# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email deplano@unica.it _publ_contact_author_name 'Paola Deplano' loop_ _publ_author_name 'D. Espa' 'L. Pilia' 'L. Marchio' 'M. Pizzotti' 'N. Robertson' 'F. Tessore' ; F.Artizzu ; 'M. L. Mercuri' 'A. Serpe' P.Deplano data_nise212 _database_code_depnum_ccdc_archive 'CCDC 884915' #TrackingRef '- Ni-Pt_dsit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 N2 S5 Se2' _chemical_formula_sum 'C21 H18 N2 Ni S5 Se2' _chemical_formula_weight 675.30 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' Ni Ni 0.3393 1.1124 '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' Se Se -0.0929 2.2259 '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/n 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 9.256(1) _cell_length_b 23.119(2) _cell_length_c 11.503(1) _cell_angle_alpha 90.00 _cell_angle_beta 98.741(2) _cell_angle_gamma 90.00 _cell_volume 2432.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12549 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 26.16 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker Smart APEXII CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29067 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.16 _reflns_number_total 4861 _reflns_number_gt 2945 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0295P)^2^+0.6561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4861 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C22 C 0.2186(5) 0.1762(2) 0.1386(4) 0.0504(12) Uani 1 1 d . . . C12 C 0.2661(5) 0.1209(2) 0.1368(4) 0.0501(12) Uani 1 1 d . . . C101 C 1.0852(6) 0.4537(2) 0.1570(6) 0.0788(17) Uani 1 1 d . . . H101 H 1.1283 0.4901 0.1587 0.095 Uiso 1 1 calc R . . Se22 Se 0.34214(6) 0.23782(2) 0.19380(5) 0.05823(17) Uani 1 1 d . . . Se12 Se 0.46246(6) 0.10133(2) 0.18892(5) 0.05850(17) Uani 1 1 d . . . Ni Ni 0.55703(6) 0.18916(3) 0.24851(5) 0.04799(17) Uani 1 1 d . . . S21 S 0.75969(14) 0.14390(5) 0.30018(12) 0.0589(3) Uani 1 1 d . . . S22 S 0.03157(14) 0.18544(6) 0.08728(12) 0.0587(4) Uani 1 1 d . . . S12 S 0.13815(15) 0.06871(6) 0.08508(12) 0.0632(4) Uani 1 1 d . . . S11 S 0.65751(14) 0.27037(5) 0.30882(12) 0.0572(3) Uani 1 1 d . . . S32 S -0.17782(16) 0.09031(7) 0.00714(14) 0.0762(4) Uani 1 1 d . . . N11 N 1.0181(4) 0.18006(17) 0.4019(3) 0.0498(10) Uani 1 1 d . . . C11 C 0.8362(5) 0.25554(19) 0.3536(4) 0.0449(11) Uani 1 1 d . . . C171 C 0.9809(7) 0.0783(3) 0.7059(5) 0.0822(18) Uani 1 1 d . . . H171 H 0.9159 0.0887 0.7565 0.099 Uiso 1 1 calc R . . C21 C 0.8815(5) 0.19362(19) 0.3574(4) 