Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method ; SHELXL-97 (Sheldrick, 1997) and enCIFer (Allen, 2004), plus manual edit of cif file ; _publ_section_title ; First Metallamacrocyclic Complexes of Pt(IV) with 3,3,3',3'-tetraalkyl-1,1'-phenylenedicarbonylbis(thioureas): Synthesis by Direct or Electrolytic Oxidative Addition of I2, Br2 and Cl2. ; _publ_contact_author_name 'Prof. Klaus R Koch' _publ_contact_author_address ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_phone '+27 21 808 3020' _publ_contact_author_fax '+27 21 808 3342' _publ_contact_author_email krk@sun.ac.za _publ_contact_letter ; Revised file for manuscript B507188G to be published in Dalton Transactions. Please refer correspondence regarding the publication to Arjan Westra, e-mail: anw@sun.ac.za. K R Koch ; loop_ _publ_author_name _publ_author_address A.N.Westra ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; S.A.Bourne ; Department of Chemistry University of Cape Town PB Rondebosch Cape Town, 7701 South Africa ; K.R.Koch ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_section_references ; enCIFer: A program for viewing, editing and visualising CIFs. Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. and Towler, M. (2004) J. Applied Cryst., 37, 331-334, 2004. Otwinowski, Z. & Minor, W. (1997) Methods Enzymol., 276, 307. Nonius BV (1998) COLLECT. Data collection software. Delft, The Netherlands. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of Gottingen, Germany. Barbour, L. J. (1999). X-Seed. University of Stellenbosch, South Africa. Bruker (2001). SMART (Version 5.625) and SADABS (Version 2.03a). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2002). SAINT. Version 6.36a. Bruker AXS Inc., Madison, Wisconsin, USA. ; #========================================END data_22MetmacPtI4 _database_code_depnum_ccdc_archive 'CCDC 272657' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; cis-Bis((mu2-3,3,3',3'-tetraethyl-1,1'-isophthaloylbis(thioureato))di iodoplatinum(IV)) ; _chemical_name_common ; cis-Bis((mu2-3,3,3',3'-tetraethyl-1,1'- isophthaloylbis(thioureato))di iodoplatinum(IV)) ; _chemical_melting_point '> 190 (decomp.)' _chemical_formula_moiety 'C36 H48 I4 N8 O4 Pt2 S4' _chemical_formula_sum 'C36 H48 I4 N8 O4 Pt2 S4' _chemical_formula_weight 1682.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 10.087(2) _cell_length_b 10.498(2) _cell_length_c 11.975(2) _cell_angle_alpha 84.50(3) _cell_angle_beta 87.24(3) _cell_angle_gamma 80.80(3) _cell_volume 1245.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 8.301 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.66 _exptl_absorpt_process_details 'Scalepack (Otwinowski &Minor,1997)' _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_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37186 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5971 _reflns_number_gt 5346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO_SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO_SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED (Barbour, 1999)' _computing_publication_material 'X-SEED (Barbour, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.7544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00297(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5971 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.646294(12) 0.241846(11) 0.737123(10) 0.02074(5) Uani 1 1 d . . . I1 I 0.52374(3) 0.42690(2) 0.86105(2) 0.04085(7) Uani 1 1 d . . . I2 I 0.77312(3) 0.05910(2) 0.61216(2) 0.03773(7) Uani 1 1 d . . . S1 S 0.54880(9) 0.09019(8) 0.85025(7) 0.02564(17) Uani 1 1 d . . . S2 S 0.17887(9) 0.79528(9) 0.14530(8) 0.0345(2) Uani 1 1 d . . . O1 O 0.4877(2) 0.2782(2) 0.6308(2) 0.0298(5) Uani 1 1 d . . . O2 O 0.2796(2) 0.6193(2) 0.3689(2) 0.0297(5) Uani 1 1 d . . . N1 N 0.3977(3) 0.0848(3) 0.6658(2) 0.0268(6) Uani 1 1 d . . . N2 N 0.4747(3) -0.1081(3) 0.7611(2) 0.0275(6) Uani 1 1 d . . . N3 N 0.0934(3) 0.5841(3) 0.2715(2) 0.0249(6) Uani 1 1 d . . . N4 N -0.0405(3) 0.6964(3) 0.1384(3) 0.0314(7) Uani 1 1 d . . . C1 C 0.0613(3) 0.2605(3) 0.4900(3) 0.0289(7) Uani 1 1 d . . . H1 H -0.0167 0.2201 0.4916 0.035 Uiso 1 1 calc R . . C2 C 0.1692(3) 0.2051(3) 0.5548(3) 0.0258(7) Uani 1 1 d . . . H2 H 0.1658 0.1260 0.5997 0.031 Uiso 1 1 calc R . . C3 C 0.2830(3) 0.2657(3) 0.5542(3) 0.0219(6) Uani 1 1 d . . . C4 C 0.2873(3) 0.3823(3) 0.4887(3) 0.0220(6) Uani 1 1 d . . . H4 H 0.3635 0.4250 0.4898 0.026 Uiso 1 1 calc R . . C5 C 0.1796(3) 0.4361(3) 0.4218(3) 0.0211(6) Uani 1 1 d . . . C6 C 0.0664(3) 0.3742(3) 0.4230(3) 0.0258(7) Uani 1 1 d . . . H6 H -0.0072 0.4107 0.3775 0.031 Uiso 1 1 calc R . . C31 C 0.3993(3) 0.2054(3) 0.6243(3) 0.0228(6) Uani 1 1 d . . . C32 C 0.4720(3) 0.0187(3) 0.7486(3) 0.0231(6) Uani 1 1 d . . . C33 C 0.5416(4) -0.1931(3) 0.8538(3) 0.0340(8) Uani 1 1 d . . . H33A H 0.4886 -0.2635 0.8769 0.041 Uiso 1 1 calc R . . H33B H 0.5442 -0.1424 0.9190 0.041 Uiso 1 1 calc R . . C34 C 0.6822(5) -0.2515(4) 0.8212(4) 0.0483(11) Uani 1 1 d . . . H34A H 0.6815 -0.2916 0.7507 0.072 Uiso 1 1 calc R . . H34B H 0.7179 -0.3174 0.8804 0.072 Uiso 1 1 calc R . . H34C H 0.7391 -0.1835 0.8113 0.072 Uiso 1 1 calc R . . C35 C 0.4116(4) -0.1752(4) 0.6797(3) 