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 ; Reaction of Halogens with Pt(II) Complexes of N-alkyl- and N,N-dialkyl-N'-benzoylthioureas: Oxidative Addition and Formation of an I2 Inclusion Compound ; _publ_contact_author_name 'Prof. Klaus R Koch' _publ_contact_author_address ; Department of Chemistry 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 3360' _publ_contact_author_email krk@sun.ac.za loop_ _publ_author_name _publ_author_address A.N.Westra ; Department of Chemistry 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 ; C.Esterhuysen ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; K.R.Koch ; Department of Chemistry 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_PtDEBTUI2 _database_code_depnum_ccdc_archive 'CCDC 213425' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; cis-Bis(N,N-diethyl-N'-benzoylthioureato)diiodoplatinum(IV) ; _chemical_name_common cis-Bis(N,N-diethyl-N'-benzoylthioureato)diiodoplatinum(IV) _chemical_melting_point 154-157 _chemical_formula_moiety 'C24 H30 I2 N4 O2 Pt S2' _chemical_formula_sum 'C24 H30 I2 N4 O2 Pt S2' _chemical_formula_weight 919.53 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 8.8108(18) _cell_length_b 10.920(2) _cell_length_c 16.228(3) _cell_angle_alpha 74.23(3) _cell_angle_beta 78.50(3) _cell_angle_gamma 75.76(3) _cell_volume 1441.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7980 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 29.58 _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 7.181 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'Scalepack (Otwinowski &Minor,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 14013 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.99 _reflns_number_total 7598 _reflns_number_gt 5540 _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^)+(0.0154P)^2^+0.0000P] 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 0.00324(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7598 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 0.265939(17) 0.814790(14) 0.272244(9) 0.01942(6) Uani 1 1 d . . . I1 I -0.03084(3) 0.78765(3) 0.280735(19) 0.03406(8) Uani 1 1 d . . . I2 I 0.56309(3) 0.84447(3) 0.258240(19) 0.03401(8) Uani 1 1 d . . . S1A S 0.18985(12) 1.03473(10) 0.22574(6) 0.0275(2) Uani 1 1 d . . . S1B S 0.21837(13) 0.84544(10) 0.40939(6) 0.0260(2) Uani 1 1 d . . . O1A O 0.3116(3) 0.7776(2) 0.15102(16) 0.0269(7) Uani 1 1 d . . . O1B O 0.3353(3) 0.6167(2) 0.31304(17) 0.0248(6) Uani 1 1 d . . . N1A N 0.2565(4) 0.9869(3) 0.0622(2) 0.0232(7) Uani 1 1 d . . . N1B N 0.2149(4) 0.5818(3) 0.4587(2) 0.0247(8) Uani 1 1 d . . . N2A N 0.2792(3) 1.1829(3) 0.0757(2) 0.0216(7) Uani 1 1 d . . . N2B N 0.0928(4) 0.7052(3) 0.5528(2) 0.0230(8) Uani 1 1 d . . . C1A C 0.2715(4) 0.8013(4) 0.0092(2) 0.0214(9) Uani 1 1 d . . . C1B C 0.3385(4) 0.4034(4) 0.3946(2) 0.0218(9) Uani 1 1 d . . . C2A C 0.2330(5) 0.8808(4) -0.0696(3) 0.0349(11) Uani 1 1 d . . . H1A H 0.2098 0.9726 -0.0775 0.042 Uiso 1 1 calc R . . C2B C 0.3042(5) 0.3174(4) 0.4732(3) 0.0321(10) Uani 1 1 d . . . H1B H 0.2551 0.3504 0.5226 0.038 Uiso 1 1 calc R . . C3A C 0.2286(5) 0.8262(5) -0.1369(3) 0.0406(12) Uani 1 1 d . . . H2A H 0.2011 0.8802 -0.1907 0.049 Uiso 1 1 calc R . . C3B C 0.3401(5) 0.1857(4) 0.4804(3) 0.0376(11) Uani 1 1 d . . . H2B H 0.3174 0.1281 0.5347 0.045 Uiso 1 1 calc R . . C4A C 0.2645(5) 0.6927(5) -0.1247(3) 0.0362(11) Uani 1 1 d . . . H3A H 0.2628 0.6552 -0.1709 0.043 Uiso 1 1 calc R . . C4B C 0.4095(5) 0.1365(4) 0.4083(3) 0.0350(11) Uani 1 1 d . . . H3B H 0.4333 0.0455 0.4126 0.042 Uiso 1 1 calc R . . C5A C 0.3026(5) 0.6137(4) -0.0475(3) 0.0367(11) Uani 1 1 d . . . H4A H 0.3270 0.5219 -0.0399 0.044 Uiso 1 1 calc R . . C5B C 0.4437(5) 0.2215(4) 0.3302(3) 0.0330(11) Uani 1 1 d . . . H4B H 0.4926 0.1881 0.2809 0.040 Uiso 1 1 calc R . . C6A C 0.3053(5) 0.6688(4) 0.0199(3) 0.0295(10) Uani 1 1 d . . . H5A H 0.3308 0.6141 0.0738 0.035 Uiso 1 1 calc R . . C6B C 0.4080(5) 0.3541(4) 0.3226(3) 0.0294(10) Uani 1 1 d . . . H5B H 0.4309 0.4115 0.2682 0.035 Uiso 1 1 calc R . . C7A C 0.2770(4) 0.8603(4) 0.0814(2) 0.0226(9) Uani 1 1 d . . . C7B C 0.2932(4) 0.5472(4) 0.3872(3) 0.0214(9) Uani 1 1 d . . . C8A C 0.2507(4) 1.0648(4) 0.1148(2) 0.0223(9) Uani 1 1 d . . . C8B C 0.1714(4) 0.7006(4) 0.4748(2) 0.0194(8) Uani 1 1 d . . . C9A C 0.3024(5) 1.2250(4) -0.0199(2) 0.0291(10) Uani 1 1 d . . . H6A H 0.3587 1.1495 -0.0442 0.035 Uiso 1 1 calc R . . H7A H 0.3699 1.2907 -0.0381 0.035 Uiso 1 1 calc R . . C9B C 0.0731(5) 0.5856(4) 0.6188(3) 0.0285(10) Uani 1 1 d . . . H6B H 0.0539 0.5217 0.5910 0.034 Uiso 1 1 calc R . . H7B H -0.0208 0.6055 0.6617 0.034 Uiso 1 1 calc R . . C10A C 0.1484(5) 1.2820(5) -0.0562(3) 0.0513(15) Uani 1 1 d . . . H9A H 0.0834 1.2159 -0.0410 0.077 Uiso 1 1 calc R . . H8A H 0.1702 1.3108 -0.1193 0.077 Uiso 1 1 calc R . . H10A H 0.0916 1.3564 -0.0319 0.077 Uiso 1 1 calc R . . C10B C 0.2170(6) 0.5261(4) 0.6651(3) 0.0490(14) Uani 1 1 d . . . H8B H 0.3093 0.5026 0.6232 0.074 Uiso 1 1 calc R . . H10B H 0.1978 0.4481 0.7094 0.074 Uiso 1 1 calc R . . H9B H 0.2369 0.5892 0.6925 0.074 Uiso 1 1 calc R . . C11A C 0.2865(5) 1.2772(4) 0.1239(3) 0.0290(10) Uani 1 1 d . . . H11A H 0.3625 1.3316 0.0895 0.035 Uiso 1 1 calc R . . H12A H 0.3279 1.2290 0.1786 0.035 Uiso 1 1 calc R . . C11B C 0.0329(4) 0.8291(4) 0.5800(2) 0.0242(9) Uani 1 1 d . . . H11B H -0.0599 0.8199 0.6253 0.029 Uiso 1 1 calc R . . H12B H -0.0033 0.8979 0.5299 0.029 Uiso 1 1 calc R . . C12A C 0.1299(5) 1.3653(4) 0.1448(3) 0.0455(13) Uani 1 1 d . . . H13A H 0.0901 1.4168 0.0910 0.068 Uiso 1 1 calc R . . H14A H 0.1444 1.4236 0.1778 0.068 Uiso 1 1 calc R . . H15A H 0.0537 1.3126 0.1793 0.068 Uiso 1 1 calc R . . C12B C 0.1539(5) 0.8715(4) 0.6146(3) 0.0352(11) Uani 1 1 d . . . H15B H 0.1824 0.8083 0.6677 0.053 Uiso 1 1 calc R . . H14B H 0.1091 0.9571 0.6271 0.053 Uiso 1 1 calc R . . H13B H 0.2486 0.8766 0.5713 0.053 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 0.02363(9) 0.01724(9) 0.01578(8) -0.00233(6) -0.00181(6) -0.00372(6) I1 0.02742(16) 0.03520(18) 0.04146(19) -0.00641(15) -0.00786(14) -0.01037(13) I2 0.02442(16) 0.03920(19) 0.03821(18) -0.00934(15) -0.00035(13) -0.00909(13) S1A 0.0400(6) 0.0189(5) 0.0184(5) -0.0021(4) -0.0008(5) -0.0016(5) S1B 0.0418(6) 0.0189(5) 0.0168(5) -0.0041(4) 0.0005(5) -0.0090(5) O1A 0.0416(17) 0.0185(15) 0.0171(15) -0.0030(12) -0.0057(13) 0.0003(13) O1B 0.0310(16) 0.0174(15) 0.0219(15) -0.0022(12) -0.0018(12) -0.0014(12) N1A 0.0318(19) 0.0195(18) 0.0185(17) -0.0014(15) -0.0058(15) -0.0070(15) N1B 0.0327(19) 0.0174(18) 0.0210(18) -0.0035(15) -0.0025(15) -0.0021(15) N2A 0.0253(18) 0.0180(18) 0.0199(18) -0.0041(15) -0.0014(14) -0.0032(14) N2B 0.0245(18) 0.0241(19) 0.0199(18) -0.0055(15) -0.0016(15) -0.0052(15) C1A 0.026(2) 0.019(2) 0.017(2) -0.0013(17) -0.0013(17) -0.0054(17) C1B 0.023(2) 0.019(2) 0.023(2) -0.0039(18) -0.0043(17) -0.0044(17) C2A 0.048(3) 0.027(2) 0.032(3) -0.008(2) -0.009(2) -0.006(2) C2B 0.041(3) 0.027(2) 0.028(2) -0.009(2) -0.004(2) -0.004(2) C3A 0.064(3) 0.039(3) 0.023(2) -0.005(2) -0.016(2) -0.013(3) C3B 0.046(3) 0.022(2) 0.039(3) -0.002(2) -0.004(2) -0.006(2) C4A 