# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1811 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Cheryl Sacht Department of Chemistry Rhodes University, PO Box 94 Grahamstown 6140 South Africa ; _publ_contact_author_phone 'Intl-27-46-6038260' _publ_contact_author_fax 'Intl-27-46-6225109' _publ_contact_author_email C.Sacht@ru.ac.za _publ_requested_journal 'J. Chem. Soc. Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a Regular Paper in J. Chem. Soc., Dalton Transactions ; #============================================================================ # 2. PROCESSING SUMMARY _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and characterisation of chiral and achiral platinum(II) complexes for potential use as chemotherapeutic agents. Crystal and molecular structures of cis-[Pt(L1)2] and [Pt(L1)Cl(MPSO)]; (HL1 = N,N-diethyl-N'-benzoylthiourea). ; loop_ _publ_author_name _publ_author_address 'Datt, Michael S.' ; Department of Chemistry Rhodes University, PO Box 94 Grahamstown 6140 South Africa ; 'Sacht, Cheryl' ; Department of Chemistry Rhodes University Grahamstown 6140 South Africa ; 'Otto, Stefanus' ; Department of Chemistry University of the Free State Bloemfontein 9300 South Africa ; 'Roodt, Andreas' ; Department of Chemistry University of the Free State Bloemfontein 9300 South Africa ; #============================================================================ 4. TEXT _publ_section_abstract ; See Text ; _publ_section_comment ; See Text ; _publ_section_experimental_prep ; See Text ; _publ_section_experimental_refinement ; See Text ; _publ_section_references ; See Text ; _publ_section_figure_captions ; See Text ; _publ_section_acknowledgements ; See Text ; #============================================================================== data_Compound1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; [Pt(Cl){SO(CH~3~)(C~6~H~5~)}{(C~6~H~5~)CONCSN(Et)~2~}] ; _chemical_formula_analytical ? _chemical_formula_sum 'C19 H23 Cl N2 O2 Pt S2' _chemical_formula_weight 606.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.612(2) _cell_length_b 11.776(2) _cell_length_c 13.374(3) _cell_angle_alpha 115.11(2) _cell_angle_beta 86.44(2) _cell_angle_gamma 66.25(2) _cell_volume 1078.