# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2159 data_global _publ_section_title ; Synthesis of Diiridium Complexes with Two Bridging Tetrachalcogenide Li gands [{(eta5-C5Me5)Ir}2(mu-E4)2] (E = Se or S) and their Reactions with Alky nes Forming Mono- or Dinuclear Dichalcogenolene Complexes (B004404K) ; _publ_contact_author_name 'Yasushi Mizobe' _publ_contact_author_address ; Institute of Industrial Scienece, The University of Tokyo, Roppongi, Minato-ku, Tokyo 106-8558, Japan ; _publ_contact_author_email 'ymizobe@iis.u-tokyo.ac.jp' _publ_contact_author_fax '(+81) 3 (3402) 6303' _publ_requested_journal 'Dalton Transaction' _publ_requested_category 'Inorganic' #------------------------------------------------------------------------------ data_[Cp*Ir(Se4)2IrCp*]-toluene_(2-toluene) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Nov 18 16:19:22 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1378.72 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H38 Ir2 Se8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 8.519(4) _cell_length_b 14.081(3) _cell_length_c 14.262(6) _cell_angle_alpha 95.60(2) _cell_angle_beta 94.51(5) _cell_angle_gamma 91.88(3) _cell_volume 1695(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 10.9 _cell_measurement_theta_max 13.3 #------------------------------------------------------------------------------ _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 'black' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252.00 _exptl_absorpt_coefficient_mu 16.464 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -9.08 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -3 1 -1 -3 2 -1 -1 -1 _diffrn_reflns_number 8248 _reflns_number_total 7723 _reflns_number_gt 1658 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.189 _diffrn_reflns_av_sigmaI/netI 0.288 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01596 _diffrn_orient_matrix_UB_12 -0.06452 _diffrn_orient_matrix_UB_13 -0.03622 _diffrn_orient_matrix_UB_21 0.04705 _diffrn_orient_matrix_UB_22 -0.02987 _diffrn_orient_matrix_UB_23 0.05592 _diffrn_orient_matrix_UB_31 -0.10686 _diffrn_orient_matrix_UB_32 -0.00673 _diffrn_orient_matrix_UB_33 0.02363 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.2219(2) 0.4025(1) 0.1918(1) 0.0350(7) Uani 1.00 d . . . Ir(2) Ir 0.1760(2) 0.1172(1) 0.2467(1) 0.0343(7) Uani 1.00 d . . . Se(1) Se 0.3478(5) 0.2601(3) 0.2440(3) 0.035(2) Uani 1.00 d . . . Se(2) Se 0.5325(5) 0.2304(4) 0.1265(4) 0.055(2) Uani 1.00 d . . . Se(3) Se 0.3523(6) 0.2159(4) -0.0020(3) 0.064(2) Uani 1.00 d . . . Se(4) Se 0.2348(6) 0.3609(4) 0.0205(3) 0.057(2) Uani 1.00 d . . . Se(5) Se -0.0078(5) 0.1624(4) 0.1220(3) 0.048(2) Uani 1.00 d . . . Se(6) Se -0.0367(5) 0.3239(4) 0.1603(3) 0.046(2) Uani 1.00 d . . . Se(7) Se -0.1377(5) 0.3050(4) 0.3094(4) 0.056(2) Uani 1.00 d . . . Se(8) Se 0.0775(5) 0.2289(4) 0.3738(3) 0.045(2) Uani 1.00 d . . . C(1) C 0.242(5) 0.551(3) 0.173(3) 0.06(1) Uiso 1.00 d . . . C(2) C 0.412(5) 0.519(3) 0.207(3) 0.04(1) Uiso 1.00 d . . . C(3) C 0.376(6) 0.498(3) 0.291(3) 0.06(1) Uiso 1.00 d . . . C(4) C 0.224(5) 0.504(3) 0.320(3) 0.03(1) Uiso 1.00 d . . . C(5) C 0.151(5) 0.542(3) 0.240(3) 0.03(1) Uiso 1.00 d . . . C(6) C 0.225(6) 0.600(4) 0.077(4) 0.08(1) Uiso 1.00 d . . . C(7) C 0.540(6) 0.520(4) 0.150(4) 0.07(1) Uiso 1.00 d . . . C(8) C 0.502(5) 0.463(3) 0.363(3) 0.05(1) Uiso 1.00 d . . . C(9) C 0.160(5) 0.495(3) 0.411(3) 0.06(1) Uiso 1.00 d . . . C(10) C -0.028(5) 0.575(3) 0.233(3) 0.05(1) Uiso 1.00 d . . . C(11) C 0.125(5) -0.032(3) 0.211(3) 0.04(1) Uiso 1.00 d . . . C(12) C 0.103(5) -0.016(3) 0.301(3) 0.05(1) Uiso 1.00 d . . . C(13) C 0.259(5) 0.019(3) 0.349(3) 0.05(1) Uiso 1.00 d . . . C(14) C 0.358(5) 0.015(3) 0.268(3) 0.04(1) Uiso 1.00 d . . . C(15) C 0.259(6) -0.003(4) 0.185(4) 0.07(1) Uiso 1.00 d . . . C(16) C -0.008(6) -0.070(4) 0.133(4) 0.08(1) Uiso 1.00 d . . . C(17) C -0.034(5) -0.031(3) 0.358(3) 0.06(1) Uiso 1.00 d . . . C(18) C 0.299(5) 0.033(3) 0.454(3) 0.06(1) Uiso 1.00 d . . . C(19) C 0.529(5) 0.035(3) 0.286(3) 0.06(1) Uiso 1.00 d . . . C(20) C 0.335(6) -0.025(4) 0.091(4) 0.08(1) Uiso 1.00 d . . . C(21) C 0.608(5) 0.253(2) 0.551(3) 0.1977 Uiso 1.00 d . . . C(22) C 0.448(4) 0.266(3) 0.558(3) 0.1977 Uiso 1.00 d . . . C(23) C 0.383(5) 0.258(3) 0.644(4) 0.1977 Uiso 1.00 d . . . C(24) C 0.478(7) 0.237(3) 0.722(3) 0.1977 Uiso 1.00 d . . . C(25) C 0.638(7) 0.223(3) 0.715(3) 0.1977 Uiso 1.00 d . . . C(26) C 0.703(4) 0.231(3) 0.629(3) 0.1977 Uiso 1.00 d . . . C(27) C 0.680(8) 0.261(4) 0.456(3) 0.1977 Uiso 1.00 d . . . H(1) H 0.2921 0.6555 0.0817 0.0920 Uiso 1.00 calc . . . H(2) H 0.2533 0.5561 0.0261 0.0920 Uiso 1.00 calc . . . H(3) H 0.1187 0.6167 0.0639 0.0920 Uiso 1.00 calc . . . H(4) H 0.6302 0.4971 0.1829 0.0896 Uiso 1.00 calc . . . H(5) H 0.5142 0.4808 0.0928 0.0896 Uiso 1.00 calc . . . H(6) H 0.5625 0.5839 0.1364 0.0896 Uiso 1.00 calc . . . H(7) H 0.4555 0.4538 0.4202 0.0656 Uiso 1.00 calc . . . H(8) H 0.5406 0.4044 0.3376 0.0656 Uiso 1.00 calc . . . H(9) H 0.5862 0.5094 0.3757 0.0656 Uiso 1.00 calc . . . H(10) H 0.2049 0.5436 0.4569 0.0699 Uiso 1.00 calc . . . H(11) H 0.0486 0.4999 0.4048 0.0699 Uiso 1.00 calc . . . H(12) H 0.1837 0.4340 0.4319 0.0699 Uiso 1.00 calc . . . H(13) H -0.0287 0.6411 0.2255 0.0645 Uiso 1.00 calc . . . H(14) H -0.0845 0.5400 0.1795 0.0645 Uiso 1.00 calc . . . H(15) H -0.0752 0.5626 0.2885 0.0645 Uiso 1.00 calc . . . H(16) H -0.1025 -0.0825 0.1616 0.0997 Uiso 1.00 calc . . . H(17) H -0.0261 -0.0221 0.0907 0.0997 Uiso 1.00 calc . . . H(18) H 0.0234 -0.1261 0.0992 0.0997 Uiso 1.00 calc . . . H(19) H -0.0022 -0.0162 0.4229 0.0726 Uiso 1.00 calc . . . H(20) H -0.1154 0.0097 0.3395 0.0726 Uiso 1.00 calc . . . H(21) H -0.0713 -0.0955 0.3463 0.0726 Uiso 1.00 calc . . . H(22) H 0.2832 -0.0257 0.4798 0.0744 Uiso 1.00 calc . . . H(23) H 0.4057 0.0549 0.4666 0.0744 Uiso 1.00 calc . . . H(24) H 0.2324 0.0792 0.4813 0.0744 Uiso 1.00 calc . . . H(25) H 0.5735 -0.0105 0.3241 0.0679 Uiso 1.00 calc . . . H(26) H 0.5763 0.0318 0.2278 0.0679 Uiso 1.00 calc . . . H(27) H 0.5474 0.0974 0.3182 0.0679 Uiso 1.00 calc . . . H(28) H 0.4016 -0.0780 0.0962 0.1023 Uiso 1.00 calc . . . H(29) H 0.2556 -0.0406 0.0413 0.1023 Uiso 1.00 calc . . . H(30) H 0.3966 0.0290 0.0789 0.1023 Uiso 1.00 calc . . . H(31) H 0.383(6) 0.281(4) 0.505(4) 0.1977 Uiso 1.00 calc . . . H(32) H 0.274(5) 0.268(4) 0.649(6) 0.1977 Uiso 1.00 calc . . . H(33) H 0.434(9) 0.231(4) 0.781(4) 0.1977 Uiso 1.00 calc . . . H(34) H 0.703(9) 0.208(5) 0.769(4) 0.1977 Uiso 1.00 calc . . . H(35) H 0.812(4) 0.221(4) 0.624(5) 0.1977 Uiso 1.00 calc . . . H(36) H 0.7906 0.2508 0.4638 0.2368 Uiso 1.00 calc . . . H(37) H 0.6318 0.2145 0.4094 0.2368 Uiso 1.00 calc . . . H(38) H 0.6650 0.3230 0.4372 0.2368 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.020(1) 0.055(2) 0.031(1) 0.007(1) -0.0024(10) 0.013(1) Ir(2) 0.023(1) 0.046(2) 0.034(1) 0.004(1) -0.0010(9) 0.004(1) Se(1) 0.021(3) 0.049(3) 0.035(3) 0.007(2) -0.004(2) 0.006(3) Se(2) 0.022(3) 0.080(4) 0.065(4) 0.006(3) 0.015(3) 0.008(3) Se(3) 0.054(4) 0.095(5) 0.043(4) -0.001(3) 0.015(3) -0.009(3) Se(4) 0.047(3) 0.094(5) 0.031(3) 0.001(3) 0.000(3) 0.016(3) Se(5) 0.032(3) 0.072(4) 0.036(3) -0.004(3) -0.011(2) 0.005(3) Se(6) 0.020(3) 0.072(4) 0.049(3) 0.005(3) -0.004(2) 0.020(3) Se(7) 0.032(3) 0.079(4) 0.063(4) 0.017(3) 0.019(3) 0.019(3) Se(8) 0.044(3) 0.062(4) 0.032(3) 0.015(3) 0.006(2) 0.009(3) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. Toluene molecule was refined as rigid group. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00017|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 1658 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.543 _refine_ls_shift/su_max 0.0140 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -1.07 _refine_diff_density_max 1.51 #------------------------------------------------------------------------------ _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) Se(1) 2.456(5) 1_555 1_555 yes Ir(1) Se(4) 2.468(5) 1_555 1_555 yes Ir(1) Se(6) 2.423(5) 1_555 1_555 yes Ir(1) C(1) 2.14(5) 1_555 1_555 yes Ir(1) C(2) 2.25(4) 1_555 1_555 yes Ir(1) C(3) 2.18(4) 1_555 1_555 yes Ir(1) C(4) 2.20(4) 1_555 1_555 yes Ir(1) C(5) 2.13(4) 1_555 1_555 yes Ir(2) Se(1) 2.454(5) 1_555 1_555 yes Ir(2) Se(5) 2.423(5) 1_555 1_555 yes Ir(2) Se(8) 2.496(5) 1_555 1_555 yes Ir(2) C(11) 2.14(4) 1_555 1_555 yes Ir(2) C(12) 2.19(5) 1_555 1_555 yes Ir(2) C(13) 2.20(5) 1_555 1_555 yes Ir(2) C(14) 2.18(4) 1_555 1_555 yes Ir(2) C(15) 2.01(5) 1_555 1_555 yes Se(1) Se(2) 2.405(7) 1_555 1_555 yes Se(2) Se(3) 2.285(7) 1_555 1_555 yes Se(3) Se(4) 2.309(8) 1_555 1_555 yes Se(5) Se(6) 2.312(7) 1_555 1_555 yes Se(6) Se(7) 2.391(7) 1_555 1_555 yes Se(7) Se(8) 2.325(7) 1_555 1_555 yes C(1) C(2) 1.58(6) 1_555 1_555 yes C(1) C(5) 1.29(6) 1_555 1_555 yes C(1) C(6) 1.59(7) 1_555 1_555 yes C(2) C(3) 1.32(7) 1_555 1_555 yes C(2) C(7) 1.42(7) 1_555 1_555 yes C(3) C(4) 1.39(6) 1_555 1_555 yes C(3) C(8) 1.55(7) 1_555 1_555 yes C(4) C(5) 1.42(6) 1_555 1_555 yes C(4) C(9) 1.46(6) 1_555 1_555 yes C(5) C(10) 1.61(6) 1_555 1_555 yes C(11) C(12) 1.31(6) 1_555 1_555 yes C(11) C(15) 1.29(7) 1_555 1_555 yes C(11) C(16) 1.57(6) 1_555 1_555 yes C(12) C(13) 1.49(6) 1_555 1_555 yes C(12) C(17) 1.48(7) 1_555 1_555 yes C(13) C(14) 1.48(6) 1_555 1_555 yes C(13) C(18) 1.49(6) 1_555 1_555 yes C(14) C(15) 1.39(6) 1_555 1_555 yes C(14) C(19) 1.48(6) 1_555 1_555 yes C(15) C(20) 1.54(8) 1_555 1_555 yes C(21) C(22) 1.39(6) 1_555 1_555 yes C(21) C(26) 1.39(6) 1_555 1_555 yes C(21) C(27) 1.54(7) 1_555 1_555 yes C(22) C(23) 1.39(8) 1_555 1_555 yes C(23) C(24) 1.39(7) 1_555 1_555 yes C(24) C(25) 1.39(8) 1_555 1_555 yes C(25) C(26) 1.39(7) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Ir(1) Se(4) 97.0(2) 1_555 1_555 1_555 yes Se(1) Ir(1) Se(6) 94.1(2) 1_555 1_555 1_555 yes Se(1) Ir(1) C(1) 148(1) 1_555 1_555 1_555 yes Se(1) Ir(1) C(2) 106(1) 1_555 1_555 1_555 yes Se(1) Ir(1) C(3) 92(1) 1_555 1_555 1_555 yes Se(1) Ir(1) C(4) 105(1) 1_555 1_555 1_555 yes Se(1) Ir(1) C(5) 143(1) 1_555 1_555 1_555 yes Se(4) Ir(1) Se(6) 82.7(2) 1_555 1_555 1_555 yes Se(4) Ir(1) C(1) 90(1) 1_555 1_555 1_555 yes Se(4) Ir(1) C(2) 96(1) 1_555 1_555 1_555 yes Se(4) Ir(1) C(3) 129(1) 1_555 1_555 1_555 yes Se(4) Ir(1) C(4) 153(1) 1_555 1_555 1_555 yes Se(4) Ir(1) C(5) 118(1) 1_555 1_555 1_555 yes Se(6) Ir(1) C(1) 117(1) 1_555 1_555 1_555 yes Se(6) Ir(1) C(2) 159(1) 1_555 1_555 1_555 yes Se(6) Ir(1) C(3) 145(1) 1_555 1_555 1_555 yes Se(6) Ir(1) C(4) 109(1) 1_555 1_555 1_555 yes Se(6) Ir(1) C(5) 98(1) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 42(1) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 60(1) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 63(1) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 35(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 34(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 64(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 64(1) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 37(1) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 59(1) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38(1) 1_555 1_555 1_555 yes Se(1) Ir(2) Se(5) 93.1(2) 1_555 1_555 1_555 yes Se(1) Ir(2) Se(8) 77.9(2) 1_555 1_555 1_555 yes Se(1) Ir(2) C(11) 150(1) 1_555 1_555 1_555 yes Se(1) Ir(2) C(12) 154(1) 1_555 1_555 1_555 yes Se(1) Ir(2) C(13) 114(1) 1_555 1_555 1_555 yes Se(1) Ir(2) C(14) 98(1) 1_555 1_555 1_555 yes Se(1) Ir(2) C(15) 114(1) 1_555 1_555 1_555 yes Se(5) Ir(2) Se(8) 95.2(2) 1_555 1_555 1_555 yes Se(5) Ir(2) C(11) 93(1) 1_555 1_555 1_555 yes Se(5) Ir(2) C(12) 112(1) 1_555 1_555 1_555 yes Se(5) Ir(2) C(13) 152(1) 1_555 1_555 1_555 yes Se(5) Ir(2) C(14) 139(1) 1_555 1_555 1_555 yes Se(5) Ir(2) C(15) 101(1) 1_555 1_555 1_555 yes Se(8) Ir(2) C(11) 129(1) 1_555 1_555 1_555 yes Se(8) Ir(2) C(12) 97(1) 1_555 1_555 1_555 yes Se(8) Ir(2) C(13) 91(1) 1_555 1_555 1_555 yes Se(8) Ir(2) C(14) 125(1) 1_555 1_555 1_555 yes Se(8) Ir(2) C(15) 158(1) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 35(1) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 62(1) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 59(1) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 36(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 39(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 63(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 63(1) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 39(1) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 67(1) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38(1) 1_555 1_555 1_555 yes Ir(1) Se(1) Ir(2) 116.7(2) 1_555 1_555 1_555 yes Ir(1) Se(1) Se(2) 101.2(2) 1_555 1_555 1_555 yes Ir(2) Se(1) Se(2) 109.5(2) 1_555 1_555 1_555 yes Se(1) Se(2) Se(3) 96.8(2) 1_555 1_555 1_555 yes Se(2) Se(3) Se(4) 99.7(3) 1_555 1_555 1_555 yes Ir(1) Se(4) Se(3) 108.5(2) 1_555 1_555 1_555 yes Ir(2) Se(5) Se(6) 104.2(2) 1_555 1_555 1_555 yes Ir(1) Se(6) Se(5) 109.0(2) 1_555 1_555 1_555 yes Ir(1) Se(6) Se(7) 107.5(2) 1_555 1_555 1_555 yes Se(5) Se(6) Se(7) 94.7(3) 1_555 1_555 1_555 yes Se(6) Se(7) Se(8) 96.7(2) 1_555 1_555 1_555 yes Ir(2) Se(8) Se(7) 108.4(2) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 72(2) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 72(2) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 128(3) 1_555 1_555 1_555 yes C(2) C(1) C(5) 107(3) 1_555 1_555 1_555 yes C(2) C(1) C(6) 117(3) 1_555 1_555 1_555 yes C(5) C(1) C(6) 134(4) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 65(2) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 69(2) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 123(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 96(3) 1_555 1_555 1_555 yes C(1) C(2) C(7) 122(4) 1_555 1_555 1_555 yes C(3) C(2) C(7) 140(4) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 75(2) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 72(2) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 123(3) 1_555 1_555 1_555 yes C(2) C(3) C(4) 122(4) 1_555 1_555 1_555 yes C(2) C(3) C(8) 121(4) 1_555 1_555 1_555 yes C(4) C(3) C(8) 115(4) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 70(2) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 68(2) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 131(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 98(3) 1_555 1_555 1_555 yes C(3) C(4) C(9) 132(3) 1_555 1_555 1_555 yes C(5) C(4) C(9) 127(3) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 72(2) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 73(2) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 124(2) 1_555 1_555 1_555 yes C(1) C(5) C(4) 114(3) 1_555 1_555 1_555 yes C(1) C(5) C(10) 121(3) 1_555 1_555 1_555 yes C(4) C(5) C(10) 123(3) 1_555 1_555 1_555 yes C(1) C(6) H(1) 109(4) 1_555 1_555 1_555 no C(1) C(6) H(2) 109(4) 1_555 1_555 1_555 no C(1) C(6) H(3) 109(4) 1_555 1_555 1_555 no H(1) C(6) H(2) 109(5) 1_555 1_555 1_555 no H(1) C(6) H(3) 109(5) 1_555 1_555 1_555 no H(2) C(6) H(3) 109(4) 1_555 1_555 1_555 no C(2) C(7) H(4) 109(4) 1_555 1_555 1_555 no C(2) C(7) H(5) 109(4) 1_555 1_555 1_555 no C(2) C(7) H(6) 109(4) 1_555 1_555 1_555 no H(4) C(7) H(5) 109(5) 1_555 1_555 1_555 no H(4) C(7) H(6) 109(4) 1_555 1_555 1_555 no H(5) C(7) H(6) 109(5) 1_555 1_555 1_555 no C(3) C(8) H(7) 109(4) 1_555 1_555 1_555 no C(3) C(8) H(8) 109(3) 1_555 1_555 1_555 no C(3) C(8) H(9) 109(4) 1_555 1_555 1_555 no H(7) C(8) H(8) 109(4) 1_555 1_555 1_555 no H(7) C(8) H(9) 109(4) 1_555 1_555 1_555 no H(8) C(8) H(9) 109(4) 1_555 1_555 1_555 no C(4) C(9) H(10) 109(4) 1_555 1_555 1_555 no C(4) C(9) H(11) 109(4) 1_555 1_555 1_555 no C(4) C(9) H(12) 109(4) 1_555 1_555 1_555 no H(10) C(9) H(11) 109(4) 1_555 1_555 1_555 no H(10) C(9) H(12) 109(4) 1_555 1_555 1_555 no H(11) C(9) H(12) 109(4) 1_555 1_555 1_555 no C(5) C(10) H(13) 109(3) 1_555 1_555 1_555 no C(5) C(10) H(14) 109(3) 1_555 1_555 1_555 no C(5) C(10) H(15) 109(3) 1_555 1_555 1_555 no H(13) C(10) H(14) 109(4) 1_555 1_555 1_555 no H(13) C(10) H(15) 109(4) 1_555 1_555 1_555 no H(14) C(10) H(15) 109(4) 1_555 1_555 1_555 no Ir(2) C(11) C(12) 74(2) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 66(2) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 121(3) 1_555 1_555 1_555 yes C(12) C(11) C(15) 117(4) 1_555 1_555 1_555 yes C(12) C(11) C(16) 123(4) 1_555 1_555 1_555 yes C(15) C(11) C(16) 118(4) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 70(2) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 70(2) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 126(3) 1_555 1_555 1_555 yes C(11) C(12) C(13) 105(3) 1_555 1_555 1_555 yes C(11) C(12) C(17) 133(4) 1_555 1_555 1_555 yes C(13) C(12) C(17) 120(3) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 69(2) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 69(2) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 132(3) 1_555 1_555 1_555 yes C(12) C(13) C(14) 101(3) 1_555 1_555 1_555 yes C(12) C(13) C(18) 125(4) 1_555 1_555 1_555 yes C(14) C(13) C(18) 132(3) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 71(2) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 64(2) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 127(3) 1_555 1_555 1_555 yes C(13) C(14) C(15) 108(3) 1_555 1_555 1_555 yes C(13) C(14) C(19) 118(3) 1_555 1_555 1_555 yes C(15) C(14) C(19) 133(4) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 77(3) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 77(2) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 132(3) 1_555 1_555 1_555 yes C(11) C(15) C(14) 105(4) 1_555 1_555 1_555 yes C(11) C(15) C(20) 130(4) 1_555 1_555 1_555 yes C(14) C(15) C(20) 117(4) 1_555 1_555 1_555 yes C(11) C(16) H(16) 109(4) 1_555 1_555 1_555 no C(11) C(16) H(17) 109(4) 1_555 1_555 1_555 no C(11) C(16) H(18) 109(4) 1_555 1_555 1_555 no H(16) C(16) H(17) 109(5) 1_555 1_555 1_555 no H(16) C(16) H(18) 109(5) 1_555 1_555 1_555 no H(17) C(16) H(18) 109(5) 1_555 1_555 1_555 no C(12) C(17) H(19) 109(4) 1_555 1_555 1_555 no C(12) C(17) H(20) 109(4) 1_555 1_555 1_555 no C(12) C(17) H(21) 109(4) 1_555 1_555 1_555 no H(19) C(17) H(20) 109(4) 1_555 1_555 1_555 no H(19) C(17) H(21) 109(4) 1_555 1_555 1_555 no H(20) C(17) H(21) 