0.042(3) 0.046(3) 0.029(3) -0.017(2) -0.006(2) -0.012(2) C4B 0.035(3) 0.019(2) 0.054(3) -0.009(2) -0.015(2) -0.004(2) C5A 0.049(3) 0.029(3) 0.038(3) -0.012(2) -0.007(2) -0.013(2) C5B 0.035(3) 0.032(3) 0.037(3) -0.017(2) -0.009(2) -0.002(2) C6A 0.036(2) 0.026(2) 0.027(2) -0.003(2) -0.0059(19) -0.009(2) C6B 0.034(2) 0.030(2) 0.023(2) -0.004(2) -0.0064(19) -0.003(2) C7A 0.018(2) 0.027(2) 0.020(2) -0.0041(19) 0.0012(17) -0.0052(18) C7B 0.022(2) 0.020(2) 0.023(2) -0.0034(18) -0.0063(17) -0.0042(17) C8A 0.020(2) 0.021(2) 0.022(2) 0.0017(18) -0.0046(17) -0.0033(17) C8B 0.019(2) 0.020(2) 0.017(2) -0.0020(17) -0.0031(16) -0.0041(17) C9A 0.042(3) 0.023(2) 0.020(2) -0.0021(18) 0.0040(19) -0.013(2) C9B 0.040(3) 0.025(2) 0.018(2) -0.0032(19) 0.0037(19) -0.012(2) C10A 0.053(3) 0.060(4) 0.028(3) -0.006(3) -0.010(2) 0.009(3) C10B 0.074(4) 0.024(3) 0.050(3) 0.010(2) -0.034(3) -0.012(3) C11A 0.045(3) 0.020(2) 0.027(2) -0.0061(19) -0.008(2) -0.012(2) C11B 0.028(2) 0.020(2) 0.022(2) -0.0108(18) 0.0035(17) -0.0001(18) C12A 0.063(3) 0.031(3) 0.042(3) -0.016(2) -0.002(3) -0.006(2) C12B 0.042(3) 0.030(3) 0.035(3) -0.015(2) -0.003(2) -0.005(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 O1B 2.055(3) . ? Pt1 O1A 2.058(2) . ? Pt1 S1B 2.2814(11) . ? Pt1 S1A 2.2828(12) . ? Pt1 I2 2.6742(6) . ? Pt1 I1 2.6758(6) . ? S1A C8A 1.737(4) . ? S1B C8B 1.742(4) . ? O1A C7A 1.277(4) . ? O1B C7B 1.276(5) . ? N1A C7A 1.307(5) . ? N1A C8A 1.345(4) . ? N1B C7B 1.325(4) . ? N1B C8B 1.340(4) . ? N2A C8A 1.334(5) . ? N2A C11A 1.471(4) . ? N2A C9A 1.481(5) . ? N2B C8B 1.324(4) . ? N2B C9B 1.470(5) . ? N2B C11B 1.477(4) . ? C1A C6A 1.373(5) . ? C1A C2A 1.389(5) . ? C1A C7A 1.496(5) . ? C1B C6B 1.388(5) . ? C1B C2B 1.391(5) . ? C1B C7B 1.499(5) . ? C2A C3A 1.391(5) . ? C2A H1A 0.9500 . ? C2B C3B 1.372(5) . ? C2B H1B 0.9500 . ? C3A C4A 1.380(6) . ? C3A H2A 0.9500 . ? C3B C4B 1.388(6) . ? C3B H2B 0.9500 . ? C4A C5A 1.366(6) . ? C4A H3A 0.9500 . ? C4B C5B 1.379(6) . ? C4B H3B 0.9500 . ? C5A C6A 1.390(5) . ? C5A H4A 0.9500 . ? C5B C6B 1.381(5) . ? C5B H4B 0.9500 . ? C6A H5A 0.9500 . ? C6B H5B 0.9500 . ? C9A C10A 1.510(5) . ? C9A H6A 0.9900 . ? C9A H7A 0.9900 . ? C9B C10B 1.517(5) . ? C9B H6B 0.9900 . ? C9B H7B 0.9900 . ? C10A H9A 0.9800 . ? C10A H8A 0.9800 . ? C10A H10A 0.9800 . ? C10B H8B 0.9800 . ? C10B H10B 0.9800 . ? C10B H9B 0.9800 . ? C11A C12A 1.510(5) . ? C11A H11A 0.9900 . ? C11A H12A 0.9900 . ? C11B C12B 1.513(5) . ? C11B H11B 0.9900 . ? C11B H12B 0.9900 . ? C12A H13A 0.9800 . ? C12A H14A 0.9800 . ? C12A H15A 0.9800 . ? C12B H15B 0.9800 . ? C12B H14B 0.9800 . ? C12B H13B 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 O1B Pt1 O1A 83.98(10) . . ? O1B Pt1 S1B 93.24(8) . . ? O1A Pt1 S1B 177.22(8) . . ? O1B Pt1 S1A 179.51(8) . . ? O1A Pt1 S1A 95.56(8) . . ? S1B Pt1 S1A 87.22(5) . . ? O1B Pt1 I2 90.90(8) . . ? O1A Pt1 I2 90.56(8) . . ? S1B Pt1 I2 89.60(4) . . ? S1A Pt1 I2 88.97(4) . . ? O1B Pt1 I1 89.80(8) . . ? O1A Pt1 I1 87.83(8) . . ? S1B Pt1 I1 92.06(4) . . ? S1A Pt1 I1 90.31(4) . . ? I2 Pt1 I1 178.16(3) . . ? C8A S1A Pt1 104.13(14) . . ? C8B S1B Pt1 104.61(13) . . ? C7A O1A Pt1 125.4(2) . . ? C7B O1B Pt1 126.2(2) . . ? C7A N1A C8A 128.1(3) . . ? C7B N1B C8B 128.8(4) . . ? C8A N2A C11A 122.7(3) . . ? C8A N2A C9A 120.2(3) . . ? C11A N2A C9A 117.1(3) . . ? C8B N2B C9B 121.1(3) . . ? C8B N2B C11B 121.9(3) . . ? C9B N2B C11B 116.9(3) . . ? C6A C1A C2A 119.5(4) . . ? C6A C1A C7A 120.6(4) . . ? C2A C1A C7A 119.9(4) . . ? C6B C1B C2B 118.9(4) . . ? C6B C1B C7B 120.8(4) . . ? C2B C1B C7B 120.2(3) . . ? C1A C2A C3A 120.0(4) . . ? C1A C2A H1A 120.0 . . ? C3A C2A H1A 120.0 . . ? C3B C2B C1B 121.0(4) . . ? C3B C2B H1B 119.5 . . ? C1B C2B H1B 119.5 . . ? C4A C3A C2A 119.3(4) . . ? C4A C3A H2A 120.3 . . ? C2A C3A H2A 120.3 . . ? C2B C3B C4B 120.0(4) . . ? C2B C3B H2B 120.0 . . ? C4B C3B H2B 120.0 . . ? C5A C4A C3A 121.1(4) . . ? C5A C4A H3A 119.4 . . ? C3A C4A H3A 119.4 . . ? C5B C4B C3B 119.2(4) . . ? C5B C4B H3B 120.4 . . ? C3B C4B H3B 120.4 . . ? C4A C5A C6A 119.3(4) . . ? C4A C5A H4A 120.3 . . ? C6A C5A H4A 120.3 . . ? C4B C5B C6B 121.1(4) . . ? C4B C5B H4B 119.5 . . ? C6B C5B H4B 119.5 . . ? C1A C6A C5A 120.7(4) . . ? C1A C6A H5A 119.6 . . ? C5A C6A H5A 119.6 . . ? C5B C6B C1B 119.8(4) . . ? C5B C6B H5B 120.1 . . ? C1B C6B H5B 120.1 . . ? O1A C7A N1A 129.9(4) . . ? O1A C7A C1A 114.3(3) . . ? N1A C7A C1A 115.6(3) . . ? O1B C7B N1B 130.3(4) . . ? O1B C7B C1B 114.9(3) . . ? N1B C7B C1B 114.8(4) . . ? N2A C8A N1A 115.8(3) . . ? N2A C8A S1A 116.8(3) . . ? N1A C8A S1A 127.0(3) . . ? N2B C8B N1B 115.1(4) . . ? N2B C8B S1B 116.6(3) . . ? N1B C8B S1B 128.1(3) . . ? N2A C9A C10A 112.6(3) . . ? N2A C9A H6A 109.1 . . ? C10A C9A H6A 109.1 . . ? N2A C9A H7A 109.1 . . ? C10A C9A H7A 109.1 . . ? H6A C9A H7A 107.8 . . ? N2B C9B C10B 112.2(4) . . ? N2B C9B H6B 109.2 . . ? C10B C9B H6B 109.2 . . ? N2B C9B H7B 109.2 . . ? C10B C9B H7B 109.2 . . ? H6B C9B H7B 107.9 . . ? C9A C10A H9A 109.5 . . ? C9A C10A H8A 109.5 . . ? H9A C10A H8A 109.5 . . ? C9A C10A H10A 109.5 . . ? H9A C10A H10A 109.5 . . ? H8A C10A H10A 109.5 . . ? C9B C10B H8B 109.5 . . ? C9B C10B H10B 109.5 . . ? H8B C10B H10B 109.5 . . ? C9B C10B H9B 109.5 . . ? H8B C10B H9B 109.5 . . ? H10B C10B H9B 109.5 . . ? N2A C11A C12A 114.5(3) . . ? N2A C11A H11A 108.6 . . ? C12A C11A H11A 108.6 . . ? N2A C11A H12A 108.6 . . ? C12A C11A H12A 108.6 . . ? H11A C11A H12A 107.6 . . ? N2B C11B C12B 113.8(3) . . ? N2B C11B H11B 108.8 . . ? C12B C11B H11B 108.8 . . ? N2B C11B H12B 108.8 . . ? C12B C11B H12B 108.8 . . ? H11B C11B H12B 107.7 . . ? C11A C12A H13A 109.5 . . ? C11A C12A H14A 109.5 . . ? H13A C12A H14A 109.5 . . ? C11A C12A H15A 109.5 . . ? H13A C12A H15A 109.5 . . ? H14A C12A H15A 109.5 . . ? C11B C12B H15B 109.5 . . ? C11B C12B H14B 109.5 . . ? H15B C12B H14B 109.5 . . ? C11B C12B H13B 109.5 . . ? H15B C12B H13B 109.5 . . ? H14B C12B H13B 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 O1A Pt1 S1A C8A -13.41(15) . . . . ? S1B Pt1 S1A C8A 166.69(14) . . . . ? I2 Pt1 S1A C8A 77.05(14) . . . . ? I1 Pt1 S1A C8A -101.26(14) . . . . ? O1B Pt1 S1B C8B -27.37(15) . . . . ? S1A Pt1 S1B C8B 152.76(13) . . . . ? I2 Pt1 S1B C8B -118.25(13) . . . . ? I1 Pt1 S1B C8B 62.55(13) . . . . ? O1B Pt1 O1A C7A 170.8(3) . . . . ? S1A Pt1 O1A C7A -9.3(3) . . . . ? I2 Pt1 O1A C7A -98.3(3) . . . . ? I1 Pt1 O1A C7A 80.8(3) . . . . ? O1A Pt1 O1B C7B -154.1(3) . . . . ? S1B Pt1 O1B C7B 25.8(3) . . . . ? I2 Pt1 O1B C7B 115.4(3) . . . . ? I1 Pt1 O1B C7B -66.3(3) . . . . ? C6A C1A C2A C3A 0.1(6) . . . . ? C7A C1A C2A C3A 179.7(4) . . . . ? C6B C1B C2B C3B 1.0(6) . . . . ? C7B C1B C2B C3B 177.8(4) . . . . ? C1A C2A C3A C4A -0.8(7) . . . . ? C1B C2B C3B C4B -1.0(7) . . . . ? C2A C3A C4A C5A 0.7(7) . . . . ? C2B C3B C4B C5B 0.9(6) . . . . ? C3A C4A C5A C6A -0.1(7) . . . . ? C3B C4B C5B C6B -0.9(6) . . . . ? C2A C1A C6A C5A 0.5(6) . . . . ? C7A C1A C6A C5A -179.1(4) . . . . ? C4A C5A C6A C1A -0.6(6) . . . . ? C4B C5B C6B C1B 0.9(6) . . . . ? C2B C1B C6B C5B -0.9(6) . . . . ? C7B C1B C6B C5B -177.7(4) . . . . ? Pt1 O1A C7A N1A 24.9(6) . . . . ? Pt1 O1A C7A C1A -160.3(2) . . . . ? C8A N1A