# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2072 data_global _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and biological activity of Platinum(II) and Palladium(II) thiosalicylate complexes with mixed ancillary ligands ; _publ_contact_author_name 'B K Nicholson' _publ_contact_author_address ; Chemistry Department University of Waikato Private Bag 3105 Hamilton New Zealand ; _publ_contact_author_email 'b.nicholson@waikato.ac.nz' data_ptpyc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; THIOSALICYLATO(TRIPHENYLPHOSPHINE)(PYRIDINE)PLATINUM(II) MONOHYDRATE ; _chemical_formula_moiety 'C30 H24 N O2 P Pt S' _chemical_formula_sum 'C30 H26 N O3 P Pt S' _chemical_formula_weight 706.64 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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.72310(10) _cell_length_b 17.30190(10) _cell_length_c 17.65430(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.3600(10) _cell_angle_gamma 90.00 _cell_volume 5564.25(5) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'NEEDLE' _exptl_crystal_colour 'YELLOW' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 5.208 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.5941 _exptl_absorpt_correction_T_max 0.8120 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'SIEMENS SMART CCD DIFFRACTOMETER' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27133 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4377 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTO' _computing_publication_material 'SHELX' _refine_special_details ; Pyridine ligand disordered over two equal sites, atoms of this part treated isotropically. Water of crystallisation also disordered over two sites. H atoms not included for disordered components 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+204.4911P] 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 4377 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.370 _refine_ls_shift/su_mean 0.037 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.23143(3) 0.12111(5) 0.02558(3) 0.0773(3) Uani 1 d . . . S1 S 0.28115(18) 0.1278(3) 0.15453(18) 0.0799(14) Uani 1 d . . . P1 P 0.3382(2) 0.0738(3) 0.01051(19) 0.0660(12) Uani 1 d . . . O1 O 0.1284(5) 0.1522(7) 0.0365(5) 0.088(4) Uani 1 d . . . O2 O 0.0281(5) 0.1579(11) 0.0762(6) 0.159(8) Uani 1 d . . . C1 C 0.2115(7) 0.1382(10) 0.2056(7) 0.071(5) Uani 1 d . . . C2 C 0.1351(7) 0.1455(11) 0.1765(8) 0.081(5) Uani 1 d . . . C3 C 0.0912(8) 0.1526(12) 0.2302(8) 0.105(7) Uani 1 d . . . H3 H 0.0402 0.1578 0.2111 0.126 Uiso 1 calc R . . C4 C 0.1185(8) 0.1523(13) 0.3098(9) 0.109(8) Uani 1 d . . . H4 H 0.0868 0.1569 0.3438 0.130 Uiso 1 calc R . . C5 C 0.1934(8) 0.1451(11) 0.3384(8) 0.083(5) Uani 1 d . . . H5 H 0.2134 0.1442 0.3923 0.100 Uiso 1 calc R . . C6 C 0.2386(7) 0.1393(10) 0.2870(7) 0.076(5) Uani 1 d . . . H6 H 0.2896 0.1359 0.3072 0.092 Uiso 1 calc R . . C7 C 0.0952(9) 0.1500(13) 0.0923(8) 0.108(8) Uani 1 d . . . C11 C 0.3409(7) -0.0305(8) 0.0227(7) 0.056(4) Uani 1 d . . . C12 C 0.3921(7) -0.0756(10) -0.0035(8) 0.064(4) Uani 1 d . . . H12 H 0.4261 -0.0515 -0.0275 0.077 Uiso 1 calc R . . C13 C 0.3936(8) -0.1539(11) 0.0050(8) 0.072(4) Uani 1 d . . . H13 H 0.4296 -0.1828 -0.0117 0.086 Uiso 1 calc R . . C14 C 0.3429(8) -0.1913(10) 0.0378(8) 0.069(4) Uani 1 d . . . H14 H 0.3433 -0.2454 0.0421 0.083 Uiso 1 calc R . . C15 C 0.2909(9) -0.1473(13) 0.0644(8) 0.084(6) Uani 1 d . . . H15 H 0.2563 -0.1717 0.0874 0.101 Uiso 1 calc R . . C16 C 0.2905(8) -0.0677(12) 0.0567(7) 0.074(5) Uani 1 d . . . H16 H 0.2556 -0.0383 0.0748 0.089 Uiso 1 calc R . . C21 C 0.3593(8) 0.0866(11) -0.0842(7) 0.074(5) Uani 1 d . . . C22 C 0.4100(9) 0.1386(12) -0.0971(8) 0.086(6) Uani 1 d . . . H22 H 0.4364 0.1682 -0.0553 0.104 Uiso 1 calc R . . C23 C 0.4236(10) 0.1489(12) -0.1718(9) 0.095(6) Uani 1 d . . . H23 H 0.4585 0.1852 -0.1796 0.114 Uiso 1 calc R . . C24 C 0.3853(11) 0.1053(12) -0.2333(9) 0.095(7) Uani 1 d . . . H24 H 0.3949 0.1112 -0.2829 0.114 Uiso 1 calc R . . C25 C 0.3338(11) 0.0538(12) -0.2226(9) 0.089(6) Uani 1 d . . . H25 H 0.3072 0.0250 -0.2649 0.107 Uiso 1 calc R . . C26 C 0.3202(9) 0.0435(9) -0.1475(7) 0.077(5) Uani 1 d . . . H26 H 0.2847 0.0076 -0.1401 0.093 Uiso 1 calc R . . C31 C 0.4182(7) 0.1120(9) 0.0791(6) 0.057(4) Uani 1 d . . . C32 C 0.4732(7) 0.0662(8) 0.1241(6) 0.051(3) Uani 1 d . . . H32 H 0.4698 0.0120 0.1216 0.061 Uiso 1 calc R . . C33 C 0.5329(7) 0.1020(9) 0.1726(7) 0.057(4) Uani 1 d . . . H33 H 0.5698 0.0714 0.2037 0.068 Uiso 1 calc R . . C34 C 0.5395(8) 0.1816(9) 0.1762(8) 0.065(4) Uani 1 d . . . H34 H 0.5810 0.2047 0.2085 0.078 Uiso 1 calc R . . C35 C 0.4844(9) 0.2272(10) 0.1318(8) 0.073(4) Uani 1 d . . . H35 H 0.4883 0.2813 0.1345 0.088 Uiso 1 calc R . . C36 C 0.4240(8) 0.1931(10) 0.0835(7) 0.073(5) Uani 1 d . . . H36 H 0.3867 0.2241 0.0536 0.088 Uiso 1 calc R . . N1 N 0.1957(10) 0.1331(12) -0.0957(12) 0.034(5) Uiso 0.50 d P . . N1A N 0.1697(12) 0.1021(13) -0.0911(12) 0.044(5) Uiso 0.50 d P . . C42 C 0.1416(15) 0.0765(17) -0.1278(17) 0.049(6) Uiso 0.50 d P . . C42A C 0.1190(17) 0.0427(19) -0.1059(18) 0.072(8) Uiso 0.50 d P . . C43 C 0.113(2) 0.070(3) -0.212(3) 0.090(13) Uiso 0.50 d P . . C43A C 0.079(2) 0.035(2) -0.190(2) 0.090(10) Uiso 0.50 d P . . C44 C 0.1413(18) 0.124(2) -0.2583(19) 0.066(8) Uiso 0.50 d P . . C44A C 0.104(2) 0.094(3) -0.238(3) 0.090(14) Uiso 0.50 d P . . C45 C 0.1921(14) 0.1840(15) -0.2243(14) 0.050(6) Uiso 0.50 d P . . C45A C 0.1473(18) 0.150(2) -0.222(2) 0.073(9) Uiso 0.50 d P . . C46 C 0.2179(12) 0.1874(14) -0.1418(12) 0.036(5) Uiso 0.50 d P . . C46A C 0.1858(15) 0.1509(17) -0.1405(18) 0.057(7) Uiso 0.50 d P . . O9 O 0.0844(15) 0.9296(16) 0.0473(15) 0.104(8) Uiso 0.50 d P . . O9A O 0.0467(17) 0.9023(18) 0.0630(18) 0.129(10) Uiso 0.50 d P . . 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 Pt1 0.0601(4) 0.1316(6) 0.0328(3) -0.0120(3) -0.0046(2) 0.0553(4) S1 0.0440(18) 0.158(4) 0.0337(16) -0.010(2) 0.0007(14) 0.038(2) P1 0.056(2) 0.105(3) 0.0337(17) -0.0015(19) 0.0042(15) 0.038(2) O1 0.065(6) 0.143(11) 0.045(5) -0.014(6) -0.011(5) 0.057(7) O2 0.042(6) 0.36(2) 0.063(7) -0.056(10) -0.011(5) 0.064(10) C1 0.052(8) 0.120(14) 0.038(7) -0.017(8) 0.003(6) 0.038(8) C2 0.052(8) 0.139(16) 0.048(8) -0.025(9) 0.005(6) 0.040(9) C3 0.044(8) 0.21(2) 0.058(9) -0.051(12) 0.006(7) 0.030(11) C4 0.048(9) 0.22(2) 0.058(9) -0.039(12) 0.010(7) 0.031(11) C5 0.062(9) 0.144(17) 0.041(7) -0.015(9) 0.008(7) 0.024(10) C6 0.050(8) 0.129(15) 0.043(7) -0.012(8) -0.002(6) 0.024(9) C7 0.067(11) 0.20(2) 0.049(9) -0.043(11) 0.001(8) 0.061(12) C11 0.047(7) 0.077(11) 0.039(7) -0.003(7) 0.000(6) 0.015(7) C12 0.058(9) 0.077(12) 0.061(9) 0.001(8) 0.020(7) 0.022(8) C13 0.055(9) 0.098(14) 0.062(9) -0.010(9) 0.012(7) 0.016(9) C14 0.075(10) 0.083(12) 0.049(8) -0.012(8) 0.012(7) -0.012(9) C15 0.065(10) 0.146(19) 0.042(8) -0.016(10) 0.010(7) -0.023(11) C16 0.057(9) 0.123(16) 0.036(7) -0.013(9) 0.001(6) 0.015(10) C21 0.065(10) 0.121(15) 0.037(7) 0.002(8) 0.011(7) 0.048(10) C22 0.072(11) 0.144(18) 0.043(8) -0.001(10) 0.014(8) 0.046(11) C23 0.104(13) 0.131(17) 0.053(10) 0.012(10) 0.023(9) 0.043(12) C24 0.121(16) 0.124(18) 0.041(9) 0.008(10) 0.019(10) 0.073(14) C25 0.110(15) 0.111(16) 0.040(9) -0.004(9) 0.007(9) 0.057(12) C26 0.104(12) 0.086(12) 0.039(8) 0.002(8) 0.009(8) 0.057(10) C31 0.054(8) 0.079(12) 0.036(6) -0.003(7) 0.006(5) 0.031(7) C32 0.055(8) 0.058(9) 0.040(7) 0.004(6) 0.015(6) 0.014(6) C33 0.045(7) 0.069(11) 0.055(8) -0.002(7) 0.008(6) 0.015(7) C34 0.059(9) 0.084(12) 0.052(8) -0.006(8) 0.017(7) 0.004(8) C35 0.094(12) 0.072(11) 0.059(9) 0.000(8) 0.030(9) 0.028(9) C36 0.080(11) 0.103(14) 0.039(8) 0.009(8) 0.017(7) 