# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1757 data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Sat Nov 27 11:29:14 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Bruker Axs Smart 1000 CCD' _computing_cell_refinement 'Bruker Axs Smart 1000 CCD' _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.9213(5) _cell_length_b 15.3887(8) _cell_length_c 18.1315(9) _cell_angle_alpha 90 _cell_angle_beta 100.632(1) _cell_angle_gamma 90 _cell_volume 2720.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1064.25 _chemical_formula_analytical ? _chemical_formula_sum 'C56 H74 N2 O2 P2 Pt ' _chemical_formula_moiety 'C56 H74 N2 O2 P2 Pt ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1096.00 _exptl_absorpt_coefficient_mu 2.667 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'Bruker Axs Smart 1000 CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 16000 _reflns_number_total 6301 _reflns_number_observed 3811 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 2.43 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0 148 0.000 0.000 'International Tables' C 0 112 0.003 0.002 'International Tables' N 0 4 0.006 0.003 'International Tables' O 0 4 0.011 0.006 'International Tables' P 0 4 0.102 0.094 'International Tables' Pt 0 2 -1.703 8.390 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Pt(1) 1.0000 0.0000 1.0000 0.05393(8) Uij ? ? P(1) 1.0490(2) 0.04244(9) 0.88630(7) 0.0592(4) Uij ? ? O(1) 0.9325(4) 0.5332(3) 0.8392(2) 0.074(1) Uij ? ? N(1) 0.9666(4) 0.3455(3) 1.0007(2) 0.052(1) Uij ? ? C(1) 0.8969(6) 0.0430(5) 0.8144(3) 0.083(2) Uij ? ? C(2) 0.7778(8) 0.1005(6) 0.8309(4) 0.140(3) Uij ? ? C(3) 0.6464(7) 0.0872(7) 0.7683(6) 0.192(5) Uij ? ? C(4) 0.624(2) 0.165(1) 0.7158(10) 0.218(9) Uij ? ? C(4a) 0.530(1) 0.140(2) 0.785(1) 0.224(9) Uij ? ? C(5) 1.1262(7) 0.1502(3) 0.8845(3) 0.072(2) Uij ? ? C(6) 1.1594(8) 0.1801(4) 0.8093(4) 0.098(2) Uij ? ? C(7) 1.2130(9) 0.2673(4) 0.8082(4) 0.105(3) Uij ? ? C(8) 1.251(1) 0.2941(6) 0.7363(4) 0.144(4) Uij ? ? C(9) 1.1645(7) -0.0307(4) 0.8492(3) 0.077(2) Uij ? ? C(10) 1.3006(8) -0.0437(6) 0.9001(4) 0.102(2) Uij ? ? C(11) 1.389(1) -0.1155(6) 0.8746(5) 0.146(4) Uij ? ? C(12) 1.522(1) -0.1333(9) 0.9266(7) 0.204(6) Uij ? ? C(13) 0.8427(6) 0.3577(3) 0.9539(3) 0.057(1) Uij ? ? C(14) 0.7247(7) 0.3075(4) 0.9611(3) 0.075(2) Uij ? ? C(15) 0.6010(7) 0.3216(5) 0.9153(4) 0.096(2) Uij ? ? C(16) 0.5880(7) 0.3848(6) 0.8601(4) 0.097(3) Uij ? ? C(17) 0.6978(7) 0.4345(4) 0.8507(3) 0.077(2) Uij ? ? C(18) 0.8268(6) 0.4206(3) 0.8968(3) 0.059(1) Uij ? ? C(19) 0.9441(6) 0.4726(3) 0.8849(3) 0.055(1) Uij ? ? C(20) 1.0755(5) 0.4465(3) 0.9289(3) 0.052(1) Uij ? ? C(21) 1.1959(6) 0.4849(3) 0.9152(3) 0.063(2) Uij ? ? C(22) 1.3206(7) 0.4615(5) 0.9537(4) 0.083(2) Uij ? ? C(23) 1.3273(6) 0.3967(4) 1.0079(4) 0.080(2) Uij ? ? C(24) 1.2142(6) 0.3575(4) 1.0237(3) 0.065(2) Uij ? ? C(25) 1.0841(5) 0.3828(3) 0.9847(3) 0.050(1) Uij ? ? C(26) 0.9752(6) 0.2900(3) 1.0677(3) 0.063(1) Uij ? ? C(27) 0.9916(6) 0.1969(3) 1.0515(3) 0.060(1) Uij ? ? C(28) 0.9985(6) 0.1236(3) 1.0337(3) 0.058(1) Uij ? ? H(1) 1.3187 0.2560 0.7244 0.1727 Uij ? ? H(2) 1.1718 0.2919 0.6976 0.1727 Uij ? ? H(3) 1.2854 0.3518 0.7407 0.1727 Uij ? ? H(4) 1.5047 -0.1493 0.9745 0.2452 Uij ? ? H(5) 1.5688 -0.1793 0.9069 0.2452 Uij ? ? H(6) 1.5777 -0.0825 0.9312 0.2452 Uij ? ? H(7) 0.7572 0.0849 0.8783 0.1684 Uij ? ? H(8) 0.8047 0.1598 0.8318 0.1684 Uij ? ? H(9) 1.0644 0.1912 0.8990 0.0859 Uij ? ? H(10) 1.2093 0.1503 0.9202 0.0859 Uij ? ? H(11) 1.2255 0.1413 0.7961 0.1171 Uij ? ? H(12) 1.0775 0.1769 0.7728 0.1171 Uij ? ? H(13) 1.1453 0.3065 0.8191 0.1263 Uij ? ? H(14) 1.2927 0.2714 0.8462 0.1263 Uij ? ? H(15) 1.1209 -0.0856 0.8405 0.0918 Uij ? ? H(16) 1.1806 -0.0075 0.8030 0.0918 Uij ? ? H(17) 1.3502 0.0093 0.9027 0.1226 Uij ? ? H(18) 1.2843 -0.0583 0.9486 0.1226 Uij ? ? H(19) 1.3371 -0.1677 0.8692 0.1755 Uij ? ? H(20) 1.4092 -0.0991 0.8273 0.1755 Uij ? ? H(21) 1.0516 0.3081 1.1040 0.0754 Uij ? ? H(22) 0.8935 0.2971 1.0874 0.0754 Uij ? ? H(23) 0.7324 0.2635 0.9984 0.0896 Uij ? ? H(24) 0.5235 0.2879 0.9214 0.1153 Uij ? ? H(25) 0.5017 0.3937 0.8283 0.1160 Uij ? ? H(26) 0.6872 0.4784 0.8133 0.0929 Uij ? ? H(27) 1.1902 0.5287 0.8779 0.0755 Uij ? ? H(28) 1.4016 0.4885 0.9440 0.0991 Uij ? ? H(29) 1.4147 0.3796 1.0348 0.0963 Uij ? ? H(30) 1.2224 0.3132 1.0608 0.0777 Uij ? ? H(31) 0.9219 0.0632 0.7692 0.0999 Uij ? ? H(32) 0.8644 -0.0151 0.8076 0.0999 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0808(2) 0.0335(1) 0.0489(1) -0.0018(2) 0.0155(1) 0.0002(2) P(1) 0.088(1) 0.0420(7) 0.0485(7) -0.0042(7) 0.0160(7) 0.0007(6) O(1) 0.107(3) 0.059(2) 0.055(2) 0.005(2) 0.013(2) 0.009(2) N(1) 0.065(3) 0.039(2) 0.055(2) -0.002(2) 0.017(2) -0.001(2) C(1) 0.096(4) 0.081(4) 0.067(4) -0.007(4) 0.000(2) 0.005(3) C(5) 0.103(5) 0.047(3) 0.068(3) -0.016(3) 0.028(3) -0.006(3) C(6) 0.161(7) 0.070(4) 0.073(4) -0.030(4) 0.049(4) -0.001(3) C(7) 0.156(7) 0.073(4) 0.089(4) -0.039(5) 0.030(5) -0.003(4) C(8) 0.181(9) 0.156(8) 0.095(5) -0.078(7) 0.025(5) 0.028(5) C(9) 0.112(4) 0.056(3) 0.071(4) 0.013(3) 0.042(3) 0.003(3) C(10) 0.111(5) 0.109(5) 0.092(5) 0.006(4) 0.032(3) 0.021(4) C(11) 0.171(8) 0.141(8) 0.142(7) 0.078(7) 