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 1.836 _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'Flottation NaI/H~2~O' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 6.837 _exptl_absorpt_correction_type 'Empirical on faced crystal' _exptl_absorpt_correction_T_min 0.075 _exptl_absorpt_correction_T_max 0.208 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet P3' _diffrn_measurement_method 'Theta/2Theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '60min' _diffrn_standards_decay_% 2% _diffrn_reflns_number 2918 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2918 _reflns_number_observed 2915 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Standard programmes Nicolet P3' _computing_cell_refinement 'Standard programmes Nicolet P3' _computing_data_reduction 'Profit (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+8.1214P] 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 'Calculated riding on adjacent carbon atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2915 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0613 _refine_ls_wR_factor_all 0.1587 _refine_ls_wR_factor_obs 0.1535 _refine_ls_goodness_of_fit_all 1.120 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.160 _refine_ls_restrained_S_obs 1.120 _refine_ls_shift/esd_max -0.246 _refine_ls_shift/esd_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt Pt 0.23227(7) 0.25358(5) 0.09789(4) 0.0375(2) Uani 1 d . . Cl1 Cl 0.2395(6) 0.0364(4) -0.0183(3) 0.0531(9) Uani 1 d . . S1 S 0.2312(6) 0.4631(4) 0.2025(3) 0.0540(10) Uani 1 d . . S2 S 0.2209(5) 0.2291(4) 0.2514(3) 0.0414(8) Uani 1 d . . O1 O 0.2496(14) 0.2657(10) -0.0479(8) 0.045(2) Uani 1 d . . O2 O 0.2696(16) 0.3163(12) 0.3458(8) 0.059(3) Uani 1 d . . N1 N 0.2019(18) 0.4947(14) 0.0079(11) 0.054(3) Uani 1 d . . N2 N 0.1748(24) 0.6806(14) 0.1697(13) 0.074(5) Uani 1 d . . C1 C 0.2022(22) 0.5457(17) 0.1191(14) 0.055(4) Uani 1 d . . C2 C 0.2321(18) 0.3687(15) -0.0627(13) 0.043(3) Uani 1 d . . C3 C 0.1471(27) 0.7616(21) 0.1072(19) 0.073(5) Uani 1 d . . H3A H 0.0920(27) 0.8627(21) 0.1620(19) 0.095(15) Uiso 1 calc R . H3B H 0.0686(27) 0.7449(21) 0.0606(19) 0.095(15) Uiso 1 calc R . C4 C 0.3261(32) 0.7152(26) 0.0291(24) 0.096(8) Uani 1 d . . H4A H 0.3059(35) 0.7660(110) -0.0131(90) 0.095(15) Uiso 1 calc R . H4B H 0.3817(88) 0.6147(39) -0.0238(76) 0.095(15) Uiso 1 calc R . H4C H 0.4015(70) 0.7361(126) 0.0758(25) 0.095(15) Uiso 1 calc R . C5 C 0.1249(49) 0.7890(57) 0.3183(40) 0.188(23) Uani 1 d . . H5A H 0.0310(49) 0.8848(57) 0.3450(40) 0.095(15) Uiso 1 calc R . H5B H 0.0930(49) 0.7488(57) 0.3610(40) 0.095(15) Uiso 1 calc R . C6 C 0.2546(59) 0.7868(59) 0.3240(40) 0.217(25) Uani 1 d . . H6A H 0.2573(89) 0.8227(145) 0.4027(41) 0.095(15) Uiso 1 calc R . H6B H 0.2700(99) 0.8451(127) 0.2956(119) 0.095(15) Uiso 1 calc R . H6C H 0.3482(60) 0.6906(61) 0.2785(94) 0.095(15) Uiso 1 calc R . C7 C 0.3540(26) 