data_f2 # start Validation Reply Form _vrf_PLAT029_f2 ; PROBLEM: diffrn_measured_fraction_theta_full value Low RESPONSE: This is caused by the limited data collection strategy with the synchrotron facility. ; _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ;C40H34; _chemical_melting_point ? _chemical_formula_moiety ;C40H34; _chemical_formula_sum 'C40 H34' _chemical_formula_weight 514.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0037 0.0023 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1200(16) _cell_length_b 12.280(3) _cell_length_c 14.770(3) _cell_angle_alpha 106.55(3) _cell_angle_beta 96.00(3) _cell_angle_gamma 93.65(3) _cell_volume 1397.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21738 _cell_measurement_theta_min 1.687 _cell_measurement_theta_max 33.975 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_F_000 548 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.095 _shelx_estimated_absorpt_T_min 0.991 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.82656 _diffrn_radiation_type synchrotron _diffrn_source 'BESSY BL MX-14.2' _diffrn_measurement_device_type PILATUS _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21738 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.687 _diffrn_reflns_theta_max 33.975 _diffrn_reflns_theta_full 29.731 _diffrn_measured_fraction_theta_max 0.881 _diffrn_measured_fraction_theta_full 0.902 _diffrn_reflns_Laue_measured_fraction_max 0.881 _diffrn_reflns_Laue_measured_fraction_full 0.902 _diffrn_reflns_point_group_measured_fraction_max 0.881 _diffrn_reflns_point_group_measured_fraction_full 0.902 _reflns_number_total 6363 _reflns_number_gt 6129 _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 XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+0.5762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6363 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 C1 C 0.55945(15) 0.24203(9) 0.79318(7) 0.0159(2) Uani 1 1 d . . . . . H1 H 0.477877 0.182874 0.802492 0.019 Uiso 1 1 calc R U . . . C2 C 0.46867(14) 0.34733(9) 0.79943(7) 0.0158(2) Uani 1 1 d . . . . . C3 C 0.42922(14) 0.36315(8) 0.70945(7) 0.0134(2) Uani 1 1 d . . . . . C4 C 0.49955(14) 0.27268(8) 0.64019(7) 0.0128(2) Uani 1 1 d . . . . . C5 C 0.58415(14) 0.20491(8) 0.68932(7) 0.0143(2) Uani 1 1 d . . . . . C6 C 0.66761(14) 0.11482(9) 0.64335(8) 0.0165(2) Uani 1 1 d . . . . . H6 H 0.724310 0.070531 0.677534 0.020 Uiso 1 1 calc R U . . . C7 C 0.66593(14) 0.09099(8) 0.54504(7) 0.0155(2) Uani 1 1 d . . . . . H7 H 0.724236 0.030640 0.511591 0.019 Uiso 1 1 calc R U . . . C8 C 0.57946(14) 