0.070(6) 0.013(6) C(12) 0.159(10) 0.24(1) 0.22(1) 0.10(1) 0.050(7) 0.04(1) C(13) 0.067(3) 0.046(3) 0.060(3) -0.001(2) 0.017(2) -0.013(2) C(14) 0.074(3) 0.066(4) 0.090(4) -0.016(3) 0.031(3) -0.012(3) C(15) 0.069(4) 0.108(6) 0.112(5) -0.018(4) 0.020(3) -0.027(3) C(16) 0.060(4) 0.126(6) 0.098(5) 0.003(3) -0.002(4) -0.022(4) C(17) 0.078(3) 0.087(5) 0.063(3) 0.013(3) 0.001(3) -0.003(3) C(18) 0.070(3) 0.052(3) 0.057(3) 0.001(2) 0.015(2) -0.011(2) C(19) 0.075(3) 0.047(3) 0.044(2) 0.000(2) 0.013(2) -0.009(2) C(20) 0.071(2) 0.038(2) 0.050(2) -0.001(2) 0.018(2) -0.009(2) C(21) 0.081(3) 0.044(4) 0.070(3) -0.012(2) 0.032(2) -0.007(2) C(22) 0.070(3) 0.088(4) 0.095(4) -0.018(3) 0.028(3) -0.018(3) C(23) 0.058(3) 0.087(5) 0.092(4) 0.000(3) 0.005(3) -0.015(3) C(24) 0.066(3) 0.057(3) 0.069(3) 0.006(3) 0.004(3) -0.004(3) C(25) 0.061(2) 0.037(2) 0.056(3) 0.002(2) 0.017(2) -0.007(2) C(26) 0.093(4) 0.040(2) 0.059(3) -0.004(3) 0.025(3) 0.004(2) C(27) 0.085(4) 0.042(2) 0.055(3) -0.003(3) 0.019(3) 0.000(2) C(28) 0.088(4) 0.037(2) 0.052(3) -0.001(3) 0.019(3) 0.004(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3811 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0337 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0404 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_shift/esd_max 0.0130 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.32 _refine_diff_density_max 0.62 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(1) 2.298(1) ? ? yes Pt(1) P(1) 2.298(1) ? ? yes Pt(1) C(28) 2.000(5) ? ? yes Pt(1) C(28) 2.000(5) ? ? yes P(1) C(1) 1.803(6) ? ? yes P(1) C(5) 1.830(6) ? ? yes P(1) C(9) 1.821(6) ? ? yes O(1) C(19) 1.239(6) ? ? yes N(1) C(13) 1.371(7) ? ? yes N(1) C(25) 1.377(7) ? ? yes N(1) C(26) 1.475(6) ? ? yes C(1) C(2) 1.549(6) ? ? yes C(2) C(3) 1.577(7) ? ? yes C(3) C(4) 1.521(8) ? ? yes C(3) C(4a) 1.494(8) ? ? yes C(4) C(4a) 1.75(3) ? ? yes C(5) C(6) 1.532(8) ? ? yes C(6) C(7) 1.445(9) ? ? yes C(7) C(8) 1.478(9) ? ? yes C(9) C(10) 1.50(1) ? ? yes C(10) C(11) 1.53(1) ? ? yes C(11) C(12) 1.50(1) ? ? yes C(13) C(14) 1.428(8) ? ? yes C(13) C(18) 1.404(7) ? ? yes C(14) C(15) 1.366(10) ? ? yes C(15) C(16) 1.38(1) ? ? yes C(16) C(17) 1.367(9) ? ? yes C(17) C(18) 1.410(8) ? ? yes C(18) C(19) 1.460(8) ? ? yes C(19) C(20) 1.454(8) ? ? yes C(20) C(21) 1.395(7) ? ? yes C(20) C(25) 1.401(7) ? ? yes C(21) C(22) 1.352(9) ? ? yes C(22) C(23) 1.393(9) ? ? yes C(23) C(24) 1.351(9) ? ? yes C(24) C(25) 1.407(8) ? ? yes C(26) C(27) 1.477(7) ? ? yes C(27) C(28) 1.178(7) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Pt(1) P(1) 180.0 ? ? ? yes