# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 loop_ _publ_author_name 'Masaaki Yoshifuji' 'Shigekazu Ito' 'Hongze Liang' _publ_contact_author_name 'Prof Masaaki Yoshifuji' _publ_contact_author_address ; Department of Chemistry Graduate School of Science, Tohoku University Aoba Sendai 980-8578 JAPAN ; _publ_contact_author_email YOSHIFJ@MAIL.CC.TOHOKU.AC.JP _publ_section_title ; Preparation,structure, and coordination properties of 3,3-bis(diisopropylamino)-3-thioxo-1(2,4,6-tri-t-butylphenyl)-1,3-diphos phapropene ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ data_amino _database_code_CSD 206703 _audit_creation_date 'Fri Oct 11 17:33:52 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C31 H57 Cl N2 P2 S ' _chemical_formula_moiety ? _chemical_formula_weight 587.27 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.2800(4) _cell_length_b 25.481(2) _cell_length_c 10.8300(3) _cell_angle_alpha 92.549(8) _cell_angle_beta 111.862(3) _cell_angle_gamma 85.841(9) _cell_volume 3647.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6786 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25003 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.8751 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.8751 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4876 _reflns_number_gt 5129 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1372 _refine_ls_wR_factor_ref 0.1851 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5129 _refine_ls_number_parameters 667 _refine_ls_goodness_of_fit_ref 1.758 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0169 _refine_diff_density_max 0.87 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl -0.5189(2) 0.2542(1) -0.8230(3) 0.061(1) Uani 1.00 d . . . Cl(2) Cl -1.0183(3) 0.2562(1) -0.3347(3) 0.066(1) Uani 1.00 d . . . S(1) S -0.2445(2) 0.3581(1) -0.5987(3) 0.066(1) Uani 1.00 d . . . S(2) S -0.7388(3) 0.3571(1) -0.1128(3) 0.068(1) Uani 1.00 d . . . P(1) P -0.3050(3) 0.2395(1) -0.6109(3) 0.059(1) Uani 1.00 d . . . P(2) P -0.3834(2) 0.3471(1) -0.7226(3) 0.045(1) Uani 1.00 d . . . P(3) P -0.8052(3) 0.2394(1) -0.1233(4) 0.066(1) Uani 1.00 d . . . P(4) P -0.8726(2) 0.3456(1) -0.2489(3) 0.044(1) Uani 1.00 d . . . N(1) N -0.4057(6) 0.3576(3) -0.8830(8) 0.045(3) Uani 1.00 d . . . N(2) N -0.4710(6) 0.3833(3) -0.6869(8) 0.044(3) Uani 1.00 d . . . N(3) N -0.8808(7) 0.3562(3) -0.4035(9) 0.055(3) Uani 1.00 d . . . N(4) N -0.9710(7) 0.3816(3) -0.2319(8) 0.052(3) Uani 1.00 d . . . C(1) C -0.4010(8) 0.2767(4) -0.7171(10) 0.043(4) Uani 1.00 d . . . C(2) C -0.3593(9) 0.1746(5) -0.635(1) 0.053(4) Uani 1.00 d . . . C(3) C -0.353(1) 0.1395(5) -0.737(1) 0.062(5) Uani 1.00 d . . . C(4) C -0.419(1) 0.0989(5) -0.775(1) 0.088(7) Uani 1.00 d . . . C(5) C -0.488(1) 0.0893(6) -0.719(2) 0.084(6) Uani 1.00 d . . . C(6) C -0.484(1) 0.1208(6) -0.610(1) 0.076(6) Uani 1.00 d . . . C(7) C -0.4189(9) 0.1618(4) -0.563(1) 0.052(5) Uani 1.00 d . . . C(8) C -0.274(1) 0.1400(5) -0.806(2) 0.090(7) Uani 1.00 d . . . C(9) C -0.322(2) 0.1683(8) -0.934(2) 0.20(1) Uani 1.00 d . . . C(10) C -0.180(2) 0.1680(10) -0.724(2) 0.20(1) Uani 1.00 d . . . C(11) C -0.240(1) 0.0854(6) -0.832(2) 0.153(9) Uani 1.00 d . . . C(12) C -0.568(2) 0.0487(7) -0.778(2) 0.115(9) Uani 1.00 d . . . C(13) C -0.636(2) 0.060(1) -0.911(3) 0.30(2) Uani 1.00 d . . . C(14) C -0.518(2) -0.0043(8) -0.773(3) 0.26(2) Uani 1.00 d . . . C(15) C -0.626(3) 0.043(1) -0.691(3) 0.33(2) Uani 1.00 d . . . C(16) C -0.421(1) 0.1901(5) -0.433(1) 0.075(6) Uani 1.00 d . . . C(17) C -0.321(1) 0.2155(6) -0.351(1) 0.118(7) Uani 1.00 d . . . C(18) C -0.506(1) 0.2330(6) -0.466(1) 0.119(7) Uani 1.00 d . . . C(19) C -0.437(1) 0.1514(6) -0.339(1) 0.119(7) Uani 1.00 d . . . C(20) C -0.3764(9) 0.3157(4) -0.961(1) 0.057(4) Uani 1.00 d . . . C(21) C -0.280(1) 0.3192(6) -0.983(2) 0.119(7) Uani 1.00 d . . . C(22) C -0.463(1) 0.3020(5) -1.094(1) 0.088(5) Uani 1.00 d . . . C(23) C -0.4122(8) 0.4141(4) -0.921(1) 0.058(4) Uani 1.00 d . . . C(24) C -0.310(1) 0.4385(5) -0.897(1) 0.101(6) Uani 1.00 d . . . C(25) C -0.487(1) 0.4252(4) -1.063(1) 0.078(5) Uani 1.00 d . . . C(26) C -0.5802(8) 0.3836(4) -0.7792(10) 0.047(3) Uani 1.00 d . . . C(27) C -0.6455(9) 0.3556(4) -0.720(1) 0.064(4) Uani 1.00 d . . . C(28) C -0.6265(9) 0.4399(5) -0.820(1) 0.069(5) Uani 1.00 d . . . C(29) C -0.4512(9) 0.4141(5) -0.559(1) 0.063(4) Uani 1.00 d . . . C(30) C -0.413(1) 0.3815(6) -0.434(1) 0.097(6) Uani 1.00 d . . . C(31) C -0.392(1) 0.4628(5) -0.549(1) 0.093(5) Uani 1.00 d . . . C(32) C -0.8991(8) 0.2776(4) -0.233(1) 0.051(4) Uani 1.00 d . . . C(33) C -0.8659(10) 0.1748(4) -0.146(1) 0.062(5) Uani 1.00 d . . . C(34) C -0.858(1) 0.1365(6) -0.242(1) 0.079(6) Uani 1.00 d . . . C(35) C -0.924(1) 0.0978(5) -0.280(1) 0.072(6) Uani 1.00 d . . . C(36) C -0.993(1) 0.0919(5) -0.219(2) 0.079(6) Uani 1.00 d . . . C(37) C -0.986(1) 0.1236(6) -0.109(1) 0.078(6) Uani 1.00 d . . . C(38) C -0.924(1) 0.1657(5) -0.070(1) 0.074(6) Uani 1.00 d . . . C(39) C -0.780(1) 0.1382(6) -0.313(2) 0.096(7) Uani 1.00 d . . . C(40) C -0.823(2) 0.1733(7) -0.434(2) 0.154(9) Uani 1.00 d . . . C(41) C -0.679(1) 0.1567(8) -0.225(2) 0.145(9) Uani 1.00 d . . . C(42) C -0.754(2) 0.0834(7) -0.359(2) 0.20(1) Uani 1.00 d . . . C(43) C -1.068(1) 0.0476(6) -0.270(2) 0.094(7) Uani 1.00 d . . . C(44) C -1.145(2) 0.0590(8) -0.402(2) 0.23(1) Uani 1.00 d . . . C(45) C -1.019(2) -0.0044(7) -0.266(3) 0.24(1) Uani 1.00 d . . . C(46) C -1.132(2) 0.045(1) -0.182(3) 0.28(2) Uani 1.00 d . . . C(47) C -0.925(1) 0.1957(6) 0.059(1) 0.082(6) Uani 1.00 d . . . C(48) C -0.929(1) 0.1554(6) 0.160(1) 0.119(7) Uani 1.00 d . . . C(49) C -0.835(2) 0.2268(8) 0.133(2) 0.154(10) Uani 1.00 d . . . C(50) C -1.021(1) 0.2311(6) 0.022(2) 0.130(8) Uani 1.00 d . . . C(51) C -0.7910(9) 0.3628(5) -0.440(1) 0.069(5) Uani 1.00 d . . . C(52) C -0.744(1) 0.4157(5) -0.395(1) 0.097(6) Uani 1.00 d . . . C(53) C -0.715(1) 0.3170(5) -0.409(1) 0.092(6) Uani 1.00 d . . . C(54) C -0.9804(8) 0.3516(4) -0.520(1) 0.053(4) Uani 1.00 d . . . C(55) C -1.0082(10) 0.4019(5) -0.602(1) 0.082(5) Uani 1.00 d . . . C(56) C -0.984(1) 0.3043(5) -0.608(1) 0.080(5) Uani 1.00 d . . . C(57) C -1.0110(9) 0.3630(4) -0.135(1) 0.061(4) Uani 1.00 d . . . C(58) C -1.126(1) 0.3640(7) -0.187(2) 0.124(7) Uani 1.00 d . . . C(59) C -0.971(1) 0.3887(6) 0.005(1) 0.118(7) Uani 1.00 d . . . C(60) C -0.9766(8) 0.4380(4) -0.264(1) 0.062(4) Uani 1.00 d . . . C(61) C -1.085(1) 0.4614(5) -0.323(1) 0.105(6) Uani 1.00 d . . . C(62) C -0.915(1) 0.4745(5) -0.148(1) 0.101(6) Uani 1.00 d . . . H(1) H -0.4160 0.0756 -0.8480 0.0997 Uiso 1.00 calc . . . H(2) H -0.5308 0.1134 -0.5664 0.0909 Uiso 1.00 calc . . . H(3) H -0.3814 0.1486 -0.9927 0.2240 Uiso 1.00 calc . . . H(4) H -0.3461 0.2027 -0.9269 0.2240 Uiso 1.00 calc . . . H(5) H -0.2789 0.1678 -0.9859 0.2240 Uiso 1.00 calc . . . H(6) H -0.1935 0.2033 -0.6996 0.2566 Uiso 1.00 calc . . . H(7) H -0.1306 0.1682 -0.7648 0.2566 Uiso 1.00 calc . . . H(8) H -0.1438 0.1496 -0.6381 0.2566 Uiso 1.00 calc . . . H(9) H -0.1934 0.0853 -0.8796 0.1763 Uiso 1.00 calc . . . H(10) H -0.2058 0.0668 -0.7522 0.1763 Uiso 1.00 calc . . . H(11) H -0.2965 0.0666 -0.8872 0.1763 Uiso 1.00 calc . . . H(12) H -0.6801 0.0926 -0.9258 0.3019 Uiso 1.00 calc . . . H(13) H -0.6076 0.0594 -0.9795 0.3019 Uiso 1.00 calc . . . H(14) H -0.6921 0.0327 -0.9523 0.3019 Uiso 1.00 calc . . . H(15) H -0.4803 -0.0063 -0.8363 0.2961 Uiso 1.00 calc . . . H(16) H -0.5616 -0.0327 -0.8016 0.2961 Uiso 1.00 calc . . . H(17) H -0.4676 -0.0118 -0.6887 0.2961 Uiso 1.00 calc . . . H(18) H -0.6590 0.0080 -0.7098 0.3617 Uiso 1.00 calc . . . H(19) H -0.5652 0.0292 -0.5970 0.3617 Uiso 1.00 calc . . . H(20) H -0.6580 0.0671 -0.6689 0.3617 Uiso 1.00 calc . . . H(21) H -0.3199 0.2336 -0.2703 0.1278 Uiso 1.00 calc . . . H(22) H -0.3013 0.2406 -0.4007 0.1278 Uiso 1.00 calc . . . H(23) H -0.2622 0.1892 -0.3210 0.1278 Uiso 1.00 calc . . . H(24) H -0.4977 0.2581 -0.5262 0.1378 Uiso 1.00 calc . . . H(25) H -0.5099 0.2514 -0.3914 0.1378 Uiso 1.00 calc . . . H(26) H -0.5705 0.2179 -0.5148 0.1378 Uiso 1.00 calc . . . H(27) H -0.4994 0.1338 -0.3793 0.1427 Uiso 1.00 calc . . . H(28) H -0.4407 0.1686 -0.2576 0.1427 Uiso 1.00 calc . . . H(29) H -0.3834 0.1240 -0.3084 0.1427 Uiso 1.00 calc . . . H(30) H -0.3659 0.2835 -0.9085 0.0790 Uiso 1.00 calc . . . H(31) H -0.2214 0.3220 -0.8995 0.1344 Uiso 1.00 calc . . . H(32) H -0.2809 0.3482 -1.0353 0.1344 Uiso 1.00 calc . . . H(33) H -0.2619 0.2875 -1.0280 0.1344 Uiso 1.00 calc . . . H(34) H -0.4773 0.3304 -1.1539 0.0992 Uiso 1.00 calc . . . H(35) H -0.4435 0.2711 -1.1377 0.0992 Uiso 1.00 calc . . . H(36) H -0.5227 0.2947 -1.0809 0.0992 Uiso 1.00 calc . . . H(37) H -0.4409 0.4339 -0.8595 0.0735 Uiso 1.00 calc . . . H(38) H -0.2664 0.4372 -0.8030 0.1075 Uiso 1.00 calc . . . H(39) H -0.3228 0.4777 -0.9129 0.1075 Uiso 1.00 calc . . . H(40) H -0.2788 0.4245 -0.9495 0.1075 Uiso 1.00 calc . . . H(41) H -0.4970 0.4644 -1.0729 0.1093 Uiso 1.00 calc . . . H(42) H -0.4667 0.4103 -1.1231 0.1093 Uiso 1.00 calc . . . H(43) H -0.5539 0.4151 -1.0698 0.1093 Uiso 1.00 calc . . . H(44) H -0.5833 0.3642 -0.8644 0.0653 Uiso 1.00 calc . . . H(45) H -0.6972 0.4394 -0.8804 0.0797 Uiso 1.00 calc . . . H(46) H -0.5917 0.4583 -0.8610 0.0797 Uiso 1.00 calc . . . H(47) H -0.6268 0.4591 -0.7414 0.0797 Uiso 1.00 calc . . . H(48) H -0.7161 0.3554 -0.7821 0.0756 Uiso 1.00 calc . . . H(49) H -0.6226 0.3197 -0.7007 0.0756 Uiso 1.00 calc . . . H(50) H -0.6455 0.3735 -0.6417 0.0756 Uiso 1.00 calc . . . H(51) H -0.5176 0.4291 -0.5621 0.0768 Uiso 1.00 calc . . . H(52) H -0.3466 0.3651 -0.4195 0.1057 Uiso 1.00 calc . . . H(53) H -0.4563 0.3533 -0.4386 0.1057 Uiso 1.00 calc . . . H(54) H -0.4071 0.4019 -0.3540 0.1057 Uiso 1.00 calc . . . H(55) H -0.3850 0.4830 -0.4678 0.1108 Uiso 1.00 calc . . . H(56) H -0.4211 0.4844 -0.6217 0.1108 Uiso 1.00 calc . . . H(57) H -0.3236 0.4512 -0.5408 0.1108 Uiso 1.00 calc . . . H(58) H -0.9241 0.0726 -0.3533 0.0991 Uiso 1.00 calc . . . H(59) H -1.0256 0.1174 -0.0547 0.0980 Uiso 1.00 calc . . . H(60) H -0.7749 0.1738 -0.4792 0.1714 Uiso 1.00 calc . . . H(61) H -0.8834 0.1613 -0.4943 0.1714 Uiso 1.00 calc . . . H(62) H -0.8329 0.2091 -0.4074 0.1714 Uiso 1.00 calc . . . H(63) H -0.6808 0.1930 -0.1923 0.1760 Uiso 1.00 calc . . . H(64) H -0.6287 0.1560 -0.2683 0.1760 Uiso 1.00 calc . . . H(65) H -0.6447 0.1359 -0.1448 0.1760 Uiso 1.00 calc . . . H(66) H -0.7153 0.0820 -0.4113 0.2093 Uiso 1.00 calc . . . H(67) H -0.7328 0.0580 -0.2930 0.2093 Uiso 1.00 calc . . . H(68) H -0.8235 0.0695 -0.4249 0.2093 Uiso 1.00 calc . . . H(69) H -1.1935 0.0334 -0.4321 0.2567 Uiso 1.00 calc . . . H(70) H -1.1790 0.0929 -0.3994 0.2567 Uiso 1.00 calc . . . H(71) H -1.1134 0.0612 -0.4665 0.2567 Uiso 1.00 calc . . . H(72) H -0.9758 -0.0100 -0.3099 0.2492 Uiso 1.00 calc . . . H(73) H -0.9708 -0.0105 -0.1644 0.2492 Uiso 1.00 calc . . . H(74) H -1.0621 -0.0331 -0.2788 0.2492 Uiso 1.00 calc . . . H(75) H -1.0834 0.0404 -0.0869 0.3021 Uiso 1.00 calc . . . H(76) H -1.1744 0.0178 -0.2016 0.3021 Uiso 1.00 calc . . . H(77) H -1.1679 0.0782 -0.1796 0.3021 Uiso 1.00 calc . . . H(78) H -0.8708 0.1317 0.1828 0.1346 Uiso 1.00 calc . . . H(79) H -0.9880 0.1356 0.1205 0.1346 Uiso 1.00 calc . . . H(80) H -0.9316 0.1722 0.2396 0.1346 Uiso 1.00 calc . . . H(81) H -0.7715 0.2070 0.1554 0.1841 Uiso 1.00 calc . . . H(82) H -0.8275 0.2558 0.0731 0.1841 Uiso 1.00 calc . . . H(83) H -0.8352 0.2467 0.2096 0.1841 Uiso 1.00 calc . . . H(84) H -1.0283 0.2580 -0.0429 0.1624 Uiso 1.00 calc . . . H(85) H -1.0365 0.2485 0.0931 0.1624 Uiso 1.00 calc . . . H(86) H -1.0831 0.2100 -0.0258 0.1624 Uiso 1.00 calc . . . H(87) H -0.8169 0.3636 -0.5374 0.0883 Uiso 1.00 calc . . . H(88) H -0.7165 0.4188 -0.2962 0.1145 Uiso 1.00 calc . . . H(89) H -0.7960 0.4452 -0.4215 0.1145 Uiso 1.00 calc . . . H(90) H -0.6925 0.4231 -0.4237 0.1145 Uiso 1.00 calc . . . H(91) H -0.6607 0.3194 -0.4408 0.1037 Uiso 1.00 calc . . . H(92) H -0.7455 0.2830 -0.4492 0.1037 Uiso 1.00 calc . . . H(93) H -0.6839 0.3100 -0.3149 0.1037 Uiso 1.00 calc . . . H(94) H -1.0347 0.3492 -0.4832 0.0689 Uiso 1.00 calc . . . H(95) H -1.0755 0.4031 -0.6697 0.0979 Uiso 1.00 calc . . . H(96) H -1.0109 0.4337 -0.5431 0.0979 Uiso 1.00 calc . . . H(97) H -0.9614 0.4085 -0.6388 0.0979 Uiso 1.00 calc . . . H(98) H -0.9354 0.3046 -0.6502 0.1003 Uiso 1.00 calc . . . H(99) H -0.9699 0.2713 -0.5602 0.1003 Uiso 1.00 calc . . . H(100) H -1.0497 0.3003 -0.6808 0.1003 Uiso 1.00 calc . . . H(101) H -0.9872 0.3260 -0.1201 0.0794 Uiso 1.00 calc . . . H(102) H -1.1514 0.3426 -0.2699 0.1451 Uiso 1.00 calc . . . H(103) H -1.1498 0.3469 -0.1258 0.1451 Uiso 1.00 calc . . . H(104) H -1.1563 0.3975 -0.2038 0.1451 Uiso 1.00 calc . . . H(105) H -0.9912 0.3734 0.0683 0.1251 Uiso 1.00 calc . . . H(106) H -0.9894 0.4259 0.0021 0.1251 Uiso 1.00 calc . . . H(107) H -0.8956 0.3864 0.0425 0.1251 Uiso 1.00 calc . . . H(108) H -0.9470 0.4393 -0.3347 0.0794 Uiso 1.00 calc . . . H(109) H -1.1238 0.4413 -0.4041 0.1233 Uiso 1.00 calc . . . H(110) H -1.1170 0.4608 -0.2635 0.1233 Uiso 1.00 calc . . . H(111) H -1.0877 0.4970 -0.3533 0.1233 Uiso 1.00 calc . . . H(112) H -0.8429 0.4634 -0.1099 0.1167 Uiso 1.00 calc . . . H(113) H -0.9390 0.4760 -0.0768 0.1167 Uiso 1.00 calc . . . H(114) H -0.9164 0.5110 -0.1748 0.1167 Uiso 1.00 calc . . . 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 Cl(1) 0.054(3) 0.066(2) 0.065(2) -0.013(2) 0.024(2) -0.009(2) Cl(2) 0.058(3) 0.082(2) 0.062(2) -0.021(2) 0.022(2) -0.004(2) S(1) 0.040(3) 0.084(2) 0.064(3) -0.007(2) 0.008(2) -0.005(2) S(2) 0.048(3) 0.095(3) 0.057(2) -0.018(2) 0.013(2) -0.008(2) P(1) 0.055(3) 0.068(2) 0.058(2) 0.006(2) 0.024(2) 0.011(2) P(2) 0.040(2) 0.058(2) 0.042(2) -0.008(2) 0.022(2) -0.005(2) P(3) 0.061(3) 0.082(3) 0.067(3) 0.000(2) 0.035(2) 0.013(2) P(4) 0.033(2) 0.064(2) 0.038(2) -0.003(2) 0.017(2) -0.001(2) N(1) 0.042(6) 0.060(6) 0.035(6) -0.010(5) 0.014(5) -0.001(4) N(2) 0.038(6) 0.061(6) 0.033(6) -0.013(5) 0.010(5) -0.019(4) N(3) 0.049(7) 0.083(7) 0.048(7) -0.008(5) 0.032(6) 0.014(5) N(4) 0.063(8) 0.051(6) 0.050(7) 0.000(5) 0.032(6) 0.005(5) C(1) 0.049(9) 0.047(7) 0.039(7) -0.005(6) 0.023(7) -0.007(5) C(2) 0.049(9) 0.075(9) 0.037(8) -0.001(7) 0.018(7) 0.000(6) C(3) 0.07(1) 0.044(8) 0.08(1) 0.005(7) 0.033(9) 0.008(7) C(4) 0.14(2) 0.08(1) 0.07(1) 0.01(1) 0.07(1) 0.005(9) C(5) 0.11(2) 0.07(1) 0.09(1) 0.00(1) 0.05(1) -0.003(9) C(6) 0.09(1) 0.08(1) 0.09(1) 0.010(9) 0.06(1) 0.015(9) C(7) 0.06(1) 0.053(8) 0.055(9) 0.000(7) 0.038(8) 0.003(7) C(8) 0.14(2) 0.07(1) 0.10(1) 0.03(1) 0.10(1) -0.002(9) C(9) 0.24(3) 0.28(2) 0.16(2) 0.15(2) 0.17(2) 0.13(2) C(10) 0.15(2) 0.27(3) 0.26(3) -0.08(2) 0.17(2) -0.11(2) C(11) 0.18(2) 0.12(1) 0.21(2) 0.05(1) 0.14(2) 0.00(1) C(12) 0.17(2) 0.09(1) 0.11(2) -0.04(1) 0.08(2) -0.03(1) C(13) 0.35(5) 0.28(3) 0.17(2) -0.22(3) -0.05(3) 0.04(2) C(14) 0.23(3) 0.10(2) 0.49(5) -0.09(2) 0.16(3) -0.07(2) C(15) 0.41(5) 0.39(4) 0.28(3) -0.36(4) 0.21(3) -0.23(3) C(16) 0.10(1) 0.09(1) 0.05(1) 0.001(10) 0.05(1) 0.006(8) C(17) 0.15(2) 0.15(1) 0.06(1) -0.03(1) 0.05(1) -0.02(1) C(18) 0.15(2) 0.12(1) 0.09(1) 0.07(1) 0.07(1) -0.007(9) C(19) 0.17(2) 0.13(1) 0.09(1) -0.01(1) 0.08(1) 0.01(1) C(20) 0.046(8) 0.083(8) 0.045(8) 0.010(7) 0.021(7) 0.009(6) C(21) 0.10(1) 0.15(1) 0.15(2) 0.03(1) 0.09(1) 0.02(1) C(22) 0.11(1) 0.10(1) 0.049(9) 0.009(9) 0.024(9) -0.025(7) C(23) 0.046(8) 0.077(8) 0.057(8) -0.013(6) 0.022(7) 0.009(6) C(24) 0.07(1) 0.10(1) 0.12(1) -0.046(9) 0.022(10) 0.010(9) C(25) 0.08(1) 0.087(10) 0.061(9) -0.014(8) 0.011(8) 0.023(7) C(26) 0.030(7) 0.062(7) 0.039(7) -0.013(6) -0.002(6) -0.006(5) C(27) 0.056(9) 0.076(8) 0.070(9) -0.018(7) 0.034(8) -0.018(7) C(28) 0.061(9) 0.086(9) 0.057(9) 0.011(7) 0.022(7) -0.003(7) C(29) 0.047(8) 0.081(9) 0.054(9) 0.008(7) 0.016(7) -0.024(7) C(30) 0.09(1) 0.14(1) 0.039(9) 0.004(10) 0.006(8) -0.028(8) C(31) 0.07(1) 0.082(10) 0.10(1) 0.005(8) 0.012(9) -0.041(8) C(32) 0.036(9) 0.072(8) 0.050(8) 0.000(7) 0.020(7) 0.000(6) C(33) 0.07(1) 0.060(9) 0.08(1) 0.000(7) 0.049(9) 0.010(7) C(34) 0.10(1) 0.08(1) 0.08(1) 0.02(1) 0.06(1) 0.016(9) C(35) 0.09(1) 0.06(1) 0.08(1) 0.010(9) 0.04(1) 0.005(8) C(36) 0.09(1) 0.07(1) 0.09(1) 0.005(9) 0.04(1) 0.026(9) C(37) 0.11(1) 0.07(1) 0.08(1) -0.007(10) 0.06(1) 0.003(8) C(38) 0.09(1) 0.08(1) 0.07(1) 0.013(9) 0.05(1) 0.014(9) C(39) 0.11(2) 0.12(1) 0.07(1) 0.01(1) 0.06(1) 0.01(1) C(40) 0.22(2) 0.18(2) 0.11(2) 0.05(2) 0.12(2) 0.04(1) C(41) 0.10(2) 0.20(2) 0.16(2) 0.01(1) 0.09(2) 0.00(2) C(42) 0.25(3) 0.13(2) 0.34(3) 0.00(2) 0.26(3) -0.04(2) C(43) 0.10(2) 0.09(1) 0.10(1) -0.03(1) 0.03(1) 0.02(1) C(44) 0.20(3) 0.17(2) 0.20(2) -0.07(2) -0.07(2) 0.05(2) C(45) 0.19(3) 0.07(2) 0.46(4) 0.00(2) 0.12(3) 0.03(2) C(46) 0.26(3) 0.35(4) 0.32(4) -0.22(3) 0.19(3) -0.12(3) C(47) 0.11(2) 0.09(1) 0.08(1) 0.00(1) 0.07(1) 0.005(9) C(48) 0.17(2) 0.12(1) 0.10(1) 0.00(1) 0.09(1) 0.02(1) C(49) 0.20(2) 0.21(2) 0.09(1) -0.10(2) 0.09(2) -0.06(1) C(50) 0.18(2) 0.13(1) 0.10(1) 0.05(1) 0.09(1) 0.00(1) C(51) 0.045(8) 0.12(1) 0.053(8) -0.006(8) 0.023(7) 0.024(8) C(52) 0.07(1) 0.12(1) 0.12(1) -0.022(9) 0.05(1) 0.028(10) C(53) 0.07(1) 0.13(1) 0.10(1) 0.010(9) 0.056(10) 0.022(9) C(54) 0.041(8) 0.079(8) 0.035(7) -0.014(6) 0.006(6) 0.003(6) C(55) 0.07(1) 0.11(1) 0.063(9) -0.003(8) 0.010(8) 0.025(8) C(56) 0.09(1) 