0.15503(8) 0.49585(7) 0.0141(2) Uani 1 1 d . . . . . H8 H 0.579089 0.136677 0.428846 0.017 Uiso 1 1 calc R U . . . C9 C 0.49249(13) 0.24604(8) 0.54168(7) 0.0119(2) Uani 1 1 d . . . . . C10 C 0.39450(13) 0.30226(8) 0.47767(7) 0.01188(19) Uani 1 1 d . . . . . H10 H 0.475964 0.318918 0.435905 0.014 Uiso 1 1 calc R U . . . C11 C 0.31778(13) 0.41611(8) 0.51464(7) 0.0122(2) Uani 1 1 d . . . . . C12 C 0.29223(13) 0.48167(8) 0.60852(7) 0.0124(2) Uani 1 1 d . . . . . C13 C 0.34073(14) 0.45625(8) 0.69873(7) 0.0132(2) Uani 1 1 d . . . . . C14 C 0.29851(15) 0.53050(9) 0.78541(7) 0.0166(2) Uani 1 1 d . . . . . C15 C 0.34002(16) 0.51119(10) 0.87467(8) 0.0199(2) Uani 1 1 d . . . . . H15 H 0.309501 0.562443 0.930399 0.024 Uiso 1 1 calc R U . . . C16 C 0.42373(16) 0.41961(10) 0.88224(7) 0.0195(2) Uani 1 1 d . . . . . H16 H 0.449965 0.406183 0.942105 0.023 Uiso 1 1 calc R U . . . C17 C 0.20972(16) 0.62763(9) 0.78537(8) 0.0197(2) Uani 1 1 d . . . . . H17 H 0.181062 0.674846 0.843480 0.024 Uiso 1 1 calc R U . . . C18 C 0.16670(15) 0.65238(9) 0.70362(8) 0.0188(2) Uani 1 1 d . . . . . H18 H 0.108174 0.717233 0.704773 0.023 Uiso 1 1 calc R U . . . C19 C 0.20758(14) 0.58264(8) 0.61474(7) 0.0146(2) Uani 1 1 d . . . . . C20 C 0.15853(15) 0.61809(9) 0.53454(8) 0.0171(2) Uani 1 1 d . . . . . H20 H 0.104482 0.685876 0.541766 0.021 Uiso 1 1 calc R U . . . C21 C 0.18799(15) 0.55574(9) 0.44598(8) 0.0173(2) Uani 1 1 d . . . . . H21 H 0.155932 0.579632 0.391471 0.021 Uiso 1 1 calc R U . . . C22 C 0.26625(14) 0.45628(8) 0.43788(7) 0.0155(2) Uani 1 1 d . . . . . H22 H 0.285794 0.413043 0.376199 0.019 Uiso 1 1 calc R U . . . C23 C 0.71284(15) 0.25186(9) 0.86483(7) 0.0157(2) Uani 1 1 d . . . . . C24 C 0.85022(16) 0.33106(10) 0.87291(8) 0.0211(2) Uani 1 1 d . . . . . C25 C 0.99079(17) 0.33523(11) 0.93761(8) 0.0234(2) Uani 1 1 d . . . . . H25 H 1.082052 0.390298 0.943638 0.028 Uiso 1 1 calc R U . . . C26 C 1.00109(16) 0.26129(10) 0.99337(8) 0.0213(2) Uani 1 1 d . . . . . C27 C 0.86462(16) 0.18333(10) 0.98450(8) 0.0203(2) Uani 1 1 d . . . . . H27 H 0.869413 0.132045 1.022011 0.024 Uiso 1 1 calc R U . . . C28 C 0.72063(15) 0.17778(9) 0.92231(7) 0.0175(2) Uani 1 1 d . . . . . C29 C 0.8546(2) 0.41019(13) 0.81151(11) 0.0373(4) Uani 1 1 d . . . . . H29A H 0.850428 0.365256 0.744671 0.056 Uiso 1 1 calc R U . . . H29B H 0.957543 0.461700 0.830976 0.056 Uiso 1 1 calc R U . . . H29C H 0.758665 0.455048 0.818954 0.056 Uiso 1 1 calc R U . . . C30 C 1.15607(19) 0.26438(13) 1.06062(9) 0.0318(3) Uani 1 1 d . . . . . H30A H 1.200328 0.189826 1.043263 0.048 Uiso 1 1 calc R U . . . H30B