C7A O1A -7.6(7) . . . . ? C8A N1A C7A C1A 177.7(3) . . . . ? C6A C1A C7A O1A -1.3(5) . . . . ? C2A C1A C7A O1A 179.1(4) . . . . ? C6A C1A C7A N1A 174.3(4) . . . . ? C2A C1A C7A N1A -5.3(6) . . . . ? Pt1 O1B C7B N1B -9.7(6) . . . . ? Pt1 O1B C7B C1B 169.8(2) . . . . ? C8B N1B C7B O1B -7.1(7) . . . . ? C8B N1B C7B C1B 173.3(3) . . . . ? C6B C1B C7B O1B -5.6(5) . . . . ? C2B C1B C7B O1B 177.7(4) . . . . ? C6B C1B C7B N1B 174.1(3) . . . . ? C2B C1B C7B N1B -2.7(5) . . . . ? C11A N2A C8A N1A -176.4(3) . . . . ? C9A N2A C8A N1A 4.6(5) . . . . ? C11A N2A C8A S1A 10.3(5) . . . . ? C9A N2A C8A S1A -168.7(3) . . . . ? C7A N1A C8A N2A 159.3(4) . . . . ? C7A N1A C8A S1A -28.1(6) . . . . ? Pt1 S1A C8A N2A -154.4(3) . . . . ? Pt1 S1A C8A N1A 33.2(3) . . . . ? C9B N2B C8B N1B 6.8(5) . . . . ? C11B N2B C8B N1B -178.4(3) . . . . ? C9B N2B C8B S1B -168.4(3) . . . . ? C11B N2B C8B S1B 6.3(5) . . . . ? C7B N1B C8B N2B 179.7(3) . . . . ? C7B N1B C8B S1B -5.7(6) . . . . ? Pt1 S1B C8B N2B -159.9(2) . . . . ? Pt1 S1B C8B N1B 25.5(4) . . . . ? C8A N2A C9A C10A 85.8(5) . . . . ? C11A N2A C9A C10A -93.2(4) . . . . ? C8B N2B C9B C10B 82.0(4) . . . . ? C11B N2B C9B C10B -93.0(4) . . . . ? C8A N2A C11A C12A -89.7(5) . . . . ? C9A N2A C11A C12A 89.3(4) . . . . ? C8B N2B C11B C12B -84.9(4) . . . . ? C9B N2B C11B C12B 90.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.316 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.151 #========================================END data_PtDEBTUBr2 _database_code_depnum_ccdc_archive 'CCDC 213426' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; cis-Bis(N,N-diethyl-N'-benzoylthioureato)platinum(IV) ; _chemical_name_common cis-Bis(N,N-diethyl-N'-benzoylthioureato)platinum(IV) _chemical_melting_point 177-180 _chemical_formula_moiety 'C24 H30 Br2 N4 O2 Pt S2' _chemical_formula_sum 'C24 H30 Br2 N4 O2 Pt S2' _chemical_formula_weight 825.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.321(5) _cell_length_b 15.743(3) _cell_length_c 18.693(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.64(3) _cell_angle_gamma 90.00 _cell_volume 5878(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8488 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 29.58 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 7.663 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.58 _exptl_absorpt_process_details 'Scalepack (Otwinowski &Minor,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 14663 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7786 _reflns_number_gt 5711 _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^)+(0.0271P)^2^+0.0000P] 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 0.000198(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7786 _refine_ls_number_parameters 337 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.012 _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 Pt1A Pt 0.5000 0.161976(11) 0.7500 0.02684(6) Uani 1 2 d S . . Pt1B Pt 0.5000 0.589523(12) 0.7500 0.03782(7) Uani 1 2 d S . . Br1A Br 0.37964(2) 0.15847(3) 0.61176(3) 0.04062(10) Uani 1 1 d . . . Br1B Br 0.42826(2) 0.59214(3) 0.79134(3) 0.05787(13) Uani 1 1 d . . . S1A S 0.48627(5) 0.26418(6) 0.82262(8) 0.0409(3) Uani 1 1 d . . . S1B S 0.43552(5) 0.48547(6) 0.64193(7) 0.0473(3) Uani 1 1 d . . . O1A O 0.48524(12) 0.06703(14) 0.80936(18) 0.0330(6) Uani 1 1 d . . . O1B O 0.44428(13) 0.68694(16) 0.65801(19) 0.0519(8) Uani 1 1 d . . . N1A N 0.41567(15) 0.13696(17) 0.8292(2) 0.0293(7) Uani 1 1 d . . . N1B N 0.34543(14) 0.61844(17) 0.5320(2) 0.0302(7) Uani 1 1 d . . . N2A N 0.39216(15) 0.27446(18) 0.8329(2) 0.0318(7) Uani 1 1 d . . . N2B N 0.30973(15) 0.48198(19) 0.4901(2) 0.0361(7) Uani 1 1 d . . . C1A C 0.43312(17) -0.0127(2) 0.8496(2) 0.0289(8) Uani 1 1 d . . . C1B C 0.35561(18) 0.7682(2) 0.5390(2) 0.0298(8) Uani 1 1 d . . . C2A C 0.41849(18) -0.0193(3) 0.9082(3) 0.0369(9) Uani 1 1 d . . . H1A H 0.4148 0.0305 0.9332 0.044 Uiso 1 1 calc R . . C2B C 0.28863(19) 0.7779(2) 0.4589(3) 0.0370(9) Uani 1 1 d . . . H1B H 0.2601 0.7298 0.4301 0.044 Uiso 1 1 calc R . . C3A C 0.4093(2) -0.0983(3) 0.9304(3) 0.0528(12) Uani 1 1 d . . . H2A H 0.4000 -0.1028 0.9716 0.063 Uiso 1 1 calc R . . C3B C 0.2636(2) 0.8590(3) 0.4208(3) 0.0497(11) Uani 1 1 d . . . H2B H 0.2178 0.8659 0.3663 0.060 Uiso 1 1 calc R . . C4A C 0.4136(2) -0.1700(3) 0.8932(4) 0.0617(14) Uani 1 1 d . . . H3A H 0.4073 -0.2241 0.9089 0.074 Uiso 1 1 calc R . . C4B C 0.3049(2) 0.9284(3) 0.4618(3) 0.0540(12) Uani 1 1 d . . . H3B H 0.2878 0.9830 0.4346 0.065 Uiso 1 1 calc R . . C5A C 0.4268(3) -0.1643(3) 0.8334(4) 0.0632(14) Uani 1 1 d . . . H4A H 0.4284 -0.2143 0.8065 0.076 Uiso 1 1 calc R . . C5B C 0.3706(2) 0.9198(2) 0.5418(3) 0.0521(12) Uani 1 1 d . . . H4B H 0.3987 0.9684 0.5707 0.062 Uiso 1 1 calc R . . C6A C 0.4379(2) -0.0856(2) 0.8125(3) 0.0462(10) Uani 1 1 d . . . H5A H 0.4487 -0.0816 0.7731 0.055 Uiso 1 1 calc R . . C6B C 0.3958(2) 0.8406(2) 0.5802(3) 0.0375(9) Uani 1 1 d . . . H5B H 0.4414 0.8349 0.6357 0.045 Uiso 1 1 calc R . . C7A C 0.44637(17) 0.0716(2) 0.8281(2) 0.0269(7) Uani 1 1 d . . . C7B C 0.38466(17) 0.6837(2) 0.5804(2) 0.0300(8) Uani 1 1 d . . . C8A C 0.42713(17) 0.2196(2) 0.8261(2) 0.0284(8) Uani 1 1 d . . . C8B C 0.35996(18) 0.5352(2) 0.5520(2) 0.0329(8) Uani 1 1 d . A . C9A C 0.34235(19) 0.2442(2) 0.8392(3) 0.0415(10) Uani 1 1 d D . . H7A H 0.3388 0.2856 0.8757 0.050 Uiso 1 1 calc R . . H6A H 0.3574 0.1894 0.8733 0.050 Uiso 1 1 calc R . . C9B C 0.24588(19) 0.5143(3) 0.4027(3) 0.0451(10) Uani 1 1 d D A . H6B H 0.2336 0.5674 0.4165 0.054 Uiso 1 1 calc R . . H7B H 0.2101 0.4721 0.3787 0.054 Uiso 1 1 calc R . . C10A C 0.2752(2) 0.2328(3) 0.7441(3) 0.0705(15) Uani 1 1 d D . . H10A H 0.2604 0.2868 0.7097 0.106 Uiso 1 1 calc R . . H8A H 0.2430 0.2147 0.7511 0.106 Uiso 1 1 calc R . . H9A H 0.2779 0.1896 0.7091 0.106 Uiso 1 1 calc R . . C10B C 0.2509(2) 0.5312(3) 0.3285(3) 0.0622(13) Uani 1 1 d D . . H8B H 0.2874 0.5712 0.3529 0.093 Uiso 1 1 calc R A . H9B H 0.2086 0.5555 0.2726 0.093 Uiso 1 1 calc R . . H10B H 0.2597 0.4778 0.3113 0.093 Uiso 1 1 calc R . . C11A C 0.4004(2) 0.3664(2) 0.8363(3) 0.0386(9) Uani 1 1 d D . . H11A H 0.3564 0.3943 0.8023 0.046 Uiso 1 1 calc R . . H12A H 0.4176 0.3819 0.8042 0.046 Uiso 1 1 calc R . . C11B C 0.3138(4) 0.3891(5) 0.5103(6) 0.0414(17) Uani 0.733(8) 1 d PD A 1 H11B H 0.3593 0.3685 0.5401 0.050 Uiso 0.733(8) 1 calc PR A 1 H12B H 0.2816 0.3583 0.4500 0.050 Uiso 0.733(8) 1 calc PR A 1 C11C C 0.3206(14) 0.3935(17) 0.492(2) 0.041(7) Uiso 0.267(8) 1 d PD A 2 H11C H 0.2762 0.3656 0.4535 0.049 Uiso 0.267(8) 1 calc PR A 2 H11D H 0.3460 0.3742 0.5577 0.049 Uiso 0.267(8) 1 calc PR A 2 C12A C 0.4483(3) 0.3980(3) 0.9368(3) 0.0636(14) Uani 1 1 d D . . H15A H 0.4316 0.3821 0.9689 0.095 Uiso 1 1 calc R . . H13A H 0.4520 0.4600 0.9371 0.095 Uiso 1 1 calc R . . H14A H 0.4925 0.3725 0.9697 0.095 Uiso 1 1 calc R . . C12B C 0.2992(3) 0.3687(3) 0.5738(4) 0.0483(18) Uani 0.733(8) 1 d PD A 1 H12C H 0.3332 0.3949 0.6356 0.072 Uiso 0.733(8) 1 calc PR A 1 H12D H 0.2998 0.3070 0.5811 0.072 Uiso 0.733(8) 1 calc PR A 1 H12E H 0.2549 0.3909 0.5460 0.072 Uiso 0.733(8) 1 calc PR A 1 C12C