# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2000 # CCDC Number: 186/2029 data_ircodte3_[Ir(cod){MeC(CH2TeMe)3}]PF6 #------------------------------------------------------------------------------ _audit_creation_date '19100-05-11' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof. W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the structure of [Ir(cod){MeC(CH2TeMe)3}]PF6 included in Dalton manuscript number B0036540. ; _publ_contact_author_phone ' 023 80593792 ' _publ_contact_author_fax ' 023 90583781 ' _publ_contact_author_email ' wxl@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. 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. 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. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 22.330(4) _cell_length_b 14.57(2) _cell_length_c 23.67(1) _cell_angle_alpha 90 _cell_angle_beta 107.55(2) _cell_angle_gamma 90 _cell_volume 7342.1(1) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.4 _cell_measurement_theta_max 24.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1157.65 _chemical_formula_analytical ? _chemical_formula_sum 'C32.50 H39 F6 Ir O0.50 P Te3 ' _chemical_formula_moiety '?' _chemical_formula_structural [Ir(cod){MeC(CH2TeMe)3}]PF6 _chemical_compound_source ? _exptl_crystal_F_000 4320.00 _exptl_absorpt_coefficient_mu 6.081 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.542 _exptl_special_details ; The scan width was (1.26+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _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 AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.22 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 2 -7 7 -3 0 6 -4 0 _diffrn_reflns_number 6921 _reflns_number_total 6732 _reflns_number_gt 5221 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04320 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01468 _diffrn_orient_matrix_UB_12 -0.02793 _diffrn_orient_matrix_UB_13 -0.03209 _diffrn_orient_matrix_UB_21 0.02922 _diffrn_orient_matrix_UB_22 0.05289 _diffrn_orient_matrix_UB_23 0.00245 _diffrn_orient_matrix_UB_31 0.03372 _diffrn_orient_matrix_UB_32 -0.03368 _diffrn_orient_matrix_UB_33 0.03046 #------------------------------------------------------------------------------ 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 0 260 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 312 0.000 0.000 ;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, Tables 4.2.6.8 and 6.1.1.1) ; F 0 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ir 0 8 -2.066 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 24 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;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 Ir(1) 0.08711(2) 0.22413(3) 0.46102(2) 0.0364(1) 1.000 . Uani d ? Te(1) 0.14432(3) 0.37718(5) 0.45333(3) 0.0291(2) 1.000 . Uani d ? Te(2) 0.00863(3) 0.32871(4) 0.49343(3) 0.0317(2) 1.000 . Uani d ? Te(3) 0.03008(3) 0.23819(6) 0.34512(4) 0.0563(3) 1.000 . Uani d ? P(1) 0.3391(1) 0.1268(2) 0.1844(1) 0.0454(9) 1.000 . Uani d ? F(1) 0.3805(4) 0.0369(5) 0.2056(3) 0.071(3) 1.000 . Uani d ? F(2) 0.3163(3) 0.0859(6) 0.1171(3) 0.072(3) 1.000 . Uani d ? F(3) 0.3973(3) 0.1739(7) 0.1700(4) 0.081(3) 1.000 . Uani d ? F(4) 0.2982(3) 0.2167(5) 0.1619(3) 0.058(2) 1.000 . Uani d ? F(5) 0.3611(3) 0.1649(5) 0.2504(3) 0.057(2) 1.000 . Uani d ? F(6) 0.2804(3) 0.0790(5) 0.1975(3) 0.063(2) 1.000 . Uani d ? O(1) 0.534(1) 0.466(2) 0.208(1) 0.117(9) 0.500 . Uiso d ? C(1) 0.0712(4) 0.4758(7) 0.4129(4) 0.034(3) 1.000 . Uani d ? C(2) 0.0041(4) 0.4461(8) 0.3780(4) 0.035(3) 1.000 . Uani d ? C(3) -0.0287(5) 0.5335(8) 0.3460(5) 0.042(3) 1.000 . Uani d ? C(4) -0.0351(4) 0.4150(7) 0.4181(5) 0.036(3) 1.000 . Uani d ? C(5) 0.0017(5) 0.381(1) 0.3282(5) 0.063(4) 1.000 . Uani d ? C(6) 0.1692(4) 0.4426(7) 0.5377(4) 0.029(3) 1.000 . Uani d ? C(7) 0.1878(4) 0.5338(7) 0.5404(5) 0.035(3) 1.000 . Uani d ? C(8) 0.2087(5) 0.5800(9) 0.5944(6) 0.055(4) 1.000 . Uani d ? C(9) 0.2116(5) 0.532(1) 0.6446(6) 0.058(4) 1.000 . Uani d ? C(10) 0.1927(5) 0.443(1) 0.6423(5) 0.054(4) 1.000 . Uani d ? C(11) 0.1716(4) 0.3957(8) 0.5888(5) 0.038(3) 1.000 . Uani d ? C(12) -0.0757(4) 0.2552(7) 0.4856(5) 0.032(3) 1.000 . Uani d ? C(13) -0.1001(5) 0.2577(7) 0.5337(5) 0.035(3) 1.000 . Uani d ? C(14) -0.1576(5) 0.2161(7) 0.5276(6) 0.044(4) 1.000 . Uani d ? C(15) -0.1902(5) 0.1728(8) 0.4767(6) 0.051(4) 1.000 . Uani d ? C(16) -0.1654(5) 0.1706(7) 0.4291(6) 0.045(3) 1.000 . Uani d ? C(17) -0.1077(5) 0.2102(7) 0.4337(6) 0.041(3) 1.000 . Uani d ? C(18) 0.1049(5) 0.242(1) 0.3071(5) 0.054(4) 1.000 . Uani d ? C(19) 0.1386(7) 0.317(1) 0.3046(6) 0.062(4) 1.000 . Uani d ? C(20) 0.1855(7) 0.319(1) 0.2775(6) 0.072(5) 1.000 . Uani d ? C(21) 0.2006(8) 0.240(1) 0.2524(8) 0.084(6) 1.000 . Uani d ? C(22) 0.1661(8) 0.165(1) 0.2526(7) 0.092(6) 1.000 . Uani d ? C(23) 0.1162(6) 0.162(1) 0.2801(7) 0.072(5) 1.000 . Uani d ? C(24) 0.0433(6) 0.0885(9) 0.4509(9) 0.082(6) 1.000 . Uani d ? C(25) 0.0616(6) 0.1140(8) 0.5110(8) 0.066(5) 1.000 . Uani d ? C(26) 0.1179(7) 0.067(1) 0.5571(9) 0.093(6) 1.000 . Uani d ? C(27) 0.1771(6) 0.1211(9) 0.5673(7) 0.072(5) 1.000 . Uani d ? C(28) 0.1796(5) 0.1757(8) 0.5143(6) 0.048(4) 1.000 . Uani d ? C(29) 0.1659(5) 0.1425(8) 0.4549(7) 0.053(4) 1.000 . Uani d ? C(30) 0.1499(7) 0.0410(8) 0.4381(9) 0.084(6) 1.000 . Uani d ? C(31) 0.0810(7) 0.0225(9) 0.4258(9) 0.097(6) 1.000 . Uani d ? C(32) 0.537(1) 0.323(2) 0.176(1) 0.053(6) 0.500 . Uiso d ? C(33) 0.567(1) 0.403(2) 0.208(1) 0.062(7) 0.500 . Uiso d ? C(34) 0.627(2) 0.394(3) 0.245(2) 0.09(1) 0.500 . Uiso d ? H(1) 0.0672 0.5140 0.4442 0.041 1.000 . Uiso c ? H(2) 0.0863 0.5111 0.3864 0.041 1.000 . Uiso c ? H(3) -0.0063 0.5560 0.3206 0.051 1.000 . Uiso c ? H(4) -0.0705 0.5190 0.3234 0.051 1.000 . Uiso c ? H(5) -0.0293 0.5789 0.3747 0.051 1.000 . Uiso c ? H(6) -0.0492 0.4689 0.4327 0.043 1.000 . Uiso c ? H(7) -0.0703 0.3823 0.3937 0.043 1.000 . Uiso c ? H(8) -0.0407 0.3796 0.3036 0.076 1.000 . Uiso c ? H(9) 0.0276 0.4061 0.3069 0.076 1.000 . Uiso c ? H(10) 0.1864 0.5654 0.5048 0.042 1.000 . Uiso c ? H(11) 0.2206 0.6427 0.5963 0.066 1.000 . Uiso c ? H(12) 0.2268 0.5618 0.6821 0.070 1.000 . Uiso c ? H(13) 0.1940 0.4118 0.6780 0.064 1.000 . Uiso c ? H(14) 0.1594 0.3330 0.5876 0.046 1.000 . Uiso c ? H(15) -0.0778 0.2874 0.5696 0.042 1.000 . Uiso c ? H(16) -0.1745 0.2178 0.5599 0.053 1.000 . Uiso c ? H(17) -0.2294 0.1445 0.4736 0.061 1.000 . Uiso c ? H(18) -0.1883 0.1416 0.3931 0.053 1.000 . Uiso c ? H(19) -0.0904 0.2066 0.4018 0.049 1.000 . Uiso c ? H(20) 0.1299 0.3719 0.3225 0.074 1.000 . Uiso c ? H(21) 0.2073 0.3739 0.2761 0.087 1.000 . Uiso c ? H(22) 0.2343 0.2393 0.2357 0.102 1.000 . Uiso c ? H(23) 0.1745 0.1107 0.2338 0.111 1.000 . Uiso c ? H(24) 0.0921 0.1085 0.2794 0.085 1.000 . Uiso c ? H(25) -0.0007 0.0880 0.4319 0.099 1.000 . Uiso c ? H(26) 0.0276 0.1284 0.5260 0.079 1.000 . Uiso c ? H(27) 0.1086 0.0612 0.5936 0.110 1.000 . Uiso c ? H(28) 0.1239 0.0078 0.5429 0.110 1.000 . Uiso c ? H(29) 0.1806 0.1622 0.5994 0.086 1.000 . Uiso c ? H(30) 0.2116 0.0797 0.5777 0.086 1.000 . Uiso c ? H(31) 0.2106 0.2227 0.5236 0.058 1.000 . Uiso c ? H(32) 0.1900 0.1712 0.4329 0.064 1.000 . Uiso c ? H(33) 0.1616 0.0273 0.4033 0.099 1.000 . Uiso c ? H(34) 0.1728 0.0030 0.4695 0.099 1.000 . Uiso c ? H(35) 0.0770 -0.0368 0.4406 0.116 1.000 . Uiso c ? H(36) 0.0627 0.0224 0.3836 0.116 1.000 . Uiso c ? H(37) 0.5097 0.3041 0.1963 0.059 0.500 . Uiso d ? H(38) 0.5170 0.3412 0.1373 0.059 0.500 . Uiso d ? H(39) 0.5687 0.2791 0.1779 0.059 0.500 . Uiso d ? H(40) 0.6239 0.3894 0.2862 0.109 0.500 . Uiso d ? H(41) 0.6481 0.3422 0.2386 0.109 0.500 . Uiso d ? H(42) 0.6526 0.4480 0.2461 0.109 0.500 . Uiso d ? 