0.0426(10) Uani 1 1 d . . . H35A H 0.4644 -0.2623 0.6732 0.051 Uiso 1 1 calc R . . H35B H 0.4132 -0.1259 0.6050 0.051 Uiso 1 1 calc R . . C36 C 0.2686(6) -0.1885(6) 0.7145(5) 0.0740(18) Uani 1 1 d . . . H36A H 0.2658 -0.2305 0.7911 0.111 Uiso 1 1 calc R . . H36B H 0.2332 -0.2412 0.6632 0.111 Uiso 1 1 calc R . . H36C H 0.2136 -0.1025 0.7119 0.111 Uiso 1 1 calc R . . C51 C 0.1862(3) 0.5577(3) 0.3470(3) 0.0216(6) Uani 1 1 d . . . C52 C 0.0743(3) 0.6836(3) 0.1915(3) 0.0243(7) Uani 1 1 d . . . C53 C -0.0751(4) 0.7942(4) 0.0435(4) 0.0497(12) Uani 1 1 d . . . H53A H -0.1322 0.7602 -0.0079 0.060 Uiso 1 1 calc R . . H53B H 0.0082 0.8105 0.0013 0.060 Uiso 1 1 calc R . . C54 C -0.1482(5) 0.9193(5) 0.0817(6) 0.082(2) Uani 1 1 d . . . H54A H -0.2314 0.9038 0.1227 0.124 Uiso 1 1 calc R . . H54B H -0.1698 0.9815 0.0163 0.124 Uiso 1 1 calc R . . H54C H -0.0911 0.9544 0.1311 0.124 Uiso 1 1 calc R . . C55 C -0.1440(4) 0.6148(4) 0.1751(4) 0.0388(9) Uani 1 1 d . . . H55A H -0.2338 0.6637 0.1568 0.047 Uiso 1 1 calc R . . H55B H -0.1419 0.5955 0.2576 0.047 Uiso 1 1 calc R . . C56 C -0.1239(5) 0.4892(4) 0.1206(4) 0.0544(12) Uani 1 1 d . . . H56A H -0.1276 0.5077 0.0390 0.082 Uiso 1 1 calc R . . H56B H -0.1948 0.4390 0.1475 0.082 Uiso 1 1 calc R . . H56C H -0.0361 0.4394 0.1401 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02538(7) 0.01529(7) 0.02226(7) 0.00436(4) -0.00486(4) -0.00768(4) I1 0.04627(15) 0.02187(12) 0.05654(17) -0.01210(11) 0.00709(12) -0.00926(10) I2 0.04599(15) 0.03209(13) 0.03525(14) -0.00568(10) 0.01240(11) -0.00907(11) S1 0.0398(5) 0.0199(4) 0.0195(4) 0.0027(3) -0.0017(3) -0.0140(3) S2 0.0355(5) 0.0330(5) 0.0364(5) 0.0171(4) -0.0172(4) -0.0171(4) O1 0.0318(13) 0.0235(12) 0.0355(13) 0.0118(10) -0.0144(10) -0.0137(10) O2 0.0336(13) 0.0276(12) 0.0294(13) 0.0125(10) -0.0113(10) -0.0153(10) N1 0.0323(15) 0.0190(13) 0.0303(15) 0.0053(11) -0.0077(12) -0.0104(11) N2 0.0410(16) 0.0169(13) 0.0261(14) 0.0029(11) -0.0091(12) -0.0093(12) N3 0.0258(14) 0.0208(13) 0.0276(14) 0.0062(11) -0.0051(11) -0.0058(11) N4 0.0269(15) 0.0304(16) 0.0368(17) 0.0125(13) -0.0096(12) -0.0101(12) C1 0.0253(16) 0.0263(17) 0.0364(19) 0.0041(14) -0.0020(14) -0.0115(13) C2 0.0300(17) 0.0205(16) 0.0277(17) 0.0039(13) -0.0008(13) -0.0099(13) C3 0.0251(15) 0.0175(15) 0.0235(15) 0.0001(12) -0.0010(12) -0.0061(12) C4 0.0235(15) 0.0191(15) 0.0243(16) 0.0017(12) 0.0001(12) -0.0083(12) C5 0.0242(15) 0.0163(14) 0.0226(15) 0.0011(12) 0.0000(12) -0.0044(12) C6 0.0212(15) 0.0267(17) 0.0293(17) 0.0015(13) -0.0027(13) -0.0053(13) C31 0.0270(16) 0.0201(15) 0.0227(16) 0.0014(12) -0.0028(12) -0.0092(12) C32 0.0278(16) 0.0191(15) 0.0233(16) 0.0025(12) -0.0027(12) -0.0084(12) C33 0.059(2) 0.0174(16) 0.0264(18) 0.0068(13) -0.0127(16) -0.0114(16) C34 0.059(3) 0.034(2) 0.052(3) 0.0028(19) -0.023(2) -0.0043(19) C35 0.070(3) 0.0213(18) 0.041(2) 0.0021(16) -0.026(2) -0.0177(18) C36 0.087(4) 0.070(4) 0.076(4) 0.023(3) -0.033(3) -0.054(3) C51 0.0237(15) 0.0176(15) 0.0233(15) 0.0008(12) 0.0017(12) -0.0052(12) C52 0.0259(16) 0.0199(15) 0.0266(16) 0.0014(13) -0.0024(13) -0.0032(12) C53 0.043(2) 0.058(3) 0.050(3) 0.028(2) -0.027(2) -0.024(2) C54 0.044(3) 0.065(4) 0.117(5) 0.058(3) 0.004(3) 0.012(2) C55 0.0247(18) 0.042(2) 0.050(2) 0.0121(18) -0.0100(16) -0.0133(16) C56 0.049(3) 0.047(3) 0.072(3) 0.001(2) -0.005(2) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O2 2.049(2) 2_666 ? Pt1 O1 2.057(2) . ? Pt1 S2 2.2712(11) 2_666 ? Pt1 S1 2.3013(11) . ? Pt1 I1 2.6671(9) . ? Pt1 I2 2.6718(9) . ? S1 C32 1.760(3) . ? S2 C52 1.734(3) . ? S2 Pt1 2.2712(11) 2_666 ? O1 C31 1.273(4) . ? O2 C51 1.275(4) . ? O2 Pt1 2.049(2) 2_666 ? N1 C31 1.317(4) . ? N1 C32 1.341(4) . ? N2 C32 1.321(4) . ? N2 C33 1.474(4) . ? N2 C35 1.479(4) . ? N3 C51 1.312(4) . ? N3 C52 1.344(4) . ? N4 C52 1.330(4) . ? N4 C53 1.471(5) . ? N4 C55 1.479(4) . ? C1 C6 1.380(5) . ? C1 C2 1.385(5) . ? C1 H1 0.9500 . ? C2 C3 1.398(4) . ? C2 H2 0.9500 . ? C3 C4 1.394(4) . ? C3 C31 1.496(4) . ? C4 C5 1.394(4) . ? C4 H4 0.9500 . ? C5 C6 1.400(4) . ? C5 C51 1.496(4) . ? C6 H6 0.9500 . ? C33 C34 1.502(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.507(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C53 C54 1.500(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.507(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pt1 O1 83.52(9) 2_666 . ? O2 Pt1 S2 95.98(7) 2_666 2_666 ? O1 Pt1 S2 179.21(7) . 2_666 ? O2 Pt1 S1 175.99(7) 2_666 . ? O1 Pt1 S1 92.56(7) . . ? S2 Pt1 S1 87.93(4) 2_666 . ? O2 Pt1 I1 89.28(8) 2_666 . ? O1 Pt1 I1 89.62(8) . . ? S2 Pt1 I1 89.75(4) 2_666 . ? S1 Pt1 I1 89.84(3) . . ? O2 Pt1 I2 89.79(8) 2_666 . ? O1 Pt1 I2 90.93(8) . . ? S2 Pt1 I2 89.69(4) 2_666 . ? S1 Pt1 I2 91.13(3) . . ? I1 Pt1 I2 178.86(3) . . ? C32 S1 Pt1 100.21(11) . . ? C52 S2 Pt1 106.11(11) . 2_666 ? C31 O1 Pt1 125.7(2) . . ? C51 O2 Pt1 125.6(2) . 