# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peter Bauerle' _publ_contact_author_address ; Department Organic Chemistry II University of Ulm Albert-Einstein-Allee 11 D-89081 Ulm Germany ; _publ_contact_author_email peter.baeuerle@chemie.uni-ulm.de _publ_contact_author_fax 49(731)50-22840 _publ_contact_author_phone 49(731)50-22850 # TITLE AND AUTHOR LIST _publ_section_title ; C-C bond formation through oxidatively induced elimination of platinum complexes - A novel approach towards conjugated macrocycles ; loop_ _publ_author_name _publ_author_address 'Peter Bauerle' ; Department Organic Chemistry II University of Ulm Albert-Einstein-Allee 11 D-89081 Ulm Germany ; 'Gerda Fuhrmann' ; Department Organic Chemistry II University of Ulm Albert-Einstein-Allee 11 D-89081 Ulm Germany ; 'Tony Debaerdemaeker' ; Division of X-ray and Electron Diffraction University of Ulm Albert-Einstein-Allee 11 D-89081 Ulm Germany ; #========================================================================= data_fuh410 _database_code_CSD 201462 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 7,8,15,16, 23,24,31,32-Octabutyl-33,34,35,36,37,38-hexathia-heptacyclo [28,2,1^6,9^,1^10,13^,1^14,17^,1^22,25^,1^26,29^,1^1,30^]-1(32),6,8,10,12,14, 16,22,24,26,28,30-dodecaene-2,4,18,20-tetrayne ; _chemical_melting_point 262 _chemical_formula_sum 'C64 H76 S6' _chemical_formula_weight 1037.61 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 monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.074(1) _cell_length_b 20.222(2) _cell_length_c 16.503(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.87(2) _cell_angle_gamma 90.00 _cell_volume 2926.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'STOE-IPDS, image plate' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 0.15 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22852 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5347 _reflns_number_gt 3949 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE-IPDS _computing_cell_refinement STOE-IPDS _computing_data_reduction STOE-IPDS _computing_structure_solution SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. The molecule of the title compound is laying on an inversion centre so that it was only necessary to determine the location of half the atoms. ; _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^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refu _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5347 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.23537(5) 0.38899(2) 0.19033(3) 0.02957(12) Uani 1 1 d . . . S2 S 0.93809(5) 0.31885(2) 0.08336(3) 0.02981(12) Uani 1 1 d . . . S3 S 0.71990(5) 0.33821(2) -0.08989(3) 0.03054(12) Uani 1 1 d . . . C2 C 1.36592(19) 0.34474(8) 0.33828(11) 0.0258(4) Uani 1 1 d . . . C7 C 0.86307(19) 0.24914(8) 0.02625(11) 0.0265(4) Uani 1 1 d . . . C12 C 0.55295(19) 0.24620(8) -0.17491(12) 0.0281(4) Uani 1 1 d . . . C4 C 1.26758(18) 0.29330(8) 0.29616(11) 0.0249(4) Uani 1 1 d . . . C3 C 1.18932(19) 0.31016(8) 0.21612(11) 0.0262(4) Uani 1 1 d . . . C11 C 0.58032(19) 0.31311(8) -0.17630(12) 0.0284(4) Uani 1 1 d . . . C17 C 1.4672(2) 0.51892(8) 0.29335(12) 0.0313(4) Uani 1 1 d . . . C13 C 0.5265(2) 0.36431(8) -0.23510(12) 0.0299(4) Uani 1 1 d . . . C9 C 0.74504(19) 0.25854(8) -0.05066(11) 0.0259(4) Uani 1 1 d . . . C102 C 0.7470(2) 0.09793(9) -0.11593(15) 0.0341(4) Uani 1 1 d . . . C21 C 1.4573(2) 0.34131(10) 0.42744(12) 0.0322(4) Uani 1 1 d . . . C10 C 0.64651(19) 0.21481(8) -0.10252(12) 0.0263(4) Uani 1 1 d . . . C1 C 1.35916(19) 0.39984(8) 0.28782(11) 0.0272(4) Uani 1 1 d . . . C101 C 0.6396(2) 0.14240(8) -0.08244(14) 0.0295(4) Uani 1 1 d . . . C22 C 1.3618(3) 0.35615(11) 0.49016(15) 0.0444(5) Uani 1 1 d . . . C5 C 1.07643(19) 0.27380(8) 0.15348(11) 0.0265(4) Uani 1 1 d . . . C15 C 0.5167(2) 0.41740(9) -0.26894(12) 0.0315(4) Uani 1 1 d . . . C19 C 1.43057(19) 0.46254(8) 0.30163(11) 0.0294(4) Uani 1 1 d . . . C41 C 1.2537(2) 0.22652(8) 0.33397(13) 0.0278(4) Uani 1 1 d . . . C43 C 1.3362(3) 0.10605(9) 0.33819(16) 0.0401(5) Uani 1 1 d . . . C8 C 0.9403(2) 0.19420(9) 0.06322(12) 0.0321(4) Uani 1 1 d . . . C42 C 1.3688(2) 0.17658(8) 0.31673(14) 0.0310(4) Uani 1 1 d . . . C103 C 0.7479(3) 0.02755(10) -0.08398(18) 0.0472(6) Uani 1 1 d . . . C122 C 0.4931(3) 0.20556(11) -0.32478(14) 0.0439(5) Uani 1 1 d . . . C6 C 1.0587(2) 0.20796(9) 0.13444(13) 0.0326(4) Uani 1 1 d . . . C23 C 1.2008(3) 0.43944(16) 0.54229(19) 0.0584(7) Uani 1 1 d . . . C124 C 0.3224(3) 0.10953(12) -0.3883(2) 0.0569(7) Uani 1 1 d . . . C121 C 0.4389(2) 0.21263(10) -0.24511(13) 0.0336(4) Uani 1 1 d . . . C123 C 0.3713(3) 0.17894(11) -0.39940(16) 0.0539(6) Uani 1 1 d . . . C24 C 1.3222(3) 0.42800(11) 0.49364(16) 0.0499(6) Uani 1 1 d . . . C44 C 1.4408(3) 0.05666(11) 0.31181(19) 0.0521(6) Uani 1 1 d . . . C104 C 0.8627(4) -0.01685(13) -0.1099(2) 0.0643(7) Uani 