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 Ir(1) 0.0202(2) 0.0326(2) 0.0577(3) 0.0015(2) 0.0137(2) -0.0067(2) Te(1) 0.0193(3) 0.0392(4) 0.0297(4) 0.0016(3) 0.0087(3) 0.0028(3) Te(2) 0.0225(3) 0.0325(4) 0.0421(4) -0.0006(3) 0.0130(3) -0.0056(3) Te(3) 0.0286(4) 0.0758(6) 0.0576(6) 0.0096(4) 0.0029(4) -0.0385(5) P(1) 0.038(2) 0.062(2) 0.041(2) 0.015(1) 0.018(1) 0.006(1) F(1) 0.077(5) 0.086(5) 0.045(4) 0.049(4) 0.012(4) -0.001(4) F(2) 0.057(4) 0.112(7) 0.043(4) 0.026(5) 0.011(3) -0.014(4) F(3) 0.042(4) 0.136(8) 0.072(6) -0.005(5) 0.029(4) 0.015(5) F(4) 0.059(4) 0.054(4) 0.061(5) 0.021(3) 0.015(4) 0.015(4) F(5) 0.063(4) 0.065(5) 0.039(4) 0.008(4) 0.012(3) -0.003(3) F(6) 0.072(5) 0.051(4) 0.081(6) 0.001(4) 0.045(4) 0.001(4) C(1) 0.025(5) 0.046(6) 0.029(6) 0.005(4) 0.005(4) 0.014(5) C(2) 0.025(5) 0.057(7) 0.020(5) 0.008(5) 0.004(4) -0.007(5) C(3) 0.036(6) 0.059(7) 0.033(6) 0.019(5) 0.011(5) 0.020(5) C(4) 0.026(5) 0.029(5) 0.059(7) 0.007(4) 0.020(5) 0.003(5) C(5) 0.039(6) 0.10(1) 0.035(7) 0.028(7) -0.007(5) -0.027(7) C(6) 0.014(4) 0.042(6) 0.031(6) 0.004(4) 0.004(4) -0.008(4) C(7) 0.025(5) 0.039(6) 0.040(6) 0.005(4) 0.009(5) -0.003(5) C(8) 0.030(6) 0.055(8) 0.07(1) 0.004(5) 0.006(6) -0.017(7) C(9) 0.029(6) 0.10(1) 0.043(8) 0.000(6) -0.001(5) -0.035(8) C(10) 0.035(6) 0.09(1) 0.034(7) 0.006(7) 0.010(5) 0.001(7) C(11) 0.026(5) 0.056(7) 0.030(6) 0.002(5) 0.006(4) -0.003(5) C(12) 0.019(5) 0.033(5) 0.047(7) 0.001(4) 0.014(5) -0.003(5) C(13) 0.027(5) 0.029(5) 0.047(7) 0.005(4) 0.007(5) 0.006(5) C(14) 0.040(6) 0.040(6) 0.065(9) 0.003(5) 0.035(6) 0.007(6) C(15) 0.026(5) 0.042(7) 0.09(1) 0.002(5) 0.022(6) 0.012(7) C(16) 0.031(6) 0.030(6) 0.069(9) 0.007(4) 0.009(6) -0.002(5) C(17) 0.028(5) 0.034(6) 0.067(8) 0.002(4) 0.025(6) -0.009(5) C(18) 0.033(6) 0.077(9) 0.044(8) 0.025(6) 0.000(5) -0.025(7) C(19) 0.074(9) 0.07(1) 0.040(8) 0.019(8) 0.018(7) -0.009(7) C(20) 0.09(1) 0.09(1) 0.040(8) 0.031(9) 0.032(8) 0.010(7) C(21) 0.07(1) 0.12(1) 0.07(1) 0.04(1) 0.035(9) 0.01(1) C(22) 0.08(1) 0.12(1) 0.08(1) 0.05(1) 0.02(1) -0.05(1) C(23) 0.048(8) 0.09(1) 0.08(1) 0.015(7) 0.017(7) -0.047(9) C(24) 0.037(7) 0.037(7) 0.18(2) 0.000(6) 0.04(1) -0.01(1) C(25) 0.031(6) 0.034(7) 0.14(1) 0.008(5) 0.037(8) 0.023(8) C(26) 0.059(9) 0.08(1) 0.15(2) 0.017(8) 0.06(1) 0.06(1) C(27) 0.052(8) 0.064(9) 0.11(1) 0.028(7) 0.036(8) 0.047(9) C(28) 0.027(6) 0.049(7) 0.065(9) 0.008(5) 0.009(5) 0.028(6) C(29) 0.031(6) 0.034(6) 0.10(1) 0.020(5) 0.032(7) 0.009(7) C(30) 0.066(9) 0.033(7) 0.17(2) 0.006(6) 0.06(1) -0.031(9) C(31) 0.052(8) 0.032(7) 0.20(2) -0.002(6) 0.03(1) -0.05(1) #------------------------------------------------------------------------------ _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) + 0.00014|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 5221 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0581 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.352 _refine_ls_shift/su_max 0.0570 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.35 _refine_diff_density_max 1.76 #------------------------------------------------------------------------------ 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 Ir(1) Te(1) 2.6033(8) . . yes Ir(1) Te(2) 2.6062(7) . . yes Ir(1) Te(3) 2.661(1) . . yes Ir(1) C(24) 2.19(1) . . yes Ir(1) C(25) 2.17(1) . . yes Ir(1) C(28) 2.19(1) . . yes Ir(1) C(29) 2.165(9) . . yes Te(1) C(1) 2.169(9) . . yes Te(1) C(6) 2.129(9) . . yes Te(2) C(4) 2.16(1) . . yes Te(2) C(12) 2.124(9) . . yes Te(3) C(5) 2.17(1) . . yes Te(3) C(18) 2.12(1) . . yes P(1) F(1) 1.594(7) . . yes P(1) F(2) 1.633(8) . . yes P(1) F(3) 1.593(7) . . yes P(1) F(4) 1.594(7) . . yes P(1) F(5) 1.589(7) . . yes P(1) F(6) 1.597(7) . . yes O(1) C(33) 1.18(3) . . yes C(1) C(2) 1.54(1) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) C(3) 1.55(1) . . yes C(2) C(4) 1.54(1) . . yes C(2) C(5) 1.51(1) . . yes C(3) H(3) 0.95 . . no C(3) H(4) 0.95 . . no C(3) H(5) 0.95 . . no C(4) H(6) 0.95 . . no C(4) H(7) 0.95 . . no C(5) H(8) 0.95 . . no C(5) H(9) 0.95 . . no C(6) C(7) 1.39(1) . . yes C(6) C(11) 1.38(1) . . yes C(7) C(8) 1.39(2) . . yes C(7) H(10) 0.95 . . no C(8) C(9) 1.36(2) . . yes C(8) H(11) 0.95 . . no C(9) C(10) 1.37(2) . . yes C(9) H(12) 0.95 . . no C(10) C(11) 1.39(2) . . yes C(10) H(13) 0.95 . . no C(11) H(14) 0.95 . . no C(12) C(13) 1.40(1) . . yes C(12) C(17) 1.39(2) . . yes C(13) C(14) 1.39(1) . . yes C(13) H(15) 0.95 . . no C(14) C(15) 1.36(2) . . yes C(14) H(16) 0.95 . . no C(15) C(16) 1.40(2) . . yes C(15) H(17) 0.95 . . no C(16) C(17) 1.38(1) . . yes C(16) H(18) 0.95 . . no C(17) H(19) 0.95 . . no C(18) C(19) 1.34(2) . . yes C(18) C(23) 1.38(2) . . yes C(19) C(20) 1.38(2) . . yes C(19) H(20) 0.95 . . no C(20) C(21) 1.37(2) . . yes C(20) H(21) 0.95 . . no C(21) C(22) 1.34(2) . . yes C(21) H(22) 0.95 . . no C(22) C(23) 1.45(2) . . yes C(22) H(23) 0.95 . . no C(23) H(24) 0.95 . . no C(24) C(25) 1.41(2) . . yes C(24) C(31) 1.51(2) . . yes C(24) H(25) 0.95 . . no C(25) C(26) 1.55(2) . . yes C(25) H(26) 0.95 . . no C(26) C(27) 1.50(2) . . yes C(26) H(27) 0.95 . . no C(26) H(28) 0.95 . . no C(27) C(28) 1.50(2) . . yes C(27) H(29) 0.95 . . no C(27) H(30) 0.95 . . no C(28) C(29) 1.43(2) . . yes C(28) H(31) 0.95 . . no C(29) C(30) 1.54(2) . . yes C(29) H(32) 0.95 . . no C(30) C(31) 1.50(2) . . yes C(30) H(33) 0.96 . . no C(30) H(34) 0.95 . . no C(31) H(35) 0.95 . . no C(31) H(36) 0.96 . . no C(32) C(33) 1.45(4) . . yes C(32) H(37) 0.92 . . no C(32) H(38) 0.93 . . no C(32) H(39) 0.94 . . no C(33) C(34) 1.36(4) . . yes C(34) H(40) 1.01 . . no C(34) H(41) 0.93 . . no C(34) H(42) 0.96 . . 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 Te(1) Ir(1) Te(2) 84.70(2) . . . yes Te(1) Ir(1) Te(3) 87.39(3) . . . yes Te(1) Ir(1) C(24) 168.4(5) . . . yes Te(1) Ir(1) C(25) 152.5(5) . . . yes Te(1) Ir(1) C(28) 85.3(3) . . . yes Te(1) Ir(1) C(29) 92.3(3) . . . yes Te(2) Ir(1) Te(3) 95.93(3) . . . yes Te(2) Ir(1) C(24) 104.0(4) . . . yes Te(2) Ir(1) C(25) 87.8(3) . . . yes Te(2) Ir(1) C(28) 128.4(4) . . . yes Te(2) Ir(1) C(29) 166.7(4) . . . yes Te(3) Ir(1) C(24) 84.1(5) . . . yes Te(3) Ir(1) C(25) 119.8(5) . . . yes Te(3) Ir(1) C(28) 134.0(4) . . . yes Te(3) Ir(1) C(29) 96.9(4) . . . yes C(24) Ir(1) C(25) 37.7(6) . . . yes C(24) Ir(1) C(28) 94.9(5) . . . yes C(24) Ir(1) C(29) 80.9(4) . . . yes C(25) Ir(1) C(28) 78.7(4) . . . yes C(25) Ir(1) C(29) 89.0(4) . . . yes C(28) Ir(1) C(29) 38.3(5) . . . yes Ir(1) Te(1) C(1) 106.1(3) . . . yes Ir(1) Te(1) C(6) 108.2(3) . . . yes C(1) Te(1) C(6) 93.8(4) . . . yes Ir(1) Te(2) C(4) 105.9(2) . . . yes Ir(1) Te(2) C(12) 109.7(3) . . . yes C(4) Te(2) C(12) 93.1(4) . . . yes Ir(1) Te(3) C(5) 106.6(3) . . . yes Ir(1) Te(3) C(18) 104.2(3) . . . yes C(5) Te(3) C(18) 97.0(5) . . . yes F(1) P(1) F(2) 89.3(4) . . . yes F(1) P(1) F(3) 89.4(5) . . . yes F(1) P(1) F(4) 178.8(4) . . . yes F(1) P(1) F(5) 90.0(4) . . . yes F(1) P(1) F(6) 90.7(4) . . . yes F(2) P(1) F(3) 89.0(4) . . . yes F(2) P(1) F(4) 89.8(4) . . . yes F(2) P(1) F(5) 179.0(5) . . . yes F(2) P(1) F(6) 89.9(4) . . . yes F(3) P(1) F(4) 89.8(5) . . . yes F(3) P(1) F(5) 91.8(4) . . . yes F(3) P(1) F(6) 178.8(5) . . . yes F(4) P(1) F(5) 90.9(4) . . . yes F(4) P(1) F(6) 90.1(4) . . . yes F(5) P(1) F(6) 89.4(4) . . . yes Te(1) C(1) C(2) 122.2(7) . . . yes Te(1) C(1) H(1) 106.2 . . . no Te(1) C(1) H(2) 106.3 . . . no C(2) C(1) H(1) 106.1 . . . no C(2) C(1) H(2) 106.3 . . . no H(1) C(1) H(2) 109.5 . . . no C(1) C(2) C(3) 105.7(9) . . . yes C(1) C(2) C(4) 113.2(8) . . . yes C(1) C(2) C(5) 113.4(8) . . . yes C(3) C(2) C(4) 105.8(8) . . . yes C(3) C(2) C(5) 103.8(9) . . . yes C(4) C(2) C(5) 114(1) . . . yes C(2) C(3) H(3) 109.5 . . . no C(2) C(3) H(4) 109.4 . . . no C(2) C(3) H(5) 109.2 . . . no H(3) C(3) H(4) 109.8 . . . no H(3) C(3) H(5) 109.6 . . . no H(4) C(3) H(5) 109.4 . . . no Te(2) C(4) C(2) 118.7(6) . . . yes Te(2) C(4) H(6) 107.3 . . . no Te(2) C(4) H(7) 107.2 . . . no C(2) C(4) H(6) 107.1 . . . no C(2) C(4) H(7) 106.9 . . . no H(6) C(4) H(7) 109.4 . . . no Te(3) C(5) C(2) 121.5(9) . . . yes Te(3) C(5) H(8) 106.3 . . . no Te(3) C(5) H(9) 106.4 . . . no C(2) C(5) H(8) 106.4 . . . no C(2) C(5) H(9) 106.5 . . . no H(8) C(5) H(9) 109.4 . . . no Te(1) C(6) C(7) 117.6(7) . . . yes Te(1) C(6) C(11) 122.1(8) . . . yes C(7) C(6) C(11) 120.2(9) . . . yes C(6) C(7) C(8) 121(1) . . . yes C(6) C(7) H(10) 119.5 . . . no C(8) C(7) H(10) 119.4 . . . no C(7) C(8) C(9) 118(1) . . . yes C(7) C(8) H(11) 121.3 . . . no C(9) C(8) H(11) 120.7 . . . no C(8) C(9) C(10) 121(1) . . . yes C(8) C(9) H(12) 119.6 . . . no C(10) C(9) H(12) 119.1 . . . no C(9) C(10) C(11) 121(1) . . . yes C(9) C(10) H(13) 119.2 . . . no C(11) C(10) H(13) 119.3 . . . no C(6) C(11) C(10) 118(1) . . . yes C(6) C(11) H(14) 121.1 . . . no C(10) C(11) H(14) 120.9 . . . no Te(2) C(12) C(13) 117.9(8) . . . yes Te(2) C(12) C(17) 121.5(7) . . . yes C(13) C(12) C(17) 120.5(9) . . . yes C(12) C(13) C(14) 