# om960769d.cif data_OM960769D_compound_3_Cp*2Ir2(SH)2Cl2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Aug 15 16:04:59 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution DIRDIF92 (PATTY) _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 8.5190(6) _cell_length_b 9.2733(7) _cell_length_c 15.6790(7) _cell_angle_alpha 90 _cell_angle_beta 104.060(5) _cell_angle_gamma 90 _cell_volume 1201.5(1) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 38.92 _cell_measurement_theta_max 39.89 #------------------------------------------------------------------------------ _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 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_measured ? _exptl_crystal_F000 744.00 _exptl_absorpt_coefficient_mu_cm 114.940 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.488 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _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 ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3123 _diffrn_reflns_av_R_equivalents 4.08 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 11 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 12 _diffrn_reflns_l_min -19 _diffrn_reflns_l_max 17 _diffrn_theta_min ? _diffrn_theta_max 27.4956 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 0.07459 _diffrn_orient_matrix_12 -0.08361 _diffrn_orient_matrix_13 0.01863 _diffrn_orient_matrix_21 -0.07945 _diffrn_orient_matrix_22 -0.04415 _diffrn_orient_matrix_23 0.02992 _diffrn_orient_matrix_31 -0.05261 _diffrn_orient_matrix_32 -0.05186 _diffrn_orient_matrix_33 -0.05551 #------------------------------------------------------------------------------ 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 40 0.003 0.002 'International Tables' H 0 64 0.000 0.000 'International Tables' Ir 0 4 -1.444 7.990 'International Tables' S 0 4 0.125 0.123 'International Tables' Cl 0 4 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ir1 0.09063(4) 0.04275(4) -0.09127(2) 0.0344 Uij ? ? Cl1 0.1243(4) -0.2125(3) -0.1058(2) 0.0787 Uij ? ? S1 0.1667(2) 0.0118(3) 0.0643(1) 0.0495 Uij ? ? C1 0.086(1) 0.116(1) -0.2226(6) 0.0549 Uij ? ? C2 0.009(1) 0.217(1) -0.1816(8) 0.0703 Uij ? ? C3 0.131(2) 0.2639(9) -0.1052(7) 0.0667 Uij ? ? C4 0.278(1) 0.1957(10) -0.1035(6) 0.0471 Uij ? ? C5 0.247(1) 0.1055(9) -0.1780(6) 0.0486 Uij ? ? C6 0.008(2) 0.044(2) -0.3076(7) 0.1387 Uij ? ? C7 -0.158(1) 0.278(2) -0.207(1) 0.2135 Uij ? ? C8 0.119(2) 0.384(1) -0.0386(9) 0.1571 Uij ? ? C9 0.438(1) 0.217(1) -0.0410(7) 0.1102 Uij ? ? C10 0.374(1) 0.007(1) -0.2014(7) 0.1068 Uij ? ? H1 0.2288 -0.1151 0.0873 0.0590 Uij ? ? H2 0.0827 -0.0178 -0.3241 0.1312 Uij ? ? H3 -0.0835 -0.0085 -0.3004 0.1312 Uij ? ? H4 -0.0265 0.1166 -0.3513 0.1312 Uij ? ? H5 -0.2173 0.2325 -0.2574 0.2274 Uij ? ? H6 -0.2092 0.2609 -0.1589 0.2274 Uij ? ? H7 -0.1530 0.3789 -0.2151 0.2274 Uij ? ? H8 0.0136 0.4200 -0.0501 0.1591 Uij ? ? H9 0.1930 0.4598 -0.0437 0.1591 Uij ? ? H10 0.1506 0.3455 0.0194 0.1591 Uij ? ? H11 0.4259 0.2866 0.0011 0.1167 Uij ? ? H12 0.5110 0.2516 -0.0734 0.1167 Uij ? ? H13 0.4731 0.1288 -0.0142 0.1167 Uij ? ? H14 0.4602 0.0630 -0.2116 0.1281 Uij ? ? H15 0.4117 -0.0594 -0.1556 0.1053 Uij ? ? H16 0.3245 -0.0448 -0.2543 0.1053 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir1 0.0457(2) 0.0291(2) 0.0341(2) 0.0039(2) 0.0205(1) 0.0050(2) Cl1 0.128(3) 0.030(1) 0.101(2) 0.010(2) 0.071(2) 0.002(2) S1 0.041(1) 0.068(2) 0.040(1) -0.002(1) 0.0107(10) 0.020(1) C1 0.066(7) 0.057(7) 0.039(6) -0.018(6) 0.009(5) 0.013(5) C2 0.053(7) 0.077(9) 0.088(8) 0.016(6) 0.031(6) 0.059(7) C3 0.12(1) 0.018(5) 0.085(8) 0.008(6) 0.076(8) 0.005(5) C4 0.071(7) 0.032(5) 0.042(5) -0.011(5) 0.021(5) 0.004(4) C5 0.071(6) 0.038(6) 0.051(6) -0.004(5) 0.041(5) 0.014(5) C6 0.19(1) 0.18(2) 0.041(6) -0.08(1) 0.024(8) 0.026(9) C7 0.069(9) 0.24(2) 0.36(2) 0.09(1) 0.10(1) 0.26(2) C8 0.33(2) 0.035(7) 0.18(1) -0.01(1) 0.21(1) -0.019(9) C9 0.11(1) 0.10(1) 0.10(1) -0.054(8) -0.004(8) 0.028(8) C10 0.121(9) 0.12(1) 0.116(9) 0.029(8) 0.096(8) 0.013(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 7.55024 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2043 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0330 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0240 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.180 _refine_ls_shift/esd_max 0.0300 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.33770 _refine_diff_density_max -1.07560 #------------------------------------------------------------------------------ _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 Ir(1) Cl(1) 2.401(3) ? ? yes Ir(1) S(1) 2.385(2) ? ? yes Ir(1) S(1) 2.385(2) ? ? yes Ir(1) C(1) 2.159(8) ? ? yes Ir(1) C(2) 2.153(9) ? ? yes Ir(1) C(3) 2.099(9) ? ? yes Ir(1) C(4) 2.179(8) ? ? yes Ir(1) C(5) 2.201(7) ? ? yes C(1) C(2) 1.39(1) ? ? yes C(1) C(5) 1.38(1) ? ? yes C(1) C(6) 1.49(1) ? ? yes C(2) C(3) 1.44(1) ? ? yes C(2) C(7) 1.49(1) ? ? yes C(3) C(4) 1.40(1) ? ? yes C(3) C(8) 1.54(1) ? ? yes C(4) C(5) 1.41(1) ? ? yes C(4) C(9) 1.49(1) ? ? yes C(5) C(10) 1.53(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_bond_publ_flag Cl(1) Ir(1) S(1) 88.25(10) ? ? ? yes Cl(1) Ir(1) S(1) 86.79(9) ? ? ? yes Cl(1) Ir(1) C(1) 101.1(3) ? ? ? yes Cl(1) Ir(1) C(2) 134.9(4) ? ? ? yes Cl(1) Ir(1) C(3) 158.0(2) ? ? ? yes Cl(1) Ir(1) C(4) 121.7(3) ? ? ? yes Cl(1) Ir(1) C(5) 95.6(2) ? ? ? yes S(1) Ir(1) S(1) 80.00(7) ? ? ? yes S(1) Ir(1) C(1) 161.9(3) ? ? ? yes S(1) Ir(1) C(2) 136.7(4) ? ? ? yes S(1) Ir(1) C(3) 102.3(3) ? ? ? yes S(1) Ir(1) C(4) 98.4(2) ? ? ? yes S(1) Ir(1) C(5) 127.5(3) ? ? ? yes S(1) Ir(1) C(1) 115.6(3) ? ? ? yes S(1) Ir(1) C(2) 96.5(2) ? ? ? yes S(1) Ir(1) C(3) 113.9(3) ? ? ? yes S(1) Ir(1) C(4) 151.4(3) ? ? ? yes S(1) Ir(1) C(5) 152.4(3) ? ? ? yes C(1) Ir(1) C(2) 37.6(4) ? ? ? yes C(1) Ir(1) C(3) 63.9(4) ? ? ? yes C(1) Ir(1) C(4) 63.6(3) ? ? ? yes C(1) Ir(1) C(5) 36.9(3) ? ? ? yes C(2) Ir(1) C(3) 39.7(4) ? ? ? yes C(2) Ir(1) C(4) 65.0(4) ? ? ? yes C(2) Ir(1) C(5) 62.6(3) ? ? ? yes C(3) Ir(1) C(4) 38.2(3) ? ? ? yes C(3) Ir(1) C(5) 62.6(3) ? ? ? yes C(4) Ir(1) C(5) 37.5(3) ? ? ? yes Ir(1) S(1) Ir(1) 100.00(7) ? ? ? yes Ir(1) C(1) C(2) 70.9(5) ? ? ? yes Ir(1) C(1) C(5) 73.2(5) ? ? ? yes Ir(1) C(1) C(6) 