# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/3918 data_global _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'm.lutz@chem.uu.nl' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' loop_ _publ_author_name _publ_author_address 'Albrecht, Martin' ; Debye Institute Department of Metal-Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Schreurs, Antoine M.M.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lutz, Egbert T.H.' ; Department of Vibrational Spectroscopy Utrecht University Sorbonnelaan 16 3584 CA Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'van Koten, Gerard' ; Debye Institute Department of Metal-Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_section_title ; Self-assembled organoplatinum(II) supermolecules as crystalline, SO~2~ gas-triggered switches ; _journal_coden_Cambridge 186 data_s1786a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H19 Cl N2 Pt' _chemical_formula_sum 'C12 H19 Cl N2 Pt' _chemical_formula_weight 421.83 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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/c' 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 12.9877(14) _cell_length_b 9.2177(6) _cell_length_c 11.6041(12) _cell_angle_alpha 90.00 _cell_angle_beta 111.104(8) _cell_angle_gamma 90.00 _cell_volume 1296.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.66 _cell_measurement_theta_max 13.77 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 11.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 6214 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2963 _reflns_number_gt 2657 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'manually editing of SHELXL output' _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^)+(0.0140P)^2^+0.6530P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2963 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 Pt Pt 0.190536(13) 0.476893(14) -0.058474(12) 0.01429(6) Uani 1 1 d . . . Cl Cl 0.03813(10) 0.47530(10) -0.25294(9) 0.0237(2) Uani 1 1 d . . . N1 N 0.2738(3) 0.6522(3) -0.0975(3) 0.0163(7) Uani 1 1 d . . . N2 N 0.1418(3) 0.3051(3) 0.0278(3) 0.0167(7) Uani 1 1 d . . . C1 C 0.3088(4) 0.4877(4) 0.0973(4) 0.0179(9) Uani 1 1 d . . . C2 C 0.3992(4) 0.5751(4) 0.1107(3) 0.0192(8) Uani 1 1 d . . . C3 C 0.4838(4) 0.5865(4) 0.2254(4) 0.0219(8) Uani 1 1 d . . . H3 H 0.5461 0.6464 0.2362 0.026 Uiso 1 1 calc R . . C4 C 0.4751(5) 0.5080(4) 0.3244(4) 0.0246(10) Uani 1 1 d . . . H4 H 0.5328 0.5144 0.4029 0.030 Uiso 1 1 calc R . . C5 C 0.3847(4) 0.4210(4) 0.3115(3) 0.0223(9) Uani 1 1 d . . . H5 H 0.3811 0.3684 0.3803 0.027 Uiso 1 1 calc R . . C6 C 0.2995(4) 0.4108(4) 0.1975(3) 0.0175(8) Uani 1 1 d . . . C8 C 0.2238(5) 0.7879(4) -0.0742(4) 0.0261(10) Uani 1 1 d . . . H8A H 0.2627 0.8713 -0.0917 0.039 Uiso 1 1 calc R . . H8B H 0.2298 0.7909 0.0124 0.039 Uiso 1 1 calc R . . H8C H 0.1459 0.7914 -0.1280 0.039 Uiso 1 1 calc R . . C9 C 0.2733(4) 0.6588(5) -0.2253(4) 0.0275(10) Uani 1 1 d . . . H9A H 0.1971 0.6653 -0.2837 0.041 Uiso 1 1 calc R . . H9B H 0.3079 0.5710 -0.2425 0.041 Uiso 1 1 calc R . . H9C H 0.3147 0.7443 -0.2342 0.041 Uiso 1 1 calc