Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KRK@SUN.AC.ZA _publ_contact_author_name 'Prof Klaus R Koch' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name K.R.Koch S.A.Bourne A.Gie A.N.Mautjana J.D.S.Miller data_1 _database_code_CSD 198812 _chemical_name_common ;fac-tris-(N-(pyrolidine)-N'-(2,2- dimethylpropanoyl)thioureato))rhodium(iii) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-tris-(N-(pyrolidine)-N'-(2,2-dimethylpropanoyl)thioureato))rhodium(III) ; _chemical_melting_point '251 - 254 0C' _chemical_formula_moiety 'C30 H51 N6 O3 Rh1 S3 . (C H Cl3)' _chemical_formula_sum 'C31 H52 Cl3 N6 O3 Rh S3' _chemical_formula_weight 862.23 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' Rh Rh -1.1178 0.9187 '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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 10.697(4) _cell_length_b 13.454(6) _cell_length_c 14.432(6) _cell_angle_alpha 84.77(3) _cell_angle_beta 89.81(3) _cell_angle_gamma 78.88(3) _cell_volume 2029.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 16 _cell_measurement_theta_max 17 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.7375 _exptl_absorpt_correction_T_max 0.7930 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4 diffractometer' _diffrn_measurement_method '\w - 2\q' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 20 _diffrn_reflns_number 7123 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 24.98 _reflns_number_total 7123 _reflns_number_gt 5673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLUTO _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^)+(0.1844P)^2^+0.3481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7123 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.2124 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _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 Rh1 Rh 0.65100(4) 0.71662(3) 0.79137(3) 0.0331(2) Uani 1 1 d . . . O1A O 0.5245(4) 0.7422(3) 0.6813(3) 0.0430(9) Uani 1 1 d . . . C2A C 0.4064(6) 0.7755(5) 0.6874(4) 0.0443(13) Uani 1 1 d . . . N3A N 0.3470(5) 0.8420(4) 0.7430(4) 0.0486(12) Uani 1 1 d . . . C4A C 0.3957(5) 0.8803(4) 0.8116(4) 0.0360(12) Uani 1 1 d . . . S5A S 0.53320(13) 0.83235(11) 0.87830(10) 0.0401(4) Uani 1 1 d . . . C2A1 C 0.3198(7) 0.7366(6) 0.6220(5) 0.0590(18) Uani 1 1 d . . . C2A2 C 0.2872(18) 0.8074(14) 0.5421(11) 0.168(6) Uiso 1 1 d . . . H2A1 H 0.2382 0.8698 0.5608 0.201 Uiso 1 1 calc R . . H2A2 H 0.2380 0.7796 0.4993 0.201 Uiso 1 1 calc R . . H2A3 H 0.3637 0.8206 0.5126 0.201 Uiso 1 1 calc R . . C2A3 C 0.1988(13) 0.7185(12) 0.6681(9) 0.131(4) Uiso 1 1 d . . . H2A4 H 0.1453 0.7827 0.6776 0.157 Uiso 1 1 calc R . . H2A5 H 0.2190 0.6796 0.7271 0.157 Uiso 1 1 calc R . . H2A6 H 0.1550 0.6818 0.6292 0.157 Uiso 1 1 calc R . . C2A4 C 0.3786(17) 0.6301(13) 0.6045(12) 0.167(7) Uiso 1 1 d . . . H2A7 H 0.3311 0.6083 0.5565 0.201 Uiso 1 1 calc R . . H2A8 H 0.3776 0.5861 0.6606 0.201 Uiso 1 1 calc R . . H2A9 H 0.4650 0.6276 0.5851 0.201 Uiso 1 1 calc R . . N4A1 N 0.3269(5) 0.9666(4) 0.8382(4) 0.0451(12) Uani 1 1 d . . . C4A2 C 0.3506(6) 1.0160(5) 0.9200(5) 0.0527(16) Uani 1 1 d . . . H4A1 H 0.4224 1.0501 0.9108 0.063 Uiso 1 1 calc R . . H4A2 H 0.3672 0.9673 0.9745 0.063 Uiso 1 1 calc R . . C4A3 C 0.2279(8) 1.0920(6) 0.9299(6) 0.071(2) Uani 1 1 d . . . H4A3 H 0.2441 1.1521 0.9562 0.085 Uiso 1 1 calc R . . H4A4 H 0.1684 1.0621 0.9691 0.085 Uiso 1 1 calc R . . C4A4 C 0.1759(8) 1.1180(6) 0.8293(7) 0.076(2) Uani 1 1 d . . . H4A5 H 0.0845 1.1425 0.8285 0.091 Uiso 1 1 calc R . . H4A6 H 0.2163 1.1695 0.7967 0.091 Uiso 1 1 calc R . . C4A5 C 0.2089(6) 1.0200(5) 0.7866(5) 0.0579(17) Uani 1 1 d . . . H4A7 H 0.2248 1.0313 0.7206 0.069 Uiso 1 1 calc R . . H4A8 H 0.1412 0.9815 0.7950 0.069 Uiso 