13.10 -9 -13 0 104.49 12.20 -9 -13 0 117.39 13.30 9 -13 0 109.99 13.40 -9 -13 0 113.89 12.00 9 -13 0 119.59 18.50 -9 13 0 96.89 12.60 9 13 0 135.49 13.50 9 13 0 107.69 12.30 -9 13 0 106.59 12.10 10 -13 0 81.19 10.20 -10 -13 0 65.09 8.50 -10 -13 0 74.89 10.00 -10 -13 0 67.69 10.70 10 -13 0 73.69 11.40 -10 -13 0 83.09 11.00 10 -13 0 45.50 12.90 10 -13 0 81.19 11.70 10 -13 0 69.39 11.10 -10 -13 0 71.29 9.40 10 13 0 54.59 9.00 -10 13 0 65.19 10.20 10 13 0 77.19 10.30 -11 -13 0 7.80 4.50 -11 -13 0 10.00 4.80 -11 -13 0 7.60 3.60 11 -13 0 3.90 6.00 11 -13 0 -6.50 8.10 -11 -13 0 -8.80 5.60 -11 -13 0 4.20 6.20 -11 13 0 3.10 3.80 11 13 0 9.90 5.00 11 13 0 4.80 4.90 -11 13 0 5.70 6.30 12 -13 0 15.10 5.60 -12 -13 0 14.80 4.70 -12 -13 0 8.10 4.20 12 -13 0 8.30 7.10 -12 -13 0 2.40 6.10 -12 13 0 12.40 4.90 12 13 0 22.60 7.40 12 13 0 18.10 5.10 -12 13 0 12.40 4.30 -13 -13 0 -1.50 5.20 -13 -13 0 10.40 6.80 13 -13 0 -1.00 7.30 -13 13 0 -1.60 3.20 13 13 0 7.60 6.00 13 13 0 -14.30 9.20 -13 13 0 0.80 2.50 13 13 0 -7.00 5.10 0 -14 0 34.80 7.30 0 -14 0 45.90 8.20 0 -14 0 55.59 8.50 0 -14 0 39.20 7.30 0 -14 0 38.50 8.70 0 -14 0 51.39 9.80 1 -14 0 51.79 10.00 -1 -14 0 41.80 7.70 1 -14 0 47.20 8.20 1 -14 0 46.90 9.20 -1 -14 0 42.60 9.00 -1 -14 0 49.50 9.10 1 -14 0 44.10 10.70 -1 -14 0 67.39 8.90 1 -14 0 35.40 7.80 1 -14 0 36.60 7.60 -1 -14 0 51.09 9.80 -1 -14 0 45.70 8.40 -1 -14 0 37.70 7.50 -1 14 0 36.00 8.20 2 -14 0 26.10 7.10 -2 -14 0 46.80 8.90 -2 -14 0 36.00 7.60 2 -14 0 45.90 8.60 2 -14 0 48.10 8.30 2 -14 0 68.59 10.80 -2 -14 0 49.99 9.40 -2 -14 0 43.80 8.70 2 -14 0 49.80 9.80 2 -14 0 34.30 7.80 -2 -14 0 40.00 7.70 -2 -14 0 35.50 7.10 -2 14 0 52.09 8.00 2 14 0 54.29 8.70 -3 -14 0 260.17 22.10 3 -14 0 235.58 26.20 -3 -14 0 260.37 21.20 3 -14 0 255.27 21.30 -3 -14 0 265.77 22.20 -3 -14 0 272.27 22.80 -3 -14 0 265.57 21.60 3 -14 0 284.97 23.30 3 -14 0 275.77 23.80 3 -14 0 251.87 21.00 3 -14 0 251.67 21.50 -3 -14 0 262.77 20.70 3 -14 0 270.57 22.30 -3 14 0 296.57 22.70 3 14 0 270.77 20.60 4 -14 0 14.90 8.70 -4 -14 0 36.40 7.70 -4 -14 0 30.30 6.00 4 -14 0 57.09 8.30 -4 -14 0 25.50 6.60 4 -14 0 40.20 9.20 4 -14 0 31.80 7.40 -4 -14 0 35.00 8.20 4 -14 0 28.50 7.10 -4 -14 0 27.30 8.10 4 -14 0 28.10 7.40 -4 -14 0 31.50 7.90 4 14 0 24.70 6.20 -5 -14 0 115.19 11.90 5 -14 0 118.69 13.80 -5 -14 0 123.49 13.20 -5 -14 0 135.49 13.00 5 -14 0 142.79 13.60 5 -14 0 122.19 15.30 -5 -14 0 124.59 14.30 -5 -14 0 141.89 14.30 5 -14 0 121.59 13.80 5 -14 0 120.29 13.40 5 -14 0 108.59 16.90 -5 -14 0 126.89 14.30 -5 14 0 129.99 13.70 5 14 0 114.19 12.70 -5 14 0 103.89 12.00 -6 -14 0 87.29 10.10 6 -14 0 78.39 12.10 -6 -14 0 95.69 11.50 -6 -14 0 119.39 13.50 6 -14 0 102.09 11.60 -6 -14 0 89.09 10.80 6 -14 0 89.99 11.90 -6 -14 0 108.99 12.40 6 -14 0 95.39 12.30 -6 -14 0 95.19 12.90 6 -14 0 107.39 13.90 6 14 0 87.19 10.80 -6 14 0 74.69 10.80 7 -14 0 50.99 15.80 7 -14 0 35.10 9.70 -7 -14 0 55.79 10.80 -7 -14 0 46.60 9.50 7 -14 0 46.10 9.30 -7 -14 0 46.60 12.10 7 -14 0 51.79 13.00 7 -14 0 46.10 10.10 7 -14 0 46.30 9.90 -7 -14 0 45.30 11.00 -7 -14 0 38.50 7.80 -7 -14 0 20.30 8.30 7 14 0 28.50 8.10 -7 14 0 43.70 8.80 -8 -14 0 78.59 11.80 -8 -14 0 81.29 10.30 8 -14 0 73.89 11.20 8 -14 0 83.89 15.10 -8 -14 0 72.09 11.40 -8 -14 0 