Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2007-06-28 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? _publ_contact_author_name 'Shigeki Kuwata' _publ_contact_author_email skuwata@apc.titech.ac.jp _publ_contact_author_fax 81(3)57342637 _publ_contact_author_phone 81(3)57342150 _publ_contact_author_address ; O-okayama 2-12-1-S1-39, Meguro-ku, Tokyo 152-8552, Japan ; _publ_requested_category CM _publ_section_title ; Silylenediamido [(CH3)2Si(NTs)22-; Ts = p-CH3C6H4SO2] complexes of iridium: synthesis, structures and facile Si-N bond cleavage ; _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Carruthers, J.R., Rollett,J.S., Betteridge, P.W., Kinna, D., Pearce, L., Larsen, A., and Gabe, E.(1999) CRYSTALS Issue 11, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Shigeki Kuwata' 'Takao Ikariya' 'Koji Ishiwata' #============================================================================== data___2 _database_code_depnum_ccdc_archive 'CCDC 647948' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H35 Ir N2 O4 S2 Si ' _chemical_formula_moiety 'C26 H35 Ir N2 O4 S2 Si ' _chemical_formula_weight 724.00 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 14.045(4) _cell_length_b 18.430(5) _cell_length_c 22.740(6) _cell_angle_alpha 90.0000 _cell_angle_beta 98.606(3) _cell_angle_gamma 90.0000 _cell_volume 5820(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 19413 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour darkred _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880.00 _exptl_absorpt_coefficient_mu 4.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.381 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 51953 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 31.42 _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 13204 _reflns_number_gt 8986 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1302 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 13188 _refine_ls_number_parameters 719 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.6000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 4.35 _refine_diff_density_min -4.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.72825(2) 0.253730(10) 0.000110(10) 0.02052(6) Uani 1.00 1 d . . . Ir(2) Ir 0.75232(2) 0.00287(2) 0.504830(10) 0.02074(6) Uani 1.00 1 d . . . S(1) S 0.77134(13) 0.34932(11) -0.11785(8) 0.0341(5) Uani 1.00 1 d . . . S(2) S 0.67659(14) 0.36416(11) 0.10888(8) 0.0347(5) Uani 1.00 1 d . . . S(3) S 0.79854(14) 0.09769(12) 0.38749(9) 0.0375(5) Uani 1.00 1 d . . . S(4) S 0.70799(13) 0.11380(11) 0.61496(8) 0.0312(4) Uani 1.00 1 d . . . Si(1) Si 0.72936(13) 0.41140(11) -0.00550(9) 0.0267(5) Uani 1.00 1 d . . . Si(2) Si 0.74610(13) 0.16081(11) 0.49746(8) 0.0266(5) Uani 1.00 1 d . . . O(1) O 0.8537(3) 0.3050(3) -0.1254(2) 0.0531(19) Uani 1.00 1 d . . . O(2) O 0.7786(4) 0.4263(3) -0.1284(2) 0.059(2) Uani 1.00 1 d . . . O(3) O 0.5914(3) 0.3251(3) 0.1182(2) 0.0518(18) Uani 1.00 1 d . . . O(4) O 0.6745(5) 0.4425(3) 0.1131(2) 0.059(2) Uani 1.00 1 d . . . O(5) O 0.8809(4) 0.0529(3) 0.3814(2) 0.057(2) Uani 1.00 1 d . . . O(6) O 0.8068(5) 0.1739(3) 0.3769(3) 0.067(2) Uani 1.00 1 d . . . O(7) O 0.6228(3) 0.0767(3) 0.6274(2) 0.0487(18) Uani 1.00 1 d . . . O(8) O 0.7071(4) 0.1920(3) 0.6188(2) 0.0490(18) Uani 1.00 1 d . . . N(1) N 0.7426(4) 0.3399(3) -0.0536(2) 0.0286(15) Uani 1.00 1 d . . . N(2) N 0.7072(4) 0.3464(3) 0.0461(2) 0.0296(16) Uani 1.00 1 d . . . N(3) N 0.7674(4) 0.0891(3) 0.4515(2) 0.0290(16) Uani 1.00 1 d . . . N(4) N 0.7327(4) 0.0945(3) 0.5508(2) 0.0250(15) Uani 1.00 1 d . . . C(1) C 0.8415(5) 0.4640(4) 0.0177(4) 0.044(2) Uani 1.00 1 d . . . C(2) C 0.6281(5) 0.4731(4) -0.0310(4) 0.046(2) Uani 1.00 1 d . . . C(3) C 0.6750(5) 0.3143(4) -0.1689(3) 0.033(2) Uani 1.00 1 d . . . C(4) C 0.5826(5) 0.3099(4) -0.1548(3) 0.041(2) Uani 1.00 1 d . . . C(5) C 0.5110(6) 0.2795(5) -0.1963(4) 0.047(2) Uani 1.00 1 d . . . C(6) C 0.5282(6) 0.2555(4) -0.2512(3) 0.043(2) Uani 1.00 1 d . . . C(7) C 0.6210(6) 0.2626(5) -0.2642(4) 0.054(2) Uani 1.00 1 d . . . C(8) C 0.6929(6) 0.2913(5) -0.2239(4) 0.051(2) Uani 1.00 1 d . . . C(9) C 0.4494(8) 0.2204(6) -0.2947(5) 0.071(3) Uani 1.00 1 d . . . C(10) C 0.7710(5) 0.3328(4) 0.1641(3) 0.038(2) Uani 1.00 1 d . . . C(11) C 0.8653(6) 0.3465(5) 0.1590(3) 0.049(2) Uani 1.00 1 d . . . C(12) C 0.9370(6) 0.3227(5) 0.2029(3) 0.052(2) Uani 1.00 1 d . . . C(13) C 0.9149(7) 0.2840(5) 0.2517(4) 0.051(2) Uani 1.00 1 d . . . C(14) C 0.8195(7) 0.2722(5) 0.2560(4) 0.054(2) Uani 1.00 1 d . . . C(15) C 0.7469(6) 0.2956(5) 0.2125(3) 0.051(2) Uani 1.00 1 d . . . C(16) C 0.9943(8) 0.2548(7) 0.2981(5) 0.084(4) Uani 1.00 1 d . . . C(17) C 0.8171(4) 0.1613(3) -0.0050(4) 0.036(2) Uani 1.00 1 d . . . C(18) C 0.7360(5) 0.1533(3) -0.0496(3) 0.0302(19) Uani 1.00 1 d . . . C(19) C 0.6528(4) 0.1544(3) -0.0204(3) 0.0320(19) Uani 1.00 1 d . . . C(20) C 0.6833(5) 0.1569(3) 0.0423(3) 0.033(2) Uani 1.00 1 d . . . C(21) C 0.7851(5) 0.1613(4) 0.0525(3) 0.036(2) Uani 1.00 1 d . . . C(22) C 0.9202(5) 0.1660(4) -0.0151(4) 0.053(2) Uani 1.00 1 d . . . C(23) C 0.7380(7) 0.1412(4) -0.1151(4) 0.052(2) Uani 1.00 1 d . . . C(24) C 0.5509(5) 0.1491(4) -0.0508(4) 0.047(2) Uani 1.00 1 d . . . C(25) C 0.6194(7) 0.1515(5) 0.0893(4) 0.057(3) Uani 1.00 1 d . . . C(26) C 0.8478(6) 0.1622(4) 0.1106(4) 0.055(2) Uani 1.00 1 d . . . C(27) C 0.8490(6) 0.2214(4) 0.5181(4) 0.045(2) Uani 1.00 1 d . . . C(28) C 0.6353(5) 0.2127(4) 0.4699(4) 0.043(2) Uani 1.00 1 d . . . C(29) C 0.7031(5) 0.0634(4) 0.3350(3) 0.035(2) Uani 1.00 1 d . . . C(30) C 0.6104(5) 0.0567(4) 0.3473(3) 0.040(2) Uani 1.00 1 d . . . C(31) C 0.5392(6) 0.0268(5) 0.3063(4) 0.057(2) Uani 1.00 1 d . . . C(32) C 0.5591(6) 0.0039(5) 0.2512(4) 0.051(2) Uani 1.00 1 d . . . C(33) C 0.6512(7) 0.0125(6) 0.2389(4) 0.063(3) Uani 1.00 1 d . . . C(34) C 0.7230(7) 0.0421(6) 0.2807(4) 0.056(3) Uani 1.00 1 d . . . C(35) C 0.4817(8) -0.0322(7) 0.2066(5) 0.082(4) Uani 1.00 1 d . . . C(36) C 0.8046(5) 0.0809(4) 0.6668(3) 0.0310(19) Uani 1.00 1 d . . . C(37) C 0.8993(5) 0.0871(4) 0.6573(3) 0.035(2) Uani 1.00 1 d . . . C(38) C 0.9732(5) 0.0611(5) 0.6981(4) 0.048(2) Uani 1.00 1 d . . . C(39) C 0.9547(6) 0.0275(4) 0.7501(3) 0.043(2) Uani 1.00 1 d . . . C(40) C 0.8597(7) 0.0213(6) 0.7594(4) 0.060(3) Uani 1.00 1 d . . . C(41) C 0.7846(6) 0.0485(5) 0.7182(3) 0.048(2) Uani 1.00 1 d . . . C(42) C 1.0349(7) -0.0054(6) 0.7938(4) 0.077(3) Uani 1.00 1 d . . . C(43) C 0.8351(4) -0.0934(3) 0.4976(4) 0.035(2) Uani 1.00 1 d . . . C(44) C 0.7509(5) -0.0970(3) 0.4537(3) 0.036(2) Uani 1.00 1 d . . . C(45) C 0.6707(4) -0.0933(3) 0.4851(3) 0.0308(19) Uani 1.00 1 d . . . C(46) C 0.7052(5) -0.0930(3) 0.5485(3) 0.036(2) Uani 1.00 1 d . . . C(47) C 0.8078(5) -0.0905(3) 0.5543(3) 0.036(2) Uani 1.00 1 d . . . C(48) C 0.9373(5) -0.0940(4) 0.4837(5) 0.072(3) Uani 1.00 1 d . . . C(49) C 0.7486(6) -0.1078(4) 0.3881(4) 0.052(2) Uani 1.00 1 d . . . C(50) C 0.5677(5) -0.0931(4) 0.4578(4) 0.048(2) Uani 1.00 1 d . . . C(51) C 0.6444(7) -0.0975(5) 0.5970(4) 0.063(3) Uani 1.00 1 d . . . C(52) C 0.8744(7) -0.0938(5) 0.6125(4) 0.067(3) Uani 1.00 1 d . . . H(1) H 0.8759 0.4432 0.0528 0.052 Uiso 1.00 1 c R . . H(2) H 0.8256 0.5129 0.0253 0.052 Uiso 1.00 1 c R . . H(3) H 0.8803 0.4628 -0.0131 0.052 Uiso 1.00 1 c R . . H(4) H 0.6496 0.5112 -0.0539 