Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'L. Canovese' 'F. Visentin' 'G. Chessa' 'C. Santo' 'P. Uguagliati' 'L. Maini' 'M. Polito' _publ_contact_author_name 'Prof Luciano Canovese' _publ_contact_author_address ; Dipartimento di Chimica Universita di Venezia Calle Larga Santa Marta 2137 Venice 30123 ITALY ; _publ_contact_author_email 'CANO@UNIVE.IT' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The mechanism of olefin exchange in platinum (0) pyridyl-methanimine and pyridyl-thioether complexes. A kinetic study. ; data_venice1 _database_code_CSD 183322 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 N4 Pt' _chemical_formula_weight 435.40 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' '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 P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.338(2) _cell_length_b 8.706(2) _cell_length_c 18.463(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.046(17) _cell_angle_gamma 90.00 _cell_volume 1492.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 9.392 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _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 2700 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2618 _reflns_number_gt 1495 _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^)+(0.0538P)^2^+3.4100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2618 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.19677(6) 0.11160(6) 0.22724(3) 0.03909(19) Uani 1 1 d . . . N1 N 0.2967(12) -0.0618(14) 0.1711(6) 0.044(3) Uani 1 1 d . . . N2 N 0.2782(12) -0.0394(13) 0.3129(7) 0.039(3) Uani 1 1 d . . . N3 N -0.0914(18) 0.1968(19) 0.0679(8) 0.073(5) Uani 1 1 d . . . N4 N 0.1863(19) 0.5206(19) 0.3211(10) 0.091(5) Uani 1 1 d . . . C1 C 0.3541(16) -0.1772(17) 0.2144(9) 0.048(4) Uani 1 1 d . . . C2 C 0.4169(18) -0.302(2) 0.1835(11) 0.072(5) Uani 1 1 d . . . H2A H 0.4530 -0.3835 0.2123 0.086 Uiso 1 1 calc R . . C3 C 0.425(2) -0.302(2) 0.1096(11) 0.079(6) Uani 1 1 d . . . H3A H 0.4708 -0.3830 0.0884 0.095 Uiso 1 1 calc R . . C4 C 0.368(2) -0.188(2) 0.0681(11) 0.075(6) Uani 1 1 d . . . H4A H 0.3747 -0.1886 0.0183 0.090 Uiso 1 1 calc R . . C5 C 0.2992(16) -0.0700(18) 0.0983(8) 0.053(4) Uani 1 1 d . . . H5A H 0.2537 0.0054 0.0685 0.063 Uiso 1 1 calc R . . C6 C 0.3410(17) -0.1564(17) 0.2928(9) 0.055(4) Uani 1 1 d . . . H6A H 0.3786 -0.2289 0.3266 0.066 Uiso 1 1 calc R . . C7 C 0.2623(18) -0.0104(19) 0.3896(10) 0.059(5) Uani 1 1 d . . . C8 C 0.1078(18) 0.000(3) 0.4000(12) 0.103(8) Uani 1 1 d . . . H8A H 0.0621 -0.0969 0.3879 0.154 Uiso 1 1 calc R . . H8B H 0.0633 0.0786 0.3690 0.154 Uiso 1 1 calc R . . H8C H 0.0978 0.0245 0.4499 0.154 Uiso 1 1 calc R . . C9 C 0.333(2) -0.138(2) 0.4383(10) 0.095(7) Uani 1 1 d . . . H9A H 0.2840 -0.2332 0.4269 0.142 Uiso 1 1 calc R . . H9B H 0.3262 -0.1125 0.4884 0.142 Uiso 1 1 calc R . . H9C H 0.4322 -0.1475 0.4301 0.142 Uiso 1 1 calc R . . C10 C 0.3408(19) 0.141(2) 0.4083(10) 0.076(5) Uani 1 1 d . . . H10A H 0.2973 0.2215 0.3779 0.114 Uiso 1 1 