data_fraser41_0m _audit_creation_date 2018-10-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2017/1' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C21 H24 O6' _chemical_formula_sum 'C21 H24 O6' _chemical_formula_weight 372.40 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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 9.1237(6) _cell_length_b 15.3257(10) _cell_length_c 13.5649(9) _cell_angle_alpha 90 _cell_angle_beta 102.7500(10) _cell_angle_gamma 90 _cell_volume 1850.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9978 _cell_measurement_temperature 163(2) _cell_measurement_theta_max 33.136 _cell_measurement_theta_min 3.623 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0586 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9214. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 792 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0167 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 40282 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.169 _diffrn_reflns_theta_min 3.354 _diffrn_ambient_temperature 163.2 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Bruker Kappa APEXII Duo' _diffrn_measurement_device_type 'Bruker Kappa APEXII Duo' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6249 _reflns_number_total 7046 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (Bruker, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.418 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.098 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 7046 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0504 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.5913P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1322 _refine_ls_wR_factor_ref 0.1407 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O3-C10 \\sim O3-C10A with sigma of 0.02 3. Others Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)= Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1) Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)= Sof(H12B)=Sof(H12C)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B), C10A(H10C,H10D), C11A(H11C,H11D) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C18(H18) 4.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B, H21C), C12A(H12D,H12E,H12F) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 O1 O 0.37727(8) 0.43521(5) 0.04638(6) 0.03080(16) Uani 1 1 d . . . . . H1 H 0.3836(19) 0.4680(12) 0.1350(13) 0.046 Uiso 1 1 d R . . . . O2 O 0.43295(8) 0.48295(5) 0.22383(6) 0.03092(16) Uani 1 1 d . . . . . O3 O 0.92067(8) 0.45504(5) 0.63414(5) 0.02898(15) Uani 1 1 d D . . . . O4 O 0.84426(8) 0.22523(5) -0.10401(5) 0.02921(15) Uani 1 1 d . . . . . O5 O 0.62841(8) 0.22220(5) -0.27759(5) 0.02619(14) Uani 1 1 d . . . . . O6 O 0.36015(7) 0.29025(5) -0.28704(5) 0.02662(14) Uani 1 1 d . . . . . C1 C 0.50464(10) 0.39426(6) 0.06322(6) 0.02219(15) Uani 1 1 d . . . . . C2 C 0.59953(10) 0.39388(6) 0.15983(6) 0.02250(15) Uani 1 1 d . . . . . H2 H 0.691781 0.362726 0.171674 0.027 Uiso 1 1 calc R . . . . C3 C 0.55766(10) 0.43986(6) 0.23935(6) 0.02213(15) Uani 1 1 d . . . . . C4 C 0.65328(9) 0.44288(6) 0.34241(6) 0.02134(15) Uani 1 1 d . . . . . C5 C 0.62340(11) 0.50562(7) 0.41015(7) 0.02666(17) Uani 1 1 d . . . . . H5 H 0.541262 0.544436 0.389138 0.032 Uiso 1 1 calc R . . . . C6 C 0.71130(11) 0.51248(7) 0.50769(7) 0.02860(18) Uani 1 1 d . . . . . H6 H 0.690498 0.556436 0.552057 0.034 Uiso 1 1 calc R . . . . C7 C 0.83008(10) 0.45454(6) 0.54004(7) 0.02375(16) Uani 1 1 d . . . . . C8 C 0.86025(11) 0.39043(6) 0.47328(7) 0.02721(17) Uani 1 1 d . . . . . H8 H 0.940293 0.350344 0.494984 0.033 Uiso 1 1 calc R . . . . C9 C 0.77343(11) 0.38557(6) 0.37580(7) 0.02575(17) Uani 1 1 d . . . . . H9 H 0.795841 0.342602 0.330836 0.031 Uiso 1 1 calc R . . . . C10 C 0.8984(2) 0.52800(11) 0.69927(12) 0.0268(3) Uani 0.883(4) 1 d D . P A 1 H10A H 0.794549 0.527208 0.710021 0.032 Uiso 0.883(4) 1 calc R . P A 1 H10B H 0.914623 0.584140 0.667188 0.032 Uiso 0.883(4) 1 calc R . P A 1 C11 C 1.01077(13) 0.51813(10) 0.79986(9) 0.0289(3) Uani 0.883(4) 1 d . . P A 1 H11A H 1.112546 0.511244 0.786538 0.035 Uiso 0.883(4) 1 calc R . P A 1 H11B H 1.010552 0.572429 0.839363 0.035 Uiso 0.883(4) 1 calc R . P A 1 C12 C 0.97987(17) 0.44152(10) 0.86335(10) 0.0397(3) Uani 0.883(4) 1 d . . P A 1 H12A H 0.881881 0.449384 0.880561 0.060 Uiso 0.883(4) 1 calc GR . P A 1 H12B H 1.058428 0.438425 0.925519 0.060 Uiso 0.883(4) 1 calc GR . P A 1 H12C H 0.979352 0.387327 0.824930 0.060 Uiso 0.883(4) 1 calc GR . P A 1 C13 C 0.54213(9) 0.34809(6) -0.02404(6) 0.02081(14) Uani 1 1 d . . . . . C14 C 0.68344(10) 0.31022(6) -0.01835(6) 0.02266(15) Uani 1 1 d . . . . . H14 H 0.758555 0.313707 0.042404 0.027 Uiso 1 1 calc R . . . . C15 C 0.71308(9) 0.26736(6) -0.10248(6) 0.02164(15) Uani 1 1 d . . . . . C16 C 0.60432(9) 0.26434(5) -0.19362(6) 0.02035(14) Uani 1 1 d . . . . . C17 C 0.46214(9) 0.30059(5) -0.19736(6) 0.02057(14) Uani 1 1 d . . . . . C18 C 0.43102(9) 0.34272(6) -0.11319(6) 0.02197(15) Uani 1 1 d . . . . . H18 H 0.334761 0.367659 -0.116384 0.026 Uiso 1 1 calc R . . . . C19 C 0.96282(11) 0.23088(8) -0.01567(7) 0.0314(2) Uani 1 1 d . . . . . H19A H 1.049439 0.197140 -0.025992 0.047 Uiso 1 1 calc GR . . . . H19B H 0.928227 0.207314 0.042406 0.047 Uiso 1 1 calc GR . . . . H19C H 0.992112 0.292061 -0.002830 0.047 Uiso 1 1 calc GR . . . . C20 C 0.75065(13) 0.25341(10) -0.31781(8) 0.0393(3) Uani 1 1 d . . . . . H20A H 0.748279 0.225205 -0.382985 0.059 Uiso 1 1 calc GR . . . . H20B H 0.845773 0.239714 -0.270741 0.059 Uiso 1 1 calc GR . . . . H20C H 0.741786 0.316734 -0.327321 0.059 Uiso 1 1 calc GR . . . . C21 C 0.21567(11) 0.32926(7) -0.29515(8) 0.0313(2) Uani 1 1 d . . . . . H21A H 0.154385 0.319490 -0.363252 0.047 Uiso 1 1 calc GR . . . . H21B H 0.227519 0.392094 -0.282482 0.047 Uiso 1 1 calc GR . . . . H21C H 0.166049 