# Copyright The Royal society of chemistry, 1998 # Neil G. Connelly # Structural studies of [Pt(CNMe)4][M(mnt)2]n (M = Pd or Pt, N = 1 or 2): # structure-dependent paramagnetism of three crystal forms of # [Pt(CNMe)4][Pt(mnt)2]2 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H12 N8 Pt2 S4' _chemical_formula_weight 834.76 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 20.000(7) _cell_length_b 6.655(3) _cell_length_c 9.182(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.13(3) _cell_angle_gamma 90.00 _cell_volume 1219.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 7.90 _cell_measurement_theta_max 14.55 _exptl_crystal_description Needles _exptl_crystal_colour Black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method ? _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 11.827 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.086 _exptl_absorpt_correction_T_max 0.107 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 single point detector diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.022 _diffrn_reflns_number 1760 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1276 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.99 _reflns_number_total 2656 _reflns_number_observed 987 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS' _computing_cell_refinement 'XSCANS' _computing_data_reduction 'XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1760 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_obs 0.0499 _refine_ls_wR_factor_all 0.1160 _refine_ls_wR_factor_obs 0.0959 _refine_ls_goodness_of_fit_all 0.954 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 0.954 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.113 _refine_ls_shift/esd_mean 0.028 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 1.0000 0.0000 0.0447(3) Uani 1 d S . Pt2 Pt 0.0000 0.5000 0.0000 0.0403(3) Uani 1 d S . S1 S -0.0332(3) 0.5000 -0.2460(5) 0.0525(11) Uani 1 d S . S2 S -0.1108(2) 0.5000 0.0559(5) 0.0491(10) Uani 1 d S . N1 N 0.1409(8) 1.0000 0.1683(22) 0.051(4) Uani 1 d S . N2 N 0.0702(9) 1.0000 -0.2904(19) 0.062(4) Uani 1 d S . N3 N -0.1862(12) 0.5000 -0.4941(27) 0.107(8) Uani 1 d S . N4 N -0.2796(10) 0.5000 -0.1273(26) 0.084(6) Uani 1 d S . C1 C 0.0915(7) 1.0000 0.1114(21) 0.041(4) Uani 1 d S . C2 C 0.2068(9) 1.0000 0.2501(22) 0.062(5) Uani 1 d S . H2A H 0.2377(12) 0.9216(91) 0.1984(45) 0.093 Uiso 1 calc R . H2B H 0.2028(11) 0.9430(101) 0.3451(36) 0.093 Uiso 1 calc R . H2C H 0.2230(20) 1.1354(10) 0.2601(73) 0.093 Uiso 1 calc R . C3 C 0.0480(11) 1.0000 -0.1836(21) 0.052(5) Uani 1 d S . C4 C 0.1101(16) 1.0000 -0.4194(29) 0.164(19) Uani 1 d S . H4A H 0.1207(83) 0.8642(15) -0.4444(127) 0.246 Uiso 1 calc R . H4B H 0.1508(51) 1.0739(249) -0.3978(81) 0.246 Uiso 1 calc R . H4C H 0.0848(43) 1.0619(265) -0.5001(70) 0.246 Uiso 1 calc R . C5 C -0.1218(11) 0.5000 -0.2406(24) 0.053(5) Uani 1 d S . C6 C -0.1574(12) 0.5000 -0.3775(26) 0.065(5) Uani 1 d S . C7 C -0.1526(11) 0.5000 -0.1145(29) 0.062(6) Uani 1 d S . C8 C -0.2241(10) 0.5000 -0.1155(31) 0.065(6) Uani 1 d S . 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 0.0344(6) 0.0547(7) 0.0443(8) 0.000 -0.0013(6) 0.000 Pt2 0.0332(6) 0.0399(6) 0.0467(8) 0.000 -0.0044(5) 0.000 S1 0.049(3) 0.065(2) 0.043(2) 0.000 -0.005(2) 0.000 S2 0.029(2) 0.060(2) 0.058(3) 0.000 0.005(2) 0.000 N1 0.040(9) 0.045(7) 0.071(13) 0.000 0.016(9) 0.000 N2 0.045(10) 0.089(11) 0.051(9) 0.000 0.005(9) 0.000 N3 0.071(16) 0.152(22) 0.092(14) 0.000 -0.038(15) 0.000 N4 0.044(10) 0.108(14) 0.097(16) 0.000 -0.012(13) 0.000 C1 0.005(5) 0.052(8) 0.063(10) 0.000 -0.015(7) 0.000 C2 0.038(10) 0.083(13) 0.061(12) 0.000 -0.020(10) 0.000 C3 0.056(12) 0.047(9) 0.054(11) 0.000 0.003(11) 0.000 C4 0.132(36) 0.280(50) 0.089(20) 0.000 0.076(26) 0.000 C5 0.049(12) 0.056(10) 0.055(11) 0.000 0.002(10) 0.000 C6 0.046(12) 0.079(13) 0.069(13) 0.000 -0.009(12) 0.000 C7 0.041(12) 0.064(12) 0.079(16) 0.000 -0.004(12) 0.000 C8 0.030(9) 0.070(11) 0.096(18) 0.000 0.010(12) 0.000 _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 C3 2.00(2) 5_575 ? Pt1 C3 2.00(2) . ? Pt1 C1 2.031(13) 5_575 ? Pt1 C1 2.032(13) . ? Pt2 S1 2.308(5) . ? Pt2 S1 2.308(5) 5_565 ? Pt2 S2 2.310(5) . ? Pt2 S2 2.310(5) 5_565 ? S1 C5 1.77(2) . ? S2 C7 1.72(3) . ? N1 C1 1.08(2) . ? N1 C2 1.47(2) . ? N2 C3 1.11(2) . ? N2 C4 1.48(3) . ? N3 C6 1.18(3) . ? N4 C8 1.11(2) . ? C5 C6 1.40(3) . ? C5 C7 1.35(3) . ? C7 C8 1.43(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Pt1 C3 179.998(1) 5_575 . ? C3 Pt1 C1 87.4(8) 5_575 5_575 ? C3 Pt1 C1 92.6(8) . 5_575 ? C3 Pt1 C1 92.6(8) 5_575 . ? C3 Pt1 C1 87.4(8) . . ? C1 Pt1 C1 179.999(2) 5_575 . ? S1 Pt2 S1 180.0 . 5_565 ? S1 Pt2 S2 90.3(2) . . ? S1 Pt2 S2 89.7(2) 5_565 . ? S1 Pt2 S2 89.7(2) . 5_565 ? S1 Pt2 S2 90.3(2) 5_565 5_565 ? S2 Pt2 S2 180.0 . 5_565 ? C5 S1 Pt2 101.0(7) . . ? C7 S2 Pt2 102.1(8) . . ? C1 N1 C2 178.2(23) . . ? C3 N2 C4 171.0(24) . . ? N1 C1 Pt1 178.7(20) . . ? N2 C3 Pt1 175.1(20) . . ? C6 C5 C7 122.3(21) . . ? C6 C5 S1 114.8(17) . . ? C7 C5 S1 122.9(17) . . ? N3 C6 C5 178.6(28) . . ? C8 C7 C5 120.9(24) . . ? C8 C7 S2 115.2(21) . . ? C5 C7 S2 123.8(17) . . ? N4 C8 C7 174.8(35) . . ? _refine_diff_density_max 1.289 _refine_diff_density_min -2.495 _refine_diff_density_rms 0.231 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H12 N8 Pd Pt S4' _chemical_formula_weight 746.06 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.933(4) _cell_length_b 6.6140(10) _cell_length_c 9.152(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.09(2) _cell_angle_gamma 90.00 _cell_volume 1203.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 6.50 _cell_measurement_theta_max 20.96 _exptl_crystal_description Needles _exptl_crystal_colour Green _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method ? _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 6.919 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.144 _exptl_absorpt_correction_T_max 0.754 _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 'Siemens P4 single point detector diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.95 _diffrn_reflns_number 1475 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2191 _reflns_number_observed 1335 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS' _computing_cell_refinement 'XSCANS' _computing_data_reduction 'XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+2.5560P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1475 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_obs 0.0329 _refine_ls_wR_factor_all 0.0848 _refine_ls_wR_factor_obs 0.0813 _refine_ls_goodness_of_fit_all 0.927 _refine_ls_goodness_of_fit_obs 0.936 _refine_ls_restrained_S_all 0.927 _refine_ls_restrained_S_obs 0.936 _refine_ls_shift/esd_max 0.020 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.04012(14) Uani 1 d S . Pd1 Pd 0.0000 0.5000 0.0000 0.0383(2) Uani 1 d S . S1 S -0.11060(9) 0.5000 0.0574(2) 0.0492(4) Uani 1 d S . S2 S -0.03289(9) 0.5000 -0.2466(2) 0.0486(4) Uani 1 d S . N1 N 0.1406(3) 0.0000 0.1715(8) 0.0499(15) Uani 1 d S . N2 N -0.0694(4) 0.0000 0.2911(9) 0.062(2) Uani 1 d S . N3 N -0.2822(4) 0.5000 -0.1279(11) 0.083(3) Uani 1 d S . N4 N -0.1863(5) 0.5000 -0.4913(11) 0.099(3) Uani 1 d S . C1 C 0.0891(3) 0.0000 0.1095(8) 0.0438(14) Uani 1 d S . C2 C 0.2065 0.0000 0.2468 0.064 Uani 1 d S . H2A H 0.2015 0.0000 0.3500 0.080 Uiso 1 d S . H2B H 0.2308 0.1185 0.2211 0.080 Uiso 1 d . . C3 C -0.0437(3) 0.0000 0.1856(8) 0.0460(15) Uani 1 d S . C4 C -0.1061 0.0000 0.4167 0.119 Uani 1 d S . H4A H -0.0745 0.0000 0.5008 0.080 Uiso 1 d S . H4B H -0.1339 0.1185 0.4184 0.080 Uiso 1 d . . C5 C -0.1518(4) 0.5000 -0.1159(9) 0.048(2) Uani 1 d S . C6 C -0.2241(4) 0.5000 -0.1197(10) 0.058(2) Uani 1 d S . C7 C -0.1204(4) 0.5000 -0.2402(9) 0.047(2) Uani 1 d S . C8 C -0.1582(5) 0.5000 -0.3797(11) 0.063(2) Uani 1 d S . 