0.051(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 Pt1 O1 2.054(9) . ? Pt1 N1 2.10(2) . ? Pt1 N1A 2.14(2) . ? Pt1 P1 2.231(3) . ? Pt1 S1 2.255(3) . ? S1 C1 1.757(13) . ? S1 C6 2.647(13) . ? S1 C2 2.865(14) . ? S1 P1 3.120(5) . ? S1 O1 3.153(9) . ? S1 C31 3.164(12) . ? S1 C46 3.21(2) 7 ? S1 C36 3.399(16) . ? S1 C7 3.421(15) . ? P1 C21 1.819(14) . ? P1 C11 1.817(15) . ? P1 C31 1.819(13) . ? O1 C7 1.281(18) . ? O2 C7 1.230(17) . ? C1 C2 1.409(17) . ? C1 C6 1.410(16) . ? C2 C3 1.396(19) . ? C2 C7 1.503(18) . ? C3 C4 1.380(19) . ? C4 C5 1.382(18) . ? C5 C6 1.379(18) . ? C11 C16 1.39(2) . ? C11 C12 1.395(17) . ? C12 C13 1.36(2) . ? C13 C14 1.38(2) . ? C14 C15 1.40(2) . ? C15 C16 1.38(2) . ? C21 C22 1.36(2) . ? C21 C26 1.40(2) . ? C22 C23 1.41(2) . ? C23 C24 1.38(2) . ? C24 C25 1.36(2) . ? C25 C26 1.42(2) . ? C31 C32 1.394(16) . ? C31 C36 1.41(2) . ? C32 C33 1.388(17) . ? C33 C34 1.384(19) . ? C34 C35 1.388(19) . ? C35 C36 1.38(2) . ? N1 N1A 0.74(2) . ? N1 C46A 0.83(3) . ? N1 C46 1.37(3) . ? N1 C42 1.43(4) . ? N1A C42 0.86(3) . ? N1A C46A 1.30(4) . ? N1A C42A 1.38(4) . ? C42 C42A 0.86(3) . ? C42 C43 1.46(5) . ? C42 C46A 1.57(4) . ? C42 C43A 1.58(5) . ? C42 C44A 1.93(5) . ? C42A C43A 1.51(4) . ? C42A C43 1.90(6) . ? C43 C44A 0.62(6) . ? C43 C43A 1.00(5) . ? C43 C44 1.43(6) . ? C43 C45A 1.56(6) . ? C43A C44A 1.47(6) . ? C44 C45A 0.77(4) . ? C44 C44A 1.00(5) . ? C44 C45 1.45(4) . ? C44A C45A 1.25(5) . ? C45 C45A 1.04(4) . ? C45 C46 1.42(3) . ? C45 C46A 1.62(4) . ? C45A C46A 1.45(4) . ? C45A C46 1.82(4) . ? C46 C46A 0.88(3) . ? C46 S1 3.21(2) 7 ? O9 O9A 0.94(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 N1 89.1(6) . . ? O1 Pt1 N1A 79.7(6) . . ? N1 Pt1 N1A 20.1(6) . . ? O1 Pt1 P1 173.4(4) . . ? N1 Pt1 P1 89.9(5) . . ? N1A Pt1 P1 97.3(5) . . ? O1 Pt1 S1 94.0(3) . . ? N1 Pt1 S1 169.8(6) . . ? N1A Pt1 S1 169.8(6) . . ? P1 Pt1 S1 88.12(12) . . ? C1 S1 Pt1 109.9(4) . . ? C1 S1 C6 29.4(5) . . ? Pt1 S1 C6 139.3(3) . . ? C1 S1 C2 22.4(5) . . ? Pt1 S1 C2 87.6(3) . . ? C6 S1 C2 51.7(4) . . ? C1 S1 P1 152.0(5) . . ? Pt1 S1 P1 45.63(8) . . ? C6 S1 P1 166.5(4) . . ? C2 S1 P1 131.2(3) . . ? C1 S1 O1 70.0(4) . . ? Pt1 S1 O1 40.52(19) . . ? C6 S1 O1 99.3(3) . . ? C2 S1 O1 47.7(3) . . ? P1 S1 O1 86.0(2) . . ? C1 S1 C31 174.1(5) . . ? Pt1 S1 C31 75.9(2) . . ? C6 S1 C31 144.8(4) . . ? C2 S1 C31 163.4(4) . . ? P1 S1 C31 33.6(2) . . ? O1 S1 C31 115.7(3) . . ? C1 S1 C46 87.2(7) . 7 ? Pt1 S1 C46 89.3(4) . 7 ? C6 S1 C46 89.7(6) . 7 ? C2 S1 C46 85.6(6) . 7 ? P1 S1 C46 103.5(4) . 7 ? O1 S1 C46 80.8(5) . 7 ? C31 S1 C46 92.2(5) . 7 ? C1 S1 C36 153.6(7) . . ? Pt1 S1 C36 79.7(3) . . ? C6 S1 C36 136.4(4) . . ? C2 S1 C36 150.6(5) . . ? P1 S1 C36 49.6(3) . . ? O1 S1 C36 112.5(3) . . ? C31 S1 C36 24.4(3) . . ? C46 S1 C36 68.0(5) 7 . ? C1 S1 C7 48.1(5) . . ? Pt1 S1 C7 61.9(3) . . ? C6 S1 C7 77.5(4) . . ? C2 S1 C7 25.8(4) . . ? P1 S1 C7 106.6(3) . . ? O1 S1 C7 22.0(3) . . ? C31 S1 C7 137.6(3) . . ? C46 S1 C7 83.5(6) 7 . ? C36 S1 C7 132.3(4) . . ? C21 P1 C11 102.9(7) . . ? C21 P1 C31 104.3(7) . . ? C11 P1 C31 106.6(6) . . ? C21 P1 Pt1 117.1(4) . . ? C11 P1 Pt1 110.6(5) . . ? C31 P1 Pt1 114.2(4) . . ? C21 P1 S1 154.3(6) . . ? C11 P1 S1 101.9(4) . . ? C31 P1 S1 74.5(4) . . ? Pt1 P1 S1 46.25(8) . . ? C7 O1 Pt1 134.2(9) . . ? C7 O1 S1 90.8(8) . . ? Pt1 O1 S1 45.51(17) . . ? C2 C1 C6 117.7(12) . . ? C2 C1 S1 129.3(10) . . ? C6 C1 S1 112.9(9) . . ? C3 C2 C1 118.0(12) . . ? C3 C2 C7 115.5(12) . . ? C1 C2 C7 126.5(13) . . ? C3 C2 S1 146.3(10) . . ? C1 C2 S1 28.3(6) . . ? C7 C2 S1 98.2(9) . . ? C4 C3 C2 123.6(13) . . ? C3 C4 C5 118.6(14) . . ? C6 C5 C4 119.5(13) . . ? C5 C6 C1 122.7(12) . . ? C5 C6 S1 160.3(10) . . ? C1 C6 S1 37.7(6) . . ? O2 C7 O1 118.0(14) . . ? O2 C7 C2 118.9(14) . . ? O1 C7 C2 122.9(13) . . ? O2 C7 S1 174.8(11) . . ? O1 C7 S1 67.2(7) . . ? C2 C7 S1 56.0(7) . . ? C16 C11 C12 118.2(15) . . ? C16 C11 P1 120.6(12) . . ? C12 C11 P1 121.2(12) . . ? C13 C12 C11 121.2(15) . . ? C12 C13 C14 120.8(15) . . ? C13 C14 C15 119.0(17) . . ? C16 C15 C14 119.7(16) . . ? C15 C16 C11 121.0(15) . . ? C22 C21 C26 118.3(14) . . ? C22 C21 P1 122.7(12) . . ? C26 C21 P1 119.0(14) . . ? C21 C22 C23 121.4(17) . . ? C24 C23 C22 120(2) . . ? C25 C24 C23 120.4(17) . . ? C24 C25 C26 120.0(18) . . ? C21 C26 C25 120.3(18) . . ? C32 C31 C36 119.8(13) . . ? C32 C31 P1 124.0(12) . . ? C36 C31 P1 116.2(10) . . ? C32 C31 S1 111.9(8) . . ? C36 C31 S1 87.2(8) . . ? P1 C31 S1 71.8(4) . . ? C33 C32 C31 118.8(13) . . ? C34 C33 C32 121.5(13) . . ? C35 C34 C33 119.5(14) . . ? C36 C35 C34 120.1(16) . . ? C35 C36 C31 120.1(13) . . ? C35 C36 S1 121.1(9) . . ? C31 C36 S1 68.4(8) . . ? N1A N1 C46A 112(4) . . ? N1A N1 C46 149(3) . . ? C46A N1 C46 38(2) . . ? N1A N1 C42 29(2) . . ? C46A N1 C42 84(3) . . ? C46 N1 C42 121(2) . . ? N1A N1 Pt1 83(3) . . ? C46A N1 Pt1 163(3) . . ? C46 N1 Pt1 127.2(16) . . ? C42 N1 Pt1 111.5(19) . . ? N1 N1A C42 127(4) . . ? N1 N1A C46A 36(2) . . ? C42 N1A C46A 91(3) . . ? N1 N1A C42A 163(4) . . ? C42 N1A C42A 37(2) . . ? C46A N1A C42A 128(3) . . ? N1 N1A Pt1 77(3) . . ? C42 N1A Pt1 155(3) . . ? C46A N1A Pt1 113(2) . . ? C42A N1A Pt1 119.4(19) . . ? N1A C42 C42A 107(4) . . ? N1A C42 N1 25(2) . . ? C42A C42 N1 131(4) . . ? N1A C42 C43 146(4) . . ? C42A C42 C43 107(4) . . ? N1 C42 C43 121(3) . . ? N1A C42 C46A 56(3) . . ? C42A C42 C46A 161(4) . . ? N1 C42 C46A 31.6(12) . . ? C43 C42 C46A 90(3) . . ? N1A C42 C43A 170(3) . . ? C42A C42 C43A 69(3) . . ? N1 C42 C43A 158(3) . . ? C43 C42 C43A 38(2) . . ? C46A C42 C43A 127(3) . . ? N1A C42 C44A 134(3) . . ? C42A C42 C44A 117(4) . . ? N1 C42 C44A 110(2) . . ? C43 C42 C44A 14(3) . . ? C46A C42 C44A 79(2) . . ? C43A C42 C44A 48(2) . . ? C42 C42A N1A 36(2) . . ? C42 C42A C43A 78(4) . . ? N1A C42A C43A 114(3) . . ? C42 C42A C43 47(3) . . ? N1A C42A C43 83(2) . . ? C43A C42A C43 31.6(18) . . ? C44A C43 C43A 128(10) . . ? C44A C43 C44 36(6) . . ? C43A C43 C44 163(6) . . ? C44A C43 C42 133(9) . . ? C43A C43 C42 78(4) . . ? C44 C43 C42 116(4) . . ? C44A C43 C45A 49(7) . . ? C43A C43 C45A 153(5) . . ? C44 C43 C45A 29.7(17) . . ? C42 C43 C45A 89(3) . . ? C44A C43 C42A 148(8) . . ? C43A C43 C42A 52(3) . . ? C44 C43 C42A 141(3) . . ? C42 C43 C42A 25.7(16) . . ? C45A C43 C42A 114(3) . . ? C43 C43A C44A 20(4) . . ? C43 C43A C42A 96(4) . . ? C44A C43A C42A 111(3) . . ? C43 C43A C42 64(4) . . ? C44A C43A C42 79(3) . . ? C42A C43A C42 32.3(15) . . ? C45A C44 C44A 89(5) . . ? C45A C44 C43 84(4) . . ? C44A C44 C43 21(4) . . ? C45A C44 C45 44(4) . . ? C44A C44 C45 132(4) . . ? C43 C44 C45 122(3) . . ? C43 C44A C44 122(9) . . ? C43 C44A C45A 108(8) . . ? C44 C44A C45A 38(3) . . ? C43 C44A C43A 33(6) . . ? C44 C44A C43A 155(5) . . ? C45A C44A C43A 133(4) . . ? C43 C44A C42 34(6) . . ? C44 C44A C42 109(4) . . ? C45A C44A C42 80(3) . . ? C43A C44A C42 53(2) . . ? C45A C45 C46 94(3) . . ? C45A C45 C44 31(2) . . ? C46 C45 C44 119(3) . . ? C45A C45 C46A 62(3) . . ? C46 C45 C46A 32.7(13) . . ? C44 C45 C46A 87(2) . . ? C44 C45A C45 105(5) . . ? C44 C45A C44A 53(4) . . ? C45 C45A C44A 157(5) . . ? C44 C45A C46A 141(5) . . ? C45 C45A C46A 79(3) . . ? C44A C45A C46A 112(4) . . ? C44 C45A C43 66(4) . . ? C45 C45A C43 151(4) . . ? C44A C45A C43 22(3) . . ? C46A C45A C43 91(3) . . ? C44 C45A C46 143(5) . . ? C45 C45A C46 51(2) . . ? C44A C45A C46 140(4) . . ? C46A C45A C46 28.3(14) . . ? C43 C45A C46 118(3) . . ? C46A C46 N1 35(2) . . ? C46A C46 C45 86(3) . . ? N1 C46 C45 120(2) . . ? C46A C46 C45A 52(3) . . ? N1 C46 C45A 87.2(19) . . ? C45 C46 C45A 34.6(14) . . ? C46A C46 S1 137(3) . 7 ? N1 C46 S1 137.2(14) . 7 ? C45 C46 S1 88.6(15) . 7 ? C45A C46 S1 108.5(14) . 