# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1979 data_salem1 #----------------------------------------------------------------------- _audit_creation_date '1999-02-07' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal 'J. Chem. Soc., Dalton ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ; Anthony C. Willis ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email 'willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_address ' Swarup Chatterjee' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Roy Doyle' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'David C. R. Hockless ' ; Research School of Chemistry,The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Completely Stereoselective Synthesis of a Chiral Tetra(Tertiary Phosphine). Crystal and Molecular Structure of [OC-6-22-(R*,R*)]-(+-)-Dichloro{1,2-bis[(2-dimethylphosphinophenyl) methylphosphino]benzene-P,Pprime,Pdouble-prime,Ptriple-prime} cobalt(III) Hexafluorophosphate ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 12.630(4) _cell_length_b 19.034(4) _cell_length_c 12.745(4) _cell_angle_alpha 90 _cell_angle_beta 95.75(2) _cell_angle_gamma 90 _cell_volume 3048(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 5.9 _cell_measurement_theta_max 9.0 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 717.20 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H30 Cl2 Co F6 P5 ' _chemical_formula_moiety 'C24 H30 Cl2 Co P4 +, P F6 - ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1456.00 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_correction_T_min 0.817 _exptl_special_details ; The scan width was (0.80+0.34tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.08 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5846 _reflns_number_total 5582 _reflns_number_gt 3206 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02435 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05608 _diffrn_orient_matrix_UB_12 0.03190 _diffrn_orient_matrix_UB_13 0.03437 _diffrn_orient_matrix_UB_21 0.04737 _diffrn_orient_matrix_UB_22 -0.04137 _diffrn_orient_matrix_UB_23 0.01723 _diffrn_orient_matrix_UB_31 0.03072 _diffrn_orient_matrix_UB_32 0.00557 _diffrn_orient_matrix_UB_33 -0.06885 #----------------------------------------------------------------------- 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 96 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 120 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) ; Co 0 4 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 24 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 20 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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 Co(1) 0.93677(6) 0.13829(4) 0.71187(6) 0.0453(2) 1.000 . Uani d ? Cl(1) 0.8034(1) 0.22076(8) 