# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Paul Raithby' _publ_contact_author_email p.r.raithby@bath.ac.uk _publ_author_name 'Paul Raithby' data_k01prr15 _database_code_depnum_ccdc_archive 'CCDC 828207' #TrackingRef '- EDOT_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'k01prr15 1a' _chemical_melting_point ? _chemical_formula_moiety 'C16 H22 O2 S Si2' _chemical_formula_sum 'C16 H22 O2 S Si2' _chemical_formula_weight 334.58 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.3848(4) _cell_length_b 27.2437(12) _cell_length_c 9.4632(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.407(2) _cell_angle_gamma 90.00 _cell_volume 1878.29(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 103602 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 1.057 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method '1078 0.3 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11695 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4099 _reflns_number_gt 2741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DirDif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0431P)^2^+2.5722P] 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 4099 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.010 _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 C1 C 0.8807(5) -0.03825(13) 0.3536(4) 0.0341(8) Uani 1 1 d . . . C2 C 0.8531(4) -0.05335(14) 0.1998(4) 0.0332(8) Uani 1 1 d . . . C3 C 0.6095(4) 0.00524(11) 0.2984(3) 0.0270(7) Uani 1 1 d . . . C4 C 0.5500(4) -0.03006(11) 0.1915(3) 0.0251(7) Uani 1 1 d . . . C5 C 0.4727(4) 0.03710(12) 0.3227(3) 0.0278(7) Uani 1 1 d . . . C6 C 0.3666(4) -0.02679(11) 0.1378(3) 0.0262(7) Uani 1 1 d . . . C7 C 0.4878(4) 0.07786(12) 0.4172(4) 0.0302(7) Uani 1 1 d . . . C8 C 0.5002(4) 0.11312(12) 0.4947(4) 0.0332(8) Uani 1 1 d . . . C9 C 0.7791(6) 0.16890(16) 0.6941(5) 0.0417(9) Uani 1 1 d . . . C10 C 0.3731(7) 0.17725(16) 0.7211(5) 0.0455(10) Uani 1 1 d . . . C11 C 0.5075(6) 0.22177(16) 0.4626(5) 0.0430(9) Uani 1 1 d . . . C12 C 0.2644(4) -0.05959(12) 0.0392(3) 0.0277(7) Uani 1 1 d . . . C13 C 0.1822(4) -0.09003(12) -0.0403(4) 0.0308(7) Uani 1 1 d . . . C14 C 0.2419(8) -0.19395(19) -0.1128(6) 0.0598(13) Uani 1 1 d . . . C15 C 0.0269(6) -0.12685(17) -0.3363(4) 0.0404(9) Uani 1 1 d . . . C16 C -0.1431(6) -0.15796(17) -0.0784(5) 0.0483(10) Uani 1 1 d . . . O1 O 0.7850(3) 0.00733(8) 0.3703(2) 0.0330(5) Uani 1 1 d . . . O2 O 0.6620(3) -0.06436(8) 0.1484(2) 0.0304(5) Uani 1 1 d . . . S1 S 0.26706(11) 0.02203(3) 0.21467(9) 0.0317(2) Uani 1 1 d . . . Si1 Si 0.53978(13) 0.17089(3) 0.59615(10) 0.0299(2) Uani 1 1 d . . . Si2 Si 0.07419(13) -0.14259(3) -0.14363(10) 0.0322(2) Uani 1 1 d . . . H1A H 0.995(4) -0.0333(10) 0.387(3) 0.017(8) Uiso 1 1 d . . . H1B H 0.832(4) -0.0647(12) 0.409(3) 0.026(8) Uiso 1 1 d . . . H2A H 0.888(4) -0.0279(12) 0.141(3) 0.029(9) Uiso 1 1 d . . . H2B H 0.911(4) -0.0858(13) 0.188(3) 0.032(9) Uiso 1 1 d . . . H16A H -0.238(7) -0.1309(18) -0.082(5) 0.080(15) Uiso 1 1 d . . . H10B H 0.390(6) 0.1502(18) 0.793(5) 0.071(14) Uiso 1 1 d . . . H9B H 0.810(6) 0.1976(16) 0.736(4) 0.057(13) Uiso 1 1 d . . . H15B H 0.130(6) -0.1183(15) -0.368(4) 0.052(12) Uiso 1 1 d . . . H11B H 0.592(6) 0.2193(17) 0.393(5) 0.075(15) Uiso 1 1 d . . . H11A H 0.531(6) 0.2515(17) 0.507(5) 0.065(14) Uiso 1 1 d . . . H14A H 0.261(6) -0.2051(17) -0.023(5) 0.072(15) Uiso 1 1 d . . . H9C H 0.794(5) 0.1448(16) 0.762(5) 0.057(13) Uiso 1 1 d . . . H10A H 0.387(5) 0.2047(17) 0.767(4) 0.055(13) Uiso 1 1 d . . . H15C H -0.026(6) -0.1539(18) -0.390(5) 0.069(14) Uiso 1 1 d . . . H15A H -0.053(6) -0.1004(17) -0.362(4) 0.067(14) Uiso 1 1 d . . . H9A H 0.881(6) 0.1623(16) 0.625(5) 0.070(13) Uiso 1 1 d . . . H14B H 0.369(9) -0.185(2) -0.145(7) 0.12(2) Uiso 1 1 d . . . H16B H -0.138(6) -0.1685(16) 0.017(5) 0.072(15) Uiso 1 1 d . . . H10C H 0.249(7) 0.1714(16) 0.675(5) 0.071(15) Uiso 1 1 d . . . H11C H 0.375(8) 0.218(2) 0.404(6) 0.108(19) Uiso 1 1 d . . . H16C H -0.202(7) -0.1864(19) -0.134(5) 0.088(16) Uiso 1 1 d . . . H14C H 0.194(7) -0.2219(19) -0.167(5) 0.082(16) 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 C1 0.0215(19) 0.035(2) 0.043(2) 0.0013(16) -0.0022(17) 0.0009(14) C2 0.0247(18) 0.033(2) 0.041(2) -0.0047(17) 0.0027(16) 0.0011(14) C3 0.0266(17) 0.0272(17) 0.0263(17) 0.0012(13) 0.0020(14) -0.0040(13) C4 0.0257(17) 0.0261(17) 0.0240(16) 0.0015(13) 0.0053(13) -0.0022(12) C5 0.0257(17) 0.0307(18) 0.0272(17) -0.0045(14) 0.0053(14) -0.0042(13) C6 0.0267(17) 0.0259(17) 0.0258(17) -0.0016(13) 0.0038(14) -0.0017(12) C7 0.0237(17) 0.0345(19) 0.0326(18) -0.0027(15) 0.0051(14) -0.0021(13) C8 0.0252(17) 0.0330(19) 0.041(2) -0.0050(16) 0.0058(15) -0.0023(13) C9 0.043(2) 0.037(2) 0.041(2) -0.001(2) -0.0055(19) -0.0061(18) C10 0.055(3) 0.032(2) 0.054(3) -0.003(2) 0.023(2) 0.0012(19) C11 0.052(3) 0.038(2) 0.039(2) 0.0042(18) 0.006(2) 0.0001(18) C12 0.0238(17) 0.0305(18) 0.0276(17) 0.0028(14) 0.0010(14) -0.0010(13) C13 0.0248(17) 0.0342(19) 0.0331(19) -0.0031(15) 0.0033(14) -0.0006(14) C14 0.079(4) 0.046(3) 0.049(3) -0.009(2) -0.006(3) 0.026(2) C15 0.043(2) 0.042(2) 0.035(2) -0.0033(18) 0.0037(18) -0.0053(19) C16 0.052(3) 0.047(3) 