# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nianyong Zhu' _publ_contact_author_email nzhu@hkucc.hku.hk loop_ _publ_author_name C.-F.Chow M.-Y.Yuen V.A.L.Roy L.Wei Y.Chen S.S.-Y.Chui N.Zhu ; C.-M.Che ; data_1a _database_code_depnum_ccdc_archive 'CCDC 763168' #TrackingRef 'MicroPt2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H17 Cl2 N5 O2 Pt' _chemical_formula_sum 'C13 H17 Cl2 N5 O2 Pt' _chemical_formula_weight 541.31 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' Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8480(14) _cell_length_b 11.736(2) _cell_length_c 12.384(3) _cell_angle_alpha 65.95(3) _cell_angle_beta 79.94(3) _cell_angle_gamma 76.84(3) _cell_volume 881.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 8.279 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.500265 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5150 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3268 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.5364P] 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 3268 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1796(7) 0.8658(4) 0.9505(4) 0.0513(10) Uani 1 1 d . . . H1 H 0.1734 0.9530 0.9120 0.062 Uiso 1 1 calc R . . C2 C 0.1502(7) 0.8019(4) 1.0703(4) 0.0493(10) Uani 1 1 d . . . H2 H 0.1207 0.8356 1.1287 0.059 Uiso 1 1 calc R . . C3 C 0.1739(6) 0.6753(4) 1.0863(3) 0.0392(8) Uani 1 1 d . . . C4 C 0.1659(6) 0.5545(4) 1.1889(3) 0.0400(8) Uani 1 1 d . . . C5 C 0.1258(7) 0.5344(4) 1.3072(4) 0.0519(10) Uani 1 1 d . . . H5 H 0.0955 0.6018 1.3321 0.062 Uiso 1 1 calc R . . C6 C 0.1317(7) 0.4101(4) 1.3887(4) 0.0576(12) Uani 1 1 d . . . H6 H 0.1061 0.3941 1.4694 0.069 Uiso 1 1 calc R . . C7 C 0.1750(7) 0.3103(4) 1.3516(4) 0.0541(11) Uani 1 1 d . . . H7 H 0.1790 0.2274 1.4066 0.065 Uiso 1 1 calc R . . C8 C 0.2120(6) 0.3352(4) 1.2320(3) 0.0435(9) Uani 1 1 d . . . C9 C 0.2564(6) 0.2472(4) 1.1709(4) 0.0454(9) Uani 1 1 d . . . C10 C 0.2758(8) 0.1174(4) 1.2045(4) 0.0601(12) Uani 1 1 d . . . H10 H 0.2648 0.0570 1.2815 0.072 Uiso 1 1 calc R . . C11 C 0.3142(8) 0.0964(4) 1.1025(5) 0.0620(13) Uani 1 1 d . . . H11 H 0.3344 0.0179 1.0968 0.074 Uiso 1 1 calc R . . C12 C 0.5000(12) 0.2704(8) 0.6889(7) 0.105(2) Uani 1 1 d . . . H12A H 0.5414 0.3349 0.7042 0.157 Uiso 1 1 calc R . . H12B H 0.4264 0.3090 0.6198 0.157 Uiso 1 1 calc R . . H12C H 0.6166 0.2128 0.6756 0.157 Uiso 1 1 calc R . . C13 C 0.2927(11) 0.8640(6) 0.5623(5) 0.0884(19) Uani 1 1 d . . . H13A H 0.3953 0.9051 0.5061 0.133 Uiso 1 1 calc R . . H13B H 0.1652 0.8975 0.5292 0.133 Uiso 1 1 calc R . . H13C H 0.3250 0.7745 0.5802 0.133 Uiso 1 1 calc R . . Cl1 Cl 0.31863(17) 0.53250(11) 0.78462(9) 0.0510(2) Uani 1 1 d . . . Cl2 Cl -0.0793(2) 0.85928(11) 1.33323(10) 0.0626(3) Uani 1 1 d . . . Pt1 Pt 0.25827(2) 0.490145(12) 0.983892(11) 0.03470(6) Uani 1 1 d . . . O1 O 0.3706(7) 0.2009(4) 0.7917(3) 0.0806(11) Uani 1 1 d . . . H1A H 0.2809 0.1830 0.7686 0.121 Uiso 1 1 calc R . . O2 O 0.2822(13) 0.8845(4) 0.6621(3) 0.144(3) Uani 1 1 d . . . H2A H 0.2558 0.9609 0.6468 0.215 Uiso 1 1 calc R . . N1 N 0.2189(5) 0.7830(3) 0.8971(3) 0.0440(8) Uani 1 1 d . . . H1B H 0.2430 0.8020 0.8218 0.053 Uiso 1 1 calc R . . N2 N 0.2148(5) 0.6650(3) 0.9800(3) 0.0379(7) Uani 1 1 d . . . N3 N 0.2065(5) 0.4559(3) 1.1543(3) 0.0367(7) Uani 1 1 d . . . N4 N 0.2824(5) 0.3012(3) 1.0512(3) 0.0415(7) Uani 1 1 d . . . N5 N 0.3180(6) 0.2087(3) 1.0105(3) 0.0516(9) Uani 1 1 d . . . H5A H 0.3400 0.2190 0.9368 0.062 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 C1 0.067(3) 0.037(2) 0.044(2) -0.0117(17) -0.002(2) -0.007(2) C2 0.059(3) 0.049(2) 0.040(2) -0.0193(18) -0.0003(19) -0.009(2) C3 0.041(2) 0.042(2) 0.0309(18) -0.0124(15) -0.0021(15) -0.0055(16) C4 0.040(2) 0.046(2) 0.0312(18) -0.0113(16) -0.0005(15) -0.0097(17) C5 0.060(3) 0.057(3) 0.036(2) -0.0183(18) 0.0003(19) -0.009(2) C6 0.069(3) 0.067(3) 0.0277(19) -0.0106(19) 0.0004(19) -0.012(2) C7 0.062(3) 0.049(2) 0.037(2) -0.0011(18) -0.0029(19) -0.012(2) C8 0.040(2) 0.044(2) 0.038(2) -0.0059(16) -0.0042(16) -0.0087(17) C9 0.044(2) 0.043(2) 0.042(2) -0.0089(17) -0.0056(17) -0.0093(18) C10 0.073(3) 0.044(2) 0.053(3) -0.007(2) -0.004(2) -0.014(2) C11 0.078(4) 0.042(2) 0.064(3) -0.015(2) -0.009(3) -0.014(2) C12 0.116(6) 0.128(6) 0.096(5) -0.066(5) -0.005(4) -0.028(5) C13 0.129(6) 0.079(4) 0.052(3) -0.021(3) -0.008(3) -0.015(4) Cl1 0.0563(6) 0.0615(6) 0.0333(5) -0.0184(4) -0.0024(4) -0.0076(5) Cl2 0.0933(9) 0.0504(6) 0.0417(6) -0.0162(4) -0.0024(6) -0.0141(6) Pt1 0.03452(9) 0.03725(9) 0.02870(9) -0.00986(6) -0.00313(5) -0.00446(6) O1 0.100(3) 0.089(3) 0.066(2) -0.041(2) -0.007(2) -0.020(2) O2 0.306(8) 0.058(2) 0.034(2) -0.0131(17) -0.006(3) 0.014(4) N1 0.053(2) 0.0383(17) 