7 ? N1 C46A C46 107(4) . . ? N1 C46A N1A 32(2) . . ? C46 C46A N1A 139(4) . . ? N1 C46A C45A 153(4) . . ? C46 C46A C45A 100(3) . . ? N1A C46A C45A 121(3) . . ? N1 C46A C42 64(3) . . ? C46 C46A C42 169(4) . . ? N1A C46A C42 33.0(13) . . ? C45A C46A C42 89(2) . . ? N1 C46A C45 163(4) . . ? C46 C46A C45 62(3) . . ? N1A C46A C45 157(3) . . ? C45A C46A C45 39.0(16) . . ? C42 C46A C45 125(2) . . ? _diffrn_measured_fraction_theta_max 0.482 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.482 _refine_diff_density_max 2.101 _refine_diff_density_min -3.591 _refine_diff_density_rms 0.161 #===END data_lmxy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; THIOSALICYLATO(TRIPHENYLPHOSPHINE)(xylylisocyanide)PLATINUM(II) ; _chemical_formula_moiety 'C33 H28 N O2 P Pt S' _chemical_formula_sum 'C37 H34 N O3 P Pt S' _chemical_formula_weight 798.77 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.51580(10) _cell_length_b 15.1613(2) _cell_length_c 21.4698(2) _cell_angle_alpha 73.3460(10) _cell_angle_beta 85.5760(10) _cell_angle_gamma 87.6300(10) _cell_volume 3268.98(6) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 4.442 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.4423 _exptl_absorpt_correction_T_max 0.7005 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27558 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 27.82 _reflns_number_total 12946 _reflns_number_gt 11618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTO' _computing_publication_material 'SHELX' _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 w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+3.5737P] 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 12946 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 1.313 _refine_ls_shift/su_mean 0.056 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.858824(10) 0.765922(8) 0.457972(5) 0.02121(4) Uani 1 d . . . P1 P 1.07664(7) 0.78537(6) 0.44499(4) 0.02119(16) Uani 1 d . . . S1 S 0.63845(7) 0.75236(7) 0.48531(4) 0.03054(19) Uani 1 d . . . N1 N 0.8037(3) 0.8463(2) 0.31540(14) 0.0315(7) Uani 1 d . . . O11 O 0.8855(2) 0.69855(16) 0.55223(10) 0.0270(5) Uani 1 d . . . O12 O 0.8524(3) 0.67491(18) 0.65802(12) 0.0405(6) Uani 1 d . . . C12 C 0.8276(3) 0.7179(2) 0.60252(16) 0.0270(7) Uani 1 d . . . C13 C 0.8283(3) 0.8171(2) 0.36946(17) 0.0280(7) Uani 1 d . . . C111 C 0.6373(3) 0.8112(2) 0.54627(16) 0.0265(7) Uani 1 d . . . C112 C 0.5414(3) 0.8777(3) 0.54728(19) 0.0373(9) Uani 1 d . . . H112 H 0.4759 0.8862 0.5186 0.045 Uiso 1 calc R . . C113 C 0.5417(4) 0.9309(3) 0.5896(2) 0.0471(10) Uani 1 d . . . H113 H 0.4762 0.9750 0.5897 0.057 Uiso 1 calc R . . C114 C 0.6376(4) 0.9199(3) 0.6322(2) 0.0452(10) Uani 1 d . . . H114 H 0.6409 0.9592 0.6588 0.054 Uiso 1 calc R . . C115 C 0.7282(3) 0.8506(3) 0.63501(17) 0.0350(8) Uani 1 d . . . H115 H 0.7898 0.8402 0.6659 0.042 Uiso 1 calc R . . C116 C 0.7297(3) 0.7956(2) 0.59266(15) 0.0261(7) Uani 1 d . . . C121 C 0.7733(3) 0.8711(2) 0.25035(15) 0.0255(7) Uani 1 d . . . C122 C 0.8490(3) 0.8350(3) 0.20713(17) 0.0308(8) Uani 1 d . . . C123 C 0.8128(3) 0.8562(3) 0.14414(18) 0.0387(9) Uani 1 d . . . H123 H 0.8606 0.8321 0.1137 0.046 Uiso 1 calc R . . C124 C 0.7078(4) 0.9120(3) 0.12509(18) 0.0455(10) Uani 1 d . . . H124 H 0.6845 0.9251 0.0819 0.055 Uiso 1 calc R . . C125 C 0.6354(3) 0.9493(3) 0.16912(19) 0.0409(9) Uani 1 d . . . H125 H 0.5650 0.9883 0.1552 0.049 Uiso 1 calc R . . C126 C 0.6670(3) 0.9291(3) 0.23302(17) 0.0302(7) Uani 1 d . . . C127 C 0.5923(4) 0.9691(3) 0.2813(2) 0.0497(11) Uani 1 d . . . H12A H 0.5218 1.0064 0.2606 0.075 Uiso 1 calc R . . H12B H 0.6474 1.0070 0.2967 0.075 Uiso 1 calc R . . H12C H 0.5596 0.9196 0.3179 0.075 Uiso 1 calc R . . C128 C 0.9657(4) 0.7761(3) 0.2293(2) 0.0483(11) Uani 1 d . . . H12D H 1.0018 0.7520 0.1944 0.072 Uiso 1 calc R . . H12E H 0.9418 0.7255 0.2671 0.072 Uiso 1 calc R . . H12F H 1.0285 0.8132 0.2404 0.072 Uiso 1 calc R . . C131 C 1.1276(3) 0.8347(2) 0.50691(15) 0.0255(7) Uani 1 d . . . C132 C 1.1564(3) 0.9275(2) 0.49247(17) 0.0308(7) Uani 1 d . . . H132 H 1.1571 0.9651 0.4492 0.037 Uiso 1 calc R . . C133 C 1.1843(4) 0.9648(3) 0.5420(2) 0.0405(9) Uani 1 d . . . H133 H 1.2040 1.0274 0.5321 0.049 Uiso 1 calc R . . C134 C 1.1829(3) 0.9097(3) 0.60558(19) 0.0403(9) Uani 1 d . . . H134 H 1.2016 0.9348 0.6390 0.048 Uiso 1 calc R . . C135 C 1.1543(3) 0.8181(3) 0.62010(18) 0.0402(9) Uani 1 d . . . H135 H 1.1527 0.7811 0.6636 0.048 Uiso 1 calc R . . C136 C 1.1278(3) 0.7798(3) 0.57148(17) 0.0333(8) Uani 1 d . . . H136 H 1.1100 0.7168 0.5819 0.040 Uiso 1 calc R . . C141 C 1.1647(3) 0.6776(2) 0.45531(15) 0.0240(7) Uani 1 d . . . C142 C 1.1049(3) 0.6032(2) 0.44520(15) 0.0267(7) Uani 1 d . . . H142 H 1.0183 0.6081 0.4363 0.032 Uiso 1 calc R . . C143 C 1.1732(3) 0.5209(2) 0.44817(16) 0.0321(8) Uani 1 d . . . H143 H 1.1324 0.4705 0.4418 0.038 Uiso 1 calc R . . C144 C 1.3002(4) 0.5143(3) 0.46050(17) 0.0374(9) Uani 1 d . . . H144 H 1.3466 0.4597 0.4615 0.045 Uiso 1 calc R . . C145 C 1.3600(3) 0.5874(3) 0.47146(18) 0.0379(9) Uani 1 d . . . H145 H 1.4466 0.5820 0.4802 0.045 Uiso 1 calc R . . C146 C 1.2928(3) 0.6690(3) 0.46971(18) 0.0329(8) Uani 1 d . . . H146 H 1.3334 0.7180 0.4782 0.040 Uiso 1 calc R . . C151 C 1.1354(3) 0.8598(2) 0.36636(15) 0.0239(7) Uani 1 d . . . C152 C 1.0732(3) 0.9440(2) 0.34138(16) 0.0299(7) Uani 1 d . . . H152 H 1.0023 0.9609 0.3652 0.036 Uiso 1 calc R . . C153 C 1.1147(4) 1.0031(3) 0.28169(18) 0.0383(9) Uani 1 d . . . H153 H 1.0734 1.0605 0.2656 0.046 Uiso 1 calc R . . C154 C 1.2181(4) 0.9770(3) 0.24562(18) 0.0401(9) Uani 1 d . . . H154 H 1.2458 1.0165 0.2049 0.048 Uiso 1 calc R . . C155 C 1.2797(3) 0.8932(3) 0.26968(17) 0.0384(9) Uani 1 d . . . H155 H 1.3491 0.8759 0.2451 0.046 Uiso 1 calc R . . C156 C 1.2399(3) 0.8342(3) 0.32979(17) 0.0305(7) Uani 1 d . . . H156 H 1.2826 0.7774 0.3460 0.037 Uiso 1 calc R . . Pt2 Pt 0.618163(10) 0.718367(8) 0.050869(5) 0.02147(4) Uani 1 d . . . P2 P 0.40325(7) 0.69837(6) 0.07658(4) 0.02114(16) Uani 1 d . . . S2 S 0.83392(8) 0.74257(7) 0.01699(4) 0.03144(19) Uani 1 d . . . N2 N 0.6999(3) 0.6313(2) 0.18863(13) 0.0289(6) Uani 1 d . . . O21 O 0.56651(18) 0.79216(16) -0.04021(10) 0.0228(5) Uani 1 d . . . O22 O 0.5821(2) 0.8712(2) -0.14153(12) 0.0471(7) Uani 1 d . . . C22 C 0.6281(3) 0.8119(3) -0.09594(17) 0.0326(8) Uani 1 d . . . C23 C 0.6655(3) 0.6607(2) 0.13654(16) 0.0251(7) Uani 1 d . . . C211 C 0.8421(3) 0.7330(2) -0.06402(16) 0.0266(7) Uani 1 d . . . C212 C 0.9576(3) 0.6942(3) -0.08384(18) 0.0366(8) Uani 1 d . . . H212 H 1.0210 0.6738 -0.0541 0.044 Uiso 1 calc R . . C213 C 0.9780(4) 0.6861(3) -0.1458(2) 0.0449(10) Uani 1 d . . . H213 H 1.0554 0.6606 -0.1584 0.054 Uiso 1 calc R . . C214 C 0.8849(4) 0.7152(3) -0.18967(19) 0.0437(10) Uani 1 d . . . H214 H 0.8984 0.7083 -0.2318 0.052 Uiso 1 calc R . . C215 C 0.7733(4) 0.7539(3) -0.17209(18) 0.0421(9) Uani 1 d . . . H215 H 0.7114 0.7744 -0.2027 0.051 Uiso 1 calc R . . C216 C 0.7491(3) 0.7638(2) -0.10823(16) 0.0304(7) Uani 1 d . . . C221 C 0.7486(3) 0.5957(2) 0.25017(15) 0.0266(7) Uani 1 d . . . C222 C 0.8586(3) 0.5407(3) 0.25455(17) 0.0311(8) Uani 1 d . . . C223 C 0.9032(3) 0.5038(3) 0.31606(18) 0.0367(8) Uani 1 d . . . H223 H 0.9758 0.4647 0.3212 0.044 Uiso 1 calc R . . C224 C 0.8418(4) 0.5238(3) 0.36995(18) 0.0404(9) Uani 1 d . . . H224 H 0.8730 0.4980 0.4113 0.048 Uiso 1 calc R . . C225 C 0.7352(3) 0.5815(3) 0.36365(17) 0.0372(9) Uani 1 d . . . H225 H 0.6963 0.5956 0.4006 0.045 Uiso 1 calc R . . C226 C 0.6848(3) 0.6190(2) 0.30327(16) 0.0283(7) Uani 1 d . . . C227 C 0.5658(3) 0.6786(3) 0.2961(2) 0.0425(9) Uani 1 d . . . H22A H 0.5773 0.7311 0.2578 0.064 Uiso 1 calc R . . H22B H 0.5489 0.7001 0.3344 0.064 Uiso 1 calc R . . H22C H 0.4942 0.6431 