0.055 Uiso 1.00 1 c R . . H(5) H 0.6044 0.4931 0.0025 0.055 Uiso 1.00 1 c R . . H(6) H 0.5781 0.4469 -0.0546 0.055 Uiso 1.00 1 c R . . H(7) H 0.5687 0.3272 -0.1177 0.051 Uiso 1.00 1 c R . . H(8) H 0.4478 0.2753 -0.1865 0.056 Uiso 1.00 1 c R . . H(9) H 0.6350 0.2472 -0.3019 0.064 Uiso 1.00 1 c R . . H(10) H 0.7561 0.2954 -0.2337 0.062 Uiso 1.00 1 c R . . H(11) H 0.4493 0.1695 -0.2881 0.083 Uiso 1.00 1 c R . . H(12) H 0.4603 0.2298 -0.3342 0.083 Uiso 1.00 1 c R . . H(13) H 0.3889 0.2401 -0.2890 0.083 Uiso 1.00 1 c R . . H(14) H 0.8810 0.3724 0.1256 0.058 Uiso 1.00 1 c R . . H(15) H 1.0025 0.3327 0.1999 0.062 Uiso 1.00 1 c R . . H(16) H 0.8032 0.2473 0.2897 0.065 Uiso 1.00 1 c R . . H(17) H 0.6814 0.2862 0.2156 0.061 Uiso 1.00 1 c R . . H(18) H 1.0111 0.2073 0.2871 0.097 Uiso 1.00 1 c R . . H(19) H 0.9726 0.2531 0.3357 0.097 Uiso 1.00 1 c R . . H(20) H 1.0491 0.2855 0.3006 0.097 Uiso 1.00 1 c R . . H(21) H 0.9227 0.1646 -0.0566 0.065 Uiso 1.00 1 c R . . H(22) H 0.9555 0.1262 0.0037 0.065 Uiso 1.00 1 c R . . H(23) H 0.9476 0.2101 0.0010 0.065 Uiso 1.00 1 c R . . H(24) H 0.6740 0.1360 -0.1351 0.063 Uiso 1.00 1 c R . . H(25) H 0.7735 0.0985 -0.1203 0.063 Uiso 1.00 1 c R . . H(26) H 0.7676 0.1816 -0.1310 0.063 Uiso 1.00 1 c R . . H(27) H 0.5086 0.1493 -0.0219 0.055 Uiso 1.00 1 c R . . H(28) H 0.5425 0.1053 -0.0731 0.055 Uiso 1.00 1 c R . . H(29) H 0.5368 0.1893 -0.0767 0.055 Uiso 1.00 1 c R . . H(30) H 0.6572 0.1540 0.1275 0.072 Uiso 1.00 1 c R . . H(31) H 0.5859 0.1066 0.0852 0.072 Uiso 1.00 1 c R . . H(32) H 0.5744 0.1903 0.0848 0.072 Uiso 1.00 1 c R . . H(33) H 0.9132 0.1622 0.1044 0.062 Uiso 1.00 1 c R . . H(34) H 0.8356 0.1205 0.1328 0.062 Uiso 1.00 1 c R . . H(35) H 0.8353 0.2046 0.1319 0.062 Uiso 1.00 1 c R . . H(36) H 0.8864 0.2045 0.5537 0.055 Uiso 1.00 1 c R . . H(37) H 0.8264 0.2690 0.5241 0.055 Uiso 1.00 1 c R . . H(38) H 0.8874 0.2221 0.4871 0.055 Uiso 1.00 1 c R . . H(39) H 0.6504 0.2510 0.4450 0.051 Uiso 1.00 1 c R . . H(40) H 0.6092 0.2323 0.5027 0.051 Uiso 1.00 1 c R . . H(41) H 0.5894 0.1813 0.4480 0.051 Uiso 1.00 1 c R . . H(42) H 0.5954 0.0731 0.3844 0.049 Uiso 1.00 1 c R . . H(43) H 0.4759 0.0220 0.3157 0.068 Uiso 1.00 1 c R . . H(44) H 0.6661 -0.0020 0.2013 0.076 Uiso 1.00 1 c R . . H(45) H 0.7862 0.0477 0.2712 0.069 Uiso 1.00 1 c R . . H(46) H 0.4835 -0.0832 0.2129 0.095 Uiso 1.00 1 c R . . H(47) H 0.4931 -0.0220 0.1673 0.095 Uiso 1.00 1 c R . . H(48) H 0.4203 -0.0140 0.2120 0.095 Uiso 1.00 1 c R . . H(49) H 0.9133 0.1098 0.6221 0.042 Uiso 1.00 1 c R . . H(50) H 1.0378 0.0660 0.6908 0.056 Uiso 1.00 1 c R . . H(51) H 0.8454 -0.0015 0.7945 0.072 Uiso 1.00 1 c R . . H(52) H 0.7200 0.0445 0.7256 0.059 Uiso 1.00 1 c R . . H(53) H 1.0435 -0.0548 0.7837 0.088 Uiso 1.00 1 c R . . H(54) H 1.0186 -0.0026 0.8328 0.088 Uiso 1.00 1 c R . . H(55) H 1.0930 0.0205 0.7924 0.088 Uiso 1.00 1 c R . . H(56) H 0.9804 -0.0924 0.5202 0.087 Uiso 1.00 1 c R . . H(57) H 0.9483 -0.1370 0.4627 0.087 Uiso 1.00 1 c R . . H(58) H 0.9478 -0.0529 0.4603 0.087 Uiso 1.00 1 c R . . H(59) H 0.8127 -0.1101 0.3795 0.063 Uiso 1.00 1 c R . . H(60) H 0.7159 -0.1517 0.3761 0.063 Uiso 1.00 1 c R . . H(61) H 0.7159 -0.0682 0.3672 0.063 Uiso 1.00 1 c R . . H(62) H 0.5634 -0.0941 0.4158 0.056 Uiso 1.00 1 c R . . H(63) H 0.5365 -0.1347 0.4708 0.056 Uiso 1.00 1 c R . . H(64) H 0.5374 -0.0505 0.4695 0.056 Uiso 1.00 1 c R . . H(65) H 0.5785 -0.1006 0.5799 0.079 Uiso 1.00 1 c R . . H(66) H 0.6617 -0.1393 0.6207 0.079 Uiso 1.00 1 c R . . H(67) H 0.6542 -0.0553 0.6212 0.079 Uiso 1.00 1 c R . . H(68) H 0.8369 -0.0946 0.6440 0.076 Uiso 1.00 1 c R . . H(69) H 0.9127 -0.1364 0.6141 0.076 Uiso 1.00 1 c R . . H(70) H 0.9151 -0.0523 0.6166 0.076 Uiso 1.00 1 c R . . 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) 0.02368(13) 0.01520(14) 0.02243(14) 0.00133(10) 0.00259(9) -0.00018(9) Ir(2) 0.02381(13) 0.01394(14) 0.02403(14) 0.00051(8) 0.00213(9) 0.00096(9) S(1) 0.0360(9) 0.0416(11) 0.0264(9) -0.0081(7) 0.0106(7) -0.0024(8) S(2) 0.0417(10) 0.0386(10) 0.0243(9) 0.0087(7) 0.0070(7) -0.0027(8) S(3) 0.0452(10) 0.0412(11) 0.0283(10) -0.0108(8) 0.0126(7) 0.0043(8) S(4) 0.0338(9) 0.0357(10) 0.0243(9) 0.0075(7) 0.0045(6) -0.0034(7) Si(1) 0.0332(9) 0.0193(10) 0.0271(10) -0.0001(7) 0.0029(7) -0.0014(7) Si(2) 0.0340(10) 0.0142(9) 0.0305(12) 0.0015(6) 0.0014(8) 0.0013(6) O(1) 0.033(2) 0.085(4) 0.043(3) 0.001(2) 0.012(2) -0.020(3) O(2) 0.090(4) 0.052(4) 0.038(3) -0.026(3) 0.018(3) 0.012(3) O(3) 0.030(2) 0.089(5) 0.038(3) 0.001(2) 0.011(2) 0.000(3) O(4) 0.095(4) 0.044(3) 0.035(3) 0.030(3) 0.005(3) -0.014(2) O(5) 0.037(3) 0.087(5) 0.050(4) -0.002(3) 0.014(2) -0.014(3) O(6) 0.103(5) 0.049(4) 0.047(4) -0.033(3) 0.010(3) 0.015(3) O(7) 0.032(2) 0.072(4) 0.043(3) 0.006(2) 0.007(2) 0.005(3) O(8) 0.067(3) 0.036(3) 0.045(3) 0.015(2) 0.014(2) -0.010(2) N(1) 0.043(3) 0.018(2) 0.025(3) 0.001(2) 0.003(2) 0.001(2) N(2) 0.041(3) 0.027(3) 0.021(3) 0.007(2) 0.007(2) -0.001(2) N(3) 0.048(3) 0.020(3) 0.020(3) -0.003(2) 0.007(2) 0.005(2) N(4) 0.038(3) 0.017(2) 0.022(3) 0.008(2) 0.007(2) -0.002(2) C(1) 0.042(4) 0.036(4) 0.050(5) -0.010(3) -0.005(3) -0.002(3) C(2) 0.053(4) 0.032(4) 0.051(5) 0.007(3) 0.008(3) 0.016(3) C(3) 0.036(3) 0.036(4) 0.029(4) 0.002(3) 0.011(3) 0.003(3) C(4) 0.038(4) 0.053(5) 0.035(4) -0.004(3) 0.013(3) -0.002(3) C(5) 0.041(4) 0.057(5) 0.043(5) -0.011(3) 0.008(3) 0.002(4) C(6) 0.051(4) 0.044(4) 0.031(4) -0.003(3) -0.004(3) -0.003(3) C(7) 0.047(4) 0.081(7) 0.032(4) 0.012(4) 0.002(3) -0.017(4) C(8) 0.037(4) 0.075(6) 0.043(5) 0.007(4) 0.014(3) -0.007(4) C(9) 0.080(7) 0.070(7) 0.057(7) -0.005(5) -0.013(5) -0.017(5) C(10) 0.049(4) 0.044(4) 0.020(3) -0.004(3) 0.001(3) 0.002(3) C(11) 0.053(5) 0.059(5) 0.034(4) -0.015(4) 0.004(3) 0.017(4) C(12) 0.042(4) 0.079(6) 0.033(4) -0.014(4) -0.002(3) 0.005(4) C(13) 0.065(5) 0.050(5) 0.035(5) 0.003(4) -0.005(4) 0.004(4) C(14) 0.072(6) 0.063(6) 0.028(4) -0.001(4) 0.011(4) 0.016(4) C(15) 0.059(5) 0.069(6) 0.026(4) -0.010(4) 0.013(3) 0.009(4) C(16) 0.081(8) 0.110(10) 0.051(7) 0.017(6) -0.017(5) 0.021(6) C(17) 0.029(3) 0.019(3) 0.059(5) 0.005(2) 0.001(3) -0.007(3) C(18) 0.044(4) 0.011(3) 0.038(4) 0.005(2) 0.015(3) -0.006(2) C(19) 0.029(3) 0.016(3) 0.049(4) -0.006(2) -0.003(3) -0.004(3) C(20) 0.038(3) 0.022(3) 0.040(4) -0.001(2) 0.013(3) 0.001(3) C(21) 0.046(4) 0.021(3) 0.038(4) 0.007(3) 0.001(3) 0.001(3) C(22) 0.041(4) 0.039(4) 0.083(7) 0.014(3) 0.022(4) 0.001(4) C(23) 0.084(6) 0.024(4) 0.049(5) -0.003(4) 0.018(4) -0.012(3) C(24) 0.034(4) 0.030(4) 0.074(6) 0.001(3) -0.002(3) -0.004(4) C(25) 0.078(6) 0.045(5) 0.057(6) -0.006(4) 0.037(5) 0.016(4) C(26) 0.072(6) 0.034(4) 0.048(5) 0.017(4) -0.023(4) 0.003(4) C(27) 0.051(4) 0.028(4) 0.058(6) -0.005(3) 0.012(4) 0.009(3) C(28) 0.046(4) 0.027(4) 0.054(5) 0.006(3) -0.003(3) 0.005(3) C(29) 0.049(4) 0.036(4) 0.022(3) 0.004(3) 0.010(3) -0.003(3) C(30) 0.046(4) 0.052(5) 0.024(4) 0.001(3) 0.010(3) -0.007(3) C(31) 0.054(5) 0.079(7) 0.036(5) -0.004(4) -0.001(3) -0.004(4) C(32) 0.064(5) 0.053(6) 0.034(4) 0.007(4) -0.001(3) -0.006(4) C(33) 0.082(7) 0.081(7) 0.025(4) 0.015(5) 0.009(4) -0.025(5) C(34) 0.065(5) 0.082(7) 0.025(4) 0.009(5) 0.019(4) -0.004(4) C(35) 0.100(8) 0.085(9) 0.052(7) 0.000(6) -0.016(6) -0.023(6) C(36) 0.036(3) 0.037(4) 0.020(3) 0.003(2) 0.004(2) -0.002(3) C(37) 0.035(3) 0.045(4) 0.026(3) -0.001(3) 0.007(2) 