H 1.128616 0.282169 1.125979 0.048 Uiso 1 1 calc R U . . . H30C H 1.239791 0.323138 1.056233 0.048 Uiso 1 1 calc R U . . . C31 C 0.57751(18) 0.09095(11) 0.91833(10) 0.0280(3) Uani 1 1 d . . . . . H31A H 0.480078 0.130403 0.937815 0.042 Uiso 1 1 calc R U . . . H31B H 0.609023 0.045981 0.961460 0.042 Uiso 1 1 calc R U . . . H31C H 0.550591 0.040139 0.853150 0.042 Uiso 1 1 calc R U . . . C32 C 0.26224(13) 0.21282(8) 0.40858(7) 0.0125(2) Uani 1 1 d . . . . . C33 C 0.27381(14) 0.17646(8) 0.30985(7) 0.0147(2) Uani 1 1 d . . . . . C34 C 0.14949(15) 0.09806(9) 0.24842(7) 0.0173(2) Uani 1 1 d . . . . . H34 H 0.157694 0.074863 0.182084 0.021 Uiso 1 1 calc R U . . . C35 C 0.01398(15) 0.05286(9) 0.28130(8) 0.0181(2) Uani 1 1 d . . . . . C36 C 0.00683(14) 0.08720(8) 0.37893(8) 0.0163(2) Uani 1 1 d . . . . . H36 H -0.083443 0.056184 0.402851 0.020 Uiso 1 1 calc R U . . . C37 C 0.12748(14) 0.16560(8) 0.44309(7) 0.0134(2) Uani 1 1 d . . . . . C38 C 0.41843(16) 0.21710(9) 0.26664(7) 0.0192(2) Uani 1 1 d . . . . . H38A H 0.423712 0.300179 0.279762 0.029 Uiso 1 1 calc R U . . . H38B H 0.402647 0.180805 0.197642 0.029 Uiso 1 1 calc R U . . . H38C H 0.522402 0.196569 0.294606 0.029 Uiso 1 1 calc R U . . . C39 C -0.11891(19) -0.03187(12) 0.21404(9) 0.0306(3) Uani 1 1 d . . . . . H39A H -0.144144 -0.009022 0.156107 0.046 Uiso 1 1 calc R U . . . H39B H -0.219716 -0.033702 0.244939 0.046 Uiso 1 1 calc R U . . . H39C H -0.079146 -0.107888 0.197416 0.046 Uiso 1 1 calc R U . . . C40 C 0.10789(14) 0.19643(9) 0.54759(7) 0.0157(2) Uani 1 1 d . . . . . H40A H 0.192303 0.162701 0.580600 0.023 Uiso 1 1 calc R U . . . H40B H -0.003214 0.166963 0.555222 0.023 Uiso 1 1 calc R U . . . H40C H 0.121844 0.279643 0.574823 0.023 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 C1 0.0171(6) 0.0171(4) 0.0145(4) 0.0070(3) -0.0007(4) 0.0025(4) C2 0.0153(6) 0.0179(5) 0.0141(4) 0.0055(4) -0.0003(4) 0.0021(4) C3 0.0129(6) 0.0138(4) 0.0129(4) 0.0037(3) -0.0001(4) 0.0020(4) C4 0.0121(6) 0.0121(4) 0.0142(4) 0.0042(3) -0.0003(4) 0.0019(4) C5 0.0139(6) 0.0146(4) 0.0146(4) 0.0058(3) -0.0020(4) 0.0009(4) C6 0.0154(6) 0.0151(4) 0.0197(5) 0.0071(4) -0.0011(4) 0.0035(4) C7 0.0137(6) 0.0128(4) 0.0202(5) 0.0049(4) 0.0014(4) 0.0036(4) C8 0.0131(6) 0.0134(4) 0.0156(4) 0.0040(3) 0.0015(4) 0.0023(4) C9 0.0098(5) 0.0115(4) 0.0144(4) 0.0045(3) -0.0005(4) 0.0008(3) C10 0.0122(6) 0.0115(4) 0.0119(4) 0.0035(3) 0.0005(4) 0.0025(3) C11 0.0108(6) 0.0106(4) 0.0151(4) 0.0044(3) 0.0000(4) 0.0007(3) C12 0.0105(5) 0.0114(4) 0.0150(4) 0.0042(3) 0.0000(4) 0.0014(3) C13 0.0123(6) 0.0130(4) 0.0137(4) 