0.0312(16) -0.0050(13) -0.0028(14) -0.0061(15) N2 0.0379(17) 0.0399(16) 0.0313(15) -0.0101(13) -0.0016(13) -0.0059(14) N3 0.0349(17) 0.0387(16) 0.0295(15) -0.0063(13) -0.0034(12) -0.0059(13) N4 0.0413(19) 0.0403(17) 0.0424(18) -0.0159(14) -0.0037(14) -0.0057(14) N5 0.058(2) 0.048(2) 0.051(2) -0.0219(17) -0.0077(18) -0.0078(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(6) . ? C1 C2 1.365(6) . ? C1 H1 0.9300 . ? C2 C3 1.392(6) . ? C2 H2 0.9300 . ? C3 N2 1.346(5) . ? C3 C4 1.473(5) . ? C4 N3 1.347(5) . ? C4 C5 1.373(6) . ? C5 C6 1.391(6) . ? C5 H5 0.9300 . ? C6 C7 1.380(7) . ? C6 H6 0.9300 . ? C7 C8 1.376(6) . ? C7 H7 0.9300 . ? C8 N3 1.346(5) . ? C8 C9 1.465(6) . ? C9 N4 1.351(5) . ? C9 C10 1.387(6) . ? C10 C11 1.354(7) . ? C10 H10 0.9300 . ? C11 N5 1.348(6) . ? C11 H11 0.9300 . ? C12 O1 1.470(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O2 1.340(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Cl1 Pt1 2.2903(12) . ? Pt1 N3 1.963(3) . ? Pt1 N2 1.987(3) . ? Pt1 N4 2.003(3) . ? O1 H1A 0.8200 . ? O2 H2A 0.8200 . ? N1 N2 1.349(4) . ? N1 H1B 0.8600 . ? N4 N5 1.332(5) . ? N5 H5A 0.8600 . ? 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 C1 C2 109.1(4) . . ? N1 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? C1 C2 C3 105.0(4) . . ? C1 C2 H2 127.5 . . ? C3 C2 H2 127.5 . . ? N2 C3 C2 109.5(3) . . ? N2 C3 C4 114.9(3) . . ? C2 C3 C4 135.6(4) . . ? N3 C4 C5 120.2(4) . . ? N3 C4 C3 111.2(3) . . ? C5 C4 C3 128.5(4) . . ? C4 C5 C6 118.0(4) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N3 C8 C7 119.3(4) . . ? N3 C8 C9 111.3(4) . . ? C7 C8 C9 129.3(4) . . ? N4 C9 C10 108.5(4) . . ? N4 C9 C8 115.4(3) . . ? C10 C9 C8 136.0(4) . . ? C11 C10 C9 106.0(4) . . ? C11 C10 H10 127.0 . . ? C9 C10 H10 127.0 . . ? N5 C11 C10 108.4(4) . . ? N5 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 Pt1 N2 79.57(13) . . ? N3 Pt1 N4 79.44(14) . . ? N2 Pt1 N4 159.02(13) . . ? N3 Pt1 Cl1 179.34(9) . . ? N2 Pt1 Cl1 99.77(10) . . ? N4 Pt1 Cl1 101.21(11) . . ? C12 O1 H1A 109.5 . . ? C13 O2 H2A 109.5 . . ? C1 N1 N2 109.4(3) . . ? C1 N1 H1B 125.3 . . ? N2 N1 H1B 125.3 . . ? C3 N2 N1 107.0(3) . . ? C3 N2 Pt1 115.7(2) . . ? N1 N2 Pt1 137.3(3) . . ? C8 N3 C4 122.5(3) . . ? C8 N3 Pt1 118.9(3) . . ? C4 N3 Pt1 118.6(2) . . ? N5 N4 C9 107.5(3) . . ? N5 N4 Pt1 137.6(3) . . ? C9 N4 Pt1 114.9(3) . . ? N4 N5 C11 109.6(4) . . ? N4 N5 H5A 125.2 . . ? C11 N5 H5A 125.2 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.822 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.129 data_wt1698 _database_code_depnum_ccdc_archive 'CCDC 763169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H14.33 Cl2 N5 O0.67 Pt' _chemical_formula_sum 'C13 H14.33 Cl2 N5 O0.67 Pt' _chemical_formula_weight 517.28 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' 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' 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' _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 12.588(2) _cell_length_b 18.736(3) _cell_length_c 20.805(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.39(2) _cell_angle_gamma 90.00 _cell_volume 4707.3(14) _cell_formula_units_Z 12 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 9.288 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.614671 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27598 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8927 _reflns_number_gt 5755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution SHELXS-97 _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.0653P] 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 8927 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3635(9) 0.3622(5) 0.1698(4) 0.069(3) Uani 1 1 d . . . H1A H -0.4049 0.3216 0.1774 0.104 Uiso 1 1 calc R . . H1B H -0.3928 0.4047 0.1841 0.104 Uiso 1 1 calc R . . H1C H -0.2872 0.3567 0.1948 0.104 Uiso 1 1 calc R . . C2 C -0.4274(8) 0.4160(5) 0.0548(5) 0.059(3) Uani 1 1 d . . . H2 H -0.4660 0.4543 0.0656 0.071 Uiso 1 1 calc R . . C3 C -0.4194(8) 0.4013(5) -0.0084(5) 0.057(2) Uani 1 1 d . . . H3 H -0.4508 0.4259 -0.0481 0.069 Uiso 1 1 calc R . . C4 C -0.3526(7) 0.3406(4) 0.0013(4) 0.044(2) Uani 1 1 d . . . C5 C -0.3084(7) 0.2974(4) -0.0426(4) 0.041(2) Uani 1 1 d . . . C6 C -0.3221(8) 0.3047(5) -0.1112(4) 0.054(2) Uani 1 1 d . . . H6 H -0.3659 0.3410 -0.1354 0.064 Uiso 1 1 calc R . . C7 C -0.2704(8) 0.2578(5) -0.1419(4) 0.060(3) Uani 1 1 d . . . H7 H -0.2799 0.2621 -0.1878 0.072 Uiso 1 1 calc R . . C8 C -0.2034(8) 0.2033(5) -0.1067(4) 0.058(3) Uani 1 1 d . . . H8 H -0.1687 0.1713 -0.1284 0.070 Uiso 1 1 calc R . . C9 C -0.1904(6) 0.1984(4) -0.0394(4) 0.0359(18) Uani 1 1 d . . . C10 C -0.1250(7) 0.1477(4) 0.0082(4) 0.046(2) Uani 1 1 d . . . C11 