calc R . . H10B H 0.4403 0.1309 0.4002 0.114 Uiso 1 1 calc R . . H10C H 0.3340 0.1660 0.4585 0.114 Uiso 1 1 calc R . . C11 C -0.0079(18) 0.2382(19) 0.1110(10) 0.054(4) Uani 1 1 d . . . C12 C 0.1041(17) 0.2831(18) 0.1666(8) 0.053(4) Uani 1 1 d . . . H12A H 0.1721 0.3583 0.1505 0.064 Uiso 1 1 calc R . . C13 C 0.0768(15) 0.2996(18) 0.2410(9) 0.051(4) Uani 1 1 d . . . H13A H -0.0227 0.2763 0.2496 0.061 Uiso 1 1 calc R . . C14 C 0.1414(19) 0.4252(18) 0.2863(11) 0.059(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 0.0388(3) 0.0392(3) 0.0394(3) 0.0004(4) 0.0046(2) 0.0011(4) N1 0.048(7) 0.055(8) 0.025(7) -0.020(6) -0.015(6) -0.011(6) N2 0.041(7) 0.033(6) 0.040(8) -0.002(6) -0.010(6) -0.005(6) N3 0.086(11) 0.099(12) 0.034(9) -0.004(9) -0.002(8) 0.024(10) N4 0.105(14) 0.064(11) 0.100(15) -0.017(10) -0.005(11) -0.013(10) C1 0.051(9) 0.040(8) 0.053(11) 0.013(8) 0.007(8) 0.001(7) C2 0.066(11) 0.063(11) 0.083(16) -0.021(11) -0.008(10) 0.018(10) C3 0.098(15) 0.079(14) 0.061(14) -0.041(12) 0.010(11) 0.021(12) C4 0.081(13) 0.079(13) 0.064(14) -0.038(12) 0.003(11) 0.011(11) C5 0.055(9) 0.071(12) 0.030(9) 0.001(8) -0.009(7) 0.017(8) C6 0.066(11) 0.037(8) 0.060(13) 0.017(8) -0.002(9) -0.008(8) C7 0.070(11) 0.051(10) 0.057(12) 0.005(9) 0.017(9) -0.021(9) C8 0.060(12) 0.17(2) 0.078(16) 0.028(16) 0.013(11) -0.017(14) C9 0.15(2) 0.089(16) 0.043(12) 0.000(11) 0.005(12) -0.014(15) C10 0.081(12) 0.080(14) 0.066(13) -0.022(11) 0.007(10) -0.009(11) C11 0.056(10) 0.052(10) 0.052(12) 0.027(9) 0.002(9) 0.021(9) C12 0.061(10) 0.066(11) 0.036(10) 0.010(8) 0.015(8) 0.017(9) C13 0.033(7) 0.063(10) 0.058(11) 0.011(9) 0.013(7) 0.008(7) C14 0.070(11) 0.040(10) 0.067(13) -0.009(9) 0.006(10) -0.004(8) _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 C12 2.007(15) . ? Pt1 C13 2.014(14) . ? Pt1 N1 2.105(11) . ? Pt1 N2 2.134(12) . ? N1 C5 1.348(18) . ? N1 C1 1.359(18) . ? N2 C6 1.251(18) . ? N2 C7 1.46(2) . ? N3 C11 1.11(2) . ? N4 C14 1.11(2) . ? C1 C2 1.38(2) . ? C1 C6 1.48(2) . ? C2 C3 1.38(2) . ? C3 C4 1.33(3) . ? C4 C5 1.36(2) . ? C7 C8 1.48(2) . ? C7 C9 1.53(2) . ? C7 C10 1.53(2) . ? C11 C12 1.44(2) . ? C12 C13 1.43(2) . ? C13 C14 1.47(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Pt1 C13 41.7(6) . . ? C12 Pt1 N1 116.5(5) . . ? C13 Pt1 N1 157.9(6) . . ? C12 Pt1 N2 166.1(5) . . ? C13 Pt1 N2 124.5(6) . . ? N1 Pt1 N2 77.4(5) . . ? C5 N1 C1 120.1(13) . . ? C5 N1 Pt1 125.7(10) . . ? C1 N1 Pt1 114.0(10) . . ? C6 N2 C7 121.8(14) . . ? C6 N2 Pt1 115.1(11) . . ? C7 N2 Pt1 123.2(10) . . ? N1 C1 C2 119.6(16) . . ? N1 C1 C6 114.8(13) . . ? C2 C1 C6 125.6(15) . . ? C3 C2 C1 118.9(18) . . ? C4 C3 C2 120.4(17) . . ? C3 C4 C5 120.4(18) . . ? N1 C5 C4 120.4(16) . . ? N2 C6 C1 118.7(14) . . ? N2 C7 C8 109.7(15) . . ? N2 C7 C9 111.3(14) . . ? C8 C7 C9 109.4(16) . . ? N2 C7 C10 105.8(12) . . ? C8 C7 C10 111.7(17) . . ? C9 C7 C10 109.0(15) . . ? N3 C11 C12 176.6(18) . . ? C13 C12 C11 121.5(14) . . ? C13 C12 Pt1 69.4(9) . . ? C11 C12 Pt1 115.7(11) . . ? C12 C13 C14 121.2(15) . . ? C12 C13 Pt1 68.9(9) . . ? C14 C13 Pt1 118.4(10) . . ? N4 C14 C13 178(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.300 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.222 data_venice2 _database_code_CSD 183323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 N2 O3 Pt' _chemical_formula_weight 455.