R . . C10 C 0.1892(4) 0.3353(4) 0.1654(3) 0.0210(9) Uani 1 1 d . . . H10A H 0.1378 0.3975 0.1889 0.025 Uiso 1 1 calc R . . H10B H 0.1988 0.2430 0.2118 0.025 Uiso 1 1 calc R . . C11 C 0.1921(4) 0.1696(4) 0.0026(4) 0.0239(9) Uani 1 1 d . . . H11A H 0.1796 0.0903 0.0523 0.036 Uiso 1 1 calc R . . H11B H 0.2716 0.1839 0.0242 0.036 Uiso 1 1 calc R . . H11C H 0.1582 0.1451 -0.0852 0.036 Uiso 1 1 calc R . . C12 C 0.0225(4) 0.2828(4) -0.0102(4) 0.0230(9) Uani 1 1 d . . . H12A H -0.0077 0.2559 -0.0977 0.034 Uiso 1 1 calc R . . H12B H -0.0125 0.3726 0.0024 0.034 Uiso 1 1 calc R . . H12C H 0.0079 0.2050 0.0394 0.034 Uiso 1 1 calc R . . C7 C 0.3934(4) 0.6465(4) -0.0088(4) 0.0219(8) Uani 1 1 d . . . H7A H 0.4382 0.5907 -0.0466 0.026 Uiso 1 1 calc R . . H7B H 0.4238 0.7460 0.0080 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01154(10) 0.01679(8) 0.01322(8) 0.00019(5) 0.00285(6) 0.00040(5) Cl 0.0189(6) 0.0269(4) 0.0192(4) -0.0002(3) -0.0007(4) 0.0000(4) N1 0.011(2) 0.0215(15) 0.0169(15) 0.0030(11) 0.0058(14) 0.0014(13) N2 0.017(2) 0.0163(14) 0.0178(15) -0.0028(11) 0.0069(15) -0.0014(12) C1 0.019(3) 0.0190(17) 0.0156(17) 0.0016(13) 0.0056(17) 0.0027(14) C2 0.016(2) 0.0209(16) 0.0210(17) -0.0033(15) 0.0067(17) 0.0037(16) C3 0.014(2) 0.0252(19) 0.0259(19) -0.0027(15) 0.0064(18) -0.0008(16) C4 0.021(3) 0.028(2) 0.0190(19) -0.0013(15) -0.0002(19) 0.0044(17) C5 0.024(3) 0.0247(18) 0.0171(17) -0.0003(15) 0.0062(18) 0.0042(17) C6 0.019(2) 0.0174(17) 0.0149(16) 0.0004(13) 0.0045(17) 0.0024(15) C8 0.026(3) 0.0190(18) 0.036(2) 0.0062(16) 0.014(2) 0.0030(17) C9 0.024(3) 0.041(2) 0.0187(19) 0.0049(16) 0.009(2) -0.0005(19) C10 0.021(3) 0.0278(19) 0.0141(17) -0.0025(14) 0.0059(17) -0.0023(17) C11 0.026(3) 0.0186(17) 0.029(2) -0.0022(15) 0.011(2) 0.0023(16) C12 0.013(2) 0.027(2) 0.030(2) 0.0022(15) 0.0074(19) -0.0016(16) C7 0.011(2) 0.0276(19) 0.0233(19) 0.0040(15) 0.0009(17) 0.0012(16) _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 Pt C1 1.907(4) . ? Pt N1 2.083(3) . ? Pt N2 2.089(3) . ? Pt Cl 2.4071(11) . ? N1 C8 1.478(5) . ? N1 C9 1.482(5) . ? N1 C7 1.524(5) . ? N2 C12 1.465(6) . ? N2 C11 1.487(5) . ? N2 C10 1.516(5) . ? C1 C2 1.386(6) . ? C1 C6 1.404(5) . ? C2 C3 1.391(6) . ? C2 C7 1.512(5) . ? C3 C4 1.397(6) . ? C3 H3 0.9500 . ? C4 C5 1.384(7) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C10 1.513(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt N1 82.02(15) . . ? C1 Pt N2 82.23(15) . . ? N1 Pt N2 164.25(14) . . ? C1 Pt Cl 177.05(11) . . ? N1 Pt Cl 96.73(9) . . ? N2 Pt Cl 98.98(10) . . ? C8 N1 C9 107.7(3) . . ? C8 N1 C7 108.3(3) . . ? C9 N1 C7 108.3(3) . . ? C8 N1 Pt 108.7(3) . . ? C9 N1 Pt 115.7(3) . . ? C7 N1 Pt 108.0(2) . . ? C12 N2 C11 108.3(3) . . ? C12 N2 C10 109.1(3) . . ? C11 N2 C10 108.7(3) . . ? C12 N2 Pt 115.6(3) . . ? C11 N2 Pt 108.2(2) . . ? C10 N2 Pt 106.7(2) . . ? C2 C1 C6 121.5(4) . . ? C2 C1 Pt 119.9(3) . . ? C6 C1 Pt 118.6(3) . . ? C1 C2 C3 119.8(4) . . ? C1 C2 C7 112.9(4) . . ? C3 C2 C7 127.3(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 121.8(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 118.5(4) . . ? C5 C6 C10 128.7(3) . . ? C1 C6 C10 112.6(4) . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 109.5(3) . . ? C6 C10 H10A 109.8 . . ? N2 C10 H10A 109.8 . . ? C6 C10 H10B 109.8 . . ? N2 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 C7 N1 109.7(4) . . ? C2 C7 H7A 109.7 . . ? N1 C7 H7A 109.7 . . ? C2 C7 H7B 109.7 . . ? N1 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt N1 C8 -95.1(3) . . . . ? N2 Pt N1 C8 -93.7(5) . . . . ? Cl Pt N1 C8 82.2(3) . . . . ? C1 Pt N1 C9 143.6(3) . . . . ? N2 Pt N1 C9 145.0(4) . . . . ? Cl Pt N1 C9 -39.1(3) . . . . ? C1 Pt N1 C7 22.1(3) . . . . ? N2 Pt N1 C7 23.5(6) . . . . ? Cl Pt N1 C7 -160.6(2) . . . . ? C1 Pt N2 C12 147.6(3) . . . . ? N1 Pt N2 C12 146.2(4) . . . . ? Cl Pt N2 C12 -29.6(3) . . . . ? C1 Pt N2 C11 -90.7(3) . . . . ? N1 Pt N2 C11 -92.1(5) . . . . ? Cl Pt N2 C11 92.0(3) . . . . ? C1 Pt N2 C10 26.1(3) . . . . ? N1 Pt N2 C10 24.7(6) . . . . ? Cl Pt N2 C10 -151.1(2) . . . . ? N1 Pt C1 C2 -11.1(3) . . . . ? N2 Pt C1 C2 169.3(3) . . . . ? Cl Pt C1 C2 -76(3) . . . . ? N1 Pt C1 C6 166.2(3) . . . . ? N2 Pt C1 C6 -13.5(3) . . . . ? Cl Pt C1 C6 101(2) . . . . ? C6 C1 C2 C3 0.7(6) . . . . ? Pt C1 C2 C3 177.9(3) . . . . ? C6 C1 C2 C7 179.3(3) . . . . ? Pt C1 C2 C7 -3.5(5) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C7 C2 C3 C4 -178.0(4) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C4 C5 C6 C1 1.3(6) . . . . ? C4 C5 C6 C10 -173.4(4) . . . . ? C2 C1 C6 C5 -1.6(6) . . . . ? Pt C1 C6 C5 -178.8(3) . . . . ? C2 C1 C6 C10 173.9(3) . . . . ? Pt C1 C6 C10 -3.3(4) . . . . ? C5 C6 C10 N2 -159.4(4) . . . . ? C1 C6 C10 N2 25.7(4) . . . . ? C12 N2 C10 C6 -159.5(3) . . . . ? C11 N2 C10 C6 82.6(4) . . . . ? Pt N2 C10 C6 -33.9(4) . . . . ? C1 C2 C7 N1 22.2(4) . . . . ? C3 C2 C7 N1 -159.3(4) . . . . ? C8 N1 C7 C2 88.4(4) . . . . ? C9 N1 C7 C2 -155.1(3) . . . . ? Pt N1 C7 C2 -29.1(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.663 _refine_diff_density_min -2.368 _refine_diff_density_rms 0.200 #===END data_s2023b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H19 Cl N2 O2 Pt S' _chemical_formula_sum 'C12 H19 Cl N2 O2 Pt S' _chemical_formula_weight 485.89 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.7796(1) _cell_length_b 10.0141(1) _cell_length_c 9.0940(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1528.09(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 9.493 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.66 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 24501 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3499 _reflns_number_gt 3428 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'manually editing of SHELXL output' _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^)+(0.0299P)^2^+1.0924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00164(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(6) _refine_ls_number_reflns 3499 _refine_ls_number_parameters 173 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.003 _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 Pt Pt 0.881381(6) 0.816080(11) 0.99178(4) 0.01214(6) Uani 1 1 d . . . Cl Cl 0.90343(7) 1.04649(9) 1.05632(11) 