0.008(3) C(38) 0.038(4) 0.059(5) 0.043(5) -0.003(3) -0.003(3) 0.000(4) C(39) 0.054(4) 0.044(5) 0.028(4) 0.003(3) -0.001(3) -0.000(3) C(40) 0.064(6) 0.078(7) 0.037(5) -0.000(5) 0.005(4) 0.027(5) C(41) 0.048(4) 0.075(6) 0.024(4) 0.012(4) 0.014(3) 0.016(4) C(42) 0.074(6) 0.105(10) 0.042(5) 0.013(6) -0.020(4) 0.004(6) C(43) 0.024(3) 0.016(3) 0.064(5) 0.002(2) 0.004(3) -0.002(3) C(44) 0.054(4) 0.010(3) 0.042(4) -0.006(2) -0.001(3) -0.002(3) C(45) 0.026(3) 0.015(3) 0.049(4) -0.004(2) 0.001(2) -0.002(3) C(46) 0.047(4) 0.016(3) 0.045(4) -0.003(2) 0.009(3) 0.009(3) C(47) 0.038(4) 0.011(3) 0.055(5) 0.002(2) -0.008(3) 0.006(3) C(48) 0.030(4) 0.035(5) 0.153(12) 0.004(3) 0.023(5) -0.010(6) C(49) 0.071(6) 0.040(5) 0.046(5) 0.004(4) 0.016(4) -0.014(4) C(50) 0.034(4) 0.033(4) 0.072(6) -0.005(3) -0.004(3) -0.002(4) C(51) 0.087(7) 0.056(6) 0.054(6) -0.020(5) 0.033(5) -0.001(5) C(52) 0.074(6) 0.035(5) 0.079(7) 0.009(4) -0.028(5) 0.009(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) N(1) 2.032(5) yes . . Ir(1) N(2) 2.048(5) yes . . Ir(1) C(17) 2.125(7) yes . . Ir(1) C(18) 2.181(7) yes . . Ir(1) C(19) 2.132(6) yes . . Ir(1) C(20) 2.165(7) yes . . Ir(1) C(21) 2.162(7) yes . . Ir(2) N(3) 2.030(6) yes . . Ir(2) N(4) 2.026(5) yes . . Ir(2) C(43) 2.141(6) yes . . Ir(2) C(44) 2.175(7) yes . . Ir(2) C(45) 2.121(6) yes . . Ir(2) C(46) 2.179(7) yes . . Ir(2) C(47) 2.138(7) yes . . S(1) O(1) 1.447(6) yes . . S(1) O(2) 1.444(6) yes . . S(1) N(1) 1.583(6) yes . . S(1) C(3) 1.769(7) yes . . S(2) O(3) 1.440(6) yes . . S(2) O(4) 1.448(6) yes . . S(2) N(2) 1.585(6) yes . . S(2) C(10) 1.780(7) yes . . S(3) O(5) 1.444(6) yes . . S(3) O(6) 1.432(7) yes . . S(3) N(3) 1.588(6) yes . . S(3) C(29) 1.772(7) yes . . S(4) O(7) 1.441(6) yes . . S(4) O(8) 1.445(6) yes . . S(4) N(4) 1.591(6) yes . . S(4) C(36) 1.767(6) yes . . Si(1) N(1) 1.740(6) yes . . Si(1) N(2) 1.737(6) yes . . Si(1) C(1) 1.857(7) yes . . Si(1) C(2) 1.846(8) yes . . Si(2) N(3) 1.740(6) yes . . Si(2) N(4) 1.751(6) yes . . Si(2) C(27) 1.831(8) yes . . Si(2) C(28) 1.854(7) yes . . C(3) C(4) 1.385(11) yes . . C(3) C(8) 1.379(12) yes . . C(4) C(5) 1.389(11) yes . . C(5) C(6) 1.380(12) yes . . C(6) C(7) 1.386(13) yes . . C(6) C(9) 1.514(13) yes . . C(7) C(8) 1.365(12) yes . . C(10) C(11) 1.369(11) yes . . C(10) C(15) 1.381(12) yes . . C(11) C(12) 1.380(11) yes . . C(12) C(13) 1.393(13) yes . . C(13) C(14) 1.376(14) yes . . C(13) C(16) 1.514(14) yes . . C(14) C(15) 1.380(12) yes . . C(17) C(18) 1.415(10) yes . . C(17) C(21) 1.443(12) yes . . C(17) C(22) 1.503(11) yes . . C(18) C(19) 1.429(11) yes . . C(18) C(23) 1.508(12) yes . . C(19) C(20) 1.428(11) yes . . C(19) C(24) 1.496(9) yes . . C(20) C(21) 1.417(10) yes . . C(20) C(25) 1.497(13) yes . . C(21) C(26) 1.474(11) yes . . C(29) C(30) 1.377(11) yes . . C(29) C(34) 1.365(12) yes . . C(30) C(31) 1.377(11) yes . . C(31) C(32) 1.389(13) yes . . C(32) C(33) 1.373(14) yes . . C(32) C(35) 1.523(14) yes . . C(33) C(34) 1.388(13) yes . . C(36) C(37) 1.383(10) yes . . C(36) C(41) 1.378(11) yes . . C(37) C(38) 1.371(10) yes . . C(38) C(39) 1.393(12) yes . . C(39) C(40) 1.387(13) yes . . C(39) C(42) 1.514(13) yes . . C(40) C(41) 1.394(12) yes . . C(43) C(44) 1.431(10) yes . . C(43) C(47) 1.399(13) yes . . C(43) C(48) 1.515(11) yes . . C(44) C(45) 1.423(11) yes . . C(44) C(49) 1.500(12) yes . . C(45) C(46) 1.450(11) yes . . C(45) C(50) 1.487(9) yes . . C(46) C(47) 1.428(10) yes . . C(46) C(51) 1.494(14) yes . . C(47) C(52) 1.505(12) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(2) H(5) 0.950 no . . C(2) H(6) 0.950 no . . C(4) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(7) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(11) H(14) 0.950 no . . C(12) H(15) 0.950 no . . C(14) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(22) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(25) H(30) 0.950 no . . C(25) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(26) H(33) 0.950 no . . C(26) H(34) 0.950 no . . C(26) H(35) 0.950 no . . C(27) H(36) 0.950 no . . C(27) H(37) 0.950 no . . C(27) H(38) 0.950 no . . C(28) H(39) 0.950 no . . C(28) H(40) 0.950 no . . C(28) H(41) 0.950 no . . C(30) H(42) 0.950 no . . C(31) H(43) 0.950 no . . C(33) H(44) 0.950 no . . C(34) H(45) 0.950 no . . C(35) H(46) 0.950 no . . C(35) H(47) 0.950 no . . C(35) H(48) 0.950 no . . C(37) H(49) 0.950 no . . C(38) H(50) 0.950 no . . C(40) H(51) 0.950 no . . C(41) H(52) 0.950 no . . C(42) H(53) 0.950 no . . C(42) H(54) 0.950 no . . C(42) H(55) 0.950 no . . C(48) H(56) 0.950 no . . C(48) H(57) 0.950 no . . C(48) H(58) 0.950 no . . C(49) H(59) 0.950 no . . C(49) H(60) 0.950 no . . C(49) H(61) 0.950 no . . C(50) H(62) 0.950 no . . C(50) H(63) 0.950 no . . C(50) H(64) 0.950 no . . C(51) H(65) 0.950 no . . C(51) H(66) 0.950 no . . C(51) H(67) 0.950 no . . C(52) H(68) 0.950 no . . C(52) H(69) 0.950 no . . C(52) H(70) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ir(1) N(2) 71.9(2) yes . . . N(1) Ir(1) C(17) 118.9(2) yes . . . N(1) Ir(1) C(18) 109.6(2) yes . . . N(1) Ir(1) C(19) 129.1(2) yes . . . N(1) Ir(1) C(20) 166.5(2) yes . . . N(1) Ir(1) C(21) 152.3(2) yes . . . N(2) Ir(1) C(17) 145.8(2) yes . . . N(2) Ir(1) C(18) 174.6(2) yes . . . N(2) Ir(1) C(19) 136.3(2) yes . . . N(2) Ir(1) C(20) 112.8(2) yes . . . N(2) Ir(1) C(21) 116.5(2) yes . . . C(17) Ir(1) C(18) 38.3(2) yes . . . C(17) Ir(1) C(19) 64.9(2) yes . . . C(17) Ir(1) C(20) 64.9(2) yes . . . C(17) Ir(1) C(21) 39.3(3) yes . . . C(18) Ir(1) C(19) 38.7(2) yes . . . C(18) Ir(1) C(20) 64.6(3) yes . . . C(18) Ir(1) C(21) 64.8(2) yes . . . C(19) Ir(1) C(20) 38.8(2) yes . . . C(19) Ir(1) C(21) 64.8(2) yes . . . C(20) Ir(1) C(21) 38.2(2) yes . . . N(3) Ir(2) N(4) 72.0(2) yes . . . N(3) Ir(2) C(43) 119.7(2) yes . . . N(3) Ir(2) C(44) 109.6(2) yes . . . N(3) Ir(2) C(45) 129.0(2) yes . . . N(3) Ir(2) C(46) 166.9(2) yes . . . N(3) Ir(2) C(47) 151.9(2) yes . . . N(4) Ir(2) C(43) 148.0(2) yes . . . N(4) Ir(2) C(44) 171.7(2) yes . . . N(4) Ir(2) C(45) 134.0(2) yes . . . N(4) Ir(2) C(46) 111.5(2) yes . . . N(4) Ir(2) C(47) 117.8(2) yes . . . C(43) Ir(2) C(44) 38.7(2) yes . . . C(43) Ir(2) C(45) 64.8(2) yes . . . C(43) Ir(2) C(46) 64.4(3) yes . . . C(43) Ir(2) C(47) 38.2(3) yes . . . C(44) Ir(2) C(45) 38.6(3) yes . . . C(44) Ir(2) C(46) 65.1(3) yes . . . C(44) Ir(2) C(47) 64.7(3) yes . . . C(45) Ir(2) C(46) 39.4(2) yes . . . C(45) Ir(2) C(47) 65.2(2) yes . . . C(46) Ir(2) C(47) 38.6(2) yes . . . O(1) S(1) O(2) 117.1(4) yes . . . O(1) S(1) N(1) 111.5(3) yes . . . O(1) S(1) C(3) 105.2(3) yes . . . O(2) S(1) N(1) 107.2(3) yes . . . O(2) S(1) C(3) 108.4(3) yes . . . N(1) S(1) C(3) 106.9(3) yes . . . O(3) S(2) O(4) 117.6(4) yes . . . O(3) S(2) N(2) 111.9(3) yes . . . O(3) S(2) C(10) 106.4(3) yes . . . O(4) S(2) N(2) 106.0(3) yes . . . O(4) S(2) C(10) 107.3(3) yes . . . N(2) S(2) C(10) 107.1(3) yes . . . O(5) S(3) O(6) 117.2(4) yes . . . O(5) S(3) N(3) 111.4(3) yes . . . O(5) S(3) C(29) 105.6(3) yes . . . O(6) S(3) N(3) 107.0(3) yes . . . O(6) S(3) C(29) 108.0(3) yes . . . N(3) S(3) C(29) 107.3(3) yes . . . O(7) S(4) O(8) 116.5(3) yes . . . O(7) S(4) N(4) 112.0(3) yes . . . O(7) S(4) C(36) 106.5(3) yes . . . O(8) S(4) N(4) 106.5(3) yes . . . O(8) S(4) C(36) 108.4(3) yes . . . N(4) S(4) C(36) 106.5(3) yes . . . N(1) Si(1) N(2) 87.1(2) yes . . . N(1) Si(1) C(1) 