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' '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 P21/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 8.362(3) _cell_length_b 10.045(3) _cell_length_c 16.811(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.47(2) _cell_angle_gamma 90.00 _cell_volume 1409.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 9.963 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _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 3812 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2465 _reflns_number_gt 1742 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2465 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 0.66694(3) 0.55976(3) 0.105505(15) 0.03385(11) Uani 1 1 d . . . C1 C 0.7547(10) 0.3765(10) -0.0294(5) 0.051(2) Uani 1 1 d . . . H1A H 0.7069 0.3095 -0.0009 0.061 Uiso 1 1 calc R . . C2 C 0.8257(10) 0.3445(10) -0.0993(5) 0.056(2) Uani 1 1 d . . . H2A H 0.8247 0.2569 -0.1172 0.067 Uiso 1 1 calc R . . C3 C 0.8963(10) 0.4403(10) -0.1417(4) 0.051(2) Uani 1 1 d . . . H3A H 0.9443 0.4196 -0.1886 0.061 Uiso 1 1 calc R . . C4 C 0.8954(10) 0.5685(9) -0.1137(4) 0.047(2) Uani 1 1 d . . . H4A H 0.9434 0.6363 -0.1415 0.056 Uiso 1 1 calc R . . C5 C 0.8223(9) 0.5962(8) -0.0436(4) 0.0373(18) Uani 1 1 d . . . C6 C 0.8131(9) 0.7275(7) -0.0091(4) 0.0381(18) Uani 1 1 d . . . H6A H 0.8520 0.8017 -0.0347 0.046 Uiso 1 1 calc R . . C7 C 0.7305(9) 0.8720(7) 0.0953(4) 0.0373(18) Uani 1 1 d . . . C8 C 0.8090(11) 0.9830(9) 0.0522(5) 0.059(2) Uani 1 1 d . . . H8A H 0.9227 0.9689 0.0543 0.088 Uiso 1 1 calc R . . H8B H 0.7863 1.0663 0.0771 0.088 Uiso 1 1 calc R . . H8C H 0.7680 0.9847 -0.0024 0.088 Uiso 1 1 calc R . . C9 C 0.5493(10) 0.8954(9) 0.0932(5) 0.052(2) Uani 1 1 d . . . H9A H 0.5081 0.9041 0.0389 0.079 Uiso 1 1 calc R . . H9B H 0.5277 0.9755 0.1218 0.079 Uiso 1 1 calc R . . H9C H 0.4985 0.8214 0.1175 0.079 Uiso 1 1 calc R . . C10 C 0.7983(11) 0.8620(8) 0.1805(4) 0.054(2) Uani 1 1 d . . . H10A H 0.9123 0.8503 0.1811 0.081 Uiso 1 1 calc R . . H10B H 0.7512 0.7873 0.2059 0.081 Uiso 1 1 calc R . . H10C H 0.7745 0.9421 0.2085 0.081 Uiso 1 1 calc R . . N1 N 0.7534(7) 0.4994(7) -0.0023(3) 0.0364(14) Uani 1 1 d . . . N2 N 0.7499(6) 0.7383(6) 0.0576(3) 0.0292(13) Uani 1 1 d . . . C11 C 0.7032(10) 0.3454(9) 0.2112(5) 0.050(2) Uani 1 1 d . . . C12 C 0.5707(9) 0.4192(8) 0.1738(4) 0.045(2) Uani 1 1 d . . . H12A H 0.4701 0.3748 0.1567 0.055 Uiso 1 1 calc R . . C13 C 0.5708(10) 0.5458(8) 0.2152(4) 0.0427(19) Uani 1 1 d . . . H13A H 0.4696 0.5905 0.2250 0.051 Uiso 1 1 calc R . . C14 C 0.6996(10) 0.5444(9) 0.2753(5) 0.046(2) Uani 1 1 d . . . O1 O 0.7527(8) 0.2349(7) 0.1998(4) 0.0737(19) Uani 1 1 d . . . O2 O 0.7836(7) 0.4227(6) 