# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name V.Kukushkin N.Bokach _publ_contact_author_name 'Kukushkin, Vadim' _publ_contact_author_email kukushkin@VK2100.spb.edu data_cis_1 _database_code_depnum_ccdc_archive 'CCDC 780216' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H12 Cl2 N2 O Pt S' _chemical_formula_sum 'C5 H12 Cl2 N2 O Pt S' _chemical_formula_weight 414.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c m' _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5581(8) _cell_length_b 18.0603(9) _cell_length_c 7.4262(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1147.81(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4602 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 12.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0962 _exptl_absorpt_correction_T_max 0.2449 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The Pt1 atom is located on a mirror plane together with N1, C1, N2, S1, Cl1, and Cl2. The Pt atom is coordinated by two Cl atoms, a S atom and a N atom in a slightly distorted square planar geometry. The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.98 \%A, and U~iso~ = 1.5 U~eq~(parent atom). The highest peak is located 0.85 \%A from atom Pt1 and the deepest hole is located 0.74 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19315 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1426 _reflns_number_gt 1209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'EvalCCD (Duisenberg, 2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 2003)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2d (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0274P)^2^+3.6314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1426 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Pt1 Pt 0.78043(3) 0.138259(13) 0.2500 0.01835(10) Uani 1 2 d S . . Cl1 Cl 0.8533(2) 0.01698(8) 0.2500 0.0241(4) Uani 1 2 d S . . Cl2 Cl 0.5211(2) 0.10367(11) 0.2500 0.0359(5) Uani 1 2 d S . . S1 S 1.0279(2) 0.17169(9) 0.2500 0.0195(3) Uani 1 2 d S . . O1 O 1.0595(6) 0.2513(2) 0.2500 0.0267(11) Uani 1 2 d S . . N1 N 0.7122(7) 0.2425(3) 0.2500 0.0278(14) Uani 1 2 d S . . N2 N 0.6330(7) 0.3716(3) 0.2500 0.0257(14) Uani 1 2 d S . . C1 C 0.6755(8) 0.3029(4) 0.2500 0.0221(15) Uani 1 2 d S . . C2 C 0.4694(9) 0.3926(4) 0.2500 0.0350(19) Uani 1 2 d S . . H2A H 0.4607 0.4467 0.2500 0.053 Uiso 1 2 calc SR . . H2B H 0.4184 0.3726 0.3577 0.053 Uiso 0.50 1 calc PR . . H2C H 0.4184 0.3726 0.1423 0.053 Uiso 0.50 1 calc PR . . C6 C 0.7474(9) 0.4307(4) 0.2500 0.034(2) Uani 1 2 d S . . H6A H 0.6936 0.4786 0.2500 0.051 Uiso 1 2 calc SR . . H6B H 0.8130 0.4268 0.1423 0.051 Uiso 0.50 1 calc PR . . H6C H 0.8130 0.4268 0.3577 0.051 Uiso 0.50 1 calc PR . . C7 C 1.1261(6) 0.1319(2) 0.0658(7) 0.0251(11) Uani 1 1 d . . . H7A H 1.0892 0.1547 -0.0461 0.038 Uiso 1 1 calc R . . H7B H 1.1051 0.0786 0.0626 0.038 Uiso 1 1 calc R . . H7C H 1.2388 0.1402 0.0784 0.038 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 Pt1 0.02378(16) 0.01184(13) 0.01942(14) 0.000 0.000 0.00289(10) Cl1 0.0310(10) 0.0109(7) 0.0304(9) 0.000 0.000 0.0012(6) Cl2 0.0265(11) 0.0328(10) 0.0485(11) 0.000 0.000 0.0002(8) S1 0.0264(10) 0.0117(7) 0.0203(8) 0.000 0.000 0.0008(6) O1 0.039(3) 0.010(2) 0.032(3) 0.000 0.000 -0.003(2) N1 0.029(3) 0.021(3) 0.034(3) 0.000 0.000 0.007(3) N2 0.024(4) 0.015(3) 0.038(4) 0.000 0.000 0.005(2) C1 0.021(4) 0.024(4) 0.022(3) 0.000 0.000 0.003(3) C2 0.027(5) 0.032(4) 0.046(5) 0.000 0.000 0.009(3) C6 0.037(6) 0.023(4) 0.042(5) 0.000 0.000 -0.006(3) C7 0.033(3) 0.020(2) 0.023(2) -0.0010(19) 0.005(2) 0.002(2) _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 N1 1.970(6) . yes Pt1 S1 2.2021(18) . yes Pt1 Cl1 2.2775(15) . yes Pt1 Cl2 2.306(2) . yes S1 O1 1.464(5) . ? S1 C7 1.759(5) 6_556 ? S1 C7 1.759(5) . ? N1 C1 1.137(9) . yes N2 C1 1.293(8) . yes N2 C6 1.448(9) . yes N2 C2 1.451(10) . yes C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 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 N1 Pt1 S1 91.32(19) . . yes N1 Pt1 Cl1 178.66(19) . . ? S1 Pt1 Cl1 90.02(6) . . ? N1 Pt1 Cl2 88.48(19) . . ? S1 Pt1 Cl2 179.81(6) . . ? Cl1 Pt1 Cl2 90.18(7) . . yes O1 S1 C7 108.2(2) . 6_556 ? O1 S1 C7 108.2(2) . . ? C7 S1 C7 102.1(3) 6_556 . ? O1 S1 Pt1 116.6(2) . . ? C7 S1 Pt1 110.35(18) 6_556 . ? C7 S1 Pt1 110.35(18) . . ? C1 N1 Pt1 178.8(6) . . yes C1 N2 C6 121.2(6) . . ? C1 N2 C2 121.4(6) . . ? C6 N2 C2 117.4(6) . . yes N1 C1 N2 179.7(8) . . yes N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.776 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.181 #===END======================================================================== data_cis_3 _database_code_depnum_ccdc_archive 'CCDC 780217' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Cl2 N2 O Pt S' _chemical_formula_sum 'C8 H16 Cl2 N2 O Pt S' _chemical_formula_weight 454.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9021(6) _cell_length_b 8.3489(5) _cell_length_c 9.9116(7) _cell_angle_alpha 85.659(5) _cell_angle_beta 87.383(7) _cell_angle_gamma 81.935(7) _cell_volume 645.17(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2644 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 11.