C 0.3556(8) 0.3594(9) 0.4598(11) 0.048(5) Uani 0.267(8) 1 d PD A 2 H1C H 0.3287 0.3708 0.3924 0.072 Uiso 0.267(8) 1 calc PR A 2 H1D H 0.3618 0.2979 0.4708 0.072 Uiso 0.267(8) 1 calc PR A 2 H1E H 0.3994 0.3869 0.4951 0.072 Uiso 0.267(8) 1 calc PR A 2 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 Pt1A 0.03063(12) 0.02239(10) 0.03854(12) 0.000 0.02741(11) 0.000 Pt1B 0.02814(12) 0.02320(11) 0.02602(12) 0.000 0.00168(10) 0.000 Br1A 0.0327(2) 0.0481(2) 0.0431(2) -0.00024(18) 0.0256(2) 0.00121(18) Br1B 0.0476(3) 0.0560(3) 0.0492(3) -0.0003(2) 0.0223(2) 0.0066(2) S1A 0.0496(7) 0.0289(5) 0.0684(7) -0.0152(5) 0.0491(6) -0.0114(4) S1B 0.0329(6) 0.0272(5) 0.0377(6) -0.0056(4) 0.0035(5) -0.0003(4) O1A 0.0402(16) 0.0278(13) 0.0495(16) 0.0025(11) 0.0374(14) 0.0004(11) O1B 0.0332(16) 0.0251(14) 0.0381(16) 0.0022(12) -0.0031(14) -0.0040(12) N1A 0.0327(18) 0.0268(16) 0.0363(17) -0.0043(12) 0.0259(16) -0.0047(13) N1B 0.0231(16) 0.0301(16) 0.0257(15) 0.0022(13) 0.0106(14) 0.0014(13) N2A 0.0376(19) 0.0276(15) 0.0396(18) -0.0034(13) 0.0293(16) 0.0008(13) N2B 0.0267(18) 0.0382(18) 0.0261(16) -0.0038(14) 0.0096(15) -0.0088(14) C1A 0.0232(19) 0.0285(18) 0.031(2) 0.0019(15) 0.0159(17) -0.0010(15) C1B 0.028(2) 0.0339(19) 0.0289(19) 0.0063(15) 0.0191(18) 0.0053(16) C2A 0.030(2) 0.046(2) 0.031(2) 0.0004(17) 0.0184(18) -0.0103(18) C2B 0.032(2) 0.045(2) 0.037(2) 0.0082(18) 0.024(2) 0.0071(18) C3A 0.042(3) 0.068(3) 0.042(3) 0.013(2) 0.024(2) -0.008(2) C3B 0.042(3) 0.067(3) 0.044(3) 0.023(2) 0.029(2) 0.029(2) C4A 0.062(3) 0.040(3) 0.087(4) 0.024(3) 0.050(3) 0.002(2) C4B 0.067(3) 0.046(3) 0.056(3) 0.020(2) 0.043(3) 0.026(2) C5A 0.076(4) 0.033(2) 0.100(4) 0.004(2) 0.066(4) 0.004(2) C5B 0.070(3) 0.031(2) 0.062(3) 0.007(2) 0.046(3) 0.011(2) C6A 0.053(3) 0.035(2) 0.064(3) 0.001(2) 0.044(3) -0.003(2) C6B 0.042(2) 0.035(2) 0.034(2) 0.0020(17) 0.024(2) 0.0031(18) C7A 0.0242(19) 0.0296(18) 0.0246(18) -0.0015(14) 0.0150(16) -0.0024(15) C7B 0.023(2) 0.035(2) 0.0214(18) 0.0049(15) 0.0097(17) 0.0007(16) C8A 0.027(2) 0.0312(19) 0.0298(19) -0.0038(15) 0.0202(17) -0.0004(15) C8B 0.027(2) 0.039(2) 0.0256(19) -0.0022(16) 0.0138(17) -0.0018(17) C9A 0.044(3) 0.044(2) 0.053(3) -0.0045(19) 0.039(2) 0.0011(19) C9B 0.025(2) 0.056(3) 0.031(2) 0.0004(19) 0.0074(19) -0.0100(19) C10A 0.053(3) 0.093(4) 0.069(4) -0.018(3) 0.042(3) -0.018(3) C10B 0.041(3) 0.087(4) 0.036(2) -0.002(2) 0.015(2) -0.015(2) C11A 0.048(3) 0.029(2) 0.053(3) -0.0038(17) 0.039(2) 0.0016(17) C11B 0.031(4) 0.034(4) 0.039(4) -0.013(3) 0.014(3) -0.013(3) C12A 0.088(4) 0.048(3) 0.059(3) -0.022(2) 0.050(3) -0.012(2) C12B 0.036(3) 0.040(3) 0.054(4) 0.008(3) 0.022(3) -0.001(3) C12C 0.041(10) 0.037(9) 0.039(9) -0.004(7) 0.014(8) 0.003(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 Pt1A O1A 2.044(2) . ? Pt1A O1A 2.044(2) 2_656 ? Pt1A S1A 2.2806(10) . ? Pt1A S1A 2.2806(10) 2_656 ? Pt1A Br1A 2.4603(7) . ? Pt1A Br1A 2.4603(14) 2_656 ? Pt1B O1B 2.043(3) 2_656 ? Pt1B O1B 2.043(3) . ? Pt1B S1B 2.2757(12) . ? Pt1B S1B 2.2757(11) 2_656 ? Pt1B Br1B 2.4626(7) . ? Pt1B Br1B 2.4626(7) 2_656 ? S1A C8A 1.747(4) . ? S1B C8B 1.744(4) . ? O1A C7A 1.281(4) . ? O1B C7B 1.267(4) . ? N1A C7A 1.317(4) . ? N1A C8A 1.345(4) . ? N1B C7B 1.312(4) . ? N1B C8B 1.348(4) . ? N2A C8A 1.327(4) . ? N2A C11A 1.459(4) . ? N2A C9A 1.470(4) . ? N2B C8B 1.340(4) . ? N2B C11C 1.42(3) . ? N2B C9B 1.476(5) . ? N2B C11B 1.496(8) . ? C1A C2A 1.382(5) . ? C1A C6A 1.388(5) . ? C1A C7A 1.492(5) . ? C1B C2B 1.391(5) . ? C1B C6B 1.396(5) . ? C1B C7B 1.478(5) . ? C2A C3A 1.381(5) . ? C2A H1A 0.9500 . ? C2B C3B 1.399(5) . ? C2B H1B 0.9500 . ? C3A C4A 1.368(6) . ? C3A H2A 0.9500 . ? C3B C4B 1.372(6) . ? C3B H2B 0.9500 . ? C4A C5A 1.374(7) . ? C4A H3A 0.9500 . ? C4B C5B 1.370(6) . ? C4B H3B 0.9500 . ? C5A C6A 1.386(5) . ? C5A H4A 0.9500 . ? C5B C6B 1.376(5) . ? C5B H4B 0.9500 . ? C6A H5A 0.9500 . ? C6B H5B 0.9500 . ? C9A C10A 1.491(6) . ? C9A H7A 0.9900 . ? C9A H6A 0.9900 . ? C9B C10B 1.499(5) . ? C9B H6B 0.9900 . ? C9B H7B 0.9900 . ? C10A H10A 0.9800 . ? C10A H8A 0.9800 . ? C10A H9A 0.9800 . ? C10B H8B 0.9800 . ? C10B H9B 0.9800 . ? C10B H10B 0.9800 . ? C11A C12A 1.511(6) . ? C11A H11A 0.9900 . ? C11A H12A 0.9900 . ? C11B C12B 1.501(9) . ? C11B H11B 0.9900 . ? C11B H12B 0.9900 . ? C11C C12C 1.490(14) . ? C11C H11C 0.9900 . ? C11C H11D 0.9900 . ? C12A H15A 0.9800 . ? C12A H13A 0.9800 . ? C12A H14A 0.9800 . ? C12B H12C 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12C H1C 0.9800 . ? C12C H1D 0.9800 . ? C12C H1E 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 O1A Pt1A O1A 86.02(13) . 2_656 ? O1A Pt1A S1A 91.89(7) . . ? O1A Pt1A S1A 177.29(7) 2_656 . ? O1A Pt1A S1A 177.29(7) . 2_656 ? O1A Pt1A S1A 91.89(7) 2_656 2_656 ? S1A Pt1A S1A 90.25(5) . 2_656 ? O1A Pt1A Br1A 89.07(7) . . ? O1A Pt1A Br1A 89.05(7) 2_656 . ? S1A Pt1A Br1A 92.65(3) . . ? S1A Pt1A Br1A 89.17(4) 2_656 . ? O1A Pt1A Br1A 89.05(7) . 2_656 ? O1A Pt1A Br1A 89.07(7) 2_656 2_656 ? S1A Pt1A Br1A 89.17(3) . 2_656 ? S1A Pt1A Br1A 92.65(3) 2_656 2_656 ? Br1A Pt1A Br1A 177.43(2) . 2_656 ? O1B Pt1B O1B 82.72(14) 2_656 . ? O1B Pt1B S1B 177.32(8) 2_656 . ? O1B Pt1B S1B 94.68(8) . . ? O1B Pt1B S1B 94.68(8) 2_656 2_656 ? O1B Pt1B S1B 177.32(8) . 2_656 ? S1B Pt1B S1B 87.92(6) . 2_656 ? O1B Pt1B Br1B 90.01(9) 2_656 . ? O1B Pt1B Br1B 88.55(9) . . ? S1B Pt1B Br1B 90.55(4) . . ? S1B Pt1B Br1B 90.83(4) 2_656 . ? O1B Pt1B Br1B 88.55(9) 2_656 2_656 ? O1B Pt1B Br1B 90.01(9) . 2_656 ? S1B Pt1B Br1B 90.83(4) . 2_656 ? S1B Pt1B Br1B 90.55(4) 2_656 2_656 ? Br1B Pt1B Br1B 178.08(2) . 2_656 ? C8A S1A Pt1A 103.23(12) . . ? C8B S1B Pt1B 104.80(13) . . ? C7A O1A Pt1A 125.1(2) . . ? C7B O1B Pt1B 127.5(2) . . ? C7A N1A C8A 126.7(3) . . ? C7B N1B C8B 128.0(3) . . ? C8A N2A C11A 123.9(3) . . ? C8A N2A C9A 120.5(3) . . ? C11A N2A C9A 115.7(3) . . ? C8B N2B C11C 121.6(12) . . ? C8B N2B C9B 120.8(3) . . ? C11C N2B C9B 115.6(12) . . ? C8B N2B C11B 121.7(4) . . ? C9B N2B C11B 117.3(4) . . ? C2A C1A C6A 119.7(3) . . ? C2A C1A C7A 121.0(3) . . ? C6A C1A C7A 119.3(3) . . ? C2B C1B C6B 118.6(3) . . ? C2B C1B C7B 121.5(3) . . ? C6B C1B C7B 119.9(3) . . ? C3A C2A C1A 120.0(4) . . ? C3A C2A H1A 120.0 . . ? C1A C2A H1A 120.0 . . ? C1B C2B C3B 119.7(4) . . ? C1B C2B H1B 120.2 . . ? C3B C2B H1B 120.2 . . ? C4A C3A C2A 120.1(4) . . ? C4A C3A H2A 120.0 . . ? C2A C3A H2A 120.0 . . ? C4B C3B C2B 120.2(4) . . ? C4B C3B H2B 119.9 . . ? C2B C3B H2B 119.9 . . ? C3A C4A C5A 120.6(4) . . ? C3A C4A H3A 119.7 . . ? C5A C4A H3A 119.7 . . ? C5B C4B C3B 120.6(4) . . ? C5B C4B H3B 119.7 . . ? C3B C4B H3B 119.7 . . ? C4A C5A C6A 119.9(4) . . ? C4A C5A H4A 120.0 . . ? C6A C5A H4A 120.0 . . ? C4B C5B C6B 119.8(4) . . ? C4B C5B H4B 120.1 . . ? C6B C5B H4B 120.1 . . ? C5A C6A C1A 119.7(4) . . ? C5A C6A H5A 120.2 . . ? C1A C6A H5A 120.2 . . ? C5B C6B C1B 121.1(4) . . ? C5B C6B H5B 119.4 . . ? C1B C6B H5B 119.4 . . ? O1A C7A N1A 131.0(3) . . ? O1A C7A C1A 113.1(3) . . ? N1A C7A C1A 115.9(3) . . ? O1B C7B N1B 130.8(3) . . ? O1B C7B C1B 113.3(3) . . ? N1B C7B C1B 116.0(3) . . ? N2A C8A N1A 115.9(3) . . ? N2A C8A S1A 115.6(3) . . ? N1A C8A S1A 128.4(3) . . ? N2B C8B N1B 115.2(3) . . ? N2B C8B S1B 