data_dccLU40 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ; ? ; _chemical_name_common DCC_LU40 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H19 B N2 O' _chemical_formula_weight 398.25 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' 'B' 'B' 0.0013 0.0007 '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' _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 10.4924(4) _cell_length_b 10.6628(4) _cell_length_c 18.4160(4) _cell_angle_alpha 74.5955(19) _cell_angle_beta 84.469(2) _cell_angle_gamma 89.0236(13) _cell_volume 1977.01(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4993 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description tablet _exptl_crystal_colour 'yellow-green dichroic' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.338 _exptl_crystal_F_000 832 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 0.081 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker-Nonius-KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 11869 _diffrn_reflns_av_unetI/netI 0.0846 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.152 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_point_group_measured_fraction_full 0.987 _reflns_number_total 8520 _reflns_number_gt 5186 _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 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _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^)+(0.0697P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8520 _refine_ls_number_parameters 559 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 O1A O -0.03102(12) 0.25594(13) 1.01304(7) 0.0260(3) Uani 1 1 d . . . . . N3A N 0.17225(15) 0.29552(15) 0.96525(8) 0.0219(4) Uani 1 1 d . . . . . N11A N 0.27067(15) 0.20690(16) 0.86070(8) 0.0238(4) Uani 1 1 d . . . . . C2A C 0.06371(18) 0.23739(19) 0.96217(10) 0.0228(4) Uani 1 1 d . . . . . C17A C 0.04714(19) 0.15683(19) 0.91301(10) 0.0241(4) Uani 1 1 d . . . . . C19A C 0.15631(19) 0.14607(19) 0.86523(10) 0.0233(4) Uani 1 1 d . . . . . C36A C 0.26774(19) 0.4837(2) 0.78399(10) 0.0267(5) Uani 1 1 d . . . . . H36A H 0.2239 0.4191 0.7688 0.032 Uiso 1 1 calc R U . . . C4A C 0.2288(2) 0.4239(2) 1.05763(10) 0.0279(5) Uani 1 1 d . . . . . H4A H 0.3163 0.4412 1.0394 0.033 Uiso 1 1 calc R U . . . C8A C 0.15009(19) 0.35518(19) 1.02510(10) 0.0233(4) Uani 1 1 d . . . . . C31A C 0.31929(18) 0.4496(2) 0.85369(10) 0.0243(4) Uani 1 1 d . . . . . C9A C 0.02425(18) 0.33045(19) 1.05352(10) 0.0234(4) Uani 1 1 d . . . . . C21A C 0.41926(19) 0.24797(19) 0.95781(10) 0.0235(4) Uani 1 1 d . . . . . C7A C -0.0342(2) 0.3722(2) 1.11318(10) 0.0277(5) Uani 1 1 d . . . . . H7A H -0.1218 0.3546 1.1310 0.033 Uiso 1 1 calc R U . . . C32A C 0.38297(19) 0.5498(2) 0.87264(11) 0.0281(5) Uani 1 1 d . . . . . H32A H 0.4184 0.5314 0.9199 0.034 Uiso 1 1 calc R U . . . C12A C 0.3486(2) 0.1696(2) 0.80519(10) 0.0278(5) Uani 1 1 d . . . . . H12A H 0.4346 0.1983 0.7898 0.033 Uiso 1 1 calc R U . . . C18A C 0.1604(2) 0.0672(2) 0.81402(10) 0.0264(5) Uani 1 1 d . . . . . C25A C 0.6460(2) 0.2398(2) 0.97681(12) 0.0341(5) Uani 1 1 d . . . . . H25A H 0.7303 0.2734 0.9605 0.041 Uiso 1 1 calc R U . . . C15A C -0.0580(2) 0.0049(2) 0.86169(11) 0.0312(5) Uani 1 1 d . . . . . H15A H -0.1322 -0.0442 0.8609 0.037 Uiso 1 1 calc R U . . . C16A C -0.0612(2) 0.0848(2) 0.91091(10) 0.0283(5) Uani 1 1 d . . . . . H16A H -0.1368 0.0898 0.9428 0.034 Uiso 1 1 calc R U . . . C13A C 0.2865(2) 0.0863(2) 0.77534(11) 0.0309(5) Uani 1 1 d . . . . . H13A H 0.3203 0.0483 0.7365 0.037 Uiso 1 1 calc R U . . . C6A C 0.0444(2) 0.4418(2) 1.14532(11) 0.0314(5) Uani 1 1 d . . . . . H6A H 0.0100 0.4737 1.1865 0.038 Uiso 1 1 calc R U . . . B1A B 0.3026(2) 0.3029(2) 0.90800(11) 0.0233(5) Uani 1 1 d . . . . . C14A C 0.0503(2) -0.0049(2) 0.81385(10) 0.0306(5) Uani 1 1 d . . . . . H14A H 0.0496 -0.0603 0.7812 0.037 Uiso 1 1 calc R U . . . C24A C 0.6246(2) 0.1380(2) 1.04125(11) 0.0343(5) Uani 1 1 d . . . . . H24A H 0.6936 0.1012 1.0694 0.041 Uiso 1 1 calc R U . . . C35A C 0.2782(2) 0.6083(2) 0.73622(11) 0.0323(5) Uani 1 1 d . . . . . H35A H 0.2410 0.6282 0.6895 0.039 Uiso 1 1 calc R U . . . C34A C 0.3432(2) 0.7043(2) 0.75671(11) 0.0329(5) Uani 1 1 d . . . . . H34A H 0.3512 0.7898 0.7239 0.039 Uiso 1 1 calc R U . . . C33A C 0.3959(2) 0.6748(2) 0.82479(11) 0.0311(5) Uani 1 1 d . . . . . H33A H 0.4410 0.7397 0.8390 0.037 Uiso 1 1 calc R U . . . C22A C 0.4020(2) 0.1449(2) 1.02326(10) 0.0296(5) Uani 1 1 d . . . . . H22A H 0.3181 0.1110 1.0402 0.035 Uiso 1 1 calc R U . . . C23A C 0.5016(2) 0.0903(2) 1.06420(11) 0.0347(5) Uani 1 1 d . . . . . H23A H 0.4857 