0.0448(11) Uani 1 1 d . . . N21 N 0.9364(4) 0.29620(16) 0.3801(3) 0.0481(10) Uani 1 1 d . . . C32 C -0.0136(5) 0.1133(2) 0.0556(4) 0.0561(13) Uani 1 1 d . . . C31 C 1.1140(5) 0.2234(2) 0.4667(4) 0.0609(14) Uani 1 1 d . . . H31A H 1.2152 0.2120 0.4685 0.073 Uiso 1 1 calc R . . H31B H 1.0948 0.2254 0.5472 0.073 Uiso 1 1 calc R . . C131 C 1.0722(5) 0.0913(2) 0.5257(4) 0.0502(12) Uani 1 1 d . . . C61 C 0.9683(5) 0.37948(19) 0.2535(4) 0.0442(11) Uani 1 1 d . . . C181 C 0.9756(6) 0.1074(2) 0.5995(4) 0.0667(15) Uani 1 1 d . . . H181 H 0.9085 0.1370 0.5788 0.080 Uiso 1 1 calc R . . C111 C 1.0312(5) 0.4330(2) 0.2548(5) 0.0610(14) Uani 1 1 d . . . H111 H 1.0378 0.4558 0.3221 0.073 Uiso 1 1 calc R . . C121 C 1.0728(5) 0.1205(2) 0.4072(4) 0.0566(13) Uani 1 1 d . . . H12A H 1.1719 0.1206 0.3894 0.068 Uiso 1 1 calc R . . H12B H 1.0132 0.0979 0.3469 0.068 Uiso 1 1 calc R . . C71 C 0.9587(5) 0.3464(2) 0.1515(4) 0.0551(13) Uani 1 1 d . . . H71 H 0.9149 0.3101 0.1488 0.066 Uiso 1 1 calc R . . C51 C 0.9043(5) 0.35777(18) 0.3590(4) 0.0541(13) Uani 1 1 d . . . H51A H 0.9447 0.3799 0.4280 0.065 Uiso 1 1 calc R . . H51B H 0.7993 0.3635 0.3456 0.065 Uiso 1 1 calc R . . C141 C 1.1709(6) 0.0479(2) 0.5577(5) 0.0688(15) Uani 1 1 d . . . H141 H 1.2362 0.0370 0.5078 0.083 Uiso 1 1 calc R . . C91 C 1.0751(6) 0.4205(3) 0.0583(5) 0.0767(17) Uani 1 1 d . . . H91 H 1.1107 0.4346 -0.0076 0.092 Uiso 1 1 calc R . . C151 C 1.1729(7) 0.0204(2) 0.6643(7) 0.089(2) Uani 1 1 d . . . H151 H 1.2405 -0.0089 0.6860 0.106 Uiso 1 1 calc R . . C81 C 1.0133(6) 0.3668(2) 0.0549(4) 0.0676(15) Uani 1 1 d . . . H81 H 1.0083 0.3442 -0.0124 0.081 Uiso 1 1 calc R . . C41 C 1.0902(5) 0.2819(2) 0.4106(5) 0.0632(14) Uani 1 1 d . . . H41A H 1.1375 0.3109 0.4642 0.076 Uiso 1 1 calc R . . H41B H 1.1356 0.2828 0.3400 0.076 Uiso 1 1 calc R . . C161 C 1.0781(8) 0.0353(3) 0.7377(6) 0.092(2) Uani 1 1 d . . . H161 H 1.0797 0.0163 0.8092 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C22 0.054(3) 0.051(3) 0.049(3) 0.007(2) 0.017(2) 0.003(2) C12 0.055(3) 0.056(3) 0.041(3) 0.006(2) 0.015(2) -0.006(2) C101 0.096(5) 0.053(4) 0.093(5) 0.005(3) 0.035(4) -0.012(3) Se22 0.0547(3) 0.0486(3) 0.0734(4) 0.0008(3) 0.0162(3) 0.0014(2) Se12 0.0619(4) 0.0495(3) 0.0625(4) 0.0027(3) 0.0043(3) 0.0054(3) Ni 0.0538(4) 0.0490(4) 0.0425(4) 0.0055(3) 0.0115(3) 0.0013(3) S21 0.0606(8) 0.0481(8) 0.0663(9) 0.0034(6) 0.0045(7) 0.0040(6) S22 0.0563(8) 0.0571(8) 0.0640(9) 0.0016(7) 0.0137(7) 0.0032(6) S12 0.0650(9) 0.0544(8) 0.0693(9) -0.0065(7) 0.0077(7) 0.0002(7) S11 0.0586(8) 0.0518(8) 