0.10(1) 0.051(9) -0.017(9) 0.031(9) -0.004(8) C(57) 0.058(9) 0.076(8) 0.060(9) 0.010(7) 0.036(8) 0.002(7) C(58) 0.07(1) 0.19(2) 0.13(1) 0.01(1) 0.05(1) 0.05(1) C(59) 0.16(2) 0.13(1) 0.07(1) -0.01(1) 0.05(1) -0.001(10) C(60) 0.036(8) 0.078(9) 0.063(9) -0.004(7) 0.011(7) -0.009(7) C(61) 0.08(1) 0.08(1) 0.13(1) 0.021(9) 0.01(1) 0.006(9) C(62) 0.11(1) 0.077(10) 0.11(1) -0.024(9) 0.03(1) -0.018(9) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl(1) C(1) 1.77(1) . . yes Cl(2) C(32) 1.76(1) . . yes S(1) P(2) 1.969(5) . . yes S(2) P(4) 1.963(5) . . yes P(1) C(1) 1.68(1) . . yes P(1) C(2) 1.84(1) . . yes P(2) N(1) 1.674(8) . . yes P(2) N(2) 1.651(8) . . yes P(2) C(1) 1.836(10) . . yes P(3) C(32) 1.70(1) . . yes P(3) C(33) 1.88(1) . . yes P(4) N(3) 1.667(9) . . yes P(4) N(4) 1.686(9) . . yes P(4) C(32) 1.83(1) . . yes N(1) C(20) 1.47(1) . . yes N(1) C(23) 1.50(1) . . yes N(2) C(26) 1.51(1) . . yes N(2) C(29) 1.50(1) . . yes N(3) C(51) 1.50(1) . . yes N(3) C(54) 1.52(1) . . yes N(4) C(57) 1.48(1) . . yes N(4) C(60) 1.48(1) . . yes C(2) C(3) 1.42(1) . . yes C(2) C(7) 1.41(1) . . yes C(3) C(4) 1.39(2) . . yes C(3) C(8) 1.57(2) . . yes C(4) C(5) 1.37(2) . . yes C(5) C(6) 1.39(2) . . yes C(5) C(12) 1.53(2) . . yes C(6) C(7) 1.40(2) . . yes C(7) C(16) 1.56(1) . . yes C(8) C(9) 1.49(2) . . yes C(8) C(10) 1.52(2) . . yes C(8) C(11) 1.49(2) . . yes C(12) C(13) 1.43(3) . . yes C(12) C(14) 1.48(2) . . yes C(12) C(15) 1.49(3) . . yes C(16) C(17) 1.54(2) . . yes C(16) C(18) 1.53(2) . . yes C(16) C(19) 1.54(2) . . yes C(20) C(21) 1.49(2) . . yes C(20) C(22) 1.55(2) . . yes C(23) C(24) 1.56(1) . . yes C(23) C(25) 1.53(1) . . yes C(26) C(27) 1.54(1) . . yes C(26) C(28) 1.54(1) . . yes C(29) C(30) 1.52(2) . . yes C(29) C(31) 1.53(2) . . yes C(33) C(34) 1.42(2) . . yes C(33) C(38) 1.41(2) . . yes C(34) C(35) 1.36(2) . . yes C(34) C(39) 1.58(2) . . yes C(35) C(36) 1.40(2) . . yes C(36) C(37) 1.38(2) . . yes C(36) C(43) 1.55(2) . . yes C(37) C(38) 1.39(2) . . yes C(38) C(47) 1.57(2) . . yes C(39) C(40) 1.53(2) . . yes C(39) C(41) 1.50(2) . . yes C(39) C(42) 1.53(2) . . yes C(43) C(44) 1.47(2) . . yes C(43) C(45) 1.45(2) . . yes C(43) C(46) 1.54(2) . . yes C(47) C(48) 1.55(2) . . yes C(47) C(49) 1.50(2) . . yes C(47) C(50) 1.52(2) . . yes C(51) C(52) 1.53(2) . . yes C(51) C(53) 1.50(2) . . yes C(54) C(55) 1.54(1) . . yes C(54) C(56) 1.50(1) . . yes C(57) C(58) 1.52(2) . . yes C(57) C(59) 1.55(2) . . yes C(60) C(61) 1.53(2) . . yes C(60) C(62) 1.55(2) . . 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 C(1) P(1) C(2) 101.8(5) . 1_555 1_555 yes S(1) P(2) N(1) 115.3(4) . 1_555 1_555 yes S(1) P(2) N(2) 113.9(4) . 1_555 1_555 yes S(1) P(2) C(1) 106.0(4) . 1_555 1_555 yes N(1) P(2) N(2) 106.2(5) . 1_555 1_555 yes N(1) P(2) C(1) 104.3(4) . 1_555 1_555 yes N(2) P(2) C(1) 110.8(5) . 1_555 1_555 yes C(32) P(3) C(33) 101.4(6) . 1_555 1_555 yes S(2) P(4) N(3) 113.8(4) . 1_555 1_555 yes S(2) P(4) N(4) 116.3(4) . 1_555 1_555 yes S(2) P(4) C(32) 106.7(4) . 1_555 1_555 yes N(3) P(4) N(4) 105.1(5) . 1_555 1_555 yes N(3) P(4) C(32) 110.5(5) . 1_555 1_555 yes N(4) P(4) C(32) 104.1(5) . 1_555 1_555 yes P(2) N(1) C(20) 118.9(7) . 1_555 1_555 yes P(2) N(1) C(23) 116.0(7) . 1_555 1_555 yes C(20) N(1) C(23) 120.1(8) . 1_555 1_555 yes P(2) N(2) C(26) 120.6(6) . 1_555 1_555 yes P(2) N(2) C(29) 124.0(7) . 1_555 1_555 yes C(26) N(2) C(29) 115.2(8) . 1_555 1_555 yes P(4) N(3) C(51) 123.6(8) . 1_555 1_555 yes P(4) N(3) C(54) 120.3(7) . 1_555 1_555 yes C(51) N(3) C(54) 115.4(8) . 1_555 1_555 yes P(4) N(4) C(57) 116.7(7) . 1_555 1_555 yes P(4) N(4) C(60) 114.7(7) . 1_555 1_555 yes C(57) N(4) C(60) 122.4(8) . 1_555 1_555 yes Cl(1) C(1) P(1) 125.7(6) . 1_555 1_555 yes Cl(1) C(1) P(2) 116.6(6) . 1_555 1_555 yes P(1) C(1) P(2) 117.7(6) . 1_555 1_555 yes P(1) C(2) C(3) 120.7(9) . 1_555 1_555 yes P(1) C(2) C(7) 120.4(9) . 1_555 1_555 yes C(3) C(2) C(7) 118(1) . 1_555 1_555 yes C(2) C(3) C(4) 117(1) . 1_555 1_555 yes C(2) C(3) C(8) 125(1) . 1_555 1_555 yes C(4) C(3) C(8) 116(1) . 1_555 1_555 yes C(3) C(4) C(5) 125(1) . 1_555 1_555 yes C(4) C(5) C(6) 115(1) . 1_555 1_555 yes C(4) C(5) C(12) 122(1) . 1_555 1_555 yes C(6) C(5) C(12) 121(1) . 1_555 1_555 yes C(5) C(6) C(7) 122(1) . 1_555 1_555 yes C(2) C(7) C(6) 119(1) . 1_555 1_555 yes C(2) C(7) C(16) 125(1) . 1_555 1_555 yes C(6) C(7) C(16) 115(1) . 1_555 1_555 yes C(3) C(8) C(9) 109(1) . 1_555 1_555 yes C(3) C(8) C(10) 113(1) . 1_555 1_555 yes C(3) C(8) C(11) 111(1) . 1_555 1_555 yes C(9) C(8) C(10) 107(1) . 1_555 1_555 yes C(9) C(8) C(11) 109(1) . 1_555 1_555 yes C(10) C(8) C(11) 106(1) . 1_555 1_555 yes C(5) C(12) C(13) 113(1) . 1_555 1_555 yes C(5) C(12) C(14) 109(1) . 1_555 1_555 yes C(5) C(12) C(15) 111(1) . 1_555 1_555 yes C(13) C(12) C(14) 109(2) . 1_555 1_555 yes C(13) C(12) C(15) 109(2) . 1_555 1_555 yes C(14) C(12) C(15) 101(2) . 1_555 1_555 yes C(7) C(16) C(17) 113(1) . 1_555 1_555 yes C(7) C(16) C(18) 110(1) . 1_555 1_555 yes C(7) C(16) C(19) 111(1) . 1_555 1_555 yes C(17) C(16) C(18) 108(1) . 1_555 1_555 yes C(17) C(16) C(19) 105(1) . 1_555 1_555 yes C(18) C(16) C(19) 107(1) . 1_555 1_555 yes N(1) C(20) C(21) 118(1) . 1_555 1_555 yes N(1) C(20) C(22) 113.8(9) . 1_555 1_555 yes C(21) C(20) C(22) 109(1) . 1_555 1_555 yes N(1) C(23) C(24) 116.1(10) . 1_555 1_555 yes N(1) C(23) C(25) 113.3(9) . 1_555 1_555 yes C(24) C(23) C(25) 110.3(9) . 1_555 1_555 yes N(2) C(26) C(27) 112.2(8) . 1_555 1_555 yes N(2) C(26) C(28) 112.3(8) . 1_555 1_555 yes C(27) C(26) C(28) 109.6(9) . 1_555 1_555 yes N(2) C(29) C(30) 115.3(10) . 1_555 1_555 yes N(2) C(29) C(31) 113(1) . 1_555 1_555 yes C(30) C(29) C(31) 113(1) . 1_555 1_555 yes Cl(2) C(32) P(3) 124.9(7) . 1_555 1_555 yes Cl(2) C(32) P(4) 117.8(6) . 1_555 1_555 yes P(3) C(32) P(4) 117.3(7) . 1_555 1_555 yes P(3) C(33) C(34) 121.7(10) . 1_555 1_555 yes P(3) C(33) C(38) 118(1) . 1_555 1_555 yes C(34) C(33) C(38) 119(1) . 1_555 1_555 yes C(33) C(34) C(35) 118(1) . 1_555 1_555 yes C(33) C(34) C(39) 123(1) . 1_555 1_555 yes C(35) C(34) C(39) 118(1) . 1_555 1_555 yes C(34) C(35) C(36) 121(1) . 1_555 1_555 yes C(35) C(36) C(37) 117(1) . 1_555 1_555 yes C(35) C(36) C(43) 118(1) . 1_555 1_555 yes C(37) C(36) C(43) 123(1) . 1_555 1_555 yes C(36) C(37) C(38) 122(1) . 1_555 1_555 yes C(33) C(38) C(37) 117(1) . 1_555 1_555 yes C(33) C(38) C(47) 128(1) . 1_555 1_555 yes C(37) C(38) C(47) 114(1) . 1_555 1_555 yes C(34) C(39) C(40) 109(1) . 1_555 1_555 yes C(34) C(39) C(41) 114(1) . 1_555 1_555 yes C(34) C(39) C(42) 111(1) . 1_555 1_555 yes C(40) C(39) C(41) 108(1) . 1_555 1_555 yes C(40) C(39) C(42) 107(1) . 1_555 1_555 yes C(41) C(39) C(42) 103(1) . 1_555 1_555 yes C(36) C(43) C(44) 111(1) . 1_555 1_555 yes C(36) C(43) C(45) 113(1) . 1_555 1_555 yes C(36) C(43) C(46) 110(1) . 1_555 1_555 yes C(44) C(43) C(45) 111(1) . 1_555 1_555 yes C(44) C(43) C(46) 103(1) . 1_555 1_555 yes C(45) C(43) C(46) 105(1) . 1_555 1_555 yes C(38) C(47) C(48) 109(1) . 1_555 1_555 yes C(38) C(47) C(49) 116(1) . 1_555 1_555 yes C(38) C(47) C(50) 108(1) . 1_555 1_555 yes C(48) C(47) C(49) 105(1) . 1_555 1_555 yes C(48) C(47) C(50) 107(1) . 1_555 1_555 yes C(49) C(47) C(50) 110(1) . 1_555 1_555 yes N(3) C(51) C(52) 113(1) . 1_555 1_555 yes N(3) C(51) C(53) 115.0(10) . 1_555 1_555 yes C(52) C(51) C(53) 113(1) . 1_555 1_555 yes N(3) C(54) C(55) 110.5(9) . 1_555 1_555 yes N(3) C(54) C(56) 114.4(10) . 1_555 1_555 yes C(55) C(54) C(56) 110.0(9) . 1_555 1_555 yes N(4) C(57) C(58) 113(1) . 1_555 1_555 yes N(4) C(57) C(59) 116(1) . 1_555 1_555 yes C(58) C(57) C(59) 109(1) . 1_555 1_555 yes N(4) C(60) C(61) 112(1) . 1_555 1_555 yes N(4) C(60) C(62) 115(1) . 