0.7209(1) 0.0633(5) 1.000 . Uani d ? Cl(2) 0.8542(1) 0.06439(9) 0.5900(1) 0.0765(6) 1.000 . Uani d ? P(1) 0.8544(1) 0.07466(8) 0.8275(1) 0.0575(5) 1.000 . Uani d ? P(2) 1.0174(1) 0.19015(7) 0.8496(1) 0.0440(4) 1.000 . Uani d ? P(3) 1.0815(1) 0.07844(8) 0.6995(1) 0.0473(4) 1.000 . Uani d ? P(4) 0.9823(1) 0.20256(8) 0.5754(1) 0.0557(5) 1.000 . Uani d ? P(5) 1.4633(2) -0.1018(1) 0.7369(2) 0.0732(7) 1.000 . Uani d ? F(1) 1.5858(3) -0.1164(3) 0.7660(4) 0.156(2) 1.000 . Uani d ? F(2) 1.4868(4) -0.0251(3) 0.7456(7) 0.234(4) 1.000 . Uani d ? F(3) 1.4464(4) -0.1072(5) 0.8520(4) 0.200(3) 1.000 . Uani d ? F(4) 1.3428(3) -0.0836(2) 0.7104(3) 0.105(2) 1.000 . Uani d ? F(5) 1.4362(6) -0.1787(3) 0.7332(7) 0.234(4) 1.000 . Uani d ? F(6) 1.4799(4) -0.1043(5) 0.6236(4) 0.217(3) 1.000 . Uani d ? C(1) 0.7137(5) 0.0592(4) 0.7905(6) 0.085(3) 1.000 . Uani d ? C(2) 0.9003(5) -0.0128(3) 0.8664(6) 0.082(2) 1.000 . Uani d ? C(3) 0.8653(5) 0.1228(3) 0.9508(5) 0.059(2) 1.000 . Uani d ? C(4) 0.8029(5) 0.1111(3) 1.0342(6) 0.077(3) 1.000 . Uani d ? C(5) 0.8192(6) 0.1502(4) 1.1246(6) 0.086(3) 1.000 . Uani d ? C(6) 0.8981(6) 0.1990(4) 1.1377(5) 0.084(3) 1.000 . Uani d ? C(7) 0.9598(5) 0.2119(3) 1.0574(5) 0.067(2) 1.000 . Uani d ? C(8) 0.9429(4) 0.1744(3) 0.9628(4) 0.053(2) 1.000 . Uani d ? C(9) 1.0454(5) 0.2837(3) 0.8550(5) 0.059(2) 1.000 . Uani d ? C(10) 1.1457(4) 0.1484(3) 0.8824(4) 0.048(2) 1.000 . Uani d ? C(11) 1.2142(5) 0.1656(3) 0.9709(5) 0.065(2) 1.000 . Uani d ? C(12) 1.3103(5) 0.1306(4) 0.9917(5) 0.078(3) 1.000 . Uani d ? C(13) 1.3376(5) 0.0783(4) 0.9248(6) 0.077(2) 1.000 . Uani d ? C(14) 1.2711(5) 0.0616(3) 0.8359(5) 0.072(2) 1.000 . Uani d ? C(15) 1.1744(4) 0.0965(3) 0.8153(4) 0.047(2) 1.000 . Uani d ? C(16) 1.0797(5) -0.0165(3) 0.6848(5) 0.066(2) 1.000 . Uani d ? C(17) 1.1442(4) 0.1071(3) 0.5850(5) 0.053(2) 1.000 . Uani d ? C(18) 1.2352(5) 0.0747(3) 0.5529(5) 0.068(2) 1.000 . Uani d ? C(19) 1.2733(6) 0.0953(4) 0.4604(6) 0.084(3) 1.000 . Uani d ? C(20) 1.2216(6) 0.1465(4) 0.3980(6) 0.088(3) 1.000 . Uani d ? C(21) 1.1339(6) 0.1796(4) 0.4294(5) 0.078(3) 1.000 . Uani d ? C(22) 1.0948(4) 0.1604(3) 0.5245(4) 0.056(2) 1.000 . Uani d ? C(23) 1.0228(5) 0.2931(3) 0.5937(5) 0.075(2) 1.000 . Uani d ? C(24) 0.8792(5) 0.2078(4) 0.4662(5) 0.083(2) 1.000 . Uani d ? H(1) 0.6803 0.1020 0.7676 0.102 1.000 . Uiso c ? H(2) 0.7055 0.0258 0.7350 0.102 1.000 . Uiso c ? H(3) 0.6818 0.0417 0.8497 0.102 1.000 . Uiso c ? H(4) 0.8633 -0.0288 0.9232 0.099 1.000 . Uiso c ? H(5) 0.8872 -0.0440 0.8083 0.099 1.000 . Uiso c ? H(6) 0.9745 -0.0115 0.8881 0.099 1.000 . Uiso c ? H(7) 0.7493 0.0759 1.0279 0.092 1.000 . Uiso c ? H(8) 0.7744 0.1430 1.1793 0.104 1.000 . Uiso c ? H(9) 0.9104 0.2241 1.2023 0.101 1.000 . Uiso c ? H(10) 1.0142 0.2465 1.0659 0.080 1.000 . Uiso c ? H(11) 