109(4) 1_555 1_555 1_555 no C(13) C(18) H(22) 109(4) 1_555 1_555 1_555 no C(13) C(18) H(23) 109(4) 1_555 1_555 1_555 no C(13) C(18) H(24) 109(4) 1_555 1_555 1_555 no H(22) C(18) H(23) 109(4) 1_555 1_555 1_555 no H(22) C(18) H(24) 109(4) 1_555 1_555 1_555 no H(23) C(18) H(24) 109(4) 1_555 1_555 1_555 no C(14) C(19) H(25) 109(4) 1_555 1_555 1_555 no C(14) C(19) H(26) 109(3) 1_555 1_555 1_555 no C(14) C(19) H(27) 109(4) 1_555 1_555 1_555 no H(25) C(19) H(26) 109(4) 1_555 1_555 1_555 no H(25) C(19) H(27) 109(4) 1_555 1_555 1_555 no H(26) C(19) H(27) 109(4) 1_555 1_555 1_555 no C(15) C(20) H(28) 109(4) 1_555 1_555 1_555 no C(15) C(20) H(29) 109(4) 1_555 1_555 1_555 no C(15) C(20) H(30) 109(4) 1_555 1_555 1_555 no H(28) C(20) H(29) 109(5) 1_555 1_555 1_555 no H(28) C(20) H(30) 109(5) 1_555 1_555 1_555 no H(29) C(20) H(30) 109(5) 1_555 1_555 1_555 no C(22) C(21) C(26) 120(3) 1_555 1_555 1_555 yes C(22) C(21) C(27) 119(4) 1_555 1_555 1_555 yes C(26) C(21) C(27) 120(4) 1_555 1_555 1_555 yes C(21) C(22) C(23) 119(3) 1_555 1_555 1_555 yes C(21) C(22) H(31) 120(5) 1_555 1_555 1_555 no C(23) C(22) H(31) 119(5) 1_555 1_555 1_555 no C(22) C(23) C(24) 119(4) 1_555 1_555 1_555 yes C(22) C(23) H(32) 120(7) 1_555 1_555 1_555 no C(24) C(23) H(32) 120(7) 1_555 1_555 1_555 no C(23) C(24) C(25) 119(4) 1_555 1_555 1_555 yes C(23) C(24) H(33) 119(7) 1_555 1_555 1_555 no C(25) C(24) H(33) 120(6) 1_555 1_555 1_555 no C(24) C(25) C(26) 120(4) 1_555 1_555 1_555 yes C(24) C(25) H(34) 120(6) 1_555 1_555 1_555 no C(26) C(25) H(34) 119(6) 1_555 1_555 1_555 no C(21) C(26) C(25) 119(3) 1_555 1_555 1_555 yes C(21) C(26) H(35) 120(6) 1_555 1_555 1_555 no C(25) C(26) H(35) 120(6) 1_555 1_555 1_555 no C(21) C(27) H(36) 109(4) 1_555 1_555 1_555 no C(21) C(27) H(37) 109(5) 1_555 1_555 1_555 no C(21) C(27) H(38) 109(4) 1_555 1_555 1_555 no H(36) C(27) H(37) 108(5) 1_555 1_555 1_555 no H(36) C(27) H(38) 109(6) 1_555 1_555 1_555 no H(37) C(27) H(38) 110(5) 1_555 1_555 1_555 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 Ir(1) Ir(2) 4.179(3) 1_555 1_555 ? Se(7) C(27) 2.81(6) 1_555 1_455 ? C(1) C(25) 3.50(6) 1_555 2_666 ? C(2) C(24) 3.56(6) 1_555 2_666 ? C(8) C(27) 3.58(8) 1_555 1_555 ? C(11) C(25) 3.60(7) 1_555 2_656 ? C(13) C(26) 3.58(6) 1_555 2_656 ? C(13) C(25) 3.59(6) 1_555 2_656 ? C(14) C(25) 3.38(6) 1_555 2_656 ? #------------------------------------------------------------------------------ #===END data_[(Cp*Ir)2(Se4){Se2C2(COOMe)2}]_(6) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jun 2 15:19:34 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1270.77 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H36 Ir2 O4 Se6 ' _chemical_formula_moiety 'C26 H36 Ir2 O4 Se6 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.523(1) _cell_length_b 11.119(1) _cell_length_c 17.255(3) _cell_angle_alpha 100.92(1) _cell_angle_beta 94.12(1) _cell_angle_gamma 113.82(1) _cell_volume 1618.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.7 _cell_measurement_theta_max 19.9 #------------------------------------------------------------------------------ _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 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 2.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164.00 _exptl_absorpt_coefficient_mu 15.014 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.33 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -3 1 -3 -1 0 -2 -2 _diffrn_reflns_number 7882 _reflns_number_total 7432 _reflns_number_gt 4828 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05453 _diffrn_orient_matrix_UB_12 -0.09138 _diffrn_orient_matrix_UB_13 0.01106 _diffrn_orient_matrix_UB_21 -0.09572 _diffrn_orient_matrix_UB_22 -0.01630 _diffrn_orient_matrix_UB_23 -0.03643 _diffrn_orient_matrix_UB_31 0.03754 _diffrn_orient_matrix_UB_32 -0.04046 _diffrn_orient_matrix_UB_33 -0.04617 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir -0.13699(7) 0.09273(5) 0.26404(3) 0.0339(2) Uani 1.00 d . . . Ir(2) Ir 0.12603(6) 0.46171(5) 0.29235(3) 0.0290(1) Uani 1.00 d . . . Se(1) Se -0.0442(2) 0.3064(1) 0.36779(9) 0.0349(4) Uani 1.00 d . . . Se(2) Se 0.1158(2) 0.2899(2) 0.4773(1) 0.0599(5) Uani 1.00 d . . . Se(3) Se 0.1194(2) 0.0806(2) 0.4273(1) 0.0630(6) Uani 1.00 d . . . Se(4) Se 0.1123(2) 0.0769(2) 0.2920(1) 0.0506(5) Uani 1.00 d . . . Se(5) Se 0.0293(2) 0.2509(1) 0.18707(8) 0.0329(4) Uani 1.00 d . . . Se(6) Se -0.1178(2) 0.4762(2) 0.24625(9) 0.0429(5) Uani 1.00 d . . . O(1) O -0.100(2) 0.110(1) 0.0151(6) 0.070(4) Uani 1.00 d . . . O(2) O -0.220(1) 0.229(1) -0.0224(6) 0.056(4) Uani 1.00 d . . . O(3) O -0.259(2) 0.477(2) 0.0548(10) 0.084(6) Uani 1.00 d . . . O(4) O -0.432(2) 0.305(2) 0.0860(8) 0.083(5) Uani 1.00 d . . . C(1) C -0.110(2) 0.283(1) 0.1122(8) 0.036(4) Uani 1.00 d . . . C(2) C -0.171(2) 0.369(2) 0.1400(9) 0.041(4) Uani 1.00 d . . . C(3) C -0.150(2) 0.209(2) 0.0304(9) 0.044(5) Uani 1.00 d . . . C(4) C -0.146(3) 0.026(2) -0.067(1) 0.093(9) Uani 1.00 d . . . C(5) C -0.297(2) 0.380(2) 0.092(1) 0.059(6) Uani 1.00 d . . . C(6a) C -0.119(5) 0.544(3) 0.044(2) 0.08(1) Uani 0.60 d P . . C(6b) C -0.358(10) 0.501(7) 0.006(3) 0.15(3) Uani 0.40 d P . . C(7) C -0.389(2) 0.033(2) 0.258(1) 0.053(5) Uani 1.00 d . . . C(8) C -0.337(2) -0.025(1) 0.3155(10) 0.043(4) Uani 1.00 d . . . C(9) C -0.281(2) -0.118(1) 0.2720(10) 0.048(5) Uani 1.00 d . . . C(10) C -0.293(2) -0.112(2) 0.1913(10) 0.067(6) Uani 1.00 d . . . C(11) C -0.363(2) -0.021(2) 0.1819(10) 0.055(5) Uani 1.00 d . . . C(12) C -0.467(2) 0.127(2) 0.278(2) 0.101(9) Uani 1.00 d . . . C(13) C -0.350(2) 0.001(2) 0.404(1) 0.076(6) Uani 1.00 d . . . C(14) C -0.228(2) -0.204(2) 0.312(1) 0.073(7) Uani 1.00 d . . . C(15) C -0.261(3) -0.199(2) 0.126(1) 0.111(9) Uani 1.00 d . . . C(16) C -0.419(3) -0.003(2) 0.106(1) 0.106(8) Uani 1.00 d . . . C(17) C 0.358(2) 0.543(2) 0.260(1) 0.050(5) Uani 1.00 d . . . C(18) C 0.290(2) 0.638(2) 0.257(1) 0.068(6) Uani 1.00 d . . . C(19) C 0.262(2) 0.684(1) 0.3361(9) 0.034(4) Uani 1.00 d . . . C(20) C 0.319(1) 0.617(1) 0.3859(7) 0.028(3) Uani 1.00 d . . . C(21) C 0.374(2) 0.531(1) 0.3400(9) 0.036(4) Uani 1.00 d . . . C(22) C 0.412(2) 0.480(2) 0.192(1) 0.077(7) Uani 1.00 d . . . C(23) C 0.261(2) 0.693(2) 0.187(1) 0.081(7) Uani 1.00 d . . . C(24) C 0.202(2) 0.786(2) 0.360(1) 0.066(6) Uani 1.00 d . . . C(25) C 0.326(2) 0.644(2) 0.475(1) 0.058(5) Uani 1.00 d . . . C(26) C 0.457(2) 0.456(2) 0.371(1) 0.069(7) Uani 1.00 d . . . H(1) H -0.2559 -0.0189 -0.0796 0.1122 Uiso 1.00 calc . . . H(2) H -0.1059 0.0807 -0.1031 0.1122 Uiso 1.00 calc . . . H(3) H -0.1048 -0.0400 -0.0708 0.1122 Uiso 1.00 calc . . . H(4a) H -0.0490 0.5286 0.0782 0.1009 Uiso 0.60 calc . . . H(4b) H -0.3322 0.5948 0.0175 0.1773 Uiso 0.40 calc . . . H(5a) H -0.1107 0.5142 -0.0103 0.1009 Uiso 0.60 calc . . . H(5b) H -0.3510 0.4703 -0.0482 0.1773 Uiso 0.40 calc . . . H(6a) H -0.0952 0.6376 0.0552 0.1009 Uiso 0.60 calc . . . H(6b) H -0.4618 0.4528 0.0147 0.1773 Uiso 0.40 calc . . . H(7) H -0.4004 0.2046 0.3189 0.1210 Uiso 1.00 calc . . . H(8) H -0.4877 0.1556 0.2314 0.1210 Uiso 1.00 calc . . . H(9) H -0.5621 0.0813 0.2959 0.1210 Uiso 1.00 calc . . . H(10) H -0.3102 -0.0509 0.4288 0.0918 Uiso 1.00 calc . . . H(11) H -0.2913 0.0943 0.4285 0.0918 Uiso 1.00 calc . . . H(12) H -0.4558 -0.0251 0.4095 0.0918 Uiso 1.00 calc . . . H(13) H -0.3126 -0.2641 0.3321 0.0874 Uiso 1.00 calc . . . H(14) H -0.1921 -0.2549 0.2749 0.0874 Uiso 1.00 calc . . . H(15) H -0.1459 -0.1478 0.3555 0.0874 Uiso 1.00 calc . . . H(16) H -0.3254 -0.2917 0.1241 0.1331 Uiso 1.00 calc . . . H(17) H -0.2832 -0.1800 0.0766 0.1331 Uiso 1.00 calc . . . H(18) H -0.1550 -0.1833 0.1358 0.1331 Uiso 1.00 calc . . . H(19) H -0.4565 0.0649 0.1163 0.1273 Uiso 1.00 calc . . . H(20) H -0.3367 0.0235 0.0763 0.1273 Uiso 1.00 calc . . . H(21) H -0.5014 -0.0860 0.0768 0.1273 Uiso 1.00 calc . . . H(22) H 0.3599 0.3840 0.1822 0.0928 Uiso 1.00 calc . . . H(23) H 0.3886 0.5070 0.1452 0.0928 Uiso 1.00 calc . . . H(24) H 0.5208 0.5081 0.2038 0.0928 Uiso 1.00 calc . . . H(25) H 0.3214 0.7888 0.1995 0.0975 Uiso 1.00 calc . . . H(26) H 0.2912 0.6531 0.1411 0.0975 Uiso 1.00 calc . . . H(27) H 0.1542 0.6734 0.1756 0.0975 Uiso 1.00 calc . . . H(28) H 0.2708 0.8699 0.3517 0.0787 Uiso 1.00 calc . . . H(29) H 0.1020 0.7570 0.3297 0.0787 Uiso 1.00 calc . . . H(30) H 0.1932 0.7959 0.4156 0.0787 Uiso 1.00 calc . . . H(31) H 0.3685 0.5900 0.4956 0.0699 Uiso 1.00 calc . . . H(32) H 0.3894 0.7366 0.4984 0.0699 Uiso 1.00 calc . . . H(33) H 0.2237 0.6206 0.4871 0.0699 Uiso 1.00 calc . . . H(34) H 0.4496 0.4601 0.4261 0.0831 Uiso 1.00 calc . . . H(35) H 0.4105 0.3643 0.3417 0.0831 Uiso 1.00 calc . . . H(36) H 0.5634 0.4966 0.3653 0.0831 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0386(3) 0.0257(3) 0.0338(3) 0.0107(2) -0.0017(2) 0.0078(2) Ir(2) 0.0336(3) 0.0263(3) 0.0260(3) 0.0119(2) 0.0023(2) 0.0065(2) Se(1) 0.0370(8) 0.0327(7) 0.0307(8) 0.0104(6) 0.0074(6) 0.0069(6) Se(2) 0.077(1) 0.055(1) 0.0322(9) 0.0143(9) -0.0083(8) 0.0145(8) Se(3) 0.080(1) 0.065(1) 0.052(1) 0.034(1) -0.0022(10) 0.0297(9) Se(4) 0.057(1) 0.058(1) 0.053(1) 0.0362(9) 0.0105(8) 0.0227(8) Se(5) 0.0437(8) 0.0312(7) 0.0256(7) 0.0182(6) 0.0033(6) 0.0063(6) Se(6) 0.0467(9) 0.0425(8) 0.0416(9) 0.0252(7) -0.0013(7) 0.0034(7) O(1) 0.12(1) 0.076(9) 0.025(6) 0.058(8) -0.009(6) -0.005(6) O(2) 0.074(8) 0.055(7) 0.033(6) 0.027(6) -0.007(6) 0.008(5) O(3) 0.10(1) 0.08(1) 0.09(1) 0.052(10) 0.021(10) 0.034(9) O(4) 0.057(9) 0.11(1) 0.07(1) 0.038(8) -0.007(7) -0.002(8) C(1) 0.042(8) 0.032(7) 0.023(7) 0.011(6) -0.011(6) -0.001(6) C(2) 0.040(9) 0.046(9) 0.038(9) 0.019(7) -0.004(7) 0.012(7) C(3) 0.048(10) 0.046(9) 0.035(9) 0.015(8) 0.003(7) 0.016(7) C(4) 0.15(2) 0.11(2) 0.04(1) 0.10(2) -0.01(1) -0.01(1) C(5) 0.08(1) 0.05(1) 0.06(1) 0.03(1) 0.01(1) 0.007(9) C(6a) 0.12(3) 0.06(2) 0.08(3) 0.04(2) -0.02(2) 0.04(2) C(6b) 0.3(1) 0.16(6) 0.03(3) 0.18(7) -0.06(4) -0.02(3) C(7) 0.036(9) 0.038(9) 0.08(1) 0.007(7) -0.014(8) 0.028(9) C(8) 0.025(7) 0.042(9) 0.05(1) 0.000(6) -0.003(7) 0.022(7) C(9) 0.07(1) 0.024(7) 0.044(10) 0.010(7) 0.008(8) 0.006(7) C(10) 0.10(2) 0.025(8) 0.032(10) -0.006(9) 0.013(9) -0.010(7) C(11) 0.07(1) 0.040(9) 0.031(9) 0.000(8) -0.006(8) 0.003(7) C(12) 0.05(1) 0.08(2) 0.17(3) 0.02(1) 0.00(1) 0.07(2) C(13) 0.05(1) 0.07(1) 0.08(1) -0.010(10) 0.02(1) 0.02(1) C(14) 0.07(1) 0.040(10) 0.12(2) 0.024(9) 0.02(1) 0.04(1) C(15) 0.16(3) 0.06(1) 0.09(2) 0.02(1) 0.04(2) -0.01(1) C(16) 0.10(2) 0.08(2) 0.08(2) -0.02(1) -0.04(1) 0.03(1) C(17) 0.046(10) 0.036(9) 0.06(1) 0.011(7) 0.007(8) 0.008(8) C(18) 0.06(1) 0.036(9) 0.07(1) -0.016(9) 0.01(1) 0.026(9) C(19) 0.028(7) 0.022(7) 0.048(9) 0.007(6) 0.005(6) 0.005(6) C(20) 0.026(7) 0.030(7) 0.019(7) 0.003(6) -0.007(5) 0.006(5) C(21) 0.028(7) 0.034(8) 0.042(9) 0.010(6) 0.004(6) 0.007(6) C(22) 0.07(1) 0.08(1) 0.07(1) 0.02(1) 0.04(1) 0.01(1) C(23) 0.10(2) 0.07(1) 0.06(1) 0.01(1) -0.02(1) 0.04(1) C(24) 0.06(1) 0.031(9) 0.10(2) 0.018(8) -0.01(1) 0.001(9) C(25) 0.07(1) 0.05(1) 0.05(1) 0.020(9) -0.006(9) 0.007(8) C(26) 0.05(1) 0.07(1) 0.10(2) 0.028(10) 0.01(1) 0.03(1) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00014|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0000(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4828 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.024 _refine_ls_shift/su_max 0.0320 _refine_ls_shift/su_mean 0.0030 _refine_diff_density_min -4.38 _refine_diff_density_max 3.29 #------------------------------------------------------------------------------ _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) Se(1) 2.469(1) 1_555 1_555 yes Ir(1) Se(4) 2.471(2) 1_555 1_555 yes Ir(1) Se(5) 2.510(2) 1_555 1_555 yes Ir(1) C(7) 2.20(2) 1_555 1_555 yes Ir(1) C(8) 2.19(1) 1_555 1_555 yes Ir(1) C(9) 2.22(1) 1_555 1_555 yes Ir(1) C(10) 2.21(1) 1_555 1_555 yes Ir(1) C(11) 2.22(2) 1_555 1_555 yes Ir(2) Se(1) 2.490(2) 1_555 1_555 yes Ir(2) Se(5) 2.458(1) 1_555 1_555 yes Ir(2) Se(6) 2.477(2) 1_555 1_555 yes Ir(2) C(17) 2.18(2) 1_555 1_555 yes Ir(2) C(18) 2.19(2) 1_555 1_555 yes Ir(2) C(19) 2.22(1) 1_555 1_555 yes Ir(2) C(20) 2.22(1) 1_555 1_555 yes Ir(2) C(21) 2.20(1) 1_555 1_555 yes Se(1) Se(2) 2.423(3) 1_555 1_555 yes Se(2) Se(3) 2.339(3) 1_555 1_555 yes Se(3) Se(4) 2.323(3) 1_555 1_555 yes Se(5) C(1) 1.96(2) 1_555 1_555 yes Se(6) C(2) 1.90(1) 1_555 1_555 yes O(1) C(3) 1.36(3) 1_555 1_555 yes O(1) C(4) 1.47(2) 1_555 1_555 yes O(2) C(3) 1.20(2) 1_555 1_555 yes O(3) C(5) 1.31(3) 1_555 1_555 yes O(3) C(6a) 1.28(4) 1_555 1_555 yes O(3) C(6b) 1.36(9) 1_555 1_555 yes O(4) C(5) 1.20(2) 1_555 1_555 yes C(1) C(2) 1.34(3) 1_555 1_555 yes C(1) C(3) 1.43(2) 1_555 1_555 yes C(2) C(5) 1.46(3) 1_555 1_555 yes C(7) C(8) 1.44(3) 1_555 1_555 yes C(7) C(11) 1.42(3) 1_555 1_555 yes C(7) C(12) 1.52(3) 1_555 1_555 yes C(8) C(9) 1.46(3) 1_555 1_555 yes C(8) C(13) 1.52(3) 1_555 1_555 yes C(9) C(10) 1.41(2) 1_555 1_555 yes C(9) C(14) 1.50(3) 1_555 1_555 yes C(10) C(11) 1.44(3) 1_555 1_555 yes C(10) C(15) 1.47(3) 1_555 1_555 yes C(11) C(16) 1.45(3) 1_555 1_555 yes C(17) C(18) 1.46(3) 1_555 1_555 yes C(17) C(21) 1.41(2) 1_555 1_555 yes C(17) C(22) 1.49(3) 1_555 1_555 yes C(18) C(19) 1.45(3) 1_555 1_555 yes C(18) C(23) 1.51(3) 1_555 1_555 yes C(19) C(20) 1.44(2) 1_555 1_555 yes C(19) C(24) 1.47(3) 1_555 1_555 yes C(20) C(21) 1.41(2) 1_555 1_555 yes C(20) C(25) 1.50(2) 1_555 1_555 yes C(21) C(26) 1.50(3) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Ir(1) Se(4) 91.56(6) 1_555 1_555 1_555 yes Se(1) Ir(1) Se(5) 81.32(5) 1_555 1_555 1_555 yes Se(1) Ir(1) C(7) 97.9(4) 1_555 1_555 1_555 yes Se(1) Ir(1) C(8) 97.1(4) 1_555 1_555 1_555 yes Se(1) Ir(1) C(9) 129.4(4) 1_555 1_555 1_555 yes Se(1) Ir(1) C(10) 159.9(6) 1_555 1_555 1_555 yes Se(1) Ir(1) C(11) 129.6(5) 1_555 1_555 1_555 yes Se(4) Ir(1) Se(5) 78.82(6) 1_555 1_555 1_555 yes Se(4) Ir(1) C(7) 156.8(5) 1_555 1_555 1_555 yes Se(4) Ir(1) C(8) 119.7(5) 1_555 1_555 1_555 yes Se(4) Ir(1) C(9) 94.0(5) 1_555 1_555 1_555 yes Se(4) Ir(1) C(10) 103.0(6) 1_555 1_555 1_555 yes Se(4) Ir(1) C(11) 138.8(5) 1_555 1_555 1_555 yes Se(5) Ir(1) C(7) 123.5(5) 1_555 1_555 1_555 yes Se(5) Ir(1) C(8) 161.4(5) 1_555 1_555 1_555 yes Se(5) Ir(1) C(9) 149.0(4) 1_555 1_555 1_555 yes Se(5) Ir(1) C(10) 114.8(5) 1_555 1_555 1_555 yes Se(5) Ir(1) C(11) 103.5(5) 1_555 1_555 1_555 yes C(7) Ir(1) C(8) 38.2(7) 1_555 1_555 1_555 yes C(7) Ir(1) C(9) 63.7(7) 1_555 1_555 1_555 yes C(7) Ir(1) C(10) 63.6(7) 1_555 1_555 1_555 yes C(7) Ir(1) C(11) 37.6(7) 1_555 1_555 1_555 yes C(8) Ir(1) C(9) 38.7(7) 1_555 1_555 1_555 yes C(8) Ir(1) C(10) 63.7(6) 1_555 1_555 1_555 yes C(8) Ir(1) C(11) 63.2(6) 1_555 1_555 1_555 yes C(9) Ir(1) C(10) 37.0(6) 1_555 1_555 1_555 yes C(9) Ir(1) C(11) 62.6(7) 1_555 1_555 1_555 yes C(10) Ir(1) C(11) 38.0(8) 1_555 1_555 1_555 yes Se(1) Ir(2) Se(5) 81.95(5) 1_555 1_555 1_555 yes Se(1) Ir(2) Se(6) 82.91(6) 1_555 1_555 1_555 yes Se(1) Ir(2) C(17) 144.2(5) 1_555 1_555 1_555 yes Se(1) Ir(2) C(18) 164.5(5) 1_555 1_555 1_555 yes Se(1) Ir(2) C(19) 126.1(4) 1_555 1_555 1_555 yes Se(1) Ir(2) C(20) 104.0(3) 1_555 1_555 1_555 yes Se(1) Ir(2) C(21) 111.2(4) 1_555 1_555 1_555 yes Se(5) Ir(2) Se(6) 86.09(6) 1_555 1_555 1_555 yes Se(5) Ir(2) C(17) 94.4(4) 1_555 1_555 1_555 yes Se(5) Ir(2) C(18) 113.5(5) 1_555 1_555 1_555 yes Se(5) Ir(2) C(19) 151.8(4) 1_555 1_555 1_555 yes Se(5) Ir(2) C(20) 148.3(4) 1_555 1_555 1_555 yes Se(5) Ir(2) C(21) 111.3(4) 1_555 1_555 1_555 yes Se(6) Ir(2) C(17) 132.6(5) 1_555 1_555 1_555 yes Se(6) Ir(2) C(18) 98.2(6) 1_555 1_555 1_555 yes Se(6) Ir(2) C(19) 94.4(4) 1_555 1_555 1_555 yes Se(6) Ir(2) C(20) 125.4(4) 1_555 1_555 1_555 yes Se(6) Ir(2) C(21) 158.5(4) 1_555 1_555 1_555 yes C(17) Ir(2) C(18) 38.9(8) 1_555 1_555 1_555 yes C(17) Ir(2) C(19) 64.8(6) 1_555 1_555 1_555 yes C(17) Ir(2) C(20) 62.4(5) 1_555 1_555 1_555 yes C(17) Ir(2) C(21) 37.5(6) 1_555 1_555 1_555 yes C(18) Ir(2) C(19) 38.5(6) 1_555 1_555 1_555 yes C(18) Ir(2) C(20) 62.8(6) 1_555 1_555 1_555 yes C(18) Ir(2) C(21) 63.8(7) 1_555 1_555 1_555 yes C(19) Ir(2) C(20) 38.0(6) 1_555 1_555 1_555 yes C(19) Ir(2) C(21) 64.2(6) 1_555 1_555 1_555 yes C(20) Ir(2) C(21) 37.3(6) 1_555 1_555 1_555 yes Ir(1) Se(1) Ir(2) 98.49(6) 1_555 1_555 1_555 yes Ir(1) Se(1) Se(2) 107.44(8) 1_555 1_555 1_555 yes Ir(2) Se(1) Se(2) 109.27(7) 1_555 1_555 1_555 yes Se(1) Se(2) Se(3) 101.95(8) 1_555 1_555 1_555 yes Se(2) Se(3) Se(4) 100.7(1) 1_555 1_555 1_555 yes Ir(1) Se(4) Se(3) 99.18(10) 1_555 1_555 1_555 yes Ir(1) Se(5) Ir(2) 98.21(5) 1_555 1_555 1_555 yes Ir(1) Se(5) C(1) 107.6(4) 1_555 1_555 1_555 yes Ir(2) Se(5) C(1) 100.8(4) 1_555 1_555 1_555 yes Ir(2) Se(6) C(2) 100.9(6) 1_555 1_555 1_555 yes C(3) O(1) C(4) 116(1) 1_555 1_555 1_555 yes C(5) O(3) C(6a) 122(2) 1_555 1_555 1_555 yes C(5) O(3) C(6b) 126(3) 1_555 1_555 1_555 yes C(6a) O(3) C(6b) 109(3) 1_555 1_555 1_555 yes Se(5) C(1) C(2) 119(1) 1_555 1_555 1_555 yes Se(5) C(1) C(3) 119(1) 1_555 1_555 1_555 yes C(2) C(1) C(3) 121(1) 1_555 1_555 1_555 yes Se(6) C(2) C(1) 124(1) 1_555 1_555 1_555 yes Se(6) C(2) C(5) 112(1) 1_555 1_555 1_555 yes C(1) C(2) C(5) 122(1) 1_555 1_555 1_555 yes O(1) C(3) O(2) 120(1) 1_555 1_555 1_555 yes O(1) C(3) C(1) 113(1) 1_555 1_555 1_555 yes O(2) C(3) C(1) 125(1) 1_555 1_555 1_555 yes O(1) C(4) H(1) 109(2) 1_555 1_555 1_555 no O(1) C(4) H(2) 109(1) 1_555 1_555 1_555 no O(1) C(4) H(3) 109(2) 1_555 1_555 1_555 no H(1) C(4) H(2) 109(2) 1_555 1_555 1_555 no H(1) C(4) H(3) 109(2) 1_555 1_555 1_555 no H(2) C(4) H(3) 109(2) 1_555 1_555 1_555 no O(3) C(5) O(4) 118(2) 1_555 1_555 1_555 yes O(3) C(5) C(2) 117(1) 1_555 1_555 1_555 yes O(4) C(5) C(2) 124(1) 1_555 1_555 1_555 yes O(3) C(6a) H(4a) 109(3) 1_555 1_555 1_555 no O(3) C(6a) H(5a) 109(2) 1_555 1_555 1_555 no O(3) C(6a) H(6a) 109(4) 1_555 1_555 1_555 no H(4a) C(6a) H(5a) 109(4) 1_555 1_555 1_555 no H(4a) C(6a) H(6a) 109(3) 1_555 1_555 1_555 no H(5a) C(6a) H(6a) 109(3) 1_555 1_555 1_555 no O(3) C(6b) H(4b) 109(4) 1_555 1_555 1_555 no O(3) C(6b) H(5b) 109(8) 1_555 1_555 1_555 no O(3) C(6b) H(6b) 109(5) 1_555 1_555 1_555 no H(4b) C(6b) H(5b) 109(6) 1_555 1_555 1_555 no H(4b) C(6b) H(6b) 109(9) 1_555 1_555 1_555 no H(5b) C(6b) H(6b) 109(5) 1_555 1_555 1_555 no Ir(1) C(7) C(8) 70.3(9) 1_555 1_555 1_555 yes Ir(1) C(7) C(11) 71(1) 1_555 1_555 1_555 yes