0.0200 1.1082 0.042 Uiso 1 1 calc R U . . . C5A C 0.1723(2) 0.4658(2) 1.11849(11) 0.0311(5) Uani 1 1 d . . . . . H5A H 0.2231 0.5127 1.1426 0.037 Uiso 1 1 calc R U . . . C26A C 0.5450(2) 0.2927(2) 0.93611(11) 0.0302(5) Uani 1 1 d . . . . . H26A H 0.5619 0.3621 0.8917 0.036 Uiso 1 1 calc R U . . . O1 O -0.03695(13) 0.25534(14) 0.50661(7) 0.0275(3) Uani 1 1 d . . . . . N3 N 0.16877(15) 0.25114(16) 0.46371(8) 0.0236(4) Uani 1 1 d . . . . . N11 N 0.27523(15) 0.42970(16) 0.36096(8) 0.0246(4) Uani 1 1 d . . . . . C2 C 0.06139(18) 0.3174(2) 0.45827(10) 0.0233(4) Uani 1 1 d . . . . . C19 C 0.15961(19) 0.4895(2) 0.36018(10) 0.0242(4) Uani 1 1 d . . . . . C8 C 0.14153(19) 0.1346(2) 0.52066(10) 0.0246(5) Uani 1 1 d . . . . . C18 C 0.1638(2) 0.6097(2) 0.30380(10) 0.0273(5) Uani 1 1 d . . . . . C16 C -0.0631(2) 0.5165(2) 0.39764(11) 0.0290(5) Uani 1 1 d . . . . . H16 H -0.1402 0.4864 0.4284 0.035 Uiso 1 1 calc R U . . . C9 C 0.01307(19) 0.1376(2) 0.54647(10) 0.0254(5) Uani 1 1 d . . . . . C21 C 0.41406(19) 0.29648(19) 0.46578(10) 0.0257(5) Uani 1 1 d . . . . . C12 C 0.3550(2) 0.5107(2) 0.30357(10) 0.0287(5) Uani 1 1 d . . . . . H12 H 0.4419 0.4928 0.2905 0.034 Uiso 1 1 calc R U . . . C32 C 0.3937(2) 0.0742(2) 0.37680(11) 0.0314(5) Uani 1 1 d . . . . . H32 H 0.4315 0.0510 0.4233 0.038 Uiso 1 1 calc R U . . . C7 C -0.0511(2) 0.0396(2) 0.60060(10) 0.0301(5) Uani 1 1 d . . . . . H7 H -0.1393 0.0445 0.6167 0.036 Uiso 1 1 calc R U . . . C17 C 0.04762(19) 0.4421(2) 0.40646(10) 0.0258(5) Uani 1 1 d . . . . . C22 C 0.3863(2) 0.3352(2) 0.53275(11) 0.0301(5) Uani 1 1 d . . . . . H22 H 0.2998 0.3511 0.5480 0.036 Uiso 1 1 calc R U . . . C13 C 0.2915(2) 0.6196(2) 0.26850(10) 0.0296(5) Uani 1 1 d . . . . . H13 H 0.3261 0.6892 0.2280 0.036 Uiso 1 1 calc R U . . . C31 C 0.32623(19) 0.1916(2) 0.35775(11) 0.0273(5) Uani 1 1 d . . . . . C36 C 0.2770(2) 0.2214(2) 0.28724(11) 0.0320(5) Uani 1 1 d . . . . . H36 H 0.2319 0.3005 0.2716 0.038 Uiso 1 1 calc R U . . . C26 C 0.5410(2) 0.2739(2) 0.44673(11) 0.0307(5) Uani 1 1 d . . . . . H26 H 0.5634 0.2465 0.4022 0.037 Uiso 1 1 calc R U . . . C4 C 0.2154(2) 0.0284(2) 0.55207(10) 0.0291(5) Uani 1 1 d . . . . . H4 H 0.3042 0.0247 0.5369 0.035 Uiso 1 1 calc R U . . . C14 C 0.0523(2) 0.6822(2) 0.29640(11) 0.0311(5) Uani 1 1 d . . . . . H14 H 0.0519 0.7636 0.2595 0.037 Uiso 1 1 calc R U . . . C5 C 0.1526(2) -0.0717(2) 0.60658(10) 0.0311(5) Uani 1 1 d . . . . . H5 H 0.1998 -0.1465 0.6290 0.037 Uiso 1 1 calc R U . . . C25 C 0.6377(2) 0.2898(2) 0.49027(11) 0.0340(5) Uani 1 1 d . . . . . H25 H 0.7240 0.2735 0.4750 0.041 Uiso 1 1 calc R U . . . C15 C -0.0591(2) 0.6360(2) 0.34296(11) 0.0326(5) Uani 1 1 d . . . . . H15 H -0.1343 0.6873 0.3373 0.039 Uiso 1 1 calc R U . . . C6 C 0.0232(2) -0.0673(2) 0.62987(10) 0.0315(5) Uani 1 1 d . . . . . H6 H -0.0155 -0.1395 0.6669 0.038 Uiso 1 1 calc R U . . . C24 C 0.6090(2) 0.3289(2) 0.55524(11) 0.0347(5) Uani 1 1 d . . . . . H24 H 0.6749 0.3408 0.5848 0.042 Uiso 1 1 calc R U . . . B1 B 0.3036(2) 0.2906(2) 0.41119(12) 0.0245(5) Uani 1 1 d . . . . . C23 C 0.4806(2) 0.3509(2) 0.57713(11) 0.0351(5) Uani 1 1 d . . . . . H23 H 0.4585 0.3765 0.6223 0.042 Uiso 1 1 calc R U . . . C34 C 0.3548(3) 0.0244(3) 0.26183(13) 0.0472(7) Uani 1 1 d . U . . . H34 H 0.3625 -0.0328 0.2299 0.057 Uiso 1 1 calc R U . . . C33 C 0.4069(2) -0.0084(2) 0.33040(13) 0.0449(6) Uani 1 1 d . U . . . H33 H 0.4519 -0.0878 0.3455 0.054 Uiso 1 1 calc R U . . . C35 C 0.2910(2) 0.1416(3) 0.23987(12) 0.0414(6) Uani 1 1 d . . . . . H35 H 0.2572 0.1664 0.1921 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 O1A 0.0210(8) 0.0321(8) 0.0253(7) -0.0092(6) 0.0004(6) 0.0000(6) N3A 0.0194(9) 0.0245(9) 0.0219(8) -0.0062(7) -0.0023(6) -0.0002(7) N11A 0.0221(9) 0.0247(10) 0.0242(8) -0.0059(7) -0.0013(7) 0.0010(7) C2A 0.0208(11) 0.0231(11) 0.0219(9) -0.0021(8) -0.0007(8) 0.0030(9) C17A 0.0229(11) 0.0256(11) 0.0227(10) -0.0044(8) -0.0026(8) 0.0005(9) C19A 0.0242(11) 0.0224(11) 0.0219(9) -0.0025(8) -0.0051(8) 0.0015(9) C36A 0.0244(11) 0.0286(12) 0.0266(10) -0.0077(9) 0.0012(8) -0.0009(9) C4A 0.0253(12) 0.0307(12) 0.0271(11) -0.0075(9) 0.0004(8) -0.0022(9) C8A 0.0245(11) 0.0250(11) 0.0197(9) -0.0057(8) -0.0002(8) 0.0030(9) C31A 0.0202(11) 0.0309(12) 0.0221(10) -0.0084(8) 0.0011(8) 0.0020(9) C9A 0.0221(11) 0.0251(11) 0.0227(10) -0.0053(8) -0.0037(8) 0.0002(9) C21A 0.0231(11) 0.0267(11) 0.0228(10) -0.0104(8) -0.0018(8) 0.0025(9) C7A 0.0241(12) 0.0318(12) 0.0260(10) -0.0071(9) 0.0016(8) 0.0028(9) C32A 0.0262(12) 0.0334(13) 0.0253(10) -0.0095(9) -0.0003(8) -0.0014(10) C12A 0.0261(12) 0.0326(12) 