0.047(3) -0.007(2) 0.013(2) -0.020(2) O1 0.0255(12) 0.0349(13) 0.0358(13) -0.0068(10) -0.0030(10) -0.0023(10) O2 0.0249(12) 0.0286(12) 0.0369(13) -0.0085(10) 0.0031(10) 0.0010(9) S1 0.0249(4) 0.0310(5) 0.0384(5) -0.0072(4) 0.0030(4) -0.0007(3) Si1 0.0335(5) 0.0246(5) 0.0317(5) -0.0034(4) 0.0063(4) -0.0015(4) Si2 0.0362(5) 0.0284(5) 0.0304(5) -0.0059(4) 0.0007(4) -0.0014(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 O1 1.450(4) . ? C1 C2 1.494(5) . ? C2 O2 1.447(4) . ? C3 O1 1.363(4) . ? C3 C5 1.379(4) . ? C3 C4 1.413(4) . ? C4 O2 1.354(4) . ? C4 C6 1.369(4) . ? C5 C7 1.419(4) . ? C5 S1 1.735(3) . ? C6 C12 1.417(4) . ? C6 S1 1.736(3) . ? C7 C8 1.203(4) . ? C8 Si1 1.842(3) . ? C9 Si1 1.858(4) . ? C10 Si1 1.850(4) . ? C11 Si1 1.865(4) . ? C12 C13 1.214(4) . ? C13 Si2 1.840(3) . ? C14 Si2 1.860(4) . ? C15 Si2 1.850(4) . ? C16 Si2 1.858(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 110.5(3) . . ? O2 C2 C1 110.8(3) . . ? O1 C3 C5 123.6(3) . . ? O1 C3 C4 123.0(3) . . ? C5 C3 C4 113.4(3) . . ? O2 C4 C6 123.3(3) . . ? O2 C4 C3 123.5(3) . . ? C6 C4 C3 113.2(3) . . ? C3 C5 C7 127.8(3) . . ? C3 C5 S1 110.3(2) . . ? C7 C5 S1 121.8(2) . . ? C4 C6 C12 126.3(3) . . ? C4 C6 S1 110.8(2) . . ? C12 C6 S1 122.9(2) . . ? C8 C7 C5 178.5(4) . . ? C7 C8 Si1 171.9(3) . . ? C13 C12 C6 176.0(3) . . ? C12 C13 Si2 172.0(3) . . ? C3 O1 C1 110.5(2) . . ? C4 O2 C2 111.4(2) . . ? C5 S1 C6 92.20(15) . . ? C8 Si1 C10 110.37(19) . . ? C8 Si1 C9 106.98(18) . . ? C10 Si1 C9 111.2(2) . . ? C8 Si1 C11 106.86(19) . . ? C10 Si1 C11 109.8(2) . . ? C9 Si1 C11 111.5(2) . . ? C13 Si2 C15 109.79(18) . . ? C13 Si2 C16 108.76(18) . . ? C15 Si2 C16 110.2(2) . . ? C13 Si2 C14 106.4(2) . . ? C15 Si2 C14 110.0(2) . . ? C16 Si2 C14 111.5(3) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.322 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.078 ###END data_k01prr31 _database_code_depnum_ccdc_archive 'CCDC 828208' #TrackingRef '- EDOT_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'k01prr31 1M' _chemical_melting_point ? _chemical_formula_moiety 'C46 H74 O2 P4 Pt2 S' _chemical_formula_sum 'C46 H74 O2 P4 Pt2 S' _chemical_formula_weight 1205.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.8940(3) _cell_length_b 9.6610(1) _cell_length_c 33.6030(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.240(1) _cell_angle_gamma 90.00 _cell_volume 10078.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 146156 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4784 _exptl_absorpt_coefficient_mu 5.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.342 _exptl_absorpt_correction_T_max 0.473 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method '850 0.6 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39442 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9063 _reflns_number_gt 7364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DirDif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0545P)^2^+168.1962P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9063 _refine_ls_number_parameters 416 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.006 _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 C1 C 0.6887(4) 0.2284(13) -0.0344(3) 0.067(3) Uani 1 1 d . . . H1A H 0.6634 0.1687 -0.0454 0.081 Uiso 1 1 calc R . . H1B H 0.7092 0.2166 -0.0522 0.081 Uiso 1 1 calc R . . C2 C 0.6748(4) 0.3683(15) -0.0367(4) 0.085(4) Uiso 1 1 d . . . H2A H 0.6600 0.3885 -0.0654 0.102 Uiso 1 1 calc R . . H2B H 0.7005 0.4285 -0.0298 0.102 Uiso 1 1 calc R . . C3 C 0.6944(3) 0.2482(9) 0.0354(3) 0.042(2) Uani 1 1 d . . . C4 C 0.6634(3) 0.3557(9) 0.0279(3) 0.043(2) Uani 1 1 d . . . C5 C 0.7089(3) 0.2158(8) 0.0765(3) 0.0380(19) Uani 1 1 d . . . C6 C 0.6523(3) 0.4043(9) 0.0628(3) 0.041(2) Uani 1 1 d . . . C7 C 0.7413(3) 0.1212(9) 0.0962(3) 0.0402(19) Uani 1 1 d . . . C8 C 0.7671(3) 0.0473(9) 0.1174(3) 0.041(2) Uani 1 1 d . . . C9 C 0.8505(3) -0.1975(11) 0.1977(3) 0.055(3) Uani 1 1 d . . . C10 C 0.8934(4) -0.2135(14) 0.1976(3) 0.074(4) Uani 1 1 d . . . H10 H 0.9052 -0.1640 0.1784 0.089 Uiso 1 1 calc R . . C11 C 0.9204(5) -0.3047(16) 0.2265(5) 0.094(4) Uiso 1 1 d . . . H11 H 0.9501 -0.3151 0.2267 0.113 Uiso 1 1 calc R . . C12 C 0.9023(5) -0.3766(17) 0.2538(4) 0.093(4) Uani 1 1 d . . . H12 H 0.9202 -0.4357 0.2731 0.111 Uiso 1 1 calc R . . C13 C 0.8617(6) -0.3668(16) 0.2543(4) 0.098(5) Uani 1 1 d . . . H13 H 0.8500 -0.4199 0.2729 0.117 Uiso 1 1 calc R . . C14 C 0.8364(4) -0.2779(13) 0.2273(3) 0.071(3) Uani 1 1 d . . . H14 H 0.8070 -0.2698 0.2285 0.085 Uiso 1 1 calc R . . C15 C 0.6228(3) 0.5085(9) 0.0681(3) 0.044(2) Uani 1 1 d . . . C16 C 0.5976(3) 0.5867(9) 0.0778(3) 0.046(2) Uani 1 1 d . . . C17 C 0.5140(3) 0.8570(11) 0.1129(3) 0.055(3) Uani 1 1 d . . . C18 C 0.4725(3) 0.8817(12) 0.0891(4) 0.064(3) Uani 1 1 d . . . H18 H 0.4635 0.8349 0.0637 0.077 Uiso 1 1 calc R . . C19 C 0.4441(3) 0.9726(14) 0.1015(4) 0.077(4) Uani 1 1 d . . . H19 H 0.4157 0.9829 0.0853 0.093 Uiso 1 1 calc R . . C20 C 0.4565(4) 1.0452(17) 0.1358(4) 0.097(5) Uani 1 1 d . . . H20 H 0.4373 1.1085 0.1440 0.116 Uiso 1 1 calc R . . C21 C 0.4971(4) 1.0273(17) 0.1590(4) 0.100(5) Uani 1 1 d . . . H21 H 0.5060 1.0792 0.1835 0.120 Uiso 1 