0.2914 0.064 Uiso 1 calc R . . C228 C 0.9256(4) 0.5223(3) 0.1942(2) 0.0469(10) Uani 1 d . . . H22D H 1.0023 0.4854 0.2060 0.070 Uiso 1 calc R . . H22E H 0.9482 0.5803 0.1626 0.070 Uiso 1 calc R . . H22F H 0.8692 0.4894 0.1754 0.070 Uiso 1 calc R . . C231 C 0.3317(3) 0.6285(2) 0.03260(15) 0.0265(7) Uani 1 d . . . C232 C 0.2145(3) 0.5877(3) 0.05575(19) 0.0407(9) Uani 1 d . . . H232 H 0.1703 0.5992 0.0925 0.049 Uiso 1 calc R . . C233 C 0.1627(4) 0.5301(3) 0.0248(2) 0.0485(11) Uani 1 d . . . H233 H 0.0839 0.5024 0.0409 0.058 Uiso 1 calc R . . C234 C 0.2257(4) 0.5133(3) -0.0290(2) 0.0474(11) Uani 1 d . . . H234 H 0.1904 0.4743 -0.0498 0.057 Uiso 1 calc R . . C235 C 0.3410(4) 0.5540(3) -0.0525(2) 0.0479(10) Uani 1 d . . . H235 H 0.3838 0.5430 -0.0897 0.057 Uiso 1 calc R . . C236 C 0.3946(3) 0.6108(3) -0.02212(18) 0.0363(8) Uani 1 d . . . H236 H 0.4739 0.6376 -0.0384 0.044 Uiso 1 calc R . . C241 C 0.3191(3) 0.8089(2) 0.06144(15) 0.0262(7) Uani 1 d . . . C242 C 0.3848(4) 0.8830(3) 0.06777(19) 0.0377(9) Uani 1 d . . . H242 H 0.4714 0.8758 0.0765 0.045 Uiso 1 calc R . . C243 C 0.3233(4) 0.9681(3) 0.0613(2) 0.0477(10) Uani 1 d . . . H243 H 0.3685 1.0180 0.0657 0.057 Uiso 1 calc R . . C244 C 0.1973(4) 0.9789(3) 0.04876(19) 0.0455(10) Uani 1 d . . . H244 H 0.1556 1.0361 0.0450 0.055 Uiso 1 calc R . . C245 C 0.1311(4) 0.9061(3) 0.04152(19) 0.0433(10) Uani 1 d . . . H245 H 0.0448 0.9143 0.0323 0.052 Uiso 1 calc R . . C246 C 0.1907(3) 0.8208(3) 0.04774(17) 0.0356(8) Uani 1 d . . . H246 H 0.1450 0.7715 0.0428 0.043 Uiso 1 calc R . . C251 C 0.3521(3) 0.6371(2) 0.16050(15) 0.0250(7) Uani 1 d . . . C252 C 0.3769(4) 0.5431(3) 0.18200(17) 0.0382(9) Uani 1 d . . . H252 H 0.4277 0.5142 0.1553 0.046 Uiso 1 calc R . . C253 C 0.3272(4) 0.4914(3) 0.24265(19) 0.0438(10) Uani 1 d . . . H253 H 0.3413 0.4273 0.2562 0.053 Uiso 1 calc R . . C254 C 0.2569(3) 0.5346(3) 0.28316(17) 0.0385(9) Uani 1 d . . . H254 H 0.2233 0.4997 0.3243 0.046 Uiso 1 calc R . . C255 C 0.2363(3) 0.6276(3) 0.26354(17) 0.0366(9) Uani 1 d . . . H255 H 0.1907 0.6566 0.2918 0.044 Uiso 1 calc R . . C256 C 0.2823(3) 0.6802(3) 0.20181(16) 0.0298(7) Uani 1 d . . . H256 H 0.2663 0.7441 0.1883 0.036 Uiso 1 calc R . . O91 O 0.8302(3) 0.1193(3) 0.23139(15) 0.0632(9) Uani 1 d . . . C91 C 0.9303(4) 0.0809(3) 0.1393(2) 0.0499(10) Uani 1 d . . . H91A H 0.9937 0.1244 0.1148 0.075 Uiso 1 calc R . . H91B H 0.8890 0.0550 0.1099 0.075 Uiso 1 calc R . . H91C H 0.9715 0.0319 0.1715 0.075 Uiso 1 calc R . . C92 C 0.8334(4) 0.1290(3) 0.1729(2) 0.0484(10) Uani 1 d . . . C93 C 0.7404(4) 0.1921(4) 0.1305(2) 0.0677(15) Uani 1 d . . . H93A H 0.6680 0.1572 0.1261 0.102 Uiso 1 calc R . . H93B H 0.7820 0.2198 0.0878 0.102 Uiso 1 calc R . . H93C H 0.7112 0.2401 0.1502 0.102 Uiso 1 calc R . . O81 O 0.6527(4) 0.4068(3) 0.2244(2) 0.0908(13) Uani 1 d . . . C81 C 0.5899(5) 0.3682(4) 0.3369(3) 0.0709(15) Uani 1 d . . . H81A H 0.6640 0.4009 0.3420 0.106 Uiso 1 calc R . . H81B H 0.5852 0.3095 0.3702 0.106 Uiso 1 calc R . . H81C H 0.5134 0.4047 0.3410 0.106 Uiso 1 calc R . . C82 C 0.6008(4) 0.3522(4) 0.2708(3) 0.0581(12) Uani 1 d . . . C83 C 0.5414(6) 0.2690(4) 0.2642(3) 0.091(2) Uani 1 d . . . H83A H 0.5281 0.2769 0.2187 0.137 Uiso 1 calc R . . H83B H 0.4601 0.2597 0.2895 0.137 Uiso 1 calc R . . H83C H 0.5971 0.2160 0.2800 0.137 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02251(6) 0.02262(7) 0.01949(6) -0.00755(5) -0.00134(4) -0.00079(5) P1 0.0226(4) 0.0199(4) 0.0211(4) -0.0059(3) -0.0021(3) -0.0001(3) S1 0.0237(4) 0.0370(5) 0.0335(4) -0.0140(4) -0.0012(3) -0.0037(4) N1 0.0314(14) 0.0397(19) 0.0235(15) -0.0074(13) -0.0057(11) -0.0065(13) O11 0.0305(11) 0.0251(13) 0.0232(11) -0.0041(9) -0.0012(9) 0.0021(10) O12 0.0562(16) 0.0362(16) 0.0234(13) 0.0003(11) -0.0039(11) 0.0053(13) C12 0.0322(16) 0.0225(18) 0.0248(17) -0.0045(13) 0.0001(13) -0.0039(14) C13 0.0229(15) 0.030(2) 0.0321(19) -0.0108(15) -0.0007(13) -0.0049(14) C111 0.0257(15) 0.0271(19) 0.0265(17) -0.0085(14) 0.0048(12) -0.0042(14) C112 0.0306(17) 0.040(2) 0.041(2) -0.0110(17) -0.0004(15) 0.0032(16) C113 0.042(2) 0.048(3) 0.054(3) -0.023(2) 0.0048(18) 0.0105(19) C114 0.048(2) 0.046(3) 0.048(2) -0.028(2) 0.0063(18) 0.0035(19) C115 0.0375(18) 0.040(2) 0.0307(19) -0.0158(16) 0.0013(14) -0.0041(16) C116 0.0282(15) 0.0258(19) 0.0216(16) -0.0039(13) 0.0046(12) -0.0027(14) C121 0.0278(15) 0.0308(19) 0.0195(15) -0.0088(13) -0.0027(12) -0.0066(14) C122 0.0293(16) 0.030(2) 0.0367(19) -0.0150(15) 0.0018(14) -0.0089(15) C123 0.0408(19) 0.052(3) 0.0306(19) -0.0225(18) 0.0063(15) -0.0168(18) C124 0.052(2) 0.061(3) 0.0246(19) -0.0087(18) -0.0063(16) -0.025(2) C125 0.0320(18) 0.045(3) 0.042(2) -0.0026(18) -0.0145(16) -0.0050(17) C126 0.0266(15) 0.033(2) 0.0331(18) -0.0134(15) -0.0009(13) -0.0055(15) C127 0.0325(19) 0.060(3) 0.066(3) -0.036(2) 0.0038(18) 0.0016(19) C128 0.0349(19) 0.045(3) 0.073(3) -0.030(2) -0.0021(19) 0.0054(18) C131 0.0241(14) 0.0292(19) 0.0252(16) -0.0109(14) -0.0017(12) -0.0012(14) C132 0.0374(18) 0.0267(19) 0.0308(18) -0.0115(15) -0.0028(14) -0.0035(15) C133 0.044(2) 0.035(2) 0.050(2) -0.0241(19) -0.0066(18) -0.0007(18) C134 0.0375(19) 0.054(3) 0.041(2) -0.029(2) -0.0077(16) 0.0020(18) C135 0.042(2) 0.056(3) 0.0257(18) -0.0142(17) -0.0088(15) -0.0014(19) C136 0.0381(18) 0.031(2) 0.0317(19) -0.0090(15) -0.0065(15) -0.0038(16) C141 0.0287(15) 0.0227(17) 0.0202(15) -0.0058(12) -0.0013(12) 0.0008(13) C142 0.0316(16) 0.0264(19) 0.0224(16) -0.0074(13) -0.0005(13) -0.0025(14) C143 0.049(2) 0.0215(19) 0.0251(17) -0.0065(14) 0.0032(15) -0.0026(16) C144 0.049(2) 0.027(2) 0.0307(19) -0.0033(15) 0.0008(16) 0.0121(17) C145 0.0336(18) 0.035(2) 0.042(2) -0.0057(17) -0.0081(16) 0.0099(16) C146 0.0323(17) 0.027(2) 0.041(2) -0.0100(15) -0.0071(15) 0.0010(15) C151 0.0244(14) 0.0265(18) 0.0222(15) -0.0087(13) -0.0030(12) -0.0021(13) C152 0.0307(16) 0.030(2) 0.0298(18) -0.0103(15) -0.0039(13) -0.0004(15) C153 0.048(2) 0.032(2) 0.0317(19) -0.0003(15) -0.0106(16) -0.0044(17) C154 0.051(2) 0.042(2) 0.0249(18) -0.0039(16) 0.0009(16) -0.0149(19) C155 0.0394(19) 0.050(3) 0.0278(19) -0.0146(17) 0.0086(15) -0.0133(18) C156 0.0307(16) 0.031(2) 0.0310(18) -0.0103(15) -0.0008(14) -0.0026(15) Pt2 0.02368(6) 0.02344(7) 0.01719(6) -0.00566(5) -0.00207(4) 0.00135(5) P2 0.0230(4) 0.0222(4) 0.0177(4) -0.0053(3) -0.0006(3) 0.0003(3) S2 0.0280(4) 0.0406(5) 0.0278(4) -0.0124(4) -0.0032(3) -0.0021(4) N2 0.0332(14) 0.0304(17) 0.0230(14) -0.0059(12) -0.0057(11) -0.0035(12) O21 0.0174(9) 0.0305(13) 0.0157(10) 0.0002(9) 0.0007(8) 0.0020(9) O22 0.0441(15) 0.0546(19) 0.0302(14) 0.0069(12) -0.0032(11) 0.0058(13) C22 0.0349(17) 0.032(2) 0.0293(18) -0.0046(15) -0.0041(14) -0.0102(15) C23 0.0271(15) 0.0212(18) 0.0283(17) -0.0087(13) -0.0013(13) -0.0034(13) C211 0.0314(16) 0.0210(18) 0.0280(17) -0.0089(13) 0.0049(13) -0.0057(14) C212 0.0385(18) 0.033(2) 0.037(2) -0.0101(16) 0.0034(15) 0.0033(16) C213 0.051(2) 0.043(3) 0.043(2) -0.0195(19) 0.0071(18) 0.0060(19) C214 0.060(2) 0.045(3) 0.029(2) -0.0190(17) 0.0061(17) -0.001(2) C215 0.050(2) 0.045(3) 0.0284(19) -0.0071(17) -0.0014(16) -0.0023(19) C216 0.0423(18) 0.0240(19) 0.0246(17) -0.0053(14) -0.0032(14) -0.0058(15) C221 0.0289(15) 0.0273(19) 0.0221(16) -0.0028(13) -0.0067(12) -0.0051(14) C222 0.0316(16) 0.030(2) 0.0343(19) -0.0127(15) -0.0022(14) -0.0028(15) C223 0.0339(18) 0.033(2) 0.042(2) -0.0069(17) -0.0132(16) 0.0002(16) C224 0.045(2) 0.045(2) 0.0269(19) 0.0006(16) -0.0143(16) -0.0096(18) C225 0.044(2) 0.043(2) 0.0253(18) -0.0100(16) -0.0022(15) -0.0103(18) C226 0.0303(16) 0.029(2) 0.0249(17) -0.0056(14) -0.0008(13) -0.0073(14) C227 0.0363(19) 0.047(3) 0.044(2) -0.0140(19) 0.0011(16) 0.0025(18) C228 0.044(2) 