114.1(3) yes . . . N(1) Si(1) C(2) 114.8(3) yes . . . N(2) Si(1) C(1) 113.4(3) yes . . . N(2) Si(1) C(2) 115.4(3) yes . . . C(1) Si(1) C(2) 110.4(3) yes . . . N(3) Si(2) N(4) 86.1(2) yes . . . N(3) Si(2) C(27) 114.6(3) yes . . . N(3) Si(2) C(28) 113.6(3) yes . . . N(4) Si(2) C(27) 114.3(3) yes . . . N(4) Si(2) C(28) 114.9(3) yes . . . C(27) Si(2) C(28) 111.3(3) yes . . . Ir(1) N(1) S(1) 134.6(3) yes . . . Ir(1) N(1) Si(1) 100.6(3) yes . . . S(1) N(1) Si(1) 124.3(3) yes . . . Ir(1) N(2) S(2) 135.3(3) yes . . . Ir(1) N(2) Si(1) 100.1(2) yes . . . S(2) N(2) Si(1) 124.5(3) yes . . . Ir(2) N(3) S(3) 133.9(3) yes . . . Ir(2) N(3) Si(2) 101.1(3) yes . . . S(3) N(3) Si(2) 124.8(3) yes . . . Ir(2) N(4) S(4) 136.5(3) yes . . . Ir(2) N(4) Si(2) 100.8(2) yes . . . S(4) N(4) Si(2) 122.7(3) yes . . . S(1) C(3) C(4) 121.4(6) yes . . . S(1) C(3) C(8) 118.8(6) yes . . . C(4) C(3) C(8) 119.8(6) yes . . . C(3) C(4) C(5) 118.3(7) yes . . . C(4) C(5) C(6) 122.5(8) yes . . . C(5) C(6) C(7) 117.4(7) yes . . . C(5) C(6) C(9) 121.2(8) yes . . . C(7) C(6) C(9) 121.4(8) yes . . . C(6) C(7) C(8) 121.3(8) yes . . . C(3) C(8) C(7) 120.7(8) yes . . . S(2) C(10) C(11) 120.5(6) yes . . . S(2) C(10) C(15) 118.5(6) yes . . . C(11) C(10) C(15) 120.9(7) yes . . . C(10) C(11) C(12) 119.4(8) yes . . . C(11) C(12) C(13) 120.9(8) yes . . . C(12) C(13) C(14) 118.3(8) yes . . . C(12) C(13) C(16) 120.6(9) yes . . . C(14) C(13) C(16) 121.2(9) yes . . . C(13) C(14) C(15) 121.5(9) yes . . . C(10) C(15) C(14) 119.0(8) yes . . . Ir(1) C(17) C(18) 73.0(4) yes . . . Ir(1) C(17) C(21) 71.7(4) yes . . . Ir(1) C(17) C(22) 123.3(5) yes . . . C(18) C(17) C(21) 108.9(6) yes . . . C(18) C(17) C(22) 125.9(8) yes . . . C(21) C(17) C(22) 125.2(7) yes . . . Ir(1) C(18) C(17) 68.7(4) yes . . . Ir(1) C(18) C(19) 68.8(4) yes . . . Ir(1) C(18) C(23) 130.3(5) yes . . . C(17) C(18) C(19) 106.9(7) yes . . . C(17) C(18) C(23) 126.3(7) yes . . . C(19) C(18) C(23) 126.7(6) yes . . . Ir(1) C(19) C(18) 72.5(3) yes . . . Ir(1) C(19) C(20) 71.9(4) yes . . . Ir(1) C(19) C(24) 124.6(4) yes . . . C(18) C(19) C(20) 108.7(6) yes . . . C(18) C(19) C(24) 125.3(7) yes . . . C(20) C(19) C(24) 125.9(7) yes . . . Ir(1) C(20) C(19) 69.3(4) yes . . . Ir(1) C(20) C(21) 70.8(4) yes . . . Ir(1) C(20) C(25) 128.0(5) yes . . . C(19) C(20) C(21) 108.0(7) yes . . . C(19) C(20) C(25) 126.0(6) yes . . . C(21) C(20) C(25) 125.8(7) yes . . . Ir(1) C(21) C(17) 68.9(4) yes . . . Ir(1) C(21) C(20) 71.0(4) yes . . . Ir(1) C(21) C(26) 127.3(5) yes . . . C(17) C(21) C(20) 107.2(6) yes . . . C(17) C(21) C(26) 125.9(7) yes . . . C(20) C(21) C(26) 126.9(8) yes . . . S(3) C(29) C(30) 122.6(6) yes . . . S(3) C(29) C(34) 118.4(6) yes . . . C(30) C(29) C(34) 119.0(7) yes . . . C(29) C(30) C(31) 120.8(8) yes . . . C(30) C(31) C(32) 120.6(8) yes . . . C(31) C(32) C(33) 118.1(8) yes . . . C(31) C(32) C(35) 120.8(9) yes . . . C(33) C(32) C(35) 121.0(9) yes . . . C(32) C(33) C(34) 121.1(9) yes . . . C(29) C(34) C(33) 120.4(9) yes . . . S(4) C(36) C(37) 121.9(5) yes . . . S(4) C(36) C(41) 118.8(5) yes . . . C(37) C(36) C(41) 119.4(6) yes . . . C(36) C(37) C(38) 120.9(7) yes . . . C(37) C(38) C(39) 120.7(7) yes . . . C(38) C(39) C(40) 118.2(7) yes . . . C(38) C(39) C(42) 121.3(8) yes . . . C(40) C(39) C(42) 120.4(8) yes . . . C(39) C(40) C(41) 121.0(9) yes . . . C(36) C(41) C(40) 119.8(8) yes . . . Ir(2) C(43) C(44) 72.0(4) yes . . . Ir(2) C(43) C(47) 70.8(4) yes . . . Ir(2) C(43) C(48) 124.4(5) yes . . . C(44) C(43) C(47) 109.4(6) yes . . . C(44) C(43) C(48) 124.4(8) yes . . . C(47) C(43) C(48) 126.2(7) yes . . . Ir(2) C(44) C(43) 69.3(4) yes . . . Ir(2) C(44) C(45) 68.6(4) yes . . . Ir(2) C(44) C(49) 129.8(5) yes . . . C(43) C(44) C(45) 106.3(7) yes . . . C(43) C(44) C(49) 126.3(7) yes . . . C(45) C(44) C(49) 127.2(7) yes . . . Ir(2) C(45) C(44) 72.7(4) yes . . . Ir(2) C(45) C(46) 72.5(3) yes . . . Ir(2) C(45) C(50) 123.2(4) yes . . . C(44) C(45) C(46) 109.2(6) yes . . . C(44) C(45) C(50) 125.7(7) yes . . . C(46) C(45) C(50) 125.0(7) yes . . . Ir(2) C(46) C(45) 68.1(4) yes . . . Ir(2) C(46) C(47) 69.1(4) yes . . . Ir(2) C(46) C(51) 128.8(5) yes . . . C(45) C(46) C(47) 105.8(7) yes . . . C(45) C(46) C(51) 126.3(7) yes . . . C(47) C(46) C(51) 127.9(7) yes . . . Ir(2) C(47) C(43) 71.0(4) yes . . . Ir(2) C(47) C(46) 72.2(4) yes . . . Ir(2) C(47) C(52) 128.7(5) yes . . . C(43) C(47) C(46) 109.1(6) yes . . . C(43) C(47) C(52) 126.1(7) yes . . . C(46) C(47) C(52) 124.4(8) yes . . . Si(1) C(1) H(1) 109.3 no . . . Si(1) C(1) H(2) 109.5 no . . . Si(1) C(1) H(3) 109.6 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . Si(1) C(2) H(4) 109.5 no . . . Si(1) C(2) H(5) 109.4 no . . . Si(1) C(2) H(6) 109.5 no . . . H(4) C(2) H(5) 109.5 no . . . H(4) C(2) H(6) 109.5 no . . . H(5) C(2) H(6) 109.5 no . . . C(3) C(4) H(7) 120.6 no . . . C(5) C(4) H(7) 121.0 no . . . C(4) C(5) H(8) 118.7 no . . . C(6) C(5) H(8) 118.9 no . . . C(6) C(7) H(9) 119.5 no . . . C(8) C(7) H(9) 119.3 no . . . C(3) C(8) H(10) 119.5 no . . . C(7) C(8) H(10) 119.8 no . . . C(6) C(9) H(11) 109.7 no . . . C(6) C(9) H(12) 109.5 no . . . C(6) C(9) H(13) 109.3 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . C(10) C(11) H(14) 120.2 no . . . C(12) C(11) H(14) 120.4 no . . . C(11) C(12) H(15) 119.7 no . . . C(13) C(12) H(15) 119.4 no . . . C(13) C(14) H(16) 119.2 no . . . C(15) C(14) H(16) 119.3 no . . . C(10) C(15) H(17) 120.5 no . . . C(14) C(15) H(17) 120.6 no . . . C(13) C(16) H(18) 109.2 no . . . C(13) C(16) H(19) 109.6 no . . . C(13) C(16) H(20) 109.5 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(17) C(22) H(21) 109.3 no . . . C(17) C(22) H(22) 109.7 no . . . C(17) C(22) H(23) 109.4 no . . . H(21) C(22) H(22) 109.5 no . . . H(21) C(22) H(23) 109.5 no . . . H(22) C(22) H(23) 109.5 no . . . C(18) C(23) H(24) 109.4 no . . . C(18) C(23) H(25) 109.4 no . . . C(18) C(23) H(26) 109.6 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . C(19) C(24) H(27) 109.5 no . . . C(19) C(24) H(28) 109.6 no . . . C(19) C(24) H(29) 109.3 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . C(20) C(25) H(30) 109.7 no . . . C(20) C(25) H(31) 109.2 no . . . C(20) C(25) H(32) 109.5 no . . . H(30) C(25) H(31) 109.5 no . . . H(30) C(25) H(32) 109.5 no . . . H(31) C(25) H(32) 109.5 no . . . C(21) C(26) H(33) 109.1 no . . . C(21) C(26) H(34) 109.6 no . . . C(21) C(26) H(35) 109.7 no . . . H(33) C(26) H(34) 109.5 no . . . H(33) C(26) H(35) 109.5 no . . . H(34) C(26) H(35) 109.5 no . . . Si(2) C(27) H(36) 109.5 no . . . Si(2) C(27) H(37) 109.4 no . . . Si(2) C(27) H(38) 109.5 no . . . H(36) C(27) H(37) 109.5 no . . . H(36) C(27) H(38) 109.5 no . . . H(37) C(27) H(38) 109.5 no . . . Si(2) C(28) H(39) 109.5 no . . . Si(2) C(28) H(40) 109.5 no . . . Si(2) C(28) H(41) 109.4 no . . . H(39) C(28) H(40) 109.5 no . . . H(39) C(28) H(41) 109.5 no . . . H(40) C(28) H(41) 109.5 no . . . C(29) C(30) H(42) 119.6 no . . . C(31) C(30) H(42) 119.6 no . . . C(30) C(31) H(43) 119.7 no . . . C(32) C(31) H(43) 119.8 no . . . C(32) C(33) H(44) 119.4 no . . . C(34) C(33) H(44) 119.5 no . . . C(29) C(34) H(45) 119.9 no . . . C(33) C(34) H(45) 119.8 no . . . C(32) C(35) H(46) 109.4 no . . . C(32) C(35) H(47) 109.6 no . . . C(32) C(35) H(48) 109.4 no . . . H(46) C(35) H(47) 109.5 no . . . H(46) C(35) H(48) 109.5 no . . . H(47) C(35) H(48) 109.5 no . . . C(36) C(37) H(49) 119.5 no . . . C(38) C(37) H(49) 119.6 no . . . C(37) C(38) H(50) 119.6 no . . . C(39) C(38) H(50) 119.7 no . . . C(39) C(40) H(51) 119.5 no . . . C(41) C(40) H(51) 119.4 no . . . C(36) C(41) H(52) 120.2 no . . . C(40) C(41) H(52) 120.0 no . . . C(39) C(42) H(53) 109.5 no . . . C(39) C(42) H(54) 109.4 no . . . C(39) C(42) H(55) 109.5 no . . . H(53) C(42) H(54) 109.5 no . . . H(53) C(42) H(55) 109.5 no . . . H(54) C(42) H(55) 109.5 no . . . C(43) C(48) H(56) 108.5 no . . . C(43) C(48) H(57) 110.0 no . . . C(43) C(48) H(58) 110.0 no . . . H(56) C(48) H(57) 109.5 no . . . H(56) C(48) H(58) 109.5 no . . . H(57) C(48) H(58) 109.5 no . . . C(44) C(49) H(59) 109.3 no . . . C(44) C(49) H(60) 109.7 no . . . C(44) C(49) H(61) 109.4 no . . . H(59) C(49) H(60) 109.5 no . . . H(59) C(49) H(61) 109.5 no . . . H(60) C(49) H(61) 109.5 no . . . C(45) C(50) H(62) 109.4 no . . . C(45) C(50) H(63) 109.5 no . . . C(45) C(50) H(64) 109.5 no . . . H(62) C(50) H(63) 109.5 no . . . H(62) C(50) H(64) 109.5 no . . . H(63) C(50) H(64) 109.5 no . . . C(46) C(51) H(65) 109.3 no . . . C(46) C(51) H(66) 109.7 no . . . C(46) C(51) H(67) 109.5 no . . . H(65) C(51) H(66) 109.5 no . . . H(65) C(51) H(67) 109.5 no . . . H(66) C(51) H(67) 109.5 no . . . C(47) C(52) H(68) 108.8 no . . . C(47) C(52) H(69) 109.8 no . . . C(47) C(52) H(70) 109.8 no . . . H(68) C(52) H(69) 109.5 no . . . H(68) C(52) H(70) 109.5 no . . . H(69) C(52) H(70) 109.5 no . . . #===END data___3a _database_code_depnum_ccdc_archive 'CCDC 647949' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C44 H50 Ir N2 O4 P S2 Si ' _chemical_formula_moiety 'C44 H50 Ir N2 O4 P S2 Si ' _chemical_formula_weight 986.29 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 10.474(4) _cell_length_b 19.550(7) _cell_length_c 20.356(7) _cell_angle_alpha 90.0000 _cell_angle_beta 91.550(5) _cell_angle_gamma 90.0000 _cell_volume 4167(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15244 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992.00 _exptl_absorpt_coefficient_mu 3.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_correction_T_max 0.504 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 37870 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_max 31.37 _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9543 _reflns_number_gt 6614 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1191 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9542 _refine_ls_number_parameters 546 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0004Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.60 _refine_diff_density_min -2.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.33961(2) 0.473420(10) 0.257260(10) 0.02866(6) Uani 1.00 1 d . . . S(1) S 0.47269(16) 0.30975(9) 0.26409(10) 0.0416(5) Uani 1.00 1 d . . . S(2) S 0.07389(16) 0.47698(10) 0.34597(8) 0.0357(4) Uani 1.00 1 d . . . P(1) P 0.21615(15) 0.45059(9) 0.16365(8) 0.0275(4) Uani 1.00 1 d . . . Si(1) Si 0.2700(2) 0.36354(12) 0.34471(11) 0.0432(6) Uani 1.00 1 d . . . O(1) O 0.5763(4) 0.3387(2) 0.2274(3) 0.0599(18) Uani 1.00 1 d . . . O(2) O 0.5055(5) 0.2749(2) 0.3251(2) 0.0580(17) Uani 1.00 1 d . . . O(3) O 0.1130(5) 0.5219(3) 0.3994(2) 0.0530(16) Uani 1.00 1 d . . . O(4) O 0.0011(4) 0.5107(2) 0.2938(2) 0.0468(16) Uani 1.00 1 d . . . N(1) N 0.3653(4) 0.3647(2) 0.2770(2) 0.0330(15) Uani 1.00 1 d . . . N(2) N 0.1873(5) 0.4351(2) 0.3167(2) 0.0348(16) Uani 1.00 1 d . . . C(1) C 0.3595(9) 0.3766(5) 0.4247(4) 0.075(3) Uani 1.00 1 d . . . C(2) C 0.1711(7) 0.2856(4) 0.3549(4) 0.063(2) Uani 1.00 1 d . . . C(3) C 0.4033(5) 0.2455(3) 0.2130(3) 0.0362(19) Uani 1.00 1 d . . . C(4) C 0.4205(6) 0.2465(4) 0.1465(4) 0.049(2) Uani 1.00 1 d . . . C(5) C 0.3529(7) 0.2013(4) 0.1048(4) 0.055(2) Uani 1.00 1 d . . . C(6) C 0.2675(6) 0.1529(3) 0.1318(4) 0.045(2) Uani 1.00 1 d . . . C(7) C 0.2580(6) 0.1497(3) 0.1988(3) 0.043(2) Uani 1.00 1 d . . . C(8) C 0.3251(6) 0.1954(3) 0.2395(3) 0.043(2) Uani 1.00 1 d . . . C(9) C 0.1876(8) 0.1082(4) 0.0860(4) 0.070(3) Uani 1.00 1 d . . . C(10) C -0.0273(5) 0.4149(3) 0.3807(3) 0.0296(17) Uani 1.00 1 d . . . C(11) C -0.0412(6) 0.4129(4) 0.4477(3) 0.041(2) Uani 1.00 1 d . . . C(12) C -0.1261(6) 0.3671(4) 0.4737(3) 0.043(2) Uani 1.00 1 d . . . C(13) C -0.1969(6) 0.3222(4) 0.4350(3) 0.042(2) Uani 1.00 1 d . . . C(14) C -0.1808(6) 0.3255(3) 0.3675(3) 0.039(2) Uani 1.00 1 d . . . C(15) C -0.0993(6) 0.3712(4) 0.3412(3) 0.038(2) Uani 1.00 1 d . . . C(16) C -0.2927(7) 0.2732(4) 0.4647(4) 0.062(2) Uani 1.00 1 d . . . C(17) C 0.4284(6) 0.5453(3) 0.3338(3) 0.041(2) Uani 1.00 1 d . . . C(18) C 0.3585(6) 0.5819(3) 0.2784(3) 0.039(2) Uani 1.00 1 d . . . C(19) C 0.4267(6) 0.5692(3) 0.2223(4) 0.044(2) Uani 1.00 1 d . . . C(20) C 0.5251(6) 0.5216(4) 0.2358(4) 0.046(2) Uani 1.00 1 d . . . C(21) C 0.5259(6) 0.5080(4) 0.3047(4) 0.051(2) Uani 1.00 1 d . . . C(22) C 0.4064(8) 0.5552(5) 0.4057(4) 0.066(3) Uani 1.00 1 d . . . C(23) C 0.2635(7) 0.6368(3) 0.2944(4) 0.053(2) Uani 1.00 1 d . . . C(24) C 0.4054(8) 0.6076(4) 0.1599(4) 0.063(2) Uani 1.00 1 d . . . C(25) C 0.6352(7) 0.5031(5) 0.1920(5) 0.086(3) Uani 1.00 1 d . . . C(26) C 0.6263(8) 0.4652(4) 0.3403(5) 0.085(3) Uani 1.00 1 d . . . C(27) C 0.2989(6) 0.4097(3) 0.0959(3) 0.0374(19) Uani 1.00 1 d . . . C(28) C 0.4297(6) 0.4136(4) 0.0926(3) 0.046(2) Uani 1.00 1 d . . . C(29) C 0.4919(8) 0.3857(5) 0.0393(4) 0.066(3) Uani 1.00 1 d . . . C(30) C 0.4248(9) 0.3537(5) -0.0096(4) 0.068(3) Uani 1.00 1 d . . . C(31) C 0.2938(9) 0.3489(5) -0.0070(4) 0.069(3) Uani 1.00 1 d . . . C(32) C 0.2314(7) 0.3768(4) 0.0457(3) 0.054(2) Uani 1.00 1 d . . . C(33) C 0.1480(6) 0.5271(3) 0.1240(3) 0.0343(18) Uani 1.00 1 d . . . C(34) C 0.0788(6) 0.5720(3) 0.1609(3) 0.040(2) Uani 1.00 1 d . . . C(35) C 0.0276(7) 0.6315(4) 0.1340(4) 0.051(2) Uani 1.00 1 d . . . C(36) C 0.0469(7) 0.6472(4) 0.0693(4) 0.053(2) Uani 1.00 1 d . . . C(37) C 0.1150(8) 0.6035(4) 0.0314(4) 0.057(2) Uani 1.00 1 d . . . C(38) C 0.1649(7) 0.5428(4) 0.0576(3) 0.046(2) Uani 1.00 1 d . . . C(39) C 0.0768(5) 0.3932(3) 0.1690(3) 0.0294(17) Uani 1.00 1 d . . . C(40) C 0.0992(5) 0.3254(3) 0.1814(3) 0.043(2) Uani 1.00 1 d . . . C(41) C 0.0004(6) 0.2782(3) 0.1795(4) 0.050(2) Uani 1.00 1 d . . . C(42) C -0.1234(6) 0.3006(4) 0.1645(3) 0.043(2) Uani 1.00 1 d . . . C(43) C -0.1462(5) 0.3677(4) 0.1539(3) 0.040(2) Uani 1.00 1 d . . . C(44) C -0.0477(5) 0.4149(3) 0.1554(3) 0.0312(17) Uani 1.00 1 d . . . H(1) H 0.3860 0.3335 0.4419 0.089 Uiso 1.00 1 c R . . H(2) H 0.3057 0.3985 0.4550 0.089 Uiso 1.00 1 c R . . H(3) H 0.4324 0.4043 0.4177 0.089 Uiso 1.00 1 c R . . H(4) H 0.1518 0.2663 0.3130 0.076 Uiso 1.00 1 c R . . H(5) H 0.0941 0.2976 0.3756 0.076 Uiso 1.00 1 c R . . H(6) H 0.2167 0.2532 0.3812 0.076 Uiso 1.00 1 c R . . H(7) H 0.4789 0.2780 0.1284 0.059 Uiso 1.00 1 c R . . H(8) H 0.3640 0.2030 0.0586 0.066 Uiso 1.00 1 c R . . H(9) H 0.2051 0.1160 0.2178 0.052 Uiso 1.00 1 c R . . H(10) H 0.3175 0.1924 0.2858 0.051 Uiso 1.00 1 c R . . H(11) H 0.2420 0.0781 0.0630 0.084 Uiso 1.00 1 c R . . H(12) H 0.1414 0.1361 0.0554 0.084 Uiso 1.00 1 c R . . H(13) H 0.1293 0.0822 0.1108 0.084 Uiso 1.00 1 c R . . H(14) H 0.0071 0.4428 0.4756 0.050 Uiso 1.00 1 c R . . H(15) H -0.1362 0.3663 0.5200 0.051 Uiso 1.00 1 c R . . H(16) H -0.2276 0.2952 