P(1) Pt(1) C(28) 91.1(2) ? ? ? yes P(1) Pt(1) C(28) 88.9(2) ? ? ? yes P(1) Pt(1) C(28) 88.9(2) ? ? ? yes P(1) Pt(1) C(28) 91.1(2) ? ? ? yes C(28) Pt(1) C(28) 180.0 ? ? ? yes Pt(1) P(1) C(1) 111.3(2) ? ? ? yes Pt(1) P(1) C(5) 115.6(2) ? ? ? yes Pt(1) P(1) C(9) 114.0(2) ? ? ? yes C(1) P(1) C(5) 106.3(3) ? ? ? yes C(1) P(1) C(9) 103.6(3) ? ? ? yes C(5) P(1) C(9) 105.0(3) ? ? ? yes C(13) N(1) C(25) 120.7(5) ? ? ? yes C(13) N(1) C(26) 119.8(4) ? ? ? yes C(25) N(1) C(26) 119.5(5) ? ? ? yes P(1) C(1) C(2) 115.4(5) ? ? ? yes C(1) C(2) C(3) 110.2(5) ? ? ? yes C(2) C(3) C(4) 110.6(5) ? ? ? yes C(2) C(3) C(4a) 110.4(6) ? ? ? yes C(4) C(3) C(4a) 70(1) ? ? ? yes C(3) C(4) C(4a) 53.8(8) ? ? ? yes C(3) C(4a) C(4) 55.3(8) ? ? ? yes P(1) C(5) C(6) 116.6(4) ? ? ? yes C(5) C(6) C(7) 115.6(6) ? ? ? yes C(6) C(7) C(8) 115.1(7) ? ? ? yes P(1) C(9) C(10) 114.3(5) ? ? ? yes C(9) C(10) C(11) 114.3(8) ? ? ? yes C(10) C(11) C(12) 115.4(10) ? ? ? yes N(1) C(13) C(14) 121.7(5) ? ? ? yes N(1) C(13) C(18) 121.1(5) ? ? ? yes C(14) C(13) C(18) 117.2(6) ? ? ? yes C(13) C(14) C(15) 121.2(7) ? ? ? yes C(14) C(15) C(16) 120.2(7) ? ? ? yes C(15) C(16) C(17) 120.9(7) ? ? ? yes C(16) C(17) C(18) 119.9(6) ? ? ? yes C(13) C(18) C(17) 120.5(6) ? ? ? yes C(13) C(18) C(19) 120.2(5) ? ? ? yes C(17) C(18) C(19) 119.3(6) ? ? ? yes O(1) C(19) C(18) 122.2(5) ? ? ? yes O(1) C(19) C(20) 122.5(5) ? ? ? yes C(18) C(19) C(20) 115.2(5) ? ? ? yes C(19) C(20) C(21) 119.8(5) ? ? ? yes C(19) C(20) C(25) 121.2(5) ? ? ? yes C(21) C(20) C(25) 119.0(5) ? ? ? yes C(20) C(21) C(22) 121.8(6) ? ? ? yes C(21) C(22) C(23) 118.4(6) ? ? ? yes C(22) C(23) C(24) 122.4(6) ? ? ? yes C(23) C(24) C(25) 119.3(6) ? ? ? yes N(1) C(25) C(20) 120.2(5) ? ? ? yes N(1) C(25) C(24) 120.8(5) ? ? ? yes C(20) C(25) C(24) 119.0(5) ? ? ? yes N(1) C(26) C(27) 112.9(4) ? ? ? yes C(26) C(27) C(28) 175.2(6) ? ? ? yes Pt(1) C(28) C(27) 176.9(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jun 3 16:37:30 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MARRESEARCH Image Plate' _computing_cell_refinement 'MARRESEARCH Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.959(1) _cell_length_b 12.718(1) _cell_length_c 13.040(2) _cell_angle_alpha 102.72(1) _cell_angle_beta 102.27(1) _cell_angle_gamma 101.84(1) _cell_volume 1518.