0.0250(10) -0.0093(9) 0.0007(8) 0.0035(9) C18A 0.0317(12) 0.0242(11) 0.0233(10) -0.0052(8) -0.0065(8) 0.0032(9) C25A 0.0211(12) 0.0374(14) 0.0446(12) -0.0119(11) -0.0054(9) 0.0018(10) C15A 0.0338(13) 0.0307(13) 0.0290(11) -0.0058(9) -0.0073(9) -0.0073(10) C16A 0.0265(12) 0.0314(12) 0.0259(10) -0.0053(9) -0.0033(8) -0.0025(10) C13A 0.0347(13) 0.0336(13) 0.0257(10) -0.0108(9) -0.0019(9) 0.0043(10) C6A 0.0352(13) 0.0345(13) 0.0252(10) -0.0107(9) 0.0011(9) 0.0033(10) B1A 0.0194(12) 0.0284(13) 0.0219(11) -0.0069(9) 0.0004(9) -0.0002(10) C14A 0.0391(14) 0.0288(12) 0.0251(10) -0.0077(9) -0.0076(9) -0.0017(10) C24A 0.0326(13) 0.0409(14) 0.0337(11) -0.0147(10) -0.0132(9) 0.0121(11) C35A 0.0365(13) 0.0352(13) 0.0233(10) -0.0043(9) -0.0026(9) -0.0005(10) C34A 0.0378(13) 0.0294(13) 0.0281(11) -0.0040(9) 0.0041(9) -0.0012(10) C33A 0.0321(13) 0.0305(13) 0.0307(11) -0.0105(9) 0.0051(9) -0.0069(10) C22A 0.0251(12) 0.0351(13) 0.0269(10) -0.0067(9) 0.0010(8) 0.0010(10) C23A 0.0376(14) 0.0395(14) 0.0240(10) -0.0042(9) -0.0007(9) 0.0084(11) C5A 0.0354(13) 0.0334(13) 0.0260(10) -0.0102(9) -0.0030(9) -0.0018(10) C26A 0.0271(12) 0.0296(12) 0.0316(11) -0.0043(9) -0.0022(9) 0.0003(10) O1 0.0212(8) 0.0316(8) 0.0285(7) -0.0064(6) -0.0003(6) -0.0011(6) N3 0.0217(9) 0.0265(10) 0.0229(8) -0.0068(7) -0.0029(6) 0.0016(7) N11 0.0213(9) 0.0292(10) 0.0240(8) -0.0080(7) -0.0034(7) -0.0003(8) C2 0.0186(11) 0.0277(12) 0.0249(10) -0.0090(9) -0.0023(8) -0.0004(9) C19 0.0242(11) 0.0261(12) 0.0237(10) -0.0082(8) -0.0040(8) 0.0004(9) C8 0.0251(11) 0.0271(12) 0.0218(10) -0.0069(8) -0.0021(8) -0.0024(9) C18 0.0325(13) 0.0263(12) 0.0235(10) -0.0066(9) -0.0054(8) 0.0009(10) C16 0.0250(12) 0.0323(13) 0.0304(11) -0.0094(9) -0.0037(8) 0.0021(10) C9 0.0239(11) 0.0296(12) 0.0239(10) -0.0088(9) -0.0038(8) 0.0026(9) C21 0.0282(12) 0.0238(11) 0.0233(10) -0.0032(8) -0.0023(8) -0.0026(9) C12 0.0262(12) 0.0333(13) 0.0264(10) -0.0085(9) 0.0006(8) -0.0030(10) C32 0.0281(12) 0.0287(13) 0.0327(11) -0.0021(9) 0.0032(9) -0.0025(10) C7 0.0258(12) 0.0398(14) 0.0242(10) -0.0083(9) 0.0010(8) -0.0071(10) C17 0.0236(11) 0.0289(12) 0.0270(10) -0.0097(9) -0.0054(8) 0.0013(9) C22 0.0257(12) 0.0327(13) 0.0329(11) -0.0109(9) -0.0022(9) 0.0038(10) C13 0.0331(13) 0.0297(12) 0.0242(10) -0.0044(9) -0.0014(9) -0.0029(10) C31 0.0204(11) 0.0293(12) 0.0301(11) -0.0063(9) 0.0038(8) -0.0056(9) C36 0.0292(13) 0.0351(13) 0.0321(11) -0.0099(10) -0.0007(9) -0.0056(10) C26 0.0265(12) 0.0405(14) 0.0247(10) -0.0086(9) -0.0010(8) -0.0007(10) C4 0.0262(12) 0.0327(13) 0.0275(10) -0.0064(9) -0.0024(8) 0.0019(10) C14 0.0377(13) 0.0256(12) 0.0290(11) -0.0036(9) -0.0096(9) 0.0036(10) C5 0.0344(13) 0.0322(13) 0.0258(10) -0.0054(9) -0.0039(9) 0.0005(10) C25 0.0233(12) 0.0381(14) 0.0384(12) -0.0065(10) -0.0032(9) 0.0003(10) C15 0.0305(13) 0.0350(13) 0.0344(11) -0.0107(10) -0.0103(9) 0.0094(10) C6 0.0359(13) 0.0356(13) 0.0216(10) -0.0057(9) 0.0005(9) -0.0082(11) C24 0.0393(14) 0.0283(13) 0.0363(12) -0.0040(10) -0.0145(10) -0.0043(10) B1 0.0197(12) 0.0255(13) 0.0258(11) -0.0030(10) -0.0001(9) -0.0002(10) C23 0.0430(15) 0.0363(14) 0.0300(11) -0.0139(10) -0.0100(10) 0.0046(11) C34 0.0594(18) 0.0456(16) 0.0367(13) -0.0193(12) 0.0218(12) -0.0136(14) C33 0.0426(15) 0.0307(14) 0.0544(15) -0.0087(11) 0.0230(12) -0.0011(11) C35 0.0453(15) 0.0510(17) 0.0290(11) -0.0141(11) 0.0030(10) -0.0143(13) _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 O1A C2A 1.348(2) . ? O1A C9A 1.392(2) . ? N3A C2A 1.319(2) . ? N3A C8A 1.411(2) . ? N3A B1A 1.634(3) . ? N11A C19A 1.359(2) . ? N11A C12A 1.384(2) . ? N11A B1A 1.569(3) . ? C2A C17A 1.427(3) . ? C17A C16A 1.392(3) . ? C17A C19A 1.398(3) . ? C19A C18A 1.418(3) . ? C36A C35A 1.384(3) . ? C36A C31A 1.397(3) . ? C4A C8A 1.388(3) . ? C4A C5A 1.392(3) . ? C8A C9A 1.376(3) . ? C31A C32A 1.406(3) . ? C31A B1A 1.620(3) . ? C9A C7A 1.379(3) . ? C21A C26A 1.396(3) . ? C21A C22A 1.398(3) . ? C21A B1A 1.609(3) . ? C7A C6A 1.390(3) . ? C32A C33A 1.390(3) . ? C12A C13A 1.366(3) . ? C18A C14A 1.399(3) . ? C18A C13A 1.432(3) . ? C25A C24A 1.382(3) . ? C25A C26A 1.382(3) . ? C15A C14A 1.389(3) . ? C15A C16A 1.396(3) . ? C6A C5A 1.387(3) . ? C24A C23A 1.380(3) . ? C35A C34A 1.391(3) . ? C34A C33A 1.377(3) . ? C22A C23A 1.377(3) . ? O1 C2 1.352(2) . ? O1 C9 1.397(2) . ? N3 C2 1.317(2) . ? N3 C8 1.410(2) . ? N3 B1 1.629(3) . ? N11 C19 1.360(3) . ? N11 C12 1.390(2) . ? N11 B1 1.566(3) . ? C2 C17 1.430(3) . ? C19 C17 1.400(3) . ? C19 C18 1.417(3) . ? C8 C4 1.387(3) . ? C8 C9 1.388(3) . ? C18 C14 1.389(3) . ? C18 C13 1.424(3) . ? C16 C17 1.394(3) . ? C16 C15 1.397(3) . ? C9 C7 1.371(3) . ? C21 C26 1.378(3) . ? C21 C22 1.405(3) . ? C21 B1 1.618(3) . ? C12 C13 1.367(3) . ? C32 C33 1.378(3) . ? C32 C31 1.405(3) . ? C7 C6 1.386(3) . ? C22 C23 1.382(3) . ? C31 C36 1.400(3) . ? C31 B1 1.624(3) . ? C36 C35 1.368(3) . ? C26 C25 1.391(3) . ? C4 C5 1.382(3) . ? C14 C15 1.395(3) . ? C5 C6 1.387(3) . ? C25 C24 1.374(3) . ? C24 C23 1.403(3) . ? C34 C33 1.381(3) . ? C34 C35 1.389(4) . ? 