0.0491(18) 0.2146(17) 0.069(5) Uani 1 d . . H7A H 0.3027(96) -0.0074(29) 0.1706(96) 0.095(15) Uiso 1 calc R . H7B H 0.3610(143) 0.0427(25) 0.2835(17) 0.095(15) Uiso 1 calc R . H7C H 0.4706(56) 0.0145(46) 0.1697(97) 0.095(15) Uiso 1 calc R . C11 C 0.2509(18) 0.3310(15) -0.1876(12) 0.043(3) Uani 1 d . . C12 C 0.2785(20) 0.2015(21) -0.2688(16) 0.064(5) Uani 1 d . . H12 H 0.2752(20) 0.1372(21) -0.2469(16) 0.095(15) Uiso 1 calc R . C13 C 0.3111(24) 0.1642(22) -0.3826(14) 0.068(5) Uani 1 d . . H13 H 0.3311(24) 0.0742(22) -0.4371(14) 0.095(15) Uiso 1 calc R . C14 C 0.3150(26) 0.2569(28) -0.4180(17) 0.086(7) Uani 1 d . . H14 H 0.3388(26) 0.2304(28) -0.4956(17) 0.095(15) Uiso 1 calc R . C15 C 0.2825(28) 0.3913(29) -0.3350(19) 0.091(7) Uani 1 d . . H15 H 0.2815(28) 0.4564(29) -0.3573(19) 0.095(15) Uiso 1 calc R . C16 C 0.2519(23) 0.4295(19) -0.2203(15) 0.064(5) Uani 1 d . . H16 H 0.2320(23) 0.5192(19) -0.1653(15) 0.095(15) Uiso 1 calc R . C21 C 0.0102(19) 0.2568(14) 0.3089(11) 0.042(3) Uani 1 d . . C22 C -0.0655(22) 0.3383(18) 0.4274(12) 0.055(4) Uani 1 d . . H22 H -0.0039(22) 0.3755(18) 0.4746(12) 0.095(15) Uiso 1 calc R . C23 C -0.2290(23) 0.3644(20) 0.4751(13) 0.061(4) Uani 1 d . . H23 H -0.2775(23) 0.4176(20) 0.5545(13) 0.095(15) Uiso 1 calc R . C24 C -0.3225(25) 0.3118(21) 0.4056(15) 0.067(5) Uani 1 d . . H24 H -0.4349(25) 0.3314(21) 0.4385(15) 0.095(15) Uiso 1 calc R . C25 C -0.2511(26) 0.2309(21) 0.2884(17) 0.078(6) Uani 1 d . . H25 H -0.3132(26) 0.1936(21) 0.2418(17) 0.095(15) Uiso 1 calc R . C26 C -0.0864(23) 0.2059(20) 0.2407(14) 0.065(5) Uani 1 d . . H26 H -0.0392(23) 0.1537(20) 0.1612(14) 0.095(15) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0559(4) 0.0372(3) 0.0228(3) 0.0130(2) -0.0093(2) -0.0273(2) Cl1 0.087(3) 0.040(2) 0.032(2) 0.0116(15) -0.010(2) -0.037(2) S1 0.092(3) 0.051(2) 0.035(2) 0.020(2) -0.020(2) -0.048(2) S2 0.059(2) 0.045(2) 0.028(2) 0.0191(15) -0.014(2) -0.031(2) O1 0.074(7) 0.046(5) 0.028(5) 0.024(4) -0.018(4) -0.033(5) O2 0.093(8) 0.072(7) 0.026(5) 0.021(5) -0.022(5) -0.054(7) N1 0.077(9) 0.055(8) 0.040(7) 0.026(6) -0.012(6) -0.040(7) N2 0.124(14) 0.041(7) 0.051(9) 0.008(7) -0.011(9) -0.052(9) C1 0.074(11) 0.061(10) 0.045(9) 0.033(8) -0.012(8) -0.039(9) C2 0.045(8) 0.047(8) 0.050(9) 0.036(8) -0.013(6) -0.022(7) C3 0.082(13) 0.062(11) 0.094(15) 0.048(11) -0.029(11) -0.042(10) C4 0.117(18) 0.102(17) 0.141(23) 0.095(18) -0.053(17) -0.073(15) C5 0.117(26) 0.335(64) 0.267(57) 0.234(55) -0.085(32) -0.146(36) C6 0.209(49) 0.387(79) 0.203(49) 0.216(57) -0.096(40) -0.188(54) C7 0.088(13) 0.055(10) 