0.0596(8) 0.0015(6) 0.0039(6) 0.0066(6) S32 0.0619(9) 0.0780(11) 0.0850(11) -0.0143(8) -0.0007(8) -0.0021(8) N11 0.056(3) 0.055(3) 0.038(2) 0.0032(19) 0.0076(19) 0.007(2) C11 0.056(3) 0.049(3) 0.033(3) 0.005(2) 0.016(2) 0.007(2) C171 0.091(5) 0.094(5) 0.063(4) 0.012(4) 0.015(3) -0.011(4) C21 0.051(3) 0.051(3) 0.032(3) 0.008(2) 0.009(2) 0.002(2) N21 0.053(3) 0.053(3) 0.038(2) 0.0001(19) 0.0081(19) -0.001(2) C32 0.066(3) 0.059(3) 0.045(3) 0.000(2) 0.016(2) -0.003(3) C31 0.063(3) 0.076(4) 0.042(3) 0.003(3) 0.001(3) 0.005(3) C131 0.050(3) 0.051(3) 0.047(3) 0.002(2) -0.002(2) -0.003(2) C61 0.055(3) 0.039(3) 0.040(3) 0.001(2) 0.009(2) 0.002(2) C181 0.082(4) 0.069(4) 0.050(3) 0.011(3) 0.013(3) 0.010(3) C111 0.073(4) 0.051(3) 0.059(4) -0.006(3) 0.007(3) -0.003(3) C121 0.056(3) 0.067(3) 0.047(3) -0.002(3) 0.007(2) 0.015(3) C71 0.066(3) 0.053(3) 0.048(3) -0.004(3) 0.016(3) -0.004(3) C51 0.070(3) 0.040(3) 0.055(3) -0.006(2) 0.016(3) 0.002(2) C141 0.069(4) 0.055(3) 0.080(4) 0.007(3) 0.006(3) 0.006(3) C91 0.096(5) 0.077(4) 0.065(4) 0.012(3) 0.040(3) -0.004(4) C151 0.092(5) 0.056(4) 0.108(6) 0.034(4) -0.017(4) -0.004(3) C81 0.093(4) 0.067(4) 0.047(3) -0.005(3) 0.024(3) -0.003(3) C41 0.062(4) 0.062(4) 0.064(4) -0.004(3) 0.006(3) -0.007(3) C161 0.116(6) 0.083(5) 0.068(5) 0.031(4) -0.011(4) -0.034(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 C22 C12 1.355(6) . ? C22 S22 1.755(5) . ? C22 Se22 1.876(5) . ? C12 S12 1.731(5) . ? C12 Se12 1.880(5) . ? C101 C91 1.362(7) . ? C101 C111 1.384(7) . ? C101 H101 0.9300 . ? Se22 Ni 2.2884(8) . ? Se12 Ni 2.2755(8) . ? Ni S21 2.1513(14) . ? Ni S11 2.1621(14) . ? S21 C21 1.673(5) . ? S22 C32 1.745(5) . ? S12 C32 1.734(5) . ? S11 C11 1.691(5) . ? S32 C32 1.626(5) . ? N11 C21 1.328(5) . ? N11 C31 1.466(6) . ? N11 C121 1.465(5) . ? C11 N21 1.323(5) . ? C11 C21 1.490(6) . ? C171 C161 1.354(8) . ? C171 C181 1.390(7) . ? C171 H171 0.9300 . ? N21 C41 1.452(6) . ? N21 C51 1.467(5) . ? C31 C41 1.499(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C131 C141 1.370(6) . ? C131 C181 1.375(6) . ? C131 C121 1.522(6) . ? C61 C111 1.367(6) . ? C61 C71 1.393(6) . ? C61 C51 1.514(6) . ? C181 H181 0.9300 . ? C111 H111 0.9300 . ? C121 H12A 0.9700 . ? C121 H12B 0.9700 . ? C71 C81 1.372(6) . ? C71 H71 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C141 C151 1.378(7) . ? C141 H141 0.9300 . ? C91 C81 1.366(7) . ? C91 H91 0.9300 . ? C151 C161 1.352(8) . ? C151 H151 0.9300 . ? C81 H81 0.9300 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C161 H161 0.9300 . ? 