0.053(3) 0.046(2) -0.021(2) 0.0018(18) 0.007(2) C231 0.0340(16) 0.0232(18) 0.0231(16) -0.0072(13) -0.0046(13) 0.0008(14) C232 0.0398(19) 0.050(3) 0.037(2) -0.0181(18) -0.0017(16) -0.0113(18) C233 0.045(2) 0.048(3) 0.055(3) -0.014(2) -0.0125(19) -0.014(2) C234 0.062(3) 0.031(2) 0.058(3) -0.022(2) -0.028(2) 0.003(2) C235 0.059(2) 0.051(3) 0.044(2) -0.029(2) -0.0084(19) 0.010(2) C236 0.0401(19) 0.035(2) 0.037(2) -0.0163(16) 0.0001(15) 0.0011(17) C241 0.0293(15) 0.0280(19) 0.0197(15) -0.0053(13) 0.0003(12) 0.0024(14) C242 0.0374(18) 0.033(2) 0.046(2) -0.0151(17) -0.0071(16) 0.0031(17) C243 0.062(3) 0.030(2) 0.053(3) -0.0168(19) 0.000(2) 0.004(2) C244 0.060(2) 0.032(2) 0.035(2) -0.0007(16) 0.0077(18) 0.019(2) C245 0.0383(19) 0.040(2) 0.043(2) -0.0001(18) 0.0007(16) 0.0149(18) C246 0.0320(17) 0.036(2) 0.0347(19) -0.0042(16) -0.0039(14) 0.0027(16) C251 0.0235(14) 0.0306(19) 0.0207(15) -0.0069(13) 0.0000(12) -0.0023(13) C252 0.050(2) 0.032(2) 0.0271(18) -0.0043(15) 0.0076(16) 0.0083(18) C253 0.059(2) 0.032(2) 0.034(2) -0.0021(16) 0.0028(18) 0.0030(19) C254 0.0392(19) 0.052(3) 0.0197(17) -0.0028(16) 0.0036(14) -0.0074(18) C255 0.0384(18) 0.048(2) 0.0247(18) -0.0141(16) 0.0067(14) -0.0003(17) C256 0.0334(17) 0.028(2) 0.0269(17) -0.0079(14) 0.0020(13) -0.0016(15) O91 0.070(2) 0.079(3) 0.0391(18) -0.0135(16) -0.0029(15) -0.0042(18) C91 0.054(2) 0.046(3) 0.050(3) -0.013(2) -0.009(2) -0.005(2) C92 0.046(2) 0.051(3) 0.043(2) -0.004(2) -0.0027(18) -0.013(2) C93 0.050(3) 0.088(4) 0.056(3) -0.007(3) -0.006(2) 0.013(3) O81 0.106(3) 0.094(3) 0.070(3) -0.017(2) 0.008(2) -0.051(3) C81 0.079(3) 0.067(4) 0.063(3) -0.007(3) -0.018(3) -0.004(3) C82 0.048(2) 0.048(3) 0.075(3) -0.011(3) -0.003(2) -0.011(2) C83 0.090(4) 0.070(4) 0.124(6) -0.048(4) 0.021(4) -0.027(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 Pt1 C13 1.883(3) . ? Pt1 O11 2.024(2) . ? Pt1 P1 2.3068(8) . ? Pt1 S1 2.3490(8) . ? P1 C141 1.810(3) . ? P1 C151 1.819(3) . ? P1 C131 1.823(3) . ? S1 C111 1.782(3) . ? S1 C112 2.739(4) . ? S1 C116 2.815(3) . ? S1 C13 3.022(3) . ? S1 O11 3.035(2) . ? S1 C12 3.240(3) . ? N1 C13 1.163(4) . ? N1 C121 1.397(4) . ? O11 C12 1.299(4) . ? O12 C12 1.225(4) . ? C12 C116 1.511(5) . ? C111 C112 1.400(5) . ? C111 C116 1.409(4) . ? C112 C113 1.378(6) . ? C113 C114 1.386(6) . ? C114 C115 1.380(5) . ? C115 C116 1.397(5) . ? C121 C122 1.391(5) . ? C121 C126 1.398(5) . ? C122 C123 1.377(5) . ? C122 C128 1.512(5) . ? C123 C124 1.377(6) . ? C124 C125 1.398(6) . ? C125 C126 1.381(5) . ? C126 C127 1.502(5) . ? C131 C132 1.393(5) . ? C131 C136 1.398(5) . ? C132 C133 1.393(5) . ? C133 C134 1.381(6) . ? C134 C135 1.374(6) . ? C135 C136 1.382(5) . ? C141 C142 1.391(5) . ? C141 C146 1.398(4) . ? C142 C143 1.401(5) . ? C143 C144 1.375(5) . ? C144 C145 1.382(6) . ? C145 C146 1.391(5) . ? C151 C152 1.392(5) . ? C151 C156 1.407(4) . ? C152 C153 1.387(5) . ? C153 C154 1.396(5) . ? C154 C155 1.382(6) . ? C155 C156 1.388(5) . ? Pt2 C23 1.892(3) . ? Pt2 O21 2.057(2) . ? Pt2 P2 2.2962(8) . ? Pt2 S2 2.3395(8) . ? P2 C241 1.818(3) . ? P2 C251 1.825(3) . ? P2 C231 1.824(3) . ? S2 C211 1.782(3) . ? S2 C212 2.704(4) . ? S2 C216 2.824(3) . ? S2 C23 2.987(3) . ? S2 O21 3.132(2) . ? S2 C22 3.291(3) . ? N2 C23 1.159(4) . ? N2 C221 1.404(4) . ? O21 C22 1.277(4) . ? O22 C22 1.238(4) . ? C22 C216 1.484(5) . ? C211 C216 1.388(5) . ? C211 C212 1.416(5) . ? C212 C213 1.370(5) . ? C213 C214 1.382(6) . ? C214 C215 1.365(5) . ? C215 C216 1.424(5) . ? C221 C222 1.392(5) . ? C221 C226 1.402(5) . ? C222 C223 1.388(5) . ? C222 C228 1.518(5) . ? C223 C224 1.385(5) . ? C224 C225 1.383(6) . ? C225 C226 1.394(5) . ? C226 C227 1.505(5) . ? C231 C236 1.392(5) . ? C231 C232 1.394(5) . ? C232 C233 1.388(5) . ? C233 C234 1.370(6) . ? C234 C235 1.376(6) . ? C235 C236 1.379(5) . ? C241 C242 1.388(5) . ? C241 C246 1.397(5) . ? C242 C243 1.394(5) . ? C243 C244 1.367(6) . ? C244 C245 1.381(6) . ? C245 C246 1.389(5) . ? C251 C252 1.387(5) . ? C251 C256 1.395(4) . ? C252 C253 1.388(5) . ? C253 C254 1.386(5) . ? C254 C255 1.363(5) . ? C255 C256 1.398(5) . ? O91 C92 1.221(5) . ? C91 C92 1.489(6) . ? C92 C93 1.503(6) . ? O81 C82 1.208(6) . ? C81 C82 1.501(7) . ? C82 C83 1.476(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Pt1 O11 174.16(12) . . ? C13 Pt1 P1 96.06(9) . . ? O11 Pt1 P1 86.45(6) . . ? C13 Pt1 S1 90.46(10) . . ? O11 Pt1 S1 87.56(6) . . ? P1 Pt1 S1 171.60(3) . . ? C141 P1 C151 105.71(15) . . ? C141 P1 C131 105.99(15) . . ? C151 P1 C131 106.88(15) . . ? C141 P1 Pt1 112.57(11) . . ? C151 P1 Pt1 115.24(10) . . ? C131 P1 Pt1 109.88(10) . . ? C111 S1 Pt1 95.00(10) . . ? C111 S1 C112 26.74(13) . . ? Pt1 S1 C112 113.24(8) . . ? C111 S1 C116 24.73(12) . . ? Pt1 S1 C116 77.15(7) . . ? C112 S1 C116 51.46(10) . . ? C111 S1 C13 116.38(13) . . ? Pt1 S1 C13 38.53(6) . . ? C112 S1 C13 118.45(11) . . ? C116 S1 C13 108.70(9) . . ? C111 S1 O11 73.44(11) . . ? Pt1 S1 O11 41.78(4) . . ? C112 S1 O11 99.88(9) . . ? C116 S1 O11 48.97(8) . . ? C13 S1 O11 80.21(8) . . ? C111 S1 C12 52.38(12) . . ? Pt1 S1 C12 61.86(6) . . ? C112 S1 C12 79.08(10) . . ? C116 S1 C12 27.79(9) . . ? C13 S1 C12 99.86(9) . . ? O11 S1 C12 23.61(7) . . ? C13 N1 C121 173.6(4) . . ? C12 O11 Pt1 125.5(2) . . ? C12 O11 S1 87.08(17) . . ? Pt1 O11 S1 50.65(5) . . ? O12 C12 O11 121.1(3) . . ? O12 C12 C116 119.2(3) . . ? O11 C12 C116 119.7(3) . . ? O12 C12 S1 148.5(2) . . ? O11 C12 S1 69.31(16) . . ? C116 C12 S1 60.25(17) . . ? N1 C13 Pt1 176.5(3) . . ? N1 C13 S1 125.9(2) . . ? Pt1 C13 S1 51.01(8) . . ? C112 C111 C116 118.3(3) . . ? C112 C111 S1 118.3(3) . . ? C116 C111 S1 123.3(2) . . ? C113 C112 C111 121.0(3) . . ? C113 C112 S1 155.6(3) . . ? C111 C112 S1 34.93(17) . . ? C112 C113 C114 120.6(4) . . ? C115 C114 C113 119.3(4) . . ? C114 C115 C116 121.0(3) . . ? C115 C116 C111 119.5(3) . . ? C115 C116 C12 116.9(3) . . ? C111 C116 C12 123.5(3) . . ? C115 C116 S1 151.2(2) . . ? C111 C116 S1 31.93(16) . . ? C12 C116 S1 92.0(2) . . ? C122 C121 N1 117.9(3) . . ? C122 C121 C126 124.1(3) . . ? N1 C121 C126 118.0(3) . . ? C123 C122 C121 116.9(3) . . ? C123 C122 C128 122.5(3) . . ? C121 C122 C128 120.6(3) . . ? C122 C123 C124 121.0(3) . . ? C123 C124 C125 120.9(3) . . ? C126 C125 C124 120.2(3) . . ? C125 C126 C121 116.9(3) . . ? C125 C126 C127 121.6(3) . . ? C121 C126 C127 121.5(3) . . ? C132 C131 C136 119.0(3) . . ? C132 C131 P1 121.6(3) . . ? C136 C131 P1 119.2(3) . . ? C131 C132 C133 120.2(3) . . ? C134 C133 C132 119.9(4) . . ? C135 C134 C133 120.1(3) . . ? C134 C135 C136 120.7(4) . . ? C135 C136 C131 120.0(4) . . ? C142 C141 C146 119.4(3) . . ? C142 C141 P1 118.9(2) . . ? C146 C141 P1 121.6(3) . . ? C141 C142 C143 120.3(3) . . ? C144 C143 C142 119.7(3) . . ? C143 C144 C145 120.5(3) . . ? C144 C145 C146 120.5(3) . . ? C145 C146 C141 119.6(3) . . ? C152 C151 C156 119.3(3) . . ? C152 C151 P1 118.6(2) . . ? C156 C151 P1 122.1(3) . . ? C153 C152 C151 120.7(3) . . ? C152 C153 C154 119.6(4) . . ? C155 C154 C153 120.1(3) . . ? C154 C155 C156 120.6(3) . . ? C155 C156 C151 119.7(3) . . ? C23 Pt2 O21 174.83(12) . . ? C23 Pt2 P2 94.84(10) . . ? O21 Pt2 P2 85.44(6) . . ? C23 Pt2 S2 89.15(10) . . ? O21 Pt2 S2 90.63(6) . . ? P2 Pt2 S2 175.98(3) . . ? C241 P2 C251 104.43(15) . . ? C241 P2 C231 109.10(15) . . ? C251 P2 C231 100.76(15) . . ? C241 P2 Pt2 110.77(11) . . ? C251 P2 Pt2 117.64(10) . . ? C231 P2 Pt2 113.29(11) . . ? C211 S2 Pt2 102.92(11) . . ? C211 S2 C212 28.34(13) . . ? Pt2 S2 C212 125.57(9) . . ? C211 S2 C216 23.58(13) . . ? Pt2 S2 C216 83.89(8) . . ? C212 S2 C216 51.90(11) . . ? C211 S2 C23 133.49(13) . . ? Pt2 S2 C23 39.30(6) . . ? C212 S2 C23 139.90(11) . . ? C216 S2 C23 120.76(10) . . ? C211 S2 O21 70.64(11) . . ? Pt2 