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.210 _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_meas ? _chemical_formula_weight 1174.44 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H84 N4 O4 P2 Pt S2 ' _chemical_formula_moiety 'C54 H84 N4 O4 P2 Pt S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 608.00 _exptl_absorpt_coefficient_mu 2.465 _exptl_absorpt_correction_type 'Interimage scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'MARRESEARCH Image Plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 9335 _reflns_number_total 4919 _reflns_number_observed 4011 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.54 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt 0 1 -1.703 8.390 'International Tables' N 0 8 0.006 0.003 'International Tables' O 0 8 0.011 0.006 'International Tables' C 0 108 0.003 0.002 'International Tables' H 0 168 0.000 0.000 'International Tables' P 0 4 0.102 0.094 'International Tables' S 0 4 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Pt(1) 0.0000 0.5000 0.5000 0.0571(2) Uij ? ? S(1) 0.2272(2) 0.4697(2) 0.0284(2) 0.0620(7) Uij ? ? P(1) 0.1588(2) 0.4416(2) 0.6158(2) 0.0625(7) Uij ? ? O(1) 0.1388(7) 0.5126(5) -0.0457(5) 0.075(2) Uij ? ? O(2) 0.3746(7) 0.5278(6) 0.0740(6) 0.080(2) Uij ? ? N(1) 0.1542(7) 0.4676(6) 0.1268(6) 0.058(2) Uij ? ? N(2) -0.0187(9) -0.0633(8) -0.2158(8) 0.091(3) Uij ? ? C(1) 0.0918(8) 0.4666(7) 0.3783(7) 0.058(2) Uij ? ? C(2) 0.1462(8) 0.4465(7) 0.3046(7) 0.058(2) Uij ? ? C(3) 0.2179(9) 0.4264(8) 0.2190(7) 0.065(2) Uij ? ? C(4) 0.2201(8) 0.3300(7) -0.0390(7) 0.054(2) Uij ? ? C(5) 0.3459(10) 0.3092(8) -0.0498(8) 0.070(2) Uij ? ? C(6) 0.349(1) 0.2043(9) -0.1050(9) 0.087(3) Uij ? ? C(7) 0.226(1) 0.1180(9) -0.1454(9) 0.081(3) Uij ? ? C(8) 0.0963(8) 0.1352(7) -0.1325(7) 0.060(2) Uij ? ? C(9) 0.0887(8) 0.2448(7) -0.0835(7) 0.056(2) Uij ? ? C(10) -0.0457(9) 0.2641(8) -0.0828(7) 0.065(2) Uij ? ? C(11) -0.167(1) 0.1759(9) -0.1294(9) 0.081(3) Uij ? ? C(12) -0.156(1) 0.0684(10) -0.1718(10) 0.088(3) Uij ? ? C(13) -0.0320(10) 0.0459(8) -0.1724(8) 0.073(2) Uij ? ? C(14) -0.146(2) -0.141(1) -0.293(1) 0.121(4) Uij ? ? C(15) 0.042(1) -0.114(1) -0.133(1) 0.111(4) Uij ? ? C(16) 0.257(1) 0.5510(9) 0.7404(9) 0.082(3) Uij ? ? C(17) 0.330(2) 0.659(1) 0.722(1) 0.119(4) Uij ? ? C(18) 0.394(2) 0.755(2) 0.829(2) 0.187(8) Uij ? ? C(19) 0.456(3) 0.862(3) 0.803(3) 0.28(1) Uij ? ? C(20) 0.2966(9) 0.3920(8) 0.5607(8) 0.070(2) Uij ? ? C(21) 0.387(1) 0.3380(10) 0.6289(10) 0.089(3) Uij ? ? C(22) 0.498(2) 0.300(1) 0.577(1) 0.118(4) Uij ? ? C(23) 0.575(2) 0.238(2) 0.643(2) 0.186(8) Uij ? ? C(24) 0.069(1) 0.3276(9) 0.6599(9) 0.083(3) Uij ? ? C(25) -0.025(2) 0.229(1) 0.558(1) 0.132(5) Uij ? ? C(26) -0.100(3) 0.131(2) 0.573(2) 0.198(9) Uij ? ? C(27) -0.194(2) 0.051(2) 0.463(2) 0.192(8) Uij ? ? H(1) 0.5093 0.1740 0.6466 0.2237 Uij ? ? H(2) 0.6448 0.2152 0.6105 0.2237 Uij ? ? H(3) 0.6205 0.2853 