Ir(1) C(7) C(12) 126(1) 1_555 1_555 1_555 yes C(8) C(7) C(11) 107(1) 1_555 1_555 1_555 yes C(8) C(7) C(12) 124(1) 1_555 1_555 1_555 yes C(11) C(7) C(12) 127(2) 1_555 1_555 1_555 yes Ir(1) C(8) C(7) 71.5(9) 1_555 1_555 1_555 yes Ir(1) C(8) C(9) 71.8(9) 1_555 1_555 1_555 yes Ir(1) C(8) C(13) 125.1(9) 1_555 1_555 1_555 yes C(7) C(8) C(9) 107(1) 1_555 1_555 1_555 yes C(7) C(8) C(13) 125(1) 1_555 1_555 1_555 yes C(9) C(8) C(13) 127(1) 1_555 1_555 1_555 yes Ir(1) C(9) C(8) 69.5(8) 1_555 1_555 1_555 yes Ir(1) C(9) C(10) 70.9(9) 1_555 1_555 1_555 yes Ir(1) C(9) C(14) 126(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 107(1) 1_555 1_555 1_555 yes C(8) C(9) C(14) 121(1) 1_555 1_555 1_555 yes C(10) C(9) C(14) 130(1) 1_555 1_555 1_555 yes Ir(1) C(10) C(9) 72.0(8) 1_555 1_555 1_555 yes Ir(1) C(10) C(11) 71.5(8) 1_555 1_555 1_555 yes Ir(1) C(10) C(15) 129(1) 1_555 1_555 1_555 yes C(9) C(10) C(11) 108(1) 1_555 1_555 1_555 yes C(9) C(10) C(15) 124(2) 1_555 1_555 1_555 yes C(11) C(10) C(15) 126(1) 1_555 1_555 1_555 yes Ir(1) C(11) C(7) 70.7(8) 1_555 1_555 1_555 yes Ir(1) C(11) C(10) 70.5(9) 1_555 1_555 1_555 yes Ir(1) C(11) C(16) 131(1) 1_555 1_555 1_555 yes C(7) C(11) C(10) 108(1) 1_555 1_555 1_555 yes C(7) C(11) C(16) 125(2) 1_555 1_555 1_555 yes C(10) C(11) C(16) 125(1) 1_555 1_555 1_555 yes C(7) C(12) H(7) 109(2) 1_555 1_555 1_555 no C(7) C(12) H(8) 109(2) 1_555 1_555 1_555 no C(7) C(12) H(9) 109(2) 1_555 1_555 1_555 no H(7) C(12) H(8) 109(2) 1_555 1_555 1_555 no H(7) C(12) H(9) 109(2) 1_555 1_555 1_555 no H(8) C(12) H(9) 109(2) 1_555 1_555 1_555 no C(8) C(13) H(10) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(11) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(12) 109(1) 1_555 1_555 1_555 no H(10) C(13) H(11) 109(1) 1_555 1_555 1_555 no H(10) C(13) H(12) 109(2) 1_555 1_555 1_555 no H(11) C(13) H(12) 109(2) 1_555 1_555 1_555 no C(9) C(14) H(13) 109(1) 1_555 1_555 1_555 no C(9) C(14) H(14) 109(2) 1_555 1_555 1_555 no C(9) C(14) H(15) 109(1) 1_555 1_555 1_555 no H(13) C(14) H(14) 109(1) 1_555 1_555 1_555 no H(13) C(14) H(15) 109(2) 1_555 1_555 1_555 no H(14) C(14) H(15) 109(2) 1_555 1_555 1_555 no C(10) C(15) H(16) 109(2) 1_555 1_555 1_555 no C(10) C(15) H(17) 109(2) 1_555 1_555 1_555 no C(10) C(15) H(18) 109(1) 1_555 1_555 1_555 no H(16) C(15) H(17) 109(2) 1_555 1_555 1_555 no H(16) C(15) H(18) 109(2) 1_555 1_555 1_555 no H(17) C(15) H(18) 109(2) 1_555 1_555 1_555 no C(11) C(16) H(19) 109(2) 1_555 1_555 1_555 no C(11) C(16) H(20) 109(2) 1_555 1_555 1_555 no C(11) C(16) H(21) 109(2) 1_555 1_555 1_555 no H(19) C(16) H(20) 109(2) 1_555 1_555 1_555 no H(19) C(16) H(21) 109(2) 1_555 1_555 1_555 no H(20) C(16) H(21) 109(2) 1_555 1_555 1_555 no Ir(2) C(17) C(18) 70(1) 1_555 1_555 1_555 yes Ir(2) C(17) C(21) 72.2(9) 1_555 1_555 1_555 yes Ir(2) C(17) C(22) 126.3(10) 1_555 1_555 1_555 yes C(18) C(17) C(21) 108(1) 1_555 1_555 1_555 yes C(18) C(17) C(22) 124(1) 1_555 1_555 1_555 yes C(21) C(17) C(22) 127(1) 1_555 1_555 1_555 yes Ir(2) C(18) C(17) 70.2(10) 1_555 1_555 1_555 yes Ir(2) C(18) C(19) 71.9(9) 1_555 1_555 1_555 yes Ir(2) C(18) C(23) 127(1) 1_555 1_555 1_555 yes C(17) C(18) C(19) 108(1) 1_555 1_555 1_555 yes C(17) C(18) C(23) 128(1) 1_555 1_555 1_555 yes C(19) C(18) C(23) 122(1) 1_555 1_555 1_555 yes Ir(2) C(19) C(18) 69.6(8) 1_555 1_555 1_555 yes Ir(2) C(19) C(20) 71.0(7) 1_555 1_555 1_555 yes Ir(2) C(19) C(24) 127.5(10) 1_555 1_555 1_555 yes C(18) C(19) C(20) 104(1) 1_555 1_555 1_555 yes C(18) C(19) C(24) 126(1) 1_555 1_555 1_555 yes C(20) C(19) C(24) 128(1) 1_555 1_555 1_555 yes Ir(2) C(20) C(19) 71.1(6) 1_555 1_555 1_555 yes Ir(2) C(20) C(21) 70.8(7) 1_555 1_555 1_555 yes Ir(2) C(20) C(25) 127.8(9) 1_555 1_555 1_555 yes C(19) C(20) C(21) 110(1) 1_555 1_555 1_555 yes C(19) C(20) C(25) 123(1) 1_555 1_555 1_555 yes C(21) C(20) C(25) 125(1) 1_555 1_555 1_555 yes Ir(2) C(21) C(17) 70.4(9) 1_555 1_555 1_555 yes Ir(2) C(21) C(20) 71.9(8) 1_555 1_555 1_555 yes Ir(2) C(21) C(26) 130.0(9) 1_555 1_555 1_555 yes C(17) C(21) C(20) 107(1) 1_555 1_555 1_555 yes C(17) C(21) C(26) 124(1) 1_555 1_555 1_555 yes C(20) C(21) C(26) 126(1) 1_555 1_555 1_555 yes C(17) C(22) H(22) 109(1) 1_555 1_555 1_555 no C(17) C(22) H(23) 109(2) 1_555 1_555 1_555 no C(17) C(22) H(24) 109(1) 1_555 1_555 1_555 no H(22) C(22) H(23) 109(1) 1_555 1_555 1_555 no H(22) C(22) H(24) 109(2) 1_555 1_555 1_555 no H(23) C(22) H(24) 109(2) 1_555 1_555 1_555 no C(18) C(23) H(25) 109(1) 1_555 1_555 1_555 no C(18) C(23) H(26) 109(2) 1_555 1_555 1_555 no C(18) C(23) H(27) 109(1) 1_555 1_555 1_555 no H(25) C(23) H(26) 109(2) 1_555 1_555 1_555 no H(25) C(23) H(27) 109(2) 1_555 1_555 1_555 no H(26) C(23) H(27) 109(1) 1_555 1_555 1_555 no C(19) C(24) H(28) 109(1) 1_555 1_555 1_555 no C(19) C(24) H(29) 109(1) 1_555 1_555 1_555 no C(19) C(24) H(30) 109(1) 1_555 1_555 1_555 no H(28) C(24) H(29) 109(2) 1_555 1_555 1_555 no H(28) C(24) H(30) 109(1) 1_555 1_555 1_555 no H(29) C(24) H(30) 109(2) 1_555 1_555 1_555 no C(20) C(25) H(31) 109(1) 1_555 1_555 1_555 no C(20) C(25) H(32) 109(1) 1_555 1_555 1_555 no C(20) C(25) H(33) 109(1) 1_555 1_555 1_555 no H(31) C(25) H(32) 109(1) 1_555 1_555 1_555 no H(31) C(25) H(33) 109(1) 1_555 1_555 1_555 no H(32) C(25) H(33) 109(2) 1_555 1_555 1_555 no C(21) C(26) H(34) 109(1) 1_555 1_555 1_555 no C(21) C(26) H(35) 109(1) 1_555 1_555 1_555 no C(21) C(26) H(36) 109(1) 1_555 1_555 1_555 no H(34) C(26) H(35) 109(2) 1_555 1_555 1_555 no H(34) C(26) H(36) 109(1) 1_555 1_555 1_555 no H(35) C(26) H(36) 109(2) 1_555 1_555 1_555 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 Ir(1) Ir(2) 3.756(1) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END data_[Cp*Ir{Se2C2(COOMe)2}]_(7) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Dec 4 13:18:55 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 627.48 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H21 Ir O4 Se2 ' _chemical_formula_moiety 'C16 H21 Ir O4 Se2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.977(1) _cell_length_b 11.6244(8) _cell_length_c 15.223(1) _cell_angle_alpha 90 _cell_angle_beta 112.210(6) _cell_angle_gamma 90 _cell_volume 1962.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.5 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _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 'darkred' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176.00 _exptl_absorpt_coefficient_mu 10.548 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.17 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 -2 0 -1 -2 0 -2 -1 _diffrn_reflns_number 4695 _reflns_number_total 4486 _reflns_number_gt 3435 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01160 _diffrn_orient_matrix_UB_12 -0.08451 _diffrn_orient_matrix_UB_13 -0.01235 _diffrn_orient_matrix_UB_21 -0.07894 _diffrn_orient_matrix_UB_22 0.01520 _diffrn_orient_matrix_UB_23 -0.05304 _diffrn_orient_matrix_UB_31 0.04203 _diffrn_orient_matrix_UB_32 0.00522 _diffrn_orient_matrix_UB_33 -0.04548 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.09846(2) 0.15618(2) 0.33740(2) 0.03524(6) Uani 1.00 d . . . Se(1) Se 0.06035(6) -0.03602(5) 0.36491(4) 0.0424(2) Uani 1.00 d . . . Se(2) Se -0.02652(7) 0.13300(6) 0.17666(5) 0.0536(2) Uani 1.00 d . . . O(1) O -0.0106(4) -0.2873(4) 0.2785(4) 0.086(2) Uani 1.00 d . . . O(2) O -0.2574(6) -0.0025(6) 0.0302(4) 0.141(3) Uani 1.00 d . . . O(3) O -0.1972(4) -0.2287(4) 0.2033(3) 0.061(2) Uani 1.00 d . . . O(4) O -0.1380(4) -0.1509(5) 0.0449(3) 0.072(2) Uani 1.00 d . . . C(1) C -0.0458(5) -0.0891(5) 0.2455(4) 0.036(2) Uani 1.00 d . . . C(2) C -0.0818(5) -0.0193(5) 0.1699(4) 0.040(2) Uani 1.00 d . . . C(3) C -0.0808(6) -0.2118(5) 0.2443(4) 0.041(2) Uani 1.00 d . . . C(4) C -0.1652(7) -0.0545(7) 0.0727(5) 0.067(2) Uani 1.00 d . . . C(5) C -0.2354(7) -0.3486(7) 0.1947(7) 0.095(3) Uani 1.00 d . . . C(6) C -0.2186(7) -0.1929(8) -0.0469(5) 0.093(3) Uani 1.00 d . . . C(7) C 0.2748(6) 0.2165(6) 0.4236(5) 0.057(2) Uani 1.00 d . . . C(8) C 0.2162(7) 0.3027(6) 0.3500(5) 0.056(2) Uani 1.00 d . . . C(9) C 0.1137(6) 0.3402(6) 0.3659(5) 0.052(2) Uani 1.00 d . . . C(10) C 0.1096(6) 0.2807(6) 0.4455(5) 0.051(2) Uani 1.00 d . . . C(11) C 0.2080(6) 0.2106(6) 0.4820(5) 0.055(2) Uani 1.00 d . . . C(12) C 0.3915(7) 0.1578(9) 0.4375(8) 0.131(4) Uani 1.00 d . . . C(13) C 0.2604(9) 0.3470(9) 0.2767(6) 0.118(4) Uani 1.00 d . . . C(14) C 0.0245(8) 0.4311(7) 0.3106(6) 0.092(3) Uani 1.00 d . . . C(15) C 0.0172(8) 0.3013(8) 0.4893(6) 0.092(3) Uani 1.00 d . . . C(16) C 0.2399(8) 0.1351(8) 0.5703(5) 0.106(3) Uani 1.00 d . . . H(1) H -0.3207 -0.3526 0.1647 0.1137 Uiso 1.00 calc . . . H(2) H -0.1999 -0.3892 0.1576 0.1137 Uiso 1.00 calc . . . H(3) H -0.2104 -0.3823 0.2560 0.1137 Uiso 1.00 calc . . . H(4) H -0.2972 -0.2023 -0.0465 0.1111 Uiso 1.00 calc . . . H(5) H -0.2213 -0.1390 -0.0946 0.1111 Uiso 1.00 calc . . . H(6) H -0.1901 -0.2647 -0.0597 0.1111 Uiso 1.00 calc . . . H(7) H 0.3813 0.0768 0.4392 0.1579 Uiso 1.00 calc . . . H(8) H 0.4156 0.1768 0.3867 0.1579 Uiso 1.00 calc . . . H(9) H 0.4516 0.1823 0.4958 0.1579 Uiso 1.00 calc . . . H(10) H 0.3316 0.3069 0.2815 0.1416 Uiso 1.00 calc . . . H(11) H 0.2001 0.3355 0.2153 0.1416 Uiso 1.00 calc . . . H(12) H 0.2776 0.4268 0.2867 0.1416 Uiso 1.00 calc . . . H(13) H 0.0255 0.4931 0.3515 0.1107 Uiso 1.00 calc . . . H(14) H 0.0460 0.4586 0.2603 0.1107 Uiso 1.00 calc . . . H(15) H -0.0541 0.3987 0.2851 0.1107 Uiso 1.00 calc . . . H(16) H 0.0555 0.3347 0.5504 0.1106 Uiso 1.00 calc . . . H(17) H -0.0434 0.3519 0.4501 0.1106 Uiso 1.00 calc . . . H(18) H -0.0185 0.2302 0.4951 0.1106 Uiso 1.00 calc . . . H(19) H 0.1769 0.0813 0.5615 0.1271 Uiso 1.00 calc . . . H(20) H 0.3129 0.0950 0.5804 0.1271 Uiso 1.00 calc . . . H(21) H 0.2499 0.1820 0.6238 0.1271 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir 0.0408(1) 0.0242(1) 0.0396(1) -0.0053(1) 0.01386(10) -0.0027(1) Se(1) 0.0585(4) 0.0270(3) 0.0366(3) -0.0075(3) 0.0124(3) 0.0006(3) Se(2) 0.0736(5) 0.0278(4) 0.0432(4) -0.0066(3) 0.0038(3) 0.0061(3) O(1) 0.067(3) 0.033(3) 0.122(5) -0.004(3) -0.008(3) 0.012(3) O(2) 0.150(6) 0.070(5) 0.104(5) 0.036(4) -0.065(4) -0.017(4) O(3) 0.049(3) 0.031(3) 0.095(4) -0.008(2) 0.019(3) 0.000(3) O(4) 0.061(3) 0.084(4) 0.055(3) 0.008(3) 0.002(2) -0.039(3) C(1) 0.035(3) 0.028(3) 0.042(3) -0.004(3) 0.010(3) -0.006(3) C(2) 0.045(4) 0.027(3) 0.041(3) 0.003(3) 0.008(3) 0.001(3) C(3) 0.048(4) 0.024(3) 0.047(4) -0.003(3) 0.013(3) -0.004(3) C(4) 0.074(5) 0.039(4) 0.053(5) -0.005(4) -0.018(4) 0.002(4) C(5) 0.082(6) 0.043(5) 0.146(8) -0.032(5) 0.028(6) -0.012(6) C(6) 0.089(6) 0.116(9) 0.060(5) -0.015(6) 0.013(5) -0.042(5) C(7) 0.036(4) 0.045(5) 0.078(5) -0.008(3) 0.008(4) -0.022(4) C(8) 0.081(5) 0.050(5) 0.046(4) -0.040(4) 0.034(4) -0.013(3) C(9) 0.064(4) 0.027(4) 0.056(4) -0.011(4) 0.011(4) -0.007(3) C(10) 0.060(4) 0.040(4) 0.056(4) -0.016(4) 0.025(4) -0.017(4) C(11) 0.057(4) 0.048(5) 0.047(4) -0.022(4) 0.006(4) -0.006(4) C(12) 0.043(5) 0.108(9) 0.22(1) -0.005(6) 0.017(6) -0.063(9) C(13) 0.170(9) 0.117(9) 0.102(7) -0.098(8) 0.093(7) -0.048(7) C(14) 0.110(7) 0.032(5) 0.095(6) 0.006(5) -0.006(5) -0.005(4) C(15) 0.110(7) 0.087(7) 0.101(7) -0.027(6) 0.064(6) -0.041(6) C(16) 0.132(8) 0.095(8) 0.049(5) -0.044(6) -0.012(5) 0.021(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 3sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00178(7) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3435 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0262 _refine_ls_wR_factor_gt 0.0262 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.747 _refine_ls_shift/su_max 0.0140 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.77 _refine_diff_density_max 1.40 #------------------------------------------------------------------------------ _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 Se(1) 2.3494(7) 1_555 1_555 yes Ir Se(2) 2.3520(6) 1_555 1_555 yes Ir C(7) 2.140(6) 1_555 1_555 yes Ir C(8) 2.173(8) 1_555 1_555 yes Ir C(9) 2.176(7) 1_555 1_555 yes Ir C(10) 2.158(7) 1_555 1_555 yes Ir C(11) 2.187(6) 1_555 1_555 yes Se(1) C(1) 1.885(5) 1_555 1_555 yes Se(2) C(2) 1.880(6) 1_555 1_555 yes O(1) C(3) 1.190(8) 1_555 1_555 yes O(2) C(4) 1.209(10) 1_555 1_555 yes O(3) C(3) 1.309(7) 1_555 1_555 yes O(3) C(5) 1.458(9) 1_555 1_555 yes O(4) C(4) 1.283(10) 1_555 1_555 yes O(4) C(6) 1.450(8) 1_555 1_555 yes C(1) C(2) 1.339(8) 1_555 1_555 yes C(1) C(3) 1.485(9) 1_555 1_555 yes C(2) C(4) 1.496(8) 1_555 1_555 yes C(7) C(8) 1.468(10) 1_555 1_555 yes C(7) C(11) 1.40(1) 1_555 1_555 yes C(7) C(12) 1.50(1) 1_555 1_555 yes C(8) C(9) 1.41(1) 1_555 1_555 yes C(8) C(13) 1.50(1) 1_555 1_555 yes C(9) C(10) 1.41(1) 1_555 1_555 yes C(9) C(14) 1.513(10) 1_555 1_555 yes C(10) C(11) 1.367(10) 1_555 1_555 yes C(10) C(15) 1.51(1) 1_555 1_555 yes C(11) C(16) 1.53(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Ir Se(2) 89.22(2) 1_555 1_555 1_555 yes Se(1) Ir C(7) 114.6(2) 1_555 1_555 1_555 yes Se(1) Ir C(8) 153.2(2) 1_555 1_555 1_555 yes Se(1) Ir C(9) 155.0(2) 1_555 1_555 1_555 yes Se(1) Ir C(10) 117.5(2) 1_555 1_555 1_555 yes Se(1) Ir C(11) 100.3(2) 1_555 1_555 1_555 yes Se(2) Ir C(7) 140.2(2) 1_555 1_555 1_555 yes Se(2) Ir C(8) 108.6(2) 1_555 1_555 1_555 yes Se(2) Ir C(9) 107.0(2) 1_555 1_555 1_555 yes Se(2) Ir C(10) 134.6(2) 1_555 1_555 1_555 yes Se(2) Ir C(11) 169.7(2) 1_555 1_555 1_555 yes C(7) Ir C(8) 39.8(3) 1_555 1_555 1_555 yes C(7) Ir C(9) 64.3(3) 1_555 1_555 1_555 yes C(7) Ir C(10) 63.2(3) 1_555 1_555 1_555 yes C(7) Ir C(11) 37.8(3) 1_555 1_555 1_555 yes C(8) Ir C(9) 37.7(3) 1_555 1_555 1_555 yes C(8) Ir C(10) 63.6(3) 1_555 1_555 1_555 yes C(8) Ir C(11) 64.0(3) 1_555 1_555 1_555 yes C(9) Ir C(10) 38.0(3) 1_555 1_555 1_555 yes C(9) Ir C(11) 62.8(2) 1_555 1_555 1_555 yes C(10) Ir C(11) 36.7(3) 1_555 1_555 1_555 yes Ir Se(1) C(1) 104.2(2) 1_555 1_555 1_555 yes Ir Se(2) C(2) 103.7(2) 1_555 1_555 1_555 yes C(3) O(3) C(5) 115.3(5) 1_555 1_555 1_555 yes C(4) O(4) C(6) 116.8(6) 1_555 1_555 1_555 yes Se(1) C(1) C(2) 120.7(4) 1_555 1_555 1_555 yes Se(1) C(1) C(3) 114.2(4) 1_555 1_555 1_555 yes C(2) C(1) C(3) 125.0(5) 1_555 1_555 1_555 yes Se(2) C(2) C(1) 122.1(4) 1_555 1_555 1_555 yes Se(2) C(2) C(4) 113.7(5) 1_555 1_555 1_555 yes C(1) C(2) C(4) 124.2(6) 1_555 1_555 1_555 yes O(1) C(3) O(3) 123.1(6) 1_555 1_555 1_555 yes O(1) C(3) C(1) 123.6(6) 1_555 1_555 1_555 yes O(3) C(3) C(1) 113.2(5) 1_555 1_555 1_555 yes O(2) C(4) O(4) 123.7(6) 1_555 1_555 1_555 yes O(2) C(4) C(2) 121.8(7) 1_555 1_555 1_555 yes O(4) C(4) C(2) 114.0(6) 1_555 1_555 1_555 yes O(3) C(5) H(1) 109.5(7) 1_555 1_555 1_555 no O(3) C(5) H(2) 109.5(9) 1_555 1_555 1_555 no O(3) C(5) H(3) 109.5(7) 1_555 1_555 1_555 no H(1) C(5) H(2) 109.5(8) 1_555 1_555 1_555 no H(1) C(5) H(3) 109(1) 1_555 1_555 1_555 no H(2) C(5) H(3) 109.5(8) 1_555 1_555 1_555 no O(4) C(6) H(4) 109.5(8) 1_555 1_555 1_555 no O(4) C(6) H(5) 109.5(8) 1_555 1_555 1_555 no O(4) C(6) H(6) 109.5(6) 1_555 1_555 1_555 no H(4) C(6) H(5) 109.5(8) 1_555 1_555 1_555 no H(4) C(6) H(6) 109.5(9) 1_555 1_555 1_555 no H(5) C(6) H(6) 109.5(9) 1_555 1_555 1_555 no Ir C(7) C(8) 71.3(4) 1_555 1_555 1_555 yes Ir C(7) C(11) 72.9(4) 1_555 1_555 1_555 yes Ir C(7) C(12) 126.1(6) 1_555 1_555 1_555 yes C(8) C(7) C(11) 107.1(6) 1_555 1_555 1_555 yes C(8) C(7) C(12) 124.8(8) 1_555 1_555 1_555 yes C(11) C(7) C(12) 127.8(8) 1_555 1_555 1_555 yes Ir C(8) C(7) 68.9(4) 1_555 1_555 1_555 yes Ir C(8) C(9) 71.3(4) 1_555 1_555 1_555 yes Ir C(8) C(13) 127.2(5) 1_555 1_555 1_555 yes C(7) C(8) C(9) 106.1(7) 1_555 1_555 1_555 yes C(7) C(8) C(13) 127.1(8) 1_555 1_555 1_555 yes C(9) C(8) C(13) 126.8(7) 1_555 1_555 1_555 yes Ir C(9) C(8) 71.0(4) 1_555 1_555 1_555 yes Ir C(9) C(10) 70.3(4) 1_555 1_555 1_555 yes Ir C(9) C(14) 126.0(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 108.1(6) 1_555 1_555 1_555 yes C(8) C(9) C(14) 126.9(7) 1_555 1_555 1_555 yes C(10) C(9) C(14) 124.9(8) 1_555 1_555 1_555 yes Ir C(10) C(9) 71.7(4) 1_555 1_555 1_555 yes Ir C(10) C(11) 72.8(4) 1_555 1_555 1_555 yes Ir C(10) C(15) 126.7(5) 1_555 1_555 1_555 yes C(9) C(10) C(11) 109.6(7) 1_555 1_555 1_555 yes C(9) C(10) C(15) 124.8(6) 1_555 1_555 1_555 yes C(11) C(10) C(15) 125.3(7) 1_555 1_555 1_555 yes Ir C(11) C(7) 69.3(4) 1_555 1_555 1_555 yes Ir C(11) C(10) 70.5(4) 1_555 1_555 1_555 yes Ir C(11) C(16) 125.1(5) 1_555 1_555 1_555 yes C(7) C(11) C(10) 108.8(6) 1_555 1_555 1_555 yes C(7) C(11) C(16) 124.9(7) 1_555 1_555 1_555 yes C(10) C(11) C(16) 126.2(8) 1_555 1_555 1_555 yes C(7) C(12) H(7) 109.5(8) 1_555 1_555 1_555 no C(7) C(12) H(8) 109.5(9) 1_555 1_555 1_555 no C(7) C(12) H(9) 109(1) 1_555 1_555 1_555 no H(7) C(12) H(8) 109(1) 1_555 1_555 1_555 no H(7) C(12) H(9) 109(1) 1_555 1_555 1_555 no H(8) C(12) H(9) 109.5(9) 1_555 1_555 1_555 no C(8) C(13) H(10) 109.5(8) 1_555 1_555 1_555 no C(8) C(13) H(11) 109.5(10) 1_555 1_555 1_555 no C(8) C(13) H(12) 109.5(9) 1_555 1_555 1_555 no H(10) C(13) H(11) 109(1) 1_555 1_555 1_555 no H(10) C(13) H(12) 109(1) 1_555 1_555 1_555 no H(11) C(13) H(12) 109.5(9) 1_555 1_555 1_555 no C(9) C(14) H(13) 109.5(7) 1_555 1_555 1_555 no C(9) C(14) H(14) 109.5(9) 1_555 1_555 1_555 no C(9) C(14) H(15) 109.5(7) 1_555 1_555 1_555 no H(13) C(14) H(14) 109.5(8) 1_555 1_555 1_555 no H(13) C(14) H(15) 109(1) 1_555 1_555 1_555 no H(14) C(14) H(15) 109.5(8) 1_555 1_555 1_555 no C(10) C(15) H(16) 109.5(8) 1_555 1_555 1_555 no C(10) C(15) H(17) 109.5(9) 1_555 1_555 1_555 no C(10) C(15) H(18) 109.5(8) 1_555 1_555 1_555 no H(16) C(15) H(17) 109.5(9) 1_555 1_555 1_555 no H(16) C(15) H(18) 109.5(10) 1_555 1_555 1_555 no H(17) C(15) H(18) 109.5(8) 1_555 1_555 1_555 no C(11) C(16) H(19) 109.5(6) 1_555 1_555 1_555 no C(11) C(16) H(20) 109.5(9) 1_555 1_555 1_555 no C(11) C(16) H(21) 109.5(8) 1_555 1_555 1_555 no H(19) C(16) H(20) 109.4(9) 1_555 1_555 1_555 no H(19) C(16) H(21) 109(1) 1_555 1_555 1_555 no H(20) C(16) H(21) 109.5(7) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===END data_[Cp*Ir{Se2C4(COOMe)4}]_(8) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Dec 3 13:32:35 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 769.59 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H27 Ir O8 Se2 ' _chemical_formula_moiety 'C22 H27 Ir O8 Se2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.951(1) _cell_length_b 10.3826(8) _cell_length_c 12.707(1) _cell_angle_alpha 87.707(8) _cell_angle_beta 87.033(9) _cell_angle_gamma 77.443(7) _cell_volume 1279.