# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Parr, Jonathan' 'Faller, J. W.' 'Lloret-Fillol, J.' _publ_contact_author_name 'Jonathan Parr' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leics LE11 3TU UNITED KINGDOM ; _publ_contact_author_email 'PARR@JAXINDY.CHEM.YALE.EDU' _publ_section_title ; Complexes of elements of group 9 and 10 with new chiral chelating bisphosphine monosulfide and monoselenide ligands ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; data__2148PdCl2[phenethylN(PPS)] _database_code_CSD 175774 #========================================================================== #== _audit_creation_date '2001-11-24' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #========================================================================== #== _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 999)' #-------------------------------------------------------------------------- #-- _cell_length_a 10.2033(5) _cell_length_b 16.3289(8) _cell_length_c 11.7551(5) _cell_angle_alpha 90 _cell_angle_beta 96.269(3) _cell_angle_gamma 90 _cell_volume 1946.8(1) _cell_formula_units_Z 2 _cell_measurement_temperature 183.2 _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 'P21' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #-------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 937.66 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H31 Cl8 N P2 Pd S ' _chemical_formula_moiety 'C32 H29 Cl2 N P2 Pd S, 2(C H Cl3)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 940.00 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 14270 _reflns_number_total 7818 _reflns_number_gt 3179 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04350 _diffrn_reflns_av_sigmaI/netI 0.103 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.47 _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 C 0 68 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 62 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 2 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd 0 2 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 2 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #========================================================================== #== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.79922(5) 0.5000 0.01386(4) 0.02480(12) 1.000 . Uani d ? Cl(1) 0.8845(2) 0.55121(13) -0.1458(2) 0.0384(6) 1.000 . Uani d ? Cl(2) 0.6405(2) 0.4193(1) -0.0975(2) 0.0407(6) 1.000 . Uani d ? Cl(3) 0.4020(3) 0.2813(2) 0.6669(2) 0.0648(8) 1.000 . Uani d ? Cl(4) 0.6630(3) 0.2311(2) 0.6263(2) 0.0647(8) 1.000 . Uani d ? Cl(5) 0.5471(3) 0.1667(2) 0.8178(3) 0.0845(11) 1.000 . Uani d ? Cl(6) 0.5005(3) 0.3148(2) 0.3535(2) 0.0751(9) 1.000 . Uani d ? Cl(7) 0.4453(4) 0.2042(3) 0.1653(3) 0.108(1) 1.000 . Uani d ? Cl(8) 0.6911(3) 0.1930(2) 0.3083(3) 0.0866(11) 1.000 . Uani d ? S(1) 0.7022(2) 0.46439(13) 0.1719(2) 0.0320(5) 1.000 . Uani d ? P(1) 0.9538(2) 0.56985(12) 0.1194(2) 0.0243(5) 1.000 . Uani d ? P(2) 0.8539(2) 0.47306(11) 0.2957(2) 0.0256(5) 1.000 . Uani d ? N(1) 0.9463(6) 0.5525(3) 0.2632(5) 0.024(2) 1.000 . Uani d ? C(1) 1.0372(7) 0.6064(4) 0.3482(6) 0.026(2) 1.000 . Uani d ? C(2) 0.9656(8) 0.6810(5) 0.3839(6) 0.035(2) 1.000 . Uani d ? C(3) 1.1096(7) 0.5606(4) 0.4492(6) 0.027(2) 1.000 . Uani d ? C(4) 1.0596(7) 0.5548(5) 0.5529(6) 0.031(2) 1.000 . Uani d ? C(5) 1.1262(8) 0.5145(5) 0.6457(6) 0.039(2) 1.000 . Uani d ? C(6) 1.2482(9) 0.4809(5) 0.6339(7) 0.046(3) 1.000 . Uani d ? C(7) 1.3039(8) 0.4878(5) 0.5319(6) 0.038(2) 1.000 . Uani d ? C(8) 1.2333(8) 0.5279(5) 0.4395(7) 0.033(2) 1.000 . Uani d ? C(9) 1.1212(7) 0.5423(4) 0.0904(6) 0.026(2) 1.000 . Uani d ? C(10) 1.1883(7) 0.4802(4) 0.1530(6) 0.031(2) 1.000 . Uani d ? C(11) 1.3085(8) 0.4559(5) 0.1247(7) 0.041(2) 1.000 . Uani d ? C(12) 1.3609(7) 0.4881(6) 0.0334(7) 0.042(3) 1.000 . Uani d ? C(13) 1.2960(8) 0.5503(5) -0.0303(7) 0.040(2) 1.000 . Uani d ? C(14) 1.1747(8) 0.5767(5) -0.0021(6) 0.034(2) 1.000 . Uani d ? C(15) 0.9368(7) 0.6798(4) 0.1012(6) 0.026(2) 1.000 . Uani d ? C(16) 1.0463(8) 0.7324(5) 0.1173(6) 0.033(2) 1.000 . Uani d ? C(17) 1.0251(8) 0.8176(5) 0.1140(6) 0.037(2) 1.000 . Uani d ? C(18) 0.9003(9) 0.8477(5) 0.0961(7) 0.042(3) 1.000 . Uani d ? C(19) 0.7932(8) 0.7953(5) 0.0793(7) 0.041(2) 1.000 . Uani d ? C(20) 0.8103(8) 0.7121(5) 0.0828(7) 0.034(2) 1.000 . Uani d ? C(21) 0.9522(8) 0.3803(4) 0.3030(6) 0.030(2) 1.000 . Uani d ? C(22) 1.0470(8) 0.3641(5) 0.3964(6) 0.029(2) 1.000 . Uani d ? C(23) 1.1316(8) 0.2996(5) 0.3939(6) 0.036(2) 1.000 . Uani d ? C(24) 1.1235(8) 0.2478(5) 0.2987(7) 0.039(2) 1.000 . Uani d ? C(25) 1.0278(9) 0.2631(5) 0.2071(7) 0.040(2) 1.000 . Uani d ? C(26) 0.9439(8) 0.3289(5) 0.2104(6) 0.034(2) 1.000 . Uani d ? C(27) 0.7811(7) 0.4901(5) 0.4255(5) 0.027(2) 1.000 . Uani d ? C(28) 0.7887(7) 0.4364(5) 0.5158(6) 0.033(2) 1.000 . Uani d ? C(29) 0.7268(8) 0.4547(6) 0.6120(7) 0.040(3) 1.000 . Uani d ? C(30) 0.6551(8) 0.5240(5) 0.6175(7) 0.042(3) 1.000 . Uani d ? C(31) 0.6391(9) 0.5771(6) 0.5224(7) 0.043(3) 1.000 . Uani d ? C(32) 0.7031(8) 0.5621(5) 0.4283(6) 0.036(2) 1.000 . Uani d ? C(33) 0.5582(8) 0.2527(5) 0.7302(7) 0.043(3) 1.000 . Uani d ? C(34) 0.5710(10) 0.2602(6) 0.2485(9) 0.062(3) 1.000 . Uani d ? H(1) 1.1042 0.6265 0.3053 0.031 1.000 . Uiso c ? H(2) 0.9669 0.6816 0.4648 0.042 1.000 . Uiso c ? H(3) 1.0078 0.7289 0.3598 0.042 1.000 . Uiso c ? H(4) 0.8769 0.6797 0.3496 0.042 1.000 . Uiso c ? H(5) 0.9766 0.5791 0.5613 0.037 1.000 . Uiso c ? H(6) 1.0888 0.5101 0.7160 0.047 1.000 . Uiso c ? H(7) 1.2946 0.4527 0.6965 0.056 1.000 . Uiso c ? H(8) 1.3888 0.4657 0.5249 0.045 1.000 . Uiso c ? H(9) 1.2706 0.5328 0.3692 0.039 1.000 . Uiso c ? H(10) 1.1510 0.4549 0.2148 0.038 1.000 . Uiso c ? H(11) 1.3566 0.4155 0.1699 0.049 1.000 . Uiso c ? H(12) 1.4425 0.4679 0.0130 0.051 1.000 . Uiso c ? H(13) 1.3343 0.5745 -0.0923 0.048 1.000 . Uiso c ? H(14) 1.1281 0.6184 -0.0460 0.041 1.000 . Uiso c ? H(15) 1.1331 0.7108 0.1303 0.040 1.000 . Uiso c ? H(16) 1.0980 0.8541 0.1243 0.044 1.000 . Uiso c ? H(17) 0.8864 0.9053 0.0951 0.051 1.000 . Uiso c ? H(18) 0.7067 0.8173 0.0652 0.049 1.000 . Uiso c ? H(19) 0.7361 0.6766 0.0727 0.040 1.000 . Uiso c ? H(20) 1.0522 0.3985 0.4620 0.035 1.000 . Uiso c ? H(21) 1.1961 0.2899 0.4570 0.043 1.000 . Uiso c ? H(22) 1.1823 0.2029 0.2964 0.047 1.000 . Uiso c ? H(23) 1.0206 0.2281 0.1422 0.048 1.000 . Uiso c ? H(24) 0.8792 0.3388 0.1474 0.040 1.000 . Uiso c ? H(25) 0.8365 0.3867 0.5125 0.040 1.000 . Uiso c ? H(26) 0.7348 0.4180 0.6750 0.048 1.000 . Uiso c ? H(27) 0.6158 0.5368 0.6849 0.051 1.000 . Uiso c ? H(28) 0.5835 0.6236 0.5238 0.052 1.000 . Uiso c ? H(29) 0.6955 0.5992 0.3657 0.043 1.000 . Uiso c ? H(30) 0.5945 0.2968 0.7761 0.052 1.000 . Uiso c ? H(31) 0.6099 0.2976 0.2002 0.074 1.000 . Uiso c ? 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 Pd(1) 0.0292(3) 0.0232(2) 0.0220(2) -0.0015(3) 0.0026(2) 0.0014(3) Cl(1) 0.0494(13) 0.0440(12) 0.0222(10) -0.0124(10) 0.0054(9) .0000(9) Cl(2) 0.0334(11) 0.0546(13) 0.0348(11) -0.0106(10) 0.0066(9) -0.0171(10) Cl(3) 0.059(2) 0.065(2) 0.067(2) 0.0236(13) -0.0082(13) .006(1) Cl(4) 0.065(2) 0.062(2) 0.068(2) 0.015(1) 0.0107(13) .0018(13) Cl(5) 0.085(2) 0.076(2) 0.090(2) 0.008(2) 0.002(2) .046(2) Cl(6) 0.088(2) 0.073(2) 0.065(2) 0.021(2) 0.008(2) .004(1) Cl(7) 0.095(3) 0.129(3) 0.094(3) 0.014(2) -0.015(2) 0.037(2) Cl(8) 0.075(2) 0.080(2) 0.104(2) 0.024(2) 0.004(2) .012(2) S(1) 0.0314(10) 0.0380(10) 0.0260(10) -0.0072(9) 0.0008(8) .0039(8) P(1) 0.0288(11) 0.0214(10) 0.0228(10) -0.0001(8) 0.0033(8) .0008(8) P(2) 0.0300(10) 0.0239(9) 0.0228(9) -0.0016(8) 0.0031(8) .0024(7) N(1) 0.026(3) 0.019(3) 0.026(3) 0.000(3) 0.000(3) .005(3) C(1) 0.031(4) 0.023(4) 0.024(4) -0.005(3) -0.002(3) 0.005(3) C(2) 0.050(5) 0.024(4) 0.031(4) 0.003(4) 0.004(4) 0.001(3) C(3) 0.034(4) 0.025(4) 0.021(4) -0.003(3) -0.000(3) 0.002(3) C(4) 0.034(4) 0.029(4) 0.029(4) -0.001(3) 0.004(3) 0.003(3) C(5) 0.047(5) 0.042(6) 0.028(4) -0.002(4) -0.002(3) 0.001(4) C(6) 0.052(5) 0.046(6) 0.037(4) 0.004(4) -0.015(4) .001(4) C(7) 0.042(4) 0.028(5) 0.042(5) -0.004(4) -0.001(4) 0.004(4) C(8) 0.039(4) 0.028(4) 0.032(4) -0.004(3) 0.004(4) .000(3) C(9) 0.026(4) 0.028(4) 0.026(4) -0.003(3) 0.010(3) .003(3) C(10) 0.035(4) 0.026(5) 0.032(4) -0.002(3) 0.001(3) 0.011(3) C(11) 0.030(4) 0.046(5) 0.047(5) 0.014(4) -0.002(4) 0.009(4) C(12) 0.032(4) 0.048(6) 0.047(5) 0.005(4) 0.005(4) 0.024(5) C(13) 0.039(5) 0.044(5) 0.039(5) -0.010(4) 0.013(4) 0.013(4) C(14) 0.034(5) 0.038(4) 0.030(4) -0.004(4) 0.000(4) 0.001(4) C(15) 0.035(4) 0.025(4) 0.018(4) 0.001(3) 0.006(3) .002(3) C(16) 0.040(5) 0.034(4) 0.027(4) -0.001(4) 0.010(4) .008(3) C(17) 0.052(5) 0.031(4) 0.026(4) -0.009(4) -0.003(4) 0.003(3) C(18) 0.063(6) 0.030(4) 0.035(5) 0.003(4) 0.011(4) .006(4) C(19) 0.044(5) 0.032(5) 0.045(5) 0.004(4) 0.000(4) .001(4) C(20) 0.037(5) 0.032(4) 0.032(4) 0.002(4) 0.001(4) .004(3) C(21) 0.035(4) 0.030(4) 0.027(4) -0.001(4) 0.004(3) .008(3) C(22) 0.042(5) 0.023(4) 0.023(4) -0.001(4) 0.006(4) .005(3) C(23) 0.045(5) 0.029(4) 0.031(4) -0.003(4) -0.003(4) .006(4) C(24) 0.047(5) 0.018(4) 0.054(5) 0.015(4) 0.013(4) .005(4) C(25) 0.055(6) 0.027(4) 0.039(5) 0.005(4) 0.011(4) 0.003(4) C(26) 0.045(5) 0.028(4) 0.027(4) 0.006(4) 0.003(4) 0.000(3) C(27) 0.031(4) 0.033(5) 0.016(3) -0.010(4) 0.001(3) 0.000(4) C(28) 0.038(5) 0.032(4) 0.031(4) -0.006(4) 0.007(4) 0.004(4) C(29) 0.038(5) 0.057(6) 0.024(4) -0.011(4) 0.003(4) .005(4) C(30) 0.045(5) 0.054(6) 0.030(4) -0.011(4) 0.013(4) 0.008(4) C(31) 0.039(5) 0.057(6) 0.035(5) 0.007(4) 0.006(4) 0.007(4) C(32) 0.042(5) 0.034(4) 0.030(4) 0.010(4) 0.000(4) .003(4) C(33) 0.045(5) 0.032(5) 0.051(5) 0.001(4) -0.008(4) .003(4) C(34) 0.064(7) 0.051(6) 0.072(7) 0.014(5) 0.018(6) .022(5) #========================================================================== #== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _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 