1.0861 0.2946 0.9197 0.071 1.000 . Uiso c ? H(12) 1.0844 0.2963 0.7979 0.071 1.000 . Uiso c ? H(13) 0.9803 0.3091 0.8502 0.071 1.000 . Uiso c ? H(14) 1.1950 0.2014 1.0174 0.077 1.000 . Uiso c ? H(15) 1.3572 0.1428 1.0519 0.094 1.000 . Uiso c ? H(16) 1.4026 0.0536 0.9401 0.092 1.000 . Uiso c ? H(17) 1.2911 0.0264 0.7890 0.086 1.000 . Uiso c ? H(18) 1.0481 -0.0371 0.7420 0.079 1.000 . Uiso c ? H(19) 1.0396 -0.0288 0.6204 0.079 1.000 . Uiso c ? H(20) 1.1505 -0.0333 0.6845 0.079 1.000 . Uiso c ? H(21) 1.2703 0.0388 0.5949 0.082 1.000 . Uiso c ? H(22) 1.3358 0.0740 0.4392 0.101 1.000 . Uiso c ? H(23) 1.2471 0.1589 0.3329 0.105 1.000 . Uiso c ? H(24) 1.0995 0.2155 0.3869 0.094 1.000 . Uiso c ? H(25) 1.0776 0.2963 0.6502 0.090 1.000 . Uiso c ? H(26) 1.0484 0.3102 0.5309 0.090 1.000 . Uiso c ? H(27) 0.9636 0.3206 0.6096 0.090 1.000 . Uiso c ? H(28) 0.8237 0.2377 0.4847 0.100 1.000 . Uiso c ? H(29) 0.9083 0.2263 0.4061 0.100 1.000 . Uiso c ? H(30) 0.8514 0.1622 0.4505 0.100 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 Co(1) 0.0406(4) 0.0419(4) 0.0540(5) -0.0013(3) 0.0073(3) -0.0008(4) Cl(1) 0.0401(8) 0.0589(9) 0.092(1) 0.0085(7) 0.0139(8) 0.0041(9) Cl(2) 0.078(1) 0.070(1) 0.078(1) -0.0165(9) -0.0101(9) -0.0144(9) P(1) 0.051(1) 0.0438(9) 0.080(1) -0.0078(7) 0.0203(8) 0.0026(8) P(2) 0.0476(9) 0.0379(8) 0.0489(9) -0.0042(7) 0.0160(7) -0.0028(7) P(3) 0.0480(9) 0.0428(9) 0.0521(9) 0.0033(7) 0.0102(7) -0.0056(7) P(4) 0.056(1) 0.058(1) 0.053(1) 0.0010(8) 0.0030(8) 0.0075(8) P(5) 0.064(1) 0.091(2) 0.067(1) 0.016(1) 0.016(1) -0.007(1) F(1) 0.071(3) 0.279(7) 0.118(4) 0.052(4) 0.011(3) 0.014(4) F(2) 0.117(5) 0.108(5) 0.47(1) -0.033(4) 0.019(6) -0.024(6) F(3) 0.112(4) 0.41(1) 0.082(4) 0.016(5) 0.019(3) 0.010(5) F(4) 0.062(3) 0.125(4) 0.129(4) 0.016(2) 0.017(2) 0.025(3) F(5) 0.233(8) 0.089(4) 0.37(1) 0.024(5) 0.001(8) -0.021(6) F(6) 0.118(4) 0.46(1) 0.082(4) 0.042(6) 0.031(3) -0.029(5) C(1) 0.056(4) 0.079(5) 0.121(6) -0.017(4) 0.022(4) -0.005(5) C(2) 0.094(5) 0.051(4) 0.108(6) 0.005(4) 0.042(4) 0.018(4) C(3) 0.058(4) 0.052(4) 0.071(4) 0.002(3) 0.027(3) 0.008(3) C(4) 0.075(5) 0.063(4) 0.099(6) -0.005(4) 0.042(4) 0.020(4) C(5) 0.102(6) 0.094(6) 0.073(5) 0.020(5) 0.053(5) 0.022(5) C(6) 0.113(6) 0.090(6) 0.055(4) 0.002(5) 0.041(4) -0.002(4) C(7) 0.085(5) 0.061(4) 0.058(4) -0.002(4) 0.026(4) -0.003(3) C(8) 0.058(4) 0.046(3) 0.059(4) 0.003(3) 0.024(3) 0.003(3) C(9) 0.073(4) 0.043(3) 0.065(4) -0.008(3) 0.027(3) -0.009(3) C(10) 0.047(3) 0.051(3) 0.046(3) -0.010(3) 0.008(3) 0.005(3) C(11) 0.066(4) 0.070(4) 0.058(4) -0.010(4) 0.008(3) -0.002(3) C(12) 0.062(5) 0.092(6) 0.078(5) -0.018(4) -0.010(4) 0.013(4) C(13) 0.051(4) 0.076(5) 0.100(6) 0.007(4) -0.005(4) 0.020(4) C(14) 0.056(4) 0.070(4) 0.088(5) 0.013(3) 0.001(4) 0.003(4) C(15) 0.049(3) 0.043(3) 0.049(3) 