0.302935 -0.245289 0.047 Uiso 1 1 calc GR . . . . C10A C 0.9028(19) 0.4998(13) 0.7144(9) 0.043(4) Uani 0.117(4) 1 d D . P A 2 H10C H 0.798554 0.492672 0.723155 0.051 Uiso 0.117(4) 1 calc R . P A 2 H10D H 0.920126 0.562625 0.704272 0.051 Uiso 0.117(4) 1 calc R . P A 2 C11A C 1.0108(11) 0.4682(9) 0.8071(7) 0.035(2) Uani 0.117(4) 1 d . . P A 2 H11C H 0.998409 0.404600 0.814779 0.042 Uiso 0.117(4) 1 calc R . P A 2 H11D H 1.115141 0.479326 0.800623 0.042 Uiso 0.117(4) 1 calc R . P A 2 C12A C 0.9823(17) 0.5145(10) 0.8975(8) 0.055(4) Uani 0.117(4) 1 d . . P A 2 H12D H 0.957568 0.575629 0.880339 0.082 Uiso 0.117(4) 1 calc GR . P A 2 H12E H 1.072418 0.511590 0.952223 0.082 Uiso 0.117(4) 1 calc GR . P A 2 H12F H 0.898122 0.486627 0.919330 0.082 Uiso 0.117(4) 1 calc GR . P A 2 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 O1 0.0245(3) 0.0417(4) 0.0249(3) -0.0035(3) 0.0027(2) 0.0091(3) O2 0.0269(3) 0.0409(4) 0.0249(3) -0.0029(3) 0.0057(2) 0.0101(3) O3 0.0288(3) 0.0349(4) 0.0217(3) -0.0036(2) 0.0022(2) 0.0001(3) O4 0.0228(3) 0.0429(4) 0.0197(3) -0.0048(3) -0.0001(2) 0.0096(3) O5 0.0265(3) 0.0322(3) 0.0197(3) -0.0067(2) 0.0048(2) -0.0015(2) O6 0.0214(3) 0.0355(3) 0.0197(3) -0.0042(2) -0.0025(2) 0.0033(2) C1 0.0213(3) 0.0256(4) 0.0198(3) -0.0016(3) 0.0047(3) -0.0002(3) C2 0.0211(3) 0.0270(4) 0.0192(3) -0.0034(3) 0.0040(3) 0.0022(3) C3 0.0224(3) 0.0244(4) 0.0203(3) -0.0011(3) 0.0064(3) -0.0003(3) C4 0.0224(3) 0.0233(3) 0.0192(3) -0.0018(3) 0.0065(3) -0.0001(3) C5 0.0288(4) 0.0293(4) 0.0219(4) -0.0036(3) 0.0055(3) 0.0056(3) C6 0.0309(4) 0.0323(4) 0.0226(4) -0.0058(3) 0.0059(3) 0.0046(3) C7 0.0236(4) 0.0281(4) 0.0197(3) -0.0011(3) 0.0052(3) -0.0018(3) C8 0.0266(4) 0.0290(4) 0.0249(4) -0.0027(3) 0.0032(3) 0.0046(3) C9 0.0277(4) 0.0263(4) 0.0230(4) -0.0046(3) 0.0052(3) 0.0035(3) C10 0.0282(6) 0.0318(6) 0.0201(6) -0.0040(5) 0.0048(5) 0.0018(5) C11 0.0287(5) 0.0310(7) 0.0256(5) -0.0061(4) 0.0030(4) -0.0011(4) C12 0.0425(7) 0.0477(7) 0.0287(6) 0.0043(5) 0.0071(5) 0.0000(5) C13 0.0206(3) 0.0237(3) 0.0179(3) -0.0015(3) 0.0037(3) -0.0008(3) C14 0.0210(3) 0.0288(4) 0.0172(3) -0.0024(3) 0.0020(3) 0.0002(3) C15 0.0198(3) 0.0269(4) 0.0172(3) -0.0012(3) 0.0019(3) 0.0016(3) C16 0.0209(3) 0.0228(3) 0.0165(3) -0.0018(2) 0.0024(2) -0.0010(3) C17 0.0200(3) 0.0229(3) 0.0172(3) -0.0007(3) 0.0007(2) -0.0012(3) C18 0.0199(3) 0.0253(4) 0.0198(3) -0.0015(3) 0.0024(3) 0.0009(3) C19 0.0234(4) 0.0462(6) 0.0218(4) -0.0017(4) -0.0012(3) 0.0081(4) C20 0.0298(5) 0.0664(8) 0.0229(4) -0.0061(5) 0.0085(4) -0.0068(5) C21 0.0241(4) 0.0367(5) 0.0290(4) -0.0038(4) -0.0034(3) 0.0055(3) C10A 0.030(5) 0.081(12) 0.020(4) 0.017(6) 0.013(3) 0.019(7) C11A 0.035(4) 0.042(6) 0.024(4) -0.004(4) -0.002(3) 0.008(4) C12A 0.065(8) 0.069(8) 0.027(5) -0.018(5) 0.004(4) 0.028(6) _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 O1 H1 1.292(17) . ? O1 C1 1.2958(11) . ? O2 H1 1.212(17) . ? O2 C3 1.2920(11) . ? O3 C7 1.3590(11) . ? O3 C10 1.4667(17) . ? O3 C10A 1.328(14) . ? O4 C15 1.3640(11) . ? O4 C19 1.4287(11) . ? O5 C16 1.3687(10) . ? O5 C20 1.4279(13) . ? O6 C17 1.3679(10) . ? O6 C21 1.4294(12) . ? C1 C2 1.4023(12) . ? C1 C13 1.4824(12) . ? C2 H2 0.9500 . ? C2 C3 1.4099(12) . ? C3 C4 1.4763(12) . ? C4 C5 1.3978(12) . ? C4 C9 1.3997(12) . ? C5 H5 0.9500 . ? C5 C6 1.3916(13) . ? C6 H6 0.9500 . ? C6 C7 1.3948(14) . ? C7 C8 1.4040(13) . ? C8 H8 0.9500 . ? C8 C9 1.3854(13) . ? C9 H9 0.9500 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.523(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.519(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.4004(12) . ? C13 C18 1.3985(11) . ? C14 H14 0.9500 . ? C14 C15 1.3940(12) . ? C15 C16 1.4050(11) . ? C16 C17 1.4017(12) . ? C17 C18 1.3943(12) . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C10A C11A 1.496(17) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C11A C12A 1.487(14) . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 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 O1 H1 99.8(8) . . ? C3 O2 H1 100.7(8) . . ? C7 O3 C10 115.70(10) . . ? C10A O3 C7 127.9(7) . . ? C15 O4 C19 117.58(7) . . ? C16 O5 C20 116.25(8) . . ? C17 O6 C21 117.05(7) . . ? O1 C1 C2 120.76(8) . . ? O1 C1 C13 116.51(8) . . ? C2 C1 C13 122.72(8) . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.82(8) . . ? C3 C2 H2 120.1 . . ? O2 C3 C2 120.56(8) . . ? O2 C3 C4 116.96(7) . . ? C2 C3 C4 122.47(8) . . ? C5 C4 C3 118.94(8) . . ? C5 C4 C9 118.13(8) . . ? C9 C4 C3 122.93(7) . . ? C4 C5 H5 119.3 . . ? C6 C5 C4 121.46(9) . . ? C6 C5 H5 119.3 . . ? C5 C6 H6 120.1 . . ? C5 C6 C7 119.72(8) . . ? C7 C6 H6 120.1 . . ? O3 C7 C6 124.14(8) . . ? O3 C7 C8 116.40(8) . . ? C6 C7 C8 119.46(8) . . ? C7 C8 H8 120.0 . . ? C9 C8 C7 120.07(8) . . ? C9 C8 H8 120.0 . . ? C4 C9 H9 119.4 . . ? C8 C9 C4 121.14(8) . . ? C8 C9 H9 119.4 . . ? O3 C10 H10A 110.1 . . ? O3 C10 H10B 110.1 . . ? O3 C10 C11 107.98(13) . . ? H10A C10 H10B 108.4 . . ? C11 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C10 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C12 C11 C10 114.35(11) . . ? C12 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C1 121.72(7) . . ? C18 C13 C1 117.88(7) . . ? C18 C13 C14 120.40(8) . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.53(8) . . ? C15 C14 H14 120.2 . . ? O4 C15 C14 124.39(8) . . ? O4 C15 C16 115.01(7) . . ? C14 C15 C16 120.59(8) . . ? O5 C16 C15 122.40(8) . . ? O5 C16 C17 118.31(7) . . ? C17 C16 C15 119.15(7) . . ? O6 C17 C16 115.38(7) . . ? O6 C17 C18 124.08(8) . . ? C18 C17 C16 120.53(7) . . ? C13 C18 H18 120.1 . . ? C17 C18 C13 119.71(8) . . ? C17 C18 H18 120.1 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? O5 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O3 C10A H10C 109.6 . . ? O3 C10A H10D 109.6 . . ? O3 C10A C11A 110.2(11) . . ? H10C C10A H10D 108.1 . . ? C11A C10A H10C 109.6 . . ? C11A C10A H10D 109.6 . . ? C10A C11A H11C 109.7 . . ? C10A C11A H11D 109.7 . . ? H11C C11A H11D 108.2 . . ? C12A C11A C10A 109.6(10) . . ? C12A C11A H11C 109.7 . . ? C12A C11A H11D 109.7 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12E 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 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 O1 C1 C2 C3 -1.21(13) . . . . ? O1 C1 C13 C14 172.46(8) . . . . ? O1 C1 C13 C18 -7.96(12) . . . . ? O2 C3 C4 C5 -14.14(12) . . . . ? O2 C3 C4 C9 165.93(9) . . . . ? O3 C7 C8 C9 -179.82(9) . . . . ? O3 C10 C11 C12 -69.23(16) . . . . ? O3 C10A C11A C12A -176.0(13) . . . . ? O4 C15 C16 O5 0.03(12) . . . . ? O4 C15 C16 C17 175.64(8) . . . . ? O5 C16 C17 O6 -0.42(12) . . . . ? O5 C16 C17 C18 178.76(8) . . . . ? O6 C17 C18 C13 178.48(8) . . . . ? C1 C2 C3 O2 -0.51(13) . . . . ? C1 C2 C3 C4 -179.28(8) . . . . ? C1 C13 C14 C15 179.88(8) . . . . ? C1 C13 C18 C17 179.38(8) . . . . ? C2 C1 C13 C14 -8.14(13) . . . . ? C2 C1 C13 C18 171.44(8) . . . . ? C2 C3 C4 C5 164.67(9) . . . . ? C2 C3 C4 C9 -15.26(13) . . . . ? C3 C4 C5 C6 -178.91(9) . . . . ? C3 C4 C9 C8 -179.83(9) . . . . ? C4 C5 C6 C7 -1.43(16) . . . . ? C5 C4 C9 C8 0.24(14) . . . . ? C5 C6 C7 O3 -178.91(9) . . . . ? C5 C6 C7 C8 0.58(15) . . . . ? C6 C7 C8 C9 0.66(15) . . . . ? C7 O3 C10 C11 -179.06(10) . . . . ? C7 O3 C10A C11A 168.9(7) . . . . ? C7 C8 C9 C4 -1.08(15) . . . . ? C9 C4 C5 C6 1.02(14) . . . . ? C10 O3 C7 C6 -6.87(15) . . . . ? C10 O3 C7 C8 173.63(11) . . . . ? C13 C1 C2 C3 179.41(8) . . . . ? C13 C14 C15 O4 -177.20(8) . . . . ? C13 C14 C15 C16 2.08(13) . . . . ? C14 C13 C18 C17 -1.04(13) . . . . ? C14 C15 C16 O5 -179.32(8) . . . . ? C14 C15 C16 C17 -3.70(13) . . . . ? C15 C16 C17 O6 -176.21(8) . . . . ? C15 C16 C17 C18 2.97(13) . . . . ? C16 C17 C18 C13 -0.62(13) . . . . ? C18 C13 C14 C15 0.32(13) . . . . ? C19 O4 C15 C14 -4.71(14) . . . . ? C19 O4 C15 C16 175.97(8) . . . . ? C20 O5 C16 C15 -60.64(12) . . . . ? C20 O5 C16 C17 123.71(10) . . . . ? C21 O6 C17 C16 -177.63(8) . . . . ? C21 O6 C17 C18 3.22(13) . . . . ? C10A O3 C7 C6 10.0(11) . . . . ? C10A O3 C7 C8 -169.5(11) . . . . ? _shelx_res_file ; TITL fraser41_0m_a.res in P2(1)/n fraser41_0m.res created by SHELXL-2017/1 at 13:32:41 on 10-Oct-2018 REM Old TITL Fraser41_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.132, Rweak 0.002, Alpha 0.019, Orientation as input REM Formula found by SHELXT: C21 O6 CELL 0.71073 9.1237 15.3257 13.5649 90 102.75 90 ZERR 4 0.0006 0.001 0.0009 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 84 96 24 SADI O3 C10 O3 C10A L.S. 4 PLAN 20 TEMP -109.95 BOND $H CONF list 4 fmap 2 acta REM REM REM WGHT 0.068900 0.591300 FVAR 0.63733 0.88301 O1 3 0.377274 0.435207 0.046376 11.00000 0.02451 0.04174 = 0.02487 -0.00346 0.00273 0.00910 H1 2 0.383616 0.468016 0.134964 11.00000 -1.50000 O2 3 0.432950 0.482950 0.223832 11.00000 0.02688 0.04092 = 0.02494 -0.00290 0.00570 0.01010 O3 3 0.920668 0.455041 0.634144 11.00000 0.02882 0.03486 = 0.02169 -0.00364 0.00218 0.00015 O4 3 0.844260 0.225230 -0.104005 11.00000 0.02275 0.04295 = 0.01971 -0.00478 -0.00009 0.00958 O5 3 0.628413 0.222196 -0.277591 11.00000 0.02649 0.03221 = 0.01972 -0.00669 0.00477 -0.00155 O6 3 0.360154 0.290247 -0.287038 11.00000 0.02138 0.03548 = 0.01975 -0.00415 -0.00247 0.00333 C1 1 0.504636 0.394265 0.063219 11.00000 0.02130 0.02559 = 0.01978 -0.00162 0.00474 -0.00015 C2 1 0.599531 0.393882 0.159832 11.00000 0.02113 0.02697 = 0.01921 -0.00345 0.00404 0.00216 AFIX 43 H2 2 0.691781 0.362726 0.171674 11.00000 -1.20000 AFIX 0 C3 1 0.557662 0.439860 0.239348 11.00000 0.02243 0.02441 = 0.02031 -0.00106 0.00636 -0.00028 C4 1 0.653278 0.442877 0.342414 11.00000 0.02242 0.02327 = 0.01921 -0.00178 0.00649 -0.00006 C5 1 0.623399 0.505617 0.410153 11.00000 0.02881 0.02925 = 0.02187 -0.00359 0.00545 0.00564 AFIX 43 H5 2 0.541262 0.544436 0.389138 11.00000 -1.20000 AFIX 0 C6 1 0.711301 0.512477 0.507690 11.00000 0.03086 0.03235 = 0.02258 -0.00580 0.00589 0.00461 AFIX 43 H6 2 0.690498 0.556436 0.552057 11.00000 -1.20000 AFIX 0 C7 1 0.830081 0.454539 0.540043 11.00000 0.02361 0.02811 = 0.01973 -0.00112 0.00524 -0.00179 C8 1 0.860254 0.390433 0.473284 11.00000 0.02661 0.02899 = 0.02487 -0.00269 0.00317 0.00461 AFIX 43 H8 2 0.940293 0.350344 0.494984 11.00000 -1.20000 AFIX 0 C9 1 0.773435 0.385571 0.375799 11.00000 0.02771 0.02633 = 0.02303 -0.00456 0.00520 0.00349 AFIX 43 H9 2 0.795841 0.342602 0.330836 11.00000 -1.20000 AFIX 0 PART 1 C10 1 0.898395 0.527996 0.699268 21.00000 0.02824 0.03177 = 0.02011 -0.00397 0.00478 0.00176 AFIX 23 H10A 2 0.794549 0.527208 0.710021 21.00000 -1.20000 H10B 2 0.914623 0.584140 0.667188 21.00000 -1.20000 AFIX 0 C11 1 1.010773 0.518129 0.799864 21.00000 0.02872 0.03098 = 0.02563 -0.00611 0.00305 -0.00111 AFIX 23 H11A 2 1.112546 0.511244 0.786538 21.00000 -1.20000 H11B 2 1.010552 0.572429 0.839363 21.00000 -1.20000 AFIX 0 C12 1 0.979867 0.441522 0.863349 21.00000 0.04249 0.04768 = 0.02872 0.00425 0.00712 -0.00001 AFIX 137 H12A 2 0.881881 0.449384 0.880561 21.00000 -1.50000 H12B 2 1.058428 0.438425 0.925519 21.00000 -1.50000 H12C 2 0.979352 0.387327 0.824930 21.00000 -1.50000 AFIX 0 PART 0 C13 1 0.542134 0.348094 -0.024035 11.00000 0.02060 0.02371 = 0.01786 -0.00154 0.00373 -0.00081 C14 1 0.683436 0.310217 -0.018353 11.00000 0.02095 0.02881 = 0.01718 -0.00236 0.00197 0.00018 AFIX 43 H14 2 0.758555 0.313707 0.042404 11.00000 -1.20000 AFIX 0 C15 1 0.713083 0.267357 -0.102480 11.00000 0.01981 0.02688 = 0.01720 -0.00121 0.00186 0.00159 C16 1 0.604318 0.264343 -0.193623 11.00000 0.02094 0.02278 = 0.01651 -0.00176 0.00240 -0.00100 C17 1 0.462141 0.300588 -0.197356 11.00000 0.02005 0.02288 = 0.01720 -0.00075 0.00069 -0.00122 C18 1 0.431021 0.342717 -0.113185 11.00000 0.01988 0.02526 = 0.01985 -0.00147 0.00243 0.00095 AFIX 43 H18 2 0.334761 0.367659 -0.116384 11.00000 -1.20000 AFIX 0 