# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'U Siemeling' _publ_contact_author_email SIEMELING@UNI-KASSEL.DE _publ_section_title ; Photoresponsive SAMs on gold fabricated from azobenzene-functionalised asparagusic acid derivatives ; loop_ _publ_author_name 'U. Siemeling' 'Waleed Azzam' 'Mihaela Badin' 'Marta Borg' 'Frauke Bretthauer' 'Clemens Bruhn' ; T.Strunskus ; 'Frank Trager' 'Florian Vogel' 'Christof Woll' # Attachment 'i0076.cif' data_i0076 _database_code_depnum_ccdc_archive 'CCDC 723720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H6 O2 S2' _chemical_formula_sum 'C4 H6 O2 S2' _chemical_formula_weight 150.21 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.2908(11) _cell_length_b 5.7842(12) _cell_length_c 10.625(2) _cell_angle_alpha 86.325(17) _cell_angle_beta 89.818(17) _cell_angle_gamma 70.457(16) _cell_volume 305.75(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3832 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.63 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5863 _exptl_absorpt_correction_T_max 0.9514 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 153(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 198 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 3225 _diffrn_reflns_av_R_equivalents 0.1147 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1062 _reflns_number_gt 979 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1129P)^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_extinction_coef ? _refine_ls_number_reflns 1062 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _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 0.5498(5) -0.2799(4) 0.1178(2) 0.0267(6) Uani 1 1 d . . . C2 C 0.5993(5) -0.1155(4) 0.2133(2) 0.0274(6) Uani 1 1 d . . . H2 H 0.7628 -0.0750 0.1883 0.033 Uiso 1 1 calc R . . C3 C 0.3654(5) 0.1243(5) 0.2189(2) 0.0328(6) Uani 1 1 d . . . H3A H 0.2731 0.1695 0.1354 0.039 Uiso 1 1 calc R . . H3B H 0.4334 0.2575 0.2396 0.039 Uiso 1 1 calc R . . C4 C 0.6509(5) -0.2491(5) 0.3449(2) 0.0290(6) Uani 1 1 d . . . H4B H 0.7145 -0.1543 0.4042 0.035 Uiso 1 1 calc R . . H4A H 0.7881 -0.4142 0.3416 0.035 Uiso 1 1 calc R . . O1 O 0.3455(3) -0.2252(3) 0.05237(16) 0.0351(5) Uani 1 1 d . . . O2 O 0.7532(4) -0.4853(3) 0.11125(17) 0.0349(5) Uani 1 1 d . . . H2A H 0.7236 -0.5656 0.0532 0.052 Uiso 1 1 calc R . . S1 S 0.12714(12) 0.09089(11) 0.33871(6) 0.0316(3) Uani 1 1 d . . . S2 S 0.33335(12) -0.27459(11) 0.39477(6) 0.0303(3) 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 0.0326(12) 0.0289(12) 0.0174(12) -0.0037(9) 0.0058(10) -0.0083(10) C2 0.0342(13) 0.0295(12) 0.0199(12) -0.0063(10) 0.0052(9) -0.0117(11) C3 0.0447(14) 0.0292(13) 0.0266(13) -0.0069(10) 0.0107(11) -0.0142(11) C4 0.0295(12) 0.0366(13) 0.0189(13) -0.0059(10) 0.0029(10) -0.0078(10) O1 0.0367(10) 0.0365(10) 0.0263(10) -0.0116(8) -0.0026(8) -0.0028(8) O2 0.0370(10) 0.0328(11) 0.0274(10) -0.0126(8) -0.0036(8) 0.0001(8) S1 0.0330(5) 0.0300(5) 0.0288(5) -0.0075(3) 0.0074(3) -0.0056(3) S2 0.0347(5) 0.0307(5) 0.0248(5) -0.0023(3) 0.0062(3) -0.0099(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 1.225(3) . ? C1 O2 1.315(3) . ? C1 C2 1.515(3) . ? C2 C3 1.523(4) . ? C2 C4 1.533(3) . ? C2 H2 1.0000 . ? C3 S1 1.835(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S2 1.810(2) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? O2 H2A 0.8400 . ? S1 S2 2.0770(10) . ? 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 O2 123.9(2) . . ? O1 C1 C2 123.7(2) . . ? O2 C1 C2 112.41(19) . . ? C1 C2 C3 112.2(2) . . ? C1 C2 C4 110.44(19) . . ? C3 C2 C4 109.13(19) . . ? C1 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C4 C2 H2 108.3 . . ? C2 C3 S1 110.30(17) . . ? C2 C3 H3A 109.6 . . ? S1 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? S1 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C2 C4 S2 106.12(15) . . ? C2 C4 H4B 110.5 . . ? S2 C4 H4B 110.5 . . ? C2 C4 H4A 110.5 . . ? S2 C4 H4A 110.5 . . ? H4B C4 H4A 108.7 . . ? C1 O2 H2A 109.5 . . ? C3 S1 S2 96.54(9) . . ? C4 S2 S1 92.30(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.607 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.122 # Attachment 'i0097.cif' data_i0097 _database_code_depnum_ccdc_archive 'CCDC 723721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 N2 O2 S2' _chemical_formula_sum 'C16 H14 N2 O2 S2' _chemical_formula_weight 330.41 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' 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 11.1961(13) _cell_length_b 5.0195(3) _cell_length_c 26.472(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.690(10) _cell_angle_gamma 90.00 _cell_volume 1487.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7545 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.09 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.590 _exptl_crystal_size_mid 0.195 _exptl_crystal_size_min 0.071 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8538 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 153(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 148 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 7146 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2605 _reflns_number_gt 1999 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0448P)^2^+0.8068P] 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 2605 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.000 _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 0.1445(2) 0.7948(5) 0.34301(9) 0.0270(5) Uani 1 1 d . . . C2 C 0.1528(2) 1.0278(5) 0.37884(10) 0.0288(6) Uani 1 1 d . . . H2 H 0.1443 1.1949 0.3585 0.035 Uiso 1 1 calc R . . C3 C 0.0530(2) 1.0224(5) 0.41651(10) 0.0309(6) Uani 1 1 d . . . H3A H -0.0239 0.9797 0.3989 0.037 Uiso 1 1 calc R . . H3B H 0.0456 1.1990 0.4328 0.037 Uiso 1 1 calc R . . C4 C 0.2715(2) 1.0411(5) 0.40848(10) 0.0324(6) Uani 1 1 d . . . H4A H 0.2792 1.2139 0.4263 0.039 Uiso 1 1 calc R . . H4B H 0.3389 1.0229 0.3853 0.039 Uiso 1 1 calc R . . C5 C 0.2542(2) 0.5845(5) 0.27806(9) 0.0294(6) Uani 1 1 d . . . C6 C 0.1731(2) 0.5785(5) 0.23773(10) 0.0312(6) Uani 1 1 d . . . H6 H 0.1077 0.6991 0.2361 0.037 Uiso 1 1 calc R . . C7 C 0.1888(2) 0.3937(5) 0.19977(9) 0.0302(6) Uani 1 1 d . . . H7 H 0.1329 0.3851 0.1721 0.036 Uiso 1 1 calc R . . C8 C 0.2856(2) 0.2203(5) 0.20172(10) 0.0272(5) Uani 1 1 d . . . C9 C 0.3666(2) 0.2284(6) 0.24266(10) 0.0341(6) Uani 1 1 d . . . H9 H 0.4325 0.1091 0.2443 0.041 Uiso 1 1 calc R . . C10 C 0.3505(2) 0.4113(6) 0.28101(10) 0.0359(6) Uani 1 1 d . . . H10A H 0.4052 0.4180 0.3091 0.043 Uiso 1 1 calc R . . C11 C 0.3931(2) -0.2816(5) 0.11952(9) 0.0265(5) Uani 1 1 d . . . C12 C 0.3032(2) -0.3236(5) 0.08266(10) 0.0314(6) Uani 1 1 d . . . H12 H 0.2318 -0.2211 0.0828 0.038 Uiso 1 1 calc R . . C13 C 0.3188(2) -0.5150(6) 0.04605(10) 0.0339(6) Uani 1 1 d . . . H13 H 0.2574 -0.5450 0.0211 0.041 Uiso 1 1 calc R . . C14 C 0.4231(2) -0.6642(5) 0.04518(10) 0.0333(6) Uani 1 1 d . . . H14 H 0.4332 -0.7952 0.0198 0.040 Uiso 1 1 calc R . . C15 C 0.5122(2) -0.6213(5) 0.08141(10) 0.0344(6) Uani 1 1 d . . . H15 H 0.5840 -0.7219 0.0808 0.041 Uiso 1 1 calc R . . C16 C 0.4972(2) -0.4317(5) 0.11878(10) 0.0307(6) Uani 1 1 d . . . H16 H 0.5582 -0.4045 0.1439 0.037 Uiso 1 1 calc R . . N1 N 0.29215(17) 0.0377(4) 0.16027(8) 0.0291(5) Uani 1 1 d . . . N2 N 0.38766(17) -0.0941(4) 0.16018(8) 0.0299(5) Uani 1 1 d . . . O1 O 0.24694(15) 0.7759(4) 0.31619(7) 0.0342(4) Uani 1 1 d . . . O2 O 0.06124(15) 0.6463(4) 0.33685(7) 0.0330(4) Uani 1 1 d . . . S1 S 0.08828(5) 0.76938(14) 0.46420(2) 0.0321(2) Uani 1 1 d . . . S2 S 0.27297(5) 0.76876(14) 0.45371(3) 0.0333(2) 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 0.0279(12) 0.0283(13) 0.0250(13) 0.0007(11) 0.0041(10) 0.0016(10) C2 0.0350(12) 0.0206(12) 0.0311(14) 0.0020(11) 0.0065(11) 0.0008(10) C3 0.0343(13) 0.0277(13) 0.0310(15) -0.0049(11) 0.0060(11) 0.0058(11) C4 0.0355(13) 0.0265(13) 0.0356(15) -0.0045(12) 0.0086(11) -0.0054(11) C5 0.0312(12) 0.0324(14) 0.0251(14) -0.0060(11) 0.0094(10) -0.0088(11) C6 0.0323(12) 0.0303(14) 0.0311(14) -0.0025(12) 0.0054(11) -0.0001(11) C7 0.0323(13) 0.0321(14) 0.0262(14) 0.0014(11) 0.0017(10) -0.0018(11) C8 0.0289(12) 0.0282(13) 0.0248(13) -0.0027(11) 0.0058(10) -0.0055(10) C9 0.0288(12) 0.0402(16) 0.0334(15) -0.0063(13) 0.0036(11) 0.0012(11) C10 0.0293(12) 0.0467(17) 0.0316(15) -0.0077(13) -0.0002(11) -0.0018(12) C11 0.0298(12) 0.0267(13) 0.0232(13) -0.0008(10) 0.0044(10) -0.0027(10) C12 0.0306(12) 0.0334(14) 0.0303(15) -0.0024(12) 0.0025(11) 0.0031(11) C13 0.0379(14) 0.0359(15) 0.0277(14) -0.0025(12) -0.0016(11) -0.0001(12) C14 0.0427(15) 0.0291(14) 0.0286(15) -0.0038(11) 0.0089(11) -0.0013(11) C15 0.0331(13) 0.0320(15) 0.0383(16) -0.0011(12) 0.0071(12) 0.0045(11) C16 0.0317(12) 0.0336(15) 0.0270(14) 0.0007(12) 0.0016(10) -0.0011(11) N1 0.0293(10) 0.0292(11) 0.0292(12) -0.0015(10) 0.0054(9) -0.0015(9) N2 0.0290(11) 0.0314(12) 0.0294(12) -0.0026(10) 0.0043(9) -0.0008(9) O1 0.0343(9) 0.0388(11) 0.0302(10) -0.0132(8) 0.0111(8) -0.0085(8) O2 0.0317(9) 0.0338(10) 0.0338(10) -0.0070(8) 0.0057(8) -0.0063(8) S1 0.0317(3) 0.0342(4) 0.0305(4) 0.0036(3) 0.0044(3) -0.0028(3) S2 0.0315(3) 0.0329(4) 0.0356(4) 0.0001(3) 0.0030(3) 0.0055(3) _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 O2 1.201(3) . ? C1 O1 1.370(3) . ? C1 C2 1.507(3) . ? C2 C3 1.520(3) . ? C2 C4 1.524(4) . ? C2 H2 1.0000 . ? C3 S1 1.826(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S2 1.817(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.382(4) . ? C5 C10 1.386(4) . ? C5 O1 1.398(3) . ? C6 C7 1.382(4) . ? C6 H6 0.9500 . ? C7 C8 1.390(4) . ? C7 H7 0.9500 . ? C8 C9 1.393(4) . ? C8 N1 1.433(3) . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 H10A 0.9500 . ? C11 C16 1.388(4) . ? C11 C12 1.398(4) . ? C11 N2 1.433(3) . ? C12 C13 1.380(4) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N1 N2 1.257(3) . ? S1 S2 2.0944(9) . ? 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 O2 C1 O1 123.0(2) . . ? O2 C1 C2 126.9(2) . . ? O1 C1 C2 110.0(2) . . ? C1 C2 C3 111.5(2) . . ? C1 C2 C4 113.3(2) . . ? C3 C2 C4 108.0(2) . . ? C1 C2 H2 108.0 . . ? C3 C2 H2 108.0 . . ? C4 C2 H2 108.0 . . ? C2 C3 S1 108.54(17) . . ? C2 C3 H3A 110.0 . . ? S1 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? S1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C2 C4 S2 107.29(17) . . ? C2 C4 H4A 110.3 . . ? S2 C4 H4A 110.3 . . ? C2 C4 H4B 110.3 . . ? S2 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? C6 C5 C10 121.5(2) . . ? C6 C5 O1 121.5(2) . . ? C10 C5 O1 116.9(2) . . ? C5 C6 C7 118.8(2) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C8 120.6(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 120.0(2) . . ? C7 C8 N1 115.4(2) . . ? C9 C8 N1 124.6(2) . . ? C10 C9 C8 119.6(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C5 119.5(2) . . ? C9 C10 H10A 120.3 . . ? C5 C10 H10A 120.3 . . ? C16 C11 C12 119.8(2) . . ? C16 C11 N2 115.0(2) . . ? C12 C11 N2 125.3(2) . . ? C13 C12 C11 119.5(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.2(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.1(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? N2 N1 C8 113.6(2) . . ? N1 N2 C11 113.7(2) . . ? C1 O1 C5 119.29(19) . . ? C3 S1 S2 95.95(8) . . ? C4 S2 S1 95.53(8) . . ? 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 O2 C1 C2 C3 13.1(4) . . . . ? O1 C1 C2 C3 -168.4(2) . . . . ? O2 C1 C2 C4 135.2(3) . . . . ? O1 C1 C2 C4 -46.4(3) . . . . ? C1 C2 C3 S1 76.0(2) . . . . ? C4 C2 C3 S1 -49.0(2) . . . . ? C1 C2 C4 S2 -70.9(2) . . . . ? C3 C2 C4 S2 53.1(2) . . . . ? C10 C5 C6 C7 0.3(4) . . . . ? O1 C5 C6 C7 176.5(2) . . . . ? C5 C6 C7 C8 -1.1(4) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C6 C7 C8 N1 179.9(2) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? N1 C8 C9 C10 -179.1(2) . . . . ? C8 C9 C10 C5 -0.2(4) . . . . ? C6 C5 C10 C9 0.3(4) . . . . ? O1 C5 C10 C9 -176.0(2) . . . . ? C16 C11 C12 C13 0.3(4) . . . . ? N2 C11 C12 C13 -178.6(2) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C14 C15 C16 C11 -0.9(4) . . . . ? C12 C11 C16 C15 0.4(4) . . . . ? N2 C11 C16 C15 179.5(2) . . . . ? C7 C8 N1 N2 172.1(2) . . . . ? C9 C8 N1 N2 -9.3(3) . . . . ? C8 N1 N2 C11 178.50(19) . . . . ? C16 C11 N2 N1 -179.4(2) . . . . ? C12 C11 N2 N1 -0.4(4) . . . . ? O2 C1 O1 C5 3.2(4) . . . . ? C2 C1 O1 C5 -175.3(2) . . . . ? C6 C5 O1 C1 57.9(3) . . . . ? C10 C5 O1 C1 -125.8(3) . . . . ? C2 C3 S1 S2 23.04(18) . . . . ? C2 C4 S2 S1 -31.63(17) . . . . ? C3 S1 S2 C4 4.74(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.346 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.073 # Attachment 'i0176.cif' data_i0176 _database_code_depnum_ccdc_archive 'CCDC 723722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 N2 O2 P2 Pt S2, C6 H6' _chemical_formula_sum 'C58 H50 N2 O2 P2 Pt S2' _chemical_formula_weight 1128.15 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3328(10) _cell_length_b 14.7162(13) _cell_length_c 15.1442(13) _cell_angle_alpha 98.983(7) _cell_angle_beta 92.568(7) _cell_angle_gamma 99.832(7) _cell_volume 2451.