0.0237(2) Uani 1 1 d . . . S S 0.97499(7) 0.80390(10) 0.76849(12) 0.0196(2) Uani 1 1 d . . . O1 O 1.03866(19) 0.7172(4) 0.8189(3) 0.0296(7) Uani 1 1 d . . . O2 O 0.9276(2) 0.7462(5) 0.6516(3) 0.0323(8) Uani 1 1 d . . . N1 N 0.95885(19) 0.7281(3) 1.1444(3) 0.0163(6) Uani 1 1 d . . . N2 N 0.77990(19) 0.8542(3) 0.8645(4) 0.0167(6) Uani 1 1 d . . . C1 C 0.8532(2) 0.6316(4) 0.9565(4) 0.0156(8) Uani 1 1 d . . . C2 C 0.8977(3) 0.5326(4) 1.0240(4) 0.0158(8) Uani 1 1 d . . . C3 C 0.8740(2) 0.3989(4) 1.0014(8) 0.0223(8) Uani 1 1 d . . . H3 H 0.9038 0.3277 1.0431 0.027 Uiso 1 1 calc R . . C4 C 0.8069(2) 0.3723(4) 0.9180(4) 0.0211(8) Uani 1 1 d . . . H4 H 0.7900 0.2823 0.9067 0.025 Uiso 1 1 calc R . . C5 C 0.7634(3) 0.4730(4) 0.8501(4) 0.0209(8) Uani 1 1 d . . . H5 H 0.7179 0.4516 0.7924 0.025 Uiso 1 1 calc R . . C6 C 0.7870(2) 0.6058(4) 0.8674(4) 0.0167(7) Uani 1 1 d . . . C7 C 0.9707(2) 0.5822(4) 1.1031(4) 0.0200(8) Uani 1 1 d . . . H7A H 1.0180 0.5730 1.0387 0.024 Uiso 1 1 calc R . . H7B H 0.9798 0.5283 1.1928 0.024 Uiso 1 1 calc R . . C8 C 0.9174(3) 0.7329(5) 1.2890(4) 0.0270(10) Uani 1 1 d . . . H8A H 0.8652 0.6898 1.2804 0.040 Uiso 1 1 calc R . . H8B H 0.9103 0.8262 1.3189 0.040 Uiso 1 1 calc R . . H8C H 0.9495 0.6860 1.3628 0.040 Uiso 1 1 calc R . . C9 C 1.0382(3) 0.7938(4) 1.1622(5) 0.0243(9) Uani 1 1 d . . . H9A H 1.0667 0.7921 1.0681 0.036 Uiso 1 1 calc R . . H9B H 1.0693 0.7459 1.2365 0.036 Uiso 1 1 calc R . . H9C H 1.0306 0.8866 1.1934 0.036 Uiso 1 1 calc R . . C10 C 0.7550(2) 0.7256(4) 0.7849(5) 0.0196(8) Uani 1 1 d . . . H10A H 0.6961 0.7205 0.7796 0.023 Uiso 1 1 calc R . . H10B H 0.7762 0.7260 0.6833 0.023 Uiso 1 1 calc R . . C11 C 0.7159(2) 0.8915(4) 0.9689(5) 0.0272(10) Uani 1 1 d . . . H11A H 0.7097 0.8209 1.0426 0.041 Uiso 1 1 calc R . . H11B H 0.6657 0.9030 0.9152 0.041 Uiso 1 1 calc R . . H11C H 0.7300 0.9754 1.0179 0.041 Uiso 1 1 calc R . . C12 C 0.7880(3) 0.9635(4) 0.7538(5) 0.0242(8) Uani 1 1 d . . . H12A H 0.8305 0.9409 0.6841 0.036 Uiso 1 1 calc R . . H12B H 0.8014 1.0472 0.8040 0.036 Uiso 1 1 calc R . . H12C H 0.7376 0.9742 0.7007 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01158(9) 0.01184(8) 0.01299(9) -0.00036(9) -0.00148(8) -0.00036(3) Cl 0.0262(5) 0.0156(4) 0.0292(5) -0.0044(4) -0.0093(4) -0.0012(4) S 0.0195(5) 0.0221(5) 0.0172(5) 0.0020(3) 0.0043(4) 0.0009(3) O1 0.0246(18) 0.0391(19) 0.0250(15) 0.0073(14) 0.0084(13) 0.0081(15) O2 0.0294(18) 0.050(2) 0.0171(14) -0.0036(17) 0.0029(13) -0.0047(16) N1 0.0188(16) 0.0170(16) 0.0132(14) 0.0001(13) -0.0031(12) 0.0006(13) N2 0.0147(16) 0.0150(14) 0.0204(16) -0.0023(14) -0.0038(12) 0.0017(13) C1 0.0158(18) 0.0121(17) 0.019(2) 0.0020(12) 0.0014(12) -0.0035(14) C2 0.0181(17) 0.0153(18) 0.014(2) 0.0002(12) 0.0070(13) -0.0016(15) C3 0.0316(19) 0.0121(16) 0.023(2) 0.004(2) 0.0046(19) 0.0017(12) C4 0.030(2) 0.0125(17) 0.0207(19) -0.0048(14) 0.0033(16) -0.0020(15) C5 0.024(2) 0.0209(19) 0.0182(17) -0.0040(15) 0.0028(15) -0.0086(16) C6 0.0221(18) 0.0154(17) 0.0127(17) -0.0021(13) -0.0025(14) -0.0044(14) C7 0.023(2) 0.0156(17) 0.0214(19) 0.0022(14) -0.0009(15) 0.0033(15) C8 0.035(3) 0.031(2) 0.0152(19) 