0.2696(3) 0.0539(15) Uani 1 1 d . . . O3 O 0.7441(9) 0.6199(7) 0.3268(3) 0.077(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 Pt1 0.03387(16) 0.03414(17) 0.03355(14) 0.00204(16) 0.00209(10) -0.00065(17) C1 0.050(5) 0.051(6) 0.052(5) -0.009(4) -0.001(4) -0.006(4) C2 0.055(5) 0.062(6) 0.050(5) -0.028(5) -0.007(4) 0.009(5) C3 0.051(5) 0.065(6) 0.036(4) -0.008(5) 0.001(3) 0.014(5) C4 0.051(5) 0.054(6) 0.036(4) -0.001(4) 0.006(3) 0.005(5) C5 0.039(4) 0.042(5) 0.030(3) 0.001(3) 0.000(3) 0.011(4) C6 0.043(4) 0.034(5) 0.037(4) 0.010(3) 0.000(3) 0.003(4) C7 0.041(4) 0.030(4) 0.041(4) 0.000(3) 0.006(3) 0.005(3) C8 0.070(6) 0.036(5) 0.074(6) -0.005(4) 0.029(5) -0.006(4) C9 0.045(5) 0.043(5) 0.071(5) 0.009(4) 0.016(4) 0.012(4) C10 0.070(6) 0.046(6) 0.045(4) -0.008(4) 0.001(4) -0.002(5) N1 0.034(4) 0.037(4) 0.037(3) -0.007(3) -0.003(3) -0.001(3) N2 0.033(3) 0.030(3) 0.025(3) 0.004(2) 0.001(2) 0.002(3) C11 0.059(6) 0.046(6) 0.048(5) 0.011(4) 0.021(4) -0.002(5) C12 0.042(4) 0.043(6) 0.051(4) 0.013(4) 0.004(3) -0.007(4) C13 0.051(5) 0.037(5) 0.042(4) 0.006(4) 0.020(3) 0.004(4) C14 0.051(5) 0.041(5) 0.049(4) 0.006(4) 0.017(4) -0.016(4) O1 0.092(5) 0.049(4) 0.082(4) 0.011(3) 0.012(4) 0.020(4) O2 0.060(4) 0.058(4) 0.043(3) 0.011(3) -0.004(2) -0.002(3) O3 0.107(6) 0.078(5) 0.044(3) -0.008(3) -0.001(3) -0.032(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 Pt1 C12 2.018(7) . ? Pt1 C13 2.061(6) . ? Pt1 N1 2.082(6) . ? Pt1 N2 2.101(5) . ? C1 N1 1.316(11) . ? C1 C2 1.386(11) . ? C2 C3 1.354(12) . ? C3 C4 1.371(12) . ? C4 C5 1.388(10) . ? C5 N1 1.345(10) . ? C5 C6 1.445(10) . ? C6 N2 1.272(8) . ? C7 C8 1.502(11) . ? C7 N2 1.497(9) . ? C7 C10 1.511(9) . ? C7 C9 1.532(11) . ? C11 O1 1.204(10) . ? C11 O2 1.393(10) . ? C11 C12 1.445(11) . ? C12 C13 1.449(11) . ? C13 C14 1.431(11) . ? C14 O3 1.194(9) . ? C14 O2 1.416(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Pt1 C13 41.6(3) . . ? C12 Pt1 N1 117.6(3) . . ? C13 Pt1 N1 159.1(3) . . ? C12 Pt1 N2 165.4(3) . . ? C13 Pt1 N2 123.8(3) . . ? N1 Pt1 N2 77.0(2) . . ? N1 C1 C2 121.6(9) . . ? C3 C2 C1 120.3(8) . . ? C2 C3 C4 118.4(7) . . ? C3 C4 C5 119.4(8) . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C6 114.6(6) . . ? C4 C5 C6 124.1(7) . . ? N2 C6 C5 117.9(6) . . ? C8 C7 N2 113.6(6) . . ? C8 C7 C10 110.9(7) . . ? N2 C7 C10 107.3(6) . . ? C8 C7 C9 109.6(7) . . ? N2 C7 C9 105.1(6) . . ? C10 C7 C9 110.2(6) . . ? C1 N1 C5 119.1(6) . . ? C1 N1 Pt1 125.8(6) . . ? C5 N1 Pt1 114.9(5) . . ? C6 N2 C7 120.7(6) . . ? C6 N2 Pt1 115.4(5) . . ? C7 N2 Pt1 123.8(4) . . ? O1 C11 O2 118.0(8) . . ? O1 C11 C12 131.7(9) . . ? O2 C11 C12 110.2(7) . . ? C11 C12 C13 105.3(7) . . ? C11 C12 Pt1 106.6(5) . . ? C13 C12 Pt1 70.8(4) . . ? C14 C13 C12 107.9(7) . . ? C14 C13 Pt1 108.3(5) . . ? C12 C13 Pt1 67.6(4) . . ? O3 C14 O2 117.6(8) . . ? O3 C14 C13 133.9(9) . . ? O2 C14 C13 108.5(7) . . ? C11 O2 C14 107.