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.1 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _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 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736.00 _exptl_absorpt_coefficient_mu 8.122 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -4.67 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -1 -1 -2 -1 -2 -2 -1 -3 _diffrn_reflns_number 6200 _reflns_number_total 5859 _reflns_number_gt 5017 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01501 _diffrn_orient_matrix_UB_12 -0.08388 _diffrn_orient_matrix_UB_13 -0.03925 _diffrn_orient_matrix_UB_21 0.00938 _diffrn_orient_matrix_UB_22 -0.05186 _diffrn_orient_matrix_UB_23 0.06825 _diffrn_orient_matrix_UB_31 -0.10152 _diffrn_orient_matrix_UB_32 0.00443 _diffrn_orient_matrix_UB_33 0.00404 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.24487(2) 0.37347(2) 0.23004(1) 0.02939(4) Uani 1.00 d . . . Se(1) Se 0.13614(4) 0.55480(4) 0.34692(3) 0.0363(1) Uani 1.00 d . . . Se(2) Se 0.29879(4) 0.54791(4) 0.10640(3) 0.0345(1) Uani 1.00 d . . . O(1) O 0.1251(3) 0.8884(3) 0.3740(3) 0.055(1) Uani 1.00 d . . . O(2) O -0.0670(3) 0.8637(3) 0.2989(2) 0.0460(9) Uani 1.00 d . . . O(3) O 0.1265(3) 0.9407(3) 0.1264(3) 0.054(1) Uani 1.00 d . . . O(4) O 0.2262(3) 0.8039(3) -0.0013(2) 0.0483(9) Uani 1.00 d . . . O(5) O 0.6272(3) 0.2512(3) 0.3035(3) 0.056(1) Uani 1.00 d . . . O(6) O 0.5035(3) 0.3687(3) 0.4318(2) 0.0524(10) Uani 1.00 d . . . O(7) O 0.5431(4) 0.6999(4) 0.1367(3) 0.081(1) Uani 1.00 d . . . O(8) O 0.6296(3) 0.5802(3) 0.2782(3) 0.057(1) Uani 1.00 d . . . C(1) C 0.1360(4) 0.7063(4) 0.2618(3) 0.033(1) Uani 1.00 d . . . C(2) C 0.1913(4) 0.7104(4) 0.1636(3) 0.033(1) Uani 1.00 d . . . C(3) C 0.0667(4) 0.8316(4) 0.3172(3) 0.037(1) Uani 1.00 d . . . C(4) C 0.1783(4) 0.8303(4) 0.0977(3) 0.036(1) Uani 1.00 d . . . C(5) C -0.1414(6) 0.9855(5) 0.3445(4) 0.064(2) Uani 1.00 d . . . C(6) C 0.2106(5) 0.9129(5) -0.0760(4) 0.053(2) Uani 1.00 d . . . C(7) C 0.4306(4) 0.4145(4) 0.2592(3) 0.032(1) Uani 1.00 d . . . C(8) C 0.4506(4) 0.5177(4) 0.1990(3) 0.035(1) Uani 1.00 d . . . C(9) C 0.5324(4) 0.3377(4) 0.3322(3) 0.035(1) Uani 1.00 d . . . C(10) C 0.5446(5) 0.6082(5) 0.1974(4) 0.046(1) Uani 1.00 d . . . C(11) C 0.5990(6) 0.2992(6) 0.5067(4) 0.073(2) Uani 1.00 d . . . C(12) C 0.7150(6) 0.6731(6) 0.2940(6) 0.086(2) Uani 1.00 d . . . C(13) C 0.1235(5) 0.2378(4) 0.3040(4) 0.045(1) Uani 1.00 d . . . C(14) C 0.2608(5) 0.1670(4) 0.2803(4) 0.046(1) Uani 1.00 d . . . C(15) C 0.2843(4) 0.1746(4) 0.1678(4) 0.042(1) Uani 1.00 d . . . C(16) C 0.1597(4) 0.2490(4) 0.1240(3) 0.037(1) Uani 1.00 d . . . C(17) C 0.0607(4) 0.2873(4) 0.2077(4) 0.041(1) Uani 1.00 d . . . C(18) C 0.0525(7) 0.2533(6) 0.4118(4) 0.080(2) Uani 1.00 d . . . C(19) C 0.3590(7) 0.0866(5) 0.3565(5) 0.083(2) Uani 1.00 d . . . C(20) C 0.4113(5) 0.1059(5) 0.1072(5) 0.072(2) Uani 1.00 d . . . C(21) C 0.1362(6) 0.2786(6) 0.0093(4) 0.064(2) Uani 1.00 d . . . C(22) C -0.0853(5) 0.3615(5) 0.1963(5) 0.071(2) Uani 1.00 d . . . H(1) H -0.1344 0.9794 0.4189 0.0765 Uiso 1.00 calc . . . H(2) H -0.1032 1.0566 0.3167 0.0765 Uiso 1.00 calc . . . H(3) H -0.2356 1.0004 0.3278 0.0765 Uiso 1.00 calc . . . H(4) H 0.2586 0.9760 -0.0535 0.0641 Uiso 1.00 calc . . . H(5) H 0.2474 0.8821 -0.1431 0.0641 Uiso 1.00 calc . . . H(6) H 0.1156 0.9528 -0.0808 0.0641 Uiso 1.00 calc . . . H(7) H 0.6035 0.2071 0.5035 0.0870 Uiso 1.00 calc . . . H(8) H 0.6876 0.3166 0.4903 0.0870 Uiso 1.00 calc . . . H(9) H 0.5687 0.3281 0.5756 0.0870 Uiso 1.00 calc . . . H(10) H 0.7714 0.6438 0.3520 0.1034 Uiso 1.00 calc . . . H(11) H 0.7716 0.6796 0.2323 0.1034 Uiso 1.00 calc . . . H(12) H 0.6581 0.7573 0.3080 0.1034 Uiso 1.00 calc . . . H(13) H 0.0217 0.3445 0.4256 0.0963 Uiso 1.00 calc . . . H(14) H -0.0242 0.2123 0.4145 0.0963 Uiso 1.00 calc . . . H(15) H 0.1154 0.2129 0.4634 0.0963 Uiso 1.00 calc . . . H(16) H 0.3197 0.0973 0.4261 0.0994 Uiso 1.00 calc . . . H(17) H 0.3758 -0.0039 0.3393 0.0994 Uiso 1.00 calc . . . H(18) H 0.4433 0.1157 0.3519 0.0994 Uiso 1.00 calc . . . H(19) H 0.4782 0.0633 0.1550 0.0858 Uiso 1.00 calc . . . H(20) H 0.3885 0.0422 0.0636 0.0858 Uiso 1.00 calc . . . H(21) H 0.4473 0.1688 0.0646 0.0858 Uiso 1.00 calc . . . H(22) H 0.1108 0.3714 -0.0027 0.0767 Uiso 1.00 calc . . . H(23) H 0.2184 0.2440 -0.0308 0.0767 Uiso 1.00 calc . . . H(24) H 0.0644 0.2391 -0.0113 0.0767 Uiso 1.00 calc . . . H(25) H -0.0856 0.4446 0.1620 0.0849 Uiso 1.00 calc . . . H(26) H -0.1325 0.3121 0.1556 0.0849 Uiso 1.00 calc . . . H(27) H -0.1300 0.3748 0.2641 0.0849 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir 0.02793(9) 0.02362(8) 0.03662(9) -0.00534(6) 0.00000(6) -0.00387(6) Se(1) 0.0403(2) 0.0288(2) 0.0387(2) -0.0061(2) 0.0058(2) -0.0055(2) Se(2) 0.0387(2) 0.0290(2) 0.0341(2) -0.0040(2) 0.0000(2) -0.0015(2) O(1) 0.061(2) 0.043(2) 0.063(2) -0.008(2) -0.013(2) -0.018(2) O(2) 0.038(2) 0.034(2) 0.063(2) 0.001(1) 0.000(1) -0.010(1) O(3) 0.068(2) 0.030(2) 0.058(2) -0.002(2) 0.003(2) 0.001(2) O(4) 0.065(2) 0.036(2) 0.039(2) -0.001(2) -0.005(2) 0.005(1) O(5) 0.046(2) 0.050(2) 0.059(2) 0.018(2) -0.002(2) -0.004(2) O(6) 0.052(2) 0.056(2) 0.040(2) 0.010(2) -0.011(1) -0.008(2) O(7) 0.077(3) 0.069(3) 0.107(3) -0.042(2) -0.013(2) 0.034(2) O(8) 0.041(2) 0.052(2) 0.084(3) -0.018(2) -0.010(2) -0.006(2) C(1) 0.029(2) 0.025(2) 0.043(2) -0.004(2) -0.005(2) -0.005(2) C(2) 0.033(2) 0.027(2) 0.038(2) -0.004(2) -0.006(2) -0.002(2) C(3) 0.038(2) 0.030(2) 0.043(2) -0.005(2) -0.002(2) -0.003(2) C(4) 0.033(2) 0.032(2) 0.043(2) -0.007(2) -0.007(2) 0.003(2) C(5) 0.068(4) 0.039(3) 0.073(4) 0.013(3) 0.007(3) -0.007(3) C(6) 0.063(3) 0.048(3) 0.045(3) -0.003(3) -0.005(2) 0.014(2) C(7) 0.031(2) 0.023(2) 0.039(2) -0.002(2) 0.003(2) -0.007(2) C(8) 0.026(2) 0.030(2) 0.046(2) -0.003(2) 0.003(2) -0.006(2) C(9) 0.033(2) 0.030(2) 0.044(2) -0.009(2) -0.003(2) -0.002(2) C(10) 0.036(3) 0.037(3) 0.066(3) -0.009(2) 0.004(2) -0.003(2) C(11) 0.072(4) 0.084(4) 0.052(3) 0.006(3) -0.027(3) 0.002(3) C(12) 0.058(4) 0.076(4) 0.135(6) -0.033(3) -0.014(4) -0.028(4) C(13) 0.054(3) 0.031(2) 0.053(3) -0.022(2) 0.012(2) -0.007(2) C(14) 0.053(3) 0.025(2) 0.065(3) -0.015(2) -0.011(2) 0.006(2) C(15) 0.039(2) 0.024(2) 0.065(3) -0.008(2) 0.003(2) -0.012(2) C(16) 0.038(2) 0.030(2) 0.047(3) -0.014(2) 0.000(2) -0.014(2) C(17) 0.028(2) 0.033(2) 0.065(3) -0.012(2) 0.002(2) -0.011(2) C(18) 0.119(5) 0.072(4) 0.063(4) -0.057(4) 0.035(3) -0.009(3) C(19) 0.099(5) 0.046(3) 0.111(5) -0.029(3) -0.042(4) 0.031(3) C(20) 0.043(3) 0.052(3) 0.117(5) -0.003(3) 0.017(3) -0.037(3) C(21) 0.078(4) 0.067(4) 0.054(3) -0.027(3) -0.008(3) -0.015(3) C(22) 0.034(3) 0.057(4) 0.123(5) -0.012(3) 0.007(3) -0.033(3) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0097(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5017 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0232 _refine_ls_wR_factor_gt 0.0232 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.520 _refine_ls_shift/su_max 0.0060 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.95 _refine_diff_density_max 0.57 #------------------------------------------------------------------------------ _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 Se(1) 2.4683(4) 1_555 1_555 yes Ir Se(2) 2.4787(4) 1_555 1_555 yes Ir C(7) 2.039(4) 1_555 1_555 yes Ir C(13) 2.201(4) 1_555 1_555 yes Ir C(14) 2.187(4) 1_555 1_555 yes Ir C(15) 2.188(4) 1_555 1_555 yes Ir C(16) 2.222(4) 1_555 1_555 yes Ir C(17) 2.242(4) 1_555 1_555 yes Se(1) C(1) 1.873(4) 1_555 1_555 yes Se(2) C(2) 1.937(4) 1_555 1_555 yes Se(2) C(8) 1.928(4) 1_555 1_555 yes O(1) C(3) 1.197(5) 1_555 1_555 yes O(2) C(3) 1.330(5) 1_555 1_555 yes O(2) C(5) 1.445(5) 1_555 1_555 yes O(3) C(4) 1.212(5) 1_555 1_555 yes O(4) C(4) 1.339(5) 1_555 1_555 yes O(4) C(6) 1.435(5) 1_555 1_555 yes O(5) C(9) 1.205(5) 1_555 1_555 yes O(6) C(9) 1.319(5) 1_555 1_555 yes O(6) C(11) 1.438(5) 1_555 1_555 yes O(7) C(10) 1.199(6) 1_555 1_555 yes O(8) C(10) 1.347(6) 1_555 1_555 yes O(8) C(12) 1.443(6) 1_555 1_555 yes C(1) C(2) 1.340(5) 1_555 1_555 yes C(1) C(3) 1.515(5) 1_555 1_555 yes C(2) C(4) 1.458(5) 1_555 1_555 yes C(7) C(8) 1.336(6) 1_555 1_555 yes C(7) C(9) 1.487(6) 1_555 1_555 yes C(8) C(10) 1.461(6) 1_555 1_555 yes C(13) C(14) 1.427(6) 1_555 1_555 yes C(13) C(17) 1.429(6) 1_555 1_555 yes C(13) C(18) 1.507(7) 1_555 1_555 yes C(14) C(15) 1.439(6) 1_555 1_555 yes C(14) C(19) 1.505(7) 1_555 1_555 yes C(15) C(16) 1.436(6) 1_555 1_555 yes C(15) C(20) 1.499(6) 1_555 1_555 yes C(16) C(17) 1.419(6) 1_555 1_555 yes C(16) C(21) 1.498(6) 1_555 1_555 yes C(17) C(22) 1.500(6) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Ir Se(2) 86.18(1) 1_555 1_555 1_555 yes Se(1) Ir C(7) 87.9(1) 1_555 1_555 1_555 yes Se(1) Ir C(13) 92.9(1) 1_555 1_555 1_555 yes Se(1) Ir C(14) 121.1(1) 1_555 1_555 1_555 yes Se(1) Ir C(15) 156.4(1) 1_555 1_555 1_555 yes Se(1) Ir C(16) 132.8(1) 1_555 1_555 1_555 yes Se(1) Ir C(17) 99.0(1) 1_555 1_555 1_555 yes Se(2) Ir C(7) 68.9(1) 1_555 1_555 1_555 yes Se(2) Ir C(13) 157.4(1) 1_555 1_555 1_555 yes Se(2) Ir C(14) 152.4(1) 1_555 1_555 1_555 yes Se(2) Ir C(15) 115.7(1) 1_555 1_555 1_555 yes Se(2) Ir C(16) 102.0(1) 1_555 1_555 1_555 yes Se(2) Ir C(17) 120.3(1) 1_555 1_555 1_555 yes C(7) Ir C(13) 133.7(2) 1_555 1_555 1_555 yes C(7) Ir C(14) 105.4(2) 1_555 1_555 1_555 yes C(7) Ir C(15) 107.6(2) 1_555 1_555 1_555 yes C(7) Ir C(16) 138.6(1) 1_555 1_555 1_555 yes C(7) Ir C(17) 168.6(2) 1_555 1_555 1_555 yes C(13) Ir C(14) 37.9(2) 1_555 1_555 1_555 yes C(13) Ir C(15) 63.5(2) 1_555 1_555 1_555 yes C(13) Ir C(16) 62.6(2) 1_555 1_555 1_555 yes C(13) Ir C(17) 37.5(2) 1_555 1_555 1_555 yes C(14) Ir C(15) 38.4(2) 1_555 1_555 1_555 yes C(14) Ir C(16) 63.5(2) 1_555 1_555 1_555 yes C(14) Ir C(17) 63.2(2) 1_555 1_555 1_555 yes C(15) Ir C(16) 38.0(2) 1_555 1_555 1_555 yes C(15) Ir C(17) 63.1(2) 1_555 1_555 1_555 yes C(16) Ir C(17) 37.1(1) 1_555 1_555 1_555 yes Ir Se(1) C(1) 103.2(1) 1_555 1_555 1_555 yes Ir Se(2) C(2) 104.1(1) 1_555 1_555 1_555 yes Ir Se(2) C(8) 77.5(1) 1_555 1_555 1_555 yes C(2) Se(2) C(8) 99.2(2) 1_555 1_555 1_555 yes C(3) O(2) C(5) 115.2(4) 1_555 1_555 1_555 yes C(4) O(4) C(6) 117.1(3) 1_555 1_555 1_555 yes C(9) O(6) C(11) 116.1(4) 1_555 1_555 1_555 yes C(10) O(8) C(12) 116.3(4) 1_555 1_555 1_555 yes Se(1) C(1) C(2) 126.5(3) 1_555 1_555 1_555 yes Se(1) C(1) C(3) 112.3(3) 1_555 1_555 1_555 yes C(2) C(1) C(3) 121.2(4) 1_555 1_555 1_555 yes Se(2) C(2) C(1) 118.2(3) 1_555 1_555 1_555 yes Se(2) C(2) C(4) 117.7(3) 1_555 1_555 1_555 yes C(1) C(2) C(4) 124.1(4) 1_555 1_555 1_555 yes O(1) C(3) O(2) 125.5(4) 1_555 1_555 1_555 yes O(1) C(3) C(1) 123.5(4) 1_555 1_555 1_555 yes O(2) C(3) C(1) 110.9(3) 1_555 1_555 1_555 yes O(3) C(4) O(4) 123.2(4) 1_555 1_555 1_555 yes O(3) C(4) C(2) 125.1(4) 1_555 1_555 1_555 yes O(4) C(4) C(2) 111.7(4) 1_555 1_555 1_555 yes O(2) C(5) H(1) 109.5(4) 1_555 1_555 1_555 no O(2) C(5) H(2) 109.5(4) 1_555 1_555 1_555 no O(2) C(5) H(3) 109.5(5) 1_555 1_555 1_555 no H(1) C(5) H(2) 109.5(6) 1_555 1_555 1_555 no H(1) C(5) H(3) 109.5(5) 1_555 1_555 1_555 no H(2) C(5) H(3) 109.5(5) 1_555 1_555 1_555 no O(4) C(6) H(4) 109.5(4) 1_555 1_555 1_555 no O(4) C(6) H(5) 109.5(4) 1_555 1_555 1_555 no O(4) C(6) H(6) 109.5(4) 1_555 1_555 1_555 no H(4) C(6) H(5) 109.5(5) 1_555 1_555 1_555 no H(4) C(6) H(6) 109.5(5) 1_555 1_555 1_555 no H(5) C(6) H(6) 109.5(5) 1_555 1_555 1_555 no Ir C(7) C(8) 109.9(3) 1_555 1_555 1_555 yes Ir C(7) C(9) 125.5(3) 1_555 1_555 1_555 yes C(8) C(7) C(9) 124.6(4) 1_555 1_555 1_555 yes Se(2) C(8) C(7) 103.1(3) 1_555 1_555 1_555 yes Se(2) C(8) C(10) 120.7(3) 1_555 1_555 1_555 yes C(7) C(8) C(10) 135.9(4) 1_555 1_555 1_555 yes O(5) C(9) O(6) 123.8(4) 1_555 1_555 1_555 yes O(5) C(9) C(7) 123.0(4) 1_555 1_555 1_555 yes O(6) C(9) C(7) 113.2(3) 1_555 1_555 1_555 yes O(7) C(10) O(8) 123.5(5) 1_555 1_555 1_555 yes O(7) C(10) C(8) 125.6(5) 1_555 1_555 1_555 yes O(8) C(10) C(8) 110.7(4) 1_555 1_555 1_555 yes O(6) C(11) H(7) 109.4(5) 1_555 1_555 1_555 no O(6) C(11) H(8) 109.5(5) 1_555 1_555 1_555 no O(6) C(11) H(9) 109.5(5) 1_555 1_555 1_555 no H(7) C(11) H(8) 109.5(6) 1_555 1_555 1_555 no H(7) C(11) H(9) 109.5(6) 1_555 1_555 1_555 no H(8) C(11) H(9) 109.5(5) 1_555 1_555 1_555 no O(8) C(12) H(10) 109.5(6) 1_555 1_555 1_555 no O(8) C(12) H(11) 109.5(5) 1_555 1_555 1_555 no O(8) C(12) H(12) 109.5(5) 1_555 1_555 1_555 no H(10) C(12) H(11) 109.5(6) 1_555 1_555 1_555 no H(10) C(12) H(12) 109.5(6) 1_555 1_555 1_555 no H(11) C(12) H(12) 109.4(7) 1_555 1_555 1_555 no Ir C(13) C(14) 70.5(2) 1_555 1_555 1_555 yes Ir C(13) C(17) 72.8(2) 1_555 1_555 1_555 yes Ir C(13) C(18) 124.9(3) 1_555 1_555 1_555 yes C(14) C(13) C(17) 108.8(4) 1_555 1_555 1_555 yes C(14) C(13) C(18) 126.2(5) 1_555 1_555 1_555 yes C(17) C(13) C(18) 124.9(5) 1_555 1_555 1_555 yes Ir C(14) C(13) 71.6(2) 1_555 1_555 1_555 yes Ir C(14) C(15) 70.9(2) 1_555 1_555 1_555 yes Ir C(14) C(19) 127.7(3) 1_555 1_555 1_555 yes C(13) C(14) C(15) 107.4(4) 1_555 1_555 1_555 yes C(13) C(14) C(19) 126.8(5) 1_555 1_555 1_555 yes C(15) C(14) C(19) 125.4(5) 1_555 1_555 1_555 yes Ir C(15) C(14) 70.7(2) 1_555 1_555 1_555 yes Ir C(15) C(16) 72.3(2) 1_555 1_555 1_555 yes Ir C(15) C(20) 126.9(3) 1_555 1_555 1_555 yes C(14) C(15) C(16) 107.5(4) 1_555 1_555 1_555 yes C(14) C(15) C(20) 125.8(5) 1_555 1_555 1_555 yes C(16) C(15) C(20) 126.5(5) 1_555 1_555 1_555 yes Ir C(16) C(15) 69.7(2) 1_555 1_555 1_555 yes Ir C(16) C(17) 72.2(2) 1_555 1_555 1_555 yes Ir C(16) C(21) 125.1(3) 1_555 1_555 1_555 yes C(15) C(16) C(17) 108.6(4) 1_555 1_555 1_555 yes C(15) C(16) C(21) 126.0(4) 1_555 1_555 1_555 yes C(17) C(16) C(21) 125.4(4) 1_555 1_555 1_555 yes Ir C(17) C(13) 69.7(2) 1_555 1_555 1_555 yes Ir C(17) C(16) 70.7(2) 1_555 1_555 1_555 yes Ir C(17) C(22) 126.9(3) 1_555 1_555 1_555 yes C(13) C(17) C(16) 107.7(4) 1_555 1_555 1_555 yes C(13) C(17) C(22) 126.3(4) 1_555 1_555 1_555 yes C(16) C(17) C(22) 126.0(5) 1_555 1_555 1_555 yes C(13) C(18) H(13) 109.5(5) 1_555 1_555 1_555 no C(13) C(18) H(14) 109.4(5) 1_555 1_555 1_555 no C(13) C(18) H(15) 109.4(6) 1_555 1_555 1_555 no H(13) C(18) H(14) 109.5(7) 1_555 1_555 1_555 no H(13) C(18) H(15) 109.5(6) 1_555 1_555 1_555 no H(14) C(18) H(15) 109.5(5) 1_555 1_555 1_555 no C(14) C(19) H(16) 109.4(6) 1_555 1_555 1_555 no C(14) C(19) H(17) 109.4(5) 1_555 1_555 1_555 no C(14) C(19) H(18) 109.4(5) 1_555 1_555 1_555 no H(16) C(19) H(17) 109.5(5) 1_555 1_555 1_555 no H(16) C(19) H(18) 109.5(6) 1_555 1_555 1_555 no H(17) C(19) H(18) 109.5(7) 1_555 1_555 1_555 no C(15) C(20) H(19) 109.5(5) 1_555 1_555 1_555 no C(15) C(20) H(20) 109.4(4) 1_555 1_555 1_555 no C(15) C(20) H(21) 109.4(5) 1_555 1_555 1_555 no H(19) C(20) H(20) 109.5(5) 1_555 1_555 1_555 no H(19) C(20) H(21) 109.5(5) 1_555 1_555 1_555 no H(20) C(20) H(21) 109.5(6) 1_555 1_555 1_555 no C(16) C(21) H(22) 109.5(4) 1_555 1_555 1_555 no C(16) C(21) H(23) 109.5(5) 1_555 1_555 1_555 no C(16) C(21) H(24) 109.5(5) 1_555 1_555 1_555 no H(22) C(21) H(23) 109.5(5) 1_555 1_555 1_555 no H(22) C(21) H(24) 109.5(6) 1_555 1_555 1_555 no H(23) C(21) H(24) 109.5(5) 1_555 1_555 1_555 no C(17) C(22) H(25) 109.4(4) 1_555 1_555 1_555 no C(17) C(22) H(26) 109.5(4) 1_555 1_555 1_555 no C(17) C(22) H(27) 109.5(5) 1_555 1_555 1_555 no H(25) C(22) H(26) 109.5(6) 1_555 1_555 1_555 no H(25) C(22) H(27) 109.5(5) 1_555 1_555 1_555 no H(26) C(22) H(27) 109.5(5) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===END data_[Cp*Ir{Se2C2H(COOMe)}]2_(10) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 8 19:11:46 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 569.44 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H19 Ir O2 Se2 ' _chemical_formula_moiety 'C14 H19 Ir O2 Se2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 19.843(5) _cell_length_b 9.233(2) _cell_length_c 17.291(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3167.