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 C2A O1A C9A 105.00(14) . . ? C2A N3A C8A 105.99(15) . . ? C2A N3A B1A 126.50(15) . . ? C8A N3A B1A 127.43(15) . . ? C19A N11A C12A 105.97(16) . . ? C19A N11A B1A 125.69(16) . . ? C12A N11A B1A 128.31(16) . . ? N3A C2A O1A 113.47(16) . . ? N3A C2A C17A 124.38(17) . . ? O1A C2A C17A 122.08(17) . . ? C16A C17A C19A 118.20(18) . . ? C16A C17A C2A 127.34(18) . . ? C19A C17A C2A 114.36(17) . . ? N11A C19A C17A 126.28(17) . . ? N11A C19A C18A 110.85(17) . . ? C17A C19A C18A 122.88(18) . . ? C35A C36A C31A 122.39(19) . . ? C8A C4A C5A 116.16(19) . . ? C9A C8A C4A 120.37(17) . . ? C9A C8A N3A 106.83(16) . . ? C4A C8A N3A 132.76(18) . . ? C36A C31A C32A 115.89(18) . . ? C36A C31A B1A 120.42(17) . . ? C32A C31A B1A 123.68(17) . . ? C8A C9A C7A 124.51(17) . . ? C8A C9A O1A 108.67(15) . . ? C7A C9A O1A 126.82(17) . . ? C26A C21A C22A 115.53(19) . . ? C26A C21A B1A 122.73(17) . . ? C22A C21A B1A 121.58(18) . . ? C9A C7A C6A 115.05(19) . . ? C33A C32A C31A 122.37(19) . . ? C13A C12A N11A 111.55(18) . . ? C14A C18A C19A 117.47(18) . . ? C14A C18A C13A 137.58(18) . . ? C19A C18A C13A 104.95(17) . . ? C24A C25A C26A 120.0(2) . . ? C14A C15A C16A 122.13(19) . . ? C17A C16A C15A 119.57(19) . . ? C12A C13A C18A 106.66(17) . . ? C5A C6A C7A 121.43(18) . . ? N11A B1A C21A 110.26(17) . . ? N11A B1A C31A 110.11(15) . . ? C21A B1A C31A 116.29(17) . . ? N11A B1A N3A 102.23(14) . . ? C21A B1A N3A 108.37(14) . . ? C31A B1A N3A 108.62(16) . . ? C15A C14A C18A 119.73(19) . . ? C23A C24A C25A 119.2(2) . . ? C36A C35A C34A 119.91(19) . . ? C33A C34A C35A 119.6(2) . . ? C34A C33A C32A 119.78(19) . . ? C23A C22A C21A 122.8(2) . . ? C22A C23A C24A 119.9(2) . . ? C6A C5A C4A 122.46(19) . . ? C25A C26A C21A 122.45(19) . . ? C2 O1 C9 105.49(15) . . ? C2 N3 C8 106.32(16) . . ? C2 N3 B1 127.01(17) . . ? C8 N3 B1 126.54(17) . . ? C19 N11 C12 105.88(17) . . ? C19 N11 B1 125.34(16) . . ? C12 N11 B1 128.45(17) . . ? N3 C2 O1 113.30(17) . . ? N3 C2 C17 124.27(18) . . ? O1 C2 C17 122.43(18) . . ? N11 C19 C17 126.61(19) . . ? N11 C19 C18 111.09(17) . . ? C17 C19 C18 122.3(2) . . ? C4 C8 C9 119.82(18) . . ? C4 C8 N3 133.13(18) . . ? C9 C8 N3 107.05(17) . . ? C14 C18 C19 117.63(19) . . ? C14 C18 C13 137.70(19) . . ? C19 C18 C13 104.67(18) . . ? C17 C16 C15 119.10(19) . . ? C7 C9 C8 124.8(2) . . ? C7 C9 O1 127.36(18) . . ? C8 C9 O1 107.84(16) . . ? C26 C21 C22 116.31(18) . . ? C26 C21 B1 122.33(17) . . ? C22 C21 B1 121.18(18) . . ? C13 C12 N11 110.86(18) . . ? C33 C32 C31 122.4(2) . . ? C9 C7 C6 114.63(19) . . ? C16 C17 C19 118.90(19) . . ? C16 C17 C2 127.04(18) . . ? C19 C17 C2 114.06(18) . . ? C23 C22 C21 122.2(2) . . ? C12 C13 C18 107.49(18) . . ? C36 C31 C32 115.56(19) . . ? C36 C31 B1 119.83(19) . . ? C32 C31 B1 124.61(17) . . ? C35 C36 C31 122.9(2) . . ? C21 C26 C25 122.50(19) . . ? C5 C4 C8 116.31(19) . . ? C18 C14 C15 120.3(2) . . ? C4 C5 C6 122.5(2) . . ? C24 C25 C26 120.4(2) . . ? C14 C15 C16 121.8(2) . . ? C7 C6 C5 121.86(19) . . ? C25 C24 C23 118.73(19) . . ? N11 B1 C21 110.90(16) . . ? N11 B1 C31 109.19(15) . . ? C21 B1 C31 116.81(18) . . ? N11 B1 N3 102.43(16) . . ? C21 B1 N3 108.32(15) . . ? C31 B1 N3 108.17(15) . . ? C22 C23 C24 119.79(19) . . ? C33 C34 C35 119.5(2) . . ? C32 C33 C34 119.9(2) . . ? C36 C35 C34 119.8(2) . . ? _refine_diff_density_max 0.433 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.056 _shelx_res_file ; dccLU40.res created by SHELXL-2014/7 TITL dccLU40 in P-1 CELL 0.71073 10.4924 10.6628 18.4160 74.5955 84.4688 89.0236 ZERR 4.00 0.0004 0.0004 0.0004 0.0019 0.0020 0.0013 LATT 1 SFAC C H B N O UNIT 108 76 4 8 4 L.S. 8 ACTA 50 omit 0 -1 1 wpdb -2 htab delu c33 c34 simu c33 c34 temp -153 FMAP 2 PLAN 10 WGHT 0.069700 FVAR 0.27979 MOLE 1 O1A 5 -0.031020 0.255942 1.013038 11.00000 0.02098 0.03214 = 0.02535 -0.00923 0.00041 0.00001 N3A 4 0.172246 0.295519 0.965247 11.00000 0.01940 0.02448 = 0.02190 -0.00617 -0.00230 -0.00021 N11A 4 0.270672 0.206896 0.860699 11.00000 0.02211 0.02469 = 0.02421 -0.00591 -0.00134 0.00104 C2A 1 0.063711 0.237388 0.962167 11.00000 0.02076 0.02312 = 0.02186 -0.00206 -0.00074 0.00304 C17A 1 0.047141 0.156828 0.913011 