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 C22 S22 114.6(4) . . ? C12 C22 Se22 122.7(4) . . ? S22 C22 Se22 122.8(3) . . ? C22 C12 S12 117.2(4) . . ? C22 C12 Se12 121.5(4) . . ? S12 C12 Se12 121.3(3) . . ? C91 C101 C111 119.7(5) . . ? C91 C101 H101 120.1 . . ? C111 C101 H101 120.1 . . ? C22 Se22 Ni 100.35(14) . . ? C12 Se12 Ni 100.98(15) . . ? S21 Ni S11 91.10(5) . . ? S21 Ni Se12 85.90(4) . . ? S11 Ni Se12 176.99(5) . . ? S21 Ni Se22 179.66(5) . . ? S11 Ni Se22 88.56(4) . . ? Se12 Ni Se22 94.44(3) . . ? C21 S21 Ni 106.36(17) . . ? C32 S22 C22 98.5(2) . . ? C12 S12 C32 98.3(2) . . ? C11 S11 Ni 105.96(17) . . ? C21 N11 C31 120.1(4) . . ? C21 N11 C121 122.7(4) . . ? C31 N11 C121 116.3(4) . . ? N21 C11 C21 119.5(4) . . ? N21 C11 S11 123.0(3) . . ? C21 C11 S11 117.5(4) . . ? C161 C171 C181 121.8(6) . . ? C161 C171 H171 119.1 . . ? C181 C171 H171 119.1 . . ? N11 C21 C11 119.0(4) . . ? N11 C21 S21 122.3(4) . . ? C11 C21 S21 118.6(3) . . ? C11 N21 C41 121.3(4) . . ? C11 N21 C51 122.3(4) . . ? C41 N21 C51 115.3(4) . . ? S32 C32 S12 124.1(3) . . ? S32 C32 S22 124.5(3) . . ? S12 C32 S22 111.5(3) . . ? N11 C31 C41 111.0(4) . . ? N11 C31 H31A 109.4 . . ? C41 C31 H31A 109.4 . . ? N11 C31 H31B 109.4 . . ? C41 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C141 C131 C181 120.2(5) . . ? C141 C131 C121 118.2(5) . . ? C181 C131 C121 121.6(4) . . ? C111 C61 C71 118.6(4) . . ? C111 C61 C51 120.6(4) . . ? C71 C61 C51 120.7(4) . . ? C131 C181 C171 118.3(5) . . ? C131 C181 H181 120.9 . . ? C171 C181 H181 120.9 . . ? C61 C111 C101 120.7(5) . . ? C61 C111 H111 119.7 . . ? C101 C111 H111 119.7 . . ? N11 C121 C131 113.9(4) . . ? N11 C121 H12A 108.8 . . ? C131 C121 H12A 108.8 . . ? N11 C121 H12B 108.8 . . ? C131 C121 H12B 108.8 . . ? H12A C121 H12B 107.7 . . ? C81 C71 C61 120.6(5) . . ? C81 C71 H71 119.7 . . ? C61 C71 H71 119.7 . . ? N21 C51 C61 111.1(4) . . ? N21 C51 H51A 109.4 . . ? C61 C51 H51A 109.4 . . ? N21 C51 H51B 109.4 . . ? C61 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C131 C141 C151 119.7(5) . . ? C131 C141 H141 120.2 . . ? C151 C141 H141 120.2 . . ? C101 C91 C81 120.7(5) . . ? C101 C91 H91 119.6 . . ? C81 C91 H91 119.6 . . ? C161 C151 C141 121.1(6) . . ? C161 C151 H151 119.5 . . ? C141 C151 H151 119.5 . . ? C91 C81 C71 119.6(5) . . ? C91 C81 H81 120.2 . . ? C71 C81 H81 120.2 . . ? N21 C41 C31 112.6(4) . . ? N21 C41 H41A 109.1 . . ? C31 C41 H41A 109.1 . . ? N21 C41 H41B 109.1 . . ? C31 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C151 C161 C171 119.1(6) . . ? C151 C161 H161 120.5 . . ? C171 C161 H161 120.