# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 777 loop_ _publ_author_name 'Wedl, Bernhard' 'Resel, Roland' 'Leising, Gunther' 'Kunert, Birgit' 'Salzmann, Ingo' 'Koch, Norbert' 'Vollmer, Antje' 'Duhm, Steffen' 'Werzer, Oliver' 'Gababode, Gabin' 'Geerts, Yves' _publ_contact_author_name 'Resel, Roland' _publ_contact_author_email roland.resel@aon.at _publ_section_title ; Crystallisation kinetics in thin films of metastable phases: The polymorphism of dihexyl-terthiophene ; # Attachment '- DH3T_alpha_phase.cif' data_matrix_0m _database_code_depnum_ccdc_archive 'CCDC 848505' #TrackingRef '- DH3T_alpha_phase.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 S3' _chemical_formula_weight 416.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.9436(7) _cell_length_b 5.6253(2) _cell_length_c 52.4024(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.817(2) _cell_angle_gamma 90.00 _cell_volume 6992.5(4) _cell_formula_units_Z 12 _cell_measurement_temperature 283(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8959 _exptl_absorpt_correction_T_max 0.9932 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 283(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41151 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 23.50 _reflns_number_total 10355 _reflns_number_gt 4899 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+4.5708P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10355 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.50218(6) 0.4923(3) 0.38015(3) 0.0802(5) Uani 1 1 d . . . S2 S 0.38029(6) 0.2522(2) 0.31553(3) 0.0656(4) Uani 1 1 d . . . S3 S 0.34448(5) 0.5922(2) 0.23986(3) 0.0628(4) Uani 1 1 d . . . S4 S 0.75339(6) 0.6028(2) 0.30781(3) 0.0742(5) Uani 1 1 d . . . S5 S 0.64000(6) 0.2598(2) 0.24616(3) 0.0708(5) Uani 1 1 d . . . S6 S 0.60331(6) 0.5188(2) 0.16699(3) 0.0811(5) Uani 1 1 d . . . S7 S 0.55180(6) 1.0956(2) 0.31980(3) 0.0719(5) Uani 1 1 d . . . S8 S 0.51493(5) 0.7486(2) 0.24462(3) 0.0670(4) Uani 1 1 d . . . S9 S 0.39477(6) 1.0032(2) 0.18015(3) 0.0767(5) Uani 1 1 d . . . C1 C 0.5941(3) 0.9317(15) 0.53143(14) 0.154(3) Uani 1 1 d . . . H1A H 0.6044 1.0757 0.5234 0.231 Uiso 1 1 calc R . . H1B H 0.6176 0.9115 0.5476 0.231 Uiso 1 1 calc R . . H1C H 0.5554 0.9405 0.5342 0.231 Uiso 1 1 calc R . . C2 C 0.6018(3) 0.7265(14) 0.51442(13) 0.118(2) Uani 1 1 d . . . H2A H 0.5935 0.5818 0.5232 0.142 Uiso 1 1 calc R . . H2B H 0.6411 0.7199 0.5118 0.142 Uiso 1 1 calc R . . C3 C 0.5664(3) 0.7302(12) 0.48858(13) 0.106(2) Uani 1 1 d . . . H3A H 0.5272 0.7413 0.4912 0.128 Uiso 1 1 calc R . . H3B H 0.5754 0.8731 0.4796 0.128 Uiso 1 1 calc R . . C4 C 0.5726(3) 0.5229(12) 0.47156(13) 0.100(2) Uani 1 1 d . . . H4A H 0.5647 0.3794 0.4807 0.120 Uiso 1 1 calc R . . H4B H 0.6115 0.5147 0.4684 0.120 Uiso 1 1 calc R . . C5 C 0.5355(2) 0.5242(10) 0.44592(12) 0.0895(19) Uani 1 1 d . . . H5A H 0.4964 0.5284 0.4489 0.107 Uiso 1 1 calc R . . H5B H 0.5428 0.6681 0.4367 0.107 Uiso 1 1 calc R . . C6 C 0.5439(3) 0.3148(11) 0.42939(12) 0.096(2) Uani 1 1 d . . . H6A H 0.5414 0.1722 0.4396 0.115 Uiso 1 1 calc R . . H6B H 0.5820 0.3221 0.4250 0.115 Uiso 1 1 calc R . . C7 C 0.5040(2) 0.2890(10) 0.40487(11) 0.0726(16) Uani 1 1 d . . . C8 C 0.4669(3) 0.1143(11) 0.39816(13) 0.0844(18) Uani 1 1 d . . . H8 H 0.4618 -0.0133 0.4089 0.101 Uiso 1 1 calc R . . C9 C 0.4363(3) 0.1414(10) 0.37337(13) 0.0805(18) Uani 1 1 d . . . H9 H 0.4094 0.0328 0.3662 0.097 Uiso 1 1 calc R . . C10 C 0.4498(2) 0.3395(9) 0.36105(12) 0.0630(15) Uani 1 1 d . . . C11 C 0.4280(2) 0.4227(8) 0.33544(11) 0.0576(14) Uani 1 1 d . . . C12 C 0.4404(2) 0.6236(9) 0.32261(12) 0.0663(16) Uani 1 1 d . . . H12 H 0.4654 0.7385 0.3301 0.080 Uiso 1 1 calc R . . C13 C 0.4126(2) 0.6432(8) 0.29752(12) 0.0632(15) Uani 1 1 d . . . H13 H 0.4171 0.7709 0.2867 0.076 Uiso 1 1 calc R . . C14 C 0.37750(19) 0.4510(7) 0.29042(11) 0.0522(14) Uani 1 1 d . . . C15 C 0.34509(19) 0.4024(8) 0.26583(11) 0.0528(13) Uani 1 1 d . . . C16 C 0.31366(18) 0.2039(8) 0.25838(11) 0.0520(14) Uani 1 1 d . . . H16 H 0.3093 