3179 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_all 0.049 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all 0.987 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.46 _refine_diff_density_max 0.84 #========================================================================== #== # MOLECULAR GEOMETRY _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 Pd(1) Cl(1) 2.310(2) . . ? Pd(1) Cl(2) 2.369(2) . . ? Pd(1) S(1) 2.274(2) . . ? Pd(1) P(1) 2.214(2) . . ? Cl(3) C(33) 1.748(8) . . ? Cl(4) C(33) 1.745(9) . . ? Cl(5) C(33) 1.752(9) . . ? Cl(6) C(34) 1.741(10) . . ? Cl(7) C(34) 1.778(11) . . ? Cl(8) C(34) 1.735(10) . . ? S(1) P(2) 2.011(3) . . ? P(1) N(1) 1.724(6) . . ? P(1) C(9) 1.834(7) . . ? P(1) C(15) 1.814(7) . . ? P(2) N(1) 1.672(6) . . ? P(2) C(21) 1.814(8) . . ? P(2) C(27) 1.791(7) . . ? N(1) C(1) 1.559(9) . . ? C(1) C(2) 1.504(10) . . ? C(1) C(3) 1.524(10) . . ? C(1) H(1) 0.95 . . no C(2) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.376(10) . . ? C(3) C(8) 1.387(10) . . ? C(4) C(5) 1.387(10) . . ? C(4) H(5) 0.95 . . no C(5) C(6) 1.381(11) . . ? C(5) H(6) 0.95 . . no C(6) C(7) 1.386(11) . . ? C(6) H(7) 0.95 . . no C(7) C(8) 1.399(11) . . ? C(7) H(8) 0.95 . . no C(8) H(9) 0.95 . . no C(9) C(10) 1.389(10) . . ? C(9) C(14) 1.387(10) . . ? C(10) C(11) 1.364(10) . . ? C(10) H(10) 0.95 . . no C(11) C(12) 1.356(12) . . ? C(11) H(11) 0.95 . . no C(12) C(13) 1.386(12) . . ? C(12) H(12) 0.95 . . no C(13) C(14) 1.385(11) . . ? C(13) H(13) 0.95 . . no C(14) H(14) 0.95 . . no C(15) C(16) 1.405(10) . . ? C(15) C(20) 1.389(10) . . ? C(16) C(17) 1.408(11) . . ? C(16) H(15) 0.95 . . no C(17) C(18) 1.360(12) . . ? C(17) H(16) 0.95 . . no C(18) C(19) 1.385(11) . . ? C(18) H(17) 0.95 . . no C(19) C(20) 1.370(10) . . ? C(19) H(18) 0.95 . . no C(20) H(19) 0.95 . . no C(21) C(22) 1.407(10) . . ? C(21) C(26) 1.370(10) . . ? C(22) C(23) 1.364(11) . . ? C(22) H(20) 0.95 . . no C(23) C(24) 1.398(11) . . ? C(23) H(21) 0.95 . . no C(24) C(25) 1.395(12) . . ? C(24) H(22) 0.95 . . no C(25) C(26) 1.376(11) . . ? C(25) H(23) 0.95 . . no C(26) H(24) 0.95 . . no C(27) C(28) 1.372(10) . . ? C(27) C(32) 1.422(11) . . ? C(28) C(29) 1.386(10) . . ? C(28) H(25) 0.95 . . no C(29) C(30) 1.352(12) . . ? C(29) H(26) 0.95 . . no C(30) C(31) 1.410(12) . . ? C(30) H(27) 0.95 . . no C(31) C(32) 1.367(11) . . ? C(31) H(28) 0.95 . . no C(32) H(29) 0.95 . . no C(33) H(30) 0.95 . . no C(34) H(31) 0.95 . . no #-------------------------------------------------------------------------- #-- 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(1) Pd(1) Cl(2) 92.73(7) . . . ? Cl(1) Pd(1) S(1) 173.01(8) . . . ? Cl(1) Pd(1) P(1) 87.73(7) . . . ? Cl(2) Pd(1) S(1) 88.67(7) . . . ? Cl(2) Pd(1) P(1) 177.11(8) . . . ? S(1) Pd(1) P(1) 91.21(7) . . . ? Pd(1) S(1) P(2) 101.75(10) . . . ? Pd(1) P(1) N(1) 111.1(2) . . . ? Pd(1) P(1) C(9) 113.0(2) . . . ? Pd(1) P(1) C(15) 113.0(2) . . . ? N(1) P(1) C(9) 106.5(3) . . . ? N(1) P(1) C(15) 105.3(3) . . . ? C(9) P(1) C(15) 107.5(3) . . . ? S(1) P(2) N(1) 107.3(2) . . . ? S(1) P(2) C(21) 110.7(3) . . . ? S(1) P(2) C(27) 105.6(2) . . . ? N(1) P(2) C(21) 109.7(3) . . . ? N(1) P(2) C(27) 111.8(3) . . . ? C(21) P(2) C(27) 111.6(4) . . . ? P(1) N(1) P(2) 116.0(3) . . . ? P(1) N(1) C(1) 116.6(4) . . . ? P(2) N(1) C(1) 127.1(5) . . . ? N(1) C(1) C(2) 111.3(6) . . . ? N(1) C(1) C(3) 115.2(6) . . . ? N(1) C(1) H(1) 105.5 . . . no C(2) C(1) C(3) 112.9(6) . . . ? C(2) C(1) H(1) 105.5 . . . no C(3) C(1) H(1) 105.5 . . . no C(1) C(2) H(2) 109.5 . . . no C(1) C(2) H(3) 109.5 . . . no C(1) C(2) H(4) 109.5 . . . no H(2) C(2) H(3) 109.5 . . . no H(2) C(2) H(4) 109.5 . . . no H(3) C(2) H(4) 109.5 . . . no C(1) C(3) C(4) 122.0(7) . . . ? C(1) C(3) C(8) 119.5(7) . . . ? C(4) C(3) C(8) 118.4(7) . . . ? C(3) C(4) C(5) 122.2(7) . . . ? C(3) C(4) H(5) 118.9 . . . no C(5) C(4) H(5) 118.9 . . . no C(4) C(5) C(6) 118.7(7) . . . ? C(4) C(5) H(6) 120.7 . . . no C(6) C(5) H(6) 120.7 . . . no C(5) C(6) C(7) 120.9(7) . . . ? C(5) C(6) H(7) 119.5 . . . no C(7) C(6) H(7) 119.5 . . . no C(6) C(7) C(8) 119.0(7) . . . ? C(6) C(7) H(8) 120.5 . . . no C(8) C(7) H(8) 120.5 . . . no C(3) C(8) C(7) 120.9(7) . . . ? C(3) C(8) H(9) 119.6 . . . no C(7) C(8) H(9) 119.6 . . . no P(1) C(9) C(10) 119.7(5) . . . ? P(1) C(9) C(14) 120.0(6) . . . ? C(10) C(9) C(14) 119.8(7) . . . ? C(9) C(10) C(11) 119.1(7) . . . ? C(9) C(10) H(10) 120.4 . . . no C(11) C(10) H(10) 120.4 . . . no C(10) C(11) C(12) 121.6(8) . . . ? C(10) C(11) H(11) 119.2 . . . no C(12) C(11) H(11) 119.2 . . . no C(11) C(12) C(13) 120.3(7) . . . ? C(11) C(12) H(12) 119.8 . . . no C(13) C(12) H(12) 119.8 . . . no C(12) C(13) C(14) 119.0(8) . . . ? C(12) C(13) H(13) 120.5 . . . no C(14) C(13) H(13) 120.5 . . . no C(9) C(14) C(13) 120.0(7) . . . ? C(9) C(14) H(14) 120.0 . . . no C(13) C(14) H(14) 120.0 . . . no P(1) C(15) C(16) 121.6(6) . . . ? P(1) C(15) C(20) 117.9(6) . . . ? C(16) C(15) C(20) 120.1(7) . . . ? C(15) C(16) C(17) 118.9(7) . . . ? C(15) C(16) H(15) 120.6 . . . no C(17) C(16) H(15) 120.6 . . . no C(16) C(17) C(18) 120.0(8) . . . ? C(16) C(17) H(16) 120.0 . . . no C(18) C(17) H(16) 120.0 . . . no C(17) C(18) C(19) 120.6(8) . . . ? C(17) C(18) H(17) 119.7 . . . no C(19) C(18) H(17) 119.7 . . . no C(18) C(19) C(20) 120.9(8) . . . ? C(18) C(19) H(18) 119.6 . . . no C(20) C(19) H(18) 119.6 . . . no C(15) C(20) C(19) 119.6(7) . . . ? C(15) C(20) H(19) 120.2 . . . no C(19) C(20) H(19) 120.2 . . . no P(2) C(21) C(22) 121.5(6) . . . ? P(2) C(21) C(26) 119.2(6) . . . ? C(22) C(21) C(26) 118.9(7) . . . ? C(21) C(22) C(23) 120.7(7) . . . ? C(21) C(22) H(20) 119.7 . . . no C(23) C(22) H(20) 119.7 . . . no C(22) C(23) C(24) 120.2(7) . . . ? C(22) C(23) H(21) 119.9 . . . no C(24) C(23) H(21) 119.9 . . . no C(23) C(24) C(25) 119.0(7) . . . ? C(23) C(24) H(22) 120.5 . . . no C(25) C(24) H(22) 120.5 . . . no C(24) C(25) C(26) 120.2(7) . . . ? C(24) C(25) H(23) 119.9 . . . no C(26) C(25) H(23) 119.9 . . . no C(21) C(26) C(25) 121.0(7) . . . ? C(21) C(26) H(24) 119.5 . . . no C(25) C(26) H(24) 119.5 . . . no P(2) C(27) C(28) 124.5(6) . . . ? P(2) C(27) C(32) 115.7(5) . . . ? C(28) C(27) C(32) 119.7(6) . . . ? C(27) C(28) C(29) 120.0(7) . . . ? C(27) C(28) H(25) 120.0 . . . no C(29) C(28) H(25) 120.0 . . . no C(28) C(29) C(30) 121.1(8) . . . ? C(28) C(29) H(26) 119.5 . . . no C(30) C(29) H(26) 119.5 . . . no C(29) C(30) C(31) 119.6(8) . . . ? C(29) C(30) H(27) 120.2 . . . no C(31) C(30) H(27) 120.2 . . . no C(30) C(31) C(32) 120.5(8) . . . ? C(30) C(31) H(28) 119.8 . . . no C(32) C(31) H(28) 119.8 . . . no C(27) C(32) C(31) 119.0(7) . . . ? C(27) C(32) H(29) 120.5 . . . no C(31) C(32) H(29) 120.5 . . . no Cl(3) C(33) Cl(4) 110.9(5) . . . ? Cl(3) C(33) Cl(5) 110.5(5) . . . ? Cl(3) C(33) H(30) 108.7 . . . no Cl(4) C(33) Cl(5) 109.4(5) . . . ? Cl(4) C(33) H(30) 108.7 . . . no Cl(5) C(33) H(30) 108.7 . . . no Cl(6) C(34) Cl(7) 108.9(5) . . . ? Cl(6) C(34) Cl(8) 111.4(6) . . . ? Cl(6) C(34) H(31) 109.0 . . . no Cl(7) C(34) Cl(8) 109.5(6) . . . ? Cl(7) C(34) H(31) 109.0 . . . no Cl(8) C(34) H(31) 109.0 . . . no #-------------------------------------------------------------------------- #-- 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 Cl(1) C(30) 3.463(9) . 1_554 no Cl(1) C(29) 3.490(8) . 1_554 no Cl(2) C(33) 3.440(9) . 1_554 no Cl(2) C(12) 3.568(8) . 1_455 no Cl(4) C(8) 3.592(8) . 2_746 no Cl(5) C(13) 3.397(9) . 2_746 no Cl(5) C(12) 3.477(9) . 2_746 no Cl(8) C(5) 3.470(9) . 2_746 no Cl(8) C(6) 3.571(9) . 2_746 no C(2) C(23) 3.482(11) . 2_756 no #-------------------------------------------------------------------------- #-- 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd(1) S(1) P(2) N(1) . . . . 36.4(2) no Pd(1) S(1) P(2) C(21) . . . . -83.3(3) no Pd(1) S(1) P(2) C(27) . . . . 155.8(3) no Pd(1) P(1) N(1) P(2) . . . . 13.9(4) no Pd(1) P(1) N(1) C(1) . . . . -172.2(4) no Pd(1) P(1) C(9) C(10) . . . . -90.5(6) no Pd(1) P(1) C(9) C(14) . . . . 82.2(6) no Pd(1) P(1) C(15) C(16) . . . . -152.1(5) no Pd(1) P(1) C(15) C(20) . . . . 34.7(6) no Cl(1) Pd(1) S(1) P(2) . . . . -105.6(6) no Cl(1) Pd(1) P(1) N(1) . . . . -177.6(2) no Cl(1) Pd(1) P(1) C(9) . . . . -58.0(3) no Cl(1) Pd(1) P(1) C(15) . . . . 64.3(3) no Cl(2) Pd(1) S(1) P(2) . . . . 152.71(10) no Cl(2) Pd(1) P(1) N(1) . . . . -78.3(15) no Cl(2) Pd(1) P(1) C(9) . . . . 41.3(16) no Cl(2) Pd(1) P(1) C(15) . . . . 163.6(14) no S(1) Pd(1) P(1) N(1) . . . . 9.3(2) no S(1) Pd(1) P(1) C(9) . . . . 128.9(3) no S(1) Pd(1) P(1) C(15) . . . . -108.8(3) no S(1) P(2) N(1) P(1) . . . . -33.5(4) no S(1) P(2) N(1) C(1) . . . . 153.4(5) no S(1) P(2) C(21) C(22) . . . . -166.9(5) no S(1) P(2) C(21) C(26) . . . . 20.1(7) no S(1) P(2) C(27) C(28) . . . . 115.1(6) no S(1) P(2) C(27) C(32) . . . . -60.2(6) no P(1) Pd(1) S(1) P(2) . . . . -24.40(10) no P(1) N(1) P(2) C(21) . . . . 86.8(4) no P(1) N(1) P(2) C(27) . . . . -148.9(3) no P(1) N(1) C(1) C(2) . . . . 93.7(6) no P(1) N(1) C(1) C(3) . . . . -136.2(5) no P(1) C(9) C(10) C(11) . . . . 174.9(6) no P(1) C(9) C(14) C(13) . . . . -174.0(6) no P(1) C(15) C(16) C(17) . . . . -173.3(6) no P(1) C(15) C(20) C(19) . . . . 174.0(6) no P(2) N(1) P(1) C(9) . . . . -109.5(4) no P(2) N(1) P(1) C(15) . . . . 136.6(4) no P(2) N(1) C(1) C(2) . . . . -93.3(7) no P(2) N(1) C(1) C(3) . . . . 36.8(8) no P(2) C(21) C(22) C(23) . . . . -171.5(6) no P(2) C(21) C(26) C(25) . . . . 172.2(6) no P(2) C(27) C(28) C(29) . . . . -178.8(6) no P(2) C(27) C(32) C(31) . . . . 176.9(6) no N(1) P(1) C(9) C(10) . . . . 31.7(6) no N(1) P(1) C(9) C(14) . . . . -155.6(6) no N(1) P(1) C(15) C(16) . . . . 86.5(6) no N(1) P(1) C(15) C(20) . . . . -86.7(6) no N(1) P(2) C(21) C(22) . . . . 