127.7(7) ? ? ? yes C(2) C(1) C(5) 109.5(9) ? ? ? yes C(2) C(1) C(6) 123(1) ? ? ? yes C(5) C(1) C(6) 126(1) ? ? ? yes Ir(1) C(2) C(1) 71.4(6) ? ? ? yes Ir(1) C(2) C(3) 68.2(5) ? ? ? yes Ir(1) C(2) C(7) 126.1(7) ? ? ? yes C(1) C(2) C(3) 105.3(8) ? ? ? yes C(1) C(2) C(7) 131(1) ? ? ? yes C(3) C(2) C(7) 123(1) ? ? ? yes Ir(1) C(3) C(2) 72.1(6) ? ? ? yes Ir(1) C(3) C(4) 74.0(5) ? ? ? yes Ir(1) C(3) C(8) 126.5(7) ? ? ? yes C(2) C(3) C(4) 109.8(8) ? ? ? yes C(2) C(3) C(8) 128(1) ? ? ? yes C(4) C(3) C(8) 120(1) ? ? ? yes Ir(1) C(4) C(3) 67.8(5) ? ? ? yes Ir(1) C(4) C(5) 72.1(5) ? ? ? yes Ir(1) C(4) C(9) 127.1(7) ? ? ? yes C(3) C(4) C(5) 105.4(9) ? ? ? yes C(3) C(4) C(9) 128(1) ? ? ? yes C(5) C(4) C(9) 125.6(10) ? ? ? yes Ir(1) C(5) C(1) 69.9(5) ? ? ? yes Ir(1) C(5) C(4) 70.4(4) ? ? ? yes Ir(1) C(5) C(10) 124.0(6) ? ? ? yes C(1) C(5) C(4) 110.0(8) ? ? ? yes C(1) C(5) C(10) 126.3(10) ? ? ? yes C(4) C(5) C(10) 123.6(9) ? ? ? yes #------------------------------------------------------------------------------ data_OM960769D_compound_4_Cp*2Rh2(SH)2Cl2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Aug 15 16:17:12 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution DIRDIF92 (PATTY) _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 8.8238(9) _cell_length_b 15.946(2) _cell_length_c 8.693(1) _cell_angle_alpha 103.753(9) _cell_angle_beta 94.079(9) _cell_angle_gamma 92.000(9) _cell_volume 1183.3(2) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 38.54 _cell_measurement_theta_max 39.84 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_measured ? _exptl_crystal_F000 616.00 _exptl_absorpt_coefficient_mu_cm 17.965 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.594 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_\% -0.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5812 _diffrn_reflns_av_R_equivalents 2.08 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 11 _diffrn_reflns_k_min -1 _diffrn_reflns_k_max 15 _diffrn_reflns_l_min -6 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 27.5014 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 0.05329 _diffrn_orient_matrix_12 -0.05435 _diffrn_orient_matrix_13 -0.00025 _diffrn_orient_matrix_21 -0.09802 _diffrn_orient_matrix_22 -0.02915 _diffrn_orient_matrix_23 0.01540 _diffrn_orient_matrix_31 -0.02231 _diffrn_orient_matrix_32 -0.01941 _diffrn_orient_matrix_33 -0.11783 #------------------------------------------------------------------------------ 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 40 0.003 0.002 'International Tables' H 0 64 0.000 0.000 'International Tables' Cl 0 4 0.148 0.159 'International Tables' Rh 0 4 -1.118 0.919 'International Tables' S 0 4 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh1 0.04628(7) -0.08507(4) 0.09904(7) 0.0267 Uij ? ? Rh2 0.54776(7) 0.58343(4) 0.40037(8) 0.0304 Uij ? ? Cl1 -0.2220(2) -0.1182(2) 0.0973(3) 0.0523 Uij ? ? Cl2 0.2893(3) 0.5701(2) 0.2844(3) 0.0659 Uij ? ? S1 -0.0012(2) 0.0662(1) 0.1659(2) 0.0368 Uij ? ? S2 0.4524(3) 0.5708(1) 0.6452(3) 0.0457 Uij ? ? C1 0.1978(8) -0.0886(5) 0.3072(9) 0.0309 Uij ? ? C2 0.2815(8) -0.0805(6) 0.175(1) 0.0354 Uij ? ? C3 0.2506(9) -0.1549(6) 0.0559(9) 0.0362 Uij ? ? C4 0.1442(10) -0.2074(6) 0.099(1) 0.0460 Uij ? ? C5 0.1082(8) -0.1657(5) 0.2638(10) 0.0350 Uij ? ? C6 0.2101(9) -0.0269(6) 0.465(1) 0.0541 Uij ? ? C7 0.3996(9) -0.0110(7) 0.179(1) 0.0583 Uij ? ? C8 0.326(1) -0.1772(7) -0.101(1) 0.0730 Uij ? ? C9 0.073(1) -0.2959(6) 0.011(1) 0.0709 Uij ? ? C10 0.0067(10) -0.2033(7) 0.362(1) 0.0600 Uij ? ? C11 0.6053(10) 0.7106(6) 0.365(1) 0.0547 Uij ? ? C12 0.6887(9) 0.6990(6) 0.504(1) 0.0412 Uij ? ? C13 0.7786(9) 0.6297(6) 0.456(1) 0.0357 Uij ? ? C14 0.7569(9) 0.5988(6) 0.293(1) 0.0429 Uij ? ? C15 0.6460(10) 0.6464(6) 0.230(1) 0.0447 Uij ? ? C16 0.487(1) 0.7782(7) 0.353(2) 0.1058 Uij ? ? C17 0.684(1) 0.7556(7) 0.667(1) 0.0751 Uij ? ? C18 0.899(1) 0.6040(7) 0.562(1) 0.0663 Uij ? ? C19 0.840(1) 0.5282(7) 0.191(1) 0.0752 Uij ? ? C20 0.583(1) 0.6361(8) 0.060(1) 0.0844 Uij ? ? H1 -0.1337 0.0400 0.1677 0.0543 Uij ? ? H2 0.1126 -0.0052 0.4882 0.0603 Uij ? ? H3 0.2788 0.0208 0.4644 0.0603 Uij ? ? H4 0.2461 -0.0543 0.5447 0.0603 Uij ? ? H5 0.3989 0.0339 0.2726 0.0620 Uij ? ? H6 0.4988 -0.0336 0.1739 0.0620 Uij ? ? H7 0.3813 0.0137 0.0885 0.0620 Uij ? ? H8 0.4341 -0.1782 -0.0808 0.0794 Uij ? ? H9 0.2880 -0.2314 -0.1642 0.0794 Uij ? ? H10 0.3068 -0.1337 -0.1591 0.0794 Uij ? ? H11 0.1079 -0.3121 -0.0921 0.0800 Uij ? ? H12 -0.0362 -0.2926 0.0000 0.0800 Uij ? ? H13 0.0968 -0.3376 0.0684 0.0800 Uij ? ? H14 -0.0398 -0.2563 0.3030 0.0663 Uij ? ? H15 -0.0702 -0.1637 0.3976 0.0663 Uij ? ? H16 0.0644 -0.2121 0.4539 0.0663 Uij ? ? H17 0.3124 0.5767 0.6393 0.0982 Uij ? ? H18 0.3928 0.7503 0.3110 0.1121 Uij ? ? H19 0.5213 0.8131 0.2848 0.1121 Uij ? ? H20 0.4788 0.8147 0.4556 0.1121 Uij ? ? H21 0.6135 0.7988 0.6662 0.0796 Uij ? ? H22 0.6564 0.7217 0.7382 0.0796 Uij ? ? H23 0.7832 0.7831 0.7040 0.0796 Uij ? ? H24 0.8559 0.5897 0.6502 0.0719 Uij ? ? H25 0.9743 0.6502 0.6000 0.0719 Uij ? ? H26 0.9475 0.5547 0.5047 0.0719 Uij ? ? H27 0.9092 0.5053 0.2588 0.0784 Uij ? ? H28 0.8961 0.5515 0.1205 0.0784 Uij ? ? H29 0.7699 0.4841 0.1342 0.0784 Uij ? ? H30 0.6301 0.5888 -0.0074 0.0889 Uij ? ? H31 0.6082 0.6874 0.0260 0.0889 Uij ? ? H32 0.4777 0.6252 0.0500 0.0966 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.0309(4) 0.0264(5) 0.0265(4) 0.0062(3) 0.0042(3) 0.0121(3) Rh2 0.0378(4) 0.0256(5) 0.0299(4) 0.0004(3) -0.0003(3) 0.0120(4) Cl1 0.036(1) 0.060(2) 0.070(2) 0.000(1) 0.006(1) 0.033(1) Cl2 0.045(1) 0.081(2) 0.081(2) -0.010(1) -0.014(1) 0.045(2) S1 0.055(1) 0.031(1) 0.027(1) 0.014(1) 0.0029(10) 0.010(1) S2 0.078(2) 0.025(1) 0.035(1) -0.001(1) 0.017(1) 0.004(1) C1 0.028(4) 0.034(5) 0.033(5) 0.010(4) -0.005(3) 0.013(4) C2 0.027(4) 0.036(6) 0.050(6) 0.005(4) 0.008(4) 0.022(5) C3 0.038(5) 0.049(6) 0.031(5) 0.016(4) 0.007(4) 0.025(5) C4 0.055(6) 0.033(6) 0.048(6) 0.031(5) -0.010(5) 0.007(5) C5 0.035(5) 0.038(6) 0.038(5) 0.007(4) -0.008(4) 0.026(4) C6 0.064(6) 0.060(7) 0.038(6) 0.015(5) -0.006(5) 0.013(5) C7 0.037(5) 0.077(8) 0.071(7) 0.010(5) -0.001(5) 0.040(6) C8 0.075(7) 0.095(10) 0.054(7) 0.047(7) 0.023(6) 0.015(7) C9 0.114(9) 0.035(7) 0.056(7) 