2_666 ? C31 N1 C32 127.4(3) . . ? C32 N2 C33 123.6(3) . . ? C32 N2 C35 121.3(3) . . ? C33 N2 C35 115.1(3) . . ? C51 N3 C52 128.9(3) . . ? C52 N4 C53 122.9(3) . . ? C52 N4 C55 121.1(3) . . ? C53 N4 C55 116.0(3) . . ? C6 C1 C2 120.3(3) . . ? C6 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C31 120.3(3) . . ? C2 C3 C31 119.8(3) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 C51 120.2(3) . . ? C6 C5 C51 120.1(3) . . ? C1 C6 C5 120.3(3) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O1 C31 N1 130.0(3) . . ? O1 C31 C3 114.1(3) . . ? N1 C31 C3 115.8(3) . . ? N2 C32 N1 116.9(3) . . ? N2 C32 S1 118.1(2) . . ? N1 C32 S1 124.6(2) . . ? N2 C33 C34 112.1(3) . . ? N2 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N2 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 C36 111.7(4) . . ? N2 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? N2 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 C51 N3 130.9(3) . . ? O2 C51 C5 114.4(3) . . ? N3 C51 C5 114.6(3) . . ? N4 C52 N3 115.1(3) . . ? N4 C52 S2 115.3(2) . . ? N3 C52 S2 129.6(2) . . ? N4 C53 C54 112.0(4) . . ? N4 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? N4 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 C56 112.6(4) . . ? N4 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? N4 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pt1 S1 C32 36.43(13) . . . . ? S2 Pt1 S1 C32 -144.20(12) 2_666 . . . ? I1 Pt1 S1 C32 126.04(11) . . . . ? I2 Pt1 S1 C32 -54.55(11) . . . . ? O2 Pt1 O1 C31 163.4(3) 2_666 . . . ? S1 Pt1 O1 C31 -17.5(3) . . . . ? I1 Pt1 O1 C31 -107.3(3) . . . . ? I2 Pt1 O1 C31 73.7(3) . . . . ? C6 C1 C2 C3 1.2(5) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C1 C2 C3 C31 -179.9(3) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? C31 C3 C4 C5 178.5(3) . . . . ? C3 C4 C5 C6 1.6(5) . . . . ? C3 C4 C5 C51 -176.9(3) . . . . ? C2 C1 C6 C5 -1.4(5) . . . . ? C4 C5 C6 C1 0.0(5) . . . . ? C51 C5 C6 C1 178.5(3) . . . . ? Pt1 O1 C31 N1 -12.8(5) . . . . ? Pt1 O1 C31 C3 170.2(2) . . . . ? C32 N1 C31 O1 18.3(6) . . . . ? C32 N1 C31 C3 -164.7(3) . . . . ? C4 C3 C31 O1 10.1(4) . . . . ? C2 C3 C31 O1 -169.6(3) . . . . ? C4 C3 C31 N1 -167.4(3) . . . . ? C2 C3 C31 N1 12.9(5) . . . . ? C33 N2 C32 N1 -174.5(3) . . . . ? C35 N2 C32 N1 6.8(5) . . . . ? C33 N2 C32 S1 -1.7(5) . . . . ? C35 N2 C32 S1 179.6(3) . . . . ? C31 N1 C32 N2 -166.3(3) . . . . ? C31 N1 C32 S1 21.4(5) . . . . ? Pt1 S1 C32 N2 140.7(3) . . . . ? Pt1 S1 C32 N1 -47.1(3) . . . . ? C32 N2 C33 C34 -94.8(4) . . . . ? C35 N2 C33 C34 83.9(4) . . . . ? C32 N2 C35 C36 -92.5(4) . . . . ? C33 N2 C35 C36 88.8(4) . . . . ? Pt1 O2 C51 N3 -19.3(5) 2_666 . . . ? Pt1 O2 C51 C5 162.2(2) 2_666 . . . ? C52 N3 C51 O2 3.0(6) . . . . ? C52 N3 C51 C5 -178.5(3) . . . . ? C4 C5 C51 O2 -15.0(4) . . . . ? C6 C5 C51 O2 166.5(3) . . . . ? C4 C5 C51 N3 166.3(3) . . . . ? C6 C5 C51 N3 -12.2(4) . . . . ? C53 N4 C52 N3 -175.9(4) . . . . ? C55 N4 C52 N3 6.5(5) . . . . ? C53 N4 C52 S2 2.7(5) . . . . ? C55 N4 C52 S2 -174.9(3) . . . . ? C51 N3 C52 N4 -169.9(3) . . . . ? C51 N3 C52 S2 11.7(6) . . . . ? Pt1 S2 C52 N4 174.8(2) 2_666 . . . ? Pt1 S2 C52 N3 -6.8(4) 2_666 . . . ? C52 N4 C53 C54 -89.9(5) . . . . ? C55 N4 C53 C54 87.8(5) . . . . ? C52 N4 C55 C56 -88.4(4) . . . . ? C53 N4 C55 C56 93.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.351 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.101 #========================================END data_22MetmacPtBr4 _database_code_depnum_ccdc_archive 'CCDC 272658' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; cis-bis((mu2-3,3,3',3'-tetraethyl-1,1'-isophthaloylbis(thioureato))di bromoplatinum(IV)) ; _chemical_name_common ; cis-bis((mu2-3,3,3',3'-tetraethyl-1,1'- isophthaloylbis(thioureato))di bromoplatinum(IV)) ; _chemical_melting_point '> 195 (decomp.)' _chemical_formula_moiety 'C36 H48 Br4 N8 O4 Pt2 S4' _chemical_formula_sum 'C36 H48 Br4 N8 O4 Pt2 S4' _chemical_formula_weight 1494.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2877(11) _cell_length_b 18.736(2) _cell_length_c 13.8036(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.137(2) _cell_angle_gamma 90.00 _cell_volume 2339.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 9.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.46 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13755 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.99 _reflns_number_total 5027 _reflns_number_gt 4538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED (Barbour, 1999)' _computing_publication_material 'X-SEED (Barbour, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+17.5147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 5027 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.68568(2) 0.375446(11) 0.722473(14) 0.01116(9) Uani 1 1 d . . . Br1 Br 0.64578(8) 0.47519(4) 0.82521(5) 0.03275(17) Uani 1 1 d . . . Br2 Br 0.71553(8) 0.27478(4) 0.61692(5) 0.02684(16) Uani 1 1 d . . . S1 S 0.60496(16) 0.29933(8) 0.82783(10) 0.0162(3) Uani 1 1 d . . . S2 S 0.08167(15) 0.64443(8) 0.18395(11) 0.0173(3) Uani 1 1 d . . . O1 O 0.4806(4) 0.3947(2) 0.6354(3) 0.0160(8) Uani 1 1 d . . . O2 O 0.2450(4) 0.5537(2) 0.3721(3) 0.0145(8) Uani 1 1 d . . . N1 N 0.3482(5) 0.2954(2) 0.6760(3) 0.0136(9) Uani 1 1 d . . . N2 N 0.3965(5) 0.2035(2) 0.7833(3) 0.0139(9) Uani 1 1 d . . . N3 N 0.0169(5) 0.5168(3) 0.2691(4) 0.0148(9) Uani 1 1 d . . . N4 N -0.1335(5) 0.5534(3) 0.1242(4) 0.0186(10) Uani 1 1 d . . . C1 C -0.0308(6) 0.3712(3) 0.4833(5) 0.0170(12) Uani 1 1 d . . . H1 H -0.1236 0.3493 0.4813 0.020 Uiso 1 1 calc R . . C2 C 0.0941(6) 0.3489(3) 0.5529(4) 