C19 1 0.962819 0.230880 -0.015669 11.00000 0.02345 0.04615 = 0.02175 -0.00175 -0.00121 0.00810 AFIX 137 H19A 2 1.049439 0.197140 -0.025992 11.00000 -1.50000 H19B 2 0.928227 0.207314 0.042406 11.00000 -1.50000 H19C 2 0.992112 0.292061 -0.002830 11.00000 -1.50000 AFIX 0 C20 1 0.750648 0.253410 -0.317814 11.00000 0.02978 0.06639 = 0.02290 -0.00605 0.00846 -0.00679 AFIX 137 H20A 2 0.748279 0.225205 -0.382985 11.00000 -1.50000 H20B 2 0.845773 0.239714 -0.270741 11.00000 -1.50000 H20C 2 0.741786 0.316734 -0.327321 11.00000 -1.50000 AFIX 0 C21 1 0.215670 0.329258 -0.295153 11.00000 0.02406 0.03666 = 0.02902 -0.00376 -0.00336 0.00545 AFIX 137 H21A 2 0.154385 0.319490 -0.363252 11.00000 -1.50000 H21B 2 0.227519 0.392094 -0.282482 11.00000 -1.50000 H21C 2 0.166049 0.302935 -0.245289 11.00000 -1.50000 AFIX 0 PART 2 C10A 1 0.902798 0.499821 0.714448 -21.00000 0.03042 0.08123 = 0.02038 0.01713 0.01340 0.01884 AFIX 23 H10C 2 0.798554 0.492672 0.723155 -21.00000 -1.20000 H10D 2 0.920126 0.562625 0.704272 -21.00000 -1.20000 AFIX 0 C11A 1 1.010781 0.468242 0.807103 -21.00000 0.03534 0.04186 = 0.02379 -0.00365 -0.00172 0.00796 AFIX 23 H11C 2 0.998409 0.404600 0.814779 -21.00000 -1.20000 H11D 2 1.115141 0.479326 0.800623 -21.00000 -1.20000 AFIX 0 C12A 1 0.982293 0.514464 0.897453 -21.00000 0.06480 0.06888 = 0.02743 -0.01781 0.00407 0.02832 AFIX 137 H12D 2 0.957568 0.575629 0.880339 -21.00000 -1.50000 H12E 2 1.072418 0.511590 0.952223 -21.00000 -1.50000 H12F 2 0.898122 0.486627 0.919330 -21.00000 -1.50000 AFIX 0 HKLF 4 REM fraser41_0m_a.res in P2(1)/n REM R1 = 0.0504 for 6249 Fo > 4sig(Fo) and 0.0564 for all 7046 data REM 280 parameters refined using 1 restraints END WGHT 0.0689 0.5913 REM Highest difference peak 0.418, deepest hole -0.515, 1-sigma level 0.098 Q1 1 0.4469 0.3219 -0.1575 11.00000 0.05 0.42 Q2 1 0.7001 0.2897 -0.0584 11.00000 0.05 0.37 Q3 1 0.5323 0.2807 -0.1946 11.00000 0.05 0.35 Q4 1 0.6194 0.3339 -0.0178 11.00000 0.05 0.34 Q5 1 0.6712 0.5130 0.4594 11.00000 0.05 0.31 Q6 1 0.6549 0.2640 -0.1481 11.00000 0.05 0.31 Q7 1 0.4951 0.3445 -0.0731 11.00000 0.05 0.30 Q8 1 0.5336 0.3758 0.0202 11.00000 0.05 0.29 Q9 1 0.5892 0.4200 0.1937 11.00000 0.05 0.29 Q10 1 0.8184 0.3920 0.4241 11.00000 0.05 0.27 Q11 1 0.8444 0.4152 0.5151 11.00000 0.05 0.27 Q12 1 0.7573 0.4772 0.5240 11.00000 0.05 0.26 Q13 1 0.9568 0.4152 0.6349 11.00000 0.05 0.26 Q14 1 0.5509 0.3945 0.1108 11.00000 0.05 0.25 Q15 1 0.5997 0.3908 -0.2732 11.00000 0.05 0.24 Q16 1 0.8283 0.2807 -0.2826 11.00000 0.05 0.24 Q17 1 0.6444 0.4836 0.3639 11.00000 0.05 0.24 Q18 1 0.7487 0.4058 0.8961 11.00000 0.05 0.24 Q19 1 0.1210 0.2718 -0.1587 11.00000 0.05 0.23 Q20 1 1.0554 0.5911 0.8224 11.00000 0.05 0.23 ; _shelx_res_checksum 289 _shelx_hkl_file ; -2 0 0 764.42 21.90 -3 0 0 0.00 0.10 3 0 0 -0.10 0.10 3 0 0 0.00 0.10 -3 0 0 0.00 0.10 3 0 0 0.00 0.10 4 0 0 995.70 28.10 4 0 0 963.70 28.20 4 0 0 963.30 28.20 -4 0 0 977.10 28.30 -4 0 0 998.10 28.20 5 0 0 -0.20 0.10 5 0 0 0.40 0.10 -6 0 0 -0.20 0.10 6 0 0 -0.10 0.10 6 0 0 -0.20 0.10 -6 0 0 -0.10 0.10 6 0 0 0.10 0.10 7 0 0 -0.10 0.10 7 0 0 -0.10 0.20 -7 0 0 -0.40 0.20 8 0 0 52.89 1.80 8 0 0 58.19 1.80 -8 0 0 56.29 1.80 -8 0 0 53.99 1.80 -9 0 0 -0.30 0.20 9 0 0 0.30 0.20 9 0 0 -0.20 0.30 -9 0 0 -0.30 0.20 -10 0 0 19.50 0.90 -10 0 0 19.40 0.90 10 0 0 19.20 0.90 -11 0 0 -0.20 0.30 11 0 0 0.00 0.30 -11 0 0 -0.40 0.30 -12 0 0 23.00 1.10 12 0 0 24.80 1.20 -12 0 0 24.90 1.10 -13 0 0 0.10 0.40 13 0 0 -0.10 0.40 -13 0 0 0.00 0.40 -13 0 0 -0.50 0.30 -2 -1 0 132.39 3.70 2 -1 0 131.59 3.80 -2 1 0 129.19 3.70 2 1 0 129.79 3.80 3 -1 0 141.89 4.10 -3 -1 0 142.59 4.10 -3 -1 0 143.29 4.10 3 -1 0 143.89 4.10 -3 1 0 139.49 4.10 -3 1 0 144.09 4.10 3 1 0 142.49 4.10 4 -1 0 106.29 3.10 -4 -1 0 109.59 3.10 4 -1 0 108.09 3.10 -4 -1 0 114.79 3.10 4 -1 0 102.89 3.10 -4 1 0 110.89 3.10 4 1 0 103.19 3.10 4 1 0 104.09 3.10 -4 1 0 103.29 3.10 4 1 0 108.19 3.10 -5 -1 0 163.38 4.80 5 -1 0 168.88 4.80 5 -1 0 165.48 4.80 -5 -1 0 172.08 4.80 5 -1 0 158.68 4.80 5 1 0 163.58 4.80 5 1 0 163.28 4.80 5 1 0 163.18 4.80 -5 1 0 168.68 4.80 -5 1 0 173.58 4.80 -6 -1 0 10.40 0.50 6 -1 0 9.70 0.50 6 -1 0 10.40 0.50 -6 -1 0 10.60 0.50 6 -1 0 9.90 0.50 6 1 0 9.90 0.40 6 1 0 10.60 0.50 -6 1 0 9.00 0.60 -6 1 0 10.10 0.50 6 1 0 10.00 0.50 -6 1 0 9.70 0.50 7 -1 0 3.70 0.40 7 -1 0 4.00 0.40 -7 -1 0 4.20 0.40 -7 -1 0 4.10 0.40 7 1 0 4.40 0.40 -7 1 0 4.50 0.40 -7 1 0 3.50 0.40 7 1 0 4.60 0.40 -8 -1 0 309.57 9.00 8 -1 0 320.57 9.00 -8 -1 0 314.07 9.00 8 -1 0 303.87 9.10 -8 1 0 311.97 9.00 8 1 0 314.07 9.10 -8 1 0 314.67 9.00 8 1 0 306.27 9.00 -9 -1 0 30.90 1.10 -9 -1 0 30.30 1.10 9 -1 0 30.10 1.10 -9 1 0 29.90 1.10 -9 1 0 29.60 1.10 9 1 0 29.30 1.10 9 1 0 29.00 1.20 -10 -1 0 1.20 0.30 -10 -1 0 1.70 0.30 10 -1 0 1.20 0.30 -10 1 0 1.10 0.30 10 1 0 1.30 0.30 -10 1 0 1.30 0.30 -11 -1 0 31.10 1.20 11 -1 0 32.00 1.30 -11 -1 0 30.90 1.30 -11 1 0 31.00 1.30 -11 1 0 32.60 1.30 11 1 0 31.00 1.30 -12 -1 0 54.49 1.90 12 -1 0 55.29 2.00 -12 -1 0 55.09 1.90 -12 1 0 55.19 1.90 -12 1 0 56.99 2.00 12 1 0 54.99 2.00 -13 -1 0 7.40 0.90 -13 -1 0 7.60 0.80 -13 -1 0 8.60 0.90 13 -1 0 8.80 0.90 -13 1 0 8.70 0.80 13 1 0 7.00 0.90 -1 -2 0 290.97 8.40 1 -2 0 294.97 8.40 -2 -2 0 2382.96 71.29 2 -2 0 2490.25 69.49 2 2 0 2411.76 72.99 -2 2 0 2468.35 71.69 -3 -2 0 4.20 0.20 -3 -2 0 3.50 0.20 3 -2 0 3.70 0.20 3 -2 0 3.60 0.20 3 2 0 3.60 0.20 -3 2 0 3.70 0.20 -3 2 0 3.90 0.20 4 -2 0 47.30 1.40 4 -2 0 43.60 1.40 -4 -2 0 46.00 1.40 -4 -2 0 45.60 1.40 4 -2 0 45.80 1.40 4 2 0 49.30 1.40 -4 2 0 46.40 1.40 4 2 0 43.90 1.40 -4 2 0 44.30 1.40 -4 2 0 43.90 1.40 5 -2 0 96.09 2.80 -5 -2 0 96.59 2.80 -5 -2 0 96.89 2.80 5 -2 0 94.69 2.80 5 -2 0 92.99 2.80 5 2 0 92.29 2.80 5 2 0 92.19 2.80 -5 2 0 96.29 2.80 -5 2 0 97.79 2.80 5 2 0 95.79 2.80 6 -2 0 95.69 2.90 6 -2 0 94.19 2.90 -6 -2 0 96.79 2.80 6 -2 0 98.19 2.90 -6 -2 0 96.39 2.80 6 2 0 