C -0.0489(8) 0.0943(5) 0.0053(5) 0.062(3) Uani 1 1 d . . . H11 H -0.0286 0.0794 -0.0322 0.074 Uiso 1 1 calc R . . C12 C -0.0109(8) 0.0689(5) 0.0686(5) 0.062(3) Uani 1 1 d . . . H12 H 0.0417 0.0330 0.0824 0.074 Uiso 1 1 calc R . . C13 C -0.0414(8) 0.0935(5) 0.1804(4) 0.064(3) Uani 1 1 d . . . H13A H -0.0010 0.1336 0.2038 0.096 Uiso 1 1 calc R . . H13B H 0.0009 0.0507 0.1941 0.096 Uiso 1 1 calc R . . H13C H -0.1109 0.0895 0.1905 0.096 Uiso 1 1 calc R . . C14 C -0.2766(9) 0.5895(5) -0.1213(6) 0.090(4) Uani 1 1 d . . . H14A H -0.3143 0.6346 -0.1283 0.135 Uiso 1 1 calc R . . H14B H -0.3234 0.5535 -0.1478 0.135 Uiso 1 1 calc R . . H14C H -0.2095 0.5931 -0.1345 0.135 Uiso 1 1 calc R . . C15 C -0.2841(9) 0.6040(6) -0.0034(7) 0.082(4) Uani 1 1 d . . . H15 H -0.3273 0.6451 -0.0101 0.099 Uiso 1 1 calc R . . C16 C -0.2461(9) 0.5689(6) 0.0556(7) 0.086(4) Uani 1 1 d . . . H16 H -0.2579 0.5808 0.0964 0.103 Uiso 1 1 calc R . . C17 C -0.1859(8) 0.5115(5) 0.0421(6) 0.062(3) Uani 1 1 d . . . C18 C -0.1230(8) 0.4538(5) 0.0814(5) 0.056(2) Uani 1 1 d . . . C19 C -0.1036(9) 0.4394(6) 0.1497(5) 0.072(3) Uani 1 1 d . . . H19 H -0.1340 0.4683 0.1763 0.086 Uiso 1 1 calc R . . C20 C -0.0371(9) 0.3805(6) 0.1775(5) 0.075(3) Uani 1 1 d . . . H20 H -0.0240 0.3697 0.2227 0.090 Uiso 1 1 calc R . . C21 C 0.0076(8) 0.3396(5) 0.1383(5) 0.059(3) Uani 1 1 d . . . H21 H 0.0515 0.3006 0.1565 0.071 Uiso 1 1 calc R . . C22 C -0.0118(7) 0.3557(5) 0.0716(4) 0.046(2) Uani 1 1 d . . . C23 C 0.0286(7) 0.3185(5) 0.0223(4) 0.048(2) Uani 1 1 d . . . C24 C 0.0963(7) 0.2585(4) 0.0246(5) 0.053(2) Uani 1 1 d . . . H24 H 0.1311 0.2305 0.0615 0.063 Uiso 1 1 calc R . . C25 C 0.0988(8) 0.2509(5) -0.0401(5) 0.062(3) Uani 1 1 d . . . H25 H 0.1373 0.2152 -0.0551 0.075 Uiso 1 1 calc R . . C26 C 0.0200(9) 0.3110(6) -0.1515(5) 0.080(3) Uani 1 1 d . . . H26A H 0.0651 0.3494 -0.1593 0.120 Uiso 1 1 calc R . . H26B H -0.0567 0.3219 -0.1719 0.120 Uiso 1 1 calc R . . H26C H 0.0390 0.2678 -0.1705 0.120 Uiso 1 1 calc R . . C27 C 0.3571(11) 0.2625(6) -0.1303(6) 0.105(5) Uani 1 1 d . . . H27A H 0.3181 0.2860 -0.1712 0.158 Uiso 1 1 calc R . . H27B H 0.4053 0.2961 -0.1013 0.158 Uiso 1 1 calc R . . H27C H 0.3050 0.2441 -0.1086 0.158 Uiso 1 1 calc R . . C28 C 0.4280(11) 0.1853(7) -0.2061(6) 0.096(4) Uani 1 1 d . . . H28 H 0.3921 0.2078 -0.2462 0.115 Uiso 1 1 calc R . . C29 C 0.4956(10) 0.1272(6) -0.1991(5) 0.080(3) Uani 1 1 d . . . H29 H 0.5138 0.1026 -0.2334 0.096 Uiso 1 1 calc R . . C30 C 0.5323(8) 0.1119(5) -0.1309(5) 0.058(3) Uani 1 1 d . . . C31 C 0.5995(8) 0.0572(5) -0.0897(5) 0.053(2) Uani 1 1 d . . . C32 C 0.6556(8) 0.0027(5) -0.1110(5) 0.067(3) Uani 1 1 d . . . H32 H 0.6521 -0.0026 -0.1560 0.080 Uiso 1 1 calc R . . C33 C 0.7171(8) -0.0437(5) -0.0632(6) 0.065(3) Uani 1 1 d . . . H33 H 0.7570 -0.0803 -0.0758 0.078 Uiso 1 1 calc R . . C34 C 0.7196(7) -0.0360(5) 0.0029(5) 0.059(3) Uani 1 1 d . . . H34 H 0.7594 -0.0681 0.0347 0.070 Uiso 1 1 calc R . . C35 C 0.6633(7) 0.0191(5) 0.0220(5) 0.051(2) Uani 1 1 d . . . C36 C 0.6481(7) 0.0356(5) 0.0879(5) 0.051(2) Uani 1 1 d . . . C37 C 0.6871(8) 0.0055(5) 0.1510(4) 0.057(3) Uani 1 1 d . . . H37 H 0.7349 -0.0331 0.1635 0.068 Uiso 1 1 calc R . . C38 C 0.6398(8) 0.0450(5) 0.1909(5) 0.061(3) Uani 1 1 d . . . H38 H 0.6514 0.0384 0.2367 0.073 Uiso 1 1 calc R . . C39 C 0.5101(8) 0.1474(5) 0.1767(4) 0.064(3) Uani 1 1 d . . . H39A H 0.5478 0.1925 0.1819 0.097 Uiso 1 1 calc R . . H39B H 0.5015 0.1325 0.2191 0.097 Uiso 1 1 calc R . . H39C H 0.4386 0.1521 0.1449 0.097 Uiso 1 1 calc R . . Cl1 Cl -0.2098(2) 0.22084(13) 0.19921(11) 0.0627(7) Uani 1 1 d . . . Cl2 Cl -0.1366(2) 0.45517(15) -0.16371(12) 0.0777(8) Uani 1 1 d . . . Cl3 Cl 0.4154(2) 0.22877(13) 0.03249(13) 0.0718(7) Uani 1 1 d . . . Cl4 Cl 0.4980(2) 0.03446(13) 0.32286(12) 0.0624(6) Uani 1 1 d . . . Cl5 Cl 0.2235(3) 0.19719(16) 0.18737(14) 0.0898(9) Uani 1 1 d . . . Cl6 Cl 0.0706(3) 0.39308(16) 0.35621(14) 0.1072(12) Uani 1 1 d . . . Pt1 Pt -0.22762(3) 0.233746(17) 0.087225(16) 0.03954(9) Uani 1 1 d . . . Pt2 Pt -0.10417(3) 0.432015(18) -0.051640(17) 0.04655(10) Uani 1 1 d . . . Pt3 Pt 0.51719(3) 0.140966(17) 0.001278(17) 0.04583(10) Uani 1 1 d . . . N1 N -0.3260(5) 0.3205(3) 0.0659(3) 0.0441(17) Uani 1 1 d . . . N2 N -0.3721(6) 0.3675(4) 0.0983(3) 0.0500(19) Uani 1 1 d . . . N3 N -0.1318(5) 0.1527(3) 0.0722(3) 0.0419(16) Uani 1 1 d . . . N4 N -0.0612(6) 0.1036(4) 0.1082(4) 0.0492(18) Uani 1 1 d . . . N5 N -0.2438(5) 0.2446(3) -0.0087(3) 0.0396(16) Uani 1 1 d . . . N6 N -0.1891(6) 0.5120(4) -0.0243(4) 0.0528(19) Uani 1 1 d . . . N7 N -0.2497(6) 0.5700(4) -0.0501(5) 0.071(3) Uani 1 1 d . . . N8 N -0.0064(5) 0.3451(4) -0.0419(3) 0.0452(17) Uani 1 1 d . . . N9 N 0.0390(6) 0.3015(4) -0.0791(3) 