1_555 1_555 yes C(61) C(60) C(62) 108(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Cl(1) C(1) P(1) C(2) -1.7(8) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) S(1) -178.3(5) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) N(1) -56.1(6) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) N(2) 57.7(7) 1_555 1_555 1_555 1_555 yes Cl(2) C(32) P(3) C(33) -0.1(8) 1_555 1_555 1_555 1_555 yes Cl(2) C(32) P(4) S(2) 175.8(5) 1_555 1_555 1_555 1_555 yes Cl(2) C(32) P(4) N(3) -60.1(7) 1_555 1_555 1_555 1_555 yes Cl(2) C(32) P(4) N(4) 52.2(7) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(1) C(20) 81.6(8) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(1) C(23) -73.2(8) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(2) C(26) 174.0(6) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(2) C(29) -11.2(10) 1_555 1_555 1_555 1_555 yes S(1) P(2) C(1) P(1) 2.6(6) 1_555 1_555 1_555 1_555 yes S(2) P(4) N(3) C(51) 12(1) 1_555 1_555 1_555 1_555 yes S(2) P(4) N(3) C(54) -177.0(7) 1_555 1_555 1_555 1_555 yes S(2) P(4) N(4) C(57) -80.2(8) 1_555 1_555 1_555 1_555 yes S(2) P(4) N(4) C(60) 72.9(8) 1_555 1_555 1_555 1_555 yes S(2) P(4) C(32) P(3) -5.8(7) 1_555 1_555 1_555 1_555 yes P(1) C(1) P(2) N(1) 124.7(6) 1_555 1_555 1_555 1_555 yes P(1) C(1) P(2) N(2) -121.4(6) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(3) C(4) -161(1) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(3) C(8) 22(1) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(7) C(6) 160.1(10) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(7) C(16) -19(1) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(20) C(21) -99(1) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(20) C(22) 128.7(9) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(23) C(24) 83(1) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(23) C(25) -147.0(8) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(26) C(27) 109.9(9) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(26) C(28) -126.1(8) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(29) C(30) -61(1) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(29) C(31) 72(1) 1_555 1_555 1_555 1_555 yes P(2) C(1) P(1) C(2) 177.3(6) 1_555 1_555 1_555 1_555 yes P(3) C(32) P(4) N(3) 118.4(6) 1_555 1_555 1_555 1_555 yes P(3) C(32) P(4) N(4) -129.3(6) 1_555 1_555 1_555 1_555 yes P(3) C(33) C(34) C(35) -162(1) 1_555 1_555 1_555 1_555 yes P(3) C(33) C(34) C(39) 14(1) 1_555 1_555 1_555 1_555 yes P(3) C(33) C(38) C(37) 165(1) 1_555 1_555 1_555 1_555 yes P(3) C(33) C(38) C(47) -16(1) 1_555 1_555 1_555 1_555 yes P(4) N(3) C(51) C(52) -73(1) 1_555 1_555 1_555 1_555 yes P(4) N(3) C(51) C(53) 59(1) 1_555 1_555 1_555 1_555 yes P(4) N(3) C(54) C(55) 126.6(8) 1_555 1_555 1_555 1_555 yes P(4) N(3) C(54) C(56) -108.6(10) 1_555 1_555 1_555 1_555 yes P(4) N(4) C(57) C(58) -135.3(10) 1_555 1_555 1_555 1_555 yes P(4) N(4) C(57) C(59) 96(1) 1_555 1_555 1_555 1_555 yes P(4) N(4) C(60) C(61) 147.7(9) 1_555 1_555 1_555 1_555 yes P(4) N(4) C(60) C(62) -86(1) 1_555 1_555 1_555 1_555 yes P(4) C(32) P(3) C(33) -178.4(6) 1_555 1_555 1_555 1_555 yes N(1) P(2) N(2) C(26) 46.1(9) 1_555 1_555 1_555 1_555 yes N(1) P(2) N(2) C(29) -139.2(9) 1_555 1_555 1_555 1_555 yes N(2) P(2) N(1) C(20) -151.4(8) 1_555 1_555 1_555 1_555 yes N(2) P(2) N(1) C(23) 53.9(9) 1_555 1_555 1_555 1_555 yes N(3) P(4) N(4) C(57) 153.0(8) 1_555 1_555 1_555 1_555 yes N(3) P(4) N(4) C(60) -53.9(9) 1_555 1_555 1_555 1_555 yes N(4) P(4) N(3) C(51) 140.5(9) 1_555 1_555 1_555 1_555 yes N(4) P(4) N(3) C(54) -48.7(9) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(2) C(3) 86(1) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(2) C(7) -85(1) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(1) C(20) -34.2(9) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(1) C(23) 171.0(8) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(2) C(26) -66.6(9) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(2) C(29) 108.2(9) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -1(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(9) -98(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(10) 21(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(11) 141(1) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(6) C(5) 4(2) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(17) -26(1) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(18) 94(1) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(19) -145(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(6) -11(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(16) 169(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -5(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(12) 171(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(7) 10(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(9) 85(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(10) -155(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(11) -35(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 3(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(13) -60(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(14) 62(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(15) 174(2) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(8) 174(1) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(16) -175(1) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(13) 115(2) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(14) -120(2) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(15) -9(2) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(17) 154(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(18) -84(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(19) 35(1) 1_555 1_555 1_555 1_555 yes C(7) C(2) C(3) C(8) -166(1) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(12) -173(1) 1_555 1_555 1_555 1_555 yes C(20) N(1) C(23) C(24) -70(1) 1_555 1_555 1_555 1_555 yes C(20) N(1) C(23) C(25) 58(1) 1_555 1_555 1_555 1_555 yes C(21) C(20) N(1) C(23) 54(1) 1_555 1_555 1_555 1_555 yes C(22) C(20) N(1) C(23) -77(1) 1_555 1_555 1_555 1_555 yes C(26) N(2) C(29) C(30) 113(1) 1_555 1_555 1_555 1_555 yes C(26) N(2) C(29) C(31) -112(1) 1_555 1_555 1_555 1_555 yes C(27) C(26) N(2) C(29) -65(1) 1_555 1_555 1_555 1_555 yes C(28) C(26) N(2) C(29) 58(1) 1_555 1_555 1_555 1_555 yes C(32) P(3) C(33) C(34) 89(1) 1_555 1_555 1_555 1_555 yes C(32) P(3) C(33) C(38) -87(1) 1_555 1_555 1_555 1_555 yes C(32) P(4) N(3) C(51) -107.8(10) 1_555 1_555 1_555 1_555 yes C(32) P(4) N(3) C(54) 63.1(9) 1_555 1_555 1_555 1_555 yes C(32) P(4) N(4) C(57) 36.9(9) 1_555 1_555 1_555 1_555 yes C(32) P(4) N(4) C(60) -170.0(8) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) -5(2) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(39) C(40) -85(1) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(39) C(41) 37(2) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(39) C(42) 154(1) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(37) C(36) 0(2) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(47) C(48) -138(1) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(47) C(49) -19(2) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(47) C(50) 105(1) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(38) C(37) -11(2) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(38) C(47) 165(1) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) -6(2) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(43) 178(1) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(33) C(38) 14(2) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(39) C(40) 91(1) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(39) C(41) -145(1) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(39) C(42) -28(2) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 9(2) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(43) C(44) -70(2) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(43) C(45) 56(2) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(43) C(46) 174(1) 1_555 1_555 1_555 1_555 yes C(36) C(35) C(34) C(39) 177(1) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(47) -178(1) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(43) C(44) 114(2) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(43) C(45) -118(1) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(43) C(46) 0(2) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(47) C(48) 39(1) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(47) C(49) 158(1) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(47) C(50) -77(1) 1_555 1_555 1_555 1_555 yes C(38) C(33) C(34) C(39) -168(1) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(43) -175(1) 1_555 1_555 1_555 1_555 yes C(51) N(3) C(54) C(55) -61(1) 1_555 1_555 1_555 1_555 yes C(51) N(3) C(54) C(56) 62(1) 1_555 1_555 1_555 1_555 yes C(52) C(51) N(3) C(54) 115(1) 1_555 1_555 1_555 1_555 yes C(53) C(51) N(3) C(54) -111(1) 1_555 1_555 1_555 1_555 yes C(57) N(4) C(60) C(61) -60(1) 1_555 1_555 1_555 1_555 yes C(57) N(4) C(60) C(62) 64(1) 1_555 1_555 1_555 1_555 yes C(58) C(57) N(4) C(60) 73(1) 1_555 1_555 1_555 1_555 yes C(59) C(57) N(4) C(60) -54(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) C(54) 3.54(1) . 1_655 ? S(2) C(26) 3.54(1) . 1_556 ? #------------------------------------------------------------------------------ data_pt _database_code_CSD 206704 _audit_creation_date 'Fri Oct 18 13:03:13 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C31 H57 Cl3 N2 P2 Pt S ' _chemical_formula_moiety 'C31 H57 Cl3 N2 P2 Pt S ' _chemical_formula_weight 853.26 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 11.0215(6) _cell_length_b 21.108(1) _cell_length_c 16.2925(5) _cell_angle_alpha 90 _cell_angle_beta 92.524(2) _cell_angle_gamma 90 _cell_volume 3786.