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.881 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.151 data_VENICE3 _database_code_CSD 183324 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 N2 O4 Pt1' _chemical_formula_weight 501.45 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.969(3) _cell_length_b 12.776(4) _cell_length_c 15.380(4) _cell_angle_alpha 92.92(3) _cell_angle_beta 95.15(2) _cell_angle_gamma 94.92(3) _cell_volume 1745.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 8.058 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _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 6369 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6122 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6122 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 0.20440(4) 0.63800(3) 0.43644(2) 0.03348(11) Uani 1 1 d . . . Pt2 Pt -0.47571(4) 0.14264(3) 0.13339(2) 0.03399(11) Uani 1 1 d . . . N1 N 0.2815(8) 0.4926(5) 0.4662(5) 0.0344(18) Uani 1 1 d . . . N2 N 0.1651(7) 0.6276(5) 0.5689(4) 0.0348(16) Uani 1 1 d . . . N3 N -0.3990(8) -0.0009(6) 0.1657(5) 0.0377(19) Uani 1 1 d . . . N4 N -0.3127(7) 0.1202(5) 0.0438(4) 0.0347(16) Uani 1 1 d . . . C1 C 0.3554(9) 0.4320(7) 0.4148(6) 0.039(2) Uani 1 1 d . . . H1A H 0.3652 0.4498 0.3576 0.047 Uiso 1 1 calc R . . C2 C 0.4175(10) 0.3439(7) 0.4443(7) 0.048(3) Uani 1 1 d . . . H2A H 0.4680 0.3029 0.4070 0.058 Uiso 1 1 calc R . . C3 C 0.4049(11) 0.3164(8) 0.5284(7) 0.050(3) Uani 1 1 d . . . H3A H 0.4485 0.2581 0.5494 0.060 Uiso 1 1 calc R . . C4 C 0.3262(10) 0.3773(7) 0.5809(7) 0.049(3) Uani 1 1 d . . . H4A H 0.3131 0.3590 0.6377 0.059 Uiso 1 1 calc R . . C5 C 0.2665(9) 0.4656(7) 0.5495(6) 0.037(2) Uani 1 1 d . . . C6 C 0.1979(10) 0.5422(7) 0.6020(6) 0.041(2) Uani 1 1 d . . . H6A H 0.1781 0.5291 0.6590 0.050 Uiso 1 1 calc R . . C7 C 0.1111(10) 0.7129(7) 0.6243(6) 0.041(2) Uani 1 1 d . . . C8 C -0.0175(9) 0.7572(8) 0.5717(6) 0.047(2) Uani 1 1 d . . . H8A H 0.0168 0.7834 0.5189 0.070 Uiso 1 1 calc R . . H8B H -0.0530 0.8135 0.6056 0.070 Uiso 1 1 calc R . . H8C H -0.0978 0.7027 0.5573 0.070 Uiso 1 1 calc R . . C9 C 0.2426(11) 0.7964(8) 0.6403(7) 0.059(3) Uani 1 1 d . . . H9A H 0.2707 0.8201 0.5854 0.088 Uiso 1 1 calc R . . H9B H 0.3262 0.7672 0.6707 0.088 Uiso 1 1 calc R . . H9C H 0.2143 0.8546 0.6751 0.088 Uiso 1 1 calc R . . C10 C 0.0617(14) 0.6744(10) 0.7099(7) 0.074(4) Uani 1 1 d . . . H10A H 0.1455 0.6490 0.7432 0.111 Uiso 1 1 calc R . . H10B H -0.0172 0.6185 0.6980 0.111 Uiso 1 1 calc R . . H10C H 0.0256 0.7314 0.7427 0.111 Uiso 1 1 calc R . . C11 C 0.1124(14) 0.4916(10) 0.1332(7) 0.079(4) Uani 1 1 d . . . H11A H 0.1801 0.4511 0.1036 0.118 Uiso 1 1 calc R . . H11B H 0.0586 0.5318 0.0919 0.118 Uiso 1 1 calc R . . H11C H 0.0423 0.4450 0.1597 0.118 Uiso 1 1 calc R . . C12 C 0.1156(12) 0.6227(7) 0.2465(6) 0.046(2) Uani 1 1 d . . . C13 C 0.2164(10) 0.6873(7) 0.3121(6) 0.045(2) Uani 1 1 d . . . H13A H 0.3181 0.7057 0.2957 0.054 Uiso 1 1 calc R . . C14 C 0.1565(11) 0.7663(7) 0.3685(5) 0.041(2) Uani 1 1 d . . . H14A H 0.0497 0.7762 0.3560 0.049 Uiso 1 1 calc R . . C15 C 0.2545(11) 0.8595(7) 0.4000(6) 0.043(2) Uani 1 1 d . . . C16 C 