1 1 calc R . . O1B O 0.7657(4) 0.6183(3) 0.7114(3) 0.0427(9) Uani 1 1 d . . . C2B C 0.7806(5) 0.5228(4) 0.7201(4) 0.0387(12) Uani 1 1 d . . . N3B N 0.7013(5) 0.4647(4) 0.7554(4) 0.0435(11) Uani 1 1 d . . . C4B C 0.5935(5) 0.4922(4) 0.8021(4) 0.0376(12) Uani 1 1 d . . . S5B S 0.54420(14) 0.59985(11) 0.85904(10) 0.0416(4) Uani 1 1 d . . . C2B1 C 0.9023(6) 0.4635(5) 0.6807(5) 0.0481(14) Uani 1 1 d . . . C2B2 C 0.8690(12) 0.4305(10) 0.5890(8) 0.118(4) Uiso 1 1 d . . . H2B1 H 0.9434 0.3905 0.5640 0.142 Uiso 1 1 calc R . . H2B2 H 0.8384 0.4893 0.5466 0.142 Uiso 1 1 calc R . . H2B3 H 0.8040 0.3905 0.5977 0.142 Uiso 1 1 calc R . . C2B3 C 0.9574(12) 0.3750(10) 0.7388(8) 0.111(4) Uiso 1 1 d . . . H2B4 H 0.9735 0.3937 0.7997 0.133 Uiso 1 1 calc R . . H2B5 H 1.0361 0.3434 0.7127 0.133 Uiso 1 1 calc R . . H2B6 H 0.8998 0.3282 0.7434 0.133 Uiso 1 1 calc R . . C2B4 C 0.9944(13) 0.5331(10) 0.6562(9) 0.118(4) Uiso 1 1 d . . . H2B7 H 1.0169 0.5611 0.7113 0.142 Uiso 1 1 calc R . . H2B8 H 0.9554 0.5873 0.6114 0.142 Uiso 1 1 calc R . . H2B9 H 1.0697 0.4954 0.6303 0.142 Uiso 1 1 calc R . . N4B1 N 0.5196(5) 0.4236(4) 0.8099(4) 0.0452(12) Uani 1 1 d . . . C4B2 C 0.4001(6) 0.4343(5) 0.8614(5) 0.0519(15) Uani 1 1 d . . . H4B1 H 0.3425 0.4971 0.8401 0.062 Uiso 1 1 calc R . . H4B2 H 0.4159 0.4335 0.9276 0.062 Uiso 1 1 calc R . . C4B3 C 0.3461(9) 0.3431(7) 0.8404(8) 0.087(3) Uani 1 1 d . . . H4B3 H 0.3020 0.3184 0.8939 0.104 Uiso 1 1 calc R . . H4B4 H 0.2869 0.3603 0.7880 0.104 Uiso 1 1 calc R . . C4B4 C 0.4558(9) 0.2667(7) 0.8183(9) 0.092(3) Uani 1 1 d . . . H4B5 H 0.4308 0.2209 0.7768 0.111 Uiso 1 1 calc R . . H4B6 H 0.4929 0.2272 0.8745 0.111 Uiso 1 1 calc R . . C4B5 C 0.5504(8) 0.3250(5) 0.7713(6) 0.066(2) Uani 1 1 d . . . H4B7 H 0.6374 0.2913 0.7866 0.079 Uiso 1 1 calc R . . H4B8 H 0.5387 0.3325 0.7043 0.079 Uiso 1 1 calc R . . O1C O 0.7321(4) 0.8321(3) 0.7269(3) 0.0402(9) Uani 1 1 d . . . C2C C 0.7967(5) 0.8822(4) 0.7702(4) 0.0373(12) Uani 1 1 d . . . N3C N 0.8811(4) 0.8487(3) 0.8390(4) 0.0415(11) Uani 1 1 d . . . C4C C 0.9044(5) 0.7566(4) 0.8845(4) 0.0364(12) Uani 1 1 d . . . S5C S 0.80164(13) 0.67260(11) 0.90581(10) 0.0406(4) Uani 1 1 d . . . C2C1 C 0.7824(6) 0.9957(4) 0.7367(4) 0.0453(14) Uani 1 1 d . . . C2C2 C 0.8833(8) 1.0052(7) 0.6653(6) 0.073(2) Uiso 1 1 d . . . H2C1 H 0.8652 0.9741 0.6109 0.088 Uiso 1 1 calc R . . H2C2 H 0.9651 0.9718 0.6907 0.088 Uiso 1 1 calc R . . H2C3 H 0.8841 1.0759 0.6488 0.088 Uiso 1 1 calc R . . C2C3 C 0.8037(8) 1.0563(7) 0.8164(6) 0.072(2) Uiso 1 1 d . . . H2C4 H 0.7935 1.1269 0.7944 0.087 Uiso 1 1 calc R . . H2C5 H 0.8884 1.0324 0.8414 0.087 Uiso 1 1 calc R . . H2C6 H 0.7429 1.0480 0.8642 0.087 Uiso 1 1 calc R . . C2C4 C 0.6523(8) 1.0348(7) 0.6939(6) 0.0683(19) Uiso 1 1 d . . . H2C7 H 0.5886 1.0286 0.7399 0.082 Uiso 1 1 calc R . . H2C8 H 0.6402 0.9958 0.6433 0.082 Uiso 1 1 calc R . . H2C9 H 0.6450 1.1050 0.6710 0.082 Uiso 1 1 calc R . . N4C1 N 1.0185(4) 0.7291(4) 0.9256(4) 0.0418(11) Uani 1 1 d . . . C4C2 C 1.0637(6) 0.6328(5) 0.9806(5) 0.0528(16) Uani 1 1 d . . . H4C1 H 1.0608 0.5758 0.9446 0.063 Uiso 1 1 calc R . . H4C2 H 1.0134 0.6267 1.0361 0.063 Uiso 1 1 calc R . . C4C3 C 1.2007(7) 0.6377(7) 1.0055(7) 0.081(3) Uani 1 1 d . . . H4C3 H 1.2222 0.6069 1.0682 0.097 Uiso 1 1 calc R . . H4C4 H 1.2594 0.6020 0.9627 0.097 Uiso 1 1 calc R . . C4C4 C 1.2075(9) 0.7440(8) 0.9985(8) 0.098(3) Uani 1 1 d . . . H4C5 H 1.2924 0.7532 0.9807 0.118 Uiso 1 1 calc R . . H4C6 H 1.1878 0.7717 1.0577 0.118 Uiso 1 1 calc R . . C4C5 C 1.1112(6) 0.7963(5) 0.9253(5) 0.0572(17) Uani 1 1 d . . . H4C7 H 1.0713 0.8635 0.9412 0.069 Uiso 1 1 calc R . . H4C8 H 1.1505 0.8025 0.8649 0.069 Uiso 1 1 calc R . . C1G C 0.7250(9) 0.7871(7) 0.5011(6) 0.082(3) Uani 1 1 d . . . H1G H 