0.0019(18) -0.0027(17) 0.006(2) C9 0.019(2) 0.025(2) 0.029(2) -0.0010(17) -0.0102(17) -0.0013(17) C10 0.018(2) 0.0177(19) 0.023(2) -0.0003(16) -0.0095(15) -0.0030(16) C11 0.0154(17) 0.036(2) 0.030(3) -0.0096(18) -0.0031(16) 0.0024(15) C12 0.028(2) 0.0170(18) 0.028(2) 0.0026(15) -0.0121(16) -0.0007(16) _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 Pt C1 1.934(4) . ? Pt N2 2.094(3) . ? Pt N1 2.096(3) . ? Pt Cl 2.4094(9) . ? Pt S 2.5701(11) . ? S O2 1.448(4) . ? S O1 1.451(3) . ? N1 C8 1.488(5) . ? N1 C9 1.494(5) . ? N1 C7 1.522(5) . ? N2 C11 1.481(5) . ? N2 C12 1.494(5) . ? N2 C10 1.536(5) . ? C1 C2 1.384(6) . ? C1 C6 1.399(5) . ? C2 C3 1.412(6) . ? C2 C7 1.505(6) . ? C3 C4 1.383(7) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C4 H4 0.9500 . ? C5 C6 1.397(5) . ? C5 H5 0.9500 . ? C6 C10 1.513(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt N2 83.32(14) . . ? C1 Pt N1 81.96(14) . . ? N2 Pt N1 161.28(13) . . ? C1 Pt Cl 173.13(11) . . ? N2 Pt Cl 94.87(10) . . ? N1 Pt Cl 98.38(10) . . ? C1 Pt S 88.46(10) . . ? N2 Pt S 93.96(10) . . ? N1 Pt S 97.14(9) . . ? Cl Pt S 98.29(4) . . ? O2 S O1 113.4(2) . . ? O2 S Pt 105.25(13) . . ? O1 S Pt 103.22(13) . . ? C8 N1 C9 107.9(3) . . ? C8 N1 C7 108.1(3) . . ? C9 N1 C7 109.5(3) . . ? C8 N1 Pt 106.4(3) . . ? C9 N1 Pt 116.1(3) . . ? C7 N1 Pt 108.7(2) . . ? C11 N2 C12 108.3(3) . . ? C11 N2 C10 108.4(3) . . ? C12 N2 C10 108.8(3) . . ? C11 N2 Pt 106.4(2) . . ? C12 N2 Pt 115.6(2) . . ? C10 N2 Pt 109.2(2) . . ? C2 C1 C6 123.5(4) . . ? C2 C1 Pt 118.6(3) . . ? C6 C1 Pt 117.8(3) . . ? C1 C2 C3 117.6(4) . . ? C1 C2 C7 114.5(3) . . ? C3 C2 C7 127.7(4) . . ? C4 C3 C2 119.4(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C1 117.8(4) . . ? C5 C6 C10 126.7(4) . . ? C1 C6 C10 115.0(3) . . ? C2 C7 N1 109.2(3) . . ? C2 C7 H7A 109.8 . . ? N1 C7 H7A 109.8 . . ? C2 C7 H7B 109.8 . . ? N1 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 109.5(3) . . ? C6 C10 H10A 109.8 . . ? N2 C10 H10A 109.8 . . ? C6 C10 H10B 109.8 . . ? N2 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt S O2 49.2(2) . . . . ? N2 Pt S O2 -34.0(2) . . . . ? N1 Pt S O2 130.9(2) . . . . ? Cl Pt S O2 -129.52(19) . . . . ? C1 Pt S O1 -70.0(2) . . . . ? N2 Pt S O1 -153.20(19) . . . . ? N1 Pt S O1 11.70(19) . . . . ? Cl Pt S O1 111.29(17) . . . . ? C1 Pt N1 C8 -96.2(3) . . . . ? N2 Pt N1 C8 -57.7(5) . . . . ? Cl Pt N1 C8 76.9(3) . . . . ? S Pt N1 C8 176.4(3) . . . . ? C1 Pt N1 C9 143.8(3) . . . . ? N2 Pt N1 C9 -177.7(4) . . . . ? Cl Pt N1 C9 -43.1(3) . . . . ? S Pt N1 C9 56.4(3) . . . . ? C1 Pt N1 C7 20.0(2) . . . . ? N2 Pt N1 C7 58.5(5) . . . . ? Cl Pt N1 C7 -167.0(2) . . . . ? S Pt N1 C7 -67.4(2) . . . . ? C1 Pt N2 C11 102.3(3) . . . . ? N1 Pt N2 C11 63.9(5) . . . . ? Cl Pt N2 C11 -71.1(2) . . . . ? S Pt N2 C11 -169.7(2) . . . . ? C1 Pt N2 C12 -137.6(3) . . . . ? N1 Pt N2 C12 -175.9(4) . . . . ? Cl Pt N2 C12 49.1(3) . . . . ? S Pt N2 C12 -49.6(3) . . . . ? C1 Pt N2 C10 -14.5(3) . . . . ? N1 Pt N2 C10 -52.9(5) . . . . ? Cl Pt N2 C10 172.1(2) . . . . ? S Pt N2 C10 73.4(2) . . . . ? N2 Pt C1 C2 -175.8(3) . . . . ? N1 Pt C1 C2 -7.5(3) . . . . ? Cl Pt C1 C2 -100.8(9) . . . . ? S Pt C1 C2 90.0(3) . . . . ? N2 Pt C1 C6 2.2(3) . . . . ? N1 Pt C1 C6 170.6(3) . . . . ? Cl Pt C1 C6 77.2(10) . . . . ? S Pt C1 C6 -92.0(3) . . . . ? C6 C1 C2 C3 -0.4(6) . . . . ? Pt C1 C2 C3 177.5(4) . . . . ? C6 C1 C2 C7 174.5(3) . . . . ? Pt C1 C2 C7 -7.6(4) . . . . ? C1 C2 C3 C4 -2.0(7) . . . . ? C7 C2 C3 C4 -176.2(4) . . . . ? C2 C3 C4 C5 2.6(7) . . . . ? C3 C4 C5 C6 -0.8(6) . . . . ? C4 C5 C6 C1 -1.6(6) . . . . ? C4 C5 C6 C10 170.3(4) . . . . ? C2 C1 C6 C5 2.2(6) . . . . ? Pt C1 C6 C5 -175.7(3) . . . . ? C2 C1 C6 C10 -170.6(4) . . . . ? Pt C1 C6 C10 11.5(4) . . . . ? C1 C2 C7 N1 24.1(4) . . . . ? C3 C2 C7 N1 -161.6(5) . . . . ? C8 N1 C7 C2 86.8(4) . . . . ? C9 N1 C7 C2 -155.9(3) . . . . ? Pt N1 C7 C2 -28.2(3) . . . . ? C5 C6 C10 N2 164.8(4) . . . . ? C1 C6 C10 N2 -23.1(5) . . . . ? C11 N2 C10 C6 -92.2(4) . . . . ? C12 N2 C10 C6 150.3(3) . . . . ? Pt N2 C10 C6 23.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.272 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.130 #===END data_s2056a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H19 I N2 O2 Pt S' _chemical_formula_sum 'C12 H19 I N2 O2 Pt S' _chemical_formula_weight 577.34 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' '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0291(9) _cell_length_b 15.1212(13) _cell_length_c 25.985(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3154.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.67 _cell_measurement_theta_max 13.95 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 10.984 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_reflns_number 7116 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3623 _reflns_number_gt 2416 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'manually editing of SHELXL output' _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^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3623 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Pt Pt 0.06727(4) 0.19106(2) 0.107636(12) 0.01547(8) Uani 1 1 d . . . I I 0.19509(8) 0.10451(4) 0.02455(2) 0.02719(15) Uani 1 1 d . . . S S 0.2471(4) 0.1387(2) 0.18065(10) 0.0344(6) Uani 1 1 d . . . O1 O 0.3689(10) 0.0866(6) 0.1564(3) 0.059(3) Uani 1 1 d . . . O2 O 0.1329(9) 0.0911(5) 0.2141(3) 0.041(2) Uani 1 1 d . . . N1 N 0.2050(9) 0.3082(5) 0.0972(3) 0.0232(16) Uani 1 1 d . . . N2 N -0.1396(9) 0.1090(5) 0.1198(3) 0.0196(16) Uani 1 1 d . . . C2 C 0.0149(10) 0.3481(6) 0.1673(3) 0.019(2) Uani 1 1 d . . . C6 C -0.1914(12) 0.2319(6) 0.1795(3) 0.021(2) Uani 1 1 d . . . C7 C 0.1838(12) 0.3643(6) 0.1447(3) 0.023(2) Uani 1 1 d . . . H7A H 0.2709 0.3493 0.1702 0.028 Uiso 1 1 calc R . . H7B H 0.1958 0.4276 0.1356 0.028 Uiso 1 1 calc R . . C5 C -0.2868(11) 0.2878(7) 0.2112(3) 0.023(2) Uani 1 1 d . . . H5 H -0.3884 0.2681 0.2260 0.027 Uiso 1 1 calc R . . C4 C -0.2264(11) 0.3739(6) 0.2202(3) 0.021(2) Uani 1 1 d . . . H4 H -0.2896 0.4128 0.2412 0.025 Uiso 1 1 calc R . . C3 C -0.0785(11) 0.4035(6) 0.1994(3) 0.0208(19) Uani 1 1 d . . . H3 H -0.0400 0.4615 0.2068 0.025 Uiso 1 1 calc R . . C8 C 0.1263(15) 0.3532(7) 0.0536(4) 0.041(3) Uani 1 1 d . . . H8A