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.468 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.082 #END #BEGIN data_pt509 _database_code_depnum_ccdc_archive 'CCDC 884916' #TrackingRef '- Ni-Pt_dsit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 N2 Pt S5 Se2' _chemical_formula_sum 'C21 H18 N2 Pt S5 Se2' _chemical_formula_weight 811.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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/n 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 9.267(2) _cell_length_b 23.189(5) _cell_length_c 11.555(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.069(4) _cell_angle_gamma 90.00 _cell_volume 2458.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18035 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 27.66 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 9.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker Smart APEXII CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 32475 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.66 _reflns_number_total 5703 _reflns_number_gt 4074 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0328P)^2^+4.7838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5703 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.45626(3) 0.187209(12) 0.26553(2) 0.04960(10) Uani 1 1 d . . . Se12 Se 0.68052(9) 0.23727(3) 0.32902(7) 0.0585(2) Uani 1 1 d . . . Se22 Se 0.56224(9) 0.09578(3) 0.32407(7) 0.0590(2) Uani 1 1 d . . . S11 S 0.2439(2) 0.14095(8) 0.20510(16) 0.0583(5) Uani 1 1 d . . . S12 S 0.9865(2) 0.18377(8) 0.42903(18) 0.0611(5) Uani 1 1 d . . . S21 S 0.3436(2) 0.27125(8) 0.20451(16) 0.0590(5) Uani 1 1 d . . . S22 S 0.8857(2) 0.06665(8) 0.42233(18) 0.0635(5) Uani 1 1 d . . . S32 S 1.1996(3) 0.08916(11) 0.4976(2) 0.0813(7) Uani 1 1 d . . . C81 C 0.0282(12) 0.0810(4) -0.1994(8) 0.091(3) Uani 1 1 d . . . H81 H 0.0945 0.0917 -0.2490 0.109 Uiso 1 1 calc R . . N21 N -0.0140(7) 0.1784(2) 0.1069(5) 0.0546(15) Uani 1 1 d . . . C12 C 0.8025(8) 0.1737(3) 0.3788(6) 0.0534(17) Uani 1 1 d . . . N11 N 0.0677(7) 0.2938(2) 0.1294(5) 0.0519(14) Uani 1 1 d . . . C22 C 0.7553(8) 0.1188(3) 0.3764(5) 0.0493(16) Uani 1 1 d . . . C61 C -0.0655(8) 0.0912(3) -0.0185(6) 0.0503(16) Uani 1 1 d . . . C11 C 0.1245(8) 0.1920(3) 0.1520(5) 0.0505(17) Uani 1 1 d . . . C191 C -0.0270(8) 0.4314(3) 0.2507(6) 0.0594(19) Uani 1 1 d . . . H191 H -0.0345 0.4535 0.1831 0.071 Uiso 1 1 calc R . . C141 C 0.0347(8) 0.3773(3) 0.2531(5) 0.0490(16) Uani 1 1 d . . . C51 C -0.0653(9) 0.1187(3) 0.1004(6) 