S2 O21 41.04(4) . . ? C212 S2 O21 98.73(9) . . ? C216 S2 O21 47.62(8) . . ? C23 S2 O21 80.24(7) . . ? C211 S2 C22 50.30(12) . . ? Pt2 S2 C22 63.18(6) . . ? C212 S2 C22 78.59(10) . . ? C216 S2 C22 26.72(10) . . ? C23 S2 C22 102.47(9) . . ? O21 S2 C22 22.77(7) . . ? C23 N2 C221 176.8(3) . . ? C22 O21 Pt2 131.7(2) . . ? C22 O21 S2 85.62(18) . . ? Pt2 O21 S2 48.32(4) . . ? O22 C22 O21 118.3(3) . . ? O22 C22 C216 119.3(3) . . ? O21 C22 C216 122.3(3) . . ? O22 C22 S2 152.0(3) . . ? O21 C22 S2 71.61(17) . . ? C216 C22 S2 58.82(17) . . ? N2 C23 Pt2 174.7(3) . . ? N2 C23 S2 125.1(2) . . ? Pt2 C23 S2 51.55(8) . . ? C216 C211 C212 119.4(3) . . ? C216 C211 S2 125.5(3) . . ? C212 C211 S2 115.0(3) . . ? C213 C212 C211 120.9(4) . . ? C213 C212 S2 157.5(3) . . ? C211 C212 S2 36.68(17) . . ? C212 C213 C214 120.0(4) . . ? C215 C214 C213 120.3(4) . . ? C214 C215 C216 121.2(4) . . ? C211 C216 C215 118.2(3) . . ? C211 C216 C22 125.3(3) . . ? C215 C216 C22 116.3(3) . . ? C211 C216 S2 30.89(16) . . ? C215 C216 S2 149.0(3) . . ? C22 C216 S2 94.5(2) . . ? C222 C221 C226 123.9(3) . . ? C222 C221 N2 117.9(3) . . ? C226 C221 N2 118.1(3) . . ? C223 C222 C221 117.1(3) . . ? C223 C222 C228 122.1(3) . . ? C221 C222 C228 120.8(3) . . ? C224 C223 C222 120.7(3) . . ? C225 C224 C223 120.8(3) . . ? C224 C225 C226 121.0(3) . . ? C225 C226 C221 116.4(3) . . ? C225 C226 C227 121.6(3) . . ? C221 C226 C227 122.0(3) . . ? C236 C231 C232 118.6(3) . . ? C236 C231 P2 121.4(3) . . ? C232 C231 P2 119.8(3) . . ? C233 C232 C231 120.3(4) . . ? C234 C233 C232 120.4(4) . . ? C233 C234 C235 119.7(4) . . ? C236 C235 C234 120.8(4) . . ? C235 C236 C231 120.2(4) . . ? C242 C241 C246 119.1(3) . . ? C242 C241 P2 117.6(2) . . ? C246 C241 P2 123.2(3) . . ? C241 C242 C243 120.6(4) . . ? C244 C243 C242 120.0(4) . . ? C243 C244 C245 120.1(4) . . ? C244 C245 C246 120.7(4) . . ? C245 C246 C241 119.5(4) . . ? C252 C251 C256 119.3(3) . . ? C252 C251 P2 118.2(2) . . ? C256 C251 P2 122.4(3) . . ? C251 C252 C253 120.5(3) . . ? C254 C253 C252 119.7(4) . . ? C255 C254 C253 120.2(3) . . ? C254 C255 C256 120.7(3) . . ? C251 C256 C255 119.4(3) . . ? O91 C92 C91 122.2(4) . . ? O91 C92 C93 121.4(4) . . ? C91 C92 C93 116.4(4) . . ? O81 C82 C83 121.2(5) . . ? O81 C82 C81 121.1(5) . . ? C83 C82 C81 117.6(5) . . ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.835 _refine_diff_density_max 1.277 _refine_diff_density_min -1.246 _refine_diff_density_rms 0.085 #===END data_lmptn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis(thioslicylato)bis(triphenylphosphine)ammine-di-platinum methanol solvate, Compound 5 ; _chemical_formula_moiety 'C50 H41 N O4 P2 Pt2 S2' _chemical_formula_sum 'C51.50 H47 N O5.50 P2 Pt2 S2' _chemical_formula_weight 1284.14 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.5133(19) _cell_length_b 11.2727(6) _cell_length_c 26.8046(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.062(2) _cell_angle_gamma 90.00 _cell_volume 9522.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'yellow' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5000 _exptl_absorpt_coefficient_mu 6.075 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.1734 _exptl_absorpt_correction_T_max 0.3879 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD Diffractometr ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25267 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.46 _reflns_number_total 9574 _reflns_number_gt 8492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTO' _computing_publication_material 'SHELX' _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 w=1/[\s^2^(Fo^2^)+(0.0089P)^2^+118.0046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson' _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 9574 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.230 _refine_ls_shift/su_max 0.133 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.635681(8) 0.38407(2) 0.876525(9) 0.02329(8) Uani 1 d . . . Pt2 Pt 0.589713(8) 0.36581(2) 0.750689(9) 0.02151(7) Uani 1 d . . . S1 S 0.64515(7) 0.25693(17) 0.94305(7) 0.0389(5) Uani 1 d . . . S2 S 0.62007(5) 0.49705(15) 0.80471(6) 0.0234(3) Uani 1 d . . . P1 P 0.65331(6) 0.53428(15) 0.92546(6) 0.0234(4) Uani 1 d . . . P2 P 0.64567(5) 0.38420(15) 0.70168(6) 0.0237(4) Uani 1 d . . . N1 N 0.5584(2) 0.2405(6) 0.7089(3) 0.0314(14) Uani 1 d . . . H1 H 0.546(3) 0.278(8) 0.686(3) 0.050 Uiso 1 d . . . H2 H 0.543(3) 0.203(8) 0.725(3) 0.050 Uiso 1 d . . . H3 H 0.576(3) 0.179(8) 0.695(3) 0.050 Uiso 1 d . . . O11 O 0.62002(16) 0.2321(4) 0.83744(18) 0.0300(11) Uani 1 d . . . O12 O 0.58276(18) 0.0720(5) 0.8209(2) 0.0404(13) Uani 1 d . . . O21 O 0.53847(15) 0.3445(4) 0.79753(18) 0.0305(11) Uani 1 d . . . O22 O 0.49111(16) 0.3868(5) 0.85486(18) 0.0355(12) Uani 1 d . . . C11 C 0.5938(3) 0.1977(6) 0.9433(3) 0.0392(19) Uani 1 d . . . C12 C 0.5729(4) 0.1887(8) 0.9895(4) 0.059(3) Uani 1 d . . . H12 H 0.5868 0.2140 1.0186 0.071 Uiso 1 calc R . . C13 C 0.5326(4) 0.1439(10) 0.9927(5) 0.078(4) Uani 1 d . . . H13 H 0.5194 0.1375 1.0240 0.093 Uiso 1 calc R . . C14 C 0.5113(4) 0.1079(10) 0.9501(5) 0.075(4) Uani 1 d . . . H14 H 0.4833 0.0799 0.9524 0.090 Uiso 1 calc R . . C15 C 0.5312(3) 0.1133(8) 0.9048(4) 0.053(2) Uani 1 d . . . H15 H 0.5169 0.0870 0.8761 0.063 Uiso 1 calc R . . C16 C 0.5721(3) 0.1568(6) 0.9005(3) 0.0381(18) Uani 1 d . . . C17 C 0.5928(2) 0.1543(6) 0.8498(3) 0.0316(16) Uani 1 d . . . C21 C 0.5756(2) 0.5890(6) 0.8191(2) 0.0226(14) Uani 1 d . . . C22 C 0.5832(2) 0.7105(6) 0.8209(3) 0.0331(17) Uani 1 d . . . H22 H 0.6102 0.7392 0.8121 0.040 Uiso 1 calc R . . C23 C 0.5522(3) 0.7901(7) 0.8352(3) 0.043(2) Uani 1 d . . . H23 H 0.5582 0.8717 0.8369 0.051 Uiso 1 calc R . . C24 C 0.5123(3) 0.7479(7) 0.8469(4) 0.048(2) Uani 1 d . . . H24 H 0.4909 0.8009 0.8568 0.058 Uiso 1 calc R . . C25 C 0.5038(3) 0.6267(7) 0.8442(3) 0.0403(19) Uani 1 d . . . H25 H 0.4765 0.5991 0.8521 0.048 Uiso 1 calc R . . C26 C 0.5347(2) 0.5457(6) 0.8301(3) 0.0272(15) Uani 1 d . . . C27 C 0.5206(2) 0.4182(6) 0.8283(2) 0.0253(14) Uani 1 d . . . C31 C 0.7004(2) 0.5130(6) 0.9633(3) 0.0280(15) Uani 1 d . . . C32 C 0.7107(2) 0.5945(6) 1.0006(3) 0.0324(16) Uani 1 d . . . H32 H 0.6928 0.6599 1.0062 0.039 Uiso 1 calc R . . C33 C 0.7467(2) 0.5800(7) 1.0292(3) 0.0367(18) Uani 1 d . . . H33 H 0.7534 0.6358 1.0541 0.044 Uiso 1 calc R . . C34 C 0.7732(2) 0.4831(7) 1.0214(3) 0.0381(18) Uani 1 d . . . H34 H 0.7973 0.4722 1.0416 0.046 Uiso 1 calc R . . C35 C 0.7640(2) 0.4034(7) 0.9842(3) 0.0360(18) Uani 1 d . . . H35 H 0.7821 0.3384 0.9789 0.043 Uiso 1 calc R . . C36 C 0.7284(2) 0.4175(7) 0.9542(3) 0.0317(16) Uani 1 d . . . H36 H 0.7229 0.3639 0.9281 0.038 Uiso 1 calc R . . C41 C 0.6101(2) 0.5586(6) 0.9689(3) 0.0289(16) Uani 1 d . . . C42 C 0.5736(2) 0.6139(7) 0.9529(3) 0.0363(18) Uani 1 d . . . H42 H 0.5723 0.6449 0.9203 0.044 Uiso 1 calc R . . C43 C 0.5386(3) 0.6245(9) 0.9841(3) 0.048(2) Uani 1 d . . . H43 H 0.5142 0.6643 0.9729 0.057 Uiso 1 calc R . . C44 C 0.5397(3) 0.5767(9) 1.0315(3) 0.052(2) Uani 1 d . . . H44 H 0.5163 0.5846 1.0530 0.062 Uiso 1 calc R . . C45 C 0.5756(3) 0.5170(9) 1.0467(3) 0.051(2) Uani 1 d . . . H45 H 0.5764 0.4822 1.0786 0.061 Uiso 1 calc R . . C46 C 0.6105(3) 0.5076(8) 1.0159(3) 0.0396(19) Uani 1 d . . . H46 H 0.6347 0.4664 1.0269 0.048 Uiso 1 calc R . . C51 C 0.6644(2) 0.6787(6) 0.8968(2) 0.0234(14) Uani 1 d . . . C52 C 0.6480(2) 0.7843(6) 0.9145(3) 0.0304(16) Uani 1 d . . . H52 H 0.6309 0.7853 0.9432 0.036 Uiso 1 calc R . . C53 C 0.6572(3) 0.8895(7) 0.8891(3) 0.043(2) Uani 1 d . . . H53 H 0.6456 0.9614 0.9005 0.052 Uiso 1 calc R . . C54 C 0.6829(3) 0.8896(8) 0.8475(3) 0.046(2) Uani 1 d . . . H54 H 0.6889 0.9611 0.8308 