114.6(3) . . ? N1B C8B S1B 130.1(3) . . ? N2A C9A C10A 111.8(3) . . ? N2A C9A H7A 109.3 . . ? C10A C9A H7A 109.3 . . ? N2A C9A H6A 109.3 . . ? C10A C9A H6A 109.3 . . ? H7A C9A H6A 107.9 . . ? N2B C9B C10B 111.3(3) . . ? N2B C9B H6B 109.4 . . ? C10B C9B H6B 109.4 . . ? N2B C9B H7B 109.4 . . ? C10B C9B H7B 109.4 . . ? H6B C9B H7B 108.0 . . ? C9A C10A H10A 109.5 . . ? C9A C10A H8A 109.5 . . ? H10A C10A H8A 109.5 . . ? C9A C10A H9A 109.5 . . ? H10A C10A H9A 109.5 . . ? H8A C10A H9A 109.5 . . ? C9B C10B H8B 109.5 . . ? C9B C10B H9B 109.5 . . ? H8B C10B H9B 109.5 . . ? C9B C10B H10B 109.5 . . ? H8B C10B H10B 109.5 . . ? H9B C10B H10B 109.5 . . ? N2A C11A C12A 111.1(3) . . ? N2A C11A H11A 109.4 . . ? C12A C11A H11A 109.4 . . ? N2A C11A H12A 109.4 . . ? C12A C11A H12A 109.4 . . ? H11A C11A H12A 108.0 . . ? N2B C11B C12B 113.3(6) . . ? N2B C11B H11B 108.9 . . ? C12B C11B H11B 108.9 . . ? N2B C11B H12B 108.9 . . ? C12B C11B H12B 108.9 . . ? H11B C11B H12B 107.7 . . ? N2B C11C C12C 120.8(18) . . ? N2B C11C H11C 107.1 . . ? C12C C11C H11C 107.1 . . ? N2B C11C H11D 107.1 . . ? C12C C11C H11D 107.1 . . ? H11C C11C H11D 106.8 . . ? C11A C12A H15A 109.5 . . ? C11A C12A H13A 109.5 . . ? H15A C12A H13A 109.5 . . ? C11A C12A H14A 109.5 . . ? H15A C12A H14A 109.5 . . ? H13A C12A H14A 109.5 . . ? C11C C12C H1C 109.5 . . ? C11C C12C H1D 109.5 . . ? H1C C12C H1D 109.5 . . ? C11C C12C H1E 109.5 . . ? H1C C12C H1E 109.5 . . ? H1D C12C H1E 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 O1A Pt1A S1A C8A -33.56(15) . . . . ? S1A Pt1A S1A C8A 144.78(14) 2_656 . . . ? Br1A Pt1A S1A C8A 55.60(13) . . . . ? Br1A Pt1A S1A C8A -122.58(13) 2_656 . . . ? O1B Pt1B S1B C8B -18.78(16) . . . . ? S1B Pt1B S1B C8B 160.62(15) 2_656 . . . ? Br1B Pt1B S1B C8B 69.81(14) . . . . ? Br1B Pt1B S1B C8B -108.85(14) 2_656 . . . ? O1A Pt1A O1A C7A -148.7(3) 2_656 . . . ? S1A Pt1A O1A C7A 33.0(3) . . . . ? Br1A Pt1A O1A C7A -59.6(3) . . . . ? Br1A Pt1A O1A C7A 122.1(3) 2_656 . . . ? O1B Pt1B O1B C7B -161.4(4) 2_656 . . . ? S1B Pt1B O1B C7B 19.2(3) . . . . ? Br1B Pt1B O1B C7B -71.2(3) . . . . ? Br1B Pt1B O1B C7B 110.0(3) 2_656 . . . ? C6A C1A C2A C3A 0.6(6) . . . . ? C7A C1A C2A C3A -177.2(3) . . . . ? C6B C1B C2B C3B 1.0(5) . . . . ? C7B C1B C2B C3B -178.5(3) . . . . ? C1A C2A C3A C4A -1.1(6) . . . . ? C1B C2B C3B C4B 0.5(6) . . . . ? C2A C3A C4A C5A -0.1(7) . . . . ? C2B C3B C4B C5B -1.7(7) . . . . ? C3A C4A C5A C6A 1.8(8) . . . . ? C3B C4B C5B C6B 1.4(7) . . . . ? C4A C5A C6A C1A -2.3(7) . . . . ? C2A C1A C6A C5A 1.1(6) . . . . ? C7A C1A C6A C5A 178.9(4) . . . . ? C4B C5B C6B C1B 0.1(6) . . . . ? C2B C1B C6B C5B -1.3(6) . . . . ? C7B C1B C6B C5B 178.2(3) . . . . ? Pt1A O1A C7A N1A -11.8(5) . . . . ? Pt1A O1A C7A C1A 166.4(2) . . . . ? C8A N1A C7A O1A -12.4(6) . . . . ? C8A N1A C7A C1A 169.4(3) . . . . ? C2A C1A C7A O1A 151.9(3) . . . . ? C6A C1A C7A O1A -25.9(5) . . . . ? C2A C1A C7A N1A -29.7(5) . . . . ? C6A C1A C7A N1A 152.6(4) . . . . ? Pt1B O1B C7B N1B -9.4(6) . . . . ? Pt1B O1B C7B C1B 170.5(2) . . . . ? C8B N1B C7B O1B -2.3(7) . . . . ? C8B N1B C7B C1B 177.8(3) . . . . ? C2B C1B C7B O1B -173.5(3) . . . . ? C6B C1B C7B O1B 6.9(5) . . . . ? C2B C1B C7B N1B 6.4(5) . . . . ? C6B C1B C7B N1B -173.2(3) . . . . ? C11A N2A C8A N1A 176.4(3) . . . . ? C9A N2A C8A N1A -2.5(5) . . . . ? C11A N2A C8A S1A 0.7(5) . . . . ? C9A N2A C8A S1A -178.2(3) . . . . ? C7A N1A C8A N2A -176.7(3) . . . . ? C7A N1A C8A S1A -1.7(5) . . . . ? Pt1A S1A C8A N2A -156.6(2) . . . . ? Pt1A S1A C8A N1A 28.4(3) . . . . ? C11C N2B C8B N1B 168.3(10) . . . . ? C9B N2B C8B N1B 5.4(5) . . . . ? C11B N2B C8B N1B -169.5(5) . . . . ? C11C N2B C8B S1B -7.8(10) . . . . ? C9B N2B C8B S1B -170.8(3) . . . . ? C11B N2B C8B S1B 14.4(6) . . . . ? C7B N1B C8B N2B 179.4(3) . . . . ? C7B N1B C8B S1B -5.1(6) . . . . ? Pt1B S1B C8B N2B -166.8(2) . . . . ? Pt1B S1B C8B N1B 17.7(4) . . . . ? C8A N2A C9A C10A -88.4(4) . . . . ? C11A N2A C9A C10A 92.6(4) . . . . ? C8B N2B C9B C10B 80.6(5) . . . . ? C11C N2B C9B C10B -83.3(9) . . . . ? C11B N2B C9B C10B -104.3(5) . . . . ? C8A N2A C11A C12A -94.7(4) . . . . ? C9A N2A C11A C12A 84.3(4) . . . . ? C8B N2B C11B C12B 79.8(7) . . . . ? C11C N2B C11B C12B 175(5) . . . . ? C9B N2B C11B C12B -95.2(6) . . . . ? C8B N2B C11C C12C -73(2) . . . . ? C9B N2B C11C C12C 91(2) . . . . ? C11B N2B C11C C12C -169(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.348 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.122 #========================================END data_PtPBTUI2I2 _database_code_depnum_ccdc_archive 'CCDC 266047' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; trans-Bis(N-benzoyl-N'-propylthiourea-kS)diiodoplatinum(II) di-iodine ; _chemical_name_common ;trans-Bis(N-benzoyl-N'-propylthiourea-kS)diiodoplatinum(ii) di-iodine ; _chemical_melting_point 153-155 _chemical_formula_moiety 'C22 H28 I2 N4 O2 Pt S2, I2' _chemical_formula_sum 'C22 H28 I4 N4 O2 Pt S2' _chemical_formula_weight 1147.29 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 8.5127(17) _cell_length_b 9.4001(19) _cell_length_c 10.064(2) _cell_angle_alpha 77.00(3) _cell_angle_beta 80.70(3) _cell_angle_gamma 86.19(3) _cell_volume 773.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.49 _cell_measurement_theta_max 26.0 _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 8.683 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details 'Scalepack (Otwinowski &Minor,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 21068 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3020 _reflns_number_gt 2923 _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^)+(0.0084P)^2^+1.2740P] 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 0.00535(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3020 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0158 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0314 _refine_ls_wR_factor_gt 0.0312 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.5000 0.5000 0.0000 0.01668(5) Uani 1 2 d S . . I1 I 0.19822(2) 0.44742(2) 0.060903(19) 0.02681(6) Uani 1 1 d . . . I2 I 0.93552(3) 0.87200(2) -0.00950(2) 0.04262(7) Uani 1 1 d . . . S1 S 0.56046(8) 0.28396(7) -0.07249(7) 0.02297(15) Uani 1 1 d . . . O1 O 0.3540(3) 0.3226(3) -0.4672(2) 0.0428(6) Uani 1 1 d . . . N1 N 0.3936(3) 0.4032(2) -0.2788(2) 0.0229(5) Uani 1 1 d . . . H6 H 0.3776 0.4775 -0.2379 0.027 Uiso 1 1 calc R . . N2 N 0.5083(3) 0.1717(2) -0.2754(2) 0.0244(5) Uani 1 1 d . . . H7 H 0.4693 0.1750 -0.3520 0.029 Uiso 1 1 calc R . . C1 C 0.2258(3) 0.5477(3) -0.4402(3) 0.0232(6) Uani 1 1 d . . . C2 C 0.1895(4) 0.5750(3) -0.5741(3) 0.0285(6) Uani 1 1 d . . . H1 H 0.2314 0.5117 -0.6336 0.034 Uiso 1 1 calc R . . C3 C 0.0930(4) 0.6936(4) -0.6204(3) 0.0359(7) Uani 1 1 d . . . H2 H 0.0697 0.7127 -0.7121 0.043 Uiso 1 1 calc R . . C4 C 0.0303(4) 0.7843(4) -0.5334(3) 0.0381(8) Uani 1 1 d . . . H3 H -0.0365 0.8657 -0.5653 0.046 Uiso 1 1 calc R . . C5 C 0.0642(4) 0.7574(4) -0.4003(3) 0.0375(7) Uani 1 1 d . . . H4 H 0.0206 0.8202 -0.3408 0.045 Uiso 1 1 calc R . . C6 C 0.1616(4) 0.6390(3) -0.3532(3) 0.0294(6) Uani 1 1 d . . . H5 H 0.1844 0.6204 -0.2614 0.035 Uiso 