1 calc R . . C22 C 0.5257(3) 0.9359(14) 0.1480(4) 0.084(4) Uani 1 1 d . . . H22 H 0.5539 0.9270 0.1648 0.100 Uiso 1 1 calc R . . C23 C 0.7523(3) -0.2381(10) 0.0679(3) 0.044(2) Uani 1 1 d . . . H23A H 0.7260 -0.2027 0.0754 0.053 Uiso 1 1 calc R . . H23B H 0.7625 -0.1648 0.0518 0.053 Uiso 1 1 calc R . . C24 C 0.7397(3) -0.3622(11) 0.0403(3) 0.056(2) Uani 1 1 d . . . H24A H 0.7175 -0.3350 0.0163 0.084 Uiso 1 1 calc R . . H24B H 0.7284 -0.4350 0.0552 0.084 Uiso 1 1 calc R . . H24C H 0.7650 -0.3969 0.0316 0.084 Uiso 1 1 calc R . . C25 C 0.7737(3) -0.4100(10) 0.1394(3) 0.050(2) Uani 1 1 d . . . H25A H 0.7677 -0.4880 0.1198 0.060 Uiso 1 1 calc R . . H25B H 0.7965 -0.4402 0.1630 0.060 Uiso 1 1 calc R . . C26 C 0.7329(3) -0.3767(12) 0.1540(3) 0.062(3) Uani 1 1 d . . . H26A H 0.7238 -0.4588 0.1670 0.092 Uiso 1 1 calc R . . H26B H 0.7099 -0.3491 0.1306 0.092 Uiso 1 1 calc R . . H26C H 0.7387 -0.3008 0.1739 0.092 Uiso 1 1 calc R . . C27 C 0.8402(3) -0.3306(10) 0.0992(3) 0.044(2) Uani 1 1 d . . . H27A H 0.8607 -0.3684 0.1235 0.053 Uiso 1 1 calc R . . H27B H 0.8311 -0.4076 0.0797 0.053 Uiso 1 1 calc R . . C28 C 0.8632(3) -0.2208(11) 0.0791(3) 0.056(3) Uani 1 1 d . . . H28A H 0.8882 -0.2627 0.0713 0.084 Uiso 1 1 calc R . . H28B H 0.8729 -0.1452 0.0985 0.084 Uiso 1 1 calc R . . H28C H 0.8434 -0.1844 0.0547 0.084 Uiso 1 1 calc R . . C29 C 0.8560(5) 0.0864(17) 0.2485(5) 0.105(5) Uiso 1 1 d . . . H29A H 0.8436 0.0068 0.2604 0.126 Uiso 1 1 calc R . . H29B H 0.8850 0.0575 0.2457 0.126 Uiso 1 1 calc R . . C30 C 0.8625(6) 0.206(2) 0.2808(6) 0.135(7) Uiso 1 1 d . . . H30A H 0.8813 0.1744 0.3064 0.202 Uiso 1 1 calc R . . H30B H 0.8346 0.2335 0.2857 0.202 Uiso 1 1 calc R . . H30C H 0.8758 0.2859 0.2704 0.202 Uiso 1 1 calc R . . C31 C 0.7828(5) 0.2355(17) 0.2001(6) 0.132(6) Uiso 1 1 d D . . H31A H 0.7941 0.3155 0.2177 0.158 Uiso 1 1 calc R . . H31B H 0.7699 0.2694 0.1722 0.158 Uiso 1 1 calc R . . C32 C 0.7495(6) 0.155(2) 0.2176(7) 0.176(9) Uiso 1 1 d D . . H32A H 0.7255 0.2162 0.2193 0.264 Uiso 1 1 calc R . . H32B H 0.7631 0.1209 0.2450 0.264 Uiso 1 1 calc R . . H32C H 0.7387 0.0763 0.1998 0.264 Uiso 1 1 calc R . . C33 C 0.8450(8) 0.261(2) 0.1739(10) 0.234(14) Uiso 1 1 d D . . H33A H 0.8221 0.2908 0.1502 0.281 Uiso 1 1 calc R . . H33B H 0.8509 0.3395 0.1934 0.281 Uiso 1 1 calc R . . C34 C 0.8832(9) 0.232(3) 0.1600(9) 0.220(13) Uiso 1 1 d D . . H34A H 0.8939 0.3169 0.1499 0.330 Uiso 1 1 calc R . . H34B H 0.8767 0.1635 0.1378 0.330 Uiso 1 1 calc R . . H34C H 0.9053 0.1944 0.1827 0.330 Uiso 1 1 calc R . . C35 C 0.5469(5) 0.3801(13) 0.1243(4) 0.088(4) Uani 1 1 d . . . H35A H 0.5269 0.3106 0.1312 0.106 Uiso 1 1 calc R . . H35B H 0.5531 0.3523 0.0979 0.106 Uiso 1 1 calc R . . C36 C 0.5914(6) 0.376(2) 0.1591(5) 0.123(6) Uiso 1 1 d . . . H36A H 0.6037 0.2824 0.1606 0.184 Uiso 1 1 calc R . . H36B H 0.5856 0.4007 0.1856 0.184 Uiso 1 1 calc R . . H36C H 0.6119 0.4419 0.1521 0.184 Uiso 1 1 calc R . . C37 C 0.4670(5) 0.5176(19) 0.0853(6) 0.117(6) Uani 1 1 d . . . H37A H 0.4538 0.4348 0.0947 0.140 Uiso 1 1 calc R . . H37B H 0.4489 0.5985 0.0881 0.140 Uiso 1 1 calc R . . C38 C 0.4676(6) 0.4990(19) 0.0397(5) 0.115(5) Uiso 1 1 d . . . H38A H 0.4381 0.4842 0.0237 0.172 Uiso 1 1 calc R . . H38B H 0.4854 0.4187 0.0367 0.172 Uiso 1 1 calc R . . H38C H 0.4795 0.5822 0.0298 0.172 Uiso 1 1 calc R . . C39 C 0.5087(6) 0.577(2) 0.1687(6) 0.127(6) Uiso 1 1 d . . . H39A H 0.5349 0.6144 0.1873 0.152 Uiso 1 1 calc R . . H39B H 0.4859 0.6485 0.1655 0.152 Uiso 1 1 calc R . . C40 C 0.4944(9) 0.452(3) 0.1874(8) 0.196(11) Uiso 1 1 d . . . H40A H 0.4876 0.4771 0.2135 0.293 Uiso 1 1 calc R . . H40B H 0.5175 0.3830 0.1922 0.293 Uiso 1 1 calc R . . H40C H 0.4688 0.4136 0.1690 0.293 Uiso 1 1 calc R . . C41 C 0.6004(5) 0.8542(13) 0.0165(4) 0.088(4) Uani 1 1 d . . . H41A H 0.6113 0.7585 0.0157 0.106 Uiso 1 1 calc R . . H41B H 0.5724 0.8606 -0.0036 0.106 Uiso 1 1 calc R . . C42 C 0.6311(8) 0.952(3) 0.0050(8) 0.182(10) Uiso 1 1 d . . . H42A H 0.6345 0.9296 -0.0225 0.273 Uiso 1 1 calc R . . H42B H 0.6590 0.9437 0.0245 0.273 Uiso 1 1 calc R . . H42C H 0.6202 1.0462 0.0055 0.273 Uiso 1 1 calc R . . C43 C 0.6484(5) 0.8980(17) 0.0971(4) 0.094(4) Uiso 1 1 d . . . H43A H 0.6613 0.8049 0.0967 0.113 Uiso 1 1 calc R . . H43B H 0.6643 0.9633 0.0832 0.113 Uiso 1 1 calc R . . C44 C 0.6519(4) 0.9482(17) 0.1448(5) 0.102(5) Uani 1 1 d . . . H44A H 0.6823 0.9514 0.1593 0.153 Uiso 1 1 calc R . . H44B H 0.6365 0.8824 0.1584 0.153 Uiso 1 1 calc R . . H44C H 0.6392 1.0404 0.1448 0.153 Uiso 1 1 calc R . . C45 C 0.5748(5) 1.0682(13) 0.0677(5) 0.099(4) Uiso 1 1 d D . . H45A H 0.5644 1.0888 0.0926 0.119 Uiso 1 1 calc R . . H45B H 0.6004 1.1271 0.0686 0.119 Uiso 1 1 calc R . . C46 C 0.5418(7) 1.111(3) 0.0330(7) 0.192(10) Uiso 1 1 d D . . H46A H 0.5348 1.2088 0.0361 0.288 Uiso 1 1 calc R . . H46B H 0.5160 1.0546 0.0313 0.288 Uiso 1 1 calc R . . H46C H 0.5523 1.0998 0.0079 0.288 Uiso 1 1 calc R . . O1 O 0.7083(2) 0.1823(7) 0.00492(19) 0.0517(16) Uani 1 1 d . . . O2 O 0.6461(2) 0.4052(7) -0.0104(2) 0.0552(17) Uani 1 1 d . . . P1 P 0.79345(7) -0.2636(2) 0.11488(6) 0.0361(5) Uani 1 1 d . . . P2 P 0.82452(10) 0.1124(3) 0.19930(9) 0.0715(9) Uani 1 1 d D . . P3 P 0.52056(10) 0.5429(4) 0.11784(9) 0.0673(8) Uani 1 1 d . . . P4 P 0.59203(8) 0.8936(3) 0.07069(10) 0.0622(8) Uani 1 1 d D . . Pt1 Pt 0.809054(10) -0.07406(4) 0.156555(9) 0.03656(11) Uani 1 1 d . . . Pt2 Pt 0.555962(10) 0.72043(4) 0.095121(11) 0.04143(12) Uani 1 1 d . . . S1 S 0.68256(7) 0.3184(2) 0.10534(7) 0.0434(5) Uani 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 C1 0.050(6) 0.085(8) 0.058(6) -0.001(6) -0.003(5) 0.025(6) C3 0.028(4) 0.032(4) 0.058(6) -0.003(4) -0.003(4) 0.002(3) C4 0.039(5) 0.031(4) 0.054(5) 0.010(4) 0.001(4) 0.008(4) C5 0.030(4) 0.031(4) 0.050(5) -0.001(4) 0.001(3) 0.001(3) C6 0.024(4) 0.033(5) 0.063(6) 0.012(4) 0.003(4) 0.008(3) C7 0.038(5) 0.032(4) 0.047(5) 0.004(4) 0.003(4) 0.001(4) C8 0.027(4) 0.042(5) 0.050(5) 0.000(4) 0.002(4) 0.005(4) C9 0.064(7) 0.059(6) 0.035(5) 0.002(4) -0.005(4) 0.027(5) C10 0.059(7) 0.115(10) 0.042(5) 0.003(6) -0.003(5) 0.040(7) C12 0.083(10) 0.112(12) 0.068(8) 0.013(8) -0.015(7) 0.003(9) C13 0.123(13) 0.099(11) 0.056(7) 0.021(7) -0.010(8) -0.008(10) C14 0.082(8) 0.084(8) 0.040(6) 0.014(6) 0.000(5) 0.011(7) C15 0.030(5) 0.037(5) 0.065(6) 0.008(4) 0.008(4) 0.004(4) C16 0.042(5) 0.042(5) 0.052(5) 0.009(4) 0.007(4) -0.001(4) C17 0.026(5) 0.065(7) 0.074(7) -0.020(5) 0.012(4) 0.000(4) C18 0.027(5) 0.079(8) 0.085(8) -0.013(6) 0.009(5) 0.003(5) C19 0.026(5) 0.101(10) 0.097(9) -0.022(8) -0.001(5) 0.014(6) C20 0.048(7) 0.132(13) 0.108(11) -0.047(10) 0.011(7) 0.024(8) C21 0.056(8) 0.139(13) 0.095(10) -0.061(10) -0.003(6) 0.032(8) C22 0.037(6) 0.112(11) 0.092(9) -0.057(8) -0.005(5) 0.010(6) C23 0.032(5) 0.057(6) 0.041(5) 0.001(4) 0.006(4) 0.006(4) C24 0.052(6) 0.065(7) 0.047(5) -0.004(5) 0.005(4) -0.010(5) C25 0.055(6) 0.047(5) 0.046(5) 0.005(4) 0.008(4) 0.000(4) C26 0.067(7) 0.074(7) 0.049(6) 0.003(5) 0.024(5) -0.009(6) C27 0.031(5) 0.046(5) 0.056(5) 0.001(4) 0.010(4) 0.009(4) C28 0.040(5) 0.065(7) 0.066(6) -0.003(5) 0.020(4) 0.004(5) C35 0.139(12) 0.064(8) 0.067(8) -0.008(6) 0.035(8) -0.049(8) C37 0.081(10) 0.110(13) 0.164(16) -0.035(12) 0.037(10) -0.043(9) C41 0.149(13) 0.055(7) 0.072(8) -0.005(6) 0.050(8) -0.007(8) C44 0.058(8) 0.110(12) 0.121(12) 0.004(10) -0.016(7) -0.011(8) O1 0.054(4) 0.041(4) 0.054(4) -0.005(3) -0.001(3) 0.011(3) O2 0.052(4) 0.049(4) 0.060(4) 0.012(3) 0.003(3) 0.017(3) P1 0.0315(11) 0.0382(12) 0.0374(11) 0.0026(9) 0.0055(8) 0.0061(9) P2 0.0677(19) 0.0664(19) 0.0667(18) -0.0242(15) -0.0131(14) 0.0257(15) P3 0.0681(19) 0.078(2) 0.0578(16) -0.0083(15) 0.0180(14) -0.0379(16) P4 0.0405(14) 0.0494(15) 0.089(2) 0.0241(14) -0.0002(13) -0.0012(12) Pt1 0.02895(18) 0.04093(19) 0.03694(18) 0.00247(14) 0.00164(12) 0.00966(13) Pt2 0.02648(18) 0.0422(2) 0.0554(2) -0.00267(16) 0.00891(14) 0.00066(14) S1 0.0321(11) 0.0389(12) 0.0569(13) 0.0070(10) 0.0056(9) 0.0060(9) _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 O1 1.399(12) . ? C1 C2 1.419(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.455(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.364(11) . ? C3 C5 1.387(12) . ? C3 C4 1.415(11) . ? C4 O2 1.367(10) . ? C4 C6 1.380(13) . ? C5 C7 1.424(11) . ? C5 S1 1.732(9) . ? C6 C15 1.418(12) . ? C6 S1 1.742(8) . ? C7 C8 1.194(11) . ? C8 Pt1 2.023(8) . ? C9 C10 1.378(15) . ? C9 C14 1.412(15) . ? C9 Pt1 2.061(9) . ? C10 C11 1.442(18) . ? C10 H10 0.9500 . ? C11 C12 1.378(19) . ? C11 H11 0.9500 . ? C12 C13 1.301(19) . ? C12 H12 0.9500 . ? C13 C14 1.370(17) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.201(12) . ? C16 Pt2 2.032(10) . ? C17 C22 1.382(14) . ? C17 C18 1.402(13) . ? C17 Pt2 2.062(9) . ? C18 C19 1.392(15) . ? C18 H18 0.9500 . ? C19 C20 1.331(17) . ? C19 H19 0.9500 . ? C20 C21 1.362(17) . ? C20 H20 0.9500 . ? C21 C22 1.379(16) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.511(13) . ? C23 P1 1.825(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.528(14) . ? C25 P1 1.820(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.533(13) . ? C27 P1 1.810(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.57(2) . ? C29 P2 1.746(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.540(16) . ? C31 P2 1.789(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.431(17) . ? C33 P2 1.864(17) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.62(2) . ? C35 P3 1.773(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.55(2) . ? C37 P3 1.821(15) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.48(3) . ? C39 P3 1.861(18) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.47(3) . ? C41 P4 1.939(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.65(2) . ? C43 P4 1.814(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.442(16) . ? C45 P4 1.770(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? P1 Pt1 2.289(2) . ? P2 Pt1 2.286(3) . ? P3 Pt2 2.279(3) . ? P4 Pt2 2.287(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 O1 C1 C2 115.0(10) . . ? O1 C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? O1 C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 O2 115.6(11) . . ? C1 C2 H2A 108.4 . . ? O2 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? O2 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? O1 C3 C5 123.4(7) . . ? O1 C3 C4 122.9(8) . . ? C5 