74.9(6) no N(1) P(2) C(21) C(26) . . . . -98.2(7) no N(1) P(2) C(27) C(28) . . . . -128.5(6) no N(1) P(2) C(27) C(32) . . . . 56.2(6) no N(1) C(1) C(3) C(4) . . . . -93.8(8) no N(1) C(1) C(3) C(8) . . . . 90.3(8) no C(1) N(1) P(1) C(9) . . . . 64.4(5) no C(1) N(1) P(1) C(15) . . . . -49.5(5) no C(1) N(1) P(2) C(21) . . . . -86.3(6) no C(1) N(1) P(2) C(27) . . . . 38.0(6) no C(1) C(3) C(4) C(5) . . . . -178.7(7) no C(1) C(3) C(8) C(7) . . . . 177.9(7) no C(2) C(1) C(3) C(4) . . . . 35.5(10) no C(2) C(1) C(3) C(8) . . . . -140.4(7) no C(3) C(4) C(5) C(6) . . . . 1.5(12) no C(3) C(8) C(7) C(6) . . . . 0.2(12) no C(4) C(3) C(8) C(7) . . . . 1.9(11) no C(4) C(5) C(6) C(7) . . . . 0.6(12) no C(5) C(4) C(3) C(8) . . . . -2.8(11) no C(5) C(6) C(7) C(8) . . . . -1.5(13) no C(9) P(1) C(15) C(16) . . . . -26.8(7) no C(9) P(1) C(15) C(20) . . . . 160.0(6) no C(9) C(10) C(11) C(12) . . . . -3.3(12) no C(9) C(14) C(13) C(12) . . . . 1.5(12) no C(10) C(9) P(1) C(15) . . . . 144.1(6) no C(10) C(9) C(14) C(13) . . . . -1.3(11) no C(10) C(11) C(12) C(13) . . . . 3.5(13) no C(11) C(10) C(9) C(14) . . . . 2.2(10) no C(11) C(12) C(13) C(14) . . . . -2.6(12) no C(14) C(9) P(1) C(15) . . . . -43.1(7) no C(15) C(16) C(17) C(18) . . . . 0.4(11) no C(15) C(20) C(19) C(18) . . . . -1.2(13) no C(16) C(15) C(20) C(19) . . . . 0.6(11) no C(16) C(17) C(18) C(19) . . . . -0.9(12) no C(17) C(16) C(15) C(20) . . . . -0.2(10) no C(17) C(18) C(19) C(20) . . . . 1.4(13) no C(21) P(2) C(27) C(28) . . . . -5.3(7) no C(21) P(2) C(27) C(32) . . . . 179.4(6) no C(21) C(22) C(23) C(24) . . . . -1.0(12) no C(21) C(26) C(25) C(24) . . . . -0.1(13) no C(22) C(21) P(2) C(27) . . . . -49.5(7) no C(22) C(21) C(26) C(25) . . . . -1.0(11) no C(22) C(23) C(24) C(25) . . . . -0.1(12) no C(23) C(22) C(21) C(26) . . . . 1.6(11) no C(23) C(24) C(25) C(26) . . . . 0.7(12) no C(26) C(21) P(2) C(27) . . . . 137.4(6) no C(27) C(28) C(29) C(30) . . . . 1.9(12) no C(27) C(32) C(31) C(30) . . . . 2.9(13) no C(28) C(27) C(32) C(31) . . . . 1.3(12) no C(28) C(29) C(30) C(31) . . . . 2.3(12) no C(29) C(28) C(27) C(32) . . . . -3.7(11) no C(29) C(30) C(31) C(32) . . . . -4.7(13) no #-------------------------------------------------------------------------- #========================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== # End of CIF #========================================================================== data__2124PdCl2[PhMeHCN(PPSe)] _database_code_CSD 175775 _audit_creation_date '2001-12-07' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 999)' #-------------------------------------------------------------------------- #-- _cell_length_a 11.8372(7) _cell_length_b 15.8445(9) _cell_length_c 16.8452(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3159.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------------- #-- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #-------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 745.80 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H29 Cl2 N P2 Pd Se ' _chemical_formula_moiety 'C32 H29 Cl2 N P2 Pd Se ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1488.00 _exptl_absorpt_coefficient_mu 2.033 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 13999 _reflns_number_total 7200 _reflns_number_gt 2368 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05379 _diffrn_reflns_av_sigmaI/netI 0.109 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.99 _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 C 0 128 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 116 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd 0 4 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 4 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #========================================================================== #== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.72355(6) 0.10374(4) 0.39435(4) 0.0291(2) 1.000 . Uani d ? Se(1) 0.55638(9) 0.17767(5) 0.35866(6) 0.0364(3) 1.000 . Uani d ? Cl(1) 0.8871(2) 0.0359(2) 0.43557(13) 0.0436(7) 1.000 . Uani d ? Cl(2) 0.8225(2) 0.22407(13) 0.34876(13) 0.0395(7) 1.000 . Uani d ? P(1) 0.6279(2) -0.0028(1) 0.44702(13) 0.0309(7) 1.000 . Uani d ? P(2) 0.4428(2) 0.07067(13) 0.35850(13) 0.0286(6) 1.000 . Uani d ? N(1) 0.4845(7) 0.0039(4) 0.4305(4) 0.033(2) 1.000 . Uani d ? C(1) 0.4094(8) -0.0558(5) 0.4797(5) 0.035(3) 1.000 . Uani d ? C(2) 0.3616(10) -0.0113(6) 0.5539(5) 0.051(3) 1.000 . Uani d ? C(3) 0.3181(8) -0.1011(6) 0.4317(5) 0.035(3) 1.000 . Uani d ? C(4) 0.2069(10) -0.0728(5) 0.4293(5) 0.045(3) 1.000 . Uani d ? C(5) 0.1239(9) -0.1170(6) 0.3860(7) 0.051(3) 1.000 . Uani d ? C(6) 0.1560(10) -0.1898(7) 0.3448(6) 0.053(4) 1.000 . Uani d ? C(7) 0.2644(10) -0.2190(5) 0.3490(6) 0.044(3) 1.000 . Uani d ? C(8) 0.3447(8) -0.1753(5) 0.3923(6) 0.039(3) 1.000 . Uani d ? C(9) 0.6702(8) -0.1058(6) 0.4131(5) 0.038(3) 1.000 . Uani d ? C(10) 0.6281(9) -0.1389(6) 0.3432(5) 0.040(3) 1.000 . Uani d ? C(11) 0.6643(11) -0.2135(6) 0.3115(6) 0.054(4) 1.000 . Uani d ? C(12) 0.7524(13) -0.2561(6) 0.3470(6) 0.070(4) 1.000 . Uani d ? C(13) 0.8039(11) -0.2242(6) 0.4158(6) 0.063(4) 1.000 . Uani d ? C(14) 0.7654(10) -0.1474(6) 0.4480(5) 0.051(3) 1.000 . Uani d ? C(15) 0.6410(8) 0.0007(5) 0.5541(5) 0.029(3) 1.000 . Uani d ? C(16) 0.6399(9) -0.0698(5) 0.6034(6) 0.041(3) 1.000 . Uani d ? C(17) 0.6407(10) -0.0601(6) 0.6857(5) 0.048(3) 1.000 . Uani d ? C(18) 0.6418(10) 0.0172(7) 0.7186(5) 0.052(3) 1.000 . Uani d ? C(19) 0.6467(11) 0.0874(6) 0.6711(5) 0.056(4) 1.000 . Uani d ? C(20) 0.6476(9) 0.0779(6) 0.5893(5) 0.049(3) 1.000 . Uani d ? C(21) 0.4453(8) 0.0203(5) 0.2622(5) 0.032(3) 1.000 . Uani d ? C(22) 0.5311(9) 0.0386(6) 0.2098(5) 0.044(3) 1.000 . Uani d ? C(23) 0.5392(9) -0.0061(7) 0.1387(6) 0.053(3) 1.000 . Uani d ? C(24) 0.4620(9) -0.0679(7) 0.1187(6) 0.049(3) 1.000 . Uani d ? C(25) 0.3730(9) -0.0871(6) 0.1710(5) 0.042(3) 1.000 . Uani d ? C(26) 0.3653(8) -0.0432(5) 0.2419(5) 0.031(3) 1.000 . Uani d ? C(27) 0.3049(7) 0.1137(5) 0.3793(5) 0.031(3) 1.000 . Uani d ? C(28) 0.2149(8) 0.1058(6) 0.3261(5) 0.035(3) 1.000 . Uani d ? C(29) 0.1125(9) 0.1444(6) 0.3447(6) 0.044(3) 1.000 . Uani d ? C(30) 0.1009(9) 0.1901(6) 0.4155(6) 0.042(3) 1.000 . Uani d ? C(31) 0.1913(9) 0.1970(6) 0.4649(5) 0.041(3) 1.000 . Uani d ? C(32) 0.2935(8) 0.1614(5) 0.4488(5) 0.032(3) 1.000 . Uani d ? H(1) 0.4582 -0.0988 0.4990 0.042 1.000 . Uiso c ? H(2) 0.3922 -0.0366 0.6003 0.061 1.000 . Uiso c ? H(3) 0.3814 0.0468 0.5526 0.061 1.000 . Uiso c ? H(4) 0.2817 -0.0167 0.5545 0.061 1.000 . Uiso c ? H(5) 0.1866 -0.0231 0.4573 0.054 1.000 . Uiso c ? H(6) 0.0480 -0.0977 0.3848 0.062 1.000 . Uiso c ? H(7) 0.1019 -0.2191 0.3136 0.063 1.000 . Uiso c ? H(8) 0.2847 -0.2695 0.3221 0.053 1.000 . Uiso c ? H(9) 0.4197 -0.1966 0.3951 0.047 1.000 . Uiso c ? H(10) 0.5711 -0.1083 0.3159 0.048 1.000 . Uiso c ? H(11) 0.6291 -0.2359 0.2654 0.065 1.000 . Uiso c ? H(12) 0.7786 -0.3076 0.3247 0.084 1.000 . Uiso c ? H(13) 0.8641 -0.2541 0.4404 0.076 1.000 . Uiso c ? H(14) 0.8023 -0.1233 0.4927 0.061 1.000 . Uiso c ? H(15) 0.6385 -0.1247 0.5809 0.049 1.000 . Uiso c ? H(16) 0.6406 -0.1087 0.7188 0.058 1.000 . Uiso c ? H(17) 0.6392 0.0231 0.7747 0.063 1.000 . Uiso c ? H(18) 0.6495 0.1421 0.6940 0.067 1.000 . Uiso c ? H(19) 0.6530 0.1268 0.5568 0.059 1.000 . Uiso c ? H(20) 0.5845 0.0814 0.2220 0.053 1.000 . Uiso c ? H(21) 0.5994 0.0062 0.1032 0.063 1.000 . Uiso c ? H(22) 0.4689 -0.0972 0.0698 0.059 1.000 . Uiso c ? H(23) 0.3193 -0.1294 0.1579 0.050 1.000 . Uiso c ? H(24) 0.3056 -0.0558 0.2777 0.038 1.000 . Uiso c ? H(25) 0.2234 0.0748 0.2782 0.042 1.000 . Uiso c ? H(26) 0.0503 0.1397 0.3093 0.053 1.000 . Uiso c ? H(27) 0.0309 0.2158 0.4287 0.050 1.000 . Uiso c ? H(28) 0.1829 0.2281 0.5127 0.050 1.000 . Uiso c ? H(29) 0.3556 0.1686 0.4839 0.038 1.000 . Uiso c ? 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 Pd(1) 0.0367(4) 0.0289(3) 0.0216(3) 0.0040(4) -0.0033(3) 0.0007(3) Se(1) 0.0396(6) 0.0275(5) 0.0421(5) -0.0013(5) -0.0094(5) .0019(4) Cl(1) 0.041(2) 0.054(2) 0.0358(13) 0.0113(13) -0.0036(12) .0048(12) Cl(2) 0.038(1) 0.0393(13) 0.0410(13) 0.0009(11) 0.0019(12) .0044(11) P(1) 0.044(2) 0.0254(12) 0.0230(12) 0.0054(13) -0.0057(12) -0.0011(10) P(2) 0.034(1) 0.0264(11) 0.0249(11) 0.0010(12) -0.0024(12) .0006(10) N(1) 0.050(5) 0.025(4) 0.024(4) 0.001(4) 0.001(4) 0.003(3) C(1) 0.050(7) 0.025(5) 0.029(5) 0.004(5) 0.005(5) 0.004(4) C(2) 0.070(8) 0.061(7) 0.022(5) -0.010(7) 0.011(5) .003(5) C(3) 0.042(6) 0.028(5) 0.035(5) -0.008(5) 0.008(5) .005(5) C(4) 0.072(9) 0.028(5) 0.036(5) -0.004(6) 0.012(6) 0.005(4) C(5) 0.050(7) 0.043(6) 0.061(7) -0.007(6) 0.007(6) 0.009(6) C(6) 0.050(8) 0.055(7) 0.052(7) -0.020(6) -0.003(6) 0.009(6) C(7) 0.053(7) 0.030(5) 0.048(6) -0.014(6) 0.012(6) 0.002(5) C(8) 0.042(6) 0.030(5) 0.046(5) -0.005(5) 0.006(5) .003(5) C(9) 0.054(7) 0.032(5) 0.028(5) 0.004(5) 0.001(4) .006(4) C(10) 0.056(7) 0.038(5) 0.027(5) 0.007(5) -0.006(5) 0.002(4) C(11) 0.077(9) 0.048(6) 0.037(6) 0.010(7) -0.010(6) 0.009(5) C(12) 0.127(13) 0.033(6) 0.051(7) 0.020(7) 0.007(8) 0.018(5) C(13) 0.087(10) 0.049(6) 0.053(7) 0.025(7) 0.004(7) .008(5) C(14) 0.072(8) 0.044(6) 0.036(5) 0.012(6) 0.001(6) 0.002(5) C(15) 0.038(6) 0.023(4) 0.026(5) 0.007(5) 0.001(4) 0.003(4) C(16) 0.055(7) 0.038(5) 0.031(5) 0.007(5) -0.001(6) .006(5) C(17) 0.065(8) 0.055(6) 0.025(5) 0.028(6) 0.002(5) .010(5) C(18) 0.069(9) 0.064(7) 0.024(5) 0.009(7) -0.000(5) .004(5) C(19) 0.094(10) 0.043(6) 0.030(5) -0.003(7) -0.005(6) 0.008(5) C(20) 0.068(8) 0.046(6) 0.033(6) -0.006(6) -0.012(5) .004(4) C(21) 0.031(6) 0.032(5) 0.034(5) -0.000(5) -0.007(5) .003(4) C(22) 0.054(7) 0.046(6) 0.032(5) -0.017(6) 0.002(5) 0.005(5) C(23) 0.047(7) 0.071(7) 0.039(6) -0.008(6) 0.016(6) 0.003(6) C(24) 0.050(7) 0.061(7) 0.036(6) -0.005(6) 0.013(5) 0.014(5) C(25) 0.055(7) 0.037(6) 0.035(5) -0.005(5) -0.007(5) 0.000(4) C(26) 0.038(6) 0.030(5) 