0.055 Uiso 1 calc R . . C55 C 0.6999(3) 0.7839(8) 0.8305(3) 0.042(2) Uani 1 d . . . H55 H 0.7178 0.7839 0.8024 0.050 Uiso 1 calc R . . C56 C 0.6908(2) 0.6777(7) 0.8547(3) 0.0305(16) Uani 1 d . . . H56 H 0.7022 0.6059 0.8428 0.037 Uiso 1 calc R . . C61 C 0.6478(2) 0.5234(6) 0.6674(3) 0.0274(15) Uani 1 d . . . C62 C 0.6798(3) 0.5414(7) 0.6315(3) 0.0361(18) Uani 1 d . . . H62 H 0.7003 0.4823 0.6261 0.043 Uiso 1 calc R . . C63 C 0.6811(3) 0.6439(7) 0.6045(3) 0.045(2) Uani 1 d . . . H63 H 0.7031 0.6564 0.5814 0.054 Uiso 1 calc R . . C64 C 0.6500(3) 0.7296(8) 0.6109(3) 0.049(2) Uani 1 d . . . H64 H 0.6504 0.7989 0.5914 0.059 Uiso 1 calc R . . C65 C 0.6184(3) 0.7127(7) 0.6461(3) 0.045(2) Uani 1 d . . . H65 H 0.5973 0.7709 0.6505 0.054 Uiso 1 calc R . . C66 C 0.6176(2) 0.6105(7) 0.6747(3) 0.0343(17) Uani 1 d . . . H66 H 0.5965 0.6004 0.6992 0.041 Uiso 1 calc R . . C71 C 0.6511(2) 0.2764(6) 0.6511(3) 0.0273(15) Uani 1 d . . . C72 C 0.6182(2) 0.2696(7) 0.6167(3) 0.0334(17) Uani 1 d . . . H72 H 0.5940 0.3175 0.6206 0.040 Uiso 1 calc R . . C73 C 0.6211(3) 0.1921(8) 0.5767(3) 0.043(2) Uani 1 d . . . H73 H 0.5987 0.1868 0.5537 0.052 Uiso 1 calc R . . C74 C 0.6567(3) 0.1230(8) 0.5706(3) 0.052(2) Uani 1 d . . . H74 H 0.6586 0.0708 0.5434 0.062 Uiso 1 calc R . . C75 C 0.6894(3) 0.1305(8) 0.6045(3) 0.047(2) Uani 1 d . . . H75 H 0.7137 0.0833 0.6002 0.056 Uiso 1 calc R . . C76 C 0.6869(2) 0.2063(7) 0.6446(3) 0.0365(18) Uani 1 d . . . H76 H 0.7094 0.2106 0.6676 0.044 Uiso 1 calc R . . C81 C 0.6944(2) 0.3771(6) 0.7388(2) 0.0263(14) Uani 1 d . . . C82 C 0.7234(2) 0.4701(7) 0.7409(3) 0.0300(16) Uani 1 d . . . H82 H 0.7199 0.5370 0.7204 0.036 Uiso 1 calc R . . C83 C 0.7576(3) 0.4636(8) 0.7736(3) 0.041(2) Uani 1 d . . . H83 H 0.7776 0.5254 0.7748 0.050 Uiso 1 calc R . . C84 C 0.7621(3) 0.3663(8) 0.8043(3) 0.044(2) Uani 1 d . . . H84 H 0.7851 0.3628 0.8267 0.052 Uiso 1 calc R . . C85 C 0.7337(2) 0.2749(7) 0.8026(3) 0.0372(18) Uani 1 d . . . H85 H 0.7372 0.2090 0.8237 0.045 Uiso 1 calc R . . C86 C 0.6997(2) 0.2794(7) 0.7697(3) 0.0361(18) Uani 1 d . . . H86 H 0.6802 0.2162 0.7684 0.043 Uiso 1 calc R . . O91 O 0.1299(2) 0.4312(5) 0.2370(2) 0.0565(17) Uani 1 d . . . C91 C 0.1241(3) 0.5434(9) 0.2157(4) 0.063(3) Uani 1 d . . . O92 O 0.0071(4) 0.4409(12) 0.2719(5) 0.093(4) Uiso 0.67 d P . . C92 C 0.0000 0.539(2) 0.2500 0.056(5) Uiso 0.66 d SP . . 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 Pt1 0.02621(14) 0.02082(13) 0.02284(13) -0.00032(10) -0.00194(10) -0.00163(10) Pt2 0.02064(13) 0.02295(13) 0.02095(13) -0.00164(10) 0.00054(9) -0.00106(10) S1 0.0523(12) 0.0298(10) 0.0346(10) 0.0072(8) -0.0111(9) -0.0031(9) S2 0.0249(9) 0.0239(8) 0.0214(8) -0.0011(7) 0.0015(6) -0.0031(7) P1 0.0277(9) 0.0230(8) 0.0195(8) 0.0002(7) -0.0009(7) -0.0019(7) P2 0.0232(9) 0.0258(9) 0.0221(8) -0.0011(7) 0.0008(7) 0.0002(7) N1 0.032(4) 0.028(3) 0.034(4) -0.007(3) 0.002(3) -0.004(3) O11 0.038(3) 0.021(2) 0.031(3) -0.004(2) 0.001(2) -0.004(2) O12 0.049(3) 0.028(3) 0.044(3) -0.006(2) -0.005(3) -0.008(2) O21 0.030(3) 0.032(3) 0.030(3) -0.003(2) 0.010(2) -0.008(2) O22 0.032(3) 0.045(3) 0.030(3) -0.003(2) 0.017(2) -0.016(2) C11 0.057(5) 0.023(4) 0.038(4) 0.007(3) 0.006(4) 0.000(4) C12 0.085(8) 0.045(5) 0.046(5) 0.004(4) 0.017(5) -0.011(5) C13 0.097(9) 0.058(7) 0.079(8) 0.011(6) 0.039(8) -0.006(6) C14 0.061(7) 0.059(7) 0.105(10) 0.026(7) 0.038(7) -0.010(5) C15 0.055(6) 0.040(5) 0.063(6) 0.003(4) 0.008(5) -0.002(4) C16 0.041(5) 0.023(4) 0.050(5) 0.004(3) 0.004(4) -0.006(3) C17 0.034(4) 0.026(4) 0.035(4) 0.004(3) -0.009(3) 0.004(3) C21 0.023(3) 0.020(3) 0.026(3) 0.000(3) -0.004(3) -0.002(3) C22 0.031(4) 0.027(4) 0.041(4) 0.003(3) -0.005(3) -0.005(3) C23 0.043(5) 0.022(4) 0.062(6) 0.003(4) -0.004(4) 0.004(3) C24 0.038(5) 0.031(4) 0.076(7) -0.004(4) 0.001(4) 0.009(4) C25 0.029(4) 0.040(4) 0.052(5) 0.001(4) -0.001(4) -0.001(3) C26 0.027(4) 0.029(4) 0.026(4) 0.002(3) -0.001(3) 0.002(3) C27 0.026(4) 0.028(3) 0.021(3) -0.003(3) -0.004(3) -0.005(3) C31 0.031(4) 0.031(4) 0.023(3) 0.002(3) -0.003(3) -0.002(3) C32 0.038(4) 0.026(4) 0.033(4) -0.003(3) 0.001(3) -0.001(3) C33 0.039(4) 0.039(4) 0.032(4) -0.003(3) -0.007(3) -0.011(4) C34 0.027(4) 0.045(5) 0.043(5) 0.009(4) -0.010(3) -0.007(3) C35 0.025(4) 0.038(4) 0.045(5) 0.007(4) -0.004(3) 0.000(3) C36 0.035(4) 0.031(4) 0.029(4) 0.005(3) 0.004(3) -0.001(3) C41 0.031(4) 0.033(4) 0.023(3) -0.008(3) 0.005(3) -0.008(3) C42 0.031(4) 0.048(5) 0.030(4) -0.006(4) 0.006(3) -0.003(4) C43 0.024(4) 0.072(6) 0.047(5) -0.010(5) 0.000(4) -0.001(4) C44 0.043(5) 0.081(7) 0.031(4) -0.012(4) 0.015(4) -0.021(5) C45 0.062(6) 0.066(6) 0.025(4) 0.005(4) 0.005(4) -0.019(5) C46 0.040(5) 0.048(5) 0.030(4) 0.000(4) 0.000(3) -0.010(4) C51 0.023(3) 0.026(3) 0.021(3) 0.002(3) -0.004(3) -0.003(3) C52 0.033(4) 0.028(4) 0.030(4) 0.003(3) -0.008(3) 0.002(3) C53 0.047(5) 0.028(4) 0.055(5) -0.006(4) -0.016(4) -0.001(4) C54 0.041(5) 0.038(5) 0.059(6) 0.017(4) -0.014(4) -0.013(4) C55 0.031(4) 0.049(5) 0.045(5) 0.011(4) 0.001(4) -0.013(4) C56 0.026(4) 0.030(4) 0.036(4) 0.005(3) -0.003(3) 0.002(3) C61 0.027(4) 0.029(4) 0.026(4) -0.002(3) -0.002(3) -0.004(3) C62 0.047(5) 0.036(4) 0.026(4) 0.004(3) 0.002(3) -0.002(4) C63 0.059(6) 0.040(5) 0.034(4) 0.010(4) 0.006(4) -0.012(4) C64 0.074(7) 0.035(5) 0.039(5) 0.013(4) -0.003(4) -0.013(4) C65 0.053(5) 0.033(4) 0.050(5) 0.002(4) -0.008(4) 0.005(4) C66 0.038(4) 0.033(4) 0.032(4) 0.001(3) -0.001(3) 0.000(3) C71 0.030(4) 0.029(4) 0.024(3) -0.002(3) 0.004(3) -0.001(3) C72 0.032(4) 0.036(4) 0.032(4) -0.003(3) -0.001(3) 0.008(3) C73 0.043(5) 0.052(5) 0.034(4) -0.011(4) -0.004(4) 0.001(4) C74 0.067(6) 0.047(5) 0.042(5) -0.021(4) 0.011(4) 0.004(5) C75 0.046(5) 0.041(5) 0.054(5) -0.017(4) 0.007(4) 0.012(4) C76 0.033(4) 0.040(4) 0.036(4) -0.007(4) 0.005(3) -0.001(3) C81 0.023(3) 0.032(4) 0.024(3) -0.005(3) 0.000(3) 0.005(3) C82 0.022(4) 0.033(4) 0.035(4) 0.001(3) 0.003(3) -0.003(3) C83 0.034(4) 0.044(5) 0.046(5) -0.012(4) 0.003(4) -0.002(4) C84 0.032(4) 0.061(6) 0.037(4) -0.010(4) -0.004(3) 0.007(4) C85 0.027(4) 0.044(5) 0.040(4) 0.005(4) -0.004(3) 0.009(3) C86 0.029(4) 0.042(4) 0.037(4) -0.008(4) -0.001(3) -0.001(3) O91 0.072(4) 0.035(3) 0.062(4) 0.007(3) 0.016(3) 0.004(3) C91 0.070(7) 0.044(5) 0.076(7) 0.018(5) 0.002(6) 0.007(5) _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 Pt1 O11 2.068(5) . ? Pt1 P1 2.2124(17) . ? Pt1 S1 2.3068(19) . ? Pt1 S2 2.3595(17) . ? Pt2 N1 2.055(6) . ? Pt2 O21 2.061(4) . ? Pt2 P2 2.2096(17) . ? Pt2 S2 2.2799(17) . ? S1 C11 1.751(9) . ? S1 C12 2.708(10) . ? S1 C16 2.805(9) . ? S1 O11 2.952(5) . ? S1 P1 3.172(3) . ? S1 C36 3.201(8) . ? S1 C17 3.208(8) . ? S1 C31 3.414(7) . ? S1 S2 4.658(3) . ? S2 C21 1.785(7) . ? S2 C22 2.707(8) . ? S2 C26 2.830(7) . ? S2 O21 3.099(5) . ? S2 O11 3.113(5) . ? S2 P2 3.147(2) . ? S2 C81 3.232(7) . ? S2 C56 3.301(8) . ? S2 C27 3.319(7) . ? S2 P1 3.427(2) . ? P1 C31 1.811(7) . ? P1 C41 1.813(7) . ? P1 C51 1.834(7) . ? P2 C61 1.820(7) . ? P2 C71 1.828(7) . ? P2 C81 1.831(7) . ? O11 C17 1.270(9) . ? O12 C17 1.249(9) . ? O21 C27 1.299(8) . ? O22 C27 1.225(8) . ? C11 C12 1.405(12) . ? C11 C16 1.412(12) . ? C12 C13 1.368(16) . ? C13 C14 1.384(18) . ? C14 C15 1.370(14) . ? C15 C16 1.383(12) . ? C16 C17 1.509(11) . ? C21 C22 1.391(9) . ? C21 C26 1.412(9) . ? C22 C23 1.381(11) . ? C23 C24 1.381(12) . ? C24 C25 1.395(11) . ? C25 C26 1.385(10) . ? C26 C27 1.504(10) . ? C31 C32 1.395(10) . ? C31 C36 1.413(10) . ? C32 C33 1.381(11) . ? C33 C34 1.390(11) . ? C34 C35 1.373(11) . ? C35 C36 1.388(10) . ? C41 C42 1.377(11) . ? C41 C46 1.385(10) . ? C42 C43 1.391(10) . ? C43 C44 1.380(12) . ? C44 C45 1.379(13) . ? C45 C46 1.381(11) . ? C51 C52 1.382(10) . ? C51 