0.0781 0.2695 0.062 Uiso 1 1 calc R . . C17 C 0.28909(19) 0.2079(8) 0.23292(12) 0.0591(15) Uani 1 1 d . . . H17 H 0.2661 0.0865 0.2255 0.071 Uiso 1 1 calc R . . C18 C 0.30165(18) 0.4062(8) 0.21967(11) 0.0553(14) Uani 1 1 d . . . C19 C 0.2839(2) 0.4721(9) 0.19207(12) 0.0721(17) Uani 1 1 d . . . H19A H 0.3174 0.4946 0.1839 0.087 Uiso 1 1 calc R . . H19B H 0.2643 0.6235 0.1916 0.087 Uiso 1 1 calc R . . C20 C 0.2464(2) 0.2958(9) 0.17651(11) 0.0684(16) Uani 1 1 d . . . H20A H 0.2645 0.1412 0.1781 0.082 Uiso 1 1 calc R . . H20B H 0.2114 0.2834 0.1838 0.082 Uiso 1 1 calc R . . C21 C 0.2330(2) 0.3555(10) 0.14845(11) 0.0745(16) Uani 1 1 d . . . H21A H 0.2682 0.3714 0.1414 0.089 Uiso 1 1 calc R . . H21B H 0.2144 0.5091 0.1469 0.089 Uiso 1 1 calc R . . C22 C 0.1964(2) 0.1798(9) 0.13223(11) 0.0727(16) Uani 1 1 d . . . H22A H 0.2136 0.0239 0.1347 0.087 Uiso 1 1 calc R . . H22B H 0.1601 0.1726 0.1385 0.087 Uiso 1 1 calc R . . C23 C 0.1866(3) 0.2320(11) 0.10399(13) 0.098(2) Uani 1 1 d . . . H23A H 0.2229 0.2398 0.0977 0.117 Uiso 1 1 calc R . . H23B H 0.1694 0.3879 0.1015 0.117 Uiso 1 1 calc R . . C24 C 0.1499(3) 0.0555(12) 0.08757(13) 0.121(2) Uani 1 1 d . . . H24A H 0.1650 -0.1016 0.0906 0.182 Uiso 1 1 calc R . . H24B H 0.1491 0.0954 0.0697 0.182 Uiso 1 1 calc R . . H24C H 0.1123 0.0608 0.0920 0.182 Uiso 1 1 calc R . . C25 C 0.9008(4) 0.0622(16) 0.46780(15) 0.169(4) Uani 1 1 d . . . H25A H 0.8670 0.0722 0.4758 0.253 Uiso 1 1 calc R . . H25B H 0.9328 0.0992 0.4803 0.253 Uiso 1 1 calc R . . H25C H 0.9046 -0.0959 0.4614 0.253 Uiso 1 1 calc R . . C26 C 0.8974(3) 0.2367(14) 0.44583(16) 0.129(3) Uani 1 1 d . . . H26A H 0.8932 0.3952 0.4526 0.155 Uiso 1 1 calc R . . H26B H 0.9328 0.2327 0.4388 0.155 Uiso 1 1 calc R . . C27 C 0.8505(3) 0.1944(13) 0.42438(14) 0.108(2) Uani 1 1 d . . . H27A H 0.8150 0.1996 0.4314 0.130 Uiso 1 1 calc R . . H27B H 0.8546 0.0357 0.4176 0.130 Uiso 1 1 calc R . . C28 C 0.8479(3) 0.3679(12) 0.40263(13) 0.095(2) Uani 1 1 d . . . H28A H 0.8844 0.3725 0.3966 0.115 Uiso 1 1 calc R . . H28B H 0.8406 0.5248 0.4091 0.115 Uiso 1 1 calc R . . C29 C 0.8039(2) 0.3149(10) 0.38012(12) 0.0836(19) Uani 1 1 d . . . H29A H 0.8111 0.1573 0.3738 0.100 Uiso 1 1 calc R . . H29B H 0.7674 0.3105 0.3862 0.100 Uiso 1 1 calc R . . C30 C 0.8005(2) 0.4854(10) 0.35802(12) 0.0812(18) Uani 1 1 d . . . H30A H 0.8379 0.5009 0.3530 0.097 Uiso 1 1 calc R . . H30B H 0.7900 0.6399 0.3641 0.097 Uiso 1 1 calc R . . C31 C 0.7604(2) 0.4232(9) 0.33448(11) 0.0616(15) Uani 1 1 d . . . C32 C 0.7280(2) 0.2236(9) 0.33000(14) 0.0777(18) Uani 1 1 d . . . H32 H 0.7263 0.1041 0.3421 0.093 Uiso 1 1 calc R . . C33 C 0.6973(2) 0.2176(8) 0.30499(12) 0.0632(16) Uani 1 1 d . . . H33 H 0.6733 0.0938 0.2990 0.076 Uiso 1 1 calc R . . C34 C 0.70649(19) 0.4113(8) 0.29058(12) 0.0612(15) Uani 1 1 d . . . C35 C 0.6840(2) 0.4580(8) 0.26409(13) 0.0605(15) Uani 1 1 d . . . C36 C 0.6945(2) 0.6495(9) 0.24949(14) 0.0745(18) Uani 1 1 d . . . H36 H 0.7170 0.7770 0.2558 0.089 Uiso 1 1 calc R . . C37 C 0.6675(2) 0.6340(9) 0.22364(13) 0.0702(17) Uani 1 1 d . . . H37 H 0.6708 0.7501 0.2113 0.084 Uiso 1 1 calc R . . C38 C 0.6361(2) 0.4305(8) 0.21863(12) 0.0615(15) Uani 1 1 d . . . C39 C 0.6041(2) 0.3539(8) 0.19481(12) 0.0602(15) Uani 1 1 d . . . C40 C 0.5713(2) 0.1570(9) 0.18996(13) 0.0703(17) Uani 1 1 d . . . H40 H 0.5666 0.0441 0.2025 0.084 Uiso 1 1 calc R . . C41 C 0.5451(2) 0.1398(10) 0.16430(13) 0.0738(17) Uani 1 1 d . . . H41 H 0.5210 0.0162 0.1583 0.089 Uiso 1 1 calc R . . C42 C 0.5586(2) 0.3223(9) 0.14913(13) 0.0690(16) Uani 1 1 d . . . C43 C 0.5405(3) 0.3704(11) 0.12149(13) 0.0912(19) Uani 1 1 d . . . H43A H 0.5739 0.3806 0.1129 0.109 Uiso 1 1 calc R . . H43B H 0.5221 0.5242 0.1199 0.109 Uiso 1 1 calc R . . C44 C 0.5008(2) 0.1863(11) 0.10757(13) 0.0859(18) Uani 1 1 d . . . H44A H 0.5178 0.0302 0.1104 0.103 Uiso 1 1 calc R . . H44B H 0.4660 0.1862 0.1151 0.103 Uiso 1 1 calc R . . C45 C 0.4873(3) 0.2287(12) 0.07904(14) 0.103(2) Uani 1 1 d . . . H45A H 0.4689 0.3819 0.0764 0.123 Uiso 1 1 calc R . . H45B H 0.5225 