0.3394 0.047 Uiso 1.00 1 c R . . H(17) H -0.0916 0.3733 0.2949 0.046 Uiso 1.00 1 c R . . H(18) H -0.2512 0.2314 0.4759 0.075 Uiso 1.00 1 c R . . H(19) H -0.3602 0.2646 0.4337 0.075 Uiso 1.00 1 c R . . H(20) H -0.3264 0.2931 0.5031 0.075 Uiso 1.00 1 c R . . H(21) H 0.3802 0.5132 0.4244 0.079 Uiso 1.00 1 c R . . H(22) H 0.4833 0.5701 0.4269 0.079 Uiso 1.00 1 c R . . H(23) H 0.3418 0.5886 0.4111 0.079 Uiso 1.00 1 c R . . H(24) H 0.3060 0.6796 0.2968 0.063 Uiso 1.00 1 c R . . H(25) H 0.1986 0.6384 0.2609 0.063 Uiso 1.00 1 c R . . H(26) H 0.2262 0.6271 0.3354 0.063 Uiso 1.00 1 c R . . H(27) H 0.4196 0.6550 0.1676 0.076 Uiso 1.00 1 c R . . H(28) H 0.4628 0.5916 0.1280 0.076 Uiso 1.00 1 c R . . H(29) H 0.3200 0.6008 0.1443 0.076 Uiso 1.00 1 c R . . H(30) H 0.7057 0.5323 0.2017 0.105 Uiso 1.00 1 c R . . H(31) H 0.6594 0.4569 0.1999 0.105 Uiso 1.00 1 c R . . H(32) H 0.6093 0.5084 0.1472 0.105 Uiso 1.00 1 c R . . H(33) H 0.5961 0.4197 0.3449 0.102 Uiso 1.00 1 c R . . H(34) H 0.7023 0.4650 0.3159 0.102 Uiso 1.00 1 c R . . H(35) H 0.6437 0.4842 0.3826 0.102 Uiso 1.00 1 c R . . H(36) H 0.4778 0.4354 0.1268 0.056 Uiso 1.00 1 c R . . H(37) H 0.5823 0.3889 0.0373 0.080 Uiso 1.00 1 c R . . H(38) H 0.4681 0.3348 -0.0458 0.082 Uiso 1.00 1 c R . . H(39) H 0.2466 0.3264 -0.0412 0.083 Uiso 1.00 1 c R . . H(40) H 0.1411 0.3735 0.0475 0.065 Uiso 1.00 1 c R . . H(41) H 0.0657 0.5621 0.2059 0.048 Uiso 1.00 1 c R . . H(42) H -0.0209 0.6614 0.1604 0.061 Uiso 1.00 1 c R . . H(43) H 0.0129 0.6882 0.0509 0.063 Uiso 1.00 1 c R . . H(44) H 0.1289 0.6147 -0.0133 0.068 Uiso 1.00 1 c R . . H(45) H 0.2100 0.5121 0.0305 0.055 Uiso 1.00 1 c R . . H(46) H 0.1837 0.3105 0.1915 0.051 Uiso 1.00 1 c R . . H(47) H 0.0169 0.2312 0.1880 0.060 Uiso 1.00 1 c R . . H(48) H -0.1918 0.2687 0.1620 0.052 Uiso 1.00 1 c R . . H(49) H -0.2312 0.3828 0.1453 0.048 Uiso 1.00 1 c R . . H(50) H -0.0649 0.4618 0.1471 0.037 Uiso 1.00 1 c R . . 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) 0.02175(12) 0.01967(13) 0.04461(17) 0.00245(11) 0.00156(9) -0.00466(13) S(1) 0.0251(8) 0.0258(9) 0.0735(13) 0.0062(7) -0.0066(8) -0.0083(9) S(2) 0.0382(8) 0.0323(9) 0.0371(9) 0.0066(8) 0.0093(7) 0.0006(8) P(1) 0.0220(7) 0.0229(8) 0.0378(9) 0.0019(6) 0.0054(6) -0.0023(7) Si(1) 0.0411(11) 0.0382(12) 0.0505(13) 0.0051(9) 0.0049(9) 0.0103(10) O(1) 0.023(2) 0.041(3) 0.116(4) -0.006(2) 0.014(2) -0.024(3) O(2) 0.057(3) 0.033(3) 0.082(4) 0.017(2) -0.030(2) -0.000(2) O(3) 0.059(3) 0.051(3) 0.050(3) -0.008(2) 0.019(2) -0.022(2) O(4) 0.052(3) 0.043(3) 0.046(3) 0.020(2) 0.016(2) 0.013(2) N(1) 0.027(2) 0.019(2) 0.053(3) 0.002(2) 0.010(2) 0.005(2) N(2) 0.035(2) 0.028(3) 0.042(3) 0.007(2) 0.004(2) 0.004(2) C(1) 0.082(6) 0.087(8) 0.054(5) 0.024(5) -0.010(4) 0.012(5) C(2) 0.055(5) 0.050(5) 0.084(6) 0.010(4) 0.019(4) 0.032(4) C(3) 0.021(3) 0.028(3) 0.060(4) 0.011(2) 0.001(2) -0.006(3) C(4) 0.040(4) 0.036(4) 0.072(5) -0.005(3) 0.010(3) -0.010(4) C(5) 0.069(5) 0.041(5) 0.055(5) -0.003(4) 0.011(4) -0.007(4) C(6) 0.037(3) 0.031(4) 0.065(5) 0.001(3) -0.003(3) -0.010(3) C(7) 0.043(4) 0.025(4) 0.061(5) -0.000(3) -0.006(3) 0.006(3) C(8) 0.043(4) 0.027(4) 0.057(5) 0.002(3) -0.002(3) -0.001(3) C(9) 0.072(6) 0.056(6) 0.082(6) -0.018(5) -0.006(5) -0.004(5) C(10) 0.029(3) 0.029(3) 0.032(3) 0.002(2) 0.007(2) 0.000(3) C(11) 0.041(3) 0.039(4) 0.044(4) -0.005(3) 0.000(3) -0.003(3) C(12) 0.043(4) 0.059(5) 0.026(3) -0.001(3) 0.004(3) 0.001(3) C(13) 0.028(3) 0.039(4) 0.058(5) 0.003(3) 0.005(3) 0.003(3) C(14) 0.031(3) 0.042(4) 0.044(4) -0.001(3) -0.008(3) -0.002(3) C(15) 0.036(3) 0.050(4) 0.029(3) 0.004(3) -0.003(2) -0.003(3) C(16) 0.047(4) 0.062(6) 0.079(6) -0.009(4) 0.014(4) 0.010(5) C(17) 0.037(3) 0.035(4) 0.051(4) -0.007(3) -0.006(3) -0.021(3) C(18) 0.037(3) 0.004(2) 0.076(5) -0.006(2) 0.009(3) 0.007(3) C(19) 0.037(3) 0.023(3) 0.074(5) -0.017(3) 0.007(3) -0.008(3) C(20) 0.027(3) 0.032(4) 0.079(5) -0.012(3) 0.009(3) -0.017(4) C(21) 0.026(3) 0.037(4) 0.089(6) -0.006(3) -0.010(3) -0.010(4) C(22) 0.057(5) 0.073(7) 0.066(5) -0.008(4) -0.012(4) -0.009(5) C(23) 0.047(4) 0.029(4) 0.082(6) 0.010(3) 0.002(4) -0.023(4) C(24) 0.082(6) 0.044(5) 0.064(5) -0.029(4) 0.014(4) 0.000(4) C(25) 0.042(4) 0.075(7) 0.144(9) -0.027(4) 0.048(5) -0.053(6) C(26) 0.048(5) 0.053(6) 0.153(10) 0.013(4) -0.028(5) -0.020(6) C(27) 0.036(3) 0.029(4) 0.047(4) -0.001(3) 0.011(3) -0.008(3) C(28) 0.040(3) 0.046(4) 0.053(4) -0.005(3) 0.017(3) -0.011(3) C(29) 0.049(5) 0.070(7) 0.080(6) -0.005(4) 0.032(4) -0.014(5) C(30) 0.074(6) 0.061(6) 0.071(6) 0.013(5) 0.041(5) -0.003(5) C(31) 0.077(6) 0.080(7) 0.051(5) -0.002(5) 0.016(4) -0.035(5) C(32) 0.038(4) 0.069(6) 0.054(5) -0.005(4) 0.012(3) -0.022(4) C(33) 0.034(3) 0.024(3) 0.045(4) 0.002(3) 0.001(2) -0.005(3) C(34) 0.039(3) 0.036(4) 0.046(4) 0.003(3) 0.015(3) -0.001(3) C(35) 0.053(4) 0.042(5) 0.059(5) 0.017(3) 0.003(3) 0.011(4) C(36) 0.052(4) 0.040(5) 0.066(5) 0.008(3) -0.007(4) 0.015(4) C(37) 0.071(5) 0.057(6) 0.042(4) 0.002(4) 0.001(4) 0.019(4) C(38) 0.048(4) 0.049(5) 0.040(4) -0.004(3) 0.007(3) -0.002(3) C(39) 0.028(3) 0.030(3) 0.030(3) -0.004(2) 0.003(2) 0.002(2) C(40) 0.018(3) 0.034(4) 0.076(5) -0.004(2) 0.000(3) 0.012(3) C(41) 0.042(4) 0.021(3) 0.086(6) -0.008(3) -0.001(3) 0.005(3) C(42) 0.022(3) 0.043(4) 0.065(5) -0.014(3) 0.003(3) 0.006(4) C(43) 0.019(3) 0.050(4) 0.050(4) 0.003(3) 0.005(2) -0.003(3) C(44) 0.029(3) 0.027(3) 0.038(3) 0.006(2) 0.003(2) 0.001(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) P(1) 2.3171(16) yes . . Ir(1) N(1) 2.179(5) yes . . Ir(1) N(2) 2.163(5) yes . . Ir(1) C(17) 2.278(7) yes . . Ir(1) C(18) 2.172(6) yes . . Ir(1) C(19) 2.209(7) yes . . Ir(1) C(20) 2.213(6) yes . . Ir(1) C(21) 2.257(7) yes . . S(1) O(1) 1.450(5) yes . . S(1) O(2) 1.449(5) yes . . S(1) N(1) 1.582(5) yes . . S(1) C(3) 1.775(7) yes . . S(2) O(3) 1.448(5) yes . . S(2) O(4) 1.450(5) yes . . S(2) N(2) 1.573(5) yes . . S(2) C(10) 1.772(6) yes . . P(1) C(27) 1.832(7) yes . . P(1) C(33) 1.836(7) yes . . P(1) C(39) 1.846(6) yes . . Si(1) N(1) 1.724(5) yes . . Si(1) N(2) 1.734(5) yes . . Si(1) C(1) 1.874(9) yes . . Si(1) C(2) 1.857(8) yes . . C(3) C(4) 1.370(11) yes . . C(3) C(8) 1.395(10) yes . . C(4) C(5) 1.404(11) yes . . C(5) C(6) 1.422(11) yes . . C(6) C(7) 1.373(11) yes . . C(6) C(9) 1.514(12) yes . . C(7) C(8) 1.395(10) yes . . C(10) C(11) 1.376(9) yes . . C(10) C(15) 1.382(9) yes . . C(11) C(12) 1.379(10) yes . . C(12) C(13) 1.381(10) yes . . C(13) C(14) 1.390(10) yes . . C(13) C(16) 1.524(11) yes . . C(14) C(15) 1.356(10) yes . . C(17) C(18) 1.508(10) yes . . C(17) C(21) 1.399(10) yes . . C(17) C(22) 1.499(11) yes . . C(18) C(19) 1.387(11) yes . . C(18) C(23) 1.505(10) yes . . C(19) C(20) 1.411(10) yes . . C(19) C(24) 1.487(11) yes . . C(20) C(21) 1.429(13) yes . . C(20) C(25) 1.519(12) yes . . C(21) C(26) 1.513(12) yes . . C(27) C(28) 1.375(9) yes . . C(27) C(32) 1.385(10) yes . . C(28) C(29) 1.392(12) yes . . C(29) C(30) 1.356(13) yes . . C(30) C(31) 1.377(13) yes . . C(31) C(32) 1.385(12) yes . . C(33) C(34) 1.375(10) yes . . C(33) C(38) 1.400(10) yes . . C(34) C(35) 1.387(11) yes . . C(35) C(36) 1.374(12) yes . . C(36) C(37) 1.364(12) yes . . C(37) C(38) 1.398(11) yes . . C(39) C(40) 1.369(10) yes . . C(39) C(44) 1.392(8) yes . . C(40) C(41) 1.385(9) yes . . C(41) C(42) 1.395(9) yes . . C(42) C(43) 1.350(11) yes . . C(43) C(44) 1.383(9) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(2) H(5) 0.950 no . . C(2) H(6) 0.950 no . . C(4) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(7) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(11) H(14) 0.950 no . . C(12) H(15) 0.950 no . . C(14) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(22) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(25) H(30) 0.950 no . . C(25) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(26) H(33) 0.950 no . . C(26) H(34) 0.950 no . . C(26) H(35) 0.950 no . . C(28) H(36) 0.950 no . . C(29) H(37) 0.950 no . . C(30) H(38) 0.950 no . . C(31) H(39) 0.950 no . . C(32) H(40) 0.950 no . . C(34) H(41) 0.950 no . . C(35) H(42) 0.950 no . . C(36) H(43) 0.950 no . . C(37) H(44) 0.950 no . . C(38) H(45) 0.950 no . . C(40) H(46) 0.950 no . . C(41) H(47) 0.950 no . . C(42) H(48) 0.950 no . . C(43) H(49) 0.950 no . . C(44) H(50) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 P(1) Ir(1) N(1) 91.55(14) yes . . . P(1) Ir(1) N(2) 89.41(14) yes . . . P(1) Ir(1) C(17) 152.85(18) yes . . . P(1) Ir(1) C(18) 113.41(19) yes . . . P(1) Ir(1) C(19) 97.1(2) yes . . . P(1) Ir(1) C(20) 113.1(2) yes . . . P(1) Ir(1) C(21) 150.0(2) yes . . . N(1) Ir(1) N(2) 69.4(2) yes . . . N(1) Ir(1) C(17) 115.4(2) yes . . . N(1) Ir(1) C(18) 154.9(2) yes . . . N(1) Ir(1) C(19) 146.8(2) yes . . . N(1) Ir(1) C(20) 110.3(2) yes . . . N(1) Ir(1) C(21) 96.4(2) yes . . . N(2) Ir(1) C(17) 97.1(2) yes . . . N(2) Ir(1) C(18) 107.0(2) yes . . . N(2) Ir(1) C(19) 142.3(2) yes . . . N(2) Ir(1) C(20) 157.4(2) yes . . . N(2) Ir(1) C(21) 120.4(2) yes . . . C(17) Ir(1) C(18) 39.5(2) yes . . . C(17) Ir(1) C(19) 62.2(2) yes . . . C(17) Ir(1) C(20) 61.9(2) yes . . . C(17) Ir(1) C(21) 35.9(2) yes . . . C(18) Ir(1) C(19) 36.9(2) yes . . . C(18) Ir(1) C(20) 63.1(2) yes . . . C(18) Ir(1) C(21) 63.2(2) yes . . . C(19) Ir(1) C(20) 37.2(2) yes . . . C(19) Ir(1) C(21) 61.6(2) yes . . . C(20) Ir(1) C(21) 37.3(3) yes . . . O(1) S(1) O(2) 117.5(3) yes . . . O(1) S(1) N(1) 111.5(3) yes . . . O(1) S(1) C(3) 105.9(3) yes . . . O(2) S(1) N(1) 109.3(3) yes . . . O(2) S(1) C(3) 104.7(3) yes . . . N(1) S(1) C(3) 107.2(2) yes . . . O(3) S(2) O(4) 114.0(3) yes . . . O(3) S(2) N(2) 113.5(3) yes . . . O(3) S(2) C(10) 106.0(3) yes . . . O(4) S(2) N(2) 110.3(3) yes . . . O(4) S(2) C(10) 107.2(2) yes . . . N(2) S(2) C(10) 105.1(3) yes . . . Ir(1) P(1) C(27) 116.0(2) yes . . . Ir(1) P(1) C(33) 114.0(2) yes . . . Ir(1) P(1) C(39) 119.5(2) yes . . . C(27) P(1) C(33) 102.2(3) yes . . . C(27) P(1) C(39) 99.8(3) yes . . . C(33) P(1) C(39) 102.9(2) yes . . . N(1) Si(1) N(2) 91.3(2) yes . . . N(1) Si(1) C(1) 114.0(3) yes . . . N(1) Si(1) C(2) 115.9(3) yes . . . N(2) Si(1) C(1) 114.2(3) yes . . . N(2) Si(1) C(2) 115.0(3) yes . . . C(1) Si(1) C(2) 106.4(4) yes . . . Ir(1) N(1) S(1) 135.8(3) yes . . . Ir(1) N(1) Si(1) 95.1(2) yes . . . S(1) N(1) Si(1) 123.6(3) yes . . . Ir(1) N(2) S(2) 127.4(3) yes . . . Ir(1) N(2) Si(1) 95.4(2) yes . . . S(2) N(2) Si(1) 132.2(3) yes . . . S(1) C(3) C(4) 120.4(5) yes . . . S(1) C(3) C(8) 120.3(5) yes . . . C(4) C(3) C(8) 119.1(6) yes . . . C(3) C(4) C(5) 120.7(7) yes . . . C(4) C(5) C(6) 119.8(7) yes . . . C(5) C(6) C(7) 118.5(7) yes . . . C(5) C(6) C(9) 119.3(7) yes . . . C(7) C(6) C(9) 122.1(7) yes . . . C(6) C(7) C(8) 120.8(6) yes . . . C(3) C(8) C(7) 120.7(7) yes . . . S(2) C(10) C(11) 119.7(5) yes . . . S(2) C(10) C(15) 120.9(5) yes . . . C(11) C(10) C(15) 119.3(6) yes . . . C(10) C(11) C(12) 119.0(6) yes . . . C(11) C(12) C(13) 122.4(6) yes . . . C(12) C(13) C(14) 117.2(6) yes . . . C(12) C(13) C(16) 121.5(7) yes . . . C(14) C(13) C(16) 121.3(6) yes . . . C(13) C(14) C(15) 121.0(6) yes . . . C(10) C(15) C(14) 121.1(6) yes . . . Ir(1) C(17) C(18) 66.4(3) yes . . . Ir(1) C(17) C(21) 71.2(4) yes . . . Ir(1) C(17) C(22) 132.6(5) yes . . . C(18) C(17) C(21) 106.0(6) yes . . . C(18) C(17) C(22) 125.7(6) yes . . . C(21) C(17) C(22) 127.8(7) yes . . . Ir(1) C(18) C(17) 74.0(3) yes . . . Ir(1) C(18) C(19) 73.0(4) yes . . . Ir(1) C(18) C(23) 133.0(4) yes . . . C(17) C(18) C(19) 106.3(5) yes . . . C(17) C(18) C(23) 119.2(6) yes . . . C(19) C(18) C(23) 131.5(6) yes . . . Ir(1) C(19) C(18) 70.1(4) yes . . . Ir(1) C(19) C(20) 71.6(4) yes . . . Ir(1) C(19) C(24) 130.5(5) yes . . . C(18) C(19) C(20) 110.3(7) yes . . . C(18) C(19) C(24) 123.0(6) yes . . . C(20) C(19) C(24) 126.3(7) yes . . . Ir(1) C(20) C(19) 71.2(3) yes . . . Ir(1) C(20) C(21) 73.0(4) yes . . . Ir(1) C(20) C(25) 134.4(5) yes . . . C(19) C(20) C(21) 107.4(6) yes . . . C(19) C(20) C(25) 127.2(8) yes . . . C(21) C(20) C(25) 123.2(6) yes . . . Ir(1) C(21) C(17) 72.8(4) yes . . . Ir(1) C(21) C(20) 69.7(4) yes . . . Ir(1) C(21) C(26) 128.4(5) yes . . . C(17) C(21) C(20) 109.5(6) yes . . . C(17) C(21) C(26) 126.3(8) yes . . . C(20) C(21) C(26) 123.9(7) yes . . . P(1) C(27) C(28) 120.3(5) yes . . . P(1) C(27) C(32) 121.0(5) yes . . . C(28) C(27) C(32) 118.6(6) yes . . . C(27) C(28) C(29) 120.3(7) yes . . . C(28) C(29) C(30) 120.6(8) yes . . . C(29) C(30) C(31) 120.0(8) yes . . . C(30) C(31) C(32) 119.6(8) yes . . . C(27) C(32) C(31) 120.9(7) yes . . . P(1) C(33) C(34) 119.0(5) yes . . . P(1) C(33) C(38) 123.0(5) yes . . . C(34) C(33) C(38) 118.0(6) yes . . . C(33) C(34) C(35) 121.6(6) yes . . . C(34) C(35) C(36) 120.0(7) yes . . . C(35) C(36) C(37) 119.7(7) yes . . . C(36) C(37) C(38) 120.8(7) yes . . . C(33) C(38) C(37) 119.9(7) yes . . . P(1) C(39) C(40) 117.9(4) yes . . . P(1) C(39) C(44) 122.8(5) yes . . . C(40) C(39) C(44) 119.0(5) yes . . . C(39) C(40) C(41) 121.1(6) yes . . . C(40) C(41) C(42) 119.1(6) yes . . . C(41) C(42) C(43) 120.0(6) yes . . . C(42) C(43) C(44) 121.0(6) yes . . . C(39) C(44) C(43) 119.8(6) yes . . . Si(1) C(1) H(1) 109.5 no . . . Si(1) C(1) H(2) 109.5 no . . . Si(1) C(1) H(3) 109.4 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . Si(1) C(2) H(4) 109.4 no . . . Si(1) C(2) H(5) 109.3 no . . . Si(1) C(2) H(6) 109.7 no . . . H(4) C(2) H(5) 109.5 no . . . H(4) C(2) H(6) 109.5 no . . . H(5) C(2) H(6) 109.5 no . . . C(3) C(4) H(7) 119.6 no . . . C(5) C(4) H(7) 119.6 no . . . C(4) C(5) H(8) 120.1 no . . . C(6) C(5) H(8) 120.1 no . . . C(6) C(7) H(9) 119.6 no . . . C(8) C(7) H(9) 119.6 no . . . C(3) C(8) H(10) 119.6 no . . . C(7) C(8) H(10) 119.6 no . . . C(6) C(9) H(11) 109.3 no . . . C(6) C(9) H(12) 109.6 no . . . C(6) C(9) H(13) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . C(10) C(11) H(14) 120.4 no . . . C(12) C(11) H(14) 120.6 no . . . C(11) C(12) H(15) 118.8 no . . . C(13) C(12) H(15) 118.8 no . . . C(13) C(14) H(16) 119.5 no . . . C(15) C(14) H(16) 119.5 no . . . C(10) C(15) H(17) 119.4 no . . . C(14) C(15) H(17) 119.5 no . . . C(13) C(16) H(18) 109.5 no . . . C(13) C(16) H(19) 109.6 no . . . C(13) C(16) H(20) 109.4 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(17) C(22) H(21) 109.6 no . . . C(17) C(22) H(22) 109.5 no . . . C(17) C(22) H(23) 109.4 no . . . H(21) C(22) H(22) 109.5 no . . . H(21) C(22) H(23) 109.5 no . . . H(22) C(22) H(23) 109.5 no . . . C(18) C(23) H(24) 109.2 no . . . C(18) C(23) H(25) 109.5 no . . . C(18) C(23) H(26) 109.7 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . C(19) C(24) H(27) 109.4 no . . . C(19) C(24) H(28) 109.5 no . . . C(19) C(24) H(29) 109.5 