0.0578(19) Uani 1 1 d . . . H51A H -0.1635 0.1177 0.1202 0.069 Uiso 1 1 calc R . . H51B H -0.0037 0.0961 0.1582 0.069 Uiso 1 1 calc R . . C32 C 1.0340(8) 0.1114(3) 0.4538(6) 0.0560(18) Uani 1 1 d . . . C151 C 0.0446(9) 0.3451(3) 0.3542(6) 0.0609(19) Uani 1 1 d . . . H151 H 0.0867 0.3086 0.3565 0.073 Uiso 1 1 calc R . . C121 C -0.1683(9) 0.0496(3) -0.0537(7) 0.071(2) Uani 1 1 d . . . H121 H -0.2373 0.0398 -0.0058 0.086 Uiso 1 1 calc R . . C171 C -0.0686(10) 0.4198(4) 0.4493(7) 0.072(2) Uani 1 1 d . . . H171 H -0.1040 0.4339 0.5151 0.086 Uiso 1 1 calc R . . C41 C -0.1081(9) 0.2211(3) 0.0435(6) 0.062(2) Uani 1 1 d . . . H41A H -0.2090 0.2096 0.0423 0.075 Uiso 1 1 calc R . . H41B H -0.0884 0.2228 -0.0367 0.075 Uiso 1 1 calc R . . C131 C 0.0972(8) 0.3555(3) 0.1472(6) 0.0557(18) Uani 1 1 d . . . H13A H 0.0544 0.3768 0.0785 0.067 Uiso 1 1 calc R . . H13B H 0.2016 0.3621 0.1578 0.067 Uiso 1 1 calc R . . C71 C 0.0296(9) 0.1066(4) -0.0921(6) 0.065(2) Uani 1 1 d . . . H71 H 0.0976 0.1354 -0.0693 0.078 Uiso 1 1 calc R . . C31 C -0.0864(8) 0.2798(3) 0.0974(7) 0.063(2) Uani 1 1 d . . . H31A H -0.1313 0.3084 0.0425 0.076 Uiso 1 1 calc R . . H31B H -0.1345 0.2814 0.1666 0.076 Uiso 1 1 calc R . . C181 C -0.0786(10) 0.4530(4) 0.3504(8) 0.077(2) Uani 1 1 d . . . H181 H -0.1194 0.4896 0.3495 0.092 Uiso 1 1 calc R . . C101 C -0.1691(12) 0.0224(4) -0.1600(10) 0.089(3) Uani 1 1 d . . . H101 H -0.2348 -0.0073 -0.1824 0.107 Uiso 1 1 calc R . . C161 C -0.0076(9) 0.3664(3) 0.4525(6) 0.067(2) Uani 1 1 d . . . H161 H -0.0009 0.3444 0.5202 0.080 Uiso 1 1 calc R . . C21 C 0.1682(8) 0.2539(3) 0.1569(5) 0.0495(17) Uani 1 1 d . . . C91 C -0.0735(14) 0.0393(5) -0.2309(8) 0.094(3) Uani 1 1 d . . . H91 H -0.0769 0.0220 -0.3038 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.06064(19) 0.04973(17) 0.04027(15) -0.00734(11) 0.01345(12) -0.00179(13) Se12 0.0620(5) 0.0477(4) 0.0683(5) -0.0023(3) 0.0174(4) -0.0038(3) Se22 0.0659(5) 0.0479(4) 0.0628(4) -0.0074(3) 0.0072(4) -0.0056(4) S11 0.0654(12) 0.0451(10) 0.0632(11) -0.0059(8) 0.0052(9) -0.0029(9) S12 0.0617(12) 0.0568(11) 0.0671(12) -0.0007(9) 0.0165(10) -0.0075(9) S21 0.0672(13) 0.0503(11) 0.0589(11) -0.0045(8) 0.0071(9) -0.0077(9) S22 0.0675(13) 0.0534(11) 0.0698(12) 0.0047(9) 0.0106(10) -0.0018(9) S32 0.0644(14) 0.0790(16) 0.0972(17) 0.0195(12) -0.0005(12) 0.0001(11) C81 0.125(9) 0.090(7) 0.062(5) -0.014(5) 0.026(6) 0.021(7) N21 0.071(4) 0.057(4) 0.036(3) -0.005(2) 0.009(3) -0.004(3) C12 0.056(4) 0.058(4) 0.050(4) -0.005(3) 0.021(3) 0.001(3) N11 0.069(4) 0.047(3) 