1 1 calc R . . C7 C 0.3276(3) 0.4158(3) -0.3984(3) 0.0259(6) Uani 1 1 d . . . C8 C 0.4822(3) 0.2852(3) -0.2179(3) 0.0205(5) Uani 1 1 d . . . C9 C 0.5984(4) 0.0402(3) -0.2192(3) 0.0289(6) Uani 1 1 d . . . H8 H 0.5489 -0.0015 -0.1235 0.035 Uiso 1 1 calc R . . H9 H 0.7087 0.0659 -0.2169 0.035 Uiso 1 1 calc R . . C10 C 0.6015(4) -0.0721(3) -0.3065(3) 0.0367(7) Uani 1 1 d . . . H11 H 0.6497 -0.0286 -0.4022 0.044 Uiso 1 1 calc R . . H10 H 0.6704 -0.1564 -0.2708 0.044 Uiso 1 1 calc R . . C11 C 0.4396(5) -0.1262(4) -0.3089(4) 0.0467(9) Uani 1 1 d . . . H14 H 0.3900 -0.1679 -0.2144 0.070 Uiso 1 1 calc R . . H12 H 0.4507 -0.2013 -0.3637 0.070 Uiso 1 1 calc R . . H13 H 0.3726 -0.0446 -0.3501 0.070 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 0.01751(8) 0.01811(8) 0.01601(8) -0.00356(5) -0.00695(5) -0.00171(5) I1 0.01852(10) 0.03207(11) 0.03238(11) -0.01152(8) -0.00313(7) -0.00535(7) I2 0.04894(14) 0.04041(13) 0.04158(13) -0.00773(9) -0.02097(10) 0.00714(10) S1 0.0296(4) 0.0199(3) 0.0227(3) -0.0061(3) -0.0127(3) 0.0020(3) O1 0.0596(16) 0.0445(14) 0.0348(12) -0.0240(11) -0.0260(11) 0.0220(11) N1 0.0277(13) 0.0221(12) 0.0223(12) -0.0081(9) -0.0109(10) 0.0035(9) N2 0.0325(13) 0.0211(12) 0.0225(12) -0.0075(9) -0.0109(10) 0.0030(10) C1 0.0208(14) 0.0280(15) 0.0207(14) -0.0025(11) -0.0055(11) -0.0036(11) C2 0.0285(15) 0.0365(17) 0.0202(14) -0.0042(12) -0.0057(12) -0.0014(12) C3 0.0316(17) 0.0441(19) 0.0282(16) 0.0052(14) -0.0113(13) -0.0026(14) C4 0.0346(18) 0.0328(17) 0.0412(19) 0.0059(14) -0.0115(15) 0.0057(14) C5 0.0387(18) 0.0330(17) 0.0384(18) -0.0064(14) -0.0048(14) 0.0079(14) C6 0.0315(16) 0.0323(16) 0.0240(15) -0.0044(12) -0.0069(12) 0.0017(13) C7 0.0263(15) 0.0316(15) 0.0213(14) -0.0068(12) -0.0074(11) 0.0006(12) C8 0.0224(14) 0.0201(13) 0.0190(13) -0.0025(10) -0.0045(11) -0.0035(10) C9 0.0357(17) 0.0218(14) 0.0307(16) -0.0047(12) -0.0131(13) 0.0038(12) C10 0.055(2) 0.0237(15) 0.0321(17) -0.0096(13) -0.0084(15) 0.0108(14) C11 0.075(3) 0.0348(18) 0.0362(19) -0.0118(15) -0.0171(18) -0.0086(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 S1 2.3082(9) . ? Pt1 S1 2.3082(9) 2_665 ? Pt1 I1 2.5967(7) . ? Pt1 I1 2.5967(7) 2_665 ? I2 I2 2.7675(8) 2_775 ? S1 C8 1.700(3) . ? O1 C7 1.222(3) . ? N1 C8 1.381(3) . ? N1 C7 1.387(3) . ? N1 H6 0.8800 . ? N2 C8 1.315(3) . ? N2 C9 1.461(4) . ? N2 H7 0.8800 . ? C1 C6 1.387(4) . ? C1 C2 1.395(4) . ? C1 C7 1.485(4) . ? C2 C3 1.379(4) . ? C2 H1 0.9500 . ? C3 C4 1.380(5) . ? C3 H2 0.9500 . ? C4 C5 1.380(5) . ? C4 H3 0.9500 . ? C5 C6 1.384(4) . ? C5 H4 0.9500 . ? C6 H5 0.9500 . ? C9 C10 1.514(4) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.506(5) . ? C10 H11 0.9900 . ? C10 H10 0.9900 . ? C11 H14 0.9800 . ? C11 H12 0.9800 . ? C11 H13 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 S1 Pt1 S1 180.0 . 2_665 ? S1 Pt1 I1 92.68(3) . . ? S1 Pt1 I1 87.32(3) 2_665 . ? S1 Pt1 I1 87.32(3) . 2_665 ? S1 Pt1 I1 92.68(3) 2_665 2_665 ? I1 Pt1 I1 180.000(8) . 2_665 ? C8 S1 Pt1 111.13(10) . . ? C8 N1 C7 126.2(2) . . ? C8 N1 H6 116.9 . . ? C7 N1 H6 116.9 . . ? C8 N2 C9 123.6(2) . . ? C8 N2 H7 118.2 . . ? C9 N2 H7 118.2 . . ? C6 C1 C2 119.5(3) . . ? C6 C1 C7 124.0(2) . . ? C2 C1 C7 116.4(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H1 119.9 . . ? C1 C2 H1 119.9 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H2 120.0 . . ? C4 C3 H2 120.0 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H3 119.8 . . ? C5 C4 H3 119.8 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H4 119.9 . . ? C6 C5 H4 119.9 . . ? C5 C6 C1 119.9(3) . . ? C5 C6 H5 120.1 . . ? C1 C6 H5 120.1 . . ? O1 C7 N1 121.1(3) . . ? O1 C7 C1 121.5(2) . . ? N1 C7 C1 117.4(2) . . ? N2 C8 N1 118.8(2) . . ? N2 C8 S1 119.3(2) . . ? N1 C8 S1 121.9(2) . . ? N2 C9 C10 110.5(2) . . ? N2 C9 H8 109.6 . . ? C10 C9 H8 109.6 . . ? N2 C9 H9 109.6 . . ? C10 C9 H9 109.6 . . ? H8 C9 H9 108.1 . . ? C11 C10 C9 113.8(3) . . ? C11 C10 H11 108.8 . . ? C9 C10 H11 108.8 . . ? C11 C10 H10 108.8 . . ? C9 C10 H10 108.8 . . ? H11 C10 H10 107.7 . . ? C10 C11 H14 109.5 . . ? C10 C11 H12 109.5 . . ? H14 C11 H12 109.5 . . ? C10 C11 H13 109.5 . . ? H14 C11 H13 109.5 . . ? H12 C11 H13 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 I1 Pt1 S1 C8 66.97(10) . . . . ? I1 Pt1 S1 C8 -113.03(10) 2_665 . . . ? C6 C1 C2 C3 1.3(4) . . . . ? C7 C1 C2 C3 178.7(3) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C1 0.3(5) . . . . ? C2 C1 C6 C5 -1.0(4) . . . . ? C7 C1 C6 C5 -178.1(3) . . . . ? C8 N1 C7 O1 -5.5(5) . . . . ? C8 N1 C7 C1 175.4(3) . . . . ? C6 C1 C7 O1 164.5(3) . . . . ? C2 C1 C7 O1 -12.8(4) . . . . ? C6 C1 C7 N1 -16.4(4) . . . . ? C2 C1 C7 N1 166.3(3) . . . . ? C9 N2 C8 N1 -179.2(3) . . . . ? C9 N2 C8 S1 1.8(4) . . . . ? C7 N1 C8 N2 -0.3(4) . . . . ? C7 N1 C8 S1 178.7(2) . . . . ? Pt1 S1 C8 N2 178.42(19) . . . . ? Pt1 S1 C8 N1 -0.6(3) . . . . ? C8 N2 C9 C10 177.8(3) . . . . ? N2 C9 C10 C11 -63.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.930 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.080 #========================================END data_PtPBTUBr4 _database_code_depnum_ccdc_archive 'CCDC 266048' _audit_creation_method 'SHELXL-97 and enCIFer' _chemical_name_systematic ; trans-Bis(N-benzoyl-N'-propylthiourea-kS)tetrabromoplatinum(IV) ; _chemical_name_common ;trans-Bis(N-benzoyl-N'-propylthiourea- kS)tetrabromoplatinum(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C22 H28 Br4 N4 O2 Pt S2, C7 H8' _chemical_formula_sum 'C29 H36 Br4 N4 O2 Pt S2' _chemical_formula_weight 1051.47 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/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 13.568(4) _cell_length_b 13.739(4) _cell_length_c 18.962(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.338(5) _cell_angle_gamma 90.00 _cell_volume 3439.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 26.0 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 8.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.45 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 34743 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6745 _reflns_number_gt 5803 _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^)+(0.0316P)^2^+2.3209P] 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 6745 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.245123(10) 0.319340(10) 0.499425(7) 0.01019(5) Uani 1 1 d . . . Br1 Br 0.10156(3) 0.43201(3) 0.49246(2) 0.01657(9) Uani 1 1 d . . . Br2 Br 0.38833(3) 0.20581(3) 0.50593(2) 0.01495(9) Uani 1 1 d . . . Br3 Br 0.16272(3) 0.25863(3) 0.377642(19) 0.01584(9) Uani 1 1 d . . . Br4 Br 0.32837(3) 0.38125(3) 0.621277(19) 0.01540(9) Uani 1 1 d . . . S1A S 0.15311(7) 0.18880(7) 0.53599(5) 0.0154(2) Uani 1 1 d . . . S1B S 0.33576(7) 0.45038(7) 0.46290(5) 0.0151(2) Uani 1 1 d . . . O1A O 0.1160(2) 0.24968(19) 0.76261(14) 0.0200(6) Uani 1 1 d . . . O1B O 0.4274(2) 0.38442(19) 0.25087(14) 0.0214(6) Uani 1 1 d . . . N1A N 0.1205(2) 0.2966(2) 0.64818(17) 0.0147(7) Uani 1 1 d . . . H6A H 0.1204 0.3471 0.6196 0.018 Uiso 1 1 calc R . . N1B N 0.3775(2) 0.3414(2) 0.35341(17) 0.0144(7) Uani 1 1 d . . . H6B H 0.3639 0.2915 0.3787 0.017 Uiso 1 1 calc R . . N2A N 