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 10345 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 26.09 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 3.058 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5649 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details 'X-red ver.1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 153(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 15978 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.1282 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8122 _reflns_number_gt 5744 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0119P)^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_extinction_coef ? _refine_ls_number_reflns 8122 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _refine_ls_shift/su_max 0.000 _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 -0.1463(7) 0.5829(5) 0.3248(6) 0.042(2) Uani 1 1 d . . . H1B H -0.0866 0.6145 0.2886 0.050 Uiso 1 1 calc R . . H1A H -0.1886 0.6306 0.3561 0.050 Uiso 1 1 calc R . . C2 C -0.0808(7) 0.5404(6) 0.3943(6) 0.044(2) Uani 1 1 d . . . H2A H -0.0497 0.5925 0.4450 0.053 Uiso 1 1 calc R . . C3 C 0.0300(7) 0.5016(6) 0.3584(6) 0.040(2) Uani 1 1 d . . . H3B H 0.0373 0.4460 0.3861 0.048 Uiso 1 1 calc R . . H3A H 0.1023 0.5495 0.3796 0.048 Uiso 1 1 calc R . . C4 C -0.1662(8) 0.4705(6) 0.4320(6) 0.043(2) Uani 1 1 d . . . C5 C -0.3514(7) 0.4483(6) 0.5002(6) 0.040(2) Uani 1 1 d . . . C6 C -0.4280(8) 0.3840(6) 0.4404(7) 0.048(2) Uani 1 1 d . . . H6A H -0.4188 0.3787 0.3779 0.057 Uiso 1 1 calc R . . C7 C -0.5212(8) 0.3256(7) 0.4735(8) 0.063(3) Uani 1 1 d . . . H7A H -0.5743 0.2779 0.4341 0.076 Uiso 1 1 calc R . . C8 C -0.5336(8) 0.3398(7) 0.5676(7) 0.054(3) Uani 1 1 d . . . C9 C -0.4609(8) 0.4077(7) 0.6226(7) 0.059(3) Uani 1 1 d . . . H9A H -0.4739 0.4185 0.6846 0.071 Uiso 1 1 calc R . . C10 C -0.3673(8) 0.4625(6) 0.5905(6) 0.049(2) Uani 1 1 d . . . H10A H -0.3141 0.5097 0.6303 0.059 Uiso 1 1 calc R . . C11 C -0.7453(8) 0.1482(7) 0.6151(7) 0.055(3) Uani 1 1 d . . . C12 C -0.7854(11) 0.0603(7) 0.5692(8) 0.075(4) Uani 1 1 d . . . H12A H -0.7532 0.0412 0.5139 0.090 Uiso 1 1 calc R . . C13 C -0.8718(10) -0.0015(7) 0.6011(8) 0.069(3) Uani 1 1 d . . . H13A H -0.9009 -0.0619 0.5673 0.083 Uiso 1 1 calc R . . C14 C -0.9148(8) 0.0251(7) 0.6817(7) 0.053(3) Uani 1 1 d . . . H14A H -0.9728 -0.0178 0.7049 0.064 Uiso 1 1 calc R . . C15 C -0.8757(8) 0.1129(7) 0.7299(7) 0.058(3) Uani 1 1 d . . . H15A H -0.9073 0.1310 0.7857 0.070 Uiso 1 1 calc R . . C16 C -0.7888(8) 0.1756(6) 0.6962(7) 0.053(2) Uani 1 1 d . . . H16A H -0.7603 0.2365 0.7292 0.064 Uiso 1 1 calc R . . C17 C -0.1227(6) 0.1518(5) 0.0695(6) 0.0319(18) Uani 1 1 d . . . C18 C -0.1456(7) 0.1343(5) -0.0224(6) 0.0375(19) Uani 1 1 d . . . H18A H -0.1198 0.1821 -0.0565 0.045 Uiso 1 1 calc R . . C19 C -0.2066(7) 0.0468(5) -0.0658(6) 0.042(2) Uani 1 1 d . . . H19A H -0.2241 0.0357 -0.1290 0.051 Uiso 1 1 calc R . . C20 C -0.2412(7) -0.0230(6) -0.0168(7) 0.046(2) Uani 1 1 d . . . H20A H -0.2823 -0.0825 -0.0462 0.055 Uiso 1 1 calc R . . C21 C -0.2167(7) -0.0072(5) 0.0740(6) 0.040(2) Uani 1 1 d . . . H21A H -0.2400 -0.0562 0.1072 0.048 Uiso 1 1 calc R . . C22 C -0.1584(7) 0.0795(5) 0.1180(6) 0.0345(19) Uani 1 1 d . . . H22A H -0.1425 0.0899 0.1813 0.041 Uiso 1 1 calc R . . C23 C 0.0601(6) 0.3019(5) 0.0490(5) 0.0304(17) Uani 1 1 d . . . C24 C 0.1266(7) 0.2408(6) 0.0043(6) 0.037(2) Uani 1 1 d . . . H24A H 0.1168 0.1785 0.0161 0.044 Uiso 1 1 calc R . . C25 C 0.2066(7) 0.2676(5) -0.0565(6) 0.037(2) Uani 1 1 d . . . H25A H 0.2535 0.2251 -0.0844 0.044 Uiso 1 1 calc R . . C26 C 0.2182(7) 0.3570(5) -0.0769(5) 0.0349(19) Uani 1 1 d . . . H26A H 0.2728 0.3759 -0.1192 0.042 Uiso 1 1 calc R . . C27 C 0.1514(7) 0.4178(5) -0.0365(5) 0.037(2) Uani 1 1 d . . . H27A H 0.1590 0.4785 -0.0521 0.045 Uiso 1 1 calc R . . C28 C 0.0713(7) 0.3933(5) 0.0278(5) 0.0312(18) Uani 1 1 d . . . H28A H 0.0260 0.4367 0.0562 0.037 Uiso 1 1 calc R . . C29 C 0.0355(7) 0.2334(5) 0.2215(5) 0.0332(18) Uani 1 1 d . . . C30 C 0.1293(7) 0.1827(6) 0.2081(6) 0.044(2) Uani 1 1 d . . . H30A H 0.1513 0.1646 0.1489 0.053 Uiso 1 1 calc R . . C31 C 0.1899(8) 0.1587(7) 0.2792(7) 0.055(3) Uani 1 1 d . . . H31A H 0.2526 0.1239 0.2684 0.066 Uiso 1 1 calc R . . C32 C 0.1613(9) 0.1841(6) 0.3650(7) 0.057(3) Uani 1 1 d . . . H32A H 0.2053 0.1691 0.4139 0.069 Uiso 1 1 calc R . . C33 C 0.0684(10) 0.2316(6) 0.3794(6) 0.062(3) Uani 1 1 d . . . H33A H 0.0460 0.2477 0.4387 0.074 Uiso 1 1 calc R . . C34 C 0.0063(8) 0.2565(6) 0.3085(6) 0.042(2) Uani 1 1 d . . . H34A H -0.0575 0.2900 0.3201 0.051 Uiso 1 1 calc R . . C35 C -0.3815(6) 0.1931(5) 0.1597(5) 0.0298(18) Uani 1 1 d . . . C36 C -0.4503(6) 0.1110(5) 0.1103(6) 0.037(2) Uani 1 1 d . . . H36A H -0.4775 0.1101 0.0499 0.045 Uiso 1 1 calc R . . C37 C -0.4793(7) 0.0308(6) 0.1488(7) 0.046(2) Uani 1 1 d . . . H37A H -0.5260 -0.0242 0.1147 0.055 Uiso 1 1 calc R . . C38 C -0.4408(8) 0.0314(6) 0.2349(7) 0.049(2) Uani 1 1 d . . . H38A H -0.4594 -0.0238 0.2606 0.059 Uiso 1 1 calc R . . C39 C -0.3753(9) 0.1109(6) 0.2852(6) 0.057(3) Uani 1 1 d . . . H39A H -0.3496 0.1107 0.3457 0.068 Uiso 1 1 calc R . . C40 C -0.3458(7) 0.1925(6) 0.2483(6) 0.040(2) Uani 1 1 d . . . H40A H -0.3013 0.2476 0.2840 0.048 Uiso 1 1 calc R . . C41 C -0.4667(6) 0.3597(5) 0.1410(5) 0.0286(17) Uani 1 1 d . . . C42 C -0.5629(7) 0.3296(5) 0.1915(5) 0.0357(19) Uani 1 1 d . . . H42A H -0.5635 0.2745 0.2169 0.043 Uiso 1 1 calc R . . C43 C -0.6561(7) 0.3781(6) 0.2048(6) 0.043(2) Uani 1 1 d . . . H43A H -0.7192 0.3562 0.2396 0.051 Uiso 1 1 calc R . . C44 C -0.6593(7) 0.4572(6) 0.1687(6) 0.043(2) Uani 1 1 d . . . H44A H -0.7242 0.4899 0.1783 0.052 Uiso 1 1 calc R . . C45 C -0.5665(7) 0.4895(5) 0.1177(6) 0.0376(19) Uani 1 1 d . . . H45A H -0.5679 0.5445 0.0923 0.045 Uiso 1 1 calc R . . C46 C -0.4731(7) 0.4416(5) 0.1042(5) 0.0342(18) Uani 1 1 d . . . H46A H -0.4106 0.4643 0.0691 0.041 Uiso 1 1 calc R . . C47 C -0.3532(7) 0.2832(5) -0.0033(5) 0.0270(18) Uani 1 1 d . . . C48 C -0.4638(7) 0.2451(5) -0.0527(6) 0.0375(19) Uani 1 1 d . . . H48A H -0.5324 0.2259 -0.0218 0.045 Uiso 1 1 calc R . . C49 C -0.4744(8) 0.2353(6) -0.1442(6) 0.046(2) Uani 1 1 d . . . H49A H -0.5493 0.2082 -0.1763 0.055 Uiso 1 1 calc R . . C50 C -0.3742(9) 0.2653(6) -0.1906(6) 0.048(2) Uani 1 1 d . . . H50A H -0.3803 0.2570 -0.2542 0.057 Uiso 1 1 calc R . . C51 C -0.2673(8) 0.3070(6) -0.1429(6) 0.042(2) Uani 1 1 d . . . H51A H -0.2003 0.3301 -0.1736 0.050 Uiso 1 1 calc R . . C52 C -0.2567(7) 0.3155(5) -0.0504(5) 0.0346(19) Uani 1 1 d . . . H52A H -0.1820 0.3440 -0.0186 0.041 Uiso 1 1 calc R . . C53 C -0.3606(19) 0.1559(16) 0.5439(11) 0.124(7) Uani 1 1 d . . . H53A H -0.4178 0.1713 0.5036 0.149 Uiso 1 1 calc R . . C54 C -0.3906(16) 0.0823(14) 0.5804(10) 0.127(7) Uani 1 1 d . . . H54A H -0.4651 0.0407 0.5654 0.152 Uiso 1 1 calc R . . C55 C -0.3070(13) 0.0696(8) 0.6418(10) 0.086(4) Uani 1 1 d . . . H55A H -0.3289 0.0187 0.6730 0.103 Uiso 1 1 calc R . . C56 C -0.1972(13) 0.1207(13) 0.6635(10) 0.105(5) Uani 1 1 d . . . H56A H -0.1429 0.1039 0.7052 0.126 Uiso 1 1 calc R . . C57 C -0.1652(17) 0.1986(15) 0.6234(14) 0.150(8) Uani 1 1 d . . . H57A H -0.0900 0.2394 0.6382 0.180 Uiso 1 1 calc R . . C58 C -0.248(3) 0.2140(11) 0.5608(13) 0.147(11) Uani 1 1 d . . . H58A H -0.2283 0.2645 0.5288 0.177 Uiso 1 1 calc R . . N1 N -0.6193(8) 0.2802(7) 0.6158(7) 0.069(3) Uani 1 1 d . . . N2 N -0.6611(7) 0.2056(7) 0.5675(7) 0.068(2) Uani 1 1 d . . . O1 O -0.2566(5) 0.5089(4) 0.4698(4) 0.0487(16) Uani 1 1 d . . . O2 O -0.1593(5) 0.3895(4) 0.4340(4) 0.0519(17) Uani 1 1 d . . . P1 P -0.04757(18) 0.26710(14) 0.12935(14) 0.0267(5) Uani 1 1 d . . . P2 P -0.34030(18) 0.30281(14) 0.11837(15) 0.0271(5) Uani 1 1 d . . . S1 S -0.25380(18) 0.49562(14) 0.25073(14) 0.0300(5) Uani 1 1 d . . . S2 S 0.03179(18) 0.46873(15) 0.23790(15) 0.0335(5) Uani 1 1 d . . . Pt1 Pt -0.15623(3) 0.37993(2) 0.18157(3) 0.02325(8) 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 0.043(5) 0.038(5) 0.043(6) -0.002(4) 0.009(5) 0.007(4) C2 0.039(5) 0.048(5) 0.041(6) 0.003(5) -0.003(4) 0.001(4) C3 0.038(5) 0.038(5) 0.037(5) -0.006(4) 0.003(4) -0.001(4) C4 0.045(5) 0.045(5) 0.037(5) 0.006(4) 0.006(5) 0.003(4) C5 0.033(4) 0.042(5) 0.042(6) 0.007(4) 0.004(4) 0.001(4) C6 0.046(5) 0.053(5) 0.046(6) 0.009(5) 0.013(5) 0.011(5) C7 0.034(5) 0.071(7) 0.073(8) 0.000(6) -0.002(5) -0.006(5) C8 0.042(5) 0.059(6) 0.065(7) 0.025(6) 0.019(5) 0.008(5) C9 0.054(6) 0.069(6) 0.057(7) 0.014(6) 0.026(6) 0.007(5) C10 0.049(5) 0.053(5) 0.041(6) 0.004(5) 0.008(5) 0.001(4) C11 0.047(5) 0.057(6) 0.072(8) 0.039(6) 0.019(5) 0.010(5) C12 0.099(9) 0.061(7) 0.076(9) 0.024(7) 0.033(7) 0.030(6) C13 0.098(9) 0.044(6) 0.066(8) 0.018(6) 0.012(7) 0.008(6) C14 0.040(5) 0.062(6) 0.061(7) 0.029(6) -0.005(5) 0.002(5) C15 0.054(6) 0.071(7) 0.051(7) 0.010(6) 0.006(5) 0.013(5) C16 0.045(5) 0.049(5) 0.061(7) 0.014(5) -0.009(5) -0.005(4) C17 0.029(4) 0.028(4) 0.041(5) 0.006(4) 0.003(4) 0.011(3) C18 0.041(5) 0.036(4) 0.035(5) 0.001(4) -0.003(4) 0.009(4) C19 0.040(5) 0.039(5) 0.041(5) -0.005(4) -0.009(4) 0.002(4) C20 0.034(4) 0.036(5) 0.062(7) -0.006(5) -0.011(5) 0.005(4) C21 0.037(4) 0.027(4) 0.056(6) 0.009(4) -0.001(5) 0.005(3) C22 0.037(4) 0.029(4) 0.038(5) 0.006(4) 0.005(4) 0.007(3) C23 0.027(4) 0.035(4) 0.030(5) 0.004(4) 0.000(4) 0.009(3) C24 0.037(4) 0.040(4) 0.041(5) 0.017(4) 0.007(4) 0.015(4) C25 0.037(4) 0.037(4) 0.036(5) 0.002(4) 0.009(4) 0.008(4) C26 0.035(4) 0.041(4) 0.027(5) 0.005(4) 0.011(4) 0.001(4) C27 0.049(5) 0.029(4) 0.033(5) 0.007(4) 0.005(4) 0.003(4) C28 0.034(4) 0.028(4) 0.031(5) 0.002(4) 0.004(4) 0.007(3) C29 0.038(4) 0.029(4) 0.033(5) 0.012(4) 0.001(4) 0.001(3) C30 0.043(5) 0.049(5) 0.046(6) 0.018(5) 0.000(4) 0.014(4) C31 0.049(5) 0.053(6) 0.069(8) 0.031(6) -0.011(5) 0.009(4) C32 0.068(6) 0.043(5) 0.054(7) 0.016(5) -0.036(6) -0.006(5) C33 0.111(9) 0.043(5) 0.031(5) 0.013(5) -0.016(6) 0.009(6) C34 0.055(5) 0.037(5) 0.031(5) 0.004(4) 0.005(5) 0.001(4) C35 0.028(4) 0.023(4) 0.037(5) 0.003(4) 0.007(4) 0.002(3) C36 0.033(4) 0.034(4) 0.045(5) 0.006(4) 0.004(4) 0.003(3) C37 0.040(5) 0.034(4) 0.056(7) 0.004(5) 0.007(5) -0.009(4) C38 0.059(6) 0.030(5) 0.055(7) 0.013(5) 0.014(5) -0.004(4) C39 0.090(7) 0.047(5) 0.037(6) 0.021(5) 0.023(6) 0.003(5) C40 0.037(4) 0.039(4) 0.042(6) 0.009(4) 0.006(4) 0.002(4) C41 0.025(4) 0.034(4) 0.024(4) 0.001(4) 0.001(3) 0.004(3) C42 0.036(4) 0.034(4) 0.036(5) 0.008(4) 0.005(4) 0.002(4) C43 0.025(4) 0.052(5) 0.043(6) -0.010(5) 0.010(4) -0.003(3) C44 0.029(4) 0.054(5) 0.048(6) 0.006(5) 0.000(4) 0.015(4) C45 0.040(4) 0.041(4) 0.034(5) 0.007(4) -0.001(4) 0.016(4) C46 0.029(4) 0.046(5) 0.028(5) 0.008(4) -0.001(4) 0.008(4) C47 0.030(4) 0.026(4) 0.025(4) 0.002(3) 0.006(4) 0.009(3) C48 0.036(4) 0.041(4) 0.035(5) 0.005(4) 0.003(4) 0.008(4) C49 0.044(5) 0.047(5) 0.048(6) 0.008(5) -0.006(5) 0.017(4) C50 0.070(6) 0.054(5) 0.026(5) 0.002(4) 0.004(5) 0.033(5) C51 0.048(5) 0.052(5) 0.032(5) 0.012(4) 0.011(5) 0.018(4) C52 0.037(4) 0.035(4) 0.036(5) 0.011(4) 0.009(4) 0.012(3) C53 0.177(18) 0.175(18) 0.064(10) 0.016(13) 0.017(13) 0.154(16) C54 0.140(14) 0.187(18) 0.100(12) 0.063(13) 0.021(11) 0.119(14) C55 0.092(9) 0.051(6) 0.117(12) 0.017(7) 0.028(9) 0.016(7) C56 0.077(9) 0.174(16) 0.079(10) 0.036(11) 0.008(8) 0.048(10) C57 0.117(14) 0.19(2) 0.122(16) 0.012(15) 0.059(13) -0.042(13) C58 0.33(4) 0.066(9) 0.067(12) 0.034(10) 0.074(19) 0.066(15) N1 0.055(5) 0.071(6) 0.079(8) 0.002(6) 0.000(5) 0.018(5) N2 0.052(5) 0.073(6) 0.077(7) 0.010(6) -0.007(5) 0.011(5) O1 0.043(3) 0.054(4) 0.046(4) 0.005(3) 0.015(3) 0.004(3) O2 0.047(3) 0.055(4) 0.059(5) 0.019(3) 0.008(3) 0.014(3) P1 0.0268(10) 0.0267(10) 0.0269(12) 0.0052(9) 0.0011(9) 0.0054(9) P2 0.0245(10) 0.0297(11) 0.0264(12) 0.0051(10) 0.0007(10) 0.0029(9) S1 0.0290(10) 0.0312(11) 0.0297(12) 0.0027(9) 0.0049(10) 0.0070(9) S2 0.0246(10) 0.0368(11) 0.0347(13) -0.0009(10) 0.0033(10) -0.0007(9) Pt1 0.02203(13) 0.02344(14) 0.02395(15) 0.00437(11) 0.00302(11) 0.00246(10) _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 1.532(12) . ? C1 S1 1.812(9) . ? C1 H1B 0.9900 . ? C1 H1A 0.9900 . ? C2 C4 1.487(11) . ? C2 C3 1.551(10) . ? C2 H2A 1.0000 . ? C3 S2 1.815(9) . ? C3 H3B 0.9900 . ? C3 H3A 0.9900 . ? C4 O2 1.212(9) . ? C4 O1 1.359(9) . ? C5 C6 1.360(12) . ? C5 C10 1.375(12) . ? C5 O1 1.417(9) . ? C6 C7 1.405(12) . ? C6 H6A 0.9500 . ? C7 C8 1.425(14) . ? C7 H7A 0.9500 . ? C8 C9 1.330(14) . ? C8 N1 1.489(11) . ? C9 C10 1.374(11) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.361(15) . ? C11 C16 1.372(13) . ? C11 N2 1.456(11) . ? C12 C13 1.376(13) . ? C12 H12A 0.9500 . ? C13 C14 1.360(14) . ? C13 H13A 0.9500 . ? C14 C15 1.371(14) . ? C14 H14A 0.9500 . ? C15 C16 1.402(12) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.379(11) . ? C17 C22 1.400(9) . ? C17 P1 1.839(8) . ? C18 C19 1.400(11) . ? C18 H18A 0.9500 . ? C19 C20 1.373(11) . ? C19 H19A 0.9500 . ? C20 C21 1.366(12) . ? C20 H20A 0.9500 . ? C21 C22 1.384(11) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.386(10) . ? C23 C28 1.417(9) . ? C23 P1 1.829(7) . ? C24 C25 1.376(10) . ? C24 H24A 0.9500 . ? C25 C26 1.383(10) . ? C25 H25A 0.9500 . ? C26 C27 1.360(10) . ? C26 H26A 0.9500 . ? C27 C28 1.407(9) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.378(11) . ? C29 C30 1.404(10) . ? C29 P1 1.827(8) . ? C30 C31 1.375(12) . ? C30 H30A 0.9500 . ? C31 C32 1.364(13) . ? C31 H31A 0.9500 . ? C32 C33 1.366(13) . ? C32 H32A 0.9500 . ? C33 C34 1.388(13) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C40 1.386(11) . ? C35 C36 1.404(11) . ? C35 P2 1.817(7) . ? C36 C37 1.392(10) . ? C36 H36A 0.9500 . ? C37 C38 1.355(13) . ? C37 H37A 0.9500 . ? C38 C39 1.370(13) . ? C38 H38A 0.9500 . ? C39 C40 1.398(10) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.409(9) . ? C41 C46 1.415(10) . ? C41 P2 1.799(7) . ? C42 C43 1.377(11) . ? C42 H42A 0.9500 . ? C43 C44 1.366(12) . ? C43 H43A 0.9500 . ? C44 C45 1.395(10) . ? C44 H44A 0.9500 . ? C45 C46 1.375(10) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C52 1.389(9) . ? C47 C48 1.412(11) . ? C47 P2 1.815(8) . ? C48 C49 1.368(12) . ? C48 H48A 0.9500 . ? C49 C50 1.405(11) . ? C49 H49A 0.9500 . ? C50 C51 1.377(13) . ? C50 H50A 0.9500 . ? C51 C52 1.384(11) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C54 1.29(2) . ? C53 C58 1.40(3) . ? C53 H53A 0.9500 . ? C54 C55 1.354(19) . ? C54 H54A 0.9500 . ? C55 C56 1.338(18) . ? C55 H55A 0.9500 . ? C56 C57 1.38(2) . ? C56 H56A 0.9500 . ? C57 C58 1.37(3) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? N1 N2 1.227(11) . ? P1 Pt1 2.297(2) . ? P2 Pt1 2.287(2) . ? S1 Pt1 2.326(2) . ? S2 Pt1 2.348(2) . ? 