0.026(5) -0.005(5) 0.005(4) .000(4) C(27) 0.032(6) 0.031(5) 0.029(5) -0.003(4) -0.005(4) .005(4) C(28) 0.040(6) 0.032(5) 0.032(5) -0.002(6) -0.003(5) 0.003(4) C(29) 0.043(7) 0.048(6) 0.041(6) -0.005(6) -0.007(5) .007(5) C(30) 0.042(7) 0.040(6) 0.043(6) 0.007(5) 0.009(5) .007(5) C(31) 0.049(7) 0.040(6) 0.035(5) 0.001(5) 0.003(5) 0.000(4) C(32) 0.034(6) 0.033(5) 0.028(5) -0.005(5) 0.002(4) 0.007(4) #========================================================================== #== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _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 2368 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.067 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.051 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.56 _refine_diff_density_max 1.01 #========================================================================== #== # MOLECULAR GEOMETRY _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 Pd(1) Se(1) 2.3769(12) . . ? Pd(1) Cl(1) 2.321(3) . . ? Pd(1) Cl(2) 2.366(2) . . ? Pd(1) P(1) 2.218(3) . . ? Se(1) P(2) 2.164(2) . . ? P(1) N(1) 1.723(8) . . ? P(1) C(9) 1.801(10) . . ? P(1) C(15) 1.811(8) . . ? P(2) N(1) 1.684(7) . . ? P(2) C(21) 1.808(9) . . ? P(2) C(27) 1.804(9) . . ? N(1) C(1) 1.539(11) . . ? C(1) C(2) 1.542(12) . . ? C(1) C(3) 1.528(13) . . ? C(1) H(1) 0.95 . . no C(2) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.39(1) . . ? C(3) C(8) 1.387(13) . . ? C(4) C(5) 1.41(1) . . ? C(4) H(5) 0.95 . . no C(5) C(6) 1.40(1) . . ? C(5) H(6) 0.95 . . no C(6) C(7) 1.37(2) . . ? C(6) H(7) 0.95 . . no C(7) C(8) 1.385(13) . . ? C(7) H(8) 0.95 . . no C(8) H(9) 0.95 . . no C(9) C(10) 1.381(12) . . ? C(9) C(14) 1.432(13) . . ? C(10) C(11) 1.366(12) . . ? C(10) H(10) 0.95 . . no C(11) C(12) 1.38(2) . . ? C(11) H(11) 0.95 . . no C(12) C(13) 1.40(2) . . ? C(12) H(12) 0.95 . . no C(13) C(14) 1.408(13) . . ? C(13) H(13) 0.95 . . no C(14) H(14) 0.95 . . no C(15) C(16) 1.392(12) . . ? C(15) C(20) 1.362(12) . . ? C(16) C(17) 1.395(13) . . ? C(16) H(15) 0.95 . . no C(17) C(18) 1.344(13) . . ? C(17) H(16) 0.95 . . no C(18) C(19) 1.372(13) . . ? C(18) H(17) 0.95 . . no C(19) C(20) 1.385(13) . . ? C(19) H(18) 0.95 . . no C(20) H(19) 0.95 . . no C(21) C(22) 1.376(13) . . ? C(21) C(26) 1.424(12) . . ? C(22) C(23) 1.395(13) . . ? C(22) H(20) 0.95 . . no C(23) C(24) 1.38(1) . . ? C(23) H(21) 0.95 . . no C(24) C(25) 1.406(13) . . ? C(24) H(22) 0.95 . . no C(25) C(26) 1.386(12) . . ? C(25) H(23) 0.95 . . no C(26) H(24) 0.95 . . no C(27) C(28) 1.398(11) . . ? C(27) C(32) 1.399(11) . . ? C(28) C(29) 1.39(1) . . ? C(28) H(25) 0.95 . . no C(29) C(30) 1.401(13) . . ? C(29) H(26) 0.95 . . no C(30) C(31) 1.360(13) . . ? C(30) H(27) 0.95 . . no C(31) C(32) 1.362(13) . . ? C(31) H(28) 0.95 . . no C(32) H(29) 0.95 . . no #-------------------------------------------------------------------------- #-- 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 Se(1) Pd(1) Cl(1) 176.86(7) . . . ? Se(1) Pd(1) Cl(2) 86.15(7) . . . ? Se(1) Pd(1) P(1) 92.94(8) . . . ? Cl(1) Pd(1) Cl(2) 93.30(9) . . . ? Cl(1) Pd(1) P(1) 87.33(9) . . . ? Cl(2) Pd(1) P(1) 174.90(9) . . . ? Pd(1) Se(1) P(2) 97.55(7) . . . ? Pd(1) P(1) N(1) 113.0(3) . . . ? Pd(1) P(1) C(9) 114.9(3) . . . ? Pd(1) P(1) C(15) 109.3(3) . . . ? N(1) P(1) C(9) 106.2(4) . . . ? N(1) P(1) C(15) 104.1(4) . . . ? C(9) P(1) C(15) 108.7(4) . . . ? Se(1) P(2) N(1) 108.0(3) . . . ? Se(1) P(2) C(21) 109.7(3) . . . ? Se(1) P(2) C(27) 105.4(3) . . . ? N(1) P(2) C(21) 111.3(4) . . . ? N(1) P(2) C(27) 111.3(4) . . . ? C(21) P(2) C(27) 110.8(4) . . . ? P(1) N(1) P(2) 116.4(4) . . . ? P(1) N(1) C(1) 116.3(6) . . . ? P(2) N(1) C(1) 127.2(6) . . . ? N(1) C(1) C(2) 111.6(7) . . . ? N(1) C(1) C(3) 114.3(7) . . . ? N(1) C(1) H(1) 105.9 . . . no C(2) C(1) C(3) 112.6(8) . . . ? C(2) C(1) H(1) 105.9 . . . no C(3) C(1) H(1) 105.9 . . . no C(1) C(2) H(2) 109.5 . . . no C(1) C(2) H(3) 109.5 . . . no C(1) C(2) H(4) 109.5 . . . no H(2) C(2) H(3) 109.5 . . . no H(2) C(2) H(4) 109.5 . . . no H(3) C(2) H(4) 109.5 . . . no C(1) C(3) C(4) 122.3(9) . . . ? C(1) C(3) C(8) 119.4(9) . . . ? C(4) C(3) C(8) 118.3(9) . . . ? C(3) C(4) C(5) 121.0(9) . . . ? C(3) C(4) H(5) 119.5 . . . no C(5) C(4) H(5) 119.5 . . . no C(4) C(5) C(6) 118.5(10) . . . ? C(4) C(5) H(6) 120.8 . . . no C(6) C(5) H(6) 120.8 . . . no C(5) C(6) C(7) 120.6(10) . . . ? C(5) C(6) H(7) 119.7 . . . no C(7) C(6) H(7) 119.7 . . . no C(6) C(7) C(8) 120.1(9) . . . ? C(6) C(7) H(8) 119.9 . . . no C(8) C(7) H(8) 119.9 . . . no C(3) C(8) C(7) 121.4(9) . . . ? C(3) C(8) H(9) 119.3 . . . no C(7) C(8) H(9) 119.3 . . . no P(1) C(9) C(10) 120.9(8) . . . ? P(1) C(9) C(14) 120.3(7) . . . ? C(10) C(9) C(14) 117.4(9) . . . ? C(9) C(10) C(11) 123.2(10) . . . ? C(9) C(10) H(10) 118.4 . . . no C(11) C(10) H(10) 118.4 . . . no C(10) C(11) C(12) 119.4(10) . . . ? C(10) C(11) H(11) 120.3 . . . no C(12) C(11) H(11) 120.3 . . . no C(11) C(12) C(13) 120.7(9) . . . ? C(11) C(12) H(12) 119.7 . . . no C(13) C(12) H(12) 119.7 . . . no C(12) C(13) C(14) 119.3(11) . . . ? C(12) C(13) H(13) 120.4 . . . no C(14) C(13) H(13) 120.4 . . . no C(9) C(14) C(13) 119.6(10) . . . ? C(9) C(14) H(14) 120.2 . . . no C(13) C(14) H(14) 120.2 . . . no P(1) C(15) C(16) 124.7(7) . . . ? P(1) C(15) C(20) 117.8(6) . . . ? C(16) C(15) C(20) 117.4(8) . . . ? C(15) C(16) C(17) 120.4(9) . . . ? C(15) C(16) H(15) 119.8 . . . no C(17) C(16) H(15) 119.8 . . . no C(16) C(17) C(18) 120.6(9) . . . ? C(16) C(17) H(16) 119.7 . . . no C(18) C(17) H(16) 119.7 . . . no C(17) C(18) C(19) 119.9(9) . . . ? C(17) C(18) H(17) 120.0 . . . no C(19) C(18) H(17) 120.0 . . . no C(18) C(19) C(20) 119.5(9) . . . ? C(18) C(19) H(18) 120.3 . . . no C(20) C(19) H(18) 120.3 . . . no C(15) C(20) C(19) 122.0(9) . . . ? C(15) C(20) H(19) 119.0 . . . no C(19) C(20) H(19) 119.0 . . . no P(2) C(21) C(22) 119.6(7) . . . ? P(2) C(21) C(26) 121.1(7) . . . ? C(22) C(21) C(26) 119.1(8) . . . ? C(21) C(22) C(23) 119.6(9) . . . ? C(21) C(22) H(20) 120.2 . . . no C(23) C(22) H(20) 120.2 . . . no C(22) C(23) C(24) 121.6(9) . . . ? C(22) C(23) H(21) 119.2 . . . no C(24) C(23) H(21) 119.2 . . . no C(23) C(24) C(25) 119.8(9) . . . ? C(23) C(24) H(22) 120.1 . . . no C(25) C(24) H(22) 120.1 . . . no C(24) C(25) C(26) 118.7(9) . . . ? C(24) C(25) H(23) 120.6 . . . no C(26) C(25) H(23) 120.6 . . . no C(21) C(26) C(25) 121.2(9) . . . ? C(21) C(26) H(24) 119.4 . . . no C(25) C(26) H(24) 119.4 . . . no P(2) C(27) C(28) 122.1(7) . . . ? P(2) C(27) C(32) 117.0(7) . . . ? C(28) C(27) C(32) 120.8(8) . . . ? C(27) C(28) C(29) 118.6(8) . . . ? C(27) C(28) H(25) 120.7 . . . no C(29) C(28) H(25) 120.7 . . . no C(28) C(29) C(30) 120.2(9) . . . ? C(28) C(29) H(26) 119.9 . . . no C(30) C(29) H(26) 119.9 . . . no C(29) C(30) C(31) 119.1(9) . . . ? C(29) C(30) H(27) 120.5 . . . no C(31) C(30) H(27) 120.5 . . . no C(30) C(31) C(32) 122.9(9) . . . ? C(30) C(31) H(28) 118.6 . . . no C(32) C(31) H(28) 118.6 . . . no C(27) C(32) C(31) 118.4(8) . . . ? C(27) C(32) H(29) 120.8 . . . no C(31) C(32) H(29) 120.8 . . . no #-------------------------------------------------------------------------- #-- 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 Cl(1) C(29) 3.524(11) . 1_655 no Cl(1) C(30) 3.534(11) . 1_655 no Cl(1) C(23) 3.563(10) . 2_655 no Cl(2) C(30) 3.524(11) . 1_655 no Cl(2) C(6) 3.544(11) . 4_655 no #-------------------------------------------------------------------------- #-- 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd(1) Se(1) P(2) N(1) . . . . 34.5(3) no Pd(1) Se(1) P(2) C(21) . . . . -87.0(3) no Pd(1) Se(1) P(2) C(27) . . . . 153.6(3) no Pd(1) P(1) N(1) P(2) . . . . 16.5(5) no Pd(1) P(1) N(1) C(1) . . . . -167.0(4) no Pd(1) P(1) C(9) C(10) . . . . -83.8(9) no Pd(1) P(1) C(9) C(14) . . . . 82.7(7) no Pd(1) P(1) C(15) C(16) . . . . -149.1(8) no Pd(1) P(1) C(15) C(20) . . . . 33.8(9) no Se(1) Pd(1) P(1) N(1) . . . . 7.5(3) no Se(1) Pd(1) P(1) C(9) . . . . 129.5(4) no Se(1) Pd(1) P(1) C(15) . . . . -108.0(3) no Se(1) P(2) N(1) P(1) . . . . -34.6(5) no Se(1) P(2) N(1) C(1) . . . . 149.4(6) no Se(1) P(2) C(21) C(22) . . . . 15.4(8) no Se(1) P(2) C(21) C(26) . . . . -169.9(6) no Se(1) P(2) C(27) C(28) . . . . 119.6(7) no Se(1) P(2) C(27) C(32) . . . . -55.7(7) no Cl(1) Pd(1) Se(1) P(2) . . . . -116.6(14) no Cl(1) Pd(1) P(1) N(1) . . . . -175.7(3) no Cl(1) Pd(1) P(1) C(9) . . . . -53.6(4) no Cl(1) Pd(1) P(1) C(15) . . . . 68.9(3) no Cl(2) Pd(1) Se(1) P(2) . . . . 163.33(9) no Cl(2) Pd(1) P(1) N(1) . . . . 87.0(11) no Cl(2) Pd(1) P(1) C(9) . . . . -150.9(11) no Cl(2) Pd(1) P(1) C(15) . . . . -28.4(12) no P(1) Pd(1) Se(1) P(2) . . . . -21.70(9) no P(1) N(1) P(2) C(21) . . . . 85.9(5) no P(1) N(1) P(2) C(27) . . . . -149.9(4) no P(1) N(1) C(1) C(2) . . . . 96.6(8) no P(1) N(1) C(1) C(3) . . . . -134.3(7) no P(1) C(9) C(10) C(11) . . . . 174.5(8) no P(1) C(9) C(14) C(13) . . . . -174.0(8) no P(1) C(15) C(16) C(17) . . . . -174.4(9) no P(1) C(15) C(20) C(19) . . . . 173.6(10) no P(2) N(1) P(1) C(9) . . . . -110.3(5) no P(2) N(1) P(1) C(15) . . . . 135.0(4) no P(2) N(1) C(1) C(2) . . . . -87.4(9) no P(2) N(1) C(1) C(3) . . . . 41.8(10) no P(2) C(21) C(22) C(23) . . . . 173.9(8) no P(2) C(21) C(26) C(25) . . . . -174.3(7) no P(2) C(27) C(28) C(29) . . . . -176.9(7) no P(2) C(27) C(32) C(31) . . . . 177.9(7) no N(1) P(1) C(9) C(10) . . . . 41.9(9) no N(1) P(1) C(9) C(14) . . . . -151.6(7) no N(1) P(1) C(15) C(16) . . . . 89.9(9) no N(1) P(1) C(15) C(20) . . . . -87.2(9) no N(1) P(2) C(21) C(22) . . . . -104.1(8) no N(1) P(2) C(21) C(26) . . . . 70.6(8) no N(1) P(2) C(27) C(28) . . . . -123.5(8) no N(1) P(2) C(27) C(32) . . . . 61.2(8) no N(1) C(1) C(3) C(4) . . . . -98.5(10) no N(1) C(1) C(3) C(8) . . . . 84.9(10) no C(1) N(1) P(1) C(9) . . . . 66.2(6) no C(1) N(1) P(1) C(15) . . . . -48.5(6) no C(1) N(1) P(2) C(21) . . . . -90.2(7) no C(1) N(1) P(2) C(27) . . . . 