0.002(3) 0.009(3) 0.009(3) C(16) 0.080(5) 0.042(4) 0.078(4) 0.007(3) 0.022(4) -0.007(3) C(17) 0.051(4) 0.051(4) 0.060(4) -0.005(3) 0.015(3) -0.016(3) C(18) 0.064(4) 0.059(4) 0.086(5) -0.002(3) 0.029(4) -0.015(4) C(19) 0.083(5) 0.077(5) 0.102(6) -0.025(4) 0.053(5) -0.032(5) C(20) 0.099(6) 0.095(6) 0.079(5) -0.032(5) 0.051(5) -0.016(5) C(21) 0.084(5) 0.082(5) 0.071(5) -0.018(4) 0.016(4) 0.006(4) C(22) 0.056(4) 0.065(4) 0.050(4) -0.010(3) 0.016(3) -0.003(3) C(23) 0.095(5) 0.055(4) 0.074(5) -0.002(4) 0.008(4) 0.019(4) C(24) 0.081(5) 0.100(6) 0.065(4) -0.001(4) -0.012(4) 0.017(4) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00010|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 3206 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_all 0.0518 _refine_ls_wR_factor_ref 0.0461 _refine_ls_goodness_of_fit_all 1.600 _refine_ls_goodness_of_fit_ref 1.887 _refine_ls_shift/su_max 0.0380 _refine_ls_shift/su_mean 0.0030 _refine_diff_density_min -0.45 _refine_diff_density_max 0.63 _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 Co(1) Cl(1) 2.314(2) . . yes Co(1) Cl(2) 2.270(2) . . yes Co(1) P(1) 2.243(2) . . yes Co(1) P(2) 2.176(2) . . yes Co(1) P(3) 2.173(2) . . yes Co(1) P(4) 2.248(2) . . yes P(1) C(1) 1.816(6) . . yes P(1) C(2) 1.816(6) . . yes P(1) C(3) 1.812(6) . . yes P(2) C(8) 1.825(5) . . yes P(2) C(9) 1.814(5) . . yes P(2) C(10) 1.814(5) . . yes P(3) C(15) 1.824(5) . . yes P(3) C(16) 1.816(5) . . yes P(3) C(17) 1.813(6) . . yes P(4) C(22) 1.809(6) . . yes P(4) C(23) 1.807(6) . . yes P(4) C(24) 1.811(6) . . yes P(5) F(1) 1.579(4) . . yes P(5) F(2) 1.491(6) . . yes P(5) F(3) 1.507(5) . . yes P(5) F(4) 1.564(4) . . yes P(5) F(5) 1.503(6) . . yes P(5) F(6) 1.481(5) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(2) H(6) 0.95 . . no C(3) C(4) 1.403(8) . . yes C(3) C(8) 1.384(7) . . yes C(4) C(5) 1.370(9) . . yes C(4) H(7) 0.95 . . no C(5) C(6) 1.362(9) . . yes C(5) H(8) 0.95 . . no C(6) C(7) 1.369(8) . . yes C(6) H(9) 0.95 . . no C(7) C(8) 1.399(7) . . yes C(7) H(10) 0.95 . . no C(9) H(11) 0.95 . . no C(9) H(12) 0.95 . . no C(9) H(13) 0.95 . . no C(10) C(11) 1.390(7) . . yes C(10) C(15) 1.379(7) . . yes C(11) C(12) 1.385(8) . . yes C(11) H(14) 0.95 . . no C(12) C(13) 1.377(9) . . yes C(12) H(15) 0.95 . . no C(13) C(14) 1.378(8) . . yes C(13) H(16) 0.95 . . no C(14) C(15) 1.392(7) . . yes C(14) H(17) 0.95 . . no C(16) H(18) 0.95 . . no C(16) H(19) 0.95 . . no C(16) H(20) 0.95 . . no C(17) C(18) 1.401(7) . . yes C(17) C(22) 1.383(7) . . yes C(18) C(19) 1.374(9) . . yes C(18) H(21) 0.95 . . no C(19) C(20) 1.38(1) . . yes C(19) H(22) 0.95 . . no C(20) C(21) 1.368(9) . . yes C(20) H(23) 0.95 . . no C(21) C(22) 1.402(8) . . yes C(21) H(24) 0.95 . . no C(23) H(25) 0.95 . . no C(23) H(26) 0.95 . . no C(23) H(27) 0.95 . . no C(24) H(28) 0.95 . . no C(24) H(29) 0.95 . . no C(24) H(30) 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) Co(1) Cl(2) 99.65(7) . . . yes Cl(1) Co(1) P(1) 86.88(6) . . . yes Cl(1) Co(1) P(2) 86.36(6) . . . yes Cl(1) Co(1) P(3) 168.88(6) . . . yes Cl(1) Co(1) P(4) 85.03(6) . . . yes Cl(2) Co(1) P(1) 84.46(7) . . . yes Cl(2) Co(1) P(2) 168.18(7) . . . yes Cl(2) Co(1) P(3) 87.55(7) . . . yes Cl(2) Co(1) P(4) 86.74(7) . . . yes P(1) Co(1) P(2) 85.73(6) . . . yes P(1) Co(1) P(3) 102.34(7) . . . yes P(1) Co(1) P(4) 166.89(7) . . . yes P(2) Co(1) P(3) 88.12(6) . . . yes P(2) Co(1) P(4) 104.00(6) . . . yes P(3) Co(1) P(4) 86.95(6) . . . yes Co(1) P(1) C(1) 115.1(2) . . . yes Co(1) P(1) C(2) 121.2(2) . . . yes Co(1) P(1) C(3) 107.2(2) . . . yes C(1) P(1) C(2) 101.5(3) . . . yes C(1) P(1) C(3) 107.1(3) . . . yes C(2) P(1) C(3) 103.4(3) . . . yes Co(1) P(2) C(8) 109.1(2) . . . yes Co(1) P(2) C(9) 123.3(2) . . . yes Co(1) P(2) C(10) 108.8(2) . . . yes C(8) P(2) C(9) 104.2(3) . . . yes C(8) P(2) C(10) 105.4(2) . . . yes C(9) P(2) C(10) 104.8(3) . . . yes Co(1) P(3) C(15) 108.7(2) . . . yes Co(1) P(3) C(16) 121.8(2) . . . yes Co(1) P(3) C(17) 109.8(2) . . . yes C(15) P(3) C(16) 105.7(3) . . . yes C(15) P(3) C(17) 107.3(2) . . . yes C(16) P(3) C(17) 102.6(3) . . . yes Co(1) P(4) C(22) 107.9(2) . . . yes Co(1) P(4) C(23) 120.7(2) . . . yes Co(1) P(4) C(24) 113.9(2) . . . yes C(22) P(4) C(23) 104.3(3) . . . yes C(22) P(4) C(24) 106.2(3) . . . yes C(23) P(4) C(24) 102.6(3) . . . yes F(1) P(5) F(2) 88.4(3) . . . yes F(1) P(5) F(3) 89.5(3) . . . yes F(1) P(5) F(4) 177.1(3) . . . yes F(1) P(5) F(5) 92.9(4) . . . yes F(1) P(5) F(6) 89.5(3) . . . yes F(2) P(5) F(3) 92.4(5) . . . yes F(2) P(5) F(4) 88.9(3) . . . yes F(2) P(5) F(5) 177.0(5) . . . yes F(2) P(5) F(6) 93.3(5) . . . yes F(3) P(5) F(4) 89.8(3) . . . yes F(3) P(5) F(5) 84.9(5) . . . yes F(3) P(5) F(6) 174.2(5) . . . yes F(4) P(5) F(5) 89.8(3) . . . yes F(4) P(5) F(6) 91.5(3) . . . yes F(5) P(5) F(6) 89.5(5) . . . yes P(1) C(1) H(1) 109.5 . . . no P(1) C(1) H(2) 109.5 . . . no P(1) C(1) H(3) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.5 . . . no H(2) C(1) H(3) 109.5 . . . no P(1) C(2) H(4) 109.5 . . . no P(1) C(2) H(5) 109.5 . . . no P(1) C(2) H(6) 109.5 . . . no H(4) C(2) H(5) 109.5 . . . no H(4) C(2) H(6) 109.5 . . . no H(5) C(2) H(6) 109.5 . . . no P(1) C(3) C(4) 125.2(5) . . . yes P(1) C(3) C(8) 116.5(4) . . . yes C(4) C(3) C(8) 118.3(6) . . . yes C(3) C(4) C(5) 120.2(6) . . . yes C(3) C(4) H(7) 119.9 . . . no C(5) C(4) H(7) 119.9 . . . no C(4) C(5) C(6) 121.4(6) . . . yes C(4) C(5) H(8) 119.3 . . . no C(6) C(5) H(8) 119.3 . . . no C(5) C(6) C(7) 119.7(7) . . . yes C(5) C(6) H(9) 120.2 . . . no C(7) C(6) H(9) 120.2 . . . no C(6) C(7) C(8) 120.2(6) . . . yes C(6) C(7) H(10) 