0.019(6) -0.028(6) 0.004(6) C10 0.060(6) 0.069(8) 0.066(7) -0.003(5) 0.010(5) 0.046(6) C11 0.042(5) 0.027(6) 0.107(9) -0.006(4) 0.021(6) 0.037(6) C12 0.037(5) 0.040(6) 0.048(6) -0.004(4) 0.003(4) 0.014(5) C13 0.038(5) 0.034(6) 0.041(6) 0.004(4) 0.004(4) 0.021(5) C14 0.040(5) 0.035(6) 0.056(6) 0.001(4) 0.010(4) 0.014(5) C15 0.052(6) 0.048(6) 0.037(6) -0.018(5) 0.004(4) 0.019(5) C16 0.063(7) 0.057(8) 0.22(2) 0.026(6) 0.020(8) 0.083(10) C17 0.090(8) 0.051(7) 0.070(8) -0.033(6) 0.015(6) -0.012(6) C18 0.060(7) 0.063(8) 0.083(8) -0.001(6) -0.003(6) 0.036(7) C19 0.082(8) 0.050(8) 0.094(9) 0.009(6) 0.037(7) 0.010(7) C20 0.114(9) 0.10(1) 0.051(7) -0.031(8) -0.017(6) 0.050(7) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 5.07622 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3570 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0380 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.660 _refine_ls_shift/esd_max 0.0350 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.33540 _refine_diff_density_max -1.49040 #------------------------------------------------------------------------------ _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 Rh(1) Cl(1) 2.405(2) ? ? yes Rh(1) S(1) 2.403(2) ? ? yes Rh(1) S(1) 2.400(2) ? ? yes Rh(1) C(1) 2.185(7) ? ? yes Rh(1) C(2) 2.126(8) ? ? yes Rh(1) C(3) 2.161(8) ? ? yes Rh(1) C(4) 2.161(8) ? ? yes Rh(1) C(5) 2.194(7) ? ? yes Rh(2) Cl(2) 2.409(2) ? ? yes Rh(2) S(2) 2.393(2) ? ? yes Rh(2) S(2) 2.397(2) ? ? yes Rh(2) C(11) 2.171(8) ? ? yes Rh(2) C(12) 2.155(9) ? ? yes Rh(2) C(13) 2.124(8) ? ? yes Rh(2) C(14) 2.161(8) ? ? yes Rh(2) C(15) 2.187(8) ? ? yes C(1) C(2) 1.439(10) ? ? yes C(1) C(5) 1.40(1) ? ? yes C(1) C(6) 1.48(1) ? ? yes C(2) C(3) 1.38(1) ? ? yes C(2) C(7) 1.49(1) ? ? yes C(3) C(4) 1.37(1) ? ? yes C(3) C(8) 1.53(1) ? ? yes C(4) C(5) 1.49(1) ? ? yes C(4) C(9) 1.53(1) ? ? yes C(5) C(10) 1.49(1) ? ? yes C(11) C(12) 1.42(1) ? ? yes C(11) C(15) 1.44(1) ? ? yes C(11) C(16) 1.54(1) ? ? yes C(12) C(13) 1.38(1) ? ? yes C(12) C(17) 1.50(1) ? ? yes C(13) C(14) 1.39(1) ? ? yes C(13) C(18) 1.49(1) ? ? yes C(14) C(15) 1.41(1) ? ? yes C(14) C(19) 1.51(1) ? ? yes C(15) C(20) 1.51(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_bond_publ_flag Cl(1) Rh(1) S(1) 89.22(8) ? ? ? yes Cl(1) Rh(1) S(1) 88.43(8) ? ? ? yes Cl(1) Rh(1) C(1) 119.8(2) ? ? ? yes Cl(1) Rh(1) C(2) 157.4(2) ? ? ? yes Cl(1) Rh(1) C(3) 137.7(3) ? ? ? yes Cl(1) Rh(1) C(4) 102.9(3) ? ? ? yes Cl(1) Rh(1) C(5) 93.4(2) ? ? ? yes S(1) Rh(1) S(1) 81.85(8) ? ? ? yes S(1) Rh(1) C(1) 98.6(2) ? ? ? yes S(1) Rh(1) C(2) 100.6(2) ? ? ? yes S(1) Rh(1) C(3) 133.1(3) ? ? ? yes S(1) Rh(1) C(4) 161.9(2) ? ? ? yes S(1) Rh(1) C(5) 127.2(2) ? ? ? yes S(1) Rh(1) C(1) 151.8(2) ? ? ? yes S(1) Rh(1) C(2) 112.9(2) ? ? ? yes S(1) Rh(1) C(3) 95.8(2) ? ? ? yes S(1) Rh(1) C(4) 111.4(2) ? ? ? yes S(1) Rh(1) C(5) 150.9(2) ? ? ? yes C(1) Rh(1) C(2) 39.0(3) ? ? ? yes C(1) Rh(1) C(3) 63.2(3) ? ? ? yes C(1) Rh(1) C(4) 63.8(3) ? ? ? yes C(1) Rh(1) C(5) 37.2(3) ? ? ? yes C(2) Rh(1) C(3) 37.6(3) ? ? ? yes C(2) Rh(1) C(4) 63.4(3) ? ? ? yes C(2) Rh(1) C(5) 64.4(3) ? ? ? yes C(3) Rh(1) C(4) 36.9(3) ? ? ? yes C(3) Rh(1) C(5) 64.0(3) ? ? ? yes C(4) Rh(1) C(5) 40.0(3) ? ? ? yes Cl(2) Rh(2) S(2) 88.62(9) ? ? ? yes Cl(2) Rh(2) S(2) 89.46(9) ? ? ? yes Cl(2) Rh(2) C(11) 97.2(3) ? ? ? yes Cl(2) Rh(2) C(12) 128.8(2) ? ? ? yes Cl(2) Rh(2) C(13) 159.5(2) ? ? ? yes Cl(2) Rh(2) C(14) 129.2(3) ? ? ? yes Cl(2) Rh(2) C(15) 96.8(2) ? ? ? yes S(2) Rh(2) S(2) 82.16(8) ? ? ? yes S(2) Rh(2) C(11) 119.6(3) ? ? ? yes S(2) Rh(2) C(12) 95.2(2) ? ? ? yes S(2) Rh(2) C(13) 106.3(2) ? ? ? yes S(2) Rh(2) C(14) 142.1(3) ? ? ? yes S(2) Rh(2) C(15) 157.9(3) ? ? ? yes S(2) Rh(2) C(11) 157.3(3) ? ? ? yes S(2) Rh(2) C(12) 141.7(2) ? ? ? yes S(2) Rh(2) C(13) 106.2(2) ? ? ? yes S(2) Rh(2) C(14) 96.1(2) ? ? ? yes S(2) Rh(2) C(15) 119.2(3) ? ? ? yes C(11) Rh(2) C(12) 38.3(3) ? ? ? yes C(11) Rh(2) C(13) 63.3(3) ? ? ? yes C(11) Rh(2) C(14) 63.0(3) ? ? ? yes C(11) Rh(2) C(15) 38.5(3) ? ? ? yes C(12) Rh(2) C(13) 37.7(3) ? ? ? yes C(12) Rh(2) C(14) 63.2(3) ? ? ? yes C(12) Rh(2) C(15) 64.7(3) ? ? ? yes C(13) Rh(2) C(14) 37.8(3) ? ? ? yes C(13) Rh(2) C(15) 64.2(3) ? ? ? yes C(14) Rh(2) C(15) 38.0(3) ? ? ? yes Rh(1) S(1) Rh(1) 98.15(8) ? ? ? yes Rh(2) S(2) Rh(2) 97.84(8) ? ? ? yes Rh(1) C(1) C(2) 68.3(4) ? ? ? yes Rh(1) C(1) C(5) 71.8(4) ? ? ? yes Rh(1) C(1) C(6) 127.6(6) ? ? ? yes C(2) C(1) C(5) 108.7(7) ? ? ? yes C(2) C(1) C(6) 125.3(8) ? ? ? yes C(5) C(1) C(6) 125.9(8) ? ? ? yes Rh(1) C(2) C(1) 72.7(4) ? ? ? yes Rh(1) C(2) C(3) 72.6(5) ? ? ? yes Rh(1) C(2) C(7) 128.3(6) ? ? ? yes C(1) C(2) C(3) 107.8(7) ? ? ? yes C(1) C(2) C(7) 124.9(8) ? ? ? yes C(3) C(2) C(7) 126.5(8) ? ? ? yes Rh(1) C(3) C(2) 69.8(5) ? ? ? yes Rh(1) C(3) C(4) 71.6(5) ? ? ? yes Rh(1) C(3) C(8) 126.1(6) ? ? ? yes C(2) C(3) C(4) 110.2(7) ? ? ? yes C(2) C(3) C(8) 125.4(8) ? ? ? yes C(4) C(3) C(8) 124.3(9) ? ? ? yes Rh(1) C(4) C(3) 71.6(5) ? ? ? yes Rh(1) C(4) C(5) 71.2(4) ? ? ? yes Rh(1) C(4) C(9) 125.1(6) ? ? ? yes C(3) C(4) C(5) 107.8(8) ? ? ? yes C(3) C(4) C(9) 130.6(9) ? ? ? yes C(5) C(4) C(9) 121.5(9) ? ? ? yes Rh(1) C(5) C(1) 71.1(4) ? ? ? yes Rh(1) C(5) C(4) 68.8(4) ? ? ? yes Rh(1) C(5) C(10) 127.8(6) ? ? ? yes C(1) C(5) C(4) 105.4(7) ? ? ? yes C(1) C(5) C(10) 128.4(8) ? ? ? yes C(4) C(5) C(10) 126.0(8) ? ? ? yes Rh(2) C(11) C(12) 70.2(5) ? ? ? yes Rh(2) C(11) C(15) 71.3(5) ? ? ? yes Rh(2) C(11) C(16) 123.5(6) ? ? ? yes C(12) C(11) C(15) 108.8(8) ? ? ? yes C(12) C(11) C(16) 127(1) ? ? ? yes C(15) C(11) C(16) 123(1) ? ? ? yes Rh(2) C(12) C(11) 71.4(5) ? ? ? yes Rh(2) C(12) C(13) 70.0(5) ? ? ? yes Rh(2) C(12) C(17) 126.5(6) ? ? ? yes C(11) C(12) C(13) 107.1(8) ? ? ? yes C(11) C(12) C(17) 125.3(9) ? ? ? yes C(13) C(12) C(17) 127.5(9) ? ? ? yes Rh(2) C(13) C(12) 72.3(5) ? ? ? yes Rh(2) C(13) C(14) 72.5(5) ? ? ? yes Rh(2) C(13) C(18) 129.8(6) ? ? ? yes C(12) C(13) C(14) 109.4(8) ? ? ? yes C(12) C(13) C(18) 124.0(9) ? ? ? yes C(14) C(13) C(18) 125.8(9) ? ? ? yes Rh(2) C(14) C(13) 69.7(5) ? ? ? yes Rh(2) C(14) C(15) 72.0(5) ? ? ? yes Rh(2) C(14) C(19) 126.7(6) ? ? ? yes C(13) C(14) C(15) 109.7(8) ? ? ? yes C(13) C(14) C(19) 126.8(9) ? ? ? yes C(15) C(14) C(19) 123.4(9) ? ? ? yes Rh(2) C(15) C(11) 