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 0.0343(2) 0.0422(2) 0.0431(2) 0.000 -0.00322(13) 0.000 Pd1 0.0342(3) 0.0347(3) 0.0451(4) 0.000 -0.0033(3) 0.000 S1 0.0383(8) 0.0552(10) 0.0538(10) 0.000 0.0014(7) 0.000 S2 0.0434(9) 0.0556(10) 0.0459(9) 0.000 -0.0034(7) 0.000 N1 0.044(3) 0.047(3) 0.058(4) 0.000 -0.005(3) 0.000 N2 0.054(4) 0.072(4) 0.060(4) 0.000 0.004(3) 0.000 N3 0.041(4) 0.101(7) 0.105(7) 0.000 -0.001(4) 0.000 N4 0.094(7) 0.119(8) 0.077(6) 0.000 -0.038(6) 0.000 C1 0.039(3) 0.041(3) 0.050(4) 0.000 -0.004(3) 0.000 C2 0.047 0.053 0.086 0.000 -0.025 0.000 C3 0.038(3) 0.053(4) 0.047(4) 0.000 -0.003(3) 0.000 C4 0.113 0.161 0.084 0.000 0.026 0.000 C5 0.037(3) 0.042(3) 0.065(5) 0.000 -0.001(3) 0.000 C6 0.048(4) 0.056(4) 0.069(5) 0.000 -0.005(4) 0.000 C7 0.044(4) 0.040(3) 0.055(4) 0.000 -0.012(3) 0.000 C8 0.055(5) 0.062(5) 0.069(6) 0.000 -0.014(4) 0.000 _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 C1 1.976(7) . ? Pt1 C1 1.976(7) 5 ? Pt1 C3 1.963(8) 5 ? Pt1 C3 1.963(8) . ? Pd1 S1 2.302(2) . ? Pd1 S1 2.302(2) 5_565 ? Pd1 S2 2.305(2) . ? Pd1 S2 2.305(2) 5_565 ? S1 C5 1.733(9) . ? S2 C7 1.750(8) . ? N1 C1 1.138(10) . ? N1 C2 1.439(7) . ? N2 C3 1.125(10) . ? N2 C4 1.406(8) . ? N3 C6 1.155(11) . ? N4 C8 1.129(12) . ? C5 C7 1.337(12) . ? C5 C6 1.439(11) . ? C7 C8 1.435(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 C1 Pt1 C1 180.0 . 5 ? C1 Pt1 C3 90.0(3) . 5 ? C1 Pt1 C3 90.0(3) 5 5 ? C1 Pt1 C3 90.0(3) . . ? C1 Pt1 C3 90.0(3) 5 . ? C3 Pt1 C3 180.0 5 . ? S1 Pd1 S1 180.0 . 5_565 ? S1 Pd1 S2 90.75(7) . . ? S1 Pd1 S2 89.25(7) 5_565 . ? S1 Pd1 S2 89.25(7) . 5_565 ? S1 Pd1 S2 90.75(7) 5_565 5_565 ? S2 Pd1 S2 180.0 . 5_565 ? C5 S1 Pd1 101.0(3) . . ? C7 S2 Pd1 100.5(3) . . ? C1 N1 C2 178.7(8) . . ? C3 N2 C4 175.8(8) . . ? N1 C1 Pt1 179.5(7) . . ? N2 C3 Pt1 179.2(7) . . ? C7 C5 C6 120.6(8) . . ? C7 C5 S1 123.9(6) . . ? C6 C5 S1 115.5(7) . . ? N3 C6 C5 177.7(11) . . ? C5 C7 C8 120.6(8) . . ? C5 C7 S2 123.8(6) . . ? C8 C7 S2 115.6(7) . . ? N4 C8 C7 178.1(12) . . ? _refine_diff_density_max 0.714 _refine_diff_density_min -1.747 _refine_diff_density_rms 0.192 #=END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H18 N14 Pt3 S8' _chemical_formula_weight 1392.299 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.071(4) _cell_length_b 14.414(4) _cell_length_c 20.747(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.16(2) _cell_angle_gamma 90.00 _cell_volume 4208.0(21) _cell_formula_units_Z 4 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.85 _cell_measurement_theta_max 14.70 _exptl_crystal_description diamond _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method ? _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 10.389 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 0.956 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 single point detector diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 8707 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.51 _reflns_number_total 11430 _reflns_number_observed 4906 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS' _computing_cell_refinement 'XSCANS' _computing_data_reduction 'XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8707 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_obs 0.0546 _refine_ls_wR_factor_all 0.1268 _refine_ls_wR_factor_obs 0.1044 _refine_ls_goodness_of_fit_all 0.937 _refine_ls_goodness_of_fit_obs 1.049 _refine_ls_restrained_S_all 0.937 _refine_ls_restrained_S_obs 1.049 _refine_ls_shift/esd_max -0.082 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.50506(4) 0.85785(3) -0.02891(2) 0.03870(14) Uani 1 d . . Pt2 Pt 0.62382(4) -0.00812(4) -0.43985(2) 0.0428(2) Uani 1 d . . Pt3 Pt 0.50013(4) 0.38589(3) 0.02929(3) 0.03779(14) Uani 1 d . . S1 S 0.6007(3) 0.0612(3) -0.3436(2) 0.0558(10) Uani 1 d . . S2 S 0.6079(3) -0.1488(3) -0.3929(2) 0.0570(10) Uani 1 d . . S3 S 0.6342(3) 0.1333(3) -0.4863(2) 0.0547(10) Uani 1 d . . S4 S 0.6438(3) -0.0760(3) -0.5371(2) 0.0559(10) Uani 1 d . . S5 S 0.6225(3) 0.3559(3) -0.0382(2) 0.0460(9) Uani 1 d . . S6 S 0.3938(3) 0.3486(3) -0.0506(2) 0.0459(9) Uani 1 d . . S7 S 0.6058(3) 0.4272(2) 0.1085(2) 0.0438(8) Uani 1 d . . S8 S 0.3787(3) 0.4197(3) 0.0956(2) 0.0467(9) Uani 1 d . . N1 N 0.5407(11) 0.0070(10) -0.1759(6) 0.081(4) Uani 1 d . . N2 N 0.5476(12) -0.2545(11) -0.2386(7) 0.087(5) Uani 1 d . . N3 N 0.6589(11) 0.2450(9) -0.6454(6) 0.070(4) Uani 1 d . . N4 N 0.6661(12) -0.0144(12) -0.7075(6) 0.092(5) Uani 1 d . . N5 N 0.6690(11) 0.2676(12) -0.2014(7) 0.089(5) Uani 1 d . . N6 N 0.3843(12) 0.2597(11) -0.2165(8) 0.089(5) Uani 1 d . . N7 N 0.6145(11) 0.5045(12) 0.2781(6) 0.088(5) Uani 1 d . . N8 N 0.3332(12) 0.4924(11) 0.2621(7) 0.091(5) Uani 1 d . . N9 N 0.6404(8) 0.9133(7) 0.0853(5) 0.040(3) Uani 1 d . . N10 N 0.3712(10) 0.8157(9) -0.1457(6) 0.058(3) Uani 1 d . . N11 N 0.3319(9) 0.8970(8) 0.0562(6) 0.048(3) Uani 1 d . . N12 N 0.6798(9) 0.8227(8) -0.1145(6) 0.051(3) Uani 1 d . . C1 C 0.5805(10) -0.0308(10) -0.2945(7) 0.051(4) Uani 1 d . . C2 C 0.5599(13) -0.0107(12) -0.2283(7) 0.068(5) Uani 1 d . . C3 C 0.5832(10) -0.1200(10) -0.3139(7) 0.048(4) Uani 1 d . . C4 C 0.5617(13) -0.1973(10) -0.2723(7) 0.063(5) Uani 1 d . . C5 C 0.6477(10) 0.1068(10) -0.5654(6) 0.042(3) Uani 1 d . . C6 C 0.6528(10) 0.1818(11) -0.6102(6) 0.050(4) Uani 1 d . . C7 C 0.6513(10) 0.0185(11) -0.5885(6) 0.053(4) Uani 1 d . . C8 C 0.6617(12) -0.0014(11) -0.6548(8) 0.064(4) Uani 1 d . . C9 C 0.5643(10) 0.3202(8) -0.1074(6) 0.036(3) Uani 1 d . . C10 C 0.6214(12) 0.2936(11) -0.1604(7) 0.059(4) Uani 1 d . . C11 C 0.4648(10) 0.3176(9) -0.1129(6) 0.039(3) Uani 1 d . . C12 C 0.4189(12) 0.2854(10) -0.1712(7) 0.056(4) Uani 1 d . . C13 C 0.5331(10) 0.4541(9) 0.1718(5) 0.038(3) Uani 1 d . . C14 C 0.5788(12) 0.4826(11) 0.2314(8) 0.061(4) Uani 1 d . . C15 C 0.4350(11) 0.4506(9) 0.1665(6) 0.047(3) Uani 1 d . . C16 C 0.3796(12) 0.4752(11) 0.2193(7) 0.056(4) Uani 1 d . . C17 C 0.5949(12) 0.8940(9) 0.0447(7) 0.050(4) Uani 1 d . . C18 C 0.7006(12) 0.9400(11) 0.1380(7) 0.068(5) Uani 1 d . . H18A H 0.7521(44) 0.8967(46) 0.1424(34) 0.103 Uiso 1 calc R . H18B H 0.6648(22) 0.9405(74) 0.1769(12) 0.103 Uiso 1 calc R . H18C H 0.7256(65) 1.0009(34) 0.1303(26) 0.103 Uiso 1 calc R . C19 C 0.4156(11) 0.8305(10) -0.1031(7) 0.051(4) Uani 1 d . . C20 C 0.3046(14) 0.7923(13) -0.1978(7) 0.085(6) Uani 1 d . . H20A H 0.2667(62) 0.8457(29) -0.2086(42) 0.128 Uiso 1 calc R . H20B H 0.2639(62) 0.7428(62) -0.1842(23) 0.128 Uiso 1 calc R . H20C H 0.3392(14) 0.7730(84) -0.2349(21) 0.128 Uiso 1 calc R . C21 C 0.3939(11) 0.8861(9) 0.0266(6) 0.041(3) Uani 1 d . . C22 C 0.2526(13) 0.9130(13) 0.0982(8) 0.086(6) Uani 1 d . . H22A H 0.2159(52) 0.8571(29) 0.1016(49) 0.128 Uiso 1 calc R . H22B H 0.2132(51) 