73.59 10.00 8 -14 0 82.19 10.80 8 -14 0 66.29 11.40 -8 -14 0 74.49 11.30 8 -14 0 53.49 9.30 -8 14 0 87.99 11.20 -8 14 0 75.59 9.90 8 14 0 81.49 10.30 9 -14 0 55.89 9.20 -9 -14 0 46.80 9.00 -9 -14 0 44.20 8.70 9 -14 0 41.90 8.60 9 -14 0 64.09 14.60 -9 -14 0 47.20 9.70 9 -14 0 32.60 7.70 9 -14 0 38.90 8.40 -9 -14 0 50.29 8.10 -9 -14 0 36.00 7.40 9 14 0 41.40 7.70 -9 14 0 51.39 8.00 10 -14 0 61.49 13.10 -10 -14 0 52.49 8.80 -10 -14 0 60.99 9.30 -10 -14 0 69.89 10.80 10 -14 0 80.79 10.10 10 -14 0 35.50 8.50 10 -14 0 37.40 10.80 10 -14 0 53.79 11.20 -10 -14 0 72.99 9.40 -10 -14 0 66.89 13.00 -10 14 0 77.19 9.60 10 14 0 74.39 9.00 10 14 0 64.69 10.90 -11 -14 0 9.50 4.50 -11 -14 0 1.50 4.60 11 -14 0 13.60 5.70 -11 -14 0 6.40 5.10 -11 -14 0 1.80 3.20 11 -14 0 4.10 7.30 -11 14 0 1.50 3.90 11 14 0 7.80 4.60 11 14 0 -5.10 8.50 -11 14 0 16.40 5.00 12 -14 0 2.30 5.90 12 -14 0 4.20 4.70 -12 -14 0 8.00 4.80 -12 -14 0 5.00 6.00 12 14 0 -6.20 5.40 -12 14 0 4.00 3.50 12 14 0 20.80 5.00 -12 14 0 8.20 4.40 0 -15 0 8.20 5.70 0 -15 0 -1.10 4.10 0 -15 0 1.00 3.70 0 -15 0 -1.80 3.90 0 -15 0 -6.00 4.50 0 -15 0 0.30 5.30 0 15 0 -3.60 4.00 1 -15 0 147.09 13.40 1 -15 0 117.99 12.50 -1 -15 0 126.39 14.00 -1 -15 0 135.39 13.40 -1 -15 0 111.79 12.70 1 -15 0 128.59 14.60 1 -15 0 94.89 12.20 -1 -15 0 111.59 11.80 1 -15 0 107.79 13.90 -1 -15 0 122.89 14.50 1 -15 0 101.79 12.40 -1 -15 0 120.49 13.80 -1 -15 0 115.29 12.40 -1 15 0 109.99 12.50 -2 -15 0 7.80 5.30 2 -15 0 8.40 5.20 2 -15 0 9.30 6.60 -2 -15 0 13.70 6.80 2 -15 0 8.30 6.40 -2 -15 0 9.00 4.70 -2 -15 0 12.30 6.60 -2 -15 0 8.10 4.80 2 -15 0 8.80 5.20 2 -15 0 7.70 4.90 2 -15 0 14.80 6.10 -2 -15 0 8.20 6.00 -2 15 0 8.60 5.00 3 -15 0 43.40 9.80 3 -15 0 35.10 7.50 -3 -15 0 43.90 8.90 3 -15 0 29.70 7.80 -3 -15 0 42.70 7.50 -3 -15 0 32.80 8.20 -3 -15 0 33.40 7.40 3 -15 0 40.20 10.00 -3 -15 0 53.79 10.30 3 -15 0 32.60 7.20 -3 -15 0 36.20 7.80 3 -15 0 27.80 7.20 3 15 0 39.20 7.10 -3 15 0 37.50 7.70 4 -15 0 -4.70 4.00 4 -15 0 -0.90 4.90 -4 -15 0 -0.40 3.40 -4 -15 0 -0.80 3.90 -4 -15 0 6.70 5.80 -4 -15 0 2.70 6.00 4 -15 0 4.80 8.50 4 -15 0 -7.30 3.90 -4 -15 0 0.10 4.30 4 -15 0 0.70 5.40 4 -15 0 1.00 4.30 -4 -15 0 2.30 5.20 4 15 0 -3.80 3.70 -4 15 0 2.80 4.70 -5 -15 0 44.80 10.10 5 -15 0 32.00 7.60 -5 -15 0 37.50 10.30 5 -15 0 42.70 8.70 -5 -15 0 52.59 8.70 -5 -15 0 33.70 6.60 -5 -15 0 48.30 8.50 5 -15 0 32.90 9.10 5 -15 0 34.10 8.30 5 -15 0 32.80 7.60 -5 -15 0 44.20 9.60 5 -15 0 32.50 9.70 -5 15 0 39.50 8.20 5 15 0 32.50 8.00 -5 15 0 24.90 6.60 -6 -15 0 5.60 5.20 -6 -15 0 0.30 4.30 -6 -15 0 3.60 4.40 6 -15 0 1.50 4.50 6 -15 0 8.60 6.70 6 -15 0 4.70 5.40 6 -15 0 3.10 5.00 -6 -15 0 7.50 4.40 6 -15 0 2.20 6.10 6 -15 0 4.50 5.00 -6 -15 0 9.00 6.30 -6 15 0 -1.30 4.10 6 15 0 7.60 4.40 -7 -15 0 45.70 9.80 7 -15 0 36.60 8.70 7 -15 0 34.30 10.30 -7 -15 0 43.30 8.40 -7 -15 0 45.30 9.50 -7 -15 0 31.90 6.80 7 -15 0 33.20 7.70 -7 -15 0 36.60 7.60 7 -15 0 28.80 7.40 7 -15 0 28.80 7.50 -7 -15 0 32.10 7.30 7 15 0 41.10 7.50 -7 15 0 28.20 6.90 8 -15 0 -3.50 5.10 -8 -15 0 0.30 5.40 8 -15 0 4.80 7.30 8 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3.90 0 -16 0 82.29 10.10 0 -16 0 68.19 11.30 0 -16 0 61.59 10.30 0 -16 0 88.39 10.70 0 -16 0 52.09 9.30 1 -16 0 40.40 8.10 1 -16 0 28.20 8.30 1 -16 0 30.50 7.50 -1 -16 0 35.60 7.60 -1 -16 0 49.30 9.40 1 -16 0 47.70 8.50 1 -16 0 31.20 7.30 -1 -16 0 32.80 8.80 1 -16 0 40.50 9.60 -1 -16 0 30.10 7.40 -1 -16 0 38.60 8.80 -1 -16 0 34.00 7.10 1 16 0 31.50 7.20 -1 16 0 29.60 7.00 2 -16 0 8.10 5.30 -2 -16 0 17.70 6.90 -2 -16 0 6.80 5.00 2 -16 0 22.40 6.50 2 -16 0 7.10 5.20 -2 -16 0 11.40 5.70 2 -16 0 13.70 6.80 2 -16 0 13.90 7.00 2 -16 0 8.20 5.10 -2 -16 0 18.70 5.60 -2 -16 0 32.20 8.40 -2 16 0 3.20 4.90 3 -16 0 88.89 14.20 -3 -16 0 90.29 14.10 -3 -16 0 75.49 17.00 -3 -16 0 70.09 16.60 3 -16 0 68.79 15.50 4 -16 0 -2.40 4.50 -4 -16 0 10.10 6.30 -4 -16 0 13.70 7.30 -4 -16 0 0.40 3.50 -4 -16 0 4.60 4.60 -4 -16 0 -1.60 3.90 4 -16 0 5.70 6.00 -4 -16 0 -2.00 5.20 4 -16 0 1.50 5.20 4 -16 0 1.10 5.00 4 -16 0 1.50 4.00 -4 16 0 8.70 5.20 4 16 0 2.60 4.00 5 -16 0 17.60 9.40 -5 -16 0 32.00 8.00 5 -16 0 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73.39 14.00 -13 -10 3 92.39 12.00 13 -10 -3 63.49 11.50 13 10 -3 110.09 12.80 -13 10 3 97.99 12.60 -13 10 3 109.59 12.40 -12 -10 3 8.10 6.00 -12 -10 3 8.60 5.60 -12 -10 3 3.80 4.00 -12 -10 3 6.80 5.80 -12 -10 3 6.80 4.80 12 -10 -3 1.70 5.10 -12 -10 3 7.80 5.70 12 -10 -3 1.60 7.80 12 -10 -3 4.20 6.30 -12 10 3 9.60 5.90 -12 10 3 7.80 5.30 -12 10 3 8.40 4.90 12 10 -3 9.40 5.50 11 -10 -3 78.49 13.70 11 -10 -3 99.49 12.80 -11 -10 3 113.19 12.50 -11 -10 3 113.49 13.50 -11 -10 3 111.49 13.40 -11 -10 3 116.69 15.50 -11 -10 3 114.29 15.60 11 -10 -3 130.19 20.60 -11 -10 3 121.99 13.30 11 10 -3 103.19 17.00 -11 10 3 113.09 13.80 -11 10 3 136.89 13.30 -11 10 3 122.49 17.60 -10 -10 3 -4.00 3.70 10 -10 -3 1.30 5.30 -10 -10 3 4.10 5.90 10 -10 -3 4.80 4.60 10 -10 -3 3.80 7.60 -10 -10 3 -0.10 4.40 -10 -10 3 12.40 6.40 -10 -10 3 -0.90 3.60 -10 -10 3 -1.90 4.40 -10 10 3 3.70 5.30 -10 10 3 -4.30 4.10 -10 10 3 0.60 5.90 10 10 -3 3.10 5.00 -9 -10 3 24.30 6.20 9 -10 -3 19.40 9.80 -9 -10 3 20.20 7.20 9 -10 -3 24.90 13.00 -9 -10 3 23.10 7.00 -9 -10 3 20.10 5.80 9 -10 -3 28.00 7.20 -9 -10 3 20.60 6.40 -9 -10 3 32.20 7.50 9 -10 -3 19.10 6.10 9 -10 -3 13.90 5.50 -9 10 3 18.90 6.40 -9 10 3 27.90 7.30 -9 10 3 22.40 7.40 9 10 -3 22.30 6.60 -8 -10 3 77.89 11.40 -8 -10 3 69.59 9.00 8 -10 -3 57.39 9.70 8 -10 -3 80.99 11.80 8 -10 -3 64.29 14.60 -8 -10 3 66.39 8.80 -8 10 3 65.39 10.40 -8 10 3 63.09 9.80 8 10 -3 76.79 9.80 -7 -10 3 101.09 18.80 7 -10 -3 120.09 12.80 -7 -10 3 98.29 10.70 -7 -10 3 106.59 12.50 7 -10 -3 89.99 11.90 7 -10 -3 126.89 11.80 -7 -10 3 106.09 11.90 7 -10 -3 87.99 12.80 -7 10 3 114.99 11.60 -7 10 3 105.49 13.80 -6 -10 3 84.49 12.20 -6 -10 3 73.79 9.60 -6 -10 3 78.59 9.30 -6 -10 3 74.19 9.50 6 -10 -3 70.69 9.20 6 -10 -3 92.69 16.20 6 -10 -3 77.29 9.10 -6 -10 3 66.59 10.60 6 -10 -3 80.29 12.50 -6 -10 3 82.59 9.70 6 -10 -3 81.69 13.00 -6 -10 3 90.09 13.40 6 -10 -3 91.89 12.30 -6 10 3 87.99 11.30 -6 10 3 83.19 9.30 -5 -10 3 87.59 10.60 5 -10 -3 65.39 8.50 5 -10 -3 92.09 11.90 -5 -10 3 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17.80 3.00 2 -10 3 58.99 9.30 -2 -10 -3 70.09 7.90 2 -10 3 55.99 8.20 -2 -10 -3 76.99 10.40 2 -10 3 63.29 8.60 -2 -10 -3 64.69 9.50 2 -10 3 75.09 10.10 2 -10 3 59.09 8.20 -2 -10 -3 63.29 7.30 -2 10 -3 57.79 7.10 3 -10 3 232.38 18.40 -3 -10 -3 202.28 