34.1(8) no C(1) C(3) C(4) C(5) . . . . -178.6(9) no C(1) C(3) C(8) C(7) . . . . 179.2(8) no C(2) C(1) C(3) C(4) . . . . 30.2(12) no C(2) C(1) C(3) C(8) . . . . -146.4(8) no C(3) C(4) C(5) C(6) . . . . -0.4(15) no C(3) C(8) C(7) C(6) . . . . -0.5(15) no C(4) C(3) C(8) C(7) . . . . 2.4(14) no C(4) C(5) C(6) C(7) . . . . 2.4(16) no C(5) C(4) C(3) C(8) . . . . -1.9(14) no C(5) C(6) C(7) C(8) . . . . -2.0(16) no C(9) P(1) C(15) C(16) . . . . -23.0(10) no C(9) P(1) C(15) C(20) . . . . 159.9(9) no C(9) C(10) C(11) C(12) . . . . -4.6(17) no C(9) C(14) C(13) C(12) . . . . 3.8(16) no C(10) C(9) P(1) C(15) . . . . 153.4(8) no C(10) C(9) C(14) C(13) . . . . -7.0(14) no C(10) C(11) C(12) C(13) . . . . 0.9(18) no C(11) C(10) C(9) C(14) . . . . 7.6(16) no C(11) C(12) C(13) C(14) . . . . -0.7(18) no C(14) C(9) P(1) C(15) . . . . -40.1(9) no C(15) C(16) C(17) C(18) . . . . 0.5(18) no C(15) C(20) C(19) C(18) . . . . 1.6(20) no C(16) C(15) C(20) C(19) . . . . -3.7(17) no C(16) C(17) C(18) C(19) . . . . -2.7(19) no C(17) C(16) C(15) C(20) . . . . 2.6(16) no C(17) C(18) C(19) C(20) . . . . 1.7(19) no C(21) P(2) C(27) C(28) . . . . 1.0(9) no C(21) P(2) C(27) C(32) . . . . -174.3(6) no C(21) C(22) C(23) C(24) . . . . 1.0(16) no C(21) C(26) C(25) C(24) . . . . 0.1(14) no C(22) C(21) P(2) C(27) . . . . 131.4(8) no C(22) C(21) C(26) C(25) . . . . 0.5(14) no C(22) C(23) C(24) C(25) . . . . -0.4(16) no C(23) C(22) C(21) C(26) . . . . -1.0(15) no C(23) C(24) C(25) C(26) . . . . -0.1(15) no C(26) C(21) P(2) C(27) . . . . -53.9(8) no C(27) C(28) C(29) C(30) . . . . 0.0(14) no C(27) C(32) C(31) C(30) . . . . -1.7(15) no C(28) C(27) C(32) C(31) . . . . 2.6(13) no C(28) C(29) C(30) C(31) . . . . 0.9(14) no C(29) C(28) C(27) C(32) . . . . -1.8(14) no C(29) C(30) C(31) C(32) . . . . -0.1(15) no #-------------------------------------------------------------------------- #-- #========================================================================== #== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== #== # End of CIF #========================================================================== #== data__2123PtCl2[(S)PhMeHCN-PSe] _database_code_CSD 175776 #========================================================================== #== _audit_creation_date '2001-06-26' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 999)' #-------------------------------------------------------------------------- #-- _cell_length_a 11.8948(4) _cell_length_b 15.3216(5) _cell_length_c 16.8763(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3075.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------------- #-- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #-------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 834.49 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H29 Cl2 N P2 Pt Se ' _chemical_formula_moiety 'C32 H29 Cl2 N P2 Pt Se ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1616.00 _exptl_absorpt_coefficient_mu 6.028 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.327 _exptl_absorpt_correction_T_max 0.507 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 17433 _reflns_number_total 8171 _reflns_number_gt 2641 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06987 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 28.40 _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 C 0 128 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 116 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 4 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #========================================================================== #== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.72106(4) 0.10416(3) 0.39547(3) 0.02381(11) 1.000 . Uani d ? Se(1) 0.55519(11) 0.17937(8) 0.35833(8) 0.0279(3) 1.000 . Uani d ? Cl(1) 0.8874(3) 0.0393(2) 0.4349(2) 0.0398(10) 1.000 . Uani d ? Cl(2) 0.8219(3) 0.2228(2) 0.3494(2) 0.0329(9) 1.000 . Uani d ? P(1) 0.6274(3) -0.0015(2) 0.4475(2) 0.0261(9) 1.000 . Uani d ? P(2) 0.4424(3) 0.0714(2) 0.3575(2) 0.0228(8) 1.000 . Uani d ? N(1) 0.4849(9) 0.0049(6) 0.4314(6) 0.027(3) 1.000 . Uani d ? C(1) 0.4090(11) -0.0558(8) 0.4785(8) 0.030(4) 1.000 . Uani d ? C(2) 0.3597(12) -0.0102(9) 0.5515(9) 0.044(5) 1.000 . Uani d ? C(3) 0.3168(11) -0.0993(9) 0.4305(8) 0.032(4) 1.000 . Uani d ? C(4) 0.2073(12) -0.0704(8) 0.4269(8) 0.035(4) 1.000 . Uani d ? C(5) 0.1273(11) -0.1150(9) 0.3836(11) 0.051(5) 1.000 . Uani d ? C(6) 0.155(2) -0.1862(10) 0.3437(10) 0.050(5) 1.000 . Uani d ? C(7) 0.2651(13) -0.2171(8) 0.3481(8) 0.038(4) 1.000 . Uani d ? C(8) 0.3422(11) -0.1728(8) 0.3917(9) 0.037(4) 1.000 . Uani d ? C(9) 0.6711(11) -0.1040(9) 0.4126(8) 0.037(4) 1.000 . Uani d ? C(10) 0.6282(12) -0.1367(9) 0.3451(8) 0.036(4) 1.000 . Uani d ? C(11) 0.664(1) -0.2128(10) 0.3133(10) 0.050(5) 1.000 . Uani d ? C(12) 0.756(2) -0.2544(10) 0.3505(10) 0.066(6) 1.000 . Uani d ? C(13) 0.809(2) -0.2226(9) 0.4183(10) 0.065(6) 1.000 . Uani d ? C(14) 0.765(2) -0.1449(9) 0.4490(10) 0.057(5) 1.000 . Uani d ? C(15) 0.6396(10) 0.0008(7) 0.5559(7) 0.023(3) 1.000 . Uani d ? C(16) 0.6367(11) -0.0703(7) 0.6023(8) 0.031(3) 1.000 . Uani d ? C(17) 0.6407(13) -0.0618(9) 0.6842(9) 0.044(5) 1.000 . Uani d ? C(18) 0.640(1) 0.0170(10) 0.7196(8) 0.048(5) 1.000 . Uani d ? C(19) 0.644(2) 0.0867(9) 0.6717(10) 0.057(5) 1.000 . Uani d ? C(20) 0.645(1) 0.0792(9) 0.5903(9) 0.048(5) 1.000 . Uani d ? C(21) 0.4447(11) 0.0189(8) 0.2612(7) 0.026(3) 1.000 . Uani d ? C(22) 0.5342(11) 0.0374(9) 0.2094(8) 0.036(4) 1.000 . Uani d ? C(23) 0.5421(12) -0.0087(10) 0.1405(8) 0.044(4) 1.000 . Uani d ? C(24) 0.4626(12) -0.0682(9) 0.1182(9) 0.042(4) 1.000 . Uani d ? C(25) 0.3739(11) -0.0855(8) 0.1702(8) 0.033(4) 1.000 . Uani d ? C(26) 0.3653(10) -0.0418(8) 0.2417(8) 0.026(4) 1.000 . Uani d ? C(27) 0.3071(8) 0.1145(8) 0.3772(6) 0.019(3) 1.000 . Uani d ? C(28) 0.2165(11) 0.1079(8) 0.3242(7) 0.031(3) 1.000 . Uani d ? C(29) 0.1126(12) 0.1460(8) 0.3411(8) 0.031(4) 1.000 . Uani d ? C(30) 0.0991(11) 0.1896(8) 0.4128(8) 0.033(4) 1.000 . Uani d ? C(31) 0.1913(11) 0.1980(8) 0.4643(8) 0.036(4) 1.000 . Uani d ? C(32) 0.2936(10) 0.1614(8) 0.4463(7) 0.025(3) 1.000 . Uani d ? H(1) 0.4557 -0.1014 0.4978 0.035 1.000 . Uiso c ? H(2) 0.3895 -0.0361 0.5981 0.052 1.000 . Uiso c ? H(3) 0.3789 0.0499 0.5503 0.052 1.000 . Uiso c ? H(4) 0.2802 -0.0163 0.5513 0.052 1.000 . Uiso c ? H(5) 0.1864 -0.0191 0.4548 0.042 1.000 . Uiso c ? H(6) 0.0520 -0.0945 0.3824 0.061 1.000 . Uiso c ? H(7) 0.1010 -0.2158 0.3124 0.060 1.000 . Uiso c ? H(8) 0.2860 -0.2688 0.3207 0.046 1.000 . Uiso c ? H(9) 0.4167 -0.1949 0.3948 0.044 1.000 . Uiso c ? H(10) 0.5704 -0.1053 0.3188 0.043 1.000 . Uiso c ? H(11) 0.6295 -0.2371 0.2677 0.060 1.000 . Uiso c ? H(12) 0.7838 -0.3070 0.3280 0.080 1.000 . Uiso c ? H(13) 0.8704 -0.2518 0.4422 0.078 1.000 . Uiso c ? H(14) 0.7981 -0.1193 0.4946 0.069 1.000 . Uiso c ? H(15) 0.6320 -0.1267 0.5791 0.037 1.000 . Uiso c ? H(16) 0.6439 -0.1128 0.7161 0.052 1.000 . Uiso c ? H(17) 0.6367 0.0228 0.7756 0.057 1.000 . Uiso c ? H(18) 0.6472 0.1433 0.6947 0.068 1.000 . Uiso c ? H(19) 0.6484 0.1303 0.5584 0.058 1.000 . Uiso c ? H(20) 0.5880 0.0810 0.2221 0.043 1.000 . Uiso c ? H(21) 0.6050 0.0009 0.1069 0.053 1.000 . Uiso c ? H(22) 0.4674 -0.0971 0.0685 0.050 1.000 . Uiso c ? H(23) 0.3189 -0.1277 0.1563 0.040 1.000 . Uiso c ? H(24) 0.3048 -0.0539 0.2769 0.031 1.000 . Uiso c ? H(25) 0.2261 0.0769 0.2759 0.037 1.000 . Uiso c ? H(26) 0.0523 0.1422 0.3043 0.038 1.000 . Uiso c ? H(27) 0.0281 0.2135 0.4268 0.040 1.000 . Uiso c ? H(28) 0.1827 0.2295 0.5124 0.044 1.000 . Uiso c ? H(29) 0.3553 0.1684 0.4815 0.030 1.000 . Uiso c ? 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) 0.0273(2) 0.0259(2) 0.0183(2) 0.0055(2) -0.0036(3) 0.0024(2) Se(1) 0.0285(7) 0.0189(6) 0.0364(8) -0.0011(6) -0.0084(7) .0009(6) Cl(1) 0.036(2) 0.049(2) 0.034(2) 0.014(2) -0.004(2) .005(2) Cl(2) 0.028(2) 0.037(2) 0.034(2) 0.000(1) 0.004(2) .001(2) P(1) 0.038(2) 0.020(2) 0.020(2) 0.006(2) -0.007(2) 0.000(2) P(2) 0.026(2) 0.019(2) 0.023(2) -0.004(1) -0.004(2) 0.002(1) N(1) 0.043(6) 0.019(5) 0.020(6) 0.007(5) 0.002(5) 0.001(5) C(1) 0.041(8) 0.016(6) 0.031(8) -0.003(6) 0.001(7) .008(6) C(2) 0.051(9) 0.043(9) 0.037(9) -0.021(8) -0.009(8) .003(8) C(3) 0.040(8) 0.021(7) 0.035(7) -0.007(7) 0.012(6) 0.003(7) C(4) 0.047(9) 0.032(7) 0.027(7) -0.003(7) -0.001(8) .001(6) C(5) 0.039(8) 0.030(8) 0.085(13) -0.007(7) -0.012(9) 0.005(10) C(6) 0.066(11) 0.028(8) 0.055(11) -0.008(8) 0.005(9) 0.007(8) C(7) 0.052(9) 0.024(7) 0.037(8) -0.010(8) -0.001(8) 0.001(6) C(8) 0.043(8) 0.034(7) 0.033(7) -0.009(7) 0.007(8) 0.008(8) C(9) 0.039(7) 0.036(7) 0.038(9) 0.006(7) -0.006(6) 0.001(8) C(10) 0.050(9) 0.036(8) 0.023(8) 0.000(7) -0.015(7) .002(6) C(11) 0.065(11) 0.048(10) 0.038(9) 0.019(9) -0.002(9) 0.020(8) C(12) 0.10(2) 0.041(9) 0.058(11) 0.031(10) 0.015(11) 0.021(8) C(13) 0.11(2) 0.034(8) 0.050(11) 0.024(10) -0.004(11) .000(8) C(14) 0.076(12) 0.041(8) 0.055(10) 0.011(9) 0.003(11) 0.003(8) C(15) 0.027(7) 0.014(6) 0.029(7) 0.004(5) -0.018(6) .006(6) C(16) 0.045(8) 0.027(6) 0.021(6) 0.001(6) 0.002(8) .002(7) C(17) 0.057(10) 0.039(8) 0.035(9) 0.016(8) -0.002(9) .013(8) C(18) 0.071(12) 0.056(10) 0.016(8) 0.009(10) -0.005(8) .003(8) C(19) 0.10(1) 0.037(9) 0.035(9) 0.004(10) -0.004(10) 0.007(8) C(20) 0.081(12) 0.034(8) 0.030(9) 0.008(8) -0.012(9) .004(7) C(21) 0.032(7) 0.028(7) 0.019(7) 0.002(7) 0.000(6) 0.003(6) C(22) 0.035(8) 0.038(8) 0.034(9) -0.014(7) 0.000(7) 0.002(7) C(23) 0.044(9) 0.063(10) 0.025(7) -0.002(8) 0.009(7) 0.007(8) C(24) 0.050(9) 0.042(8) 0.033(9) -0.005(7) -0.001(8) 0.015(7) C(25) 0.039(8) 0.030(8) 0.030(7) -0.018(6) -0.005(7) 0.008(6) C(26) 0.029(7) 0.023(7) 0.027(7) -0.002(6) 0.000(6) .007(6) C(27) 0.017(6) 0.026(6) 0.013(6) -0.000(5) -0.004(4) 0.005(5) C(28) 0.036(7) 