0.066(12) 0.036(9) -0.016(10) -0.031(10) C11 0.047(8) 0.047(8) 0.035(7) 0.022(7) -0.011(6) -0.021(7) C12 0.043(9) 0.089(13) 0.058(11) 0.040(10) -0.016(8) -0.026(9) C13 0.074(12) 0.089(13) 0.026(8) 0.025(9) -0.014(8) -0.030(10) C14 0.063(12) 0.136(21) 0.045(11) 0.049(14) -0.018(9) -0.027(13) C15 0.090(15) 0.122(19) 0.060(13) 0.066(15) -0.004(11) -0.029(14) C16 0.075(11) 0.055(9) 0.054(10) 0.038(9) -0.010(9) -0.013(8) C21 0.064(9) 0.038(7) 0.027(7) 0.015(6) -0.012(6) -0.029(7) C22 0.073(11) 0.067(10) 0.021(7) 0.016(7) -0.007(7) -0.035(9) C23 0.077(11) 0.081(12) 0.029(8) 0.019(8) -0.003(8) -0.051(10) C24 0.065(11) 0.076(12) 0.045(10) 0.025(9) 0.001(8) -0.028(10) C25 0.080(13) 0.081(13) 0.064(12) 0.013(10) -0.011(10) -0.056(12) C26 0.062(10) 0.081(12) 0.034(8) 0.012(8) -0.005(7) -0.037(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 Pt O1 2.016(9) . ? Pt S2 2.192(3) . ? Pt S1 2.257(4) . ? Pt Cl1 2.334(3) . ? S1 C1 1.736(14) . ? S2 O2 1.462(11) . ? S2 C21 1.769(15) . ? S2 C7 1.77(2) . ? O1 C2 1.26(2) . ? N1 C2 1.28(2) . ? N1 C1 1.35(2) . ? N2 C1 1.34(2) . ? N2 C3 1.48(2) . ? N2 C5 1.75(5) . ? C2 C11 1.51(2) . ? C3 C4 1.55(3) . ? C5 C6 1.11(4) . ? C11 C12 1.35(2) . ? C11 C16 1.41(2) . ? C12 C13 1.37(2) . ? C13 C14 1.37(3) . ? C14 C15 1.39(3) . ? C15 C16 1.38(3) . ? C21 C26 1.38(2) . ? C21 C22 1.39(2) . ? C22 C23 1.36(2) . ? C23 C24 1.38(3) . ? C24 C25 1.37(2) . ? C25 C26 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt S2 177.2(3) . . ? O1 Pt S1 93.3(3) . . ? S2 Pt S1 89.09(13) . . ? O1 Pt Cl1 84.1(3) . . ? S2 Pt Cl1 93.48(13) . . ? S1 Pt Cl1 177.24(13) . . ? C1 S1 Pt 107.2(6) . . ? O2 S2 C21 107.6(6) . . ? O2 S2 C7 107.4(8) . . ? C21 S2 C7 100.7(8) . . ? O2 S2 Pt 117.4(4) . . ? C21 S2 Pt 111.7(4) . . ? C7 S2 Pt 110.7(6) . . ? C2 O1 Pt 129.9(9) . . ? C2 N1 C1 126.8(13) . . ? C1 N2 C3 122.1(16) . . ? C1 N2 C5 124.3(19) . . ? C3 N2 C5 112.5(18) . . ? N2 C1 N1 113.0(13) . . ? N2 C1 S1 117.5(13) . . ? N1 C1 S1 129.5(12) . . ? O1 C2 N1 131.6(14) . . ? O1 C2 C11 111.8(13) . . ? N1 C2 C11 116.6(12) . . ? N2 C3 C4 110.3(16) . . ? C6 C5 N2 99.9(41) . . ? C12 C11 C16 119.6(15) . . ? C12 C11 C2 121.4(13) . . ? C16 C11 C2 118.9(14) . . ? C11 C12 C13 120.8(18) . . ? C12 C13 C14 121.2(20) . . ? C13 C14 C15 118.4(18) . . ? C16 C15 C14 120.9(20) . . ? C15 C16 C11 119.0(19) . . ? C26 C21 C22 118.3(14) . . ? C26 C21 S2 122.8(11) . . ? C22 C21 S2 118.8(11) . . ? C23 C22 C21 120.6(15) . . ? C22 C23 C24 120.0(15) . . ? C25 C24 C23 120.6(17) . . ? C24 C25 C26 119.0(18) . . ? C25 C26 C21 121.3(16) . . ? _refine_diff_density_max 