18.30 3 -10 3 227.68 23.20 3 -10 3 225.68 17.60 -3 -10 -3 218.58 17.60 -3 -10 -3 185.08 22.80 -3 -10 -3 222.78 18.70 -3 10 -3 228.88 16.90 4 -10 3 0.00 6.80 4 -10 3 14.50 7.90 4 -10 3 6.80 4.50 -4 -10 -3 11.20 4.40 4 -10 3 5.60 6.60 -4 -10 -3 3.00 3.80 4 -10 3 4.50 4.40 -4 -10 -3 6.90 4.40 -4 -10 -3 -4.30 4.50 4 -10 3 6.90 4.90 4 -10 3 6.60 3.90 4 10 3 10.50 4.80 -4 10 -3 9.10 4.10 -5 -10 -3 92.99 11.50 5 -10 3 79.49 9.60 5 -10 3 106.29 11.20 -5 -10 -3 95.39 10.00 -5 -10 -3 105.09 10.70 -5 -10 -3 91.39 11.10 5 -10 3 102.29 15.50 -5 -10 -3 76.59 10.40 5 -10 3 97.69 11.60 5 -10 3 79.69 10.60 -5 -10 -3 104.19 9.70 5 -10 3 102.79 11.10 -5 10 -3 88.49 10.10 5 10 3 89.89 11.00 5 10 3 113.59 15.70 6 -10 3 8.30 6.30 -6 -10 -3 7.00 5.20 -6 -10 -3 3.20 4.90 -6 -10 -3 16.20 5.00 6 -10 3 3.00 4.30 -6 -10 -3 11.30 4.30 -6 -10 -3 7.10 4.00 -6 -10 -3 4.40 3.80 6 -10 3 2.30 4.60 6 -10 3 5.10 8.20 6 -10 3 7.80 5.70 6 -10 3 2.30 4.40 -6 10 -3 6.00 5.40 -6 10 -3 0.80 4.00 6 10 3 -3.90 4.40 6 10 3 2.60 4.80 -7 -10 -3 153.68 14.20 7 -10 3 189.18 15.80 -7 -10 -3 147.59 15.90 7 -10 3 157.58 15.20 7 -10 3 159.08 16.20 -7 -10 -3 162.78 14.60 -7 -10 -3 180.78 16.40 7 -10 3 153.68 15.70 -7 -10 -3 167.98 14.30 7 -10 3 111.29 18.60 -7 -10 -3 168.18 15.00 7 -10 3 157.88 15.90 7 10 3 152.88 15.00 7 10 3 180.08 18.80 8 -10 3 5.80 4.70 8 -10 3 -6.60 6.10 8 -10 3 0.10 4.40 -8 -10 -3 22.50 7.40 -8 -10 -3 1.30 4.00 -8 -10 -3 5.50 5.90 8 -10 3 -4.20 4.70 -8 -10 -3 1.90 3.50 8 -10 3 3.20 6.20 -8 -10 -3 3.60 4.70 -8 -10 -3 4.90 4.30 8 -10 3 1.80 4.90 -8 10 -3 -4.40 3.90 8 10 3 -0.10 3.90 8 10 3 -3.10 5.10 -8 10 -3 0.60 4.10 -9 -10 -3 16.00 6.40 9 -10 3 12.80 6.60 9 -10 3 8.60 5.20 -9 -10 -3 7.80 5.20 -9 -10 -3 9.50 4.90 9 -10 3 13.30 7.00 9 -10 3 10.20 5.10 9 -10 3 8.00 5.90 -9 -10 -3 17.30 5.60 9 -10 3 17.40 10.30 -9 10 -3 14.30 5.60 -9 10 -3 10.50 5.80 9 10 3 18.30 6.60 9 10 3 17.70 6.20 10 -10 3 -2.00 4.80 10 -10 3 10.90 6.40 -10 -10 -3 0.30 3.90 10 -10 3 1.20 4.40 -10 -10 -3 -2.30 4.60 10 -10 3 -2.30 8.30 -10 -10 -3 10.00 5.90 10 -10 3 -3.00 4.50 -10 -10 -3 0.10 3.90 10 10 3 -0.40 4.60 -10 10 -3 -3.00 3.90 10 10 3 4.90 4.70 11 -10 3 17.30 6.70 11 -10 3 20.10 6.50 11 -10 3 22.80 6.90 11 -10 3 5.00 9.00 -11 -10 -3 7.20 4.40 -11 -10 -3 12.00 5.00 -11 -10 -3 18.50 9.00 11 -10 3 6.40 5.60 -11 10 -3 8.30 5.00 11 10 3 10.90 5.00 -11 10 -3 8.60 4.60 11 10 3 13.80 5.80 12 -10 3 26.50 7.20 -12 -10 -3 33.50 7.80 -12 -10 -3 36.90 7.70 12 -10 3 25.00 15.70 12 -10 3 18.10 6.70 12 -10 3 23.90 6.70 -12 10 -3 28.40 6.00 12 10 3 40.00 7.80 12 10 3 49.99 10.00 13 -10 3 6.30 7.50 -13 -10 -3 27.20 5.50 13 -10 3 23.00 6.50 -13 -10 -3 29.20 5.30 -13 10 -3 13.80 7.30 -13 10 -3 16.90 4.50 13 10 3 15.90 5.40 13 10 3 22.10 6.40 -13 10 -3 17.70 5.60 -14 -10 -3 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14.10 6.30 -11 -11 3 7.60 5.50 11 11 -3 10.70 5.30 -11 11 3 6.80 4.40 -11 11 3 5.40 6.40 -11 11 3 11.70 5.50 -10 -11 3 92.59 11.10 10 -11 -3 104.09 14.00 -10 -11 3 90.99 10.20 -10 -11 3 105.59 16.00 10 -11 -3 93.69 13.00 -10 -11 3 84.99 12.10 -10 -11 3 92.49 12.60 -10 -11 3 123.39 13.80 10 -11 -3 73.69 16.40 -10 11 3 87.89 13.30 -10 11 3 93.09 12.90 10 11 -3 108.59 12.00 9 -11 -3 184.38 16.90 -9 -11 3 162.78 16.20 9 -11 -3 146.59 