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.2 _cell_measurement_theta_max 19.9 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,1/2+z 1/2+x,1/2-y,-z -x,y,1/2-z -x,-y,-z 1/2+x,1/2+y,1/2-z 1/2-x,1/2+y,z x,-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112.00 _exptl_absorpt_coefficient_mu 13.046 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 1 2 0 2 3 1 1 2 _diffrn_reflns_number 0 _reflns_number_total 0 _reflns_number_gt 2380 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03606 _diffrn_orient_matrix_UB_12 0.07294 _diffrn_orient_matrix_UB_13 -0.01073 _diffrn_orient_matrix_UB_21 -0.03234 _diffrn_orient_matrix_UB_22 0.05728 _diffrn_orient_matrix_UB_23 -0.03212 _diffrn_orient_matrix_UB_31 -0.01391 _diffrn_orient_matrix_UB_32 0.05595 _diffrn_orient_matrix_UB_33 0.04688 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.08348(3) 0.08529(5) 0.19953(3) 0.0292(1) Uani 1.00 d . . . Se(1) Se 0.09257(8) 0.3470(2) 0.17820(10) 0.0473(5) Uani 1.00 d . . . Se(2) Se -0.03692(7) 0.1032(1) 0.16671(7) 0.0293(3) Uani 1.00 d . . . O(1) O -0.1564(7) 0.269(1) 0.0963(7) 0.067(4) Uani 1.00 d . . . O(2) O -0.1082(6) 0.477(1) 0.0712(7) 0.070(4) Uani 1.00 d . . . C(1) C 0.0104(9) 0.390(2) 0.126(1) 0.081(7) Uani 1.00 d . . . C(2) C -0.0450(9) 0.303(2) 0.1287(7) 0.040(4) Uani 1.00 d . . . C(3) C -0.1014(9) 0.338(1) 0.1062(9) 0.046(5) Uani 1.00 d . . . C(4) C -0.171(1) 0.528(2) 0.037(1) 0.087(8) Uani 1.00 d . . . C(5) C 0.1881(7) 0.051(2) 0.1579(9) 0.040(4) Uani 1.00 d . . . C(6) C 0.1769(7) -0.033(2) 0.2266(9) 0.046(4) Uani 1.00 d . . . C(7) C 0.1229(7) -0.134(1) 0.2137(9) 0.039(4) Uani 1.00 d . . . C(8) C 0.1020(7) -0.117(2) 0.1345(9) 0.039(4) Uani 1.00 d . . . C(9) C 0.1405(7) -0.002(2) 0.1000(8) 0.038(4) Uani 1.00 d . . . C(10) C 0.2413(9) 0.162(2) 0.147(1) 0.068(6) Uani 1.00 d . . . C(11) C 0.2157(9) -0.025(2) 0.2993(10) 0.071(6) Uani 1.00 d . . . C(12) C 0.1017(10) -0.251(2) 0.267(1) 0.066(6) Uani 1.00 d . . . C(13) C 0.0536(9) -0.209(2) 0.092(1) 0.070(6) Uani 1.00 d . . . C(14) C 0.1381(9) 0.049(2) 0.018(1) 0.070(6) Uani 1.00 d . . . H(1) H 0.0079 0.4761 0.0965 0.0967 Uiso 1.00 calc . . . H(2) H -0.1648 0.6236 0.0178 0.1043 Uiso 1.00 calc . . . H(3) H -0.1840 0.4657 -0.0034 0.1043 Uiso 1.00 calc . . . H(4) H -0.2051 0.5294 0.0760 0.1043 Uiso 1.00 calc . . . H(5) H 0.2844 0.1189 0.1536 0.0820 Uiso 1.00 calc . . . H(6) H 0.2380 0.2017 0.0964 0.0820 Uiso 1.00 calc . . . H(7) H 0.2356 0.2372 0.1841 0.0820 Uiso 1.00 calc . . . H(8) H 0.2370 -0.1151 0.3088 0.0847 Uiso 1.00 calc . . . H(9) H 0.2489 0.0490 0.2950 0.0847 Uiso 1.00 calc . . . H(10) H 0.1861 -0.0026 0.3408 0.0847 Uiso 1.00 calc . . . H(11) H 0.0887 -0.2093 0.3152 0.0790 Uiso 1.00 calc . . . H(12) H 0.0646 -0.3013 0.2454 0.0790 Uiso 1.00 calc . . . H(13) H 0.1381 -0.3157 0.2750 0.0790 Uiso 1.00 calc . . . H(14) H 0.0196 -0.1496 0.0696 0.0839 Uiso 1.00 calc . . . H(15) H 0.0766 -0.2598 0.0521 0.0839 Uiso 1.00 calc . . . H(16) H 0.0335 -0.2761 0.1264 0.0839 Uiso 1.00 calc . . . H(17) H 0.1801 0.0301 -0.0061 0.0837 Uiso 1.00 calc . . . H(18) H 0.1033 -0.0003 -0.0086 0.0837 Uiso 1.00 calc . . . H(19) H 0.1294 0.1504 0.0173 0.0837 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir 0.0265(3) 0.0360(3) 0.0251(3) -0.0023(2) 0.0015(2) -0.0042(2) Se(1) 0.0478(10) 0.0425(8) 0.0518(10) -0.0133(7) -0.0014(8) 0.0041(7) Se(2) 0.0318(7) 0.0330(6) 0.0230(6) -0.0009(6) -0.0022(6) 0.0005(6) O(1) 0.066(9) 0.062(7) 0.073(9) 0.011(7) 0.000(7) 0.021(7) O(2) 0.066(8) 0.076(8) 0.067(8) 0.010(7) -0.007(7) 0.022(7) C(1) 0.05(1) 0.022(7) 0.17(2) 0.014(7) -0.04(1) -0.002(10) C(2) 0.07(1) 0.039(8) 0.010(6) -0.007(8) 0.003(7) -0.001(5) C(3) 0.07(1) 0.028(7) 0.038(9) 0.004(8) 0.050(9) 0.004(7) C(4) 0.08(1) 0.11(2) 0.07(1) 0.01(1) -0.01(1) 0.05(1) C(5) 0.023(7) 0.057(9) 0.040(9) -0.002(6) 0.009(6) -0.020(7) C(6) 0.031(8) 0.065(10) 0.041(9) 0.014(7) -0.007(7) -0.007(8) C(7) 0.025(7) 0.040(7) 0.053(10) -0.001(6) 0.001(7) -0.008(7) C(8) 0.036(8) 0.048(8) 0.033(8) -0.006(6) 0.010(7) -0.016(7) C(9) 0.032(8) 0.051(8) 0.032(8) -0.008(7) 0.011(7) -0.008(7) C(10) 0.04(1) 0.09(1) 0.07(1) -0.019(10) 0.019(10) -0.03(1) C(11) 0.05(1) 0.11(2) 0.05(1) 0.03(1) -0.022(9) -0.03(1) C(12) 0.08(1) 0.06(1) 0.06(1) 0.024(10) 0.03(1) 0.006(10) C(13) 0.07(1) 0.06(1) 0.09(1) -0.024(9) 0.03(1) -0.038(10) C(14) 0.06(1) 0.11(2) 0.04(1) -0.01(1) 0.012(9) -0.01(1) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00031|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0006(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2380 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.927 _refine_ls_shift/su_max 0.0480 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -2.64 _refine_diff_density_max 3.60 #------------------------------------------------------------------------------ _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 Se(1) 2.451(2) 1_555 1_555 yes Ir Se(2) 2.461(2) 1_555 1_555 yes Ir Se(2) 2.496(1) 1_555 4_555 yes Ir C(5) 2.22(1) 1_555 1_555 yes Ir C(6) 2.20(2) 1_555 1_555 yes Ir C(7) 2.19(1) 1_555 1_555 yes Ir C(8) 2.21(1) 1_555 1_555 yes Ir C(9) 2.21(1) 1_555 1_555 yes Se(1) C(1) 1.91(2) 1_555 1_555 yes Se(2) C(2) 1.97(1) 1_555 1_555 yes O(1) C(3) 1.27(2) 1_555 1_555 yes O(2) C(3) 1.43(2) 1_555 1_555 yes O(2) C(4) 1.45(2) 1_555 1_555 yes C(1) C(2) 1.36(2) 1_555 1_555 yes C(2) C(3) 1.23(3) 1_555 1_555 yes C(5) C(6) 1.44(2) 1_555 1_555 yes C(5) C(9) 1.46(2) 1_555 1_555 yes C(5) C(10) 1.48(2) 1_555 1_555 yes C(6) C(7) 1.44(2) 1_555 1_555 yes C(6) C(11) 1.48(2) 1_555 1_555 yes C(7) C(8) 1.44(2) 1_555 1_555 yes C(7) C(12) 1.48(2) 1_555 1_555 yes C(8) C(9) 1.44(2) 1_555 1_555 yes C(8) C(13) 1.48(2) 1_555 1_555 yes C(9) C(14) 1.49(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Ir Se(2) 88.32(5) 1_555 1_555 1_555 yes Se(1) Ir Se(2) 95.83(5) 1_555 1_555 4_555 yes Se(1) Ir C(5) 91.3(4) 1_555 1_555 1_555 yes Se(1) Ir C(6) 117.4(4) 1_555 1_555 1_555 yes Se(1) Ir C(7) 154.8(4) 1_555 1_555 1_555 yes Se(1) Ir C(8) 138.1(4) 1_555 1_555 1_555 yes Se(1) Ir C(9) 101.8(4) 1_555 1_555 1_555 yes Se(2) Ir Se(2) 81.37(5) 1_555 1_555 4_555 yes Se(2) Ir C(5) 147.4(4) 1_555 1_555 1_555 yes Se(2) Ir C(6) 154.1(4) 1_555 1_555 1_555 yes Se(2) Ir C(7) 115.8(4) 1_555 1_555 1_555 yes Se(2) Ir C(8) 95.8(4) 1_555 1_555 1_555 yes Se(2) Ir C(9) 110.0(4) 1_555 1_555 1_555 yes Se(2) Ir C(5) 131.0(4) 4_555 1_555 1_555 yes Se(2) Ir C(6) 98.5(4) 4_555 1_555 1_555 yes Se(2) Ir C(7) 95.1(4) 4_555 1_555 1_555 yes Se(2) Ir C(8) 126.0(4) 4_555 1_555 1_555 yes Se(2) Ir C(9) 159.1(4) 4_555 1_555 1_555 yes C(5) Ir C(6) 37.9(6) 1_555 1_555 1_555 yes C(5) Ir C(7) 64.5(5) 1_555 1_555 1_555 yes C(5) Ir C(8) 63.9(5) 1_555 1_555 1_555 yes C(5) Ir C(9) 38.5(5) 1_555 1_555 1_555 yes C(6) Ir C(7) 38.3(6) 1_555 1_555 1_555 yes C(6) Ir C(8) 63.2(6) 1_555 1_555 1_555 yes C(6) Ir C(9) 63.5(5) 1_555 1_555 1_555 yes C(7) Ir C(8) 38.2(6) 1_555 1_555 1_555 yes C(7) Ir C(9) 64.3(6) 1_555 1_555 1_555 yes C(8) Ir C(9) 37.9(5) 1_555 1_555 1_555 yes Ir Se(1) C(1) 102.2(4) 1_555 1_555 1_555 yes Ir Se(2) Ir 98.12(5) 1_555 1_555 4_555 yes Ir Se(2) C(2) 102.7(5) 1_555 1_555 1_555 yes Ir Se(2) C(2) 110.0(4) 4_555 1_555 1_555 yes C(3) O(2) C(4) 122(1) 1_555 1_555 1_555 yes Se(1) C(1) C(2) 123(1) 1_555 1_555 1_555 yes Se(1) C(1) H(1) 118(1) 1_555 1_555 1_555 no C(2) C(1) H(1) 118(1) 1_555 1_555 1_555 no Se(2) C(2) C(1) 119(1) 1_555 1_555 1_555 yes Se(2) C(2) C(3) 115(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 125(1) 1_555 1_555 1_555 yes O(1) C(3) O(2) 107(1) 1_555 1_555 1_555 yes O(1) C(3) C(2) 134(1) 1_555 1_555 1_555 yes O(2) C(3) C(2) 117(1) 1_555 1_555 1_555 yes O(2) C(4) H(2) 109(1) 1_555 1_555 1_555 no O(2) C(4) H(3) 109(1) 1_555 1_555 1_555 no O(2) C(4) H(4) 109(1) 1_555 1_555 1_555 no H(2) C(4) H(3) 109(1) 1_555 1_555 1_555 no H(2) C(4) H(4) 109(2) 1_555 1_555 1_555 no H(3) C(4) H(4) 109(2) 1_555 1_555 1_555 no Ir C(5) C(6) 70.4(8) 1_555 1_555 1_555 yes Ir C(5) C(9) 70.4(7) 1_555 1_555 1_555 yes Ir C(5) C(10) 127(1) 1_555 1_555 1_555 yes C(6) C(5) C(9) 106(1) 1_555 1_555 1_555 yes C(6) C(5) C(10) 126(1) 1_555 1_555 1_555 yes C(9) C(5) C(10) 127(1) 1_555 1_555 1_555 yes Ir C(6) C(5) 71.7(8) 1_555 1_555 1_555 yes Ir C(6) C(7) 70.3(8) 1_555 1_555 1_555 yes Ir C(6) C(11) 126(1) 1_555 1_555 1_555 yes C(5) C(6) C(7) 109(1) 1_555 1_555 1_555 yes C(5) C(6) C(11) 126(1) 1_555 1_555 1_555 yes C(7) C(6) C(11) 123(1) 1_555 1_555 1_555 yes Ir C(7) C(6) 71.4(8) 1_555 1_555 1_555 yes Ir C(7) C(8) 71.7(8) 1_555 1_555 1_555 yes Ir C(7) C(12) 129(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 106(1) 1_555 1_555 1_555 yes C(6) C(7) C(12) 125(1) 1_555 1_555 1_555 yes C(8) C(7) C(12) 126(1) 1_555 1_555 1_555 yes Ir C(8) C(7) 70.0(8) 1_555 1_555 1_555 yes Ir C(8) C(9) 71.1(8) 1_555 1_555 1_555 yes Ir C(8) C(13) 129(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 108(1) 1_555 1_555 1_555 yes C(7) C(8) C(13) 126(1) 1_555 1_555 1_555 yes C(9) C(8) C(13) 124(1) 1_555 1_555 1_555 yes Ir C(9) C(5) 71.1(8) 1_555 1_555 1_555 yes Ir C(9) C(8) 71.0(8) 1_555 1_555 1_555 yes Ir C(9) C(14) 127(1) 1_555 1_555 1_555 yes C(5) C(9) C(8) 107(1) 1_555 1_555 1_555 yes C(5) C(9) C(14) 124(1) 1_555 1_555 1_555 yes C(8) C(9) C(14) 127(1) 1_555 1_555 1_555 yes C(5) C(10) H(5) 109(1) 1_555 1_555 1_555 no C(5) C(10) H(6) 109(1) 1_555 1_555 1_555 no C(5) C(10) H(7) 109(1) 1_555 1_555 1_555 no H(5) C(10) H(6) 109(1) 1_555 1_555 1_555 no H(5) C(10) H(7) 109(1) 1_555 1_555 1_555 no H(6) C(10) H(7) 109(1) 1_555 1_555 1_555 no C(6) C(11) H(8) 109(1) 1_555 1_555 1_555 no C(6) C(11) H(9) 109(1) 1_555 1_555 1_555 no C(6) C(11) H(10) 109(1) 1_555 1_555 1_555 no H(8) C(11) H(9) 109(1) 1_555 1_555 1_555 no H(8) C(11) H(10) 109(1) 1_555 1_555 1_555 no H(9) C(11) H(10) 109(1) 1_555 1_555 1_555 no C(7) C(12) H(11) 109(1) 1_555 1_555 1_555 no C(7) C(12) H(12) 109(1) 1_555 1_555 1_555 no C(7) C(12) H(13) 109(1) 1_555 1_555 1_555 no H(11) C(12) H(12) 109(1) 1_555 1_555 1_555 no H(11) C(12) H(13) 109(1) 1_555 1_555 1_555 no H(12) C(12) H(13) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(14) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(15) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(16) 109(1) 1_555 1_555 1_555 no H(14) C(13) H(15) 109(2) 1_555 1_555 1_555 no H(14) C(13) H(16) 109(1) 1_555 1_555 1_555 no H(15) C(13) H(16) 109(1) 1_555 1_555 1_555 no C(9) C(14) H(17) 109(1) 1_555 1_555 1_555 no C(9) C(14) H(18) 109(1) 1_555 1_555 1_555 no C(9) C(14) H(19) 109(1) 1_555 1_555 1_555 no H(17) C(14) H(18) 109(1) 1_555 1_555 1_555 no H(17) C(14) H(19) 109(1) 1_555 1_555 1_555 no H(18) C(14) H(19) 109(1) 1_555 1_555 1_555 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 Ir Ir 3.745(1) 1_555 4_555 yes #------------------------------------------------------------------------------ #===END data_[Cp*Ir{S2C2(COOMe)2}]_(11) #------------------------------------------------------------------------------ _audit_creation_date 'Sat Jan 16 16:24:23 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 533.68 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H21 Ir O4 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 16.064(2) _cell_length_b 16.083(2) _cell_length_c 16.387(1) _cell_angle_alpha 115.234(7) _cell_angle_beta 92.887(9) _cell_angle_gamma 91.30(1) _cell_volume 3820.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.9 _cell_measurement_theta_max 19.4 #------------------------------------------------------------------------------ _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 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064.00 _exptl_absorpt_coefficient_mu 7.242 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.06 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 -3 -2 -2 -1 -2 -1 -1 _diffrn_reflns_number 18158 _reflns_number_total 17526 _reflns_number_gt 8972 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.084 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05740 _diffrn_orient_matrix_UB_12 0.00195 _diffrn_orient_matrix_UB_13 -0.02555 _diffrn_orient_matrix_UB_21 0.01105 _diffrn_orient_matrix_UB_22 0.06618 _diffrn_orient_matrix_UB_23 0.01353 _diffrn_orient_matrix_UB_31 0.02185 _diffrn_orient_matrix_UB_32 -0.01875 _diffrn_orient_matrix_UB_33 -0.06112 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.58879(5) 0.15802(5) 0.23785(5) 0.0438(2) Uani 1.00 d . . . Ir(2) Ir 0.30784(5) 0.47870(5) 0.25797(6) 0.0540(3) Uani 1.00 d . . . Ir(3) Ir 0.62401(5) 0.78453(5) 0.25103(5) 0.0448(2) Uani 1.00 d . . . Ir(4) Ir 0.91939(5) 0.45078(5) 0.24866(6) 0.0554(3) Uani 1.00 d . . . S(1) S 0.4742(3) 0.0828(3) 0.1524(3) 0.053(1) Uani 1.00 d . . . S(2) S 0.5082(3) 0.2159(3) 0.3537(3) 0.053(2) Uani 1.00 d . . . S(3) S 0.2924(4) 0.5236(4) 0.1470(4) 0.066(2) Uani 1.00 d . . . S(4) S 0.2926(4) 0.6239(4) 0.3545(4) 0.070(2) Uani 1.00 d . . . S(5) S 0.7164(3) 0.7492(4) 0.1464(4) 0.057(2) Uani 1.00 d . . . S(6) S 0.7315(3) 0.8423(4) 0.3541(4) 0.062(2) Uani 1.00 d . . . S(7) S 0.9036(3) 0.3083(4) 0.1415(4) 0.059(2) Uani 1.00 d . . . S(8) S 0.9485(4) 0.3898(4) 0.3461(4) 0.062(2) Uani 1.00 d . . . O(1) O 0.306(1) -0.023(1) 0.148(1) 0.105(7) Uani 1.00 d . . . O(2) O 0.2535(9) 0.1142(10) 0.183(1) 0.082(6) Uani 1.00 d . . . O(3) O 0.347(1) 0.264(1) 0.446(1) 0.085(6) Uani 1.00 d . . . O(4) O 0.2846(9) 0.130(1) 0.3595(10) 0.068(5) Uani 1.00 d . . . O(5) O 0.300(1) 0.674(1) 0.075(1) 0.101(7) Uani 1.00 d . . . O(6) O 0.1944(9) 0.739(1) 0.162(1) 0.077(6) Uani 1.00 d . . . O(7) O 0.225(2) 0.813(1) 0.409(2) 0.17(1) Uani 1.00 d . . . O(8) O 0.306(1) 0.837(1) 0.317(2) 0.118(8) Uani 1.00 d . . . O(9) O 0.949(1) 0.730(1) 0.168(1) 0.117(8) Uani 1.00 d . . . O(10) O 0.879(1) 0.771(1) 0.075(1) 0.103(7) Uani 1.00 d . . . O(11) O 0.915(1) 0.850(2) 0.419(1) 0.136(9) Uani 1.00 d . . . O(12) O 0.9517(9) 0.899(1) 0.317(1) 0.093(7) Uani 1.00 d . . . O(13) O 0.918(2) 0.105(1) 0.051(1) 0.139(9) Uani 1.00 d . . . O(14) O 0.924(1) 0.0850(10) 0.174(1) 0.100(7) Uani 1.00 d . . . O(15) O 1.042(1) 0.192(2) 0.334(1) 0.120(9) Uani 1.00 d . . . O(16) O 0.9159(9) 0.2039(10) 0.3791(10) 0.069(5) Uani 1.00 d . . . C(1) C 0.684(1) 0.175(2) 0.155(1) 0.063(7) Uani 1.00 d . . . C(2) C 0.694(1) 0.249(1) 0.248(1) 0.054(6) Uani 1.00 d . . . C(3) C 0.714(1) 0.211(1) 0.304(1) 0.047(5) Uani 1.00 d . . . C(4) C 0.711(1) 0.111(1) 0.253(1) 0.050(6) Uani 1.00 d . . . C(5) C 0.693(1) 0.090(1) 0.160(1) 0.062(7) Uani 1.00 d . . . C(6) C 0.669(2) 0.188(3) 0.072(2) 0.13(1) Uani 1.00 d . . . C(7) C 0.692(1) 0.347(2) 0.272(2) 0.083(9) Uani 1.00 d . . . C(8) C 0.728(2) 0.264(2) 0.407(1) 0.087(8) Uani 1.00 d . . . C(9) C 0.730(2) 0.042(2) 0.288(2) 0.093(10) Uani 1.00 d . . . C(10) C 0.691(1) -0.002(2) 0.086(2) 0.105(9) Uani 1.00 d . . . C(11) C 0.397(1) 0.108(1) 0.221(1) 0.042(5) Uani 1.00 d . . . C(12) C 0.409(1) 0.169(1) 0.315(1) 0.045(6) Uani 1.00 d . . . C(13) C 0.313(1) 0.059(2) 0.179(1) 0.063(7) Uani 1.00 d . . . C(14) C 0.170(1) 0.069(2) 0.149(2) 0.11(1) Uani 1.00 d . . . C(15) C 0.345(1) 0.194(1) 0.380(1) 0.061(7) Uani 1.00 d . . . C(16) C 0.215(1) 0.151(2) 0.414(2) 0.081(8) Uani 1.00 d . . . C(17) C 0.254(1) 0.359(2) 0.259(2) 0.081(8) Uani 1.00 d . . . C(18) C 0.293(3) 0.403(2) 0.334(2) 0.15(2) Uani 1.00 d . . . C(19) C 0.375(3) 0.410(2) 0.329(3) 0.19(2) Uani 1.00 d . . . C(20) C 0.385(2) 0.364(2) 0.230(2) 0.071(9) Uani 1.00 d . . . C(21) C 0.308(1) 0.329(1) 0.190(1) 0.056(6) Uani 1.00 d . . . C(22) C 0.158(3) 0.333(2) 0.246(3) 0.17(2) Uani 1.00 d . . . C(23) C 0.263(5) 0.446(3) 0.433(3) 0.34(3) Uani 1.00 d . . . C(24) C 0.454(4) 0.457(2) 0.390(4) 0.34(3) Uani 1.00 d . . . C(25) C 0.462(2) 0.350(2) 0.179(4) 0.20(2) Uani 1.00 d . . . C(26) C 0.285(3) 0.270(2) 0.094(2) 0.15(1) Uani 1.00 d . . . C(27) C 0.277(1) 0.641(1) 0.200(1) 0.048(6) Uani 1.00 d . . . C(28) C 0.277(1) 0.683(1) 0.291(2) 0.060(7) Uani 1.00 d . . . C(29) C 0.261(2) 0.685(1) 0.135(2) 0.074(9) Uani 1.00 d . . . C(30) C 0.178(2) 0.793(2) 0.113(2) 0.12(1) Uani 1.00 d . . . C(31) C 0.266(2) 0.782(2) 0.342(2) 0.084(9) Uani 1.00 d . . . C(32) C 0.282(2) 0.932(2) 0.381(4) 0.25(2) Uani 1.00 d . . . C(33) C 0.512(1) 0.700(2) 0.187(2) 0.068(7) Uani 1.00 d . . . C(34) C 0.498(1) 0.787(2) 0.189(1) 0.061(7) Uani 1.00 d . . . C(35) C 0.508(1) 0.851(1) 0.274(1) 0.059(7) Uani 1.00 d . . . C(36) C 0.516(1) 0.805(1) 0.337(1) 0.055(6) Uani 1.00 d . . . C(37) C 0.523(1) 0.708(1) 0.274(2) 0.070(8) Uani 1.00 d . . . C(38) C 0.511(2) 0.610(2) 0.098(2) 0.12(1) Uani 1.00 d . . . C(39) C 0.486(2) 0.809(2) 0.105(2) 0.10(1) Uani 1.00 d . . . C(40) C 0.499(2) 0.954(2) 0.311(2) 0.12(1) Uani 1.00 d . . . C(41) C 0.519(2) 0.847(2) 0.433(2) 0.10(1) Uani 1.00 d . . . C(42) C 0.531(2) 0.638(2) 0.310(2) 0.10(1) Uani 1.00 d . . . C(43) C 0.815(1) 0.786(1) 0.202(1) 0.050(6) Uani 1.00 d . . . C(44) C 0.819(1) 0.825(1) 0.296(2) 0.057(7) Uani 1.00 d . . . C(45) C 0.888(1) 0.758(2) 0.150(2) 0.085(10) Uani 1.00 d . . . C(46) C 0.946(2) 0.741(2) 0.016(2) 0.13(1) Uani 1.00 d . . . C(47) C 0.898(1) 0.859(2) 0.354(2) 0.069(8) Uani 1.00 d . . . C(48) C 1.037(2) 0.919(2) 0.357(3) 0.14(1) Uani 1.00 d . . . C(49) C 0.899(2) 0.534(2) 0.176(2) 0.09(1) Uani 1.00 d . . . C(50) C 0.840(2) 0.556(2) 0.248(4) 0.13(2) Uani 1.00 d . . . C(51) C 0.894(4) 0.590(2) 0.322(3) 0.13(2) Uani 1.00 d . . . C(52) C 0.971(4) 0.590(2) 0.312(3) 0.16(2) Uani 1.00 d . . . C(53) C 0.974(1) 0.555(2) 0.219(2) 0.070(8) Uani 1.00 d . . . C(54) C 0.873(3) 0.497(2) 0.074(3) 0.19(2) Uani 1.00 d . . . C(55) C 0.747(2) 0.549(3) 0.234(5) 0.31(3) Uani 1.00 d . . . C(56) C 0.862(4) 0.629(2) 0.418(3) 0.32(3) Uani 1.00 d . . . C(57) C 1.053(3) 0.621(2) 0.369(3) 0.22(2) Uani 1.00 d . . . C(58) C 1.054(2) 0.547(3) 0.168(3) 0.18(2) Uani 1.00 d . . . C(59) C 0.926(1) 0.236(1) 0.192(1) 0.046(5) Uani 1.00 d . . . C(60) C 0.945(1) 0.274(1) 0.285(1) 0.043(5) Uani 1.00 d . . . C(61) C 0.921(1) 0.137(1) 0.134(2) 0.067(8) Uani 1.00 d . . . C(62) C 0.931(2) -0.013(1) 0.123(2) 0.11(1) Uani 1.00 d . . . C(63) C 0.973(1) 0.215(1) 0.329(2) 0.064(7) Uani 1.00 d . . . C(64) C 0.934(2) 0.149(2) 0.427(2) 0.10(1) Uani 1.00 d . . . H(1) H 0.6677 0.2519 0.0868 0.1564 Uiso 1.00 calc . . . H(2) H 0.7136 0.1628 0.0333 0.1564 Uiso 1.00 calc . . . H(3) H 0.6180 0.1579 0.0412 0.1564 Uiso 1.00 calc . . . H(4) H 0.7466 0.3746 0.2932 0.1000 Uiso 1.00 calc . . . H(5) H 0.6749 0.3556 0.2195 0.1000 Uiso 1.00 calc . . . H(6) H 0.6545 0.3745 0.3173 0.1000 Uiso 1.00 calc . . . H(7) H 0.7419 0.2227 0.4322 0.1045 Uiso 1.00 calc . . . H(8) H 0.7716 0.3092 0.4205 0.1045 Uiso 1.00 calc . . . H(9) H 0.6779 0.2929 0.4307 0.1045 Uiso 1.00 calc . . . H(10) H 0.6836 -0.0012 0.2730 0.1117 Uiso 1.00 calc . . . H(11) H 0.7778 0.0111 0.2618 0.1117 Uiso 1.00 calc . . . H(12) H 0.7395 0.0722 0.3519 0.1117 Uiso 1.00 calc . . . H(13) H 0.6496 -0.0402 0.0944 0.1264 Uiso 1.00 calc . . . H(14) H 0.6786 0.0009 0.0298 0.1264 Uiso 1.00 calc . . . H(15) H 0.7441 -0.0278 0.0847 0.1264 Uiso 1.00 calc . . . H(16) H 0.1303 0.1151 0.1561 0.1268 Uiso 1.00 calc . . . H(17) H 0.1702 0.0285 0.0866 0.1268 Uiso 1.00 calc . . . H(18) H 0.1541 0.0361 0.1821 0.1268 Uiso 1.00 calc . . . H(19) H 0.2342 0.1653 0.4750 0.0973 Uiso 1.00 calc . . . H(20) H 0.1889 0.2023 0.4122 0.0973 Uiso 1.00 calc . . . H(21) H 0.1768 0.0994 0.3926 0.0973 Uiso 1.00 calc . . . H(22) H 0.1285 0.3882 0.2736 0.2146 Uiso 1.00 calc . . . H(23) H 0.1408 0.3015 0.1850 0.2146 Uiso 1.00 calc . . . H(24) H 0.1466 0.2954 0.2771 0.2146 Uiso 1.00 calc . . . H(25) H 0.2878 0.4175 0.4673 0.3950 Uiso 1.00 calc . . . H(26) H 0.2762 0.5102 0.4611 0.3950 Uiso 1.00 calc . . . H(27) H 0.2035 0.4360 0.4291 0.3950 Uiso 1.00 calc . . . H(28) H 0.4942 0.4131 0.3839 0.4171 Uiso 1.00 calc . . . H(29) H 0.4757 0.5033 0.3751 0.4171 Uiso 1.00 calc . . . H(30) H 0.4386 0.4846 0.4515 0.4171 Uiso 1.00 calc . . . H(31) H 0.4706 0.2856 0.1481 0.2382 Uiso 1.00 calc . . . H(32) H 0.4555 0.3744 0.1354 0.2382 Uiso 1.00 calc . . . H(33) H 0.5088 0.3796 0.2192 0.2382 Uiso 1.00 calc . . . H(34) H 0.2269 0.2567 0.0858 0.1787 Uiso 1.00 calc . . . H(35) H 0.3007 0.3018 0.0592 0.1787 Uiso 1.00 calc . . . H(36) H 0.3140 0.2148 0.0757 0.1787 Uiso 1.00 calc . . . H(37) H 0.2249 0.8325 0.1206 0.1386 Uiso 1.00 calc . . . H(38) H 0.1667 0.7529 0.0510 0.1386 Uiso 1.00 calc . . . H(39) H 0.1307 0.8280 0.1358 0.1386 Uiso 1.00 calc . . . H(40) H 0.3004 0.9440 0.4405 0.3037 Uiso 1.00 calc . . . H(41) H 0.3084 0.9763 0.3644 0.3037 Uiso 1.00 calc . . . H(42) H 0.2235 0.9362 0.3760 0.3037 