0.0157(11) Uani 1 1 d . . . H2 H 0.0865 0.3111 0.5973 0.019 Uiso 1 1 calc R . . C3 C 0.2304(6) 0.3816(3) 0.5579(4) 0.0126(10) Uani 1 1 d . . . C4 C 0.2399(6) 0.4389(3) 0.4935(4) 0.0116(10) Uani 1 1 d . . . H4 H 0.3306 0.4638 0.4994 0.014 Uiso 1 1 calc R . . C5 C 0.1163(6) 0.4589(3) 0.4211(4) 0.0120(10) Uani 1 1 d . . . C6 C -0.0201(6) 0.4250(3) 0.4173(4) 0.0137(11) Uani 1 1 d . . . H6 H -0.1053 0.4393 0.3690 0.016 Uiso 1 1 calc R . . C31 C 0.3657(6) 0.3561(3) 0.6302(4) 0.0119(10) Uani 1 1 d . . . C32 C 0.4411(6) 0.2652(3) 0.7551(4) 0.0126(10) Uani 1 1 d . . . C33 C 0.4775(7) 0.1659(3) 0.8742(5) 0.0210(13) Uani 1 1 d . . . H33A H 0.4058 0.1408 0.9053 0.025 Uiso 1 1 calc R . . H33B H 0.5307 0.2014 0.9225 0.025 Uiso 1 1 calc R . . C34 C 0.5875(8) 0.1124(4) 0.8505(7) 0.039(2) Uani 1 1 d . . . H34A H 0.5362 0.0794 0.7991 0.058 Uiso 1 1 calc R . . H34B H 0.6324 0.0856 0.9107 0.058 Uiso 1 1 calc R . . H34C H 0.6648 0.1378 0.8264 0.058 Uiso 1 1 calc R . . C35 C 0.2544(6) 0.1702(3) 0.7326(4) 0.0166(11) Uani 1 1 d . . . H35A H 0.2619 0.1178 0.7413 0.020 Uiso 1 1 calc R . . H35B H 0.2353 0.1806 0.6605 0.020 Uiso 1 1 calc R . . C36 C 0.1258(7) 0.1976(3) 0.7734(5) 0.0220(13) Uani 1 1 d . . . H36A H 0.1483 0.1913 0.8457 0.033 Uiso 1 1 calc R . . H36B H 0.0362 0.1708 0.7433 0.033 Uiso 1 1 calc R . . H36C H 0.1100 0.2484 0.7573 0.033 Uiso 1 1 calc R . . C51 C 0.1264(6) 0.5161(3) 0.3482(4) 0.0127(10) Uani 1 1 d . . . C52 C -0.0126(6) 0.5654(3) 0.1947(4) 0.0141(11) Uani 1 1 d . . . C53 C -0.1824(7) 0.5980(3) 0.0355(4) 0.0181(12) Uani 1 1 d . . . H53A H -0.2213 0.5670 -0.0226 0.022 Uiso 1 1 calc R . . H53B H -0.0967 0.6246 0.0224 0.022 Uiso 1 1 calc R . . C54 C -0.3017(8) 0.6508(4) 0.0476(5) 0.0276(14) Uani 1 1 d . . . H54A H -0.3845 0.6249 0.0643 0.041 Uiso 1 1 calc R . . H54B H -0.3366 0.6770 -0.0148 0.041 Uiso 1 1 calc R . . H54C H -0.2607 0.6845 0.1011 0.041 Uiso 1 1 calc R . . C55 C -0.2272(8) 0.4905(4) 0.1302(6) 0.0359(18) Uani 1 1 d . . . H55A H -0.3291 0.4999 0.0919 0.043 Uiso 1 1 calc R . . H55B H -0.2310 0.4823 0.2005 0.043 Uiso 1 1 calc R . . C56 C -0.1675(12) 0.4235(4) 0.0892(7) 0.057(3) Uani 1 1 d . . . H56A H -0.1894 0.4259 0.0164 0.086 Uiso 1 1 calc R . . H56B H -0.2145 0.3811 0.1099 0.086 Uiso 1 1 calc R . . H56C H -0.0602 0.4207 0.1151 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00942(12) 0.01065(12) 0.01259(12) 0.00282(7) 0.00078(8) -0.00082(7) Br1 0.0369(4) 0.0268(4) 0.0332(4) -0.0026(3) 0.0050(3) 0.0009(3) Br2 0.0298(3) 0.0250(3) 0.0265(3) -0.0011(3) 0.0078(3) -0.0016(3) S1 0.0146(6) 0.0186(7) 0.0136(6) 0.0056(5) -0.0002(5) -0.0052(5) S2 0.0118(6) 0.0139(6) 0.0231(7) 0.0050(5) -0.0024(5) -0.0011(5) O1 0.0107(18) 0.0168(19) 0.018(2) 0.0082(16) -0.0018(16) -0.0008(15) O2 0.0129(18) 0.0142(19) 0.0149(18) 0.0038(15) -0.0002(15) -0.0049(15) N1 0.013(2) 0.012(2) 0.014(2) 0.0036(18) -0.0008(18) 0.0001(17) N2 0.015(2) 0.012(2) 0.015(2) 0.0047(18) 0.0030(18) -0.0007(18) N3 0.012(2) 0.017(2) 0.014(2) 0.0040(19) 0.0013(18) -0.0017(18) N4 0.016(2) 0.018(2) 0.018(2) 0.0037(19) -0.004(2) -0.0033(19) C1 0.010(3) 0.019(3) 0.022(3) 0.002(2) 0.004(2) -0.005(2) C2 0.015(3) 0.015(3) 0.017(3) 0.004(2) 0.004(2) -0.001(2) C3 0.012(3) 0.013(3) 0.013(2) 0.000(2) 0.002(2) -0.001(2) C4 0.011(2) 0.013(3) 0.011(2) 0.0006(19) 0.003(2) -0.0009(19) C5 0.012(2) 0.012(2) 0.013(2) 0.002(2) 0.006(2) 0.003(2) C6 0.008(2) 0.017(3) 0.014(2) 0.000(2) 0.000(2) -0.002(2) C31 0.012(2) 0.013(2) 0.011(2) 0.000(2) 0.003(2) 0.000(2) C32 0.012(2) 0.013(3) 0.013(2) -0.001(2) 0.005(2) 0.000(2) C33 0.017(3) 0.021(3) 0.021(3) 0.013(2) -0.003(2) -0.002(2) C34 0.027(4) 0.018(3) 0.059(5) 0.004(3) -0.016(4) 0.005(3) C35 0.015(3) 0.013(3) 0.021(3) 0.001(2) 0.003(2) -0.002(2) C36 0.017(3) 0.021(3) 0.028(3) 0.005(2) 0.003(2) -0.001(2) C51 0.013(2) 0.011(2) 0.016(3) 0.003(2) 0.007(2) 0.002(2) C52 0.010(2) 0.015(3) 0.017(3) 0.001(2) 0.003(2) -0.001(2) C53 0.018(3) 0.018(3) 0.016(3) 0.002(2) 0.000(2) 0.002(2) C54 0.026(3) 0.034(4) 0.022(3) 0.003(3) 0.004(3) 0.009(3) C55 0.031(4) 0.036(4) 0.032(4) 0.016(3) -0.013(3) -0.020(3) C56 0.073(7) 0.027(4) 0.053(5) 0.002(4) -0.025(5) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.040(4) . ? Pt1 O2 2.064(4) 3_666 ? Pt1 S1 2.2818(14) . ? Pt1 S2 2.2820(14) 3_666 ? Pt1 Br1 2.4248(8) . ? Pt1 Br2 2.4374(7) . ? S1 C32 1.743(6) . ? S2 C52 1.743(6) . ? S2 Pt1 2.2820(14) 3_666 ? O1 C31 1.277(7) . ? O2 C51 1.286(7) . ? O2 Pt1 2.064(4) 3_666 ? N1 C31 1.329(7) . ? N1 C32 1.352(7) . ? N2 C32 1.317(7) . ? N2 C35 1.483(7) . ? N2 C33 1.485(7) . ? N3 C51 1.312(7) . ? N3 C52 1.353(7) . ? N4 C52 1.328(7) . ? N4 C53 1.467(7) . ? N4 C55 1.479(8) . ? C1 C6 1.378(8) . ? C1 C2 1.392(8) . ? C1 H1 0.9500 . ? C2 C3 1.394(8) . ? C2 H2 0.9500 . ? C3 C4 1.409(7) . ? C3 C31 1.495(8) . ? C4 C5 1.391(7) . ? C4 H4 0.9500 . ? C5 C6 1.408(7) . ? C5 C51 1.487(7) . ? C6 H6 0.9500 . ? C33 C34 1.519(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.521(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C53 C54 1.522(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.532(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 84.13(15) . 3_666 ? O1 Pt1 S1 95.03(12) . . ? O2 Pt1 S1 178.53(12) 3_666 . ? O1 Pt1 S2 178.18(12) . 