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 S1 112.3(6) . . ? C2 C1 H1B 109.1 . . ? S1 C1 H1B 109.1 . . ? C2 C1 H1A 109.1 . . ? S1 C1 H1A 109.1 . . ? H1B C1 H1A 107.9 . . ? C4 C2 C1 110.7(7) . . ? C4 C2 C3 113.1(7) . . ? C1 C2 C3 112.8(7) . . ? C4 C2 H2A 106.6 . . ? C1 C2 H2A 106.6 . . ? C3 C2 H2A 106.6 . . ? C2 C3 S2 117.5(6) . . ? C2 C3 H3B 107.9 . . ? S2 C3 H3B 107.9 . . ? C2 C3 H3A 107.9 . . ? S2 C3 H3A 107.9 . . ? H3B C3 H3A 107.2 . . ? O2 C4 O1 121.1(7) . . ? O2 C4 C2 127.3(8) . . ? O1 C4 C2 111.5(7) . . ? C6 C5 C10 122.3(7) . . ? C6 C5 O1 120.2(7) . . ? C10 C5 O1 117.3(8) . . ? C5 C6 C7 118.4(9) . . ? C5 C6 H6A 120.8 . . ? C7 C6 H6A 120.8 . . ? C6 C7 C8 118.1(9) . . ? C6 C7 H7A 120.9 . . ? C8 C7 H7A 120.9 . . ? C9 C8 C7 121.1(8) . . ? C9 C8 N1 112.9(9) . . ? C7 C8 N1 125.9(10) . . ? C8 C9 C10 120.6(9) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C9 C10 C5 119.3(9) . . ? C9 C10 H10A 120.4 . . ? C5 C10 H10A 120.4 . . ? C12 C11 C16 119.8(8) . . ? C12 C11 N2 113.5(9) . . ? C16 C11 N2 126.7(10) . . ? C11 C12 C13 121.5(10) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C12 119.0(10) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 121.0(9) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C14 C15 C16 119.4(9) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C11 C16 C15 119.3(9) . . ? C11 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C18 C17 C22 118.7(7) . . ? C18 C17 P1 121.8(6) . . ? C22 C17 P1 119.5(6) . . ? C17 C18 C19 120.6(7) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 119.7(8) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C21 C20 C19 120.3(8) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 120.6(8) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C17 120.1(8) . . ? C21 C22 H22A 120.0 . . ? C17 C22 H22A 120.0 . . ? C24 C23 C28 118.5(6) . . ? C24 C23 P1 122.6(5) . . ? C28 C23 P1 118.8(5) . . ? C25 C24 C23 122.0(7) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C24 C25 C26 119.5(7) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? C27 C26 C25 120.1(6) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 121.8(7) . . ? C26 C27 H27A 119.1 . . ? C28 C27 H27A 119.1 . . ? C27 C28 C23 118.1(7) . . ? C27 C28 H28A 121.0 . . ? C23 C28 H28A 121.0 . . ? C34 C29 C30 117.1(8) . . ? C34 C29 P1 120.2(6) . . ? C30 C29 P1 122.7(6) . . ? C31 C30 C29 121.0(8) . . ? C31 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C32 C31 C30 121.0(9) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C33 119.0(9) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? C32 C33 C34 120.9(9) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C29 C34 C33 121.1(9) . . ? C29 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C40 C35 C36 118.0(7) . . ? C40 C35 P2 116.7(6) . . ? C36 C35 P2 125.2(6) . . ? C37 C36 C35 120.8(8) . . ? C37 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? C38 C37 C36 120.0(8) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C39 120.4(8) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C39 C40 120.7(9) . . ? C38 C39 H39A 119.7 . . ? C40 C39 H39A 119.7 . . ? C35 C40 C39 120.0(8) . . ? C35 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C42 C41 C46 115.9(6) . . ? C42 C41 P2 126.0(6) . . ? C46 C41 P2 118.2(5) . . ? C43 C42 C41 121.6(7) . . ? C43 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C44 C43 C42 121.1(7) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 119.5(7) . . ? C43 C44 H44A 120.2 . . ? C45 C44 H44A 120.2 . . ? C46 C45 C44 119.7(7) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C46 C41 122.2(6) . . ? C45 C46 H46A 118.9 . . ? C41 C46 H46A 118.9 . . ? C52 C47 C48 117.6(7) . . ? C52 C47 P2 120.4(6) . . ? C48 C47 P2 121.6(5) . . ? C49 C48 C47 121.4(7) . . ? C49 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C48 C49 C50 119.9(9) . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C51 C50 C49 119.3(8) . . ? C51 C50 H50A 120.3 . . ? C49 C50 H50A 120.3 . . ? C50 C51 C52 120.5(7) . . ? C50 C51 H51A 119.7 . . ? C52 C51 H51A 119.7 . . ? C51 C52 C47 121.2(8) . . ? C51 C52 H52A 119.4 . . ? C47 C52 H52A 119.4 . . ? C54 C53 C58 123.2(18) . . ? C54 C53 H53A 118.4 . . ? C58 C53 H53A 118.4 . . ? C53 C54 C55 114.4(19) . . ? C53 C54 H54A 122.8 . . ? C55 C54 H54A 122.8 . . ? C56 C55 C54 127.3(15) . . ? C56 C55 H55A 116.4 . . ? C54 C55 H55A 116.4 . . ? C55 C56 C57 117.8(15) . . ? C55 C56 H56A 121.1 . . ? C57 C56 H56A 121.1 . . ? C58 C57 C56 116.5(17) . . ? C58 C57 H57A 121.8 . . ? C56 C57 H57A 121.8 . . ? C57 C58 C53 120.6(16) . . ? C57 C58 H58A 119.7 . . ? C53 C58 H58A 119.7 . . ? N2 N1 C8 110.6(9) . . ? N1 N2 C11 110.2(10) . . ? C4 O1 C5 117.7(6) . . ? C29 P1 C23 107.7(3) . . ? C29 P1 C17 100.8(3) . . ? C23 P1 C17 100.7(3) . . ? C29 P1 Pt1 111.1(3) . . ? C23 P1 Pt1 114.0(2) . . ? C17 P1 Pt1 121.0(2) . . ? C41 P2 C47 100.1(3) . . ? C41 P2 C35 103.2(3) . . ? C47 P2 C35 110.5(4) . . ? C41 P2 Pt1 117.3(3) . . ? C47 P2 Pt1 114.4(2) . . ? C35 P2 Pt1 110.4(3) . . ? C1 S1 Pt1 109.3(3) . . ? C3 S2 Pt1 108.7(3) . . ? P2 Pt1 P1 97.55(8) . . ? P2 Pt1 S1 87.25(8) . . ? P1 Pt1 S1 173.23(9) . . ? P2 Pt1 S2 174.93(9) . . ? P1 Pt1 S2 84.47(8) . . ? S1 Pt1 S2 91.14(8) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.949 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.123 # Attachment 'i0188.cif' data_i0188 _database_code_depnum_ccdc_archive 'CCDC 723723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H45 N3 O P2 Pt S2, C6 H6' _chemical_formula_sum 'C58 H51 N3 O P2 Pt S2' _chemical_formula_weight 1127.17 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 19.2645(14) _cell_length_b 14.7195(9) _cell_length_c 19.8911(19) _cell_angle_alpha 90.00 _cell_angle_beta 116.214(7) _cell_angle_gamma 90.00 _cell_volume 5060.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15275 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.382 _exptl_crystal_size_mid 0.187 _exptl_crystal_size_min 0.046 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 2.962 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4195 _exptl_absorpt_correction_T_max 0.8535 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 153(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 114 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 19815 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8517 _reflns_number_gt 5715 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8517 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.015 _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 0.6196(4) 0.1287(4) 0.7053(4) 0.0421(16) Uani 1 1 d . . . H1A H 0.5906 0.0906 0.7253 0.051 Uiso 1 1 calc R . . H1B H 0.6619 0.0909 0.7050 0.051 Uiso 1 1 calc R . . C2 C 0.6565(3) 0.2079(4) 0.7604(4) 0.0400(15) Uani 1 1 d . . . H2 H 0.6990 0.1811 0.8062 0.048 Uiso 1 1 calc R . . C3 C 0.6947(3) 0.2775(5) 0.7291(3) 0.0368(13) Uani 1 1 d . . . H3A H 0.7353 0.3106 0.7716 0.044 Uiso 1 1 calc R . . H3B H 0.6552 0.3224 0.6983 0.044 Uiso 1 1 calc R . . C4 C 0.6023(3) 0.2554(4) 0.7858(4) 0.0387(16) Uani 1 1 d . . . C5 C 0.4693(4) 0.3241(4) 0.7297(4) 0.0413(16) Uani 1 1 d . . . C6 C 0.4023(4) 0.3257(5) 0.6626(5) 0.0503(18) Uani 1 1 d . . . H6 H 0.4003 0.2933 0.6205 0.060 Uiso 1 1 calc R . . C7 C 0.3389(4) 0.3737(5) 0.6567(5) 0.055(2) Uani 1 1 d . . . H7 H 0.2933 0.3740 0.6105 0.066 Uiso 1 1 calc R . . C8 C 0.3402(4) 0.4212(4) 0.7163(5) 0.0439(17) Uani 1 1 d . . . C9 C 0.4063(4) 0.4201(5) 0.7832(5) 0.0457(17) Uani 1 1 d . . . H9 H 0.4073 0.4527 0.8248 0.055 Uiso 1 1 calc R . . C10 C 0.4720(4) 0.3718(4) 0.7910(4) 0.0426(16) Uani 1 1 d . . . H10 H 0.5175 0.3717 0.8373 0.051 Uiso 1 1 calc R . . C11 C 0.1534(4) 0.5216(5) 0.6526(5) 0.052(2) Uani 1 1 d . . . C12 C 0.0792(4) 0.4911(7) 0.6099(5) 0.063(2) Uani 1 1 d . . . H12 H 0.0696 0.4318 0.5889 0.075 Uiso 1 1 calc R . . C13 C 0.0192(5) 0.5498(9) 0.5988(6) 0.081(3) Uani 1 1 d . . . H13 H -0.0325 0.5299 0.5700 0.098 Uiso 1 1 calc R . . C14 C 0.0318(6) 0.6347(8) 0.6278(6) 0.082(3) Uani 1 1 d . . . H14 H -0.0106 0.6737 0.6190 0.099 Uiso 1 1 calc R . . C15 C 0.1055(6) 0.6640(7) 0.6694(7) 0.083(3) Uani 1 1 d . . . H15 H 0.1147 0.7236 0.6898 0.100 Uiso 1 1 calc R . . C16 C 0.1673(5) 0.6068(6) 0.6822(6) 0.066(3) Uani 1 1 d . . . H16 H 0.2188 0.6270 0.7113 0.079 Uiso 1 1 calc R . . C17 C 0.5365(3) 0.1356(4) 0.3780(4) 0.0362(15) Uani 1 1 d . . . C18 C 0.5079(4) 0.1479(5) 0.3005(4) 0.0452(17) Uani 1 1 d . . . H18 H 0.4815 0.2023 0.2775 0.054 Uiso 1 1 calc R . . C19 C 0.5185(4) 0.0801(5) 0.2580(5) 0.0506(18) Uani 1 1 d . . . H19 H 0.4994 0.0889 0.2055 0.061 Uiso 1 1 calc R . . C20 C 0.5558(4) 0.0002(5) 0.2893(5) 0.053(2) Uani 1 1 d . . . H20 H 0.5623 -0.0456 0.2589 0.064 Uiso 1 1 calc R . . C21 C 0.5834(4) -0.0120(5) 0.3649(5) 0.0477(18) Uani 1 1 d . . . H21 H 0.6091 -0.0670 0.3871 0.057 Uiso 1 1 calc R . . C22 C 0.5744(3) 0.0553(4) 0.4100(4) 0.0406(16) Uani 1 1 d . . . H22 H 0.5942 0.0460 0.4625 0.049 Uiso 1 1 calc R . . C23 C 0.4324(3) 0.1735(4) 0.4407(4) 0.0344(14) Uani 1 1 d . . . C24 C 0.4013(4) 0.0886(4) 0.4126(4) 0.0421(16) Uani 1 1 d . . . H24 H 0.4284 0.0485 0.3951 0.051 Uiso 1 1 calc R . . C25 C 0.3307(4) 0.0619(4) 0.4099(4) 0.0442(17) Uani 1 1 d . . . H25 H 0.3098 0.0039 0.3907 0.053 Uiso 1 1 calc R . . C26 C 0.2912(4) 0.1200(5) 0.4352(5) 0.0481(18) Uani 1 1 d . . . H26 H 0.2428 0.1022 0.4328 0.058 Uiso 1 1 calc R . . C27 C 0.3221(4) 0.2046(5) 0.4644(5) 0.0472(18) Uani 1 1 d . . . H27 H 0.2952 0.2439 0.4827 0.057 Uiso 1 1 calc R . . C28 C 0.3916(3) 0.2315(4) 0.4666(4) 0.0409(16) Uani 1 1 d . . . H28 H 0.4120 0.2897 0.4858 0.049 Uiso 1 1 calc R . . C29 C 0.4904(3) 0.3240(4) 0.3973(4) 0.0378(15) Uani 1 1 d . . . C30 C 0.4236(4) 0.3323(5) 0.3282(4) 0.0435(16) Uani 1 1 d . . . H30 H 0.3955 0.2797 0.3033 0.052 Uiso 1 1 calc R . . C31 C 0.3992(4) 0.4176(5) 0.2970(5) 0.055(2) Uani 1 1 d . . . H31 H 0.3541 0.4232 0.2508 0.065 Uiso 1 1 calc R . . C32 C 0.4400(4) 0.4944(5) 0.3326(5) 0.059(2) Uani 1 1 d . . . H32 H 0.4241 0.5522 0.3096 0.070 Uiso 1 1 calc R . . C33 C 0.5039(4) 0.4876(5) 0.4014(5) 0.057(2) Uani 1 1 d . . . H33 H 0.5304 0.5407 0.4271 0.068 Uiso 1 1 calc R . . C34 C 0.5290(4) 0.4019(4) 0.4328(5) 0.0481(19) Uani 1 1 d . . . H34 H 0.5736 0.3972 0.4796 0.058 Uiso 1 1 calc R . . C35 C 0.8058(3) 0.2097(4) 0.5586(4) 0.0368(14) Uani 1 1 d . . . C36 C 0.8787(4) 0.2525(5) 0.5873(5) 0.060(2) Uani 1 1 d . . . H36 H 0.8822 0.3163 0.5822 0.072 Uiso 1 1 calc R . . C37 C 0.9457(4) 0.2005(6) 0.6234(6) 0.065(2) Uani 1 1 d . . . H37 H 0.9947 0.2297 0.6437 0.078 Uiso 1 1 calc R . . C38 C 0.9420(4) 0.1087(5) 0.6299(6) 0.064(3) Uani 1 1 d . . . H38 H 0.9882 0.0742 0.6538 0.077 Uiso 1 1 calc R . . C39 C 0.8714(4) 0.0659(5) 0.6019(5) 0.055(2) Uani 1 1 d . . . H39 H 0.8691 0.0017 0.6053 0.067 Uiso 1 1 calc R . . C40 C 0.8033(4) 0.1157(5) 0.5687(4) 0.0449(17) Uani 1 1 d . . . H40 H 0.7548 0.0860 0.5528 0.054 Uiso 1 1 calc R . . C41 C 0.7413(3) 0.3910(4) 0.5324(4) 0.0375(15) Uani 1 1 d . . . C42 C 0.7202(4) 0.4386(4) 0.5803(4) 0.0437(17) Uani 1 1 d . . . H42 H 0.6906 0.4091 0.6015 0.052 Uiso 1 1 calc R . . C43 C 0.7417(4) 0.5296(5) 0.5984(5) 0.0497(18) Uani 1 1 d . . . H43 H 0.7281 0.5614 0.6324 0.060 Uiso 1 1 calc R . . C44 C 0.7839(4) 0.5728(5) 0.5650(5) 0.053(2) Uani 1 1 d . . . H44 H 0.7984 0.6347 0.5757 0.064 Uiso 1 1 calc R . . C45 C 0.8038(4) 0.5257(5) 0.5177(4) 0.0442(17) Uani 1 1 d . . . H45 H 0.8333 0.5551 0.4964 0.053 Uiso 1 1 calc R . . C46 C 0.7825(4) 0.4362(4) 0.4995(4) 0.0424(16) Uani 1 1 d . . . H46 H 0.7957 0.4054 0.4647 0.051 Uiso 1 1 calc R . . C47 C 0.6940(3) 0.2609(4) 0.4144(4) 0.0395(16) Uani 1 1 d . . . C48 C 0.6530(3) 0.3275(5) 0.3607(4) 0.0398(15) Uani 1 1 d . . . H48 H 0.6350 0.3803 0.3756 0.048 Uiso 1 1 calc R . . C49 C 0.6386(4) 0.3169(5) 0.2873(4) 0.0491(18) Uani 1 1 d . . . H49 H 0.6118 0.3634 0.2523 0.059 Uiso 1 1 calc R . . C50 C 0.6618(4) 0.2414(6) 0.2635(5) 0.059(2) Uani 1 1 d . . . H50 H 0.6500 0.2351 0.2120 0.071 Uiso 1 1 calc R . . C51 C 0.7021(4) 0.1746(6) 0.3130(5) 0.0537(19) Uani 1 1 d . . . H51 H 0.7188 0.1221 0.2964 0.064 Uiso 1 1 calc R . . C52 C 0.7182(4) 0.1845(5) 0.3880(5) 0.0464(17) Uani 1 1 d . . . H52 H 0.7464 0.1381 0.4225 0.056 Uiso 1 1 calc R . . C53 C 0.0873(10) 0.1907(13) 0.5283(10) 0.138(6) Uani 1 1 d . . . H53 H 0.0456 0.2314 0.5025 0.165 Uiso 1 1 calc R . . C54 C 0.0731(9) 0.1006(14) 0.5248(11) 0.144(6) Uani 1 1 d . . . H54 H 0.0218 0.0781 0.4992 0.173 Uiso 1 1 calc R . . C55 C 0.1342(9) 0.0424(9) 0.5588(9) 0.102(4) Uani 1 1 d . . . H55 H 0.1259 -0.0213 0.5528 0.122 Uiso 1 1 calc R . . C56 C 0.2064(7) 0.0747(8) 0.6008(8) 0.101(4) Uani 1 1 d . . . H56 H 0.2479 0.0344 0.6278 0.121 Uiso 1 1 calc R . . C57 C 0.2184(7) 0.1651(8) 0.6035(8) 0.096(4) Uani 1 1 d . . . H57 H 0.2693 0.1881 0.6313 0.115 Uiso 1 1 calc R . . C58 C 0.1590(9) 0.2243(9) 0.5673(8) 0.101(4) Uani 1 1 d . . . H58 H 0.1680 0.2879 0.5696 0.121 Uiso 1 1 calc R . . N1 N 0.5318(3) 0.2757(5) 0.7287(4) 0.0469(14) Uani 1 1 d . . . H1 H 0.524(4) 0.265(5) 0.683(5) 0.06(3) Uiso 1 1 d . . . N2 N 0.2780(3) 0.4767(4) 0.7146(4) 0.0488(16) Uani 1 1 d . . . N3 N 0.2138(3) 0.4593(4) 0.6586(4) 0.0549(17) Uani 1 1 d . . . O O 0.6203(3) 0.2758(4) 0.8515(3) 0.0560(13) Uani 1 1 d . . . P1 P 0.52230(8) 0.21390(12) 0.44129(9) 0.0346(4) Uani 1 1 d . . . P2 P 0.71526(8) 0.27138(11) 0.51222(9) 0.0347(3) Uani 1 1 d . . . S1 S 0.55445(8) 0.15747(11) 0.60860(10) 0.0382(4) Uani 1 1 d . . . S2 S 0.73771(8) 0.22918(13) 0.67288(10) 0.0410(4) Uani 1 1 d . . . Pt Pt 0.629594(14) 0.219517(16) 0.554638(16) 0.03257(8) 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 0.046(4) 0.039(3) 0.042(4) 0.008(3) 0.020(3) 0.005(3) C2 0.033(3) 0.046(4) 0.037(4) 0.010(3) 0.011(3) 0.010(3) C3 0.036(3) 0.045(3) 0.025(3) -0.004(3) 0.009(2) -0.006(3) C4 0.035(3) 0.042(3) 0.041(5) 0.001(3) 0.017(3) 0.000(2) C5 0.040(3) 0.043(3) 0.045(5) -0.001(3) 0.022(3) 0.003(3) C6 0.043(4) 0.062(4) 0.042(5) 0.000(4) 0.015(3) 0.012(3) C7 0.042(4) 0.076(5) 0.044(5) 0.005(4) 0.015(3) 0.014(4) C8 0.038(3) 0.043(4) 0.057(5) -0.002(3) 0.026(3) 0.003(3) C9 0.042(4) 0.045(4) 0.051(5) -0.010(3) 0.022(3) -0.002(3) C10 0.041(3) 0.043(4) 0.045(5) -0.005(3) 0.021(3) -0.005(3) C11 0.044(4) 0.064(5) 0.059(6) 0.020(4) 0.032(4) 0.021(3) C12 0.051(4) 0.101(7) 0.036(5) 0.004(4) 0.018(4) 0.019(4) C13 0.051(5) 0.151(10) 0.036(6) 0.001(6) 0.014(4) 0.029(6) C14 0.068(6) 0.125(9) 0.065(7) 0.038(6) 0.040(5) 0.047(6) C15 0.092(7) 0.070(6) 0.115(10) 0.031(6) 0.071(7) 0.032(5) C16 0.052(4) 0.059(5) 0.100(8) 0.010(5) 0.047(5) 0.005(4) C17 0.034(3) 0.038(3) 0.037(4) -0.007(3) 0.016(3) -0.005(3) C18 0.045(4) 0.041(4) 0.047(5) -0.001(3) 0.018(3) -0.002(3) C19 0.056(4) 0.061(4) 0.034(5) -0.006(3) 