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1737 _exptl_absorpt_correction_T_max 0.4017 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The Pt atom is coordinated by two Cl atoms, a S atom, and a N atom in a slightly distorted square planar geometry. The hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.98-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.80 \%A from atom Pt1 and the deepest hole is located 0.95 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10663 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2949 _reflns_number_gt 2742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0094P)^2^+0.3426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2949 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0360 _refine_ls_wR_factor_gt 0.0350 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Pt1 Pt 0.722353(13) 0.461641(12) 0.614850(10) 0.01518(4) Uani 1 1 d . . . Cl1 Cl 0.71414(10) 0.33546(9) 0.82710(7) 0.02194(15) Uani 1 1 d . . . Cl2 Cl 0.57989(10) 0.69975(9) 0.69549(8) 0.02424(16) Uani 1 1 d . . . S1 S 0.85184(9) 0.22890(8) 0.54403(7) 0.01621(14) Uani 1 1 d . . . O1 O 1.0103(2) 0.1549(2) 0.6091(2) 0.0222(5) Uani 1 1 d . . . N1 N 0.7276(3) 0.5749(3) 0.4324(3) 0.0224(6) Uani 1 1 d . . . N2 N 0.7254(3) 0.7151(3) 0.2063(2) 0.0209(5) Uani 1 1 d . . . C1 C 0.7240(4) 0.6410(3) 0.3263(3) 0.0187(6) Uani 1 1 d . . . C2 C 0.6622(4) 0.8895(3) 0.1882(3) 0.0216(6) Uani 1 1 d . . . H2A H 0.6660 0.9401 0.2750 0.026 Uiso 1 1 calc R . . H2B H 0.5419 0.9049 0.1603 0.026 Uiso 1 1 calc R . . C3 C 0.7716(4) 0.9699(4) 0.0814(3) 0.0276(7) Uani 1 1 d . . . H3A H 0.8875 0.9690 0.1155 0.033 Uiso 1 1 calc R . . H3B H 0.7210 1.0842 0.0621 0.033 Uiso 1 1 calc R . . C4 C 0.7842(4) 0.8809(4) -0.0489(3) 0.0259(7) Uani 1 1 d . . . H4A H 0.6691 0.8885 -0.0865 0.031 Uiso 1 1 calc R . . H4B H 0.8585 0.9332 -0.1168 0.031 Uiso 1 1 calc R . . C5 C 0.8570(4) 0.7036(4) -0.0217(3) 0.0254(7) Uani 1 1 d . . . H5A H 0.9746 0.6958 0.0111 0.031 Uiso 1 1 calc R . . H5B H 0.8628 0.6479 -0.1068 0.031 Uiso 1 1 calc R . . C6 C 0.7457(4) 0.6212(4) 0.0836(3) 0.0239(7) Uani 1 1 d . . . H6A H 0.6323 0.6166 0.0468 0.029 Uiso 1 1 calc R . . H6B H 0.7998 0.5089 0.1072 0.029 Uiso 1 1 calc R . . C7 C 0.8932(4) 0.2416(4) 0.3659(3) 0.0225(6) Uani 1 1 d . . . H7A H 0.9775 0.3159 0.3430 0.034 Uiso 1 1 calc R . . H7B H 0.7869 0.2822 0.3199 0.034 Uiso 1 1 calc R . . H7C H 0.9380 0.1338 0.3366 0.034 Uiso 1 1 calc R . . C8 C 0.7035(4) 0.0869(3) 0.5616(3) 0.0198(6) Uani 1 1 d . . . H8A H 0.7549 -0.0146 0.5239 0.030 Uiso 1 1 calc R . . H8B H 0.6001 0.1310 0.5130 0.030 Uiso 1 1 calc R . . H8C H 0.6735 0.0659 0.6577 0.030 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 Pt1 0.01848(6) 0.01286(6) 0.01453(7) 0.00069(4) -0.00208(4) -0.00369(4) Cl1 0.0308(4) 0.0197(4) 0.0149(3) 0.0018(3) 0.0003(3) -0.0039(3) Cl2 0.0313(4) 0.0170(4) 0.0239(4) -0.0046(3) -0.0080(3) 0.0024(3) S1 0.0175(3) 0.0155(3) 0.0158(3) -0.0001(3) -0.0008(3) -0.0033(3) O1 0.0186(10) 0.0224(11) 0.0257(11) -0.0017(9) -0.0040(9) -0.0016(8) N1 0.0312(14) 0.0139(12) 0.0222(14) 0.0006(11) -0.0015(11) -0.0037(11) N2 0.0303(14) 0.0168(13) 0.0143(12) 0.0019(10) -0.0002(10) -0.0001(11) C1 0.0204(15) 0.0137(14) 0.0221(16) -0.0028(13) -0.0008(12) -0.0020(11) C2 0.0296(16) 0.0163(15) 0.0182(15) 0.0012(12) -0.0020(13) -0.0017(12) C3 0.0377(18) 0.0255(17) 0.0217(16) 0.0037(13) -0.0032(14) -0.0134(14) C4 0.0308(17) 0.0319(18) 0.0165(15) 0.0020(13) -0.0006(13) -0.0117(14) C5 0.0199(15) 0.0378(19) 0.0181(15) -0.0074(14) -0.0001(12) 0.0003(13) C6 0.0355(18) 0.0178(15) 0.0171(15) -0.0023(12) -0.0024(13) 0.0021(13) C7 0.0277(16) 0.0222(16) 0.0177(15) -0.0006(12) 0.0023(12) -0.0047(13) C8 0.0201(14) 0.0179(15) 0.0224(15) -0.0007(12) -0.0019(12) -0.0067(12) _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 N1 1.978(3) . yes Pt1 S1 2.2133(7) . yes Pt1 Cl1 2.2827(7) . yes Pt1 Cl2 2.3213(7) . yes S1 O1 1.471(2) . ? S1 C8 1.775(3) . ? S1 C7 1.779(3) . ? N1 C1 1.150(4) . yes N2 C1 1.298(4) . yes N2 C2 1.472(4) . ? N2 C6 1.486(4) . ? C2 C3 1.514(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.530(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 N1 Pt1 S1 93.57(7) . . yes N1 Pt1 Cl1 178.89(7) . . ? S1 Pt1 Cl1 87.53(3) . . ? N1 Pt1 Cl2 88.37(7) . . ? S1 Pt1 Cl2 177.63(3) . . ? Cl1 Pt1 Cl2 90.53(3) . . yes O1 S1 C8 108.33(13) . . ? O1 S1 C7 108.01(14) . . ? C8 S1 C7 101.54(15) . . ? O1 S1 Pt1 117.97(9) . . ? C8 S1 Pt1 108.00(10) . . ? C7 S1 Pt1 111.68(10) . . ? C1 N1 Pt1 177.4(3) . . ? C1 N2 C2 120.0(2) . . ? C1 N2 C6 120.5(2) . . ? C2 N2 C6 117.5(2) . . ? N1 C1 N2 178.1(3) . . yes N2 C2 C3 109.8(3) . . ? N2 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 110.5(3) . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 110.8(3) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.4(2) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N2 C6 C5 108.9(3) . . ? N2 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N2 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 C8 H8A 109.5 . . ? S1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.942 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.113 #===END======================================================================== data_4_[PtCl3(Me2SO)]2_(H2O)2 _database_code_depnum_ccdc_archive 'CCDC 780218' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N8 O2 Pt, 2(C2 H6 Cl3 O Pt S), 2(H2 O)' _chemical_formula_sum 'C16 H44 Cl6 N8 O6 Pt3 S2' _chemical_formula_weight 1306.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.49360(10) _cell_length_b 25.2769(4) _cell_length_c 11.1728(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.3670(10) _cell_angle_gamma 90.00 _cell_volume 1784.20(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6467 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 12.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1753 _exptl_absorpt_correction_T_max 0.4233 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The Pt1 atom is located on a center of symmetry (inversion centre) and is coordinated by four N atoms in a slightly distorted square planar geometry. Pt2 is coordinated by three Cl atoms and one S atom also in a slightly distorted square planar geometry. The H~2~O hydrogens were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A, N---H 0.88 \%A and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.94 \%A from atom Pt1 and the deepest hole is located 0.68 \%A from atom Pt2. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24291 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 29.29 _reflns_number_total 4844 _reflns_number_gt 4190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0105P)^2^+6.9810P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4844 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.01853(6) Uani 1 2 d S . . Pt2 Pt 0.17064(3) 0.162938(6) 0.458681(16) 0.01868(5) Uani 1 1 d . . . Cl1 Cl -0.0166(2) 0.10431(5) 0.55186(12) 0.0360(3) Uani 1 1 d . . . Cl2 Cl 0.1961(2) 0.09860(5) 0.31638(12) 0.0335(3) Uani 1 1 d . . . Cl3 Cl 0.1518(2) 0.22286(5) 0.60990(12) 0.0332(3) Uani 1 1 d . . . S1 S 0.33793(18) 0.21865(4) 0.36472(11) 0.0204(2) Uani 1 1 d . . . O1 O 0.4831(5) 0.04262(13) 0.1218(3) 0.0272(7) Uani 1 1 d . . . O2 O 0.3677(6) 0.27325(13) 0.4113(3) 0.0339(9) Uani 1 1 d . . . O3 O 0.1221(6) -0.12936(13) 0.1991(3) 0.0345(9) Uani 1 1 d . . . H3O H 0.1353 -0.1629 0.1835 0.052 Uiso 1 1 d R . . H3P H 0.0523 -0.1281 0.2590 0.052 Uiso 1 1 d R . . N1 N 0.2367(6) -0.02298(16) 0.1371(4) 0.0250(9) Uani 1 1 d . . . H1 H 0.2179 -0.0530 0.1729 0.030 Uiso 1 1 calc R . . N2 N 0.1770(6) 0.06282(15) -0.0239(3) 0.0227(8) Uani 1 1 d . . . H2 H 0.1156 0.0857 -0.0804 0.027 Uiso 1 1 calc R . . N3 N 0.5548(7) -0.01230(16) 0.2815(4) 0.0268(9) Uani 1 1 d . . . N4 N 0.4781(7) 0.11579(16) 0.0111(4) 0.0298(9) Uani 1 1 d . . . C1 C 0.4128(8) 0.00049(18) 0.1796(4) 0.0245(10) Uani 1 1 d . . . C2 C 0.4928(9) -0.0497(2) 0.3663(5) 0.0369(13) Uani 1 1 d . . . H2A H 0.3500 -0.0411 0.3753 0.055 Uiso 1 1 calc R . . H2B H 0.5926 -0.0474 0.4466 0.055 Uiso 1 1 calc R . . H2C H 0.4943 -0.0857 0.3338 0.055 Uiso 1 1 calc R . . C3 C 0.7575(9) 0.0156(2) 0.3179(5) 0.0372(13) Uani 1 1 d . . . H3A H 0.8210 0.0187 0.2467 0.056 Uiso 1 1 calc R . . H3B H 0.8531 -0.0043 0.3832 0.056 Uiso 1 1 calc R . . H3C H 0.7341 0.0510 0.3481 0.056 Uiso 1 1 calc R . . C4 C 0.3648(8) 0.07366(18) 0.0317(4) 0.0228(10) Uani 1 1 d . . . C5 C 0.3873(9) 0.1517(2) -0.0899(6) 0.0402(14) Uani 1 1 d . . . H5A H 0.3515 0.1319 -0.1673 0.060 Uiso 1 1 calc R . . H5B H 0.4906 0.1793 -0.0957 0.060 Uiso 1 1 calc R . . H5C H 0.2591 0.1681 -0.0745 0.060 Uiso 1 1 calc R . . C6 C 0.6967(8) 0.12492(19) 0.0801(5) 0.0291(11) Uani 1 1 d . . . H6A H 0.7076 0.1178 0.1675 0.044 Uiso 1 1 calc R . . H6B H 0.7360 0.1618 0.0695 0.044 Uiso 1 1 calc R . . H6C H 0.7923 0.1013 0.0492 0.044 Uiso 1 1 calc R . . C7 C 0.2118(8) 0.2210(2) 0.2070(4) 0.0330(12) Uani 1 1 d . . . H7A H 0.0700 0.2362 0.1970 0.049 Uiso 1 1 calc R . . H7B H 0.2004 0.1852 0.1728 0.049 Uiso 1 1 calc R . . H7C H 0.2951 0.2431 0.1634 0.049 Uiso 1 1 calc R . . C8 C 0.5898(8) 0.1930(2) 0.3631(5) 0.0277(11) Uani 1 1 d . . . H8A H 0.6551 0.2148 0.3095 0.041 Uiso 1 1 calc R . . H8B H 0.5750 0.1566 0.3323 0.041 Uiso 1 1 calc R . . H8C H 0.6793 0.1934 0.4468 0.041 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 Pt1 0.02069(13) 0.01490(11) 0.02091(12) -0.00098(9) 0.00666(10) -0.00202(9) Pt2 0.01850(9) 0.01883(9) 0.02015(9) -0.00025(6) 0.00740(7) -0.00021(7) Cl1 0.0423(8) 0.0324(7) 0.0392(7) 0.0015(5) 0.0215(6) -0.0107(6) Cl2 0.0441(8) 0.0270(6) 0.0332(7) -0.0107(5) 0.0165(6) -0.0074(5) Cl3 0.0379(7) 0.0322(6) 0.0353(7) -0.0120(5) 0.0207(6) -0.0029(5) S1 0.0193(6) 0.0200(5) 0.0238(6) 0.0028(4) 0.0085(5) 0.0019(4) O1 0.0245(18) 0.0234(17) 0.0347(19) 0.0087(14) 0.0088(15) -0.0031(14) O2 0.044(2) 0.0204(17) 0.043(2) -0.0018(16) 