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16504 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.3 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour unknown _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.233 _exptl_absorpt_correction_T_max 0.362 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17979 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 25.34 _diffrn_measured_fraction_theta_max 0.9144 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.9144 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6348 _reflns_number_gt 5429 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0542 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5429 _refine_ls_number_parameters 361 _refine_ls_goodness_of_fit_ref 1.571 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0039 _refine_diff_density_max 1.16 _refine_diff_density_min -2.05 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt 0.99020(2) 0.06204(1) 0.23646(2) 0.03909(8) Uani 1.00 d . . . Cl(1) Cl 1.3862(1) -0.04443(8) 0.2769(1) 0.0502(5) Uani 1.00 d . . . Cl(2) Cl 0.8546(2) 0.14665(9) 0.2319(2) 0.0822(7) Uani 1.00 d . . . Cl(3) Cl 0.8368(2) -0.00555(10) 0.1892(2) 0.0761(7) Uani 1.00 d . . . S(1) S 1.1328(1) 0.13333(7) 0.2869(1) 0.0423(4) Uani 1.00 d . . . P(1) P 1.1235(1) -0.01367(7) 0.24586(9) 0.0318(4) Uani 1.00 d . . . P(2) P 1.2976(1) 0.09265(7) 0.26795(9) 0.0292(4) Uani 1.00 d . . . N(1) N 1.3923(5) 0.1137(3) 0.3433(3) 0.044(1) Uani 1.00 d . . . N(2) N 1.3557(4) 0.1127(2) 0.1810(3) 0.031(1) Uani 1.00 d . . . C(1) C 1.2674(5) 0.0084(3) 0.2638(3) 0.031(1) Uani 1.00 d . . . C(2) C 1.1123(5) -0.0994(2) 0.2395(3) 0.029(1) Uani 1.00 d . . . C(3) C 1.1010(5) -0.1360(3) 0.3125(3) 0.037(2) Uani 1.00 d . . . C(4) C 1.1169(6) -0.2012(3) 0.3058(4) 0.040(2) Uani 1.00 d . . . C(5) C 1.1401(5) -0.2325(3) 0.2332(4) 0.037(2) Uani 1.00 d . . . C(6) C 1.1415(5) -0.1955(3) 0.1641(3) 0.038(2) Uani 1.00 d . . . C(7) C 1.1290(5) -0.1300(3) 0.1638(3) 0.032(1) Uani 1.00 d . . . C(8) C 1.0724(7) -0.1109(3) 0.3993(4) 0.051(2) Uani 1.00 d . . . C(9) C 1.189(1) -0.0923(8) 0.4438(6) 0.156(6) Uani 1.00 d . . . C(10) C 0.989(1) -0.0547(5) 0.3983(7) 0.115(5) Uani 1.00 d . . . C(11) C 1.008(1) -0.1609(4) 0.4494(6) 0.096(4) Uani 1.00 d . . . C(12) C 1.1593(7) -0.3042(3) 0.2273(4) 0.053(2) Uani 1.00 d . . . C(13) C 1.145(1) -0.3390(4) 0.3067(5) 0.093(3) Uani 1.00 d . . . C(14) C 1.066(1) -0.3319(4) 0.1663(5) 0.097(4) Uani 1.00 d . . . C(15) C 1.2817(9) -0.3167(4) 0.1922(8) 0.117(4) Uani 1.00 d . . . C(16) C 1.1328(6) -0.1016(3) 0.0755(4) 0.042(2) Uani 1.00 d . . . C(17) C 1.0299(9) -0.1313(4) 0.0211(4) 0.078(3) Uani 1.00 d . . . C(18) C 1.2558(8) -0.1157(5) 0.0397(6) 0.085(3) Uani 1.00 d . . . C(19) C 1.1145(8) -0.0305(3) 0.0683(4) 0.062(2) Uani 1.00 d . . . C(20) C 1.5261(6) 0.1223(4) 0.3290(5) 0.058(2) Uani 1.00 d . . . C(21) C 1.6038(8) 0.0702(5) 0.3686(7) 0.085(3) Uani 1.00 d . . . C(22) C 1.5737(8) 0.1867(4) 0.3567(6) 0.081(3) Uani 1.00 d . . . C(23) C 1.3541(9) 0.1226(5) 0.4300(5) 0.077(3) Uani 1.00 d . . . C(24) C 1.3047(9) 0.1874(5) 0.4467(5) 0.088(3) Uani 1.00 d . . . C(25) C 1.316(2) 0.0708(6) 0.4706(8) 0.196(8) Uani 1.00 d . . . C(26) C 1.3604(6) 0.1832(3) 0.1654(4) 0.044(2) Uani 1.00 d . . . C(27) C 1.2577(7) 0.2071(4) 0.1098(5) 0.065(2) Uani 1.00 d . . . C(28) C 1.4835(7) 0.2066(4) 0.1379(5) 0.065(2) Uani 1.00 d . . . C(29) C 1.3955(7) 0.0656(3) 0.1205(5) 0.053(2) Uani 1.00 d . . . C(30) C 1.5338(9) 0.0526(4) 0.1289(7) 0.089(4) Uani 1.00 d . . . C(31) C 1.348(1) 0.0797(4) 0.0325(5) 0.084(3) Uani 1.00 d . . . H(1) H 1.1080 -0.2268 0.3549 0.0501 Uiso 1.00 calc . . . H(2) H 1.1533 -0.2159 0.1116 0.0453 Uiso 1.00 calc . . . H(3) H 1.1806 -0.0802 0.4980 0.1854 Uiso 1.00 calc . . . H(4) H 1.2429 -0.1327 0.4483 0.1854 Uiso 1.00 calc . . . H(5) H 1.2357 -0.0640 0.4146 0.1854 Uiso 1.00 calc . . . H(6) H 0.9681 -0.0402 0.4499 0.1355 Uiso 1.00 calc . . . H(7) H 1.0169 -0.0204 0.3658 0.1355 Uiso 1.00 calc . . . H(8) H 0.9086 -0.0671 0.3692 0.1355 Uiso 1.00 calc . . . H(9) H 0.9893 -0.1430 0.5027 0.1223 Uiso 1.00 calc . . . H(10) H 1.0530 -0.1972 0.4569 0.1223 Uiso 1.00 calc . . . H(11) H 0.9300 -0.1705 0.4223 0.1223 Uiso 1.00 calc . . . H(12) H 1.2067 -0.3245 0.3474 0.1052 Uiso 1.00 calc . . . H(13) H 1.0684 -0.3311 0.3272 0.1052 Uiso 1.00 calc . . . H(14) H 1.1569 -0.3832 0.2996 0.1052 Uiso 1.00 calc . . . H(15) H 0.9818 -0.3232 0.1858 0.1131 Uiso 1.00 calc . . . H(16) H 1.0705 -0.3751 0.1579 0.1131 Uiso 1.00 calc . . . H(17) H 1.0653 -0.3101 0.1135 0.1131 Uiso 1.00 calc . . . H(18) H 1.3025 -0.3601 0.1905 0.1254 Uiso 1.00 calc . . . H(19) H 1.2918 -0.2973 0.1412 0.1254 Uiso 1.00 calc . . . H(20) H 1.3481 -0.2972 0.2302 0.1254 Uiso 1.00 calc . . . H(21) H 1.0361 -0.0184 0.0894 0.0714 Uiso 1.00 calc . . . H(22) H 1.1751 -0.0075 0.1002 0.0714 Uiso 1.00 calc . . . H(23) H 1.1150 -0.0160 0.0129 0.0714 Uiso 1.00 calc . . . H(24) H 0.9498 -0.1195 0.0415 0.0949 Uiso 1.00 calc . . . H(25) H 1.0322 -0.1766 0.0216 0.0949 Uiso 1.00 calc . . . H(26) H 1.0294 -0.1173 -0.0347 0.0949 Uiso 1.00 calc . . . H(27) H 1.2722 -0.1610 0.0412 0.1010 Uiso 1.00 calc . . . H(28) H 1.2560 -0.1037 -0.0180 0.1010 Uiso 1.00 calc . . . H(29) H 1.3203 -0.0947 0.0679 0.1010 Uiso 1.00 calc . . . H(30) H 1.5360 0.1188 0.2696 0.0751 Uiso 1.00 calc . . . H(31) H 1.5963 0.0729 0.4276 0.0986 Uiso 1.00 calc . . . H(32) H 1.5766 0.0298 0.3511 0.0986 Uiso 1.00 calc . . . H(33) H 1.6867 0.0756 0.3573 0.0986 Uiso 1.00 calc . . . H(34) H 1.5672 0.1916 0.4135 0.0953 Uiso 1.00 calc . . . H(35) H 1.5320 0.2200 0.3280 0.0953 Uiso 1.00 calc . . . H(36) H 1.6597 0.1905 0.3444 0.0953 Uiso 1.00 calc . . . H(37) H 1.4301 0.1247 0.4598 0.0896 Uiso 1.00 calc . . . H(38) H 1.3570 0.2194 0.4257 0.0997 Uiso 1.00 calc . . . H(39) H 1.2961 0.1940 0.5033 0.0997 Uiso 1.00 calc . . . H(40) H 1.2261 0.1923 0.4186 0.0997 Uiso 1.00 calc . . . H(41) H 1.2918 0.0776 0.5229 0.1291 Uiso 1.00 calc . . . H(42) H 1.2203 0.0642 0.4406 0.1291 Uiso 1.00 calc . . . H(43) H 1.3470 0.0338 0.4578 0.1291 Uiso 1.00 calc . . . H(44) H 1.3504 0.2033 0.2192 0.0562 Uiso 1.00 calc . . . H(45) H 1.1795 0.1952 0.1297 0.0792 Uiso 1.00 calc . . . H(46) H 1.2625 0.1892 0.0557 0.0792 Uiso 1.00 calc . . . H(47) H 1.2580 0.2523 0.1043 0.0792 Uiso 1.00 calc . . . H(48) H 1.5001 0.1878 0.0862 0.0771 Uiso 1.00 calc . . . H(49) H 1.4855 0.2512 0.1331 0.0771 Uiso 1.00 calc . . . H(50) H 1.5480 0.1937 0.1769 0.0771 Uiso 1.00 calc . . . H(51) H 1.3582 0.0257 0.1350 0.0646 Uiso 1.00 calc . . . H(52) H 1.5562 0.0398 0.1823 0.1063 Uiso 1.00 calc . . . H(53) H 1.5753 0.0899 0.1144 0.1063 Uiso 1.00 calc . . . H(54) H 1.5532 0.0195 0.0907 0.1063 Uiso 1.00 calc . . . H(55) H 1.3855 0.1196 0.0136 0.1058 Uiso 1.00 calc . . . H(56) H 1.3703 0.0479 -0.0057 0.1058 Uiso 1.00 calc . . . H(57) H 1.2633 0.0859 0.0288 0.1058 Uiso 1.00 calc . . . 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) 0.0279(1) 0.0250(1) 0.0648(2) 0.00387(9) 0.0067(1) 0.0046(1) Cl(1) 0.0349(8) 0.0341(8) 0.081(1) 0.0116(6) -0.0013(8) 0.0002(8) Cl(2) 0.0455(10) 0.040(1) 0.162(2) 0.0206(8) 0.020(1) 0.016(1) Cl(3) 0.0385(9) 0.053(1) 0.135(2) -0.0055(8) -0.018(1) -0.002(1) S(1) 0.0349(8) 0.0268(8) 0.066(1) 0.0004(6) 0.0169(7) -0.0105(7) P(1) 0.0290(7) 0.0204(7) 0.0457(8) 0.0021(6) 0.0010(6) -0.0010(6) P(2) 0.0282(7) 0.0238(7) 0.0358(8) 0.0003(6) 0.0049(6) -0.0042(6) N(1) 0.043(3) 0.045(3) 0.042(3) -0.010(2) 0.002(2) -0.007(2) N(2) 0.035(2) 0.027(2) 0.031(2) 0.002(2) 0.010(2) -0.001(2) C(1) 0.025(3) 0.023(3) 0.046(3) 0.003(2) 0.006(2) 0.000(2) C(2) 0.027(3) 0.022(3) 0.038(3) -0.002(2) 0.003(2) 0.000(2) C(3) 0.040(3) 0.034(3) 0.035(3) -0.001(2) -0.005(3) -0.006(2) C(4) 0.050(4) 0.027(3) 0.044(3) -0.004(3) 0.001(3) 0.008(3) C(5) 0.039(3) 0.028(3) 0.044(3) 0.000(2) -0.001(3) -0.003(2) C(6) 0.046(3) 0.029(3) 0.038(3) 0.003(3) -0.002(3) -0.004(2) C(7) 0.032(3) 0.030(3) 0.034(3) 0.000(2) -0.003(2) 0.004(2) C(8) 0.066(5) 0.043(4) 0.043(4) -0.009(3) 0.009(3) 0.000(3) C(9) 0.096(9) 0.31(2) 0.058(6) -0.06(1) -0.002(6) -0.065(9) C(10) 0.20(1) 0.076(7) 0.075(7) 0.048(7) 0.072(8) 0.006(5) C(11) 0.16(1) 0.058(6) 0.073(6) 0.010(6) 0.064(6) 0.013(5) C(12) 0.067(5) 0.024(3) 0.068(4) 0.002(3) 0.007(4) -0.002(3) C(13) 0.18(1) 0.038(4) 0.064(5) 0.010(6) -0.003(6) 0.008(4) C(14) 0.18(1) 0.042(5) 0.071(6) -0.029(6) -0.006(6) -0.012(4) C(15) 0.094(7) 0.042(5) 0.22(1) 0.027(5) 0.061(8) 0.011(7) C(16) 0.049(4) 0.043(4) 0.034(3) 0.001(3) 0.002(3) 0.008(3) C(17) 0.117(7) 