0.7151 0.2237 Uij ? ? H(4) 0.2504 0.3388 0.4919 0.0839 Uij ? ? H(5) 0.3582 0.4544 0.5507 0.0839 Uij ? ? H(6) 0.4347 0.3905 0.6978 0.1071 Uij ? ? H(7) 0.3270 0.2749 0.6388 0.1071 Uij ? ? H(8) 0.4521 0.2524 0.5054 0.1416 Uij ? ? H(9) 0.5642 0.3635 0.5731 0.1416 Uij ? ? H(12) 0.1921 0.5662 0.7820 0.0980 Uij ? ? H(13) 0.3276 0.5242 0.7804 0.0980 Uij ? ? H(14) 0.4042 0.6465 0.6901 0.1431 Uij ? ? H(15) 0.2620 0.6807 0.6740 0.1431 Uij ? ? H(16) 0.3214 0.7650 0.8644 0.2250 Uij ? ? H(17) 0.4669 0.7360 0.8762 0.2250 Uij ? ? H(18) 0.1386 0.3017 0.7025 0.1000 Uij ? ? H(19) 0.0104 0.3533 0.7027 0.1000 Uij ? ? H(20) -0.0930 0.2578 0.5180 0.1590 Uij ? ? H(21) 0.0368 0.2087 0.5150 0.1590 Uij ? ? H(22) -0.0338 0.0953 0.6055 0.2383 Uij ? ? H(23) -0.1580 0.1485 0.6195 0.2383 Uij ? ? H(24) 0.5334 0.8528 0.7731 0.3344 Uij ? ? H(25) 0.3850 0.8771 0.7525 0.3344 Uij ? ? H(26) 0.4896 0.9212 0.8686 0.3344 Uij ? ? H(27) -0.2585 0.0865 0.4288 0.2303 Uij ? ? H(28) -0.1358 0.0309 0.4166 0.2303 Uij ? ? H(29) -0.2463 -0.0148 0.4747 0.2303 Uij ? ? H(30) 0.4320 0.3671 -0.0192 0.0843 Uij ? ? H(31) 0.4361 0.1915 -0.1154 0.1043 Uij ? ? H(32) 0.2302 0.0460 -0.1824 0.0972 Uij ? ? H(33) -0.0530 0.3367 -0.0508 0.0776 Uij ? ? H(34) -0.2577 0.1889 -0.1324 0.0976 Uij ? ? H(36) -0.2151 -0.1607 -0.2547 0.1460 Uij ? ? H(37) -0.1838 -0.1073 -0.3461 0.1460 Uij ? ? H(38) -0.1233 -0.2066 -0.3270 0.1460 Uij ? ? H(39) -0.0255 -0.1346 -0.0946 0.1332 Uij ? ? H(40) 0.0674 -0.1783 -0.1670 0.1332 Uij ? ? H(41) 0.1252 -0.0615 -0.0828 0.1332 Uij ? ? H(42) 0.2079 0.3485 0.1935 0.0783 Uij ? ? H(43) 0.3161 0.4647 0.2475 0.0783 Uij ? ? H(44) -0.2411 0.0090 -0.2012 0.1053 Uij ? ? H(45) 0.0705 0.4925 0.1261 0.0692 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0703(3) 0.0757(4) 0.0316(3) 0.0185(2) 0.0227(2) 0.0196(2) S(1) 0.074(1) 0.065(1) 0.051(1) 0.008(1) 0.034(1) 0.015(1) P(1) 0.075(1) 0.081(2) 0.038(1) 0.023(1) 0.0193(10) 0.022(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4011 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0521 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0733 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.922 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.17 _refine_diff_density_max 0.81 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(1) 2.301(2) ? ? yes Pt(1) P(1) 2.301(2) ? ? yes Pt(1) C(1) 2.003(8) ? ? yes Pt(1) C(1) 2.003(8) ? ? yes S(1) O(1) 1.440(7) ? ? yes S(1) O(2) 1.430(7) ? ? yes S(1) N(1) 1.605(7) ? ? yes S(1) C(4) 1.781(9) ? ? yes P(1) C(16) 1.82(1) ? ? yes P(1) C(20) 1.837(9) ? ? yes P(1) C(24) 1.81(1) ? ? yes N(1) C(3) 