119(1) . . . yes C(12) C(13) H(15) 120.7 . . . no C(14) C(13) H(15) 120.8 . . . no C(13) C(14) C(15) 122(1) . . . yes C(13) C(14) H(16) 119.0 . . . no C(15) C(14) H(16) 119.2 . . . no C(14) C(15) C(16) 119(1) . . . yes C(14) C(15) H(17) 120.3 . . . no C(16) C(15) H(17) 120.5 . . . no C(15) C(16) C(17) 121(1) . . . yes C(15) C(16) H(18) 119.7 . . . no C(17) C(16) H(18) 119.5 . . . no C(12) C(17) C(16) 119(1) . . . yes C(12) C(17) H(19) 120.4 . . . no C(16) C(17) H(19) 120.5 . . . no Te(3) C(18) C(19) 124.3(9) . . . yes Te(3) C(18) C(23) 117(1) . . . yes C(19) C(18) C(23) 119(1) . . . yes C(18) C(19) C(20) 123(1) . . . yes C(18) C(19) H(20) 118.3 . . . no C(20) C(19) H(20) 118.4 . . . no C(19) C(20) C(21) 120(2) . . . yes C(19) C(20) H(21) 119.9 . . . no C(21) C(20) H(21) 119.9 . . . no C(20) C(21) C(22) 118(2) . . . yes C(20) C(21) H(22) 121.2 . . . no C(22) C(21) H(22) 121.2 . . . no C(21) C(22) C(23) 123(1) . . . yes C(21) C(22) H(23) 118.9 . . . no C(23) C(22) H(23) 118.4 . . . no C(18) C(23) C(22) 117(2) . . . yes C(18) C(23) H(24) 121.3 . . . no C(22) C(23) H(24) 121.4 . . . no Ir(1) C(24) C(25) 70.5(8) . . . yes Ir(1) C(24) C(31) 109.5(9) . . . yes Ir(1) C(24) H(25) 115.1 . . . no C(25) C(24) C(31) 123(1) . . . yes C(25) C(24) H(25) 115.0 . . . no C(31) C(24) H(25) 115.5 . . . no Ir(1) C(25) C(24) 71.8(9) . . . yes Ir(1) C(25) C(26) 114.9(8) . . . yes Ir(1) C(25) H(26) 114.2 . . . no C(24) C(25) C(26) 121(1) . . . yes C(24) C(25) H(26) 114.5 . . . no C(26) C(25) H(26) 113.6 . . . no C(25) C(26) C(27) 112(1) . . . yes C(25) C(26) H(27) 109.1 . . . no C(25) C(26) H(28) 108.8 . . . no C(27) C(26) H(27) 108.9 . . . no C(27) C(26) H(28) 108.9 . . . no H(27) C(26) H(28) 109.6 . . . no C(26) C(27) C(28) 114(1) . . . yes C(26) C(27) H(29) 108.4 . . . no C(26) C(27) H(30) 108.4 . . . no C(28) C(27) H(29) 108.6 . . . no C(28) C(27) H(30) 108.7 . . . no H(29) C(27) H(30) 109.1 . . . no Ir(1) C(28) C(27) 112.7(8) . . . yes Ir(1) C(28) C(29) 70.0(6) . . . yes Ir(1) C(28) H(31) 113.3 . . . no C(27) C(28) C(29) 126(1) . . . yes C(27) C(28) H(31) 113.4 . . . no C(29) C(28) H(31) 113.4 . . . no Ir(1) C(29) C(28) 71.7(6) . . . yes Ir(1) C(29) C(30) 114.4(8) . . . yes Ir(1) C(29) H(32) 113.6 . . . no C(28) C(29) C(30) 123(1) . . . yes C(28) C(29) H(32) 113.7 . . . no C(30) C(29) H(32) 113.8 . . . no C(29) C(30) C(31) 111.5(9) . . . yes C(29) C(30) H(33) 108.8 . . . no C(29) C(30) H(34) 109.3 . . . no C(31) C(30) H(33) 108.9 . . . no C(31) C(30) H(34) 109.0 . . . no H(33) C(30) H(34) 109.4 . . . no C(24) C(31) C(30) 118(1) . . . yes C(24) C(31) H(35) 108.0 . . . no C(24) C(31) H(36) 107.3 . . . no C(30) C(31) H(35) 107.3 . . . no C(30) C(31) H(36) 107.0 . . . no H(35) C(31) H(36) 109.1 . . . no C(33) C(32) H(37) 104.6 . . . no C(33) C(32) H(38) 106.8 . . . no C(33) C(32) H(39) 107.2 . . . no H(37) C(32) H(38) 113.7 . . . no H(37) C(32) H(39) 112.6 . . . no H(38) C(32) H(39) 111.3 . . . no O(1) C(33) C(32) 115(3) . . . yes O(1) C(33) C(34) 125(3) . . . yes C(32) C(33) C(34) 118(3) . . . yes C(33) C(34) H(40) 106.5 . . . no C(33) C(34) H(41) 115.3 . . . no C(33) C(34) H(42) 113.5 . . . no H(40) C(34) H(41) 106.4 . . . no H(40) C(34) H(42) 103.7 . . . no H(41) C(34) H(42) 110.4 . . . 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 F(1) C(19) 3.23(2) . 6_545 no F(1) C(3) 3.33(1) . 5_545 no F(1) C(1) 3.41(1) . 6_545 no F(1) C(20) 3.58(2) . 6_545 no F(2) C(1) 3.23(1) . 6_545 no F(2) C(15) 3.27(1) . 2 no F(2) C(16) 3.44(1) . 2 no F(3) C(13) 3.39(1) . 8_554 no F(3) C(14) 3.60(2) . 8_554 no F(4) C(16) 3.17(1) . 2 no F(4) C(34) 3.48(4) . 2_655 no F(4) C(15) 3.50(2) . 2 no F(4) C(21) 3.50(2) . . no F(5) C(32) 3.33(3) . 2_655 no F(5) C(34) 3.35(4) . 2_655 no F(5) C(3) 3.39(1) . 5_545 no F(5) C(10) 3.49(1) . 7_556 no F(6) C(21) 3.43(2) . . no F(6) C(22) 3.43(1) . . no F(6) C(16) 3.57(1) . 2 no O(1) O(1) 2.85(5) . 2_655 no O(1) C(31) 3.51(3) . 6 no O(1) C(23) 3.54(3) . 5 no O(1) C(33) 3.55(4) . 2_655 no #------------------------------------------------------------------------------ data_sdoircod[_[ir(cod)(setripod)]PF6 #------------------------------------------------------------------------------ _audit_creation_date '19100-05-11' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof. W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the structure of [Ir(cod){MeC(CH2SeMe)3}]PF6 included in Dalton manuscript number B0036540. ; _publ_contact_author_phone ' 023 80593792 ' _publ_contact_author_fax ' 023 80593781 ' _publ_contact_author_email ' wxl@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. 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. 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. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.889(4) _cell_length_b 12.274(6) _cell_length_c 14.492(3) _cell_angle_alpha 90 _cell_angle_beta 105.28(2) _cell_angle_gamma 90 _cell_volume 2211(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.1 _cell_measurement_theta_max 20.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _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,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.392 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 796.48 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H30 F6 Ir P Se3 ' _chemical_formula_moiety '?' _chemical_formula_structural [Ir(cod){MeC(CH2SeMe)3}]PF6 _chemical_compound_source ? _exptl_crystal_F_000 1496.00 _exptl_absorpt_coefficient_mu 11.115 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.466 _exptl_special_details ; The scan width was (1.05+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _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 AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -6.13 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 5 -4 2 3 -4 -1 4 _diffrn_reflns_number 4293 _reflns_number_total 4102 _reflns_number_gt 3014 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06535 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02427 _diffrn_orient_matrix_UB_12 -0.04802 _diffrn_orient_matrix_UB_13 0.04602 _diffrn_orient_matrix_UB_21 0.07667 _diffrn_orient_matrix_UB_22 -0.01616 _diffrn_orient_matrix_UB_23 0.03369 _diffrn_orient_matrix_UB_31 0.00116 _diffrn_orient_matrix_UB_32 0.06380 _diffrn_orient_matrix_UB_33 0.04317 #------------------------------------------------------------------------------ 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 64 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) ; 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 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 12 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ir 0 4 -2.066 7.990 ;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 Ir(1) 0.25770(3) 0.11576(4) 0.09810(3) 0.0223(1) 1.000 . Uani d ? Se(1) 0.35599(9) 0.04352(9) -0.02234(8) 0.0253(3) 1.000 . Uani d ? Se(2) 0.16210(8) 0.2409(1) -0.03084(8) 0.0267(3) 1.000 . Uani d ? Se(3) 0.40165(9) 0.2525(1) 0.15581(8) 0.0270(3) 1.000 . Uani d ? P(1) 0.2935(3) 0.1560(3) 0.5988(2) 0.0337(9) 1.000 . Uani d ? F(1) 0.2145(6) 0.2505(6) 0.5427(5) 0.050(2) 1.000 . Uani d ? F(2) 0.3677(6) 0.0594(7) 0.6549(6) 0.060(3) 1.000 . Uani d ? F(3) 0.3795(9) 0.2450(8) 0.6446(9) 0.120(4) 1.000 . Uani d ? F(4) 0.240(1) 0.167(1) 0.6818(7) 0.116(5) 1.000 . Uani d ? F(5) 0.2078(7) 0.0672(7) 0.5473(7) 0.077(3) 1.000 . Uani d ? F(6) 0.3481(7) 0.1442(8) 0.5138(6) 0.073(3) 1.000 . Uani d ? C(1) 0.4390(9) 0.359(1) -0.1174(8) 0.034(3) 1.000 . Uani d ? C(2) 0.3864(8) 0.2865(9) -0.0565(7) 0.024(3) 1.000 . Uani d ? C(3) 0.4222(8) 0.1691(9) -0.0698(7) 0.025(3) 1.000 . Uani d ? C(4) 0.246(1) 0.007(1) -0.1376(8) 0.032(3) 1.000 . Uani d ? C(5) 0.2648(8) 0.300(1) -0.0974(8) 0.029(3) 1.000 . Uani d ? C(6) 0.128(1) 0.374(1) 0.0303(9) 0.041(4) 1.000 . Uani d ? C(7) 0.4257(8) 0.3312(9) 0.0458(8) 0.027(3) 1.000 . Uani d ? C(8) 0.5350(9) 0.169(1) 0.1893(9) 0.043(4) 1.000 . Uani d ? C(9) 0.0953(9) 0.090(1) 0.1095(9) 0.039(4) 1.000 . Uani d ? C(10) 0.1311(8) -0.0013(9) 0.0651(8) 0.026(3) 1.000 . Uani d ? C(11) 0.156(1) -0.109(1) 0.1139(9) 0.040(4) 1.000 . Uani d ? C(12) 0.274(1) -0.119(1) 0.1671(9) 0.038(4) 1.000 . Uani d ? C(13) 0.3296(9) -0.010(1) 0.1972(8) 0.031(3) 1.000 . Uani d ? C(14) 0.287(1) 0.068(1) 0.2484(8) 0.035(3) 1.000 . Uani d ? C(15) 0.187(1) 