0.7070 0.7701 0.5666 0.098 Uiso 1 1 calc R . . Cl1G Cl 0.6240(3) 0.8993(2) 0.4611(2) 0.1160(10) Uani 1 1 d . . . Cl2G Cl 0.7072(4) 0.6885(3) 0.4390(3) 0.1392(13) Uani 1 1 d . . . Cl3G Cl 0.8839(3) 0.8031(4) 0.4918(3) 0.1488(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0311(3) 0.0247(3) 0.0433(3) -0.00842(18) -0.00229(18) -0.00215(18) O1A 0.040(2) 0.047(2) 0.042(2) -0.0143(18) -0.0084(17) -0.0048(18) C2A 0.046(3) 0.035(3) 0.051(3) -0.006(3) -0.008(3) -0.003(3) N3A 0.040(3) 0.044(3) 0.062(3) -0.019(2) -0.008(2) 0.000(2) C4A 0.030(2) 0.026(3) 0.052(3) -0.007(2) 0.000(2) -0.004(2) S5A 0.0367(7) 0.0348(8) 0.0483(8) -0.0167(6) -0.0056(6) 0.0005(6) C2A1 0.057(4) 0.055(4) 0.068(4) -0.019(3) -0.020(3) -0.013(3) N4A1 0.038(2) 0.032(3) 0.064(3) -0.013(2) -0.008(2) 0.002(2) C4A2 0.055(4) 0.037(3) 0.067(4) -0.022(3) 0.005(3) -0.002(3) C4A3 0.075(5) 0.048(4) 0.084(5) -0.024(4) 0.011(4) 0.012(4) C4A4 0.062(4) 0.036(4) 0.126(7) -0.014(4) -0.015(5) 0.005(3) C4A5 0.046(3) 0.043(4) 0.079(4) -0.004(3) -0.007(3) 0.005(3) O1B 0.042(2) 0.033(2) 0.052(2) -0.0081(18) 0.0097(18) -0.0050(17) C2B 0.038(3) 0.030(3) 0.048(3) -0.009(2) 0.001(2) -0.003(2) N3B 0.037(2) 0.027(2) 0.066(3) -0.010(2) 0.011(2) -0.002(2) C4B 0.037(3) 0.024(3) 0.050(3) -0.003(2) 0.000(2) -0.001(2) S5B 0.0424(8) 0.0328(8) 0.0518(8) -0.0127(6) 0.0085(6) -0.0090(6) C2B1 0.040(3) 0.038(3) 0.062(4) -0.011(3) 0.011(3) 0.005(3) N4B1 0.043(3) 0.026(2) 0.069(3) -0.014(2) 0.011(2) -0.007(2) C4B2 0.049(3) 0.046(4) 0.065(4) -0.015(3) 0.008(3) -0.014(3) C4B3 0.076(6) 0.074(6) 0.126(8) -0.034(5) 0.033(5) -0.042(5) C4B4 0.088(6) 0.049(5) 0.149(9) -0.026(5) 0.029(6) -0.027(5) C4B5 0.068(4) 0.030(3) 0.105(6) -0.023(4) 0.027(4) -0.016(3) O1C 0.045(2) 0.033(2) 0.042(2) 0.0006(17) -0.0078(17) -0.0093(18) C2C 0.030(3) 0.028(3) 0.052(3) -0.007(2) 0.003(2) 0.000(2) N3C 0.037(2) 0.024(2) 0.062(3) -0.002(2) -0.010(2) -0.0013(19) C4C 0.033(3) 0.027(3) 0.047(3) -0.007(2) -0.002(2) 0.001(2) S5C 0.0396(7) 0.0305(7) 0.0508(8) 0.0012(6) -0.0087(6) -0.0064(6) C2C1 0.046(3) 0.028(3) 0.059(3) 0.003(3) -0.012(3) -0.003(2) N4C1 0.034(2) 0.032(3) 0.057(3) 0.004(2) -0.007(2) -0.004(2) C4C2 0.045(3) 0.033(3) 0.074(4) 0.010(3) -0.015(3) 0.002(3) C4C3 0.050(4) 0.074(6) 0.108(6) 0.019(5) -0.026(4) 0.003(4) C4C4 0.072(5) 0.079(6) 0.143(9) 0.018(6) -0.050(6) -0.022(5) C4C5 0.044(3) 0.046(4) 0.082(5) 0.002(3) -0.014(3) -0.014(3) C1G 0.079(6) 0.077(6) 0.076(5) -0.008(4) 0.004(4) 0.020(5) Cl1G 0.0963(19) 0.0897(19) 0.141(2) -0.0005(17) -0.0146(17) 0.0302(15) Cl2G 0.153(3) 0.105(2) 0.160(3) -0.060(2) -0.010(2) -0.003(2) Cl3G 0.0761(17) 0.162(4) 0.205(4) -0.078(3) -0.002(2) 0.013(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 Rh1 O1A 2.051(4) . ? Rh1 O1B 2.058(4) . ? Rh1 O1C 2.070(4) . ? Rh1 S5B 2.2654(17) . ? Rh1 S5C 2.2686(17) . ? Rh1 S5A 2.2749(17) . ? O1A C2A 1.262(7) . ? C2A N3A 1.325(8) . ? C2A C2A1 1.518(9) . ? N3A C4A 1.311(8) . ? C4A N4A1 1.337(8) . ? C4A S5A 1.742(6) . ? C2A1 C2A2 1.425(17) . ? C2A1 C2A4 1.493(18) . ? C2A1 C2A3 1.504(14) . ? N4A1 C4A2 1.454(8) . ? N4A1 C4A5 1.491(8) . ? C4A2 C4A3 1.516(10) . ? C4A3 C4A4 1.541(12) . ? C4A4 C4A5 1.487(10) . ? O1B C2B 1.258(7) . ? C2B N3B 1.331(7) . ? C2B C2B1 1.527(8) . ? N3B C4B 1.340(7) . ? C4B N4B1 1.324(7) . ? C4B S5B 1.723(6) . ? C2B1 C2B3 1.421(13) . ? C2B1 C2B2 1.499(14) . ? C2B1 C2B4 1.505(14) . ? N4B1 C4B5 1.464(8) . ? N4B1 C4B2 1.466(8) . ? C4B2 C4B3 1.508(10) . ? C4B3 C4B4 1.459(13) . ? C4B4 C4B5 1.517(11) . ? O1C C2C 1.257(7) . ? C2C N3C 1.332(8) . ? C2C C2C1 1.538(8) . ? N3C C4C 1.327(7) . ? C4C N4C1 1.329(7) . ? C4C S5C 1.731(6) . ? C2C1 C2C4 1.503(10) . ? C2C1 C2C2 1.506(10) . ? C2C1 C2C3 1.512(10) . ? N4C1 C4C2 1.455(7) . ? N4C1 C4C5 1.465(8) . ? C4C2 C4C3 1.524(10) . ? C4C3 