0.041(3) -0.005(2) 0.014(3) 0.003(3) C22 0.064(5) 0.040(4) 0.047(4) -0.004(3) 0.018(3) -0.007(3) C61 0.053(4) 0.042(4) 0.055(4) 0.000(3) 0.006(3) -0.003(3) C11 0.066(5) 0.058(4) 0.029(3) -0.007(3) 0.013(3) -0.005(4) C191 0.074(5) 0.050(4) 0.053(4) 0.007(3) 0.005(4) 0.005(4) C141 0.060(4) 0.046(4) 0.043(4) -0.001(3) 0.014(3) -0.002(3) C51 0.074(5) 0.058(5) 0.042(4) 0.000(3) 0.012(3) -0.010(4) C32 0.067(5) 0.056(4) 0.046(4) 0.007(3) 0.013(3) 0.000(4) C151 0.077(5) 0.062(5) 0.045(4) 0.007(3) 0.014(4) 0.006(4) C121 0.076(6) 0.057(5) 0.079(6) -0.002(4) 0.004(4) -0.002(4) C171 0.093(6) 0.064(5) 0.063(5) -0.013(4) 0.030(4) 0.004(5) C41 0.068(5) 0.070(5) 0.047(4) 0.004(4) 0.001(4) -0.004(4) C131 0.075(5) 0.046(4) 0.050(4) 0.005(3) 0.023(4) 0.001(4) C71 0.066(5) 0.081(6) 0.049(4) -0.008(4) 0.015(4) -0.003(4) C31 0.062(5) 0.064(5) 0.063(5) -0.002(4) 0.008(4) 0.006(4) C181 0.096(7) 0.061(5) 0.077(6) -0.009(4) 0.026(5) 0.015(5) C101 0.100(8) 0.060(6) 0.098(7) -0.024(5) -0.015(6) 0.002(5) C161 0.092(6) 0.065(5) 0.047(4) -0.001(3) 0.022(4) -0.010(4) C21 0.069(5) 0.047(4) 0.036(3) -0.007(3) 0.016(3) -0.003(3) C91 0.130(10) 0.082(7) 0.060(6) -0.022(5) -0.019(6) 0.044(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt S11 2.2642(19) . ? Pt S21 2.276(2) . ? Pt Se22 2.3939(9) . ? Pt Se12 2.4034(9) . ? Se12 C12 1.896(7) . ? Se22 C22 1.883(7) . ? S11 C11 1.676(7) . ? S12 C12 1.738(8) . ? S12 C32 1.747(8) . ? S21 C21 1.690(8) . ? S22 C32 1.721(8) . ? S22 C22 1.739(7) . ? S32 C32 1.631(8) . ? C81 C91 1.363(15) . ? C81 C71 1.374(11) . ? C81 H81 0.9300 . ? N21 C11 1.353(9) . ? N21 C41 1.449(9) . ? N21 C51 1.461(9) . ? C12 C22 1.347(9) . ? N11 C21 1.318(9) . ? N11 C31 1.461(9) . ? N11 C131 1.468(9) . ? C61 C71 1.356(10) . ? C61 C121 1.377(10) . ? C61 C51 1.514(9) . ? C11 C21 1.491(9) . ? C191 C141 1.377(10) . ? C191 C181 1.399(10) . ? C191 H191 0.9300 . ? C141 C151 1.379(9) . ? C141 C131 1.512(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C151 C161 1.386(10) . ? C151 H151 0.9300 . ? C121 C101 1.380(12) . ? C121 H121 0.9300 . ? C171 C161 1.358(11) . ? C171 C181 1.370(11) . ? C171 H171 0.9300 . ? C41 C31 1.498(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C131 H13A 0.9700 . ? C131 H13B 0.9700 . ? C71 H71 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C181 H181 0.9300 . ? C101 C91 1.347(14) . ? C101 H101 0.9300 . ? C161 H161 0.9300 . ? C91 H91 0.9300 . ? 