3.141 _refine_diff_density_min -3.613 _refine_diff_density_rms 0.280 #============================================================================== data_Compound2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Pt{(C~6~H~5~)CONCSN(Et)~2~}~2~] _chemical_formula_analytical ? _chemical_formula_sum 'C24 H30 N4 O2 Pt S2' _chemical_formula_weight 665.73 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 'P2~1~/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.926(2) _cell_length_b 12.265(3) _cell_length_c 21.168(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.00(2) _cell_angle_gamma 90.00 _cell_volume 2576.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 1.695 _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'Flotation NaI/H~2~O' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 5.636 _exptl_absorpt_correction_type 'Empirical on faced crystal' _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.340 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet P3' _diffrn_measurement_method 'Theta/2Theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '60min' _diffrn_standards_decay_% 0.2% _diffrn_reflns_number 3454 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3454 _reflns_number_observed 3453 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Standard programes Nicolet P3' _computing_cell_refinement 'Standard programes Nicolet P3' _computing_data_reduction 'Profit (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+6.9658P] 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 'Calculated riding on adjacent Carbon atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3453 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_obs 0.0355 _refine_ls_wR_factor_all 0.0925 _refine_ls_wR_factor_obs 0.0918 _refine_ls_goodness_of_fit_all 1.130 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 1.139 _refine_ls_restrained_S_obs 1.130 _refine_ls_shift/esd_max 0.019 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.59332(3) 0.48240(2) 0.391053(12) 0.03938(12) Uani 1 d . . S1A S 0.7426(2) 0.4795(2) 0.47108(10) 0.0532(5) Uani 1 d . . S1B S 0.7063(2) 0.6234(2) 0.35137(10) 0.0608(6) Uani 1 d . . O1A O 0.4844(6) 0.3558(4) 0.4233(2) 0.0539(14) Uani 1 d . . O1B O 0.4534(6) 0.4799(4) 0.3204(3) 0.058(2) Uani 1 d . . N1A N 0.6003(6) 0.3014(5) 0.5157(3) 0.0396(14) Uani 1 d . . N2A N 0.8019(6) 0.3413(5) 0.5620(3) 0.0435(15) Uani 1 d . . N1B N 0.5128(6) 0.6270(5) 0.2549(3) 0.0403(14) Uani 1 d . . N2B N 0.7026(6) 0.7254(5) 0.2431(3) 0.0438(14) Uani 1 d . . C2A C 0.4999(8) 0.3028(5) 0.4745(3) 0.039(2) Uani 