0.2379 0.0718 0.123 Uiso 1 1 calc R . . C46 C 0.4509(3) 0.0460(13) 0.06445(15) 0.114(2) Uani 1 1 d . . . H46A H 0.4142 0.0483 0.0704 0.137 Uiso 1 1 calc R . . H46B H 0.4673 -0.1095 0.0684 0.137 Uiso 1 1 calc R . . C47 C 0.4427(4) 0.0786(15) 0.03558(17) 0.150(3) Uani 1 1 d . . . H47A H 0.4235 0.2286 0.0315 0.180 Uiso 1 1 calc R . . H47B H 0.4795 0.0894 0.0299 0.180 Uiso 1 1 calc R . . C48 C 0.4112(4) -0.1067(18) 0.02119(17) 0.205(5) Uani 1 1 d . . . H48A H 0.4279 -0.2580 0.0260 0.307 Uiso 1 1 calc R . . H48B H 0.4116 -0.0812 0.0031 0.307 Uiso 1 1 calc R . . H48C H 0.3730 -0.1047 0.0248 0.307 Uiso 1 1 calc R . . C49 C 0.7584(4) 0.6152(18) 0.47038(16) 0.189(4) Uani 1 1 d . . . H49A H 0.7410 0.4617 0.4680 0.284 Uiso 1 1 calc R . . H49B H 0.7616 0.6587 0.4882 0.284 Uiso 1 1 calc R . . H49C H 0.7952 0.6097 0.4651 0.284 Uiso 1 1 calc R . . C50 C 0.7233(3) 0.7937(15) 0.45465(15) 0.129(3) Uani 1 1 d . . . H50A H 0.7437 0.9431 0.4553 0.155 Uiso 1 1 calc R . . H50B H 0.6890 0.8200 0.4622 0.155 Uiso 1 1 calc R . . C51 C 0.7081(3) 0.7211(13) 0.42707(14) 0.110(2) Uani 1 1 d . . . H51A H 0.7426 0.7014 0.4195 0.132 Uiso 1 1 calc R . . H51B H 0.6896 0.5674 0.4266 0.132 Uiso 1 1 calc R . . C52 C 0.6707(3) 0.8896(12) 0.41074(13) 0.099(2) Uani 1 1 d . . . H52A H 0.6899 1.0414 0.4106 0.118 Uiso 1 1 calc R . . H52B H 0.6369 0.9145 0.4188 0.118 Uiso 1 1 calc R . . C53 C 0.6530(2) 0.8138(10) 0.38305(12) 0.0814(18) Uani 1 1 d . . . H53A H 0.6865 0.7942 0.3747 0.098 Uiso 1 1 calc R . . H53B H 0.6345 0.6604 0.3830 0.098 Uiso 1 1 calc R . . C54 C 0.6138(2) 0.9865(10) 0.36750(12) 0.0833(18) Uani 1 1 d . . . H54A H 0.5803 1.0055 0.3758 0.100 Uiso 1 1 calc R . . H54B H 0.6323 1.1401 0.3677 0.100 Uiso 1 1 calc R . . C55 C 0.59603(19) 0.9147(9) 0.33992(12) 0.0638(15) Uani 1 1 d . . . C56 C 0.6091(2) 0.7173(9) 0.32691(13) 0.0683(16) Uani 1 1 d . . . H56 H 0.6326 0.5978 0.3345 0.082 Uiso 1 1 calc R . . C57 C 0.5843(2) 0.7097(8) 0.30136(12) 0.0573(14) Uani 1 1 d . . . H57 H 0.5894 0.5847 0.2903 0.069 Uiso 1 1 calc R . . C58 C 0.5518(2) 0.9033(8) 0.29414(11) 0.0593(15) Uani 1 1 d . . . C59 C 0.5182(2) 0.9505(8) 0.26970(12) 0.0584(15) Uani 1 1 d . . . C60 C 0.4833(2) 1.1409(8) 0.26241(12) 0.0645(16) Uani 1 1 d . . . H60 H 0.4791 1.2694 0.2732 0.077 Uiso 1 1 calc R . . C61 C 0.4553(2) 1.1227(8) 0.23772(12) 0.0622(15) Uani 1 1 d . . . H61 H 0.4305 1.2384 0.2303 0.075 Uiso 1 1 calc R . . C62 C 0.46701(19) 0.9202(8) 0.22524(12) 0.0598(15) Uani 1 1 d . . . C63 C 0.44515(19) 0.8427(8) 0.19965(12) 0.0591(15) Uani 1 1 d . . . C64 C 0.4588(2) 0.6443(9) 0.18626(13) 0.0677(16) Uani 1 1 d . . . H64 H 0.4854 0.5335 0.1932 0.081 Uiso 1 1 calc R . . C65 C 0.4292(2) 0.6234(9) 0.16146(13) 0.0725(17) Uani 1 1 d . . . H65 H 0.4338 0.4977 0.1504 0.087 Uiso 1 1 calc R . . C66 C 0.3929(2) 0.8080(9) 0.15524(11) 0.0676(16) Uani 1 1 d . . . C67 C 0.3534(2) 0.8441(10) 0.13104(13) 0.0848(18) Uani 1 1 d . . . H67A H 0.3613 0.9984 0.1241 0.102 Uiso 1 1 calc R . . H67B H 0.3154 0.8495 0.1354 0.102 Uiso 1 1 calc R . . C68 C 0.3549(2) 0.6622(11) 0.11015(12) 0.0847(18) Uani 1 1 d . . . H68A H 0.3918 0.6670 0.1044 0.102 Uiso 1 1 calc R . . H68B H 0.3503 0.5057 0.1173 0.102 Uiso 1 1 calc R . . C69 C 0.3109(3) 0.6950(12) 0.08724(14) 0.098(2) Uani 1 1 d . . . H69A H 0.2743 0.6985 0.0931 0.117 Uiso 1 1 calc R . . H69B H 0.3167 0.8485 0.0796 0.117 Uiso 1 1 calc R . . C70 C 0.3101(3) 0.5091(13) 0.06688(14) 0.107(2) Uani 1 1 d . . . H70A H 0.3067 0.3547 0.0748 0.129 Uiso 1 1 calc R . . H70B H 0.3460 0.5125 0.0602 0.129 Uiso 1 1 calc R . . C71 C 0.2637(4) 0.5330(15) 0.04461(16) 0.137(3) Uani 1 1 d . . . H71A H 0.2686 0.6825 0.0360 0.165 Uiso 1 1 calc R . . H71B H 0.2280 0.5404 0.0513 0.165 Uiso 1 1 calc R . . C72 C 0.2608(4) 0.3356(18) 0.02501(16) 0.182(4) Uani 1 1 d . . . H72A H 0.2966 0.3208 0.0188 0.273 Uiso 1 1 calc R . . H72B H 0.2321 0.3714 0.0109 0.273 Uiso 1 1 calc R . . H72C H 0.2518 0.1888 0.0329 0.273 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0799(10) 0.0568(9) 0.1053(13) -0.0118(9) 0.0182(9) -0.0110(8) S2 