C56 1.403(10) . ? C52 C53 1.399(11) . ? C53 C54 1.380(12) . ? C54 C55 1.384(12) . ? C55 C56 1.392(10) . ? C61 C66 1.382(10) . ? C61 C62 1.408(10) . ? C62 C63 1.365(11) . ? C63 C64 1.386(13) . ? C64 C65 1.386(12) . ? C65 C66 1.385(11) . ? C71 C72 1.388(10) . ? C71 C76 1.389(10) . ? C72 C73 1.387(11) . ? C73 C74 1.374(12) . ? C74 C75 1.376(13) . ? C75 C76 1.375(11) . ? C81 C86 1.390(11) . ? C81 C82 1.392(10) . ? C82 C83 1.391(11) . ? C83 C84 1.377(12) . ? C84 C85 1.365(12) . ? C85 C86 1.389(10) . ? O91 C91 1.399(11) . ? O92 O92 1.26(2) 2 ? O92 C92 1.28(2) . ? C92 O92 1.28(2) 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 O11 Pt1 P1 173.83(14) . . ? O11 Pt1 S1 84.69(15) . . ? P1 Pt1 S1 89.14(7) . . ? O11 Pt1 S2 89.11(14) . . ? P1 Pt1 S2 97.04(6) . . ? S1 Pt1 S2 173.04(7) . . ? N1 Pt2 O21 82.8(2) . . ? N1 Pt2 P2 97.1(2) . . ? O21 Pt2 P2 178.24(15) . . ? N1 Pt2 S2 173.4(2) . . ? O21 Pt2 S2 90.98(14) . . ? P2 Pt2 S2 88.98(6) . . ? C11 S1 Pt1 97.0(3) . . ? C11 S1 C12 27.3(4) . . ? Pt1 S1 C12 115.0(2) . . ? C11 S1 C16 24.5(3) . . ? Pt1 S1 C16 80.26(17) . . ? C12 S1 C16 51.8(3) . . ? C11 S1 O11 73.8(3) . . ? Pt1 S1 O11 44.23(9) . . ? C12 S1 O11 100.9(3) . . ? C16 S1 O11 49.68(19) . . ? C11 S1 P1 116.8(3) . . ? Pt1 S1 P1 44.21(5) . . ? C12 S1 P1 114.6(2) . . ? C16 S1 P1 113.77(17) . . ? O11 S1 P1 88.44(11) . . ? C11 S1 C36 166.6(3) . . ? Pt1 S1 C36 80.01(14) . . ? C12 S1 C36 143.8(3) . . ? C16 S1 C36 159.7(2) . . ? O11 S1 C36 111.26(17) . . ? P1 S1 C36 52.41(14) . . ? C11 S1 C17 52.5(3) . . ? Pt1 S1 C17 63.65(13) . . ? C12 S1 C17 79.8(3) . . ? C16 S1 C17 28.1(2) . . ? O11 S1 C17 23.33(16) . . ? P1 S1 C17 106.35(14) . . ? C36 S1 C17 134.2(2) . . ? C11 S1 C31 142.4(3) . . ? Pt1 S1 C31 70.29(12) . . ? C12 S1 C31 126.6(2) . . ? C16 S1 C31 145.4(2) . . ? O11 S1 C31 111.63(15) . . ? P1 S1 C31 31.65(12) . . ? C36 S1 C31 24.40(18) . . ? C17 S1 C31 133.64(18) . . ? C11 S1 S2 93.9(3) . . ? Pt1 S1 S2 3.52(3) . . ? C12 S1 S2 112.9(2) . . ? C16 S1 S2 76.83(17) . . ? O11 S1 S2 41.12(9) . . ? P1 S1 S2 47.36(4) . . ? C36 S1 S2 83.36(14) . . ? C17 S1 S2 60.20(13) . . ? C31 S1 S2 73.80(12) . . ? C21 S2 Pt2 100.7(2) . . ? C21 S2 Pt1 107.5(2) . . ? Pt2 S2 Pt1 104.77(7) . . ? C21 S2 C22 27.4(3) . . ? Pt2 S2 C22 119.90(17) . . ? Pt1 S2 C22 116.00(17) . . ? C21 S2 C26 24.4(2) . . ? Pt2 S2 C26 83.12(15) . . ? Pt1 S2 C26 96.06(15) . . ? C22 S2 C26 51.8(2) . . ? C21 S2 O21 71.6(2) . . ? Pt2 S2 O21 41.66(9) . . ? Pt1 S2 O21 85.61(11) . . ? C22 S2 O21 98.45(19) . . ? C26 S2 O21 48.20(17) . . ? C21 S2 O11 119.7(2) . . ? Pt2 S2 O11 63.64(10) . . ? Pt1 S2 O11 41.62(9) . . ? C22 S2 O11 143.84(19) . . ? C26 S2 O11 96.73(17) . . ? O21 S2 O11 58.96(14) . . ? C21 S2 P2 128.7(2) . . ? Pt2 S2 P2 44.60(4) . . ? Pt1 S2 P2 116.38(7) . . ? C22 S2 P2 127.61(17) . . ? C26 S2 P2 122.30(16) . . ? O21 S2 P2 86.25(10) . . ? O11 S2 P2 81.93(10) . . ? C21 S2 C81 158.5(3) . . ? Pt2 S2 C81 71.65(13) . . ? Pt1 S2 C81 93.99(13) . . ? C22 S2 C81 140.4(2) . . ? C26 S2 C81 154.5(2) . . ? O21 S2 C81 109.62(16) . . ? O11 S2 C81 75.73(16) . . ? P2 S2 C81 33.32(13) . . ? C21 S2 C56 94.8(3) . . ? Pt2 S2 C56 160.11(14) . . ? Pt1 S2 C56 82.07(13) . . ? C22 S2 C56 71.1(2) . . ? C26 S2 C56 115.1(2) . . ? O21 S2 C56 158.00(16) . . ? O11 S2 C56 118.56(16) . . ? P2 S2 C56 115.57(14) . . ? C81 S2 C56 89.43(18) . . ? C21 S2 C27 51.2(2) . . ? Pt2 S2 C27 63.35(12) . . ? Pt1 S2 C27 84.06(13) . . ? C22 S2 C27 78.6(2) . . ? C26 S2 C27 26.84(18) . . ? O21 S2 C27 23.03(14) . . ? O11 S2 C27 71.87(16) . . ? P2 S2 C27 107.56(13) . . ? C81 S2 C27 132.63(18) . . ? C56 S2 C27 136.49(18) . . ? C21 S2 P1 88.0(2) . . ? Pt2 S2 P1 143.81(7) . . ? Pt1 S2 P1 39.85(4) . . ? C22 S2 P1 82.58(17) . . ? C26 S2 P1 92.22(15) . . ? O21 S2 P1 112.30(10) . . ? O11 S2 P1 81.47(10) . . ? P2 S2 P1 143.14(7) . . ? C81 S2 P1 110.28(13) . . ? C56 S2 P1 48.39(13) . . ? C27 S2 P1 98.11(13) . . ? C31 P1 C41 106.0(3) . . ? C31 P1 C51 101.2(3) . . ? C41 P1 C51 106.2(3) . . ? C31 P1 Pt1 115.8(2) . . ? C41 P1 Pt1 107.9(2) . . ? C51 P1 Pt1 118.6(2) . . ? C31 P1 S1 81.5(2) . . ? C41 P1 S1 89.6(2) . . ? C51 P1 S1 162.3(2) . . ? Pt1 P1 S1 46.64(5) . . ? C31 P1 S2 139.6(2) . . ? C41 P1 S2 113.3(2) . . ? C51 P1 S2 76.8(2) . . ? Pt1 P1 S2 43.11(4) . . ? S1 P1 S2 89.71(6) . . ? C61 P2 C71 101.3(3) . . ? C61 P2 C81 106.2(3) . . ? C71 P2 C81 107.1(3) . . ? C61 P2 Pt2 114.3(2) . . ? C71 P2 Pt2 117.0(2) . . ? C81 P2 Pt2 110.0(2) . . ? C61 P2 S2 96.0(2) . . ? C71 P2 S2 160.6(2) . . ? C81 P2 S2 75.9(2) . . ? Pt2 P2 S2 46.42(4) . . ? C17 O11 Pt1 126.9(5) . . ? C17 O11 S1 89.7(4) . . ? Pt1 O11 S1 51.09(11) . . ? C17 O11 S2 137.4(4) . . ? Pt1 O11 S2 49.27(10) . . ? S1 O11 S2 100.31(14) . . ? C27 O21 Pt2 130.7(4) . . ? C27 O21 S2 88.0(4) . . ? Pt2 O21 S2 47.35(10) . . ? C12 C11 C16 117.7(8) . . ? C12 C11 S1 117.7(7) . . ? C16 C11 S1 124.6(6) . . ? C13 C12 C11 121.2(11) . . ? C13 C12 S1 156.1(9) . . ? C11 C12 S1 34.9(5) . . ? C12 C13 C14 120.3(10) . . ? C15 C14 C13 119.7(10) . . ? C14 C15 C16 121.1(11) . . ? C15 C16 C11 119.9(8) . . ? C15 C16 C17 118.1(8) . . ? C11 C16 C17 121.9(7) . . ? C15 C16 S1 150.8(7) . . ? C11 C16 S1 31.0(4) . . ? C17 C16 S1 91.0(4) . . ? O12 C17 O11 121.4(7) . . ? O12 C17 C16 117.6(7) . . ? O11 C17 C16 121.0(7) . . ? O12 C17 S1 151.8(5) . . ? O11 C17 S1 66.9(4) . . ? C16 C17 S1 60.9(4) . . ? C22 C21 C26 119.4(6) . . ? C22 C21 S2 116.4(5) . . ? C26 C21 S2 124.2(5) . . ? C23 C22 C21 121.8(7) . . ? C23 C22 S2 157.8(6) . . ? C21 C22 S2 36.2(3) . . ? C24 C23 C22 119.0(7) . . ? C23 C24 C25 119.9(7) . . ? C26 C25 C24 121.7(7) . . ? C25 C26 C21 118.1(7) . . ? C25 C26 C27 115.6(6) . . ? C21 C26 C27 126.3(6) . . ? C25 C26 S2 149.3(5) . . ? C21 C26 S2 31.4(3) . . ? C27 C26 S2 95.0(4) . . ? O22 C27 O21 120.9(6) . . ? O22 C27 C26 118.7(6) . . ? O21 C27 C26 120.3(6) . . ? O22 C27 S2 154.9(5) . . ? O21 C27 S2 68.9(4) . . ? C26 C27 S2 58.2(3) . . ? C32 C31 C36 118.6(7) . . ? C32 C31 P1 120.2(6) . . ? C36 C31 P1 121.1(5) . . ? C32 C31 S1 142.0(5) . . ? C36 C31 S1 69.3(4) . . ? P1 C31 S1 66.8(2) . . ? C33 C32 C31 120.8(7) . . ? C32 C33 C34 120.2(7) . . ? C35 C34 C33 119.8(7) . . ? C34 C35 C36 121.0(7) . . ? C35 C36 C31 119.5(7) . . ? C35 C36 S1 130.7(5) . . ? C31 C36 S1 86.3(4) . . ? C42 C41 C46 118.6(7) . . ? C42 C41 P1 119.7(5) . . ? C46 C41 P1 121.0(6) . . ? C41 C42 C43 120.9(7) . . ? C44 C43 C42 120.2(8) . . ? C45 C44 C43 118.8(8) . . ? C44 C45 C46 121.0(8) . . ? C45 C46 C41 120.4(8) . . ? C52 C51 C56 120.4(6) . . ? C52 C51 P1 123.3(5) . . ? C56 C51 P1 116.3(5) . . ? C51 C52 C53 119.0(7) . . ? C54 C53 C52 121.1(8) . . ? C53 C54 C55 119.5(8) . . ? C54 C55 C56 120.5(8) . . ? C55 C56 C51 119.4(7) . . ? C55 C56 S2 118.8(5) . . ? C51 C56 S2 86.1(4) . . ? C66 C61 C62 119.2(7) . . ? C66 C61 P2 121.0(5) . . ? C62 C61 P2 119.8(6) . . ? C63 C62 C61 120.4(8) . . ? C62 C63 C64 120.2(8) . . ? C63 C64 C65 119.8(8) . . ? C66 C65 C64 120.3(8) . . ? C61 C66 C65 120.0(7) . . ? C72 C71 C76 119.4(7) . . ? C72 C71 P2 117.3(5) . . ? C76 C71 P2 123.2(6) . . ? C73 C72 C71 120.0(7) . . ? C74 C73 C72 120.2(8) . . ? C73 C74 C75 119.8(8) . . ? C76 C75 C74 120.7(8) . . ? C75 C76 C71 119.9(8) . . ? C86 C81 C82 119.6(7) . . ? C86 C81 P2 117.3(5) . . ? C82 C81 P2 122.7(5) . . ? C86 C81 S2 95.3(4) . . ? C82 C81 S2 98.0(4) . . ? P2 C81 S2 70.8(2) . . ? C83 C82 C81 119.7(7) . . ? C84 C83 C82 119.8(8) . . ? C85 C84 C83 121.0(8) . . ? C84 C85 C86 119.9(8) . . ? C85 C86 C81 120.0(7) . . ? O92 O92 C92 60.5(7) 2 . ? O92 C92 O92 58.9(15) 2 . ? _diffrn_measured_fraction_theta_max 0.463 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.463 _refine_diff_density_max 2.205 _refine_diff_density_min -1.619 _refine_diff_density_rms 0.161 #===END