96.09 2.90 6 2 0 94.19 2.80 6 2 0 97.69 2.90 -6 2 0 99.29 2.90 -6 2 0 91.09 2.90 -6 2 0 96.39 2.90 -7 -2 0 40.10 1.30 7 -2 0 38.80 1.30 -7 -2 0 40.70 1.30 7 -2 0 38.50 1.30 -7 2 0 39.10 1.30 -7 2 0 38.90 1.30 7 2 0 39.20 1.30 7 2 0 41.60 1.30 -8 -2 0 14.70 0.60 -8 -2 0 14.50 0.60 8 -2 0 15.10 0.70 8 -2 0 13.30 0.70 8 2 0 15.00 0.70 8 2 0 13.20 0.70 -8 2 0 13.70 0.70 -8 2 0 13.90 0.70 -9 -2 0 0.50 0.20 9 -2 0 0.70 0.30 -9 -2 0 0.40 0.20 9 2 0 0.80 0.30 -9 2 0 0.90 0.30 -9 2 0 0.90 0.20 9 2 0 0.80 0.30 -10 -2 0 63.99 2.10 -10 -2 0 63.79 2.10 10 -2 0 66.49 2.10 10 2 0 63.99 2.10 -10 2 0 63.19 2.10 10 2 0 61.09 2.20 -10 2 0 64.59 2.10 11 -2 0 1.20 0.40 -11 -2 0 0.50 0.30 -11 -2 0 0.50 0.30 11 2 0 0.70 0.30 -11 2 0 0.70 0.30 -11 2 0 0.50 0.30 -12 -2 0 38.50 1.50 12 -2 0 39.50 1.60 -12 -2 0 36.70 1.40 12 2 0 36.30 1.50 -12 2 0 40.20 1.50 -12 2 0 36.70 1.60 -13 -2 0 17.90 1.10 13 -2 0 20.00 1.20 13 2 0 18.10 1.20 -13 2 0 21.00 1.10 0 3 0 0.60 0.10 1 -3 0 2460.35 70.09 -1 -3 0 2368.56 69.49 1 3 0 2354.16 70.29 -1 3 0 2414.16 71.69 2 -3 0 602.64 17.10 -2 -3 0 586.64 17.30 2 -3 0 596.94 19.50 2 3 0 582.74 19.30 -2 3 0 596.94 17.10 -2 3 0 597.84 17.10 3 -3 0 718.23 20.60 3 -3 0 716.03 20.60 -3 -3 0 748.03 20.70 -3 -3 0 702.03 20.60 -3 3 0 720.83 20.80 -3 3 0 711.43 20.80 -3 3 0 707.73 20.60 3 3 0 736.13 20.80 -4 -3 0 146.49 4.20 4 -3 0 144.99 4.20 4 -3 0 146.59 4.20 4 -3 0 137.29 4.20 -4 -3 0 149.29 4.20 -4 3 0 148.49 4.20 -4 3 0 144.59 4.20 -4 3 0 146.09 4.30 4 3 0 143.29 4.20 4 3 0 148.79 4.20 5 -3 0 27.10 0.90 5 -3 0 25.30 0.90 -5 -3 0 27.50 0.90 -5 -3 0 27.00 0.90 5 -3 0 26.00 0.90 -5 3 0 26.60 0.90 5 3 0 26.60 0.90 -5 3 0 24.70 0.90 5 3 0 27.00 0.90 -5 3 0 25.60 0.90 -6 -3 0 23.60 0.80 6 -3 0 23.80 0.80 6 -3 0 24.50 0.90 6 -3 0 22.80 0.90 -6 -3 0 24.30 0.80 6 3 0 23.30 0.80 6 3 0 24.10 0.90 -6 3 0 23.90 0.90 -6 3 0 23.60 0.80 -7 -3 0 28.60 0.90 7 -3 0 27.10 1.00 -7 -3 0 27.80 0.90 7 -3 0 28.40 1.00 7 -3 0 25.40 1.00 -7 3 0 26.80 1.00 7 3 0 27.10 1.00 -7 3 0 28.20 1.00 7 3 0 28.00 1.00 -8 -3 0 258.17 7.50 8 -3 0 253.17 7.50 8 -3 0 259.97 7.50 -8 -3 0 262.07 7.50 8 3 0 250.47 7.50 -8 3 0 263.07 7.50 -8 3 0 255.17 7.50 8 3 0 253.17 7.50 -9 -3 0 62.99 2.00 9 -3 0 61.49 2.00 -9 -3 0 59.89 1.90 9 3 0 63.29 2.00 -9 3 0 59.29 2.00 -9 3 0 61.09 2.00 9 3 0 58.09 2.00 -10 -3 0 14.40 0.70 10 -3 0 14.80 0.90 -10 -3 0 15.30 0.80 -10 3 0 15.50 0.80 10 3 0 14.50 0.80 -10 3 0 15.20 0.80 10 3 0 15.40 0.80 11 -3 0 71.89 2.30 -11 -3 0 67.39 2.30 -11 -3 0 66.49 2.20 -11 3 0 67.79 2.30 -11 3 0 70.89 2.30 11 3 0 67.99 2.30 -12 -3 0 1.40 0.40 -12 -3 0 1.40 0.40 12 -3 0 2.00 0.40 -12 3 0 1.40 0.40 12 3 0 1.60 0.40 13 -3 0 1.70 0.40 -13 -3 0 0.70 0.40 -13 3 0 1.70 0.40 13 3 0 1.00 0.40 0 -4 0 6045.99 174.08 0 4 0 6070.49 174.88 -1 -4 0 1220.28 36.90 1 -4 0 1310.57 36.00 -1 4 0 1277.57 36.10 1 4 0 1230.48 37.10 2 -4 0 15.70 0.50 -2 -4 0 15.80 0.50 2 -4 0 15.30 0.50 2 4 0 15.30 0.50 -2 4 0 14.90 0.50 3 -4 0 935.91 27.10 -3 -4 0 920.61 28.90 3 -4 0 935.11 27.30 -3 -4 0 969.10 27.00 3 -4 0 962.40 30.00 -3 4 0 915.81 26.90 -3 4 0 931.61 27.00 3 4 0 973.90 27.10 -3 4 0 928.21 27.20 -4 -4 0 516.55 14.70 4 -4 0 506.05 14.40 -4 -4 0 501.75 14.40 4 -4 0 515.85 14.40 4 4 0 490.75 14.40 -4 4 0 485.55 14.40 -4 4 0 508.45 14.30 4 4 0 501.65 15.90 -4 4 0 495.25 14.40 -5 -4 0 14.40 0.50 5 -4 0 11.70 0.50 -5 -4 0 13.10 0.50 5 -4 0 13.40 0.50 -5 4 0 13.30 0.60 5 4 0 13.70 0.50 -5 4 0 12.20 0.60 5 4 0 15.40 0.50 -5 4 0 12.30 0.50 -6 -4 0 1.10 0.20 6 -4 0 1.30 0.20 6 -4 0 0.90 0.20 -6 -4 0 0.80 0.10 6 -4 0 1.40 0.20 -6 4 0 0.90 0.20 -6 4 0 0.80 0.20 6 4 0 0.80 0.20 -6 4 0 0.90 0.20 6 4 0 0.80 0.20 7 -4 0 121.99 3.60 -7 -4 0 122.89 3.60 -7 -4 0 121.09 3.60 7 -4 0 118.49 3.60 7 4 0 115.89 3.60 7 4 0 125.59 3.60 -7 4 0 119.79 3.60 -7 4 0 120.29 3.60 -8 -4 0 15.40 0.60 -8 -4 0 14.40 0.70 8 -4 0 16.80 0.70 8 -4 0 15.10 0.70 8 4 0 14.70 0.70 -8 4 0 14.90 0.70 8 4 0 15.70 0.70 -8 4 0 14.40 0.70 -9 -4 0 74.79 2.30 9 -4 0 76.19 2.40 -9 -4 0 74.79 2.30 9 4 0 71.49 2.30 -9 4 0 73.89 2.40 9 4 0 75.19 2.40 -9 4 0 71.29 2.30 -10 -4 0 1.30 0.30 -10 -4 0 0.90 0.30 10 -4 0 0.90 0.30 -10 4 0 1.00 0.30 -10 4 0 1.50 0.30 10 4 0 1.10 0.30 10 4 0 1.40 0.30 -11 -4 0 55.99 1.90 -11 -4 0 53.39 1.90 11 -4 0 60.19 2.00 11 4 0 56.09 2.00 -11 4 0 57.69 2.00 -12 -4 0 3.00 0.40 12 -4 0 3.60 0.50 -12 4 0 3.60 0.50 12 4 0 2.80 0.40 -13 -4 0 2.50 0.50 13 -4 0 3.50 0.50 13 4 0 2.90 0.50 -13 4 0 3.40 0.50 0 -5 0 -0.10 0.10 0 5 0 -0.10 0.10 -1 -5 0 439.36 12.90 1 -5 0 468.55 12.90 1 5 0 442.76 13.80 -1 5 0 449.06 12.90 2 -5 0 428.96 12.20 -2 -5 0 420.66 12.20 2 -5 0 425.96 12.10 2 -5 0 431.06 12.10 -2 5 0 421.26 12.10 2 5 0 430.96 12.40 -2 5 0 404.46 12.10 3 -5 0 534.65 15.20 3 -5 0 538.15 15.20 -3 -5 0 544.05 15.30 3 -5 0 523.95 15.20 -3 5 0 523.95 15.20 3 5 0 551.64 15.40 -3 5 0 531.35 15.20 -3 5 0 512.25 15.20 4 -5 0 2.40 0.20 -4 -5 0 2.00 0.20 4 -5 0 1.60 0.30 4 -5 0 1.80 0.20 4 5 0 2.20 0.20 -4 5 0 2.00 0.30 5 -5 0 62.49 1.90 -5 -5 0 62.39 1.80 -5 -5 0 61.49 1.80 5 -5 0 57.19 1.90 5 -5 0 60.09 1.90 -5 5 0 59.09 1.80 -5 5 0 59.49 1.90 5 5 0 62.39 1.90 -5 5 0 61.19 1.90 5 5 0 61.29 1.80 6 -5 0 59.69 1.90 -6 -5 0 60.79 1.80 -6 -5 0 60.39 1.80 6 -5 0 60.39 1.90 6 5 0 59.69 1.80 -6 5 0 58.49 1.90 6 5 0 62.99 1.90 -6 5 0 59.29 1.90 -6 5 0 60.69 1.90 7 -5 0 49.50 1.60 -7 -5 0 49.60 1.50 7 -5 0 47.00 1.60 -7 -5 0 49.00 1.50 -7 5 0 47.90 1.60 7 5 0 49.10 1.60 -7 5 0 47.40 1.60 7 5 0 47.60 1.50 -8 -5 0 93.09 2.70 8 -5 0 89.89 2.80 -8 -5 0 89.19 2.70 8 -5 0 89.39 2.80 -8 5 0 92.79 2.80 -8 5 0 90.69 2.70 8 5 0 89.19 2.80 8 5 0 83.89 2.70 -9 -5 0 94.99 2.90 9 -5 0 98.89 3.00 9 -5 0 95.79 3.10 -9 -5 0 100.09 3.00 -9 5 0 98.39 3.00 9 5 0 98.39 3.00 -9 5 0 93.39 3.00 9 5 0 95.49 3.00 -10 -5 0 1.00 0.30 -10 -5 0 1.50 0.30 10 -5 0 1.80 0.40 10 5 0 1.10 0.30 -10 5 0 1.20 0.30 10 5 0 1.40 0.30 -11 -5 0 100.79 3.20 11 -5 0 