0.0033(3) 0.0004(4) 0.0020(4) C14 0.0158(6) 0.0166(4) 0.0157(4) 0.0019(4) 0.0018(4) 0.0028(4) C15 0.0206(7) 0.0231(5) 0.0140(4) 0.0019(4) 0.0022(4) 0.0044(4) C16 0.0210(7) 0.0237(5) 0.0133(4) 0.0051(4) 0.0005(4) 0.0033(4) C17 0.0197(7) 0.0175(5) 0.0200(5) 0.0010(4) 0.0044(4) 0.0055(4) C18 0.0182(6) 0.0140(4) 0.0234(5) 0.0030(4) 0.0038(4) 0.0052(4) C19 0.0128(6) 0.0116(4) 0.0192(5) 0.0045(3) 0.0014(4) 0.0019(4) C20 0.0157(6) 0.0132(4) 0.0241(5) 0.0083(4) 0.0012(4) 0.0035(4) C21 0.0176(6) 0.0158(4) 0.0209(5) 0.0100(4) -0.0002(4) 0.0018(4) C22 0.0166(6) 0.0144(4) 0.0163(4) 0.0065(3) 0.0005(4) 0.0019(4) C23 0.0173(6) 0.0178(4) 0.0131(4) 0.0064(4) 0.0000(4) 0.0034(4) C24 0.0221(7) 0.0241(5) 0.0188(5) 0.0113(4) -0.0023(4) -0.0012(4) C25 0.0203(7) 0.0291(6) 0.0209(5) 0.0103(4) -0.0026(5) -0.0020(5) C26 0.0200(7) 0.0291(6) 0.0154(4) 0.0073(4) 0.0000(4) 0.0076(5) C27 0.0246(7) 0.0241(5) 0.0156(4) 0.0099(4) 0.0026(4) 0.0090(5) C28 0.0210(6) 0.0187(5) 0.0152(4) 0.0078(4) 0.0036(4) 0.0053(4) C29 0.0341(9) 0.0425(8) 0.0402(7) 0.0312(6) -0.0147(6) -0.0162(6) C30 0.0245(8) 0.0465(8) 0.0261(6) 0.0158(5) -0.0054(5) 0.0073(6) C31 0.0269(8) 0.0307(6) 0.0328(6) 0.0215(5) 0.0000(5) -0.0013(5) C32 0.0125(6) 0.0112(4) 0.0136(4) 0.0039(3) -0.0008(4) 0.0030(3) C33 0.0161(6) 0.0142(4) 0.0140(4) 0.0047(3) 0.0004(4) 0.0041(4) C34 0.0193(6) 0.0165(4) 0.0146(4) 0.0027(3) -0.0014(4) 0.0049(4) C35 0.0159(6) 0.0150(4) 0.0200(5) 0.0012(4) -0.0031(4) 0.0030(4) C36 0.0141(6) 0.0131(4) 0.0207(5) 0.0039(4) 0.0009(4) 0.0020(4) C37 0.0135(6) 0.0116(4) 0.0156(4) 0.0047(3) 0.0005(4) 0.0039(4) C38 0.0213(7) 0.0224(5) 0.0142(4) 0.0054(4) 0.0036(4) 0.0019(4) C39 0.0242(8) 0.0307(6) 0.0264(6) -0.0042(5) -0.0031(5) -0.0060(5) C40 0.0147(6) 0.0164(4) 0.0162(4) 0.0054(3) 0.0018(4) 0.0008(4) _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 C1 C5 1.5096(14) . ? C1 C2 1.5138(15) . ? C1 C23 1.5225(16) . ? C1 H1 1.0000 . ? C2 C16 1.3903(15) . ? C2 C3 1.4045(13) . ? C3 C13 1.4256(13) . ? C3 C4 1.4705(14) . ? C4 C9 1.3916(13) . ? C4 C5 1.4156(13) . ? C5 C6 1.3812(15) . ? C6 C7 1.3955(15) . ? C6 H6 0.9500 . ? C7 C8 1.3886(14) . ? C7 H7 0.9500 . ? C8 C9 1.4054(14) . ? C8 H8 0.9500 . ? C9 C10 1.5126(14) . ? C10 C32 1.5438(16) . ? C10 C11 1.5452(13) . ? C10 H10 1.0000 . ? C11 C22 1.3963(13) . ? C11 C12 1.4350(14) . ? C12 C19 1.4404(13) . ? C12 C13 1.4733(13) . ? C13 C14 1.4334(14) . ? C14 C15 1.4153(15) . ? C14 C17 1.4326(15) . ? C15 C16 1.3757(16) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.3442(16) . ? C17 H17 0.9500 . ? C18 C19 1.4330(15) . ? C18 H18 0.9500 . ? C19 