0.0224(18) -0.0019(16) O3 0.049(2) 0.0227(17) 0.033(2) 0.0020(15) 0.0126(18) -0.0043(16) N1 0.023(2) 0.022(2) 0.030(2) 0.0006(17) 0.0056(17) -0.0051(16) N2 0.025(2) 0.0193(18) 0.023(2) -0.0003(15) 0.0037(17) -0.0022(16) N3 0.027(2) 0.023(2) 0.029(2) 0.0012(17) 0.0027(18) -0.0053(17) N4 0.025(2) 0.023(2) 0.043(3) 0.0087(18) 0.0126(19) -0.0032(17) C1 0.027(3) 0.019(2) 0.029(3) -0.0001(19) 0.009(2) 0.0015(19) C2 0.038(3) 0.035(3) 0.034(3) 0.010(2) 0.001(2) -0.009(2) C3 0.034(3) 0.032(3) 0.040(3) 0.007(2) -0.004(2) -0.010(2) C4 0.026(3) 0.021(2) 0.024(2) 0.0000(18) 0.010(2) 0.0000(18) C5 0.029(3) 0.035(3) 0.057(4) 0.020(3) 0.011(3) -0.002(2) C6 0.026(3) 0.022(2) 0.039(3) -0.002(2) 0.008(2) -0.005(2) C7 0.025(3) 0.050(3) 0.023(3) 0.014(2) 0.002(2) -0.002(2) C8 0.020(2) 0.033(3) 0.032(3) 0.006(2) 0.011(2) 0.005(2) _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 N1 1.990(4) 3 ? Pt1 N1 1.990(4) . yes Pt1 N2 2.014(4) 3 ? Pt1 N2 2.014(4) . yes Pt2 S1 2.1892(11) . yes Pt2 Cl3 2.2932(12) . yes Pt2 Cl2 2.3067(12) . yes Pt2 Cl1 2.3117(12) . yes S1 O2 1.472(4) . ? S1 C8 1.763(5) . ? S1 C7 1.765(5) . ? O1 C4 1.364(6) . yes O1 C1 1.377(6) . yes O3 H3O 0.8728 . ? O3 H3P 0.8908 . ? N1 C1 1.278(6) . yes N1 H1 0.8800 . ? N2 C4 1.264(6) . yes N2 H2 0.8800 . ? N3 C1 1.329(6) . yes N3 C2 1.459(6) . ? N3 C3 1.466(7) . ? N4 C4 1.344(6) . yes N4 C5 1.462(7) . ? N4 C6 1.468(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 N1 Pt1 N1 180.0 3 . ? N1 Pt1 N2 88.24(16) 3 3 ? N1 Pt1 N2 91.76(16) . 3 ? N1 Pt1 N2 91.76(16) 3 . yes N1 Pt1 N2 88.24(16) . . ? N2 Pt1 N2 180.0 3 . ? S1 Pt2 Cl3 92.59(4) . . yes S1 Pt2 Cl2 90.02(4) . . ? Cl3 Pt2 Cl2 176.30(5) . . ? S1 Pt2 Cl1 177.90(5) . . ? Cl3 Pt2 Cl1 88.19(5) . . ? Cl2 Pt2 Cl1 89.28(5) . . yes O2 S1 C8 107.6(2) . . ? O2 S1 C7 108.3(3) . . ? C8 S1 C7 102.7(3) . . ? O2 S1 Pt2 118.23(15) . . ? C8 S1 Pt2 109.43(17) . . ? C7 S1 Pt2 109.50(18) . . ? C4 O1 C1 126.8(4) . . yes H3O O3 H3P 106.1 . . ? C1 N1 Pt1 128.0(3) . . ? C1 N1 H1 116.0 . . ? Pt1 N1 H1 116.0 . . ? C4 N2 Pt1 128.4(3) . . ? C4 N2 H2 115.8 . . ? Pt1 N2 H2 115.8 . . ? C1 N3 C2 118.2(4) . . ? C1 N3 C3 121.4(4) . . ? C2 N3 C3 119.8(4) . . ? C4 N4 C5 119.1(4) . . ? C4 N4 C6 122.4(4) . . ? C5 N4 C6 118.4(4) . . ? N1 C1 N3 126.1(4) . . ? N1 C1 O1 123.3(4) . . yes N3 C1 O1 110.5(4) . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N4 126.3(4) . . ? N2 C4 O1 123.5(4) . . yes N4 C4 O1 110.2(4) . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 C8 H8A 109.5 . . ? S1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O3 H3O O2 0.87 1.93 2.761(5) 159.0 2_545 yes O3 H3P Cl1 0.89 2.26 3.081(4) 153.1 3_556 yes N1 H1 O3 0.88 2.07 2.916(5) 161.3 . yes N2 H2 O3 0.88 2.10 2.945(5) 160.5 3 yes _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.918 _refine_diff_density_min -1.552 _refine_diff_density_rms 0.264 #===END======================================================================== data_4_[BPh4]2_(NH2CONMe2) _database_code_depnum_ccdc_archive 'CCDC 780219' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N8 O2 Pt, 2(C24 H20 B), 2(C3 H8 N2 O)' _chemical_formula_sum 'C66 H84 B2 N12 O4 Pt' _chemical_formula_weight 1326.16 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7414(10) _cell_length_b 13.1182(10) _cell_length_c 13.6130(10) _cell_angle_alpha 63.951(4) _cell_angle_beta 81.114(8) _cell_angle_gamma 88.180(7) _cell_volume 1542.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6902 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6775 _exptl_absorpt_correction_T_max 0.8923 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The Pt atom is located on a center of symmetry and is coordinated by four N atoms in a slightly distorted square planar geometry. The NH and NH~2~ hydrogen aotms were located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and also constrained to ride on their parent atoms, with C---H = 0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.81 \%A from atom C25 and the deepest hole is located 0.96 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31470 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7064 _reflns_number_gt 6888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0191P)^2^+0.7164P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7064 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0510 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.01204(5) Uani 1 2 d S . . O1 O 0.51622(16) 0.29478(13) 0.42145(12) 0.0178(3) Uani 1 1 d . . . O2 O -0.12843(17) 0.60638(14) 0.34755(13) 0.0245(4) Uani 1 1 d . . . N1 N 0.63501(19) 0.45460(16) 0.40229(14) 0.0152(4) Uani 1 1 d . . . H1N H 0.7157 0.4947 0.3670 0.023 Uiso 1 1 d R . . N2 N 0.37935(19) 0.36658(16) 0.53090(15) 0.0158(4) Uani 1 1 d . . . H2N H 0.2962 0.3624 0.5734 0.024 Uiso 1 1 d R . . N3 N 0.7086(2) 0.35465(17) 0.29938(15) 0.0195(4) Uani 1 1 d . . . N4 N 0.3283(2) 0.19477(17) 0.52878(16) 0.0200(4) Uani 1 1 d . . . N5 N 0.0796(2) 0.70195(18) 0.29339(16) 0.0227(5) Uani 1 1 d . . . N6 N -0.0815(2) 0.7491(2) 0.17459(16) 0.0282(5) Uani 