0.0938(2) 0.1309(2) 0.65096(17) 0.0166(7) Uani 1 1 d . . . H7A H 0.0727 0.1422 0.6907 0.020 Uiso 1 1 calc R . . N2B N 0.4061(2) 0.5069(2) 0.35239(17) 0.0143(7) Uani 1 1 d . . . H7B H 0.4321 0.4948 0.3148 0.017 Uiso 1 1 calc R . . C1A C 0.1237(3) 0.4195(3) 0.7420(2) 0.0171(8) Uani 1 1 d . . . C1B C 0.3849(3) 0.2182(3) 0.2622(2) 0.0141(8) Uani 1 1 d . . . C2A C 0.1323(3) 0.4383(3) 0.8157(2) 0.0201(9) Uani 1 1 d . . . H1A H 0.1366 0.3858 0.8490 0.024 Uiso 1 1 calc R . . C2B C 0.3770(3) 0.2012(3) 0.1884(2) 0.0163(8) Uani 1 1 d . . . H1B H 0.3797 0.2542 0.1567 0.020 Uiso 1 1 calc R . . C3A C 0.1344(3) 0.5331(3) 0.8401(2) 0.0257(10) Uani 1 1 d . . . H2A H 0.1404 0.5456 0.8902 0.031 Uiso 1 1 calc R . . C3B C 0.3653(3) 0.1071(3) 0.1615(2) 0.0188(8) Uani 1 1 d . . . H2B H 0.3590 0.0957 0.1112 0.023 Uiso 1 1 calc R . . C4A C 0.1280(3) 0.6098(3) 0.7923(2) 0.0264(10) Uani 1 1 d . . . H3A H 0.1305 0.6749 0.8095 0.032 Uiso 1 1 calc R . . C4B C 0.3628(3) 0.0294(3) 0.2078(2) 0.0192(9) Uani 1 1 d . . . H3B H 0.3557 -0.0352 0.1893 0.023 Uiso 1 1 calc R . . C5A C 0.1180(3) 0.5916(3) 0.7188(2) 0.0291(10) Uani 1 1 d . . . H4A H 0.1121 0.6444 0.6858 0.035 Uiso 1 1 calc R . . C5B C 0.3707(3) 0.0458(3) 0.2809(2) 0.0190(8) Uani 1 1 d . . . H4B H 0.3691 -0.0075 0.3126 0.023 Uiso 1 1 calc R . . C6A C 0.1164(3) 0.4973(3) 0.6937(2) 0.0250(9) Uani 1 1 d . . . H5A H 0.1103 0.4853 0.6436 0.030 Uiso 1 1 calc R . . C6B C 0.3810(3) 0.1399(3) 0.3080(2) 0.0180(8) Uani 1 1 d . . . H5B H 0.3854 0.1510 0.3581 0.022 Uiso 1 1 calc R . . C7A C 0.1199(3) 0.3158(3) 0.7203(2) 0.0151(8) Uani 1 1 d . . . C7B C 0.3993(3) 0.3202(3) 0.2869(2) 0.0150(8) Uani 1 1 d . . . C8A C 0.1213(3) 0.2066(3) 0.6178(2) 0.0143(8) Uani 1 1 d . . . C8B C 0.3748(3) 0.4318(3) 0.3838(2) 0.0122(7) Uani 1 1 d . . . C9A C 0.0951(3) 0.0296(3) 0.6278(2) 0.0161(8) Uani 1 1 d . . . H9A H 0.1564 0.0174 0.6091 0.019 Uiso 1 1 calc R . . H8A H 0.0349 0.0163 0.5883 0.019 Uiso 1 1 calc R . . C9B C 0.4020(3) 0.6095(2) 0.3740(2) 0.0136(8) Uani 1 1 d . . . H9B H 0.4640 0.6266 0.4108 0.016 Uiso 1 1 calc R . . H8B H 0.3427 0.6201 0.3953 0.016 Uiso 1 1 calc R . . C10A C 0.0949(3) -0.0370(3) 0.6911(2) 0.0227(9) Uani 1 1 d . . . H10A H 0.0320 -0.0262 0.7081 0.027 Uiso 1 1 calc R . . H11A H 0.1530 -0.0206 0.7314 0.027 Uiso 1 1 calc R . . C10B C 0.3933(3) 0.6729(3) 0.3071(2) 0.0163(8) Uani 1 1 d . . . H11B H 0.4535 0.6624 0.2868 0.020 Uiso 1 1 calc R . . H10B H 0.3327 0.6531 0.2699 0.020 Uiso 1 1 calc R . . C11A C 0.1015(3) -0.1439(3) 0.6713(2) 0.0228(9) Uani 1 1 d . . . H13A H 0.0464 -0.1595 0.6295 0.034 Uiso 1 1 calc R . . H14A H 0.0956 -0.1846 0.7126 0.034 Uiso 1 1 calc R . . H12A H 0.1667 -0.1563 0.6591 0.034 Uiso 1 1 calc R . . C11B C 0.3853(3) 0.7798(3) 0.3238(2) 0.0191(9) Uani 1 1 d . . . H12B H 0.3271 0.7902 0.3454 0.029 Uiso 1 1 calc R . . H14B H 0.3763 0.8176 0.2790 0.029 Uiso 1 1 calc R . . H13B H 0.4474 0.8008 0.3580 0.029 Uiso 1 1 calc R . . C21 C 0.2639(4) 0.3615(4) 0.0214(3) 0.0369(12) Uani 1 1 d . . . C22 C 0.1679(4) 0.3180(4) -0.0032(3) 0.0398(13) Uani 1 1 d . . . H21 H 0.1101 0.3514 0.0047 0.048 Uiso 1 1 calc R . . C23 C 0.1535(4) 0.2271(4) -0.0391(3) 0.0466(14) Uani 1 1 d . . . H22 H 0.0880 0.1996 -0.0555 0.056 Uiso 1 1 calc R . . C24 C 0.2410(4) 0.1795(4) -0.0495(3) 0.0454(14) Uani 1 1 d . . . H23 H 0.2343 0.1187 -0.0740 0.054 Uiso 1 1 calc R . . C25 C 0.3362(3) 0.2191(3) -0.0248(2) 0.0254(10) Uani 1 1 d . . . H24 H 0.3943 0.1843 -0.0306 0.031 Uiso 1 1 calc R . . C26 C 0.3473(4) 0.3107(4) 0.0087(3) 0.0361(12) Uani 1 1 d . . . H25 H 0.4129 0.3387 0.0232 0.043 Uiso 1 1 calc R . . C27 C 0.2780(5) 0.4548(4) 0.0632(3) 0.0537(16) Uani 1 1 d . . . H27 H 0.2126 0.4879 0.0571 0.080 Uiso 1 1 calc R . . H26 H 0.3253 0.4968 0.0452 0.080 Uiso 1 1 calc R . . H28 H 0.3054 0.4409 0.1147 0.080 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 0.01342(8) 0.00844(8) 0.00911(8) 0.00098(5) 0.00343(6) 0.00025(5) Br1 0.0187(2) 0.0150(2) 0.0171(2) 0.00339(15) 0.00623(16) 0.00527(15) Br2 0.01766(19) 0.01368(19) 0.01396(19) 0.00236(15) 0.00454(15) 0.00420(14) Br3 0.01820(19) 0.0182(2) 0.01060(18) -0.00089(15) 0.00228(15) -0.00293(15) Br4 0.01805(19) 0.0172(2) 0.01100(18) -0.00193(15) 0.00345(15) -0.00148(14) S1A 0.0232(5) 0.0104(5) 0.0152(5) -0.0010(4) 0.0100(4) -0.0035(4) S1B 0.0236(5) 0.0099(5) 0.0142(5) -0.0004(4) 0.0088(4) -0.0029(4) O1A 0.0316(16) 0.0127(14) 0.0172(14) 0.0015(12) 0.0087(12) 0.0021(12) O1B 0.0351(17) 0.0144(15) 0.0192(15) 0.0009(12) 0.0155(13) -0.0016(12) N1A 0.0235(18) 0.0076(15) 0.0146(17) 0.0006(13) 0.0076(14) -0.0006(13) N1B 0.0207(17) 0.0110(16) 0.0134(16) 0.0032(13) 0.0079(14) -0.0017(13) N2A 0.0260(18) 0.0129(16) 0.0138(16) -0.0003(13) 0.0105(14) 0.0001(14) N2B 0.0182(16) 0.0106(16) 0.0155(17) 0.0002(13) 0.0067(13) 0.0003(13) C1A 0.0143(19) 0.017(2) 0.021(2) -0.0038(17) 0.0064(16) 0.0000(15) C1B 0.0143(19) 0.0130(19) 0.017(2) -0.0032(16) 0.0080(16) 0.0000(15) C2A 0.018(2) 0.022(2) 0.020(2) -0.0045(17) 0.0037(17) -0.0056(16) C2B 0.0138(19) 0.018(2) 0.017(2) 0.0012(16) 0.0042(16) 0.0013(15) C3A 0.028(2) 0.027(2) 0.022(2) -0.0100(19) 0.0068(18) -0.0032(19) C3B 0.020(2) 0.021(2) 0.0145(19) -0.0050(17) 0.0016(16) -0.0006(16) C4A 0.028(2) 0.014(2) 0.038(3) -0.0124(19) 0.009(2) -0.0030(17) C4B 0.018(2) 0.017(2) 0.023(2) -0.0056(17) 0.0044(17) -0.0012(16) C5A 0.046(3) 0.011(2) 0.033(3) 0.0011(19) 0.015(2) 0.004(2) C5B 0.022(2) 0.013(2) 0.023(2) -0.0007(17) 0.0092(17) 0.0024(16) C6A 0.038(3) 0.017(2) 0.023(2) -0.0019(18) 0.0134(19) 0.0026(18) C6B 0.020(2) 0.017(2) 0.018(2) -0.0026(17) 0.0073(16) 0.0011(16) C7A 0.0123(19) 0.019(2) 0.014(2) -0.0006(16) 0.0037(16) 0.0016(15) C7B 0.0176(19) 0.015(2) 0.0126(19) 0.0003(15) 0.0037(16) 0.0042(15) C8A 0.0170(19) 0.0115(19) 0.0148(19) -0.0003(15) 0.0041(16) -0.0032(15) C8B 0.0133(18) 0.0098(18) 0.0134(18) -0.0018(15) 0.0027(15) -0.0004(14) C9A 0.023(2) 0.0113(19) 0.0141(19) 0.0011(15) 0.0041(16) 0.0011(16) C9B 0.0174(19) 0.0092(19) 0.0144(19) -0.0022(15) 0.0042(15) -0.0010(14) C10A 0.036(2) 0.014(2) 0.023(2) 0.0008(18) 0.0159(19) 0.0034(18) C10B 0.018(2) 0.014(2) 0.016(2) 0.0014(16) 0.0026(16) -0.0009(15) C11A 0.035(2) 0.013(2) 0.023(2) 0.0043(17) 0.0120(19) -0.0011(18) C11B 0.030(2) 0.0085(19) 0.016(2) 0.0014(16) -0.0004(17) -0.0025(16) C21 0.046(3) 0.042(3) 0.025(2) 0.012(2) 0.014(2) 0.009(2) C22 0.031(3) 0.055(4) 0.034(3) 0.016(3) 0.010(2) 0.006(2) C23 0.058(4) 0.055(4) 0.030(3) 0.024(3) 0.016(3) 0.016(3) C24 0.070(4) 0.033(3) 0.031(3) 0.014(2) 0.008(3) -0.003(3) C25 0.029(2) 0.027(2) 0.022(2) 0.0111(19) 0.0081(19) 0.0086(19) C26 0.030(3) 0.050(3) 0.030(3) 0.017(2) 0.010(2) 0.005(2) C27 0.073(4) 0.026(3) 0.076(4) -0.002(3) 0.046(4) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S1B 2.3721(10) . ? Pt1 S1A 2.3781(10) . ? Pt1 Br3 2.4672(7) . ? Pt1 Br1 2.4676(6) . ? Pt1 Br2 2.4724(7) . ? Pt1 Br4 2.4766(7) . ? S1A C8A 1.722(4) . ? S1B C8B 1.721(4) . ? O1A C7A 1.221(5) . ? O1B C7B 1.229(4) . ? N1A C8A 1.364(5) . ? N1A C7A 1.395(5) . ? N1A H6A 0.8800 . ? N1B C8B 1.373(5) . ? N1B C7B 1.391(5) . ? N1B H6B 0.8800 . ? N2A C8A 1.313(5) . ? N2A C9A 1.461(5) . ? N2A H7A 0.8800 . ? N2B C8B 1.310(5) . ? N2B C9B 