H 0.0061 0.3575 0.0596 0.061 Uiso 1 1 calc R . . H8B H 0.1469 0.3195 0.0220 0.061 Uiso 1 1 calc R . . H8C H 0.1733 0.4127 0.0501 0.061 Uiso 1 1 calc R . . C1 C -0.0499(10) 0.2639(6) 0.1576(3) 0.0137(17) Uani 1 1 d . . . C10 C -0.2203(11) 0.1348(6) 0.1698(3) 0.020(2) Uani 1 1 d . . . H10A H -0.1723 0.0997 0.1983 0.024 Uiso 1 1 calc R . . H10B H -0.3414 0.1227 0.1683 0.024 Uiso 1 1 calc R . . C12 C -0.1088(12) 0.0118(6) 0.1199(4) 0.028(2) Uani 1 1 d . . . H12A H -0.0342 -0.0034 0.1484 0.042 Uiso 1 1 calc R . . H12B H -0.0571 -0.0057 0.0873 0.042 Uiso 1 1 calc R . . H12C H -0.2147 -0.0196 0.1241 0.042 Uiso 1 1 calc R . . C11 C -0.2538(13) 0.1285(7) 0.0765(3) 0.032(3) Uani 1 1 d . . . H11A H -0.2774 0.1921 0.0756 0.049 Uiso 1 1 calc R . . H11B H -0.3580 0.0958 0.0811 0.049 Uiso 1 1 calc R . . H11C H -0.2014 0.1107 0.0440 0.049 Uiso 1 1 calc R . . C9 C 0.3891(12) 0.2996(7) 0.0874(4) 0.040(3) Uani 1 1 d . . . H9A H 0.4411 0.2673 0.1159 0.060 Uiso 1 1 calc R . . H9B H 0.4389 0.3586 0.0847 0.060 Uiso 1 1 calc R . . H9C H 0.4072 0.2673 0.0552 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01497(14) 0.01543(15) 0.01603(13) 0.00000(16) 0.00215(15) 0.00012(17) I 0.0311(3) 0.0258(3) 0.0246(3) -0.0071(3) 0.0088(3) -0.0004(3) S 0.0286(13) 0.0393(16) 0.0352(13) 0.0076(13) -0.0092(12) 0.0080(12) O1 0.047(5) 0.056(6) 0.074(6) -0.012(5) -0.009(5) 0.017(5) O2 0.034(4) 0.049(5) 0.041(4) 0.025(4) -0.011(3) -0.006(4) N1 0.022(4) 0.023(4) 0.025(4) 0.004(4) 0.007(3) -0.009(4) N2 0.021(4) 0.014(4) 0.024(4) -0.001(3) 0.005(3) 0.000(3) C2 0.008(4) 0.024(5) 0.024(4) -0.003(4) -0.008(3) 0.005(4) C6 0.022(5) 0.022(5) 0.018(4) 0.002(4) -0.002(4) 0.010(4) C7 0.021(5) 0.018(5) 0.031(5) -0.004(4) -0.003(4) -0.003(4) C5 0.009(4) 0.047(7) 0.013(4) 0.009(4) 0.007(3) 0.001(4) C4 0.020(5) 0.022(6) 0.021(4) 0.000(4) -0.003(4) 0.018(4) C3 0.011(4) 0.024(5) 0.027(4) 0.002(4) -0.004(4) 0.008(4) C8 0.063(8) 0.028(6) 0.031(5) 0.020(5) 0.008(5) 0.006(6) C1 0.007(4) 0.025(5) 0.009(3) 0.003(3) 0.002(3) 0.004(4) C10 0.011(5) 0.027(5) 0.023(4) 0.002(4) 0.004(4) -0.003(4) C12 0.032(6) 0.021(5) 0.032(5) 0.004(4) 0.008(4) 0.001(4) C11 0.025(5) 0.048(8) 0.024(5) 0.005(5) -0.007(4) -0.003(5) C9 0.029(6) 0.030(6) 0.061(7) -0.017(6) 0.022(5) -0.013(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 Pt C1 1.944(8) . ? Pt N2 2.098(7) . ? Pt N1 2.106(8) . ? Pt S 2.512(3) . ? Pt I 2.7252(7) . ? S O1 1.405(9) . ? S O2 1.453(7) . ? N1 C8 1.465(12) . ? N1 C9 1.506(12) . ? N1 C7 1.507(11) . ? N2 C11 1.482(11) . ? N2 C12 1.490(11) . ? N2 C10 1.505(10) . ? C2 C3 1.398(12) . ? C2 C1 1.400(12) . ? C2 C7 1.499(13) . ? C6 C1 1.360(12) . ? C6 C5 1.407(12) . ? C6 C10 1.507(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C5 C4 1.409(13) . ? C5 H5 0.9500 . ? C4 C3 1.380(13) . ? C4 H4 0.9500 . ? C3 H3 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt N2 81.5(3) . . ? C1 Pt N1 82.2(3) . . ? N2 Pt N1 158.9(3) . . ? C1 Pt S 87.3(2) . . ? N2 Pt S 98.9(2) . . ? N1 Pt S 93.5(2) . . ? C1 Pt I 169.3(2) . . ? N2 Pt I 97.65(19) . . ? N1 Pt I 95.99(19) . . ? S Pt I 103.33(7) . . ? O1 S O2 115.5(5) . . ? O1 S Pt 103.7(4) . . ? O2 S