0.2659(14) 1.0253(8) 0.4807(8) 0.083(4) Uani 1 1 d . . . H16A H 0.2011 1.0699 0.5083 0.124 Uiso 1 1 calc R . . H16B H 0.3133 1.0623 0.4363 0.124 Uiso 1 1 calc R . . H16C H 0.3414 1.0056 0.5235 0.124 Uiso 1 1 calc R . . C17 C -0.4272(11) -0.0556(8) 0.2353(6) 0.049(3) Uani 1 1 d . . . H17A H -0.4937 -0.0309 0.2729 0.059 Uiso 1 1 calc R . . C18 C -0.3622(12) -0.1469(8) 0.2539(7) 0.062(3) Uani 1 1 d . . . H18A H -0.3803 -0.1809 0.3045 0.074 Uiso 1 1 calc R . . C19 C -0.2696(12) -0.1866(9) 0.1958(9) 0.066(3) Uani 1 1 d . . . H19A H -0.2261 -0.2489 0.2062 0.079 Uiso 1 1 calc R . . C20 C -0.2421(10) -0.1341(7) 0.1230(7) 0.049(3) Uani 1 1 d . . . H20A H -0.1812 -0.1608 0.0829 0.059 Uiso 1 1 calc R . . C21 C -0.3059(9) -0.0407(7) 0.1095(7) 0.043(2) Uani 1 1 d . . . C22 C -0.2678(9) 0.0285(7) 0.0427(6) 0.040(2) Uani 1 1 d . . . H22A H -0.2107 0.0064 -0.0011 0.049 Uiso 1 1 calc R . . C23 C -0.2550(9) 0.2012(7) -0.0135(5) 0.036(2) Uani 1 1 d . . . C24 C -0.1629(13) 0.1575(9) -0.0815(8) 0.071(3) Uani 1 1 d . . . H24A H -0.2250 0.1068 -0.1201 0.106 Uiso 1 1 calc R . . H24B H -0.0812 0.1242 -0.0534 0.106 Uiso 1 1 calc R . . H24C H -0.1237 0.2137 -0.1146 0.106 Uiso 1 1 calc R . . C25 C -0.3868(10) 0.2502(8) -0.0582(6) 0.049(2) Uani 1 1 d . . . H25A H -0.4453 0.1985 -0.0976 0.073 Uiso 1 1 calc R . . H25B H -0.3505 0.3081 -0.0903 0.073 Uiso 1 1 calc R . . H25C H -0.4483 0.2752 -0.0150 0.073 Uiso 1 1 calc R . . C26 C -0.1603(11) 0.2820(8) 0.0479(7) 0.060(3) Uani 1 1 d . . . H26A H -0.2208 0.3087 0.0909 0.090 Uiso 1 1 calc R . . H26B H -0.1220 0.3388 0.0153 0.090 Uiso 1 1 calc R . . H26C H -0.0779 0.2497 0.0765 0.090 Uiso 1 1 calc R . . C27 C -0.3952(14) 0.5314(8) 0.1276(8) 0.077(4) Uani 1 1 d . . . H27A H -0.3864 0.5728 0.0777 0.116 Uiso 1 1 calc R . . H27B H -0.2972 0.5154 0.1505 0.116 Uiso 1 1 calc R . . H27C H -0.4405 0.5703 0.1717 0.116 Uiso 1 1 calc R . . C28 C -0.5077(10) 0.3696(8) 0.1680(7) 0.042(2) Uani 1 1 d . . . C29 C -0.5964(10) 0.2717(7) 0.1355(6) 0.041(2) Uani 1 1 d . . . H29A H -0.6686 0.2770 0.0845 0.049 Uiso 1 1 calc R . . C30 C -0.6433(9) 0.1996(7) 0.1985(6) 0.039(2) Uani 1 1 d . . . H30A H -0.6141 0.2234 0.2597 0.047 Uiso 1 1 calc R . . C31 C -0.7876(10) 0.1331(8) 0.1827(6) 0.043(2) Uani 1 1 d . . . C32 C -0.9585(11) 0.0195(9) 0.2472(7) 0.065(3) Uani 1 1 d . . . H32A H -0.9724 -0.0109 0.3020 0.097 Uiso 1 1 calc R . . H32B H -0.9556 -0.0356 0.2026 0.097 Uiso 1 1 calc R . . H32C H -1.0403 0.0608 0.2318 0.097 Uiso 1 1 calc R . . O1 O -0.0169(8) 0.6224(6) 0.2342(5) 0.063(2) Uani 1 1 d . . . O2 O 0.1952(8) 0.5606(5) 0.1987(4) 0.0571(19) Uani 1 1 d . . . O3 O 0.3870(8) 0.8763(5) 0.3945(5) 0.0584(18) Uani 1 1 d . . . O4 O 0.1787(8) 0.9320(5) 0.4414(5) 0.0584(19) Uani 1 1 d . . . O5 O -0.4563(8) 0.3926(5) 0.2413(5) 0.0561(18) Uani 1 1 d . . . O6 O -0.4875(8) 0.4350(5) 0.1021(4) 0.0578(18) Uani 1 1 d . . . O7 O -0.8686(8) 0.1228(6) 0.1142(5) 0.062(2) Uani 1 1 d . . . O8 O -0.8202(7) 0.0852(5) 0.2549(4) 0.0527(17) 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 