1 1 d . . . H1 H 1.147(2) 0.2097(8) 0.3084(12) 0.027(5) Uiso 1 1 d . . . H2 H 1.2673(19) 0.2302(8) 0.3926(13) 0.025(5) Uiso 1 1 d . . . H3 H 0.533(2) 0.1267(9) -0.1051(12) 0.034(5) Uiso 1 1 d . . . H4 H 0.662(2) 0.1365(9) -0.0228(14) 0.033(5) Uiso 1 1 d . . . H5 H 1.365(2) 0.1777(8) 0.2561(13) 0.027(5) Uiso 1 1 d . . . H6 H 1.471(2) 0.1897(9) 0.3498(13) 0.036(5) Uiso 1 1 d . . . H7 H 0.921(2) 0.1515(10) 0.0407(13) 0.037(5) Uiso 1 1 d . . . H8 H 0.413(2) 0.1698(11) -0.2267(14) 0.046(6) Uiso 1 1 d . . . H9 H 0.850(2) 0.1164(9) -0.0977(13) 0.033(5) Uiso 1 1 d . . . H10 H 1.121(2) 0.1764(10) 0.1661(13) 0.040(5) Uiso 1 1 d . . . H11 H 0.344(2) 0.2359(10) -0.2567(13) 0.043(6) Uiso 1 1 d . . . H12 H 1.545(2) 0.3704(10) 0.4345(13) 0.038(5) Uiso 1 1 d . . . H13 H 0.721(2) 0.0981(9) -0.1747(15) 0.041(6) Uiso 1 1 d . . . H16 H 1.345(3) 0.1021(10) 0.3978(16) 0.050(6) Uiso 1 1 d . . . H17 H 0.582(3) 0.1774(11) -0.3114(15) 0.051(6) Uiso 1 1 d . . . H18 H 1.228(3) 0.0957(10) 0.3098(14) 0.045(6) Uiso 1 1 d . . . H19 H 1.498(2) 0.2975(11) 0.4402(13) 0.044(6) Uiso 1 1 d . . . H20 H 0.639(3) 0.0078(11) -0.1032(15) 0.056(7) Uiso 1 1 d . . . H21 H 1.551(3) 0.0656(12) 0.3420(17) 0.071(8) Uiso 1 1 d . . . H22 H 1.237(3) 0.4212(12) 0.6017(19) 0.069(8) Uiso 1 1 d . . . H23 H 1.250(3) 0.3440(12) 0.4836(17) 0.074(8) Uiso 1 1 d . . . H24 H 0.419(3) 0.1793(11) -0.4469(18) 0.063(7) Uiso 1 1 d . . . H25 H 1.434(3) 0.0599(11) 0.2520(17) 0.056(7) Uiso 1 1 d . . . H26 H 0.533(3) 0.2468(12) -0.3399(16) 0.063(7) Uiso 1 1 d . . . H27 H 1.425(3) 0.4535(12) 0.5202(16) 0.066(7) Uiso 1 1 d . . . H28 H 0.284(3) 0.2096(13) -0.4100(17) 0.075(8) Uiso 1 1 d . . . H29 H 0.769(2) 0.0275(10) -0.0251(16) 0.048(7) Uiso 1 1 d . . . H30 H 0.840(3) -0.0185(13) -0.176(2) 0.079(9) Uiso 1 1 d . . . H31 H 0.416(3) 0.0814(13) -0.3714(17) 0.075(8) Uiso 1 1 d . . . H32 H 0.971(3) 0.0008(13) -0.0895(18) 0.073(8) Uiso 1 1 d . . . H33 H 1.111(4) 0.4190(14) 0.5191(19) 0.081(9) Uiso 1 1 d . . . H34 H 0.281(4) 0.1056(14) -0.343(2) 0.087(10) Uiso 1 1 d . . . H35 H 0.250(3) 0.0929(13) -0.4385(19) 0.074(8) Uiso 1 1 d . . . H36 H 1.284(3) 0.4474(13) 0.4290(19) 0.084(9) Uiso 1 1 d . . . H37 H 0.862(4) -0.0601(17) -0.087(2) 0.109(11) Uiso 1 1 d . . . H38 H 1.174(4) 0.4863(17) 0.545(2) 0.106(11) Uiso 1 1 d . . . H39 H 1.419(3) 0.3420(12) 0.5477(18) 0.068(8) Uiso 1 1 d . . . H40 H 1.419(3) 0.0110(13) 0.3228(17) 0.070(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0362(2) 