11.00000 0.02286 0.02561 = 0.02275 -0.00436 -0.00259 0.00046 C19A 1 0.156309 0.146073 0.865230 11.00000 0.02418 0.02241 = 0.02191 -0.00245 -0.00511 0.00145 C36A 1 0.267743 0.483742 0.783991 11.00000 0.02440 0.02863 = 0.02659 -0.00774 0.00123 -0.00088 AFIX 43 H36A 2 0.223917 0.419093 0.768825 11.00000 -1.20000 AFIX 0 C4A 1 0.228835 0.423864 1.057635 11.00000 0.02528 0.03068 = 0.02708 -0.00751 0.00041 -0.00222 AFIX 43 H4A 2 0.316302 0.441220 1.039416 11.00000 -1.20000 AFIX 0 C8A 1 0.150089 0.355185 1.025104 11.00000 0.02454 0.02501 = 0.01970 -0.00567 -0.00016 0.00300 C31A 1 0.319292 0.449620 0.853686 11.00000 0.02018 0.03089 = 0.02207 -0.00843 0.00108 0.00200 C9A 1 0.024247 0.330452 1.053523 11.00000 0.02214 0.02511 = 0.02270 -0.00531 -0.00365 0.00024 C21A 1 0.419259 0.247970 0.957811 11.00000 0.02308 0.02673 = 0.02278 -0.01041 -0.00177 0.00249 C7A 1 -0.034236 0.372193 1.113181 11.00000 0.02406 0.03178 = 0.02597 -0.00710 0.00155 0.00282 AFIX 43 H7A 2 -0.121833 0.354642 1.130992 11.00000 -1.20000 AFIX 0 C32A 1 0.382970 0.549826 0.872643 11.00000 0.02622 0.03343 = 0.02528 -0.00947 -0.00029 -0.00142 AFIX 43 H32A 2 0.418413 0.531397 0.919873 11.00000 -1.20000 AFIX 0 C12A 1 0.348627 0.169579 0.805194 11.00000 0.02608 0.03264 = 0.02495 -0.00930 0.00072 0.00350 AFIX 43 H12A 2 0.434622 0.198333 0.789788 11.00000 -1.20000 AFIX 0 C18A 1 0.160355 0.067234 0.814023 11.00000 0.03167 0.02421 = 0.02332 -0.00523 -0.00651 0.00317 C25A 1 0.646045 0.239781 0.976809 11.00000 0.02112 0.03739 = 0.04464 -0.01189 -0.00537 0.00178 AFIX 43 H25A 2 0.730278 0.273412 0.960462 11.00000 -1.20000 AFIX 0 C15A 1 -0.057974 0.004940 0.861688 11.00000 0.03385 0.03066 = 0.02905 -0.00584 -0.00731 -0.00730 AFIX 43 H15A 2 -0.132231 -0.044238 0.860887 11.00000 -1.20000 AFIX 0 C16A 1 -0.061208 0.084756 0.910912 11.00000 0.02648 0.03142 = 0.02590 -0.00534 -0.00334 -0.00248 AFIX 43 H16A 2 -0.136848 0.089844 0.942760 11.00000 -1.20000 AFIX 0 C13A 1 0.286463 0.086252 0.775341 11.00000 0.03473 0.03356 = 0.02572 -0.01078 -0.00192 0.00428 AFIX 43 H13A 2 0.320317 0.048291 0.736468 11.00000 -1.20000 AFIX 0 C6A 1 0.044444 0.441825 1.145316 11.00000 0.03518 0.03450 = 0.02525 -0.01073 0.00111 0.00335 AFIX 43 H6A 2 0.009957 0.473668 1.186544 11.00000 -1.20000 AFIX 0 B1A 3 0.302605 0.302895 0.907998 11.00000 0.01936 0.02838 = 0.02187 -0.00691 0.00035 -0.00025 C14A 1 0.050328 -0.004876 0.813849 11.00000 0.03912 0.02883 = 0.02507 -0.00771 -0.00757 -0.00169 AFIX 43 H14A 2 0.049649 -0.060339 0.781153 11.00000 -1.20000 AFIX 0 C24A 1 0.624564 0.137979 1.041253 11.00000 0.03263 0.04090 = 0.03371 -0.01472 -0.01317 0.01212 AFIX 43 H24A 2 0.693631 0.101234 1.069417 11.00000 -1.20000 AFIX 0 C35A 1 0.278197 0.608330 0.736220 11.00000 0.03646 0.03524 = 0.02325 -0.00429 -0.00259 -0.00054 AFIX 43 H35A 2 0.241002 0.628234 0.689501 11.00000 -1.20000 AFIX 0 C34A 1 0.343210 0.704307 0.756707 11.00000 0.03785 0.02938 = 0.02806 -0.00405 0.00412 -0.00123 AFIX 43 H34A 2 0.351205 0.789752 0.723903 11.00000 -1.20000 AFIX 0 C33A 1 0.395920 0.674826 0.824785 11.00000 0.03206 0.03048 = 0.03068 -0.01053 0.00508 -0.00694 AFIX 43 H33A 2 0.441004 0.739728 0.839001 11.00000 -1.20000 AFIX 0 C22A 1 0.402047 0.144881 1.023259 11.00000 0.02508 0.03513 = 0.02688 -0.00671 0.00095 0.00104 AFIX 43 H22A 2 0.318059 0.110994 1.040216 11.00000 -1.20000 AFIX 0 C23A 1 0.501646 0.090347 1.064202 11.00000 0.03762 0.03947 = 0.02402 -0.00425 -0.00070 0.00843 AFIX 43 H23A 2 0.485713 0.019999 1.108204 11.00000 -1.20000 AFIX 0 C5A 1 0.172262 0.465846 1.118494 11.00000 0.03540 0.03341 = 0.02605 -0.01021 -0.00299 -0.00183 AFIX 43 H5A 2 0.223079 0.512696 1.142559 11.00000 -1.20000 AFIX 0 C26A 1 0.545043 0.292711 0.936115 11.00000 0.02712 0.02963 = 0.03164 -0.00427 -0.00216 0.00030 AFIX 43 H26A 2 0.561890 0.362129 0.891727 11.00000 -1.20000 AFIX 0 MOLE 2 O1 5 -0.036946 0.255339 0.506609 11.00000 0.02123 0.03163 = 0.02847 -0.00636 -0.00031 -0.00113 N3 4 0.168771 0.251144 0.463714 11.00000 0.02172 0.02651 = 0.02291 -0.00678 -0.00286 0.00162 N11 4 0.275225 0.429702 0.360962 11.00000 0.02129 0.02925 = 0.02396 -0.00805 -0.00340 -0.00025 C2 1 0.061393 0.317371 0.458269 11.00000 0.01864 0.02768 = 0.02486 -0.00903 -0.00231 -0.00042 C19 1 0.159611 0.489534 0.360178 11.00000 0.02419 0.02614 = 0.02368 -0.00823 -0.00400 0.00040 C8 1 0.141531 0.134555 0.520664 11.00000 0.02506 0.02712 = 0.02180 -0.00687 -0.00210 -0.00240 C18 1 0.163793 0.609713 0.303800 11.00000 0.03252 0.02629 = 0.02351 -0.00661 -0.00538 0.00090 C16 1 -0.063074 0.516504 0.397637 11.00000 0.02496 0.03230 = 0.03045 -0.00941 -0.00368 0.00205 AFIX 