0.020(3) 0.000(4) C20 0.056(4) 0.047(4) 0.064(6) -0.011(4) 0.034(4) -0.004(3) C21 0.055(4) 0.042(4) 0.053(5) -0.003(3) 0.029(4) 0.003(3) C22 0.038(3) 0.039(3) 0.042(4) -0.001(3) 0.015(3) 0.002(3) C23 0.036(3) 0.028(3) 0.033(4) 0.005(3) 0.009(3) 0.004(2) C24 0.043(3) 0.038(3) 0.049(5) 0.001(3) 0.024(3) 0.003(3) C25 0.045(4) 0.037(3) 0.049(5) -0.002(3) 0.018(3) -0.008(3) C26 0.033(3) 0.060(4) 0.047(5) 0.006(4) 0.013(3) -0.003(3) C27 0.042(3) 0.047(4) 0.054(5) 0.002(4) 0.024(3) 0.002(3) C28 0.038(3) 0.038(3) 0.046(4) -0.004(3) 0.017(3) -0.001(3) C29 0.031(3) 0.037(3) 0.044(4) 0.000(3) 0.015(3) 0.002(3) C30 0.038(3) 0.044(4) 0.042(5) 0.005(3) 0.012(3) 0.000(3) C31 0.049(4) 0.060(4) 0.048(5) 0.014(4) 0.015(4) 0.013(3) C32 0.054(4) 0.039(4) 0.077(7) 0.007(4) 0.024(4) 0.006(3) C33 0.047(4) 0.037(4) 0.077(7) 0.003(4) 0.019(4) -0.002(3) C34 0.039(3) 0.041(4) 0.059(6) -0.012(3) 0.017(3) -0.005(3) C35 0.029(3) 0.044(3) 0.035(4) -0.001(3) 0.013(2) 0.004(3) C36 0.038(4) 0.046(4) 0.078(7) -0.002(4) 0.010(4) 0.002(3) C37 0.035(4) 0.068(6) 0.074(7) -0.007(4) 0.007(4) -0.001(3) C38 0.036(4) 0.053(5) 0.082(7) 0.003(4) 0.008(4) 0.010(3) C39 0.046(4) 0.049(4) 0.067(6) 0.003(4) 0.021(4) 0.014(3) C40 0.045(4) 0.049(4) 0.040(5) 0.004(3) 0.019(3) 0.004(3) C41 0.027(3) 0.044(3) 0.039(4) -0.003(3) 0.012(3) 0.002(3) C42 0.036(3) 0.046(4) 0.047(5) -0.001(3) 0.017(3) -0.002(3) C43 0.059(4) 0.048(4) 0.048(5) -0.015(3) 0.029(4) -0.008(3) C44 0.050(4) 0.043(4) 0.058(6) -0.003(4) 0.016(4) -0.007(3) C45 0.041(4) 0.048(4) 0.045(5) 0.000(3) 0.020(3) -0.003(3) C46 0.036(3) 0.046(4) 0.038(4) -0.001(3) 0.010(3) 0.003(3) C47 0.030(3) 0.038(3) 0.048(5) -0.005(3) 0.015(3) -0.005(2) C48 0.036(3) 0.052(4) 0.029(4) -0.003(3) 0.012(3) -0.001(3) C49 0.042(4) 0.059(4) 0.038(5) 0.001(3) 0.010(3) -0.012(3) C50 0.058(4) 0.077(6) 0.047(5) -0.018(4) 0.028(4) -0.025(4) C51 0.056(4) 0.065(5) 0.048(5) -0.009(4) 0.030(4) 0.001(4) C52 0.046(4) 0.051(4) 0.047(5) -0.005(3) 0.024(3) 0.003(3) C53 0.133(13) 0.152(16) 0.123(15) 0.057(12) 0.052(11) 0.032(11) C54 0.097(10) 0.166(16) 0.159(18) 0.025(13) 0.047(10) -0.012(11) C55 0.126(10) 0.097(8) 0.097(10) -0.004(8) 0.062(8) 0.000(9) C56 0.097(8) 0.077(7) 0.119(12) -0.005(7) 0.040(8) 0.002(6) C57 0.101(8) 0.082(7) 0.106(11) 0.001(7) 0.045(7) -0.009(7) C58 0.137(10) 0.080(7) 0.102(10) 0.024(7) 0.068(9) 0.007(8) N1 0.039(3) 0.059(4) 0.038(4) 0.004(3) 0.012(3) 0.011(3) N2 0.042(3) 0.046(3) 0.060(5) 0.007(3) 0.025(3) 0.011(3) N3 0.047(3) 0.059(4) 0.062(5) 0.016(3) 0.026(3) 0.010(3) O 0.049(3) 0.083(4) 0.035(3) -0.006(3) 0.018(2) 0.004(3) P1 0.0310(7) 0.0351(8) 0.0319(9) 0.0000(8) 0.0086(6) 0.0015(7) P2 0.0311(7) 0.0387(8) 0.0310(9) -0.0019(8) 0.0107(6) 0.0012(7) S1 0.0355(7) 0.0385(8) 0.0386(10) 0.0013(7) 0.0146(7) -0.0007(6) S2 0.0295(7) 0.0573(10) 0.0315(9) 0.0006(9) 0.0094(6) 0.0034(8) Pt 0.02850(11) 0.03472(11) 0.03042(13) -0.00044(14) 0.00931(8) 0.00184(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 C1 C2 1.541(10) . ? C1 S1 1.823(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.517(9) . ? C2 C3 1.545(9) . ? C2 H2 1.0000 . ? C3 S2 1.805(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O 1.232(9) . ? C4 N1 1.364(9) . ? C5 C10 1.388(10) . ? C5 C6 1.389(10) . ? C5 N1 1.406(8) . ? C6 C7 1.371(9) . ? C6 H6 0.9500 . ? C7 C8 1.367(11) . ? C7 H7 0.9500 . ? C8 C9 1.376(10) . ? C8 N2 1.438(8) . ? C9 C10 1.399(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.361(12) . ? C11 C12 1.376(11) . ? C11 N3 1.445(9) . ? C12 C13 1.381(12) . ? C12 H12 0.9500 . ? C13 C14 1.352(15) . ? C13 H13 0.9500 . ? C14 C15 1.360(15) . ? C14 H14 0.9500 . ? C15 C16 1.386(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.388(9) . ? C17 C18 1.400(10) . ? C17 P1 1.814(7) . ? C18 C19 1.381(10) . ? C18 H18 0.9500 . ? C19 C20 1.376(10) . ? C19 H19 0.9500 . ? C20 C21 1.369(11) . ? C20 H20 0.9500 . ? C21 C22 1.397(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.392(9) . ? C23 C28 1.403(9) . ? C23 P1 1.826(6) . ? C24 C25 1.394(9) . ? C24 H24 0.9500 . ? C25 C26 1.378(10) . ? C25 H25 0.9500 . ? C26 C27 1.391(10) . ? C26 H26 0.9500 . ? C27 C28 1.379(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.381(9) . ? C29 C30 1.412(9) . ? C29 P1 1.815(7) . ? C30 C31 1.387(9) . ? C30 H30 0.9500 . ? C31 C32 1.380(11) . ? C31 H31 0.9500 . ? C32 C33 1.382(11) . ? C32 H32 0.9500 . ? C33 C34 1.395(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.402(9) . ? C35 C36 1.409(9) . ? C35 P2 1.816(6) . ? C36 C37 1.395(10) . ? C36 H36 0.9500 . ? C37 C38 1.363(10) . ? C37 H37 0.9500 . ? C38 C39 1.374(10) . ? C38 H38 0.9500 . ? C39 C40 1.389(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.382(10) . ? C41 C46 1.400(10) . ? C41 P2 1.826(6) . ? C42 C43 1.400(9) . ? C42 H42 0.9500 . ? C43 C44 1.408(11) . ? C43 H43 0.9500 . ? C44 C45 1.352(11) . ? C44 H44 0.9500 . ? C45 C46 1.380(9) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.404(9) . ? C47 C48 1.407(9) . ? C47 P2 1.810(8) . ? C48 C49 1.370(10) . ? C48 H48 0.9500 . ? C49 C50 1.359(11) . ? C49 H49 0.9500 . ? C50 C51 1.365(12) . ? C50 H50 0.9500 . ? C51 C52 1.391(11) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.34(2) . ? C53 C54 1.35(2) . ? C53 H53 0.9500 . ? C54 C55 1.369(19) . ? C54 H54 0.9500 . ? C55 C56 1.353(16) . ? C55 H55 0.9500 . ? C56 C57 1.347(14) . ? C56 H56 0.9500 . ? C57 C58 1.364(15) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? N1 H1 0.87(9) . ? N2 N3 1.273(9) . ? P1 Pt 2.2904(16) . ? P2 Pt 2.2909(16) . ? S1 Pt 2.3355(17) . ? S2 Pt 2.3585(16) . ? 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 S1 117.4(4) . . ? C2 C1 H1A 107.9 . . ? S1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? S1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C4 C2 C1 114.6(5) . . ? C4 C2 C3 110.5(5) . . ? C1 C2 C3 111.6(6) . . ? C4 C2 H2 106.5 . . ? C1 C2 H2 106.5 . . ? C3 C2 H2 106.5 . . ? C2 C3 S2 114.8(5) . . ? C2 C3 H3A 108.6 . . ? S2 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? S2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? O C4 N1 122.6(6) . . ? O C4 C2 123.6(6) . . ? N1 C4 C2 113.7(7) . . ? C10 C5 C6 119.6(6) . . ? C10 C5 N1 124.6(6) . . ? C6 C5 N1 115.7(7) . . ? C7 C6 C5 120.4(7) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 121.0(7) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 119.1(6) . . ? C7 C8 N2 125.0(7) . . ? C9 C8 N2 115.8(7) . . ? C8 C9 C10 121.3(7) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C5 C10 C9 118.5(6) . . ? C5 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C16 C11 C12 121.4(7) . . ? C16 C11 N3 123.5(7) . . ? C12 C11 N3 115.0(8) . . ? C13 C12 C11 117.5(9) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? C14 C13 C12 122.0(9) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.7(9) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.0(10) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.4(8) . . ? C11 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C22 C17 C18 119.1(6) . . ? C22 C17 P1 115.6(5) . . ? C18 C17 P1 125.1(5) . . ? C19 C18 C17 119.2(7) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 122.0(8) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C21 C20 C19 118.8(7) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 121.0(7) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C17 C22 C21 119.9(7) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C28 118.8(6) . . ? C24 C23 P1 122.3(5) . . ? C28 C23 P1 118.9(4) . . ? C23 C24 C25 120.5(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.9(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.3(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.0(7) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 120.5(6) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C34 C29 C30 118.6(6) . . ? C34 C29 P1 120.3(5) . . ? C30 C29 P1 121.0(5) . . ? C31 C30 C29 119.8(7) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 120.6(7) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.3(7) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 119.4(7) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C29 C34 C33 121.3(7) . . ? C29 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C40 C35 C36 118.3(6) . . ? C40 C35 P2 118.6(5) . . ? C36 C35 P2 123.0(5) . . ? C37 C36 C35 119.5(7) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 121.2(7) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 119.9(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.6(7) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 120.2(6) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C42 C41 C46 118.8(6) . . ? C42 C41 P2 120.3(5) . . ? C46 C41 P2 120.9(5) . . ? C41 C42 C43 121.2(7) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C42 C43 C44 118.5(7) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C45 C44 C43 119.8(7) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 121.9(7) . . ? C44 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C45 C46 C41 119.7(7) . . ? C45 C46 H46 120.2 . . ? C41 C46 H46 120.2 . . ? C52 C47 C48 116.3(7) . . ? C52 C47 P2 121.0(5) . . ? C48 C47 P2 122.7(5) . . ? C49 C48 C47 120.7(7) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.6 . . ? C50 C49 C48 121.4(8) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C49 C50 C51 120.5(8) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C50 C51 C52 119.0(7) . . ? C50 C51 H51 120.5 . . ? C52 C51 H51 120.5 . . ? C51 C52 C47 122.1(7) . . ? C51 C52 H52 119.0 . . ? C47 C52 H52 119.0 . . ? C58 C53 C54 121.6(15) . . ? C58 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C53 C54 C55 118.7(15) . . ? C53 C54 H54 120.7 . . ? C55 C54 H54 120.7 . . ? C56 C55 C54 120.6(13) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C57 C56 C55 118.9(12) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C56 C57 C58 121.4(12) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C53 C58 C57 118.6(13) . . ? C53 C58 H58 120.7 . . ? C57 C58 H58 120.7 . . ? C4 N1 C5 130.0(7) . . ? C4 N1 H1 119(5) . . ? C5 N1 H1 111(5) . . ? N3 N2 C8 112.6(6) . . ? N2 N3 C11 112.3(7) . . ? C29 P1 C17 110.8(3) . . ? C29 P1 C23 99.7(3) . . ? C17 P1 C23 102.9(3) . . ? C29 P1 Pt 114.1(2) . . ? C17 P1 Pt 111.0(2) . . ? C23 P1 Pt 117.3(2) . . ? C47 P2 C35 102.3(3) . . ? C47 P2 C41 103.2(3) . . ? C35 P2 C41 105.1(3) . . ? C47 P2 Pt 120.68(19) . . ? C35 P2 Pt 109.5(2) . . ? C41 P2 Pt 114.4(2) . . ? C1 S1 Pt 107.4(2) . . ? C3 S2 Pt 101.34(19) . . ? P1 Pt P2 97.65(6) . . ? P1 Pt S1 88.01(6) . . ? P2 Pt S1 173.30(6) . . ? P1 Pt S2 177.90(6) . . ? P2 Pt S2 83.38(6) . . ? S1 Pt S2 91.08(6) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.200 _refine_diff_density_min -1.501 _refine_diff_density_rms 0.099 # Attachment 'i0194.cif' data_i0194 _database_code_depnum_ccdc_archive 'CCDC 723724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 I N2 O2 S2' _chemical_formula_sum 'C16 H13 I N2 O2 S2' _chemical_formula_weight 456.30 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.938(3) _cell_length_b 5.0191(3) _cell_length_c 11.4987(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.528(8) _cell_angle_gamma 90.00 _cell_volume 1659.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9454 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.04 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.294 _exptl_crystal_size_mid 0.244 _exptl_crystal_size_min 0.064 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.191 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6304 _exptl_absorpt_correction_T_max 0.8572 _exptl_absorpt_process_details 'X-red ver.1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 153(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 152 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 8385 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2891 _reflns_number_gt 2372 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^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_extinction_coef ? _refine_ls_number_reflns 2891 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 0.35544(14) 2.3061(9) 1.3107(3) 0.0351(9) Uani 1 1 d . . . C2 C 0.38807(16) 2.5408(9) 1.3162(4) 0.0404(10) Uani 1 1 d . . . H2 H 0.3693 2.7069 1.3215 0.048 Uiso 1 1 calc R . . C3 C 0.42406(17) 2.5274(9) 1.4232(4) 0.0436(11) Uani 1 1 d . . . H3A H 0.4089 2.4756 1.4928 0.052 Uiso 1 1 calc R . . H3B H 0.4386 2.7044 1.4382 0.052 Uiso 1 1 calc R . . C4 C 0.41437(17) 2.5622(10) 1.2078(4) 0.0468(11) Uani 1 1 d . . . H4A H 0.4309 2.7349 1.2077 0.056 Uiso 1 1 calc R . . H4B H 0.3923 2.5503 1.1355 0.056 Uiso 1 1 calc R . . C5 C 0.29616(15) 2.0961(9) 1.1800(4) 0.0379(10) Uani 1 1 d . . . C6 C 0.26028(16) 2.0594(10) 1.2478(4) 0.0438(10) Uani 1 1 d . . . H6 H 0.2582 2.1649 1.3156 0.053 Uiso 1 1 calc R . . C7 C 0.22766(17) 1.8666(10) 1.2149(5) 0.0537(13) Uani 1 1 d . . . H7 H 0.2031 1.8369 1.2614 0.064 Uiso 1 1 calc R . . C8 C 0.22996(16) 1.7163(10) 1.1160(5) 0.0553(15) Uani 1 1 d . . . C9 C 0.2666(2) 1.7541(11) 1.0487(5) 0.0593(15) Uani 1 1 d . . . H9 H 0.2686 1.6483 0.9810 0.071 Uiso 1 1 calc R . . C10 C 0.30037(17) 1.9474(11) 1.0809(4) 0.0480(11) Uani 1 1 d . . . H10 H 0.3255 1.9756 1.0359 0.058 Uiso 1 1 calc R . . C11 C 0.15367(18) 1.2207(10) 0.9879(5) 0.0555(14) Uani 1 1 d . . . C12 C 0.1199(2) 1.1457(10) 1.0594(4) 0.0592(17) Uani 1 1 d . . . H12 H 0.1197 1.2242 1.1346 0.071 Uiso 1 1 calc R . . C13 C 0.08616(18) 0.9551(9) 1.0206(4) 0.0440(11) Uani 1 1 d . . . H13 H 0.0632 0.9025 1.0687 0.053 Uiso 1 1 calc R . . C14 C 0.08723(15) 0.8455(8) 0.9105(3) 0.0346(9) Uani 1 1 d . . . C15 C 0.12098(14) 0.9199(9) 0.8397(4) 0.0389(10) Uani 1 1 d . . . H15 H 0.1214 0.8425 0.7644 0.047 Uiso 1 1 calc R . . C16 C 0.15382(18) 1.1079(10) 0.8803(5) 0.0513(12) Uani 1 1 d . . . H16 H 0.1769 1.1592 0.8323 0.062 Uiso 1 1 calc R . . I I 0.036852(9) 0.56800(6) 0.84273(2) 0.03723(11) Uani 1 1 d . . . N1 N 0.1885(2) 1.5140(11) 1.0984(4) 0.0721(16) Uani 1 1 d . . . N2 N 0.19468(18) 1.4284(10) 1.0089(4) 0.0637(13) Uani 1 1 d . . . O1 O 0.32887(11) 2.2986(7) 1.2052(3) 0.0443(8) Uani 1 1 d . . . O2 O 0.35159(11) 2.1471(6) 1.3871(3) 0.0410(7) Uani 1 1 d . . . S1 S 0.46829(4) 2.2822(3) 1.39684(10) 