0.9615(63) 0.0806(33) 0.128 Uiso 1 calc R . H22C H 0.2761(14) 0.9308(84) 0.1401(19) 0.128 Uiso 1 calc R . C23 C 0.6155(12) 0.8351(10) -0.0838(7) 0.050(4) Uani 1 d . . C24 C 0.7611(12) 0.8007(13) -0.1533(8) 0.079(6) Uani 1 d . . H24A H 0.7887(53) 0.8571(14) -0.1690(48) 0.118 Uiso 1 calc R . H24B H 0.7412(19) 0.7628(70) -0.1891(33) 0.118 Uiso 1 calc R . H24C H 0.8074(39) 0.7677(74) -0.1276(17) 0.118 Uiso 1 calc R . N14 N 0.8556(18) 0.9033(14) -0.0130(11) 0.120(7) Uani 1 d . . C28 C 0.9084(19) 0.9015(16) 0.0254(12) 0.092(7) Uani 1 d . . C26 C 0.8859(17) 0.1699(14) 0.0877(11) 0.084(6) Uani 1 d . . N13 N 0.8320(16) 0.1396(14) 0.0570(10) 0.116(7) Uani 1 d . . C27 C 0.9606(16) 0.2081(16) 0.1271(11) 0.113(8) Uani 1 d . . H27A H 0.9424(50) 0.2687(49) 0.1416(65) 0.170 Uiso 1 calc R . H27B H 1.0174(35) 0.2128(106) 0.1024(26) 0.170 Uiso 1 calc R . H27C H 0.9721(80) 0.1686(61) 0.1637(42) 0.170 Uiso 1 calc R . C29 C 0.9774(19) 0.9098(15) 0.0771(11) 0.118(8) Uani 1 d . . H29A H 1.0144(81) 0.8540(50) 0.0799(54) 0.176 Uiso 1 calc R . H29B H 0.9453(19) 0.9194(117) 0.1170(16) 0.176 Uiso 1 calc R . H29C H 1.0184(79) 0.9615(75) 0.0690(42) 0.176 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0404(3) 0.0472(3) 0.0284(3) 0.0041(2) -0.0002(2) 0.0005(3) Pt2 0.0351(3) 0.0551(3) 0.0382(3) 0.0060(3) 0.0015(2) -0.0020(3) Pt3 0.0347(3) 0.0430(3) 0.0357(3) 0.0042(2) 0.0008(2) -0.0014(3) S1 0.068(3) 0.058(2) 0.041(2) 0.008(2) 0.005(2) 0.000(2) S2 0.065(3) 0.055(2) 0.051(2) 0.009(2) 0.004(2) 0.001(2) S3 0.063(3) 0.058(2) 0.044(2) 0.003(2) 0.006(2) -0.005(2) S4 0.061(3) 0.060(2) 0.047(2) -0.003(2) 0.004(2) 0.007(2) S5 0.033(2) 0.058(2) 0.047(2) 0.000(2) 0.002(2) -0.002(2) S6 0.035(2) 0.056(2) 0.047(2) 0.001(2) -0.002(2) -0.003(2) S7 0.038(2) 0.056(2) 0.037(2) -0.002(2) -0.0055(15) 0.001(2) S8 0.038(2) 0.057(2) 0.046(2) 0.001(2) 0.005(2) -0.001(2) N1 0.091(12) 0.101(11) 0.051(9) 0.005(9) -0.005(8) 0.010(10) N2 0.094(13) 0.103(12) 0.065(10) 0.022(9) 0.004(9) -0.003(11) N3 0.083(11) 0.082(9) 0.044(7) 0.022(7) 0.010(7) -0.008(9) N4 0.101(13) 0.143(15) 0.030(7) -0.016(9) -0.007(7) 0.012(11) N5 0.076(11) 0.132(14) 0.058(9) -0.001(9) 0.023(8) -0.007(11) N6 0.081(12) 0.118(13) 0.066(10) 0.015(10) -0.011(8) -0.028(11) N7 0.080(12) 0.138(14) 0.046(8) -0.014(9) -0.027(7) 0.018(11) N8 0.105(14) 0.092(11) 0.076(10) -0.009(9) 0.036(9) 0.009(10) N9 0.041(7) 0.036(6) 0.044(7) -0.003(5) -0.004(5) 0.011(5) N10 0.068(10) 0.071(8) 0.034(7) 0.005(6) -0.010(6) 0.010(8) N11 0.032(7) 0.059(7) 0.054(8) 0.008(6) -0.001(6) -0.006(6) N12 0.047(8) 0.056(7) 0.049(7) 0.021(6) 0.011(6) -0.001(7) C1 0.041(9) 0.065(9) 0.046(8) 0.012(7) 0.008(6) 0.000(8) C2 0.093(14) 0.079(11) 0.031(8) 0.031(9) 0.013(8) 0.005(10) C3 0.029(8) 0.059(9) 0.058(9) 0.000(7) 0.001(7) 0.008(7) C4 0.084(13) 0.053(9) 0.051(10) 0.030(8) -0.002(9) -0.016(9) C5 0.036(8) 0.063(9) 0.027(7) 0.008(6) 0.008(6) 0.009(7) C6 0.045(9) 0.078(10) 0.028(7) -0.005(7) 0.004(6) -0.013(8) C7 0.042(9) 0.085(11) 0.031(7) -0.012(8) 0.001(6) 0.000(8) C8 0.052(11) 0.080(11) 0.059(10) -0.006(9) -0.015(8) 0.014(9) C9 0.039(8) 0.031(6) 0.037(7) 0.001(5) 0.007(6) 0.005(6) C10 0.052(10) 0.078(11) 0.047(9) 0.002(8) 0.016(8) -0.002(9) C11 0.037(8) 0.042(7) 0.038(7) 0.004(6) 0.001(6) 0.004(6) C12 0.064(11) 0.058(9) 0.045(9) 0.009(7) -0.017(8) 0.003(8) C13 0.049(9) 0.047(7) 0.019(6) 0.014(5) 0.005(5) 0.011(7) C14 0.064(12) 0.066(10) 0.055(10) 0.013(8) 0.006(8) -0.005(9) C15 0.046(10) 0.053(8) 0.043(8) 0.003(7) 0.005(7) 0.006(7) C16 0.065(11) 0.070(10) 0.035(8) -0.003(7) 0.015(7) 0.007(9) C17 0.057(11) 0.038(7) 0.054(10) -0.007(7) 0.004(8) 0.002(7) C18 0.069(12) 0.066(10) 0.069(11) 0.004(8) -0.021(9) -0.030(9) C19 0.047(10) 0.067(10) 0.038(8) 0.005(7) 0.001(7) 0.019(8) C20 0.089(14) 0.121(15) 0.044(10) 0.000(10) -0.030(9) -0.028(13) C21 0.035(9) 0.053(8) 0.035(7) 0.010(6) -0.014(6) -0.012(7) C22 0.075(14) 0.101(13) 0.083(13) 0.036(11) 0.038(11) 0.007(12) C23 0.057(11) 0.049(8) 0.044(9) 0.000(7) -0.007(8) -0.010(8) C24 0.063(12) 0.116(14) 0.059(11) -0.011(10) 0.026(9) 0.020(11) N14 0.145(23) 0.104(14) 0.111(18) -0.001(13) 0.001(15) 0.015(15) C28 0.091(19) 0.087(14) 0.097(19) 0.037(14) -0.003(14) 0.004(14) C26 0.085(17) 0.080(14) 0.089(16) 0.004(12) -0.002(12) -0.008(13) N13 0.113(19) 0.120(15) 0.115(17) -0.017(12) -0.027(14) -0.017(13) C27 0.099(19) 0.143(20) 0.100(17) -0.022(15) 0.028(14) -0.031(17) C29 0.141(25) 0.099(16) 0.113(20) 0.006(15) 0.031(18) -0.006(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 Pt1 C23 1.97(2) . ? Pt1 C21 2.00(2) . ? Pt1 C19 2.01(2) . ? Pt1 C17 2.03(2) . ? Pt2 S1 2.262(4) . ? Pt2 S3 2.260(4) . ? Pt2 S2 2.263(4) . ? Pt2 S4 2.265(4) . ? Pt3 S8 2.268(4) . ? Pt3 S7 2.273(3) . ? Pt3 S6 2.275(4) . ? Pt3 S5 2.282(4) . ? S1 C1 1.700(14) . ? S2 C3 1.733(15) . ? S3 C5 1.699(13) . ? S4 C7 1.73(2) . ? S5 C9 1.718(13) . ? S6 C11 1.708(13) . ? S7 C13 1.724(12) . ? S8 C15 1.716(15) . ? N1 C2 1.15(2) . ? N2 C4 1.10(2) . ? N3 C6 1.17(2) . ? N4 C8 1.11(2) . ? N5 C10 1.16(2) . ? N6 C12 1.12(2) . ? N7 C14 1.13(2) . ? N8 C16 1.14(2) . ? N9 C17 1.08(2) . ? N9 C18 1.42(2) . ? N10 C19 1.09(2) . ? N10 C20 1.46(2) . ? N11 C21 1.09(2) . ? N11 C22 1.45(2) . ? N12 C23 1.13(2) . ? N12 C24 1.45(2) . ? C1 C3 1.35(2) . ? C1 C2 1.44(2) . ? C3 C4 1.45(2) . ? C5 C7 1.36(2) . ? C5 C6 1.43(2) . ? C7 C8 1.42(2) . ? C9 C11 1.40(2) . ? C9 C10 1.43(2) . ? C11 C12 1.44(2) . ? C13 C15 1.38(2) . ? C13 C14 1.44(2) . ? C15 C16 1.40(2) . ? N14 C28 1.08(3) . ? C28 C29 1.44(3) . ? C26 N13 1.07(2) . ? C26 C27 1.43(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Pt1 C21 177.8(6) . . ? C23 Pt1 C19 90.8(6) . . ? C21 Pt1 C19 89.8(5) . . ? C23 Pt1 C17 89.5(6) . . ? C21 Pt1 C17 89.8(6) . . ? C19 Pt1 C17 176.4(6) . . ? S1 Pt2 S3 89.41(13) . . ? S1 Pt2 S2 89.91(14) . . ? S3 Pt2 S2 178.0(2) . . ? S1 Pt2 S4 178.7(2) . . ? S3 Pt2 S4 89.98(14) . . ? S2 Pt2 S4 90.66(14) . . ? S8 Pt3 S7 89.72(13) . . ? S8 Pt3 S6 90.01(14) . . ? S7 Pt3 S6 178.48(13) . . ? S8 Pt3 S5 178.47(13) . . ? S7 Pt3 S5 90.18(13) . . ? S6 Pt3 S5 90.06(13) . . ? C1 S1 Pt2 102.3(5) . . ? C3 S2 Pt2 102.5(5) . . ? C5 S3 Pt2 102.6(5) . . ? C7 S4 Pt2 102.6(5) . . ? C9 S5 Pt3 102.5(5) . . ? C11 S6 Pt3 103.1(5) . . ? C13 S7 Pt3 102.7(5) . . ? C15 S8 Pt3 103.6(5) . . ? C17 N9 C18 179.0(15) . . ? C19 N10 C20 174.1(17) . . ? C21 N11 C22 177.1(16) . . ? C23 N12 C24 176.5(16) . . ? C3 C1 C2 119.0(13) . . ? C3 C1 S1 124.0(11) . . ? C2 C1 S1 117.0(12) . . ? N1 C2 C1 177.7(18) . . ? C1 C3 C4 123.4(14) . . ? C1 C3 S2 121.2(11) . . ? C4 C3 S2 115.4(11) . . ? N2 C4 C3 177.0(18) . . ? C7 C5 C6 118.4(12) . . ? C7 C5 S3 123.7(10) . . ? C6 C5 S3 117.9(11) . . ? N3 C6 C5 177.6(15) . . ? C5 C7 C8 122.4(14) . . ? C5 C7 S4 121.0(10) . . ? C8 C7 S4 116.6(12) . . ? N4 C8 C7 176.6(18) . . ? C11 C9 C10 120.5(12) . . ? C11 C9 S5 122.2(9) . . ? C10 C9 S5 117.2(11) . . ? N5 C10 C9 176.1(18) . . ? C9 C11 C12 120.5(12) . . ? C9 C11 S6 122.1(10) . . ? C12 C11 S6 117.5(11) . . ? N6 C12 C11 179.1(19) . . ? C15 C13 C14 120.3(12) . . ? C15 C13 S7 122.5(10) . . ? C14 C13 S7 117.1(11) . . ? N7 C14 C13 179.6(18) . . ? C13 C15 C16 119.9(13) . . ? C13 C15 S8 121.4(10) . . ? C16 C15 S8 118.7(12) . . ? N8 C16 C15 177.8(19) . . ? N9 C17 Pt1 177.7(15) . . ? N10 C19 Pt1 176.1(15) . . ? N11 C21 Pt1 176.3(14) . . ? N12 C23 Pt1 178.9(13) . . ? N14 C28 