C4C4 1.440(13) . ? C4C4 C4C5 1.505(11) . ? C1G Cl2G 1.708(11) . ? C1G Cl1G 1.730(9) . ? C1G Cl3G 1.756(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Rh1 O1B 85.93(17) . . ? O1A Rh1 O1C 86.79(16) . . ? O1B Rh1 O1C 87.72(16) . . ? O1A Rh1 S5B 89.43(13) . . ? O1B Rh1 S5B 95.85(12) . . ? O1C Rh1 S5B 174.61(11) . . ? O1A Rh1 S5C 173.63(12) . . ? O1B Rh1 S5C 87.96(13) . . ? O1C Rh1 S5C 94.79(11) . . ? S5B Rh1 S5C 89.39(6) . . ? O1A Rh1 S5A 95.25(13) . . ? O1B Rh1 S5A 176.29(11) . . ? O1C Rh1 S5A 88.84(13) . . ? S5B Rh1 S5A 87.69(6) . . ? S5C Rh1 S5A 90.96(6) . . ? C2A O1A Rh1 124.5(4) . . ? O1A C2A N3A 128.3(5) . . ? O1A C2A C2A1 116.8(6) . . ? N3A C2A C2A1 114.9(6) . . ? C4A N3A C2A 128.0(5) . . ? N3A C4A N4A1 115.7(5) . . ? N3A C4A S5A 129.8(4) . . ? N4A1 C4A S5A 114.4(4) . . ? C4A S5A Rh1 104.4(2) . . ? C2A2 C2A1 C2A4 116.6(11) . . ? C2A2 C2A1 C2A3 108.6(11) . . ? C2A4 C2A1 C2A3 99.9(10) . . ? C2A2 C2A1 C2A 110.4(9) . . ? C2A4 C2A1 C2A 108.8(8) . . ? C2A3 C2A1 C2A 112.2(8) . . ? C4A N4A1 C4A2 126.2(5) . . ? C4A N4A1 C4A5 121.5(5) . . ? C4A2 N4A1 C4A5 112.3(5) . . ? N4A1 C4A2 C4A3 103.3(6) . . ? C4A2 C4A3 C4A4 103.8(6) . . ? C4A5 C4A4 C4A3 104.1(6) . . ? C4A4 C4A5 N4A1 103.4(6) . . ? C2B O1B Rh1 126.1(4) . . ? O1B C2B N3B 128.9(5) . . ? O1B C2B C2B1 116.9(5) . . ? N3B C2B C2B1 114.1(5) . . ? C2B N3B C4B 128.5(5) . . ? N4B1 C4B N3B 114.6(5) . . ? N4B1 C4B S5B 116.3(4) . . ? N3B C4B S5B 128.9(4) . . ? C4B S5B Rh1 105.2(2) . . ? C2B3 C2B1 C2B2 107.9(9) . . ? C2B3 C2B1 C2B4 113.1(8) . . ? C2B2 C2B1 C2B4 104.1(8) . . ? C2B3 C2B1 C2B 113.2(7) . . ? C2B2 C2B1 C2B 107.8(7) . . ? C2B4 C2B1 C2B 110.2(7) . . ? C4B N4B1 C4B5 123.9(5) . . ? C4B N4B1 C4B2 124.6(5) . . ? C4B5 N4B1 C4B2 111.4(5) . . ? N4B1 C4B2 C4B3 104.0(6) . . ? C4B4 C4B3 C4B2 105.3(7) . . ? C4B3 C4B4 C4B5 106.0(7) . . ? N4B1 C4B5 C4B4 103.0(6) . . ? C2C O1C Rh1 122.9(3) . . ? O1C C2C N3C 128.3(5) . . ? O1C C2C C2C1 116.4(5) . . ? N3C C2C C2C1 115.2(5) . . ? C4C N3C C2C 126.9(5) . . ? N3C C4C N4C1 115.4(5) . . ? N3C C4C S5C 128.5(4) . . ? N4C1 C4C S5C 115.8(4) . . ? C4C S5C Rh1 104.9(2) . . ? C2C4 C2C1 C2C2 110.1(6) . . ? C2C4 C2C1 C2C3 110.4(6) . . ? C2C2 C2C1 C2C3 108.4(6) . . ? C2C4 C2C1 C2C 109.8(5) . . ? C2C2 C2C1 C2C 107.4(6) . . ? C2C3 C2C1 C2C 110.7(5) . . ? C4C N4C1 C4C2 125.0(5) . . ? C4C N4C1 C4C5 123.2(5) . . ? C4C2 N4C1 C4C5 111.7(5) . . ? N4C1 C4C2 C4C3 103.4(5) . . ? C4C4 C4C3 C4C2 106.3(7) . . ? C4C3 C4C4 C4C5 106.6(7) . . ? N4C1 C4C5 C4C4 103.6(6) . . ? Cl2G C1G Cl1G 112.0(6) . . ? Cl2G C1G Cl3G 108.2(5) . . ? Cl1G C1G Cl3G 109.6(6) . . ? 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 O1B Rh1 O1A C2A 157.6(5) . . . . ? O1C Rh1 O1A C2A -114.5(5) . . . . ? S5B Rh1 O1A C2A 61.7(5) . . . . ? S5C Rh1 O1A C2A 141.0(9) . . . . ? S5A Rh1 O1A C2A -26.0(5) . . . . ? Rh1 O1A C2A N3A 34.8(9) . . . . ? Rh1 O1A C2A C2A1 -146.4(5) . . . . ? O1A C2A N3A C4A -8.2(11) . . . . ? C2A1 C2A N3A C4A 173.0(6) . . . . ? C2A N3A C4A N4A1 160.5(6) . . . . ? C2A N3A C4A S5A -23.4(10) . . . . ? N3A C4A S5A Rh1 19.5(6) . . . . ? N4A1 C4A S5A Rh1 -164.5(4) . . . . ? O1A Rh1 S5A C4A 2.0(2) . . . . ? O1B Rh1 S5A C4A 110.4(18) . . . . ? O1C Rh1 S5A C4A 88.6(2) . . . . ? S5B Rh1 S5A C4A -87.24(19) . . . . ? S5C Rh1 S5A C4A -176.59(19) . . . . ? O1A C2A C2A1 C2A2 -97.1(10) . . . . ? N3A C2A C2A1 C2A2 81.9(11) . . . . ? O1A C2A C2A1 C2A4 32.1(11) . . . . ? N3A C2A C2A1 C2A4 -148.9(9) . . . . ? O1A C2A C2A1 C2A3 141.7(8) . . . . ? N3A C2A C2A1 C2A3 -39.3(10) . . . . ? N3A C4A N4A1 C4A2 170.8(6) . . . . ? S5A C4A N4A1 C4A2 -5.9(8) . . . . ? N3A C4A N4A1 C4A5 -5.7(9) . . . . ? S5A C4A N4A1 C4A5 177.7(5) . . . . ? C4A N4A1 C4A2 C4A3 -165.6(6) . . . . ? C4A5 N4A1 C4A2 C4A3 11.1(8) . . . . ? N4A1 C4A2 C4A3 C4A4 -28.8(8) . . . . ? C4A2 C4A3 C4A4 C4A5 36.9(8) . . . . ? C4A3 C4A4 C4A5 N4A1 -29.4(8) . . . . ? C4A N4A1 C4A5 C4A4 -171.2(6) . . . . ? C4A2 N4A1 C4A5 C4A4 11.9(8) . . . . ? O1A Rh1 O1B C2B -102.0(5) . . . . ? O1C Rh1 O1B C2B 171.1(5) . . . . ? S5B Rh1 O1B C2B -13.0(5) . . . . ? S5C Rh1 O1B C2B 76.2(5) . . . . ? S5A Rh1 O1B C2B 149.3(16) . . . . ? Rh1 O1B C2B N3B 25.8(9) . . . . ? Rh1 O1B C2B C2B1 -157.8(4) . . . . ? O1B C2B N3B C4B -10.1(11) . . . . ? C2B1 C2B N3B C4B 173.4(6) . . . . ? C2B N3B C4B N4B1 165.0(6) . . . . ? C2B N3B C4B S5B -19.7(9) . . . . ? N4B1 C4B S5B Rh1 -161.3(4) . . . . ? N3B C4B S5B Rh1 23.5(6) . . . . ? O1A Rh1 S5B C4B 78.5(2) . . . . ? O1B Rh1 S5B C4B -7.4(2) . . . . ? O1C Rh1 S5B C4B 123.9(12) . . . . ? S5C Rh1 S5B C4B -95.2(2) . . . . ? S5A Rh1 S5B C4B 173.8(2) . . . . ? O1B C2B C2B1 C2B3 139.6(8) . . . . ? N3B C2B C2B1 C2B3 -43.4(9) . . . . ? O1B C2B C2B1 C2B2 -101.2(8) . . . . ? N3B C2B C2B1 C2B2 75.8(8) . . . . ? O1B C2B C2B1 C2B4 11.9(9) . . . . ? N3B C2B C2B1 C2B4 -171.2(7) . . . . ? N3B C4B N4B1 C4B5 -0.1(9) . . . . ? S5B C4B N4B1 C4B5 -176.0(6) . . . . ? N3B C4B N4B1 C4B2 177.1(6) . . . . ? S5B C4B N4B1 C4B2 1.1(8) . . . . ? C4B N4B1 C4B2 C4B3 173.9(7) . . . . ? C4B5 N4B1 C4B2 C4B3 -8.7(9) . . . . ? N4B1 C4B2 C4B3 C4B4 25.5(10) . . . . ? C4B2 C4B3 C4B4 C4B5 -32.9(11) . . . . ? C4B N4B1 C4B5 C4B4 166.7(7) . . . . ? C4B2 N4B1 C4B5 C4B4 -10.8(10) . . . . ? C4B3 C4B4 C4B5 N4B1 26.9(11) . . . . ? O1A Rh1 O1C C2C 157.0(4) . . . . ? O1B Rh1 O1C C2C -117.0(4) . . . . ? S5B Rh1 O1C C2C 111.5(11) . . . . ? S5C Rh1 O1C C2C -29.2(4) . . . . ? S5A Rh1 O1C C2C 61.6(4) . . . . ? Rh1 O1C C2C N3C 39.7(8) . . . . ? Rh1 O1C C2C C2C1 -143.8(4) . . . . ? O1C C2C N3C C4C -8.7(10) . . . . ? C2C1 C2C N3C C4C 174.8(6) . . . . ? C2C N3C C4C N4C1 157.2(6) . . . . ? C2C N3C C4C S5C -28.9(9) . . . . ? N3C C4C S5C Rh1 24.3(6) . . . . ? N4C1 C4C S5C Rh1 -161.8(4) . . . . ? O1A Rh1 S5C C4C 105.3(11) . . . . ? O1B Rh1 S5C C4C 88.8(2) . . . . ? O1C Rh1 S5C C4C 1.2(2) . . . . ? S5B Rh1 S5C C4C -175.4(2) . . . . ? S5A Rh1 S5C C4C -87.7(2) . . . . ? O1C C2C C2C1 C2C4 28.4(8) . . . . ? N3C C2C C2C1 C2C4 -154.7(6) . . . . ? O1C C2C C2C1 C2C2 -91.4(6) . . . . ? N3C C2C C2C1 C2C2 85.6(7) . . . . ? O1C C2C C2C1 C2C3 150.5(6) . . . . ? N3C C2C C2C1 C2C3 -32.5(8) . . . . ? N3C C4C N4C1 C4C2 178.7(6) . . . . ? S5C C4C N4C1 C4C2 4.1(8) . . . . ? N3C C4C N4C1 C4C5 2.8(9) . . . . ? S5C C4C N4C1 C4C5 -171.8(5) . . . . ? C4C N4C1 C4C2 C4C3 176.6(7) . . . . ? C4C5 N4C1 C4C2 C4C3 -7.1(8) . . . . ? N4C1 C4C2 C4C3 C4C4 22.8(10) . . . . ? C4C2 C4C3 C4C4 C4C5 -29.9(12) . . . . ? C4C N4C1 C4C5 C4C4 166.1(7) . . . . ? C4C2 N4C1 C4C5 C4C4 -10.3(9) . . . . ? C4C3 C4C4 C4C5 N4C1 24.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.293 _refine_diff_density_min -2.611 _refine_diff_density_rms 0.170 data_2 _database_code_CSD 198813 _chemical_name_common ;bis-(N-piperidyl-N'-(2,2- dimethylpropanoyl)thioureato)platinum(ii) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(N-piperidyl-N'-(2,2-dimethylpropanoyl)thioureato)platinum(II) ; _chemical_melting_point '206 - 210 oC' _chemical_formula_moiety 'C22 H38 N4 O2 Pt S2' _chemical_formula_sum 'C22 H38 N4 O2 Pt S2' _chemical_formula_weight 649.77 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 9.951(2) _cell_length_b 15.235(3) _cell_length_c 18.358(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.20(3) _cell_angle_gamma 90.00 _cell_volume 2685.