119.9 . . . no C(8) C(7) H(10) 119.9 . . . no P(2) C(8) C(3) 116.4(4) . . . yes P(2) C(8) C(7) 123.4(4) . . . yes C(3) C(8) C(7) 120.2(5) . . . yes P(2) C(9) H(11) 109.5 . . . no P(2) C(9) H(12) 109.5 . . . no P(2) C(9) H(13) 109.5 . . . no H(11) C(9) H(12) 109.5 . . . no H(11) C(9) H(13) 109.5 . . . no H(12) C(9) H(13) 109.5 . . . no P(2) C(10) C(11) 123.5(5) . . . yes P(2) C(10) C(15) 117.1(4) . . . yes C(11) C(10) C(15) 119.4(5) . . . yes C(10) C(11) C(12) 120.3(6) . . . yes C(10) C(11) H(14) 119.8 . . . no C(12) C(11) H(14) 119.8 . . . no C(11) C(12) C(13) 119.8(6) . . . yes C(11) C(12) H(15) 120.1 . . . no C(13) C(12) H(15) 120.1 . . . no C(12) C(13) C(14) 120.4(6) . . . yes C(12) C(13) H(16) 119.8 . . . no C(14) C(13) H(16) 119.8 . . . no C(13) C(14) C(15) 119.7(6) . . . yes C(13) C(14) H(17) 120.1 . . . no C(15) C(14) H(17) 120.2 . . . no P(3) C(15) C(10) 116.7(4) . . . yes P(3) C(15) C(14) 122.9(5) . . . yes C(10) C(15) C(14) 120.4(5) . . . yes P(3) C(16) H(18) 109.5 . . . no P(3) C(16) H(19) 109.5 . . . no P(3) C(16) H(20) 109.5 . . . no H(18) C(16) H(19) 109.5 . . . no H(18) C(16) H(20) 109.5 . . . no H(19) C(16) H(20) 109.5 . . . no P(3) C(17) C(18) 122.6(5) . . . yes P(3) C(17) C(22) 117.4(4) . . . yes C(18) C(17) C(22) 119.8(6) . . . yes C(17) C(18) C(19) 119.5(6) . . . yes C(17) C(18) H(21) 120.2 . . . no C(19) C(18) H(21) 120.2 . . . no C(18) C(19) C(20) 120.7(7) . . . yes C(18) C(19) H(22) 119.7 . . . no C(20) C(19) H(22) 119.7 . . . no C(19) C(20) C(21) 120.4(7) . . . yes C(19) C(20) H(23) 119.8 . . . no C(21) C(20) H(23) 119.8 . . . no C(20) C(21) C(22) 119.9(7) . . . yes C(20) C(21) H(24) 120.1 . . . no C(22) C(21) H(24) 120.1 . . . no P(4) C(22) C(17) 116.9(4) . . . yes P(4) C(22) C(21) 123.5(5) . . . yes C(17) C(22) C(21) 119.7(6) . . . yes P(4) C(23) H(25) 109.5 . . . no P(4) C(23) H(26) 109.5 . . . no P(4) C(23) H(27) 109.5 . . . no H(25) C(23) H(26) 109.5 . . . no H(25) C(23) H(27) 109.5 . . . no H(26) C(23) H(27) 109.5 . . . no P(4) C(24) H(28) 109.5 . . . no P(4) C(24) H(29) 109.5 . . . no P(4) C(24) H(30) 109.5 . . . no H(28) C(24) H(29) 109.5 . . . no H(28) C(24) H(30) 109.5 . . . no H(29) C(24) H(30) 109.5 . . . 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(2) C(18) 3.346(6) . 3_756 no Cl(2) C(19) 3.470(7) . 3_756 no F(1) C(12) 3.243(8) . 3_857 no F(1) C(20) 3.411(8) . 3_856 no F(1) C(19) 3.562(9) . 3_856 no F(2) C(1) 3.285(8) . 1_655 no F(2) C(14) 3.478(9) . . no F(3) C(5) 3.49(1) . 3_757 no F(3) C(12) 3.520(8) . 3_857 no F(3) C(4) 3.597(8) . 3_757 no F(4) C(5) 3.328(8) . 3_757 no F(4) C(14) 3.362(8) . . no F(4) C(16) 3.543(7) . . no F(5) C(6) 3.44(1) . 2_747 no F(5) C(21) 3.46(1) . 2_746 no F(5) C(7) 3.53(1) . 2_747 no F(6) C(23) 3.385(9) . 2_746 no F(6) C(19) 3.401(8) . 