C3 C4 113.7(8) . . ? O2 C4 C6 123.6(7) . . ? O2 C4 C3 122.6(8) . . ? C6 C4 C3 113.8(8) . . ? C3 C5 C7 130.4(8) . . ? C3 C5 S1 109.5(6) . . ? C7 C5 S1 120.0(7) . . ? C4 C6 C15 131.0(8) . . ? C4 C6 S1 109.5(6) . . ? C15 C6 S1 119.5(7) . . ? C8 C7 C5 171.4(10) . . ? C7 C8 Pt1 176.1(8) . . ? C10 C9 C14 114.6(9) . . ? C10 C9 Pt1 123.2(8) . . ? C14 C9 Pt1 122.2(8) . . ? C9 C10 C11 120.4(12) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 118.7(14) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C13 C12 C11 122.7(14) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 118.3(15) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C9 125.2(13) . . ? C13 C14 H14 117.4 . . ? C9 C14 H14 117.4 . . ? C16 C15 C6 170.5(10) . . ? C15 C16 Pt2 178.9(9) . . ? C22 C17 C18 115.3(9) . . ? C22 C17 Pt2 122.3(7) . . ? C18 C17 Pt2 122.3(8) . . ? C19 C18 C17 122.1(10) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C20 C19 C18 120.5(10) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.0(11) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C20 C21 C22 121.8(12) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C17 121.2(10) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? C24 C23 P1 117.5(7) . . ? C24 C23 H23A 107.9 . . ? P1 C23 H23A 107.9 . . ? C24 C23 H23B 107.9 . . ? P1 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? 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 P1 113.0(7) . . ? C26 C25 H25A 109.0 . . ? P1 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? P1 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 P1 113.0(6) . . ? C28 C27 H27A 109.0 . . ? P1 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? P1 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P2 120.3(12) . . ? C30 C29 H29A 107.2 . . ? P2 C29 H29A 107.2 . . ? C30 C29 H29B 107.2 . . ? P2 C29 H29B 107.2 . . ? H29A C29 H29B 106.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 P2 104.5(11) . . ? C32 C31 H31A 110.9 . . ? P2 C31 H31A 110.9 . . ? C32 C31 H31B 110.9 . . ? P2 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 P2 114(2) . . ? C34 C33 H33A 108.7 . . ? P2 C33 H33A 108.7 . . ? C34 C33 H33B 108.7 . . ? P2 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 P3 115.0(10) . . ? C36 C35 H35A 108.5 . . ? P3 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? P3 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 P3 113.0(11) . . ? C38 C37 H37A 109.0 . . ? P3 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? P3 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 P3 113.2(16) . . ? C40 C39 H39A 108.9 . . ? P3 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? P3 C39 H39B 108.9 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 P4 111.3(13) . . ? C42 C41 H41A 109.4 . . ? P4 C41 H41A 109.4 . . ? C42 C41 H41B 109.4 . . ? P4 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 P4 108.7(9) . . ? C44 C43 H43A 109.9 . . ? P4 C43 H43A 109.9 . . ? C44 C43 H43B 109.9 . . ? P4 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 P4 118.7(15) . . ? C46 C45 H45A 107.6 . . ? P4 C45 H45A 107.6 . . ? C46 C45 H45B 107.6 . . ? P4 C45 H45B 107.6 . . ? H45A C45 H45B 107.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C3 O1 C1 114.1(7) . . ? C4 O2 C2 108.2(8) . . ? C27 P1 C25 104.3(4) . . ? C27 P1 C23 105.9(4) . . ? C25 P1 C23 104.0(4) . . ? C27 P1 Pt1 112.7(3) . . ? C25 P1 Pt1 113.2(3) . . ? C23 P1 Pt1 115.8(3) . . ? C29 P2 C31 110.5(9) . . ? C29 P2 C33 111.0(12) . . ? C31 P2 C33 80.4(8) . . ? C29 P2 Pt1 118.4(6) . . ? C31 P2 Pt1 118.6(7) . . ? C33 P2 Pt1 111.6(10) . . ? C35 P3 C37 107.9(7) . . ? C35 P3 C39 103.6(8) . . ? C37 P3 C39 102.4(8) . . ? C35 P3 Pt2 116.8(4) . . ? C37 P3 Pt2 111.6(6) . . ? C39 P3 Pt2 113.2(6) . . ? C45 P4 C43 105.4(7) . . ? C45 P4 C41 104.0(7) . . ? C43 P4 C41 97.4(7) . . ? C45 P4 Pt2 122.9(6) . . ? C43 P4 Pt2 111.4(5) . . ? C41 P4 Pt2 112.5(4) . . ? C8 Pt1 C9 178.1(4) . . ? C8 Pt1 P2 88.1(3) . . ? C9 Pt1 P2 91.2(3) . . ? C8 Pt1 P1 92.7(3) . . ? C9 Pt1 P1 87.9(3) . . ? P2 Pt1 P1 178.82(11) . . ? C16 Pt2 C17 179.6(4) . . ? C16 Pt2 P3 91.4(3) . . ? C17 Pt2 P3 88.9(3) . . ? C16 Pt2 P4 86.9(3) . . ? C17 Pt2 P4 92.8(3) . . ? P3 Pt2 P4 178.04(12) . . ? C5 S1 C6 93.5(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.995 _refine_diff_density_min -1.496 _refine_diff_density_rms 0.163 ###END data_bath99 _database_code_depnum_ccdc_archive 'CCDC 828209' #TrackingRef '- EDOT_all.cif' _audit_creation_date 2011-04-27T20:17:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H78 O4 P4 Pt2 S2' _chemical_formula_sum 'C52 H78 O4 P4 Pt2 S2' _chemical_formula_weight 1345.32 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.980(4) _cell_length_b 13.4875(13) _cell_length_c 9.8161(9) _cell_angle_alpha 90 _cell_angle_beta 101.078(1) _cell_angle_gamma 90 _cell_volume 5584.