Uiso 1.00 calc . . . H(43) H 0.4691 0.5680 0.0983 0.1443 Uiso 1.00 calc . . . H(44) H 0.4996 0.6242 0.0476 0.1443 Uiso 1.00 calc . . . H(45) H 0.5639 0.5839 0.0930 0.1443 Uiso 1.00 calc . . . H(46) H 0.5340 0.8429 0.1014 0.1220 Uiso 1.00 calc . . . H(47) H 0.4783 0.7534 0.0513 0.1220 Uiso 1.00 calc . . . H(48) H 0.4384 0.8448 0.1108 0.1220 Uiso 1.00 calc . . . H(49) H 0.5137 0.9821 0.3743 0.1403 Uiso 1.00 calc . . . H(50) H 0.5343 0.9795 0.2818 0.1403 Uiso 1.00 calc . . . H(51) H 0.4425 0.9663 0.3010 0.1403 Uiso 1.00 calc . . . H(52) H 0.5711 0.8365 0.4562 0.1255 Uiso 1.00 calc . . . H(53) H 0.5131 0.9115 0.4543 0.1255 Uiso 1.00 calc . . . H(54) H 0.4751 0.8213 0.4529 0.1255 Uiso 1.00 calc . . . H(55) H 0.4829 0.6362 0.3405 0.1214 Uiso 1.00 calc . . . H(56) H 0.5370 0.5791 0.2616 0.1214 Uiso 1.00 calc . . . H(57) H 0.5791 0.6532 0.3512 0.1214 Uiso 1.00 calc . . . H(58) H 0.9529 0.6773 -0.0020 0.1580 Uiso 1.00 calc . . . H(59) H 0.9346 0.7522 -0.0357 0.1580 Uiso 1.00 calc . . . H(60) H 0.9964 0.7746 0.0476 0.1580 Uiso 1.00 calc . . . H(61) H 1.0610 0.8637 0.3519 0.1675 Uiso 1.00 calc . . . H(62) H 1.0691 0.9459 0.3264 0.1675 Uiso 1.00 calc . . . H(63) H 1.0371 0.9609 0.4192 0.1675 Uiso 1.00 calc . . . H(64) H 0.8140 0.4921 0.0656 0.2257 Uiso 1.00 calc . . . H(65) H 0.8946 0.5382 0.0517 0.2257 Uiso 1.00 calc . . . H(66) H 0.8950 0.4382 0.0428 0.2257 Uiso 1.00 calc . . . H(67) H 0.7237 0.5669 0.2911 0.3748 Uiso 1.00 calc . . . H(68) H 0.7295 0.5877 0.2073 0.3748 Uiso 1.00 calc . . . H(69) H 0.7296 0.4868 0.1959 0.3748 Uiso 1.00 calc . . . H(70) H 0.9085 0.6478 0.4612 0.3849 Uiso 1.00 calc . . . H(71) H 0.8293 0.6800 0.4271 0.3849 Uiso 1.00 calc . . . H(72) H 0.8295 0.5823 0.4241 0.3849 Uiso 1.00 calc . . . H(73) H 1.0589 0.5882 0.4054 0.2683 Uiso 1.00 calc . . . H(74) H 1.0976 0.6085 0.3306 0.2683 Uiso 1.00 calc . . . H(75) H 1.0531 0.6850 0.4069 0.2683 Uiso 1.00 calc . . . H(76) H 1.0907 0.5080 0.1793 0.2179 Uiso 1.00 calc . . . H(77) H 1.0388 0.5227 0.1044 0.2179 Uiso 1.00 calc . . . H(78) H 1.0805 0.6067 0.1868 0.2179 Uiso 1.00 calc . . . H(79) H 0.8829 -0.0379 0.0821 0.1304 Uiso 1.00 calc . . . H(80) H 0.9794 -0.0249 0.0907 0.1304 Uiso 1.00 calc . . . H(81) H 0.9333 -0.0416 0.1637 0.1304 Uiso 1.00 calc . . . H(82) H 0.8879 0.1485 0.4607 0.1179 Uiso 1.00 calc . . . H(83) H 0.9435 0.0883 0.3848 0.1179 Uiso 1.00 calc . . . H(84) H 0.9822 0.1750 0.4666 0.1179 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0388(4) 0.0471(4) 0.0467(5) 0.0026(3) 0.0000(3) 0.0217(4) Ir(2) 0.0660(6) 0.0493(5) 0.0529(5) 0.0057(4) 0.0036(4) 0.0278(4) Ir(3) 0.0386(4) 0.0485(4) 0.0484(5) 0.0047(3) -0.0006(3) 0.0221(4) Ir(4) 0.0565(5) 0.0483(5) 0.0690(6) 0.0128(4) 0.0199(4) 0.0303(4) S(1) 0.046(3) 0.058(3) 0.045(3) -0.004(2) -0.004(2) 0.014(3) S(2) 0.044(3) 0.055(3) 0.054(3) -0.002(2) -0.003(2) 0.019(3) S(3) 0.088(4) 0.061(3) 0.059(4) 0.007(3) 0.007(3) 0.034(3) S(4) 0.099(5) 0.057(3) 0.056(4) 0.019(3) 0.002(3) 0.025(3) S(5) 0.043(3) 0.064(3) 0.056(3) -0.004(2) -0.005(2) 0.018(3) S(6) 0.055(3) 0.074(4) 0.058(3) -0.002(3) -0.012(3) 0.031(3) S(7) 0.062(3) 0.059(3) 0.063(3) 0.012(3) 0.008(3) 0.031(3) S(8) 0.078(4) 0.051(3) 0.051(3) 0.011(3) 0.004(3) 0.014(3) O(1) 0.06(1) 0.06(1) 0.16(2) -0.012(9) -0.01(1) 0.02(1) O(2) 0.046(9) 0.063(9) 0.13(1) -0.001(7) -0.025(9) 0.043(10) O(3) 0.09(1) 0.08(1) 0.06(1) 0.006(9) 0.026(9) 0.004(9) O(4) 0.048(9) 0.08(1) 0.07(1) -0.004(8) 0.025(8) 0.028(9) O(5) 0.12(2) 0.14(2) 0.10(1) 0.05(1) 0.06(1) 0.09(1) O(6) 0.064(10) 0.10(1) 0.10(1) 0.028(9) 0.023(9) 0.08(1) O(7) 0.32(4) 0.07(1) 0.14(2) 0.07(2) 0.06(2) 0.05(1) O(8) 0.07(1) 0.046(10) 0.21(2) -0.007(8) -0.02(1) 0.04(1) O(9) 0.06(1) 0.17(2) 0.16(2) 0.05(1) 0.03(1) 0.10(2) O(10) 0.06(1) 0.17(2) 0.10(1) 0.03(1) 0.04(1) 0.06(1) O(11) 0.07(1) 0.24(3) 0.12(2) -0.04(1) -0.06(1) 0.12(2) O(12) 0.05(1) 0.13(1) 0.12(1) -0.022(10) -0.033(10) 0.09(1) O(13) 0.25(3) 0.07(1) 0.08(1) 0.02(1) -0.01(2) 0.01(1) O(14) 0.17(2) 0.037(8) 0.09(1) 0.016(10) 0.02(1) 0.020(9) O(15) 0.07(1) 0.21(2) 0.14(2) 0.06(1) 0.03(1) 0.13(2) O(16) 0.07(1) 0.08(1) 0.07(1) 0.017(8) 0.003(8) 0.049(9) C(1) 0.04(1) 0.11(2) 0.06(1) 0.00(1) 0.011(10) 0.05(1) C(2) 0.06(1) 0.06(1) 0.05(1) 0.00(1) 0.003(10) 0.02(1) C(3) 0.05(1) 0.05(1) 0.026(9) 0.000(9) 0.022(8) 0.001(9) C(4) 0.06(1) 0.05(1) 0.05(1) 0.008(9) 0.000(10) 0.02(1) C(5) 0.03(1) 0.06(1) 0.07(2) 0.002(9) 0.006(10) 0.00(1) C(6) 0.06(2) 0.24(4) 0.13(3) -0.01(2) 0.01(2) 0.12(3) C(7) 0.07(2) 0.11(2) 0.08(2) 0.01(1) 0.03(1) 0.04(2) C(8) 0.09(2) 0.12(2) 0.03(1) 0.01(2) 0.01(1) 0.00(1) C(9) 0.08(2) 0.11(2) 0.12(2) 0.05(2) 0.05(2) 0.07(2) C(10) 0.05(1) 0.11(2) 0.08(2) 0.02(1) 0.01(1) -0.03(2) C(11) 0.04(1) 0.05(1) 0.05(1) 0.017(9) 0.021(9) 0.029(10) C(12) 0.032(10) 0.06(1) 0.05(1) 0.012(9) 0.020(9) 0.03(1) C(13) 0.06(1) 0.07(2) 0.06(1) 0.00(1) 0.00(1) 0.03(1) C(14) 0.04(1) 0.09(2) 0.17(3) -0.01(1) -0.04(2) 0.05(2) C(15) 0.09(2) 0.05(1) 0.04(1) 0.01(1) -0.01(1) 0.02(1) C(16) 0.05(1) 0.12(2) 0.07(2) 0.00(1) 0.01(1) 0.04(2) C(17) 0.08(2) 0.11(2) 0.07(2) 0.04(1) 0.07(1) 0.05(1) C(18) 0.33(6) 0.11(3) 0.04(2) 0.11(4) 0.07(3) 0.05(2) C(19) 0.28(5) 0.05(2) 0.21(5) -0.02(3) -0.18(5) 0.08(3) C(20) 0.08(2) 0.08(2) 0.08(2) 0.01(1) 0.01(1) 0.06(2) C(21) 0.07(2) 0.06(1) 0.02(1) 0.01(1) 0.020(10) 0.010(10) C(22) 0.18(4) 0.12(3) 0.25(5) 0.03(3) 0.14(4) 0.10(3) C(23) 0.8(1) 0.15(3) 0.21(5) 0.24(6) 0.30(7) 0.14(4) C(24) 0.51(9) 0.07(2) 0.38(7) -0.05(4) -0.39(7) 0.08(3) C(25) 0.10(3) 0.14(3) 0.44(7) 0.06(2) 0.07(4) 0.20(4) C(26) 0.25(4) 0.06(2) 0.12(3) -0.01(2) -0.05(3) 0.03(2) C(27) 0.05(1) 0.07(1) 0.04(1) 0.007(9) 0.016(9) 0.03(1) C(28) 0.05(1) 0.05(1) 0.09(2) 0.014(10) 0.00(1) 0.04(1) C(29) 0.08(2) 0.05(1) 0.10(2) -0.02(1) -0.02(2) 0.04(1) C(30) 0.11(2) 0.11(2) 0.15(3) 0.01(2) -0.03(2) 0.09(2) C(31) 0.12(2) 0.05(2) 0.06(2) 0.02(2) -0.04(2) 0.01(1) C(32) 0.10(3) 0.06(2) 0.50(9) -0.01(2) -0.06(4) 0.03(3) C(33) 0.03(1) 0.09(2) 0.06(2) 0.02(1) 0.03(1) 0.01(1) C(34) 0.03(1) 0.11(2) 0.04(1) 0.01(1) 0.013(9) 0.03(1) C(35) 0.06(1) 0.06(1) 0.06(1) 0.02(1) 0.00(1) 0.03(1) C(36) 0.06(1) 0.08(1) 0.03(1) 0.00(1) 0.003(9) 0.02(1) C(37) 0.03(1) 0.06(1) 0.11(2) -0.012(10) -0.01(1) 0.04(1) C(38) 0.07(2) 0.10(2) 0.12(2) -0.02(2) -0.01(2) -0.01(2) C(39) 0.09(2) 0.16(3) 0.07(2) 0.01(2) 0.00(1) 0.07(2) C(40) 0.08(2) 0.09(2) 0.21(3) 0.02(2) -0.01(2) 0.09(2) C(41) 0.08(2) 0.13(2) 0.12(3) 0.03(2) 0.02(2) 0.07(2) C(42) 0.07(2) 0.09(2) 0.19(3) 0.01(1) 0.02(2) 0.10(2) C(43) 0.04(1) 0.05(1) 0.06(1) 0.012(9) 0.009(10) 0.03(1) C(44) 0.04(1) 0.06(1) 0.09(2) 0.008(9) 0.01(1) 0.04(1) C(45) 0.05(2) 0.06(2) 0.15(3) 0.01(1) 0.01(2) 0.06(2) C(46) 0.09(2) 0.20(3) 0.11(3) 0.03(2) 0.04(2) 0.06(2) C(47) 0.06(1) 0.08(2) 0.08(2) -0.01(1) -0.02(1) 0.05(1) C(48) 0.05(2) 0.14(3) 0.20(4) -0.03(2) -0.04(2) 0.05(3) C(49) 0.12(2) 0.06(1) 0.12(2) 0.01(2) 0.04(2) 0.07(2) C(50) 0.06(2) 0.11(3) 0.31(6) 0.04(2) 0.09(3) 0.16(4) C(51) 0.22(6) 0.06(2) 0.15(4) 0.06(3) 0.10(4) 0.06(3) C(52) 0.28(6) 0.03(2) 0.14(4) -0.05(3) -0.14(4) 0.03(2) C(53) 0.04(1) 0.06(1) 0.13(2) 0.00(1) 0.01(1) 0.05(2) C(54) 0.28(5) 0.12(3) 0.19(4) -0.05(3) -0.09(4) 0.11(3) C(55) 0.07(2) 0.24(5) 0.8(1) 0.07(3) 0.10(4) 0.41(7) C(56) 0.7(1) 0.11(3) 0.26(5) 0.18(5) 0.38(7) 0.10(3) C(57) 0.35(7) 0.09(3) 0.21(5) -0.08(3) -0.14(5) 0.06(3) C(58) 0.15(3) 0.16(3) 0.31(5) 0.04(3) 0.14(4) 0.15(4) C(59) 0.05(1) 0.05(1) 0.05(1) 0.025(9) 0.020(9) 0.017(9) C(60) 0.04(1) 0.05(1) 0.04(1) 0.015(9) 0.015(8) 0.018(9) C(61) 0.05(1) 0.05(1) 0.09(2) 0.00(1) 0.00(1) 0.02(1) C(62) 0.15(3) 0.03(1) 0.12(2) 0.01(1) -0.03(2) 0.01(1) C(63) 0.06(1) 0.06(1) 0.08(2) 0.00(1) -0.01(1) 0.03(1) C(64) 0.12(2) 0.11(2) 0.10(2) 0.01(2) 0.00(2) 0.08(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0002(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8972 _refine_ls_number_parameters 830 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.995 _refine_ls_shift/su_max 1.0810 _refine_ls_shift/su_mean 0.0400 _refine_diff_density_min -2.99 _refine_diff_density_max 2.29 #------------------------------------------------------------------------------ _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) S(1) 2.238(5) 1_555 1_555 yes Ir(1) S(2) 2.223(5) 1_555 1_555 yes Ir(1) C(1) 2.17(2) 1_555 1_555 yes Ir(1) C(2) 2.16(2) 1_555 1_555 yes Ir(1) C(3) 2.20(2) 1_555 1_555 yes Ir(1) C(4) 2.16(2) 1_555 1_555 yes Ir(1) C(5) 2.17(2) 1_555 1_555 yes Ir(2) S(3) 2.230(7) 1_555 1_555 yes Ir(2) S(4) 2.221(5) 1_555 1_555 yes Ir(2) C(17) 2.10(3) 1_555 1_555 yes Ir(2) C(18) 2.10(4) 1_555 1_555 yes Ir(2) C(19) 2.19(6) 1_555 1_555 yes Ir(2) C(20) 2.14(3) 1_555 1_555 yes Ir(2) C(21) 2.18(2) 1_555 1_555 yes Ir(3) S(5) 2.221(6) 1_555 1_555 yes Ir(3) S(6) 2.235(5) 1_555 1_555 yes Ir(3) C(33) 2.16(2) 1_555 1_555 yes Ir(3) C(34) 2.22(2) 1_555 1_555 yes Ir(3) C(35) 2.14(2) 1_555 1_555 yes Ir(3) C(36) 2.23(2) 1_555 1_555 yes Ir(3) C(37) 2.15(2) 1_555 1_555 yes Ir(4) S(7) 2.213(5) 1_555 1_555 yes Ir(4) S(8) 2.239(7) 1_555 1_555 yes Ir(4) C(49) 2.16(3) 1_555 1_555 yes Ir(4) C(50) 2.15(4) 1_555 1_555 yes Ir(4) C(51) 2.11(4) 1_555 1_555 yes Ir(4) C(52) 2.15(3) 1_555 1_555 yes Ir(4) C(53) 2.13(3) 1_555 1_555 yes S(1) C(11) 1.66(2) 1_555 1_555 yes S(2) C(12) 1.72(2) 1_555 1_555 yes S(3) C(27) 1.74(2) 1_555 1_555 yes S(4) C(28) 1.70(3) 1_555 1_555 yes S(5) C(43) 1.75(2) 1_555 1_555 yes S(6) C(44) 1.70(2) 1_555 1_555 yes S(7) C(59) 1.73(2) 1_555 1_555 yes S(8) C(60) 1.69(2) 1_555 1_555 yes O(1) C(13) 1.19(3) 1_555 1_555 yes O(2) C(13) 1.31(3) 1_555 1_555 yes O(2) C(14) 1.48(3) 1_555 1_555 yes O(3) C(15) 1.19(2) 1_555 1_555 yes O(4) C(15) 1.31(3) 1_555 1_555 yes O(4) C(16) 1.42(3) 1_555 1_555 yes O(5) C(29) 1.15(4) 1_555 1_555 yes O(6) C(29) 1.37(3) 1_555 1_555 yes O(6) C(30) 1.42(4) 1_555 1_555 yes O(7) C(31) 1.24(4) 1_555 1_555 yes O(8) C(31) 1.29(4) 1_555 1_555 yes O(8) C(32) 1.51(4) 1_555 1_555 yes O(9) C(45) 1.17(3) 1_555 1_555 yes O(10) C(45) 1.34(4) 1_555 1_555 yes O(10) C(46) 1.44(4) 1_555 1_555 yes O(11) C(47) 1.16(4) 1_555 1_555 yes O(12) C(47) 1.37(3) 1_555 1_555 yes O(12) C(48) 1.46(3) 1_555 1_555 yes O(13) C(61) 1.23(4) 1_555 1_555 yes O(14) C(61) 1.27(4) 1_555 1_555 yes O(14) C(62) 1.45(2) 1_555 1_555 yes O(15) C(63) 1.19(3) 1_555 1_555 yes O(16) C(63) 1.32(3) 1_555 1_555 yes O(16) C(64) 1.43(4) 1_555 1_555 yes C(1) C(2) 1.48(3) 1_555 1_555 yes C(1) C(5) 1.40(4) 1_555 1_555 yes C(1) C(6) 1.48(5) 1_555 1_555 yes C(2) C(3) 1.35(3) 1_555 1_555 yes C(2) C(7) 1.45(4) 1_555 1_555 yes C(3) C(4) 1.46(2) 1_555 1_555 yes C(3) C(8) 1.52(2) 1_555 1_555 yes C(4) C(5) 1.43(3) 1_555 1_555 yes C(4) C(9) 1.48(4) 1_555 1_555 yes C(5) C(10) 1.47(3) 1_555 1_555 yes C(11) C(12) 1.42(2) 1_555 1_555 yes C(11) C(13) 1.52(3) 1_555 1_555 yes C(12) C(15) 1.46(3) 1_555 1_555 yes C(17) C(18) 1.26(4) 1_555 1_555 yes C(17) C(21) 1.39(3) 1_555 1_555 yes C(17) C(22) 1.57(5) 1_555 1_555 yes C(18) C(19) 1.34(8) 1_555 1_555 yes C(18) C(23) 1.57(6) 1_555 1_555 yes C(19) C(20) 1.49(6) 1_555 1_555 yes C(19) C(24) 1.53(7) 1_555 1_555 yes C(20) C(21) 1.36(3) 1_555 1_555 yes C(20) C(25) 1.50(5) 1_555 1_555 yes C(21) C(26) 1.46(3) 1_555 1_555 yes C(27) C(28) 1.35(3) 1_555 1_555 yes C(27) C(29) 1.51(4) 1_555 1_555 yes C(28) C(31) 1.47(3) 1_555 1_555 yes C(33) C(34) 1.40(4) 1_555 1_555 yes C(33) C(37) 1.38(4) 1_555 1_555 yes C(33) C(38) 1.55(3) 1_555 1_555 yes C(34) C(35) 1.33(3) 1_555 1_555 yes C(34) C(39) 1.58(4) 1_555 1_555 yes C(35) C(36) 1.51(4) 1_555 1_555 yes C(35) C(40) 1.52(3) 1_555 1_555 yes C(36) C(37) 1.47(3) 1_555 1_555 yes C(36) C(41) 1.43(4) 1_555 1_555 yes C(37) C(42) 1.49(5) 1_555 1_555 yes C(43) C(44) 1.39(3) 1_555 1_555 yes C(43) C(45) 1.45(3) 1_555 1_555 yes C(44) C(47) 1.48(3) 1_555 1_555 yes C(49) C(50) 1.48(6) 1_555 1_555 yes C(49) C(53) 1.33(4) 1_555 1_555 yes C(49) C(54) 1.55(5) 1_555 1_555 yes C(50) C(51) 1.35(7) 1_555 1_555 yes C(50) C(55) 1.49(4) 1_555 1_555 yes C(51) C(52) 1.26(8) 1_555 1_555 yes C(51) C(56) 1.54(8) 1_555 1_555 yes C(52) C(53) 1.39(6) 1_555 1_555 yes C(52) C(57) 1.51(7) 1_555 1_555 yes C(53) C(58) 1.54(5) 1_555 1_555 yes C(59) C(60) 1.38(2) 1_555 1_555 yes C(59) C(61) 1.46(3) 1_555 1_555 yes C(60) C(63) 1.50(4) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 87.4(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 111.0(5) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 143.9(6) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 169.5(4) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 131.2(4) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 105.2(5) 1_555 1_555 1_555 yes S(2) Ir(1) C(1) 151.0(6) 1_555 1_555 1_555 yes S(2) Ir(1) C(2) 113.2(5) 1_555 1_555 1_555 yes S(2) Ir(1) C(3) 101.7(4) 1_555 1_555 1_555 yes S(2) Ir(1) C(4) 121.2(6) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 159.6(7) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 39.8(7) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 62.8(7) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 63.4(9) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 37(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 36.0(9) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 64.0(8) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 65.3(7) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 39.1(6) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 64.5(6) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38.7(8) 1_555 1_555 1_555 yes S(3) Ir(2) S(4) 87.6(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(17) 126.4(7) 1_555 1_555 1_555 yes S(3) Ir(2) C(18) 161(1) 1_555 1_555 1_555 yes S(3) Ir(2) C(19) 152(1) 1_555 1_555 1_555 yes S(3) Ir(2) C(20) 115.1(9) 1_555 1_555 1_555 yes S(3) Ir(2) C(21) 105.1(6) 1_555 1_555 1_555 yes S(4) Ir(2) C(17) 127.9(6) 1_555 1_555 1_555 yes S(4) Ir(2) C(18) 104.8(8) 1_555 1_555 1_555 yes S(4) Ir(2) C(19) 108.7(10) 1_555 1_555 1_555 yes S(4) Ir(2) C(20) 143.3(7) 1_555 1_555 1_555 yes S(4) Ir(2) C(21) 165.2(6) 1_555 1_555 1_555 yes C(17) Ir(2) C(18) 34(1) 1_555 1_555 1_555 yes C(17) Ir(2) C(19) 60(1) 1_555 1_555 1_555 yes C(17) Ir(2) C(20) 62.2(10) 1_555 1_555 1_555 yes C(17) Ir(2) C(21) 37.8(9) 1_555 1_555 1_555 yes C(18) Ir(2) C(19) 36(2) 1_555 1_555 1_555 yes C(18) Ir(2) C(20) 62(1) 1_555 1_555 1_555 yes C(18) Ir(2) C(21) 61.0(10) 1_555 1_555 1_555 yes C(19) Ir(2) C(20) 40(1) 1_555 1_555 1_555 yes C(19) Ir(2) C(21) 63(1) 1_555 1_555 1_555 yes C(20) Ir(2) C(21) 36.6(9) 1_555 1_555 1_555 yes S(5) Ir(3) S(6) 87.2(2) 1_555 1_555 1_555 yes S(5) Ir(3) C(33) 106.9(6) 1_555 1_555 1_555 yes S(5) Ir(3) C(34) 109.3(6) 1_555 1_555 1_555 yes S(5) Ir(3) C(35) 135.5(7) 1_555 1_555 1_555 yes S(5) Ir(3) C(36) 170.3(4) 1_555 1_555 1_555 yes S(5) Ir(3) C(37) 133.7(6) 1_555 1_555 1_555 yes S(6) Ir(3) C(33) 156.1(8) 1_555 1_555 1_555 yes S(6) Ir(3) C(34) 154.7(5) 1_555 1_555 1_555 yes S(6) Ir(3) C(35) 119.9(5) 1_555 1_555 1_555 yes S(6) Ir(3) C(36) 102.3(5) 1_555 1_555 1_555 yes S(6) Ir(3) C(37) 119.6(8) 1_555 1_555 1_555 yes C(33) Ir(3) C(34) 37(1) 1_555 1_555 1_555 yes C(33) Ir(3) C(35) 62.9(8) 1_555 1_555 1_555 yes C(33) Ir(3) C(36) 63.6(7) 1_555 1_555 1_555 yes C(33) Ir(3) C(37) 37(1) 1_555 1_555 1_555 yes C(34) Ir(3) C(35) 35.5(7) 1_555 1_555 1_555 yes C(34) Ir(3) C(36) 62.4(8) 1_555 1_555 1_555 yes C(34) Ir(3) C(37) 62(1) 1_555 1_555 1_555 yes C(35) Ir(3) C(36) 40.3(10) 1_555 1_555 1_555 yes C(35) Ir(3) C(37) 65.6(9) 1_555 1_555 1_555 yes C(36) Ir(3) C(37) 39.2(8) 1_555 1_555 1_555 yes S(7) Ir(4) S(8) 87.3(2) 1_555 1_555 1_555 yes S(7) Ir(4) C(49) 103.4(6) 1_555 1_555 1_555 yes S(7) Ir(4) C(50) 121(1) 1_555 1_555 1_555 yes S(7) Ir(4) C(51) 158(1) 1_555 1_555 1_555 yes S(7) Ir(4) C(52) 155(1) 1_555 1_555 1_555 yes S(7) Ir(4) C(53) 119.4(7) 1_555 1_555 1_555 yes S(8) Ir(4) C(49) 169.1(6) 1_555 1_555 1_555 yes S(8) Ir(4) C(50) 134(1) 1_555 1_555 1_555 yes S(8) Ir(4) C(51) 108(1) 1_555 1_555 1_555 yes S(8) Ir(4) C(52) 106(1) 1_555 1_555 1_555 yes S(8) Ir(4) C(53) 136.0(8) 1_555 1_555 1_555 yes C(49) Ir(4) C(50) 40(1) 1_555 1_555 1_555 yes C(49) Ir(4) C(51) 61(1) 1_555 1_555 1_555 yes C(49) Ir(4) C(52) 63(1) 1_555 1_555 1_555 yes C(49) Ir(4) C(53) 36(1) 1_555 1_555 1_555 yes C(50) Ir(4) C(51) 36(1) 1_555 1_555 1_555 yes C(50) Ir(4) C(52) 63(1) 1_555 1_555 1_555 yes C(50) Ir(4) C(53) 62(1) 1_555 1_555 1_555 yes C(51) Ir(4) C(52) 34(2) 1_555 1_555 1_555 yes C(51) Ir(4) C(53) 58(1) 1_555 1_555 1_555 yes C(52) Ir(4) C(53) 37(1) 1_555 1_555 1_555 yes Ir(1) S(1) C(11) 106.2(6) 1_555 1_555 1_555 yes Ir(1) S(2) C(12) 107.3(6) 1_555 1_555 1_555 yes Ir(2) S(3) C(27) 105.8(8) 1_555 1_555 1_555 yes Ir(2) S(4) C(28) 106.2(7) 1_555 1_555 1_555 yes Ir(3) S(5) C(43) 107.5(7) 1_555 1_555 1_555 yes Ir(3) S(6) C(44) 106.7(7) 1_555 1_555 1_555 yes Ir(4) S(7) C(59) 106.8(6) 1_555 1_555 1_555 yes Ir(4) S(8) C(60) 106.4(8) 1_555 1_555 1_555 yes C(13) O(2) C(14) 115(1) 1_555 1_555 1_555 yes C(15) O(4) C(16) 118(1) 1_555 1_555 1_555 yes C(29) O(6) C(30) 114(2) 1_555 1_555 1_555 yes C(31) O(8) C(32) 104(2) 1_555 1_555 1_555 yes C(45) O(10) C(46) 114(2) 1_555 1_555 1_555 yes C(47) O(12) C(48) 116(2) 1_555 1_555 1_555 yes C(61) O(14) C(62) 120(2) 1_555 1_555 1_555 yes C(63) O(16) C(64) 118(1) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 69(1) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 71(1) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 126(1) 1_555 1_555 1_555 yes C(2) C(1) C(5) 108(2) 1_555 1_555 1_555 yes C(2) C(1) C(6) 125(2) 1_555 1_555 1_555 yes C(5) C(1) C(6) 125(2) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 70(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 73(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 127(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 107(1) 1_555 1_555 1_555 yes C(1) C(2) C(7) 125(2) 1_555 1_555 1_555 yes C(3) C(2) C(7) 126(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 70(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 68.7(10) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 121(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 109(1) 1_555 1_555 1_555 yes C(2) C(3) C(8) 124(1) 1_555 1_555 1_555 yes C(4) C(3) C(8) 126(2) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 72(1) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 71(1) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 