108.69 3.30 -11 -5 0 103.79 3.20 -11 5 0 108.59 3.30 11 5 0 100.79 3.30 11 5 0 98.99 3.30 -12 -5 0 4.40 0.50 12 5 0 4.50 0.50 13 -5 0 0.60 0.40 -13 -5 0 0.60 0.40 13 5 0 0.80 0.40 -13 5 0 0.70 0.40 0 -6 0 351.66 10.00 0 6 0 348.57 10.00 1 -6 0 953.80 28.10 1 -6 0 1014.70 28.20 -1 -6 0 992.60 28.10 -1 6 0 994.00 28.30 1 6 0 954.90 28.30 1 6 0 996.90 31.00 2 -6 0 41.60 1.20 2 -6 0 40.20 1.20 2 -6 0 39.90 1.30 -2 -6 0 39.90 1.20 2 6 0 40.30 1.20 -2 6 0 41.60 1.30 2 6 0 38.50 1.20 -2 6 0 38.70 1.20 3 -6 0 490.95 14.00 3 -6 0 493.75 13.90 -3 -6 0 498.65 16.00 3 -6 0 490.15 14.00 -3 6 0 470.25 13.90 3 6 0 493.35 14.10 -3 6 0 479.25 13.90 -3 6 0 480.05 13.90 -4 -6 0 228.98 6.70 4 -6 0 243.08 6.80 4 -6 0 233.98 6.80 4 -6 0 243.28 6.80 -4 -6 0 240.58 6.70 4 6 0 237.08 6.80 -4 6 0 231.38 6.80 4 6 0 228.08 6.70 -4 6 0 228.58 6.80 -4 6 0 231.98 6.80 -5 -6 0 95.09 2.70 5 -6 0 89.79 2.70 5 -6 0 90.49 2.80 -5 -6 0 89.49 2.70 5 -6 0 92.19 2.70 -5 6 0 91.99 2.70 -5 6 0 90.19 2.80 5 6 0 92.29 2.70 -5 6 0 90.89 2.70 5 6 0 90.09 2.70 -6 -6 0 24.10 0.80 6 -6 0 23.50 0.90 -6 -6 0 23.70 0.80 6 6 0 23.40 0.80 -6 6 0 23.90 0.90 -6 6 0 23.00 0.90 -6 6 0 23.30 0.80 6 6 0 25.00 0.90 7 -6 0 51.39 1.70 -7 -6 0 51.09 1.60 -7 -6 0 52.29 1.60 7 -6 0 51.19 1.70 -7 6 0 51.79 1.70 -7 6 0 49.80 1.60 7 6 0 52.79 1.70 7 6 0 48.60 1.60 8 -6 0 246.88 7.10 8 -6 0 240.98 7.10 -8 -6 0 251.27 7.00 -8 -6 0 240.68 7.00 -8 6 0 245.48 7.10 -8 6 0 234.68 7.10 8 6 0 230.18 7.00 8 6 0 242.98 7.10 9 -6 0 185.28 5.70 -9 -6 0 192.78 5.60 9 -6 0 195.28 5.70 -9 6 0 195.88 5.70 9 6 0 193.68 5.70 9 6 0 183.38 5.60 -10 -6 0 7.40 0.70 -10 -6 0 6.00 0.70 10 -6 0 8.90 0.80 10 6 0 7.00 0.70 -10 6 0 8.70 0.80 10 6 0 6.90 0.70 11 -6 0 34.20 1.40 -11 -6 0 31.90 1.30 11 6 0 31.30 1.30 11 6 0 29.90 1.30 -11 6 0 33.90 1.40 12 -6 0 2.50 0.40 -12 -6 0 1.30 0.40 -12 6 0 2.90 0.50 12 6 0 1.20 0.40 -13 -6 0 15.20 1.10 13 -6 0 16.80 1.20 -13 6 0 15.80 1.10 13 6 0 13.40 1.10 0 -7 0 0.10 0.10 0 7 0 0.20 0.10 1 -7 0 107.49 3.20 1 -7 0 113.99 3.20 -1 -7 0 113.09 3.20 -1 7 0 109.39 3.20 1 7 0 112.39 3.20 1 7 0 105.89 3.20 2 -7 0 292.37 8.60 2 -7 0 295.97 8.70 2 -7 0 306.47 8.60 -2 -7 0 298.47 9.00 2 7 0 307.77 8.70 -2 7 0 305.37 8.60 2 7 0 293.47 8.60 -2 7 0 295.37 8.60 3 -7 0 336.27 9.60 3 -7 0 337.67 9.70 -3 -7 0 344.57 9.60 3 -7 0 344.87 9.60 -3 7 0 333.87 9.60 3 7 0 344.57 9.70 3 7 0 318.77 9.60 -3 7 0 327.27 9.60 3 7 0 321.17 9.60 -3 7 0 345.37 9.70 4 -7 0 600.84 17.20 4 -7 0 605.34 17.20 -4 -7 0 607.04 18.70 4 -7 0 605.74 17.30 4 7 0 612.44 17.40 4 7 0 568.44 17.20 -4 7 0 600.44 17.20 -4 7 0 614.74 17.20 -4 7 0 588.74 17.10 5 -7 0 37.60 1.20 5 -7 0 37.00 1.20 -5 -7 0 34.60 1.10 5 -7 0 36.70 1.30 -5 -7 0 38.30 1.20 -5 -7 0 37.40 1.20 5 7 0 35.70 1.20 -5 7 0 37.10 1.20 5 7 0 38.40 1.20 -5 7 0 37.50 1.30 -5 7 0 36.80 1.20 -6 -7 0 1.60 0.20 -6 -7 0 2.20 0.20 6 -7 0 1.70 0.20 6 -7 0 2.10 0.20 6 7 0 2.40 0.30 -6 7 0 1.90 0.30 6 7 0 2.20 0.30 -6 7 0 1.60 0.20 -6 7 0 1.90 0.20 7 -7 0 61.29 2.00 7 -7 0 64.79 2.00 -7 -7 0 63.89 1.90 7 7 0 58.69 1.90 -7 7 0 61.29 2.20 7 7 0 64.69 2.00 -7 7 0 62.59 2.00 8 -7 0 66.79 2.10 -8 -7 0 66.79 2.10 8 -7 0 63.99 2.10 -8 -7 0 69.09 2.10 8 7 0 65.59 2.10 8 7 0 62.09 2.10 -8 7 0 66.49 2.20 9 -7 0 1.90 0.30 9 7 0 1.40 0.30 -9 7 0 2.00 0.40 9 7 0 1.40 0.30 -10 -7 0 6.90 0.70 10 7 0 6.10 0.70 10 7 0 6.20 0.70 -10 7 0 9.20 0.80 -11 -7 0 12.90 0.90 11 -7 0 15.40 1.00 -11 7 0 14.60 1.00 11 7 0 12.20 0.90 11 7 0 13.20 0.90 -12 -7 0 13.30 1.00 12 -7 0 17.20 1.10 12 7 0 15.50 1.40 -12 7 0 17.80 1.20 12 7 0 14.40 1.10 -13 -7 0 -0.20 0.40 13 -7 0 0.20 0.50 -13 7 0 -0.10 0.50 0 -8 0 2.10 0.20 0 8 0 3.00 0.20 0 8 0 2.10 0.20 1 -8 0 1.10 0.10 -1 -8 0 1.90 0.20 1 -8 0 1.60 0.10 1 8 0 1.50 0.20 1 8 0 1.30 0.20 -2 -8 0 48.20 1.40 2 -8 0 46.70 1.40 2 -8 0 48.80 1.50 2 -8 0 47.10 1.60 2 8 0 46.70 1.50 2 8 0 49.60 1.40 -2 8 0 49.90 1.50 -2 8 0 47.00 1.50 -3 -8 0 144.69 4.20 3 -8 0 144.89 4.20 3 -8 0 145.09 4.40 3 -8 0 145.39 4.20 -3 8 0 143.89 4.20 3 8 0 141.39 4.20 -3 8 0 148.89 4.30 3 8 0 145.09 4.20 -4 -8 0 104.19 3.00 4 -8 0 104.19 3.10 4 -8 0 105.19 3.00 4 -8 0 102.89 3.00 4 8 0 103.29 3.00 -4 8 0 103.69 3.10 -4 8 0 103.29 3.00 4 8 0 98.09 3.00 4 8 0 95.39 3.10 -4 8 0 97.89 3.00 5 -8 0 225.48 6.50 5 -8 0 228.38 6.50 -5 -8 0 228.58 6.50 5 -8 0 226.18 6.60 5 8 0 227.88 6.50 -5 8 0 224.68 6.60 5 8 0 209.98 6.50 -5 8 0 225.38 6.50 6 -8 0 73.19 2.20 -6 -8 0 75.39 2.20 6 -8 0 71.79 2.30 6 8 0 68.69 2.20 -6 8 0 72.69 2.30 -6 8 0 73.59 2.30 6 8 0 73.39 2.20 7 -8 0 208.18 6.10 -7 -8 0 213.38 6.00 7 -8 0 203.28 6.10 -7 8 0 212.38 6.10 7 8 0 209.38 6.10 7 8 0 195.88 6.00 8 -8 0 118.69 3.60 -8 -8 0 123.69 3.50 8 -8 0 114.09 3.60 -8 8 0 118.19 3.60 8 8 0 115.59 3.60 9 -8 0 218.98 6.50 -9 -8 0 220.28 6.40 9 -8 0 219.08 6.50 9 8 0 211.08 6.50 -9 8 0 223.68 6.50 10 -8 0 28.00 1.20 -10 -8 0 25.50 1.10 -10 8 0 27.60 1.30 10 8 0 24.50 1.20 -11 -8 0 17.60 1.00 11 -8 0 19.50 1.10 -11 8 0 19.70 1.10 11 8 0 17.10 1.00 12 -8 0 0.10 0.40 -12 -8 0 -0.70 0.40 -12 8 0 -0.10 0.40 12 8 0 -0.30 0.40 0 -9 0 0.10 0.10 0 9 0 0.00 0.10 0 9 0 0.10 0.10 1 -9 0 214.68 6.20 -1 -9 0 223.98 6.20 1 -9 0 210.48 6.20 -1 9 0 221.78 6.30 1 9 0 228.88 6.20 1 9 0 210.88 6.20 -1 9 0 207.78 6.20 2 -9 0 24.90 0.80 -2 -9 0 26.20 0.80 2 -9 0 25.50 1.00 2 -9 0 26.20 0.90 -2 9 0 26.10 0.90 -2 9 0 28.00 0.90 2 9 0 27.60 0.80 2 9 0 25.30 0.90 3 -9 0 4.20 0.50 3 -9 0 4.00 0.30 3 -9 0 4.20 0.30 -3 -9 0 4.20 0.20 -3 9 0 4.40 0.30 3 9 0 4.20 0.30 3 9 0 5.10 0.30 -3 9 0 3.90 0.40 4 -9 0 4.00 0.50 -4 -9 0 4.30 0.30 4 -9 0 4.50 0.30 4 -9 0 4.40 0.40 -4 9 0 4.20 0.40 4 9 0 4.80 0.30 -4 9 0 3.90 0.40 4 9 0 4.30 0.30 5 -9 0 70.59 2.20 5 -9 0 70.99 2.10 -5 -9 0 70.59 2.10 5 -9 0 69.89 2.30 -5 9 0 72.29 2.20 5 9 0 71.09 2.10 -5 9 0 67.69 2.20 6 -9 0 72.59 2.40 6 -9 0 75.19 2.30 6 -9 0 76.09 2.30 -6 -9 0 74.59 2.30 -6 9 0 76.19 2.40 6 9 0 76.79 2.30 -6 9 