0.066(5) 0.047(4) -0.028(5) -0.025(4) 0.008(4) C(18) 0.083(6) 0.090(7) 0.084(6) 0.013(5) 0.037(5) 0.034(5) C(19) 0.098(6) 0.049(4) 0.036(3) -0.007(4) -0.018(4) 0.014(3) C(20) 0.045(4) 0.065(5) 0.064(4) -0.013(3) -0.005(3) -0.008(4) C(21) 0.054(5) 0.097(8) 0.101(7) -0.004(4) -0.026(5) 0.009(5) C(22) 0.066(5) 0.079(6) 0.098(6) -0.033(5) -0.011(5) -0.009(5) C(23) 0.100(7) 0.088(7) 0.041(4) 0.005(5) -0.001(4) -0.009(4) C(24) 0.117(8) 0.083(7) 0.065(5) -0.013(6) 0.024(5) -0.042(5) C(25) 0.43(3) 0.080(9) 0.088(9) -0.06(1) 0.15(1) -0.019(6) C(26) 0.045(3) 0.031(3) 0.055(4) -0.005(3) 0.008(3) 0.004(3) C(27) 0.068(5) 0.044(4) 0.082(5) 0.002(4) 0.009(4) 0.017(4) C(28) 0.061(5) 0.060(5) 0.075(5) -0.022(4) 0.021(4) 0.019(4) C(29) 0.060(5) 0.044(4) 0.057(4) 0.004(3) 0.031(4) -0.011(3) C(30) 0.073(6) 0.074(6) 0.126(9) 0.015(5) 0.065(6) -0.004(5) C(31) 0.145(9) 0.067(6) 0.042(4) -0.004(6) 0.027(5) -0.005(4) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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) Cl(2) 2.328(2) . . yes Pt(1) Cl(3) 2.318(2) . . yes Pt(1) S(1) 2.301(2) . . yes Pt(1) P(1) 2.172(1) . . yes Cl(1) C(1) 1.726(5) . . yes S(1) P(2) 2.046(2) . . yes P(1) C(1) 1.666(5) . . yes P(1) C(2) 1.816(5) . . yes P(2) N(1) 1.638(5) . . yes P(2) N(2) 1.636(5) . . yes P(2) C(1) 1.810(6) . . yes N(1) C(20) 1.514(8) . . yes N(1) C(23) 1.503(9) . . yes N(2) C(26) 1.510(7) . . yes N(2) C(29) 1.479(8) . . yes C(2) C(3) 1.430(8) . . yes C(2) C(7) 1.411(8) . . yes C(3) C(4) 1.392(8) . . yes C(3) C(8) 1.555(9) . . yes C(4) C(5) 1.388(8) . . yes C(5) C(6) 1.371(8) . . yes C(5) C(12) 1.534(8) . . yes C(6) C(7) 1.388(8) . . yes C(7) C(16) 1.561(8) . . yes C(8) C(9) 1.50(1) . . yes C(8) C(10) 1.50(1) . . yes C(8) C(11) 1.53(1) . . yes C(12) C(13) 1.50(1) . . yes C(12) C(14) 1.52(1) . . yes C(12) C(15) 1.51(1) . . yes C(16) C(17) 1.540(9) . . yes C(16) C(18) 1.53(1) . . yes C(16) C(19) 1.519(10) . . yes C(20) C(21) 1.52(1) . . yes C(20) C(22) 1.52(1) . . yes C(23) C(24) 1.50(1) . . yes C(23) C(25) 1.36(1) . . yes C(26) C(27) 1.505(10) . . yes C(26) C(28) 1.529(9) . . yes C(29) C(30) 1.55(1) . . yes C(29) C(31) 1.54(1) . . 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 Cl(2) Pt(1) Cl(3) 90.21(7) . 1_555 1_555 yes Cl(2) Pt(1) S(1) 86.38(7) . 1_555 1_555 yes Cl(2) Pt(1) P(1) 176.58(7) . 1_555 1_555 yes Cl(3) Pt(1) S(1) 176.21(6) . 1_555 1_555 yes Cl(3) Pt(1) P(1) 92.98(6) . 1_555 1_555 yes S(1) Pt(1) P(1) 90.39(5) . 1_555 1_555 yes Pt(1) S(1) P(2) 105.60(7) . 1_555 1_555 yes Pt(1) P(1) C(1) 116.2(2) . 1_555 1_555 yes Pt(1) P(1) C(2) 133.2(2) . 1_555 1_555 yes C(1) P(1) C(2) 110.5(2) . 1_555 1_555 yes S(1) P(2) N(1) 108.3(2) . 1_555 1_555 yes S(1) P(2) N(2) 114.0(2) . 1_555 1_555 yes S(1) P(2) C(1) 104.8(2) . 1_555 1_555 yes N(1) P(2) N(2) 108.5(3) . 1_555 1_555 yes N(1) P(2) C(1) 113.9(3) . 1_555 1_555 yes N(2) P(2) C(1) 107.5(2) . 1_555 1_555 yes P(2) N(1) C(20) 120.6(4) . 1_555 1_555 yes P(2) N(1) C(23) 122.8(5) . 1_555 1_555 yes C(20) N(1) C(23) 116.5(6) . 1_555 1_555 yes P(2) N(2) C(26) 114.7(4) . 1_555 1_555 yes P(2) N(2) C(29) 122.8(4) . 1_555 1_555 yes C(26) N(2) C(29) 122.4(5) . 1_555 1_555 yes Cl(1) C(1) P(1) 123.5(3) . 1_555 1_555 yes Cl(1) C(1) P(2) 119.5(3) . 1_555 1_555 yes P(1) C(1) P(2) 117.0(3) . 1_555 1_555 yes P(1) C(2) C(3) 120.0(4) . 1_555 1_555 yes P(1) C(2) C(7) 119.7(4) . 1_555 1_555 yes C(3) C(2) C(7) 119.9(5) . 1_555 1_555 yes C(2) C(3) C(4) 117.0(5) . 1_555 1_555 yes C(2) C(3) C(8) 126.9(5) . 1_555 1_555 yes C(4) C(3) C(8) 116.1(5) . 1_555 1_555 yes C(3) C(4) C(5) 124.4(5) . 1_555 1_555 yes C(4) C(5) C(6) 116.0(5) . 1_555 1_555 yes C(4) C(5) C(12) 123.6(6) . 1_555 1_555 yes C(6) C(5) C(12) 120.3(5) . 1_555 1_555 yes C(5) C(6) C(7) 124.4(5) . 1_555 1_555 yes C(2) C(7) C(6) 118.0(5) . 1_555 1_555 yes C(2) C(7) C(16) 129.7(5) . 1_555 1_555 yes C(6) C(7) C(16) 112.3(5) . 1_555 1_555 yes C(3) C(8) C(9) 108.9(7) . 1_555 1_555 yes C(3) C(8) C(10) 114.1(6) . 1_555 1_555 yes C(3) C(8) C(11) 111.5(6) . 1_555 1_555 yes C(9) C(8) C(10) 108.0(9) . 1_555 1_555 yes C(9) C(8) C(11) 109.3(8) . 1_555 1_555 yes C(10) C(8) C(11) 104.8(7) . 1_555 1_555 yes C(5) C(12) C(13) 114.2(6) . 1_555 1_555 yes C(5) C(12) C(14) 109.2(6) . 1_555 1_555 yes C(5) C(12) C(15) 108.9(6) . 1_555 1_555 yes C(13) C(12) C(14) 106.6(7) . 1_555 1_555 yes C(13) C(12) C(15) 111.6(8) . 1_555 1_555 yes C(14) C(12) C(15) 106.0(8) . 1_555 1_555 yes C(7) C(16) C(17) 109.0(5) . 1_555 1_555 yes C(7) C(16) C(18) 109.7(5) . 1_555 1_555 yes C(7) C(16) C(19) 116.3(5) . 1_555 1_555 yes C(17) C(16) C(18) 110.1(7) . 1_555 1_555 yes C(17) C(16) C(19) 105.4(5) . 1_555 1_555 yes C(18) C(16) C(19) 106.2(6) . 1_555 1_555 yes N(1) C(20) C(21) 112.4(7) . 1_555 1_555 yes N(1) C(20) C(22) 112.8(7) . 1_555 1_555 yes C(21) C(20) C(22) 109.9(6) . 1_555 1_555 yes N(1) C(23) C(24) 113.8(7) . 1_555 1_555 yes N(1) C(23) C(25) 117.7(8) . 1_555 1_555 yes C(24) C(23) C(25) 121(1) . 1_555 1_555 yes N(2) C(26) C(27) 113.7(5) . 1_555 1_555 yes N(2) C(26) C(28) 113.8(5) . 1_555 1_555 yes C(27) C(26) C(28) 111.6(6) . 1_555 1_555 yes N(2) C(29) C(30) 112.3(6) . 1_555 1_555 yes N(2) C(29) C(31) 113.1(6) . 1_555 1_555 yes C(30) C(29) C(31) 114.3(7) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Pt(1) S(1) P(2) N(1) -146.6(2) 1_555 1_555 1_555 1_555 yes Pt(1) S(1) P(2) N(2) 92.5(2) 1_555 1_555 1_555 1_555 yes Pt(1) S(1) P(2) C(1) -24.7(2) 1_555 1_555 1_555 1_555 yes Pt(1) P(1) C(1) Cl(1) 177.6(3) 1_555 1_555 1_555 1_555 yes Pt(1) P(1) C(1) P(2) -3.2(4) 1_555 1_555 1_555 1_555 yes Pt(1) P(1) C(2) C(3) -92.8(4) 1_555 1_555 1_555 1_555 yes Pt(1) P(1) C(2) C(7) 94.5(5) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(1) C(2) -1.7(5) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) S(1) -162.2(3) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) N(1) -44.0(4) 1_555 1_555 1_555 1_555 yes Cl(1) C(1) P(2) N(2) 76.3(4) 1_555 1_555 1_555 1_555 yes Cl(2) Pt(1) S(1) P(2) -160.8(1) 1_555 1_555 1_555 1_555 yes Cl(2) Pt(1) P(1) C(1) -30(1) 1_555 1_555 1_555 1_555 yes Cl(2) Pt(1) P(1) C(2) 148(1) 1_555 1_555 1_555 1_555 yes Cl(3) Pt(1) S(1) P(2) 173(1) 1_555 1_555 1_555 1_555 yes Cl(3) Pt(1) P(1) C(1) 170.0(2) 1_555 1_555 1_555 1_555 yes Cl(3) Pt(1) P(1) C(2) -10.9(3) 1_555 1_555 1_555 1_555 yes S(1) Pt(1) P(1) C(1) -11.7(2) 1_555 1_555 1_555 1_555 yes S(1) Pt(1) P(1) C(2) 167.4(3) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(1) C(20) -147.7(5) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(1) C(23) 35.1(6) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(2) C(26) 51.1(4) 1_555 1_555 1_555 1_555 yes S(1) P(2) N(2) C(29) -126.2(5) 1_555 1_555 1_555 1_555 yes S(1) P(2) C(1) P(1) 18.6(4) 1_555 1_555 1_555 1_555 yes P(1) Pt(1) S(1) P(2) 20.37(9) 1_555 1_555 1_555 1_555 yes P(1) C(1) P(2) N(1) 136.8(3) 1_555 1_555 1_555 1_555 yes P(1) C(1) P(2) N(2) -102.9(4) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(3) C(4) -167.7(4) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(3) C(8) 12.4(8) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(7) C(6) 168.7(4) 1_555 1_555 1_555 1_555 yes P(1) C(2) C(7) C(16) -13.1(8) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(20) C(21) -108.7(7) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(20) C(22) 126.3(6) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(23) C(24) -85.5(9) 1_555 1_555 1_555 1_555 yes P(2) N(1) C(23) C(25) 65(1) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(26) C(27) -98.8(6) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(26) C(28) 131.9(5) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(29) C(30) -96.9(7) 1_555 1_555 1_555 1_555 yes P(2) N(2) C(29) C(31) 131.8(6) 1_555 1_555 1_555 1_555 yes P(2) C(1) P(1) C(2) 177.5(3) 1_555 1_555 1_555 1_555 yes N(1) P(2) N(2) C(26) -69.6(4) 1_555 1_555 1_555 1_555 yes N(1) P(2) N(2) C(29) 113.1(5) 1_555 1_555 1_555 1_555 yes N(2) P(2) N(1) C(20) -23.5(6) 1_555 1_555 1_555 1_555 yes N(2) P(2) N(1) C(23) 159.3(6) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(2) C(3) 86.3(5) 1_555 1_555 1_555 1_555 yes C(1) P(1) C(2) C(7) -86.3(5) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(1) C(20) 96.2(5) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(1) C(23) -81.0(7) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(2) C(26) 166.7(4) 1_555 1_555 1_555 1_555 yes C(1) P(2) N(2) C(29) -10.6(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -1.5(9) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(9) -87.0(10) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(10) 33(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(8) C(11) 152.3(7) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(6) C(5) -0.8(9) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(17) -119.