1 1 d . . . H6N H -0.1674 0.7376 0.1543 0.042 Uiso 1 1 d R . . H6M H -0.0272 0.7929 0.1167 0.042 Uiso 1 1 d R . . C1 C 0.6218(2) 0.3747(2) 0.37397(17) 0.0153(5) Uani 1 1 d . . . C2 C 0.8269(3) 0.4337(2) 0.2385(2) 0.0261(6) Uani 1 1 d . . . H2A H 0.7938 0.5104 0.1998 0.039 Uiso 1 1 calc R . . H2B H 0.8798 0.4110 0.1846 0.039 Uiso 1 1 calc R . . H2C H 0.8870 0.4331 0.2903 0.039 Uiso 1 1 calc R . . C3 C 0.6890(3) 0.2585(2) 0.2754(2) 0.0255(6) Uani 1 1 d . . . H3A H 0.6700 0.1890 0.3449 0.038 Uiso 1 1 calc R . . H3B H 0.7735 0.2504 0.2304 0.038 Uiso 1 1 calc R . . H3C H 0.6105 0.2716 0.2347 0.038 Uiso 1 1 calc R . . C4 C 0.4031(2) 0.28988(19) 0.49671(17) 0.0149(5) Uani 1 1 d . . . C5 C 0.2163(3) 0.1621(2) 0.6223(2) 0.0315(6) Uani 1 1 d . . . H5A H 0.2454 0.1795 0.6792 0.047 Uiso 1 1 calc R . . H5B H 0.1945 0.0805 0.6531 0.047 Uiso 1 1 calc R . . H5C H 0.1337 0.2044 0.5975 0.047 Uiso 1 1 calc R . . C6 C 0.3440(3) 0.1280(2) 0.4658(2) 0.0259(6) Uani 1 1 d . . . H6A H 0.3634 0.1791 0.3865 0.039 Uiso 1 1 calc R . . H6B H 0.2579 0.0830 0.4817 0.039 Uiso 1 1 calc R . . H6C H 0.4211 0.0770 0.4870 0.039 Uiso 1 1 calc R . . C7 C 0.2437(2) 0.29671(19) 0.16916(17) 0.0154(5) Uani 1 1 d . . . C8 C 0.3706(2) 0.3581(2) 0.13361(19) 0.0196(5) Uani 1 1 d . . . H8 H 0.4383 0.3457 0.0822 0.024 Uiso 1 1 calc R . . C9 C 0.4019(3) 0.4367(2) 0.1705(2) 0.0239(5) Uani 1 1 d . . . H9 H 0.4886 0.4782 0.1424 0.029 Uiso 1 1 calc R . . C10 C 0.3084(3) 0.4548(2) 0.2473(2) 0.0247(6) Uani 1 1 d . . . H10 H 0.3292 0.5092 0.2719 0.030 Uiso 1 1 calc R . . C11 C 0.1833(3) 0.3926(2) 0.2880(2) 0.0237(5) Uani 1 1 d . . . H11 H 0.1186 0.4021 0.3429 0.028 Uiso 1 1 calc R . . C12 C 0.1529(2) 0.3165(2) 0.24856(19) 0.0190(5) Uani 1 1 d . . . H12 H 0.0659 0.2755 0.2769 0.023 Uiso 1 1 calc R . . C13 C 0.2096(2) 0.08034(19) 0.24299(18) 0.0154(5) Uani 1 1 d . . . C14 C 0.3368(2) 0.0296(2) 0.26411(19) 0.0187(5) Uani 1 1 d . . . H14 H 0.4172 0.0631 0.2105 0.022 Uiso 1 1 calc R . . C15 C 0.3511(3) -0.0670(2) 0.3595(2) 0.0240(6) Uani 1 1 d . . . H15 H 0.4396 -0.0990 0.3701 0.029 Uiso 1 1 calc R . . C16 C 0.2358(3) -0.1170(2) 0.43929(19) 0.0253(6) Uani 1 1 d . . . H16 H 0.2442 -0.1845 0.5043 0.030 Uiso 1 1 calc R . . C17 C 0.1097(3) -0.0684(2) 0.42370(19) 0.0230(5) Uani 1 1 d . . . H17 H 0.0307 -0.1009 0.4791 0.028 Uiso 1 1 calc R . . C18 C 0.0967(2) 0.0281(2) 0.32751(18) 0.0183(5) Uani 1 1 d . . . H18 H 0.0080 0.0601 0.3184 0.022 Uiso 1 1 calc R . . C19 C 0.2994(2) 0.2013(2) 0.02326(18) 0.0151(5) Uani 1 1 d . . . C20 C 0.3495(2) 0.3026(2) -0.06782(18) 0.0181(5) Uani 1 1 d . . . H20 H 0.3323 0.3720 -0.0629 0.022 Uiso 1 1 calc R . . C21 C 0.4233(2) 0.3065(2) -0.16524(19) 0.0211(5) Uani 1 1 d . . . H21 H 0.4556 0.3775 -0.2249 0.025 Uiso 1 1 calc R . . C22 C 0.4498(2) 0.2075(2) -0.17572(19) 0.0224(5) Uani 1 1 d . . . H22 H 0.5003 0.2097 -0.2422 0.027 Uiso 1 1 calc R . . C23 C 0.4016(2) 0.1055(2) -0.0881(2) 0.0234(5) Uani 1 1 d . . . H23 H 0.4188 0.0365 -0.0940 0.028 Uiso 1 1 calc R . . C24 C 0.3280(2) 0.1034(2) 0.00887(19) 0.0189(5) Uani 1 1 d . . . H24 H 0.2958 0.0320 0.0680 0.023 Uiso 1 1 calc R . . C25 C 0.0448(2) 0.2215(2) 0.09631(17) 0.0150(5) Uani 1 1 d . . . C26 C -0.0008(2) 0.3313(2) 0.03930(18) 0.0179(5) Uani 1 1 d . . . H26 H 0.0557 0.3939 0.0293 0.021 Uiso 1 1 calc R . . C27 C -0.1246(2) 0.3530(2) -0.00315(19) 0.0224(5) Uani 1 1 d . . . H27 H -0.1504 0.4291 -0.0423 0.027 Uiso 1 1 calc R . . C28 C -0.2103(2) 0.2647(2) 0.01123(19) 0.0248(6) Uani 1 1 d . . . H28 H -0.2962 0.2790 -0.0164 0.030 Uiso 1 1 calc R . . C29 C -0.1694(2) 0.1545(2) 0.06666(19) 0.0244(6) Uani 1 1 d . . . H29 H -0.2273 0.0926 0.0769 0.029 Uiso 1 1 calc R . . C30 C -0.0440(2) 0.1341(2) 0.10738(18) 0.0186(5) Uani 1 1 d . . . H30 H -0.0175 0.0578 0.1442 0.022 Uiso 1 1 calc R . . C31 C 0.1675(3) 0.8013(2) 0.2192(2) 0.0268(6) Uani 1 1 d . . . H31A H 0.2406 0.7805 0.1739 0.040 Uiso 1 1 calc R . . H31B H 0.2102 0.8310 0.2625 0.040 Uiso 1 1 calc R . . H31C H 0.1113 0.8596 0.1709 0.040 Uiso 1 1 calc R . . C32 C 0.1241(3) 0.6295(2) 0.3983(2) 0.0320(6) Uani 1 1 d . . . H32A H 0.0914 0.6589 0.4523 0.048 Uiso 1 1 calc R . . H32B H 0.2259 0.6283 0.3881 0.048 Uiso 1 1 calc R . . H32C H 0.0852 0.5522 0.4253 0.048 Uiso 1 1 calc R . . C33 C -0.0454(2) 0.6815(2) 0.2746(2) 0.0215(5) Uani 1 1 d . . . B1 B 0.1998(3) 0.1995(2) 0.1330(2) 0.0145(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01310(7) 0.01275(7) 0.01209(7) -0.00742(5) -0.00089(4) 0.00021(5) O1 0.0195(8) 0.0175(9) 0.0193(8) -0.0118(7) 0.0006(6) -0.0005(7) O2 0.0210(9) 0.0244(10) 0.0276(10) -0.0126(8) 0.0032(7) -0.0075(8) N1 0.0148(10) 0.0162(10) 0.0137(9) -0.0068(8) 0.0015(7) -0.0018(8) N2 0.0140(10) 0.0165(10) 0.0183(10) -0.0099(8) 0.0008(7) -0.0006(8) N3 0.0234(11) 0.0211(11) 0.0177(10) -0.0130(9) -0.0001(8) 0.0029(9) N4 0.0202(11) 0.0179(11) 0.0265(11) -0.0140(9) -0.0034(8) -0.0017(9) N5 0.0207(11) 0.0250(12) 0.0226(11) -0.0103(9) -0.0034(8) -0.0040(9) N6 0.0215(11) 0.0426(15) 0.0201(11) -0.0132(10) -0.0032(9) -0.0032(10) C1 0.0173(12) 0.0177(13) 