0.0272(2) 0.0236(3) 0.00273(17) 0.00444(19) -0.00050(18) S2 0.0342(2) 0.0261(2) 0.0259(3) -0.00068(17) 0.00165(19) 0.00203(17) S3 0.0341(2) 0.0252(2) 0.0290(3) 0.00039(17) 0.00211(19) -0.00130(18) C2 0.0235(8) 0.0299(9) 0.0245(11) 0.0013(7) 0.0071(7) 0.0049(7) C7 0.0280(9) 0.0272(9) 0.0253(11) -0.0020(7) 0.0085(8) -0.0011(7) C12 0.0257(8) 0.0311(9) 0.0283(11) -0.0007(7) 0.0085(8) -0.0008(7) C4 0.0251(8) 0.0270(8) 0.0236(11) 0.0015(7) 0.0084(7) 0.0032(7) C3 0.0273(9) 0.0261(8) 0.0262(11) 0.0008(7) 0.0087(7) 0.0021(7) C11 0.0283(9) 0.0306(9) 0.0251(11) -0.0001(7) 0.0047(7) -0.0008(7) C17 0.0325(9) 0.0326(10) 0.0253(12) 0.0005(7) 0.0010(8) 0.0009(8) C13 0.0302(9) 0.0311(9) 0.0258(11) -0.0016(7) 0.0027(8) -0.0023(7) C9 0.0271(8) 0.0254(8) 0.0260(11) 0.0013(7) 0.0080(7) 0.0016(7) C102 0.0386(11) 0.0314(10) 0.0329(14) -0.0023(8) 0.0103(9) -0.0001(8) C21 0.0303(10) 0.0367(10) 0.0267(12) 0.0023(8) 0.0024(8) 0.0043(8) C10 0.0246(8) 0.0269(9) 0.0284(11) -0.0004(7) 0.0086(7) 0.0013(7) C1 0.0277(9) 0.0287(9) 0.0246(11) -0.0006(7) 0.0056(8) 0.0025(7) C101 0.0285(10) 0.0273(9) 0.0325(13) 0.0005(7) 0.0076(8) -0.0030(7) C22 0.0496(13) 0.0548(13) 0.0276(14) 0.0023(9) 0.0076(10) 0.0084(10) C5 0.0290(9) 0.0295(9) 0.0218(11) 0.0020(7) 0.0076(7) 0.0022(7) C15 0.0304(9) 0.0331(10) 0.0276(12) -0.0018(8) 0.0013(8) -0.0019(7) C19 0.0296(9) 0.0326(10) 0.0245(11) 0.0000(7) 0.0044(8) 0.0020(7) C41 0.0291(10) 0.0309(9) 0.0233(12) 0.0049(7) 0.0067(8) -0.0008(7) C43 0.0451(12) 0.0310(10) 0.0473(16) 0.0080(9) 0.0173(11) 0.0016(9) C8 0.0374(10) 0.0251(9) 0.0315(12) -0.0016(7) 0.0044(8) -0.0006(7) C42 0.0278(10) 0.0308(9) 0.0339(13) 0.0069(8) 0.0071(8) -0.0001(7) C103 0.0613(15) 0.0310(10) 0.0506(18) 0.0026(9) 0.0169(12) 0.0066(10) C122 0.0538(14) 0.0439(12) 0.0325(14) -0.0011(9) 0.0084(10) -0.0136(11) C6 0.0347(10) 0.0286(9) 0.0317(12) 0.0027(8) 0.0034(8) 0.0051(8) C23 0.0558(16) 0.0792(19) 0.0428(18) -0.0111(13) 0.0171(13) 0.0138(14) C124 0.0586(16) 0.0506(14) 0.0539(19) -0.0121(12) 0.0006(14) -0.0115(12) C121 0.0302(10) 0.0345(10) 0.0331(13) 0.0003(8) 0.0029(8) -0.0039(8) C123 0.0716(17) 0.0463(13) 0.0345(16) -0.0031(10) -0.0031(12) -0.0039(12) C24 0.0582(14) 0.0487(13) 0.0432(16) -0.0062(10) 0.0139(11) -0.0002(11) C44 0.0581(16) 0.0380(12) 0.064(2) 0.0091(11) 0.0223(13) 0.0115(10) C104 0.079(2) 0.0434(14) 0.070(2) -0.0024(13) 0.0192(16) 0.0224(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.7235(19) . ? S1 