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(18) 119.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(7) C(16) C(19) -0.8(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(6) -4.0(8) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(7) C(16) 174.3(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -3.0(9) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(12) 179.0(6) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(7) 5.0(8) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(9) 93.1(9) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(10) -146.1(8) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(8) C(11) -27.6(9) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 4.2(9) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(13) 2.6(10) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(14) 121.8(8) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(12) C(15) -122.8(8) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(8) 178.4(6) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(16) -179.3(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(13) -175.3(7) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(14) -56.1(9) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(12) C(15) 59.2(9) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(17) 58.7(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(18) -62.0(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(16) C(19) 177.5(6) 1_555 1_555 1_555 1_555 yes C(7) C(2) C(3) C(8) -174.9(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(12) -177.7(6) 1_555 1_555 1_555 1_555 yes C(20) N(1) C(23) C(24) 97.2(8) 1_555 1_555 1_555 1_555 yes C(20) N(1) C(23) C(25) -111(1) 1_555 1_555 1_555 1_555 yes C(21) C(20) N(1) C(23) 68.6(9) 1_555 1_555 1_555 1_555 yes C(22) C(20) N(1) C(23) -56.4(9) 1_555 1_555 1_555 1_555 yes C(26) N(2) C(29) C(30) 86.0(7) 1_555 1_555 1_555 1_555 yes C(26) N(2) C(29) C(31) -45.3(9) 1_555 1_555 1_555 1_555 yes C(27) C(26) N(2) C(29) 78.5(8) 1_555 1_555 1_555 1_555 yes C(28) C(26) N(2) C(29) -50.8(8) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(19) C(19) 3.53(1) . 3_755 ? C(27) C(28) 3.58(1) . 4_455 ? #------------------------------------------------------------------------------ data_liang _database_code_CSD 206705 _audit_creation_date 'Thu Jan 9 16:53:29 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C34.50 H61 Cl3 N2 P2 Pt S ' _chemical_formula_moiety ? _chemical_formula_weight 899.33 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.7395(7) _cell_length_b 16.5550(5) _cell_length_c 11.8561(6) _cell_angle_alpha 90 _cell_angle_beta 90.060(2) _cell_angle_gamma 90 _cell_volume 4070.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 26620 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.469 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31362 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9797 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9797 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9148 _reflns_number_gt 6989 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.0651 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6989 _refine_ls_number_parameters 377 _refine_ls_goodness_of_fit_ref 1.466 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0141 _refine_diff_density_max 0.88 _refine_diff_density_min -2.80 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt 0.33650(1) 0.02138(2) 0.54656(2) 0.03655(8) Uani 1.00 d . . . Cl(1) Cl 0.3539(1) 0.2896(1) 0.3693(2) 0.0628(6) Uani 1.00 d . . . Cl(2) Cl 0.3175(1) 0.0279(1) 0.7387(2) 0.0694(7) Uani 1.00 d . . . Cl(3) Cl 0.3421(1) -0.1197(1) 0.5552(2) 0.0560(6) Uani 1.00 d . . . S(1) S 0.3564(1) 0.0064(1) 0.3580(2) 0.0475(5) Uani 1.00 d . . . P(1) P 0.32980(9) 0.1536(1) 0.5362(2) 0.0385(5) Uani 1.00 d . . . P(2) P 0.34359(9) 0.1159(1) 0.2844(2) 0.0386(5) Uani 1.00 d . . . N(1) N 0.2688(3) 0.1301(4) 0.2405(6) 0.049(2) Uani 1.00 d . . . N(2) N 0.3939(3) 0.1301(4) 0.1792(5) 0.049(2) Uani 1.00 d . . . C(1) C 0.3659(4) 0.1853(4) 0.3988(6) 0.044(2) Uani 1.00 d . . . C(2) C 0.3600(3) 0.2247(4) 0.6413(6) 0.040(2) Uani 1.00 d . . . C(3) C 0.4223(3) 0.2391(4) 0.6838(6) 0.042(2) Uani 1.00 d . . . C(4) C 0.4273(4) 0.3008(5) 0.7648(7) 0.050(2) Uani 1.00 d . . . C(5) C 0.3753(4) 0.3454(4) 0.8064(8) 0.054(2) Uani 1.00 d . . . C(6) C 0.3151(4) 0.3291(5) 0.7611(7) 0.051(2) Uani 1.00 d . . . C(7) C 0.3067(3) 0.2705(4) 0.6804(6) 0.041(2) Uani 1.00 d . . . C(8) C 0.4860(3) 0.1987(5) 0.6493(7) 0.050(2) Uani 1.00 d . . . C(9) C 0.4787(4) 0.1140(5) 0.6055(8) 0.059(3) Uani 1.00 d . . . C(10) C 0.5185(5) 0.2525(6) 0.5614(10) 0.077(3) Uani 1.00 d . . . C(11) C 0.5326(4) 0.1898(7) 0.7514(10) 0.085(4) Uani 1.00 d . . . C(12) C 0.3837(5) 0.4086(6) 0.8986(10) 0.075(3) Uani 1.00 d . . . C(13) C 0.3611(9) 0.4887(7) 0.857(2) 0.139(7) Uani 1.00 d . . . C(14) C 0.4529(5) 0.4143(8) 0.941(1) 0.129(5) Uani 1.00 d . . . C(15) C 0.3407(6) 0.3858(10) 1.002(1) 0.121(6) Uani 1.00 d . . . C(16) C 0.2394(4) 0.2520(4) 0.6356(6) 0.046(2) Uani 1.00 d . . . C(17) C 0.1989(4) 0.2129(7) 0.7288(8) 0.071(3) Uani 1.00 d . . . C(18) C 0.2053(5) 0.3277(6) 0.5950(10) 0.086(4) Uani 1.00 d . . . C(19) C 0.2475(3) 0.1921(4) 0.5365(6) 0.044(2) Uani 1.00 d . . . C(20) C 0.2185(5) 0.0674(5) 0.2705(9) 0.069(3) Uani 1.00 d . . . C(21) C 0.1540(5) 0.1010(8) 0.2985(10) 0.085(4) Uani 1.00 d . . . C(22) C 0.2168(6) -0.0008(6) 0.182(1) 0.089(4) Uani 1.00 d . . . C(23) C 0.2547(4) 0.2005(5) 0.1649(7) 0.053(2) Uani 1.00 d . . . C(24) C 0.2147(5) 0.2675(6) 0.2199(8) 0.069(3) Uani 1.00 d . . . C(25) C 0.2232(6) 0.1776(6) 0.0538(9) 0.089(4) Uani 1.00 d . . . C(26) C 0.4638(5) 0.1481(8) 0.194(1) 0.086(4) Uani 1.00 d . . . C(27) C 0.5038(6) 0.094(1) 0.255(1) 0.131(6) Uani 1.00 d . . . C(28) C 0.4821(6) 0.2329(8) 0.196(1) 0.118(5) Uani 1.00 d . . . C(29) C 0.3760(5) 0.0913(6) 0.0697(7) 0.069(3) Uani 1.00 d . . . C(30) C 0.4037(7) 0.0057(8) 0.054(1) 0.096(4) Uani 1.00 d . . . C(31) C 0.3876(7) 0.1457(9) -0.0295(9) 0.118(5) Uani 1.00 d . . . C(32) C 0.543(3) 0.495(3) 0.558(5) 0.35(1) Uiso 1.00 d . . . C(33) C 0.506(3) 0.531(3) 0.616(4) 0.32(1) Uiso 1.00 d . . . C(34) C 0.431(5) 0.561(6) 0.593(9) 0.400(7) Uiso 0.50 d P . . C(35) C 0.446(3) 0.484(2) 0.535(5) 0.35(1) Uiso 1.00 d . . . H(1) H 0.4120 0.1794 0.4086 0.0529 Uiso 1.00 calc . . . H(2) H 0.4778 0.3045 0.8001 0.0708 Uiso 1.00 calc . . . H(3) H 0.2792 0.3607 0.7959 0.0708 Uiso 1.00 calc . . . H(4) H 0.4602 0.0794 0.6619 0.0665 Uiso 1.00 calc . . . H(5) H 0.4502 0.1125 0.5407 0.0665 Uiso 1.00 calc . . . H(6) H 0.5190 0.0916 0.5829 0.0665 Uiso 1.00 calc . . . H(7) H 0.4923 0.2602 0.4967 0.0883 Uiso 1.00 calc . . . H(8) H 0.5591 0.2299 0.5378 0.0883 Uiso 1.00 calc . . . H(9) H 0.5278 0.3051 0.5933 0.0883 Uiso 1.00 calc . . . H(10) H 0.5728 0.1678 0.7272 0.1007 Uiso 1.00 calc . . . H(11) H 0.5405 0.2418 0.7841 0.1007 Uiso 1.00 calc . . . H(12) H 0.5142 0.1556 0.8066 0.1007 Uiso 1.00 calc . . . H(13) H 0.4676 0.3649 0.9699 0.1520 Uiso 1.00 calc . . . H(14) H 0.4800 0.4303 0.8787 0.1520 Uiso 1.00 calc . . . H(15) H 0.4568 0.4554 0.9980 0.1520 Uiso 1.00 calc . . . H(16) H 0.3858 0.5045 0.7918 0.1594 Uiso 1.00 calc . . . H(17) H 0.3647 0.5302 0.9121 0.1594 Uiso 1.00 calc . . . H(18) H 0.3164 0.4859 0.8335 0.1594 Uiso 1.00 calc . . . H(19) H 0.3415 0.4226 1.0599 0.1339 Uiso 1.00 calc . . . H(20) H 0.2960 0.3783 0.9765 0.1339 Uiso 1.00 calc . . . H(21) H 0.3532 0.3324 1.0310 0.1339 Uiso 1.00 calc . . . H(22) H 0.2184 0.1630 0.7540 0.0845 Uiso 1.00 calc . . . H(23) H 0.1953 0.2475 0.7935 0.0845 Uiso 1.00 calc . . . H(24) H 0.1562 0.2003 0.7034 0.0845 Uiso 1.00 calc . . . H(25) H 0.2000 0.3666 0.6524 0.1002 Uiso 1.00 calc . . . H(26) H 0.1641 0.3158 0.5620 0.1002 Uiso 1.00 calc . . . H(27) H 0.2307 0.3538 0.5344 0.1002 Uiso 1.00 calc . . . H(28) H 0.2176 0.1485 0.5422 0.0551 Uiso 1.00 calc . . . H(29) H 0.2391 0.2192 0.4650 0.0551 Uiso 1.00 calc . . . H(30) H 0.2324 0.0424 0.3429 0.0840 Uiso 1.00 calc . . . H(31) H 0.1237 0.0590 0.3193 0.0959 Uiso 1.00 calc . . . H(32) H 0.1366 0.1278 0.2334 0.0959 Uiso 1.00 calc . . . H(33) H 0.1555 0.1390 0.3590 0.0959 Uiso 1.00 calc . . . H(34) H 0.2059 0.0198 0.1107 0.1035 Uiso 1.00 calc . . . H(35) H 0.1855 -0.0423 0.2019 0.1035 Uiso 1.00 calc . . . H(36) H 0.2581 -0.0274 0.1776 0.1035 Uiso 1.00 calc . . . H(37) H 0.2961 0.2254 0.1455 0.0663 Uiso 1.00 calc . . . H(38) H 0.2477 0.1360 0.0149 0.1034 Uiso 1.00 calc . . . H(39) H 0.2188 0.2221 0.0031 0.1034 Uiso 1.00 calc . . . H(40) H 0.1808 0.1554 0.0666 0.1034 Uiso 1.00 calc . . . H(41) H 0.2097 0.3143 0.1734 0.0810 Uiso 1.00 calc . . . H(42) H 0.1715 0.2480 0.2374 0.0810 Uiso 1.00 calc . . . H(43) H 0.2331 0.2852 0.2909 0.0810 Uiso 1.00 calc . . . H(44) H 0.4779 0.1340 0.1175 0.1042 Uiso 1.00 calc . . . H(45) H 0.4527 0.2644 0.1498 0.1370 Uiso 1.00 calc . . . H(46) H 0.5247 0.2404 0.1613 0.1370 Uiso 1.00 calc . . . H(47) H 0.4831 0.2535 0.2684 0.1370 Uiso 1.00 calc . . . H(48) H 0.5469 0.0938 0.2242 0.1428 Uiso 1.00 calc . . . H(49) H 0.5047 0.1069 0.3306 0.1428 Uiso 1.00 calc . . . H(50) H 0.4875 0.0390 0.2456 0.1428 Uiso 1.00 calc . . . H(51) H 0.3285 0.0853 0.0708 0.0897 Uiso 1.00 calc . . . H(52) H 0.4501 0.0081 0.0546 0.1128 Uiso 1.00 calc . . . H(53) H 0.3905 -0.0297 0.1135 0.1128 Uiso 1.00 calc . . . H(54) H 0.3907 -0.0179 -0.0163 0.1128 Uiso 1.00 calc . . . H(55) H 0.4353 0.1573 -0.0340 0.1304 Uiso 1.00 calc . . . H(56) H 0.3679 0.1973 -0.0240 0.1304 Uiso 1.00 calc . . . H(57) H 0.3773 0.1222 -0.1004 0.1304 Uiso 1.00 calc . . . 