0.0729(9) 0.0369(7) 0.0918(12) -0.0055(7) 0.0287(8) -0.0142(7) S3 0.0609(8) 0.0308(7) 0.1030(12) 0.0033(7) 0.0333(8) -0.0044(6) S4 0.0688(9) 0.0386(8) 0.1225(14) -0.0057(8) 0.0398(9) -0.0081(7) S5 0.0697(9) 0.0359(7) 0.1136(13) 0.0075(8) 0.0368(9) -0.0052(7) S6 0.0859(10) 0.0469(8) 0.1181(14) 0.0175(9) 0.0418(10) -0.0059(8) S7 0.0678(9) 0.0362(7) 0.1180(13) -0.0071(8) 0.0360(9) 0.0032(7) S8 0.0653(9) 0.0354(7) 0.1063(13) 0.0059(8) 0.0334(8) 0.0109(7) S9 0.0651(9) 0.0454(8) 0.1226(14) 0.0081(9) 0.0236(9) 0.0145(7) C1 0.178(8) 0.164(8) 0.112(7) -0.023(6) -0.005(6) 0.030(7) C2 0.122(6) 0.132(7) 0.092(6) -0.004(5) -0.016(5) 0.006(5) C3 0.109(5) 0.107(6) 0.098(6) -0.005(5) -0.002(4) 0.010(4) C4 0.108(5) 0.097(5) 0.092(5) -0.007(4) -0.002(4) 0.009(4) C5 0.095(4) 0.079(4) 0.093(5) -0.013(4) 0.006(4) 0.008(4) C6 0.099(5) 0.078(4) 0.107(6) -0.006(4) 0.001(4) 0.013(4) C7 0.083(4) 0.056(4) 0.081(5) -0.014(3) 0.017(4) 0.015(3) C8 0.111(5) 0.059(4) 0.088(5) -0.005(4) 0.032(4) -0.004(4) C9 0.096(5) 0.055(4) 0.095(5) -0.009(4) 0.029(4) -0.020(3) C10 0.067(3) 0.046(3) 0.082(5) -0.018(3) 0.028(3) -0.009(3) C11 0.061(3) 0.039(3) 0.080(4) -0.021(3) 0.035(3) -0.009(3) C12 0.071(4) 0.038(3) 0.097(5) -0.022(3) 0.039(4) -0.020(3) C13 0.069(4) 0.033(3) 0.094(5) -0.007(3) 0.035(3) -0.007(3) C14 0.050(3) 0.027(3) 0.086(4) -0.005(3) 0.034(3) -0.001(2) C15 0.044(3) 0.033(3) 0.088(4) 0.000(3) 0.033(3) 0.003(2) C16 0.051(3) 0.030(3) 0.079(4) -0.001(3) 0.026(3) -0.004(2) C17 0.051(3) 0.032(3) 0.098(5) -0.002(3) 0.025(3) -0.003(2) C18 0.049(3) 0.035(3) 0.086(4) 0.005(3) 0.024(3) 0.002(2) C19 0.062(3) 0.046(3) 0.114(5) 0.004(3) 0.031(3) 0.000(3) C20 0.061(3) 0.051(3) 0.099(5) 0.011(3) 0.029(3) 0.001(3) C21 0.076(4) 0.062(4) 0.090(5) 0.011(4) 0.027(4) -0.003(3) C22 0.066(4) 0.059(4) 0.095(5) 0.013(3) 0.017(3) 0.002(3) C23 0.105(5) 0.091(5) 0.100(6) 0.009(4) 0.025(4) -0.013(4) C24 0.137(6) 0.120(6) 0.106(6) -0.002(5) 0.014(5) -0.023(5) C25 0.226(10) 0.161(9) 0.119(7) 0.008(7) 0.024(7) 0.013(8) C26 0.142(7) 0.119(7) 0.125(7) -0.013(6) 0.017(6) -0.008(6) C27 0.122(6) 0.113(6) 0.095(6) -0.012(5) 0.031(5) -0.018(5) C28 0.093(5) 0.094(5) 0.104(6) -0.024(5) 0.028(4) -0.010(4) C29 0.082(4) 0.070(4) 0.107(6) -0.022(4) 0.041(4) -0.010(3) C30 0.074(4) 0.060(4) 0.114(6) -0.012(4) 0.031(4) 0.000(3) C31 0.053(3) 0.049(3) 0.089(5) -0.009(3) 0.032(3) 0.002(3) C32 0.066(4) 0.043(3) 0.132(6) 0.005(4) 0.042(4) -0.007(3) C33 0.052(3) 0.033(3) 0.110(5) -0.005(3) 0.030(3) -0.004(2) C34 0.049(3) 0.032(3) 0.111(5) -0.002(3) 0.039(3) 0.004(2) C35 0.054(3) 0.028(3) 0.109(5) 0.002(3) 0.044(3) 0.006(2) C36 0.063(4) 0.032(3) 0.136(6) -0.006(4) 0.044(4) -0.007(3) C37 0.061(4) 0.039(3) 0.119(6) 0.010(3) 0.042(4) 0.000(3) C38 0.052(3) 0.036(3) 0.106(5) 0.015(3) 0.043(3) 0.008(3) C39 0.044(3) 0.034(3) 0.109(5) 0.009(3) 0.033(3) 0.004(2) C40 0.055(3) 0.043(3) 0.120(6) 0.025(3) 0.035(4) 0.002(3) C41 0.058(4) 0.054(4) 0.115(6) 0.020(4) 0.033(4) 0.004(3) C42 0.059(3) 0.051(3) 0.102(5) 0.013(3) 0.029(3) 0.005(3) C43 0.099(5) 0.071(4) 0.111(6) 0.023(4) 0.042(4) 0.011(4) C44 0.084(4) 0.073(4) 0.106(6) 0.007(4) 0.032(4) 0.006(4) C45 0.118(5) 0.093(5) 0.103(6) 0.014(5) 0.035(5) 0.000(4) C46 0.128(6) 0.110(6) 0.105(6) 0.007(5) 0.016(5) 0.000(5) C47 0.177(8) 0.140(8) 0.126(8) 0.014(7) -0.004(6) -0.024(7) C48 0.274(13) 0.187(10) 0.139(9) -0.010(8) -0.024(8) -0.061(10) C49 0.223(10) 0.208(11) 0.127(8) -0.007(8) -0.011(7) 0.055(9) C50 0.151(7) 0.143(7) 0.096(7) -0.017(6) 0.030(5) 0.000(6) C51 0.124(6) 0.105(6) 0.100(6) -0.009(5) 0.012(5) 0.009(5) C52 0.105(5) 0.097(5) 0.100(6) -0.013(5) 0.035(4) -0.004(4) C53 0.077(4) 0.070(4) 0.102(5) -0.012(4) 0.028(4) -0.001(3) C54 0.079(4) 0.067(4) 0.109(6) -0.014(4) 0.031(4) -0.004(3) C55 0.055(3) 0.049(3) 0.094(5) -0.004(3) 0.034(3) -0.003(3) C56 0.062(3) 0.041(3) 0.108(5) 0.003(3) 0.035(4) 0.008(3) C57 0.058(3) 0.030(3) 0.091(5) -0.002(3) 0.034(3) 0.007(2) C58 0.053(3) 0.037(3) 0.096(5) 0.000(3) 0.039(3) -0.007(3) C59 0.051(3) 0.029(3) 0.104(5) 0.002(3) 0.042(3) 0.000(2) C60 