C29 173.8(29) . . ? N13 C26 C27 177.6(29) . . ? _refine_diff_density_max 1.648 _refine_diff_density_min -1.297 _refine_diff_density_rms 0.229 #=END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H18 N14 Pd2 Pt S8' _chemical_formula_weight 1214.93 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.063(6) _cell_length_b 14.385(6) _cell_length_c 20.668(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.28(3) _cell_angle_gamma 90.00 _cell_volume 4180.0(31) _cell_formula_units_Z 4 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 5.61 _cell_measurement_theta_max 26.42 _exptl_crystal_description diamond _exptl_crystal_colour black _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method ? _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 4.630 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.012 _exptl_absorpt_correction_T_max 0.029 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 single point detector diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0047 _diffrn_reflns_number 5409 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 22.49 _reflns_number_total 7349 _reflns_number_observed 3382 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS' _computing_cell_refinement 'XSCANS' _computing_data_reduction 'XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5409 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_obs 0.0465 _refine_ls_wR_factor_all 0.1161 _refine_ls_wR_factor_obs 0.0990 _refine_ls_goodness_of_fit_all 0.955 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 0.955 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max 0.072 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.50478(4) 0.85686(4) -0.02839(2) 0.0552(2) Uani 1 d . . Pd1 Pd 0.62316(7) -0.00933(8) -0.43933(5) 0.0589(3) Uani 1 d . . Pd2 Pd 0.50007(8) 0.38850(7) 0.02900(5) 0.0529(4) Uani 0.898(3) d P . Pd2' Pd 0.3796(7) -0.5044(7) -0.0004(5) 0.063(4) Uiso 0.102(3) d P . S1 S 0.6023(3) 0.0597(3) -0.3424(2) 0.0731(10) Uani 1 d . . S2 S 0.6064(3) -0.1506(3) -0.3927(2) 0.0720(10) Uani 1 d . . S3 S 0.6330(3) 0.1333(3) -0.4852(2) 0.0717(10) Uani 1 d . . S4 S 0.6406(3) -0.0761(3) -0.5375(2) 0.0755(11) Uani 1 d . . S5 S 0.6237(2) 0.3584(3) -0.0391(2) 0.0647(9) Uani 1 d . . S6 S 0.3929(2) 0.3489(3) -0.0501(2) 0.0625(9) Uani 1 d . . S7 S 0.6067(2) 0.4313(3) 0.1082(2) 0.0644(9) Uani 1 d . . S8 S 0.3772(2) 0.4227(3) 0.0960(2) 0.0652(9) Uani 1 d . . N1 N 0.5419(10) 0.0039(10) -0.1743(6) 0.098(4) Uani 1 d . . N2 N 0.5441(11) -0.2578(10) -0.2378(7) 0.103(5) Uani 1 d . . N3 N 0.6576(10) 0.2449(9) -0.6433(6) 0.088(4) Uani 1 d . . N4 N 0.6645(10) -0.0147(12) -0.7097(6) 0.113(5) Uani 1 d . . N5 N 0.6670(10) 0.2676(12) -0.2006(6) 0.103(5) Uani 1 d . . N6 N 0.3839(10) 0.2561(10) -0.2151(6) 0.098(4) Uani 1 d . . N7 N 0.6130(11) 0.5084(11) 0.2782(6) 0.105(5) Uani 1 d . . N8 N 0.3324(11) 0.4963(11) 0.2637(6) 0.109(5) Uani 1 d . . N9 N 0.6425(7) 0.9137(7) 0.0847(5) 0.055(3) Uani 1 d . . N10 N 0.3687(8) 0.8114(8) -0.1439(5) 0.067(3) Uani 1 d . . N11 N 0.3310(8) 0.8967(8) 0.0581(5) 0.066(3) Uani 1 d . . N12 N 0.6799(8) 0.8195(8) -0.1145(5) 0.062(3) Uani 1 d . . C1 C 0.5812(9) -0.0320(11) -0.2939(6) 0.065(4) Uani 1 d . . C2 C 0.5585(10) -0.0127(11) -0.2270(7) 0.073(4) Uani 1 d . . C3 C 0.5829(9) -0.1238(11) -0.3133(6) 0.069(4) Uani 1 d . . C4 C 0.5605(10) -0.1960(11) -0.2718(7) 0.071(4) Uani 1 d . . C5 C 0.6447(9) 0.1044(11) -0.5662(6) 0.064(4) Uani 1 d . . C6 C 0.6520(10) 0.1821(12) -0.6085(7) 0.075(4) Uani 1 d . . C7 C 0.6490(9) 0.0172(11) -0.5873(6) 0.066(4) Uani 1 d . . C8 C 0.6570(10) 0.0009(11) -0.6559(8) 0.075(4) Uani 1 d . . C9 C 0.5653(11) 0.3227(11) -0.1061(6) 0.075(4) Uani 1 d . . C10 C 0.6231(11) 0.2926(12) -0.1596(8) 0.081(4) Uani 1 d . . C11 C 0.4659(9) 0.3162(9) -0.1114(6) 0.062(3) Uani 1 d . . C12 C 0.4194(10) 0.2860(11) -0.1697(7) 0.072(4) Uani 1 d . . C13 C 0.5348(12) 0.4591(11) 0.1715(7) 0.080(4) Uani 1 d . . C14 C 0.5792(11) 0.4866(12) 0.2311(8) 0.085(5) Uani 1 d . . C15 C 0.4351(10) 0.4549(9) 0.1655(6) 0.065(4) Uani 1 d . . C16 C 0.3751(12) 0.4770(12) 0.2206(7) 0.083(5) Uani 1 d . . C17 C 0.5914(9) 0.8938(10) 0.0437(7) 0.059(4) Uani 1 d . . C18 C 0.7037(10) 0.9419(11) 0.1371(6) 0.079(4) Uani 1 d . . H18A H 0.7411(49) 0.8898(19) 0.1517(31) 0.118 Uiso 1 calc R . H18B H 0.6661(10) 0.9643(63) 0.1721(19) 0.118 Uiso 1 calc R . H18C H 0.7450(48) 0.9906(47) 0.1229(14) 0.118 Uiso 1 calc R . C19 C 0.4187(9) 0.8260(10) -0.1016(6) 0.060(4) Uani 1 d . . C20 C 0.3074(12) 0.7844(13) -0.1972(7) 0.098(5) Uani 1 d . . H20A H 0.2627(53) 0.8334(35) -0.2064(36) 0.147 Uiso 1 calc R . H20B H 0.2737(62) 0.7288(46) -0.1861(22) 0.147 Uiso 1 calc R . H20C H 0.3448(14) 0.7731(78) -0.2347(17) 0.147 Uiso 1 calc R . C21 C 0.3939(9) 0.8838(9) 0.0251(6) 0.055(3) Uani 1 d . . C22 C 0.2512(9) 0.9141(13) 0.0979(7) 0.090(5) Uani 1 d . . H22A H 0.2451(48) 0.8646(40) 0.1286(36) 0.135 Uiso 1 calc R . H22B H 0.1944(14) 0.9177(79) 0.0713(9) 0.135 Uiso 1 calc R . H22C H 0.2603(37) 0.9718(39) 0.1205(41) 0.135 Uiso 1 calc R . C23 C 0.6172(9) 0.8326(9) -0.0820(6) 0.059(4) Uani 1 d . . C24 C 0.7574(10) 0.7963(12) -0.1537(7) 0.090(5) Uani 1 d . . H24A H 0.7778(50) 0.8505(20) -0.1766(41) 0.136 Uiso 1 calc R . H24B H 0.7382(25) 0.7491(55) -0.1841(36) 0.136 Uiso 1 calc R . H24C H 0.8089(30) 0.7733(73) -0.1269(9) 0.136 Uiso 1 calc R . N13 N 0.8307(11) 0.1413(13) 0.0545(9) 0.127(6) Uani 1 d . . N14 N 0.8593(17) 0.9020(14) -0.0124(9) 0.138(7) Uani 1 d . . C28 C 0.9098(17) 0.9065(14) 0.0274(10) 0.102(6) Uani 1 d . . C26 C 0.8890(14) 0.1677(12) 0.0854(8) 0.092(5) Uani 1 d . . C25 C 0.9653(13) 0.2070(15) 0.1284(8) 0.120(7) Uani 1 d . . H25A H 1.0263(13) 0.1931(85) 0.1109(37) 0.179 Uiso 1 calc R . H25B H 0.9611(64) 0.1801(73) 0.1708(21) 0.179 Uiso 1 calc R . H25C H 0.9576(59) 0.2732(19) 0.1313(53) 0.179 Uiso 1 calc R . C27 C 0.9797(12) 0.9067(14) 0.0792(9) 0.109(6) Uani 1 d . . H27A H 0.9483(13) 0.9105(91) 0.1199(9) 0.164 Uiso 1 calc R . H27B H 1.0211(57) 0.9592(50) 0.0746(36) 0.164 Uiso 1 calc R . H27C H 1.0163(60) 0.8504(41) 0.0778(38) 0.164 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0590(3) 0.0595(3) 0.0472(3) 0.0038(3) -0.0002(2) 0.0002(3) Pd1 0.0551(6) 0.0667(7) 0.0550(6) 0.0049(5) 0.0011(4) -0.0021(5) Pd2 0.0543(7) 0.0555(7) 0.0489(6) 0.0035(5) 0.0006(5) -0.0010(6) S1 0.092(3) 0.068(2) 0.059(2) 0.003(2) 0.007(2) -0.006(2) S2 0.082(2) 0.069(2) 0.065(2) 0.005(2) 0.005(2) 0.003(2) S3 0.091(3) 0.068(2) 0.056(2) 0.005(2) 0.004(2) -0.007(2) S4 0.086(3) 0.076(3) 0.065(2) -0.005(2) 0.002(2) 0.002(2) S5 0.062(2) 0.070(2) 0.061(2) 0.001(2) -0.001(2) 0.003(2) S6 0.061(2) 0.069(2) 0.057(2) 0.000(2) -0.004(2) -0.005(2) S7 0.061(2) 0.072(2) 0.060(2) -0.004(2) -0.006(2) 0.002(2) S8 0.061(2) 0.076(2) 0.059(2) 0.002(2) 0.006(2) -0.005(2) N1 0.123(12) 0.109(11) 0.061(8) 0.007(9) 0.003(8) 0.010(9) N2 0.117(11) 0.098(11) 0.093(10) 0.027(9) -0.007(8) -0.004(9) N3 0.121(11) 0.084(10) 0.059(8) 0.018(7) 0.007(7) -0.002(8) N4 0.107(11) 0.170(16) 0.063(8) -0.021(10) 0.004(8) 0.015(11) N5 0.088(9) 0.151(14) 0.073(8) 0.004(9) 0.027(7) -0.009(10) N6 0.112(11) 0.106(11) 0.076(9) -0.001(8) -0.017(8) -0.016(9) N7 0.123(12) 0.134(13) 0.057(8) -0.013(9) -0.010(8) 0.010(10) N8 0.133(13) 0.114(12) 0.080(9) -0.021(9) 0.035(9) 0.000(10) N9 0.050(6) 0.056(7) 0.058(7) 0.007(5) -0.017(5) 