0.0534(19) Uani 1 1 d . . . N10 N -0.0771(6) 0.4113(4) 0.0438(4) 0.0475(18) Uani 1 1 d . . . N11 N 0.4860(7) 0.1605(4) -0.0977(4) 0.060(2) Uani 1 1 d . . . N12 N 0.4223(8) 0.2041(5) -0.1453(4) 0.077(3) Uani 1 1 d . . . N13 N 0.5790(6) 0.0905(3) 0.0901(3) 0.0456(18) Uani 1 1 d . . . N14 N 0.5737(6) 0.0951(4) 0.1533(3) 0.0479(18) Uani 1 1 d . . . N15 N 0.6023(6) 0.0640(3) -0.0255(4) 0.0464(17) Uani 1 1 d . . . O1 O 0.2448(6) 0.0625(4) 0.2735(4) 0.101(3) Uani 1 1 d . . . O2 O -0.1681(9) 0.4445(5) 0.3125(5) 0.141(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.105(9) 0.063(6) 0.052(6) 0.000(5) 0.041(6) 0.022(6) C2 0.075(7) 0.037(5) 0.073(7) 0.004(5) 0.035(6) 0.010(5) C3 0.062(7) 0.049(6) 0.064(7) 0.004(5) 0.021(5) 0.007(5) C4 0.053(6) 0.040(5) 0.038(5) 0.002(4) 0.010(4) 0.001(4) C5 0.052(6) 0.039(5) 0.036(5) 0.001(4) 0.019(4) -0.003(4) C6 0.065(6) 0.050(6) 0.043(5) 0.000(4) 0.012(5) 0.001(5) C7 0.088(8) 0.066(7) 0.030(5) -0.005(5) 0.021(5) -0.012(6) C8 0.094(8) 0.048(5) 0.043(6) -0.008(4) 0.034(5) -0.005(5) C9 0.043(5) 0.033(4) 0.038(5) -0.002(4) 0.021(4) -0.008(4) C10 0.062(6) 0.036(5) 0.048(5) -0.007(4) 0.029(5) -0.005(4) C11 0.093(8) 0.048(6) 0.057(6) -0.007(5) 0.043(6) 0.007(5) C12 0.069(7) 0.046(6) 0.076(7) -0.011(5) 0.030(6) 0.014(5) C13 0.081(8) 0.064(6) 0.047(6) 0.005(5) 0.018(5) 0.014(5) C14 0.075(8) 0.050(7) 0.113(10) 0.012(6) -0.024(7) 0.007(6) C15 0.058(7) 0.052(7) 0.131(12) -0.013(8) 0.016(8) 0.005(6) C16 0.079(9) 0.060(7) 0.126(11) -0.027(7) 0.041(8) -0.006(6) C17 0.053(6) 0.050(6) 0.083(8) -0.023(5) 0.019(6) -0.011(5) C18 0.052(6) 0.053(6) 0.066(7) -0.012(5) 0.019(5) -0.011(5) C19 0.080(8) 0.077(8) 0.062(7) -0.030(6) 0.028(6) -0.025(6) C20 0.091(9) 0.082(8) 0.057(7) -0.013(6) 0.027(6) -0.023(7) C21 0.071(7) 0.056(6) 0.050(6) -0.002(5) 0.014(5) -0.015(5) C22 0.042(5) 0.053(6) 0.037(5) -0.006(4) 0.004(4) -0.006(4) C23 0.050(6) 0.049(6) 0.039(5) -0.006(4) 0.005(4) -0.010(4) C24 0.056(6) 0.037(5) 0.056(6) -0.003(4) 0.001(5) -0.001(4) C25 0.066(7) 0.050(6) 0.064(7) -0.008(5) 0.005(5) 0.008(5) C26 0.090(8) 0.100(9) 0.052(7) -0.012(6) 0.023(6) 0.006(7) C27 0.165(13) 0.078(8) 0.070(8) 0.019(6) 0.029(8) 0.045(9) C28 0.145(12) 0.089(10) 0.058(8) 0.017(7) 0.037(8) 0.018(9) C29 0.114(10) 0.081(8) 0.055(7) 0.003(6) 0.041(7) 0.001(7) C30 0.076(7) 0.062(6) 0.045(6) -0.004(5) 0.030(5) -0.018(5) C31 0.064(6) 0.051(6) 0.052(6) -0.002(5) 0.028(5) -0.010(5) C32 0.070(7) 0.070(7) 0.076(7) -0.013(6) 0.045(6) -0.010(6) C33 0.057(7) 0.065(7) 0.085(8) -0.010(6) 0.037(6) 0.003(5) C34 0.053(6) 0.044(6) 0.080(8) 0.001(5) 0.021(5) 0.001(5) C35 0.043(6) 0.045(5) 0.063(6) 0.003(5) 0.014(5) -0.002(4) C36 0.043(5) 0.045(5) 0.058(6) -0.002(4) 0.006(5) -0.006(4) C37 0.064(7) 0.054(6) 0.047(6) 0.006(5) 0.007(5) 0.004(5) C38 0.067(7) 0.064(7) 0.046(6) 0.010(5) 0.009(5) -0.010(5) C39 0.086(8) 0.058(6) 0.051(6) -0.009(5) 0.023(5) 0.006(5) Cl1 0.0795(18) 0.0738(17) 0.0384(13) 0.0051(11) 0.0226(12) 0.0204(13) Cl2 0.083(2) 0.084(2) 0.0553(16) 0.0194(13) 0.0014(14) 0.0040(15) Cl3 0.096(2) 0.0591(15) 0.0634(16) 0.0082(12) 0.0268(15) 0.0299(14) Cl4 0.0713(17) 0.0569(14) 0.0599(15) 0.0073(12) 0.0200(13) -0.0036(12) Cl5 0.093(2) 0.087(2) 0.0723(19) 0.0145(16) -0.0044(16) 0.0097(17) Cl6 0.174(3) 0.076(2) 0.0569(18) 0.0095(15) 0.008(2) -0.038(2) Pt1 0.0480(2) 0.03759(18) 0.03568(18) -0.00207(14) 0.01608(15) -0.00007(15) Pt2 0.0433(2) 0.04143(19) 0.0493(2) 0.00037(16) 0.00390(16) -0.00399(16) Pt3 0.0547(2) 0.03924(19) 0.0453(2) 0.00207(15) 0.01695(17) -0.00148(16) N1 0.049(4) 0.046(4) 0.039(4) -0.004(3) 0.016(3) 0.002(3) N2 0.069(5) 0.041(4) 0.044(4) -0.005(3) 0.024(4) 0.009(4) N3 0.050(4) 0.036(4) 0.045(4) 0.001(3) 0.021(3) 0.005(3) N4 0.054(5) 0.036(4) 0.057(5) 0.002(4) 0.016(4) 0.002(4) N5 0.047(4) 0.030(4) 0.046(4) -0.007(3) 0.021(3) -0.003(3) N6 0.041(5) 0.041(4) 0.069(6) -0.004(4) 0.005(4) -0.004(3) N7 0.051(5) 0.041(5) 0.113(8) 0.004(5) 0.009(5) 0.008(4) N8 0.042(4) 0.051(4) 0.038(4) -0.006(3) 0.005(3) -0.004(3) N9 0.062(5) 0.055(5) 0.040(4) -0.011(4) 0.009(4) -0.003(4) N10 0.043(4) 0.040(4) 0.057(5) -0.013(3) 0.009(4) -0.009(3) N11 0.078(6) 0.047(5) 0.059(5) 0.002(4) 0.024(5) -0.001(4) N12 0.116(8) 0.066(6) 0.052(6) 0.014(5) 0.026(5) 0.021(5) N13 0.053(5) 0.037(4) 0.045(5) 0.002(3) 0.010(4) -0.003(3) N14 0.060(5) 0.048(4) 0.036(4) -0.002(3) 0.014(4) -0.002(4) N15 0.053(5) 0.039(4) 0.051(5) -0.005(3) 0.022(4) -0.010(3) O1 0.076(5) 0.097(6) 0.127(7) 0.031(5) 0.025(5) 0.002(4) O2 0.196(11) 0.108(7) 0.161(9) 0.006(6) 0.118(8) -0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.464(10) . ? C2 N2 1.331(10) . ? C2 C3 1.375(12) . ? C3 C4 1.394(11) . ? C4 N1 1.345(9) . ? C4 C5 1.444(11) . ? C5 N5 1.347(10) . ? C5 C6 1.396(11) . ? C6 