0.0443(3) Uani 1 1 d . . . S2 S 0.45558(4) 2.2892(3) 1.21412(10) 0.0467(3) 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 0.035(2) 0.030(2) 0.041(2) -0.0036(18) 0.0008(17) 0.0074(19) C2 0.038(2) 0.029(2) 0.052(2) -0.0023(19) -0.001(2) 0.000(2) C3 0.041(3) 0.037(2) 0.051(2) -0.0128(19) -0.002(2) 0.002(2) C4 0.046(3) 0.039(3) 0.053(3) 0.010(2) -0.004(2) -0.017(2) C5 0.033(2) 0.037(2) 0.042(2) 0.0075(18) -0.0006(17) -0.008(2) C6 0.035(2) 0.042(3) 0.055(3) 0.010(2) 0.006(2) -0.002(2) C7 0.036(3) 0.046(3) 0.077(3) 0.019(3) 0.002(2) -0.005(2) C8 0.031(2) 0.040(3) 0.087(4) 0.021(3) -0.025(3) -0.013(2) C9 0.067(4) 0.053(3) 0.052(3) -0.009(2) -0.015(3) -0.002(3) C10 0.044(3) 0.060(3) 0.040(2) -0.001(2) 0.005(2) -0.009(3) C11 0.045(3) 0.032(3) 0.083(4) 0.010(3) -0.022(3) -0.006(2) C12 0.087(4) 0.035(3) 0.047(3) -0.013(2) -0.030(3) 0.011(3) C13 0.055(3) 0.038(2) 0.038(2) 0.0043(19) 0.001(2) 0.000(2) C14 0.034(2) 0.030(2) 0.038(2) -0.0002(17) -0.0018(17) 0.0034(18) C15 0.029(2) 0.039(2) 0.048(2) 0.0054(19) 0.0021(18) 0.001(2) C16 0.039(3) 0.041(3) 0.071(3) 0.008(2) -0.006(2) -0.007(2) I 0.03212(16) 0.03308(17) 0.04535(17) 0.00284(12) -0.00050(11) -0.00326(13) N1 0.084(4) 0.085(4) 0.050(3) 0.027(2) 0.020(2) 0.051(3) N2 0.075(3) 0.073(3) 0.046(2) 0.014(2) 0.021(2) 0.039(3) O1 0.0429(18) 0.0416(18) 0.0452(16) 0.0105(14) -0.0083(13) -0.0160(15) O2 0.0421(17) 0.0388(17) 0.0418(16) 0.0040(13) 0.0029(13) -0.0036(14) S1 0.0374(6) 0.0478(7) 0.0472(6) 0.0023(5) 0.0024(5) 0.0059(5) S2 0.0502(7) 0.0442(7) 0.0459(6) -0.0060(5) 0.0067(5) -0.0056(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.201(5) . ? C1 O1 1.362(5) . ? C1 C2 1.506(6) . ? C2 C3 1.521(6) . ? C2 C4 1.536(7) . ? C2 H2 1.0000 . ? C3 S1 1.826(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S2 1.813(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.379(7) . ? C5 C6 1.380(7) . ? C5 O1 1.397(5) . ? C6 C7 1.375(7) . ? C6 H6 0.9500 . ? C7 C8 1.372(8) . ? C7 H7 0.9500 . ? C8 C9 1.395(8) . ? C8 N1 1.567(8) . ? C9 C10 1.397(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.361(8) . ? C11 C12 1.399(9) . ? C11 N2 1.577(7) . ? C12 C13 1.402(7) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.391(6) . ? C14 I 2.101(4) . ? C15 C16 1.382(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N1 N2 1.148(6) . ? S1 S2 2.0916(16) . ? 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 O2 C1 O1 122.9(4) . . ? O2 C1 C2 126.8(4) . . ? O1 C1 C2 110.3(4) . . ? C1 C2 C3 111.6(4) . . ? C1 C2 C4 112.8(4) . . ? C3 C2 C4 107.6(4) . . ? C1 C2 H2 108.2 . . ? C3 C2 H2 108.2 . . ? C4 C2 H2 108.2 . . ? C2 C3 S1 108.9(3) . . ? C2 C3 H3A 109.9 . . ? S1 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? S1 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C2 C4 S2 107.4(3) . . ? C2 C4 H4A 110.2 . . ? S2 C4 H4A 110.2 . . ? C2 C4 H4B 110.2 . . ? S2 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C10 C5 C6 122.5(4) . . ? C10 C5 O1 116.3(4) . . ? C6 C5 O1 121.1(4) . . ? C7 C6 C5 118.4(5) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C8 C7 C6 121.3(5) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 119.7(5) . . ? C7 C8 N1 110.8(5) . . ? C9 C8 N1 129.5(5) . . ? C8 C9 C10 120.0(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C5 C10 C9 118.1(5) . . ? C5 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C16 C11 C12 119.8(5) . . ? C16 C11 N2 109.5(5) . . ? C12 C11 N2 130.7(5) . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 121.2(4) . . ? C13 C14 I 121.1(3) . . ? C15 C14 I 117.7(3) . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C11 C16 C15 121.2(5) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? N2 N1 C8 99.4(6) . . ? N1 N2 C11 101.1(5) . . ? C1 O1 C5 120.4(3) . . ? C3 S1 S2 96.26(16) . . ? C4 S2 S1 95.33(16) . . ? 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 O2 C1 C2 C3 11.7(7) . . . . ? O1 C1 C2 C3 -169.7(4) . . . . ? O2 C1 C2 C4 133.0(5) . . . . ? O1 C1 C2 C4 -48.4(5) . . . . ? C1 C2 C3 S1 76.5(4) . . . . ? C4 C2 C3 S1 -47.7(4) . . . . ? C1 C2 C4 S2 -70.2(4) . . . . ? C3 C2 C4 S2 53.3(4) . . . . ? C10 C5 C6 C7 0.1(7) . . . . ? O1 C5 C6 C7 176.4(4) . . . . ? C5 C6 C7 C8 -1.1(7) . . . . ? C6 C7 C8 C9 1.6(7) . . . . ? C6 C7 C8 N1 -179.5(4) . . . . ? C7 C8 C9 C10 -1.1(8) . . . . ? N1 C8 C9 C10 -179.7(4) . . . . ? C6 C5 C10 C9 0.4(7) . . . . ? O1 C5 C10 C9 -176.0(4) . . . . ? C8 C9 C10 C5 0.1(8) . . . . ? C16 C11 C12 C13 0.0(7) . . . . ? N2 C11 C12 C13 179.4(4) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? C12 C13 C14 C15 0.5(7) . . . . ? C12 C13 C14 I -178.0(3) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? I C14 C15 C16 178.1(3) . . . . ? C12 C11 C16 C15 0.2(7) . . . . ? N2 C11 C16 C15 -179.4(4) . . . . ? C14 C15 C16 C11 0.0(7) . . . . ? C7 C8 N1 N2 174.2(4) . . . . ? C9 C8 N1 N2 -7.0(7) . . . . ? C8 N1 N2 C11 179.6(3) . . . . ? C16 C11 N2 N1 176.5(4) . . . . ? C12 C11 N2 N1 -3.0(7) . . . . ? O2 C1 O1 C5 -1.8(6) . . . . ? C2 C1 O1 C5 179.6(4) . . . . ? C10 C5 O1 C1 -124.1(5) . . . . ? C6 C5 O1 C1 59.4(6) . . . . ? C2 C3 S1 S2 21.5(4) . . . . ? C2 C4 S2 S1 -33.0(3) . . . . ? C3 S1 S2 C4 6.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.009 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.089 # Attachment 'i0197.cif' data_i0197 _database_code_depnum_ccdc_archive 'CCDC 723725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C45 H44 O4 P2 Pt S2), C6 H6' _chemical_formula_sum 'C96 H94 O8 P4 Pt2 S4' _chemical_formula_weight 2018.01 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 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.7209(16) _cell_length_b 15.7228(7) _cell_length_c 29.671(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.562(5) _cell_angle_gamma 90.00 _cell_volume 8899.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 16046 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.84 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 3.361 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3804 _exptl_absorpt_correction_T_max 0.5290 _exptl_absorpt_process_details 'X-red ver 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 298(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 59875 _diffrn_reflns_av_R_equivalents 0.1619 _diffrn_reflns_av_sigmaI/netI 0.1819 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.71 _reflns_number_total 16484 _reflns_number_gt 7063 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^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_extinction_coef ? _refine_ls_number_reflns 16484 _refine_ls_number_parameters 985 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1557 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 0.773 _refine_ls_restrained_S_all 0.773 _refine_ls_shift/su_max 0.002 _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 0.5079(5) 0.5742(7) 0.8347(5) 0.056(3) Uani 1 1 d . . . H1B H 0.4877 0.5278 0.8103 0.067 Uiso 1 1 calc R . . H1A H 0.5459 0.5509 0.8659 0.067 Uiso 1 1 calc R . . C2 C 0.4521(6) 0.6093(9) 0.8468(4) 0.054(3) Uani 1 1 d . . . C3 C 0.4061(6) 0.6757(7) 0.8067(4) 0.052(3) Uani 1 1 d . . . H3B H 0.4339 0.7266 0.8119 0.063 Uiso 1 1 calc R . . H3A H 0.3677 0.6905 0.8131 0.063 Uiso 1 1 calc R . . C4 C 0.4070(7) 0.5329(10) 0.8472(5) 0.062(4) Uani 1 1 d . . . C5 C 0.3122(8) 0.4999(10) 0.8608(6) 0.101(5) Uani 1 1 d . . . H5A H 0.3379 0.4549 0.8849 0.121 Uiso 1 1 calc R . . H5B H 0.2844 0.4754 0.8270 0.121 Uiso 1 1 calc R . . C6 C 0.2663(8) 0.5476(11) 0.8778(8) 0.134(7) Uani 1 1 d . . . H6A H 0.2950 0.5723 0.9110 0.161 Uiso 1 1 calc R . . H6B H 0.2333 0.5090 0.8796 0.161 Uiso 1 1 calc R . . H6C H 0.2414 0.5918 0.8535 0.161 Uiso 1 1 calc R . . C7 C 0.4851(7) 0.6492(10) 0.8995(6) 0.063(4) Uani 1 1 d . . . C8 C 0.5477(10) 0.6112(14) 0.9884(6) 0.126(7) Uani 1 1 d . . . H8B H 0.5676 0.6679 0.9939 0.152 Uiso 1 1 calc R . . H8A H 0.5849 0.5717 1.0090 0.152 Uiso 1 1 calc R . . C9 C 0.4925(13) 0.608(2) 1.0045(10) 0.268(16) Uani 1 1 d . . . H9C H 0.4712 0.5531 0.9974 0.321 Uiso 1 1 calc R . . H9B H 0.4575 0.6506 0.9858 0.321 Uiso 1 1 calc R . . H9A H 0.5132 0.6199 1.0406 0.321 Uiso 1 1 calc R . . C10 C 0.3721(5) 0.7306(7) 0.5961(4) 0.045(3) Uani 1 1 d . . . C11 C 0.4208(6) 0.7952(8) 0.6171(5) 0.061(3) Uani 1 1 d . . . H11A H 0.4567 0.7909 0.6507 0.073 Uiso 1 1 calc R . . C12 C 0.4163(7) 0.8665(9) 0.5881(6) 0.078(4) Uani 1 1 d . . . H12A H 0.4504 0.9086 0.6016 0.093 Uiso 1 1 calc R . . C13 C 0.3622(8) 0.8745(9) 0.5402(7) 0.082(5) Uani 1 1 d . . . H13A H 0.3592 0.9232 0.5215 0.098 Uiso 1 1 calc R . . C14 C 0.3115(7) 0.8133(9) 0.5183(6) 0.082(4) Uani 1 1 d . . . H14A H 0.2744 0.8191 0.4852 0.099 Uiso 1 1 calc R . . C15 C 0.3184(6) 0.7428(8) 0.5478(5) 0.067(3) Uani 1 1 d . . . H15A H 0.2843 0.7008 0.5339 0.080 Uiso 1 1 calc R . . C16 C 0.3889(5) 0.5434(8) 0.6050(5) 0.050(3) Uani 1 1 d . . . C17 C 0.3737(6) 0.5374(9) 0.5553(5) 0.068(3) Uani 1 1 d . . . H17A H 0.3545 0.5835 0.5333 0.082 Uiso 1 1 calc R . . C18 C 0.3870(8) 0.4621(10) 0.5372(6) 0.094(5) Uani 1 1 d . . . H18A H 0.3756 0.4583 0.5028 0.113 Uiso 1 1 calc R . . C19 C 0.4154(8) 0.3954(11) 0.5673(7) 0.093(5) Uani 1 1 d . . . H19A H 0.4264 0.3469 0.5546 0.111 Uiso 1 1 calc R . . C20 C 0.4285(7) 0.3981(10) 0.6174(7) 0.082(4) Uani 1 1 d . . . H20A H 0.4457 0.3502 0.6382 0.099 Uiso 1 1 calc R . . C21 C 0.4162(6) 0.4713(8) 0.6368(6) 0.069(4) Uani 1 1 d . . . H21A H 0.4258 0.4735 0.6708 0.083 Uiso 1 1 calc R . . C22 C 0.2853(5) 0.6308(8) 0.6210(4) 0.052(3) Uani 1 1 d . . . C23 C 0.2531(6) 0.7042(8) 0.6267(5) 0.062(3) Uani 1 1 d . . . H23A H 0.2784 0.7544 0.6386 0.075 Uiso 1 1 calc R . . C24 C 0.1830(7) 0.7009(11) 0.6144(6) 0.082(4) Uani 1 1 d . . . H24A H 0.1605 0.7501 0.6163 0.098 Uiso 1 1 calc R . . C25 C 0.1475(7) 0.6281(14) 0.5998(6) 0.097(6) Uani 1 1 d . . . H25A H 0.1008 0.6268 0.5925 0.117 Uiso 1 1 calc R . . C26 C 0.1785(7) 0.5554(11) 0.5955(6) 0.086(5) Uani 1 1 d . . . H26A H 0.1533 0.5048 0.5858 0.103 Uiso 1 1 calc R . . C27 C 0.2484(6) 0.5573(8) 0.6057(5) 0.068(4) Uani 1 1 d . . . H27A H 0.2695 0.5082 0.6020 0.082 Uiso 1 1 calc R . . C28 C 0.5610(5) 0.6620(8) 0.6511(5) 0.048(3) Uani 1 1 d . . . C29 C 0.5366(5) 0.5980(10) 0.6144(5) 0.059(3) Uani 1 1 d . . . H29A H 0.5240 0.5458 0.6223 0.071 Uiso 1 1 calc R . . C30 C 0.5305(7) 0.6110(10) 0.5646(6) 0.074(4) Uani 1 1 d . . . H30A H 0.5103 0.5701 0.5389 0.089 Uiso 1 1 calc R . . C31 C 0.5558(9) 0.6863(12) 0.5561(7) 0.102(5) Uani 1 1 d . . . H31A H 0.5563 0.6948 0.5252 0.122 Uiso 1 1 calc R . . C32 C 0.5802(9) 0.7489(11) 0.5927(7) 0.112(6) Uani 1 1 d . . . H32A H 0.5952 0.8002 0.5856 0.134 Uiso 1 1 calc R . . C33 C 0.5833(7) 0.7379(9) 0.6401(5) 0.074(4) Uani 1 1 d . . . H33A H 0.6002 0.7812 0.6644 0.088 Uiso 1 1 calc R . . C34 C 0.6268(6) 0.7177(8) 0.7546(5) 0.055(3) Uani 1 1 d . . . C35 C 0.6055(7) 0.7986(11) 0.7552(5) 0.080(4) Uani 1 1 d . . . H35A H 0.5584 0.8131 0.7359 0.096 Uiso 1 1 calc R . . C36 C 0.6544(9) 0.8599(11) 0.7848(8) 0.106(6) Uani 1 1 d . . . H36A H 0.6393 0.9153 0.7846 0.128 Uiso 1 1 calc R . . C37 C 0.7226(11) 0.8418(13) 0.8136(8) 0.112(6) Uani 1 1 d . . . H37A H 0.7546 0.8839 0.8325 0.135 Uiso 1 1 calc R . . C38 C 0.7423(8) 0.7649(13) 0.8144(7) 0.114(6) Uani 1 1 d . . . H38A H 0.7893 0.7515 0.8354 0.137 Uiso 1 1 calc R . . C39 C 0.6968(6) 0.7005(9) 0.7852(6) 0.081(4) Uani 1 1 d . . . H39A H 0.7138 0.6458 0.7864 0.098 Uiso 1 1 calc R . . C40 C 0.6013(5) 0.5359(8) 0.7274(4) 0.053(3) Uani 1 1 d . . . C41 C 0.5793(6) 0.4735(8) 0.7503(5) 0.058(3) Uani 1 1 d . . . H41A H 0.5444 0.4864 0.7589 0.069 Uiso 1 1 calc R . . C42 C 0.6080(6) 0.3942(9) 0.7602(6) 0.069(4) Uani 1 1 d . . . H42A H 0.5914 0.3532 0.7743 0.083 Uiso 1 1 calc R . . C43 C 0.6615(7) 0.3742(8) 0.7497(5) 0.068(3) Uani 1 1 d . . . H43A H 0.6812 0.3201 0.7568 0.082 Uiso 1 1 calc R . . C44 C 0.6858(7) 0.4354(9) 0.7284(5) 0.073(4) Uani 1 1 d . . . H44A H 0.7220 0.4225 0.7212 0.087 Uiso 1 1 calc R . . C45 C 0.6563(6) 0.5150(8) 0.7179(5) 0.060(3) Uani 1 1 d . . . H45A H 0.6735 0.5559 0.7041 0.072 Uiso 1 1 calc R . . C46 C -0.0149(7) 0.4612(9) 0.8291(5) 0.084(4) Uani 1 1 d . . . H46B H 0.0203 0.4886 0.8600 0.100 Uiso 1 1 calc R . . H46A H -0.0398 0.5054 0.8041 0.100 Uiso 1 1 calc R . . C47 C -0.0678(7) 0.4139(9) 0.8419(5) 0.063(4) Uani 1 1 d . . . C48 C -0.1131(6) 0.3561(8) 0.7964(5) 0.061(3) Uani 1 1 d . . . H48B H -0.1537 0.3403 0.8000 0.074 Uiso 1 1 calc R . . H48A H -0.0866 0.3044 0.8006 0.074 Uiso 1 1 calc R . . C49 C -0.1171(8) 0.4825(10) 0.8451(5) 0.077(4) Uani 1 1 d . . . C50 C -0.2115(9) 0.4979(10) 0.8663(6) 0.103(5) Uani 1 1 d . . . H50A H -0.1891 0.5497 0.8846 0.123 Uiso 1 1 calc R . . H50B H -0.2487 0.5137 0.8326 0.123 Uiso 1 1 calc R . . C51 C -0.2407(9) 0.4535(11) 0.8937(8) 0.131(7) Uani 1 1 d . . . H51A H -0.2679 0.4922 0.9021 0.157 Uiso 1 1 calc R . . H51B H -0.2035 0.4301 0.9247 0.157 Uiso 1 1 calc R . . H51C H -0.2702 0.4083 0.8727 0.157 Uiso 1 1 calc R . . C52 C -0.0312(6) 0.3645(11) 0.8926(5) 0.061(4) Uani 1 1 d . . . C53 C 0.0369(12) 0.3850(18) 0.9807(9) 0.176(11) Uani 1 1 d . . . H53B H 0.0193 0.4131 1.0014 0.212 Uiso 1 1 calc R . . H53A H 0.0234 0.3256 0.9782 0.212 Uiso 1 1 calc R . . C54 C 0.1001(16) 0.388(2) 1.0042(11) 0.33(3) Uani 1 1 d . . . H54A H 0.1171 0.3482 1.0322 0.393 Uiso 1 1 calc R . . H54B H 0.1147 0.4443 1.0174 0.393 Uiso 1 1 calc R . . H54C H 0.1189 0.3736 0.9817 0.393 Uiso 1 1 calc R . . C55 C -0.1209(5) 0.2956(7) 0.5979(5) 0.049(3) Uani 1 1 d . . . C56 C -0.1107(6) 0.2180(9) 0.6238(5) 0.072(4) Uani 1 1 d . . . H56A H -0.1068 0.2174 0.6564 0.087 Uiso 1 1 calc R . . C57 C -0.1063(6) 0.1441(10) 0.6023(6) 0.080(4) Uani 1 1 d . . . H57A H -0.0986 0.0943 0.6212 0.095 Uiso 1 1 calc R . . C58 C -0.1127(8) 0.1385(11) 0.5550(8) 0.092(5) Uani 1 1 d . . . H58A H -0.1117 0.0865 0.5404 0.111 Uiso 1 1 calc R . . C59 C -0.1207(6) 0.2144(11) 0.5295(6) 0.084(4) Uani 1 1 d . . . H59A H -0.1225 0.2127 0.4975 0.100 Uiso 1 1 calc R . . C60 C -0.1263(5) 0.2936(8) 0.5484(4) 0.055(3) Uani 1 1 d . . . H60A H -0.1332 0.3431 0.5294 0.066 Uiso 1 1 calc R . . C61 C -0.2219(6) 0.3879(9) 0.6132(5) 0.060(3) Uani 1 1 d . . . C62 C -0.2558(6) 0.4656(9) 0.6113(5) 0.069(4) Uani 1 1 d . . . H62A