1 d . . C1A C 0.7093(8) 0.3661(6) 0.5169(3) 0.040(2) Uani 1 d . . C3A C 0.7771(9) 0.2543(6) 0.6080(3) 0.052(2) Uani 1 d . . H3AA H 0.6813(9) 0.2506(6) 0.6162(3) 0.067(5) Uiso 1 calc R . H3AB H 0.8233(9) 0.2716(6) 0.6475(3) 0.067(5) Uiso 1 calc R . C4A C 0.8241(10) 0.1461(7) 0.5850(4) 0.069(3) Uani 1 d . . H4AA H 0.7721(35) 0.1253(20) 0.5483(15) 0.067(5) Uiso 1 calc R . H4AB H 0.8130(49) 0.0926(11) 0.6176(10) 0.067(5) Uiso 1 calc R . H4AC H 0.9175(16) 0.1508(13) 0.5744(23) 0.067(5) Uiso 1 calc R . C5A C 0.9332(8) 0.3963(6) 0.5681(3) 0.048(2) Uani 1 d . . H5AA H 0.9586(8) 0.4240(6) 0.5270(3) 0.067(5) Uiso 1 calc R . H5AB H 1.0007(8) 0.3436(6) 0.5815(3) 0.067(5) Uiso 1 calc R . C6A C 0.9321(10) 0.4880(8) 0.6140(5) 0.073(3) Uani 1 d . . H6AA H 1.0166(22) 0.5260(27) 0.6128(18) 0.067(5) Uiso 1 calc R . H6AB H 0.9188(54) 0.4600(9) 0.6558(5) 0.067(5) Uiso 1 calc R . H6AC H 0.8603(34) 0.5374(23) 0.6031(15) 0.067(5) Uiso 1 calc R . C11A C 0.3900(7) 0.2242(6) 0.4889(3) 0.039(2) Uani 1 d . . C12A C 0.4118(9) 0.1352(7) 0.5266(4) 0.055(2) Uani 1 d . . H12A H 0.4971(9) 0.1230(7) 0.5441(4) 0.067(5) Uiso 1 calc R . C13A C 0.3093(9) 0.0634(8) 0.5391(4) 0.065(2) Uani 1 d . . H13A H 0.3261(9) 0.0022(8) 0.5640(4) 0.067(5) Uiso 1 calc R . C14A C 0.1816(10) 0.0821(8) 0.5149(5) 0.066(2) Uani 1 d . . H14A H 0.1114(10) 0.0347(8) 0.5239(5) 0.067(5) Uiso 1 calc R . C15A C 0.1596(10) 0.1700(8) 0.4780(5) 0.072(3) Uani 1 d . . H15A H 0.0734(10) 0.1831(8) 0.4617(5) 0.067(5) Uiso 1 calc R . C16A C 0.2620(9) 0.2407(7) 0.4639(4) 0.058(2) Uani 1 d . . H16A H 0.2452(9) 0.2998(7) 0.4374(4) 0.067(5) Uiso 1 calc R . C2B C 0.4355(8) 0.5485(6) 0.2767(3) 0.039(2) Uani 1 d . . C1B C 0.6340(8) 0.6564(5) 0.2793(3) 0.040(2) Uani 1 d . . C3B C 0.6500(9) 0.7642(6) 0.1813(3) 0.051(2) Uani 1 d . . H3BA H 0.6831(9) 0.8373(6) 0.1736(3) 0.067(5) Uiso 1 calc R . H3BB H 0.5524(9) 0.7673(6) 0.1823(3) 0.067(5) Uiso 1 calc R . C4B C 0.6918(10) 0.6909(8) 0.1285(4) 0.070(3) Uani 1 d . . H4BA H 0.6583(45) 0.7195(24) 0.0890(5) 0.067(5) Uiso 1 calc R . H4BB H 0.6556(45) 0.6192(14) 0.1349(14) 0.067(5) Uiso 1 calc R . H4BC H 0.7884(10) 0.6870(34) 0.1276(16) 0.067(5) Uiso 1 calc R . C5B C 0.8378(9) 0.7669(7) 0.2603(4) 0.059(2) Uani 1 d . . H5BA H 0.8873(9) 0.7814(7) 0.2220(4) 0.067(5) Uiso 1 calc R . H5BB H 0.8865(9) 0.7116(7) 0.2842(4) 0.067(5) Uiso 1 calc R . C6B C 0.8306(11) 0.8696(9) 0.2989(5) 0.083(3) Uani 1 d . . H6BA H 0.9202(11) 0.8937(24) 0.3096(21) 0.067(5) Uiso 1 calc R . H6BB H 0.7821(46) 0.8555(14) 0.3369(13) 0.067(5) Uiso 1 calc R . H6BC H 0.7849(46) 0.9252(15) 