70.1(5) ? ? ? yes Rh(2) C(15) C(14) 70.0(5) ? ? ? yes Rh(2) C(15) C(20) 125.0(6) ? ? ? yes C(11) C(15) C(14) 104.9(8) ? ? ? yes C(11) C(15) C(20) 125.8(10) ? ? ? yes C(14) C(15) C(20) 129.2(10) ? ? ? yes #------------------------------------------------------------------------------ data_OM960769D_compound_9_Cp*2Ir2S2Rh2Cl2(cod)2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Aug 15 16:01:04 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution ? _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 10.737(3) _cell_length_b 11.115(3) _cell_length_c 32.890(4) _cell_angle_alpha 89 _cell_angle_beta 90.19(2) _cell_angle_gamma 89 _cell_volume 3924(2) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 32.51 _cell_measurement_theta_max 37.28 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_measured ? _exptl_crystal_F000 2320.00 _exptl_absorpt_coefficient_mu_cm 78.690 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.739 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_\% -1.96 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7433 _diffrn_reflns_av_R_equivalents 2.13 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min -12 _diffrn_reflns_h_max 12 _diffrn_reflns_k_min -13 _diffrn_reflns_k_max 0 _diffrn_reflns_l_min 0 _diffrn_reflns_l_max 28 _diffrn_theta_min ? _diffrn_theta_max 24.9924 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.08035 _diffrn_orient_matrix_12 0.03729 _diffrn_orient_matrix_13 -0.00890 _diffrn_orient_matrix_21 0.03740 _diffrn_orient_matrix_22 0.08185 _diffrn_orient_matrix_23 0.00325 _diffrn_orient_matrix_31 0.02865 _diffrn_orient_matrix_32 -0.00228 _diffrn_orient_matrix_33 -0.02889 #------------------------------------------------------------------------------ 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 0 144 0.003 0.002 'International Tables' H 0 216 0.000 0.000 'International Tables' Rh 0 8 -1.118 0.919 'International Tables' Ir 0 8 -1.444 7.990 'International Tables' S 0 8 0.125 0.123 'International Tables' Cl 0 8 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ir1 0.17757(4) 0.45943(4) 0.40034(1) 0.0369 Uij ? ? Ir2 0.00898(3) 0.27466(4) 0.37454(1) 0.0351 Uij ? ? Rh1 0.20709(7) 0.21705(7) 0.43205(2) 0.0360 Uij ? ? Rh2 0.62892(8) 0.84808(8) 0.31610(3) 0.0482 Uij ? ? Cl1 0.7895(3) 0.7239(4) 0.2910(1) 0.1062 Uij ? ? Cl2 0.6542(3) 0.7641(3) 0.38196(9) 0.0874 Uij ? ? S1 0.2206(2) 0.2853(2) 0.36619(7) 0.0372 Uij ? ? S2 0.0434(2) 0.3480(2) 0.43868(7) 0.0404 Uij ? ? C1 0.222(1) 0.6151(9) 0.4360(3) 0.0624 Uij ? ? C2 0.328(1) 0.5801(9) 0.4136(4) 0.0543 Uij ? ? C3 0.3042(10) 0.5876(9) 0.3725(3) 0.0442 Uij ? ? C4 0.179(1) 0.6303(10) 0.3680(4) 0.0669 Uij ? ? C5 0.130(1) 0.645(1) 0.4062(4) 0.0634 Uij ? ? C6 0.214(2) 0.623(1) 0.4819(4) 0.1215 Uij ? ? C7 0.453(1) 0.542(1) 0.4318(4) 0.0849 Uij ? ? C8 0.394(1) 0.5618(10) 0.3384(3) 0.0646 Uij ? ? C9 0.113(1) 0.654(1) 0.3279(4) 0.0967 Uij ? ? C10 0.003(1) 0.694(1) 0.4172(6) 0.1286 Uij ? ? C11 -0.0937(9) 0.286(1) 0.3172(3) 0.0558 Uij ? ? C12 -0.1708(10) 0.320(1) 0.3499(4) 0.0606 Uij ? ? C13 -0.1850(10) 0.220(1) 0.3763(3) 0.0618 Uij ? ? C14 -0.110(1) 0.126(1) 0.3608(4) 0.0662 Uij ? ? C15 -0.0565(10) 0.165(1) 0.3239(4) 0.0566 Uij ? ? C16 -0.059(1) 0.362(1) 0.2813(4) 0.0961 Uij ? ? C17 -0.242(1) 0.437(1) 0.3554(5) 0.1169 Uij ? ? C18 -0.264(1) 0.212(2) 0.4139(4) 0.1395 Uij ? ? C19 -0.096(2) 0.001(1) 0.3769(5) 0.1279 Uij ? ? C20 0.023(1) 0.091(1) 0.2953(4) 0.1137 Uij ? ? C21 0.3945(9) 0.151(1) 0.4313(3) 0.0573 Uij ? ? C22 0.320(1) 0.061(1) 0.4203(3) 0.0560 Uij ? ? C23 0.281(1) -0.046(1) 0.4446(5) 0.0916 Uij ? ? C24 0.183(2) -0.020(1) 0.4758(5) 0.1207 Uij ? ? C25 0.152(1) 0.108(1) 0.4837(4) 0.0685 Uij ? ? C26 0.235(1) 0.196(1) 0.4969(3) 0.0683 Uij ? ? C27 0.366(1) 0.172(2) 0.5069(4) 0.1234 Uij ? ? C28 0.451(1) 0.167(1) 0.4736(4) 0.0891 Uij ? ? C29 0.530(1) 0.996(1) 0.3388(4) 0.0691 Uij ? ? C30 0.449(1) 0.904(1) 0.3311(4) 0.0757 Uij ? ? C31 0.362(1) 0.901(1) 0.2940(5) 0.0984 Uij ? ? C32 0.431(1) 0.920(1) 0.2543(4) 0.0870 Uij ? ? C33 0.563(1) 0.8866(9) 0.2565(3) 0.0556 Uij ? ? C34 0.659(1) 0.969(1) 0.2677(3) 0.0548 Uij ? ? C35 0.636(1) 1.095(1) 0.2791(4) 0.0818 Uij ? ? C36 0.540(1) 1.110(1) 0.3132(4) 0.0758 Uij ? ? H1 0.1465 0.5748 0.4911 0.1301 Uij ? ? H2 0.2891 0.5962 0.4937 0.1301 Uij ? ? H3 0.1990 0.7047 0.4895 0.1301 Uij ? ? H4 0.5167 0.5948 0.4227 0.0871 Uij ? ? H5 0.4485 0.5447 0.4606 0.0871 Uij ? ? H6 0.4720 0.4621 0.4234 0.0871 Uij ? ? H7 0.3546 0.5776 0.3131 0.0674 Uij ? ? H8 0.4652 0.6121 0.3412 0.0674 Uij ? ? H9 0.4189 0.4800 0.3395 0.0674 Uij ? ? H10 0.1069 0.5811 0.3130 0.1016 Uij ? ? H11 0.0322 0.6846 0.3331 0.1016 Uij ? ? H12 0.1593 0.7112 0.3127 0.1016 Uij ? ? H13 -0.0434 0.7094 0.3930 0.1502 Uij ? ? H14 -0.0406 0.6357 0.4330 0.1502 Uij ? ? H15 0.0115 0.7658 0.4323 0.1502 Uij ? ? H16 -0.0871 0.3240 0.2570 0.1067 Uij ? ? H17 -0.0962 0.4386 0.2837 0.1067 Uij ? ? H18 0.0292 0.3702 0.2803 0.1067 Uij ? ? H19 -0.3282 0.4222 0.3536 0.1412 Uij ? ? H20 -0.2221 0.4706 0.3812 0.1412 Uij ? ? H21 -0.2177 0.4923 0.3347 0.1412 Uij ? ? H22 -0.3234 0.1499 0.4108 0.1446 Uij ? ? H23 -0.2118 0.1951 0.4367 0.1446 Uij ? ? H24 -0.3050 0.2867 0.4182 0.1446 Uij ? ? H25 -0.0404 -0.0424 0.3602 0.1440 Uij ? ? H26 -0.0656 0.0041 0.4039 0.1440 Uij ? ? H27 -0.1756 -0.0375 0.3766 0.1440 Uij ? ? H28 0.1013 0.1294 0.2919 0.1208 Uij ? ? H29 0.0347 0.0131 0.3062 0.1208 Uij ? ? H30 -0.0178 0.0853 0.2696 0.1208 Uij ? ? H31 0.4140 0.2100 0.4114 0.0686 Uij ? ? H32 0.2869 0.0654 0.3935 0.0673 Uij ? ? H33 0.2496 -0.1048 0.4265 0.1157 Uij ? ? H34 0.3528 -0.0762 0.4582 0.1157 Uij ? ? H35 0.1092 -0.0588 0.4674 0.1440 Uij ? ? H36 0.2112 -0.0534 0.5009 0.1440 Uij ? ? H37 0.0686 0.1320 0.4791 0.0857 Uij ? ? H38 0.2050 0.2763 0.4996 0.0894 Uij ? ? H39 0.3938 0.2330 0.5248 0.1372 Uij ? ? H40 0.3694 0.0961 0.5203 0.1372 Uij ? ? H41 0.5059 0.1014 0.4782 0.0997 Uij ? ? H42 0.4969 0.2400 0.4736 0.0997 Uij ? ? H43 0.5828 0.9894 0.3618 0.0789 Uij ? ? H44 0.4462 0.8389 0.3496 0.0827 Uij ? ? H45 0.3223 0.8245 0.2933 0.1258 Uij ? ? H46 0.3010 0.9621 0.2971 0.1258 Uij ? ? H47 0.3913 0.8732 0.2339 0.1566 Uij ? ? H48 0.4247 1.0031 0.2473 0.1566 Uij ? ? H49 0.5853 0.8063 0.2501 0.0710 Uij ? ? H50 0.7430 0.9405 0.2678 0.0713 Uij ? ? H51 0.7123 1.1300 0.2879 0.1096 Uij ? ? H52 0.6064 1.1371 0.2558 0.1096 Uij ? ? H53 0.4612 1.1268 0.3015 0.0952 Uij ? ? H54 0.5647 1.1745 0.3303 0.0901 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir1 0.0322(2) 0.0373(2) 0.0412(2) -0.0020(2) 0.0017(2) -0.0020(2) Ir2 0.0270(2) 0.0419(2) 0.0362(2) -0.0019(2) -0.0016(2) 0.0005(2) Rh1 0.0292(4) 0.0432(5) 0.0356(4) -0.0012(4) -0.0017(3) 0.0025(4) Rh2 0.0438(5) 0.0558(6) 0.0449(5) -0.0039(4) -0.0015(4) 0.0029(4) Cl1 0.090(3) 0.121(3) 0.108(3) 0.053(3) 0.023(2) 0.025(3) Cl2 0.106(3) 0.101(3) 0.055(2) -0.037(2) -0.013(2) 0.020(2) S1 0.032(1) 0.044(2) 0.036(1) 0.000(1) 0.004(1) -0.001(1) S2 0.033(1) 0.050(2) 0.038(1) 0.000(1) 0.005(1) -0.004(1) C1 0.10(1) 0.040(7) 0.049(7) -0.034(7) 0.038(7) -0.018(6) C2 0.056(8) 0.043(7) 0.063(8) -0.023(6) -0.011(6) -0.009(6) C3 0.046(7) 0.037(6) 0.050(7) -0.011(5) -0.004(5) -0.005(5) C4 0.071(9) 0.031(7) 0.10(1) 0.001(6) -0.027(8) 0.008(7) C5 0.059(9) 0.048(8) 0.083(10) -0.001(6) 0.008(8) -0.005(7) C6 0.20(2) 0.10(1) 0.063(9) -0.08(1) 0.06(1) -0.044(9) C7 0.082(10) 0.10(1) 0.075(9) -0.045(9) -0.038(8) 0.018(8) C8 0.077(9) 0.063(8) 0.054(7) -0.023(7) 0.009(7) -0.002(6) C9 0.071(10) 0.09(1) 0.13(1) -0.021(8) -0.043(9) 0.049(10) C10 0.08(1) 0.058(10) 0.25(2) 0.012(8) 0.04(1) -0.01(1) C11 0.031(6) 0.089(10) 0.048(7) -0.017(6) -0.012(5) 0.000(7) C12 0.038(7) 0.078(9) 0.066(8) 0.008(6) -0.024(6) -0.022(7) C13 0.032(6) 0.12(1) 0.036(6) -0.023(7) 0.002(5) 0.005(8) C14 0.057(8) 0.055(9) 0.09(1) -0.027(7) -0.032(7) 0.016(7) C15 0.038(7) 0.068(9) 0.064(8) 0.001(6) -0.021(6) -0.019(7) C16 0.10(1) 0.13(1) 0.056(8) -0.034(10) -0.033(8) 0.029(9) C17 0.065(10) 0.11(1) 0.17(2) 0.049(9) -0.044(10) -0.04(1) C18 0.067(10) 0.29(2) 0.058(9) -0.09(1) 0.012(7) -0.02(1) C19 0.16(2) 0.08(1) 0.14(1) -0.06(1) -0.07(1) 0.03(1) C20 0.08(1) 0.15(2) 0.12(1) 0.01(1) -0.010(9) -0.07(1) C21 0.030(6) 0.074(9) 0.068(8) 0.018(6) 0.007(6) 0.022(7) C22 0.049(7) 0.050(7) 0.069(8) 0.016(6) -0.003(6) 0.010(6) C23 0.09(1) 0.055(9) 0.13(1) 0.005(8) -0.014(10) 0.019(9) C24 0.17(2) 0.07(1) 0.13(1) 0.01(1) 0.05(1) 0.05(1) C25 0.051(8) 0.09(1) 0.068(9) 0.005(7) 0.003(6) 0.033(8) C26 0.064(9) 0.10(1) 0.045(7) 0.007(8) -0.005(6) 0.011(7) C27 0.056(9) 0.26(2) 0.053(9) 0.00(1) -0.019(7) -0.01(1) C28 0.044(8) 0.14(1) 0.09(1) 0.007(8) -0.023(7) 0.020(10) C29 0.059(8) 0.077(10) 0.071(9) -0.008(7) 0.011(7) -0.010(7) C30 0.067(9) 0.067(9) 0.09(1) 0.002(8) 0.026(8) -0.009(8) C31 0.037(8) 0.11(1) 0.15(2) 0.005(8) -0.006(9) -0.02(1) C32 0.09(1) 0.070(10) 0.10(1) -0.005(8) -0.058(9) 0.010(9) C33 0.071(9) 0.042(7) 0.053(7) 0.007(6) -0.016(6) -0.002(6) C34 0.058(8) 0.065(8) 0.041(6) 0.006(7) -0.013(5) 0.014(6) C35 0.11(1) 0.065(9) 0.068(9) -0.024(9) -0.015(8) 0.008(8) C36 0.09(1) 0.059(9) 0.083(10) -0.009(8) 0.004(8) -0.022(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.24082 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4985 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0300 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.560 _refine_ls_shift/esd_max 0.0570 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.45530 _refine_diff_density_max -1.10470 #------------------------------------------------------------------------------ _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 Ir(1) Ir(2) 2.8643(8) ? ? yes Ir(1) Rh(1) 2.906(1) ? ? yes Ir(1) S(1) 2.286(3) ? ? yes Ir(1) S(2) 2.283(3) ? ? yes Ir(1) C(1) 2.14(1) ? ? yes Ir(1) C(2) 2.146(10) ? ? yes Ir(1) C(3) 2.173(10) ? ? yes Ir(1) C(4) 2.18(1) ? ? yes Ir(1) C(5) 2.14(1) ? ? yes Ir(2) Rh(1) 2.9130(9) ? ? yes Ir(2) S(1) 2.292(2) ? ? yes Ir(2) S(2) 2.290(3) ? ? yes Ir(2) C(11) 2.19(1) ? ? yes Ir(2) C(12) 2.15(1) ? ? yes Ir(2) C(13) 2.170(10) ? ? yes Ir(2) C(14) 2.14(1) ? ? yes Ir(2) C(15) 2.18(1) ? ? yes Rh(1) S(1) 2.300(3) ? ? yes Rh(1) S(2) 2.293(3) ? ? yes Rh(1) C(21) 2.141(10) ? ? yes Rh(1) C(22) 2.15(1) ? ? yes Rh(1) C(25) 2.17(1) ? ? yes Rh(1) C(26) 2.16(1) ? ? yes Rh(2) Cl(1) 2.360(4) ? ? yes Rh(2) Cl(2) 2.374(3) ? ? yes Rh(2) C(29) 2.10(1) ? ? yes Rh(2) C(30) 2.09(1) ? ? yes Rh(2) C(33) 2.13(1) ? ? yes Rh(2) C(34) 2.11(1) ? ? yes C(1) C(2) 1.41(1) ? ? yes C(1) C(5) 1.43(2) ? ? yes C(1) C(6) 1.52(1) ? ? yes C(2) C(3) 1.38(1) ? ? yes C(2) C(7) 1.53(1) ? ? yes C(3) C(4) 1.43(1) ? ? yes C(3) C(8) 1.51(1) ? ? yes C(4) C(5) 1.38(2) ? ? yes C(4) C(9) 1.52(2) ? ? yes C(5) C(10) 1.51(2) ? ? yes C(11) C(12) 1.41(1) ? ? yes C(11) C(15) 1.42(2) ? ? yes C(11) C(16) 1.50(1) ? ? yes C(12) C(13) 1.42(2) ? ? yes C(12) C(17) 1.51(2) ? ? yes C(13) C(14) 1.42(2) ? ? yes C(13) C(18) 1.50(1) ? ? yes C(14) C(15) 1.42(2) ? ? yes C(14) C(19) 1.49(2) ? ? yes C(15) C(20) 1.51(2) ? ? yes C(21) C(22) 1.33(1) ? ? yes C(21) C(28) 1.53(2) ? ? yes C(22) C(23) 1.49(2) ? ? yes C(23) C(24) 1.50(2) ? ? yes C(24) C(25) 1.48(2) ? ? yes C(25) C(26) 1.39(2) ? ? yes C(26) C(27) 1.47(2) ? ? yes C(27) C(28) 1.43(2) ? ? yes C(29) C(30) 1.37(2) ? ? yes C(29) C(36) 1.52(2) ? ? yes C(30) C(31) 1.53(2) ? ? yes C(31) C(32) 1.52(2) ? ? yes C(32) C(33) 1.47(2) ? ? yes C(33) C(34) 1.43(1) ? ? yes C(34) C(35) 1.48(2) ? ? yes C(35) C(36) 1.53(2) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_bond_publ_flag Ir(2) Ir(1) Rh(1) 60.64(2) ? ? ? yes Ir(2) Ir(1) S(1) 51.37(6) ? ? ? yes Ir(2) Ir(1) S(2) 51.33(6) ? ? ? yes Ir(2) Ir(1) C(1) 151.8(3) ? ? ? yes Ir(2) Ir(1) C(2) 169.7(3) ? ? ? yes Ir(2) Ir(1) C(3) 137.8(3) ? ? ? yes Ir(2) Ir(1) C(4) 119.2(3) ? ? ? yes Ir(2) Ir(1) C(5) 124.6(3) ? ? ? yes Rh(1) Ir(1) S(1) 50.90(6) ? ? ? yes Rh(1) Ir(1) S(2) 50.73(7) ? ? ? yes Rh(1) Ir(1) C(1) 121.9(3) ? ? ? yes Rh(1) Ir(1) C(2) 115.2(3) ? ? ? yes Rh(1) Ir(1) C(3) 133.7(3) ? ? ? yes Rh(1) Ir(1) C(4) 169.4(4) ? ? ? yes Rh(1) Ir(1) C(5) 152.8(4) ? ? ? yes S(1) Ir(1) S(2) 86.60(9) ? ? ? yes S(1) Ir(1) C(1) 155.1(4) ? ? ? yes S(1) Ir(1) C(2) 118.4(3) ? ? ? yes S(1) Ir(1) C(3) 102.7(3) ? ? ? yes S(1) Ir(1) C(4) 119.8(4) ? ? ? yes S(1) Ir(1) C(5) 155.7(4) ? ? ? yes S(2) Ir(1) C(1) 106.1(3) ? ? ? yes S(2) Ir(1) C(2) 134.8(3) ? ? ? yes S(2) Ir(1) C(3) 170.1(3) ? ? ? yes S(2) Ir(1) C(4) 138.6(4) ? ? ? yes S(2) Ir(1) C(5) 108.8(3) ? ? ? yes C(1) Ir(1) C(2) 38.5(4) ? ? ? yes C(1) Ir(1) C(3) 64.0(4) ? ? ? yes C(1) Ir(1) C(4) 63.9(4) ? ? ? yes