0.062(3) 0.033(3) 0.106(5) 0.006(3) 0.040(4) 0.006(3) C61 0.059(3) 0.036(3) 0.099(5) 0.010(3) 0.036(3) 0.015(3) C62 0.051(3) 0.038(3) 0.096(5) 0.010(3) 0.032(3) 0.002(3) C63 0.047(3) 0.032(3) 0.107(5) 0.013(3) 0.041(3) 0.011(2) C64 0.059(3) 0.049(3) 0.101(5) 0.016(3) 0.030(4) 0.016(3) C65 0.067(4) 0.049(3) 0.108(5) 0.008(4) 0.034(4) 0.016(3) C66 0.061(3) 0.061(4) 0.084(5) 0.019(3) 0.023(3) -0.003(3) C67 0.080(4) 0.061(4) 0.118(6) 0.003(4) 0.031(4) 0.001(3) C68 0.072(4) 0.078(4) 0.107(5) 0.017(4) 0.024(4) 0.007(3) C69 0.086(5) 0.083(5) 0.127(6) 0.012(5) 0.025(5) 0.000(4) C70 0.105(5) 0.108(6) 0.110(6) 0.019(5) 0.017(5) 0.007(4) C71 0.157(7) 0.133(7) 0.118(7) 0.003(6) 0.005(6) 0.008(6) C72 0.224(10) 0.182(10) 0.129(8) -0.016(7) -0.015(7) 0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C10 1.724(5) . ? S1 C7 1.724(6) . ? S2 C14 1.722(5) . ? S2 C11 1.729(5) . ? S3 C18 1.724(5) . ? S3 C15 1.728(5) . ? S4 C31 1.714(5) . ? S4 C34 1.721(5) . ? S5 C35 1.722(5) . ? S5 C38 1.725(5) . ? S6 C42 1.724(6) . ? S6 C39 1.726(5) . ? S7 C55 1.722(5) . ? S7 C58 1.726(5) . ? S8 C62 1.721(5) . ? S8 C59 1.731(5) . ? S9 C66 1.702(6) . ? S9 C63 1.726(5) . ? C1 C2 1.485(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.497(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.488(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.507(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.492(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.500(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.340(7) . ? C8 C9 1.410(7) . ? C8 H8 0.9300 . ? C9 C10 1.349(7) . ? C9 H9 0.9300 . ? C10 C11 1.450(7) . ? C11 C12 1.368(7) . ? C12 C13 1.394(7) . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 H13 0.9300 . ? C14 C15 1.437(6) . ? C15 C16 1.373(6) . ? C16 C17 1.383(6) . ? C16 H16 0.9300 . ? C17 C18 1.369(6) . ? C17 H17 0.9300 . ? C18 C19 1.498(7) . ? C19 C20 1.501(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.500(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.505(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.496(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.514(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.507(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.495(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.495(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.500(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.497(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.498(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.367(7) . ? C32 C33 1.413(7) . ? C32 H32 0.9300 . ? C33 C34 1.360(7) . ? C33 H33 0.9300 . ? C34 C35 1.443(7) . ? C35 C36 1.365(7) . ? C36 C37 1.422(7) . ? C36 H36 0.9300 . ? C37 C38 1.375(7) . ? C37 H37 0.9300 . ? C38 C39 1.439(7) . ? C39 C40 1.362(6) . ? C40 C41 1.408(7) . ? C40 H40 0.9300 . ? C41 C42 1.364(7) . ? C41 H41 0.9300 . ? C42 C43 1.478(7) . ? C43 C44 1.523(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.505(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.491(8) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.510(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.438(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.485(9) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.499(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.492(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.516(7) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.509(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.506(7) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.361(6) . ? C56 C57 1.389(7) . ? C56 H56 0.9300 . ? C57 C58 1.362(6) . ? C57 H57 0.9300 . ? C58 C59 1.441(7) . ? C59 C60 1.380(6) . ? C60 C61 1.378(7) . ? C60 H60 0.9300 . ? C61 C62 1.362(7) . ? C61 H61 0.9300 . ? C62 C63 1.439(7) . ? C63 C64 1.381(7) . ? C64 C65 1.398(7) . ? C64 H64 0.9300 . ? C65 C66 1.365(7) . ? C65 H65 0.9300 . ? C66 C67 1.488(7) . ? C67 C68 1.502(7) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.497(7) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.492(8) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.503(8) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.508(9) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 S1 C7 92.7(3) . . ? C14 S2 C11 93.1(3) . . ? C18 S3 C15 92.8(3) . . ? C31 S4 C34 92.5(3) . . ? C35 S5 C38 93.2(3) . . ? C42 S6 C39 92.8(3) . . ? C55 S7 C58 92.4(3) . . ? C62 S8 C59 92.2(3) . . ? C66 S9 C63 93.5(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 115.5(6) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C2 116.2(6) . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 115.9(5) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? C5 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C6 C5 C4 113.8(5) . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 116.9(5) . . ? C5 C6 H6A 108.1 . . ? C7 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? C7 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 128.2(6) . . ? C8 C7 S1 109.9(5) . . ? C6 C7 S1 121.9(5) . . ? C7 C8 C9 113.9(6) . . ? C7 C8 H8 123.0 . . ? C9 C8 H8 123.0 . . ? C10 C9 C8 113.7(6) . . ? C10 C9 H9 123.2 . . ? C8 C9 H9 123.2 . . ? C9 C10 C11 129.0(5) . . ? C9 C10 S1 109.7(5) . . ? C11 C10 S1 121.2(4) . . ? C12 C11 C10 130.3(5) . . ? C12 C11 S2 109.4(4) . . ? C10 C11 S2 120.3(4) . . ? C11 C12 C13 114.9(5) . . ? C11 C12 H12 122.5 . . ? C13 C12 H12 122.5 . . ? C14 C13 C12 112.6(5) . . ? C14 C13 H13 123.7 . . ? C12 C13 H13 123.7 . . ? C13 C14 C15 128.5(5) . . ? C13 C14 S2 110.0(4) . . ? C15 C14 S2 121.5(3) . . ? C16 C15 C14 128.2(5) . . ? C16 C15 S3 109.4(4) . . ? C14 C15 S3 122.3(4) . . ? C15 C16 C17 113.9(5) . . ? C15 C16 H16 123.0 . . ? C17 C16 H16 123.0 . . ? C18 C17 C16 114.1(5) . . ? C18 C17 H17 122.9 . . ? C16 C17 H17 122.9 . . ? C17 C18 C19 129.7(5) . . ? C17 C18 S3 109.7(4) . . ? C19 C18 S3 120.7(4) . . ? C18 C19 C20 115.6(4) . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C19 114.7(5) . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C19 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 116.0(5) . . ? C20 C21 H21A 108.3 . . ? C22 C21 H21A 108.3 . . ? C20 C21 H21B 108.3 . . ? C22 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C21 115.5(5) . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22B 108.4 . . ? C21 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C22 C23 C24 115.8(5) . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23B 108.3 . . ? C24 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C25 115.3(7) . . ? C27 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C26 C27 C28 114.8(6) . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C29 115.0(6) . . ? C27 C28 H28A 108.5 . . ? C29 C28 H28A 108.5 . . ? C27 C28 H28B 108.5 . . ? C29 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C30 C29 C28 116.1(5) . . ? C30 C29 H29A 108.3 . . ? C28 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? C28 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 116.6(5) . . ? C29 C30 H30A 108.1 . . ? C31 C30 H30A 108.1 . . ? C29 C30 H30B 108.1 . . ? C31 C30 H30B 108.1 . . ? H30A C30 H30B 107.3 . . ? C32 C31 C30 128.2(5) . . ? C32 C31 S4 110.7(5) . . ? C30 C31 S4 120.9(4) . . ? C31 C32 C33 113.0(5) . . ? C31 C32 H32 123.5 . . ? C33 C32 H32 123.5 . . ? C34 C33 C32 113.2(5) . . ? C34 C33 H33 123.4 . . ? C32 C33 H33 123.4 . . ? C33 C34 C35 127.8(5) . . ? C33 C34 S4 110.7(5) . . ? C35 C34 S4 121.5(4) . . ? C36 C35 C34 127.6(5) . . ? C36 C35 S5 110.6(5) . . ? C34 C35 S5 121.8(4) . . ? C35 C36 C37 113.0(5) . . ? C35 C36 H36 123.5 . . ? C37 C36 H36 123.5 . . ? C38 C37 C36 113.5(5) . . ? C38 C37 H37 123.2 . . ? C36 C37 H37 123.2 . . ? C37 C38 C39 128.9(5) . . ? C37 C38 S5 109.7(5) . . ? C39 C38 S5 121.4(4) . . ? C40 C39 C38 129.1(5) . . ? C40 C39 S6 109.9(5) . . ? C38 C39 S6 121.0(4) . . ? C39 C40 C41 113.9(5) . . ? C39 C40 H40 123.1 . . ? C41 C40 H40 123.1 . . ? C42 C41 C40 113.3(6) . . ? C42 C41 H41 123.4 . . ? C40 C41 H41 123.4 . . ? C41 C42 C43 130.4(6) . . ? C41 C42 S6 110.2(5) . . ? C43 C42 S6 119.4(4) . . ? C42 C43 C44 115.1(5) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C45 C44 C43 113.8(5) . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44A 108.8 . . ? C45 C44 H44B 108.8 . . ? C43 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C46 C45 C44 115.6(6) . . ? C46 C45 H45A 108.4 . . ? C44 C45 H45A 108.4 . . ? C46 C45 H45B 108.4 . . ? C44 C45 H45B 108.4 . . ? H45A C45 H45B 107.4 . . ? C45 C46 C47 114.6(7) . . ? C45 C46 H46A 108.6 . . ? C47 C46 H46A 108.6 . . ? C45 C46 H46B 108.6 . . ? C47 C46 H46B 108.6 . . ? H46A C46 H46B 107.6 . . ? C48 C47 C46 115.1(8) . . ? C48 C47 H47A 108.5 . . ? C46 C47 H47A 108.5 . . ? C48 C47 H47B 108.5 . . ? C46 C47 H47B 108.5 . . ? H47A C47 H47B 107.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 C51 113.3(7) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 115.4(6) . . ? C52 C51 H51A 108.4 . . ? C50 C51 H51A 108.4 . . ? C52 C51 H51B 108.4 . . ? C50 C51 H51B 108.4 . . ? H51A C51 H51B 107.5 . . ? C51 C52 C53 116.0(6) . . ? C51 C52 H52A 108.3 . . ? C53 C52 H52A 108.3 . . ? C51 C52 H52B 108.3 . . ? C53 C52 H52B 108.3 . . ? H52A C52 H52B 107.4 . . ? C54 C53 C52 114.1(5) . . ? C54 C53 H53A 108.7 . . ? C52 C53 H53A 108.7 . . ? C54 C53 H53B 108.7 . . ? C52 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C55 C54 C53 114.8(5) . . ? C55 C54 H54A 108.6 . . ? C53 C54 H54A 108.6 . . ? C55 C54 H54B 108.6 . . ? C53 C54 H54B 108.6 . . ? H54A C54 H54B 107.5 . . ? C56 C55 C54 130.2(5) . . ? C56 C55 S7 109.8(5) . . ? C54 C55 S7 120.0(4) . . ? C55 C56 C57 114.3(5) . . ? C55 C56 H56 122.9 . . ? C57 C56 H56 122.9 . . ? C58 C57 C56 113.3(5) . . ? C58 C57 H57 123.3 . . ? C56 C57 H57 123.3 . . ? C57 C58 C59 128.5(5) . . ? C57 C58 S7 110.2(5) . . ? C59 C58 S7 121.2(4) . . ? C60 C59 C58 129.2(5) . . ? C60 C59 S8 109.6(5) . . ? C58 C59 S8 121.1(4) . . ? C61 C60 C59 113.7(5) . . ? C61 C60 H60 123.2 . . ? C59 C60 H60 123.2 . . ? C62 C61 C60 114.0(5) . . ? C62 C61 H61 123.0 . . ? C60 C61 H61 123.0 . . ? C61 C62 C63 128.9(5) . . ? C61 C62 S8 110.5(5) . . ? C63 C62 S8 120.6(4) . . ? C64 C63 C62 129.6(5) . . ? C64 C63 S9 108.4(5) . . ? C62 C63 S9 122.0(4) . . ? C63 C64 C65 114.6(5) . . ? C63 C64 H64 122.7 . . ? C65 C64 H64 122.7 . . ? C66 C65 C64 112.6(5) . . ? C66 C65 H65 123.7 . . ? C64 C65 H65 123.7 . . ? C65 C66 C67 128.1(6) . . ? C65 C66 S9 111.0(5) . . ? C67 C66 S9 120.9(4) . . ? C66 C67 C68 116.9(5) . . ? C66 C67 H67A 108.1 . . ? C68 C67 H67A 108.1 . . ? C66 C67 H67B 108.1 . . ? C68 C67 H67B 108.1 . . ? H67A C67 H67B 107.3 . . ? C69 C68 C67 114.6(5) . . ? C69 C68 H68A 108.6 . . ? C67 C68 H68A 108.6 . . ? C69 C68 H68B 108.6 . . ? C67 C68 H68B 108.6 . . ? H68A C68 H68B 107.6 . . ? C70 C69 C68 115.3(6) . . ? C70 C69 H69A 108.5 . . ? C68 C69 H69A 108.5 . . ? C70 C69 H69B 108.5 . . ? C68 C69 H69B 108.5 . . ? H69A C69 H69B 107.5 . . ? C69 C70 C71 115.4(6) . . ? C69 C70 H70A 108.4 . . ? C71 C70 H70A 108.4 . . ? C69 C70 H70B 108.4 . . ? C71 C70 H70B 108.4 . . ? H70A C70 H70B 107.5 . . ? C70 C71 C72 115.1(7) . . ? C70 C71 H71A 108.5 . . ? C72 C71 H71A 108.5 . . ? C70 C71 H71B 108.5 . . ? C72 C71 H71B 108.5 . . ? H71A C71 H71B 107.5 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 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 C1 C2 C3 C4 -178.5(7) . . . . ? C2 C3 C4 C5 178.2(6) . . . . ? C3 C4 C5 C6 179.0(6) . . . . ? C4 C5 C6 C7 173.2(5) . . . . ? C5 C6 C7 C8 -116.6(7) . . . . ? C5 C6 C7 S1 65.2(7) . . . . ? C10 S1 C7 C8 1.0(4) . . . . ? C10 S1 C7 C6 179.5(5) . . . . ? C6 C7 C8 C9 -178.8(5) . . . . ? S1 C7 C8 C9 -0.4(6) . . . . ? C7 C8 C9 C10 -0.5(8) . . . . ? C8 C9 C10 C11 178.9(5) . . . . ? C8 C9 C10 S1 1.2(6) . . . . ? C7 S1 C10 C9 -1.2(4) . . . . ? C7 S1 C10 C11 -179.1(4) . . . . ? C9 C10 C11 C12 179.1(5) . . . . ? S1 C10 C11 C12 -3.4(7) . . . . ? C9 C10 C11 S2 -3.5(8) . . . . ? S1 C10 C11 S2 173.9(2) . . . . ? C14 S2 C11 C12 0.0(4) . . . . ? C14 S2 C11 C10 -177.9(4) . . . . ? C10 C11 C12 C13 177.7(5) . . . . ? S2 C11 C12 C13 0.1(5) . . . . ? C11 C12 C13 C14 -0.2(6) . . . . ? C12 C13 C14 C15 -175.9(4) . . . . ? C12 C13 C14 S2 0.2(5) . . . . ? C11 