0.0360(2) 0.0320(2) 0.0319(2) 0.00269(17) 0.00101(17) 0.00202(18) Pt2 0.0318(2) 0.0355(2) 0.0353(2) 0.00127(18) 0.00558(17) 0.00464(18) N1 0.036(4) 0.027(4) 0.040(5) -0.002(4) 0.003(4) 0.004(3) N2 0.028(4) 0.037(4) 0.038(4) 0.000(3) -0.002(3) 0.004(3) N3 0.032(4) 0.037(5) 0.042(5) -0.006(4) -0.002(4) 0.000(4) N4 0.028(4) 0.039(4) 0.036(4) -0.001(3) 0.005(3) 0.001(3) C1 0.037(5) 0.049(6) 0.031(5) 0.003(4) 0.006(4) 0.000(4) C2 0.038(5) 0.035(5) 0.067(7) -0.011(5) -0.008(5) 0.003(4) C3 0.046(6) 0.044(6) 0.060(7) 0.006(5) -0.008(5) 0.010(5) C4 0.051(6) 0.039(6) 0.055(6) 0.010(5) -0.004(5) 0.000(5) C5 0.035(5) 0.036(5) 0.039(5) 0.008(4) 0.004(4) -0.001(4) C6 0.040(5) 0.052(6) 0.033(5) 0.005(4) 0.007(4) 0.009(5) C7 0.047(5) 0.035(5) 0.039(5) -0.008(4) 0.003(4) 0.007(4) C8 0.028(5) 0.050(6) 0.061(7) -0.003(5) -0.003(4) 0.007(4) C9 0.047(6) 0.052(6) 0.072(7) -0.031(6) -0.015(5) 0.012(5) C10 0.097(9) 0.092(9) 0.042(6) 0.016(6) 0.032(6) 0.031(8) C11 0.102(10) 0.076(9) 0.053(7) -0.016(7) 0.016(7) -0.020(8) C12 0.052(7) 0.037(6) 0.046(6) 0.016(5) 0.002(5) -0.008(5) C13 0.041(5) 0.042(6) 0.051(6) 0.010(5) 0.013(5) -0.003(4) C14 0.051(6) 0.042(6) 0.030(5) 0.004(4) 0.000(4) 0.007(5) C15 0.051(6) 0.041(6) 0.038(5) 0.013(4) -0.001(5) 0.006(5) C16 0.111(11) 0.035(6) 0.097(10) -0.016(6) -0.021(8) 0.014(7) C17 0.054(6) 0.046(6) 0.049(6) 0.008(5) 0.012(5) -0.001(5) C18 0.069(8) 0.052(7) 0.063(7) 0.025(6) -0.012(6) 0.004(6) C19 0.050(7) 0.047(7) 0.099(10) 0.022(7) -0.011(7) 0.007(5) C20 0.031(5) 0.037(5) 0.080(8) -0.002(5) 0.009(5) 0.006(4) C21 0.028(5) 0.034(5) 0.067(7) -0.002(5) 0.005(5) 0.004(4) C22 0.029(5) 0.045(6) 0.048(6) -0.005(5) 0.012(4) 0.001(4) C23 0.033(5) 0.044(5) 0.032(5) 0.010(4) 0.009(4) 0.005(4) C24 0.075(8) 0.063(7) 0.085(9) 0.019(6) 0.040(7) 0.020(6) C25 0.042(6) 0.060(6) 0.045(6) 0.016(5) 0.000(5) 0.003(5) C26 0.052(6) 0.051(6) 0.070(7) 0.017(6) -0.019(5) -0.017(5) C27 0.096(10) 0.043(7) 0.089(9) 0.012(6) -0.006(8) -0.005(7) C28 0.035(5) 0.046(6) 0.048(6) 0.000(5) 0.007(5) 0.018(5) C29 0.045(5) 0.043(5) 0.037(5) -0.002(4) 0.013(4) 0.012(5) C30 0.028(5) 0.045(5) 0.045(5) -0.010(4) 0.009(4) 0.014(4) C31 0.035(5) 0.052(6) 0.042(6) -0.008(5) 0.006(5) 0.019(5) C32 0.046(7) 0.084(9) 0.061(7) -0.009(6) 0.019(6) -0.016(6) O1 0.055(5) 0.069(5) 0.061(5) 0.002(4) -0.010(4) 0.004(4) O2 0.068(5) 0.059(5) 0.042(4) -0.009(4) 0.012(4) -0.006(4) O3 0.049(4) 0.050(4) 0.075(5) 0.006(4) 0.009(4) -0.007(3) O4 0.063(5) 0.040(4) 0.070(5) -0.004(4) -0.003(4) 0.006(4) O5 0.066(5) 0.051(4) 0.048(4) -0.005(4) -0.003(4) -0.002(4) O6 0.075(5) 0.048(4) 0.049(4) 0.006(4) 0.001(4) 0.005(4) O7 0.050(4) 0.078(5) 0.055(5) 0.004(4) -0.005(4) 0.005(4) O8 0.045(4) 0.065(5) 0.046(4) 0.003(3) 0.008(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C14 2.044(9) . ? Pt1 C13 2.052(9) . ? Pt1 N1 2.094(7) . ? Pt1 N2 2.107(7) . ? Pt2 C30 2.043(7) . ? Pt2 C29 2.049(8) . ? Pt2 N3 2.081(7) . ? Pt2 N4 2.125(6) . ? N1 C1 1.335(10) . ? N1 C5 1.359(10) . ? N2 C6 1.274(10) . ? N2 C7 1.490(10) . ? N3 C17 