0.027(6) 0.030(7) -0.009(8) 0.001(7) 0.002(7) C(29) 0.039(8) 0.032(7) 0.024(8) -0.003(7) -0.005(7) .008(6) C(30) 0.035(7) 0.022(7) 0.043(10) 0.003(6) -0.003(7) .002(7) C(31) 0.042(9) 0.030(8) 0.038(8) -0.008(7) 0.009(7) .002(7) C(32) 0.019(7) 0.028(7) 0.027(7) -0.001(6) 0.000(6) .001(6) #========================================================================== #== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Wrong R = 0.0555; Rw = 0.0632' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2641 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.037 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_all 0.039 _refine_ls_wR_factor_ref 0.039 _refine_ls_goodness_of_fit_all 0.920 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.33 _refine_diff_density_max 1.12 #========================================================================== #== # MOLECULAR GEOMETRY _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 PT1 SE1 2.3692(13) . . ? PT1 CL1 2.313(3) . . ? PT1 CL2 2.312(3) . . ? PT1 P1 2.152(3) . . ? SE1 P2 2.129(3) . . ? P1 N1 1.720(10) . . ? P1 C9 1.76(1) . . ? P1 C15 1.834(12) . . ? P2 N1 1.688(10) . . ? P2 C21 1.814(12) . . ? P2 C27 1.771(10) . . ? N1 C1 1.52(1) . . ? C1 C2 1.53(2) . . ? C1 C3 1.52(2) . . ? C1 H1 0.95 . . no C2 H2 0.95 . . no C2 H3 0.95 . . no C2 H4 0.95 . . no C3 C4 1.38(2) . . ? C3 C8 1.34(2) . . ? C4 C5 1.38(2) . . ? C4 H5 0.95 . . no C5 C6 1.32(2) . . ? C5 H6 0.95 . . no C6 C7 1.39(2) . . ? C6 H7 0.95 . . no C7 C8 1.36(2) . . ? C7 H8 0.95 . . no C8 H9 0.95 . . no C9 C10 1.34(2) . . ? C9 C14 1.42(2) . . ? C10 C11 1.35(2) . . ? C10 H10 0.95 . . no C11 C12 1.41(2) . . ? C11 H11 0.95 . . no C12 C13 1.39(2) . . ? C12 H12 0.95 . . no C13 C14 1.40(2) . . ? C13 H13 0.95 . . no C14 H14 0.95 . . no C15 C16 1.34(2) . . ? C15 C20 1.34(2) . . ? C16 C17 1.39(2) . . ? C16 H15 0.95 . . no C17 C18 1.35(2) . . ? C17 H16 0.95 . . no C18 C19 1.34(2) . . ? C18 H17 0.95 . . no C19 C20 1.38(2) . . ? C19 H18 0.95 . . no C20 H19 0.95 . . no C21 C22 1.41(2) . . ? C21 C26 1.37(2) . . ? C22 C23 1.36(2) . . ? C22 H20 0.95 . . no C23 C24 1.37(2) . . ? C23 H21 0.95 . . no C24 C25 1.40(2) . . ? C24 H22 0.95 . . no C25 C26 1.38(2) . . ? C25 H23 0.95 . . no C26 H24 0.95 . . no C27 C28 1.40(2) . . ? C27 C32 1.38(1) . . ? C28 C29 1.40(2) . . ? C28 H25 0.95 . . no C29 C30 1.39(2) . . ? C29 H26 0.95 . . no C30 C31 1.41(2) . . ? C30 H27 0.95 . . no C31 C32 1.37(2) . . ? C31 H28 0.95 . . no C32 H29 0.95 . . no #-------------------------------------------------------------------------- #-- 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 SE1 PT1 CL1 176.25(10) . . . ? SE1 PT1 CL2 87.76(8) . . . ? SE1 PT1 P1 92.44(9) . . . ? CL1 PT1 CL2 89.46(12) . . . ? CL1 PT1 P1 90.14(12) . . . ? CL2 PT1 P1 175.43(12) . . . ? PT1 SE1 P2 98.54(10) . . . ? PT1 P1 N1 113.8(4) . . . ? PT1 P1 C9 112.5(5) . . . ? PT1 P1 C15 110.6(4) . . . ? N1 P1 C9 106.8(6) . . . ? N1 P1 C15 103.6(5) . . . ? C9 P1 C15 109.2(6) . . . ? SE1 P2 N1 106.0(4) . . . ? SE1 P2 C21 109.9(4) . . . ? SE1 P2 C27 106.4(4) . . . ? N1 P2 C21 112.9(5) . . . ? N1 P2 C27 111.0(5) . . . ? C21 P2 C27 110.3(5) . . . ? P1 N1 P2 116.5(6) . . . ? P1 N1 C1 117.9(7) . . . ? P2 N1 C1 125.3(8) . . . ? N1 C1 C2 111.6(9) . . . ? N1 C1 C3 114.8(10) . . . ? N1 C1 H1 106.4 . . . no C2 C1 C3 110.6(10) . . . ? C2 C1 H1 106.4 . . . no C3 C1 H1 106.4 . . . no C1 C2 H2 109.5 . . . no C1 C2 H3 109.5 . . . no C1 C2 H4 109.5 . . . no H2 C2 H3 109.5 . . . no H2 C2 H4 109.5 . . . no H3 C2 H4 109.5 . . . no C1 C3 C4 124.5(11) . . . ? C1 C3 C8 117.9(11) . . . ? C4 C3 C8 117.6(12) . . . ? C3 C4 C5 121.1(12) . . . ? C3 C4 H5 119.4 . . . no C5 C4 H5 119.4 . . . no C4 C5 C6 120.2(14) . . . ? C4 C5 H6 119.9 . . . no C6 C5 H6 119.9 . . . no C5 C6 C7 119.3(15) . . . ? C5 C6 H7 120.4 . . . no C7 C6 H7 120.3 . . . no C6 C7 C8 119.6(13) . . . ? C6 C7 H8 120.2 . . . no C8 C7 H8 120.2 . . . no C3 C8 C7 122.2(13) . . . ? C3 C8 H9 118.9 . . . no C7 C8 H9 118.9 . . . no P1 C9 C10 120.4(11) . . . ? P1 C9 C14 118.9(10) . . . ? C10 C9 C14 119.9(13) . . . ? C9 C10 C11 122.5(14) . . . ? C9 C10 H10 118.7 . . . no C11 C10 H10 118.7 . . . no C10 C11 C12 117.2(14) . . . ? C10 C11 H11 121.4 . . . no C12 C11 H11 121.4 . . . no C11 C12 C13 123.7(13) . . . ? C11 C12 H12 118.2 . . . no C13 C12 H12 118.2 . . . no C12 C13 C14 115.8(16) . . . ? C12 C13 H13 122.1 . . . no C14 C13 H13 122.1 . . . no C9 C14 C13 120.6(15) . . . ? C9 C14 H14 119.7 . . . no C13 C14 H14 119.7 . . . no P1 C15 C16 124.3(9) . . . ? P1 C15 C20 117.0(9) . . . ? C16 C15 C20 118.5(12) . . . ? C15 C16 C17 120.2(11) . . . ? C15 C16 H15 119.9 . . . no C17 C16 H15 119.9 . . . no C16 C17 C18 121.7(12) . . . ? C16 C17 H16 119.1 . . . no C18 C17 H16 119.1 . . . no C17 C18 C19 116.5(13) . . . ? C17 C18 H17 121.7 . . . no C19 C18 H17 121.7 . . . no C18 C19 C20 122.3(14) . . . ? C18 C19 H18 118.8 . . . no C20 C19 H18 118.8 . . . no C15 C20 C19 120.5(13) . . . ? C15 C20 H19 119.7 . . . no C19 C20 H19 119.7 . . . no P2 C21 C22 118.7(9) . . . ? P2 C21 C26 120.5(9) . . . ? C22 C21 C26 120.7(11) . . . ? C21 C22 C23 118.6(12) . . . ? C21 C22 H20 120.7 . . . no C23 C22 H20 120.7 . . . no C22 C23 C24 122.2(13) . . . ? C22 C23 H21 118.9 . . . no C24 C23 H21 118.9 . . . no C23 C24 C25 118.3(12) . . . ? C23 C24 H22 120.8 . . . no C25 C24 H22 120.8 . . . no C24 C25 C26 120.9(11) . . . ? C24 C25 H23 119.6 . . . no C26 C25 H23 119.6 . . . no C21 C26 C25 119.2(12) . . . ? C21 C26 H24 120.4 . . . no C25 C26 H24 120.4 . . . no P2 C27 C28 123.4(8) . . . ? P2 C27 C32 117.3(8) . . . ? C28 C27 C32 119.2(10) . . . ? C27 C28 C29 121.2(10) . . . ? C27 C28 H25 119.4 . . . no C29 C28 H25 119.4 . . . no C28 C29 C30 118.7(12) . . . ? C28 C29 H26 120.6 . . . no C30 C29 H26 120.6 . . . no C29 C30 C31 119.5(12) . . . ? C29 C30 H27 120.3 . . . no C31 C30 H27 120.3 . . . no C30 C31 C32 121.1(12) . . . ? C30 C31 H28 119.4 . . . no C32 C31 H28 119.4 . . . no C27 C32 C31 120.2(11) . . . ? C27 C32 H29 119.9 . . . no C31 C32 H29 119.9 . . . no #-------------------------------------------------------------------------- #-- 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 C20 C31 3.58(2) . 3_556 no C20 C30 3.58(2) . 3_556 no #-------------------------------------------------------------------------- #-- 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag PT1 SE1 P2 N1 . . . . 34.9(4) no PT1 SE1 P2 C21 . . . . -87.4(4) no PT1 SE1 P2 C27 . . . . 153.1(4) no PT1 P1 N1 P2 . . . . 17.6(7) no PT1 P1 N1 C1 . . . . -168.4(7) no PT1 P1 C9 C10 . . . . -85.5(12) no PT1 P1 C9 C14 . . . . 84.2(11) no PT1 P1 C15 C16 . . . . -149.1(10) no PT1 P1 C15 C20 . . . . 35.2(12) no SE1 PT1 P1 N1 . . . . 7.0(4) no SE1 PT1 P1 C9 . . . . 128.6(5) no SE1 PT1 P1 C15 . . . . -109.1(4) no SE1 P2 N1 P1 . . . . -35.4(6) no SE1 P2 N1 C1 . . . . 151.1(8) no SE1 P2 C21 C22 . . . . 16.2(11) no SE1 P2 C21 C26 . . . . -168.3(9) no SE1 P2 C27 C28 . . . . 118.9(10) no SE1 P2 C27 C32 . . . . -56.8(10) no CL1 PT1 SE1 P2 . . . . -155.6(15) no CL1 PT1 P1 N1 . . . . -175.7(4) no CL1 PT1 P1 C9 . . . . -54.1(5) no CL1 PT1 P1 C15 . . . . 68.2(4) no CL2 PT1 SE1 P2 . . . . 162.22(12) no CL2 PT1 P1 N1 . . . . 99.4(15) no CL2 PT1 P1 C9 . . . . -139.0(15) no CL2 PT1 P1 C15 . . . . -16.7(17) no P1 PT1 SE1 P2 . . . . -22.35(13) no P1 N1 P2 C21 . . . . 85.0(7) no P1 N1 P2 C27 . . . . -150.6(6) no P1 N1 C1 C2 . . . . 97.2(10) no P1 N1 C1 C3 . . . . -135.9(9) no P1 C9 C10 C11 . . . . 175.7(11) no P1 C9 C14 C13 . . . . -174.0(12) no P1 C15 C16 C17 . . . . -176.6(11) no P1 C15 C20 C19 . . . . 174.5(13) no P2 N1 P1 C9 . . . . -107.1(7) no P2 N1 P1 C15 . . . . 137.7(6) no P2 N1 C1 C2 . . . . -89.3(12) no P2 N1 C1 C3 . . . . 37.6(13) no P2 C21 C22 C23 . . . . 173.4(11) no P2 C21 C26 C25 . . . . -175.3(10) no P2 C27 C28 C29 . . . . -177.4(9) no P2 C27 C32 C31 . . . . 178.7(9) no N1 P1 C9 C10 . . . . 40.0(13) no N1 P1 C9 C14 . . . . -150.3(11) no N1 P1 C15 C16 . . . . 88.6(12) no N1 P1 C15 C20 . . . . -87.0(12) no N1 P2 C21 C22 . . . . -102.0(10) no N1 P2 C21 C26 . . . . 73.6(11) no N1 P2 C27 C28 . . . . -126.2(10) no N1 P2 C27 C32 . . . . 58.1(10) no N1 C1 C3 C4 . . . . -98.1(14) no N1 C1 C3 C8 . . . . 85.0(14) no C1 N1 P1 C9 . . . . 66.9(9) no C1 N1 P1 C15 . . . . -48.3(9) no C1 N1 P2 C21 . . . . -88.5(10) no C1 N1 P2 C27 . . . . 35.9(10) no C1 C3 C4 C5 . . . . -178.2(13) no C1 C3 C8 C7 . . . . 179.2(12) no C2 C1 C3 C4 . . . . 29.3(17) no C2 C1 C3 C8 . . . . -147.6(12) no C3 C4 C5 C6 . . . . -0.8(22) no C3 C8 C7 C6 . . . . -0.7(21) no C4 C3 C8 C7 . . . . 2.0(20) no C4 C5 C6 C7 . . . . 2.1(23) no C5 C4 C3 C8 . . . . -1.3(20) no C5 C6 C7 C8 . . . . -1.4(22) no C9 P1 C15 C16 . . . . -24.9(13) no C9 P1 C15 C20 . . . . 159.5(12) no C9 C10 C11 C12 . . . . -4.7(22) no C9 C14 C13 C12 . . . . 1.3(23) no C10 C9 P1 C15 . . . . 151.4(11) no C10 C9 C14 C13 . . . . -4.3(22) no C10 C11 C12 C13 . . . . 1.6(25) no C11 C10 C9 C14 . . . . 6.1(22) no C11 C12 C13 C14 . . . . 0.0(25) no C14 C9 P1 C15 . . . . -38.9(13) no C15 C16 C17 C18 . . . . 4.4(23) no C15 C20 C19 C18 . . . . 0.5(29) no C16 C15 C20 C19 . . . . -1.4(24) no C16 C17 C18 C19 . . . . -5.1(25) no C17 C16 C15 C20 . . . . -1.0(21) no C17 C18 C19 C20 . . . . 2.7(27) no C21 P2 C27 C28 . . . . -0.2(12) no C21 P2 C27 C32 . . . . -176.0(9) no C21 C22 C23 C24 . . . . 4.0(22) no C21 C26 C25 C24 . . . . 0.1(19) no C22 C21 P2 C27 . . . . 133.2(10) no C22 C21 C26 C25 . . . . 0.2(18) no C22 C23 C24 C25 . . . . -3.7(22) no C23 C22 C21 C26 . . . . -2.2(20) no C23 C24 C25 C26 . . . . 1.6(20) no C26 C21 P2 C27 . . . . -51.2(11) no C27 C28 C29 C30 . . . . -1.3(19) no C27 C32 C31 C30 . . . . -0.8(18) no C28 C27 C32 C31 . . . . 2.7(17) no C28 C29 C30 C31 . . . . 