3_666 ? O2 Pt1 S2 94.10(11) 3_666 3_666 ? S1 Pt1 S2 86.74(5) . 3_666 ? O1 Pt1 Br1 87.83(12) . . ? O2 Pt1 Br1 89.17(12) 3_666 . ? S1 Pt1 Br1 89.59(4) . . ? S2 Pt1 Br1 92.62(4) 3_666 . ? O1 Pt1 Br2 90.13(12) . . ? O2 Pt1 Br2 91.44(11) 3_666 . ? S1 Pt1 Br2 89.76(4) . . ? S2 Pt1 Br2 89.45(4) 3_666 . ? Br1 Pt1 Br2 177.80(3) . . ? C32 S1 Pt1 103.45(19) . . ? C52 S2 Pt1 104.04(19) . 3_666 ? C31 O1 Pt1 126.1(4) . . ? C51 O2 Pt1 124.2(3) . 3_666 ? C31 N1 C32 128.1(5) . . ? C32 N2 C35 122.4(5) . . ? C32 N2 C33 122.2(5) . . ? C35 N2 C33 115.2(4) . . ? C51 N3 C52 128.5(5) . . ? C52 N4 C53 124.4(5) . . ? C52 N4 C55 120.3(5) . . ? C53 N4 C55 115.2(5) . . ? C6 C1 C2 120.2(5) . . ? C6 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C1 C2 C3 120.5(5) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 C31 120.6(5) . . ? C4 C3 C31 120.1(5) . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.5(5) . . ? C4 C5 C51 120.8(5) . . ? C6 C5 C51 119.6(5) . . ? C1 C6 C5 120.4(5) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O1 C31 N1 130.4(5) . . ? O1 C31 C3 114.9(5) . . ? N1 C31 C3 114.6(5) . . ? N2 C32 N1 114.9(5) . . ? N2 C32 S1 116.4(4) . . ? N1 C32 S1 128.7(4) . . ? N2 C33 C34 111.6(6) . . ? N2 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? N2 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 C36 111.9(5) . . ? N2 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? N2 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 C51 N3 131.7(5) . . ? O2 C51 C5 113.7(5) . . ? N3 C51 C5 114.5(5) . . ? N4 C52 N3 115.7(5) . . ? N4 C52 S2 116.1(4) . . ? N3 C52 S2 128.1(4) . . ? N4 C53 C54 112.0(5) . . ? N4 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? N4 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 C56 111.4(7) . . ? N4 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? N4 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pt1 S1 C32 26.0(2) . . . . ? S2 Pt1 S1 C32 -153.6(2) 3_666 . . . ? Br1 Pt1 S1 C32 113.74(19) . . . . ? Br2 Pt1 S1 C32 -64.15(19) . . . . ? O2 Pt1 O1 C31 162.2(5) 3_666 . . . ? S1 Pt1 O1 C31 -19.0(5) . . . . ? Br1 Pt1 O1 C31 -108.4(4) . . . . ? Br2 Pt1 O1 C31 70.8(4) . . . . ? C6 C1 C2 C3 1.3(9) . . . . ? C1 C2 C3 C4 1.6(8) . . . . ? C1 C2 C3 C31 -177.9(5) . . . . ? C2 C3 C4 C5 -4.5(8) . . . . ? C31 C3 C4 C5 175.0(5) . . . . ? C3 C4 C5 C6 4.4(8) . . . . ? C3 C4 C5 C51 -176.1(5) . . . . ? C2 C1 C6 C5 -1.4(9) . . . . ? C4 C5 C6 C1 -1.5(8) . . . . ? C51 C5 C6 C1 179.0(5) . . . . ? Pt1 O1 C31 N1 -1.1(9) . . . . ? Pt1 O1 C31 C3 -178.3(4) . . . . ? C32 N1 C31 O1 14.1(10) . . . . ? C32 N1 C31 C3 -168.7(5) . . . . ? C2 C3 C31 O1 -173.0(5) . . . . ? C4 C3 C31 O1 7.5(7) . . . . ? C2 C3 C31 N1 9.3(8) . . . . ? C4 C3 C31 N1 -170.1(5) . . . . ? C35 N2 C32 N1 -0.6(8) . . . . ? C33 N2 C32 N1 -174.3(5) . . . . ? C35 N2 C32 S1 176.0(4) . . . . ? C33 N2 C32 S1 2.3(7) . . . . ? C31 N1 C32 N2 -178.3(5) . . . . ? C31 N1 C32 S1 5.7(9) . . . . ? Pt1 S1 C32 N2 157.5(4) . . . . ? Pt1 S1 C32 N1 -26.5(5) . . . . ? C32 N2 C33 C34 -93.5(7) . . . . ? C35 N2 C33 C34 92.3(6) . . . . ? C32 N2 C35 C36 -85.6(7) . . . . ? C33 N2 C35 C36 88.5(6) . . . . ? Pt1 O2 C51 N3 -7.9(9) 3_666 . . . ? Pt1 O2 C51 C5 168.2(3) 3_666 . . . ? C52 N3 C51 O2 -10.5(10) . . . . ? C52 N3 C51 C5 173.4(5) . . . . ? C4 C5 C51 O2 -14.4(7) . . . . ? C6 C5 C51 O2 165.1(5) . . . . ? C4 C5 C51 N3 162.4(5) . . . . ? C6 C5 C51 N3 -18.1(7) . . . . ? C53 N4 C52 N3 -177.8(5) . . . . ? C55 N4 C52 N3 0.6(9) . . . . ? C53 N4 C52 S2 5.9(8) . . . . ? C55 N4 C52 S2 -175.7(5) . . . . ? C51 N3 C52 N4 -178.9(6) . . . . ? C51 N3 C52 S2 -3.1(9) . . . . ? Pt1 S2 C52 N4 -159.2(4) 3_666 . . . ? Pt1 S2 C52 N3 25.0(6) 3_666 . . . ? C52 N4 C53 C54 -98.5(7) . . . . ? C55 N4 C53 C54 83.1(7) . . . . ? C52 N4 C55 C56 -83.5(8) . . . . ? C53 N4 C55 C56 94.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.707 _refine_diff_density_min -2.221 _refine_diff_density_rms 0.200 #========================================END data_22MetmacPtCl4 _database_code_depnum_ccdc_archive 'CCDC 272659' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; cis-bis((mu2-3,3,3',3'-tetraethyl-1,1'-isophthaloylbis(thioureato))di chloroplatinum(IV)) ; _chemical_name_common ; cis-bis((mu2-3,3,3',3'-tetraethyl-1,1'- isophthaloylbis(thioureato))di chloroplatinum(IV)) ; _chemical_melting_point '> 210 (decomp.)' _chemical_formula_moiety 'C36 H48 Cl4 N8 O4 Pt2 S4' _chemical_formula_sum 'C36 H48 Cl4 N8 O4 Pt2 S4' _chemical_formula_weight 1317.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2600(19) _cell_length_b 17.863(4) _cell_length_c 14.504(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.08(3) _cell_angle_gamma 90.00 _cell_volume 2293.