0 74.49 2.40 7 -9 0 16.40 0.80 7 -9 0 17.20 0.80 -7 -9 0 17.80 0.70 -7 9 0 17.30 0.80 -7 9 0 17.20 0.90 7 9 0 17.10 0.80 8 -9 0 5.30 0.60 -8 -9 0 5.90 0.50 8 -9 0 5.60 0.60 -8 9 0 5.50 0.60 8 9 0 5.40 0.50 -9 -9 0 27.80 1.10 9 -9 0 28.00 1.20 9 -9 0 26.20 1.20 -9 9 0 28.70 1.20 9 9 0 25.80 1.10 10 -9 0 68.99 2.60 10 -9 0 72.39 2.30 -10 -9 0 67.79 2.30 10 9 0 66.79 2.30 -10 9 0 71.29 2.40 11 -9 0 31.70 1.40 -11 -9 0 30.00 1.30 -11 9 0 32.00 1.50 11 9 0 29.40 1.30 -12 -9 0 1.80 0.50 12 -9 0 1.10 0.50 12 9 0 1.70 0.50 -12 9 0 1.40 0.50 0 -10 0 6.40 0.30 0 10 0 7.50 0.40 0 10 0 5.80 0.40 0 10 0 6.80 0.30 -1 -10 0 29.20 0.90 1 -10 0 27.10 0.80 1 -10 0 28.70 0.90 1 10 0 28.80 0.90 1 10 0 30.00 0.90 -1 10 0 26.70 0.90 -1 10 0 28.50 1.00 -2 -10 0 19.40 0.60 2 -10 0 18.50 0.70 2 -10 0 18.60 0.60 2 -10 0 18.90 0.90 -2 10 0 19.10 0.70 2 10 0 19.80 0.70 2 10 0 18.80 0.70 -2 10 0 18.40 0.70 3 -10 0 186.28 5.30 3 -10 0 185.28 5.50 3 -10 0 181.58 5.30 -3 -10 0 180.98 5.30 -3 10 0 179.38 5.30 3 10 0 184.18 5.30 -3 10 0 181.58 5.40 4 -10 0 0.00 0.10 -4 -10 0 0.00 0.10 4 -10 0 0.00 0.30 4 -10 0 0.10 0.20 4 10 0 0.10 0.10 -4 10 0 0.00 0.20 -4 10 0 0.00 0.20 5 -10 0 47.30 1.70 -5 -10 0 48.70 1.50 5 -10 0 49.90 1.60 5 -10 0 48.60 1.50 -5 10 0 48.30 1.60 5 10 0 49.90 1.60 -5 10 0 49.90 1.70 -6 -10 0 86.49 2.50 6 -10 0 82.29 2.70 6 -10 0 83.89 2.60 6 -10 0 86.69 2.60 -6 10 0 83.29 2.60 -6 10 0 84.39 2.70 6 10 0 84.59 2.60 7 -10 0 55.29 1.80 -7 -10 0 58.19 1.80 7 -10 0 57.39 1.80 -7 10 0 55.19 1.90 -7 10 0 53.09 1.90 7 10 0 56.49 1.80 8 -10 0 51.99 1.70 -8 -10 0 51.09 1.60 8 -10 0 49.70 1.70 -8 10 0 49.30 1.80 8 10 0 49.50 1.70 9 -10 0 14.90 0.90 -9 -10 0 16.20 0.80 9 -10 0 15.10 0.90 -9 10 0 15.30 1.00 9 10 0 16.70 0.90 10 -10 0 20.40 1.10 10 -10 0 22.90 1.10 -10 -10 0 21.60 1.00 -10 10 0 22.60 1.20 10 10 0 21.40 1.10 11 -10 0 19.80 1.20 -11 -10 0 21.80 1.10 -11 10 0 20.90 1.30 11 10 0 19.60 1.20 -12 -10 0 9.40 1.00 12 -10 0 10.60 1.10 12 10 0 8.60 1.10 -12 10 0 9.90 1.20 0 -11 0 -0.10 0.10 0 11 0 0.00 0.20 0 11 0 -0.10 0.10 1 -11 0 12.60 0.50 -1 -11 0 12.80 0.50 1 11 0 13.80 0.50 1 11 0 12.70 0.60 -1 11 0 13.40 0.60 -1 11 0 11.60 0.50 2 -11 0 117.59 3.50 2 -11 0 116.69 3.70 -2 -11 0 119.39 3.40 2 -11 0 111.49 3.40 -2 11 0 119.99 3.50 -2 11 0 116.79 3.50 2 11 0 120.19 3.40 3 -11 0 2.40 0.20 3 -11 0 1.70 0.40 3 -11 0 3.00 0.40 -3 -11 0 2.70 0.30 -3 11 0 2.00 0.20 -3 11 0 3.70 0.40 4 -11 0 8.70 0.70 4 -11 0 8.70 0.40 -4 -11 0 8.60 0.40 4 -11 0 8.70 0.50 -4 11 0 8.70 0.60 -4 11 0 8.10 0.50 4 11 0 8.80 0.40 5 -11 0 18.90 0.80 5 -11 0 16.00 0.90 -5 -11 0 17.10 0.70 5 -11 0 17.00 0.70 -5 11 0 17.40 0.80 -5 11 0 18.30 0.80 5 11 0 16.50 0.70 6 -11 0 101.29 3.30 6 -11 0 105.49 3.10 -6 -11 0 101.29 3.10 6 -11 0 102.09 3.10 -6 11 0 103.09 3.20 -6 11 0 101.19 3.20 6 11 0 103.59 3.10 7 -11 0 0.00 0.30 -7 -11 0 -0.10 0.20 7 -11 0 0.20 0.20 -7 11 0 -0.10 0.30 7 11 0 -0.10 0.20 -7 11 0 0.30 0.30 -8 -11 0 20.90 0.90 8 -11 0 20.50 1.00 8 -11 0 19.20 0.90 -8 11 0 20.00 1.00 8 11 0 21.50 0.90 9 -11 0 0.90 0.40 9 -11 0 0.90 0.30 -9 -11 0 1.00 0.30 9 11 0 1.10 0.30 -9 11 0 0.80 0.40 10 -11 0 17.60 1.10 10 -11 0 19.90 1.00 -10 -11 0 20.00 1.00 10 11 0 19.60 1.10 -10 11 0 19.90 1.20 -11 -11 0 35.60 1.50 11 -11 0 35.30 1.50 11 11 0 35.90 1.60 -11 11 0 35.20 1.70 -12 -11 0 52.39 2.00 12 -11 0 58.59 2.10 -12 11 0 57.89 2.20 12 11 0 51.69 2.10 0 -12 0 105.69 3.20 0 12 0 108.89 3.20 -1 -12 0 1.10 0.20 1 -12 0 1.00 0.20 1 12 0 1.20 0.20 -1 12 0 1.20 0.20 -1 12 0 1.10 0.20 -2 -12 0 5.40 0.30 2 -12 0 3.70 0.60 2 -12 0 4.70 0.40 -2 12 0 4.60 0.40 2 12 0 5.00 0.40 -2 12 0 4.50 0.50 3 -12 0 0.50 0.20 -3 -12 0 0.80 0.20 3 -12 0 0.70 0.10 3 -12 0 0.80 0.30 -3 12 0 0.60 0.20 -3 12 0 0.30 0.20 3 12 0 0.60 0.20 4 -12 0 83.69 2.50 4 -12 0 81.49 2.70 4 -12 0 82.19 2.50 -4 -12 0 83.19 2.50 4 12 0 83.49 2.50 -4 12 0 79.69 2.50 -4 12 0 82.89 2.60 5 -12 0 203.98 5.80 5 -12 0 194.18 5.70 5 -12 0 192.68 5.90 -5 -12 0 193.68 5.70 5 12 0 202.68 5.70 -5 12 0 194.58 5.80 -5 12 0 190.18 5.80 6 -12 0 55.09 1.80 6 -12 0 53.29 2.00 -6 -12 0 55.49 1.70 6 -12 0 57.19 1.80 6 12 0 56.49 1.80 -6 12 0 54.79 1.90 -6 12 0 55.99 1.90 7 -12 0 12.30 0.70 7 -12 0 13.00 0.80 -7 -12 0 13.20 0.60 7 12 0 13.00 0.70 -7 12 0 12.30 0.80 -7 12 0 13.20 0.80 -8 -12 0 0.10 0.20 8 -12 0 0.10 0.30 8 -12 0 0.20 0.20 8 12 0 0.40 0.30 -8 12 0 0.10 0.30 -9 -12 0 19.30 0.90 9 -12 0 19.40 0.90 9 -12 0 18.30 1.00 9 12 0 19.30 1.00 -9 12 0 20.00 1.10 10 -12 0 8.40 0.90 -10 -12 0 11.10 0.80 10 -12 0 9.00 0.90 -10 12 0 8.60 1.00 10 12 0 11.50 0.90 -11 12 0 1.30 0.50 11 12 0 1.20 0.50 0 -13 0 0.00 0.20 0 13 0 0.20 0.20 1 -13 0 217.08 6.40 -1 -13 0 218.38 6.40 -1 13 0 221.68 6.50 1 13 0 226.18 6.40 -2 -13 0 20.90 0.70 2 -13 0 20.20 0.80 2 -13 0 22.00 1.20 -2 13 0 21.10 0.90 -2 13 0 19.00 0.90 2 13 0 20.40 0.80 -3 -13 0 91.89 2.70 3 -13 0 91.29 2.80 3 -13 0 92.99 3.00 3 13 0 90.89 2.70 -3 13 0 88.99 2.80 -3 13 0 88.09 2.80 4 -13 0 6.20 0.40 -4 -13 0 6.00 0.40 4 -13 0 6.10 0.50 4 -13 0 6.40 0.80 -4 13 0 6.30 0.50 4 13 0 6.50 0.40 -4 13 0 6.00 0.60 -5 -13 0 9.70 0.50 5 -13 0 9.70 0.90 5 -13 0 10.70 0.50 5 -13 0 11.50 0.70 -5 13 0 9.80 0.70 -5 13 0 10.40 0.70 5 13 0 9.80 0.60 6 -13 0 13.00 0.80 -6 -13 0 12.20 0.60 6 -13 0 11.10 0.90 6 -13 0 12.40 0.60 6 13 0 13.30 0.70 -6 13 0 11.80 0.80 -6 13 0 12.30 0.80 7 -13 0 37.00 1.30 7 -13 0 38.80 1.40 -7 -13 0 37.10 1.30 -7 13 0 37.40 1.50 -7 13 0 37.90 1.50 7 13 0 37.50 1.40 -8 -13 0 5.10 0.50 8 -13 0 5.30 0.70 8 -13 0 4.80 0.50 8 13 0 5.60 0.60 -8 13 0 4.00 0.50 9 -13 0 1.00 0.30 -9 -13 0 1.60 0.30 9 -13 0 1.00 0.40 -9 13 0 0.80 0.40 9 13 0 1.40 0.40 10 -13 0 2.40 0.40 10 -13 0 2.20 0.50 -10 13 0 2.00 0.50 -11 -13 0 32.50 1.40 11 -13 0 32.50 1.40 11 13 0 33.20 1.50 -11 13 0 31.80 1.70 0 -14 0 1.00 0.20 0 14 0 1.10 0.30 -1 -14 0 207.28 6.00 1 -14 0 210.48 6.40 1 -14 0 204.48 6.00 -1 14 0 208.28 