3.2(18) no C29 C28 C27 C32 . . . . -1.7(18) no C29 C30 C31 C32 . . . . -2.2(19) no #-------------------------------------------------------------------------- #-- #========================================================================== #== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== #== # End of CIF #========================================================================== #== data__2113PtCl2[phenethylN(PS)] _database_code_CSD 175777 #========================================================================== #== _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 999)' #-------------------------------------------------------------------------- #-- _cell_length_a 10.2048(3) _cell_length_b 16.3146(9) _cell_length_c 11.7788(5) _cell_angle_alpha 90 _cell_angle_beta 96.615(3) _cell_angle_gamma 90 _cell_volume 1947.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 183.2 _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 'P21' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #-------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1026.35 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H31 Cl8 N P2 Pt S ' _chemical_formula_moiety 'C32 H29 Cl2 N P2 Pt S, 2C H Cl3)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1004.00 _exptl_absorpt_coefficient_mu 4.298 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 12258 _reflns_number_total 7557 _reflns_number_gt 3685 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05745 _diffrn_reflns_av_sigmaI/netI 0.096 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.54 _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 C 0 68 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 62 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt 0 2 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 2 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 2 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #========================================================================== #== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) -0.20224(3) 0.5000 0.01362(3) 0.02057(9) 1.000 . Uani d ? Cl(1) -0.1212(3) 0.5501(2) -0.1493(2) 0.0342(8) 1.000 . Uani d ? Cl(2) -0.3619(3) 0.4227(2) -0.0989(3) 0.0366(9) 1.000 . Uani d ? Cl(3) 0.4030(4) 0.2830(3) 0.6678(4) 0.0612(13) 1.000 . Uani d ? Cl(4) 0.6618(4) 0.2290(3) 0.6253(4) 0.0597(12) 1.000 . Uani d ? Cl(5) 0.5479(5) 0.1678(3) 0.8193(5) 0.083(2) 1.000 . Uani d ? Cl(6) 0.6934(5) 0.1950(3) 0.3116(5) 0.082(2) 1.000 . Uani d ? Cl(7) 0.4977(5) 0.3155(3) 0.3529(4) 0.072(2) 1.000 . Uani d ? Cl(8) 0.4474(6) 0.2016(5) 0.1668(5) 0.103(2) 1.000 . Uani d ? S(1) -0.2997(3) 0.4641(2) 0.1692(3) 0.0287(8) 1.000 . Uani d ? P(1) -0.0484(3) 0.5716(2) 0.1179(2) 0.0199(7) 1.000 . Uani d ? P(2) -0.1469(3) 0.4728(2) 0.2932(2) 0.0218(7) 1.000 . Uani d ? N(1) -0.0556(8) 0.5550(6) 0.2618(8) 0.025(3) 1.000 . Uani d ? C(1) 0.0350(12) 0.6060(8) 0.3485(10) 0.026(3) 1.000 . Uani d ? C(2) -0.0394(12) 0.6814(7) 0.3823(10) 0.029(3) 1.000 . Uani d ? C(3) 0.1049(10) 0.5619(6) 0.4478(9) 0.019(3) 1.000 . Uani d ? C(4) 0.0560(11) 0.5547(9) 0.5527(10) 0.034(4) 1.000 . Uani d ? C(5) 0.1265(12) 0.5148(8) 0.6451(10) 0.033(4) 1.000 . Uani d ? C(6) 0.2469(13) 0.4810(8) 0.6327(11) 0.043(4) 1.000 . Uani d ? C(7) 0.3000(10) 0.4885(13) 0.5317(10) 0.036(4) 1.000 . Uani d ? C(8) 0.2322(11) 0.5287(8) 0.4393(10) 0.030(3) 1.000 . Uani d ? C(9) 0.1187(10) 0.5464(7) 0.0906(9) 0.022(3) 1.000 . Uani d ? C(10) 0.1878(11) 0.4836(7) 0.1520(9) 0.027(3) 1.000 . Uani d ? C(11) 0.3082(12) 0.4594(8) 0.1214(12) 0.038(4) 1.000 . Uani d ? C(12) 0.3569(11) 0.4884(11) 0.0300(11) 0.041(4) 1.000 . Uani d ? C(13) 0.2897(12) 0.5547(8) -0.0326(10) 0.031(3) 1.000 . Uani d ? C(14) 0.1703(11) 0.5801(8) -0.0045(10) 0.030(3) 1.000 . Uani d ? C(15) -0.0642(11) 0.6817(7) 0.1035(9) 0.026(3) 1.000 . Uani d ? C(16) 0.0457(11) 0.7331(8) 0.1189(11) 0.029(3) 1.000 . Uani d ? C(17) 0.0252(13) 0.8195(7) 0.1182(10) 0.031(3) 1.000 . Uani d ? C(18) -0.099(1) 0.8510(8) 0.0963(11) 0.039(4) 1.000 . Uani d ? C(19) -0.2051(12) 0.8003(8) 0.0792(11) 0.033(3) 1.000 . Uani d ? C(20) -0.1898(11) 0.7138(7) 0.0824(9) 0.025(3) 1.000 . Uani d ? C(21) -0.0480(12) 0.3821(7) 0.3008(11) 0.030(3) 1.000 . Uani d ? C(22) 0.0453(12) 0.3644(8) 0.3962(12) 0.029(3) 1.000 . Uani d ? C(23) 0.1312(13) 0.3004(9) 0.3948(11) 0.038(4) 1.000 . Uani d ? C(24) 0.122(1) 0.2456(7) 0.2982(12) 0.037(4) 1.000 . Uani d ? C(25) 0.032(1) 0.2622(8) 0.2074(11) 0.040(4) 1.000 . Uani d ? C(26) -0.0549(11) 0.3306(7) 0.2065(10) 0.027(3) 1.000 . Uani d ? C(27) -0.2220(10) 0.4913(11) 0.4214(8) 0.026(3) 1.000 . Uani d ? C(28) -0.2127(11) 0.4358(9) 0.5116(10) 0.033(3) 1.000 . Uani d ? C(29) -0.276(1) 0.4526(9) 0.6048(11) 0.038(4) 1.000 . Uani d ? C(30) -0.3490(13) 0.5214(10) 0.6150(11) 0.043(4) 1.000 . Uani d ? C(31) -0.3657(13) 0.5797(11) 0.5213(12) 0.047(4) 1.000 . Uani d ? C(32) -0.2982(12) 0.5620(9) 0.4279(11) 0.035(4) 1.000 . Uani d ? C(33) 0.5612(13) 0.2516(9) 0.7290(12) 0.048(4) 1.000 . Uani d ? C(34) 0.569(2) 0.2590(10) 0.252(2) 0.064(6) 1.000 . Uani d ? H(1) 0.1025 0.6264 0.3070 0.031 1.000 . Uiso c ? H(2) -0.0388 0.6826 0.4630 0.035 1.000 . Uiso c ? H(3) 0.0021 0.7293 0.3579 0.035 1.000 . Uiso c ? H(4) -0.1279 0.6792 0.3471 0.035 1.000 . Uiso c ? H(5) -0.0278 0.5776 0.5618 0.041 1.000 . Uiso c ? H(6) 0.0913 0.5111 0.7162 0.039 1.000 . Uiso c ? H(7) 0.2939 0.4521 0.6945 0.052 1.000 . Uiso c ? H(8) 0.3845 0.4659 0.5248 0.043 1.000 . Uiso c ? H(9) 0.2708 0.5341 0.3700 0.036 1.000 . Uiso c ? H(10) 0.1523 0.4580 0.2141 0.032 1.000 . Uiso c ? H(11) 0.3583 0.4203 0.1678 0.046 1.000 . Uiso c ? H(12) 0.4350 0.4657 0.0062 0.049 1.000 . Uiso c ? H(13) 0.3282 0.5805 -0.0930 0.037 1.000 . Uiso c ? H(14) 0.1220 0.6208 -0.0494 0.036 1.000 . Uiso c ? H(15) 0.1323 0.7110 0.1297 0.035 1.000 . Uiso c ? H(16) 0.0985 0.8554 0.1330 0.038 1.000 . Uiso c ? H(17) -0.1112 0.9087 0.0930 0.047 1.000 . Uiso c ? H(18) -0.2911 0.8231 0.0648 0.039 1.000 . Uiso c ? H(19) -0.2644 0.6788 0.0703 0.030 1.000 . Uiso c ? H(20) 0.0482 0.3977 0.4626 0.034 1.000 . Uiso c ? H(21) 0.1971 0.2919 0.4576 0.046 1.000 . Uiso c ? H(22) 0.1781 0.1991 0.2980 0.044 1.000 . Uiso c ? H(23) 0.0257 0.2271 0.1427 0.048 1.000 . Uiso c ? H(24) -0.1171 0.3411 0.1417 0.033 1.000 . Uiso c ? H(25) -0.1628 0.3868 0.5083 0.040 1.000 . Uiso c ? H(26) -0.2691 0.4142 0.6658 0.046 1.000 . Uiso c ? H(27) -0.3885 0.5314 0.6829 0.052 1.000 . Uiso c ? H(28) -0.4194 0.6271 0.5234 0.057 1.000 . Uiso c ? H(29) -0.3043 0.5996 0.3659 0.042 1.000 . Uiso c ? H(30) 0.6001 0.2957 0.7738 0.057 1.000 . Uiso c ? H(31) 0.6067 0.2965 0.2029 0.077 1.000 . Uiso c ? 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) 0.0221(2) 0.0181(2) 0.0216(2) -0.0013(3) 0.00258(12) 0.0023(3) Cl(1) 0.043(2) 0.040(2) 0.019(1) -0.007(1) 0.0040(13) .0005(13) Cl(2) 0.028(2) 0.044(2) 0.038(2) -0.011(1) 0.0054(13) 0.019(2) Cl(3) 0.053(2) 0.064(3) 0.064(3) 0.025(2) -0.005(2) .007(2) Cl(4) 0.059(2) 0.058(3) 0.062(3) 0.022(2) 0.006(2) 0.001(2) Cl(5) 0.075(3) 0.079(3) 0.093(4) 0.005(3) -0.000(3) .053(3) Cl(6) 0.067(3) 0.078(4) 0.100(4) 0.031(3) 0.009(3) .012(3) Cl(7) 0.078(3) 0.071(3) 0.066(3) 0.021(3) 0.008(2) .004(3) Cl(8) 0.086(4) 0.126(6) 0.093(4) 0.002(4) -0.010(3) 0.039(4) S(1) 0.026(1) 0.033(2) 0.026(2) -0.0063(13) 0.0016(12) .0020(13) P(1) 0.023(1) 0.019(1) 0.018(1) -0.0012(12) 0.0053(11) .0021(12) P(2) 0.028(2) 0.020(1) 0.0170(13) -0.0025(11) -0.0015(11) .0020(10) N(1) 0.011(4) 0.031(6) 0.031(6) -0.011(4) 0.001(4) .005(4) C(1) 0.034(7) 0.021(7) 0.021(6) -0.009(5) -0.002(6) 0.006(5) C(2) 0.047(8) 0.011(6) 0.028(6) 0.004(5) 0.004(6) .004(5) C(3) 0.029(6) 0.010(5) 0.016(5) -0.003(5) -0.001(4) .001(4) C(4) 0.030(6) 0.046(8) 0.028(7) -0.013(6) 0.010(5) 0.001(6) C(5) 0.046(7) 0.023(10) 0.029(6) 0.003(6) -0.001(5) .004(5) C(6) 0.055(8) 0.039(11) 0.029(6) 0.002(6) -0.026(6) .003(6) C(7) 0.026(5) 0.039(13) 0.041(7) -0.010(7) -0.008(5) 0.002(7) C(8) 0.031(6) 0.032(7) 0.027(6) -0.003(5) 0.008(5) 0.016(5) C(9) 0.017(5) 0.023(6) 0.027(6) 0.002(5) 0.005(5) 0.000(5) C(10) 0.037(6) 0.020(9) 0.023(5) -0.002(5) 0.002(5) .000(5) C(11) 0.030(7) 0.034(7) 0.047(8) 0.002(6) -0.008(6) 0.011(6) C(12) 0.032(6) 0.046(12) 0.046(7) 0.011(7) 0.013(5) 0.023(8) C(13) 0.037(7) 0.039(8) 0.017(6) -0.016(6) 0.011(5) .001(5) C(14) 0.031(6) 0.026(7) 0.031(7) -0.018(5) -0.009(5) .008(5) C(15) 0.033(6) 0.027(6) 0.017(6) 0.001(5) 0.001(5) 0.008(5) C(16) 0.022(6) 0.025(6) 0.037(8) -0.002(5) -0.006(5) .001(6) C(17) 0.050(8) 0.017(6) 0.026(6) -0.006(6) 0.001(6) .002(5) C(18) 0.054(9) 0.027(7) 0.037(8) -0.000(6) 0.009(6) .008(6) C(19) 0.037(7) 0.029(7) 0.032(7) 0.016(6) 0.001(5) .003(6) C(20) 0.030(6) 0.025(6) 0.018(6) 0.005(5) -0.000(5) .013(5) C(21) 0.028(7) 0.023(7) 0.038(7) 0.009(5) 0.005(5) .012(6) C(22) 0.031(7) 0.014(6) 0.041(8) -0.010(5) 0.003(6) 0.006(6) C(23) 0.042(8) 0.032(7) 0.039(7) -0.004(6) -0.004(6) .017(6) C(24) 0.056(8) 0.011(6) 0.044(8) 0.017(6) 0.006(6) .005(6) C(25) 0.064(9) 0.026(7) 0.029(7) -0.000(7) -0.004(7) 0.004(6) C(26) 0.032(6) 0.022(6) 0.025(6) 0.005(5) -0.008(5) .003(5) C(27) 0.025(5) 0.034(9) 0.020(5) -0.020(7) 0.004(4) .010(6) C(28) 0.036(7) 0.035(7) 0.030(6) -0.023(6) 0.009(5) 0.011(6) C(29) 0.053(9) 0.042(9) 0.020(6) -0.015(7) 0.010(6) .004(6) C(30) 0.038(7) 0.063(13) 0.031(7) -0.020(7) 0.010(6) .003(7) C(31) 0.037(7) 0.067(11) 0.037(8) 0.003(7) 0.005(6) .001(8) C(32) 0.036(7) 0.041(8) 0.028(7) 0.002(6) 0.003(6) .003(6) C(33) 0.042(8) 0.047(9) 0.049(9) -0.013(7) -0.019(7) .017(8) C(34) 0.083(12) 0.035(9) 0.074(12) 0.009(9) 0.007(10) .010(9) #========================================================================== #== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Wrong R = 0.0569; Rw = 0.0681' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3685 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_all 0.056 _refine_ls_wR_factor_ref 0.051 _refine_ls_goodness_of_fit_all 1.180 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_min -1.14 _refine_diff_density_max 2.05 #========================================================================== #== # MOLECULAR GEOMETRY _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 PT1 CL1 2.324(3) . . ? PT1 CL2 2.346(3) . . ? PT1 S1 2.260(3) . . ? PT1 P1 2.212(3) . . ? CL3 C33 1.77(2) . . ? CL4 C33 1.72(2) . . ? CL5 C33 1.75(2) . . ? CL6 C34 1.73(2) . . ? CL7 C34 1.73(2) . . ? CL8 C34 1.77(2) . . ? S1 P2 2.016(4) . . ? P1 N1 1.727(11) . . ? P1 C9 1.818(12) . . ? P1 C15 1.81(1) . . ? P2 N1 1.697(10) . . ? P2 C21 1.789(13) . . ? P2 C27 1.796(12) . . ? N1 C1 1.54(2) . . ? C1 C2 1.52(2) . . ? C1 C3 1.48(2) . . ? C1 H1 0.95 . . no C2 H2 0.95 . . no C2 H3 0.95 . . no C2 H4 0.95 . . no C3 C4 1.39(2) . . ? C3 C8 1.42(2) . . ? C4 C5 1.40(2) . . ? C4 H5 0.95 . . no C5 C6 1.37(2) . . ? C5 H6 0.95 . . no C6 C7 1.37(2) . . ? C6 H7 0.95 . . no C7 C8 1.39(2) . . ? C7 H8 0.95 . . no C8 H9 0.95 . . no C9 C10 1.40(2) . . ? C9 C14 1.40(2) . . ? C10 C11 1.38(2) . . ? C10 H10 0.95 . . no C11 C12 1.32(2) . . ? C11 H11 0.95 . . no C12 C13 1.44(2) . . ? C12 H12 0.95 . . no C13 C14 1.36(2) . . ? C13 H13 0.95 . . no C14 H14 0.95 . . no C15 C16 1.40(2) . . ? C15 C20 1.38(2) . . ? C16 C17 1.42(2) . . ? C16 H15 0.95 . . no C17 C18 1.36(2) . . ? C17 H16 0.95 . . no C18 C19 1.36(2) . . ? C18 H17 0.95 . . no C19 C20 1.42(2) . . ? C19 H18 0.95 . . no C20 H19 0.95 . . no C21 C22 1.42(2) . . ? C21 C26 1.39(2) . . ? C22 C23 1.36(2) . . ? C22 H20 0.95 . . no C23 C24 1.44(2) . . ? C23 H21 0.95 . . no C24 C25 1.36(2) . . ? C24 H22 0.95 . . no C25 C26 1.42(2) . . ? C25 H23 0.95 . . no C26 H24 0.95 . . no C27 C28 1.39(2) . . ? C27 C32 1.40(2) . . ? C28 C29 1.37(2) . . ? C28 H25 0.95 . . no C29 C30 1.36(2) . . ? C29 H26 0.95 . . no C30 C31 1.45(2) . . ? C30 H27 0.95 . . no C31 C32 1.39(2) . . ? C31 H28 0.95 . . no C32 H29 0.95 . . no C33 H30 0.95 . . no C34 H31 0.95 . . no #-------------------------------------------------------------------------- #-- 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 CL1 PT1 CL2 90.71(12) . . . ? CL1 PT1 S1 172.81(13) . . . ? CL1 PT1 P1 88.59(12) . . . ? CL2 PT1 S1 88.69(12) . . . ? CL2 PT1 P1 178.78(12) . . . ? S1 PT1 P1 92.12(11) . . . ? PT1 S1 P2 101.2(2) . . . ? PT1 P1 N1 110.7(4) . . . ? PT1 P1 C9 113.7(4) . . . ? PT1 P1 C15 115.0(4) . . . ? N1 P1 C9 106.5(5) . . . ? N1 P1 C15 103.6(6) . . . ? C9 P1 C15 106.5(6) . . . ? S1 P2 N1 107.2(4) . . . ? S1 P2 C21 111.3(5) . . . ? S1 P2 C27 104.6(4) . . . ? N1 P2 C21 110.1(6) . . . ? N1 P2 C27 110.4(7) . . . ? C21 P2 C27 113.0(7) . . . ? P1 N1 P2 115.1(6) . . . ? P1 N1 C1 118.4(8) . . . ? P2 N1 C1 125.8(8) . . . ? N1 C1 C2 109.3(10) . . . ? N1 C1 C3 117.3(11) . . . ? N1 C1 H1 105.3 . . . no C2 C1 C3 113.2(11) . . . ? C2 C1 H1 105.3 . . . no C3 C1 H1 105.3 . . . no C1 C2 H2 109.5 . . . no C1 C2 H3 109.5 . . . no C1 C2 H4 109.5 . . . no H2 C2 H3 109.5 . . . no H2 C2 H4 109.5 . . . no H3 C2 H4 109.5 . . . no C1 C3 C4 123.5(12) . . . ? C1 C3 C8 119.3(11) . . . ? C4 C3 C8 117.1(11) . . . ? C3 C4 C5 121.8(12) . . . ? C3 C4 H5 119.1 . . . no C5 C4 H5 119.1 . . . no C4 C5 C6 119.5(12) . . . ? C4 C5 H6 120.2 . . . no C6 C5 H6 120.2 . . . no C5 C6 C7 120.5(13) . . . ? C5 C6 H7 119.8 . . . no C7 C6 H7 119.8 . . . no C6 C7 C8 120.9(13) . . . ? C6 C7 H8 119.5 . . . no C8 C7 H8 119.5 . . . no C3 C8 C7 120.2(12) . . . ? C3 C8 H9 119.9 . . . no C7 C8 H9 119.9 . . . no P1 C9 C10 120.1(9) . . . ? P1 C9 C14 119.9(10) . . . ? C10 C9 C14 119.1(11) . . . ? C9 C10 C11 119.1(12) . . . ? C9 C10 H10 120.4 . . . no C11 C10 H10 120.4 . . . no C10 C11 C12 122.7(14) . . . ? C10 C11 H11 118.7 . . . no C12 C11 H11 118.7 . . . no C11 C12 C13 119.0(12) . . . ? C11 C12 H12 120.5 . . . no C13 C12 H12 120.5 . . . no C12 C13 C14 119.4(12) . . . ? C12 C13 H13 120.3 . . . no C14 C13 H13 120.3 . . . no C9 C14 C13 120.1(12) . . . ? C9 C14 H14 119.9 . . . no C13 C14 H14 119.9 . . . no P1 C15 C16 121.5(10) . . . ? P1 C15 C20 117.7(10) . . . ? C16 C15 C20 120.7(12) . . . ? C15 C16 C17 118.6(12) . . . ? C15 C16 H15 120.7 . . . no C17 C16 H15 120.7 . . . no C16 C17 C18 120.5(13) . . . ? C16 C17 H16 119.8 . . . no C18 C17 H16 119.8 . . . no C17 C18 C19 120.3(14) . . . ? C17 C18 H17 119.9 . . . no C19 C18 H17 119.8 . . . no C18 C19 C20 121.2(13) . . . ? C18 C19 H18 119.4 . . . no C20 C19 H18 119.4 . . . no C15 C20 C19 118.7(12) . . . ? C15 C20 H19 120.7 . . . no C19 C20 H19 120.7 . . . no P2 C21 C22 122.2(11) . . . ? P2 C21 C26 119.0(10) . . . ? C22 C21 C26 118.7(12) . . . ? C21 C22 C23 121.4(13) . . . ? C21 C22 H20 119.3 . . . no C23 C22 H20 119.3 . . . no C22 C23 C24 120.0(13) . . . ? C22 C23 H21 120.0 . . . no C24 C23 H21 120.0 . . . no C23 C24 C25 118.3(12) . . . ? C23 C24 H22 120.8 . . . no C25 C24 H22 120.8 . . . no C24 C25 C26 121.9(13) . . . ? C24 C25 H23 119.1 . . . no C26 C25 H23 119.1 . . . no C21 C26 C25 119.6(11) . . . ? C21 C26 H24 120.2 . . . no C25 C26 H24 120.2 . . . no P2 C27 C28 122.3(13) . . . ? P2 C27 C32 118.6(11) . . . ? C28 C27 C32 119.0(12) . . . ? C27 C28 C29 119.0(15) . . . ? C27 C28 H25 120.5 . . . no C29 C28 H25 120.5 . . . no C28 C29 C30 123.5(14) . . . ? C28 C29 H26 118.2 . . . no C30 C29 H26 118.2 . . . no C29 C30 C31 119.4(14) . . . ? C29 C30 H27 120.3 . . . no C31 C30 H27 120.3 . . . no C30 C31 C32 116.1(15) . . . ? C30 C31 H28 122.0 . . . no C32 C31 H28 122.0 . . . no C27 C32 C31 122.9(14) . . . ? C27 C32 H29 118.6 . . . no C31 C32 H29 118.6 . . . no CL3 C33 CL4 111.3(9) . . . ? CL3 C33 CL5 110.1(9) . . . ? CL3 C33 H30 108.1 . . . no CL4 C33 CL5 111.0(10) . . . ? CL4 C33 H30 108.1 . . . no CL5 C33 H30 108.1 . . . no CL6 C34 CL7 112.8(11) . . . ? CL6 C34 CL8 110.1(10) . . . ? CL6 C34 H31 107.8 . . . no CL7 C34 CL8 110.4(11) . . . ? CL7 C34 H31 107.8 . . . no CL8 C34 H31 107.8 . . . no #-------------------------------------------------------------------------- #-- 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 C2 C23 3.48(2) . 2_556 no C11 C19 3.59(2) . 2_545 no #-------------------------------------------------------------------------- #-- 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag PT1 S1 P2 N1 . . . . 37.6(4) no PT1 S1 P2 C21 . . . . -82.9(5) no PT1 S1 P2 C27 . . . . 154.9(6) no PT1 P1 N1 P2 . . . . 14.7(7) no PT1 P1 N1 C1 . . . . -174.2(8) no PT1 P1 C9 C10 . . . . -88.7(10) no PT1 P1 C9 C14 . . . . 80.7(11) no PT1 P1 C15 C16 . . . . -151.2(10) no PT1 P1 C15 C20 . . . . 32.0(11) no CL1 PT1 S1 P2 . . . . -120.8(10) no CL1 PT1 P1 N1 . . . . -177.8(4) no CL1 PT1 P1 C9 . . . . -57.9(5) no CL1 PT1 P1 C15 . . . . 65.2(5) no CL2 PT1 S1 P2 . . . . 153.9(2) no CL2 PT1 P1 N1 . . . . -122.9(64) no CL2 PT1 P1 C9 . . . . -3.0(65) no CL2 PT1 P1 C15 . . . . 120.2(64) no S1 PT1 P1 N1 . . . . 9.3(4) no S1 PT1 P1 C9 . . . . 129.2(5) no S1 PT1 P1 C15 . . . . -107.6(5) no S1 P2 N1 P1 . . . . -34.9(7) no S1 P2 N1 C1 . . . . 154.8(9) no S1 P2 C21 C22 . . . . -164.7(10) no S1 P2 C21 C26 . . . . 20.7(12) no S1 P2 C27 C28 . . . . 115.5(9) no S1 P2 C27 C32 . . . . -61.0(12) no P1 PT1 S1 P2 . . . . -25.2(2) no P1 N1 P2 C21 . . . . 86.3(7) no P1 N1 P2 C27 . . . . -148.2(6) no P1 N1 C1 C2 . . . . 93.6(11) no P1 N1 C1 C3 . . . . -135.8(10) no P1 C9 C10 C11 . . . . 172.8(10) no P1 C9 C14 C13 . . . . -172.8(10) no P1 C15 C16 C17 . . . . -173.6(10) no P1 C15 C20 C19 . . . . 175.4(10) no P2 N1 P1 C9 . . . . -109.4(7) no P2 N1 P1 C15 . . . . 138.5(7) no P2 N1 C1 C2 . . . . -96.4(12) no P2 N1 C1 C3 . . . . 34.2(16) no P2 C21 C22 C23 . . . . -171.8(11) no P2 C21 C26 C25 . . . . 174.4(11) no P2 C27 C28 C29 . . . . -177.7(10) no P2 C27 C32 C31 . . . . 176.8(12) no N1 P1 C9 C10 . . . . 33.6(11) no N1 P1 C9 C14 . . . . -157.0(10) no N1 P1 C15 C16 . . . . 87.9(11) no N1 P1 C15 C20 . . . . -88.9(10) no N1 P2 C21 C22 . . . . 76.5(12) no N1 P2 C21 C26 . . . . -98.0(12) no N1 P2 C27 C28 . . . . -129.5(11) no N1 P2 C27 C32 . . . . 54.0(12) no N1 C1 C3 C4 . . . . -93.2(15) no N1 C1 C3 C8 . . . . 90.5(14) no C1 N1 P1 C9 . . . . 61.7(10) no C1 N1 P1 C15 . . . . -50.4(10) no C1 N1 P2 C21 . . . . -84.0(11) no C1 N1 P2 C27 . . . . 41.4(12) no C1 C3 C4 C5 . . . . -178.1(12) no C1 C3 C8 C7 . . . . 178.9(14) no C2 C1 C3 C4 . . . . 35.6(17) no C2 C1 C3 C8 . . . . -140.8(12) no C3 C4 C5 C6 . . . . -0.5(21) no C3 C8 C7 C6 . . . . -0.8(26) no C4 C3 C8 C7 . . . . 2.4(20) no C4 C5 C6 C7 . . . . 2.2(23) no C5 C4 C3 C8 . . . . -1.7(19) no C5 C6 C7 C8 . . . . -1.5(27) no C9 P1 C15 C16 . . . . -24.3(13) no C9 P1 C15 C20 . . . . 158.9(10) no C9 C10 C11 C12 . . . . -5.7(21) no C9 C14 C13 C12 . . . . 5.1(20) no C10 C9 P1 C15 . . . . 143.6(10) no C10 C9 C14 C13 . . . . -3.3(19) no C10 C11 C12 C13 . . . . 7.5(23) no C11 C10 C9 C14 . . . . 3.4(18) no C11 C12 C13 C14 . . . . -7.2(22) no C14 C9 P1 C15 . . . . -47.0(12) no C15 C16 C17 C18 . . . . -3.7(22) no C15 C20 C19 C18 . . . . 0.1(21) no C16 C15 C20 C19 . . . . -1.4(19) no C16 C17 C18 C19 . . . . 2.5(23) no C17 C16 C15 C20 . . . . 3.1(20) no C17 C18 C19 C20 . . . . -0.7(22) no C21 P2 C27 C28 . . . . -5.7(13) no C21 P2 C27 C32 . . . . 177.8(11) no C21 C22 C23 C24 . . . . -4.4(22) no C21 C26 C25 C24 . . . . -0.4(23) no C22 C21 P2 C27 . . . . -47.5(13) no C22 C21 C26 C25 . . . . -0.3(20) no C22 C23 C24 C25 . . . . 3.5(23) no C23 C22 C21 C26 . . . . 2.8(20) no C23 C24 C25 C26 . . . . -1.1(24) no C26 C21 P2 C27 . . . . 138.0(11) no C27 C28 C29 C30 . . . . -0.0(21) no C27 C32 C31 C30 . . . . 2.1(22) no C28 C27 C32 C31 . . . . 0.1(21) no C28 C29 C30 C31 . . . . 2.4(22) no C29 C28 C27 C32 . . . . -1.3(19) no C29 C30 C31 C32 . . . . -3.3(21) no #-------------------------------------------------------------------------- #-- #========================================================================== #== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== #== # End of CIF #========================================================================== #==