C(1) Ir(1) C(5) 39.1(4) ? ? ? yes C(2) Ir(1) C(3) 37.2(4) ? ? ? yes C(2) Ir(1) C(4) 63.0(4) ? ? ? yes C(2) Ir(1) C(5) 63.9(4) ? ? ? yes C(3) Ir(1) C(4) 38.4(4) ? ? ? yes C(3) Ir(1) C(5) 63.6(4) ? ? ? yes C(4) Ir(1) C(5) 37.2(4) ? ? ? yes Ir(1) Ir(2) Rh(1) 60.39(3) ? ? ? yes Ir(1) Ir(2) S(1) 51.17(6) ? ? ? yes Ir(1) Ir(2) S(2) 51.12(6) ? ? ? yes Ir(1) Ir(2) C(11) 122.2(3) ? ? ? yes Ir(1) Ir(2) C(12) 120.5(3) ? ? ? yes Ir(1) Ir(2) C(13) 142.9(4) ? ? ? yes Ir(1) Ir(2) C(14) 173.8(3) ? ? ? yes Ir(1) Ir(2) C(15) 146.1(3) ? ? ? yes Rh(1) Ir(2) S(1) 50.75(6) ? ? ? yes Rh(1) Ir(2) S(2) 50.58(7) ? ? ? yes Rh(1) Ir(2) C(11) 159.7(3) ? ? ? yes Rh(1) Ir(2) C(12) 161.5(3) ? ? ? yes Rh(1) Ir(2) C(13) 128.3(3) ? ? ? yes Rh(1) Ir(2) C(14) 113.7(3) ? ? ? yes Rh(1) Ir(2) C(15) 127.3(3) ? ? ? yes S(1) Ir(2) S(2) 86.29(8) ? ? ? yes S(1) Ir(2) C(11) 113.0(3) ? ? ? yes S(1) Ir(2) C(12) 146.2(4) ? ? ? yes S(1) Ir(2) C(13) 165.7(4) ? ? ? yes S(1) Ir(2) C(14) 127.4(4) ? ? ? yes S(1) Ir(2) C(15) 104.7(3) ? ? ? yes S(2) Ir(2) C(11) 148.8(4) ? ? ? yes S(2) Ir(2) C(12) 113.8(3) ? ? ? yes S(2) Ir(2) C(13) 103.1(3) ? ? ? yes S(2) Ir(2) C(14) 124.3(4) ? ? ? yes S(2) Ir(2) C(15) 162.5(4) ? ? ? yes C(11) Ir(2) C(12) 38.1(4) ? ? ? yes C(11) Ir(2) C(13) 63.7(4) ? ? ? yes C(11) Ir(2) C(14) 64.0(4) ? ? ? yes C(11) Ir(2) C(15) 37.9(4) ? ? ? yes C(12) Ir(2) C(13) 38.4(4) ? ? ? yes C(12) Ir(2) C(14) 64.4(4) ? ? ? yes C(12) Ir(2) C(15) 63.8(4) ? ? ? yes C(13) Ir(2) C(14) 38.4(4) ? ? ? yes C(13) Ir(2) C(15) 63.7(4) ? ? ? yes C(14) Ir(2) C(15) 38.2(4) ? ? ? yes Ir(1) Rh(1) Ir(2) 58.98(2) ? ? ? yes Ir(1) Rh(1) S(1) 50.46(7) ? ? ? yes Ir(1) Rh(1) S(2) 50.44(7) ? ? ? yes Ir(1) Rh(1) C(21) 114.5(3) ? ? ? yes Ir(1) Rh(1) C(22) 138.0(3) ? ? ? yes Ir(1) Rh(1) C(25) 140.3(4) ? ? ? yes Ir(1) Rh(1) C(26) 117.8(4) ? ? ? yes Ir(2) Rh(1) S(1) 50.51(6) ? ? ? yes Ir(2) Rh(1) S(2) 50.49(6) ? ? ? yes Ir(2) Rh(1) C(21) 138.8(3) ? ? ? yes Ir(2) Rh(1) C(22) 118.1(3) ? ? ? yes Ir(2) Rh(1) C(25) 115.6(3) ? ? ? yes Ir(2) Rh(1) C(26) 139.5(3) ? ? ? yes S(1) Rh(1) S(2) 86.04(9) ? ? ? yes S(1) Rh(1) C(21) 92.3(3) ? ? ? yes S(1) Rh(1) C(22) 93.4(3) ? ? ? yes S(1) Rh(1) C(25) 160.0(4) ? ? ? yes S(1) Rh(1) C(26) 162.6(4) ? ? ? yes S(2) Rh(1) C(21) 159.8(4) ? ? ? yes S(2) Rh(1) C(22) 163.9(3) ? ? ? yes S(2) Rh(1) C(25) 94.1(3) ? ? ? yes S(2) Rh(1) C(26) 94.4(3) ? ? ? yes C(21) Rh(1) C(22) 36.2(4) ? ? ? yes C(21) Rh(1) C(25) 94.3(4) ? ? ? yes C(21) Rh(1) C(26) 81.3(4) ? ? ? yes C(22) Rh(1) C(25) 81.1(5) ? ? ? yes C(22) Rh(1) C(26) 90.9(4) ? ? ? yes C(25) Rh(1) C(26) 37.4(4) ? ? ? yes Cl(1) Rh(2) Cl(2) 90.4(1) ? ? ? yes Cl(1) Rh(2) C(29) 162.8(4) ? ? ? yes Cl(1) Rh(2) C(30) 159.0(4) ? ? ? yes Cl(1) Rh(2) C(33) 92.1(3) ? ? ? yes Cl(1) Rh(2) C(34) 89.5(3) ? ? ? yes Cl(2) Rh(2) C(29) 92.4(4) ? ? ? yes Cl(2) Rh(2) C(30) 90.3(4) ? ? ? yes Cl(2) Rh(2) C(33) 163.3(3) ? ? ? yes Cl(2) Rh(2) C(34) 157.2(3) ? ? ? yes C(29) Rh(2) C(30) 38.0(4) ? ? ? yes C(29) Rh(2) C(33) 90.1(4) ? ? ? yes C(29) Rh(2) C(34) 81.4(5) ? ? ? yes C(30) Rh(2) C(33) 81.5(5) ? ? ? yes C(30) Rh(2) C(34) 97.7(5) ? ? ? yes C(33) Rh(2) C(34) 39.4(4) ? ? ? yes Ir(1) S(1) Ir(2) 77.46(7) ? ? ? yes Ir(1) S(1) Rh(1) 78.63(8) ? ? ? yes Ir(2) S(1) Rh(1) 78.73(7) ? ? ? yes Ir(1) S(2) Ir(2) 77.55(8) ? ? ? yes Ir(1) S(2) Rh(1) 78.84(8) ? ? ? yes Ir(2) S(2) Rh(1) 78.93(8) ? ? ? yes Ir(1) C(1) C(2) 70.9(6) ? ? ? yes Ir(1) C(1) C(5) 70.3(7) ? ? ? yes Ir(1) C(1) C(6) 125.4(8) ? ? ? yes C(2) C(1) C(5) 105.5(10) ? ? ? yes C(2) C(1) C(6) 125(1) ? ? ? yes C(5) C(1) C(6) 128(1) ? ? ? yes Ir(1) C(2) C(1) 70.6(6) ? ? ? yes Ir(1) C(2) C(3) 72.5(6) ? ? ? yes Ir(1) C(2) C(7) 124.5(8) ? ? ? yes C(1) C(2) C(3) 110(1) ? ? ? yes C(1) C(2) C(7) 125(1) ? ? ? yes C(3) C(2) C(7) 124(1) ? ? ? yes Ir(1) C(3) C(2) 70.3(6) ? ? ? yes Ir(1) C(3) C(4) 70.9(6) ? ? ? yes Ir(1) C(3) C(8) 126.2(7) ? ? ? yes C(2) C(3) C(4) 107(1) ? ? ? yes C(2) C(3) C(8) 126(1) ? ? ? yes C(4) C(3) C(8) 125(1) ? ? ? yes Ir(1) C(4) C(3) 70.7(6) ? ? ? yes Ir(1) C(4) C(5) 69.9(7) ? ? ? yes Ir(1) C(4) C(9) 124.8(8) ? ? ? yes C(3) C(4) C(5) 108(1) ? ? ? yes C(3) C(4) C(9) 125(1) ? ? ? yes C(5) C(4) C(9) 126(1) ? ? ? yes Ir(1) C(5) C(1) 70.6(6) ? ? ? yes Ir(1) C(5) C(4) 72.9(7) ? ? ? yes Ir(1) C(5) C(10) 125.6(9) ? ? ? yes C(1) C(5) C(4) 108(1) ? ? ? yes C(1) C(5) C(10) 122(1) ? ? ? yes C(4) C(5) C(10) 128(1) ? ? ? yes Ir(2) C(11) C(12) 69.7(6) ? ? ? yes Ir(2) C(11) C(15) 70.9(6) ? ? ? yes Ir(2) C(11) C(16) 125.8(8) ? ? ? yes C(12) C(11) C(15) 107(1) ? ? ? yes C(12) C(11) C(16) 126(1) ? ? ? yes C(15) C(11) C(16) 125(1) ? ? ? yes Ir(2) C(12) C(11) 72.3(6) ? ? ? yes Ir(2) C(12) C(13) 71.5(6) ? ? ? yes Ir(2) C(12) C(17) 127.5(8) ? ? ? yes C(11) C(12) C(13) 108(1) ? ? ? yes C(11) C(12) C(17) 128(1) ? ? ? yes C(13) C(12) C(17) 122(1) ? ? ? yes Ir(2) C(13) C(12) 70.1(6) ? ? ? yes Ir(2) C(13) C(14) 69.6(6) ? ? ? yes Ir(2) C(13) C(18) 125.5(8) ? ? ? yes C(12) C(13) C(14) 107.4(10) ? ? ? yes C(12) C(13) C(18) 127(1) ? ? ? yes C(14) C(13) C(18) 125(1) ? ? ? yes Ir(2) C(14) C(13) 72.0(6) ? ? ? yes Ir(2) C(14) C(15) 72.5(6) ? ? ? yes Ir(2) C(14) C(19) 125.9(9) ? ? ? yes C(13) C(14) C(15) 108(1) ? ? ? yes C(13) C(14) C(19) 128(1) ? ? ? yes C(15) C(14) C(19) 123(1) ? ? ? yes Ir(2) C(15) C(11) 71.3(6) ? ? ? yes Ir(2) C(15) C(14) 69.3(6) ? ? ? yes Ir(2) C(15) C(20) 126.8(8) ? ? ? yes C(11) C(15) C(14) 107(1) ? ? ? yes C(11) C(15) C(20) 125(1) ? ? ? yes C(14) C(15) C(20) 126(1) ? ? ? yes Rh(1) C(21) C(22) 72.3(6) ? ? ? yes Rh(1) C(21) C(28) 108.7(8) ? ? ? yes C(22) C(21) C(28) 124(1) ? ? ? yes Rh(1) C(22) C(21) 71.6(6) ? ? ? yes Rh(1) C(22) C(23) 112.8(8) ? ? ? yes C(21) C(22) C(23) 128(1) ? ? ? yes C(22) C(23) C(24) 114(1) ? ? ? yes C(23) C(24) C(25) 117(1) ? ? ? yes Rh(1) C(25) C(24) 109.7(9) ? ? ? yes Rh(1) C(25) C(26) 71.2(7) ? ? ? yes C(24) C(25) C(26) 126(1) ? ? ? yes Rh(1) C(26) C(25) 71.5(7) ? ? ? yes Rh(1) C(26) C(27) 111.6(8) ? ? ? yes C(25) C(26) C(27) 123(1) ? ? ? yes C(26) C(27) C(28) 116(1) ? ? ? yes C(21) C(28) C(27) 116(1) ? ? ? yes Rh(2) C(29) C(30) 70.7(8) ? ? ? yes Rh(2) C(29) C(36) 114.5(8) ? ? ? yes C(30) C(29) C(36) 124(1) ? ? ? yes Rh(2) C(30) C(29) 71.3(8) ? ? ? yes Rh(2) C(30) C(31) 111.3(8) ? ? ? yes C(29) C(30) C(31) 123(1) ? ? ? yes C(30) C(31) C(32) 