43 H16 2 -0.140195 0.486384 0.428387 11.00000 -1.20000 AFIX 0 C9 1 0.013067 0.137643 0.546467 11.00000 0.02393 0.02955 = 0.02394 -0.00878 -0.00377 0.00256 C21 1 0.414060 0.296482 0.465782 11.00000 0.02824 0.02380 = 0.02331 -0.00316 -0.00232 -0.00264 C12 1 0.354972 0.510723 0.303572 11.00000 0.02616 0.03335 = 0.02635 -0.00851 0.00062 -0.00298 AFIX 43 H12 2 0.441897 0.492807 0.290494 11.00000 -1.20000 AFIX 0 C32 1 0.393675 0.074233 0.376805 11.00000 0.02807 0.02874 = 0.03274 -0.00214 0.00323 -0.00252 AFIX 43 H32 2 0.431483 0.051028 0.423338 11.00000 -1.20000 AFIX 0 C7 1 -0.051052 0.039569 0.600602 11.00000 0.02577 0.03981 = 0.02423 -0.00833 0.00099 -0.00706 AFIX 43 H7 2 -0.139324 0.044487 0.616745 11.00000 -1.20000 AFIX 0 C17 1 0.047622 0.442057 0.406456 11.00000 0.02356 0.02885 = 0.02697 -0.00973 -0.00542 0.00130 C22 1 0.386340 0.335161 0.532751 11.00000 0.02566 0.03271 = 0.03288 -0.01090 -0.00221 0.00384 AFIX 43 H22 2 0.299847 0.351053 0.548047 11.00000 -1.20000 AFIX 0 C13 1 0.291458 0.619626 0.268502 11.00000 0.03314 0.02967 = 0.02425 -0.00444 -0.00144 -0.00295 AFIX 43 H13 2 0.326127 0.689222 0.227984 11.00000 -1.20000 AFIX 0 C31 1 0.326230 0.191593 0.357755 11.00000 0.02043 0.02932 = 0.03007 -0.00631 0.00385 -0.00565 C36 1 0.276998 0.221368 0.287240 11.00000 0.02917 0.03511 = 0.03211 -0.00994 -0.00072 -0.00557 AFIX 43 H36 2 0.231865 0.300482 0.271582 11.00000 -1.20000 AFIX 0 C26 1 0.541019 0.273904 0.446727 11.00000 0.02654 0.04047 = 0.02468 -0.00858 -0.00099 -0.00072 AFIX 43 H26 2 0.563375 0.246454 0.402160 11.00000 -1.20000 AFIX 0 C4 1 0.215371 0.028391 0.552069 11.00000 0.02621 0.03265 = 0.02749 -0.00643 -0.00239 0.00187 AFIX 43 H4 2 0.304207 0.024746 0.536926 11.00000 -1.20000 AFIX 0 C14 1 0.052282 0.682206 0.296396 11.00000 0.03770 0.02556 = 0.02903 -0.00358 -0.00960 0.00359 AFIX 43 H14 2 0.051869 0.763583 0.259460 11.00000 -1.20000 AFIX 0 C5 1 0.152576 -0.071732 0.606579 11.00000 0.03436 0.03219 = 0.02576 -0.00539 -0.00393 0.00053 AFIX 43 H5 2 0.199797 -0.146507 0.628974 11.00000 -1.20000 AFIX 0 C25 1 0.637660 0.289781 0.490271 11.00000 0.02330 0.03809 = 0.03841 -0.00648 -0.00318 0.00032 AFIX 43 H25 2 0.724045 0.273474 0.474979 11.00000 -1.20000 AFIX 0 C15 1 -0.059105 0.636045 0.342957 11.00000 0.03045 0.03503 = 0.03440 -0.01070 -0.01034 0.00943 AFIX 43 H15 2 -0.134300 0.687266 0.337340 11.00000 -1.20000 AFIX 0 C6 1 0.023244 -0.067297 0.629873 11.00000 0.03592 0.03560 = 0.02160 -0.00570 0.00051 -0.00818 AFIX 43 H6 2 -0.015504 -0.139547 0.666937 11.00000 -1.20000 AFIX 0 C24 1 0.609033 0.328885 0.555241 11.00000 0.03935 0.02832 = 0.03625 -0.00400 -0.01447 -0.00427 AFIX 43 H24 2 0.674940 0.340806 0.584778 11.00000 -1.20000 AFIX 0 B1 3 0.303567 0.290609 0.411188 11.00000 0.01969 0.02545 = 0.02583 -0.00296 -0.00014 -0.00021 C23 1 0.480613 0.350876 0.577133 11.00000 0.04301 0.03634 = 0.02999 -0.01386 -0.00999 0.00457 AFIX 43 H23 2 0.458540 0.376491 0.622329 11.00000 -1.20000 AFIX 0 C34 1 0.354780 0.024369 0.261828 11.00000 0.05945 0.04559 = 0.03667 -0.01932 0.02179 -0.01360 AFIX 43 H34 2 0.362476 -0.032811 0.229940 11.00000 -1.20000 AFIX 0 C33 1 0.406945 -0.008432 0.330396 11.00000 0.04262 0.03068 = 0.05438 -0.00874 0.02299 -0.00113 AFIX 43 H33 2 0.451872 -0.087799 0.345531 11.00000 -1.20000 AFIX 0 C35 1 0.290973 0.141637 0.239873 11.00000 0.04526 0.05100 = 0.02905 -0.01406 0.00300 -0.01428 AFIX 43 H35 2 0.257166 0.166352 0.192120 11.00000 -1.20000 AFIX 0 HKLF 4 REM dccLU40 in P-1 REM R1 = 0.0547 for 5186 Fo > 4sig(Fo) and 0.1020 for all 8520 data REM 559 parameters refined using 7 restraints END WGHT 0.0689 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.433, deepest hole -0.315, 1-sigma level 0.056 Q1 1 0.3233 -0.0850 0.2652 11.00000 0.05 0.43 Q2 1 0.4024 0.2948 0.5998 11.00000 0.05 0.36 Q3 1 0.6976 0.3167 0.5364 11.00000 0.05 0.33 Q4 1 0.4799 0.0572 0.4533 11.00000 0.05 0.24 Q5 1 0.4651 0.2144 0.4734 11.00000 0.05 0.22 Q6 1 0.4800 -0.0833 1.0696 11.00000 0.05 0.22 Q7 1 0.2971 0.3835 0.8812 11.00000 0.05 0.21 Q8 1 0.5467 0.2617 0.4279 11.00000 0.05 0.20 Q9 1 0.3572 0.2681 0.4503 11.00000 0.05 0.20 Q10 1 0.2985 0.4967 0.5361 11.00000 0.05 0.19 ; _shelx_res_checksum 11422 _shelx_hkl_file ; 0 0 1 -0.10 0.00 0 0 -1 -0.10 0.00 0 0 3 1.30 0.10 0 0 -3 2.00 0.10 0 0 4 5.00 0.20 0 0 -4 5.70 0.20 0 0 5 0.10 0.10 0 0 -5 0.40 0.10 0 0 6 0.10 0.10 0 0 -6 0.30 0.20 0 0 7 3.60 0.30 0 0 -7 3.70 0.30 0 0 8 20.80 0.60 0 0 -8 22.80 0.80 0 0 9 26.00 0.90 0 0 -9 26.00 0.90 0 0 10 89.50 2.70 0 0 -10 92.40 2.50 0 0 11 3.10 0.40 0 0 -11 4.40 0.30 0 0 12 131.50 3.90 0 0 -12 130.10 5.80 0 0 13 