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 6.556 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.63 _exptl_absorpt_process_details 'Scalepack (Otwinowski &Minor,1997)' _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_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41212 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4480 _reflns_number_gt 3673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO_SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO_SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED (Barbour, 1999)' _computing_publication_material 'X-SEED (Barbour, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.4104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4480 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.69419(2) 0.379806(11) 0.728622(13) 0.03524(10) Uani 1 1 d . . . Cl1A Cl 0.6764(6) 0.47949(16) 0.81903(17) 0.0455(12) Uani 0.593(10) 1 d P A 6 Cl1B Cl 0.5826(11) 0.4675(2) 0.8189(3) 0.0546(19) Uani 0.407(10) 1 d P A 5 Cl2A Cl 0.7190(6) 0.2745(2) 0.6294(3) 0.0426(9) Uani 0.593(10) 1 d P A 9 Cl2B Cl 0.7733(8) 0.2993(4) 0.6404(4) 0.0443(15) Uani 0.407(10) 1 d P A 10 S1A S 0.6228(18) 0.3003(9) 0.8288(8) 0.044(2) Uani 0.593(10) 1 d P A 11 S1B S 0.631(3) 0.2844(13) 0.8129(13) 0.069(5) Uani 0.407(10) 1 d P A 12 S2A S 0.0586(4) 0.6440(2) 0.1827(4) 0.0451(11) Uani 0.593(10) 1 d P . 7 S2B S 0.0903(7) 0.6138(5) 0.1465(4) 0.056(2) Uani 0.407(10) 1 d P . 8 O1 O 0.4841(4) 0.39287(19) 0.6338(2) 0.0420(9) Uani 1 1 d . A . O2 O 0.2431(4) 0.5433(2) 0.3578(3) 0.0626(13) Uani 1 1 d . . . N1 N 0.3444(4) 0.3043(2) 0.6898(3) 0.0424(11) Uani 1 1 d . A . N2 N 0.3879(5) 0.2170(3) 0.8079(3) 0.0531(13) Uani 1 1 d . . . N3 N -0.0041(4) 0.5187(2) 0.2688(3) 0.0390(10) Uani 1 1 d . . . N4 N -0.1628(5) 0.5520(3) 0.1240(3) 0.0687(17) Uani 1 1 d . . . C1 C -0.0386(5) 0.3690(3) 0.4771(4) 0.0447(14) Uani 1 1 d . . . H1 H -0.1330 0.3463 0.4731 0.054 Uiso 1 1 calc R . . C2 C 0.0880(5) 0.3488(3) 0.5506(4) 0.0374(12) Uani 1 1 d . . . H2 H 0.0806 0.3120 0.5963 0.045 Uiso 1 1 calc R . . C3 C 0.2262(5) 0.3822(2) 0.5575(3) 0.0248(10) Uani 1 1 d . A . C4 C 0.2348(5) 0.4367(2) 0.4911(3) 0.0234(9) Uani 1 1 d . . . H4 H 0.3284 0.4609 0.4968 0.028 Uiso 1 1 calc R . . C5 C 0.1072(5) 0.4564(2) 0.4158(3) 0.0242(10) Uani 1 1 d . . . C6 C -0.0299(5) 0.4215(3) 0.4100(3) 0.0365(12) Uani 1 1 d . . . H6 H -0.1177 0.4342 0.3592 0.044 Uiso 1 1 calc R . . C31 C 0.3649(5) 0.3583(2) 0.6343(3) 0.0245(9) Uani 1 1 d . . . C32 C 0.4417(5) 0.2720(3) 0.7670(3) 0.0320(11) Uani 1 1 d . A . C33 C 0.4769(6) 0.1791(3) 0.8964(4) 0.0479(14) Uani 1 1 d . B . H33A H 0.4097 0.1673 0.9364 0.058 Uiso 1 1 calc R . . H33B H 0.5557 0.2140 0.9337 0.058 Uiso 1 1 calc R . . C34 C 0.5506(7) 0.1091(3) 0.8786(5) 0.0692(19) Uani 1 1 d . . . H34A H 0.4731 0.0732 0.8448 0.104 Uiso 1 1 calc R B . H34B H 0.6100 0.0878 0.9403 0.104 Uiso 1 1 calc R . . H34C H 0.6172 0.1202 0.8389 0.104 Uiso 1 1 calc R . . C35 C 0.247(2) 0.1768(9) 0.7505(16) 0.046(5) Uani 0.51(3) 1 d P B 1 H35A H 0.2549 0.1224 0.7640 0.055 Uiso 0.51(3) 1 calc PR B 1 H35B H 0.2290 0.1847 0.6804 0.055 Uiso 0.51(3) 1 calc PR B 1 C36 C 0.123(3) 0.2119(8) 0.7846(11) 0.070(6) Uani 0.51(3) 1 d P B 1 H36A H 0.1448 0.2039 0.8541 0.105 Uiso 0.51(3) 1 calc PR B 1 H36B H 0.0263 0.1888 0.7507 0.105 Uiso 0.51(3) 1 calc PR B 1 H36C H 0.1188 0.2657 0.7710 0.105 Uiso 0.51(3) 1 calc PR B 1 C37 C 0.218(2) 0.2068(10) 0.7861(12) 0.045(5) Uani 0.49(3) 1 d P B 2 H37A H 0.1657 0.2556 0.7723 0.053 Uiso 0.49(3) 1 calc PR B 2 H37B H 0.1935 0.1831 0.8413 0.053 Uiso 0.49(3) 1 calc PR B 2 C38 C 0.172(2) 0.1562(9) 0.6977(15) 0.060(5) Uani 0.49(3) 1 d P B 2 H38A H 0.1920 0.1818 0.6428 0.091 Uiso 0.49(3) 1 calc PR B 2 H38B H 0.0646 0.1444 0.6822 0.091 Uiso 0.49(3) 1 calc PR B 2 H38C H 0.2313 0.1097 0.7111 0.091 Uiso 0.49(3) 1 calc PR B 2 C51 C 0.1170(5) 0.5120(2) 0.3416(3) 0.0247(10) Uani 1 1 d . . . C52 C -0.0333(5) 0.5624(3) 0.1897(3) 0.0314(11) Uani 1 1 d . C . C53 C -0.2081(7) 0.5896(4) 0.0297(4) 0.0592(16) Uani 1 1 d . C . H53A H -0.1178 0.6127 0.0182 0.071 Uiso 1 1 calc R . . H53B H -0.2476 0.5516 -0.0212 0.071 Uiso 1 1 calc R . . C54 C -0.3231(9) 0.6474(5) 0.0219(5) 0.089(2) Uani 1 1 d . . . H54A H -0.3987 0.6295 0.0518 0.133 Uiso 1 1 calc R C . H54B H -0.3722 0.6586 -0.0463 0.133 Uiso 1 1 calc R . . H54C H -0.2753 0.6929 0.0549 0.133 Uiso 1 1 calc R . . C55 C -0.241(2) 0.4767(10) 0.1176(12) 0.073(6) Uani 0.510(14) 1 d P C 4 H55A H -0.3463 0.4840 0.0766 0.088 Uiso 0.510(14) 1 calc PR C 4 H55B H -0.2467 0.4650 0.1832 0.088 Uiso 0.510(14) 1 calc PR C 4 C56 C -0.182(2) 0.4069(8) 0.0808(11) 0.098(7) Uani 0.510(14) 1 d P C 4 H56A H -0.1781 0.4156 0.0150 0.148 Uiso 0.510(14) 1 calc PR C 4 H56B H -0.2500 0.3648 0.0811 0.148 Uiso 0.510(14) 1 calc PR C 4 H56C H -0.0808 0.3953 0.1228 0.148 Uiso 0.510(14) 1 calc PR C 4 C57 C -0.2939(12) 0.5192(9) 0.1617(10) 0.055(4) Uani 0.490(14) 1 d P C 3 H57A H -0.2696 0.5233 0.2327 0.066 Uiso 0.490(14) 1 calc PR C 3 H57B H -0.3914 0.5445 0.1310 0.066 Uiso 0.490(14) 1 calc PR C 3 C58 C -0.296(2) 0.4392(11) 0.1300(12) 0.080(6) Uani 0.490(14) 1 d P C 3 H58A H -0.3007 0.4374 0.0617 0.121 Uiso 0.490(14) 1 calc PR C 3 H58B H -0.3850 0.4140 0.1391 0.121 Uiso 0.490(14) 1 calc PR C 3 H58C H -0.2044 0.4138 0.1685 0.121 Uiso 0.490(14) 1 calc PR C 3 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 0.02655(13) 0.03988(14) 0.03305(13) 0.01782(9) -0.00098(8) -0.00852(8) Cl1A 0.047(3) 0.0477(15) 0.0435(14) -0.0017(11) 0.0161(12) 0.0000(13) Cl1B 0.062(5) 0.067(3) 0.040(2) -0.0084(17) 0.022(2) -0.007(2) Cl2A 0.048(2) 0.0335(19) 0.0424(15) -0.0021(13) 0.0064(15) -0.0091(14) Cl2B 0.035(3) 0.041(4) 0.056(3) 0.001(2) 0.012(2) 0.011(2) S1A 0.034(4) 0.063(5) 0.0274(17) 0.022(2) -0.0029(17) -0.019(3) S1B 0.031(4) 0.076(10) 0.092(11) 0.069(8) 