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min -23 _cell_measurement_theta_max 23 _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 5.404 _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.5387 _exptl_absorpt_correction_T_max 0.9962 _diffrn_ambient_temperature 198(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 CAD4 diffractometer' _diffrn_measurement_method '\w - 2\q' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 20 _diffrn_reflns_number 21204 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5902 _reflns_number_gt 5195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'Nonius CAD4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLUTO _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^)+(0.0459P)^2^+3.8184P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00280(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5902 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.661 _refine_ls_shift/su_mean 0.074 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 0.035012(14) 0.985322(10) 0.149611(7) 0.02542(8) Uani 1 1 d . . . S1A S -0.14850(12) 0.99210(7) 0.04926(6) 0.0313(2) Uani 1 1 d . . . O1 O 0.2012(4) 0.9886(2) 0.2418(2) 0.0425(8) Uani 1 1 d . . . S1 S -0.03188(11) 0.84967(7) 0.17203(6) 0.0365(2) Uani 1 1 d . . . O1A O 0.1063(3) 1.1052(2) 0.13325(16) 0.0394(7) Uani 1 1 d . . . N1A N -0.0607(3) 1.1624(2) 0.02984(19) 0.0311(7) Uani 1 1 d . . . N2 N 0.1097(4) 0.7178(3) 0.2480(2) 0.0427(9) Uani 1 1 d . . . N2A N -0.2591(4) 1.1122(3) -0.0504(2) 0.0387(9) Uani 1 1 d . . . C1A C -0.1509(4) 1.0950(3) 0.0096(2) 0.0281(8) Uani 1 1 d . . . N1 N 0.2034(4) 0.8490(3) 0.29276(19) 0.0372(8) Uani 1 1 d . . . C1 C 0.1053(4) 0.8049(3) 0.2414(2) 0.0326(9) Uani 1 1 d . . . C2A C 0.0558(4) 1.1626(3) 0.0845(2) 0.0301(8) Uani 1 1 d . . . C8 C 0.3467(5) 0.9633(4) 0.3633(3) 0.0470(12) Uani 1 1 d . . . C2 C 0.2383(4) 0.9318(3) 0.2928(2) 0.0328(9) Uani 1 1 d . . . C8A C 0.1457(5) 1.2459(3) 0.0902(2) 0.0411(10) Uani 1 1 d . . . C7A C -0.3708(4) 1.0500(3) -0.0829(3) 0.0419(10) Uani 1 1 d . . . H7A1 H -0.3549 0.9954 -0.0547 0.050 Uiso 1 1 calc R . . H7A2 H -0.3716 1.0374 -0.1348 0.050 Uiso 1 1 calc R . . C3A C -0.2759(5) 1.1965(3) -0.0899(3) 0.0479(12) Uani 1 1 d . . . H3A1 H -0.2739 1.1876 -0.1419 0.057 Uiso 1 1 calc R . . H3A2 H -0.1994 1.2351 -0.0661 0.057 Uiso 1 1 calc R . . C3 C 0.2185(6) 0.6721(3) 0.3067(3) 0.0536(13) Uani 1 1 d . . . H3A H 0.1748 0.6357 0.3373 0.064 Uiso 1 1 calc R . . H3B H 0.2766 0.7150 0.3395 0.064 Uiso 1 1 calc R . . C4A C -0.4133(6) 1.2387(4) -0.0876(3) 0.0602(14) Uani 1 1 d . . . H4A1 H -0.4109 1.2535 -0.0359 0.072 Uiso 1 1 calc R . . H4A2 H -0.4263 1.2926 -0.1168 0.072 Uiso 1 1 calc R . . C6A C -0.5099(5) 1.0885(4) -0.0802(3) 0.0567(14) Uani 1 1 d . . . H6A1 H -0.5122 1.0952 -0.0280 0.068 Uiso 1 1 calc R . . H6A2 H -0.5839 1.0486 -0.1046 0.068 Uiso 1 1 calc R . . C5A C -0.5344(5) 1.1774(5) -0.1193(4) 0.0713(17) Uani 1 1 d . . . H5A1 H -0.5457 1.1697 -0.1731 0.086 Uiso 1 1 calc R . . H5A2 H -0.6194 1.2030 -0.1124 0.086 Uiso 1 1 calc R . . C4 C 0.3066(6) 0.6162(4) 0.2703(4) 0.0673(16) Uani 1 1 d . . . H4A H 0.3767 0.5861 0.3090 0.081 Uiso 1 1 calc R . . H4B H 0.3539 0.6531 0.2418 0.081 Uiso 1 1 calc R . . C9A C 0.2306(8) 1.2609(5) 0.1701(3) 0.089(3) Uani 1 1 d . . . H9A1 H 0.1696 1.2660 0.2026 0.134 Uiso 1 1 calc R . . H9A2 H 0.2837 1.3139 0.1725 0.134 Uiso 1 1 calc R . . H9A3 H 0.2928 1.2123 0.1861 0.134 Uiso 1 1 calc R . . C5 C 0.2178(8) 0.5496(5) 0.2184(4) 0.079(2) Uani 1 1 d . . . H5A H 0.1783 0.5089 0.2477 0.095 Uiso 1 1 calc R . . H5B H 0.2750 0.5165 0.1927 0.095 Uiso 1 1 calc R . . C11A C 0.2303(10) 1.2372(6) 0.0361(5) 0.123(4) Uani 1 1 d . . . H11A H 0.1705 1.2278 -0.0135 0.184 Uiso 1 1 calc R . . H11B H 0.2924 1.1883 0.0501 0.184 Uiso 1 1 calc R . . H11C H 0.2833 1.2899 0.0364 0.184 Uiso 1 1 calc R . . C10A C 0.0525(9) 1.3270(5) 0.0708(6) 0.129(4) Uani 1 1 d . . . H10A H -0.0027 1.3325 0.1063 0.193 Uiso 1 1 calc R . . H10B H -0.0077 1.3210 0.0208 0.193 Uiso 1 1 calc R . . H10C H 