20.50 -9 -11 3 168.58 14.70 -9 -11 3 163.58 16.60 9 -11 -3 162.78 15.60 -9 -11 3 175.68 15.70 9 -11 -3 148.29 15.30 -9 -11 3 136.49 15.80 -9 -11 3 139.49 16.10 -9 11 3 152.28 16.60 -9 11 3 167.58 16.00 -9 11 3 154.08 15.00 9 11 -3 168.38 15.90 -8 -11 3 24.70 7.60 -8 -11 3 16.50 5.50 -8 -11 3 15.90 6.50 -8 -11 3 11.20 6.40 -8 -11 3 20.30 7.80 -8 -11 3 14.70 5.70 8 -11 -3 14.30 6.00 8 -11 -3 23.70 10.70 8 -11 -3 22.40 6.50 8 -11 -3 28.30 6.40 -8 11 3 14.90 6.30 8 11 -3 15.00 6.10 -8 11 3 19.90 5.80 -8 11 3 17.00 7.20 7 -11 -3 422.46 29.50 -7 -11 3 388.36 30.40 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5.90 4 -11 -3 11.90 8.40 4 -11 -3 6.80 4.80 -4 -11 3 9.40 5.90 -4 -11 3 11.50 5.00 -4 11 3 17.80 4.70 3 -11 -3 80.89 9.00 -3 -11 3 78.69 10.20 -3 -11 3 96.09 10.00 -3 -11 3 94.39 9.50 3 -11 -3 79.69 10.90 -3 -11 3 86.69 10.70 -3 -11 3 95.19 10.20 3 -11 -3 111.19 12.20 -3 -11 3 86.59 10.60 3 -11 -3 95.89 9.90 3 -11 -3 79.29 10.40 -3 11 3 81.89 11.00 2 -11 -3 28.40 6.50 -2 -11 3 21.10 6.20 -2 -11 3 29.40 6.80 -2 -11 3 30.60 6.40 2 -11 -3 38.30 8.40 2 -11 -3 27.60 7.20 -2 -11 3 33.50 7.10 -2 -11 3 29.70 6.00 2 -11 -3 19.00 5.50 -2 -11 3 37.00 8.70 2 -11 -3 31.70 5.80 -2 11 3 26.10 4.60 -2 11 3 36.20 9.90 -1 -11 3 228.48 17.80 1 -11 -3 221.88 17.10 1 -11 -3 211.98 17.90 1 -11 -3 217.38 17.90 1 -11 -3 220.48 19.60 -1 -11 3 211.08 19.70 -1 -11 3 176.68 19.30 -1 -11 3 208.48 18.40 -1 -11 3 207.08 19.80 1 -11 -3 230.68 18.50 -1 11 3 206.98 15.20 0 -11 -3 43.00 8.40 0 -11 -3 54.09 8.80 0 -11 3 51.09 8.10 0 -11 -3 49.10 7.80 0 -11 3 47.80 9.90 0 -11 3 38.70 9.50 0 -11 3 44.10 10.80 0 -11 -3 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14 -3 23.30 6.30 8 14 3 27.30 6.50 9 -14 3 -2.30 4.30 9 -14 3 -6.00 7.00 9 -14 3 -4.70 4.90 9 -14 3 15.80 8.60 9 -14 3 4.20 6.80 -9 -14 -3 2.40 3.80 -9 -14 -3 -2.40 3.90 -9 -14 -3 -13.20 5.70 9 14 3 5.00 7.60 9 14 3 0.40 3.90 -9 14 -3 -4.80 4.40 -10 -14 -3 130.99 13.20 10 -14 3 144.29 19.40 10 -14 3 175.38 15.70 10 -14 3 155.48 14.90 -10 -14 -3 163.78 13.90 10 14 3 171.18 14.20 10 14 3 171.98 14.50 -10 14 -3 148.29 13.50 -11 -14 -3 1.00 3.20 11 -14 3 -2.50 5.90 11 -14 3 -3.20 6.10 11 -14 3 -15.10 7.90 -11 -14 -3 0.60 3.20 11 -14 3 -4.20 4.70 -11 14 -3 -0.30 4.30 11 14 3 -1.60 5.50 11 14 3 3.40 3.80 -11 14 -3 -1.40 2.70 -12 -14 -3 8.60 4.20 12 -14 3 4.80 7.20 -12 14 -3 10.50 5.30 -12 -15 3 62.69 10.00 -12 -15 3 91.39 9.20 -12 -15 3 59.49 8.50 -12 -15 3 81.19 12.20 12 -15 -3 80.99 10.00 12 15 -3 73.69 9.50 -12 15 3 80.19 10.20 -11 -15 3 -1.90 3.10 11 -15 -3 -2.00 4.80 11 -15 -3 2.10 6.70 -11 -15 3 1.90 4.00 -11 -15 3 5.10 5.20 -11 -15 3 -1.20 4.80 -11 -15 3 9.20 5.00 11 15 -3 4.20 4.50 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9.20 -10 -12 4 42.80 9.00 -10 -12 4 37.60 9.50 10 -12 -4 37.70 8.40 -10 -12 4 40.80 9.50 10 -12 -4 48.40 13.30 -10 12 4 37.10 8.20 10 12 -4 44.70 8.20 -10 12 4 46.20 10.30 -9 -12 4 122.99 12.70 -9 -12 4 108.59 13.60 -9 -12 4 106.59 13.20 -9 -12 4 104.39 11.50 9 -12 -4 117.79 12.90 -9 -12 4 127.19 14.00 9 -12 -4 113.29 12.60 -9 -12 4 107.69 13.80 -9 12 4 107.39 12.10 -9 12 4 117.09 14.30 9 12 -4 91.89 11.80 -9 12 4 108.39 13.10 -8 -12 4 279.07 21.90 -8 -12 4 248.28 22.10 -8 -12 4 260.97 20.80 8 -12 -4 