1.49(1) ? ? yes N(2) C(13) 1.42(1) ? ? yes N(2) C(14) 1.45(2) ? ? yes N(2) C(15) 1.46(2) ? ? yes C(1) C(2) 1.21(1) ? ? yes C(2) C(3) 1.45(1) ? ? yes C(4) C(5) 1.36(1) ? ? yes C(4) C(9) 1.43(1) ? ? yes C(5) C(6) 1.38(1) ? ? yes C(6) C(7) 1.38(1) ? ? yes C(7) C(8) 1.39(1) ? ? yes C(8) C(9) 1.42(1) ? ? yes C(8) C(13) 1.43(1) ? ? yes C(9) C(10) 1.41(1) ? ? yes C(10) C(11) 1.38(1) ? ? yes C(11) C(12) 1.39(1) ? ? yes C(12) C(13) 1.33(1) ? ? yes C(16) C(17) 1.51(2) ? ? yes C(17) C(18) 1.55(3) ? ? yes C(18) C(19) 1.51(4) ? ? yes C(20) C(21) 1.50(1) ? ? yes C(21) C(22) 1.52(2) ? ? yes C(22) C(23) 1.49(3) ? ? yes C(24) C(25) 1.57(2) ? ? yes C(25) C(26) 1.39(3) ? ? yes C(26) C(27) 1.54(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Pt(1) P(1) 180.0 ? ? ? yes P(1) Pt(1) C(1) 92.9(2) ? ? ? yes P(1) Pt(1) C(1) 87.1(2) ? ? ? yes P(1) Pt(1) C(1) 87.1(2) ? ? ? yes P(1) Pt(1) C(1) 92.9(2) ? ? ? yes C(1) Pt(1) C(1) 180.0 ? ? ? yes O(1) S(1) O(2) 118.9(4) ? ? ? yes O(1) S(1) N(1) 105.3(4) ? ? ? yes O(1) S(1) C(4) 108.7(4) ? ? ? yes O(2) S(1) N(1) 108.3(4) ? ? ? yes O(2) S(1) C(4) 106.7(4) ? ? ? yes N(1) S(1) C(4) 108.6(4) ? ? ? yes Pt(1) P(1) C(16) 112.6(3) ? ? ? yes Pt(1) P(1) C(20) 116.2(3) ? ? ? yes Pt(1) P(1) C(24) 111.7(4) ? ? ? yes C(16) P(1) C(20) 104.7(4) ? ? ? yes C(16) P(1) C(24) 105.4(5) ? ? ? yes C(20) P(1) C(24) 105.3(5) ? ? ? yes S(1) N(1) C(3) 119.9(6) ? ? ? yes C(13) N(2) C(14) 115.3(9) ? ? ? yes C(13) N(2) C(15) 114.0(9) ? ? ? yes C(14) N(2) C(15) 110.6(10) ? ? ? yes Pt(1) C(1) C(2) 179.6(7) ? ? ? yes C(1) C(2) C(3) 177.2(9) ? ? ? yes N(1) C(3) C(2) 110.0(7) ? ? ? yes S(1) C(4) C(5) 116.6(6) ? ? ? yes S(1) C(4) C(9) 121.9(6) ? ? ? yes C(5) C(4) C(9) 121.5(8) ? ? ? yes C(4) C(5) C(6) 120.1(9) ? ? ? yes C(5) C(6) C(7) 120.8(10) ? ? ? yes C(6) C(7) C(8) 120.6(10) ? ? ? yes C(7) C(8) C(9) 119.6(8) ? ? ? yes C(7) C(8) C(13) 121.5(8) ? ? ? yes C(9) C(8) C(13) 118.9(7) ? ? ? yes C(4) C(9) C(8) 117.0(7) ? ? ? yes C(4) C(9) C(10) 123.7(8) ? ? ? yes C(8) C(9) C(10) 119.3(7) ? ? ? yes C(9) C(10) C(11) 119.0(8) ? ? ? yes C(10) C(11) C(12) 120.9(9) ? ? ? yes C(11) C(12) C(13) 122(1) ? ? ? yes N(2) C(13) C(8) 117.1(8) ? ? ? yes N(2) C(13) C(12) 123.3(9) ? ? ? yes C(8) C(13) C(12) 119.6(9) ? ? ? yes P(1) C(16) C(17) 114.4(9) ? ? ? yes C(16) C(17) C(18) 112(1) ? ? ? yes C(17) C(18) C(19) 109(2) ? ? ? yes P(1) C(20) C(21) 116.6(7) ? ? ? yes C(20) C(21) C(22) 112(1) ? ? ? yes C(21) C(22) C(23) 110(1) ? ? ? yes P(1) C(24) C(25) 110.0(9) ? ? ? yes C(24) C(25) C(26) 119(1) ? ? ? yes C(25) C(26) C(27) 110(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;