0.1094 1.3783 0.0731 0.193 Uiso 1 1 calc R . . C7 C 0.0167(5) 0.6563(3) 0.1978(3) 0.0496(12) Uani 1 1 d . . . H7A H -0.0512 0.6886 0.1597 0.060 Uiso 1 1 calc R . . H7B H -0.0330 0.6216 0.2266 0.060 Uiso 1 1 calc R . . C6 C 0.0999(8) 0.5960(4) 0.1598(3) 0.0691(17) Uani 1 1 d . . . H6A H 0.1394 0.6300 0.1258 0.083 Uiso 1 1 calc R . . H6B H 0.0383 0.5523 0.1301 0.083 Uiso 1 1 calc R . . C10 C 0.3068(15) 0.9331(10) 0.4313(4) 0.216(9) Uani 1 1 d . . . H10D H 0.2200 0.9597 0.4327 0.324 Uiso 1 1 calc R . . H10E H 0.3777 0.9496 0.4756 0.324 Uiso 1 1 calc R . . H10F H 0.2968 0.8704 0.4298 0.324 Uiso 1 1 calc R . . C9 C 0.3543(13) 1.0596(6) 0.3671(6) 0.193(8) Uani 1 1 d . . . H9A H 0.2643 1.0830 0.3664 0.290 Uiso 1 1 calc R . . H9B H 0.3828 1.0817 0.3245 0.290 Uiso 1 1 calc R . . H9C H 0.4206 1.0771 0.4128 0.290 Uiso 1 1 calc R . . C11 C 0.4779(8) 0.9230(13) 0.3635(8) 0.248(11) Uani 1 1 d . . . H11D H 0.4670 0.8604 0.3609 0.373 Uiso 1 1 calc R . . H11E H 0.5464 0.9385 0.4091 0.373 Uiso 1 1 calc R . . H11F H 0.5076 0.9432 0.3208 0.373 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 0.02718(11) 0.02200(11) 0.02456(11) 0.00003(5) 0.00230(7) -0.00226(5) S1A 0.0304(5) 0.0260(5) 0.0317(5) 0.0018(4) -0.0023(4) -0.0051(4) O1 0.0413(19) 0.0329(18) 0.0386(18) 0.0064(13) -0.0156(15) -0.0103(13) S1 0.0360(5) 0.0274(5) 0.0398(6) 0.0049(4) -0.0012(4) -0.0068(4) O1A 0.0416(16) 0.0276(16) 0.0389(16) 0.0046(13) -0.0073(13) -0.0134(13) N1A 0.0318(17) 0.0239(18) 0.0358(17) 0.0047(14) 0.0055(14) -0.0032(14) N2 0.055(2) 0.027(2) 0.040(2) 0.0090(16) 0.0030(17) -0.0033(17) N2A 0.0298(18) 0.037(2) 0.043(2) 0.0107(17) -0.0005(15) -0.0039(15) C1A 0.0285(19) 0.030(2) 0.0245(18) 0.0011(15) 0.0052(15) 0.0023(16) N1 0.040(2) 0.034(2) 0.0311(17) 0.0059(15) -0.0029(15) -0.0017(16) C1 0.035(2) 0.031(2) 0.031(2) 0.0050(17) 0.0064(16) -0.0012(17) C2A 0.035(2) 0.023(2) 0.0315(19) -0.0008(16) 0.0073(16) -0.0033(16) C8 0.042(3) 0.044(3) 0.042(3) 0.004(2) -0.011(2) -0.006(2) C2 0.0287(19) 0.037(3) 0.0274(19) 0.0041(17) -0.0013(15) 0.0012(17) C8A 0.052(3) 0.028(2) 0.038(2) 0.0008(18) 0.003(2) -0.014(2) C7A 0.035(2) 0.045(3) 0.036(2) 0.004(2) -0.0066(18) -0.006(2) C3A 0.036(2) 0.052(3) 0.049(3) 0.023(2) 0.001(2) 0.000(2) C3 0.062(3) 0.037(3) 0.058(3) 0.022(2) 0.008(2) 0.011(2) C4A 0.058(3) 0.050(3) 0.072(4) 0.017(3) 0.015(3) 0.016(3) C6A 0.033(2) 0.066(4) 0.070(3) -0.001(3) 0.012(2) -0.010(2) C5A 0.037(3) 0.076(5) 0.097(5) 0.012(4) 0.011(3) 0.014(3) C4 0.062(4) 0.052(4) 0.091(4) 0.023(3) 0.025(3) 0.010(3) C9A 0.127(6) 0.077(5) 0.055(3) -0.011(3) 0.008(4) -0.070(5) C5 0.102(5) 0.047(4) 0.104(5) 0.007(4) 0.057(4) 0.012(4) C11A 0.165(8) 0.111(7) 0.130(7) -0.069(6) 0.107(6) -0.106(6) C10A 0.100(6) 0.039(4) 0.216(11) 0.014(5) -0.015(6) -0.019(4) C7 0.061(3) 0.025(2) 0.058(3) 0.004(2) 0.006(2) -0.008(2) C6 0.106(5) 0.037(3) 0.072(4) -0.007(3) 0.035(3) -0.017(3) C10 0.303(17) 0.258(16) 0.041(4) 0.015(7) -0.038(7) -0.202(15) C9 0.245(13) 0.060(6) 0.157(9) -0.015(6) -0.157(9) -0.011(7) C11 0.050(5) 0.39(3) 0.243(15) -0.224(17) -0.066(7) 0.060(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1A 2.010(3) . ? Pt1 O1 2.033(3) . ? Pt1 S1A 2.2304(14) . ? Pt1 S1 2.2422(11) . ? S1A C1A 1.726(4) . ? O1 C2 1.258(5) . ? S1 C1 1.744(4) . ? O1A C2A 1.257(5) . ? N1A C2A 1.319(5) . ? N1A C1A 1.350(5) . ? N2 C1 1.332(6) . ? N2 C7 1.462(6) . ? N2 C3 1.485(6) . ? N2A C1A 1.349(5) . ? N2A C3A 1.463(6) . ? N2A C7A 1.463(6) . ? N1 C2 1.308(6) . ? N1 C1 1.345(5) . ? C2A C8A 1.541(6) . ? C8 C11 1.441(10) . ? C8 C9 1.470(10) . ? C8 C10 1.480(11) . ? C8 C2 1.528(6) . ? C8A C11A 1.465(8) . ? C8A C9A 1.507(7) . ? C8A C10A 1.530(9) . ? C7A C6A 1.515(7) . ? C3A C4A 1.522(7) . ? C3 C4 1.499(8) . ? C4A C5A 1.515(8) . ? C6A C5A 1.522(9) . ? C4 C5 1.508(9) . ? C5 C6 1.539(9) . ? C7 C6 1.523(8) . ? 