126(1) 1_555 1_555 1_555 yes C(3) C(4) C(5) 107(1) 1_555 1_555 1_555 yes C(3) C(4) C(9) 127(1) 1_555 1_555 1_555 yes C(5) C(4) C(9) 125(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 71(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 70(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 126(1) 1_555 1_555 1_555 yes C(1) C(5) C(4) 106(1) 1_555 1_555 1_555 yes C(1) C(5) C(10) 128(2) 1_555 1_555 1_555 yes C(4) C(5) C(10) 124(2) 1_555 1_555 1_555 yes C(1) C(6) H(1) 109(2) 1_555 1_555 1_555 no C(1) C(6) H(2) 109(3) 1_555 1_555 1_555 no C(1) C(6) H(3) 109(3) 1_555 1_555 1_555 no H(1) C(6) H(2) 109(3) 1_555 1_555 1_555 no H(1) C(6) H(3) 109(3) 1_555 1_555 1_555 no H(2) C(6) H(3) 109(2) 1_555 1_555 1_555 no C(2) C(7) H(4) 109(2) 1_555 1_555 1_555 no C(2) C(7) H(5) 109(1) 1_555 1_555 1_555 no C(2) C(7) H(6) 109(2) 1_555 1_555 1_555 no H(4) C(7) H(5) 109(3) 1_555 1_555 1_555 no H(4) C(7) H(6) 109(2) 1_555 1_555 1_555 no H(5) C(7) H(6) 109(2) 1_555 1_555 1_555 no C(3) C(8) H(7) 109(1) 1_555 1_555 1_555 no C(3) C(8) H(8) 109(2) 1_555 1_555 1_555 no C(3) C(8) H(9) 109(1) 1_555 1_555 1_555 no H(7) C(8) H(8) 109(2) 1_555 1_555 1_555 no H(7) C(8) H(9) 109(2) 1_555 1_555 1_555 no H(8) C(8) H(9) 109(2) 1_555 1_555 1_555 no C(4) C(9) H(10) 109(2) 1_555 1_555 1_555 no C(4) C(9) H(11) 109(2) 1_555 1_555 1_555 no C(4) C(9) H(12) 109(2) 1_555 1_555 1_555 no H(10) C(9) H(11) 109(2) 1_555 1_555 1_555 no H(10) C(9) H(12) 109(3) 1_555 1_555 1_555 no H(11) C(9) H(12) 109(2) 1_555 1_555 1_555 no C(5) C(10) H(13) 109(2) 1_555 1_555 1_555 no C(5) C(10) H(14) 109(2) 1_555 1_555 1_555 no C(5) C(10) H(15) 109(1) 1_555 1_555 1_555 no H(13) C(10) H(14) 109(2) 1_555 1_555 1_555 no H(13) C(10) H(15) 109(3) 1_555 1_555 1_555 no H(14) C(10) H(15) 109(2) 1_555 1_555 1_555 no S(1) C(11) C(12) 122(1) 1_555 1_555 1_555 yes S(1) C(11) C(13) 115(1) 1_555 1_555 1_555 yes C(12) C(11) C(13) 121(1) 1_555 1_555 1_555 yes S(2) C(12) C(11) 116(1) 1_555 1_555 1_555 yes S(2) C(12) C(15) 117(1) 1_555 1_555 1_555 yes C(11) C(12) C(15) 125(1) 1_555 1_555 1_555 yes O(1) C(13) O(2) 125(1) 1_555 1_555 1_555 yes O(1) C(13) C(11) 120(2) 1_555 1_555 1_555 yes O(2) C(13) C(11) 113(1) 1_555 1_555 1_555 yes O(2) C(14) H(16) 109(2) 1_555 1_555 1_555 no O(2) C(14) H(17) 109(2) 1_555 1_555 1_555 no O(2) C(14) H(18) 109(2) 1_555 1_555 1_555 no H(16) C(14) H(17) 109(3) 1_555 1_555 1_555 no H(16) C(14) H(18) 109(2) 1_555 1_555 1_555 no H(17) C(14) H(18) 109(2) 1_555 1_555 1_555 no O(3) C(15) O(4) 122(2) 1_555 1_555 1_555 yes O(3) C(15) C(12) 122(2) 1_555 1_555 1_555 yes O(4) C(15) C(12) 114(1) 1_555 1_555 1_555 yes O(4) C(16) H(19) 109(1) 1_555 1_555 1_555 no O(4) C(16) H(20) 109(2) 1_555 1_555 1_555 no O(4) C(16) H(21) 109(1) 1_555 1_555 1_555 no H(19) C(16) H(20) 109(2) 1_555 1_555 1_555 no H(19) C(16) H(21) 109(3) 1_555 1_555 1_555 no H(20) C(16) H(21) 109(2) 1_555 1_555 1_555 no Ir(2) C(17) C(18) 72(2) 1_555 1_555 1_555 yes Ir(2) C(17) C(21) 74(1) 1_555 1_555 1_555 yes Ir(2) C(17) C(22) 125(2) 1_555 1_555 1_555 yes C(18) C(17) C(21) 110(2) 1_555 1_555 1_555 yes C(18) C(17) C(22) 124(3) 1_555 1_555 1_555 yes C(21) C(17) C(22) 124(2) 1_555 1_555 1_555 yes Ir(2) C(18) C(17) 72(2) 1_555 1_555 1_555 yes Ir(2) C(18) C(19) 75(3) 1_555 1_555 1_555 yes Ir(2) C(18) C(23) 122(2) 1_555 1_555 1_555 yes C(17) C(18) C(19) 113(3) 1_555 1_555 1_555 yes C(17) C(18) C(23) 131(4) 1_555 1_555 1_555 yes C(19) C(18) C(23) 114(4) 1_555 1_555 1_555 yes Ir(2) C(19) C(18) 68(2) 1_555 1_555 1_555 yes Ir(2) C(19) C(20) 67(2) 1_555 1_555 1_555 yes Ir(2) C(19) C(24) 119(3) 1_555 1_555 1_555 yes C(18) C(19) C(20) 102(3) 1_555 1_555 1_555 yes C(18) C(19) C(24) 139(4) 1_555 1_555 1_555 yes C(20) C(19) C(24) 116(4) 1_555 1_555 1_555 yes Ir(2) C(20) C(19) 71(2) 1_555 1_555 1_555 yes Ir(2) C(20) C(21) 73(1) 1_555 1_555 1_555 yes Ir(2) C(20) C(25) 123(2) 1_555 1_555 1_555 yes C(19) C(20) C(21) 106(2) 1_555 1_555 1_555 yes C(19) C(20) C(25) 130(3) 1_555 1_555 1_555 yes C(21) C(20) C(25) 122(2) 1_555 1_555 1_555 yes Ir(2) C(21) C(17) 67(1) 1_555 1_555 1_555 yes Ir(2) C(21) C(20) 69(1) 1_555 1_555 1_555 yes Ir(2) C(21) C(26) 126(2) 1_555 1_555 1_555 yes C(17) C(21) C(20) 105(1) 1_555 1_555 1_555 yes C(17) C(21) C(26) 125(2) 1_555 1_555 1_555 yes C(20) C(21) C(26) 128(2) 1_555 1_555 1_555 yes C(17) C(22) H(22) 108(2) 1_555 1_555 1_555 no C(17) C(22) H(23) 110(3) 1_555 1_555 1_555 no C(17) C(22) H(24) 108(3) 1_555 1_555 1_555 no H(22) C(22) H(23) 110(4) 1_555 1_555 1_555 no H(22) C(22) H(24) 108(4) 1_555 1_555 1_555 no H(23) C(22) H(24) 110(3) 1_555 1_555 1_555 no C(18) C(23) H(25) 110(5) 1_555 1_555 1_555 no C(18) C(23) H(26) 110(5) 1_555 1_555 1_555 no C(18) C(23) H(27) 107(4) 1_555 1_555 1_555 no H(25) C(23) H(26) 110(5) 1_555 1_555 1_555 no H(25) C(23) H(27) 109(6) 1_555 1_555 1_555 no H(26) C(23) H(27) 109(6) 1_555 1_555 1_555 no C(19) C(24) H(28) 110(3) 1_555 1_555 1_555 no C(19) C(24) H(29) 110(5) 1_555 1_555 1_555 no C(19) C(24) H(30) 108(5) 1_555 1_555 1_555 no H(28) C(24) H(29) 110(6) 1_555 1_555 1_555 no H(28) C(24) H(30) 109(6) 1_555 1_555 1_555 no H(29) C(24) H(30) 109(3) 1_555 1_555 1_555 no C(20) C(25) H(31) 109(3) 1_555 1_555 1_555 no C(20) C(25) H(32) 109(3) 1_555 1_555 1_555 no C(20) C(25) H(33) 109(4) 1_555 1_555 1_555 no H(31) C(25) H(32) 109(5) 1_555 1_555 1_555 no H(31) C(25) H(33) 109(4) 1_555 1_555 1_555 no H(32) C(25) H(33) 109(4) 1_555 1_555 1_555 no C(21) C(26) H(34) 109(3) 1_555 1_555 1_555 no C(21) C(26) H(35) 109(2) 1_555 1_555 1_555 no C(21) C(26) H(36) 109(3) 1_555 1_555 1_555 no H(34) C(26) H(35) 109(3) 1_555 1_555 1_555 no H(34) C(26) H(36) 109(2) 1_555 1_555 1_555 no H(35) C(26) H(36) 109(3) 1_555 1_555 1_555 no S(3) C(27) C(28) 118(1) 1_555 1_555 1_555 yes S(3) C(27) C(29) 114(1) 1_555 1_555 1_555 yes C(28) C(27) C(29) 126(1) 1_555 1_555 1_555 yes S(4) C(28) C(27) 121(1) 1_555 1_555 1_555 yes S(4) C(28) C(31) 115(1) 1_555 1_555 1_555 yes C(27) C(28) C(31) 123(2) 1_555 1_555 1_555 yes O(5) C(29) O(6) 126(2) 1_555 1_555 1_555 yes O(5) C(29) C(27) 124(2) 1_555 1_555 1_555 yes O(6) C(29) C(27) 108(2) 1_555 1_555 1_555 yes O(6) C(30) H(37) 109(2) 1_555 1_555 1_555 no O(6) C(30) H(38) 109(2) 1_555 1_555 1_555 no O(6) C(30) H(39) 109(3) 1_555 1_555 1_555 no H(37) C(30) H(38) 109(3) 1_555 1_555 1_555 no H(37) C(30) H(39) 109(2) 1_555 1_555 1_555 no H(38) C(30) H(39) 109(3) 1_555 1_555 1_555 no O(7) C(31) O(8) 120(2) 1_555 1_555 1_555 yes O(7) C(31) C(28) 121(2) 1_555 1_555 1_555 yes O(8) C(31) C(28) 117(2) 1_555 1_555 1_555 yes O(8) C(32) H(40) 109(3) 1_555 1_555 1_555 no O(8) C(32) H(41) 109(4) 1_555 1_555 1_555 no O(8) C(32) H(42) 109(2) 1_555 1_555 1_555 no H(40) C(32) H(41) 109(3) 1_555 1_555 1_555 no H(40) C(32) H(42) 109(5) 1_555 1_555 1_555 no H(41) C(32) H(42) 109(5) 1_555 1_555 1_555 no Ir(3) C(33) C(34) 73(1) 1_555 1_555 1_555 yes Ir(3) C(33) C(37) 71(1) 1_555 1_555 1_555 yes Ir(3) C(33) C(38) 123(1) 1_555 1_555 1_555 yes C(34) C(33) C(37) 109(1) 1_555 1_555 1_555 yes C(34) C(33) C(38) 123(2) 1_555 1_555 1_555 yes C(37) C(33) C(38) 127(2) 1_555 1_555 1_555 yes Ir(3) C(34) C(33) 69(1) 1_555 1_555 1_555 yes Ir(3) C(34) C(35) 68(1) 1_555 1_555 1_555 yes Ir(3) C(34) C(39) 121(1) 1_555 1_555 1_555 yes C(33) C(34) C(35) 110(2) 1_555 1_555 1_555 yes C(33) C(34) C(39) 126(1) 1_555 1_555 1_555 yes C(35) C(34) C(39) 123(2) 1_555 1_555 1_555 yes Ir(3) C(35) C(34) 75(1) 1_555 1_555 1_555 yes Ir(3) C(35) C(36) 73(1) 1_555 1_555 1_555 yes Ir(3) C(35) C(40) 125(1) 1_555 1_555 1_555 yes C(34) C(35) C(36) 108(2) 1_555 1_555 1_555 yes C(34) C(35) C(40) 130(2) 1_555 1_555 1_555 yes C(36) C(35) C(40) 120(2) 1_555 1_555 1_555 yes Ir(3) C(36) C(35) 66(1) 1_555 1_555 1_555 yes Ir(3) C(36) C(37) 67(1) 1_555 1_555 1_555 yes Ir(3) C(36) C(41) 126(1) 1_555 1_555 1_555 yes C(35) C(36) C(37) 102(1) 1_555 1_555 1_555 yes C(35) C(36) C(41) 128(2) 1_555 1_555 1_555 yes C(37) C(36) C(41) 129(2) 1_555 1_555 1_555 yes Ir(3) C(37) C(33) 71(1) 1_555 1_555 1_555 yes Ir(3) C(37) C(36) 73(1) 1_555 1_555 1_555 yes Ir(3) C(37) C(42) 126(1) 1_555 1_555 1_555 yes C(33) C(37) C(36) 108(2) 1_555 1_555 1_555 yes C(33) C(37) C(42) 131(2) 1_555 1_555 1_555 yes C(36) C(37) C(42) 119(2) 1_555 1_555 1_555 yes C(33) C(38) H(43) 109(2) 1_555 1_555 1_555 no C(33) C(38) H(44) 109(2) 1_555 1_555 1_555 no C(33) C(38) H(45) 109(2) 1_555 1_555 1_555 no H(43) C(38) H(44) 109(2) 1_555 1_555 1_555 no H(43) C(38) H(45) 109(3) 1_555 1_555 1_555 no H(44) C(38) H(45) 109(3) 1_555 1_555 1_555 no C(34) C(39) H(46) 109(2) 1_555 1_555 1_555 no C(34) C(39) H(47) 109(3) 1_555 1_555 1_555 no C(34) C(39) H(48) 109(2) 1_555 1_555 1_555 no H(46) C(39) H(47) 109(2) 1_555 1_555 1_555 no H(46) C(39) H(48) 109(3) 1_555 1_555 1_555 no H(47) C(39) H(48) 109(2) 1_555 1_555 1_555 no C(35) C(40) H(49) 109(3) 1_555 1_555 1_555 no C(35) C(40) H(50) 109(2) 1_555 1_555 1_555 no C(35) C(40) H(51) 109(2) 1_555 1_555 1_555 no H(49) C(40) H(50) 109(2) 1_555 1_555 1_555 no H(49) C(40) H(51) 109(2) 1_555 1_555 1_555 no H(50) C(40) H(51) 109(3) 1_555 1_555 1_555 no C(36) C(41) H(52) 109(2) 1_555 1_555 1_555 no C(36) C(41) H(53) 109(3) 1_555 1_555 1_555 no C(36) C(41) H(54) 109(2) 1_555 1_555 1_555 no H(52) C(41) H(53) 109(2) 1_555 1_555 1_555 no H(52) C(41) H(54) 109(3) 1_555 1_555 1_555 no H(53) C(41) H(54) 109(2) 1_555 1_555 1_555 no C(37) C(42) H(55) 109(2) 1_555 1_555 1_555 no C(37) C(42) H(56) 109(3) 1_555 1_555 1_555 no C(37) C(42) H(57) 109(2) 1_555 1_555 1_555 no H(55) C(42) H(56) 109(2) 1_555 1_555 1_555 no H(55) C(42) H(57) 109(3) 1_555 1_555 1_555 no H(56) C(42) H(57) 109(2) 1_555 1_555 1_555 no S(5) C(43) C(44) 117(1) 1_555 1_555 1_555 yes S(5) C(43) C(45) 118(1) 1_555 1_555 1_555 yes C(44) C(43) C(45) 123(1) 1_555 1_555 1_555 yes S(6) C(44) C(43) 121(1) 1_555 1_555 1_555 yes S(6) C(44) C(47) 114(1) 1_555 1_555 1_555 yes C(43) C(44) C(47) 123(1) 1_555 1_555 1_555 yes O(9) C(45) O(10) 121(2) 1_555 1_555 1_555 yes O(9) C(45) C(43) 127(3) 1_555 1_555 1_555 yes O(10) C(45) C(43) 110(2) 1_555 1_555 1_555 yes O(10) C(46) H(58) 109(3) 1_555 1_555 1_555 no O(10) C(46) H(59) 109(2) 1_555 1_555 1_555 no O(10) C(46) H(60) 109(2) 1_555 1_555 1_555 no H(58) C(46) H(59) 109(2) 1_555 1_555 1_555 no H(58) C(46) H(60) 109(3) 1_555 1_555 1_555 no H(59) C(46) H(60) 109(4) 1_555 1_555 1_555 no O(11) C(47) O(12) 123(2) 1_555 1_555 1_555 yes O(11) C(47) C(44) 126(2) 1_555 1_555 1_555 yes O(12) C(47) C(44) 110(2) 1_555 1_555 1_555 yes O(12) C(48) H(61) 109(2) 1_555 1_555 1_555 no O(12) C(48) H(62) 109(3) 1_555 1_555 1_555 no O(12) C(48) H(63) 109(2) 1_555 1_555 1_555 no H(61) C(48) H(62) 109(2) 1_555 1_555 1_555 no H(61) C(48) H(63) 109(4) 1_555 1_555 1_555 no H(62) C(48) H(63) 109(3) 1_555 1_555 1_555 no Ir(4) C(49) C(50) 69(2) 1_555 1_555 1_555 yes Ir(4) C(49) C(53) 70(2) 1_555 1_555 1_555 yes Ir(4) C(49) C(54) 125(2) 1_555 1_555 1_555 yes C(50) C(49) C(53) 105(2) 1_555 1_555 1_555 yes C(50) C(49) C(54) 124(3) 1_555 1_555 1_555 yes C(53) C(49) C(54) 129(3) 1_555 1_555 1_555 yes Ir(4) C(50) C(49) 70(1) 1_555 1_555 1_555 yes Ir(4) C(50) C(51) 69(2) 1_555 1_555 1_555 yes Ir(4) C(50) C(55) 126(3) 1_555 1_555 1_555 yes C(49) C(50) C(51) 100(3) 1_555 1_555 1_555 yes C(49) C(50) C(55) 125(4) 1_555 1_555 1_555 yes C(51) C(50) C(55) 134(5) 1_555 1_555 1_555 yes Ir(4) C(51) C(50) 73(2) 1_555 1_555 1_555 yes Ir(4) C(51) C(52) 74(2) 1_555 1_555 1_555 yes Ir(4) C(51) C(56) 122(3) 1_555 1_555 1_555 yes C(50) C(51) C(52) 119(4) 1_555 1_555 1_555 yes C(50) C(51) C(56) 120(5) 1_555 1_555 1_555 yes C(52) C(51) C(56) 119(4) 1_555 1_555 1_555 yes Ir(4) C(52) C(51) 70(2) 1_555 1_555 1_555 yes Ir(4) C(52) C(53) 69(1) 1_555 1_555 1_555 yes Ir(4) C(52) C(57) 125(3) 1_555 1_555 1_555 yes C(51) C(52) C(53) 102(4) 1_555 1_555 1_555 yes C(51) C(52) C(57) 139(4) 1_555 1_555 1_555 yes C(53) C(52) C(57) 117(4) 1_555 1_555 1_555 yes Ir(4) C(53) C(49) 73(1) 1_555 1_555 1_555 yes Ir(4) C(53) C(52) 72(2) 1_555 1_555 1_555 yes Ir(4) C(53) C(58) 125(2) 1_555 1_555 1_555 yes C(49) C(53) C(52) 112(3) 1_555 1_555 1_555 yes C(49) C(53) C(58) 121(3) 1_555 1_555 1_555 yes C(52) C(53) C(58) 125(3) 1_555 1_555 1_555 yes C(49) C(54) H(64) 109(3) 1_555 1_555 1_555 no C(49) C(54) H(65) 109(3) 1_555 1_555 1_555 no C(49) C(54) H(66) 109(4) 1_555 1_555 1_555 no H(64) C(54) H(65) 109(4) 1_555 1_555 1_555 no H(64) C(54) H(66) 109(3) 1_555 1_555 1_555 no H(65) C(54) H(66) 109(4) 1_555 1_555 1_555 no C(50) C(55) H(67) 109(5) 1_555 1_555 1_555 no C(50) C(55) H(68) 109(5) 1_555 1_555 1_555 no C(50) C(55) H(69) 109(3) 1_555 1_555 1_555 no H(67) C(55) H(68) 109(4) 1_555 1_555 1_555 no H(67) C(55) H(69) 109(6) 1_555 1_555 1_555 no H(68) C(55) H(69) 109(6) 1_555 1_555 1_555 no C(51) C(56) H(70) 109(5) 1_555 1_555 1_555 no C(51) C(56) H(71) 109(5) 1_555 1_555 1_555 no C(51) C(56) H(72) 109(3) 1_555 1_555 1_555 no H(70) C(56) H(71) 109(3) 1_555 1_555 1_555 no H(70) C(56) H(72) 109(5) 1_555 1_555 1_555 no H(71) C(56) H(72) 109(6) 1_555 1_555 1_555 no C(52) C(57) H(73) 109(4) 1_555 1_555 1_555 no C(52) C(57) H(74) 109(4) 1_555 1_555 1_555 no C(52) C(57) H(75) 109(4) 1_555 1_555 1_555 no H(73) C(57) H(74) 109(5) 1_555 1_555 1_555 no H(73) C(57) H(75) 109(4) 1_555 1_555 1_555 no H(74) C(57) H(75) 109(4) 1_555 1_555 1_555 no C(53) C(58) H(76) 109(4) 1_555 1_555 1_555 no C(53) C(58) H(77) 109(3) 1_555 1_555 1_555 no C(53) C(58) H(78) 109(3) 1_555 1_555 1_555 no H(76) C(58) H(77) 109(3) 1_555 1_555 1_555 no H(76) C(58) H(78) 109(3) 1_555 1_555 1_555 no H(77) C(58) H(78) 109(5) 1_555 1_555 1_555 no S(7) C(59) C(60) 118(1) 1_555 1_555 1_555 yes S(7) C(59) C(61) 116(1) 1_555 1_555 1_555 yes C(60) C(59) C(61) 124(2) 1_555 1_555 1_555 yes S(8) C(60) C(59) 121(1) 1_555 1_555 1_555 yes S(8) C(60) C(63) 118(1) 1_555 1_555 1_555 yes C(59) C(60) C(63) 119(1) 1_555 1_555 1_555 yes O(13) C(61) O(14) 121(1) 1_555 1_555 1_555 yes O(13) C(61) C(59) 123(2) 1_555 1_555 1_555 yes O(14) C(61) C(59) 115(2) 1_555 1_555 1_555 yes O(14) C(62) H(79) 109(2) 1_555 1_555 1_555 no O(14) C(62) H(80) 109(2) 1_555 1_555 1_555 no O(14) C(62) H(81) 109(2) 1_555 1_555 1_555 no H(79) C(62) H(80) 109(2) 1_555 1_555 1_555 no H(79) C(62) H(81) 109(2) 1_555 1_555 1_555 no H(80) C(62) H(81) 109(2) 1_555 1_555 1_555 no O(15) C(63) O(16) 121(2) 1_555 1_555 1_555 yes O(15) C(63) C(60) 125(2) 1_555 1_555 1_555 yes O(16) C(63) C(60) 111(1) 1_555 1_555 1_555 yes O(16) C(64) H(82) 109(2) 1_555 1_555 1_555 no O(16) C(64) H(83) 109(2) 1_555 1_555 1_555 no O(16) C(64) H(84) 109(2) 1_555 1_555 1_555 no H(82) C(64) H(83) 109(2) 1_555 1_555 1_555 no H(82) C(64) H(84) 109(2) 1_555 1_555 1_555 no H(83) C(64) H(84) 109(2) 1_555 1_555 1_555 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 S(4) C(8) 3.58(2) 1_555 2_666 ? S(7) C(46) 3.47(3) 1_555 2_765 ? O(1) C(30) 3.39(4) 1_555 1_545 ? O(1) C(6) 3.49(3) 1_555 2_655 ? O(2) C(26) 3.43(4) 1_555 1_555 ? O(2) C(21) 3.49(3) 1_555 1_555 ? O(2) C(17) 3.59(3) 1_555 1_555 ? O(3) C(23) 3.34(6) 1_555 1_555 ? O(3) C(18) 3.54(5) 1_555 1_555 ? O(4) C(32) 3.34(5) 1_555 1_545 ? O(5) C(39) 3.54(3) 1_555 1_555 ? O(8) C(35) 3.39(3) 1_555 1_555 ? O(8) C(36) 3.45(3) 1_555 1_555 ? O(9) C(53) 3.27(4) 1_555 1_555 ? O(9) C(49) 3.29(4) 1_555 1_555 ? O(9) C(58) 3.41(5) 1_555 1_555 ? O(9) C(54) 3.55(4) 1_555 1_555 ? O(10) C(62) 3.29(3) 1_555 1_565 ? O(10) C(26) 3.56(4) 1_555 2_665 ? O(11) C(64) 3.41(4) 1_555 2_766 ? O(11) C(16) 3.53(4) 1_555 2_666 ? O(13) C(14) 3.48(3) 1_555 2_655 ? O(15) C(16) 3.22(3) 1_555 1_655 ? O(15) C(14) 3.60(3) 1_555 1_655 ? O(16) C(8) 3.19(3) 1_555 1_555 ? O(16) C(3) 3.43(2) 1_555 1_555 ? C(16) C(32) 3.52(5) 1_555 1_545 ? C(24) C(24) 3.5(1) 1_555 2_666 ? C(46) C(62) 3.59(4) 1_555 1_565 ? #------------------------------------------------------------------------------ #===END data_[Cp*Ir{S2C2H(COOMe)}]_(13) #------------------------------------------------------------------------------ _audit_creation_date 'Mon Feb 15 13:44:51 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 475.64 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H19 Ir O2 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.237(2) _cell_length_b 12.154(3) _cell_length_c 15.017(3) _cell_angle_alpha 76.46(2) _cell_angle_beta 79.22(1) _cell_angle_gamma 87.65(2) _cell_volume 1610.