112(1) ? ? ? yes C(31) C(32) C(33) 113(1) ? ? ? yes Rh(2) C(33) C(32) 114.6(9) ? ? ? yes Rh(2) C(33) C(34) 69.6(6) ? ? ? yes C(32) C(33) C(34) 123(1) ? ? ? yes Rh(2) C(34) C(33) 71.0(6) ? ? ? yes Rh(2) C(34) C(35) 112.7(8) ? ? ? yes C(33) C(34) C(35) 123(1) ? ? ? yes C(34) C(35) C(36) 113(1) ? ? ? yes C(29) C(36) C(35) 111(1) ? ? ? yes #------------------------------------------------------------------------------ data_OM960769D_compound_11_Cp*2Ir2S2Pd(PPh3)Cl2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Nov 21 07:18:15 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution DIRDIF92 (PATTY) _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 12.057(1) _cell_length_b 12.521(2) _cell_length_c 14.701(1) _cell_angle_alpha 90 _cell_angle_beta 93.219(7) _cell_angle_gamma 90 _cell_volume 2215.8(3) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 37.74 _cell_measurement_theta_max 39.28 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m ' _symmetry_Int_Tables_number 11 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' ' -x, -y, -z' ' +x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_measured ? _exptl_crystal_F000 1192.00 _exptl_absorpt_coefficient_mu_cm 68.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.594 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_\% -0.42 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5564 _diffrn_reflns_av_R_equivalents 3.29 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 15 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 16 _diffrn_reflns_l_min -4 _diffrn_reflns_l_max 18 _diffrn_theta_min ? _diffrn_theta_max 27.5014 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.07787 _diffrn_orient_matrix_12 0.00268 _diffrn_orient_matrix_13 -0.02716 _diffrn_orient_matrix_21 0.02005 _diffrn_orient_matrix_22 0.06231 _diffrn_orient_matrix_23 -0.03834 _diffrn_orient_matrix_31 0.02085 _diffrn_orient_matrix_32 -0.04990 _diffrn_orient_matrix_33 -0.04933 #------------------------------------------------------------------------------ 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 78 0.003 0.002 'International Tables' H 0 94 0.000 0.000 'International Tables' Pd 0 2 -0.999 1.007 'International Tables' S 0 4 0.125 0.123 'International Tables' Cl 0 8 0.148 0.159 'International Tables' P 0 2 0.102 0.094 'International Tables' Ir 0 4 -1.444 7.990 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ir1 0.22011(3) 0.13392(3) 0.76615(3) 0.0378 Uij ? ? Pd1 0.16838(7) 0.2500 0.59042(6) 0.0333 Uij ? ? Cl1 0.0011(2) 0.2500 0.5008(2) 0.0485 Uij ? ? Cl2 0.4497(4) 0.2500 1.1305(3) 0.0931 Uij ? ? Cl3 0.7147(9) 0.2500 0.9063(7) 0.2977 Uij ? ? Cl4 0.828(1) 0.2500 1.0680(8) 0.3538 Uij ? ? S1 0.0778(2) 0.2500 0.7288(2) 0.0389 Uij ? ? S2 0.3241(2) 0.2500 0.6864(2) 0.0385 Uij ? ? P1 0.2674(2) 0.2500 0.4620(2) 0.0341 Uij ? ? C1 0.1880(8) -0.0351(7) 0.7609(7) 0.0558 Uij ? ? C2 0.3079(8) -0.0178(7) 0.7667(6) 0.0553 Uij ? ? C3 0.3347(7) 0.0361(8) 0.8514(7) 0.0548 Uij ? ? C4 0.2327(8) 0.0529(8) 0.8961(6) 0.0560 Uij ? ? C5 0.1466(8) 0.0052(8) 0.8433(7) 0.0585 Uij ? ? C6 0.127(1) -0.0913(8) 0.6839(8) 0.1094 Uij ? ? C7 0.3881(10) -0.0564(9) 0.7021(8) 0.1075 Uij ? ? C8 0.4490(8) 0.0664(9) 0.8881(7) 0.0868 Uij ? ? C9 0.2258(9) 0.0986(9) 0.9891(7) 0.0907 Uij ? ? C10 0.0250(9) -0.0015(9) 0.8662(8) 0.0950 Uij ? ? C11 0.2425(6) 0.1303(7) 0.3934(5) 0.0372 Uij ? ? C12 0.1731(7) 0.0511(7) 0.4253(6) 0.0475 Uij ? ? C13 0.1560(7) -0.0424(7) 0.3773(7) 0.0573 Uij ? ? C14 0.2072(8) -0.0593(8) 0.2962(7) 0.0680 Uij ? ? C15 0.2752(8) 0.0179(8) 0.2649(6) 0.0641 Uij ? ? C16 0.2940(7) 0.1125(8) 0.3130(6) 0.0537 Uij ? ? C17 0.4187(9) 0.2500 0.4869(7) 0.0313 Uij ? ? C18 0.4743(7) 0.1555(6) 0.5026(6) 0.0533 Uij ? ? C19 0.5854(7) 0.1568(7) 0.5319(7) 0.0650 Uij ? ? C20 0.6414(10) 0.2500 0.5457(9) 0.0551 Uij ? ? C21 0.697(2) 0.2500 1.022(2) 0.1761 Uij ? ? H1 0.0496 -0.0930 0.6946 0.1079 Uij ? ? H2 0.1373 -0.0543 0.6287 0.1079 Uij ? ? H3 0.1538 -0.1622 0.6796 0.1079 Uij ? ? H4 0.4365 -0.1071 0.7314 0.1135 Uij ? ? H5 0.3491 -0.0891 0.6514 0.1135 Uij ? ? H6 0.4302 0.0020 0.6815 0.1135 Uij ? ? H7 0.4937 0.0041 0.8947 0.0958 Uij ? ? H8 0.4814 0.1144 0.8470 0.0958 Uij ? ? H9 0.4444 0.1001 0.9457 0.0958 Uij ? ? H10 0.2969 0.1241 1.0102 0.0941 Uij ? ? H11 0.1741 0.1559 0.9872 0.0941 Uij ? ? H12 0.2021 0.0448 1.0293 0.0941 Uij ? ? H13 -0.0037 0.0686 0.8730 0.1004 Uij ? ? H14 -0.0164 -0.0373 0.8187 0.1004 Uij ? ? H15 0.0194 -0.0397 0.9217 0.1004 Uij ? ? H16 0.1372 0.0619 0.4805 0.0566 Uij ? ? H17 0.1088 -0.0959 0.3998 0.0649 Uij ? ? H18 0.1950 -0.1237 0.2630 0.0756 Uij ? ? H19 0.3102 0.0068 0.2094 0.0697 Uij ? ? H20 0.3424 0.1650 0.2906 0.0621 Uij ? ? H21 0.4367 0.0894 0.4934 0.0622 Uij ? ? H22 0.6233 0.0910 0.5424 0.0719 Uij ? ? H23 0.7191 0.2500 0.5656 0.0602 Uij ? ? H24 0.6580 0.1881 1.0385 0.0779 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir1 0.0372(2) 0.0396(2) 0.0366(2) 0.0015(2) 0.0027(1) 0.0035(2) Pd1 0.0281(5) 0.0370(6) 0.0351(6) 0.0000 0.0036(4) 0.0000 Cl1 0.032(2) 0.061(2) 0.051(2) 0.0000 -0.004(1) 0.0000 Cl2 0.115(4) 0.090(3) 0.074(3) 0.0000 -0.004(3) 0.0000 Cl3 0.35(1) 0.33(1) 0.21(1) 0.0000 0.052(10) 0.0000 Cl4 0.47(2) 0.103(6) 0.46(2) 0.0000 -0.29(1) 0.0000 S1 0.031(2) 0.042(2) 0.045(2) 0.0000 0.008(1) 0.0000 S2 0.032(2) 0.044(2) 0.040(2) 0.0000 0.003(1) 0.0000 P1 0.030(2) 0.034(2) 0.039(2) 0.0000 0.005(2) 0.0000 C1 0.080(8) 0.037(6) 0.047(7) 0.000(5) -0.028(6) 0.009(5) C2 0.072(7) 0.056(7) 0.038(6) 0.019(6) 0.006(5) 0.009(5) C3 0.042(6) 0.066(7) 0.056(7) 0.006(5) -0.001(5) 0.027(6) C4 0.070(7) 0.060(7) 0.037(6) -0.013(6) -0.005(5) 0.002(5) C5 0.056(7) 0.053(7) 0.068(8) 0.003(6) 0.011(6) 0.026(6) C6 0.17(1) 0.045(7) 0.11(1) -0.015(8) -0.041(9) 0.003(7) C7 0.12(1) 0.101(10) 0.11(1) 0.059(9) 0.050(9) 0.019(9) C8 0.056(7) 0.110(10) 0.093(9) -0.010(7) -0.012(6) 0.020(8) C9 0.119(10) 0.099(10) 0.056(8) -0.006(8) 0.022(7) 0.016(7) C10 0.069(8) 0.107(10) 0.11(1) -0.016(7) 0.008(7) 0.052(8) C11 0.034(4) 0.038(5) 0.040(5) 0.002(5) -0.001(4) -0.002(5) C12 0.043(5) 0.039(5) 0.061(7) 0.002(5) 0.004(5) -0.006(5) C13 0.043(6) 0.034(6) 0.094(9) -0.004(5) -0.011(6) -0.005(6) C14 0.062(7) 0.056(7) 0.084(9) 0.001(6) -0.014(6) -0.019(7) C15 0.073(7) 0.069(8) 0.051(7) 