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 Pt1 O1 81.95(12) . . ? O1A Pt1 S1A 94.53(8) . . ? O1 Pt1 S1A 175.89(10) . . ? O1A Pt1 S1 176.63(9) . . ? O1 Pt1 S1 94.93(9) . . ? S1A Pt1 S1 88.63(4) . . ? C1A S1A Pt1 107.95(13) . . ? C2 O1 Pt1 128.2(3) . . ? C1 S1 Pt1 106.33(15) . . ? C2A O1A Pt1 130.3(3) . . ? C2A N1A C1A 126.8(3) . . ? C1 N2 C7 125.5(4) . . ? C1 N2 C3 122.2(4) . . ? C7 N2 C3 112.1(4) . . ? C1A N2A C3A 122.5(4) . . ? C1A N2A C7A 124.5(4) . . ? C3A N2A C7A 113.0(3) . . ? N1A C1A N2A 114.1(4) . . ? N1A C1A S1A 129.8(3) . . ? N2A C1A S1A 116.1(3) . . ? C2 N1 C1 128.7(4) . . ? N2 C1 N1 115.7(4) . . ? N2 C1 S1 117.1(3) . . ? N1 C1 S1 127.0(3) . . ? O1A C2A N1A 130.3(4) . . ? O1A C2A C8A 114.1(3) . . ? N1A C2A C8A 115.6(4) . . ? C11 C8 C9 113.0(10) . . ? C11 C8 C10 107.9(11) . . ? C9 C8 C10 107.0(9) . . ? C11 C8 C2 107.9(5) . . ? C9 C8 C2 111.7(4) . . ? C10 C8 C2 109.3(5) . . ? O1 C2 N1 129.6(4) . . ? O1 C2 C8 114.7(4) . . ? N1 C2 C8 115.6(4) . . ? C11A C8A C9A 113.5(6) . . ? C11A C8A C10A 109.6(7) . . ? C9A C8A C10A 104.8(6) . . ? C11A C8A C2A 107.9(4) . . ? C9A C8A C2A 111.0(4) . . ? C10A C8A C2A 110.1(4) . . ? N2A C7A C6A 109.8(4) . . ? N2A C3A C4A 110.1(4) . . ? N2 C3 C4 110.1(4) . . ? C5A C4A C3A 111.0(5) . . ? C7A C6A C5A 111.3(4) . . ? C4A C5A C6A 110.7(5) . . ? C3 C4 C5 110.4(5) . . ? C4 C5 C6 110.2(5) . . ? N2 C7 C6 110.2(5) . . ? C7 C6 C5 111.3(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 C1A -3.83(17) . . . . ? O1 Pt1 S1A C1A 27.2(15) . . . . ? S1 Pt1 S1A C1A 177.33(14) . . . . ? O1A Pt1 O1 C2 177.5(4) . . . . ? S1A Pt1 O1 C2 146.3(13) . . . . ? S1 Pt1 O1 C2 -3.8(4) . . . . ? O1A Pt1 S1 C1 9.6(17) . . . . ? O1 Pt1 S1 C1 -12.63(19) . . . . ? S1A Pt1 S1 C1 169.42(15) . . . . ? O1 Pt1 O1A C2A -174.7(4) . . . . ? S1A Pt1 O1A C2A 3.2(4) . . . . ? S1 Pt1 O1A C2A 163.0(14) . . . . ? C2A N1A C1A N2A -177.6(4) . . . . ? C2A N1A C1A S1A 2.9(6) . . . . ? C3A N2A C1A N1A 0.2(6) . . . . ? C7A N2A C1A N1A -179.8(4) . . . . ? C3A N2A C1A S1A 179.8(3) . . . . ? C7A N2A C1A S1A -0.2(6) . . . . ? Pt1 S1A C1A N1A 2.1(4) . . . . ? Pt1 S1A C1A N2A -177.3(3) . . . . ? C7 N2 C1 N1 -178.3(4) . . . . ? C3 N2 C1 N1 -1.8(6) . . . . ? C7 N2 C1 S1 5.8(6) . . . . ? C3 N2 C1 S1 -177.8(4) . . . . ? C2 N1 C1 N2 167.7(4) . . . . ? C2 N1 C1 S1 -16.8(7) . . . . ? Pt1 S1 C1 N2 -160.0(3) . . . . ? Pt1 S1 C1 N1 24.6(4) . . . . ? Pt1 O1A C2A N1A 1.2(7) . . . . ? Pt1 O1A C2A C8A -178.5(3) . . . . ? C1A N1A C2A O1A -5.4(7) . . . . ? C1A N1A C2A C8A 174.4(4) . . . . ? Pt1 O1 C2 N1 17.9(7) . . . . ? Pt1 O1 C2 C8 -166.2(3) . . . . ? C1 N1 C2 O1 -9.0(8) . . . . ? C1 N1 C2 C8 175.1(4) . . . . ? C11 C8 C2 O1 -107.2(10) . . . . ? C9 C8 C2 O1 17.5(9) . . . . ? C10 C8 C2 O1 135.7(9) . . . . ? C11 C8 C2 N1 69.3(11) . . . . ? C9 C8 C2 N1 -166.0(8) . . . . ? C10 C8 C2 N1 -47.8(9) . . . . ? O1A C2A C8A C11A 96.6(6) . . . . ? N1A C2A C8A C11A -83.2(6) . . . . ? O1A C2A C8A C9A -28.2(6) . . . . ? N1A C2A C8A C9A 152.0(5) . . . . ? O1A C2A C8A C10A -143.8(6) . . . . ? N1A C2A C8A C10A 36.4(7) . . . . ? C1A N2A C7A C6A 120.7(5) . . . . ? C3A N2A C7A C6A -59.3(5) . . . . ? C1A N2A C3A C4A -120.8(5) . . . . ? C7A N2A C3A C4A 59.2(6) . . . . ? C1 N2 C3 C4 -116.3(5) . . . . ? C7 N2 C3 C4 60.6(6) . . . . ? N2A C3A C4A C5A -55.3(6) . . . . ? N2A C7A C6A C5A 55.6(6) . . . . ? C3A C4A C5A C6A 53.1(7) . . . . ? C7A C6A C5A C4A -53.5(7) . . . . ? N2 C3 C4 C5 -58.7(6) . . . . ? C3 C4 C5 C6 55.5(7) . . . . ? C1 N2 C7 C6 118.8(5) . . . . ? C3 N2 C7 C6 -57.9(5) . . . . ? N2 C7 C6 C5 54.1(6) . . . . ? C4 C5 C6 C7 -53.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.779 _refine_diff_density_min -1.757 _refine_diff_density_rms 0.129