H -0.2319 0.5168 0.6168 0.083 Uiso 1 1 calc R . . C63 C -0.3249(8) 0.4645(12) 0.6012(7) 0.099(5) Uani 1 1 d . . . H63A H -0.3478 0.5154 0.5993 0.119 Uiso 1 1 calc R . . C64 C -0.3596(8) 0.3889(16) 0.5940(7) 0.109(6) Uani 1 1 d . . . H64A H -0.4064 0.3895 0.5864 0.131 Uiso 1 1 calc R . . C65 C -0.3284(8) 0.3148(13) 0.5977(7) 0.112(6) Uani 1 1 d . . . H65A H -0.3520 0.2641 0.5949 0.134 Uiso 1 1 calc R . . C66 C -0.2586(6) 0.3136(9) 0.6057(6) 0.079(4) Uani 1 1 d . . . H66A H -0.2376 0.2620 0.6059 0.095 Uiso 1 1 calc R . . C67 C -0.1267(6) 0.4848(8) 0.5963(5) 0.055(3) Uani 1 1 d . . . C68 C -0.0819(6) 0.5493(8) 0.6234(6) 0.066(4) Uani 1 1 d . . . H68A H -0.0538 0.5447 0.6587 0.080 Uiso 1 1 calc R . . C69 C -0.0786(8) 0.6232(11) 0.5973(8) 0.097(5) Uani 1 1 d . . . H69A H -0.0472 0.6665 0.6152 0.116 Uiso 1 1 calc R . . C70 C -0.1215(11) 0.6303(11) 0.5463(9) 0.113(6) Uani 1 1 d . . . H70A H -0.1197 0.6793 0.5294 0.135 Uiso 1 1 calc R . . C71 C -0.1675(11) 0.5673(12) 0.5189(7) 0.119(6) Uani 1 1 d . . . H71A H -0.1966 0.5740 0.4839 0.143 Uiso 1 1 calc R . . C72 C -0.1711(8) 0.4948(9) 0.5424(5) 0.080(4) Uani 1 1 d . . . H72A H -0.2023 0.4519 0.5235 0.096 Uiso 1 1 calc R . . C73 C 0.0473(5) 0.3596(9) 0.6473(4) 0.046(3) Uani 1 1 d . . . C74 C 0.0332(6) 0.4221(9) 0.6110(6) 0.068(4) Uani 1 1 d . . . H74A H 0.0259 0.4776 0.6181 0.082 Uiso 1 1 calc R . . C75 C 0.0296(7) 0.4035(13) 0.5631(6) 0.089(5) Uani 1 1 d . . . H75A H 0.0201 0.4459 0.5388 0.107 Uiso 1 1 calc R . . C76 C 0.0403(8) 0.3229(13) 0.5538(7) 0.094(5) Uani 1 1 d . . . H76A H 0.0386 0.3103 0.5226 0.113 Uiso 1 1 calc R . . C77 C 0.0535(7) 0.2583(10) 0.5882(7) 0.086(4) Uani 1 1 d . . . H77A H 0.0603 0.2030 0.5803 0.104 Uiso 1 1 calc R . . C78 C 0.0568(6) 0.2765(10) 0.6350(5) 0.067(4) Uani 1 1 d . . . H78A H 0.0655 0.2329 0.6584 0.081 Uiso 1 1 calc R . . C79 C 0.1087(5) 0.3002(7) 0.7490(4) 0.054(3) Uani 1 1 d . . . C80 C 0.0788(7) 0.2254(8) 0.7514(6) 0.079(4) Uani 1 1 d . . . H80A H 0.0303 0.2204 0.7356 0.095 Uiso 1 1 calc R . . C81 C 0.1199(9) 0.1586(10) 0.7767(6) 0.094(5) Uani 1 1 d . . . H81A H 0.0982 0.1078 0.7773 0.113 Uiso 1 1 calc R . . C82 C 0.1893(10) 0.1611(12) 0.8009(8) 0.116(7) Uani 1 1 d . . . H82A H 0.2159 0.1130 0.8166 0.139 Uiso 1 1 calc R . . C83 C 0.2205(9) 0.2380(13) 0.8018(8) 0.128(7) Uani 1 1 d . . . H83A H 0.2689 0.2440 0.8207 0.153 Uiso 1 1 calc R . . C84 C 0.1789(7) 0.3069(10) 0.7743(6) 0.094(5) Uani 1 1 d . . . H84A H 0.2001 0.3579 0.7734 0.113 Uiso 1 1 calc R . . C85 C 0.1006(6) 0.4862(8) 0.7249(5) 0.056(3) Uani 1 1 d . . . C86 C 0.0814(6) 0.5542(8) 0.7442(5) 0.065(4) Uani 1 1 d . . . H86A H 0.0449 0.5483 0.7519 0.078 Uiso 1 1 calc R . . C87 C 0.1154(8) 0.6318(8) 0.7522(6) 0.077(4) Uani 1 1 d . . . H87A H 0.0999 0.6791 0.7628 0.093 Uiso 1 1 calc R . . C88 C 0.1736(7) 0.6370(9) 0.7441(5) 0.074(4) Uani 1 1 d . . . H88A H 0.1984 0.6878 0.7509 0.089 Uiso 1 1 calc R . . C89 C 0.1940(6) 0.5717(8) 0.7269(5) 0.067(4) Uani 1 1 d . . . H89A H 0.2330 0.5768 0.7220 0.080 Uiso 1 1 calc R . . C90 C 0.1573(6) 0.4943(8) 0.7158(5) 0.064(4) Uani 1 1 d . . . H90A H 0.1708 0.4490 0.7024 0.077 Uiso 1 1 calc R . . C91 C 0.2279(10) 0.2847(14) 0.9378(7) 0.219(11) Uiso 1 1 d G . . H91 H 0.2075 0.2505 0.9087 0.263 Uiso 1 1 calc R . . C92 C 0.2123(9) 0.3710(16) 0.9339(7) 0.220(11) Uiso 1 1 d G . . H92 H 0.1815 0.3945 0.9023 0.263 Uiso 1 1 calc R . . C93 C 0.2427(11) 0.4222(9) 0.9774(11) 0.246(14) Uiso 1 1 d G . . H93 H 0.2322 0.4799 0.9748 0.295 Uiso 1 1 calc R . . C94 C 0.2887(10) 0.3871(15) 1.0247(8) 0.244(13) Uiso 1 1 d G . . H94 H 0.3091 0.4213 1.0538 0.292 Uiso 1 1 calc R . . C95 C 0.3044(8) 0.3008(16) 1.0285(7) 0.225(13) Uiso 1 1 d G . . H95 H 0.3352 0.2773 1.0602 0.270 Uiso 1 1 calc R . . C96 C 0.2739(10) 0.2496(9) 0.9851(10) 0.213(11) Uiso 1 1 d G . . H96 H 0.2844 0.1919 0.9876 0.255 Uiso 1 1 calc R . . O1 O 0.4141(5) 0.4621(6) 0.8388(4) 0.086(3) Uani 1 1 d . . . O2 O 0.3596(4) 0.5640(5) 0.8600(3) 0.070(2) Uani 1 1 d . . . O3 O 0.4828(5) 0.7209(6) 0.9101(4) 0.082(3) Uani 1 1 d . . . O4 O 0.5184(6) 0.5890(6) 0.9349(4) 0.095(3) Uani 1 1 d . . . O5 O -0.1172(7) 0.5556(7) 0.8379(5) 0.124(4) Uani 1 1 d . . . O6 O -0.1591(5) 0.4448(6) 0.8604(3) 0.079(3) Uani 1 1 d . . . O7 O -0.0327(5) 0.2914(6) 0.8961(4) 0.087(3) Uani 1 1 d . . . O8 O 0.0004(6) 0.4207(7) 0.9299(4) 0.107(4) Uani 1 1 d . . . P1 P 0.37771(14) 0.63936(19) 0.63613(12) 0.0453(7) Uani 1 1 d . . . P2 P 0.56128(14) 0.6421(2) 0.71226(12) 0.0483(8) Uani 1 1 d . . . P3 P -0.12887(14) 0.3904(2) 0.62965(13) 0.0485(8) Uani 1 1 d . . . P4 P 0.05050(14) 0.3858(2) 0.70878(12) 0.0501(8) Uani 1 1 d . . . Pt1 Pt 0.46151(2) 0.64861(3) 0.72034(2) 0.04306(11) Uani 1 1 d . . . Pt2 Pt -0.05038(2) 0.39024(3) 0.71562(2) 0.04932(13) Uani 1 1 d . . . S1 S 0.54438(15) 0.6536(2) 0.80780(12) 0.0592(8) Uani 1 1 d . . . S2 S 0.37051(14) 0.6442(2) 0.74138(13) 0.0565(8) Uani 1 1 d . . . S3 S 0.02802(17) 0.3929(3) 0.80422(14) 0.0846(12) Uani 1 1 d . . . S4 S -0.14458(15) 0.3901(2) 0.73241(13) 0.0624(9) 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 0.051(6) 0.069(9) 0.046(7) 0.003(6) 0.021(6) 0.015(6) C2 0.069(7) 0.053(7) 0.054(7) -0.015(7) 0.040(6) 0.001(7) C3 0.066(7) 0.055(8) 0.058(7) 0.008(6) 0.047(6) 0.008(6) C4 0.077(9) 0.059(10) 0.042(8) -0.001(7) 0.023(7) 0.010(7) C5 0.108(12) 0.109(13) 0.097(12) 0.035(10) 0.058(10) -0.024(10) C6 0.080(11) 0.192(19) 0.149(19) 0.040(14) 0.070(12) -0.008(11) C7 0.087(9) 0.044(9) 0.062(9) 0.002(8) 0.039(8) 0.000(8) C8 0.149(16) 0.176(19) 0.031(8) -0.037(10) 0.024(10) -0.004(14) C9 0.23(3) 0.42(5) 0.20(3) -0.09(3) 0.14(3) -0.12(3) C10 0.029(5) 0.055(8) 0.045(7) 0.003(6) 0.013(5) 0.007(5) C11 0.050(7) 0.069(9) 0.058(8) 0.002(7) 0.022(6) 0.006(6) C12 0.086(9) 0.070(11) 0.094(12) -0.012(9) 0.057(9) -0.020(8) C13 0.100(10) 0.044(10) 0.092(12) 0.025(9) 0.039(10) 0.005(8) C14 0.092(9) 0.070(10) 0.075(10) 0.023(8) 0.032(8) 0.008(8) C15 0.061(7) 0.068(9) 0.057(8) 0.013(7) 0.017(7) -0.010(6) C16 0.038(6) 0.066(9) 0.048(7) -0.013(6) 0.023(5) 0.000(5) C17 0.065(7) 0.077(10) 0.050(8) 0.002(7) 0.018(7) 0.004(6) C18 0.114(12) 0.094(13) 0.083(11) -0.031(10) 0.055(10) 0.013(10) C19 0.133(13) 0.059(10) 0.082(12) 0.011(10) 0.047(11) 0.038(10) C20 0.098(10) 0.052(10) 0.099(13) -0.018(9) 0.049(9) 0.007(8) C21 0.066(8) 0.059(9) 0.078(10) 0.005(8) 0.031(7) 0.007(6) C22 0.038(5) 0.067(9) 0.052(7) 0.009(6) 0.023(5) 0.007(5) C23 0.052(7) 0.070(9) 0.068(9) 0.014(7) 0.032(6) 0.007(6) C24 0.071(9) 0.103(13) 0.071(10) 0.022(9) 0.034(8) 0.033(9) C25 0.055(8) 0.159(19) 0.082(12) -0.004(11) 0.036(8) -0.014(10) C26 0.064(9) 0.100(13) 0.096(12) -0.010(9) 0.039(9) -0.027(8) C27 0.054(7) 0.066(9) 0.091(11) -0.014(7) 0.039(7) -0.021(6) C28 0.049(6) 0.038(8) 0.040(7) 0.006(6) 0.007(5) 0.016(5) C29 0.049(6) 0.078(10) 0.061(8) 0.005(8) 0.035(6) 0.004(6) C30 0.075(8) 0.088(11) 0.071(10) -0.011(9) 0.043(8) 0.012(8) C31 0.138(14) 0.118(14) 0.088(12) 0.004(10) 0.086(11) -0.008(11) C32 0.162(16) 0.111(14) 0.087(13) 0.003(10) 0.080(12) -0.039(11) C33 0.086(9) 0.082(11) 0.070(10) 0.001(8) 0.052(8) -0.017(8) C34 0.054(7) 0.057(8) 0.057(8) 0.000(6) 0.028(6) -0.007(6) C35 0.064(8) 0.099(13) 0.066(10) -0.007(9) 0.023(7) -0.003(8) C36 0.105(13) 0.103(14) 0.139(16) -0.038(12) 0.081(13) -0.018(11) C37 0.121(15) 0.098(14) 0.138(16) -0.047(14) 0.079(13) -0.067(13) C38 0.058(9) 0.133(17) 0.113(15) -0.012(13) 0.010(9) -0.037(11) C39 0.047(7) 0.074(10) 0.096(12) -0.017(8) 0.011(7) -0.016(6) C40 0.045(6) 0.063(8) 0.042(7) -0.003(6) 0.014(6) 0.005(5) C41 0.045(6) 0.079(10) 0.056(8) 0.019(7) 0.030(6) 0.008(6) C42 0.066(7) 0.061(9) 0.081(10) 0.012(8) 0.035(7) 0.005(7) C43 0.087(9) 0.046(8) 0.062(8) -0.001(7) 0.028(7) 0.008(6) C44 0.072(8) 0.070(10) 0.082(10) 0.010(8) 0.042(8) 0.025(7) C45 0.061(7) 0.065(9) 0.053(8) 0.010(6) 0.026(6) 0.015(6) C46 0.113(11) 0.097(11) 0.045(8) -0.023(7) 0.041(8) -0.055(9) C47 0.086(9) 0.054(9) 0.076(10) -0.007(8) 0.061(8) -0.005(7) C48 0.067(7) 0.058(8) 0.073(9) -0.021(7) 0.045(7) -0.013(6) C49 0.122(12) 0.052(10) 0.055(9) 0.003(7) 0.040(9) -0.015(9) C50 0.112(13) 0.127(14) 0.086(12) -0.015(10) 0.061(11) 0.019(10) C51 0.124(14) 0.150(16) 0.148(18) -0.039(13) 0.089(14) 0.013(11) C52 0.062(7) 0.065(11) 0.055(8) 0.000(8) 0.027(6) 0.000(7) C53 0.112(15) 0.24(3) 0.107(18) 0.077(19) -0.007(13) -0.011(17) C54 0.25(3) 0.36(5) 0.20(3) 0.16(3) -0.03(3) -0.12(4) C55 0.040(6) 0.050(8) 0.054(8) -0.004(6) 0.019(6) 0.001(5) C56 0.063(8) 0.088(11) 0.054(8) 0.004(8) 0.019(7) 0.002(7) C57 0.080(8) 0.052(9) 0.096(12) -0.017(9) 0.033(8) 0.005(7) C58 0.100(11) 0.053(11) 0.115(15) -0.036(11) 0.045(11) 0.006(8) C59 0.078(9) 0.101(12) 0.064(9) -0.035(9) 0.028(8) 0.012(8) C60 0.049(6) 0.068(8) 0.049(7) 0.006(6) 0.024(6) 0.010(5) C61 0.057(6) 0.068(9) 0.049(7) -0.004(7) 0.021(6) 0.007(7) C62 0.056(7) 0.080(10) 0.077(10) 0.011(7) 0.036(7) 0.016(6) C63 0.077(10) 0.108(14) 0.118(15) 0.017(11) 0.052(10) 0.040(9) C64 0.051(8) 0.18(2) 0.095(13) -0.013(13) 0.031(8) 0.009(12) C65 0.064(9) 0.133(16) 0.154(18) -0.056(13) 0.065(11) -0.045(10) C66 0.066(8) 0.079(10) 0.099(12) -0.028(8) 0.045(8) -0.017(7) C67 0.057(7) 0.054(8) 0.061(8) -0.009(7) 0.035(7) -0.003(6) C68 0.069(8) 0.048(9) 0.076(10) -0.003(7) 0.030(7) -0.007(6) C69 0.095(10) 0.070(12) 0.112(15) -0.005(12) 0.038(11) -0.025(9) C70 0.169(17) 0.073(14) 0.115(17) 0.012(12) 0.084(15) -0.019(12) C71 0.190(19) 0.092(14) 0.064(11) -0.004(11) 0.052(12) -0.013(13) C72 0.113(11) 0.066(10) 0.052(9) -0.006(8) 0.032(8) -0.005(8) C73 0.050(6) 0.045(8) 0.039(6) -0.014(7) 0.018(5) -0.020(6) C74 0.061(7) 0.062(10) 0.088(11) -0.016(8) 0.040(8) -0.019(6) C75 0.075(9) 0.139(17) 0.056(10) -0.003(10) 0.032(8) -0.018(10) C76 0.088(10) 0.125(16) 0.081(12) -0.012(11) 0.051(9) 0.003(10) C77 0.078(9) 0.091(12) 0.092(13) -0.022(10) 0.043(9) -0.002(8) C78 0.046(7) 0.102(12) 0.060(9) -0.019(8) 0.030(6) -0.006(7) C79 0.037(6) 0.069(9) 0.052(7) 0.014(6) 0.017(5) 0.008(5) C80 0.088(9) 0.041(8) 0.097(11) 0.021(8) 0.036(9) -0.013(7) C81 0.116(12) 0.069(11) 0.122(14) 0.033(10) 0.077(11) 0.010(10) C82 0.123(14) 0.116(15) 0.145(17) 0.090(13) 0.092(14) 0.070(12) C83 0.074(11) 0.145(18) 0.150(19) 0.071(15) 0.043(12) 0.035(11) C84 0.073(9) 0.094(12) 0.095(12) 0.019(9) 0.025(9) -0.006(8) C85 0.050(7) 0.058(8) 0.062(8) 0.000(6) 0.028(6) -0.003(6) C86 0.064(8) 0.053(9) 0.069(9) 0.002(7) 0.025(7) 0.003(6) C87 0.097(10) 0.049(10) 0.085(11) -0.009(7) 0.042(9) -0.008(7) C88 0.074(8) 0.060(10) 0.075(10) 0.009(8) 0.024(7) -0.014(7) C89 0.065(7) 0.062(9) 0.083(10) -0.010(7) 0.042(7) -0.021(7) C90 0.055(7) 0.072(10) 0.069(9) 0.003(7) 0.032(7) -0.005(6) O1 0.112(7) 0.056(6) 0.098(8) -0.007(6) 0.057(6) -0.006(5) O2 0.084(6) 0.056(6) 0.081(7) 0.009(5) 0.047(5) 0.000(4) O3 0.113(7) 0.056(6) 0.079(7) -0.006(6) 0.046(6) -0.001(5) O4 0.146(8) 0.078(8) 0.046(6) -0.008(5) 0.035(6) 0.011(6) O5 0.206(12) 0.065(7) 0.133(11) 0.008(7) 0.108(10) 0.007(8) O6 0.104(7) 0.077(7) 0.068(6) 0.002(5) 0.050(6) 0.012(5) O7 0.116(8) 0.059(7) 0.102(8) 0.014(6) 0.065(7) 0.004(6) O8 0.149(9) 0.090(8) 0.046(6) -0.001(6) 0.018(6) -0.022(7) P1 0.0451(14) 0.047(2) 0.0487(18) 0.0009(15) 0.0264(14) 0.0002(13) P2 0.0455(15) 0.058(2) 0.0481(18) 0.0045(16) 0.0276(14) 0.0014(14) P3 0.0447(15) 0.052(2) 0.0485(19) -0.0083(16) 0.0216(14) 0.0002(14) P4 0.0445(15) 0.057(2) 0.0473(19) -0.0016(16) 0.0210(14) -0.0068(14) Pt1 0.0397(2) 0.0498(3) 0.0426(3) 0.0006(3) 0.02208(19) 0.0014(2) Pt2 0.0409(2) 0.0644(3) 0.0457(3) -0.0040(3) 0.0231(2) -0.0079(2) S1 0.0530(16) 0.078(2) 0.0461(19) -0.0035(18) 0.0236(14) 0.0008(16) S2 0.0514(15) 0.072(2) 0.0551(19) 0.0056(17) 0.0327(14) 0.0027(15) S3 0.0615(18) 0.140(4) 0.054(2) -0.004(2) 0.0288(17) -0.033(2) S4 0.0523(16) 0.089(3) 0.0520(19) -0.0130(18) 0.0302(15) -0.0108(17) _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 1.523(13) . ? C1 S1 1.851(12) . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C2 C7 1.510(18) . ? C2 C3 1.538(16) . ? C2 C4 1.554(18) . ? C3 S2 1.780(11) . ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? C4 O1 1.167(14) . ? C4 O2 1.349(14) . ? C5 O2 1.448(14) . ? C5 C6 1.51(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O3 1.178(14) . ? C7 O4 1.340(16) . ? C8 O4 1.442(16) . ? C8 C9 1.49(3) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9C 0.9600 . ? C9 H9B 0.9600 . ? C9 H9A 0.9600 . ? C10 C15 1.360(15) . ? C10 C11 1.381(15) . ? C10 P1 1.829(12) . ? C11 C12 1.388(17) . ? C11 H11A 0.9300 . ? C12 C13 1.347(19) . ? C12 H12A 0.9300 . ? C13 C14 1.370(18) . ? C13 H13A 0.9300 . ? C14 C15 1.376(16) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.352(16) . ? C16 C21 1.411(16) . ? C16 P1 1.844(12) . ? C17 C18 1.386(17) . ? C17 H17A 0.9300 . ? C18 C19 1.323(19) . ? C18 H18A 0.9300 . ? C19 C20 1.37(2) . ? C19 H19A 0.9300 . ? C20 C21 1.369(17) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.355(15) . ? C22 C23 1.400(15) . ? C22 P1 1.841(10) . ? C23 C24 1.388(16) . ? C23 H23A 0.9300 . ? C24 C25 1.33(2) . ? C24 H24A 0.9300 . ? C25 C26 1.36(2) . ? C25 H25A 0.9300 . ? C26 C27 1.399(16) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C33 1.383(16) . ? C28 C29 1.388(17) . ? C28 P2 1.840(13) . ? C29 C30 1.435(18) . ? C29 H29A 0.9300 . ? C30 C31 1.38(2) . ? C30 H30A 0.9300 . ? C31 C32 1.37(2) . ? C31 H31A 0.9300 . ? C32 C33 1.386(19) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.357(17) . ? C34 C39 1.375(16) . ? C34 P2 1.818(12) . ? C35 C36 1.392(19) . ? C35 H35A 0.9300 . ? C36 C37 1.34(2) . ? C36 H36A 0.9300 . ? C37 C38 1.28(2) . ? C37 H37A 0.9300 . ? C38 C39 1.391(19) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C45 1.392(14) . ? C40 C41 1.400(16) . ? C40 P2 1.836(12) . ? C41 C42 1.362(16) . ? C41 H41A 0.9300 . ? C42 C43 1.377(17) . ? C42 H42A 0.9300 . ? C43 C44 1.385(17) . ? C43 H43A 0.9300 . ? C44 C45 1.372(15) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C47 1.559(16) . ? C46 S3 1.797(14) . ? C46 H46B 0.9700 . ? C46 H46A 0.9700 . ? C47 C48 1.531(17) . ? C47 C52 1.534(19) . ? C47 C49 1.56(2) . ? C48 S4 1.765(12) . ? C48 H48B 0.9700 . ? C48 H48A 0.9700 . ? C49 O5 1.169(14) . ? C49 O6 1.336(16) . ? C50 C51 1.43(2) . ? C50 O6 1.488(15) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 O7 1.157(15) . ? C52 O8 1.323(16) . ? C53 C54 1.21(3) . ? C53 O8 1.44(2) . ? C53 H53B 0.9700 . ? C53 H53A 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.401(16) . ? C55 C60 1.416(15) . ? C55 P3 1.814(12) . ? C56 C57 1.351(17) . ? C56 H56A 0.9300 . ? C57 C58 1.35(2) . ? C57 H57A 0.9300 . ? C58 C59 1.38(2) . ? C58 H58A 0.9300 . ? C59 C60 1.396(16) . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? C61 C66 1.371(16) . ? C61 C62 1.414(15) . ? C61 P3 1.839(11) . ? C62 C63 1.382(18) . ? C62 H62A 0.9300 . ? C63 C64 1.37(2) . ? C63 H63A 0.9300 . ? C64 C65 1.33(2) . ? C64 H64A 0.9300 . ? C65 C66 1.416(17) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C67 C68 1.369(16) . ? C67 C72 1.429(17) . ? C67 P3 1.797(13) . ? C68 C69 1.41(2) . ? C68 H68A 0.9300 . ? C69 C70 1.35(2) . ? C69 H69A 0.9300 . ? C70 C71 1.37(2) . ? C70 H70A 0.9300 . ? C71 C72 1.36(2) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C74 1.381(18) . ? C73 C78 1.399(16) . ? C73 P4 1.837(12) . ? C74 C75 1.417(19) . ? C74 H74A 0.9300 . ? C75 C76 1.34(2) . ? C75 H75A 0.9300 . ? C76 C77 1.37(2) . ? C76 H76A 0.9300 . ? C77 C78 1.385(19) . ? C77 H77A 0.9300 . ? C78 H78A 0.9300 . ? C79 C84 1.343(16) . ? C79 C80 1.361(15) . ? C79 P4 1.842(11) . ? C80 C81 1.351(17) . ? C80 H80A 0.9300 . ? C81 C82 1.33(2) . ? C81 H81A 0.9300 . ? C82 C83 1.38(2) . ? C82 H82A 0.9300 . ? C83 C84 1.396(19) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? C85 C86 1.369(16) . ? C85 C90 1.387(14) . ? C85 P4 1.846(12) . ? C86 C87 1.386(16) . ? C86 H86A 0.9300 . ? C87 C88 1.399(18) . ? C87 H87A 0.9300 . ? C88 C89 1.314(17) . ? C88 H88A 0.9300 . ? C89 C90 1.404(15) . ? C89 H89A 0.9300 . ? C90 H90A 0.9300 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 H91 0.9300 . ? C92 C93 1.3900 . ? C92 H92 0.9300 . ? C93 C94 1.3900 . ? C93 H93 0.9300 . ? C94 C95 1.3900 . ? C94 H94 0.9300 . ? C95 C96 1.3900 . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? P1 Pt1 2.287(3) . ? P2 Pt1 2.294(3) . ? P3 Pt2 2.292(3) . ? P4 Pt2 2.296(3) . ? Pt1 S2 2.341(3) . ? Pt1 S1 2.348(3) . ? Pt2 S4 2.326(3) . ? Pt2 S3 2.352(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 C2 C1 S1 114.2(8) . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? H1B C1 H1A 107.6 . . ? C7 C2 C1 111.0(10) . . ? C7 C2 C3 109.3(11) . . ? C1 C2 C3 111.0(9) . . ? C7 C2 C4 107.6(10) . . ? C1 C2 C4 107.3(10) . . ? C3 C2 C4 110.6(10) . . ? C2 C3 S2 115.9(8) . . ? C2 C3 H3B 108.3 . . ? S2 C3 H3B 108.3 . . ? C2 C3 H3A 108.3 . . ? S2 C3 H3A 108.3 . . ? H3B C3 H3A 107.4 . . ? O1 C4 O2 127.1(14) . . ? O1 C4 C2 125.9(12) . . ? O2 C4 C2 106.9(11) . . ? O2 C5 C6 104.4(13) . . ? O2 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? O2 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O4 122.9(14) . . ? O3 C7 C2 127.9(15) . . ? O4 C7 C2 109.3(13) . . ? O4 C8 C9 110.3(17) . . ? O4 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? O4 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? H8B C8 H8A 108.1 . . ? C8 C9 H9C 109.5 . . ? C8 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? C8 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? C15 C10 C11 117.2(11) . . ? C15 C10 P1 123.5(9) . . ? C11 C10 P1 119.0(9) . . ? C10 C11 C12 120.2(12) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C13 C12 C11 119.7(13) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 122.2(14) . . ? C12 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C13 C14 C15 116.4(13) . . ? C13 C14 H14A 121.8 . . ? C15 C14 H14A 121.8 . . ? C10 C15 C14 124.2(12) . . ? C10 C15 H15A 117.9 . . ? C14 C15 H15A 117.9 . . ? C17 C16 C21 118.5(12) . . ? C17 C16 P1 125.6(10) . . ? C21 C16 P1 115.9(10) . . ? C16 C17 C18 119.7(13) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C19 C18 C17 122.1(16) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C18 C19 C20 119.6(15) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C21 C20 C19 119.9(16) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C16 120.0(14) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? C27 C22 C23 119.6(10) . . ? C27 C22 P1 123.0(9) . . ? C23 C22 P1 117.4(9) . . ? C24 C23 C22 119.1(12) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C25 C24 C23 120.7(14) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C26 121.0(14) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 119.7(14) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C22 C27 C26 119.8(12) . . ? C22 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C33 C28 C29 119.1(13) . . ? C33 C28 P2 122.9(10) . . ? C29 C28 P2 118.0(10) . . ? C28 C29 C30 121.1(13) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C31 C30 C29 117.5(14) . . ? C31 C30 H30A 121.2 . . ? C29 C30 H30A 121.2 . . ? C32 C31 C30 120.6(15) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 121.8(14) . . ? C31 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? C28 C33 C32 119.6(14) . . ? C28 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C35 C34 C39 116.8(12) . . ? C35 C34 P2 117.6(10) . . ? C39 C34 P2 125.5(10) . . ? C34 C35 C36 119.7(14) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C37 C36 C35 122.2(16) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C38 C37 C36 118.1(17) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? C37 C38 C39 123.0(17) . . ? C37 C38 H38A 118.5 . . ? C39 C38 H38A 118.5 . . ? C34 C39 C38 120.1(14) . . ? C34 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C45 C40 C41 117.2(11) . . ? C45 C40 P2 121.1(9) . . ? C41 C40 P2 121.7(9) . . ? C42 C41 C40 121.3(11) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C41 C42 C43 120.6(12) . . ? C41 C42 H42A 119.7 . . ? C43 C42 H42A 119.7 . . ? C42 C43 C44 119.4(13) . . ? C42 C43 H43A 120.3 . . ? C44 C43 H43A 120.3 . . ? C45 C44 C43 119.9(12) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C40 121.5(12) . . ? C44 C45 H45A 119.3 . . ? C40 C45 H45A 119.3 . . ? C47 C46 S3 113.7(9) . . ? C47 C46 H46B 108.8 . . ? S3 C46 H46B 108.8 . . ? C47 C46 H46A 108.8 . . ? S3 C46 H46A 108.8 . . ? H46B C46 H46A 107.7 . . ? C48 C47 C52 112.2(11) . . ? C48 C47 C49 107.1(11) . . ? C52 C47 C49 109.9(11) . . ? C48 C47 C46 107.9(10) . . ? C52 C47 C46 112.6(11) . . ? C49 C47 C46 107.0(12) . . ? C47 C48 S4 121.6(9) . . ? C47 C48 H48B 106.9 . . ? S4 C48 H48B 106.9 . . ? C47 C48 H48A 106.9 . . ? S4 C48 H48A 106.9 . . ? H48B C48 H48A 106.7 . . ? O5 C49 O6 123.8(15) . . ? O5 C49 C47 127.8(15) . . ? O6 C49 C47 108.3(12) . . ? C51 C50 O6 111.4(14) . . ? C51 C50 H50A 109.4 . . ? O6 C50 H50A 109.4 . . ? C51 C50 H50B 109.4 . . ? O6 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O7 C52 O8 127.8(14) . . ? O7 C52 C47 124.6(14) . . ? O8 C52 C47 107.6(13) . . ? C54 C53 O8 120(2) . . ? C54 C53 H53B 107.4 . . ? O8 C53 H53B 107.4 . . ? C54 C53 H53A 107.4 . . ? O8 C53 H53A 107.4 . . ? H53B C53 H53A 107.0 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 117.5(11) . . ? C56 C55 P3 117.4(10) . . ? C60 C55 P3 125.1(9) . . ? C57 C56 C55 121.3(14) . . ? C57 C56 H56A 119.4 . . ? C55 C56 H56A 119.4 . . ? C58 C57 C56 123.6(16) . . ? C58 C57 H57A 118.2 . . ? C56 C57 H57A 118.2 . . ? C57 C58 C59 116.1(15) . . ? C57 C58 H58A 122.0 . . ? C59 C58 H58A 122.0 . . ? C58 C59 C60 124.2(14) . . ? C58 C59 H59A 117.9 . . ? C60 C59 H59A 117.9 . . ? C59 C60 C55 117.2(12) . . ? C59 C60 H60A 121.4 . . ? C55 C60 H60A 121.4 . . ? C66 C61 C62 118.6(11) . . ? C66 C61 P3 122.8(10) . . ? C62 C61 P3 118.5(10) . . ? C63 C62 C61 119.3(13) . . ? C63 C62 H62A 120.4 . . ? C61 C62 H62A 120.4 . . ? C64 C63 C62 120.3(14) . . ? C64 C63 H63A 119.8 . . ? C62 C63 H63A 119.8 . . ? C65 C64 C63 121.8(15) . . ? C65 C64 H64A 119.1 . . ? C63 C64 H64A 119.1 . . ? C64 C65 C66 119.4(16) . . ? C64 C65 H65A 120.3 . . ? C66 C65 H65A 120.3 . . ? C61 C66 C65 120.6(14) . . ? C61 C66 H66A 119.7 . . ? C65 C66 H66A 119.7 . . ? C68 C67 C72 119.0(13) . . ? C68 C67 P3 119.2(11) . . ? C72 C67 P3 121.7(10) . . ? C67 C68 C69 119.7(14) . . ? C67 C68 H68A 120.1 . . ? C69 C68 H68A 120.1 . . ? C70 C69 C68 119.5(15) . . ? C70 C69 H69A 120.2 . . ? C68 C69 H69A 120.2 . . ? C69 C70 C71 121.5(17) . . ? C69 C70 H70A 119.3 . . ? C71 C70 H70A 119.3 . . ? C72 C71 C70 120.7(17) . . ? C72 C71 H71A 119.7 . . ? C70 C71 H71A 119.7 . . ? C71 C72 C67 119.5(14) . . ? C71 C72 H72A 120.2 . . ? C67 C72 H72A 120.2 . . ? C74 C73 C78 117.7(12) . . ? C74 C73 P4 120.3(11) . . ? C78 C73 P4 122.0(10) . . ? C73 C74 C75 121.5(14) . . ? C73 C74 H74A 119.3 . . ? C75 C74 H74A 119.3 . . ? C76 C75 C74 118.0(17) . . ? C76 C75 H75A 121.0 . . ? C74 C75 H75A 121.0 . . ? C75 C76 C77 122.9(17) . . ? C75 C76 H76A 118.6 . . ? C77 C76 H76A 118.6 . . ? C76 C77 C78 119.0(15) . . ? C76 C77 H77A 120.5 . . ? C78 C77 H77A 120.5 . . ? C77 C78 C73 120.9(14) . . ? C77 C78 H78A 119.6 . . ? C73 C78 H78A 119.6 . . ? C84 C79 C80 118.8(12) . . ? C84 C79 P4 123.3(10) . . ? C80 C79 P4 117.9(9) . . ? C81 C80 C79 119.8(14) . . ? C81 C80 H80A 120.1 . . ? C79 C80 H80A 120.1 . . ? C82 C81 C80 123.7(15) . . ? C82 C81 H81A 118.1 . . ? C80 C81 H81A 118.1 . . ? C81 C82 C83 117.3(15) . . ? C81 C82 H82A 121.4 . . ? C83 C82 H82A 121.4 . . ? C82 C83 C84 119.6(16) . . ? C82 C83 H83A 120.2 . . ? C84 C83 H83A 120.2 . . ? C79 C84 C83 120.7(14) . . ? C79 C84 H84A 119.7 . . ? C83 C84 H84A 119.7 . . ? C86 C85 C90 119.1(12) . . ? C86 C85 P4 121.1(9) . . ? C90 C85 P4 119.8(9) . . ? C85 C86 C87 121.1(13) . . ? C85 C86 H86A 119.5 . . ? C87 C86 H86A 119.5 . . ? C86 C87 C88 118.2(12) . . ? C86 C87 H87A 120.9 . . ? C88 C87 H87A 120.9 . . ? C89 C88 C87 121.5(13) . . ? C89 C88 H88A 119.3 . . ? C87 C88 H88A 119.3 . . ? C88 C89 C90 120.6(12) . . ? C88 C89 H89A 119.7 . . ? C90 C89 H89A 119.7 . . ? C85 C90 C89 119.4(12) . . ? C85 C90 H90A 120.3 . . ? C89 C90 H90A 120.3 . . ? C92 C91 C96 120.0 . . ? C92 C91 H91 120.0 . . ? C96 C91 H91 120.0 . . ? C91 C92 C93 120.0 . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95 120.0 . . ? C94 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C4 O2 C5 113.4(11) . . ? C7 O4 C8 118.7(13) . . ? C49 O6 C50 118.3(12) . . ? C52 O8 C53 115.0(16) . . ? C10 P1 C22 99.9(5) . . ? C10 P1 C16 107.5(6) . . ? C22 P1 C16 102.0(5) . . ? C10 P1 Pt1 115.5(4) . . ? C22 P1 Pt1 118.5(4) . . ? C16 P1 Pt1 111.9(4) . . ? C34 P2 C40 107.7(5) . . ? C34 P2 C28 101.7(5) . . ? C40 P2 C28 100.0(5) . . ? C34 P2 Pt1 111.4(4) . . ? C40 P2 Pt1 112.0(4) . . ? C28 P2 Pt1 122.6(3) . . ? C67 P3 C55 111.0(6) . . ? C67 P3 C61 100.8(6) . . ? C55 P3 C61 102.1(5) . . ? C67 P3 Pt2 114.3(4) . . ? C55 P3 Pt2 111.8(4) . . ? C61 P3 Pt2 115.7(4) . . ? C73 P4 C79 99.6(6) . . ? C73 P4 C85 100.8(6) . . ? C79 P4 C85 108.6(5) . . ? C73 P4 Pt2 120.6(3) . . ? C79 P4 Pt2 110.7(4) . . ? C85 P4 Pt2 114.9(4) . . ? P1 Pt1 P2 100.44(11) . . ? P1 Pt1 S2 87.54(11) . . ? P2 Pt1 S2 170.69(12) . . ? P1 Pt1 S1 177.25(11) . . ? P2 Pt1 S1 81.58(11) . . ? S2 Pt1 S1 90.29(11) . . ? P3 Pt2 P4 97.77(11) . . ? P3 Pt2 S4 88.62(11) . . ? P4 Pt2 S4 173.36(13) . . ? P3 Pt2 S3 178.32(13) . . ? P4 Pt2 S3 83.56(12) . . ? S4 Pt2 S3 90.08(12) . . ? C1 S1 Pt1 101.2(4) . . ? C3 S2 Pt1 107.4(3) . . ? C46 S3 Pt2 103.2(5) . . ? C48 S4 Pt2 107.6(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.779 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.097 # Attachment 'i0251.cif' data_i0251 #recalc for x-parameter _database_code_depnum_ccdc_archive 'CCDC 723726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H17 N3 O2 S2' _chemical_formula_sum 'C23 H17 N3 O2 S2' _chemical_formula_weight 431.52 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.1130(4) _cell_length_b 36.802(3) _cell_length_c 9.3982(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.080(6) _cell_angle_gamma 90.00 _cell_volume 2021.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12374 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.290 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8454 _exptl_absorpt_correction_T_max 0.9470 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 10340 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6507 _reflns_number_gt 5565 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0580P)^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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.30(6) _refine_ls_number_reflns 6507 _refine_ls_number_parameters 541 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _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 C1 C -0.0005(5) 0.50634(8) 0.2529(3) 0.0296(6) Uani 1 1 d . . . C2 C -0.1666(5) 0.53359(9) 0.1582(3) 0.0316(7) Uani 1 1 d . . . H2 H -0.1529 0.5322 0.0549 0.038 Uiso 1 1 calc R . . C3 C -0.1045(5) 0.57241(9) 0.2146(4) 0.0393(8) Uani 1 1 d . . . H3A H -0.0533 0.5863 0.1398 0.047 Uiso 1 1 calc R . . H3B H 0.0237 0.5717 0.3079 0.047 Uiso 1 1 calc R . . C4 C -0.4151(5) 0.52378(9) 0.1501(4) 0.0348(7) Uani 1 1 d . . . H4A H -0.4236 0.5155 0.2485 0.042 Uiso 1 1 calc R . . H4B H -0.4721 0.5040 0.0770 0.042 Uiso 1 1 calc R . . C5 C 0.1151(5) 0.44536(8) 0.2642(3) 0.0311(7) Uani 1 1 d . . . C6 C 0.2888(5) 0.43833(9) 0.2005(4) 0.0332(7) Uani 1 1 d . . . H6 H 0.2955 0.4511 0.1140 0.040 Uiso 1 1 calc R . . C7 C 0.4521(5) 0.41249(9) 0.2651(3) 0.0319(7) Uani 1 1 d . . . H7 H 0.5735 0.4077 0.2237 0.038 Uiso 1 1 calc R . . C8 C 0.4392(5) 0.39356(9) 0.3898(3) 0.0302(7) Uani 1 1 d . . . C9 C 0.2596(6) 0.40048(9) 0.4518(3) 0.0344(7) Uani 1 1 d . . . H9 H 0.2498 0.3873 0.5366 0.041 Uiso 1 1 calc R . . C10 C 0.0979(6) 0.42659(9) 0.3886(4) 0.0350(7) Uani 1 1 d . . . H10 H -0.0234 0.4316 0.4297 0.042 Uiso 1 1 calc R . . C11 C 0.7620(5) 0.32116(8) 0.6032(3) 0.0301(7) Uani 1 1 d . . . C12 C 0.9451(5) 0.31512(9) 0.5434(4) 0.0307(7) Uani 1 1 d . . . H12 H 0.9546 0.3283 0.4586 0.037 Uiso 1 1 calc R . . C13 C 1.1099(5) 0.28990(9) 0.6089(3) 0.0320(7) Uani 1 1 d . . . H13 H 1.2326 0.2857 0.5682 0.038 Uiso 1 1 calc R . . C14 C 1.0999(5) 0.27018(8) 0.7355(3) 0.0305(7) Uani 1 1 d . . . C15 C 0.9172(5) 0.27658(9) 0.7934(4) 0.0327(7) Uani 1 1 d . . . H15 H 0.9080 0.2637 0.8790 0.039 Uiso 1 1 calc R . . C16 C 0.7495(5) 0.30169(8) 0.7263(4) 0.0313(7) Uani 1 1 d . . . H16 H 0.6246 0.3055 0.7655 0.038 Uiso 1 1 calc R . . C17 C 1.2690(6) 