0.003(8) -0.004(5) S2A 0.0295(15) 0.0475(19) 0.049(2) 0.0236(16) -0.0032(13) -0.0019(12) S2B 0.034(3) 0.088(5) 0.033(3) 0.031(3) -0.0089(19) -0.027(3) O1 0.0233(18) 0.054(2) 0.043(2) 0.0279(17) 0.0000(14) -0.0054(15) O2 0.035(2) 0.077(3) 0.058(3) 0.047(2) -0.0132(18) -0.028(2) N1 0.029(2) 0.041(3) 0.048(3) 0.023(2) -0.0035(19) -0.0080(18) N2 0.031(2) 0.055(3) 0.060(3) 0.036(2) -0.007(2) -0.014(2) N3 0.028(2) 0.052(3) 0.032(2) 0.015(2) 0.0016(18) -0.0051(19) N4 0.050(3) 0.086(4) 0.048(3) 0.035(3) -0.020(2) -0.027(3) C1 0.023(3) 0.052(3) 0.054(3) 0.024(3) 0.003(2) -0.011(2) C2 0.030(3) 0.037(3) 0.045(3) 0.017(2) 0.010(2) -0.006(2) C3 0.024(2) 0.025(2) 0.025(2) 0.0038(19) 0.0071(18) 0.0028(18) C4 0.022(2) 0.023(2) 0.026(2) -0.0034(19) 0.0089(19) -0.0034(17) C5 0.021(2) 0.026(2) 0.025(2) -0.0022(19) 0.0072(18) -0.0011(18) C6 0.022(3) 0.044(3) 0.039(3) 0.011(2) 0.000(2) -0.002(2) C31 0.029(3) 0.020(2) 0.025(2) 0.0013(19) 0.0083(19) 0.0020(19) C32 0.029(3) 0.029(3) 0.038(3) 0.009(2) 0.010(2) -0.005(2) C33 0.037(3) 0.051(4) 0.050(3) 0.029(3) 0.004(2) -0.006(2) C34 0.065(4) 0.041(4) 0.081(5) 0.013(3) -0.011(3) -0.002(3) C35 0.047(11) 0.029(8) 0.054(13) 0.017(8) 0.003(10) -0.007(8) C36 0.033(11) 0.071(10) 0.098(12) 0.033(8) 0.008(8) -0.007(7) C37 0.032(14) 0.052(10) 0.049(10) 0.028(8) 0.012(8) -0.006(8) C38 0.057(10) 0.053(9) 0.061(11) -0.004(8) 0.002(9) -0.010(7) C51 0.022(2) 0.025(2) 0.026(2) 0.0002(19) 0.0053(19) -0.0004(18) C52 0.022(2) 0.041(3) 0.030(3) 0.002(2) 0.005(2) 0.001(2) C53 0.058(4) 0.074(4) 0.029(3) 0.010(3) -0.013(3) -0.005(3) C54 0.098(6) 0.109(6) 0.060(4) 0.029(4) 0.023(4) 0.037(5) C55 0.066(11) 0.075(13) 0.053(9) 0.022(9) -0.022(8) -0.025(9) C56 0.156(18) 0.046(9) 0.065(10) 0.003(7) -0.012(10) 0.004(9) C57 0.016(6) 0.083(11) 0.065(9) 0.023(8) 0.009(5) 0.002(6) C58 0.075(12) 0.091(15) 0.062(10) -0.011(10) 0.000(8) -0.029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.040(3) . ? Pt1 O2 2.055(3) 3_666 ? Pt1 Cl2B 2.189(6) . ? Pt1 Cl1A 2.246(2) . ? Pt1 S1A 2.265(15) . ? Pt1 S1B 2.27(2) . ? Pt1 S2B 2.270(4) 3_666 ? Pt1 S2A 2.312(3) 3_666 ? Pt1 Cl2A 2.420(4) . ? Pt1 Cl1B 2.456(5) . ? S1A C32 1.729(15) . ? S1B C32 1.70(2) . ? S2A C52 1.707(6) . ? S2A Pt1 2.312(3) 3_666 ? S2B C52 1.724(6) . ? S2B Pt1 2.270(4) 3_666 ? O1 C31 1.267(5) . ? O2 C51 1.253(5) . ? O2 Pt1 2.055(3) 3_666 ? N1 C31 1.304(6) . ? N1 C32 1.344(6) . ? N2 C32 1.319(6) . ? N2 C33 1.470(6) . ? N2 C35 1.51(2) . ? N2 C37 1.52(2) . ? N3 C51 1.301(6) . ? N3 C52 1.347(6) . ? N4 C52 1.307(6) . ? N4 C53 1.470(7) . ? N4 C55 1.517(16) . ? N4 C57 1.583(12) . ? C1 C6 1.372(6) . ? C1 C2 1.381(7) . ? C1 H1 0.9500 . ? C2 C3 1.388(6) . ? C2 H2 0.9500 . ? C3 C4 1.389(6) . ? C3 C31 1.494(6) . ? C4 C5 1.398(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(6) . ? C5 C51 1.487(6) . ? C6 H6 0.9500 . ? C33 C34 1.483(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.51(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.52(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C53 C54 1.465(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.52(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.50(2) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 84.06(13) . 3_666 ? O1 Pt1 Cl2B 95.6(2) . . ? O2 Pt1 Cl2B 83.0(2) 3_666 . ? O1 Pt1 Cl1A 94.82(16) . . ? O2 Pt1 Cl1A 84.78(18) 3_666 . ? Cl2B Pt1 Cl1A 163.06(15) . . ? O1 Pt1 S1A 96.0(4) . . ? O2 Pt1 S1A 176.9(3) 3_666 . ? Cl2B Pt1 S1A 100.0(4) . . ? Cl1A Pt1 S1A 92.1(3) . . ? O1 Pt1 S1B 96.0(6) . . ? O2 Pt1 S1B 173.3(5) 3_666 . ? Cl2B Pt1 S1B 90.3(5) . . ? Cl1A Pt1 S1B 101.9(5) . . ? S1A Pt1 S1B 9.8(8) . . ? O1 Pt1 S2B 166.7(3) . 3_666 ? O2 Pt1 S2B 96.54(14) 3_666 3_666 ? Cl2B Pt1 S2B 97.6(2) . 3_666 ? Cl1A Pt1 S2B 72.1(2) . 3_666 ? S1A Pt1 S2B 82.7(4) . 3_666 ? S1B Pt1 S2B 85.0(6) . 3_666 ? O1 Pt1 S2A 171.38(19) . 3_666 ? O2 Pt1 S2A 92.94(14) 3_666 3_666 ? Cl2B Pt1 S2A 75.99(16) . 3_666 ? Cl1A Pt1 S2A 92.96(12) . 3_666 ? S1A Pt1 S2A 87.5(4) . 3_666 ? S1B Pt1 S2A 86.0(6) . 3_666 ? S2B Pt1 S2A 21.66(18) 3_666 3_666 ? O1 Pt1 Cl2A 85.77(16) . . ? O2 Pt1 Cl2A 93.62(17) 3_666 . ? Cl2B Pt1 Cl2A 15.27(16) . . ? Cl1A Pt1 Cl2A 178.23(11) . . ? S1A Pt1 Cl2A 89.5(3) . . ? S1B Pt1 Cl2A 79.7(5) . . ? S2B Pt1 Cl2A 107.4(3) 3_666 . ? S2A Pt1 Cl2A 86.36(13) 3_666 . ? O1 Pt1 Cl1B 79.6(2) . . ? O2 Pt1 Cl1B 97.9(2) 3_666 . ? Cl2B Pt1 Cl1B 174.93(16) . . ? Cl1A Pt1 Cl1B 21.31(10) . . ? S1A Pt1 Cl1B 79.0(4) . . ? S1B Pt1 Cl1B 88.7(5) . . ? S2B Pt1 Cl1B 87.2(2) 3_666 . ? S2A Pt1 Cl1B 108.87(14) 3_666 . ? Cl2A Pt1 Cl1B 160.26(16) . . ? C32 S1A Pt1 105.8(6) . . ? C32 S1B Pt1 106.6(11) . . ? C52 S2A Pt1 103.8(2) . 3_666 ? C52 S2B Pt1 105.0(3) . 3_666 ? C31 O1 Pt1 126.9(3) . . ? C51 O2 Pt1 126.8(3) . 