0.000(5) N10 0.067(7) 0.080(8) 0.055(7) -0.003(6) 0.005(6) 0.004(7) N11 0.050(7) 0.080(8) 0.069(7) 0.004(6) -0.007(6) 0.011(6) N12 0.065(7) 0.067(7) 0.055(7) 0.001(6) -0.001(6) 0.013(6) C1 0.072(9) 0.085(11) 0.039(7) 0.000(7) 0.010(6) 0.009(8) C2 0.067(9) 0.089(12) 0.061(9) 0.019(9) -0.019(7) -0.009(8) C3 0.057(9) 0.084(12) 0.065(8) 0.015(8) 0.000(7) 0.002(8) C4 0.075(10) 0.074(10) 0.066(9) 0.012(8) 0.012(7) 0.001(8) C5 0.066(9) 0.085(11) 0.041(7) 0.013(8) -0.004(6) 0.004(8) C6 0.079(10) 0.086(11) 0.059(9) -0.010(9) -0.004(8) 0.020(9) C7 0.056(8) 0.089(12) 0.052(8) -0.011(8) -0.003(6) 0.006(8) C8 0.066(9) 0.078(10) 0.080(10) -0.024(9) -0.005(8) 0.002(8) C9 0.079(10) 0.091(11) 0.053(8) 0.006(7) -0.006(7) 0.011(9) C10 0.076(10) 0.095(13) 0.072(10) 0.003(9) 0.010(9) 0.011(9) C11 0.063(9) 0.063(8) 0.060(8) -0.002(7) -0.010(7) -0.013(7) C12 0.072(10) 0.074(11) 0.071(10) 0.010(8) -0.003(8) 0.000(8) C13 0.098(12) 0.081(11) 0.061(9) 0.007(8) -0.005(8) 0.020(10) C14 0.081(11) 0.095(13) 0.079(11) -0.002(10) 0.001(9) 0.021(10) C15 0.077(10) 0.050(8) 0.068(9) 0.012(7) 0.016(7) 0.002(8) C16 0.099(12) 0.095(12) 0.053(9) -0.003(8) 0.003(8) -0.020(10) C17 0.042(8) 0.071(9) 0.064(9) 0.015(7) 0.021(7) 0.014(7) C18 0.074(10) 0.089(11) 0.073(9) -0.011(8) -0.019(8) -0.010(9) C19 0.057(8) 0.075(10) 0.049(8) 0.003(7) 0.006(7) -0.005(7) C20 0.105(12) 0.124(15) 0.064(9) 0.009(10) -0.026(9) -0.018(11) C21 0.043(8) 0.055(9) 0.066(8) 0.001(6) -0.026(7) 0.002(6) C22 0.051(9) 0.129(14) 0.091(11) -0.001(10) 0.015(8) 0.012(9) C23 0.054(8) 0.071(10) 0.050(8) 0.000(7) -0.030(7) 0.012(7) C24 0.072(10) 0.121(14) 0.080(10) 0.004(10) 0.019(8) 0.017(10) N13 0.084(11) 0.149(16) 0.145(15) -0.021(12) -0.022(10) -0.011(11) N14 0.196(22) 0.107(13) 0.111(15) -0.014(12) 0.016(13) -0.016(14) C28 0.136(19) 0.087(13) 0.082(14) -0.023(12) 0.014(12) -0.011(13) C26 0.104(14) 0.085(13) 0.086(12) 0.010(10) -0.003(11) 0.005(11) C25 0.107(14) 0.163(20) 0.089(12) -0.004(13) 0.005(11) -0.009(14) C27 0.086(12) 0.115(15) 0.127(15) 0.022(13) -0.013(11) -0.013(11) _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 C21 1.970(15) . ? Pt1 C19 1.968(14) . ? Pt1 C17 1.98(2) . ? Pt1 C23 1.982(15) . ? Pd1 S1 2.261(4) . ? Pd1 S2 2.264(4) . ? Pd1 S3 2.267(4) . ? Pd1 S4 2.264(4) . ? Pd2 S6 2.271(3) . ? Pd2 S7 2.280(4) . ? Pd2 S8 2.291(4) . ? Pd2 S5 2.302(4) . ? Pd2 Pd2' 2.359(11) 1_565 ? Pd2 Pd2' 2.457(11) 3_655 ? Pd2' S5 2.255(11) 3_655 ? Pd2' S8 2.251(11) 1_545 ? Pd2' S6 2.356(11) 1_545 ? Pd2' Pd2 2.359(11) 1_545 ? Pd2' Pd2 2.457(11) 3_655 ? Pd2' S7 2.475(11) 3_655 ? S1 C1 1.687(14) . ? S2 C3 1.723(14) . ? S3 C5 1.736(13) . ? S4 C7 1.70(2) . ? S5 C9 1.675(14) . ? S5 Pd2' 2.255(11) 3_655 ? S6 C11 1.714(13) . ? S6 Pd2' 2.356(11) 1_565 ? S7 C13 1.719(15) . ? S7 Pd2' 2.475(11) 3_655 ? S8 C15 1.701(15) . ? S8 Pd2' 2.251(11) 1_565 ? N1 C2 1.14(2) . ? N2 C4 1.16(2) . ? N3 C6 1.16(2) . ? N4 C8 1.14(2) . ? N5 C10 1.12(2) . ? N6 C12 1.14(2) . ? N7 C14 1.12(2) . ? N8 C16 1.12(2) . ? N9 C17 1.136(15) . ? N9 C18 1.43(2) . ? N10 C19 1.130(15) . ? N10 C20 1.44(2) . ? N11 C21 1.144(15) . ? N11 C22 1.43(2) . ? N12 C23 1.135(15) . ? N12 C24 1.41(2) . ? C1 C3 1.38(2) . ? C1 C2 1.45(2) . ? C3 C4 1.39(2) . ? C5 C7 1.33(2) . ? C5 C6 1.42(2) . ? C7 C8 1.44(2) . ? C9 C11 1.40(2) . ? C9 C10 1.45(2) . ? C11 C12 1.43(2) . ? C13 C15 1.40(2) . ? C13 C14 1.43(2) . ? C15 C16 1.47(2) . ? N13 C26 1.10(2) . ? N14 C28 1.08(2) . ? C28 C27 1.44(2) . ? C26 C25 1.49(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 C21 Pt1 C19 89.8(5) . . ? C21 Pt1 C17 90.3(4) . . ? C19 Pt1 C17 177.4(6) . . ? C21 Pt1 C23 178.8(6) . . ? C19 Pt1 C23 90.8(5) . . ? C17 Pt1 C23 89.0(5) . . ? S1 Pd1 S2 89.98(14) . . ? S1 Pd1 S3 89.07(14) . . ? S2 Pd1 S3 177.45(15) . . ? S1 Pd1 S4 178.4(2) . . ? S2 Pd1 S4 90.89(14) . . ? S3 Pd1 S4 90.01(14) . . ? S6 Pd2 S7 178.85(14) . . ? S6 Pd2 S8 89.50(13) . . ? S7 Pd2 S8 90.07(13) . . ? S6 Pd2 S5 90.63(13) . . ? S7 Pd2 S5 89.78(13) . . ? S8 Pd2 S5 178.43(14) . . ? S6 Pd2 Pd2' 61.2(3) . 1_565 ? S7 Pd2 Pd2' 117.7(3) . 1_565 ? S8 Pd2 Pd2' 57.9(3) . 1_565 ? S5 Pd2 Pd2' 120.9(3) . 1_565 ? S6 Pd2 Pd2' 116.5(2) . 3_655 ? S7 Pd2 Pd2' 62.9(3) . 3_655 ? S8 Pd2 Pd2' 122.2(3) . 3_655 ? S5 Pd2 Pd2' 56.4(3) . 3_655 ? Pd2' Pd2 Pd2' 89.4(4) 1_565 3_655 ? S5 Pd2' S8 96.5(4) 3_655 1_545 ? S5 Pd2' S6 174.2(5) 3_655 1_545 ? S8 Pd2' S6 88.3(4) 1_545 1_545 ? S5 Pd2' Pd2 122.4(5) 3_655 1_545 ? S8 Pd2' Pd2 59.5(3) 1_545 1_545 ? S6 Pd2' Pd2 57.6(3) 1_545 1_545 ? S5 Pd2' Pd2 58.3(3) 3_655 3_655 ? S8 Pd2' Pd2 123.6(5) 1_545 3_655 ? S6 Pd2' Pd2 116.2(4) 1_545 3_655 ? Pd2 Pd2' Pd2 90.6(4) 1_545 3_655 ? S5 Pd2' S7 86.1(4) 3_655 3_655 ? S8 Pd2' S7 175.6(5) 1_545 3_655 ? S6 Pd2' S7 88.8(3) 1_545 3_655 ? Pd2 Pd2' S7 116.1(4) 1_545 3_655 ? Pd2 Pd2' S7 55.1(2) 3_655 3_655 ? C1 S1 Pd1 102.2(5) . . ? C3 S2 Pd1 103.2(5) . . ? C5 S3 Pd1 101.2(5) . . ? C7 S4 Pd1 102.6(5) . . ? C9 S5 Pd2' 124.8(6) . 3_655 ? C9 S5 Pd2 101.6(5) . . ? Pd2' S5 Pd2 65.3(3) 3_655 . ? C11 S6 Pd2 101.7(4) . . ? C11 S6 Pd2' 128.5(5) . 1_565 ? Pd2 S6 Pd2' 61.3(3) . 1_565 ? C13 S7 Pd2 102.7(6) . . ? C13 S7 Pd2' 130.2(6) . 3_655 ? Pd2 S7 Pd2' 62.1(3) . 3_655 ? C15 S8 Pd2' 127.2(5) . 1_565 ? C15 S8 Pd2 102.5(5) . . ? Pd2' S8 Pd2 62.6(3) 1_565 . ? C17 N9 C18 177.4(13) . . ? C19 N10 C20 175.0(15) . . ? C21 N11 C22 178.5(13) . . ? C23 N12 C24 175.8(15) . . ? C3 C1 C2 117.8(13) . . ? C3 C1 S1 124.8(10) . . ? C2 C1 S1 117.4(12) . . ? N1 C2 C1 178.7(16) . . ? C1 C3 C4 122.0(13) . . ? C1 C3 S2 119.7(10) . . ? C4 C3 S2 118.1(12) . . ? N2 C4 C3 178.0(16) . . ? C7 C5 C6 122.4(12) . . ? C7 C5 S3 123.2(11) . . ? C6 C5 S3 114.4(12) . . ? N3 C6 C5 179.4(17) . . ? C5 C7 C8 118.7(13) . . ? C5 C7 S4 122.9(10) . . ? C8 C7 S4 118.4(12) . . ? N4 C8 C7 177.8(17) . . ? C11 C9 C10 119.6(13) . . ? C11 C9 S5 123.6(11) . . ? C10 C9 S5 116.7(11) . . ? N5 C10 C9 178.6(19) . . ? C9 C11 C12 121.5(12) . . ? C9 C11 S6 122.4(10) . . ? C12 C11 S6 116.0(10) . . ? N6 C12 C11 175.5(17) . . ? C15 C13 C14 120.3(13) . . ? C15 C13 S7 121.8(11) . . ? C14 C13 S7 117.9(12) . . ? N7 C14 C13 179.2(17) . . ? C13 C15 C16 120.9(13) . . ? C13 C15 S8 122.9(10) . . ? C16 C15 S8 116.2(11) . . ? N8 C16 C15 176.9(17) . . ? N9 C17 Pt1 178.6(12) . . ? N10 C19 Pt1 177.6(13) . . ? N11 C21 Pt1 177.1(11) . . ? N12 C23 Pt1 177.8(10) . . ? N14 C28 C27 176.2(26) . . ? N13 C26 C25 177.3(21) . . ? _refine_diff_density_max 1.078 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.122 #=END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H15 N13 O2 Pt3 S8' _chemical_formula_weight 1371.234 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 1 2(1)/c 1' 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 15.913(3) _cell_length_b 16.807(3) _cell_length_c 14.799(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.417(3) _cell_angle_gamma 90.00 _cell_volume 3933.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 272 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 24.00 _exptl_crystal_description needles _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_method ? _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 11.