0.24349(9) 0.8020(4) 0.0348(7) Uani 1 1 d . . . C18 C 1.4067(6) 0.22048(10) 0.8580(4) 0.0360(7) Uani 1 1 d . . . C19 C 1.5727(5) 0.19329(9) 0.9264(3) 0.0321(7) Uani 1 1 d . . . C20 C 1.7531(6) 0.18473(9) 0.8716(4) 0.0373(7) Uani 1 1 d . . . H20 H 1.7675 0.1962 0.7843 0.045 Uiso 1 1 calc R . . C21 C 1.9128(6) 0.15916(9) 0.9457(4) 0.0394(8) Uani 1 1 d . . . H21 H 2.0355 0.1537 0.9064 0.047 Uiso 1 1 calc R . . C22 C 1.7257(6) 0.14970(10) 1.1189(4) 0.0415(8) Uani 1 1 d . . . H22 H 1.7138 0.1373 1.2050 0.050 Uiso 1 1 calc R . . C23 C 1.5590(6) 0.17452(9) 1.0537(4) 0.0357(7) Uani 1 1 d . . . H23 H 1.4360 0.1790 1.0941 0.043 Uiso 1 1 calc R . . C24 C 0.0039(5) 0.50493(9) -0.2445(4) 0.0301(7) Uani 1 1 d . . . C25 C -0.1000(5) 0.53484(9) -0.3560(3) 0.0331(7) Uani 1 1 d . . . H25 H -0.0290 0.5337 -0.4392 0.040 Uiso 1 1 calc R . . C26 C -0.0571(5) 0.57220(9) -0.2856(4) 0.0349(7) Uani 1 1 d . . . H26A H -0.0605 0.5905 -0.3634 0.042 Uiso 1 1 calc R . . H26B H 0.0968 0.5728 -0.2122 0.042 Uiso 1 1 calc R . . C27 C -0.3620(5) 0.52921(10) -0.4214(4) 0.0386(8) Uani 1 1 d . . . H27A H -0.3962 0.5038 -0.4555 0.046 Uiso 1 1 calc R . . H27B H -0.4249 0.5457 -0.5070 0.046 Uiso 1 1 calc R . . C28 C 0.1267(5) 0.44326(9) -0.2392(3) 0.0329(7) Uani 1 1 d . . . C29 C 0.0139(5) 0.41094(9) -0.2309(4) 0.0341(7) Uani 1 1 d . . . H29 H -0.1475 0.4092 -0.2718 0.041 Uiso 1 1 calc R . . C30 C 0.1411(5) 0.38108(9) -0.1619(4) 0.0343(7) Uani 1 1 d . . . H30 H 0.0671 0.3587 -0.1561 0.041 Uiso 1 1 calc R . . C31 C 0.3762(5) 0.38417(9) -0.1015(3) 0.0322(7) Uani 1 1 d . . . C32 C 0.4869(5) 0.41699(9) -0.1107(3) 0.0336(7) Uani 1 1 d . . . H32 H 0.6480 0.4190 -0.0690 0.040 Uiso 1 1 calc R . . C33 C 0.3602(5) 0.44654(9) -0.1811(4) 0.0353(7) Uani 1 1 d . . . H33 H 0.4339 0.4688 -0.1893 0.042 Uiso 1 1 calc R . . C34 C 0.8242(5) 0.32641(9) 0.1038(3) 0.0321(7) Uani 1 1 d . . . C35 C 0.7314(6) 0.29200(9) 0.1146(4) 0.0344(7) Uani 1 1 d . . . H35 H 0.5713 0.2881 0.0758 0.041 Uiso 1 1 calc R . . C36 C 0.8742(6) 0.26381(9) 0.1819(4) 0.0346(7) Uani 1 1 d . . . H36 H 0.8118 0.2405 0.1898 0.041 Uiso 1 1 calc R . . C37 C 1.1119(6) 0.26956(9) 0.2388(3) 0.0325(7) Uani 1 1 d . . . C38 C 1.2002(5) 0.30397(9) 0.2275(3) 0.0332(7) Uani 1 1 d . . . H38 H 1.3604 0.3080 0.2653 0.040 Uiso 1 1 calc R . . C39 C 1.0582(5) 0.33214(9) 0.1623(3) 0.0342(7) Uani 1 1 d . . . H39 H 1.1204 0.3556 0.1572 0.041 Uiso 1 1 calc R . . C40 C 1.2627(6) 0.24079(10) 0.3083(4) 0.0362(7) Uani 1 1 d . . . C41 C 1.4010(6) 0.21832(10) 0.3684(4) 0.0377(8) Uani 1 1 d . . . C42 C 1.5732(5) 0.19169(9) 0.4358(4) 0.0332(7) Uani 1 1 d . . . C43 C 1.5151(6) 0.15551(9) 0.4528(4) 0.0387(8) Uani 1 1 d . . . H43 H 1.3597 0.1479 0.4238 0.046 Uiso 1 1 calc R . . C44 C 1.6895(6) 0.13108(10) 0.5129(4) 0.0424(8) Uani 1 1 d . . . H44 H 1.6487 0.1065 0.5234 0.051 Uiso 1 1 calc R . . C45 C 1.9645(6) 0.17455(10) 0.5420(4) 0.0384(8) Uani 1 1 d . . . H45 H 2.1213 0.1814 0.5738 0.046 Uiso 1 1 calc R . . C46 C 1.8040(6) 0.20102(9) 0.4829(3) 0.0357(7) Uani 1 1 d . . . H46 H 1.8504 0.2254 0.4743 0.043 Uiso 1 1 calc R . . N1 N 0.6137(4) 0.36703(7) 0.4451(3) 0.0325(6) Uani 1 1 d . . . N2 N 0.5861(4) 0.34752(7) 0.5475(3) 0.0331(6) Uani 1 1 d . . . N3 N 1.9048(5) 0.14177(8) 1.0690(3) 0.0427(7) Uani 1 1 d . . . N4 N 0.4928(5) 0.35200(7) -0.0322(3) 0.0342(6) Uani 1 1 d . . . N5 N 0.6964(5) 0.35780(8) 0.0362(3) 0.0346(6) Uani 1 1 d . . . N6 N 1.9116(5) 0.13965(8) 0.5571(3) 0.0397(7) Uani 1 1 d . . . O1 O -0.0489(4) 0.47184(6) 0.1973(2) 0.0345(5) Uani 1 1 d . . . O2 O 0.1550(4) 0.51229(7) 0.3613(3) 0.0479(6) Uani 1 1 d . . . O3 O -0.0038(4) 0.47212(6) -0.3194(2) 0.0371(5) Uani 1 1 d . . . O4 O 0.0895(4) 0.50765(7) -0.1143(2) 0.0384(5) Uani 1 1 d . . . S1 S -0.34739(15) 0.59516(2) 0.24858(10) 0.0428(2) Uani 1 1 d . . . S2 S -0.58466(13) 0.56431(2) 0.09344(10) 0.0410(2) Uani 1 1 d . . . S3 S -0.27216(14) 0.58370(2) -0.19312(9) 0.03813(19) Uani 1 1 d . . . S4 S -0.48461(14) 0.53939(3) -0.27306(11) 0.0430(2) 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 0.0299(15) 0.0251(15) 0.0331(16) -0.0034(12) 0.0080(13) -0.0012(12) C2 0.0287(15) 0.0286(17) 0.0357(16) -0.0017(13) 0.0066(13) -0.0012(12) C3 0.0347(17) 0.0279(18) 0.055(2) -0.0023(14) 0.0121(15) 0.0011(13) C4 0.0312(16) 0.0348(18) 0.0372(17) 0.0018(14) 0.0079(14) -0.0009(13) C5 0.0330(16) 0.0227(16) 0.0325(16) 0.0000(12) 0.0019(14) 0.0020(12) C6 0.0369(17) 0.0299(17) 0.0335(17) 0.0025(13) 0.0113(14) -0.0026(13) C7 0.0323(16) 0.0299(16) 0.0360(17) -0.0009(13) 0.0139(14) -0.0001(13) C8 0.0310(16) 0.0272(15) 0.0317(16) -0.0032(13) 0.0083(13) 0.0003(12) C9 0.0391(18) 0.0347(19) 0.0312(17) 0.0021(13) 0.0134(15) 0.0008(14) C10 0.0340(16) 0.0359(18) 0.0370(18) -0.0006(14) 0.0131(14) 0.0056(14) C11 0.0303(15) 0.0245(16) 0.0333(17) -0.0035(12) 0.0058(13) -0.0009(12) C12 0.0339(16) 0.0273(16) 0.0329(16) 0.0003(12) 0.0132(14) -0.0019(12) C13 0.0328(17) 0.0304(17) 0.0342(17) -0.0015(13) 0.0119(14) 0.0003(13) C14 0.0303(16) 0.0242(16) 0.0358(17) -0.0040(12) 0.0077(14) -0.0001(12) C15 0.0378(18) 0.0286(16) 0.0337(16) 0.0016(13) 0.0138(14) -0.0009(13) C16 0.0320(16) 0.0277(16) 0.0360(17) 0.0009(13) 0.0127(14) -0.0012(13) C17 0.0364(17) 0.0288(17) 0.0375(18) -0.0006(14) 0.0084(14) 0.0001(14) C18 0.0376(17) 0.0309(17) 0.0389(17) -0.0061(14) 0.0103(14) -0.0027(15) C19 0.0350(17) 0.0245(15) 0.0345(17) -0.0018(13) 0.0068(14) -0.0002(13) C20 0.0429(19) 0.0311(18) 0.0409(19) 0.0012(14) 0.0170(15) -0.0010(14) C21 0.0405(18) 0.0296(17) 0.053(2) 0.0010(15) 0.0217(16) 0.0045(14) C22 0.049(2) 0.0349(19) 0.0412(19) 0.0051(15) 0.0143(16) 0.0020(16) C23 0.0349(17) 0.0326(18) 0.0409(19) -0.0005(14) 0.0131(15) 0.0046(14) C24 0.0249(14) 0.0287(16) 0.0365(18) -0.0050(13) 0.0090(13) -0.0004(12) C25 0.0288(15) 0.0341(17) 0.0361(16) -0.0008(14) 0.0092(13) 0.0007(13) C26 0.0340(16) 0.0290(17) 0.0437(18) -0.0013(13) 0.0148(14) -0.0025(13) C27 0.0341(17) 0.0354(19) 0.0421(18) -0.0005(14) 0.0048(15) 0.0003(13) C28 0.0387(18) 0.0267(16) 0.0332(17) -0.0020(13) 0.0103(14) 0.0073(13) C29 0.0315(16) 0.0332(18) 0.0364(18) -0.0023(13) 0.0081(14) 0.0007(13) C30 0.0345(17) 0.0313(18) 0.0379(18) -0.0040(14) 0.0118(14) -0.0054(13) C31 0.0387(17) 0.0285(16) 0.0320(17) 0.0019(13) 0.0144(14) 0.0072(13) C32 0.0295(16) 0.0346(18) 0.0376(17) -0.0011(14) 0.0114(14) -0.0020(13) C33 0.0357(17) 0.0268(17) 0.0458(19) 0.0011(14) 0.0157(15) 0.0011(13) C34 0.0352(17) 0.0318(17) 0.0301(17) -0.0021(13) 0.0111(14) 0.0043(13) C35 0.0336(17) 0.0352(18) 0.0353(18) -0.0006(14) 0.0116(14) -0.0001(13) C36 0.0397(18) 0.0289(17) 0.0362(17) -0.0014(13) 0.0130(14) -0.0018(14) C37 0.0383(17) 0.0319(17) 0.0283(16) -0.0008(12) 0.0113(14) 0.0073(13) C38 0.0318(17) 0.0351(18) 0.0333(17) -0.0031(13) 0.0105(14) -0.0004(13) C39 0.0379(18) 0.0278(17) 0.0371(18) -0.0015(13) 0.0115(14) -0.0006(13) C40 0.0407(18) 0.0330(18) 0.0353(18) -0.0039(14) 0.0118(15) 0.0012(14) C41 0.0457(19) 0.0307(18) 0.0375(17) 0.0019(14) 0.0134(15) 0.0060(15) C42 0.0369(18) 0.0280(17) 0.0353(17) 0.0014(13) 0.0117(14) 0.0048(13) C43 0.0339(17) 0.0303(17) 0.053(2) -0.0003(14) 0.0146(16) 0.0012(13) C44 0.045(2) 0.0257(17) 0.058(2) 0.0025(16) 0.0168(17) -0.0007(14) C45 0.0353(17) 0.042(2) 0.0398(19) -0.0052(15) 0.0136(15) -0.0046(14) C46 0.045(2) 0.0288(17) 0.0358(17) -0.0005(13) 0.0151(15) -0.0025(14) N1 0.0359(15) 0.0290(14) 0.0334(14) 0.0030(12) 0.0116(12) 0.0028(11) N2 0.0323(14) 0.0297(15) 0.0367(15) -0.0001(12) 0.0093(12) 0.0013(11) N3 0.0387(16) 0.0335(16) 0.0543(18) 0.0041(13) 0.0113(14) 0.0083(12) N4 0.0365(15) 0.0296(15) 0.0369(15) 0.0001(11) 0.0116(13) 0.0012(11) N5 0.0345(15) 0.0314(15) 0.0377(15) 0.0001(11) 0.0101(13) 0.0019(11) N6 0.0370(15) 0.0388(18) 0.0432(16) 0.0050(12) 0.0116(13) 0.0051(12) O1 0.0330(12) 0.0272(12) 0.0374(12) -0.0024(9) 0.0013(9) 0.0051(9) O2 0.0434(14) 0.0348(14) 0.0520(14) -0.0061(11) -0.0068(12) 0.0050(11) O3 0.0429(12) 0.0277(12) 0.0363(12) -0.0020(9) 0.0046(10) 0.0072(9) O4 0.0401(12) 0.0351(13) 0.0373(13) -0.0027(10) 0.0070(10) 0.0050(10) S1 0.0442(5) 0.0329(4) 0.0547(5) -0.0072(4) 0.0199(4) 0.0049(4) S2 0.0306(4) 0.0375(5) 0.0540(5) 0.0023(4) 0.0111(4) 0.0055(4) S3 0.0374(4) 0.0332(4) 0.0475(5) -0.0009(4) 0.0183(4) 0.0012(3) S4 0.0308(4) 0.0389(5) 0.0625(6) 0.0020(4) 0.0188(4) -0.0024(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 O2 1.192(4) . ? C1 O1 1.372(4) . ? C1 C2 1.516(4) . ? C2 C3 1.532(4) . ? C2 C4 1.542(4) . ? C2 H2 1.0000 . ? C3 S1 1.813(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S2 1.805(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.388(5) . ? C5 C6 1.388(5) . ? C5 O1 1.407(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.386(5) . ? C7 H7 0.9500 . ? C8 C9 1.409(5) . ? C8 N1 1.427(4) . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.383(5) . ? C11 C12 1.410(5) . ? C11 N2 1.428(4) . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 C14 1.410(5) . ? C13 H13 0.9500 . ? C14 C15 1.398(5) . ? C14 C17 1.430(5) . ? C15 C16 1.387(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.201(5) . ? C18 C19 1.435(5) . ? C19 C20 1.384(5) . ? C19 C23 1.406(5) . ? C20 C21 1.387(5) . ? C20 H20 0.9500 . ? C21 N3 1.337(5) . ? C21 H21 0.9500 . ? C22 N3 1.344(5) . ? C22 C23 1.372(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O4 1.186(4) . ? C24 O3 1.391(4) . ? C24 C25 1.524(5) . ? C25 C26 1.515(5) . ? C25 C27 1.552(4) . ? C25 H25 1.0000 . ? C26 S3 1.826(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 S4 1.806(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.376(4) . ? C28 C29 1.388(5) . ? C28 O3 1.407(4) . ? C29 C30 1.392(5) . ? C29 H29 0.9500 . ? C30 C31 1.386(5) . ? C30 H30 0.9500 . ? C31 C32 1.400(5) . ? C31 N4 1.436(4) . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.390(5) . ? C34 C35 1.403(5) . ? C34 N5 1.434(4) . ? C35 C36 1.383(5) . ? C35 H35 0.9500 . ? C36 C37 1.409(5) . ? C36 H36 0.9500 . ? C37 C38 1.393(5) . ? C37 C40 1.430(5) . ? C38 C39 1.376(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.199(5) . ? C41 C42 1.442(5) . ? C42 C46 1.392(5) . ? C42 C43 1.399(5) . ? C43 C44 1.382(5) . ? C43 H43 0.9500 . ? C44 N6 1.336(4) . ? C44 H44 0.9500 . ? C45 N6 1.342(5) . ? C45 C46 1.378(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? N1 N2 1.251(4) . ? N4 N5 1.240(4) . ? S1 S2 2.0681(12) . ? S3 S4 2.0824(13) . ? 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 O2 C1 O1 121.6(3) . . ? O2 C1 C2 127.5(3) . . ? O1 C1 C2 110.9(2) . . ? C1 C2 C3 111.0(2) . . ? C1 C2 C4 110.8(3) . . ? C3 C2 C4 112.1(3) . . ? C1 C2 H2 107.6 . . ? C3 C2 H2 107.6 . . ? C4 C2 H2 107.6 . . ? C2 C3 S1 111.0(2) . . ? C2 C3 H3A 109.4 . . ? S1 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? S1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C2 C4 S2 107.0(2) . . ? C2 C4 H4A 110.3 . . ? S2 C4 H4A 110.3 . . ? C2 C4 H4B 110.3 . . ? S2 C4 H4B 110.3 . . ? H4A C4 H4B 108.6 . . ? C10 C5 C6 121.8(3) . . ? C10 C5 O1 120.1(3) . . ? C6 C5 O1 118.1(3) . . ? C7 C6 C5 119.0(3) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.2(3) . . ? C7 C8 N1 115.5(3) . . ? C9 C8 N1 124.3(3) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C5 119.1(3) . . ? C9 C10 H10 120.4 . . ? C5 C10 H10 120.4 . . ? C16 C11 C12 119.8(3) . . ? C16 C11 N2 116.0(3) . . ? C12 C11 N2 124.2(3) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.2(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 118.6(3) . . ? C15 C14 C17 120.2(3) . . ? C13 C14 C17 121.2(3) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C11 C16 C15 120.7(3) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C14 178.4(4) . . ? C17 C18 C19 179.3(4) . . ? C20 C19 C23 117.3(3) . . ? C20 C19 C18 121.9(3) . . ? C23 C19 C18 120.8(3) . . ? C19 C20 C21 119.2(3) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N3 C21 C20 124.1(3) . . ? N3 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? N3 C22 C23 124.3(3) . . ? N3 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? C22 C23 C19 119.0(3) . . ? C22 C23 H23 120.5 . . ? C19 C23 H23 120.5 . . ? O4 C24 O3 122.3(3) . . ? O4 C24 C25 128.1(3) . . ? O3 C24 C25 109.5(3) . . ? C26 C25 C24 111.8(3) . . ? C26 C25 C27 108.7(3) . . ? C24 C25 C27 110.4(3) . . ? C26 C25 H25 108.6 . . ? C24 C25 H25 108.6 . . ? C27 C25 H25 108.6 . . ? C25 C26 S3 111.2(2) . . ? C25 C26 H26A 109.4 . . ? S3 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? S3 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C25 C27 S4 106.3(2) . . ? C25 C27 H27A 110.5 . . ? S4 C27 H27A 110.5 . . ? C25 C27 H27B 110.5 . . ? S4 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C33 C28 C29 121.8(3) . . ? C33 C28 O3 120.4(3) . . ? C29 C28 O3 117.6(3) . . ? C28 C29 C30 118.9(3) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 N4 115.8(3) . . ? C32 C31 N4 123.7(3) . . ? C33 C32 C31 119.6(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C28 C33 C32 119.3(3) . . ? C28 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C39 C34 C35 119.9(3) . . ? C39 C34 N5 114.6(3) . . ? C35 C34 N5 125.4(3) . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.2(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.2(3) . . ? C38 C37 C40 119.7(3) . . ? C36 C37 C40 121.1(3) . . ? C39 C38 C37 120.7(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C34 120.2(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C41 C40 C37 175.6(4) . . ? C40 C41 C42 177.3(4) . . ? C46 C42 C43 117.8(3) . . ? C46 C42 C41 120.9(3) . . ? C43 C42 C41 121.3(3) . . ? C44 C43 C42 118.3(3) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? N6 C44 C43 124.4(3) . . ? N6 C44 H44 117.8 . . ? C43 C44 H44 117.8 . . ? N6 C45 C46 123.6(3) . . ? N6 C45 H45 118.2 . . ? C46 C45 H45 118.2 . . ? C45 C46 C42 119.3(3) . . ? C45 C46 H46 120.4 . . ? C42 C46 H46 120.4 . . ? N2 N1 C8 114.7(3) . . ? N1 N2 C11 114.5(3) . . ? C21 N3 C22 116.1(3) . . ? N5 N4 C31 112.5(3) . . ? N4 N5 C34 115.1(3) . . ? C45 N6 C44 116.6(3) . . ? C1 O1 C5 115.1(2) . . ? C24 O3 C28 117.0(2) . . ? C3 S1 S2 93.63(11) . . ? C4 S2 S1 91.31(11) . . ? C26 S3 S4 96.12(11) . . ? C27 S4 S3 94.86(12) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.293 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.050