3_856 no C(7) C(12) 3.596(9) . 4_455 no C(20) C(24) 3.47(1) . 4 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 Co(1) P(1) C(3) C(4) . . . . 162.9(5) no Co(1) P(1) C(3) C(8) . . . . -18.2(5) no Co(1) P(2) C(8) C(3) . . . . 13.0(5) no Co(1) P(2) C(8) C(7) . . . . -166.0(5) no Co(1) P(2) C(10) C(11) . . . . -175.2(4) no Co(1) P(2) C(10) C(15) . . . . 4.0(4) no Co(1) P(3) C(15) C(10) . . . . -7.2(4) no Co(1) P(3) C(15) C(14) . . . . 174.2(4) no Co(1) P(3) C(17) C(18) . . . . -175.6(4) no Co(1) P(3) C(17) C(22) . . . . 0.2(5) no Co(1) P(4) C(22) C(17) . . . . -11.3(5) no Co(1) P(4) C(22) C(21) . . . . 169.6(5) no Cl(1) Co(1) P(1) C(1) . . . . 52.3(3) no Cl(1) Co(1) P(1) C(2) . . . . 175.1(3) no Cl(1) Co(1) P(1) C(3) . . . . -66.7(2) no Cl(1) Co(1) P(2) C(8) . . . . 68.7(2) no Cl(1) Co(1) P(2) C(9) . . . . -53.8(2) no Cl(1) Co(1) P(2) C(10) . . . . -176.9(2) no Cl(1) Co(1) P(3) C(15) . . . . 67.6(4) no Cl(1) Co(1) P(3) C(16) . . . . -169.2(4) no Cl(1) Co(1) P(3) C(17) . . . . -49.4(4) no Cl(1) Co(1) P(4) C(22) . . . . -179.1(2) no Cl(1) Co(1) P(4) C(23) . . . . 61.3(3) no Cl(1) Co(1) P(4) C(24) . . . . -61.5(3) no Cl(2) Co(1) P(1) C(1) . . . . -47.7(3) no Cl(2) Co(1) P(1) C(2) . . . . 75.1(3) no Cl(2) Co(1) P(1) C(3) . . . . -166.7(2) no Cl(2) Co(1) P(2) C(8) . . . . -52.4(4) no Cl(2) Co(1) P(2) C(9) . . . . -174.9(4) no Cl(2) Co(1) P(2) C(10) . . . . 62.1(4) no Cl(2) Co(1) P(3) C(15) . . . . -161.6(2) no Cl(2) Co(1) P(3) C(16) . . . . -38.5(2) no Cl(2) Co(1) P(3) C(17) . . . . 81.3(2) no Cl(2) Co(1) P(4) C(22) . . . . -79.1(2) no Cl(2) Co(1) P(4) C(23) . . . . 161.3(3) no Cl(2) Co(1) P(4) C(24) . . . . 38.5(3) no P(1) Co(1) P(2) C(8) . . . . -18.4(2) no P(1) Co(1) P(2) C(9) . . . . -141.0(2) no P(1) Co(1) P(2) C(10) . . . . 96.0(2) no P(1) Co(1) P(3) C(15) . . . . -77.8(2) no P(1) Co(1) P(3) C(16) . . . . 45.3(3) no P(1) Co(1) P(3) C(17) . . . . 165.1(2) no P(1) Co(1) P(4) C(22) . . . . -127.0(3) no P(1) Co(1) P(4) C(23) . . . . 113.4(4) no P(1) Co(1) P(4) C(24) . . . . -9.4(4) no P(1) C(3) C(4) C(5) . . . . 179.1(5) no P(1) C(3) C(8) P(2) . . . . 3.7(6) no P(1) C(3) C(8) C(7) . . . . -177.2(5) no P(2) Co(1) P(1) C(1) . . . . 138.9(3) no P(2) Co(1) P(1) C(2) . . . . -98.3(3) no P(2) Co(1) P(1) C(3) . . . . 19.9(2) no P(2) Co(1) P(3) C(15) . . . . 7.4(2) no P(2) Co(1) P(3) C(16) . . . . 130.5(2) no P(2) Co(1) P(3) C(17) . . . . -109.7(2) no P(2) Co(1) P(4) C(22) . . . . 95.9(2) no P(2) Co(1) P(4) C(23) . . . . -23.7(3) no P(2) Co(1) P(4) C(24) . . . . -146.5(3) no P(2) C(8) C(3) C(4) . . . . -177.2(5) no P(2) C(8) C(7) C(6) . . . . 177.5(5) no P(2) C(10) C(11) C(12) . . . . 179.0(5) no P(2) C(10) C(15) P(3) . . . . 2.0(6) no P(2) C(10) C(15) C(14) . . . . -179.3(4) no P(3) Co(1) P(1) C(1) . . . . -133.9(3) no P(3) Co(1) P(1) C(2) . . . . -11.2(3) no P(3) Co(1) P(1) C(3) . . . . 