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8618 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.9 _cell_measurement_wavelength 0.6775 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Needle _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.6 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS v2.1 (Bruker, 2003)' _exptl_absorpt_correction_T_min 0.4701 _exptl_absorpt_correction_T_max 0.8083 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source synchrotron _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6775 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator 'silicon 111' _diffrn_detector APEXII _diffrn_measurement_device 'Burker APEX II Diffractometer' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_unetI/netI 0.0607 _diffrn_reflns_number 31903 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.95 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 8384 _reflns_number_gt 7251 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process "'Bruker APEX2 software'" #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'DIRDIF (Buerskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8384 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.267 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.137 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0027 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0097 0.0055 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0946 0.0859 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1156 0.1126 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.275 7.788 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.15158(7) 0.2546(2) 1.0091(3) 0.0220(5) Uani 1 1 d . . . C2 C 0.17103(7) 0.27189(19) 1.1109(3) 0.0222(5) Uani 1 1 d . . . C3 C 0.19396(6) 0.2889(2) 1.2333(3) 0.0207(5) Uani 1 1 d . . . C4 C 0.19984(6) 0.37289(19) 1.3128(3) 0.0194(5) Uani 1 1 d . A . C5 C 0.22425(6) 0.3610(2) 1.4313(3) 0.0200(5) Uani 1 1 d . A . C6 C 0.23738(6) 0.26806(18) 1.4462(3) 0.0186(5) Uani 1 1 d . . . C7 C 0.18834(13) 0.5299(3) 1.3971(5) 0.0296(14) Uani 0.713(12) 1 d P A 1 H7A H 0.1755 0.5101 1.4664 0.035 Uiso 0.713(12) 1 calc PR A 1 H7B H 0.1814 0.5968 1.3626 0.035 Uiso 0.713(12) 1 calc PR A 1 C8 C 0.22292(16) 0.5322(4) 1.4642(7) 0.0315(13) Uani 0.713(12) 1 d P A 1 H8A H 0.2355 0.5519 1.3943 0.038 Uiso 0.713(12) 1 calc PR A 1 H8B H 0.2263 0.5826 1.5389 0.038 Uiso 0.713(12) 1 calc PR A 1 C7' C 0.2020(3) 0.5431(6) 1.3476(12) 0.021(3) Uani 0.287(12) 1 d P A 2 H7'1 H 0.189 0.6043 1.3368 0.025 Uiso 0.287(12) 1 calc PR A 2 H7'2 H 0.2206 0.5538 1.3035 0.025 Uiso 0.287(12) 1 calc PR A 2 C8' C 0.2129(4) 0.5186(10) 1.5022(15) 0.026(3) Uani 0.287(12) 1 d P A 2 H8'1 H 0.2236 0.5773 1.5509 0.031 Uiso 0.287(12) 1 calc PR A 2 H8'2 H 0.1942 0.5031 1.5433 0.031 Uiso 0.287(12) 1 calc PR A 2 C9 C 0.07872(6) 0.2014(2) 0.6805(3) 0.0260(6) Uani 1 1 d . . . C10 C 0.07026(8) 0.2661(3) 0.5672(4) 0.0376(8) Uani 1 1 d . . . H10 H 0.0821 0.3251 0.5632 0.045 Uiso 1 1 calc R . . C11 C 0.04469(10) 0.2447(4) 0.4607(4) 0.0539(11) Uani 1 1 d . . . H11 H 0.0395 0.2892 0.3847 0.065 Uiso 1 1 calc R . . C12 C 0.02669(9) 0.1604(4) 0.4633(5) 0.0646(14) Uani 1 1 d . . . H12 H 0.0092 0.1468 0.3904 0.078 Uiso 1 1 calc R . . C13 C 0.03446(9) 0.0966(4) 0.5729(5) 0.0613(12) Uani 1 1 d . . . H13 H 0.0223 0.0381 0.5762 0.074 Uiso 1 1 calc R . . C14 C 0.06015(8) 0.1166(3) 0.6802(4) 0.0424(8) Uani 1 1 d . . . H14 H 0.0651 0.0711 0.7552 0.051 Uiso 1 1 calc R . . C15 C 0.04220(7) 0.3288(3) 0.8790(4) 0.0391(8) Uani 1 1 d . . . H15A H 0.0412 0.3539 0.7835 0.047 Uiso 1 1 calc R . . H15B H 0.0323 0.2622 0.8715 0.047 Uiso 1 1 calc R . . C16 C 0.02252(8) 0.3969(3) 0.9525(5) 0.0540(11) Uani 1 1 d . . . H16A H 0.0221 0.3707 1.0452 0.081 Uiso 1 1 calc R . . H16B H 0.0008 0.4006 0.8987 0.081 Uiso 1 1 calc R . . H16C H 0.0319 0.4633 0.9608 0.081 Uiso 1 1 calc R . . C17 C 0.09795(7) 0.4430(2) 0.9933(3) 0.0268(6) Uani 1 1 d . . . H17A H 0.0842 0.4782 1.0475 0.032 Uiso 1 1 calc R . . H17B H 0.1198 0.4423 1.0489 0.032 Uiso 1 1 calc R . . C18 C 0.09777(9) 0.4986(3) 0.8571(4) 0.0389(7) Uani 1 1 d . . . H18A H 0.1127 0.4669 0.8067 0.058 Uiso 1 1 calc R . . H18B H 0.1041 0.5676 0.8774 0.058 Uiso 1 1 calc R . . H18C H 0.0764 0.4968 0.8001 0.058 Uiso 1 1 calc R . . C19 C 0.08306(8) 0.2663(2) 1.1344(4) 0.0310(7) Uani 1 1 d . . . H19A H 0.1049 0.2642 1.1893 0.037 Uiso 1 1 calc R . . H19B H 0.0704 0.3112 1.1823 0.037 Uiso 1 1 calc R . . C20 C 0.06869(9) 0.1620(3) 1.1274(5) 0.0469(9) Uani 1 1 d . . . H20A H 0.0465 0.1648 1.0798 0.07 Uiso 1 1 calc R . . H20B H 0.0699 0.1365 1.2217 0.07 Uiso 1 1 calc R . . H20C H 0.0805 0.118 1.0763 0.07 Uiso 1 1 calc R . . C21 C 0.14870(7) 0.2176(2) 0.5516(3) 0.0254(6) Uani 1 1 d . . . H21A H 0.1644 0.1858 0.5039 0.03 Uiso 1 1 calc R . . H21B H 0.1275 0.2102 0.4915 0.03 Uiso 1 1 calc R . . C22 C 0.15643(8) 0.3276(2) 0.5695(4) 0.0364(7) Uani 1 1 d . . . H22A H 0.1412 0.3596 0.6179 0.055 Uiso 1 1 calc R . . H22B H 0.1552 0.3583 0.4781 0.055 Uiso 1 1 calc R . . H22C H 0.1779 0.3357 0.624 0.055 Uiso 1 1 calc R . . C23 C 0.13804(7) 0.0269(2) 0.6604(3) 0.0259(6) Uani 1 1 d . . . H23A H 0.1162 0.0263 0.6051 0.031 Uiso 1 1 calc R . . H23B H 0.1525 0.0029 0.6 0.031 Uiso 1 1 calc R . . C24 C 0.13988(8) -0.0431(2) 0.7832(3) 0.0353(7) Uani 1 1 d . . . H24A H 0.1609 -0.0385 0.8426 0.053 Uiso 1 1 calc R . . H24B H 0.1361 -0.1113 0.7494 0.053 Uiso 1 1 calc R . . H24C H 0.1237 -0.0247 0.8368 0.053 Uiso 1 1 calc R . . C25 C 0.19079(7) 0.1455(3) 0.7980(3) 0.0323(7) Uani 1 1 d . . . H25A