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.119 _exptl_absorpt_correction_T_max 0.327 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.8 _diffrn_reflns_number 14791 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5600 _reflns_number_observed 4374 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+95.7607P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5592 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_obs 0.0677 _refine_ls_wR_factor_all 0.1755 _refine_ls_wR_factor_obs 0.1542 _refine_ls_goodness_of_fit_all 1.262 _refine_ls_goodness_of_fit_obs 1.294 _refine_ls_restrained_S_all 1.288 _refine_ls_restrained_S_obs 1.294 _refine_ls_shift/esd_max 0.283 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt -0.31370(5) -0.29374(5) 0.74080(5) 0.0436(3) Uani 1 d . . Pt2 Pt -0.60845(5) 0.21035(5) 0.56104(5) 0.0401(2) Uani 1 d . . Pt3 Pt -0.00171(5) 0.20078(5) 0.89289(5) 0.0442(3) Uani 1 d . . S1 S -0.7039(3) 0.3024(3) 0.5033(4) 0.0471(13) Uani 1 d . . S2 S -0.5181(3) 0.3076(3) 0.6136(4) 0.0506(13) Uani 1 d . . S3 S -0.5121(3) 0.1189(3) 0.6178(4) 0.0509(13) Uani 1 d . . S4 S -0.6984(3) 0.1119(3) 0.5076(4) 0.0477(13) Uani 1 d . . S5 S -0.1023(3) 0.2951(3) 0.9047(4) 0.0528(14) Uani 1 d . . S6 S 0.0961(4) 0.2972(3) 0.8828(4) 0.0549(14) Uani 1 d . . S7 S 0.0960(4) 0.1053(3) 0.8748(4) 0.0543(14) Uani 1 d . . S8 S -0.1014(4) 0.1057(4) 0.9003(4) 0.0581(15) Uani 1 d . . N1 N -0.4992(13) -0.2886(11) 0.6441(12) 0.054(5) Uani 1 d . . N2 N -0.3062(9) -0.1098(9) 0.7397(9) 0.021(3) Uiso 1 d . . N3 N -0.1283(11) -0.2985(9) 0.8319(11) 0.041(4) Uani 1 d . . N4 N -0.3121(12) -0.4772(14) 0.7327(13) 0.065(5) Uani 1 d . . N5 N -0.7255(17) 0.5235(15) 0.4858(18) 0.092(8) Uani 1 d . . N6 N -0.5013(16) 0.5235(13) 0.6216(17) 0.091(8) Uani 1 d . . N7 N -0.4902(14) -0.0976(12) 0.6473(16) 0.075(6) Uani 1 d . . N8 N -0.7082(16) -0.1092(13) 0.5096(18) 0.091(7) Uani 1 d . . N9 N -0.1352(16) 0.5117(14) 0.8848(18) 0.091(8) Uani 1 d . . N10 N 0.1107(16) 0.5159(15) 0.8607(18) 0.094(8) Uani 1 d . . N11 N 0.1091(15) -0.1101(14) 0.8323(16) 0.083(7) Uani 1 d . . N12 N -0.1320(14) -0.1087(12) 0.8684(16) 0.078(6) Uani 1 d . . C1 C -0.4320(15) -0.2910(11) 0.6774(14) 0.044(5) Uani 1 d . . C2 C -0.5831(14) -0.2834(14) 0.6022(17) 0.063(6) Uani 1 d . . H2A H -0.5917(31) -0.2324(37) 0.5734(90) 0.095 Uiso 1 calc R . H2B H -0.6215(14) -0.2895(91) 0.6472(23) 0.095 Uiso 1 calc R . H2C H -0.5930(32) -0.3246(57) 0.5574(74) 0.095 Uiso 1 calc R . C3 C -0.3097(12) -0.1666(21) 0.7392(15) 0.067(8) Uani 1 d . . C4 C -0.2987(14) -0.0246(12) 0.7361(15) 0.056(6) Uani 1 d . . H4A H -0.3441(52) -0.0006(12) 0.7639(87) 0.084 Uiso 1 calc R . H4B H -0.3015(90) -0.0078(14) 0.6738(15) 0.084 Uiso 1 calc R . H4C H -0.2456(41) -0.0085(14) 0.7680(82) 0.084 Uiso 1 calc R . C5 C -0.1954(16) -0.2968(14) 0.7976(15) 0.056(6) Uani 1 d . . C6 C -0.0387(14) -0.3015(15) 0.8673(17) 0.068(7) Uani 1 d . . H6A H -0.0335(14) -0.3125(95) 0.9313(27) 0.102 Uiso 1 calc R . H6B H -0.0127(27) -0.2512(35) 0.8572(99) 0.102 Uiso 1 calc R . H6C H -0.0111(26) -0.3426(66) 0.8367(79) 0.102 Uiso 1 calc R . C7 C -0.3129(13) -0.4096(14) 0.7361(13) 0.045(5) Uani 1 d . . C8 C -0.3082(14) -0.5634(11) 0.7281(16) 0.057(6) Uani 1 d . . H8A H -0.3581(44) -0.5856(11) 0.7489(93) 0.086 Uiso 1 calc R . H8B H -0.2592(51) -0.5819(12) 0.7659(76) 0.086 Uiso 1 calc R . H8C H -0.3047(91) -0.5795(11) 0.6664(22) 0.086 Uiso 1 calc R . C9 C -0.6452(14) 0.3878(12) 0.5347(13) 0.041(5) Uiso 1 d . . C10 C -0.6942(15) 0.4642(14) 0.5077(15) 0.052(6) Uani 1 d . . C11 C -0.5866(11) 0.3860(9) 0.5743(12) 0.030(4) Uani 1 d . . C12 C -0.5308(16) 0.4629(14) 0.6078(17) 0.060(6) Uani 1 d . . C13 C -0.5617(14) 0.0314(14) 0.5883(15) 0.056(6) Uani 1 d . . C14 C -0.5206(14) -0.0398(11) 0.6233(15) 0.050(5) Uani 1 d . . C15 C -0.6426(15) 0.0289(12) 0.5457(15) 0.052(6) Uani 1 d . . C16 C -0.6802(16) -0.0477(14) 0.5210(17) 0.061(6) Uani 1 d . . C17 C -0.0334(21) 0.3827(15) 0.8943(17) 0.061(8) Uani 1 d . . C18 C -0.0950(16) 0.4570(18) 0.8914(16) 0.067(7) Uani 1 d . . C19 C 0.0263(18) 0.3824(12) 0.8854(14) 0.044(6) Uani 1 d . . C20 C 0.0786(14) 0.4589(15) 0.8722(16) 0.056(6) Uani 1 d . . C21 C 0.0405(14) 0.0200(12) 0.8721(14) 0.049(5) Uani 1 d . . C22 C 0.0767(15) -0.0531(14) 0.8520(17) 0.061(6) Uani 1 d . . C23 C -0.0493(15) 0.0203(14) 0.8828(14) 0.057(6) Uani 1 d . . C24 C -0.0954(16) -0.0508(14) 0.8761(17) 0.065(7) Uani 1 d . . N13 N -0.7237(15) -0.2953(17) 0.8023(20) 0.092(8) Uani 1 d . . C25 C -0.8065(18) -0.2923(17) 0.8439(20) 0.086(8) Uani 1 d . . H25A H -0.8228(68) -0.3453(20) 0.8588(130) 0.129 Uiso 1 calc R . H25B H -0.8495(36) -0.2694(113) 0.8011(55) 0.129 Uiso 1 calc R . H25C H -0.7996(40) -0.2605(101) 0.8980(78) 0.129 Uiso 1 calc R . O1 O -0.6837(18) -0.2375(18) 0.8088(31) 0.209(19) Uani 1 d . . O2 O -0.7052(17) -0.3537(16) 0.7657(21) 0.147(12) Uani 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 0.0461(5) 0.0373(5) 0.0482(5) -0.0004(4) 0.0087(4) 0.0002(4) Pt2 0.0392(4) 0.0389(5) 0.0427(4) 0.0008(4) 0.0069(3) 0.0000(4) Pt3 0.0445(5) 0.0411(5) 0.0470(5) -0.0023(4) 0.0048(4) -0.0013(4) S1 0.047(3) 0.045(3) 0.050(3) -0.003(2) 0.004(2) 0.005(3) S2 0.039(3) 0.048(3) 0.063(3) 0.000(3) -0.004(2) -0.004(3) S3 0.044(3) 0.045(3) 0.063(3) -0.004(3) 0.000(3) -0.001(3) S4 0.039(3) 0.048(3) 0.054(3) -0.004(3) -0.004(2) 0.002(3) S5 0.044(3) 0.044(3) 0.070(4) -0.003(3) 0.004(3) 0.002(3) S6 0.047(3) 0.042(3) 0.077(4) -0.004(3) 0.014(3) -0.002(3) S7 0.049(3) 0.046(3) 0.069(4) 0.002(3) 0.009(3) 0.001(3) S8 0.048(3) 0.053(4) 0.074(4) -0.002(3) 0.008(3) -0.005(3) N1 0.054(13) 0.051(12) 0.054(11) -0.010(9) -0.002(10) -0.008(10) N3 0.049(11) 0.027(9) 0.046(10) -0.011(7) -0.003(9) -0.002(8) N4 0.061(13) 0.073(16) 0.060(12) 0.000(11) -0.003(10) 0.012(12) N5 0.106(20) 0.071(17) 0.104(19) 0.011(15) 0.025(15) 0.009(15) N6 0.100(19) 0.049(14) 0.122(21) 0.030(14) 0.002(15) 0.020(14) N7 0.077(15) 0.038(12) 0.108(17) -0.008(11) 0.000(12) 0.013(11) N8 0.095(18) 0.051(15) 0.124(21) -0.013(14) -0.008(15) 0.007(13) N9 0.088(18) 0.065(15) 0.124(21) 0.000(14) 0.025(15) 0.044(14) N10 0.082(17) 0.078(18) 0.126(22) 0.009(16) 0.030(16) -0.007(15) N11 0.084(16) 0.069(16) 0.092(17) -0.005(13) -0.002(13) 0.024(13) N12 0.076(15) 0.048(13) 0.107(18) 0.023(12) -0.005(13) -0.002(12) C1 0.059(14) 0.023(10) 0.051(12) 0.002(9) 0.010(11) -0.019(10) C2 0.051(14) 0.065(16) 0.074(16) 0.015(13) 0.008(12) -0.001(12) C3 0.016(10) 0.139(28) 0.049(14) -0.001(15) 0.007(9) -0.021(13) C4 0.054(14) 0.046(14) 0.066(15) -0.005(11) 0.002(11) -0.008(11) C5 0.069(17) 0.055(15) 0.044(12) -0.014(11) 0.010(12) -0.012(13) C6 0.052(14) 0.069(17) 0.076(16) -0.002(13) -0.024(12) 0.010(13) C7 0.050(13) 0.047(14) 0.040(12) -0.004(10) 0.016(10) 0.006(11) C8 0.063(15) 0.013(10) 0.092(18) -0.006(10) -0.007(13) 0.008(10) C10 0.066(15) 0.041(13) 0.050(13) 0.004(11) 0.010(11) -0.016(12) C11 0.037(11) 0.006(8) 0.053(11) 0.013(8) 0.030(9) 0.022(7) C12 0.070(16) 0.034(13) 0.081(17) 0.004(12) 0.028(14) -0.004(12) C13 0.047(14) 0.070(16) 0.052(13) -0.012(12) 0.014(11) 0.006(12) C14 0.059(14) 0.019(11) 0.069(14) -0.007(10) -0.008(11) 0.018(10) C15 0.064(15) 0.023(11) 0.070(15) -0.003(10) 0.013(12) 0.007(10) C16 0.074(17) 0.033(13) 0.076(16) -0.004(12) 0.006(13) -0.006(12) C17 0.114(24) 0.029(13) 0.041(13) -0.004(10) 0.007(16) 0.041(17) C18 0.056(16) 0.094(21) 0.053(14) -0.007(14) 0.017(12) -0.007(15) C19 0.096(20) 0.008(10) 0.028(11) -0.001(8) 0.009(13) -0.002(13) C20 0.041(13) 0.066(16) 0.064(15) -0.004(12) 