0.2748(10) 0.067(5) Uiso 1 calc R . C11B C 0.3036(8) 0.5336(6) 0.2422(3) 0.043(2) Uani 1 d . . C12B C 0.2483(9) 0.6150(7) 0.2045(4) 0.058(2) Uani 1 d . . H12B H 0.2965(9) 0.6790(7) 0.1982(4) 0.067(5) Uiso 1 calc R . C13B C 0.1220(10) 0.6028(9) 0.1756(4) 0.073(3) Uani 1 d . . H13B H 0.0839(10) 0.6593(9) 0.1521(4) 0.067(5) Uiso 1 calc R . C14B C 0.0551(10) 0.5062(10) 0.1826(5) 0.076(3) Uani 1 d . . H14B H -0.0287(10) 0.4968(10) 0.1630(5) 0.067(5) Uiso 1 calc R . C15B C 0.1097(10) 0.4223(9) 0.2181(4) 0.065(3) Uani 1 d . . H15B H 0.0638(10) 0.3565(9) 0.2216(4) 0.067(5) Uiso 1 calc R . C16B C 0.2316(8) 0.4362(7) 0.2484(4) 0.052(2) Uani 1 d . . H16B H 0.2669(8) 0.3803(7) 0.2733(4) 0.067(5) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0427(2) 0.0384(2) 0.0369(2) 0.00557(11) -0.00338(11) -0.00360(13) S1A 0.0607(14) 0.0522(11) 0.0463(11) 0.0124(9) -0.0144(9) -0.0195(10) S1B 0.063(2) 0.0646(13) 0.0544(12) 0.0216(10) -0.0206(10) -0.0254(11) O1A 0.054(4) 0.056(3) 0.052(3) 0.020(3) -0.016(3) -0.015(3) O1B 0.063(4) 0.060(3) 0.051(3) 0.020(3) -0.012(3) -0.018(3) N1A 0.032(4) 0.046(3) 0.041(3) 0.006(3) -0.001(3) -0.008(3) N2A 0.037(4) 0.054(4) 0.039(3) 0.006(3) -0.005(3) -0.009(3) N1B 0.039(4) 0.037(3) 0.044(3) 0.007(3) -0.002(3) -0.002(3) N2B 0.037(4) 0.043(3) 0.051(3) 0.004(3) 0.002(3) -0.006(3) C2A 0.041(5) 0.033(3) 0.044(4) 0.001(3) 0.006(3) -0.002(3) C1A 0.042(5) 0.046(4) 0.032(3) -0.002(3) 0.005(3) -0.004(3) C3A 0.056(6) 0.058(5) 0.040(4) 0.009(3) -0.008(4) -0.006(4) C4A 0.070(7) 0.065(6) 0.071(6) 0.022(5) 0.008(5) 0.004(5) C5A 0.044(5) 0.055(4) 0.045(4) 0.000(3) -0.006(3) -0.007(4) C6A 0.056(7) 0.090(7) 0.074(7) -0.016(5) -0.009(5) -0.002(5) C11A 0.038(4) 0.042(4) 0.035(3) 0.000(3) -0.004(3) -0.005(3) C12A 0.046(5) 0.057(5) 0.062(5) 0.017(4) -0.002(4) -0.014(4) C13A 0.059(6) 0.064(5) 0.070(6) 0.021(5) -0.018(5) -0.019(5) C14A 0.054(6) 0.062(6) 0.081(6) -0.004(5) 0.007(5) -0.018(4) C15A 0.039(6) 0.084(7) 0.094(7) 0.001(6) -0.015(5) -0.010(5) C16A 0.048(6) 0.053(5) 0.074(6) 0.008(4) -0.013(4) -0.002(4) C2B 0.047(5) 0.038(4) 0.032(3) 0.002(3) -0.001(3) 0.004(3) C1B 0.049(5) 0.030(3) 0.042(4) 0.002(3) 0.005(3) -0.002(3) C3B 0.058(6) 0.049(4) 0.044(4) 0.018(3) 0.001(4) -0.005(4) C4B 0.077(7) 0.079(6) 0.053(5) -0.003(5) 0.001(5) 0.000(5) C5B 0.053(6) 0.065(5) 0.061(5) 0.013(4) -0.001(4) -0.019(4) C6B 0.078(8) 0.084(7) 0.086(7) 0.002(6) -0.007(6) -0.034(6) C11B 0.038(5) 0.055(5) 0.037(4) -0.002(3) 0.000(3) 0.002(3) C12B 0.048(6) 0.057(5) 0.070(5) 0.012(4) -0.010(4) -0.001(4) C13B 0.059(7) 0.097(8) 0.061(5) 0.014(5) -0.022(5) 