C20 1.4032(14) . ? C20 C21 1.3684(16) . ? C20 H20 0.9500 . ? C21 C22 1.3933(14) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.4045(17) . ? C23 C28 1.4102(14) . ? C24 C25 1.3984(18) . ? C24 C29 1.5074(16) . ? C25 C26 1.3895(16) . ? C25 H25 0.9500 . ? C26 C27 1.3873(19) . ? C26 C30 1.5110(18) . ? C27 C28 1.3946(17) . ? C27 H27 0.9500 . ? C28 C31 1.5111(18) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.4134(15) . ? C32 C33 1.4134(13) . ? C33 C34 1.3986(17) . ? C33 C38 1.5161(16) . ? C34 C35 1.3937(17) . ? C34 H34 0.9500 . ? C35 C36 1.3909(15) . ? C35 C39 1.5092(18) . ? C36 C37 1.3967(17) . ? C36 H36 0.9500 . ? C37 C40 1.5090(14) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 C5 C1 C2 101.61(8) . . ? C5 C1 C23 116.52(9) . . ? C2 C1 C23 118.07(9) . . ? C5 C1 H1 106.6 . . ? C2 C1 H1 106.6 . . ? C23 C1 H1 106.6 . . ? C16 C2 C3 122.70(10) . . ? C16 C2 C1 125.60(9) . . ? C3 C2 C1 111.68(9) . . ? C2 C3 C13 121.01(9) . . ? C2 C3 C4 107.24(9) . . ? C13 C3 C4 131.72(9) . . ? C9 C4 C5 119.84(9) . . ? C9 C4 C3 131.36(9) . . ? C5 C4 C3 108.80(9) . . ? C6 C5 C4 122.23(9) . . ? C6 C5 C1 127.42(9) . . ? C4 C5 C1 110.26(9) . . ? C5 C6 C7 117.83(10) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C8 C7 C6 120.35(9) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 122.34(9) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C4 C9 C8 117.32(9) . . ? C4 C9 C10 126.51(9) . . ? C8 C9 C10 116.11(9) . . ? C9 C10 C32 109.16(8) . . ? C9 C10 C11 123.67(8) . . ? C32 C10 C11 109.59(8) . . ? C9 C10 H10 104.2 . . ? C32 C10 H10 104.2 . . ? C11 C10 H10 104.2 . . ? C22 C11 C12 118.59(9) . . ? C22 C11 C10 109.30(8) . . ? C12 C11 C10 132.12(9) . . ? C11 C12 C19 116.15(9) . . ? C11 C12 C13 127.24(9) . . ? C19 C12 C13 116.60(9) . . ? C3 C13 C14 115.11(9) . . ? C3 C13 C12 126.02(9) . . ? C14 C13 C12 118.87(9) . . ? C15 C14 C17 116.72(10) . . ? C15 C14 C13 122.09(10) . . ? C17 C14 C13 121.18(10) . . ? C16 C15 C14 121.25(10) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C2 117.83(10) . . ? C15 C16 H16 121.1 . . ? C2 C16 H16 121.1 . . ? C18 C17 C14 120.42(10) . . ? C18 C17 H17 119.8 . . ? C14 C17 H17 119.8 . . ? C17 C18 C19 121.15(10) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 115.93(9) . . ? C20 C19 C12 122.33(9) . . ? C18 C19 C12 121.74(10) . . ? C21 C20 C19 120.47(9) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 118.23(10) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C21 C22 C11 124.18(10) . . ? C21 C22 H22 117.9 . . ? C11 C22 H22 117.9 . . ? C24 C23 C28 118.87(11) . . ? C24 C23 C1 121.31(9) . . ? C28 C23 