0.028(11) 0.002(12) C21 0.053(13) 0.037(12) 0.060(13) -0.003(10) 0.023(11) -0.001(10) C22 0.054(14) 0.048(15) 0.080(17) -0.024(13) 0.003(12) 0.002(12) C23 0.069(16) 0.058(15) 0.045(13) 0.008(11) 0.006(11) -0.013(13) C24 0.074(18) 0.040(14) 0.078(17) 0.003(12) 0.003(13) -0.006(13) N13 0.058(15) 0.084(19) 0.130(22) 0.015(17) -0.010(14) -0.024(15) C25 0.080(20) 0.080(20) 0.096(21) 0.012(16) -0.007(16) 0.011(16) O1 0.103(21) 0.105(21) 0.429(60) -0.049(29) 0.072(29) -0.042(18) O2 0.150(25) 0.089(18) 0.215(31) -0.042(19) 0.084(22) 0.000(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 Pt1 C7 1.95(2) . ? Pt1 C5 1.98(3) . ? Pt1 C1 2.01(2) . ? Pt1 C3 2.14(4) . ? Pt2 S2 2.257(5) . ? Pt2 S3 2.265(6) . ? Pt2 S1 2.267(5) . ? Pt2 S4 2.272(5) . ? Pt3 S6 2.264(6) . ? Pt3 S8 2.263(6) . ? Pt3 S7 2.271(6) . ? Pt3 S5 2.274(5) . ? S1 C9 1.75(2) . ? S2 C11 1.77(2) . ? S3 C13 1.70(2) . ? S4 C15 1.71(2) . ? S5 C17 1.85(3) . ? S6 C19 1.82(2) . ? S7 C21 1.68(2) . ? S8 C23 1.69(2) . ? N1 C1 1.13(3) . ? N1 C2 1.41(3) . ? N2 C3 0.96(3) . ? N2 C4 1.44(2) . ? N3 C5 1.13(3) . ? N3 C6 1.46(3) . ? N4 C7 1.14(3) . ? N4 C8 1.45(3) . ? N5 C10 1.14(3) . ? N6 C12 1.13(3) . ? N7 C14 1.13(3) . ? N8 C16 1.13(3) . ? N9 C18 1.12(3) . ? N10 C20 1.11(3) . ? N11 C22 1.14(3) . ? N12 C24 1.13(3) . ? C9 C11 1.05(2) . ? C9 C10 1.53(3) . ? C11 C12 1.61(3) . ? C13 C15 1.37(3) . ? C13 C14 1.43(3) . ? C15 C16 1.45(3) . ? C17 C19 0.97(3) . ? C17 C18 1.58(4) . ? C19 C20 1.56(3) . ? C21 C22 1.40(3) . ? C21 C23 1.46(3) . ? C23 C24 1.40(3) . ? N13 O1 1.16(3) . ? N13 O2 1.17(3) . ? N13 C25 1.52(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 C7 Pt1 C5 88.8(9) . . ? C7 Pt1 C1 90.9(8) . . ? C5 Pt1 C1 177.3(8) . . ? C7 Pt1 C3 176.4(7) . . ? C5 Pt1 C3 90.2(9) . . ? C1 Pt1 C3 90.0(8) . . ? S2 Pt2 S3 89.2(2) . . ? S2 Pt2 S1 90.5(2) . . ? S3 Pt2 S1 179.4(2) . . ? S2 Pt2 S4 179.5(2) . . ? S3 Pt2 S4 90.5(2) . . ? S1 Pt2 S4 89.8(2) . . ? S6 Pt3 S8 178.7(2) . . ? S6 Pt3 S7 90.8(2) . . ? S8 Pt3 S7 90.0(2) . . ? S6 Pt3 S5 90.0(2) . . ? S8 Pt3 S5 89.2(2) . . ? S7 Pt3 S5 177.5(2) . . ? C9 S1 Pt2 98.3(8) . . ? C11 S2 Pt2 94.7(7) . . ? C13 S3 Pt2 102.5(8) . . ? C15 S4 Pt2 101.2(8) . . ? C17 S5 Pt3 96.9(8) . . ? C19 S6 Pt3 97.9(8) . . ? C21 S7 Pt3 103.9(7) . . ? C23 S8 Pt3 103.5(8) . . ? C1 N1 C2 178.4(23) . . ? C3 N2 C4 176.9(22) . . ? C5 N3 C6 174.3(21) . . ? C7 N4 C8 178.2(24) . . ? N1 C1 Pt1 177.9(18) . . ? N2 C3 Pt1 178.1(22) . . ? N3 C5 Pt1 178.5(19) . . ? N4 C7 Pt1 179.4(18) . . ? C11 C9 C10 124.4(21) . . ? C11 C9 S1 122.9(19) . . ? C10 C9 S1 112.2(15) . . ? N5 C10 C9 175.1(25) . . ? C9 C11 C12 125.2(19) . . ? C9 C11 S2 133.2(19) . . ? C12 C11 S2 101.5(14) . . ? N6 C12 C11 168.5(27) . . ? C15 C13 C14 120.5(21) . . ? C15 C13 S3 122.0(18) . . ? C14 C13 S3 116.7(17) . . ? N7 C14 C13 176.7(25) . . ? C13 C15 C16 119.0(20) . . ? C13 C15 S4 123.5(18) . . ? C16 C15 S4 117.1(18) . . ? N8 C16 C15 173.9(29) . . ? C19 C17 C18 127.5(33) . . ? C19 C17 S5 127.1(25) . . ? C18 C17 S5 105.0(20) . . ? N9 C18 C17 175.1(27) . . ? C17 C19 C20 123.9(30) . . ? C17 C19 S6 127.9(27) . . ? C20 C19 S6 108.1(17) . . ? N10 C20 C19 175.0(28) . . ? C22 C21 C23 117.3(19) . . ? C22 C21 S7 121.6(16) . . ? C23 C21 S7 120.9(16) . . ? N11 C22 C21 175.9(27) . . ? C24 C23 C21 120.2(22) . . ? C24 C23 S8 118.2(19) . . ? C21 C23 S8 121.6(17) . . ? N12 C24 C23 178.1(29) . . ? O1 N13 O2 125.1(33) . . ? O1 N13 C25 115.6(32) . . ? O2 N13 C25 119.3(26) . . ? _refine_diff_density_max 1.923 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.254 #=END data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H12 N12 Pt3 S8' _chemical_formula_weight 1310.194 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.069(2) _cell_length_b 12.463(3) _cell_length_c 13.514(3) _cell_angle_alpha 100.323(10) _cell_angle_beta 91.272(12) _cell_angle_gamma 96.547(11) _cell_volume 1820.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 195 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.50 _exptl_crystal_description cuboid _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.390 _exptl_crystal_density_method ? _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 11.994 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 0.976 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7818 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5103 _reflns_number_observed 4673 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 47 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+18.6616P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5056 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all 0.1364 _refine_ls_wR_factor_obs 0.1274 _refine_ls_goodness_of_fit_all 1.183 _refine_ls_goodness_of_fit_obs 1.182 _refine_ls_restrained_S_all 1.206 _refine_ls_restrained_S_obs 1.182 _refine_ls_shift/esd_max -0.032 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.0403(2) Uani 1 d S . Pt2 Pt -0.5000 0.5000 0.5000 0.0556(2) Uani 1 d S . Pt3 Pt -0.02489(5) -0.34906(4) 0.04791(4) 0.0468(2) Uani 1 d . . Pt4 Pt -0.21318(5) 0.36686(5) 0.49429(4) 0.0497(2) Uani 1 d . . S1 S 0.0837(3) -0.2646(3) -0.0629(3) 0.0558(9) Uani 1 d . . S2 S 0.1242(4) -0.2871(3) 0.1686(3) 0.0571(9) Uani 1 d . . S3 S -0.1294(4) -0.4365(3) 0.1582(3) 0.0614(10) Uani 1 d . . S4 S -0.1738(3) -0.4159(3) -0.0721(3) 0.0547(9) Uani 1 d . . S5 S -0.1983(4) 0.2484(3) 0.3489(3) 0.0605(9) Uani 1 d . . S6 S -0.2898(4) 0.2262(3) 0.5679(3) 0.0569(9) Uani 1 d . . S7 S -0.2161(4) 0.4834(3) 0.6422(3) 0.0582(9) Uani 1 d . . S8 S -0.1429(4) 0.5082(3) 0.4191(3) 0.0594(9) Uani 1 d . . N1 N 0.2525(11) 0.1317(10) -0.0054(8) 0.049(3) Uani 1 d . . N2 N 0.0477(11) -0.0164(10) 0.2223(10) 0.053(3) Uani 1 d . . N3 N -0.5340(11) 0.2802(11) 0.3447(9) 0.056(3) Uani 1 d . . N4 N -0.5936(11) 0.3469(10) 0.6459(9) 0.056(3) Uani 1 d . . N5 N 0.3711(14) -0.0947(13) -0.0780(13) 0.081(4) Uani 1 d . . N6 N 0.4151(15) -0.1058(15) 0.2149(13) 0.088(5) Uani 1 d . . N7 N -0.4075(16) -0.6247(13) 0.1716(14) 0.094(5) Uani 1 d . . N8 N -0.4601(16) -0.6037(14) -0.1116(14) 0.092(5) Uani 1 d . . N9 N -0.2422(14) -0.0476(12) 0.2416(11) 0.075(4) Uani 1 d . . N10 N -0.3639(14) -0.0741(13) 0.5144(11) 0.078(4) Uani 1 d . . N11 N -0.1598(15) 0.7763(13) 0.7551(12) 0.084(4) Uani 1 d . . N12 N -0.0667(17) 0.8079(15) 0.4713(13) 0.092(5) Uani 1 d . . C1 C 0.1589(13) 0.0850(11) -0.0033(10) 0.045(3) Uani 1 d . . C2 C 0.3705(13) 0.1897(15) -0.0175(15) 0.075(5) Uani 1 d . . H2A H 0.3874(53) 0.2518(64) 0.0363(56) 0.112 Uiso 1 calc R . H2B H 0.3706(40) 0.2145(94) -0.0808(46) 0.112 Uiso 1 calc R . H2C H 0.4318(19) 0.1414(35) -0.0160(100) 0.112 Uiso 1 calc R . C3 C 0.0310(12) -0.0114(10) 0.1418(12) 0.046(3) Uani 1 d . . C4 C 0.0730(20) -0.0252(18) 0.3247(12) 0.089(6) Uani 1 d . . H4A H 0.0341(115) -0.0940(57) 0.3372(33) 0.133 Uiso 1 calc R . H4B H 0.0427(123) 0.0340(72) 0.3689(12) 0.133 Uiso 1 calc R . H4C H 0.1594(21) -0.0215(126) 0.3366(33) 0.133 Uiso 1 calc R . C5 C -0.5179(13) 0.3632(13) 0.3983(11) 0.053(3) Uani 1 d . . C6 C -0.5439(17) 0.1763(13) 0.2774(12) 0.068(4) Uani 1 d . . H6A H -0.6248(36) 0.1595(48) 0.2472(70) 0.102 Uiso 1 calc R . H6B H -0.5275(110) 0.1201(20) 0.3142(21) 0.102 Uiso 1 calc R . H6C H -0.4862(78) 0.1798(34) 0.2258(54) 0.102 Uiso 1 calc R . C7 C -0.5544(12) 0.4085(14) 0.5967(10) 0.053(4) Uani 1 d . . C8 C -0.6414(17) 