0.053(1) 0.2820(8) 0.041(4) 1.000 . Uani d ? C(16) 0.087(1) 0.093(1) 0.2111(8) 0.037(4) 1.000 . Uani d ? H(1b) 0.4184 0.4332 -0.1147 0.039 1.000 . Uiso c ? H(1c) 0.4194 0.3357 -0.1825 0.039 1.000 . Uiso c ? H(1a) 0.5164 0.3550 -0.0944 0.039 1.000 . Uiso c ? H(3b) 0.4109 0.1581 -0.1377 0.029 1.000 . Uiso c ? H(3a) 0.4979 0.1650 -0.0408 0.029 1.000 . Uiso c ? H(4b) 0.2036 -0.0541 -0.1268 0.039 1.000 . Uiso c ? H(4c) 0.2765 -0.0115 -0.1887 0.039 1.000 . Uiso c ? H(4a) 0.1973 0.0671 -0.1582 0.039 1.000 . Uiso c ? H(5b) 0.2509 0.3768 -0.1061 0.035 1.000 . Uiso c ? H(5a) 0.2474 0.2675 -0.1605 0.035 1.000 . Uiso c ? H(6b) 0.0788 0.3580 0.0688 0.046 1.000 . Uiso c ? H(6c) 0.0966 0.4276 -0.0151 0.046 1.000 . Uiso c ? H(6a) 0.1921 0.4040 0.0732 0.046 1.000 . Uiso c ? H(7b) 0.3934 0.4021 0.0458 0.033 1.000 . Uiso c ? H(7a) 0.5020 0.3419 0.0583 0.033 1.000 . Uiso c ? H(8b) 0.5393 0.1231 0.1352 0.051 1.000 . Uiso c ? H(8c) 0.5373 0.1218 0.2418 0.051 1.000 . Uiso c ? H(8a) 0.5958 0.2151 0.2036 0.051 1.000 . Uiso c ? H(9) 0.0419 0.1343 0.0647 0.047 1.000 . Uiso c ? H(10) 0.0975 -0.0066 -0.0032 0.031 1.000 . Uiso c ? H(11b) 0.1105 -0.1177 0.1567 0.047 1.000 . Uiso c ? H(11a) 0.1352 -0.1664 0.0660 0.047 1.000 . Uiso c ? H(12b) 0.2814 -0.1623 0.2239 0.045 1.000 . Uiso c ? H(12a) 0.3124 -0.1555 0.1276 0.045 1.000 . Uiso c ? H(13) 0.4062 -0.0113 0.2129 0.037 1.000 . Uiso c ? H(14) 0.3414 0.1117 0.2915 0.043 1.000 . Uiso c ? H(15b) 0.1788 -0.0232 0.2932 0.047 1.000 . Uiso c ? H(15a) 0.1951 0.0905 0.3415 0.047 1.000 . Uiso c ? H(16b) 0.0269 0.0488 0.2163 0.045 1.000 . Uiso c ? H(16a) 0.0727 0.1663 0.2276 0.045 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 Ir(1) 0.0180(2) 0.0253(2) 0.0251(2) -0.0005(2) 0.0080(2) 0.0005(2) Se(1) 0.0250(6) 0.0244(6) 0.0289(6) 0.0028(5) 0.0111(5) 0.0004(5) Se(2) 0.0187(5) 0.0293(6) 0.0324(6) 0.0016(5) 0.0071(5) 0.0034(5) Se(3) 0.0250(6) 0.0298(6) 0.0274(6) -0.0040(5) 0.0091(5) -0.0038(5) P(1) 0.037(2) 0.030(2) 0.033(2) 0.002(1) 0.007(1) -0.002(1) F(1) 0.051(5) 0.039(5) 0.059(5) 0.011(4) 0.013(4) 0.014(4) F(2) 0.053(5) 0.057(6) 0.063(5) 0.021(5) 0.005(4) 0.010(4) F(3) 0.083(7) 0.059(7) 0.17(1) -0.014(6) -0.045(8) -0.039(7) F(4) 0.17(1) 0.13(1) 0.070(6) 0.103(9) 0.082(7) 0.055(7) F(5) 0.056(6) 0.045(5) 0.115(8) -0.019(5) -0.002(5) 0.001(5) F(6) 0.081(7) 0.082(7) 0.073(6) 0.022(6) 0.050(5) 0.025(5) C(1) 0.033(7) 0.031(7) 0.042(7) 0.004(6) 0.016(6) 0.015(6) C(2) 0.017(5) 0.029(7) 0.030(6) -0.004(5) 0.013(5) 0.007(5) C(3) 0.027(6) 0.028(6) 0.023(6) -0.001(5) 0.014(5) 0.002(5) C(4) 0.040(7) 0.023(6) 0.033(6) -0.001(5) 0.010(5) 0.000(5) C(5) 0.019(6) 0.033(7) 0.038(6) -0.002(5) 0.013(5) 0.000(5) C(6) 0.044(8) 0.030(7) 0.053(8) 0.011(6) 0.022(6) 0.001(6) C(7) 0.023(6) 0.028(7) 0.031(6) -0.001(5) 0.009(5) 0.003(5) C(8) 0.021(6) 0.049(9) 0.057(8) 0.001(6) 0.005(6) 0.027(7) C(9) 0.019(6) 0.050(9) 0.055(8) -0.013(6) 0.021(6) 0.006(7) C(10) 0.021(6) 0.028(6) 0.029(6) -0.007(5) 0.006(5) 0.004(5) C(11) 0.051(8) 0.029(7) 0.047(7) -0.017(6) 0.024(6) -0.006(6) C(12) 0.045(8) 0.027(7) 0.046(7) 0.004(6) 0.018(6) 0.008(6) C(13) 0.024(6) 0.033(7) 0.035(6) 0.002(5) 0.004(5) 0.020(5) C(14) 0.037(7) 0.041(8) 0.029(6) 0.002(6) 0.008(5) 0.019(6) C(15) 0.047(8) 0.054(9) 0.026(6) -0.015(7) 0.019(6) -0.008(6) C(16) 0.036(7) 0.049(8) 0.035(7) -0.002(6) 0.023(6) -0.004(6) #------------------------------------------------------------------------------ _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) + 0.00006|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 3014 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0487 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.174 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.15 _refine_diff_density_max 1.46 #------------------------------------------------------------------------------ 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 Ir(1) Se(1) 2.570(1) . . yes Ir(1) Se(2) 2.481(1) . . yes Ir(1) Se(3) 2.478(1) . . yes Ir(1) C(9) 2.17(1) . . yes Ir(1) C(10) 2.13(1) . . yes Ir(1) C(13) 2.15(1) . . yes Ir(1) C(14) 2.19(1) . . yes Se(1) C(3) 1.97(1) . . yes Se(1) C(4) 1.94(1) . . yes Se(2) C(5) 1.97(1) . . yes Se(2) C(6) 1.96(1) . . yes Se(3) C(7) 1.96(1) . . yes Se(3) C(8) 1.95(1) . . yes P(1) F(1) 1.614(7) . . yes P(1) F(2) 1.604(8) . . yes P(1) F(3) 1.573(9) . . yes P(1) F(4) 1.542(9) . . yes P(1) F(5) 1.591(9) . . yes P(1) F(6) 1.580(9) . . yes C(1) C(2) 1.53(1) . . yes C(1) H(1a) 0.97 . . no C(1) H(1b) 0.95 . . no C(1) H(1c) 0.95 . . no C(2) C(3) 1.54(2) . . yes C(2) C(5) 1.53(1) . . yes C(2) C(7) 1.54(1) . . yes C(3) H(3a) 0.96 . . no C(3) H(3b) 0.97 . . no C(4) H(4a) 0.96 . . no C(4) H(4b) 0.96 . . no C(4) H(4c) 0.96 . . no C(5) H(5a) 0.97 . . no C(5) H(5b) 0.96 . . no C(6) H(6a) 0.97 . . no C(6) H(6b) 0.97 . . no C(6) H(6c) 0.95 . . no C(7) H(7a) 0.96 . . no C(7) H(7b) 0.96 . . no C(8) H(8a) 0.95 . . no C(8) H(8b) 0.98 . . no C(8) H(8c) 0.95 . . no C(9) C(10) 1.43(2) . . yes C(9) C(16) 1.51(2) . . yes C(9) H(9) 0.98 . . no C(10) C(11) 1.50(2) . . yes C(10) H(10) 0.97 . . no C(11) C(12) 1.53(2) . . yes C(11) H(11a) 0.97 . . no C(11) H(11b) 0.96 . . no C(12) C(13) 1.52(2) . . yes C(12) H(12a) 0.96 . . no C(12) H(12b) 0.96 . . no C(13) C(14) 1.41(2) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.51(2) . . yes C(14) H(14) 0.97 . . no C(15) C(16) 1.50(2) . . yes C(15) H(15a) 0.96 . . no C(15) H(15b) 0.96 . . no C(16) H(16a) 0.96 . . no C(16) H(16b) 0.96 . . 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) Ir(1) Se(2) 86.44(4) . . . yes Se(1) Ir(1) Se(3) 90.21(4) . . . yes Se(1) Ir(1) C(9) 131.4(4) . . . yes Se(1) Ir(1) C(10) 95.7(3) . . . yes Se(1) Ir(1) C(13) 90.2(3) . . . yes Se(1) Ir(1) C(14) 126.5(3) . . . yes Se(2) Ir(1) Se(3) 90.79(4) . . . yes Se(2) Ir(1) C(9) 81.3(3) . . . yes Se(2) Ir(1) C(10) 92.8(3) . . . yes Se(2) Ir(1) C(13) 172.2(3) . . . yes Se(2) Ir(1) C(14) 146.9(3) . . . yes Se(3) Ir(1) C(9) 136.5(4) . . . yes Se(3) Ir(1) C(10) 173.2(3) . . . yes Se(3) Ir(1) C(13) 96.3(3) . . . yes Se(3) Ir(1) C(14) 85.8(3) . . . yes C(9) Ir(1) C(10) 38.9(5) . . . yes C(9) Ir(1) C(13) 95.8(5) . . . yes C(9) Ir(1) C(14) 78.7(5) . . . yes C(10) Ir(1) C(13) 80.5(4) . . . yes C(10) Ir(1) C(14) 88.0(4) . . . yes C(13) Ir(1) C(14) 37.8(5) . . . yes Ir(1) Se(1) C(3) 107.7(3) . . . yes Ir(1) Se(1) C(4) 106.5(4) . . . yes C(3) Se(1) C(4) 99.6(5) . . . yes Ir(1) Se(2) C(5) 109.4(3) . . . yes Ir(1) Se(2) C(6) 107.5(4) . . . yes C(5) Se(2) C(6) 100.2(5) . . . yes Ir(1) Se(3) C(7) 108.9(3) . . . yes Ir(1) Se(3) C(8) 105.0(4) . . . yes C(7) Se(3) C(8) 98.3(5) . . . yes F(1) P(1) F(2) 177.7(5) . . . yes F(1) P(1) F(3) 89.7(5) . . . yes F(1) P(1) F(4) 88.8(5) . . . yes F(1) P(1) F(5) 89.3(4) . . . yes F(1) P(1) F(6) 91.4(4) . . . yes F(2) P(1) F(3) 92.3(5) . . . yes F(2) P(1) F(4) 89.9(5) . . . yes F(2) P(1) F(5) 88.8(5) . . . yes F(2) P(1) F(6) 89.9(5) . . . yes F(3) P(1) F(4) 91.4(7) . . . yes F(3) P(1) F(5) 177.0(7) . . . yes F(3) P(1) F(6) 89.0(7) . . . yes F(4) P(1) F(5) 91.5(7) . . . yes F(4) P(1) F(6) 179.6(7) . . . yes F(5) P(1) F(6) 88.2(5) . . . yes C(2) C(1) H(1a) 110.1 . . . no C(2) C(1) H(1b) 111.2 . . . no C(2) C(1) H(1c) 110.6 . . . no H(1a) C(1) H(1b) 108.1 . . . no H(1a) C(1) H(1c) 107.8 . . . no H(1b) C(1) H(1c) 109.0 . . . no C(1) C(2) C(3) 106.3(9) . . . yes C(1) C(2) C(5) 106.2(9) . . . yes C(1) C(2) C(7) 105.4(9) . . . yes C(3) C(2) C(5) 111.2(9) . . . yes C(3) C(2) C(7) 114.9(9) . . . yes C(5) C(2) C(7) 112.3(9) . . . yes Se(1) C(3) C(2) 121.1(7) . . . yes Se(1) C(3) H(3a) 106.9 . . . no Se(1) C(3) H(3b) 106.5 . . . no C(2) C(3) H(3a) 107.4 . . . no C(2) C(3) H(3b) 106.7 . . . no H(3a) C(3) H(3b) 107.6 . . . no Se(1) C(4) H(4a) 111.1 . . . no Se(1) C(4) H(4b) 110.9 . . . no Se(1) C(4) H(4c) 111.3 . . . no H(4a) C(4) H(4b) 107.5 . . . no H(4a) C(4) H(4c) 108.1 . . . no H(4b) C(4) H(4c) 107.9 . . . no Se(2) C(5) C(2) 121.5(8) . . . yes Se(2) C(5) H(5a) 107.1 . . . no Se(2) C(5) H(5b) 107.3 . . . no C(2) C(5) H(5a) 106.3 . . . no C(2) C(5) H(5b) 107.0 . . . no H(5a) C(5) H(5b) 106.9 . . . no Se(2) C(6) H(6a) 110.7 . . . no Se(2) C(6) H(6b) 110.8 . . . no Se(2) C(6) H(6c) 111.9 . . . no H(6a) C(6) H(6b) 106.5 . . . no H(6a) C(6) H(6c) 108.3 . . . no H(6b) C(6) H(6c) 108.4 . . . no Se(3) C(7) C(2) 121.8(8) . . . yes Se(3) C(7) H(7a) 