C7 1.356(12) . ? C7 C8 1.393(12) . ? C8 C9 1.367(10) . ? C9 N5 1.361(9) . ? C9 C10 1.449(11) . ? C10 N3 1.362(10) . ? C10 C11 1.399(11) . ? C11 C12 1.354(12) . ? C12 N4 1.340(10) . ? C13 N4 1.464(10) . ? C14 N7 1.469(13) . ? C15 N7 1.333(13) . ? C15 C16 1.354(15) . ? C16 C17 1.390(13) . ? C17 N6 1.371(12) . ? C17 C18 1.448(13) . ? C18 N10 1.354(11) . ? C18 C19 1.399(13) . ? C19 C20 1.407(14) . ? C20 C21 1.353(13) . ? C21 C22 1.371(11) . ? C22 N10 1.351(10) . ? C22 C23 1.447(11) . ? C23 N8 1.375(10) . ? C23 C24 1.404(11) . ? C24 C25 1.363(12) . ? C25 N9 1.333(11) . ? C26 N9 1.467(11) . ? C27 N12 1.454(13) . ? C28 N12 1.334(12) . ? C28 C29 1.364(14) . ? C29 C30 1.393(13) . ? C30 N11 1.369(11) . ? C30 C31 1.445(13) . ? C31 N15 1.332(10) . ? C31 C32 1.384(12) . ? C32 C33 1.381(13) . ? C33 C34 1.374(12) . ? C34 C35 1.373(12) . ? C35 N15 1.359(10) . ? C35 C36 1.469(12) . ? C36 N13 1.357(10) . ? C36 C37 1.385(11) . ? C37 C38 1.368(12) . ? C38 N14 1.349(11) . ? C39 N14 1.434(10) . ? Cl1 Pt1 2.289(2) . ? Cl2 Pt2 2.292(3) . ? Cl3 Pt3 2.289(2) . ? Pt1 N5 1.958(6) . ? Pt1 N1 2.015(6) . ? Pt1 N3 2.018(6) . ? Pt2 N10 1.957(7) . ? Pt2 N6 2.014(7) . ? Pt2 N8 2.017(7) . ? Pt3 N15 1.969(7) . ? Pt3 N11 2.019(8) . ? Pt3 N13 2.025(7) . ? N1 N2 1.339(8) . ? N3 N4 1.348(9) . ? N6 N7 1.350(10) . ? N8 N9 1.358(9) . ? N11 N12 1.357(10) . ? N13 N14 1.338(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C2 C3 110.5(8) . . ? C2 C3 C4 103.2(8) . . ? N1 C4 C3 110.1(8) . . ? N1 C4 C5 116.2(7) . . ? C3 C4 C5 133.6(8) . . ? N5 C5 C6 119.3(7) . . ? N5 C5 C4 111.4(7) . . ? C6 C5 C4 129.3(8) . . ? C7 C6 C5 118.8(9) . . ? C6 C7 C8 121.7(8) . . ? C9 C8 C7 118.0(8) . . ? N5 C9 C8 120.3(8) . . ? N5 C9 C10 111.0(7) . . ? C8 C9 C10 128.7(8) . . ? N3 C10 C11 108.9(8) . . ? N3 C10 C9 116.3(7) . . ? C11 C10 C9 134.7(8) . . ? C12 C11 C10 105.5(8) . . ? N4 C12 C11 109.2(9) . . ? N7 C15 C16 109.0(11) . . ? C15 C16 C17 105.5(12) . . ? N6 C17 C16 109.6(10) . . ? N6 C17 C18 115.4(8) . . ? C16 C17 C18 135.0(12) . . ? N10 C18 C19 119.5(9) . . ? N10 C18 C17 111.6(9) . . ? C19 C18 C17 128.9(10) . . ? C18 C19 C20 118.8(10) . . ? C21 C20 C19 119.7(10) . . ? C20 C21 C22 120.1(10) . . ? N10 C22 C21 121.0(8) . . ? N10 C22 C23 111.1(7) . . ? C21 C22 C23 127.9(9) . . ? N8 C23 C24 110.4(8) . . ? N8 C23 C22 115.7(8) . . ? C24 C23 C22 133.9(8) . . ? C25 C24 C23 103.4(8) . . ? N9 C25 C24 111.2(8) . . ? N12 C28 C29 107.9(10) . . ? C28 C29 C30 106.9(10) . . ? N11 C30 C29 108.1(9) . . ? N11 C30 C31 115.7(8) . . ? C29 C30 C31 136.1(10) . . ? N15 C31 C32 121.3(9) . . ? N15 C31 C30 111.9(8) . . ? C32 C31 C30 126.8(9) . . ? C33 C32 C31 117.8(10) . . ? C34 C33 C32 120.3(9) . . ? C35 C34 C33 120.0(9) . . ? N15 C35 C34 119.1(9) . . ? N15 C35 C36 110.7(8) . . ? C34 C35 C36 129.9(9) . . ? N13 C36 C37 109.6(8) . . ? N13 C36 C35 116.4(8) . . ? C37 C36 C35 134.0(9) . . ? C38 C37 C36 104.9(9) . . ? N14 C38 C37 109.0(8) . . ? N5 Pt1 N1 79.1(3) . . ? N5 Pt1 N3 79.4(3) . . ? N1 Pt1 N3 158.4(3) . . ? N5 Pt1 Cl1 179.7(2) . . ? N1 Pt1 Cl1 100.79(19) . . ? N3 Pt1 Cl1 100.75(19) . . ? N10 Pt2 N6 79.3(3) . . ? N10 Pt2 N8 79.1(3) . . ? N6 Pt2 N8 158.4(3) . . ? N10 Pt2 Cl2 179.4(2) . . ? N6 Pt2 Cl2 101.0(2) . . ? N8 Pt2 Cl2 100.6(2) . . ? N15 Pt3 N11 78.9(3) . . ? N15 Pt3 N13 79.5(3) . . ? N11 Pt3 N13 158.4(3) . . ? N15 Pt3 Cl3 178.8(2) . . ? N11 Pt3 Cl3 101.3(2) . . ? N13 Pt3 Cl3 100.3(2) . . ? N2 N1 C4 107.3(7) . . ? N2 N1 Pt1 138.3(5) . . ? C4 N1 Pt1 114.3(5) . . ? C2 N2 N1 108.9(7) . . ? C2 N2 C1 127.8(7) . . ? N1 N2 C1 123.3(7) . . ? N4 N3 C10 106.4(6) . . ? N4 N3 Pt1 139.1(5) . . ? C10 N3 Pt1 114.1(5) . . ? C12 N4 N3 110.0(7) . . ? C12 N4 C13 126.4(8) . . ? N3 N4 C13 123.5(7) . . ? C5 N5 C9 121.8(7) . . ? C5 N5 Pt1 118.9(5) . . ? C9 N5 Pt1 119.3(5) . . ? N7 N6 C17 105.0(8) . . ? N7 N6 Pt2 140.6(7) . . ? C17 N6 Pt2 114.4(6) . . ? C15 N7 N6 110.9(10) . . ? C15 N7 C14 126.0(10) . . ? N6 N7 C14 123.0(9) . . ? N9 N8 C23 105.3(7) . . ? N9 N8 Pt2 140.5(6) . . ? C23 N8 Pt2 114.2(6) . . ? C25 N9 N8 109.7(7) . . ? C25 N9 C26 127.7(8) . . ? N8 N9 C26 122.6(8) . . ? C22 N10 C18 120.9(8) . . ? C22 N10 Pt2 119.9(6) . . ? C18 N10 Pt2 119.2(6) . . ? N12 N11 C30 106.3(8) . . ? N12 N11 Pt3 139.3(7) . . ? C30 N11 Pt3 114.0(6) . . ? C28 N12 N11 110.8(9) . . ? C28 N12 C27 125.9(10) . . ? N11 N12 C27 123.3(8) . . ? N14 N13 C36 107.0(7) . . ? N14 N13 Pt3 138.9(6) . . ? C36 N13 Pt3 114.1(6) . . ? N13 N14 C38 109.4(7) . . ? N13 N14 C39 124.5(7) . . ? C38 N14 C39 126.1(8) . . ? C31 N15 C35 121.4(8) . . ? C31 N15 Pt3 119.4(6) . . ? C35 N15 Pt3 119.2(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.356 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.156 data_wt1535 _database_code_depnum_ccdc_archive 'CCDC 763170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl4 N10 O8 Pt2' _chemical_formula_sum 'C26 H26 Cl4 N10 O8 Pt2' _chemical_formula_weight 1138.55 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' Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 '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' _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 10.669(2) _cell_length_b 10.411(2) _cell_length_c 15.689(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.89(3) _cell_angle_gamma 90.00 _cell_volume 1648.