C1 119.79(10) . . ? C25 C24 C23 119.62(10) . . ? C25 C24 C29 118.13(12) . . ? C23 C24 C29 122.22(11) . . ? C26 C25 C24 122.02(12) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 C25 117.73(11) . . ? C27 C26 C30 120.92(11) . . ? C25 C26 C30 121.35(13) . . ? C26 C27 C28 122.15(10) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C23 119.59(11) . . ? C27 C28 C31 118.40(10) . . ? C23 C28 C31 122.02(11) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 118.81(10) . . ? C37 C32 C10 120.49(9) . . ? C33 C32 C10 120.70(9) . . ? C34 C33 C32 119.55(10) . . ? C34 C33 C38 117.67(9) . . ? C32 C33 C38 122.76(10) . . ? C35 C34 C33 122.17(10) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C36 C35 C34 117.53(11) . . ? C36 C35 C39 120.97(11) . . ? C34 C35 C39 121.49(11) . . ? C35 C36 C37 122.43(10) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C36 C37 C32 119.46(9) . . ? C36 C37 C40 118.00(10) . . ? C32 C37 C40 122.53(10) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 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 C5 C1 C2 C16 -176.03(11) . . . . ? C23 C1 C2 C16 -47.26(16) . . . . ? C5 C1 C2 C3 5.66(12) . . . . ? C23 C1 C2 C3 134.43(10) . . . . ? C16 C2 C3 C13 0.48(18) . . . . ? C1 C2 C3 C13 178.85(10) . . . . ? C16 C2 C3 C4 178.74(11) . . . . ? C1 C2 C3 C4 -2.89(13) . . . . ? C2 C3 C4 C9 177.49(11) . . . . ? C13 C3 C4 C9 -4.5(2) . . . . ? C2 C3 C4 C5 -1.42(12) . . . . ? C13 C3 C4 C5 176.58(11) . . . . ? C9 C4 C5 C6 2.91(17) . . . . ? C3 C4 C5 C6 -178.04(10) . . . . ? C9 C4 C5 C1 -173.88(10) . . . . ? C3 C4 C5 C1 5.17(13) . . . . ? C2 C1 C5 C6 176.96(11) . . . . ? C23 C1 C5 C6 47.21(16) . . . . ? C2 C1 C5 C4 -6.46(12) . . . . ? C23 C1 C5 C4 -136.21(10) . . . . ? C4 C5 C6 C7 -0.39(17) . . . . ? C1 C5 C6 C7 175.82(11) . . . . ? C5 C6 C7 C8 -1.38(17) . . . . ? C6 C7 C8 C9 0.69(17) . . . . ? C5 C4 C9 C8 -3.48(15) . . . . ? C3 C4 C9 C8 177.71(11) . . . . ? C5 C4 C9 C10 173.88(10) . . . . ? C3 C4 C9 C10 -4.93(19) . . . . ? C7 C8 C9 C4 1.78(16) . . . . ? C7 C8 C9 C10 -175.86(10) . . . . ? C4 C9 C10 C32 -116.99(11) . . . . ? C8 C9 C10 C32 60.40(12) . . . . ? C4 C9 C10 C11 14.15(16) . . . . ? C8 C9 C10 C11 -168.46(9) . . . . ? C9 C10 C11 C22 167.87(10) . . . . ? C32 C10 C11 C22 -61.16(11) . . . . ? C9 C10 C11 C12 -12.56(17) . . . . ? C32 C10 C11 C12 118.41(12) . . . . ? C22 C11 C12 C19 2.58(15) . . . . ? C10 C11 C12 C19 -176.95(10) . . . . ? C22 C11 C12 C13 -178.37(10) . . . . ? C10 C11 C12 C13 2.09(19) . . . . ? C2 C3 C13 C14 0.59(16) . . . . ? C4 C3 C13 C14 -177.19(11) . . . . ? C2 C3 C13 C12 -179.94(10) . . . . ? C4 