H 0.1992 0.2137 0.8143 0.039 Uiso 1 1 calc R . . H25B H 0.1923 0.1134 0.8897 0.039 Uiso 1 1 calc R . . C26 C 0.21174(7) 0.0884(3) 0.7156(4) 0.0379(8) Uani 1 1 d . . . H26A H 0.2337 0.0882 0.7672 0.057 Uiso 1 1 calc R . . H26B H 0.2109 0.1204 0.6253 0.057 Uiso 1 1 calc R . . H26C H 0.2041 0.02 0.7015 0.057 Uiso 1 1 calc R . . O1 O 0.18321(5) 0.45960(15) 1.2819(2) 0.0265(4) Uani 1 1 d . . . O2 O 0.23402(5) 0.43720(15) 1.5222(2) 0.0276(4) Uani 1 1 d . . . P1 P 0.083927(16) 0.31542(6) 0.96151(7) 0.02276(14) Uani 1 1 d . . . P2 P 0.148818(16) 0.15340(5) 0.71485(7) 0.02025(13) Uani 1 1 d . . . S1 S 0.219456(15) 0.19394(5) 1.30780(7) 0.02164(13) Uani 1 1 d . . . Pt1 Pt 0.116162(2) 0.229165(7) 0.842724(9) 0.01790(4) Uani 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 C1 0.0227(13) 0.0221(12) 0.0195(12) 0.0025(10) -0.0004(10) 0.0013(10) C2 0.0249(13) 0.0191(12) 0.0226(13) 0.0003(10) 0.0048(10) 0.0013(10) C3 0.0200(12) 0.0200(12) 0.0214(13) 0.0000(10) 0.0021(10) 0.0013(9) C4 0.0184(11) 0.0174(11) 0.0213(12) -0.0002(9) 0.0010(9) 0.0002(9) C5 0.0170(11) 0.0226(12) 0.0194(11) -0.0024(10) 0.0008(9) 0.0010(10) C6 0.0172(11) 0.0207(13) 0.0161(11) -0.0039(9) -0.0017(9) -0.0020(9) C7 0.035(3) 0.0208(19) 0.031(2) -0.0052(17) 0.001(2) 0.0079(18) C8 0.039(3) 0.016(2) 0.034(3) -0.004(2) -0.006(2) 0.001(2) C7' 0.019(5) 0.011(4) 0.031(6) 0.001(4) 0.000(4) 0.000(3) C8' 0.037(7) 0.017(5) 0.025(6) 0.001(4) 0.009(5) 0.002(5) C9 0.0182(12) 0.0323(14) 0.0249(14) -0.0115(12) -0.0024(10) 0.0012(11) C10 0.0257(15) 0.062(2) 0.0247(15) 0.0008(15) 0.0025(12) 0.0065(14) C11 0.0301(18) 0.104(3) 0.0239(17) 0.001(2) -0.0049(14) 0.016(2) C12 0.0257(17) 0.116(4) 0.044(2) -0.028(3) -0.0116(15) -0.004(2) C13 0.037(2) 0.065(3) 0.075(3) -0.030(3) -0.0074(19) -0.016(2) C14 0.0287(16) 0.0402(19) 0.053(2) -0.0121(17) -0.0067(14) -0.0055(14) C15 0.0255(14) 0.047(2) 0.0425(19) -0.0158(16) 0.0024(13) 0.0069(14) C16 0.0277(17) 0.068(3) 0.067(3) -0.024(2) 0.0110(17) 0.0122(17) C17 0.0321(14) 0.0233(13) 0.0245(13) -0.0007(11) 0.0046(11) 0.0035(11) C18 0.055(2) 0.0298(16) 0.0317(17) 0.0040(13) 0.0075(15) 0.0053(15) C19 0.0379(17) 0.0279(15) 0.0310(16) -0.0001(12) 0.0159(13) 0.0009(12) C20 0.0428(19) 0.0327(18) 0.070(3) 0.0068(18) 0.0223(19) -0.0021(15) C21 0.0288(14) 0.0270(14) 0.0216(13) 0.0016(10) 0.0078(11) 0.0014(11) C22 0.0447(18) 0.0268(15) 0.0421(19) 0.0049(14) 0.0194(15) -0.0009(13) C23 0.0381(15) 0.0230(13) 0.0175(12) -0.0013(11) 0.0078(11) 0.0016(12) C24 0.0497(19) 0.0243(14) 0.0323(16) 0.0071(13) 0.0086(14) 0.0056(13) C25 0.0223(13) 0.0444(18) 0.0290(15) -0.0005(13) 0.0015(11) 0.0057(13) C26 0.0259(14) 0.049(2) 0.0414(18) 0.0120(16) 0.0132(13) 0.0127(14) O1 0.0288(10) 0.0213(10) 0.0252(10) -0.0005(8) -0.0054(8) 0.0062(8) O2 0.0315(10) 0.0198(9) 0.0261(10) -0.0072(8) -0.0079(8) 0.0041(8) P1 0.0221(3) 0.0236(3) 0.0223(3) -0.0046(3) 0.0036(2) 0.0029(3) P2 0.0207(3) 0.0212(3) 0.0182(3) -0.0020(3) 0.0023(2) 0.0030(3) S1 0.0223(3) 0.0195(3) 0.0204(3) -0.0031(3) -0.0027(2) 0.0019(2) Pt1 0.01711(6) 0.01939(6) 0.01610(6) -0.00316(3) 0.00049(4) 0.00072(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 1.195(4) . ? C1 Pt1 2.037(3) . ? C2 C3 1.419(4) . ? C3 C4 1.371(4) . ? C3 S1 1.752(3) . ? C4 O1 1.374(3) . ? C4 C5 1.418(4) . ? C5 C6 1.371(4) . ? C5 O2 1.373(3) . ? C6 C6 1.446(5) 7_558 ? C6 S1 1.742(3) . ? C7 O1 1.459(5) . ? C7 C8 1.506(9) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O2 1.445(6) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C7' O1 1.461(9) . ? C7' C8' 1.536(19) . ? C7' H7'1 0.99 . ? C7' H7'2 0.99 . ? C8' O2 1.413(13) . ? C8' H8'1 0.99 . ? C8' H8'2 0.99 . ? C9 C14 1.394(5) . ? C9 C10 1.405(5) . ? C9 Pt1 2.069(3) . ? C10 C11 1.394(5) . ? C10 H10 0.95 . ? C11 C12 1.378(7) . ? C11 H11 0.95 . ? C12 C13 1.368(7) . ? C12 H12 0.95 . ? C13 C14 1.398(5) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.521(5) . ? C15 P1 1.829(3) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.532(4) . ? C17 P1 1.830(3) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.533(5) . ? C19 P1 1.828(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.522(4) . ? C21 P2 1.820(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.522(4) . ? C23 P2 1.821(3) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.529(4) . ? C25 P2 1.834(3) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? P1 Pt1 2.2920(7) . ? P2 Pt1 2.2950(7) . ? 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 C2 C1 Pt1 176.0(3) . . ? C1 C2 C3 177.9(3) . . ? C4 C3 C2 129.6(3) . . ? C4 C3 S1 109.5(2) . . ? C2 C3 S1 120.8(2) . . ? C3 C4 O1 123.1(2) . . ? C3 C4 C5 113.6(2) . . ? O1 C4 C5 123.3(2) . . ? C6 C5 O2 123.2(2) . . ? C6 C5 C4 114.5(2) . . ? O2 C5 C4 122.3(2) . . ? C5 C6 C6 128.4(3) . 