106.7 . . . no Se(3) C(7) H(7b) 106.5 . . . no C(2) C(7) H(7a) 106.9 . . . no C(2) C(7) H(7b) 106.8 . . . no H(7a) C(7) H(7b) 107.3 . . . no Se(3) C(8) H(8a) 111.2 . . . no Se(3) C(8) H(8b) 109.6 . . . no Se(3) C(8) H(8c) 111.1 . . . no H(8a) C(8) H(8b) 107.5 . . . no H(8a) C(8) H(8c) 109.9 . . . no H(8b) C(8) H(8c) 107.4 . . . no Ir(1) C(9) C(10) 69.3(6) . . . yes Ir(1) C(9) C(16) 113.1(8) . . . yes Ir(1) C(9) H(9) 113.3 . . . no C(10) C(9) C(16) 125(1) . . . yes C(10) C(9) H(9) 113.1 . . . no C(16) C(9) H(9) 114.7 . . . no Ir(1) C(10) C(9) 71.9(6) . . . yes Ir(1) C(10) C(11) 116.0(7) . . . yes Ir(1) C(10) H(10) 112.6 . . . no C(9) C(10) C(11) 122(1) . . . yes C(9) C(10) H(10) 113.6 . . . no C(11) C(10) H(10) 113.7 . . . no C(10) C(11) C(12) 111(1) . . . yes C(10) C(11) H(11a) 108.5 . . . no C(10) C(11) H(11b) 108.1 . . . no C(12) C(11) H(11a) 110.6 . . . no C(12) C(11) H(11b) 111.2 . . . no H(11a) C(11) H(11b) 106.9 . . . no C(11) C(12) C(13) 114(1) . . . yes C(11) C(12) H(12a) 109.8 . . . no C(11) C(12) H(12b) 109.4 . . . no C(13) C(12) H(12a) 107.8 . . . no C(13) C(12) H(12b) 107.9 . . . no H(12a) C(12) H(12b) 107.8 . . . no Ir(1) C(13) C(12) 110.7(7) . . . yes Ir(1) C(13) C(14) 72.8(7) . . . yes Ir(1) C(13) H(13) 114.1 . . . no C(12) C(13) C(14) 122(1) . . . yes C(12) C(13) H(13) 115.6 . . . no C(14) C(13) H(13) 113.8 . . . no Ir(1) C(14) C(13) 69.4(6) . . . yes Ir(1) C(14) C(15) 114.4(8) . . . yes Ir(1) C(14) H(14) 113.5 . . . no C(13) C(14) C(15) 125(1) . . . yes C(13) C(14) H(14) 114.1 . . . no C(15) C(14) H(14) 113.0 . . . no C(14) C(15) C(16) 113(1) . . . yes C(14) C(15) H(15a) 109.6 . . . no C(14) C(15) H(15b) 108.2 . . . no C(16) C(15) H(15a) 109.2 . . . no C(16) C(15) H(15b) 108.4 . . . no H(15a) C(15) H(15b) 107.8 . . . no C(9) C(16) C(15) 113(1) . . . yes C(9) C(16) H(16a) 109.2 . . . no C(9) C(16) H(16b) 109.4 . . . no C(15) C(16) H(16a) 108.5 . . . no C(15) C(16) H(16b) 109.2 . . . no H(16a) C(16) H(16b) 107.5 . . . 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 F(1) C(4) 3.42(1) . 2 no F(1) C(12) 3.47(1) . 2 no F(1) C(11) 3.59(2) . 2 no F(2) C(6) 3.53(2) . 2_545 no F(3) C(16) 3.27(2) . 4 no F(3) C(9) 3.58(2) . 4 no F(3) C(4) 3.59(2) . 2 no F(4) C(4) 3.25(1) . 1_556 no F(4) C(8) 3.35(2) . 4_455 no F(4) C(5) 3.53(2) . 1_556 no F(5) C(5) 3.36(1) . 2_545 no F(5) C(7) 3.46(1) . 2_545 no F(5) C(1) 3.48(2) . 2_545 no F(5) C(6) 3.56(2) . 2_545 no F(6) C(6) 3.41(2) . 2_545 no F(6) C(11) 3.54(2) . 2 no F(6) C(6) 3.56(2) . 4 no C(1) C(16) 3.56(2) . 4_554 no C(9) C(10) 3.49(2) . 3 no C(10) C(10) 3.41(2) . 3 no #------------------------------------------------------------------------------ data_te3cod_[Rh(COD)(MeTe-tripod)]PF6 #------------------------------------------------------------------------------ _audit_creation_date '19100-05-11' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof. W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the structure of [Rh(cod){MeC(CH2TeMe)3}]PF6 included in Dalton manuscript number B0036540. ; _publ_contact_author_phone ' 023 80593792 ' _publ_contact_author_fax ' 023 80593781 ' _publ_contact_author_email ' wxl@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. 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. 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. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 27.203(3) _cell_length_b 14.998(4) _cell_length_c 12.658(3) _cell_angle_alpha 90 _cell_angle_beta 114.75(1) _cell_angle_gamma 90 _cell_volume 4690(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 15.6 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 853.08 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H30 F6 P Rh Te3 ' _chemical_formula_moiety '?' _chemical_formula_structural [Rh(cod){MeC(CH2TeMe)3}]PF6 _chemical_compound_source ? _exptl_crystal_F_000 3168.00 _exptl_absorpt_coefficient_mu 4.502 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.843 _exptl_special_details ; The scan width was (1.15+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _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 AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.88 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 -1 -3 7 -3 -3 8 -2 0 _diffrn_reflns_number 4400 _reflns_number_total 4303 _reflns_number_gt 2906 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02708 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02825 _diffrn_orient_matrix_UB_12 -0.04289 _diffrn_orient_matrix_UB_13 0.05030 _diffrn_orient_matrix_UB_21 -0.02674 _diffrn_orient_matrix_UB_22 -0.04987 _diffrn_orient_matrix_UB_23 -0.02914 _diffrn_orient_matrix_UB_31 0.01121 _diffrn_orient_matrix_UB_32 -0.01089 _diffrn_orient_matrix_UB_33 -0.06472 #------------------------------------------------------------------------------ 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, Tables 4.2.6.8 and 6.1.1.1) ; H 0 240 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 8 -1.287 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 24 -0.772 1.675 ;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 Te(1) 0.06324(2) 0.35382(3) 0.61120(5) 0.0374(1) 1.000 . Uani d ? Te(2) 0.18776(2) 0.22669(3) 0.68340(4) 0.0327(1) 1.000 . Uani d ? Te(3) 0.08317(2) 0.20078(3) 0.38989(4) 0.0324(1) 1.000 . Uani d ? Rh(1) 0.13487(2) 0.34066(4) 0.52352(5) 0.0321(2) 1.000 . Uani d ? P(1) 0.13483(8) 0.1616(1) 0.0602(2) 0.0363(5) 1.000 . Uani d ? F(1) 0.0981(2) 0.1827(4) 0.1259(5) 0.076(2) 1.000 . Uani d ? F(2) 0.1707(2) 0.1385(4) -0.0087(4) 0.068(2) 1.000 . Uani d ? F(3) 0.1012(2) 0.2326(3) -0.0378(4) 0.065(2) 1.000 . Uani d ? F(4) 0.1759(2) 0.2362(4) 0.1298(5) 0.079(2) 1.000 . Uani d ? F(5) 0.1682(2) 0.0902(4) 0.1545(5) 0.074(2) 1.000 . Uani d ? F(6) 0.0933(2) 0.0864(4) -0.0126(5) 0.079(2) 1.000 . Uani d ? C(1) 0.0462(3) 0.0592(5) 0.6655(7) 0.039(2) 1.000 . Uani d ? C(2) 0.0709(3) 0.1380(5) 0.6235(6) 0.031(2) 1.000 . Uani d ? C(3) 0.0495(3) 0.2221(5) 0.6616(6) 0.035(2) 1.000 . Uani d ? C(4) 0.1322(3) 0.1265(5) 0.6903(6) 0.030(2) 1.000 . Uani d ? C(5) 0.0503(3) 0.1278(5) 0.4923(6) 0.034(2) 1.000 . Uani d ? C(6) -0.0121(3) 0.3599(5) 0.4591(7) 0.046(2) 1.000 . Uani d ? C(7) 0.1992(3) 0.2889(6) 0.8423(7) 0.051(3) 1.000 . Uani d ? C(8) 0.1446(3) 0.1045(5) 0.4064(7) 0.042(2) 1.000 . Uani d ? C(9) 0.1102(4) 0.4784(6) 0.459(1) 0.073(4) 1.000 . Uani d ? C(10) 0.0967(4) 0.4207(6) 0.3664(8) 0.054(3) 1.000 . Uani d ? C(11) 0.1296(4) 0.4113(6) 0.2968(8) 0.057(3) 1.000 . Uani d ? C(12) 0.1902(4) 0.4042(6) 0.3684(8) 0.056(3) 1.000 . Uani d ? C(13) 0.1558(6) 0.5428(6) 0.500(1) 0.092(5) 1.000 . Uani d ? C(14) 0.2072(7) 0.506(1) 0.590(1) 0.109(6) 1.000 . Uani d ? C(15) 0.2125(4) 0.4076(6) 0.5849(8) 0.057(3) 1.000 . Uani d ? C(16) 0.2033(3) 0.3586(6) 0.4841(8) 0.051(3) 1.000 . Uani d ? H(1) 0.0078 0.0631 0.6293 0.046 1.000 . Uiso c ? H(2) 0.0573 0.0043 0.6450 0.046 1.000 . Uiso c ? H(3) 0.0584 0.0623 0.7475 0.046 1.000 . Uiso c ? H(4) 0.0114 0.2152 0.6327 0.042 1.000 . Uiso c ? H(5) 0.0650 0.2215 0.7442 0.042 1.000 . Uiso c ? H(6) 0.1413 0.0727 0.6630 0.036 1.000 . Uiso c ? H(7) 0.1391 0.1200 0.7700 0.036 1.000 . Uiso c ? H(8) 0.0129 0.1423 0.4609 0.040 1.000 . Uiso c ? H(9) 0.0545 0.0665 0.4790 0.040 1.000 . Uiso c ? H(10) -0.0413 0.3550 0.4815 0.055 1.000 . Uiso c ? H(11) -0.0138 0.3123 0.4083 0.055 1.000 . Uiso c ? H(12) -0.0145 0.4152 0.4206 0.055 1.000 . Uiso c ? H(13) 0.1654 0.3101 0.8374 0.061 1.000 . Uiso c ? H(14) 0.2235 0.3375 0.8566 0.061 1.000 . Uiso c ? H(15) 0.2137 0.2469 0.9039 0.061 1.000 . Uiso c ? H(16) 0.1678 0.0963 0.4862 0.050 1.000 . Uiso c ? H(17) 0.1279 0.0494 0.3737 0.050 1.000 . Uiso c ? H(18) 0.1651 0.1254 0.3663 0.050 1.000 . Uiso c ? H(19) 0.0796 0.4989 0.4702 0.088 1.000 . Uiso c ? H(20) 0.0590 0.4107 0.3237 0.065 1.000 . Uiso c ? H(21) 0.1179 0.3590 0.2505 0.068 1.000 . Uiso c ? H(22) 0.1229 0.4619 0.2477 0.068 1.000 . Uiso c ? H(23) 0.2055 0.3706 0.3260 0.068 1.000 . Uiso c ? H(24) 0.2053 0.4624 0.3822 0.068 1.000 . Uiso c ? H(25) 0.1624 0.5608 0.4349 0.110 1.000 . Uiso c ? H(26) 0.1458 0.5931 0.5318 0.110 1.000 . Uiso c ? H(27) 0.2366 0.5329 0.5800 0.130 1.000 . Uiso c ? H(28) 0.2089 0.5212 0.6643 0.130 1.000 . Uiso c ? H(29) 0.2394 0.3825 0.6540 0.069 1.000 . Uiso c ? H(30) 0.2254 0.3072 0.4972 0.061 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 