S2 C14 C13 -0.1(3) . . . . ? C11 S2 C14 C15 176.3(4) . . . . ? C13 C14 C15 C16 174.8(4) . . . . ? S2 C14 C15 C16 -0.9(6) . . . . ? C13 C14 C15 S3 -0.9(7) . . . . ? S2 C14 C15 S3 -176.7(2) . . . . ? C18 S3 C15 C16 0.8(3) . . . . ? C18 S3 C15 C14 177.3(4) . . . . ? C14 C15 C16 C17 -177.6(4) . . . . ? S3 C15 C16 C17 -1.4(5) . . . . ? C15 C16 C17 C18 1.4(6) . . . . ? C16 C17 C18 C19 179.1(4) . . . . ? C16 C17 C18 S3 -0.8(5) . . . . ? C15 S3 C18 C17 0.0(3) . . . . ? C15 S3 C18 C19 -179.9(4) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? S3 C18 C19 C20 -179.8(3) . . . . ? C18 C19 C20 C21 -175.2(4) . . . . ? C19 C20 C21 C22 178.9(4) . . . . ? C20 C21 C22 C23 -175.9(5) . . . . ? C21 C22 C23 C24 179.9(5) . . . . ? C25 C26 C27 C28 -179.6(6) . . . . ? C26 C27 C28 C29 175.2(6) . . . . ? C27 C28 C29 C30 -179.7(5) . . . . ? C28 C29 C30 C31 174.8(5) . . . . ? C29 C30 C31 C32 -3.4(8) . . . . ? C29 C30 C31 S4 -179.3(4) . . . . ? C34 S4 C31 C32 0.4(4) . . . . ? C34 S4 C31 C30 176.9(4) . . . . ? C30 C31 C32 C33 -176.6(5) . . . . ? S4 C31 C32 C33 -0.3(5) . . . . ? C31 C32 C33 C34 0.1(6) . . . . ? C32 C33 C34 C35 177.3(5) . . . . ? C32 C33 C34 S4 0.2(5) . . . . ? C31 S4 C34 C33 -0.3(4) . . . . ? C31 S4 C34 C35 -177.7(4) . . . . ? C33 C34 C35 C36 -178.0(5) . . . . ? S4 C34 C35 C36 -1.1(7) . . . . ? C33 C34 C35 S5 -0.5(7) . . . . ? S4 C34 C35 S5 176.4(2) . . . . ? C38 S5 C35 C36 0.8(4) . . . . ? C38 S5 C35 C34 -177.2(4) . . . . ? C34 C35 C36 C37 177.0(5) . . . . ? S5 C35 C36 C37 -0.8(5) . . . . ? C35 C36 C37 C38 0.4(6) . . . . ? C36 C37 C38 C39 -178.9(5) . . . . ? C36 C37 C38 S5 0.2(5) . . . . ? C35 S5 C38 C37 -0.5(4) . . . . ? C35 S5 C38 C39 178.7(4) . . . . ? C37 C38 C39 C40 -177.4(5) . . . . ? S5 C38 C39 C40 3.5(7) . . . . ? C37 C38 C39 S6 2.4(7) . . . . ? S5 C38 C39 S6 -176.7(2) . . . . ? C42 S6 C39 C40 0.3(4) . . . . ? C42 S6 C39 C38 -179.5(4) . . . . ? C38 C39 C40 C41 178.9(5) . . . . ? S6 C39 C40 C41 -0.9(5) . . . . ? C39 C40 C41 C42 1.1(7) . . . . ? C40 C41 C42 C43 179.8(5) . . . . ? C40 C41 C42 S6 -0.8(6) . . . . ? C39 S6 C42 C41 0.3(4) . . . . ? C39 S6 C42 C43 179.7(4) . . . . ? C41 C42 C43 C44 -0.4(8) . . . . ? S6 C42 C43 C44 -179.7(4) . . . . ? C42 C43 C44 C45 -174.9(5) . . . . ? C43 C44 C45 C46 177.1(5) . . . . ? C44 C45 C46 C47 -174.1(6) . . . . ? C45 C46 C47 C48 175.4(8) . . . . ? C49 C50 C51 C52 177.3(7) . . . . ? C50 C51 C52 C53 -177.6(6) . . . . ? C51 C52 C53 C54 178.3(5) . . . . ? C52 C53 C54 C55 179.7(5) . . . . ? C53 C54 C55 C56 0.9(8) . . . . ? C53 C54 C55 S7 -179.5(4) . . . . ? C58 S7 C55 C56 -0.2(4) . . . . ? C58 S7 C55 C54 -179.8(4) . . . . ? C54 C55 C56 C57 179.5(5) . . . . ? S7 C55 C56 C57 -0.1(6) . . . . ? C55 C56 C57 C58 0.4(6) . . . . ? C56 C57 C58 C59 -177.2(4) . . . . ? C56 C57 C58 S7 -0.6(5) . . . . ? C55 S7 C58 C57 0.4(4) . . . . ? C55 S7 C58 C59 177.4(4) . . . . ? C57 C58 C59 C60 177.1(4) . . . . ? S7 C58 C59 C60 0.8(7) . . . . ? C57 C58 C59 S8 0.3(7) . . . . ? S7 C58 C59 S8 -176.0(2) . . . . ? C62 S8 C59 C60 -0.4(3) . . . . ? C62 S8 C59 C58 176.9(4) . . . . ? C58 C59 C60 C61 -176.9(5) . . . . ? S8 C59 C60 C61 0.2(5) . . . . ? C59 C60 C61 C62 0.3(6) . . . . ? C60 C61 C62 C63 179.3(5) . . . . ? C60 C61 C62 S8 -0.7(5) . . . . ? C59 S8 C62 C61 0.6(4) . . . . ? C59 S8 C62 C63 -179.3(4) . . . . ? C61 C62 C63 C64 176.3(5) . . . . ? S8 C62 C63 C64 -3.7(7) . . . . ? C61 C62 C63 S9 -2.9(7) . . . . ? S8 C62 C63 S9 177.1(2) . . . . ? C66 S9 C63 C64 0.0(4) . . . . ? C66 S9 C63 C62 179.4(4) . . . . ? C62 C63 C64 C65 -179.8(5) . . . . ? S9 C63 C64 C65 -0.5(5) . . . . ? C63 C64 C65 C66 0.9(7) . . . . ? C64 C65 C66 C67 -178.2(5) . . . . ? C64 C65 C66 S9 -0.8(6) . . . . ? C63 S9 C66 C65 0.4(4) . . . . ? C63 S9 C66 C67 178.1(4) . . . . ? C65 C66 C67 C68 -2.9(8) . . . . ? S9 C66 C67 C68 179.9(4) . . . . ? C66 C67 C68 C69 174.7(5) . . . . ? C67 C68 C69 C70 -177.2(5) . . . . ? C68 C69 C70 C71 176.4(6) . . . . ? C69 C70 C71 C72 -176.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.482 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.052