7_558 ? C5 C6 S1 109.30(19) . . ? C6 C6 S1 122.3(3) 7_558 . ? O1 C7 C8 110.0(5) . . ? O1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O2 C8 C7 112.2(5) . . ? O2 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? O2 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O1 C7' C8' 107.9(10) . . ? O1 C7' H7'1 110.1 . . ? C8' C7' H7'1 110.1 . . ? O1 C7' H7'2 110.1 . . ? C8' C7' H7'2 110.1 . . ? H7'1 C7' H7'2 108.4 . . ? O2 C8' C7' 111.7(10) . . ? O2 C8' H8'1 109.3 . . ? C7' C8' H8'1 109.3 . . ? O2 C8' H8'2 109.3 . . ? C7' C8' H8'2 109.3 . . ? H8'1 C8' H8'2 107.9 . . ? C14 C9 C10 116.6(3) . . ? C14 C9 Pt1 120.7(2) . . ? C10 C9 Pt1 122.8(3) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 118.7(3) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 120.6(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 121.9(4) . . ? C9 C14 H14 119 . . ? C13 C14 H14 119 . . ? C16 C15 P1 115.9(3) . . ? C16 C15 H15A 108.3 . . ? P1 C15 H15A 108.3 . . ? C16 C15 H15B 108.3 . . ? P1 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P1 111.4(2) . . ? C18 C17 H17A 109.3 . . ? P1 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? P1 C17 H17B 109.3 . . ? H17A C17 H17B 108 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P1 111.8(3) . . ? C20 C19 H19A 109.3 . . ? P1 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? P1 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P2 113.5(2) . . ? C22 C21 H21A 108.9 . . ? P2 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? P2 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P2 112.1(2) . . ? C24 C23 H23A 109.2 . . ? P2 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? P2 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? 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 P2 115.0(2) . . ? C26 C25 H25A 108.5 . . ? P2 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? P2 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C4 O1 C7 112.8(2) . . ? C4 O1 C7' 109.8(4) . . ? C7 O1 C7' 33.8(4) . . ? C5 O2 C8' 112.6(6) . . ? C5 O2 C8 111.8(3) . . ? C8' O2 C8 26.1(5) . . ? C19 P1 C15 104.68(17) . . ? C19 P1 C17 104.31(14) . . ? C15 P1 C17 104.23(15) . . ? C19 P1 Pt1 114.22(11) . . ? C15 P1 Pt1 117.51(11) . . ? C17 P1 Pt1 110.64(10) . . ? C21 P2 C23 103.29(13) . . ? C21 P2 C25 104.80(15) . . ? C23 P2 C25 104.44(15) . . ? C21 P2 Pt1 111.76(10) . . ? C23 P2 Pt1 115.47(10) . . ? C25 P2 Pt1 115.77(11) . . ? C6 S1 C3 93.05(13) . . ? C1 Pt1 C9 177.13(11) . . ? C1 Pt1 P1 86.46(9) . . ? C9 Pt1 P1 91.52(8) . . ? C1 Pt1 P2 94.14(9) . . ? C9 Pt1 P2 88.02(8) . . ? P1 Pt1 P2 175.75(3) . . ? 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 Pt1 C1 C2 C3 93(10) . . . . ? C1 C2 C3 C4 -142(9) . . . . ? C1 C2 C3 S1 36(9) . . . . ? C2 C3 C4 O1 -0.7(5) . . . . ? S1 C3 C4 O1 -179.0(2) . . . . ? C2 C3 C4 C5 178.1(3) . . . . ? S1 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? O1 C4 C5 C6 178.2(2) . . . . ? C3 C4 C5 O2 178.7(2) . . . . ? O1 C4 C5 O2 -2.6(4) . . . . ? O2 C5 C6 C6 0.3(5) . . . 7_558 ? C4 C5 C6 C6 179.5(3) . . . 7_558 ? O2 C5 C6 S1 -178.2(2) . . . . ? C4 C5 C6 S1 1.1(3) . . . . ? O1 C7 C8 O2 -61.9(8) . . . . ? O1 C7' C8' O2 65.5(15) . . . . ? C14 C9 C10 C11 -0.5(5) . . . . ? Pt1 C9 C10 C11 -179.5(3) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C13 -0.4(7) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C10 C9 C14 C13 0.1(5) . . . . ? Pt1 C9 C14 C13 179.2(3) . . . . ? C12 C13 C14 C9 0.1(6) . . . . ? C3 C4 O1 C7 166.2(4) . . . . ? C5 C4 O1 C7 -12.5(4) . . . . ? C3 C4 O1 C7' -157.6(6) . . . . ? C5 C4 O1 C7' 23.8(7) . . . . ? C8 C7 O1 C4 42.4(6) . . . . ? C8 C7 O1 C7' -49.5(8) . . . . ? C8' C7' O1 C4 -51.8(11) . . . . ? C8' C7' O1 C7 49.8(10) . . . . ? C6 C5 O2 C8' -167.7(7) . . . . ? C4 C5 O2 C8' 13.2(8) . . . . ? C6 C5 O2 C8 164.1(4) . . . . ? C4 C5 O2 C8 -15.1(5) . . . . ? C7' C8' O2 C5 -43.7(14) . . . . ? C7' C8' O2 C8 50.1(13) . . . . ? C7 C8 O2 C5 46.4(7) . . . . ? C7 C8 O2 C8' -50.6(15) . . . . ? C20 C19 P1 C15 65.3(3) . . . . ? C20 C19 P1 C17 174.5(2) . . . . ? C20 C19 P1 Pt1 -64.6(3) . . . . ? C16 C15 P1 C19 59.4(4) . . . . ? C16 C15 P1 C17 -49.9(4) . . . . ? C16 C15 P1 Pt1 -172.7(3) . . . . ? C18 C17 P1 C19 -175.7(2) . . . . ? C18 C17 P1 C15 -66.2(3) . . . . ? C18 C17 P1 Pt1 61.0(2) . . . . ? C22 C21 P2 C23 178.7(2) . . . . ? C22 C21 P2 C25 -72.2(3) . . . . ? C22 C21 P2 Pt1 53.9(2) . . . . ? C24 C23 P2 C21 174.4(2) . . . . ? C24 C23 P2 C25 65.0(2) . . . . ? C24 C23 P2 Pt1 -63.3(2) . . . . ? C26 C25 P2 C21 -60.5(3) . . . . ? C26 C25 P2 C23 47.7(3) . . . . ? C26 C25 P2 Pt1 175.9(2) . . . . ? C5 C6 S1 C3 -1.0(2) . . . . ? C6 C6 S1 C3 -179.5(3) 7_558 . . . ? C4 C3 S1 C6 0.7(2) . . . . ? C2 C3 S1 C6 -177.8(2) . . . . ? C2 C1 Pt1 C9 -39(5) . . . . ? C2 C1 Pt1 P1 7(4) . . . . ? C2 C1 Pt1 P2 -18E1(10) . . . . ? C14 C9 Pt1 C1 -45(2) . . . . ? C10 C9 Pt1 C1 134(2) . . . . ? C14 C9 Pt1 P1 -90.1(3) . . . . ? C10 C9 Pt1 P1 88.8(3) . . . . ? C14 C9 Pt1 P2 94.1(3) . . . . ? C10 C9 Pt1 P2 -86.9(3) . . . . ? C19 P1 Pt1 C1 -55.72(15) . . . . ? C15 P1 Pt1 C1 -178.91(17) . . . . ? C17 P1 Pt1 C1 61.60(13) . . . . ? C19 P1 Pt1 C9 122.23(16) . . . . ? C15 P1 Pt1 C9 -0.96(18) . . . . ? C17 P1 Pt1 C9 -120.45(14) . . . . ? C19 P1 Pt1 P2 -154.0(3) . . . . ? C15 P1 Pt1 P2 82.8(4) . . . . ? C17 P1 Pt1 P2 -36.7(4) . . . . ? C21 P2 Pt1 C1 -120.79(14) . . . . ? C23 P2 Pt1 C1 121.53(13) . . . . ? C25 P2 Pt1 C1 -0.92(15) . . . . ? C21 P2 Pt1 C9 61.10(15) . . . . ? C23 P2 Pt1 C9 -56.58(14) . . . . ? C25 P2 Pt1 C9 -179.03(16) . . . . ? C21 P2 Pt1 P1 -22.8(4) . . . . ? C23 P2 Pt1 P1 -140.5(3) . . . . ? C25 P2 Pt1 P1 97.1(3) . . . . ? ###END