254.27 21.70 8 -12 -4 271.47 22.30 8 -12 -4 316.87 21.80 -8 -12 4 242.88 22.00 -8 -12 4 229.78 22.30 8 -12 -4 298.87 29.10 -8 -12 4 230.68 21.80 -8 12 4 258.47 22.80 -8 12 4 248.38 22.20 -8 12 4 235.58 20.90 8 12 -4 282.97 22.40 -7 -12 4 10.40 5.10 7 -12 -4 8.20 8.20 7 -12 -4 10.50 6.30 -7 -12 4 2.80 5.40 7 -12 -4 14.20 5.40 -7 -12 4 9.60 6.40 7 -12 -4 -0.60 5.60 -7 -12 4 4.70 4.40 -7 -12 4 15.30 5.80 7 -12 -4 3.50 5.00 -7 -12 4 1.60 5.90 -7 12 4 7.70 4.80 -7 12 4 8.10 5.80 -6 -12 4 197.58 21.00 6 -12 -4 238.18 21.70 -6 -12 4 236.78 21.00 -6 -12 4 259.47 20.90 6 -12 -4 231.98 28.30 6 -12 -4 237.08 20.10 -6 -12 4 255.37 20.60 6 -12 -4 273.67 21.40 -6 -12 4 249.08 21.20 6 -12 -4 252.97 23.20 -6 -12 4 234.08 20.50 -6 12 4 276.97 20.00 -6 12 4 244.08 21.60 -5 -12 4 32.60 8.80 5 -12 -4 41.40 7.60 -5 -12 4 38.50 9.60 5 -12 -4 34.20 9.10 5 -12 -4 46.80 8.20 5 -12 -4 49.90 7.80 -5 -12 4 43.80 8.80 -5 -12 4 43.40 10.30 -5 -12 4 44.10 7.70 -5 -12 4 45.40 9.20 5 -12 -4 62.89 10.10 -5 -12 4 41.40 7.30 -5 12 4 45.70 7.50 -5 12 4 54.59 11.00 -5 12 4 40.30 8.00 -4 -12 4 6.60 4.10 4 -12 -4 1.50 6.90 -4 -12 4 2.70 4.70 4 -12 -4 -0.40 4.70 -4 -12 4 7.40 6.90 -4 -12 4 3.80 5.60 -4 -12 4 3.50 5.00 -4 -12 4 2.30 3.80 4 -12 -4 2.30 4.20 4 -12 -4 4.00 4.30 -4 12 4 2.20 3.30 -4 12 4 3.20 4.50 -4 12 4 4.30 4.40 -3 -12 4 86.19 10.00 3 -12 -4 87.79 14.20 3 -12 -4 71.49 21.20 3 -12 -4 78.59 9.20 -3 -12 4 68.59 9.00 -3 -12 4 77.09 12.00 -3 -12 4 71.09 13.70 3 -12 -4 89.09 11.40 -3 -12 4 82.99 11.70 3 -12 -4 86.29 9.90 -3 -12 4 78.79 10.40 3 -12 -4 75.89 9.30 3 -12 -4 100.59 10.80 -3 12 4 69.89 7.80 -2 -12 4 29.70 6.10 -2 -12 4 23.40 5.80 2 -12 -4 28.30 6.40 2 -12 -4 25.50 7.70 -2 -12 4 24.50 6.70 2 -12 -4 29.00 6.10 2 -12 -4 19.10 6.40 2 -12 -4 30.30 6.00 2 -12 -4 29.00 6.20 -2 -12 4 17.90 6.90 -2 -12 4 21.00 7.10 -2 -12 4 26.60 7.90 -2 -12 4 21.70 6.20 -2 12 4 28.20 6.50 -2 12 4 22.50 4.90 1 -12 -4 86.09 9.60 1 -12 -4 83.59 12.20 1 -12 -4 83.29 9.60 -1 -12 4 75.39 11.40 -1 -12 4 73.09 9.60 1 -12 -4 89.69 11.30 -1 -12 4 63.69 9.20 1 -12 -4 77.69 9.50 1 -12 -4 85.09 9.50 -1 -12 4 86.69 11.60 -1 -12 4 83.99 11.90 -1 -12 4 76.29 10.20 -1 -12 4 75.69 9.80 -1 12 4 96.09 7.80 -1 12 4 78.79 10.90 -1 12 4 87.79 10.40 0 -12 4 368.16 28.50 0 -12 -4 360.56 28.90 0 -12 4 397.26 30.10 0 -12 -4 378.36 28.00 0 -12 -4 433.46 29.30 0 -12 4 413.46 29.60 0 -12 4 389.06 28.40 0 -12 -4 414.76 28.40 0 -12 -4 403.66 28.10 0 -12 4 430.66 36.50 0 -12 -4 405.56 29.70 0 -12 4 390.06 29.40 0 -12 4 380.56 28.80 0 12 4 380.66 28.90 -1 -12 -4 83.39 9.60 1 -12 4 92.29 11.40 1 -12 4 93.59 12.60 1 -12 4 90.39 20.90 1 -12 4 76.49 10.20 -1 -12 -4 104.59 11.10 1 -12 4 78.59 12.50 -1 -12 -4 87.59 10.10 -1 -12 -4 75.49 9.50 -1 -12 -4 78.19 11.10 1 -12 4 101.49 10.90 1 -12 4 82.69 10.00 -1 -12 -4 114.39 10.60 1 12 4 96.89 10.40 -1 12 -4 88.99 9.20 2 -12 4 454.05 34.00 -2 -12 -4 494.65 36.70 -2 -12 -4 534.25 34.70 2 -12 4 472.55 35.80 -2 -12 -4 498.45 34.90 2 -12 4 481.25 35.10 -2 -12 -4 453.15 33.20 2 -12 4 483.05 40.90 2 -12 4 469.85 34.30 -2 -12 -4 464.05 34.20 -2 -12 -4 489.85 35.60 2 -12 4 484.75 35.90 2 12 4 460.75 33.70 -2 12 -4 529.05 33.30 -3 -12 -4 119.89 12.10 3 -12 4 122.29 12.70 3 -12 4 115.59 14.10 -3 -12 -4 127.29 13.70 3 -12 4 