0.50 0.40 0 0 -13 0.90 1.20 0 0 14 5.20 0.60 0 0 15 1.90 0.50 0 0 16 1.80 0.40 0 0 17 -0.40 0.40 0 0 18 31.70 2.70 0 0 19 11.70 2.30 0 0 20 7.30 1.70 0 0 21 3.50 1.80 0 0 22 24.10 3.40 0 -1 22 20.20 3.40 0 -1 21 26.60 3.40 0 -1 20 22.70 2.90 0 -1 19 2.10 1.30 0 -1 18 23.10 2.40 0 -1 17 11.80 1.20 0 -1 16 0.70 0.50 0 1 -15 2.90 0.40 0 -1 15 2.70 0.60 0 1 -14 4.20 0.50 0 -1 14 2.60 0.60 0 1 -13 15.60 0.80 0 -1 13 16.70 1.00 0 1 -12 14.40 0.70 0 -1 12 15.00 0.90 0 1 -11 16.30 0.80 0 -1 11 19.00 0.90 0 1 -10 6.10 0.60 0 -1 10 7.10 0.40 0 1 -9 44.60 1.50 0 -1 9 47.50 1.20 0 1 -8 0.30 0.30 0 -1 8 0.40 0.30 0 1 -7 184.60 4.60 0 -1 7 190.30 3.80 0 1 -6 4.10 0.40 0 -1 6 5.00 0.30 0 1 -5 122.60 4.70 0 -1 5 116.90 2.40 0 1 -4 3.30 0.30 0 -1 4 2.90 0.30 0 1 -3 37.30 1.40 0 -1 3 37.80 0.90 0 1 -2 159.00 3.90 0 -1 2 153.90 3.00 0 1 -1 -0.70 0.20 0 -1 1 -0.30 0.10 0 1 1 0.50 0.10 0 -1 -1 -0.10 0.10 0 1 3 5.60 0.30 0 1 4 75.50 1.90 0 -1 -4 77.80 1.90 0 1 5 97.60 2.40 0 -1 -5 96.00 2.40 0 1 6 22.90 0.50 0 -1 -6 21.40 1.20 0 1 7 40.70 2.00 0 -1 -7 40.00 2.00 0 1 8 4.40 0.60 0 -1 -8 5.30 0.70 0 1 9 103.10 2.60 0 -1 -9 89.80 4.00 0 1 10 31.30 1.90 0 -1 -10 22.80 1.70 0 1 11 26.40 1.60 0 -1 -11 23.40 1.80 0 1 12 1.20 1.10 0 -1 -12 -0.60 1.00 0 1 13 -0.20 0.90 0 -1 -13 1.10 1.20 0 1 14 20.90 1.80 0 1 15 22.00 2.20 0 1 16 9.20 1.40 0 1 17 23.70 2.40 0 1 18 27.50 2.40 0 1 19 51.50 4.10 0 1 20 70.10 4.70 0 1 21 7.80 1.90 0 1 22 4.20 2.50 0 1 23 3.20 2.00 0 -2 21 -2.20 1.60 0 -2 20 0.50 1.60 0 -2 19 5.10 1.70 0 -2 18 -0.20 1.30 0 2 -17 0.10 0.60 0 -2 17 0.50 0.80 0 2 -16 2.20 0.50 0 -2 16 2.20 0.80 0 2 -15 21.00 1.40 0 -2 15 22.40 1.30 0 2 -14 33.90 1.70 0 -2 14 39.20 1.80 0 2 -13 0.30 0.70 0 -2 13 -1.10 1.20 0 2 -12 0.40 0.40 0 -2 12 -0.30 0.60 0 2 -11 6.80 0.60 0 -2 11 6.10 0.50 0 2 -10 13.00 0.80 0 -2 10 13.30 0.60 0 2 -9 5.50 0.40 0 -2 9 5.70 0.40 0 2 -8 89.60 2.50 0 -2 8 88.30 2.20 0 2 -7 1.10 0.40 0 -2 7 1.20 0.30 0 2 -6 0.00 0.30 0 -2 6 0.20 0.30 0 2 -5 63.30 1.80 0 -2 5 65.40 1.60 0 2 -4 377.40 9.40 0 -2 4 390.10 9.00 0 2 -3 49.90 1.40 0 -2 3 51.20 1.30 0 2 -2 3036.80 68.60 0 -2 2 2903.50 52.90 0 2 -1 56.40 2.20 0 -2 1 56.40 1.50 0 2 0 55.60 2.40 0 -2 0 49.40 2.20 0 2 1 1.00 0.30 0 -2 -1 1.00 0.30 0 2 2 138.40 4.80 0 -2 -2 147.50 5.00 0 2 3 68.80 2.40 0 -2 -3 70.50 2.50 0 2 4 2639.50 82.00 0 2 5 41.80 1.20 0 2 6 302.60 7.40 0 2 7 0.90 0.70 0 2 8 3.80 0.20 0 -2 -8 4.10 0.30 0 2 9 4.30 0.10 0 2 10 14.10 1.10 0 2 11 -0.90 0.90 0 2 12 -0.30 1.10 0 2 13 24.00 1.90 0 2 14 3.00 1.30 0 2 15 11.10 1.70 0 2 16 36.80 2.40 0 2 17 -1.00 0.90 0 2 18 12.80 2.10 0 2 19 1.90 1.50 0 2 20 -0.80 1.30 0 2 21 14.00 2.70 0 2 22 -0.20 1.60 0 2 23 23.30 3.40 0 -3 20 0.80 2.70 0 -3 19 1.20 1.60 0 -3 18 0.20 1.40 0 3 -17 2.90 0.80 0 -3 17 8.20 2.10 0 3 -16 2.60 0.80 0 -3 16 0.40 0.90 0 3 -15 5.20 0.90 0 -3 15 4.80 1.90 0 3 -14 80.20 3.60 0 -3 14 87.10 3.10 0 3 -13 19.30 1.40 0 -3 13 21.70 1.30 0 3 -12 7.60 0.80 0 -3 12 7.60 0.70 0 3 -11 18.40 1.10 0 -3 11 19.50 0.90 0 3 -10 0.20 0.50 0 -3 10 0.10 0.40 0 3 -9 34.00 1.30 0 -3 9 35.80 1.20 0 3 -8 4.40 0.50 0 -3 8 4.60 0.40 0 3 -7 0.60 0.50 0 -3 7 0.50 0.40 0 3 -6 164.60 4.30 0 -3 6 158.30 3.80 0 3 -5 31.30 1.20 0 -3 5 32.40 1.30 0 3 -4 677.00 16.30 0 -3 4 733.20 17.20 0 3 -3 161.00 4.10 0 -3 3 155.30 4.10 0 3 -2 329.60 8.40 0 -3 2 359.30 8.90 0 3 -1 146.10 4.10 0 -3 1 146.60 3.50 0 3 0 200.80 7.20 0 -3 0 204.60 5.10 0 3 1 201.30 7.10 0 -3 -1 206.20 7.10 0 3 2 25.40 1.50 0 -3 -2 24.30 1.20 0 3 3 274.20 9.40 0 -3 -3 275.80 9.20 0 3 4 103.20 3.80 0 -3 -4 104.20 3.80 0 3 5 1.80 0.50 0 3 6 586.10 19.30 0 3 7 114.30 3.00 0 3 8 521.40 12.10 0 3 9 94.60 2.60 0 -3 -9 94.80 3.40 0 3 10 47.00 1.40 0 -3 -10 53.60 2.00 0 3 11 30.70 1.00 0 3 12 19.60 1.60 0 3 13 6.50 1.40 0 3 14 6.70 1.50 0 3 15 24.60 2.20 0 3 16 14.30 1.90 0 3 17 4.50 1.80 0 3 18 77.60 4.40 0 3 19 -0.80 1.80 0 3 20 0.60 1.30 0 3 21 0.30 1.40 0 3 22 -1.00 2.10 0 3 23 2.10 2.20 0 -4 19 0.40 2.70 0 -4 18 -0.70 1.70 0 4 -17 1.10 0.90 0 -4 17 -0.60 2.10 0 4 -16 5.60 1.10 0 -4 16 2.60 2.90 0 4 -15 3.30 1.00 0 -4 15 1.30 1.00 0 4 -14 1.30 0.90 0 -4 14 1.30 0.90 0 4 -13 2.00 0.90 0 -4 13 2.90 0.90 0 4 -12 29.20 1.90 0 -4 12 28.40 2.00 0 4 -11 2.80 0.70 0 -4 11 3.50 0.60 0 4 -10 1.00 0.50 0 -4 10 0.50 0.40 0 4 -9 1.20 0.50 0 -4 9 1.30 0.40 0 4 -8 11.40 0.80 0 -4 8 12.60 0.70 0 4 -7 11.40 0.80 0 -4 7 10.90 0.70 0 4 -6 44.50 1.60 0 -4 6 43.10 1.30 0 4 -5 9.50 0.70 0 -4 5 8.50 0.60 0 4 -4 29.10 1.20 0 -4 4 30.40 1.30 0 4 -3 38.20 1.50 0 -4 3 34.10 1.40 0 4 -2 55.00 2.50 0 -4 2 57.20 1.80 0 4 -1 51.40 2.20 0 -4 1 50.20 1.60 0 4 0 85.50 