Te(1) 0.0418(3) 0.0298(3) 0.0488(3) -0.0006(2) 0.0270(2) -0.0071(2) Te(2) 0.0257(2) 0.0396(3) 0.0315(3) -0.0032(2) 0.0107(2) -0.0043(2) Te(3) 0.0322(3) 0.0370(3) 0.0261(2) -0.0009(2) 0.0102(2) -0.0028(2) Rh(1) 0.0350(3) 0.0270(3) 0.0392(3) -0.0010(2) 0.0206(3) -0.0016(3) P(1) 0.036(1) 0.041(1) 0.032(1) -0.0056(9) 0.0143(9) -0.0001(9) F(1) 0.083(4) 0.094(4) 0.073(4) 0.028(4) 0.056(3) 0.022(3) F(2) 0.070(4) 0.089(4) 0.065(3) -0.006(3) 0.047(3) -0.004(3) F(3) 0.070(3) 0.065(3) 0.051(3) 0.013(3) 0.015(3) 0.023(3) F(4) 0.060(3) 0.059(4) 0.091(4) -0.021(3) 0.006(3) -0.030(3) F(5) 0.088(4) 0.070(4) 0.064(3) 0.030(3) 0.032(3) 0.025(3) F(6) 0.064(3) 0.067(4) 0.097(4) -0.030(3) 0.024(3) -0.021(3) C(1) 0.041(4) 0.036(4) 0.044(4) -0.008(4) 0.022(4) 0.000(4) C(2) 0.029(4) 0.030(4) 0.033(4) -0.002(3) 0.013(3) -0.002(3) C(3) 0.041(4) 0.038(4) 0.029(4) -0.002(3) 0.019(3) 0.002(3) C(4) 0.032(4) 0.027(4) 0.027(4) -0.004(3) 0.008(3) 0.001(3) C(5) 0.025(4) 0.034(4) 0.042(4) -0.005(3) 0.014(3) -0.009(3) C(6) 0.040(5) 0.035(4) 0.064(6) 0.009(4) 0.023(4) 0.011(4) C(7) 0.045(5) 0.069(6) 0.041(5) -0.018(4) 0.019(4) -0.024(4) C(8) 0.048(5) 0.044(5) 0.041(4) 0.005(4) 0.025(4) -0.007(4) C(9) 0.086(8) 0.040(5) 0.13(1) 0.023(5) 0.081(8) 0.015(6) C(10) 0.064(6) 0.036(5) 0.070(6) 0.018(4) 0.035(5) 0.023(5) C(11) 0.077(6) 0.056(6) 0.052(5) 0.025(5) 0.041(5) 0.017(4) C(12) 0.064(6) 0.055(6) 0.066(6) 0.008(5) 0.043(5) 0.010(5) C(13) 0.15(1) 0.028(5) 0.16(1) -0.016(7) 0.12(1) -0.014(7) C(14) 0.16(1) 0.09(1) 0.12(1) -0.07(1) 0.10(1) -0.053(9) C(15) 0.064(6) 0.060(6) 0.058(6) -0.031(5) 0.035(5) -0.013(5) C(16) 0.039(5) 0.056(6) 0.062(6) -0.002(4) 0.026(4) 0.006(5) #------------------------------------------------------------------------------ _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) + 0.00016|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 2906 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0343 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.65 _refine_diff_density_max 0.56 #------------------------------------------------------------------------------ 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 Te(1) Rh(1) 2.6226(8) . . yes Te(1) C(3) 2.156(7) . . yes Te(1) C(6) 2.147(8) . . yes Te(2) Rh(1) 2.5786(8) . . yes Te(2) C(4) 2.158(7) . . yes Te(2) C(7) 2.118(8) . . yes Te(3) Rh(1) 2.6924(7) . . yes Te(3) C(5) 2.156(7) . . yes Te(3) C(8) 2.151(7) . . yes Rh(1) C(9) 2.219(9) . . yes Rh(1) C(10) 2.178(8) . . yes Rh(1) C(15) 2.167(8) . . yes Rh(1) C(16) 2.135(8) . . yes P(1) F(1) 1.577(5) . . yes P(1) F(2) 1.595(5) . . yes P(1) F(3) 1.600(5) . . yes P(1) F(4) 1.566(5) . . yes P(1) F(5) 1.578(5) . . yes P(1) F(6) 1.589(5) . . yes C(1) C(2) 1.558(9) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.55(1) . . yes C(2) C(4) 1.532(9) . . yes C(2) C(5) 1.52(1) . . yes C(3) H(4) 0.95 . . no C(3) H(5) 0.95 . . no C(4) H(6) 0.95 . . no C(4) H(7) 0.95 . . no C(5) H(8) 0.95 . . no C(5) H(9) 0.95 . . no C(6) H(10) 0.95 . . no C(6) H(11) 0.95 . . no C(6) H(12) 0.95 . . no C(7) H(13) 0.95 . . no C(7) H(14) 0.95 . . no C(7) H(15) 0.95 . . no C(8) H(16) 0.95 . . no C(8) H(17) 0.95 . . no C(8) H(18) 0.95 . . no C(9) C(10) 1.38(1) . . yes C(9) C(13) 1.49(2) . . yes C(9) H(19) 0.95 . . no C(10) C(11) 1.50(1) . . yes C(10) H(20) 0.95 . . no C(11) C(12) 1.51(1) . . yes C(11) H(21) 0.95 . . no C(11) H(22) 0.95 . . no C(12) C(16) 1.52(1) . . yes C(12) H(23) 0.95 . . no C(12) H(24) 0.95 . . no C(13) C(14) 1.49(2) . . yes C(13) H(25) 0.95 . . no C(13) H(26) 0.95 . . no C(14) C(15) 1.49(2) . . yes C(14) H(27) 0.95 . . no C(14) H(28) 0.95 . . no C(15) C(16) 1.40(1) . . yes C(15) H(29) 0.95 . . no C(16) 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 Rh(1) Te(1) C(3) 107.9(2) . . . yes Rh(1) Te(1) C(6) 102.9(2) . . . yes C(3) Te(1) C(6) 94.9(3) . . . yes Rh(1) Te(2) C(4) 108.9(2) . . . yes Rh(1) Te(2) C(7) 105.4(3) . . . yes C(4) Te(2) C(7) 95.4(3) . . . yes Rh(1) Te(3) C(5) 104.9(2) . . . yes Rh(1) Te(3) C(8) 106.4(2) . . . yes C(5) Te(3) C(8) 95.8(3) . . . yes Te(1) Rh(1) Te(2) 89.26(2) . . . yes Te(1) Rh(1) Te(3) 92.25(2) . . . yes Te(1) Rh(1) C(9) 85.5(2) . . . yes Te(1) Rh(1) C(10) 101.0(2) . . . yes Te(1) Rh(1) C(15) 126.7(2) . . . yes Te(1) Rh(1) C(16) 164.5(2) . . . yes Te(2) Rh(1) Te(3) 87.11(2) . . . yes Te(2) Rh(1) C(9) 152.8(3) . . . yes Te(2) Rh(1) C(10) 167.9(2) . . . yes Te(2) Rh(1) C(15) 83.5(3) . . . yes Te(2) Rh(1) C(16) 90.7(2) . . . yes Te(3) Rh(1) C(9) 119.8(3) . . . yes Te(3) Rh(1) C(10) 86.1(3) . . . yes Te(3) Rh(1) C(15) 139.5(3) . . . yes Te(3) Rh(1) C(16) 103.2(2) . . . yes C(9) Rh(1) C(10) 36.5(4) . . . yes C(9) Rh(1) C(15) 78.5(4) . . . yes C(9) Rh(1) C(16) 87.5(3) . . . yes C(10) Rh(1) C(15) 95.3(4) . . . yes C(10) Rh(1) C(16) 81.1(3) . . . yes C(15) Rh(1) C(16) 38.0(3) . . . yes F(1) P(1) F(2) 178.4(3) . . . yes F(1) P(1) F(3) 89.6(3) . . . yes F(1) P(1) F(4) 91.2(3) . . . yes F(1) P(1) F(5) 91.6(3) . . . yes F(1) P(1) F(6) 89.7(3) . . . yes F(2) P(1) F(3) 90.2(3) . . . yes F(2) P(1) F(4) 90.4(3) . . . yes F(2) P(1) F(5) 88.6(3) . . . yes F(2) P(1) F(6) 88.8(3) . . . yes F(3) P(1) F(4) 90.1(3) . . . yes F(3) P(1) F(5) 178.6(3) . . . yes F(3) P(1) F(6) 89.2(3) . . . yes F(4) P(1) F(5) 90.5(3) . . . yes F(4) P(1) F(6) 178.9(4) . . . yes F(5) P(1) F(6) 90.1(3) . . . yes C(2) C(1) H(1) 109.4 . . . no C(2) C(1) H(2) 109.4 . . . no C(2) C(1) H(3) 109.4 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.6 . . . no H(2) C(1) H(3) 109.5 . . . no C(1) C(2) C(3) 103.9(6) . . . yes C(1) C(2) C(4) 104.6(6) . . . yes C(1) C(2) C(5) 106.4(6) . . . yes C(3) C(2) C(4) 112.6(6) . . . yes C(3) C(2) C(5) 114.0(6) . . . yes C(4) C(2) C(5) 114.1(6) . . . yes Te(1) C(3) C(2) 121.4(5) . . . yes Te(1) C(3) H(4) 106.4 . . . no Te(1) C(3) H(5) 106.4 . . . no C(2) C(3) H(4) 106.4 . . . no C(2) C(3) H(5) 106.4 . . . no H(4) C(3) H(5) 109.5 . . . no Te(2) C(4) C(2) 121.3(5) . . . yes Te(2) C(4) H(6) 106.5 . . . no Te(2) C(4) H(7) 106.5 . . . no C(2) C(4) H(6) 106.5 . . . no C(2) C(4) H(7) 106.4 . . . no H(6) C(4) H(7) 109.4 . . . no Te(3) C(5) C(2) 123.4(5) . . . yes Te(3) C(5) H(8) 105.9 . . . no Te(3) C(5) H(9) 105.9 . . . no C(2) C(5) H(8) 105.8 . . . no C(2) C(5) H(9) 105.8 . . . no H(8) C(5) H(9) 109.5 . . . no Te(1) C(6) H(10) 109.4 . . . no Te(1) C(6) H(11) 109.4 . . . no Te(1) C(6) H(12) 109.4 . . . no H(10) C(6) H(11) 109.6 . . . no H(10) C(6) H(12) 109.5 . . . no H(11) C(6) H(12) 109.6 . . . no Te(2) C(7) H(13) 109.4 . . . no Te(2) C(7) H(14) 109.4 . . . no Te(2) C(7) H(15) 109.4 . . . no H(13) C(7) H(14) 109.5 . . . no H(13) C(7) H(15) 109.5 . . . no H(14) C(7) H(15) 109.5 . . . no Te(3) C(8) H(16) 109.5 . . . no Te(3) C(8) H(17) 109.4 . . . no Te(3) C(8) H(18) 109.4 . . . no H(16) C(8) H(17) 109.5 . . . no H(16) C(8) H(18) 109.5 . . . no H(17) C(8) H(18) 109.5 . . . no Rh(1) C(9) C(10) 70.1(5) . . . yes Rh(1) C(9) C(13) 113.4(8) . . . yes Rh(1) C(9) H(19) 113.3 . . . no C(10) C(9) C(13) 126.0(9) . . . yes C(10) C(9) H(19) 113.1 . . . no C(13) C(9) H(19) 113.3 . . . no Rh(1) C(10) C(9) 73.3(6) . . . yes Rh(1) C(10) C(11) 108.1(5) . . . yes Rh(1) C(10) H(20) 114.9 . . . no C(9) C(10) C(11) 123.2(9) . . . yes C(9) C(10) H(20) 114.9 . . . no C(11) C(10) H(20) 114.8 . . . no C(10) C(11) C(12) 114.9(8) . . . yes C(10) C(11) H(21) 108.1 . . . no C(10) C(11) H(22) 108.1 . . . no C(12) C(11) H(21) 108.1 . . . no C(12) C(11) H(22) 108.1 . . . no H(21) C(11) H(22) 109.5 . . . no C(11) C(12) C(16) 111.5(7) . . . yes C(11) C(12) H(23) 108.9 . . . no C(11) C(12) H(24) 109.0 . . . no C(16) C(12) H(23) 108.9 . . . no C(16) C(12) H(24) 109.1 . . . no H(23) C(12) H(24) 109.5 . . . no C(9) C(13) C(14) 114(1) . . . yes C(9) C(13) H(25) 108.7 . . . no C(9) C(13) H(26) 108.4 . . . no C(14) C(13) H(25) 108.2 . . . no C(14) C(13) H(26) 108.0 . . . no H(25) C(13) H(26) 109.6 . . . no C(13) C(14) C(15) 114(1) . . . yes C(13) C(14) H(27) 108.3 . . . no C(13) C(14) H(28) 108.4 . . . no C(15) C(14) H(27) 108.2 . . . no C(15) C(14) H(28) 108.2 . . . no H(27) C(14) H(28) 109.6 . . . no Rh(1) C(15) C(14) 112.2(9) . . . yes Rh(1) C(15) C(16) 69.8(5) . . . yes Rh(1) C(15) H(29) 113.9 . . . no C(14) C(15) C(16) 125(1) . . . yes C(14) C(15) H(29) 113.9 . . . no C(16) C(15) H(29) 113.9 . . . no Rh(1) C(16) C(12) 114.0(6) . . . yes Rh(1) C(16) C(15) 72.2(5) . . . yes Rh(1) C(16) H(30) 114.1 . . . no C(12) C(16) C(15) 121.6(8) . . . yes C(12) C(16) H(30) 114.2 . . . no C(15) C(16) H(30) 114.1 . . . 