0.2654(14) 0.7018(13) 0.073(5) Uani 1 d . . H8A H -0.6680(108) 0.3009(14) 0.7652(43) 0.110 Uiso 1 calc R . H8B H -0.5792(39) 0.2207(68) 0.7133(84) 0.110 Uiso 1 calc R . H8C H -0.7091(76) 0.2200(68) 0.6643(45) 0.110 Uiso 1 calc R . C9 C 0.2125(13) -0.2039(12) 0.0079(11) 0.054(4) Uani 1 d . . C10 C 0.3031(14) -0.1426(12) -0.0382(12) 0.054(3) Uani 1 d . . C11 C 0.2276(12) -0.2120(11) 0.1086(10) 0.050(3) Uani 1 d . . C12 C 0.3345(14) -0.1524(14) 0.1659(12) 0.060(4) Uani 1 d . . C13 C -0.2562(15) -0.5017(12) 0.0864(11) 0.056(4) Uani 1 d . . C14 C -0.3422(16) -0.5695(13) 0.1328(13) 0.065(4) Uani 1 d . . C15 C -0.2722(13) -0.4948(11) -0.0111(11) 0.052(3) Uani 1 d . . C16 C -0.3769(16) -0.5539(14) -0.0659(14) 0.069(4) Uani 1 d . . C17 C -0.2493(13) 0.1264(12) 0.3789(10) 0.054(3) Uani 1 d . . C18 C -0.2458(14) 0.0276(13) 0.3030(11) 0.057(4) Uani 1 d . . C19 C -0.2883(13) 0.1158(12) 0.4735(9) 0.050(3) Uani 1 d . . C20 C -0.3324(14) 0.0098(15) 0.4969(11) 0.058(4) Uani 1 d . . C21 C -0.1661(13) 0.6087(11) 0.6122(12) 0.055(4) Uani 1 d . . C22 C -0.1619(15) 0.7030(14) 0.6892(13) 0.064(4) Uani 1 d . . C23 C -0.1363(12) 0.6184(12) 0.5178(11) 0.050(3) Uani 1 d . . C24 C -0.0940(17) 0.7274(15) 0.4939(13) 0.068(4) Uani 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 0.0402(4) 0.0432(4) 0.0395(4) 0.0105(3) 0.0077(3) 0.0075(3) Pt2 0.0535(5) 0.0593(5) 0.0518(5) 0.0114(4) 0.0013(4) -0.0049(4) Pt3 0.0526(3) 0.0503(3) 0.0415(3) 0.0122(2) 0.0120(2) 0.0150(2) Pt4 0.0520(3) 0.0584(4) 0.0392(3) 0.0116(2) 0.0033(2) 0.0037(2) S1 0.055(2) 0.068(2) 0.052(2) 0.025(2) 0.016(2) 0.017(2) S2 0.064(2) 0.066(2) 0.043(2) 0.013(2) 0.008(2) 0.008(2) S3 0.072(2) 0.066(2) 0.049(2) 0.018(2) 0.014(2) 0.008(2) S4 0.062(2) 0.061(2) 0.044(2) 0.017(2) 0.007(2) 0.008(2) S5 0.067(2) 0.068(2) 0.045(2) 0.011(2) 0.011(2) 0.000(2) S6 0.073(2) 0.061(2) 0.036(2) 0.010(2) 0.013(2) 0.005(2) S7 0.073(2) 0.057(2) 0.043(2) 0.010(2) 0.006(2) -0.002(2) S8 0.069(2) 0.071(2) 0.042(2) 0.020(2) 0.008(2) 0.009(2) N1 0.049(7) 0.061(7) 0.038(6) 0.006(5) 0.009(5) 0.013(6) N2 0.054(7) 0.054(7) 0.048(8) 0.006(6) 0.011(6) 0.001(5) N3 0.054(7) 0.061(8) 0.052(7) 0.014(7) -0.002(6) -0.006(6) N4 0.059(7) 0.057(7) 0.046(7) 0.002(6) -0.005(6) -0.002(6) N5 0.076(10) 0.082(10) 0.094(11) 0.032(9) 0.027(9) 0.019(8) N6 0.072(10) 0.105(12) 0.083(11) 0.020(9) -0.007(9) -0.001(9) N7 0.103(12) 0.072(10) 0.114(14) 0.041(10) 0.030(11) -0.001(9) N8 0.085(11) 0.085(11) 0.099(13) 0.002(9) 0.003(10) 0.000(9) N9 0.099(11) 0.066(9) 0.055(8) 0.001(7) 0.020(7) 0.004(8) N10 0.091(11) 0.072(10) 0.071(10) 0.014(8) 0.016(8) 0.006(8) N11 0.104(12) 0.066(9) 0.074(10) 0.006(8) 0.006(9) -0.009(8) N12 0.117(14) 0.087(12) 0.082(11) 0.041(10) 0.020(10) 0.009(10) C1 0.041(8) 0.054(8) 0.045(8) 0.014(6) 0.015(6) 0.014(6) C2 0.042(8) 0.087(12) 0.095(13) 0.025(10) 0.018(8) -0.008(8) C3 0.043(7) 0.038(7) 0.057(10) 0.009(6) 0.007(6) 0.007(5) C4 0.116(15) 0.124(17) 0.033(9) 0.029(9) -0.009(9) 0.021(12) C5 0.055(8) 0.061(9) 0.042(8) 0.012(7) 0.007(6) -0.001(7) C6 0.091(12) 0.056(9) 0.056(9) 0.009(8) 0.017(8) 0.005(8) C7 0.044(8) 0.076(10) 0.037(7) 0.001(7) 0.009(6) 0.011(7) C8 0.090(12) 0.067(10) 0.062(10) 0.018(8) -0.002(9) -0.007(9) C9 0.049(8) 0.060(9) 0.057(9) 0.005(7) 0.008(7) 0.029(7) C10 0.057(9) 0.054(8) 0.060(9) 0.020(7) 0.019(7) 0.020(7) C11 0.048(8) 0.056(8) 0.047(8) 0.001(6) 0.017(6) 0.024(6) C12 0.053(9) 0.080(11) 0.051(9) 0.011(8) 0.010(8) 0.025(8) C13 0.076(10) 0.046(8) 0.047(9) 0.004(6) 0.016(7) 0.011(7) C14 0.078(11) 0.053(9) 0.067(10) 0.013(8) 0.035(9) 0.012(8) C15 0.058(8) 0.049(8) 0.050(8) 0.009(6) 0.008(7) 0.014(7) C16 0.069(11) 0.053(9) 0.087(12) 0.014(9) -0.005(10) 0.020(8) C17 0.056(8) 0.059(9) 0.044(8) 0.002(7) -0.007(6) 0.004(7) C18 0.062(9) 0.066(10) 0.041(8) 0.007(8) 0.012(7) 0.003(7) C19 0.059(8) 0.061(9) 0.029(7) 0.011(6) 0.000(6) 0.007(7) C20 0.058(9) 0.072(11) 0.040(8) 0.007(7) -0.002(6) 0.001(8) C21 0.058(8) 0.041(8) 0.065(10) 0.010(7) -0.002(7) 0.002(6) C22 0.066(10) 0.064(10) 0.065(11) 0.027(9) 0.007(8) -0.003(8) C23 0.039(7) 0.061(9) 0.055(9) 0.028(7) 0.003(6) 0.007(6) C24 0.083(12) 0.067(11) 0.056(10) 0.016(8) 0.008(8) 0.011(9) _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 C1 1.953(15) 2 ? Pt1 C1 1.953(15) . ? Pt1 C3 1.97(2) . ? Pt1 C3 1.97(2) 2 ? Pt2 C7 1.94(2) 2_466 ? Pt2 C7 1.94(2) . ? Pt2 C5 1.98(2) 2_466 ? Pt2 C5 1.98(2) . ? Pt3 S2 2.262(4) . ? Pt3 S3 2.263(4) . ? Pt3 S4 2.264(4) . ? Pt3 S1 2.270(4) . ? Pt4 S7 2.254(4) . ? Pt4 S5 2.258(4) . ? Pt4 S8 2.259(4) . ? Pt4 S6 2.259(4) . ? S1 C9 1.72(2) . ? S2 C11 1.706(15) . ? S3 C13 1.72(2) . ? S4 C15 1.708(15) . ? S5 C17 1.68(2) . ? S6 C19 1.703(14) . ? S7 C21 1.717(14) . ? S8 C23 1.73(2) . ? N1 C1 1.13(2) . ? N1 C2 1.45(2) . ? N2 C3 1.11(2) . ? N2 C4 1.43(2) . ? N3 C5 1.14(2) . ? N3 C6 1.43(2) . ? N4 C7 1.16(2) . ? N4 C8 1.43(2) . ? N5 C10 1.11(2) . ? N6 C12 1.14(2) . ? N7 C14 1.14(2) . ? N8 C16 1.15(2) . ? N9 C18 1.14(2) . ? N10 C20 1.13(2) . ? N11 C22 1.15(2) . ? N12 C24 1.11(2) . ? C9 C11 1.39(2) . ? C9 C10 1.42(2) . ? C11 C12 1.45(2) . ? C13 C15 1.35(2) . ? C13 C14 1.43(2) . ? C15 C16 1.42(2) . ? C17 C19 1.38(2) . ? C17 C18 1.46(2) . ? C19 C20 1.45(2) . ? C21 C23 1.35(2) . ? C21 C22 1.42(2) . ? C23 C24 1.48(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 C1 Pt1 C1 180.0 2 . ? C1 Pt1 C3 88.8(5) 2 . ? C1 Pt1 C3 91.2(5) . . ? C1 Pt1 C3 91.2(5) 2 2 ? C1 Pt1 C3 88.8(5) . 2 ? C3 Pt1 C3 180.0 . 2 ? C7 Pt2 C7 179.997(3) 2_466 . ? C7 Pt2 C5 86.6(6) 2_466 2_466 ? C7 Pt2 C5 93.4(6) . 2_466 ? C7 Pt2 C5 93.4(6) 2_466 . ? C7 Pt2 C5 86.6(6) . . ? C5 Pt2 C5 179.999(2) 2_466 . ? S2 Pt3 S3 89.03(14) . . ? S2 Pt3 S4 178.39(14) . . ? S3 Pt3 S4 89.98(14) . . ? S2 Pt3 S1 90.44(14) . . ? S3 Pt3 S1 178.46(14) . . ? S4 Pt3 S1 90.52(14) . . ? S7 Pt4 S5 176.40(15) . . ? S7 Pt4 S8 90.23(14) . . ? S5 Pt4 S8 89.86(14) . . ? S7 Pt4 S6 89.89(13) . . ? S5 Pt4 S6 90.14(14) . . ? S8 Pt4 S6 178.10(15) . . ? C9 S1 Pt3 102.5(5) . . ? C11 S2 Pt3 102.6(5) . . ? C13 S3 Pt3 102.3(5) . . ? C15 S4 Pt3 102.2(5) . . ? C17 S5 Pt4 102.7(5) . . ? C19 S6 Pt4 102.3(5) . . ? C21 S7 Pt4 103.1(5) . . ? C23 S8 Pt4 101.7(5) . . ? C1 N1 C2 175.0(14) . . ? C3 N2 C4 177.8(16) . . ? C5 N3 C6 175.5(15) . . ? C7 N4 C8 176.6(15) . . ? N1 C1 Pt1 178.1(12) . . ? N2 C3 Pt1 178.9(12) . . ? N3 C5 Pt2 174.5(13) . . ? N4 C7 Pt2 172.9(13) . . ? C11 C9 C10 120.1(14) . . ? C11 C9 S1 121.7(12) . . ? C10 C9 S1 118.2(12) . . ? N5 C10 C9 177.1(18) . . ? C9 C11 C12 118.8(13) . . ? C9 C11 S2 122.8(11) . . ? C12 C11 S2 118.5(11) . . ? N6 C12 C11 176.6(17) . . ? C15 C13 C14 120.4(15) . . ? C15 C13 S3 122.1(12) . . ? C14 C13 S3 117.4(12) . . ? N7 C14 C13 177.7(20) . . ? C13 C15 C16 118.7(15) . . ? C13 C15 S4 123.2(12) . . ? C16 C15 S4 118.1(12) . . ? N8 C16 C15 178.2(19) . . ? C19 C17 C18 119.0(14) . . ? C19 C17 S5 122.8(11) . . ? C18 C17 S5 118.2(11) . . ? N9 C18 C17 177.8(16) . . ? C17 C19 C20 121.5(13) . . ? C17 C19 S6 122.1(11) . . ? C20 C19 S6 116.3(10) . . ? N10 C20 C19 178.0(18) . . ? C23 C21 C22 120.7(13) . . ? C23 C21 S7 121.4(11) . . ? C22 C21 S7 117.9(12) . . ? N11 C22 C21 176.7(17) . . ? C21 C23 C24 120.3(14) . . ? C21 C23 S8 123.5(11) . . ? C24 C23 S8 116.2(11) . . ? N12 C24 C23 176.0(20) . . ? _refine_diff_density_max 1.346 _refine_diff_density_min -1.916 _refine_diff_density_rms 0.237 #=END