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 8.865 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.641508 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9437 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3116 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.1486P] 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 3116 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0484 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1771(4) 0.0991(5) 0.1879(3) 0.0515(10) Uani 1 1 d . . . H1 H 0.1007 0.1151 0.2024 0.062 Uiso 1 1 calc R . . C2 C 0.2359(4) -0.0186(4) 0.1911(3) 0.0475(9) Uani 1 1 d . . . H2 H 0.2085 -0.0967 0.2078 0.057 Uiso 1 1 calc R . . C3 C 0.3452(3) 0.0044(3) 0.1641(2) 0.0370(8) Uani 1 1 d . . . C4 C 0.4487(3) -0.0761(3) 0.1504(2) 0.0338(7) Uani 1 1 d . . . C5 C 0.4610(4) -0.2088(4) 0.1564(3) 0.0422(9) Uani 1 1 d . . . H5 H 0.3993 -0.2584 0.1720 0.051 Uiso 1 1 calc R . . C6 C 0.5674(4) -0.2659(4) 0.1384(3) 0.0463(9) Uani 1 1 d . . . H6 H 0.5769 -0.3548 0.1421 0.056 Uiso 1 1 calc R . . C7 C 0.6588(4) -0.1932(3) 0.1155(3) 0.0429(9) Uani 1 1 d . . . H7 H 0.7298 -0.2321 0.1035 0.052 Uiso 1 1 calc R . . C8 C 0.6438(3) -0.0611(3) 0.1103(2) 0.0345(7) Uani 1 1 d . . . C9 C 0.7248(3) 0.0352(4) 0.0850(2) 0.0370(7) Uani 1 1 d . . . C10 C 0.8367(4) 0.0300(4) 0.0589(3) 0.0483(9) Uani 1 1 d . . . H10 H 0.8856 -0.0424 0.0550 0.058 Uiso 1 1 calc R . . C11 C 0.8600(4) 0.1535(5) 0.0403(3) 0.0536(11) Uani 1 1 d . . . H11 H 0.9288 0.1808 0.0205 0.064 Uiso 1 1 calc R . . C12 C 0.2153(5) 0.3231(4) 0.1457(3) 0.0573(12) Uani 1 1 d . . . H12A H 0.2899 0.3734 0.1802 0.086 Uiso 1 1 calc R . . H12B H 0.1401 0.3428 0.1642 0.086 Uiso 1 1 calc R . . H12C H 0.1951 0.3426 0.0829 0.086 Uiso 1 1 calc R . . C13 C 0.7593(5) 0.3688(4) 0.0477(3) 0.0607(12) Uani 1 1 d . . . H13A H 0.6745 0.3928 0.0063 0.091 Uiso 1 1 calc R . . H13B H 0.8281 0.4004 0.0261 0.091 Uiso 1 1 calc R . . H13C H 0.7697 0.4052 0.1058 0.091 Uiso 1 1 calc R . . Pt1 Pt 0.513401(12) 0.180082(12) 0.112635(8) 0.02950(6) Uani 1 1 d . . . O1 O 1.0041(4) 0.5354(3) 0.1836(3) 0.0940(13) Uani 1 1 d . . . O2 O 0.9637(5) 0.7029(6) 0.0782(3) 0.121(2) Uani 1 1 d . . . O3 O 1.1785(4) 0.6471(4) 0.1592(3) 0.0926(13) Uani 1 1 d . . . O4 O 1.0442(5) 0.7457(4) 0.2302(3) 0.0923(13) Uani 1 1 d . . . N1 N 0.2470(3) 0.1874(3) 0.1604(2) 0.0424(8) Uani 1 1 d . . . N2 N 0.3524(3) 0.1307(3) 0.14562(19) 0.0346(6) Uani 1 1 d . . . N3 N 0.5393(3) -0.0070(3) 0.12681(17) 0.0315(6) Uani 1 1 d . . . N4 N 0.6823(3) 0.1579(3) 0.0827(2) 0.0362(7) Uani 1 1 d . . . N5 N 0.7678(3) 0.2296(3) 0.0550(2) 0.0429(7) Uani 1 1 d . . . Cl1 Cl 0.48254(12) 0.39731(9) 0.09714(8) 0.0564(3) Uani 1 1 d . . . Cl2 Cl 1.04732(10) 0.65613(10) 0.16130(7) 0.0476(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0361(19) 0.076(3) 0.047(2) -0.009(2) 0.0192(17) -0.006(2) C2 0.043(2) 0.060(3) 0.043(2) 0.0011(19) 0.0184(16) -0.0149(19) C3 0.0389(18) 0.0392(18) 0.0320(17) -0.0007(15) 0.0103(14) -0.0062(14) C4 0.0410(18) 0.0302(17) 0.0292(16) 0.0011(13) 0.0100(13) -0.0068(14) C5 0.054(2) 0.0326(18) 0.0355(19) 0.0025(15) 0.0087(16) -0.0110(17) C6 0.063(3) 0.0279(18) 0.040(2) 0.0033(16) 0.0054(18) 0.0026(17) C7 0.051(2) 0.0366(19) 0.038(2) -0.0015(15) 0.0098(17) 0.0097(16) C8 0.0387(17) 0.0360(18) 0.0273(16) 0.0012(14) 0.0087(13) 0.0025(14) C9 0.0345(17) 0.042(2) 0.0339(17) 0.0012(15) 0.0108(13) 0.0037(15) C10 0.0369(19) 0.066(3) 0.044(2) 0.0019(19) 0.0160(16) 0.0063(18) C11 0.035(2) 0.084(3) 0.047(2) 0.003(2) 0.0191(17) -0.008(2) C12 0.056(3) 0.057(3) 0.058(3) -0.002(2) 0.017(2) 0.018(2) C13 0.071(3) 0.051(3) 0.065(3) 0.006(2) 0.028(2) -0.023(2) Pt1 0.03332(9) 0.02547(8) 0.02964(9) 0.00085(5) 0.01011(6) -0.00280(4) O1 0.113(3) 0.053(2) 0.147(4) -0.012(2) 0.084(3) -0.025(2) O2 0.097(3) 0.186(6) 0.075(3) 0.034(3) 0.022(3) 0.024(3) O3 0.058(2) 0.092(3) 0.144(4) -0.008(3) 0.056(2) -0.008(2) O4 0.127(3) 0.072(2) 0.106(3) -0.036(2) 0.076(3) -0.037(2) N1 0.0318(16) 0.056(2) 0.0400(17) -0.0062(14) 0.0129(13) 0.0056(13) N2 0.0351(15) 0.0346(15) 0.0351(15) -0.0017(12) 0.0126(12) -0.0014(12) N3 0.0363(14) 0.0288(14) 0.0295(13) 0.0009(11) 0.0107(11) -0.0015(11) N4 0.0350(15) 0.0404(16) 0.0344(16) 0.0039(12) 0.0129(12) -0.0091(12) N5 0.0382(17) 0.0520(19) 0.0390(17) 0.0067(15) 0.0134(13) -0.0134(15) Cl1 0.0756(7) 0.0265(4) 0.0704(7) 0.0051(4) 0.0282(5) 0.0011(4) Cl2 0.0464(5) 0.0454(5) 0.0588(6) -0.0018(4) 0.0277(5) -0.0093(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.340(5) . ? C1 C2 1.370(6) . ? C1 H1 0.9300 . ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C3 N2 1.354(5) . ? C3 C4 1.457(5) . ? C4 N3 1.349(4) . ? C4 C5 1.389(5) . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 C7 1.372(6) . ? C6 H6 0.9300 . ? C7 C8 1.383(5) . ? C7 H7 0.9300 . ? C8 N3 1.347(4) . ? C8 C9 1.460(5) . ? C9 N4 1.352(5) . ? C9 C10 1.384(5) . ? C10 C11 1.359(6) . ? C10 H10 0.9300 . ? C11 N5 1.339(6) . ? C11 H11 0.9300 . ? C12 N1 1.453(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N5 1.455(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Pt1 N3 1.969(3) . ? Pt1 N2 2.015(3) . ? Pt1 N4 2.017(3) . ? Pt1 Cl1 2.2870(11) . ? O1 Cl2 1.421(3) . ? O2 Cl2 1.407(5) . ? O3 Cl2 1.414(4) . ? O4 Cl2 1.436(4) . ? N1 N2 1.355(4) . ? N4 N5 1.355(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.3(3) . . ? N1 C1 H1 125.3 . . ? C2 C1 H1 125.3 . . ? C1 C2 C3 104.7(4) . . ? C1 C2 H2 127.6 . . ? C3 C2 H2 127.6 . . ? N2 C3 C2 110.2(3) . . ? N2 C3 C4 115.4(3) . . ? C2 C3 C4 134.4(4) . . ? N3 C4 C5 119.2(3) . . ? N3 C4 C3 112.2(3) . . ? C5 C4 C3 128.5(3) . . ? C6 C5 C4 118.6(4) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 119.1(4) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? N3 C8 C7 119.5(3) . . ? N3 C8 C9 111.4(3) . . ? C7 C8 C9 129.1(3) . . ? N4 C9 C10 110.1(3) . . ? N4 C9 C8 115.7(3) . . ? C10 C9 C8 134.2(4) . . ? C11 C10 C9 105.2(4) . . ? C11 C10 H10 127.4 . . ? C9 C10 H10 127.4 . . ? N5 C11 C10 109.1(4) . . ? N5 C11 H11 125.5 . . ? C10 C11 H11 125.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 Pt1 N2 79.56(11) . . ? N3 Pt1 N4 79.03(12) . . ? N2 Pt1 N4 158.56(13) . . ? N3 Pt1 Cl1 179.51(8) . . ? N2 Pt1 Cl1 100.04(9) . . ? N4 Pt1 Cl1 101.38(9) . . ? C1 N1 N2 109.5(3) . . ? C1 N1 C12 126.4(4) . . ? N2 N1 C12 124.0(3) . . ? C3 N2 N1 106.2(3) . . ? C3 N2 Pt1 114.5(2) . . ? N1 N2 Pt1 139.2(2) . . ? C8 N3 C4 122.7(3) . . ? C8 N3 Pt1 119.1(2) . . ? C4 N3 Pt1 118.1(2) . . ? C9 N4 N5 105.9(3) . . ? C9 N4 Pt1 114.8(2) . . ? N5 N4 Pt1 139.2(3) . . ? C11 N5 N4 109.7(3) . . ? C11 N5 C13 127.3(3) . . ? N4 N5 C13 122.9(3) . . ? O2 Cl2 O3 109.7(3) . . ? O2 Cl2 O1 112.1(3) . . ? O3 Cl2 O1 110.4(3) . . ? O2 Cl2 O4 108.1(3) . . ? O3 Cl2 O4 109.0(3) . . ? O1 Cl2 O4 107.5(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.545 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.196 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 793196' #TrackingRef 'MicroPt2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H9 Cl N5 Pt, C2 H6 O S, 2 (H2 O), Cl' _chemical_formula_sum 'C13 H19 Cl2 N5 O3 Pt S' _chemical_formula_weight 591.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 9.4740(3) _cell_length_b 7.1809(2) _cell_length_c 27.9371(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.9400(10) _cell_angle_gamma 90.00 _cell_volume 1899.52(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 4 _cell_measurement_theta_max 80 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 17.648 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 15256 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 65.86 _reflns_number_total 3123 _reflns_number_gt 2986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+22.4193P] 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 3123 _refine_ls_number_parameters 228 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 5.739 _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 0.36433(19) 0.2325(3) 0.48030(6) 0.0278(9) Uani 1 1 d . . . Cl1 Cl 0.1333(12) 0.1969(18) 0.4536(4) 0.039(3) Uani 1 1 d . . . Cl2 Cl 0.2806(13) 0.5788(19) 0.2470(4) 0.046(3) Uani 1 1 d . . . N1 N 0.348(4) 0.148(5) 0.5490(12) 0.029(8) Uani 1 1 d . . . N2 N 0.454(4) 0.100(5) 0.6182(13) 0.037(9) Uani 1 1 d . . . H1N H 0.5202 0.0943 0.6411 0.044 Uiso 1 1 calc R . . N3 N 0.559(4) 0.266(5) 0.5037(14) 0.032(9) Uani 1 1 d . . . N4 N 0.450(4) 0.328(5) 0.4199(12) 0.029(8) Uani 1 1 d . . . N5 N 0.641(4) 0.428(5) 0.3859(12) 0.032(8) Uani 1 1 d . . . H2N H 0.7288 0.4614 0.3818 0.039 Uiso 1 1 calc R . . C1 C 0.250(5) 0.081(7) 0.5792(16) 0.038(11) Uani 1 1 d . . . H1A H 0.1525 0.0594 0.5714 0.045 Uiso 1 1 calc R . . C2 C 0.316(6) 0.051(7) 0.6224(17) 0.043(12) Uani 1 1 d . . . H2A H 0.2733 0.0041 0.6503 0.052 Uiso 1 1 calc R . . C3 C 0.471(5) 0.157(7) 0.5738(15) 0.033(10) Uani 1 1 d . . . C4 C 0.593(5) 0.222(6) 0.5491(16) 0.033(10) Uani 1 1 d . . . C5 C 0.733(5) 0.241(6) 0.5662(17) 