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 Te(2) F(4) 3.508(5) . 7_556 no Te(3) F(1) 3.541(5) . . no F(1) H(8) 2.8126 . 2 no F(1) H(11) 2.8977 . 2 no F(1) H(18) 2.9450 . . no F(1) H(21) 3.0104 . . no F(1) H(10) 3.0269 . 2 no F(1) C(6) 3.40(1) . 2 no F(1) C(8) 3.438(9) . . no F(2) H(15) 2.5161 . 1_554 no F(2) H(7) 2.5786 . 1_554 no F(2) H(14) 2.7347 . 7_556 no F(2) C(7) 3.24(1) . 1_554 no F(2) C(7) 3.451(9) . 7_556 no F(2) C(4) 3.508(8) . 1_554 no F(3) H(5) 2.5169 . 1_554 no F(3) H(10) 2.7406 . 2 no F(3) H(4) 2.7950 . 2 no F(3) H(26) 2.8603 . 4_564 no F(3) H(13) 3.0332 . 1_554 no F(3) C(3) 3.464(9) . 1_554 no F(3) C(6) 3.54(1) . 2 no F(4) H(26) 2.8133 . 4_564 no F(4) H(14) 2.8871 . 7_556 no F(4) H(23) 3.0337 . . no F(4) C(7) 3.29(1) . 7_556 no F(5) H(6) 2.5660 . 4_554 no F(5) H(29) 2.6944 . 7_556 no F(5) H(18) 2.7684 . . no F(5) C(4) 3.479(9) . 4_554 no F(5) C(8) 3.513(9) . . no F(5) C(15) 3.53(1) . 7_556 no F(6) H(9) 2.5086 . 4_554 no F(6) H(1) 2.5427 . 2 no F(6) H(3) 2.7999 . 1_554 no F(6) H(17) 2.8714 . 4_554 no F(6) H(2) 2.9026 . 4_554 no F(6) C(5) 3.429(9) . 4_554 no F(6) C(1) 3.487(9) . 2 no F(6) C(8) 3.52(1) . 4_554 no C(6) H(21) 2.9882 . 2 no C(6) C(11) 3.55(1) . 2 no C(7) H(25) 2.9046 . 4_565 no C(12) H(28) 3.0481 . 4_564 no H(1) H(9) 2.5666 . 3_556 no H(3) H(17) 2.5306 . 4 no H(10) H(19) 2.6078 . 3_566 no H(13) H(25) 2.3158 . 4_565 no H(15) H(15) 2.4090 . 7_557 no H(23) H(28) 2.6445 . 4_564 no H(30) H(30) 2.1584 . 7_556 no #------------------------------------------------------------------------------ data_sdocod_[Rh(COD)(Se-tripod)]PF6 #------------------------------------------------------------------------------ _audit_creation_date '19100-05-11' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Rh(cod){MeC(CH2SeMe)3}]PF6 included in manuscript number B0036540. ; _publ_contact_author_phone ' 023 80593792 ' _publ_contact_author_fax ' 023 80593781 ' _publ_contact_author_email ' wxl@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. 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. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.857(3) _cell_length_b 12.278(3) _cell_length_c 14.514(3) _cell_angle_alpha 90 _cell_angle_beta 105.40(2) _cell_angle_gamma 90 _cell_volume 2209.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 9.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _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,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rod' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 707.16 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H30 F6 P Rh Se3 ' _chemical_formula_moiety '?' _chemical_formula_structural [Rh(cod){MeC(CH2SeMe)3}]PF6 _chemical_compound_source ? _exptl_crystal_F_000 1368.00 _exptl_absorpt_coefficient_mu 5.838 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; DIFABS (Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.611 _exptl_special_details ; The scan width was (0.73+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _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 AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.57 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -3 -4 -1 -4 -3 -2 -3 -2 _diffrn_reflns_number 4289 _reflns_number_total 4098 _reflns_number_gt 1792 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.07138 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05263 _diffrn_orient_matrix_UB_12 -0.05863 _diffrn_orient_matrix_UB_13 0.00395 _diffrn_orient_matrix_UB_21 -0.05664 _diffrn_orient_matrix_UB_22 0.05634 _diffrn_orient_matrix_UB_23 -0.00168 _diffrn_orient_matrix_UB_31 -0.02304 _diffrn_orient_matrix_UB_32 -0.00457 _diffrn_orient_matrix_UB_33 -0.07133 #------------------------------------------------------------------------------ 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 64 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) ; 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 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 12 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 4 -1.287 0.919 ;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 Rh(1) 0.2569(1) 0.1160(1) 0.10107(9) 0.0175(3) 1.000 . Uani d ? Se(1) 0.4027(1) 0.2520(1) 0.1553(1) 0.0221(4) 1.000 . Uani d ? Se(2) 0.3547(1) 0.0416(1) -0.0243(1) 0.0194(4) 1.000 . Uani d ? Se(3) 0.1611(1) 0.2399(1) -0.0291(1) 0.0205(4) 1.000 . Uani d ? P(1) 0.2955(4) 0.1569(4) 0.5962(3) 0.029(1) 1.000 . Uani d ? F(1) 0.345(1) 0.1426(9) 0.5091(8) 0.065(4) 1.000 . Uani d ? F(2) 0.247(1) 0.172(1) 0.6838(7) 0.088(5) 1.000 . Uani d ? F(3) 0.3742(9) 0.0630(8) 0.6533(7) 0.053(4) 1.000 . Uani d ? F(4) 0.385(1) 0.244(1) 0.6377(9) 0.088(5) 1.000 . Uani d ? F(5) 0.2165(8) 0.2498(8) 0.5414(7) 0.044(3) 1.000 . Uani d ? F(6) 0.2058(9) 0.0684(9) 0.5504(9) 0.069(4) 1.000 . Uani d ? C(1) 0.286(1) 0.070(1) 0.251(1) 0.023(5) 1.000 . Uani d ? C(2) 0.330(1) -0.008(1) 0.199(1) 0.030(5) 1.000 . Uani d ? C(3) 0.276(2) -0.116(1) 0.168(1) 0.036(6) 1.000 . Uani d ? C(4) 0.157(1) -0.107(1) 0.117(1) 0.023(5) 1.000 . Uani d ? C(5) 0.131(1) -0.002(1) 0.069(1) 0.023(5) 1.000 . Uani d ? C(6) 0.093(1) 0.089(1) 0.111(1) 0.027(5) 1.000 . Uani d ? C(7) 0.087(1) 0.094(1) 0.215(1) 0.024(5) 1.000 . Uani d ? C(8) 0.188(1) 0.051(1) 0.285(1) 0.027(5) 1.000 . Uani d ? C(9) 0.536(1) 0.166(1) 0.189(1) 0.042(6) 1.000 . Uani d ? C(10) 0.244(1) 0.006(1) -0.140(1) 0.032(5) 1.000 . Uani d ? C(11) 0.124(1) 0.374(1) 0.030(1) 0.033(5) 1.000 . Uani d ? C(12) 0.437(1) 0.356(1) -0.121(1) 0.030(5) 1.000 . Uani d ? C(13) 0.385(1) 0.285(1) -0.056(1) 0.015(4) 1.000 . Uani d ? C(14) 0.427(1) 0.330(1) 0.045(1) 0.023(5) 1.000 . Uani d ? C(15) 0.425(1) 0.166(1) -0.071(1) 0.022(5) 1.000 . Uani d ? C(16) 0.263(1) 0.299(1) -0.096(1) 0.017(4) 1.000 . Uani d ? H(1) 0.3395 0.1135 0.2932 0.027 1.000 . Uiso c ? H(2) 0.4070 -0.0100 0.2146 0.035 1.000 . Uiso c ? H(3) 0.3112 -0.1510 0.1268 0.043 1.000 . Uiso c ? H(4) 0.2825 -0.1601 0.2238 0.043 1.000 . Uiso c ? H(5) 0.1378 -0.1639 0.0709 0.028 1.000 . Uiso c ? H(6) 0.1154 -0.1150 0.1623 0.028 1.000 . Uiso c ? H(7) 0.0983 -0.0086 0.0021 0.028 1.000 . Uiso c ? H(8) 0.0402 0.1314 0.0672 0.033 1.000 . Uiso c ? H(9) 0.0770 0.1682 0.2300 0.028 1.000 . Uiso c ? H(10) 0.0272 0.0523 0.2202 0.028 1.000 . Uiso c ? H(11) 0.1971 0.0872 0.3447 0.033 1.000 . Uiso c ? H(12) 0.1803 -0.0248 0.2934 0.033 1.000 . Uiso c ? H(13) 0.5360 0.1212 0.2425 0.051 1.000 . Uiso c ? H(14) 0.5960 0.2136 0.2048 0.051 1.000 . Uiso c ? H(15) 0.5391 0.1218 0.1364 0.051 1.000 . Uiso c ? H(16) 0.2769 -0.0131 -0.1894 0.038 1.000 . Uiso c ? H(17) 0.1986 0.0678 -0.1601 0.038 1.000 . Uiso c ? H(18) 0.2019 -0.0531 -0.1284 0.038 1.000 . Uiso c ? H(19) 0.1880 0.4043 0.0702 0.039 1.000 . Uiso c ? H(20) 0.0923 0.4245 -0.0190 0.039 1.000 . Uiso c ? H(21) 0.0750 0.3569 0.0661 0.039 1.000 . Uiso c ? H(22) 0.5139 0.3515 -0.0987 0.037 1.000 . Uiso c ? H(23) 0.4155 0.4295 -0.1193 0.037 1.000 . Uiso c ? H(24) 0.4151 0.3296 -0.1849 0.037 1.000 . Uiso c ? H(25) 0.5032 0.3369 0.0565 0.027 1.000 . Uiso c ? H(26) 0.3960 0.4000 0.0451 0.027 1.000 . Uiso c ? H(27) 0.4997 0.1628 -0.0396 0.027 1.000 . Uiso c ? H(28) 0.4146 0.1564 -0.1377 0.027 1.000 . Uiso c ? H(29) 0.2449 0.2660 -0.1576 0.020 1.000 . Uiso c ? H(30) 0.2497 0.3747 -0.1022 0.020 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 Rh(1) 0.0163(7) 0.0178(7) 0.0186(7) -0.0012(6) 0.0050(5) 0.0006(6) Se(1) 0.024(1) 0.0230(8) 0.0193(9) -0.0047(8) 0.0058(7) -0.0035(7) Se(2) 0.022(1) 0.0168(8) 0.0204(9) 0.0024(7) 0.0068(7) -0.0003(7) Se(3) 0.0173(9) 0.0221(9) 0.0210(9) 0.0010(8) 0.0034(7) 0.0033(7) P(1) 0.038(3) 0.024(2) 0.026(3) 0.008(2) 0.007(2) -0.001(2) F(1) 0.10(1) 0.066(8) 0.046(7) 0.016(7) 0.045(7) 0.012(6) F(2) 0.13(1) 0.13(1) 0.027(7) 0.08(1) 0.046(8) 0.023(7) F(3) 0.051(8) 0.055(7) 0.049(7) 0.037(6) 0.005(6) 0.004(6) F(4) 0.07(1) 0.058(8) 0.11(1) -0.016(7) -0.023(8) -0.023(8) F(5) 0.059(8) 0.033(6) 0.043(6) 0.016(6) 0.016(6) 0.009(5) F(6) 0.049(8) 0.054(8) 0.10(1) -0.021(6) 0.006(7) -0.001(7) C(1) 0.03(1) 0.028(9) 0.006(8) 0.000(8) -0.002(8) 0.012(7) C(2) 0.03(1) 0.03(1) 0.03(1) 0.002(8) 0.008(8) 0.016(8) C(3) 0.05(1) 