6.10 1 14 0 207.28 6.10 2 -14 0 24.70 0.90 2 -14 0 25.10 1.30 -2 -14 0 24.30 0.90 -2 14 0 23.80 1.00 2 14 0 25.30 0.90 3 -14 0 26.30 1.30 -3 -14 0 26.10 0.90 3 -14 0 26.60 1.00 -3 14 0 27.30 1.10 -3 14 0 25.70 1.40 3 14 0 28.20 1.00 4 -14 0 48.30 1.90 -4 -14 0 46.80 1.50 4 -14 0 50.59 1.60 4 14 0 47.50 1.50 -4 14 0 45.20 1.60 -4 14 0 45.70 1.60 5 -14 0 1.20 0.30 5 -14 0 1.00 0.40 -5 -14 0 1.00 0.20 5 14 0 1.00 0.20 -5 14 0 1.10 0.30 -5 14 0 1.10 0.30 -6 -14 0 16.90 0.70 6 -14 0 14.70 1.10 6 -14 0 16.60 0.90 6 -14 0 15.90 0.70 -6 14 0 16.10 0.90 6 14 0 16.50 0.80 -6 14 0 15.80 0.90 -7 -14 0 14.90 0.70 7 -14 0 16.30 0.90 7 -14 0 15.50 0.70 -7 14 0 15.70 1.00 -7 14 0 17.20 1.00 7 14 0 15.80 0.80 8 -14 0 0.20 0.20 8 -14 0 -0.20 0.30 -8 -14 0 0.30 0.20 -8 14 0 0.30 0.40 8 14 0 0.60 0.30 9 -14 0 3.50 0.40 9 -14 0 3.90 0.50 -9 -14 0 3.80 0.40 -9 14 0 3.20 0.50 9 14 0 4.10 0.50 -10 -14 0 71.79 2.30 10 -14 0 69.09 2.50 10 -14 0 70.49 2.30 -10 14 0 72.99 2.60 10 14 0 63.69 2.40 -11 -14 0 62.49 2.20 11 14 0 58.49 2.30 -11 14 0 65.99 2.40 1 -15 0 18.90 1.30 -1 -15 0 22.00 0.80 1 -15 0 22.40 0.90 -1 15 0 22.50 1.00 1 15 0 23.40 0.90 2 -15 0 20.90 1.30 -2 -15 0 20.60 0.80 2 -15 0 20.50 0.90 -2 15 0 20.70 0.90 2 15 0 21.70 0.90 3 -15 0 100.69 3.00 3 -15 0 98.59 3.40 -3 -15 0 96.09 2.90 -3 15 0 96.69 3.10 3 15 0 100.29 3.00 4 -15 0 0.90 0.50 -4 -15 0 0.90 0.20 4 -15 0 0.80 0.30 -4 15 0 1.10 0.30 4 15 0 1.00 0.30 5 -15 0 2.80 0.30 -5 -15 0 2.70 0.30 5 -15 0 2.30 0.50 5 15 0 3.60 0.50 -5 15 0 4.10 0.60 -5 15 0 2.60 0.40 6 -15 0 2.30 0.50 -6 -15 0 2.60 0.30 6 -15 0 2.80 0.40 -6 15 0 2.20 0.40 6 15 0 2.50 0.30 -6 15 0 2.90 0.40 -7 -15 0 4.60 0.50 7 -15 0 3.70 0.40 7 15 0 4.50 0.60 -7 15 0 3.50 0.40 -7 15 0 3.80 0.50 -8 -15 0 0.40 0.30 8 -15 0 0.90 0.40 -8 15 0 0.90 0.40 8 15 0 0.80 0.30 9 -15 0 3.70 0.50 -9 -15 0 6.40 0.60 9 15 0 5.90 0.70 -9 15 0 4.60 0.60 10 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0 0.40 0.30 2 -18 0 1.20 0.30 2 -18 0 0.90 0.60 -2 -18 0 1.20 0.30 2 18 0 1.40 0.30 -2 18 0 1.40 0.40 3 -18 0 6.00 0.70 -3 -18 0 4.50 0.50 3 -18 0 4.50 0.70 3 18 0 5.80 0.60 -3 18 0 6.50 0.80 4 -18 0 30.80 1.20 4 -18 0 30.20 1.70 -4 -18 0 28.10 1.10 -4 18 0 29.50 1.30 4 18 0 28.10 1.20 5 -18 0 0.00 0.50 5 -18 0 0.20 0.30 -5 -18 0 0.00 0.20 -5 18 0 0.00 0.40 5 18 0 0.10 0.30 -6 -18 0 1.30 0.30 6 -18 0 1.10 0.40 6 -18 0 0.90 0.60 -6 18 0 1.00 0.40 6 18 0 1.40 0.30 7 -18 0 1.10 0.40 -7 -18 0 0.90 0.30 7 18 0 1.00 0.40 -7 18 0 0.90 0.50 -8 -18 0 8.10 0.70 8 -18 0 9.30 1.00 8 18 0 8.70 0.80 -8 18 0 9.90 1.00 0 -19 0 1.40 0.30 0 -19 0 1.40 0.70 0 19 0 1.60 0.40 1 -19 0 32.10 1.90 -1 -19 0 31.90 1.20 -1 -19 0 39.70 2.00 1 -19 0 31.50 1.30 -1 19 0 30.70 1.40 1 19 0 34.60 1.40 -2 -19 0 0.30 0.30 2 -19 0 0.40 0.30 2 -19 0 -0.20 0.60 2 19 0 0.10 0.30 -2 19 0 0.50 0.40 -3 -19 0 20.00 0.90 3 -19 0 22.00 1.60 3 -19 0 21.10 1.00 -3 19 0 20.90 1.10 3 19 0 20.50 1.00 4 -19 0 2.20 0.40 -4 -19 0 1.60 0.30 4 -19 0 1.70 0.60 -4 19 0 1.90 0.40 4 19 0 2.00 0.40 5 -19 0 6.90 1.20 -5 -19 0 7.00 0.60 5 -19 0 7.30 0.80 -5 19 0 7.60 0.90 5 19 0 7.70 0.70 -6 -19 0 -0.10 0.30 6 -19 0 -0.30 0.40 6 19 0 -0.40 0.30 -6 19 0 -0.30 0.40 -7 -19 0 5.90 0.60 7 -19 0 4.40 0.50 7 19 0 5.80 0.70 -7 19 0 4.70 0.70 8 -19 0 1.10 0.50 -8 -19 0 0.70 0.30 8 19 0 0.80 0.40 0 -20 0 23.30 1.10 0 -20 0 24.50 1.90 0 20 0 22.60 1.20 -1 -20 0 24.20 1.10 -1 -20 0 27.60 1.90 1 -20 0 23.10 1.80 1 -20 0 25.20 1.10 1 20 0 24.40 1.20 -1 20 0 26.50 1.20 2 -20 0 27.30 1.80 -2 -20 0 31.70 2.00 -2 -20 0 27.20 1.20 2 -20 0 28.50 1.20 -2 20 0 28.40 1.30 2 20 0 29.10 1.30 -3 -20 0 0.80 0.70 3 -20 0 -0.10 0.60 -3 -20 0 -0.20 0.30 3 -20 0 0.70 0.40 3 20 0 -0.20 0.30 -3 20 0 0.10 0.40 -4 -20 0 -0.40 0.30 4 -20 0 -0.40 0.30 4 -20 0 -0.50 0.60 4 20 0 -0.30 0.30 -4 20 0 0.00 0.40 5 -20 0 3.40 0.50 5 -20 0 3.70 0.80 -5 -20 0 3.40 0.40 -5 20 0 3.90 0.60 5 20 0 3.80 0.50 6 -20 0 0.60 0.40 -6 -20 0 0.40 0.30 6 20 0 0.90 0.40 -6 20 0 0.40 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14 90.39 2.70 1 5 -14 88.49 2.70 1 5 -14 85.49 2.70 0 -5 14 -0.10 0.30 0 -5 -14 0.10 0.20 0 -5 14 0.20 0.40 0 5 -14 0.00 0.30 0 5 14 0.40 0.30 0 5 -14 0.00 0.20 1 -5 14 19.70 1.10 -1 -5 -14 20.00 0.80 1 -5 14 19.40 1.00 1 5 14 20.60 0.90 -1 5 -14 20.90 1.00 -1 5 -14 20.10 0.90 -2 -5 -14 12.60 0.70 -2 -5 -14 9.30 1.70 2 -5 14 10.90 0.80 -2 5 -14 12.00 0.70 -2 5 -14 12.20 0.80 2 5 14 12.20 0.70 -3 -5 -14 57.79 3.10 -3 -5 -14 57.69 1.90 3 -5 14 58.19 2.10 -3 5 -14 58.09 1.90 -3 5 -14 58.19 2.00 3 5 14 59.59 2.00 -4 -5 -14 34.20 1.30 -4 -5 -14 31.50 2.30 4 -5 14 35.00 1.50 -4 5 -14 34.90 1.30 4 5 14 35.00 1.40 -4 5 -14 34.10 1.40 5 -5 14 0.50 0.40 5 -5 14 0.80 0.40 -5 -5 -14 1.40 0.30 5 5 14 1.20 0.40 -5 5 -14 1.00 0.40 -6 -5 -14 67.79 2.20 6 -5 14 60.59 2.40 6 5 14 66.89 2.30 -6 5 -14 64.59 2.30 -7 -5 -14 1.80 0.50 7 -5 14 2.30 0.60 7 5 14 2.40 0.50 -7 5 -14 1.40 0.50 -11 -6 14 0.10 0.50 11 -6 -14 0.60 0.40 -11 6 14 0.50 0.40 11 6 -14 -0.20 0.40 10 -6 -14 0.70 0.40 -10 -6 14 0.60 0.50 10 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32.50 1.50 5 -5 -20 0.80 0.40 -5 -5 20 1.40 0.50 5 5 -20 1.00 0.40 -5 5 20 0.80 0.40 -4 -5 20 17.00 1.30 4 -5 -20 17.80 1.00 -4 5 20 17.60 1.10 4 5 -20 17.00 1.10 -3 -5 20 -0.30 0.40 3 -5 -20 -0.10 0.30 3 5 -20 -0.70 0.40 -3 5 20 -0.10 0.40 -2 -5 20 0.20 0.40 2 -5 -20 0.20 0.30 2 5 -20 0.40 0.40 -2 5 20 0.30 0.40 1 -5 -20 6.20 0.70 -1 -5 20 5.30 0.60 1 -5 -20 6.00 1.40 -1 5 20 6.30 0.80 1 5 -20 5.00 0.60 -4 -6 20 3.20 0.60 4 -6 -20 2.70 0.40 -4 6 20 2.90 0.50 4 6 -20 3.00 0.50 -3 -6 20 -0.40 0.40 3 -6 -20 0.50 1.10 3 -6 -20 0.20 0.30 -3 6 20 0.00 0.40 3 6 -20 -0.30 0.40 2 -6 -20 1.40 1.10 2 -6 -20 0.60 0.30 -2 -6 20 0.50 0.50 -2 6 20 0.50 0.40 2 6 -20 1.00 0.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 8568 _olex2_submission_special_instructions 'No special instructions were received'