0.014(6) C14B 0.036(6) 0.131(10) 0.060(6) 0.003(6) -0.007(4) -0.006(6) C15B 0.055(6) 0.084(7) 0.056(5) -0.008(5) 0.005(4) -0.025(5) C16B 0.048(5) 0.057(5) 0.050(4) 0.002(4) 0.004(4) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1A 2.018(5) . ? Pt1 O1B 2.023(6) . ? Pt1 S1A 2.231(2) . ? Pt1 S1B 2.233(2) . ? S1A C1A 1.731(7) . ? S1B C1B 1.723(7) . ? O1A C2A 1.271(8) . ? O1B C2B 1.262(8) . ? N1A C2A 1.313(9) . ? N1A C1A 1.341(9) . ? N2A C1A 1.350(9) . ? N2A C3A 1.467(9) . ? N2A C5A 1.471(9) . ? N1B C2B 1.319(9) . ? N1B C1B 1.350(9) . ? N2B C1B 1.336(9) . ? N2B C5B 1.475(10) . ? N2B C3B 1.479(9) . ? C2A C11A 1.491(10) . ? C3A C4A 1.491(12) . ? C5A C6A 1.487(11) . ? C11A C12A 1.369(10) . ? C11A C16A 1.382(11) . ? C12A C13A 1.374(11) . ? C13A C14A 1.378(13) . ? C14A C15A 1.347(13) . ? C15A C16A 1.372(12) . ? C2B C11B 1.498(11) . ? C3B C4B 1.499(11) . ? C5B C6B 1.503(13) . ? C11B C12B 1.386(11) . ? C11B C16B 1.400(11) . ? C12B C13B 1.393(12) . ? C13B C14B 1.368(14) . ? C14B C15B 1.380(14) . ? C15B C16B 1.370(12) . ? 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 O1B 82.7(2) . . ? O1A Pt1 S1A 94.77(15) . . ? O1B Pt1 S1A 177.5(2) . . ? O1A Pt1 S1B 177.12(15) . . ? O1B Pt1 S1B 94.4(2) . . ? S1A Pt1 S1B 88.10(7) . . ? C1A S1A Pt1 107.9(3) . . ? C1B S1B Pt1 108.1(3) . . ? C2A O1A Pt1 128.7(5) . . ? C2B O1B Pt1 128.2(5) . . ? C2A N1A C1A 127.4(6) . . ? C1A N2A C3A 120.9(6) . . ? C1A N2A C5A 123.3(6) . . ? C3A N2A C5A 115.8(6) . . ? C2B N1B C1B 125.5(6) . . ? C1B N2B C5B 123.3(7) . . ? C1B N2B C3B 122.4(7) . . ? C5B N2B C3B 114.3(6) . . ? O1A C2A N1A 130.7(7) . . ? O1A C2A C11A 115.3(6) . . ? N1A C2A C11A 113.9(6) . . ? N1A C1A N2A 114.8(6) . . ? N1A C1A S1A 128.8(6) . . ? N2A C1A S1A 116.3(5) . . ? N2A C3A C4A 111.9(6) . . ? N2A C5A C6A 112.8(7) . . ? C12A C11A C16A 118.4(7) . . ? C12A C11A C2A 121.7(7) . . ? C16A C11A C2A 119.9(7) . . ? C11A C12A C13A 120.9(8) . . ? C12A C13A C14A 120.1(9) . . ? C15A C14A C13A 119.2(9) . . ? C14A C15A C16A 121.2(9) . . ? C15A C16A C11A 120.2(8) . . ? O1B C2B N1B 131.9(7) . . ? O1B C2B C11B 112.7(7) . . ? N1B C2B C11B 115.3(6) . . ? N2B C1B N1B 114.2(6) . . ? N2B C1B S1B 116.6(6) . . ? N1B C1B S1B 129.2(5) . . ? N2B C3B C4B 111.7(7) . . ? N2B C5B C6B 111.8(8) . . ? C12B C11B C16B 118.0(7) . . ? C12B C11B C2B 121.8(7) . . ? C16B C11B C2B 120.2(7) . . ? C11B C12B C13B 121.4(9) . . ? C14B C13B C12B 118.7(9) . . ? C13B C14B C15B 121.2(9) . . ? C16B C15B C14B 119.8(9) . . ? C15B C16B C11B 120.7(8) . . ? _refine_diff_density_max 0.807 _refine_diff_density_min -1.624 _refine_diff_density_rms 0.163