C3 1.7287(17) . ? S2 C5 1.7316(18) . ? S2 C7 1.7348(17) . ? S3 C11 1.7227(19) . ? S3 C9 1.7293(16) . ? C2 C1 1.383(2) . ? C2 C4 1.429(2) . ? C2 C21 1.494(3) . ? C7 C8 1.370(2) . ? C7 C9 1.448(3) . ? C12 C11 1.377(2) . ? C12 C10 1.425(3) . ? C12 C121 1.503(3) . ? C4 C3 1.373(3) . ? C4 C41 1.506(2) . ? C3 C5 1.454(2) . ? C11 C13 1.417(2) . ? C17 C19 1.205(2) . ? C17 C15 1.368(2) 3_765 ? C13 C15 1.203(2) . ? C9 C10 1.386(2) . ? C102 C103 1.517(3) . ? C102 C101 1.530(3) . ? C21 C22 1.540(3) . ? C10 C101 1.506(2) . ? C1 C19 1.416(2) . ? C22 C24 1.501(3) . ? C5 C6 1.368(2) . ? C15 C17 1.368(2) 3_765 ? C41 C42 1.531(3) . ? C43 C44 1.516(3) . ? C43 C42 1.517(3) . ? C8 C6 1.402(3) . ? C103 C104 1.518(3) . ? C122 C121 1.524(3) . ? C122 C123 1.526(3) . ? C23 C24 1.538(3) . ? C124 C123 1.497(3) . ? 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 S1 C3 91.62(8) . . ? C5 S2 C7 92.96(8) . . ? C11 S3 C9 91.94(8) . . ? C1 C2 C4 111.58(16) . . ? C1 C2 C21 123.93(16) . . ? C4 C2 C21 124.38(16) . . ? C8 C7 C9 132.49(16) . . ? C8 C7 S2 109.41(14) . . ? C9 C7 S2 117.93(12) . . ? C11 C12 C10 112.36(15) . . ? C11 C12 C121 121.50(16) . . ? C10 C12 C121 126.11(15) . . ? C3 C4 C2 113.05(15) . . ? C3 C4 C41 122.93(16) . . ? C2 C4 C41 124.00(16) . . ? C4 C3 C5 130.89(15) . . ? C4 C3 S1 111.59(13) . . ? C5 C3 S1 117.51(13) . . ? C12 C11 C13 134.22(17) . . ? C12 C11 S3 111.91(13) . . ? C13 C11 S3 113.72(13) . . ? C19 C17 C15 167.7(2) . 3_765 ? C15 C13 C11 160.28(19) . . ? C10 C9 C7 132.24(15) . . ? C10 C9 S3 111.16(13) . . ? C7 C9 S3 116.58(12) . . ? C103 C102 C101 111.91(17) . . ? C2 C21 C22 112.78(16) . . ? C9 C10 C12 112.62(15) . . ? C9 C10 C101 122.76(17) . . ? C12 C10 C101 124.61(16) . . ? C2 C1 C19 132.61(17) . . ? C2 C1 S1 112.16(13) . . ? C19 C1 S1 115.21(13) . . ? C10 C101 C102 115.20(15) . . ? C24 C22 C21 113.30(18) . . ? C6 C5 C3 132.47(16) . . ? C6 C5 S2 109.64(14) . . ? C3 C5 S2 117.81(12) . . ? C13 C15 C17 167.4(2) . 3_765 ? C17 C19 C1 163.21(19) . . ? C4 C41 C42 112.38(15) . . ? C44 C43 C42 112.23(18) . . ? C7 C8 C6 114.00(16) . . ? C43 C42 C41 113.18(16) . . ? C102 C103 C104 113.6(2) . . ? C121 C122 C123 113.7(2) . . ? C5 C6 C8 113.91(16) . . ? C12 C121 C122 113.38(16) . . ? C124 C123 C122 114.1(2) . . ? C22 C24 C23 112.1(2) . . ? 