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _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 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912.00 _exptl_absorpt_coefficient_mu 8.569 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.57 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 0 2 0 -1 2 -1 -2 0 _diffrn_reflns_number 7819 _reflns_number_total 7363 _reflns_number_gt 4761 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.043 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04047 _diffrn_orient_matrix_UB_12 -0.07736 _diffrn_orient_matrix_UB_13 0.03114 _diffrn_orient_matrix_UB_21 0.06590 _diffrn_orient_matrix_UB_22 -0.00709 _diffrn_orient_matrix_UB_23 0.04683 _diffrn_orient_matrix_UB_31 -0.07851 _diffrn_orient_matrix_UB_32 0.03357 _diffrn_orient_matrix_UB_33 0.04112 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.09193(3) 0.25349(2) 0.55836(2) 0.04280(10) Uani 1.00 d . . . Ir(2) Ir 0.27257(3) 0.17607(3) 0.11758(2) 0.0455(1) Uani 1.00 d . . . S(1) S 0.0725(2) 0.3072(2) 0.6921(1) 0.0532(6) Uani 1.00 d . . . S(2) S -0.1470(2) 0.2047(2) 0.6012(2) 0.0598(7) Uani 1.00 d . . . S(3) S 0.3750(2) 0.3055(2) 0.1698(1) 0.0527(6) Uani 1.00 d . . . S(4) S 0.4122(3) 0.0470(2) 0.1952(2) 0.0732(8) Uani 1.00 d . . . O(1) O -0.0780(7) 0.3694(8) 0.8670(5) 0.116(3) Uani 1.00 d . . . O(2) O -0.2996(6) 0.3168(5) 0.8639(4) 0.073(2) Uani 1.00 d . . . O(3) O 0.6675(7) 0.2471(6) 0.3336(5) 0.089(3) Uani 1.00 d . . . O(4) O 0.5741(7) 0.4034(6) 0.2572(5) 0.077(2) Uani 1.00 d . . . C(1) C -0.1122(8) 0.2880(6) 0.7447(5) 0.045(2) Uani 1.00 d . . . C(2) C -0.2043(8) 0.2429(6) 0.7040(5) 0.048(2) Uani 1.00 d . . . C(3) C -0.1572(10) 0.3278(7) 0.8300(6) 0.056(3) Uani 1.00 d . . . C(4) C -0.354(1) 0.3534(9) 0.9494(8) 0.093(4) Uani 1.00 d . . . C(5) C 0.3288(8) 0.2538(8) 0.5028(6) 0.060(3) Uani 1.00 d . . . C(6) C 0.2623(9) 0.3537(7) 0.4561(6) 0.058(3) Uani 1.00 d . . . C(7) C 0.1562(9) 0.3196(6) 0.4106(5) 0.052(2) Uani 1.00 d . . . C(8) C 0.1568(8) 0.1991(7) 0.4268(5) 0.050(2) Uani 1.00 d . . . C(9) C 0.2596(8) 0.1589(6) 0.4862(6) 0.052(2) Uani 1.00 d . . . C(10) C 0.4500(10) 0.2480(10) 0.5576(8) 0.092(4) Uani 1.00 d . . . C(11) C 0.297(1) 0.4755(8) 0.4494(8) 0.089(4) Uani 1.00 d . . . C(12) C 0.064(1) 0.3974(8) 0.3494(6) 0.076(3) Uani 1.00 d . . . C(13) C 0.0690(10) 0.1294(8) 0.3862(6) 0.067(3) Uani 1.00 d . . . C(14) C 0.2998(10) 0.0383(8) 0.5176(8) 0.083(3) Uani 1.00 d . . . C(15) C 0.4976(8) 0.2318(7) 0.2374(5) 0.048(2) Uani 1.00 d . . . C(16) C 0.5103(9) 0.1209(8) 0.2469(6) 0.066(3) Uani 1.00 d . . . C(17) C 0.5891(9) 0.2905(9) 0.2819(6) 0.063(3) Uani 1.00 d . . . C(18) C 0.668(1) 0.4679(10) 0.2938(8) 0.096(4) Uani 1.00 d . . . C(19) C 0.1607(9) 0.2741(7) 0.0082(6) 0.054(3) Uani 1.00 d . . . C(20) C 0.0557(9) 0.2314(8) 0.0904(6) 0.058(3) Uani 1.00 d . . . C(21) C 0.0651(10) 0.1082(8) 0.1079(6) 0.063(3) Uani 1.00 d . . . C(22) C 0.173(1) 0.0772(7) 0.0394(6) 0.061(3) Uani 1.00 d . . . C(23) C 0.2368(9) 0.1809(7) -0.0222(6) 0.054(3) Uani 1.00 d . . . C(24) C 0.187(1) 0.3971(8) -0.0366(7) 0.073(3) Uani 1.00 d . . . C(25) C -0.054(1) 0.2988(9) 0.1422(7) 0.084(4) Uani 1.00 d . . . C(26) C -0.036(1) 0.0291(9) 0.1854(7) 0.086(4) Uani 1.00 d . . . C(27) C 0.213(1) -0.0402(8) 0.0312(8) 0.090(4) Uani 1.00 d . . . C(28) C 0.349(1) 0.1885(8) -0.1083(6) 0.078(3) Uani 1.00 d . . . H(1) H -0.3047 0.2319 0.7334 0.0573 Uiso 1.00 calc . . . H(2) H -0.3335 0.4316 0.9400 0.1112 Uiso 1.00 calc . . . H(3) H -0.4575 0.3412 0.9665 0.1112 Uiso 1.00 calc . . . H(4) H -0.3070 0.3112 0.9976 0.1112 Uiso 1.00 calc . . . H(5) H 0.4727 0.1711 0.5816 0.1109 Uiso 1.00 calc . . . H(6) H 0.5351 0.2853 0.5183 0.1109 Uiso 1.00 calc . . . H(7) H 0.4191 0.2840 0.6077 0.1109 Uiso 1.00 calc . . . H(8) H 0.3723 0.4790 0.4842 0.1067 Uiso 1.00 calc . . . H(9) H 0.3307 0.5122 0.3860 0.1067 Uiso 1.00 calc . . . H(10) H 0.2113 0.5121 0.4737 0.1067 Uiso 1.00 calc . . . H(11) H 0.0821 0.4737 0.3499 0.0913 Uiso 1.00 calc . . . H(12) H 0.0899 0.3875 0.2875 0.0913 Uiso 1.00 calc . . . H(13) H -0.0372 0.3801 0.3724 0.0913 Uiso 1.00 calc . . . H(14) H 0.0099 0.1777 0.3482 0.0810 Uiso 1.00 calc . . . H(15) H 0.1338 0.0876 0.3496 0.0810 Uiso 1.00 calc . . . H(16) H 0.0074 0.0787 0.4350 0.0810 Uiso 1.00 calc . . . H(17) H 0.2142 -0.0040 0.5506 0.0994 Uiso 1.00 calc . . . H(18) H 0.3411 0.0092 0.4650 0.0994 Uiso 1.00 calc . . . H(19) H 0.3700 0.0326 0.5574 0.0994 Uiso 1.00 calc . . . H(20) H 0.5769 0.0811 0.2841 0.0787 Uiso 1.00 calc . . . H(21) H 0.6451 0.4487 0.3600 0.1149 Uiso 1.00 calc . . . H(22) H 0.7681 0.4507 0.2737 0.1149 Uiso 1.00 calc . . . H(23) H 0.6516 0.5464 0.2718 0.1149 Uiso 1.00 calc . . . H(24) H 0.2171 0.4339 0.0062 0.0881 Uiso 1.00 calc . . . H(25) H 0.2615 0.4049 -0.0905 0.0881 Uiso 1.00 calc . . . H(26) H 0.0983 0.4305 -0.0538 0.0881 Uiso 1.00 calc . . . H(27) H -0.0030 0.3519 0.1627 0.1010 Uiso 1.00 calc . . . H(28) H -0.1168 0.3379 0.1022 0.1010 Uiso 1.00 calc . . . H(29) H -0.1104 0.2495 0.1945 0.1010 Uiso 1.00 calc . . . H(30) H -0.0995 0.0720 0.2217 0.1034 Uiso 1.00 calc . . . H(31) H -0.0933 -0.0138 0.1592 0.1034 Uiso 1.00 calc . . . H(32) H 0.0213 -0.0206 0.2238 0.1034 Uiso 1.00 calc . . . H(33) H 0.1297 -0.0776 0.0237 0.1076 Uiso 1.00 calc . . . H(34) H 0.2898 -0.0378 -0.0212 0.1076 Uiso 1.00 calc . . . H(35) H 0.2467 -0.0801 0.0860 0.1076 Uiso 1.00 calc . . . H(36) H 0.3836 0.1148 -0.1123 0.0932 Uiso 1.00 calc . . . H(37) H 0.3056 0.2213 -0.1611 0.0932 Uiso 1.00 calc . . . H(38) H 0.4289 0.2342 -0.1068 0.0932 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0325(2) 0.0458(2) 0.0473(2) 0.0010(1) -0.0037(1) -0.0085(2) Ir(2) 0.0417(2) 0.0515(2) 0.0432(2) 0.0011(1) -0.0113(1) -0.0083(2) S(1) 0.037(1) 0.068(1) 0.055(1) -0.0082(9) -0.0088(9) -0.014(1) S(2) 0.038(1) 0.084(2) 0.064(1) -0.011(1) -0.0015(10) -0.035(1) S(3) 0.052(1) 0.054(1) 0.054(1) 0.0012(9) -0.0180(10) -0.0114(10) S(4) 0.071(2) 0.057(1) 0.097(2) 0.014(1) -0.037(2) -0.015(1) O(1) 0.064(5) 0.222(10) 0.088(6) -0.035(5) -0.002(4) -0.091(6) O(2) 0.054(4) 0.097(5) 0.073(4) -0.021(3) 0.013(3) -0.046(4) O(3) 0.076(5) 0.128(6) 0.072(5) 0.000(4) -0.042(4) -0.019(4) O(4) 0.065(4) 0.091(5) 0.089(5) -0.009(4) -0.029(4) -0.036(4) C(1) 0.044(4) 0.049(4) 0.038(4) -0.002(3) -0.004(3) -0.006(3) C(2) 0.041(4) 0.053(5) 0.052(5) -0.004(4) -0.003(4) -0.022(4) C(3) 0.056(6) 0.064(5) 0.048(5) -0.013(4) -0.006(4) -0.015(4) C(4) 0.082(8) 0.121(9) 0.084(8) -0.016(6) 0.008(6) -0.058(7) C(5) 0.028(4) 0.085(6) 0.064(6) -0.002(4) 0.002(4) -0.021(5) C(6) 0.045(5) 0.058(5) 0.060(6) -0.007(4) 0.009(4) -0.008(4) C(7) 0.051(5) 0.048(5) 0.048(5) 0.005(4) 0.003(4) -0.004(4) C(8) 0.042(4) 0.056(5) 0.047(5) 0.001(4) 0.007(4) -0.015(4) C(9) 0.031(4) 0.051(5) 0.069(6) 0.007(3) -0.003(4) -0.009(4) C(10) 0.038(5) 0.14(1) 0.099(8) -0.008(6) -0.011(5) -0.035(7) C(11) 0.082(7) 0.071(6) 0.106(9) -0.023(5) 0.017(6) -0.027(6) C(12) 0.085(7) 0.069(6) 0.062(6) 0.028(5) -0.010(5) 0.002(5) C(13) 0.069(6) 0.080(6) 0.055(6) 0.005(5) -0.010(5) -0.021(5) C(14) 0.052(6) 0.075(7) 0.110(9) 0.022(5) -0.011(5) -0.005(6) C(15) 0.029(4) 0.075(6) 0.039(4) 0.003(4) -0.004(3) -0.015(4) C(16) 0.056(6) 0.082(7) 0.060(6) 0.004(5) -0.029(4) -0.003(5) C(17) 0.043(5) 0.097(8) 0.048(5) -0.008(5) -0.007(4) -0.015(5) C(18) 0.082(8) 0.126(10) 0.091(8) -0.027(7) -0.008(6) -0.052(7) C(19) 0.048(5) 0.057(5) 0.058(5) -0.003(4) -0.024(4) -0.004(4) C(20) 0.046(5) 0.075(6) 0.060(6) 0.007(4) -0.022(4) -0.018(5) C(21) 0.064(6) 0.079(6) 0.050(5) -0.013(5) -0.030(5) -0.003(5) C(22) 0.070(6) 0.062(6) 0.057(6) -0.014(5) -0.034(5) -0.008(4) C(23) 0.057(5) 0.062(5) 0.045(5) -0.002(4) -0.019(4) -0.012(4) C(24) 0.071(6) 0.067(6) 0.082(7) -0.006(5) -0.036(5) 0.003(5) C(25) 0.064(6) 0.119(9) 0.072(7) 0.023(6) -0.021(5) -0.025(6) C(26) 0.077(7) 0.113(8) 0.060(6) -0.035(6) -0.019(5) 0.009(6) C(27) 0.119(9) 0.070(7) 0.092(8) 0.000(6) -0.046(7) -0.022(6) C(28) 0.086(7) 0.099(8) 0.047(6) -0.009(6) -0.011(5) -0.016(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0006(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4761 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0323 _refine_ls_wR_factor_gt 0.0323 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.647 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.31 _refine_diff_density_max 1.44 #------------------------------------------------------------------------------ _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) S(1) 2.228(2) 1_555 1_555 yes Ir(1) S(2) 2.243(2) 1_555 1_555 yes Ir(1) C(5) 2.191(7) 1_555 1_555 yes Ir(1) C(6) 2.167(7) 1_555 1_555 yes Ir(1) C(7) 2.152(7) 1_555 1_555 yes Ir(1) C(8) 2.199(9) 1_555 1_555 yes Ir(1) C(9) 2.169(8) 1_555 1_555 yes Ir(2) S(3) 2.227(2) 1_555 1_555 yes Ir(2) S(4) 2.241(3) 1_555 1_555 yes Ir(2) C(19) 2.192(8) 1_555 1_555 yes Ir(2) C(20) 2.168(9) 1_555 1_555 yes Ir(2) C(21) 2.160(10) 1_555 1_555 yes Ir(2) C(22) 2.20(1) 1_555 1_555 yes Ir(2) C(23) 2.172(9) 1_555 1_555 yes S(1) C(1) 1.741(7) 1_555 1_555 yes S(2) C(2) 1.700(9) 1_555 1_555 yes S(3) C(15) 1.743(8) 1_555 1_555 yes S(4) C(16) 1.70(1) 1_555 1_555 yes O(1) C(3) 1.19(1) 1_555 1_555 yes O(2) C(3) 1.32(1) 1_555 1_555 yes O(2) C(4) 1.45(1) 1_555 1_555 yes O(3) C(17) 1.18(1) 1_555 1_555 yes O(4) C(17) 1.34(1) 1_555 1_555 yes O(4) C(18) 1.45(2) 1_555 1_555 yes C(1) C(2) 1.34(1) 1_555 1_555 yes C(1) C(3) 1.46(1) 1_555 1_555 yes C(5) C(6) 1.43(1) 1_555 1_555 yes C(5) C(9) 1.44(1) 1_555 1_555 yes C(5) C(10) 1.50(1) 1_555 1_555 yes C(6) C(7) 1.42(1) 1_555 1_555 yes C(6) C(11) 1.50(1) 1_555 1_555 yes C(7) C(8) 1.43(1) 1_555 1_555 yes C(7) C(12) 1.51(1) 1_555 1_555 yes C(8) C(9) 1.42(1) 1_555 1_555 yes C(8) C(13) 1.49(1) 1_555 1_555 yes C(9) C(14) 1.49(1) 1_555 1_555 yes C(15) C(16) 1.32(1) 1_555 1_555 yes C(15) C(17) 1.47(1) 1_555 1_555 yes C(19) C(20) 1.42(1) 1_555 1_555 yes C(19) C(23) 1.43(1) 1_555 1_555 yes C(19) C(24) 1.50(1) 1_555 1_555 yes C(20) C(21) 1.46(1) 1_555 1_555 yes C(20) C(25) 1.49(1) 1_555 1_555 yes C(21) C(22) 1.40(1) 1_555 1_555 yes C(21) C(26) 1.51(1) 1_555 1_555 yes C(22) C(23) 1.45(1) 1_555 1_555 yes C(22) C(27) 1.49(1) 1_555 1_555 yes C(23) C(28) 1.49(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 87.52(8) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 105.2(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(6) 108.8(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(7) 140.4(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(8) 169.0(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(9) 132.2(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 162.9(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(6) 147.7(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(7) 113.0(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(8) 102.8(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(9) 124.5(2) 1_555 1_555 1_555 yes C(5) Ir(1) C(6) 38.3(3) 1_555 1_555 1_555 yes C(5) Ir(1) C(7) 64.0(3) 1_555 1_555 1_555 yes C(5) Ir(1) C(8) 63.9(3) 1_555 1_555 1_555 yes C(5) Ir(1) C(9) 38.4(3) 1_555 1_555 1_555 yes C(6) Ir(1) C(7) 38.4(3) 1_555 1_555 1_555 yes C(6) Ir(1) C(8) 64.1(3) 1_555 1_555 1_555 yes C(6) Ir(1) C(9) 64.2(3) 1_555 1_555 1_555 yes C(7) Ir(1) C(8) 38.3(3) 1_555 1_555 1_555 yes C(7) Ir(1) C(9) 63.9(3) 1_555 1_555 1_555 yes C(8) Ir(1) C(9) 37.9(3) 1_555 1_555 1_555 yes S(3) Ir(2) S(4) 87.41(9) 1_555 1_555 1_555 yes S(3) Ir(2) C(19) 104.7(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(20) 110.0(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(21) 144.0(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(22) 167.8(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(23) 129.3(2) 1_555 1_555 1_555 yes S(4) Ir(2) C(19) 162.3(2) 1_555 1_555 1_555 yes S(4) Ir(2) C(20) 148.7(2) 1_555 1_555 1_555 yes S(4) Ir(2) C(21) 113.0(2) 1_555 1_555 1_555 yes S(4) Ir(2) C(22) 102.4(2) 1_555 1_555 1_555 yes S(4) Ir(2) C(23) 124.1(2) 1_555 1_555 1_555 yes C(19) Ir(2) C(20) 38.1(3) 1_555 1_555 1_555 yes C(19) Ir(2) C(21) 64.1(3) 1_555 1_555 1_555 yes C(19) Ir(2) C(22) 64.1(3) 1_555 1_555 1_555 yes C(19) Ir(2) C(23) 38.2(3) 1_555 1_555 1_555 yes C(20) Ir(2) C(21) 39.4(3) 1_555 1_555 1_555 yes C(20) Ir(2) C(22) 64.7(4) 1_555 1_555 1_555 yes C(20) Ir(2) C(23) 64.6(3) 1_555 1_555 1_555 yes C(21) Ir(2) C(22) 37.5(3) 1_555 1_555 1_555 yes C(21) Ir(2) C(23) 63.9(3) 1_555 1_555 1_555 yes C(22) Ir(2) C(23) 38.8(3) 1_555 1_555 1_555 yes Ir(1) S(1) C(1) 105.5(3) 1_555 1_555 1_555 yes Ir(1) S(2) C(2) 105.4(3) 1_555 1_555 1_555 yes Ir(2) S(3) C(15) 105.7(3) 1_555 1_555 1_555 yes Ir(2) S(4) C(16) 105.2(3) 1_555 1_555 1_555 yes C(3) O(2) C(4) 117.6(8) 1_555 1_555 1_555 yes C(17) O(4) C(18) 115.2(8) 1_555 1_555 1_555 yes S(1) C(1) C(2) 119.5(6) 1_555 1_555 1_555 yes S(1) C(1) C(3) 116.4(6) 1_555 1_555 1_555 yes C(2) C(1) C(3) 124.1(7) 1_555 1_555 1_555 yes S(2) C(2) C(1) 121.9(6) 1_555 1_555 1_555 yes S(2) C(2) H(1) 119.0(7) 1_555 1_555 1_555 no C(1) C(2) H(1) 119.0(8) 1_555 1_555 1_555 no O(1) C(3) O(2) 120.7(8) 1_555 1_555 1_555 yes O(1) C(3) C(1) 125.5(8) 1_555 1_555 1_555 yes O(2) C(3) C(1) 113.8(8) 1_555 1_555 1_555 yes O(2) C(4) H(2) 109.5(8) 1_555 1_555 1_555 no O(2) C(4) H(3) 109(1) 1_555 1_555 1_555 no O(2) C(4) H(4) 109.5(9) 1_555 1_555 1_555 no H(2) C(4) H(3) 109(1) 1_555 1_555 1_555 no H(2) C(4) H(4) 109(1) 1_555 1_555 1_555 no H(3) C(4) H(4) 109.5(9) 1_555 1_555 1_555 no Ir(1) C(5) C(6) 69.9(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(9) 70.0(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 126.1(6) 1_555 1_555 1_555 yes C(6) C(5) C(9) 107.1(8) 1_555 1_555 1_555 yes C(6) C(5) C(10) 127.0(9) 1_555 1_555 1_555 yes C(9) C(5) C(10) 125.9(8) 1_555 1_555 1_555 yes Ir(1) C(6) C(5) 71.7(4) 1_555 1_555 1_555 yes Ir(1) C(6) C(7) 70.2(4) 1_555 1_555 1_555 yes Ir(1) C(6) C(11) 125.6(6) 1_555 1_555 1_555 yes C(5) C(6) C(7) 107.8(8) 1_555 1_555 1_555 yes C(5) C(6) C(11) 128.7(9) 1_555 1_555 1_555 yes C(7) C(6) C(11) 123.5(8) 1_555 1_555 1_555 yes Ir(1) C(7) C(6) 71.4(4) 1_555 1_555 1_555 yes Ir(1) C(7) C(8) 72.6(4) 1_555 1_555 1_555 yes Ir(1) C(7) C(12) 125.2(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 109.0(7) 1_555 1_555 1_555 yes C(6) C(7) C(12) 126.0(7) 1_555 1_555 1_555 yes C(8) C(7) C(12) 124.9(8) 1_555 1_555 1_555 yes Ir(1) C(8) C(7) 69.1(5) 1_555 1_555 1_555 yes Ir(1) C(8) C(9) 69.9(5) 1_555 1_555 1_555 yes Ir(1) C(8) C(13) 127.5(5) 1_555 1_555 1_555 yes C(7) C(8) C(9) 107.0(8) 1_555 1_555 1_555 yes C(7) C(8) C(13) 126.2(7) 1_555 1_555 1_555 yes C(9) C(8) C(13) 126.8(7) 1_555 1_555 1_555 yes Ir(1) C(9) C(5) 71.6(5) 1_555 1_555 1_555 yes Ir(1) C(9) C(8) 72.2(4) 1_555 1_555 1_555 yes Ir(1) C(9) C(14) 127.2(6) 1_555 1_555 1_555 yes C(5) C(9) C(8) 109.0(7) 1_555 1_555 1_555 yes C(5) C(9) C(14) 125.6(8) 1_555 1_555 1_555 yes C(8) C(9) C(14) 125.1(8) 1_555 1_555 1_555 yes C(5) C(10) H(5) 109(1) 1_555 1_555 1_555 no C(5) C(10) H(6) 109.5(9) 1_555 1_555 1_555 no C(5) C(10) H(7) 109.5(8) 1_555 1_555 1_555 no H(5) C(10) H(6) 109.5(9) 1_555 1_555 1_555 no H(5) C(10) H(7) 109(1) 1_555 1_555 1_555 no H(6) C(10) H(7) 109(1) 1_555 1_555 1_555 no C(6) C(11) H(8) 109.5(8) 1_555 1_555 1_555 no C(6) C(11) H(9) 109(1) 1_555 1_555 1_555 no C(6) C(11) H(10) 109.5(9) 1_555 1_555 1_555 no H(8) C(11) H(9) 109.5(10) 1_555 1_555 1_555 no H(8) C(11) H(10) 109(1) 1_555 1_555 1_555 no H(9) C(11) H(10) 109.5(10) 1_555 1_555 1_555 no C(7) C(12) H(11) 109.5(9) 1_555 1_555 1_555 no C(7) C(12) H(12) 109.5(8) 1_555 1_555 1_555 no C(7) C(12) H(13) 109.5(7) 1_555 1_555 1_555 no H(11) C(12) H(12) 109.5(8) 1_555 1_555 1_555 no H(11) C(12) H(13) 109.5(9) 1_555 1_555 1_555 no H(12) C(12) H(13) 109(1) 1_555 1_555 1_555 no C(8) C(13) H(14) 109.5(8) 1_555 1_555 1_555 no C(8) C(13) H(15) 109.5(8) 1_555 1_555 1_555 no C(8) C(13) H(16) 109.5(8) 1_555 1_555 1_555 no H(14) C(13) H(15) 109.5(9) 1_555 1_555 1_555 no H(14) C(13) H(16) 109.5(9) 1_555 1_555 1_555 no H(15) C(13) H(16) 109.5(9) 1_555 1_555 1_555 no C(9) C(14) H(17) 109.5(8) 1_555 1_555 1_555 no C(9) C(14) H(18) 109.5(9) 1_555 1_555 1_555 no C(9) C(14) H(19) 109.5(9) 1_555 1_555 1_555 no H(17) C(14) H(18) 109(1) 1_555 1_555 1_555 no H(17) C(14) H(19) 109.5(10) 1_555 1_555 1_555 no H(18) C(14) H(19) 109.5(9) 1_555 1_555 1_555 no S(3) C(15) C(16) 119.0(7) 1_555 1_555 1_555 yes S(3) C(15) C(17) 121.3(7) 1_555 1_555 1_555 yes C(16) C(15) C(17) 119.6(8) 1_555 1_555 1_555 yes S(4) C(16) C(15) 122.6(7) 1_555 1_555 1_555 yes S(4) C(16) H(20) 118.7(8) 1_555 1_555 1_555 no C(15) C(16) H(20) 118(1) 1_555 1_555 1_555 no O(3) C(17) O(4) 122(1) 1_555 1_555 1_555 yes O(3) C(17) C(15) 126.0(10) 1_555 1_555 1_555 yes O(4) C(17) C(15) 111.8(8) 1_555 1_555 1_555 yes O(4) C(18) H(21) 109.5(9) 1_555 1_555 1_555 no O(4) C(18) H(22) 109(1) 1_555 1_555 1_555 no O(4) C(18) H(23) 109(1) 1_555 1_555 1_555 no H(21) C(18) H(22) 109(1) 1_555 1_555 1_555 no H(21) C(18) H(23) 109(1) 1_555 1_555 1_555 no H(22) C(18) H(23) 109(1) 1_555 1_555 1_555 no Ir(2) C(19) C(20) 70.0(5) 1_555 1_555 1_555 yes Ir(2) C(19) C(23) 70.1(5) 1_555 1_555 1_555 yes Ir(2) C(19) C(24) 124.9(7) 1_555 1_555 1_555 yes C(20) C(19) C(23) 108.7(7) 1_555 1_555 1_555 yes C(20) C(19) C(24) 124.7(8) 1_555 1_555 1_555 yes C(23) C(19) C(24) 126.6(7) 1_555 1_555 1_555 yes Ir(2) C(20) C(19) 71.8(5) 1_555 1_555 1_555 yes Ir(2) C(20) C(21) 70.0(5) 1_555 1_555 1_555 yes Ir(2) C(20) C(25) 127.9(7) 1_555 1_555 1_555 yes C(19) C(20) C(21) 106.3(7) 1_555 1_555 1_555 yes C(19) C(20) C(25) 126.6(8) 1_555 1_555 1_555 yes C(21) C(20) C(25) 126.8(7) 1_555 1_555 1_555 yes Ir(2) C(21) C(20) 70.6(5) 1_555 1_555 1_555 yes Ir(2) C(21) C(22) 72.7(6) 1_555 1_555 1_555 yes Ir(2) C(21) C(26) 126.3(7) 1_555 1_555 1_555 yes C(20) C(21) C(22) 109.7(7) 1_555 1_555 1_555 yes C(20) C(21) C(26) 123.6(8) 1_555 1_555 1_555 yes C(22) C(21) C(26) 126.6(9) 1_555 1_555 1_555 yes Ir(2) C(22) C(21) 69.8(6) 1_555 1_555 1_555 yes Ir(2) C(22) C(23) 69.7(5) 1_555 1_555 1_555 yes Ir(2) C(22) C(27) 125.8(7) 1_555 1_555 1_555 yes C(21) C(22) C(23) 107.2(8) 1_555 1_555 1_555 yes C(21) C(22) C(27) 126.3(8) 1_555 1_555 1_555 yes C(23) C(22) C(27) 126.5(8) 1_555 1_555 1_555 yes Ir(2) C(23) C(19) 71.6(5) 1_555 1_555 1_555 yes Ir(2) C(23) C(22) 71.6(5) 1_555 1_555 1_555 yes Ir(2) C(23) C(28) 128.1(7) 1_555 1_555 1_555 yes C(19) C(23) C(22) 108.1(7) 1_555 1_555 1_555 yes C(19) C(23) C(28) 125.8(7) 1_555 1_555 1_555 yes C(22) C(23) C(28) 125.7(8) 1_555 1_555 1_555 yes C(19) C(24) H(24) 109.5(8) 1_555 1_555 1_555 no C(19) C(24) H(25) 109.5(8) 1_555 1_555 1_555 no C(19) C(24) H(26) 109.5(8) 1_555 1_555 1_555 no H(24) C(24) H(25) 109.5(9) 1_555 1_555 1_555 no H(24) C(24) H(26) 109.5(10) 1_555 1_555 1_555 no H(25) C(24) H(26) 109.5(10) 1_555 1_555 1_555 no C(20) C(25) H(27) 109.5(9) 1_555 1_555 1_555 no C(20) C(25) H(28) 109.5(10) 1_555 1_555 1_555 no C(20) C(25) H(29) 109.5(9) 1_555 1_555 1_555 no H(27) C(25) H(28) 109(1) 1_555 1_555 1_555 no H(27) C(25) H(29) 109(1) 1_555 1_555 1_555 no H(28) C(25) H(29) 109.5(10) 1_555 1_555 1_555 no C(21) C(26) H(30) 109.5(9) 1_555 1_555 1_555 no C(21) C(26) H(31) 109.5(9) 1_555 1_555 1_555 no C(21) C(26) H(32) 109.5(9) 1_555 1_555 1_555 no H(30) C(26) H(31) 109.5(10) 1_555 1_555 1_555 no H(30) C(26) H(32) 109(1) 1_555 1_555 1_555 no H(31) C(26) H(32) 109(1) 1_555 1_555 1_555 no C(22) C(27) H(33) 109.5(10) 1_555 1_555 1_555 no C(22) C(27) H(34) 109.5(8) 1_555 1_555 1_555 no C(22) C(27) H(35) 109(1) 1_555 1_555 1_555 no H(33) C(27) H(34) 109(1) 1_555 1_555 1_555 no H(33) C(27) H(35) 109.5(9) 1_555 1_555 1_555 no H(34) C(27) H(35) 109(1) 1_555 1_555 1_555 no C(23) C(28) H(36) 109.5(8) 1_555 1_555 1_555 no C(23) C(28) H(37) 109.5(9) 1_555 1_555 1_555 no C(23) C(28) H(38) 109.5(9) 1_555 1_555 1_555 no H(36) C(28) H(37) 109(1) 1_555 1_555 1_555 no H(36) C(28) H(38) 109.5(10) 1_555 1_555 1_555 no H(37) C(28) H(38) 109.5(9) 1_555 1_555 1_555 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 O(1) C(24) 3.13(1) 1_555 1_556 ? O(1) C(19) 3.33(1) 1_555 1_556 ? O(2) C(27) 3.49(1) 1_555 2_556 ? O(2) C(28) 3.57(1) 1_555 1_456 ? O(3) C(25) 3.44(1) 1_555 1_655 ? O(3) C(10) 3.58(1) 1_555 1_555 ? C(17) C(25) 3.56(1) 1_555 1_655 ? #------------------------------------------------------------------------------ #===END