1.473(4) . ? N2B H7B 0.8800 . ? C1A C6A 1.397(6) . ? C1A C2A 1.399(5) . ? C1A C7A 1.480(5) . ? C1B C6B 1.391(5) . ? C1B C2B 1.397(5) . ? C1B C7B 1.476(5) . ? C2A C3A 1.380(6) . ? C2A H1A 0.9500 . ? C2B C3B 1.386(5) . ? C2B H1B 0.9500 . ? C3A C4A 1.380(6) . ? C3A H2A 0.9500 . ? C3B C4B 1.388(6) . ? C3B H2B 0.9500 . ? C4A C5A 1.391(6) . ? C4A H3A 0.9500 . ? C4B C5B 1.384(5) . ? C4B H3B 0.9500 . ? C5A C6A 1.379(6) . ? C5A H4A 0.9500 . ? C5B C6B 1.387(5) . ? C5B H4B 0.9500 . ? C6A H5A 0.9500 . ? C6B H5B 0.9500 . ? C9A C10A 1.510(5) . ? C9A H9A 0.9900 . ? C9A H8A 0.9900 . ? C9B C10B 1.521(5) . ? C9B H9B 0.9900 . ? C9B H8B 0.9900 . ? C10A C11A 1.523(5) . ? C10A H10A 0.9900 . ? C10A H11A 0.9900 . ? C10B C11B 1.512(5) . ? C10B H11B 0.9900 . ? C10B H10B 0.9900 . ? C11A H13A 0.9800 . ? C11A H14A 0.9800 . ? C11A H12A 0.9800 . ? C11B H12B 0.9800 . ? C11B H14B 0.9800 . ? C11B H13B 0.9800 . ? C21 C26 1.397(6) . ? C21 C22 1.412(7) . ? C21 C27 1.496(7) . ? C22 C23 1.414(8) . ? C22 H21 0.9500 . ? C23 C24 1.408(7) . ? C23 H22 0.9500 . ? C24 C25 1.381(7) . ? C24 H23 0.9500 . ? C25 C26 1.401(7) . ? C25 H24 0.9500 . ? C26 H25 0.9500 . ? C27 H27 0.9800 . ? C27 H26 0.9800 . ? C27 H28 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 S1B Pt1 S1A 179.54(3) . . ? S1B Pt1 Br3 97.86(3) . . ? S1A Pt1 Br3 82.12(3) . . ? S1B Pt1 Br1 87.95(3) . . ? S1A Pt1 Br1 91.59(3) . . ? Br3 Pt1 Br1 88.872(18) . . ? S1B Pt1 Br2 92.24(3) . . ? S1A Pt1 Br2 88.22(3) . . ? Br3 Pt1 Br2 90.839(18) . . ? Br1 Pt1 Br2 179.675(15) . . ? S1B Pt1 Br4 81.73(3) . . ? S1A Pt1 Br4 98.29(3) . . ? Br3 Pt1 Br4 179.593(14) . . ? Br1 Pt1 Br4 91.085(18) . . ? Br2 Pt1 Br4 89.204(18) . . ? C8A S1A Pt1 114.41(13) . . ? C8B S1B Pt1 115.22(13) . . ? C8A N1A C7A 126.0(3) . . ? C8A N1A H6A 117.0 . . ? C7A N1A H6A 117.0 . . ? C8B N1B C7B 127.0(3) . . ? C8B N1B H6B 116.5 . . ? C7B N1B H6B 116.5 . . ? C8A N2A C9A 125.9(3) . . ? C8A N2A H7A 117.0 . . ? C9A N2A H7A 117.0 . . ? C8B N2B C9B 126.1(3) . . ? C8B N2B H7B 116.9 . . ? C9B N2B H7B 116.9 . . ? C6A C1A C2A 119.4(4) . . ? C6A C1A C7A 124.2(4) . . ? C2A C1A C7A 116.4(4) . . ? C6B C1B C2B 119.4(3) . . ? C6B C1B C7B 123.8(3) . . ? C2B C1B C7B 116.8(3) . . ? C3A C2A C1A 119.9(4) . . ? C3A C2A H1A 120.0 . . ? C1A C2A H1A 120.0 . . ? C3B C2B C1B 120.0(4) . . ? C3B C2B H1B 120.0 . . ? C1B C2B H1B 120.0 . . ? C2A C3A C4A 120.5(4) . . ? C2A C3A H2A 119.8 . . ? C4A C3A H2A 119.8 . . ? C2B C3B C4B 120.1(4) . . ? C2B C3B H2B 119.9 . . ? C4B C3B H2B 119.9 . . ? C3A C4A C5A 119.8(4) . . ? C3A C4A H3A 120.1 . . ? C5A C4A H3A 120.1 . . ? C5B C4B C3B 120.1(4) . . ? C5B C4B H3B 120.0 . . ? C3B C4B H3B 120.0 . . ? C6A C5A C4A 120.4(4) . . ? C6A C5A H4A 119.8 . . ? C4A C5A H4A 119.8 . . ? C4B C5B C6B 120.1(4) . . ? C4B C5B H4B 120.0 . . ? C6B C5B H4B 120.0 . . ? C5A C6A C1A 120.0(4) . . ? C5A C6A H5A 120.0 . . ? C1A C6A H5A 120.0 . . ? C5B C6B C1B 120.3(4) . . ? C5B C6B H5B 119.8 . . ? C1B C6B H5B 119.8 . . ? O1A C7A N1A 120.9(3) . . ? O1A C7A C1A 122.5(3) . . ? N1A C7A C1A 116.6(3) . . ? O1B C7B N1B 120.8(3) . . ? O1B C7B C1B 122.7(3) . . ? N1B C7B C1B 116.5(3) . . ? N2A C8A N1A 119.0(3) . . ? N2A C8A S1A 118.4(3) . . ? N1A C8A S1A 122.5(3) . . ? N2B C8B N1B 118.6(3) . . ? N2B C8B S1B 118.5(3) . . ? N1B C8B S1B 122.9(3) . . ? N2A C9A C10A 109.7(3) . . ? N2A C9A H9A 109.7 . . ? C10A C9A H9A 109.7 . . ? N2A C9A H8A 109.7 . . ? C10A C9A H8A 109.7 . . ? H9A C9A H8A 108.2 . . ? N2B C9B C10B 108.5(3) . . ? N2B C9B H9B 110.0 . . ? C10B C9B H9B 110.0 . . ? N2B C9B H8B 110.0 . . ? C10B C9B H8B 110.0 . . ? H9B C9B H8B 108.4 . . ? C9A C10A C11A 112.2(3) . . ? C9A C10A H10A 109.2 . . ? C11A C10A H10A 109.2 . . ? C9A C10A H11A 109.2 . . ? C11A C10A H11A 109.2 . . ? H10A C10A H11A 107.9 . . ? C11B C10B C9B 112.1(3) . . ? C11B C10B H11B 109.2 . . ? C9B C10B H11B 109.2 . . ? C11B C10B H10B 109.2 . . ? C9B C10B H10B 109.2 . . ? H11B C10B H10B 107.9 . . ? C10A C11A H13A 109.5 . . ? C10A C11A H14A 109.5 . . ? H13A C11A H14A 109.5 . . ? C10A C11A H12A 109.5 . . ? H13A C11A H12A 109.5 . . ? H14A C11A H12A 109.5 . . ? C10B C11B H12B 109.5 . . ? C10B C11B H14B 109.5 . . ? H12B C11B H14B 109.5 . . ? C10B C11B H13B 109.5 . . ? H12B C11B H13B 109.5 . . ? H14B C11B H13B 109.5 . . ? C26 C21 C22 117.0(5) . . ? C26 C21 C27 120.7(5) . . ? C22 C21 C27 122.2(5) . . ? C21 C22 C23 123.1(5) . . ? C21 C22 H21 118.4 . . ? C23 C22 H21 118.4 . . ? C24 C23 C22 116.8(5) . . ? C24 C23 H22 121.6 . . ? C22 C23 H22 121.6 . . ? C25 C24 C23 121.5(5) . . ? C25 C24 H23 119.3 . . ? C23 C24 H23 119.3 . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H24 119.9 . . ? C26 C25 H24 119.9 . . ? C21 C26 C25 121.4(5) . . ? C21 C26 H25 119.3 . . ? C25 C26 H25 119.3 . . ? C21 C27 H27 109.5 . . ? C21 C27 H26 109.5 . . ? H27 C27 H26 109.5 . . ? C21 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? H26 C27 H28 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 Br3 Pt1 S1A C8A -151.77(15) . . . . ? Br1 Pt1 S1A C8A -63.13(15) . . . . ? Br2 Pt1 S1A C8A 117.14(15) . . . . ? Br4 Pt1 S1A C8A 28.20(15) . . . . ? Br3 Pt1 S1B C8B -31.98(14) . . . . ? Br1 Pt1 S1B C8B -120.56(14) . . . . ? Br2 Pt1 S1B C8B 59.18(14) . . . . ? Br4 Pt1 S1B C8B 148.04(14) . . . . ? C6A C1A C2A C3A -0.6(6) . . . . ? C7A C1A C2A C3A -178.8(4) . . . . ? C6B C1B C2B C3B 0.1(5) . . . . ? C7B C1B C2B C3B 178.8(3) . . . . ? C1A C2A C3A C4A 0.1(6) . . . . ? C1B C2B C3B C4B -0.9(6) . . . . ? C2A C3A C4A C5A 0.9(6) . . . . ? C2B C3B C4B C5B 0.9(6) . . . . ? C3A C4A C5A C6A -1.3(7) . . . . ? C3B C4B C5B C6B 0.0(6) . . . . ? C4A C5A C6A C1A 0.8(7) . . . . ? C2A C1A C6A C5A 0.2(6) . . . . ? C7A C1A C6A C5A 178.2(4) . . . . ? C4B C5B C6B C1B -0.9(6) . . . . ? C2B C1B C6B C5B 0.8(6) . . . . ? C7B C1B C6B C5B -177.8(4) . . . . ? C8A N1A C7A O1A -2.9(6) . . . . ? C8A N1A C7A C1A 177.4(3) . . . . ? C6A C1A C7A O1A -172.2(4) . . . . ? C2A C1A C7A O1A 5.8(6) . . . . ? C6A C1A C7A N1A 7.5(6) . . . . ? C2A C1A C7A N1A -174.4(3) . . . . ? C8B N1B C7B O1B 6.2(6) . . . . ? C8B N1B C7B C1B -172.6(3) . . . . ? C6B C1B C7B O1B 161.4(4) . . . . ? C2B C1B C7B O1B -17.2(5) . . . . ? C6B C1B C7B N1B -19.8(5) . . . . ? C2B C1B C7B N1B 161.6(3) . . . . ? C9A N2A C8A N1A -176.8(3) . . . . ? C9A N2A C8A S1A 5.3(5) . . . . ? C7A N1A C8A N2A 18.5(6) . . . . ? C7A N1A C8A S1A -163.6(3) . . . . ? Pt1 S1A C8A N2A -163.1(3) . . . . ? Pt1 S1A C8A N1A 19.0(4) . . . . ? C9B N2B C8B N1B 175.3(3) . . . . ? C9B N2B C8B S1B -6.7(5) . . . . ? C7B N1B C8B N2B -8.1(6) . . . . ? C7B N1B C8B S1B 174.0(3) . . . . ? Pt1 S1B C8B N2B 166.0(2) . . . . ? Pt1 S1B C8B N1B -16.0(4) . . . . ? C8A N2A C9A C10A 159.9(4) . . . . ? C8B N2B C9B C10B -151.4(4) . . . . ? N2A C9A C10A C11A -177.2(3) . . . . ? N2B C9B C10B C11B 178.3(3) . . . . ? C26 C21 C22 C23 0.1(7) . . . . ? C27 C21 C22 C23 -176.2(5) . . . . ? C21 C22 C23 C24 0.4(7) . . . . ? C22 C23 C24 C25 0.9(7) . . . . ? C23 C24 C25 C26 -2.7(7) . . . . ? C22 C21 C26 C25 -1.9(6) . . . . ? C27 C21 C26 C25 174.4(4) . . . . ? C24 C25 C26 C21 3.3(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.798 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.148 #========================================END