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 S2 C7 C8 2.19(14) . . . . ? C5 S2 C7 C9 -173.61(13) . . . . ? C1 C2 C4 C3 -0.2(2) . . . . ? C21 C2 C4 C3 176.24(15) . . . . ? C1 C2 C4 C41 178.10(15) . . . . ? C21 C2 C4 C41 -5.5(3) . . . . ? C2 C4 C3 C5 -178.09(16) . . . . ? C41 C4 C3 C5 3.6(3) . . . . ? C2 C4 C3 S1 0.47(18) . . . . ? C41 C4 C3 S1 -177.80(13) . . . . ? C1 S1 C3 C4 -0.52(13) . . . . ? C1 S1 C3 C5 178.26(13) . . . . ? C10 C12 C11 C13 175.23(19) . . . . ? C121 C12 C11 C13 -3.1(3) . . . . ? C10 C12 C11 S3 0.11(19) . . . . ? C121 C12 C11 S3 -178.22(14) . . . . ? C9 S3 C11 C12 0.46(14) . . . . ? C9 S3 C11 C13 -175.72(14) . . . . ? C12 C11 C13 C15 -167.5(5) . . . . ? S3 C11 C13 C15 7.5(6) . . . . ? C8 C7 C9 C10 17.3(3) . . . . ? S2 C7 C9 C10 -168.11(16) . . . . ? C8 C7 C9 S3 -160.84(17) . . . . ? S2 C7 C9 S3 13.79(18) . . . . ? C11 S3 C9 C10 -0.93(14) . . . . ? C11 S3 C9 C7 177.56(13) . . . . ? C1 C2 C21 C22 96.5(2) . . . . ? C4 C2 C21 C22 -79.5(2) . . . . ? C7 C9 C10 C12 -177.02(17) . . . . ? S3 C9 C10 C12 1.16(19) . . . . ? C7 C9 C10 C101 3.9(3) . . . . ? S3 C9 C10 C101 -177.95(13) . . . . ? C11 C12 C10 C9 -0.8(2) . . . . ? C121 C12 C10 C9 177.41(16) . . . . ? C11 C12 C10 C101 178.26(16) . . . . ? C121 C12 C10 C101 -3.5(3) . . . . ? C4 C2 C1 C19 178.08(17) . . . . ? C21 C2 C1 C19 1.7(3) . . . . ? C4 C2 C1 S1 -0.24(18) . . . . ? C21 C2 C1 S1 -176.65(13) . . . . ? C3 S1 C1 C2 0.43(13) . . . . ? C3 S1 C1 C19 -178.20(14) . . . . ? C9 C10 C101 C102 -89.9(2) . . . . ? C12 C10 C101 C102 91.1(2) . . . . ? C103 C102 C101 C10 172.79(19) . . . . ? C2 C21 C22 C24 -73.7(2) . . . . ? C4 C3 C5 C6 -34.2(3) . . . . ? S1 C3 C5 C6 147.33(18) . . . . ? C4 C3 C5 S2 149.41(16) . . . . ? S1 C3 C5 S2 -29.09(18) . . . . ? C7 S2 C5 C6 -2.53(14) . . . . ? C7 S2 C5 C3 174.67(14) . . . . ? C11 C13 C15 C17 0.6(14) . . . 3_765 ? C15 C17 C19 C1 8.0(14) 3_765 . . . ? C2 C1 C19 C17 -174.0(6) . . . . ? S1 C1 C19 C17 4.3(7) . . . . ? C3 C4 C41 C42 89.1(2) . . . . ? C2 C4 C41 C42 -89.0(2) . . . . ? C9 C7 C8 C6 173.65(18) . . . . ? S2 C7 C8 C6 -1.3(2) . . . . ? C44 C43 C42 C41 173.7(2) . . . . ? C4 C41 C42 C43 -168.11(18) . . . . ? C101 C102 C103 C104 -175.2(2) . . . . ? C3 C5 C6 C8 -174.41(18) . . . . ? S2 C5 C6 C8 2.2(2) . . . . ? C7 C8 C6 C5 -0.6(2) . . . . ? C11 C12 C121 C122 73.0(2) . . . . ? C10 C12 C121 C122 -105.1(2) . . . . ? C123 C122 C121 C12 -173.25(18) . . . . ? C121 C122 C123 C124 -65.0(3) . . . . ? C21 C22 C24 C23 168.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.539 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.038