0.034(11) Uani 1 1 d . . . H5A H 0.7587 0.2090 0.5983 0.040 Uiso 1 1 calc R . . C6 C 0.833(5) 0.306(7) 0.5355(17) 0.036(11) Uani 1 1 d . . . H6A H 0.9279 0.3223 0.5469 0.043 Uiso 1 1 calc R . . C7 C 0.797(5) 0.349(6) 0.4876(16) 0.032(10) Uani 1 1 d . . . H7A H 0.8658 0.3910 0.4662 0.038 Uiso 1 1 calc R . . C8 C 0.658(4) 0.327(6) 0.4728(15) 0.027(9) Uani 1 1 d . . . C9 C 0.588(4) 0.362(6) 0.4259(14) 0.028(9) Uani 1 1 d . . . C10 C 0.532(5) 0.434(7) 0.3520(15) 0.035(10) Uani 1 1 d . . . H10A H 0.5378 0.4744 0.3197 0.042 Uiso 1 1 calc R . . C11 C 0.414(5) 0.373(7) 0.3733(15) 0.034(10) Uani 1 1 d . . . H11A H 0.3221 0.3633 0.3586 0.041 Uiso 1 1 calc R . . O1W O 0.393(4) 1.169(6) 0.2508(12) 0.046(8) Uani 1 1 d D . . H1WA H 0.3858 1.2848 0.2534 0.069 Uiso 1 1 calc RD . . H1WB H 0.4823 1.1901 0.2484 0.069 Uiso 1 1 d RD . . O2W O 0.322(4) 0.915(5) 0.3178(12) 0.051(9) Uani 1 1 d D . . H2WA H 0.2909 1.0067 0.3022 0.076 Uiso 1 1 calc RD . . H2WB H 0.3078 0.8081 0.3045 0.076 Uiso 1 1 d RD . . S1 S 1.0176(12) -0.025(2) 0.8475(4) 0.047(3) Uani 1 1 d . . . C12 C 0.936(8) -0.121(17) 0.796(3) 0.11(4) Uani 1 1 d . . . H12A H 0.9308 -0.2563 0.7989 0.171 Uiso 1 1 calc R . . H12B H 0.9906 -0.0887 0.7677 0.171 Uiso 1 1 calc R . . H12C H 0.8400 -0.0699 0.7915 0.171 Uiso 1 1 calc R . . C13 C 1.027(7) 0.214(10) 0.827(2) 0.07(2) Uani 1 1 d . . . H13A H 1.0605 0.2933 0.8541 0.102 Uiso 1 1 calc R . . H13B H 0.9334 0.2556 0.8161 0.102 Uiso 1 1 calc R . . H13C H 1.0931 0.2231 0.8012 0.102 Uiso 1 1 calc R . . O1 O 0.908(3) -0.031(6) 0.8850(12) 0.050(10) 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 0.0311(13) 0.0244(13) 0.0282(12) -0.0017(7) 0.0015(8) 0.0051(7) Cl1 0.028(5) 0.040(6) 0.049(6) -0.001(5) -0.001(4) 0.003(5) Cl2 0.040(6) 0.053(8) 0.044(6) -0.008(6) 0.000(5) 0.003(6) N1 0.04(2) 0.013(17) 0.031(18) 0.007(15) 0.004(15) 0.006(16) N2 0.05(2) 0.03(2) 0.031(19) -0.002(17) 0.002(16) 0.004(19) N3 0.04(2) 0.03(2) 0.027(19) -0.006(15) 0.000(16) 0.011(17) N4 0.032(19) 0.026(19) 0.029(18) -0.007(16) 0.003(14) 0.002(17) N5 0.027(18) 0.04(2) 0.032(18) -0.003(17) 0.002(14) 0.005(17) C1 0.05(3) 0.03(3) 0.03(2) 0.00(2) 0.01(2) 0.01(2) C2 0.06(3) 0.03(3) 0.04(3) 0.01(2) 0.02(2) 0.01(2) C3 0.04(2) 0.03(3) 0.03(2) -0.01(2) -0.003(18) 0.00(2) C4 0.04(3) 0.03(2) 0.03(2) -0.005(18) 0.01(2) 0.01(2) C5 0.04(3) 0.03(3) 0.03(2) -0.001(18) -0.006(19) 0.01(2) C6 0.04(3) 0.02(2) 0.04(3) -0.01(2) -0.01(2) 0.02(2) C7 0.03(2) 0.03(2) 0.04(2) 0.00(2) -0.005(18) 0.00(2) C8 0.03(2) 0.02(2) 0.03(2) -0.008(19) 0.000(17) 0.003(19) C9 0.03(2) 0.02(2) 0.03(2) -0.002(18) -0.001(17) 0.002(19) C10 0.04(3) 0.04(3) 0.03(2) 0.00(2) -0.003(18) 0.01(2) C11 0.04(2) 0.03(3) 0.03(2) -0.01(2) -0.004(18) 0.00(2) O1W 0.041(19) 0.05(2) 0.05(2) -0.004(18) -0.002(15) -0.005(18) O2W 0.07(2) 0.04(2) 0.039(18) -0.006(16) -0.001(16) 0.004(19) S1 0.030(6) 0.071(10) 0.041(6) -0.001(6) 0.000(5) -0.002(6) C12 0.06(4) 0.22(12) 0.06(4) -0.06(6) 0.02(3) -0.04(6) C13 0.05(3) 0.10(6) 0.06(4) 0.02(4) 0.01(3) 0.01(4) O1 0.034(18) 0.08(3) 0.042(18) 0.000(19) 0.002(14) -0.002(19) _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 N3 1.95(4) . ? Pt1 N4 2.02(4) . ? Pt1 N1 2.02(3) . ? Pt1 Cl1 2.303(11) . ? N1 C3 1.34(6) . ? N1 C1 1.36(6) . ? N2 C3 1.32(6) . ? N2 C2 1.37(7) . ? N3 C4 1.34(6) . ? N3 C8 1.36(6) . ? N4 C9 1.34(6) . ? N4 C11 1.37(6) . ? N5 C9 1.33(5) . ? N5 C10 1.38(5) . ? C1 C2 1.36(7) . ? C3 C4 1.45(7) . ? C4 C5 1.40(7) . ? C5 C6 1.38(7) . ? C6 C7 1.40(6) . ? C7 C8 1.38(6) . ? C8 C9 1.47(6) . ? C10 C11 1.36(7) . ? S1 O1 1.50(3) . ? S1 C12 1.76(7) . ? S1 C13 1.81(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pt1 N4 80.5(15) . . ? N3 Pt1 N1 79.8(16) . . ? N4 Pt1 N1 160.3(15) . . ? N3 Pt1 Cl1 179.1(11) . . ? N4 Pt1 Cl1 99.9(11) . . ? N1 Pt1 Cl1 99.8(11) . . ? C3 N1 C1 107(4) . . ? C3 N1 Pt1 112(3) . . ? C1 N1 Pt1 140(3) . . ? C3 N2 C2 108(4) . . ? C4 N3 C8 122(4) . . ? C4 N3 Pt1 119(3) . . ? C8 N3 Pt1 119(3) . . ? C9 N4 C11 107(4) . . ? C9 N4 Pt1 112(3) . . ? C11 N4 Pt1 141(3) . . ? C9 N5 C10 107(4) . . ? C2 C1 N1 108(5) . . ? C1 C2 N2 107(4) . . ? N2 C3 N1 110(4) . . ? N2 C3 C4 132(4) . . ? N1 C3 C4 118(4) . . ? N3 C4 C5 120(4) . . ? N3 C4 C3 111(4) . . ? C5 C4 C3 129(4) . . ? C6 C5 C4 119(4) . . ? C5 C6 C7 121(4) . . ? C8 C7 C6 118(4) . . ? N3 C8 C7 121(4) . . ? N3 C8 C9 109(4) . . ? C7 C8 C9 130(4) . . ? N5 C9 N4 111(4) . . ? N5 C9 C8 130(4) . . ? N4 C9 C8 119(4) . . ? C11 C10 N5 107(4) . . ? C10 C11 N4 108(4) . . ? O1 S1 C12 106(3) . . ? O1 S1 C13 107(3) . . ? C12 S1 C13 98(5) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 65.86 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 3.032 _refine_diff_density_min -1.750 _refine_diff_density_rms 0.205 #===END