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 S11 Pt S21 88.22(7) . . ? S11 Pt Se22 88.39(5) . . ? S21 Pt Se22 176.57(5) . . ? S11 Pt Se12 179.39(5) . . ? S21 Pt Se12 91.17(5) . . ? Se22 Pt Se12 92.21(3) . . ? C12 Se12 Pt 99.8(2) . . ? C22 Se22 Pt 100.0(2) . . ? C11 S11 Pt 106.2(3) . . ? C12 S12 C32 98.0(4) . . ? C21 S21 Pt 106.0(2) . . ? C32 S22 C22 98.4(3) . . ? C91 C81 C71 117.7(10) . . ? C91 C81 H81 121.1 . . ? C71 C81 H81 121.1 . . ? C11 N21 C41 120.4(6) . . ? C11 N21 C51 121.6(6) . . ? C41 N21 C51 116.9(6) . . ? C22 C12 S12 115.8(6) . . ? C22 C12 Se12 123.4(6) . . ? S12 C12 Se12 120.8(4) . . ? C21 N11 C31 122.5(6) . . ? C21 N11 C131 122.6(6) . . ? C31 N11 C131 114.1(6) . . ? C12 C22 S22 116.2(6) . . ? C12 C22 Se22 124.5(6) . . ? S22 C22 Se22 119.3(4) . . ? C71 C61 C121 118.9(7) . . ? C71 C61 C51 122.6(6) . . ? C121 C61 C51 118.5(7) . . ? N21 C11 C21 118.5(6) . . ? N21 C11 S11 121.2(5) . . ? C21 C11 S11 120.3(6) . . ? C141 C191 C181 119.9(7) . . ? C141 C191 H191 120.1 . . ? C181 C191 H191 120.1 . . ? C191 C141 C151 119.2(6) . . ? C191 C141 C131 119.5(6) . . ? C151 C141 C131 121.2(6) . . ? N21 C51 C61 113.9(5) . . ? N21 C51 H51A 108.8 . . ? C61 C51 H51A 108.8 . . ? N21 C51 H51B 108.8 . . ? C61 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? S32 C32 S22 124.3(5) . . ? S32 C32 S12 124.0(5) . . ? S22 C32 S12 111.7(4) . . ? C141 C151 C161 120.7(7) . . ? C141 C151 H151 119.6 . . ? C161 C151 H151 119.6 . . ? C61 C121 C101 120.1(9) . . ? C61 C121 H121 120.0 . . ? C101 C121 H121 120.0 . . ? C161 C171 C181 120.9(7) . . ? C161 C171 H171 119.5 . . ? C181 C171 H171 119.5 . . ? N21 C41 C31 112.0(6) . . ? N21 C41 H41A 109.2 . . ? C31 C41 H41A 109.2 . . ? N21 C41 H41B 109.2 . . ? C31 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? N11 C131 C141 110.8(5) . . ? N11 C131 H13A 109.5 . . ? C141 C131 H13A 109.5 . . ? N11 C131 H13B 109.5 . . ? C141 C131 H13B 109.5 . . ? H13A C131 H13B 108.1 . . ? C61 C71 C81 121.9(8) . . ? C61 C71 H71 119.1 . . ? C81 C71 H71 119.1 . . ? N11 C31 C41 112.1(6) . . ? N11 C31 H31A 109.2 . . ? C41 C31 H31A 109.2 . . ? N11 C31 H31B 109.2 . . ? C41 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C171 C181 C191 119.6(8) . . ? C171 C181 H181 120.2 . . ? C191 C181 H181 120.2 . . ? C91 C101 C121 119.0(9) . . ? C91 C101 H101 120.5 . . ? C121 C101 H101 120.5 . . ? C171 C161 C151 119.6(7) . . ? C171 C161 H161 120.2 . . ? C151 C161 H161 120.2 . . ? N11 C21 C11 119.1(7) . . ? N11 C21 S21 121.8(5) . . ? C11 C21 S21 119.0(6) . . ? C101 C91 C81 122.3(9) . . ? C101 C91 H91 118.8 . . ? C81 C91 H91 118.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.452 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.131 #END