0.0109(11) -0.0060(9) -0.0036(9) 0.0039(10) C2 0.0246(13) 0.0286(15) 0.0260(14) -0.0159(12) 0.0050(10) 0.0027(11) C3 0.0337(15) 0.0268(15) 0.0242(13) -0.0191(12) -0.0047(11) 0.0063(12) C4 0.0148(11) 0.0176(13) 0.0136(11) -0.0074(10) -0.0046(9) 0.0006(9) C5 0.0277(15) 0.0284(16) 0.0396(16) -0.0197(13) 0.0090(12) -0.0135(12) C6 0.0264(14) 0.0247(14) 0.0396(15) -0.0237(12) -0.0120(11) 0.0020(11) C7 0.0176(12) 0.0132(12) 0.0148(11) -0.0041(9) -0.0077(9) 0.0039(9) C8 0.0195(12) 0.0209(13) 0.0206(12) -0.0102(10) -0.0061(9) 0.0005(10) C9 0.0232(13) 0.0227(14) 0.0265(13) -0.0094(11) -0.0091(10) -0.0040(11) C10 0.0318(14) 0.0204(14) 0.0307(14) -0.0164(11) -0.0143(11) 0.0025(11) C11 0.0265(14) 0.0257(14) 0.0254(13) -0.0161(11) -0.0081(10) 0.0067(11) C12 0.0193(12) 0.0182(13) 0.0230(13) -0.0111(10) -0.0074(9) 0.0033(10) C13 0.0200(12) 0.0159(12) 0.0168(12) -0.0120(10) -0.0059(9) 0.0012(10) C14 0.0207(12) 0.0205(13) 0.0219(12) -0.0147(10) -0.0065(9) 0.0008(10) C15 0.0324(14) 0.0241(14) 0.0269(14) -0.0177(12) -0.0193(11) 0.0136(11) C16 0.0452(16) 0.0172(13) 0.0174(13) -0.0083(10) -0.0145(11) 0.0045(12) C17 0.0343(15) 0.0199(13) 0.0161(12) -0.0084(10) -0.0047(10) -0.0041(11) C18 0.0222(12) 0.0179(13) 0.0179(12) -0.0097(10) -0.0062(9) 0.0003(10) C19 0.0103(11) 0.0192(13) 0.0175(12) -0.0089(10) -0.0048(8) 0.0011(9) C20 0.0176(12) 0.0188(13) 0.0206(12) -0.0102(10) -0.0056(9) 0.0006(10) C21 0.0179(12) 0.0266(14) 0.0163(12) -0.0067(10) -0.0035(9) -0.0033(10) C22 0.0145(12) 0.0374(16) 0.0196(13) -0.0164(12) -0.0025(9) 0.0017(11) C23 0.0218(13) 0.0292(15) 0.0277(14) -0.0195(12) -0.0071(10) 0.0057(11) C24 0.0168(12) 0.0207(13) 0.0203(12) -0.0096(10) -0.0037(9) -0.0003(10) C25 0.0150(11) 0.0205(13) 0.0115(11) -0.0098(10) 0.0003(8) 0.0020(9) C26 0.0195(12) 0.0207(13) 0.0153(12) -0.0100(10) -0.0019(9) 0.0025(10) C27 0.0252(13) 0.0276(14) 0.0191(12) -0.0140(11) -0.0073(10) 0.0112(11) C28 0.0172(12) 0.0429(17) 0.0216(13) -0.0201(12) -0.0073(10) 0.0077(12) C29 0.0209(13) 0.0345(16) 0.0226(13) -0.0175(12) -0.0005(10) -0.0061(11) C30 0.0201(12) 0.0208(13) 0.0162(12) -0.0092(10) -0.0027(9) -0.0021(10) C31 0.0235(13) 0.0352(16) 0.0250(14) -0.0168(12) -0.0001(10) -0.0105(12) C32 0.0335(15) 0.0331(16) 0.0316(15) -0.0137(13) -0.0138(12) 0.0035(13) C33 0.0192(13) 0.0249(14) 0.0280(14) -0.0197(12) 0.0002(10) -0.0005(11) B1 0.0144(13) 0.0152(14) 0.0157(13) -0.0079(11) -0.0043(10) 0.0026(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 N2 1.9882(18) . yes Pt1 N2 1.9882(18) 2_666 ? Pt1 N1 1.9898(17) . yes Pt1 N1 1.9898(17) 2_666 ? O1 C1 1.358(3) . yes O1 C4 1.366(3) . yes O2 C33 1.246(3) . yes N1 C1 1.281(3) . yes N1 H1N 0.9018 . ? N2 C4 1.283(3) . yes N2 H2N 0.9076 . ? N3 C1 1.330(3) . ? N3 C2 1.456(3) . ? N3 C3 1.460(3) . ? N4 C4 1.327(3) . ? N4 C5 1.454(3) . ? N4 C6 1.462(3) . ? N5 C33 1.341(3) . ? N5 C31 1.449(3) . ? N5 C32 1.451(3) . ? N6 C33 1.354(3) . yes N6 H6N 0.9563 . ? N6 H6M 0.8505 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.396(3) . ? C7 C12 1.398(3) . ? C7 B1 1.643(3) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.375(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.397(3) . ? C13 C18 1.402(3) . ? C13 B1 1.635(3) . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.369(4) . ? C16 H16 0.9500 . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 C24 1.396(3) . ? C19 B1 1.642(3) . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.378(4) . ? C22 H22 0.9500 . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.399(3) . ? C25 C26 1.400(3) . ? C25 B1 1.641(3) . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 C28 1.374(4) . ? C27 H27 0.9500 . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C29 C30 1.389(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 N2 Pt1 N2 180.0 . 2_666 ? N2 Pt1 N1 88.18(7) . . yes N2 Pt1 N1 91.82(7) 2_666 . ? N2 Pt1 N1 91.82(7) . 2_666 ? N2 Pt1 N1 88.18(7) 2_666 2_666 ? N1 Pt1 N1 179.997(2) . 2_666 ? C1 O1 C4 127.88(17) . . yes C1 N1 Pt1 128.52(16) . . ? C1 N1 H1N 110.3 . . ? Pt1 N1 H1N 121.1 . . ? C4 N2 Pt1 128.53(15) . . ? C4 N2 H2N 117.7 . . ? Pt1 N2 H2N 113.7 . . ? C1 N3 C2 117.84(19) . . ? C1 N3 C3 123.0(2) . . ? C2 N3 C3 119.12(18) . . ? C4 N4 C5 119.2(2) . . ? C4 N4 C6 122.1(2) . . ? C5 N4 C6 118.3(2) . . ? C33 N5 C31 123.2(2) . . ? C33 N5 C32 119.3(2) . . ? C31 N5 C32 117.1(2) . . ? C33 N6 H6N 122.1 . . ? C33 N6 H6M 126.6 . . ? H6N N6 H6M 109.2 . . ? N1 C1 N3 126.5(2) . . ? N1 C1 O1 123.05(19) . . yes N3 C1 O1 110.41(19) . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N4 127.1(2) . . ? N2 C4 O1 123.1(2) . . yes N4 C4 O1 109.76(19) . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 114.9(2) . . ? C8 C7 B1 125.9(2) . . ? C12 C7 B1 119.12(19) . . ? C9 C8 C7 122.6(2) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 118.9(2) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 123.4(2) . . ? C11 C12 H12 118.3 . . ? C7 C12 H12 118.3 . . ? C14 C13 C18 115.1(2) . . ? C14 C13 B1 121.1(2) . . ? C18 C13 B1 123.5(2) . . ? C15 C14 C13 123.0(2) . . ? C15 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 119.4(2) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.3(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 122.5(2) . . ? C17 C18 H18 118.8 . . ? C13 C18 H18 118.8 . . ? C20 C19 C24 114.8(2) . . ? C20 C19 B1 122.1(2) . . ? C24 C19 B1 122.8(2) . . ? C21 C20 C19 123.0(2) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 118.8(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 123.0(2) . . ? C23 C24 H24 118.5 . . ? C19 C24 H24 118.5 . . ? C30 C25 C26 115.0(2) . . ? C30 C25 B1 123.0(2) . . ? C26 C25 B1 121.6(2) . . ? C27 C26 C25 123.0(2) . . ? C27 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 118.9(2) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 122.6(2) . . ? C29 C30 H30 118.7 . . ? C25 C30 H30 118.7 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 N5 121.8(2) . . ? O2 C33 N6 120.7(2) . . yes N5 C33 N6 117.5(2) . . ? C13 B1 C25 113.98(19) . . ? C13 B1 C19 111.56(18) . . ? C25 B1 C19 103.39(17) . . ? C13 B1 C7 103.50(17) . . ? C25 B1 C7 110.52(18) . . ? C19 B1 C7 114.23(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1N O2 0.90 2.05 2.879(2) 152.4 1_655 yes N2 H2N O2 0.91 1.95 2.837(2) 165.6 2_566 yes _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.508 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.105 #===END======================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 780220' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H23 Cl N4 O4 Pt S' _chemical_formula_sum 'C12 H23 Cl N4 O4 Pt S' _chemical_formula_weight 549.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7585(2) _cell_length_b 17.3396(5) _cell_length_c 8.3188(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.168(2) _cell_angle_gamma 90.00 _cell_volume 1748.60(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9555 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 8.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2584 _exptl_absorpt_correction_T_max 0.5135 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; The NH hydrogen atom was located from the difference Fourier map but constrained to ride on its parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.98-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.44 \%A from atom N5 and the deepest hole is located 0.73 \%A from atom Pt1. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43768 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.08 _reflns_number_total 5120 _reflns_number_gt 4407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.1f (Brandenburg, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0286P)^2^+2.1860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5120 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Pt1 Pt 0.156244(9) 0.178091(6) 0.470844(13) 0.01648(4) Uani 1 1 d . . . Cl1 Cl 0.14222(6) 0.04502(4) 0.45483(10) 0.02507(16) Uani 1 1 d . . . S2 S -0.01423(6) 0.18947(4) 0.46783(9) 0.01624(14) Uani 1 1 d . . . O1 O 0.3101(2) 0.16801(13) 0.4574(3) 0.0235(5) Uani 1 1 d . . . O2 O -0.05257(19) 0.26983(12) 0.4712(3) 0.0215(5) Uani 1 1 d . . . O3 O 0.2719(2) 0.57254(13) 0.5251(3) 0.0257(5) Uani 1 1 d . . . O4 O 0.6812(2) 0.16129(15) 0.4225(3) 0.0292(5) Uani 1 1 d . . . N1 N 0.1766(2) 0.29096(16) 0.4917(3) 0.0201(5) Uani 1 1 d . . . H1N H 0.1203 0.3207 0.4917 0.030 Uiso 1 1 d R . . N2 N 0.3523(2) 0.30067(16) 0.4494(3) 0.0208(5) Uani 1 1 d . . . N3 N 0.2641(2) 0.40924(15) 0.4960(3) 0.0212(5) Uani 1 1 d . . . N5 N 0.4678(2) 0.20518(16) 0.4187(4) 0.0228(5) Uani 1 1 d . . . C1 C 0.2623(3) 0.33019(17) 0.4774(4) 0.0187(6) Uani 1 1 d . . . C2 C 0.3701(3) 0.22563(18) 0.4404(4) 0.0194(6) Uani 1 1 d . . . C3 C 0.1711(3) 0.45230(19) 0.5196(5) 0.0262(7) Uani 1 1 d . . . H3A H 0.1346 0.4211 0.5864 0.031 Uiso 1 1 calc R . . H3B H 0.1163 0.4635 0.4082 0.031 Uiso 1 1 calc R . . C4 C 0.2133(3) 0.52687(19) 0.6111(4) 0.0263(7) Uani 1 1 d . . . H4A H 0.1501 0.5570 0.6227 0.032 Uiso 1 1 calc R . . H4B H 0.2625 0.5149 0.7262 0.032 Uiso 1 1 calc R . . C5 C 0.3633(3) 0.5307(2) 0.5073(4) 0.0261(7) Uani 1 1 d . . . H5A H 0.4152 0.5192 0.6208 0.031 Uiso 1 1 calc R . . H5B H 0.4026 0.5628 0.4460 0.031 Uiso 1 1 calc R . . C6 C 0.3275(3) 0.45600(19) 0.4120(4) 0.0253(7) Uani 1 1 d . . . H6A H 0.2815 0.4674 0.2945 0.030 Uiso 1 1 calc R . . H6B H 0.3932 0.4269 0.4074 0.030 Uiso 1 1 calc R . . C7 C 0.5427(3) 0.26177(19) 0.3833(5) 0.0258(7) Uani 1 1 d . . . H7A H 0.5292 0.3131 0.4249 0.031 Uiso 1 1 calc R . . H7B H 0.5291 0.2654 0.2597 0.031 Uiso 1 1 calc R . . C8 C 0.6604(3) 0.2379(2) 0.4694(4) 0.0268(7) Uani 1 1 d . . . H8A H 0.7106 0.2743 0.4385 0.032 Uiso 1 1 calc R . . H8B H 0.6760 0.2403 0.5936 0.032 Uiso 1 1 calc R . . C9 C 0.6102(3) 0.1076(2) 0.4683(5) 0.0296(7) Uani 1 1 d . . . H9A H 0.6242 0.1094 0.5922 0.035 Uiso 1 1 calc R . . H9B H 0.6266 0.0547 0.4381 0.035 Uiso 1 1 calc R . . C10 C 0.4904(3) 0.12600(19) 0.3789(4) 0.0260(7) Uani 1 1 d . . . H10A H 0.4743 0.1202 0.2552 0.031 Uiso 1 1 calc R . . H10B H 0.4426 0.0898 0.4163 0.031 Uiso 1 1 calc R . . C11 C -0.1035(3) 0.14246(19) 0.2888(4) 0.0222(6) Uani 1 1 d . . . H11A H -0.1794 0.1453 0.2926 0.033 Uiso 1 1 calc R . . H11B H -0.0816 0.0883 0.2888 0.033 Uiso 1 1 calc R . . H11C H -0.0990 0.1677 0.1858 0.033 Uiso 1 1 calc R . . C12 C -0.0411(3) 0.13809(18) 0.6337(4) 0.0213(6) Uani 1 1 d . . . H12A H -0.0037 0.1634 0.7417 0.032 Uiso 1 1 calc R . . H12B H -0.0137 0.0852 0.6360 0.032 Uiso 1 1 calc R . . H12C H -0.1207 0.1372 0.6156 0.032 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 Pt1 0.01398(7) 0.01554(6) 0.02029(7) -0.00107(4) 0.00588(5) -0.00118(4) Cl1 0.0233(4) 0.0160(3) 0.0386(4) -0.0019(3) 0.0134(3) -0.0012(3) S2 0.0149(4) 0.0175(3) 0.0167(3) 0.0000(2) 0.0055(3) -0.0015(3) O1 0.0149(11) 0.0216(11) 0.0373(13) 0.0008(9) 0.0129(10) 0.0020(9) O2 0.0231(12) 0.0176(10) 0.0266(11) 0.0007(8) 0.0120(9) 0.0002(9) O3 0.0275(13) 0.0170(11) 0.0334(12) -0.0005(9) 0.0106(10) -0.0022(9) O4 0.0189(12) 0.0289(13) 0.0420(14) -0.0013(11) 0.0128(11) 0.0007(10) N1 0.0162(13) 0.0175(13) 0.0287(13) -0.0039(10) 0.0098(11) -0.0026(10) N2 0.0166(13) 0.0198(12) 0.0268(13) -0.0016(10) 0.0077(11) -0.0016(10) N3 0.0160(13) 0.0183(12) 0.0311(14) -0.0018(10) 0.0101(11) -0.0019(10) N5 0.0181(14) 0.0182(12) 0.0351(15) -0.0026(11) 0.0123(11) -0.0008(11) C1 0.0127(14) 0.0221(15) 0.0201(14) -0.0008(11) 0.0036(11) 0.0005(11) C2 0.0146(15) 0.0233(15) 0.0196(14) -0.0012(11) 0.0044(11) -0.0007(11) C3 0.0192(16) 0.0197(16) 0.0434(19) -0.0158(14) 0.0152(14) -0.0069(12) C4 0.0277(18) 0.0230(16) 0.0295(16) -0.0063(13) 0.0110(14) -0.0027(13) C5 0.0211(17) 0.0199(15) 0.0365(18) 0.0007(13) 0.0080(14) -0.0047(13) C6 0.0221(17) 0.0223(16) 0.0342(17) 0.0035(13) 0.0125(14) -0.0015(13) C7 0.0200(17) 0.0215(16) 0.0386(18) 0.0011(13) 0.0133(14) -0.0018(12) C8 0.0173(16) 0.0303(18) 0.0337(18) -0.0042(13) 0.0095(14) -0.0049(13) C9 0.0216(18) 0.0260(17) 0.041(2) 0.0022(14) 0.0095(14) 0.0019(14) C10 0.0198(17) 0.0229(16) 0.0364(18) -0.0025(13) 0.0103(14) -0.0014(13) C11 0.0200(16) 0.0264(16) 0.0195(14) -0.0025(12) 0.0053(12) -0.0040(12) C12 0.0248(17) 0.0218(15) 0.0181(14) 0.0005(11) 0.0080(12) -0.0007(12) _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 N1 1.975(3) . yes Pt1 O1 2.008(2) . yes Pt1 S2 2.1762(8) . yes Pt1 Cl1 2.3150(8) . yes S2 O2 1.480(2) . ? S2 C12 1.763(3) . ? S2 C11 1.767(3) . ? O1 C2 1.293(4) . ? O3 C5 1.419(4) . ? O3 C4 1.426(4) . ? O4 C9 1.432(4) . ? O4 C8 1.432(4) . ? N1 C1 1.324(4) . ? N1 H1N 0.8847 . ? N2 C2 1.327(4) . ? N2 C1 1.342(4) . ? N3 C1 1.379(4) . ? N3 C6 1.467(4) . ? N3 C3 1.467(4) . ? N5 C2 1.361(4) . ? N5 C10 1.462(4) . ? N5 C7 1.463(4) . ? C3 C4 1.512(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.506(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.510(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? 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 N1 Pt1 O1 89.25(10) . . yes N1 Pt1 S2 90.86(8) . . ? O1 Pt1 S2 176.34(7) . . ? N1 Pt1 Cl1 176.93(8) . . ? O1 Pt1 Cl1 88.24(7) . . ? S2 Pt1 Cl1 91.76(3) . . yes O2 S2 C12 108.37(14) . . ? O2 S2 C11 108.67(15) . . ? C12 S2 C11 101.24(15) . . ? O2 S2 Pt1 114.84(10) . . ? C12 S2 Pt1 112.48(11) . . ? C11 S2 Pt1 110.32(11) . . ? C2 O1 Pt1 124.1(2) . . ? C5 O3 C4 110.2(3) . . ? C9 O4 C8 110.1(3) . . ? C1 N1 Pt1 126.2(2) . . ? C1 N1 H1N 113.2 . . ? Pt1 N1 H1N 119.6 . . ? C2 N2 C1 123.7(3) . . ? C1 N3 C6 119.2(3) . . ? C1 N3 C3 122.4(3) . . ? C6 N3 C3 111.8(3) . . ? C2 N5 C10 121.9(3) . . ? C2 N5 C7 122.4(3) . . ? C10 N5 C7 113.4(3) . . ? N1 C1 N2 126.5(3) . . ? N1 C1 N3 119.1(3) . . ? N2 C1 N3 114.4(3) . . ? O1 C2 N2 129.3(3) . . ? O1 C2 N5 114.3(3) . . ? N2 C2 N5 116.3(3) . . ? N3 C3 C4 109.1(3) . . ? N3 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N3 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O3 C4 C3 112.5(3) . . ? O3 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? O3 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? O3 C5 C6 111.7(3) . . ? O3 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O3 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N3 C6 C5 110.2(3) . . ? N3 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N3 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N5 C7 C8 109.7(3) . . ? N5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N5 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O4 C8 C7 111.6(3) . . ? O4 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? O4 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O4 C9 C10 111.0(3) . . ? O4 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? O4 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N5 C10 C9 109.1(3) . . ? N5 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N5 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? S2 C11 H11A 109.5 . . ? S2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S2 C12 H12A 109.5 . . ? S2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1N O2 0.88 2.33 2.899(3) 121.9 . yes _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.587 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.188