3_666 ? C31 N1 C32 130.4(4) . . ? C32 N2 C33 123.1(4) . . ? C32 N2 C35 119.0(7) . . ? C33 N2 C35 115.8(6) . . ? C32 N2 C37 120.0(6) . . ? C33 N2 C37 114.0(6) . . ? C51 N3 C52 130.9(4) . . ? C52 N4 C53 124.3(5) . . ? C52 N4 C55 119.3(7) . . ? C53 N4 C55 110.3(7) . . ? C52 N4 C57 115.7(6) . . ? C53 N4 C57 116.9(6) . . ? C6 C1 C2 120.9(4) . . ? C6 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C1 C2 C3 119.9(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 C31 120.2(4) . . ? C4 C3 C31 120.4(4) . . ? C3 C4 C5 120.7(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 C51 120.2(4) . . ? C4 C5 C51 121.0(4) . . ? C1 C6 C5 120.3(4) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O1 C31 N1 130.5(4) . . ? O1 C31 C3 114.5(4) . . ? N1 C31 C3 115.0(4) . . ? N2 C32 N1 116.5(4) . . ? N2 C32 S1B 113.9(9) . . ? N1 C32 S1B 129.2(8) . . ? N2 C32 S1A 114.9(6) . . ? N1 C32 S1A 128.1(6) . . ? N2 C33 C34 113.9(5) . . ? N2 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? N2 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 C36 103.7(17) . . ? N2 C35 H35A 111.0 . . ? C36 C35 H35A 111.0 . . ? N2 C35 H35B 111.0 . . ? C36 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? N2 C37 C38 105.2(18) . . ? N2 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? N2 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C51 N3 130.2(4) . . ? O2 C51 C5 114.5(4) . . ? N3 C51 C5 115.3(4) . . ? N4 C52 N3 116.8(4) . . ? N4 C52 S2A 116.4(4) . . ? N3 C52 S2A 124.5(4) . . ? N4 C52 S2B 112.0(4) . . ? N3 C52 S2B 129.0(4) . . ? C54 C53 N4 113.4(6) . . ? C54 C53 H53A 108.9 . . ? N4 C53 H53A 108.9 . . ? C54 C53 H53B 108.9 . . ? N4 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 C56 122.3(16) . . ? N4 C55 H55A 106.8 . . ? C56 C55 H55A 106.8 . . ? N4 C55 H55B 106.8 . . ? C56 C55 H55B 106.8 . . ? H55A C55 H55B 106.6 . . ? C58 C57 N4 101.0(12) . . ? C58 C57 H57A 111.6 . . ? N4 C57 H57A 111.6 . . ? C58 C57 H57B 111.6 . . ? N4 C57 H57B 111.6 . . ? H57A C57 H57B 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pt1 S1A C32 13.0(6) . . . . ? Cl2B Pt1 S1A C32 -83.7(7) . . . . ? Cl1A Pt1 S1A C32 108.1(6) . . . . ? S1B Pt1 S1A C32 -78(5) . . . . ? S2B Pt1 S1A C32 179.7(7) 3_666 . . . ? S2A Pt1 S1A C32 -159.0(6) 3_666 . . . ? Cl2A Pt1 S1A C32 -72.7(6) . . . . ? Cl1B Pt1 S1A C32 91.2(7) . . . . ? O1 Pt1 S1B C32 -4.5(9) . . . . ? Cl2B Pt1 S1B C32 -100.1(9) . . . . ? Cl1A Pt1 S1B C32 91.8(9) . . . . ? S1A Pt1 S1B C32 86(6) . . . . ? S2B Pt1 S1B C32 162.2(11) 3_666 . . . ? S2A Pt1 S1B C32 -176.1(10) 3_666 . . . ? Cl2A Pt1 S1B C32 -89.0(9) . . . . ? Cl1B Pt1 S1B C32 74.9(9) . . . . ? O2 Pt1 O1 C31 177.1(4) 3_666 . . . ? Cl2B Pt1 O1 C31 94.8(4) . . . . ? Cl1A Pt1 O1 C31 -98.6(4) . . . . ? S1A Pt1 O1 C31 -6.0(5) . . . . ? S1B Pt1 O1 C31 3.9(6) . . . . ? S2B Pt1 O1 C31 -89.5(7) 3_666 . . . ? Cl2A Pt1 O1 C31 83.1(4) . . . . ? Cl1B Pt1 O1 C31 -83.6(4) . . . . ? C6 C1 C2 C3 0.6(8) . . . . ? C1 C2 C3 C4 1.0(7) . . . . ? C1 C2 C3 C31 -177.4(5) . . . . ? C2 C3 C4 C5 -2.1(6) . . . . ? C31 C3 C4 C5 176.3(4) . . . . ? C3 C4 C5 C6 1.5(6) . . . . ? C3 C4 C5 C51 -177.1(4) . . . . ? C2 C1 C6 C5 -1.1(8) . . . . ? C4 C5 C6 C1 0.1(7) . . . . ? C51 C5 C6 C1 178.7(4) . . . . ? Pt1 O1 C31 N1 -3.8(7) . . . . ? Pt1 O1 C31 C3 177.7(3) . . . . ? C32 N1 C31 O1 4.5(9) . . . . ? C32 N1 C31 C3 -176.9(5) . . . . ? C2 C3 C31 O1 -179.7(4) . . . . ? C4 C3 C31 O1 1.8(6) . . . . ? C2 C3 C31 N1 1.5(6) . . . . ? C4 C3 C31 N1 -176.9(4) . . . . ? C33 N2 C32 N1 -176.1(5) . . . . ? C35 N2 C32 N1 20.8(11) . . . . ? C37 N2 C32 N1 -16.4(11) . . . . ? C33 N2 C32 S1B 10.7(10) . . . . ? C35 N2 C32 S1B -152.4(11) . . . . ? C37 N2 C32 S1B 170.4(12) . . . . ? C33 N2 C32 S1A -3.5(9) . . . . ? C35 N2 C32 S1A -166.6(10) . . . . ? C37 N2 C32 S1A 156.2(10) . . . . ? C31 N1 C32 N2 -178.9(5) . . . . ? C31 N1 C32 S1B -6.9(13) . . . . ? C31 N1 C32 S1A 9.7(10) . . . . ? Pt1 S1B C32 N2 178.9(6) . . . . ? Pt1 S1B C32 N1 6.8(14) . . . . ? Pt1 S1B C32 S1A -83(6) . . . . ? Pt1 S1A C32 N2 170.7(5) . . . . ? Pt1 S1A C32 N1 -17.7(9) . . . . ? Pt1 S1A C32 S1B 82(5) . . . . ? C32 N2 C33 C34 -95.5(7) . . . . ? C35 N2 C33 C34 68.1(10) . . . . ? C37 N2 C33 C34 103.7(10) . . . . ? C32 N2 C35 C36 -100.0(11) . . . . ? C33 N2 C35 C36 95.7(10) . . . . ? C37 N2 C35 C36 1.1(12) . . . . ? C32 N2 C37 C38 88.6(12) . . . . ? C33 N2 C37 C38 -109.9(9) . . . . ? C35 N2 C37 C38 -9.2(13) . . . . ? Pt1 O2 C51 N3 0.3(8) 3_666 . . . ? Pt1 O2 C51 C5 177.6(3) 3_666 . . . ? C52 N3 C51 O2 -1.9(9) . . . . ? C52 N3 C51 C5 -179.2(5) . . . . ? C6 C5 C51 O2 175.4(4) . . . . ? C4 C5 C51 O2 -6.0(6) . . . . ? C6 C5 C51 N3 -6.9(6) . . . . ? C4 C5 C51 N3 171.7(4) . . . . ? C53 N4 C52 N3 -174.4(5) . . . . ? C55 N4 C52 N3 -24.4(13) . . . . ? C57 N4 C52 N3 26.4(10) . . . . ? C53 N4 C52 S2A 22.2(8) . . . . ? C55 N4 C52 S2A 172.1(11) . . . . ? C57 N4 C52 S2A -137.0(8) . . . . ? C53 N4 C52 S2B -9.5(9) . . . . ? C55 N4 C52 S2B 140.5(12) . . . . ? C57 N4 C52 S2B -168.7(9) . . . . ? C51 N3 C52 N4 174.2(5) . . . . ? C51 N3 C52 S2A -23.9(8) . . . . ? C51 N3 C52 S2B 12.3(10) . . . . ? Pt1 S2A C52 N4 -160.4(4) 3_666 . . . ? Pt1 S2A C52 N3 37.6(6) 3_666 . . . ? Pt1 S2A C52 S2B -72.1(4) 3_666 . . . ? Pt1 S2B C52 N4 -178.1(5) 3_666 . . . ? Pt1 S2B C52 N3 -15.5(9) 3_666 . . . ? Pt1 S2B C52 S2A 76.9(4) 3_666 . . . ? C52 N4 C53 C54 -107.1(8) . . . . ? C55 N4 C53 C54 100.6(12) . . . . ? C57 N4 C53 C54 51.9(10) . . . . ? C52 N4 C55 C56 -71.3(14) . . . . ? C53 N4 C55 C56 82.5(13) . . . . ? C57 N4 C55 C56 -169.4(18) . . . . ? C52 N4 C57 C58 -103.3(10) . . . . ? C53 N4 C57 C58 95.9(10) . . . . ? C55 N4 C57 C58 3.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.337 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.113 #========================================END