3.50 0 -4 0 80.00 2.40 0 4 1 -0.30 0.50 0 -4 -1 0.00 0.40 0 4 2 6.10 0.70 0 -4 -2 7.30 0.80 0 4 3 0.80 0.70 0 -4 -3 -0.20 0.60 0 4 4 144.00 5.10 0 -4 -4 137.50 4.80 0 4 5 25.40 1.40 0 -4 -5 24.80 1.20 0 4 6 119.20 4.90 0 4 7 13.60 1.00 0 4 8 3.10 0.40 0 4 9 29.10 1.10 0 -4 -9 27.40 1.30 0 4 10 49.80 1.60 0 4 11 26.80 1.00 0 -4 -11 29.00 1.30 0 4 12 10.90 0.60 0 -4 -12 11.80 0.40 0 4 13 2.30 0.30 0 4 14 0.30 0.80 0 4 15 10.20 1.70 0 4 16 18.50 2.10 0 4 18 6.00 1.40 0 4 20 5.20 2.20 0 4 21 0.90 2.00 0 4 22 2.70 1.80 0 4 23 -1.10 1.60 0 5 -17 0.00 1.10 0 -5 17 -0.80 1.60 0 5 -16 5.50 1.10 0 -5 16 4.00 2.30 0 5 -15 18.60 1.60 0 -5 15 17.30 2.90 0 5 -14 0.30 0.70 0 -5 14 1.10 1.30 0 5 -13 74.90 4.70 0 -5 13 66.80 5.80 0 5 -12 1.60 0.70 0 -5 12 0.70 1.00 0 5 -11 0.20 0.70 0 -5 11 1.20 0.80 0 5 -10 39.90 2.00 0 -5 10 39.70 1.70 0 5 -9 -0.10 0.70 0 -5 9 0.10 0.50 0 5 -8 4.70 0.60 0 -5 8 5.80 0.70 0 5 -7 4.90 0.60 0 -5 7 6.60 0.60 0 5 -6 32.60 1.40 0 -5 6 32.90 1.50 0 5 -5 35.20 1.40 0 -5 5 31.90 1.40 0 5 -4 119.80 3.50 0 -5 4 117.80 3.40 0 5 -3 92.00 3.00 0 -5 3 87.80 2.80 0 5 -2 562.80 19.40 0 -5 2 566.40 14.20 0 5 -1 107.80 3.30 0 -5 1 106.90 3.20 0 5 0 165.20 5.80 0 -5 0 166.60 4.30 0 5 1 3.60 0.90 0 -5 -1 4.90 0.50 0 5 2 5.30 1.00 0 -5 -2 5.70 0.50 0 5 3 23.40 1.40 0 -5 -3 25.60 1.10 0 5 4 1.60 0.80 0 -5 -4 1.90 0.50 0 5 5 2.70 0.80 0 -5 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1.10 0.80 0 -8 5 -0.60 1.00 0 8 -4 13.30 1.00 0 -8 4 17.10 1.80 0 8 -3 -0.40 0.60 0 -8 3 0.40 1.00 0 8 -2 0.20 0.80 0 -8 2 0.40 1.30 0 8 -1 1.30 0.80 0 -8 1 3.80 1.50 0 8 0 0.10 0.70 0 -8 0 1.30 1.30 0 -8 -1 -0.50 0.90 0 8 2 25.20 1.80 0 -8 -2 23.40 1.40 0 8 3 53.50 3.00 0 -8 -3 53.30 2.50 0 8 4 211.00 8.60 0 -8 -4 203.60 9.60 0 8 5 57.30 3.20 0 -8 -5 49.50 3.20 0 8 6 18.30 1.50 0 -8 -6 14.10 1.70 0 8 7 11.60 1.40 0 -8 -7 7.40 1.10 0 8 8 4.30 1.00 0 -8 -8 4.80 1.20 0 8 9 1.50 1.00 0 -8 -9 0.30 0.70 0 8 10 2.30 1.10 0 -8 -10 1.70 0.70 0 8 11 0.30 0.70 0 -8 -11 1.20 1.00 0 8 12 0.20 0.70 0 -8 -12 0.60 0.60 0 8 13 41.70 1.90 0 -8 -13 37.80 2.30 0 8 14 9.20 1.00 0 -8 -14 8.80 1.30 0 8 15 12.80 1.00 0 -8 -15 11.10 1.20 0 8 16 0.40 0.70 0 8 17 2.90 0.70 0 8 18 11.40 2.20 0 8 19 0.90 1.50 0 8 20 6.80 1.70 0 8 21 1.50 1.50 0 8 22 5.30 2.60 0 9 -12 4.30 2.20 0 9 -11 0.50 1.80 0 9 -10 -0.20 1.80 0 9 -9 -1.50 1.70 0 9 -8 -0.50 1.10 0 9 -7 2.60 1.30 0 9 -6 3.70 1.70 0 9 -5 0.40 0.80 0 9 -4 0.40 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3 53.00 3.10 -1 -7 -3 60.60 3.30 1 7 4 39.30 2.20 -1 -7 -4 40.00 2.20 1 7 5 0.00 0.70 -1 -7 -5 1.00 0.80 1 7 6 0.90 0.90 -1 -7 -6 0.80 1.00 1 7 7 4.60 0.80 -1 -7 -7 3.00 0.80 1 7 8 2.30 0.90 -1 -7 -8 1.60 0.70 1 7 9 3.50 0.70 -1 -7 -9 3.50 1.00 1 7 10 3.20 0.70 1 7 11 9.50 0.80 1 7 12 32.30 1.50 1 7 13 74.60 2.60 -1 -7 -13 65.30 3.20 1 7 14 29.10 1.50 -1 -7 -14 29.50 2.00 1 7 15 -0.20 0.50 1 7 16 -0.10 0.50 -1 -7 -16 -0.10 0.40 1 7 17 19.50 1.10 1 7 18 0.20 0.40 1 7 19 0.60 1.20 1 7 20 13.60 2.10 1 7 21 6.60 1.70 1 7 22 6.40 2.60 1 8 -14 6.50 2.00 1 8 -13 1.60 1.40 1 8 -12 -0.30 1.60 1 8 -11 0.70 1.50 1 8 -10 -0.80 1.60 1 8 -9 3.40 1.70 1 8 -8 26.10 1.80 -1 -8 8 29.70 2.80 1 8 -7 2.30 0.80 -1 -8 7 6.40 1.80 1 8 -6 33.10 1.70 -1 -8 6 35.90 2.70 1 8 -5 30.30 1.60 -1 -8 5 33.80 2.90 1 8 -4 13.00 1.20 -1 -8 4 18.30 1.90 1 8 -3 125.00 4.10 -1 -8 3 110.80 5.70 1 8 -2 13.80 1.20 -1 -8 2 13.30 1.50 1 8 -1 -0.10 0.50 -1 -8 1 1.50 1.00 1 8 0 28.80 1.60 -1 -8 0 30.00 2.50 1 8 1 2.90 0.90 -1 -8 -1 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4.10 -5 8 17 3.50 2.40 -5 8 16 4.40 1.20 -5 8 15 12.30 2.00 -5 8 14 0.90 1.10 -5 8 13 0.20 1.40 5 -8 -12 -0.10 1.20 -5 8 12 0.70 1.00 5 -8 -11 -0.40 1.20 -5 8 11 1.70 1.00 5 -8 -10 6.10 1.60 -5 8 10 9.00 1.80 5 -8 -9 23.00 2.40 -5 8 9 26.80 2.40 -5 8 8 2.30 0.70 -5 8 7 97.80 3.40 -5 8 6 -0.60 0.90 -5 8 5 99.10 3.50 -5 8 4 14.70 1.20 -5 8 3 1.00 0.70 -5 8 2 8.40 1.00 -5 8 1 7.40 1.10 -5 8 0 2.50 0.90 -5 8 -1 17.80 1.40 -5 8 -2 3.30 1.00 -5 8 -3 18.40 1.50 -5 8 -4 4.30 1.00 -5 8 -5 1.80 0.90 -5 8 -6 9.30 1.30 -5 8 -7 10.60 1.20 -5 8 -8 -0.10 0.90 -5 8 -9 6.60 1.20 -5 8 -10 3.40 1.90 -5 8 -11 24.80 3.00 -5 8 -12 3.40 2.00 -5 8 -13 9.70 2.00 -5 7 19 4.00 2.70 -5 7 18 12.90 2.30 -5 7 17 -0.10 0.80 -5 7 16 9.60 1.30 -5 7 15 37.80 2.80 5 -7 -13 0.30 0.90 5 -7 -12 1.40 1.00 5 -7 -11 -0.20 0.70 5 -7 -10 15.50 1.50 -5 7 10 14.40 1.40 5 -7 -9 138.40 8.10 -5 7 9 174.80 7.10 5 -7 -8 1.20 1.20 -5 7 8 2.50 1.10 5 -7 -7 18.10 1.70 -5 7 7 22.20 1.70 -5 7 6 0.50 0.70 5 -7 -5 6.20 1.50 -5 7 5 9.50 1.10 5 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