1.339(11) . ? N3 C21 1.365(11) . ? N4 C22 1.270(10) . ? N4 C23 1.483(10) . ? C1 C2 1.378(12) . ? C2 C3 1.370(13) . ? C3 C4 1.374(12) . ? C4 C5 1.380(12) . ? C5 C6 1.450(11) . ? C7 C9 1.515(13) . ? C7 C8 1.516(12) . ? C7 C10 1.518(13) . ? C11 O2 1.417(12) . ? C12 O1 1.185(11) . ? C12 O2 1.346(11) . ? C12 C13 1.463(13) . ? C13 C14 1.465(12) . ? C14 C15 1.453(13) . ? C15 O3 1.201(11) . ? C15 O4 1.360(10) . ? C16 O4 1.441(12) . ? C17 C18 1.379(13) . ? C18 C19 1.381(15) . ? C19 C20 1.365(14) . ? C20 C21 1.384(12) . ? C21 C22 1.435(13) . ? C23 C25 1.512(11) . ? C23 C24 1.504(12) . ? C23 C26 1.512(12) . ? C27 O6 1.440(12) . ? C28 O5 1.191(11) . ? C28 O6 1.360(11) . ? C28 C29 1.463(13) . ? C29 C30 1.436(12) . ? C30 C31 1.480(13) . ? C31 O7 1.221(11) . ? C31 O8 1.337(11) . ? C32 O8 1.429(11) . ? 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 C14 Pt1 C13 41.9(3) . . ? C14 Pt1 N1 160.7(3) . . ? C13 Pt1 N1 118.8(3) . . ? C14 Pt1 N2 122.0(3) . . ? C13 Pt1 N2 163.9(3) . . ? N1 Pt1 N2 77.3(3) . . ? C30 Pt2 C29 41.1(3) . . ? C30 Pt2 N3 119.1(3) . . ? C29 Pt2 N3 160.2(3) . . ? C30 Pt2 N4 163.7(3) . . ? C29 Pt2 N4 122.8(3) . . ? N3 Pt2 N4 77.0(3) . . ? C1 N1 C5 118.7(7) . . ? C1 N1 Pt1 126.2(6) . . ? C5 N1 Pt1 114.7(5) . . ? C6 N2 C7 120.1(7) . . ? C6 N2 Pt1 114.9(6) . . ? C7 N2 Pt1 124.9(5) . . ? C17 N3 C21 117.5(8) . . ? C17 N3 Pt2 127.7(6) . . ? C21 N3 Pt2 114.7(6) . . ? C22 N4 C23 121.8(7) . . ? C22 N4 Pt2 113.4(6) . . ? C23 N4 Pt2 124.8(5) . . ? N1 C1 C2 121.8(8) . . ? C3 C2 C1 120.1(9) . . ? C2 C3 C4 118.3(9) . . ? C5 C4 C3 120.0(9) . . ? N1 C5 C4 121.0(8) . . ? N1 C5 C6 114.1(7) . . ? C4 C5 C6 124.6(8) . . ? N2 C6 C5 118.9(8) . . ? N2 C7 C9 105.3(7) . . ? N2 C7 C8 107.8(7) . . ? C9 C7 C8 109.3(8) . . ? N2 C7 C10 112.4(8) . . ? C9 C7 C10 111.1(9) . . ? C8 C7 C10 110.7(8) . . ? O1 C12 O2 122.7(10) . . ? O1 C12 C13 127.4(10) . . ? O2 C12 C13 110.0(9) . . ? C14 C13 C12 120.0(8) . . ? C14 C13 Pt1 68.7(5) . . ? C12 C13 Pt1 113.0(6) . . ? C13 C14 C15 118.2(8) . . ? C13 C14 Pt1 69.4(5) . . ? C15 C14 Pt1 112.0(6) . . ? O3 C15 O4 120.2(9) . . ? O3 C15 C14 128.1(9) . . ? O4 C15 C14 111.8(8) . . ? N3 C17 C18 123.0(10) . . ? C17 C18 C19 118.6(10) . . ? C20 C19 C18 119.7(10) . . ? C19 C20 C21 119.2(9) . . ? N3 C21 C20 121.9(9) . . ? N3 C21 C22 113.8(8) . . ? C20 C21 C22 123.9(9) . . ? N4 C22 C21 119.7(8) . . ? N4 C23 C25 108.8(7) . . ? N4 C23 C24 112.9(7) . . ? C25 C23 C24 109.4(8) . . ? N4 C23 C26 104.8(7) . . ? C25 C23 C26 110.2(8) . . ? C24 C23 C26 110.7(8) . . ? O5 C28 O6 122.0(10) . . ? O5 C28 C29 126.9(9) . . ? O6 C28 C29 111.1(8) . . ? C30 C29 C28 117.9(8) . . ? C30 C29 Pt2 69.2(5) . . ? C28 C29 Pt2 114.1(6) . . ? C29 C30 C31 120.9(8) . . ? C29 C30 Pt2 69.7(4) . . ? C31 C30 Pt2 113.2(6) . . ? O7 C31 O8 123.4(9) . . ? O7 C31 C30 125.8(9) . . ? O8 C31 C30 110.8(8) . . ? C12 O2 C11 116.7(8) . . ? C15 O4 C16 117.0(8) . . ? C28 O6 C27 114.7(8) . . ? C31 O8 C32 115.5(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.745 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.154