0.020(9) 0.04(1) 0.004(9) 0.01(1) -0.004(9) C(4) 0.03(1) 0.024(9) 0.017(9) -0.013(8) 0.005(8) -0.007(7) C(5) 0.013(9) 0.03(1) 0.018(9) -0.018(8) -0.002(7) 0.008(8) C(6) 0.03(1) 0.03(1) 0.025(9) -0.002(8) 0.012(8) 0.001(8) C(7) 0.018(9) 0.03(1) 0.025(9) -0.013(8) 0.016(8) -0.010(8) C(8) 0.04(1) 0.03(1) 0.012(8) 0.017(9) 0.009(8) 0.003(7) C(9) 0.03(1) 0.05(1) 0.04(1) 0.010(9) 0.00(1) 0.01(1) C(10) 0.05(1) 0.017(9) 0.023(9) -0.011(8) 0.002(9) -0.014(7) C(11) 0.05(1) 0.021(9) 0.027(9) 0.013(9) 0.016(9) -0.003(8) C(12) 0.03(1) 0.021(9) 0.04(1) -0.002(8) 0.014(9) 0.008(8) C(13) 0.009(9) 0.021(9) 0.018(8) 0.006(6) 0.007(7) 0.003(6) C(14) 0.04(1) 0.008(8) 0.019(9) 0.002(7) 0.005(8) 0.000(7) C(15) 0.009(9) 0.025(9) 0.04(1) -0.004(7) 0.015(8) -0.008(8) C(16) 0.02(1) 0.001(7) 0.031(9) 0.002(6) 0.008(8) 0.003(7) #------------------------------------------------------------------------------ _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) + 0.00024|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 1792 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0537 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.279 _refine_ls_shift/su_max 0.0280 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.82 _refine_diff_density_max 0.80 #------------------------------------------------------------------------------ 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 Rh(1) Se(1) 2.479(2) . . yes Rh(1) Se(2) 2.635(2) . . yes Rh(1) Se(3) 2.483(2) . . yes Rh(1) C(1) 2.18(1) . . yes Rh(1) C(2) 2.13(1) . . yes Rh(1) C(5) 2.13(1) . . yes Rh(1) C(6) 2.17(2) . . yes Se(1) C(9) 1.96(2) . . yes Se(1) C(14) 1.96(1) . . yes Se(2) C(10) 1.94(2) . . yes Se(2) C(15) 1.99(1) . . yes Se(3) C(11) 1.97(1) . . yes Se(3) C(16) 1.96(1) . . yes P(1) F(1) 1.57(1) . . yes P(1) F(2) 1.57(1) . . yes P(1) F(3) 1.61(1) . . yes P(1) F(4) 1.57(1) . . yes P(1) F(5) 1.59(1) . . yes P(1) F(6) 1.59(1) . . yes C(1) C(2) 1.43(2) . . yes C(1) C(8) 1.49(2) . . yes C(1) H(1) 0.95 . . no C(2) C(3) 1.51(2) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.52(2) . . yes C(3) H(3) 0.95 . . no C(3) H(4) 0.95 . . no C(4) C(5) 1.47(2) . . yes C(4) H(5) 0.95 . . no C(4) H(6) 0.95 . . no C(5) C(6) 1.42(2) . . yes C(5) H(7) 0.95 . . no C(6) C(7) 1.53(2) . . yes C(6) H(8) 0.95 . . no C(7) C(8) 1.52(2) . . yes C(7) H(9) 0.95 . . no C(7) H(10) 0.95 . . no C(8) H(11) 0.95 . . no C(8) H(12) 0.95 . . no C(9) H(13) 0.95 . . no C(9) H(14) 0.95 . . no C(9) H(15) 0.95 . . no C(10) H(16) 0.95 . . no C(10) H(17) 0.95 . . no C(10) H(18) 0.95 . . no C(11) H(19) 0.95 . . no C(11) H(20) 0.95 . . no C(11) H(21) 0.95 . . no C(12) C(13) 1.56(2) . . yes C(12) H(22) 0.95 . . no C(12) H(23) 0.95 . . no C(12) H(24) 0.95 . . no C(13) C(14) 1.52(2) . . yes C(13) C(15) 1.58(2) . . yes C(13) C(16) 1.53(2) . . yes C(14) H(25) 0.95 . . no C(14) H(26) 0.95 . . no C(15) H(27) 0.95 . . no C(15) H(28) 0.95 . . no C(16) H(29) 0.95 . . no C(16) 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 Se(1) Rh(1) Se(2) 89.64(7) . . . yes Se(1) Rh(1) Se(3) 90.55(7) . . . yes Se(1) Rh(1) C(1) 86.6(4) . . . yes Se(1) Rh(1) C(2) 96.1(5) . . . yes Se(1) Rh(1) C(5) 174.4(4) . . . yes Se(1) Rh(1) C(6) 138.3(4) . . . yes Se(2) Rh(1) Se(3) 85.29(6) . . . yes Se(2) Rh(1) C(1) 127.6(4) . . . yes Se(2) Rh(1) C(2) 90.3(5) . . . yes Se(2) Rh(1) C(5) 94.9(5) . . . yes Se(2) Rh(1) C(6) 129.8(4) . . . yes Se(3) Rh(1) C(1) 146.9(4) . . . yes Se(3) Rh(1) C(2) 172.0(5) . . . yes Se(3) Rh(1) C(5) 93.1(4) . . . yes Se(3) Rh(1) C(6) 81.3(4) . . . yes C(1) Rh(1) C(2) 38.6(6) . . . yes C(1) Rh(1) C(5) 88.0(6) . . . yes C(1) Rh(1) C(6) 79.1(6) . . . yes C(2) Rh(1) C(5) 80.6(6) . . . yes C(2) Rh(1) C(6) 96.6(6) . . . yes C(5) Rh(1) C(6) 38.6(6) . . . yes Rh(1) Se(1) C(9) 104.6(5) . . . yes Rh(1) Se(1) C(14) 110.0(4) . . . yes C(9) Se(1) C(14) 98.5(7) . . . yes Rh(1) Se(2) C(10) 107.6(5) . . . yes Rh(1) Se(2) C(15) 108.1(4) . . . yes C(10) Se(2) C(15) 99.8(7) . . . yes Rh(1) Se(3) C(11) 108.0(5) . . . yes Rh(1) Se(3) C(16) 109.9(4) . . . yes C(11) Se(3) C(16) 100.2(6) . . . yes F(1) P(1) F(2) 179.3(8) . . . yes F(1) P(1) F(3) 89.9(6) . . . yes F(1) P(1) F(4) 88.3(7) . . . yes F(1) P(1) F(5) 91.2(6) . . . yes F(1) P(1) F(6) 89.6(7) . . . yes F(2) P(1) F(3) 90.0(6) . . . yes F(2) P(1) F(4) 91.0(8) . . . yes F(2) P(1) F(5) 88.9(6) . . . yes F(2) P(1) F(6) 91.1(8) . . . yes F(3) P(1) F(4) 89.8(7) . . . yes F(3) P(1) F(5) 178.8(6) . . . yes F(3) P(1) F(6) 90.7(6) . . . yes F(4) P(1) F(5) 90.4(7) . . . yes F(4) P(1) F(6) 177.9(8) . . . yes F(5) P(1) F(6) 89.2(6) . . . yes Rh(1) C(1) C(2) 68.6(8) . . . yes Rh(1) C(1) C(8) 116(1) . . . yes Rh(1) C(1) H(1) 113.6 . . . no C(2) C(1) C(8) 124(1) . . . yes C(2) C(1) H(1) 113.6 . . . no C(8) C(1) H(1) 113.6 . . . no Rh(1) C(2) C(1) 72.8(9) . . . yes Rh(1) C(2) C(3) 110(1) . . . yes Rh(1) C(2) H(2) 115.0 . . . no C(1) C(2) C(3) 122(2) . . . yes C(1) C(2) H(2) 115.0 . . . no C(3) C(2) H(2) 115.0 . . . no C(2) C(3) C(4) 114(1) . . . yes C(2) C(3) H(3) 108.3 . . . no C(2) C(3) H(4) 108.3 . . . no C(4) C(3) H(3) 108.2 . . . no C(4) C(3) H(4) 108.2 . . . no H(3) C(3) H(4) 109.5 . . . no C(3) C(4) C(5) 111(1) . . . yes C(3) C(4) H(5) 109.1 . . . no C(3) C(4) H(6) 109.1 . . . no C(5) C(4) H(5) 108.9 . . . no C(5) C(4) H(6) 108.8 . . . no H(5) C(4) H(6) 109.4 . . . no Rh(1) C(5) C(4) 116(1) . . . yes Rh(1) C(5) C(6) 72.3(9) . . . yes Rh(1) C(5) H(7) 113.0 . . . no C(4) C(5) C(6) 123(1) . . . yes C(4) C(5) H(7) 113.1 . . . no C(6) C(5) H(7) 113.3 . . . no Rh(1) C(6) C(5) 69.1(9) . . . yes Rh(1) C(6) C(7) 111(1) . . . yes Rh(1) C(6) H(8) 114.4 . . . no C(5) C(6) C(7) 125(1) . . . yes C(5) C(6) H(8) 114.3 . . . no C(7) C(6) H(8) 114.5 . . . no C(6) C(7) C(8) 113(1) . . . yes C(6) C(7) H(9) 108.6 . . . no C(6) C(7) H(10) 108.6 . . . no C(8) C(7) H(9) 108.6 . . . no C(8) C(7) H(10) 108.6 . . . no H(9) C(7) H(10) 109.4 . . . no C(1) C(8) C(7) 112(1) . . . yes C(1) C(8) H(11) 108.9 . . . no C(1) C(8) H(12) 108.9 . . . no C(7) C(8) H(11) 108.9 . . . no C(7) C(8) H(12) 108.9 . . . no H(11) C(8) H(12) 109.5 . . . no Se(1) C(9) H(13) 109.4 . . . no Se(1) C(9) H(14) 109.4 . . . no Se(1) C(9) H(15) 109.4 . . . no H(13) C(9) H(14) 109.6 . . . no H(13) C(9) H(15) 109.5 . . . no H(14) C(9) H(15) 109.5 . . . no Se(2) C(10) H(16) 109.6 . . . no Se(2) C(10) H(17) 109.5 . . . no Se(2) C(10) H(18) 109.5 . . . no H(16) C(10) H(17) 109.5 . . . no H(16) C(10) H(18) 109.4 . . . no H(17) C(10) H(18) 109.3 . . . no Se(3) C(11) H(19) 109.4 . . . no Se(3) C(11) H(20) 109.5 . . . no Se(3) C(11) H(21) 109.5 . . . no H(19) C(11) H(20) 109.4 . . . no H(19) C(11) H(21) 109.4 . . . no H(20) C(11) H(21) 109.5 . . . no C(13) C(12) H(22) 109.6 . . . no C(13) C(12) H(23) 109.6 . . . no C(13) C(12) H(24) 109.5 . . . no H(22) C(12) H(23) 109.4 . . . no H(22) C(12) H(24) 109.4 . . . no H(23) C(12) H(24) 109.4 . . . no C(12) C(13) C(14) 106(1) . . . yes C(12) C(13) C(15) 103(1) . . . yes C(12) C(13) C(16) 106(1) . . . yes C(14) C(13) C(15) 115(1) . . . yes C(14) C(13) C(16) 113(1) . . . yes C(15) C(13) C(16) 113(1) . . . yes Se(1) C(14) C(13) 121(1) . . . yes Se(1) C(14) H(25) 106.5 . . . no Se(1) C(14) H(26) 106.5 . . . no C(13) C(14) H(25) 106.6 . . . no C(13) C(14) H(26) 106.5 . . . no H(25) C(14) H(26) 109.5 . . . no Se(2) C(15) C(13) 118(1) . . . yes Se(2) C(15) H(27) 107.2 . . . no Se(2) C(15) H(28) 107.3 . . . no C(13) C(15) H(27) 107.3 . . . no C(13) C(15) H(28) 107.3 . . . no H(27) C(15) H(28) 109.4 . . . no Se(3) C(16) C(13) 121(1) . . . yes Se(3) C(16) H(29) 106.4 . . . no Se(3) C(16) H(30) 106.4 . . . no C(13) C(16) H(29) 106.4 . . . no C(13) C(16) H(30) 106.4 . . . no H(29) C(16) H(30) 109.4 . . . 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 F(1) C(11) 3.39(2) . 2_545 no F(1) C(8) 3.52(2) . . no F(1) C(11) 3.52(2) . 4 no F(1) C(4) 3.57(2) . 2 no F(2) C(10) 3.27(2) . 1_556 no F(2) C(9) 3.38(2) . 4_455 no F(2) C(16) 3.51(2) . 1_556 no F(3) C(11) 3.53(2) . 2_545 no F(4) C(7) 3.22(2) . 4 no F(4) C(6) 3.47(2) . 4 no F(5) C(10) 3.44(2) . 2 no F(5) C(3) 3.49(2) . 2 no F(6) C(16) 3.38(2) . 2_545 no F(6) C(14) 3.49(2) . 2_545 no F(6) C(12) 3.50(2) . 2_545 no C(5) C(5) 3.43(3) . 3 no C(5) C(6) 3.50(2) . 3 no C(7) C(12) 3.49(2) . 4_455 no #------------------------------------------------------------------------------