133.49 19.30 -3 -12 -4 111.69 11.40 3 -12 4 126.19 13.40 3 -12 4 103.99 11.70 3 -12 4 131.29 16.40 -3 -12 -4 112.09 11.60 3 -12 4 110.79 12.20 -3 -12 -4 131.59 13.60 -3 12 -4 118.69 11.40 3 12 4 110.69 12.10 -4 -12 -4 122.49 12.70 4 -12 4 119.99 12.90 -4 -12 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68.49 8.30 -6 -13 4 0.70 4.30 -6 -13 4 -0.10 3.90 6 -13 -4 -2.00 5.00 6 -13 -4 1.30 7.10 6 -13 -4 4.40 4.90 -6 -13 4 -7.70 5.60 6 -13 -4 3.60 6.10 -6 -13 4 8.80 7.00 6 -13 -4 13.90 5.00 -6 -13 4 8.50 5.20 -6 -13 4 -1.50 5.00 6 -13 -4 -2.30 3.90 -6 -13 4 2.40 4.60 -6 13 4 3.60 3.60 -6 13 4 7.00 5.40 -5 -13 4 9.00 5.30 -5 -13 4 18.40 6.10 5 -13 -4 2.00 5.40 -5 -13 4 10.00 6.10 -5 -13 4 11.60 7.40 -5 -13 4 12.40 6.50 5 -13 -4 4.20 5.10 5 -13 -4 10.00 6.30 5 -13 -4 4.30 4.70 -5 -13 4 1.00 5.90 5 -13 -4 2.90 7.80 5 -13 -4 8.90 4.60 -5 13 4 10.70 4.10 -5 13 4 12.60 5.90 -5 13 4 6.00 4.40 4 -13 -4 150.08 14.20 -4 -13 4 143.09 16.20 -4 -13 4 135.99 14.00 -4 -13 4 162.48 15.00 -4 -13 4 167.38 16.10 4 -13 -4 134.99 13.90 -4 -13 4 131.59 14.90 4 -13 -4 168.88 15.40 4 -13 -4 163.88 15.70 4 -13 -4 178.68 19.80 4 -13 -4 147.29 13.70 -4 -13 4 167.68 15.70 -4 -13 4 135.29 13.50 -4 13 4 136.19 12.80 -4 13 4 140.69 14.30 -4 13 4 164.88 15.90 -3 -13 4 7.20 5.50 -3 -13 4 0.10 3.90 -3 -13 4 6.40 3.80 -3 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1 -13 4 138.29 15.10 1 -13 4 160.18 16.70 -1 -13 -4 146.79 14.80 1 -13 4 176.08 15.50 1 -13 4 176.48 18.60 -1 -13 -4 163.08 14.60 1 13 4 190.28 17.60 -1 13 -4 137.49 13.40 -2 -13 -4 38.20 7.30 2 -13 4 42.30 8.10 -2 -13 -4 29.00 6.20 -2 -13 -4 30.40 7.90 2 -13 4 37.30 9.10 -2 -13 -4 38.00 6.90 2 -13 4 33.90 7.50 2 -13 4 31.00 7.20 -2 -13 -4 41.50 7.40 2 -13 4 35.30 7.80 2 13 4 41.30 8.20 -2 13 -4 28.60 6.20 -3 -13 -4 187.48 17.30 3 -13 4 182.08 16.70 3 -13 4 180.88 26.10 3 -13 4 166.98 17.30 3 -13 4 156.08 16.10 3 -13 4 196.08 19.00 3 -13 4 160.48 16.20 -3 -13 -4 200.28 16.40 -3 -13 -4 154.68 17.80 -3 -13 -4 177.48 17.40 3 -13 4 175.48 16.90 -3 -13 -4 158.38 15.20 -3 -13 -4 183.48 15.80 -3 13 -4 181.88 15.50 3 13 4 184.88 16.00 4 -13 4 5.30 4.80 4 -13 4 0.60 4.60 -4 -13 -4 5.60 4.30 -4 -13 -4 4.70 5.50 4 -13 4 1.90 6.10 -4 -13 -4 5.10 4.40 -4 -13 -4 -2.40 3.40 4 -13 4 1.90 5.00 -4 -13 -4 4.30 5.00 4 -13 4 5.90 5.00 -4 -13 -4 0.50 3.60 4 -13 4 9.80 8.60 4 13 4 8.50 4.80 -4 13 -4 2.40 4.50 -5 -13 -4 27.50 7.70 5 -13 4 12.30 6.40 -5 -13 -4 31.50 6.50 5 -13 4 24.00 8.00 -5 -13 -4 21.10 6.20 5 -13 4 21.10 7.50 5 -13 4 17.20 6.90 -5 -13 -4 23.00 6.00 5 -13 4 17.80 9.20 5 -13 4 13.10 6.00 -5 -13 -4 24.30 7.60 -5 13 -4 17.30 6.50 5 13 4 24.40 6.50 -5 13 -4 17.20 6.70 6 -13 4 103.49 17.10 -6 -13 -4 113.29 13.50 6 -13 4 109.59 14.10 6 -13 4 127.39 13.50 -6 -13 -4 119.29 12.80 6 -13 4 95.59 12.50 -6 -13 -4 103.89 11.40 -6 -13 -4 108.09 11.10 -6 -13 -4 97.59 12.80 6 -13 4 94.79 12.40 -6 -13 -4 121.59 12.20 6 -13 4 110.59 13.20 -6 13 -4 92.49 12.40 6 13 4 99.89 11.90 7 -13 4 13.60 6.00 -7 -13 -4 20.40 5.50 -7 -13 -4 27.70 6.40 7 -13 4 17.80 6.60 -7 -13 -4 12.60 4.80 -7 -13 -4 7.70 4.80 -7 -13 -4 7.30 6.70 7 -13 4 13.00 6.00 7 -13 4 10.90 8.40 7 -13 4 10.60 5.90 7 13 4 2.90 5.80 7 13 4 22.10 6.10 -8 -13 -4 8.30 4.90 8 -13 4 0.60 7.60 -8 -13 -4 -0.80 