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) 0.0394(2) 0.0308(1) 0.0395(2) 0.0002(1) -0.0017(1) -0.0006(1) Cl(1) 0.085(2) 0.0323(8) 0.071(1) -0.002(1) -0.004(1) 0.0082(9) Cl(2) 0.108(2) 0.059(1) 0.041(1) -0.006(1) 0.008(1) 0.0014(10) Cl(3) 0.070(1) 0.0313(8) 0.067(1) -0.0023(9) 0.003(1) 0.0041(9) S(1) 0.067(1) 0.0347(8) 0.041(1) 0.0152(9) 0.0008(9) -0.0011(8) P(1) 0.043(1) 0.0309(8) 0.041(1) 0.0024(8) -0.0022(8) -0.0033(8) P(2) 0.0399(10) 0.0355(9) 0.040(1) 0.0064(8) 0.0013(8) 0.0024(8) N(1) 0.049(4) 0.041(3) 0.057(4) -0.001(3) -0.010(3) 0.011(3) N(2) 0.044(4) 0.057(4) 0.046(4) 0.004(3) 0.004(3) 0.001(3) C(1) 0.049(4) 0.033(3) 0.049(4) 0.003(3) 0.004(3) 0.001(3) C(2) 0.039(4) 0.037(3) 0.045(4) 0.002(3) -0.001(3) 0.001(3) C(3) 0.037(4) 0.043(4) 0.047(4) 0.006(3) 0.005(3) -0.005(3) C(4) 0.037(4) 0.046(4) 0.067(5) -0.002(3) -0.006(4) -0.014(4) C(5) 0.048(5) 0.037(4) 0.077(6) 0.005(4) -0.004(4) -0.022(4) C(6) 0.038(4) 0.046(4) 0.070(6) 0.007(3) -0.008(4) -0.021(4) C(7) 0.033(3) 0.036(3) 0.052(4) 0.004(3) 0.000(3) -0.011(3) C(8) 0.031(4) 0.054(4) 0.065(5) 0.002(4) 0.004(3) -0.008(4) C(9) 0.039(4) 0.050(4) 0.089(7) 0.016(4) 0.002(4) -0.002(5) C(10) 0.068(6) 0.065(6) 0.098(8) 0.006(5) 0.035(6) 0.001(5) C(11) 0.044(5) 0.096(8) 0.115(9) 0.026(5) -0.014(5) -0.027(7) C(12) 0.059(6) 0.061(5) 0.105(8) 0.000(5) -0.015(6) -0.043(6) C(13) 0.17(2) 0.064(7) 0.19(2) 0.023(9) -0.06(1) -0.062(9) C(14) 0.065(7) 0.13(1) 0.19(1) 0.006(7) -0.028(8) -0.12(1) C(15) 0.100(10) 0.15(1) 0.11(1) 0.003(9) 0.003(8) -0.08(1) C(16) 0.039(4) 0.047(4) 0.052(5) 0.009(3) -0.005(3) -0.022(4) C(17) 0.049(5) 0.102(8) 0.062(6) -0.014(5) 0.014(4) -0.022(5) C(18) 0.075(7) 0.067(6) 0.115(9) 0.038(5) -0.041(6) -0.039(6) C(19) 0.040(4) 0.042(4) 0.051(5) 0.003(3) -0.005(3) -0.009(3) C(20) 0.058(5) 0.053(5) 0.096(7) -0.002(5) -0.019(5) 0.007(5) C(21) 0.052(6) 0.106(8) 0.097(8) -0.018(6) -0.009(5) 0.005(7) C(22) 0.091(8) 0.060(5) 0.114(10) -0.014(6) -0.037(7) -0.007(6) C(23) 0.055(5) 0.040(4) 0.063(5) 0.008(4) -0.014(4) 0.008(4) C(24) 0.067(6) 0.062(5) 0.079(7) 0.020(5) -0.007(5) 0.010(5) C(25) 0.118(9) 0.075(6) 0.073(7) 0.026(7) -0.049(6) 0.002(6) C(26) 0.045(5) 0.110(9) 0.103(9) 0.000(6) 0.012(5) 0.007(7) C(27) 0.063(7) 0.16(1) 0.17(1) 0.023(9) -0.028(9) 0.03(1) C(28) 0.075(8) 0.104(10) 0.17(1) -0.029(8) -0.010(8) 0.018(10) C(29) 0.083(7) 0.080(7) 0.042(5) 0.004(6) 0.006(5) -0.009(5) C(30) 0.106(10) 0.099(8) 0.084(8) 0.016(7) 0.020(7) -0.033(7) C(31) 0.17(1) 0.14(1) 0.038(6) -0.03(1) 0.011(7) -0.003(7) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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) Cl(2) 2.314(2) . . yes Pt(1) Cl(3) 2.341(2) . . yes Pt(1) S(1) 2.288(2) . . yes Pt(1) P(1) 2.197(2) . . yes Cl(1) C(1) 1.778(7) . . yes S(1) P(2) 2.029(3) . . yes P(1) C(1) 1.869(8) . . yes P(1) C(2) 1.825(7) . . yes P(1) C(19) 1.823(7) . . yes P(2) N(1) 1.653(6) . . yes P(2) N(2) 1.645(6) . . yes P(2) C(1) 1.836(8) . . yes N(1) C(20) 1.51(1) . . yes N(1) C(23) 1.497(9) . . yes N(2) C(26) 1.49(1) . . yes N(2) C(29) 1.49(1) . . yes C(2) C(3) 1.406(10) . . yes C(2) C(7) 1.419(9) . . yes C(3) C(4) 1.405(10) . . yes C(3) C(8) 1.538(10) . . yes C(4) C(5) 1.40(1) . . yes C(5) C(6) 1.39(1) . . yes C(5) C(12) 1.52(1) . . yes C(6) C(7) 1.372(10) . . yes C(7) C(16) 1.525(10) . . yes C(8) C(9) 1.50(1) . . yes C(8) C(10) 1.53(1) . . yes C(8) C(11) 1.55(1) . . yes C(12) C(13) 1.49(2) . . yes C(12) C(14) 1.52(1) . . yes C(12) C(15) 1.56(2) . . yes C(16) C(17) 1.53(1) . . yes C(16) C(18) 1.52(1) . . yes C(16) C(19) 1.547(9) . . yes C(20) C(21) 1.49(1) . . yes C(20) C(22) 1.54(1) . . yes C(23) C(24) 1.53(1) . . yes C(23) C(25) 1.52(1) . . yes C(26) C(27) 1.42(2) . . yes C(26) C(28) 1.46(2) . . yes C(29) C(30) 1.54(1) . . yes C(29) C(31) 1.50(1) . . yes C(32) C(33) 1.18(6) . . yes C(32) C(35) 1.19(6) . 3_666 yes C(33) C(34) 1.67(9) . . yes C(33) C(35) 1.76(7) . . yes C(34) C(35) 1.49(9) . . 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 Cl(2) Pt(1) Cl(3) 90.67(8) . 1_555 1_555 yes Cl(2) Pt(1) S(1) 176.38(7) . 1_555 1_555 yes Cl(2) Pt(1) P(1) 89.89(7) . 1_555 1_555 yes Cl(3) Pt(1) S(1) 85.74(7) . 1_555 1_555 yes Cl(3) Pt(1) P(1) 178.97(7) . 1_555 1_555 yes S(1) Pt(1) P(1) 93.72(7) . 1_555 1_555 yes Pt(1) S(1) P(2) 107.41(10) . 1_555 1_555 yes Pt(1) P(1) C(1) 107.7(2) . 1_555 1_555 yes Pt(1) P(1) C(2) 125.6(2) . 1_555 1_555 yes Pt(1) P(1) C(19) 114.1(2) . 1_555 1_555 yes C(1) P(1) C(2) 106.1(3) . 1_555 1_555 yes C(1) P(1) C(19) 106.2(3) . 1_555 1_555 yes C(2) P(1) C(19) 95.4(3) . 1_555 1_555 yes S(1) P(2) N(1) 112.7(2) . 1_555 1_555 yes S(1) P(2) N(2) 111.8(2) . 1_555 1_555 yes S(1) P(2) C(1) 102.1(2) . 1_555 1_555 yes N(1) P(2) N(2) 109.6(3) . 1_555 1_555 yes N(1) P(2) C(1) 112.3(3) . 1_555 1_555 yes N(2) P(2) C(1) 108.1(3) . 1_555 1_555 yes P(2) N(1) C(20) 118.3(5) . 1_555 1_555 yes P(2) N(1) C(23) 118.8(5) . 1_555 1_555 yes C(20) N(1) C(23) 122.7(6) . 1_555 1_555 yes P(2) N(2) C(26) 123.9(6) . 1_555 1_555 yes P(2) N(2) C(29) 116.1(6) . 1_555 1_555 yes C(26) N(2) C(29) 115.3(7) . 1_555 1_555 yes Cl(1) C(1) P(1) 112.8(4) . 1_555 1_555 yes Cl(1) C(1) P(2) 115.3(4) . 1_555 1_555 yes P(1) C(1) P(2) 111.5(4) . 1_555 1_555 yes P(1) C(2) C(3) 132.0(6) . 1_555 1_555 yes P(1) C(2) C(7) 107.5(5) . 1_555 1_555 yes C(3) C(2) C(7) 120.6(6) . 1_555 1_555 yes C(2) C(3) C(4) 115.8(6) . 1_555 1_555 yes C(2) C(3) C(8) 128.4(7) . 1_555 1_555 yes C(4) C(3) C(8) 115.8(6) . 1_555 1_555 yes C(3) C(4) C(5) 124.7(7) . 1_555 1_555 yes C(4) C(5) C(6) 117.1(7) . 1_555 1_555 yes C(4) C(5) C(12) 122.0(7) . 1_555 1_555 yes C(6) C(5) C(12) 120.9(7) . 1_555 1_555 yes C(5) C(6) C(7) 121.4(7) . 1_555 1_555 yes C(2) C(7) C(6) 120.5(7) . 1_555 1_555 yes C(2) C(7) C(16) 119.5(6) . 1_555 1_555 yes C(6) C(7) C(16) 120.0(6) . 1_555 1_555 yes C(3) C(8) C(9) 114.3(6) . 1_555 1_555 yes C(3) C(8) C(10) 107.9(7) . 1_555 1_555 yes C(3) C(8) C(11) 111.6(7) . 1_555 1_555 yes C(9) C(8) C(10) 110.6(7) . 1_555 1_555 yes C(9) C(8) C(11) 104.1(7) . 1_555 1_555 yes C(10) C(8) C(11) 108.3(8) . 1_555 1_555 yes C(5) C(12) C(13) 109.7(10) . 1_555 1_555 yes C(5) C(12) C(14) 112.7(8) . 1_555 1_555 yes C(5) C(12) C(15) 109.4(8) . 1_555 1_555 yes C(13) C(12) C(14) 110(1) . 1_555 1_555 yes C(13) C(12) C(15) 107(1) . 1_555 1_555 yes C(14) C(12) C(15) 107(1) . 1_555 1_555 yes C(7) C(16) C(17) 109.7(7) . 1_555 1_555 yes C(7) C(16) C(18) 111.8(7) . 1_555 1_555 yes C(7) C(16) C(19) 107.1(6) . 1_555 1_555 yes C(17) C(16) C(18) 108.8(8) . 1_555 1_555 yes C(17) C(16) C(19) 109.7(7) . 1_555 1_555 yes C(18) C(16) C(19) 109.8(7) . 1_555 1_555 yes P(1) C(19) C(16) 109.1(5) . 1_555 1_555 yes N(1) C(20) C(21) 114.6(8) . 1_555 1_555 yes N(1) C(20) C(22) 111.1(9) . 1_555 1_555 yes C(21) C(20) C(22) 113.9(9) . 1_555 1_555 yes N(1) C(23) C(24) 114.5(7) . 1_555 1_555 yes N(1) C(23) C(25) 114.1(7) . 1_555 1_555 yes C(24) C(23) C(25) 108.5(7) . 1_555 1_555 yes N(2) C(26) C(27) 120(1) . 1_555 1_555 yes N(2) C(26) C(28) 116.7(10) . 1_555 1_555 yes C(27) C(26) C(28) 116(1) . 1_555 1_555 yes N(2) C(29) C(30) 114.3(8) . 1_555 1_555 yes N(2) C(29) C(31) 112.5(9) . 1_555 1_555 yes C(30) C(29) C(31) 113.3(9) . 1_555 1_555 yes C(33) C(32) C(35) 121(6) . 1_555 3_666 yes C(32) C(33) C(34) 130(6) . 1_555 1_555 yes C(32) C(33) C(35) 85(4) . 1_555 1_555 yes C(34) C(33) C(35) 51(3) . 1_555 1_555 yes C(33) C(34) C(35) 67(4) . 1_555 1_555 yes C(32) C(35) C(33) 103(5) . 3_666 1_555 yes C(32) C(35) C(34) 102(5) . 3_666 1_555 yes C(33) C(35) C(34) 61(4) . 1_555 1_555 yes #------------------------------------------------------------------------------