C3 C13 C12 2.28(19) . . . . ? C11 C12 C13 C3 2.84(18) . . . . ? C19 C12 C13 C3 -178.11(10) . . . . ? C11 C12 C13 C14 -177.70(10) . . . . ? C19 C12 C13 C14 1.34(15) . . . . ? C3 C13 C14 C15 -0.88(17) . . . . ? C12 C13 C14 C15 179.61(10) . . . . ? C3 C13 C14 C17 179.93(10) . . . . ? C12 C13 C14 C17 0.42(17) . . . . ? C17 C14 C15 C16 179.34(11) . . . . ? C13 C14 C15 C16 0.12(19) . . . . ? C14 C15 C16 C2 0.96(19) . . . . ? C3 C2 C16 C15 -1.27(18) . . . . ? C1 C2 C16 C15 -179.40(11) . . . . ? C15 C14 C17 C18 179.52(12) . . . . ? C13 C14 C17 C18 -1.25(19) . . . . ? C14 C17 C18 C19 0.21(19) . . . . ? C17 C18 C19 C20 -179.00(11) . . . . ? C17 C18 C19 C12 1.68(18) . . . . ? C11 C12 C19 C20 -2.52(16) . . . . ? C13 C12 C19 C20 178.32(10) . . . . ? C11 C12 C19 C18 176.75(10) . . . . ? C13 C12 C19 C18 -2.40(16) . . . . ? C18 C19 C20 C21 -178.34(11) . . . . ? C12 C19 C20 C21 0.97(18) . . . . ? C19 C20 C21 C22 0.54(17) . . . . ? C20 C21 C22 C11 -0.39(18) . . . . ? C12 C11 C22 C21 -1.26(17) . . . . ? C10 C11 C22 C21 178.38(10) . . . . ? C5 C1 C23 C24 63.39(13) . . . . ? C2 C1 C23 C24 -58.01(14) . . . . ? C5 C1 C23 C28 -114.46(11) . . . . ? C2 C1 C23 C28 124.14(11) . . . . ? C28 C23 C24 C25 -0.26(16) . . . . ? C1 C23 C24 C25 -178.13(10) . . . . ? C28 C23 C24 C29 177.63(12) . . . . ? C1 C23 C24 C29 -0.23(18) . . . . ? C23 C24 C25 C26 1.47(18) . . . . ? C29 C24 C25 C26 -176.51(13) . . . . ? C24 C25 C26 C27 -1.30(18) . . . . ? C24 C25 C26 C30 177.99(12) . . . . ? C25 C26 C27 C28 -0.05(17) . . . . ? C30 C26 C27 C28 -179.34(11) . . . . ? C26 C27 C28 C23 1.21(16) . . . . ? C26 C27 C28 C31 -179.29(11) . . . . ? C24 C23 C28 C27 -1.03(15) . . . . ? C1 C23 C28 C27 176.87(9) . . . . ? C24 C23 C28 C31 179.49(11) . . . . ? C1 C23 C28 C31 -2.61(16) . . . . ? C9 C10 C32 C37 67.32(11) . . . . ? C11 C10 C32 C37 -70.98(11) . . . . ? C9 C10 C32 C33 -112.52(10) . . . . ? C11 C10 C32 C33 109.18(10) . . . . ? C37 C32 C33 C34 2.19(14) . . . . ? C10 C32 C33 C34 -177.96(9) . . . . ? C37 C32 C33 C38 -176.56(9) . . . . ? C10 C32 C33 C38 3.29(14) . . . . ? C32 C33 C34 C35 -0.76(15) . . . . ? C38 C33 C34 C35 178.05(9) . . . . ? C33 C34 C35 C36 -0.94(15) . . . . ? C33 C34 C35 C39 -179.87(11) . . . . ? C34 C35 C36 C37 1.22(15) . . . . ? C39 C35 C36 C37 -179.85(10) . . . . ? C35 C36 C37 C32 0.22(15) . . . . ? C35 C36 C37 C40 -179.73(9) . . . . ? C33 C32 C37 C36 -1.94(14) . . . . ? C10 C32 C37 C36 178.22(8) . . . . ? C33 C32 C37 C40 178.01(9) . . . . ? C10 C32 C37 C40 -1.83(14) . . . . ? _refine_diff_density_max 0.406 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.066