0.013(6) 0.009(6) -0.023(6) C16 0.056(6) 0.055(7) 0.051(6) -0.005(5) 0.009(5) -0.001(5) C17 0.027(6) 0.034(7) 0.033(7) 0.0000 0.002(5) 0.0000 C18 0.046(6) 0.032(6) 0.079(7) 0.004(4) -0.017(5) -0.009(5) C19 0.054(6) 0.040(6) 0.099(9) 0.021(5) -0.020(6) -0.016(6) C20 0.039(8) 0.052(9) 0.07(1) 0.0000 -0.023(7) 0.0000 C21 0.19(2) 0.12(2) 0.24(3) 0.0000 0.17(2) 0.0000 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.32487 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3398 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0280 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.100 _refine_ls_shift/esd_max 0.2430 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.78610 _refine_diff_density_max -1.30990 #------------------------------------------------------------------------------ _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 Ir(1) Ir(1) 2.9068(8) ? ? yes Ir(1) Pd(1) 2.9991(9) ? ? yes Ir(1) S(1) 2.292(2) ? ? yes Ir(1) S(2) 2.286(2) ? ? yes Ir(1) C(1) 2.152(9) ? ? yes Ir(1) C(2) 2.174(9) ? ? yes Ir(1) C(3) 2.188(9) ? ? yes Ir(1) C(4) 2.161(9) ? ? yes Ir(1) C(5) 2.187(9) ? ? yes Pd(1) Cl(1) 2.347(3) ? ? yes Pd(1) S(1) 2.363(3) ? ? yes Pd(1) S(2) 2.284(3) ? ? yes Pd(1) P(1) 2.289(3) ? ? yes Cl(3) C(21) 1.72(3) ? ? yes Cl(4) C(21) 1.68(3) ? ? yes P(1) C(11) 1.822(8) ? ? yes P(1) C(11) 1.822(8) ? ? yes P(1) C(17) 1.84(1) ? ? yes C(1) C(2) 1.46(1) ? ? yes C(1) C(5) 1.43(1) ? ? yes C(1) C(6) 1.49(1) ? ? yes C(2) C(3) 1.44(1) ? ? yes C(2) C(7) 1.48(1) ? ? yes C(3) C(4) 1.44(1) ? ? yes C(3) C(8) 1.50(1) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(4) C(9) 1.49(1) ? ? yes C(5) C(10) 1.52(1) ? ? yes C(11) C(12) 1.40(1) ? ? yes C(11) C(16) 1.384(10) ? ? yes C(12) C(13) 1.38(1) ? ? yes C(13) C(14) 1.39(1) ? ? yes C(14) C(15) 1.36(1) ? ? yes C(15) C(16) 1.39(1) ? ? yes C(17) C(18) 1.373(9) ? ? yes C(17) C(18) 1.373(9) ? ? yes C(18) C(19) 1.38(1) ? ? yes C(19) C(20) 1.36(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_bond_publ_flag Ir(1) Ir(1) Pd(1) 61.01(1) ? ? ? yes Ir(1) Ir(1) S(1) 50.64(5) ? ? ? yes Ir(1) Ir(1) S(2) 50.51(5) ? ? ? yes Ir(1) Ir(1) C(1) 169.5(3) ? ? ? yes Ir(1) Ir(1) C(2) 150.9(3) ? ? ? yes Ir(1) Ir(1) C(3) 124.0(3) ? ? ? yes Ir(1) Ir(1) C(4) 118.0(3) ? ? ? yes Ir(1) Ir(1) C(5) 137.5(3) ? ? ? yes Pd(1) Ir(1) S(1) 50.93(8) ? ? ? yes Pd(1) Ir(1) S(2) 48.96(8) ? ? ? yes Pd(1) Ir(1) C(1) 114.7(3) ? ? ? yes Pd(1) Ir(1) C(2) 120.3(2) ? ? ? yes Pd(1) Ir(1) C(3) 149.2(2) ? ? ? yes Pd(1) Ir(1) C(4) 171.9(3) ? ? ? yes Pd(1) Ir(1) C(5) 137.1(3) ? ? ? yes S(1) Ir(1) S(2) 84.19(8) ? ? ? yes S(1) Ir(1) C(1) 119.0(3) ? ? ? yes S(1) Ir(1) C(2) 155.9(3) ? ? ? yes S(1) Ir(1) C(3) 158.8(3) ? ? ? yes S(1) Ir(1) C(4) 121.6(3) ? ? ? yes S(1) Ir(1) C(5) 105.8(3) ? ? ? yes S(2) Ir(1) C(1) 135.2(3) ? ? ? yes S(2) Ir(1) C(2) 106.1(3) ? ? ? yes S(2) Ir(1) C(3) 107.6(2) ? ? ? yes S(2) Ir(1) C(4) 137.6(3) ? ? ? yes S(2) Ir(1) C(5) 170.0(3) ? ? ? yes C(1) Ir(1) C(2) 39.4(3) ? ? ? yes C(1) Ir(1) C(3) 65.0(4) ? ? ? yes C(1) Ir(1) C(4) 64.8(3) ? ? ? yes C(1) Ir(1) C(5) 38.4(3) ? ? ? yes C(2) Ir(1) C(3) 38.5(3) ? ? ? yes C(2) Ir(1) C(4) 64.9(3) ? ? ? yes C(2) Ir(1) C(5) 64.2(3) ? ? ? yes C(3) Ir(1) C(4) 38.7(3) ? ? ? yes C(3) Ir(1) C(5) 63.4(3) ? ? ? yes C(4) Ir(1) C(5) 37.4(3) ? ? ? yes Ir(1) Pd(1) Ir(1) 57.97(2) ? ? ? yes Ir(1) Pd(1) Cl(1) 127.91(7) ? ? ? yes Ir(1) Pd(1) S(1) 48.86(6) ? ? ? yes Ir(1) Pd(1) S(2) 49.00(6) ? ? ? yes Ir(1) Pd(1) P(1) 128.12(7) ? ? ? yes Ir(1) Pd(1) Cl(1) 127.91(7) ? ? ? yes Ir(1) Pd(1) S(1) 48.86(6) ? ? ? yes Ir(1) Pd(1) S(2) 49.00(6) ? ? ? yes Ir(1) Pd(1) P(1) 128.12(7) ? ? ? yes Cl(1) Pd(1) S(1) 93.4(1) ? ? ? yes Cl(1) Pd(1) S(2) 176.0(1) ? ? ? yes Cl(1) Pd(1) P(1) 90.5(1) ? ? ? yes S(1) Pd(1) S(2) 82.6(1) ? ? ? yes S(1) Pd(1) P(1) 176.1(1) ? ? ? yes S(2) Pd(1) P(1) 93.5(1) ? ? ? yes Ir(1) S(1) Ir(1) 78.71(10) ? ? ? yes Ir(1) S(1) Pd(1) 80.21(8) ? ? ? yes Ir(1) S(1) Pd(1) 80.21(8) ? ? ? yes Ir(1) S(2) Ir(1) 78.98(9) ? ? ? yes Ir(1) S(2) Pd(1) 82.04(9) ? ? ? yes Ir(1) S(2) Pd(1) 82.04(9) ? ? ? yes Pd(1) P(1) C(11) 112.3(3) ? ? ? yes Pd(1) P(1) C(11) 112.3(3) ? ? ? yes Pd(1) P(1) C(17) 113.2(4) ? ? ? yes C(11) P(1) C(11) 110.7(5) ? ? ? yes C(11) P(1) C(17) 103.9(3) ? ? ? yes C(11) P(1) C(17) 103.9(3) ? ? ? yes Ir(1) C(1) C(2) 71.1(5) ? ? ? yes Ir(1) C(1) C(5) 72.1(6) ? ? ? yes Ir(1) C(1) C(6) 124.8(7) ? ? ? yes C(2) C(1) C(5) 106.8(9) ? ? ? yes C(2) C(1) C(6) 124(1) ? ? ? yes C(5) C(1) C(6) 128(1) ? ? ? yes Ir(1) C(2) C(1) 69.5(5) ? ? ? yes Ir(1) C(2) C(3) 71.3(5) ? ? ? yes Ir(1) C(2) C(7) 128.3(7) ? ? ? yes C(1) C(2) C(3) 107.2(8) ? ? ? yes C(1) C(2) C(7) 126(1) ? ? ? yes C(3) C(2) C(7) 126(1) ? ? ? yes Ir(1) C(3) C(2) 70.2(5) ? ? ? yes Ir(1) C(3) C(4) 69.6(5) ? ? ? yes Ir(1) C(3) C(8) 127.0(7) ? ? ? yes C(2) C(3) C(4) 107.8(8) ? ? ? yes C(2) C(3) C(8) 126.0(9) ? ? ? yes C(4) C(3) C(8) 126.2(10) ? ? ? yes Ir(1) C(4) C(3) 71.6(5) ? ? ? yes Ir(1) C(4) C(5) 72.3(6) ? ? ? yes Ir(1) C(4) C(9) 128.8(7) ? ? ? yes C(3) C(4) C(5) 108.2(9) ? ? ? yes C(3) C(4) C(9) 124.6(10) ? ? ? yes C(5) C(4) C(9) 126.7(10) ? ? ? yes Ir(1) C(5) C(1) 69.5(5) ? ? ? yes Ir(1) C(5) C(4) 70.3(6) ? ? ? yes Ir(1) C(5) C(10) 125.3(7) ? ? ? yes C(1) C(5) C(4) 109.8(9) ? ? ? yes C(1) C(5) C(10) 123(1) ? ? ? yes C(4) C(5) C(10) 126(1) ? ? ? yes P(1) C(11) C(12) 118.8(6) ? ? ? yes P(1) C(11) C(16) 122.5(7) ? ? ? yes C(12) C(11) C(16) 118.6(8) ? ? ? yes C(11) C(12) C(13) 120.5(8) ? ? ? yes C(12) C(13) C(14) 120.6(9) ? ? ? yes C(13) C(14) C(15) 119.1(9) ? ? ? yes C(14) C(15) C(16) 121.0(9) ? ? ? yes C(11) C(16) C(15) 120.2(9) ? ? ? yes P(1) C(17) C(18) 120.2(5) ? ? ? yes P(1) C(17) C(18) 120.2(5) ? ? ? yes C(18) C(17) C(18) 118(1) ? ? ? yes C(17) C(18) C(19) 119.9(8) ? ? ? yes C(18) C(19) C(20) 121.4(9) ? ? ? yes C(19) C(20) C(19) 118(1) ? ? ? yes Cl(3) C(21) Cl(4) 103(1) ? ? ? yes #------------------------------------------------------------------------------ --============_-1363580662==_============ Content-Type: text/plain; charset="ISO-2022-JP" Zhen TANG 唐 振 Lab of Hidai Department of Chemistry and Biotechnology Graduate School of Engineering The University of Tokyo e-mail: tt37192@hongo.ecc.u-tokyo.ac.jp Tel: 03-3812-2111 ext. 7263 --============_-1363580662==_============--