Pt 104.2(3) . . ? C8 N1 C9 109.4(8) . . ? C8 N1 C7 108.8(8) . . ? C9 N1 C7 107.4(7) . . ? C8 N1 Pt 105.3(6) . . ? C9 N1 Pt 117.7(7) . . ? C7 N1 Pt 108.0(5) . . ? C11 N2 C12 107.6(7) . . ? C11 N2 C10 109.8(7) . . ? C12 N2 C10 109.0(7) . . ? C11 N2 Pt 104.9(6) . . ? C12 N2 Pt 116.9(6) . . ? C10 N2 Pt 108.5(5) . . ? C3 C2 C1 117.0(8) . . ? C3 C2 C7 128.4(9) . . ? C1 C2 C7 114.5(8) . . ? C1 C6 C5 119.1(9) . . ? C1 C6 C10 113.9(8) . . ? C5 C6 C10 126.7(9) . . ? C2 C7 N1 109.3(7) . . ? C2 C7 H7A 109.8 . . ? N1 C7 H7A 109.8 . . ? C2 C7 H7B 109.8 . . ? N1 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C6 C5 C4 117.7(8) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C3 C4 C5 122.1(8) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C4 C3 C2 120.1(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C1 C2 124.0(8) . . ? C6 C1 Pt 118.8(7) . . ? C2 C1 Pt 117.2(6) . . ? N2 C10 C6 109.3(7) . . ? N2 C10 H10A 109.8 . . ? C6 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C6 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt S O1 -173.9(5) . . . . ? N2 Pt S O1 105.1(5) . . . . ? N1 Pt S O1 -92.0(5) . . . . ? I Pt S O1 5.0(4) . . . . ? C1 Pt S O2 64.8(4) . . . . ? N2 Pt S O2 -16.1(4) . . . . ? N1 Pt S O2 146.8(4) . . . . ? I Pt S O2 -116.2(4) . . . . ? C1 Pt N1 C8 -94.8(6) . . . . ? N2 Pt N1 C8 -55.5(10) . . . . ? S Pt N1 C8 178.4(6) . . . . ? I Pt N1 C8 74.6(6) . . . . ? C1 Pt N1 C9 143.0(7) . . . . ? N2 Pt N1 C9 -177.7(7) . . . . ? S Pt N1 C9 56.2(7) . . . . ? I Pt N1 C9 -47.6(7) . . . . ? C1 Pt N1 C7 21.3(6) . . . . ? N2 Pt N1 C7 60.6(10) . . . . ? S Pt N1 C7 -65.5(5) . . . . ? I Pt N1 C7 -169.3(5) . . . . ? C1 Pt N2 C11 98.0(6) . . . . ? N1 Pt N2 C11 58.6(10) . . . . ? S Pt N2 C11 -176.1(5) . . . . ? I Pt N2 C11 -71.3(6) . . . . ? C1 Pt N2 C12 -143.0(6) . . . . ? N1 Pt N2 C12 177.6(6) . . . . ? S Pt N2 C12 -57.1(6) . . . . ? I Pt N2 C12 47.7(6) . . . . ? C1 Pt N2 C10 -19.3(5) . . . . ? N1 Pt N2 C10 -58.6(10) . . . . ? S Pt N2 C10 66.6(5) . . . . ? I Pt N2 C10 171.4(5) . . . . ? C3 C2 C7 N1 -156.7(8) . . . . ? C1 C2 C7 N1 28.3(10) . . . . ? C8 N1 C7 C2 82.4(9) . . . . ? C9 N1 C7 C2 -159.3(8) . . . . ? Pt N1 C7 C2 -31.4(8) . . . . ? C1 C6 C5 C4 -2.3(12) . . . . ? C10 C6 C5 C4 172.0(8) . . . . ? C6 C5 C4 C3 -0.6(12) . . . . ? C5 C4 C3 C2 1.4(13) . . . . ? C1 C2 C3 C4 0.6(12) . . . . ? C7 C2 C3 C4 -174.3(8) . . . . ? C5 C6 C1 C2 4.6(12) . . . . ? C10 C6 C1 C2 -170.5(8) . . . . ? C5 C6 C1 Pt -173.0(6) . . . . ? C10 C6 C1 Pt 12.0(10) . . . . ? C3 C2 C1 C6 -3.7(12) . . . . ? C7 C2 C1 C6 171.9(8) . . . . ? C3 C2 C1 Pt 173.9(6) . . . . ? C7 C2 C1 Pt -10.5(9) . . . . ? N2 Pt C1 C6 4.5(6) . . . . ? N1 Pt C1 C6 171.2(7) . . . . ? S Pt C1 C6 -94.9(6) . . . . ? I Pt C1 C6 90.5(15) . . . . ? N2 Pt C1 C2 -173.2(6) . . . . ? N1 Pt C1 C2 -6.5(6) . . . . ? S Pt C1 C2 87.3(6) . . . . ? I Pt C1 C2 -87.2(15) . . . . ? C11 N2 C10 C6 -84.5(9) . . . . ? C12 N2 C10 C6 157.9(7) . . . . ? Pt N2 C10 C6 29.6(8) . . . . ? C1 C6 C10 N2 -27.8(10) . . . . ? C5 C6 C10 N2 157.6(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.504 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.244