3.70 -8 -13 -4 3.50 4.40 8 -13 4 3.00 4.60 8 -13 4 0.10 4.80 8 -13 4 -2.80 5.20 8 -13 4 0.70 4.10 8 13 4 9.60 4.80 8 13 4 6.50 4.90 -8 13 -4 0.50 4.00 -9 -13 -4 50.39 8.20 9 -13 4 63.39 10.10 -9 -13 -4 51.39 8.40 9 -13 4 61.09 10.40 9 -13 4 55.39 9.70 9 -13 4 55.09 14.70 9 -13 4 49.00 9.70 9 13 4 54.19 8.70 9 13 4 49.50 8.40 -9 13 -4 51.69 8.20 9 13 4 56.29 10.00 10 -13 4 2.20 5.10 -10 -13 -4 -1.50 3.20 10 -13 4 -0.30 4.10 10 -13 4 5.10 7.50 -10 -13 -4 0.00 3.40 10 -13 4 -1.70 5.00 10 13 4 -3.30 5.30 10 13 4 1.90 5.10 10 13 4 6.80 4.60 -10 13 -4 -2.60 3.90 11 -13 4 29.50 6.80 11 -13 4 40.80 9.60 -11 -13 -4 31.20 5.70 -11 -13 -4 19.20 4.70 11 -13 4 33.90 8.80 11 -13 4 9.60 7.90 11 13 4 42.80 7.80 11 13 4 17.00 9.50 11 13 4 30.30 6.10 -11 13 -4 25.70 5.20 -11 13 -4 33.50 5.80 -12 -13 -4 0.60 3.50 -12 -13 -4 1.50 2.90 12 -13 4 -0.90 5.20 -12 13 -4 1.90 2.90 12 13 4 0.90 3.50 -13 -14 4 16.50 6.20 -13 -14 4 13.20 6.50 -13 -14 4 2.20 4.60 13 -14 -4 12.50 7.40 13 -14 -4 17.00 6.40 -13 -14 4 15.80 5.10 -13 14 4 10.90 5.30 13 14 -4 12.80 5.30 -12 -14 4 23.50 6.70 -12 -14 4 20.70 8.60 12 -14 -4 6.50 6.60 12 -14 -4 17.00 5.80 -12 -14 4 13.40 6.00 -12 -14 4 20.70 5.40 -12 -14 4 28.00 7.10 12 14 -4 19.50 5.40 -12 14 4 17.50 5.70 -12 14 4 12.20 5.50 -12 14 4 23.20 6.80 -11 -14 4 49.30 8.80 11 -14 -4 46.90 8.60 -11 -14 4 37.20 7.10 -11 -14 4 36.70 8.40 -11 -14 4 44.40 8.40 -11 -14 4 50.39 7.50 11 14 -4 81.39 14.40 -11 14 4 34.50 7.10 11 14 -4 49.70 7.80 -11 14 4 46.20 7.80 -11 14 4 53.69 8.70 -10 -14 4 3.10 5.30 10 -14 -4 5.30 6.50 -10 -14 4 6.20 5.10 -10 -14 4 5.70 4.50 10 -14 -4 11.60 8.40 -10 -14 4 9.70 6.00 10 -14 -4 10.60 5.80 -10 -14 4 -0.10 3.70 -10 14 4 18.20 6.20 -10 14 4 12.60 5.40 -9 -14 4 49.10 10.00 -9 -14 4 44.60 9.10 9 -14 -4 60.39 9.90 9 -14 -4 58.99 9.40 9 -14 -4 54.29 8.80 -9 -14 4 53.39 10.00 -9 -14 4 60.19 8.70 -9 -14 4 48.10 9.70 -9 -14 4 54.69 9.40 9 -14 -4 51.79 13.10 -9 14 4 58.79 10.30 -9 14 4 66.79 10.10 -8 -14 4 107.69 12.20 8 -14 -4 133.29 12.10 -8 -14 4 111.19 13.60 -8 -14 4 98.39 11.20 -8 -14 4 106.79 12.70 8 -14 -4 106.89 16.90 8 -14 -4 104.19 12.60 8 -14 -4 78.39 11.10 -8 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-5 10 252.27 19.30 -11 -5 10 174.58 17.90 -11 -5 10 196.28 18.20 11 -5 -10 213.18 23.60 -11 5 10 198.78 18.10 -11 5 10 222.18 18.30 -11 5 10 224.78 18.60 -11 5 10 226.38 17.90 -11 5 10 219.98 18.30 -11 5 10 209.98 17.50 -10 -5 10 16.70 6.40 -10 -5 10 31.00 7.90 10 -5 -10 24.90 10.10 -10 -5 10 26.30 7.40 -10 -5 10 27.50 7.20 -10 -5 10 20.40 6.80 -10 -5 10 22.40 6.00 -10 5 10 37.20 7.10 -10 5 10 23.10 6.50 -10 5 10 23.90 6.50 -10 5 10 33.00 7.30 -10 5 10 26.50 6.40 -9 -5 10 88.39 11.30 9 -5 -10 92.39 11.20 -9 -5 10 89.19 11.80 9 -5 -10 115.59 15.70 -9 -5 10 88.79 11.60 -9 -5 10 91.79 11.20 -9 -5 10 112.59 12.10 -9 5 10 124.79 11.70 -9 5 10 105.79 11.00 -9 5 10 105.89 15.50 -9 5 10 101.49 11.00 -9 5 10 120.89 12.10 -9 5 10 115.29 11.20 -9 5 10 83.09 11.20 -8 -5 10 7.70 4.70 -8 -5 10 9.40 4.80 8 -5 -10 12.10 7.50 -8 -5 10 5.60 4.90 -8 -5 10 15.30 5.20 -8 -5 10 8.20 5.20 -8 -5 10 11.30 4.80 -8 -5 10 16.60 4.80 8 -5 -10 3.70 5.10 -8 5 10 14.20 5.40 -8 5 10 11.40 4.50 -8 5 10 13.90 7.40 -8 5 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