107.0(2) no P(3) Co(1) P(2) C(8) . . . . -120.9(2) no P(3) Co(1) P(2) C(9) . . . . 116.5(2) no P(3) Co(1) P(2) C(10) . . . . -6.5(2) no P(3) Co(1) P(4) C(22) . . . . 8.6(2) no P(3) Co(1) P(4) C(23) . . . . -111.0(3) no P(3) Co(1) P(4) C(24) . . . . 126.2(3) no P(3) C(15) C(10) C(11) . . . . -178.7(4) no P(3) C(15) C(14) C(13) . . . . 179.6(5) no P(3) C(17) C(18) C(19) . . . . 174.5(5) no P(3) C(17) C(22) P(4) . . . . 7.3(6) no P(3) C(17) C(22) C(21) . . . . -173.5(5) no P(4) Co(1) P(1) C(1) . . . . 0.4(4) no P(4) Co(1) P(1) C(2) . . . . 123.2(4) no P(4) Co(1) P(1) C(3) . . . . -118.6(3) no P(4) Co(1) P(2) C(8) . . . . 152.7(2) no P(4) Co(1) P(2) C(9) . . . . 30.1(2) no P(4) Co(1) P(2) C(10) . . . . -92.9(2) no P(4) Co(1) P(3) C(15) . . . . 111.5(2) no P(4) Co(1) P(3) C(16) . . . . -125.4(2) no P(4) Co(1) P(3) C(17) . . . . -5.6(2) no P(4) C(22) C(17) C(18) . . . . -176.7(4) no P(4) C(22) C(21) C(20) . . . . 177.9(5) no C(1) P(1) C(3) C(4) . . . . 38.8(6) no C(1) P(1) C(3) C(8) . . . . -142.2(5) no C(2) P(1) C(3) C(4) . . . . -67.9(6) no C(2) P(1) C(3) C(8) . . . . 111.0(5) no C(3) C(4) C(5) C(6) . . . . -3(1) no C(3) C(8) P(2) C(9) . . . . 146.4(5) no C(3) C(8) P(2) C(10) . . . . -103.6(5) no C(3) C(8) C(7) C(6) . . . . -1(1) no C(4) C(3) C(8) C(7) . . . . 1.8(9) no C(4) C(5) C(6) C(7) . . . . 3(1) no C(5) C(4) C(3) C(8) . . . . 0(1) no C(5) C(6) C(7) C(8) . . . . -1(1) no C(7) C(8) P(2) C(9) . . . . -32.6(6) no C(7) C(8) P(2) C(10) . . . . 77.4(5) no C(8) P(2) C(10) C(11) . . . . -58.4(5) no C(8) P(2) C(10) C(15) . . . . 120.8(4) no C(9) P(2) C(10) C(11) . . . . 51.3(5) no C(9) P(2) C(10) C(15) . . . . -129.6(4) no C(10) C(11) C(12) C(13) . . . . -1(1) no C(10) C(15) P(3) C(16) . . . . -139.5(4) no C(10) C(15) P(3) C(17) . . . . 111.5(4) no C(10) C(15) C(14) C(13) . . . . 1.0(9) no C(11) C(10) C(15) C(14) . . . . -0.1(8) no C(11) C(12) C(13) C(14) . . . . 2(1) no C(12) C(11) C(10) C(15) . . . . -0.2(9) no C(12) C(13) C(14) C(15) . . . . -2(1) no C(14) C(15) P(3) C(16) . . . . 41.9(6) no C(14) C(15) P(3) C(17) . . . . -67.1(5) no C(15) P(3) C(17) C(18) . . . . 66.4(5) no C(15) P(3) C(17) C(22) . . . . -117.7(5) no C(16) P(3) C(17) C(18) . . . . -44.7(6) no C(16) P(3) C(17) C(22) . . . . 131.2(5) no C(17) C(18) C(19) C(20) . . . . -1(1) no C(17) C(22) P(4) C(23) . . . . 118.2(5) no C(17) C(22) P(4) C(24) . . . . -133.7(5) no C(17) C(22) C(21) C(20) . . . . -1(1) no C(18) C(17) C(22) C(21) . . . . 2.4(9) no C(18) C(19) C(20) C(21) . . . . 3(1) no C(19) C(18) C(17) C(22) . . . . -1.3(9) no C(19) C(20) C(21) C(22) . . . . -1(1) no C(21) C(22) P(4) C(23) . . . . -60.8(6) no C(21) C(22) P(4) C(24) . . . . 47.2(6) no #----------------------------------------------------------------------- #===END