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . C(20) C(25) H(30) 109.6 no . . . C(20) C(25) H(31) 109.3 no . . . C(20) C(25) H(32) 109.6 no . . . H(30) C(25) H(31) 109.5 no . . . H(30) C(25) H(32) 109.5 no . . . H(31) C(25) H(32) 109.5 no . . . C(21) C(26) H(33) 109.6 no . . . C(21) C(26) H(34) 109.5 no . . . C(21) C(26) H(35) 109.3 no . . . H(33) C(26) H(34) 109.5 no . . . H(33) C(26) H(35) 109.5 no . . . H(34) C(26) H(35) 109.5 no . . . C(27) C(28) H(36) 119.9 no . . . C(29) C(28) H(36) 119.8 no . . . C(28) C(29) H(37) 119.7 no . . . C(30) C(29) H(37) 119.7 no . . . C(29) C(30) H(38) 120.0 no . . . C(31) C(30) H(38) 120.0 no . . . C(30) C(31) H(39) 120.2 no . . . C(32) C(31) H(39) 120.2 no . . . C(27) C(32) H(40) 119.6 no . . . C(31) C(32) H(40) 119.6 no . . . C(33) C(34) H(41) 119.2 no . . . C(35) C(34) H(41) 119.2 no . . . C(34) C(35) H(42) 120.0 no . . . C(36) C(35) H(42) 120.0 no . . . C(35) C(36) H(43) 120.1 no . . . C(37) C(36) H(43) 120.2 no . . . C(36) C(37) H(44) 119.6 no . . . C(38) C(37) H(44) 119.6 no . . . C(33) C(38) H(45) 120.1 no . . . C(37) C(38) H(45) 120.0 no . . . C(39) C(40) H(46) 119.4 no . . . C(41) C(40) H(46) 119.5 no . . . C(40) C(41) H(47) 120.5 no . . . C(42) C(41) H(47) 120.4 no . . . C(41) C(42) H(48) 120.1 no . . . C(43) C(42) H(48) 120.0 no . . . C(42) C(43) H(49) 119.5 no . . . C(44) C(43) H(49) 119.5 no . . . C(39) C(44) H(50) 120.1 no . . . C(43) C(44) H(50) 120.1 no . . . #===END data___3b _database_code_depnum_ccdc_archive 'CCDC 647950' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C32 H50 Ir N2 O7 P S2 Si ' _chemical_formula_moiety 'C32 H50 Ir N2 O7 P S2 Si ' _chemical_formula_weight 890.16 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.945(3) _cell_length_b 18.337(4) _cell_length_c 17.387(4) _cell_angle_alpha 90.0000 _cell_angle_beta 104.708(3) _cell_angle_gamma 90.0000 _cell_volume 3683.8(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15633 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800.00 _exptl_absorpt_coefficient_mu 3.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.048 _exptl_absorpt_correction_T_max 0.144 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 33325 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_theta_max 31.37 _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8397 _reflns_number_gt 6940 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1053 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8396 _refine_ls_number_parameters 465 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 0.7000\s(Fo^2^) + 0.6000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.22 _refine_diff_density_min -1.59 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.707830(10) 0.145330(10) 0.843120(10) 0.01695(5) Uani 1.00 1 d . . . S(1) S 0.94302(10) 0.07865(7) 0.78243(8) 0.0281(3) Uani 1.00 1 d . . . S(2) S 0.54111(10) 0.23995(6) 0.68178(7) 0.0233(2) Uani 1.00 1 d . . . P(1) P 0.62391(10) 0.03648(6) 0.81601(7) 0.0198(2) Uani 1.00 1 d . . . Si(1) Si 0.76578(12) 0.17600(8) 0.68942(8) 0.0252(3) Uani 1.00 1 d . . . O(1) O 1.0059(3) 0.0737(2) 0.8645(2) 0.0403(10) Uani 1.00 1 d . . . O(2) O 1.0035(3) 0.1083(2) 0.7272(2) 0.0411(11) Uani 1.00 1 d . . . O(3) O 0.5091(3) 0.29136(19) 0.7353(2) 0.0359(10) Uani 1.00 1 d . . . O(4) O 0.5684(3) 0.2702(2) 0.6112(2) 0.0345(9) Uani 1.00 1 d . . . O(5) O 0.6941(2) -0.02295(17) 0.8749(2) 0.0250(8) Uani 1.00 1 d . . . O(6) O 0.6147(3) 0.01161(17) 0.7279(2) 0.0272(8) Uani 1.00 1 d . . . O(7) O 0.4993(2) 0.02168(18) 0.8308(2) 0.0271(8) Uani 1.00 1 d . . . N(1) N 0.8266(3) 0.1221(2) 0.7722(2) 0.0234(9) Uani 1.00 1 d . . . N(2) N 0.6426(3) 0.1888(2) 0.7243(2) 0.0220(9) Uani 1.00 1 d . . . C(1) C 0.8478(5) 0.2611(3) 0.6846(4) 0.0470(18) Uani 1.00 1 d . . . C(2) C 0.7385(5) 0.1292(3) 0.5920(3) 0.0401(15) Uani 1.00 1 d . . . C(3) C 0.9092(4) -0.0141(2) 0.7502(3) 0.0270(12) Uani 1.00 1 d . . . C(4) C 0.8968(5) -0.0325(3) 0.6721(3) 0.0397(15) Uani 1.00 1 d . . . C(5) C 0.8721(5) -0.1035(3) 0.6478(3) 0.0390(15) Uani 1.00 1 d . . . C(6) C 0.8574(4) -0.1577(2) 0.7000(3) 0.0336(14) Uani 1.00 1 d . . . C(7) C 0.8716(4) -0.1381(2) 0.7792(3) 0.0330(14) Uani 1.00 1 d . . . C(8) C 0.8978(4) -0.0662(2) 0.8047(3) 0.0284(12) Uani 1.00 1 d . . . C(9) C 0.8257(5) -0.2345(3) 0.6715(4) 0.0479(18) Uani 1.00 1 d . . . C(10) C 0.4151(4) 0.1865(2) 0.6452(2) 0.0275(12) Uani 1.00 1 d . . . C(11) C 0.3136(4) 0.2026(3) 0.6668(3) 0.0371(15) Uani 1.00 1 d . . . C(12) C 0.2148(5) 0.1608(3) 0.6381(3) 0.0428(16) Uani 1.00 1 d . . . C(13) C 0.2150(4) 0.1029(3) 0.5881(3) 0.0387(15) Uani 1.00 1 d . . . C(14) C 0.3166(5) 0.0878(3) 0.5656(3) 0.0441(16) Uani 1.00 1 d . . . C(15) C 0.4153(4) 0.1289(3) 0.5939(3) 0.0342(14) Uani 1.00 1 d . . . C(16) C 0.1106(5) 0.0545(4) 0.5607(4) 0.065(2) Uani 1.00 1 d . . . C(17) C 0.8345(4) 0.2120(2) 0.9380(2) 0.0271(12) Uani 1.00 1 d . . . C(18) C 0.8015(4) 0.1428(2) 0.9671(3) 0.0268(12) Uani 1.00 1 d . . . C(19) C 0.6800(4) 0.1463(2) 0.9625(3) 0.0256(12) Uani 1.00 1 d . . . C(20) C 0.6345(4) 0.2116(2) 0.9227(2) 0.0252(11) Uani 1.00 1 d . . . C(21) C 0.7329(4) 0.2535(2) 0.9102(2) 0.0260(12) Uani 1.00 1 d . . . C(22) C 0.9532(4) 0.2339(3) 0.9384(3) 0.0436(16) Uani 1.00 1 d . . . C(23) C 0.8849(5) 0.0862(3) 1.0116(3) 0.0416(15) Uani 1.00 1 d . . . C(24) C 0.6148(5) 0.0932(2) 1.0010(3) 0.0355(14) Uani 1.00 1 d . . . C(25) C 0.5145(4) 0.2392(2) 0.9130(3) 0.0318(13) Uani 1.00 1 d . . . C(26) C 0.7254(5) 0.3291(2) 0.8759(3) 0.0358(14) Uani 1.00 1 d . . . C(27) C 0.6505(5) -0.0918(3) 0.8965(4) 0.0448(16) Uani 1.00 1 d . . . C(28) C 0.7344(6) -0.1241(3) 0.9647(4) 0.0529(19) Uani 1.00 1 d . . . C(29) C 0.5671(6) -0.0579(3) 0.6947(3) 0.0439(16) Uani 1.00 1 d . . . C(30) C 0.5557(6) -0.0583(3) 0.6082(3) 0.0508(19) Uani 1.00 1 d . . . C(31) C 0.3967(4) 0.0599(3) 0.7876(3) 0.0432(16) Uani 1.00 1 d . . . C(32) C 0.2952(6) 0.0260(6) 0.8077(6) 0.118(3) Uani 1.00 1 d . . . H(1) H 0.8188 0.2989 0.7115 0.057 Uiso 1.00 1 c R . . H(2) H 0.8393 0.2746 0.6307 0.057 Uiso 1.00 1 c R . . H(3) H 0.9274 0.2533 0.7095 0.057 Uiso 1.00 1 c R . . H(4) H 0.8049 0.1333 0.5717 0.050 Uiso 1.00 1 c R . . H(5) H 0.6740 0.1508 0.5557 0.050 Uiso 1.00 1 c R . . H(6) H 0.7227 0.0792 0.5989 0.050 Uiso 1.00 1 c R . . H(7) H 0.9063 0.0037 0.6353 0.049 Uiso 1.00 1 c R . . H(8) H 0.8622 -0.1157 0.5933 0.047 Uiso 1.00 1 c R . . H(9) H 0.8626 -0.1742 0.8164 0.040 Uiso 1.00 1 c R . . H(10) H 0.9076 -0.0535 0.8590 0.034 Uiso 1.00 1 c R . . H(11) H 0.7439 -0.2397 0.6572 0.059 Uiso 1.00 1 c R . . H(12) H 0.8585 -0.2673 0.7134 0.059 Uiso 1.00 1 c R . . H(13) H 0.8549 -0.2450 0.6267 0.059 Uiso 1.00 1 c R . . H(14) H 0.3117 0.2425 0.7013 0.046 Uiso 1.00 1 c R . . H(15) H 0.1464 0.1719 0.6542 0.052 Uiso 1.00 1 c R . . H(16) H 0.3178 0.0483 0.5303 0.054 Uiso 1.00 1 c R . . H(17) H 0.4837 0.1180 0.5777 0.042 Uiso 1.00 1 c R . . H(18) H 0.1133 0.0150 0.5965 0.078 Uiso 1.00 1 c R . . H(19) H 0.1081 0.0360 0.5092 0.077 Uiso 1.00 1 c R . . H(20) H 0.0434 0.0830 0.5584 0.077 Uiso 1.00 1 c R . . H(21) H 1.0061 0.1975 0.9641 0.050 Uiso 1.00 1 c R . . H(22) H 0.9716 0.2789 0.9657 0.050 Uiso 1.00 1 c R . . H(23) H 0.9584 0.2393 0.8850 0.051 Uiso 1.00 1 c R . . H(24) H 0.8434 0.0502 1.0324 0.047 Uiso 1.00 1 c R . . H(25) H 0.9401 0.1088 1.0540 0.047 Uiso 1.00 1 c R . . H(26) H 0.9236 0.0639 0.9763 0.047 Uiso 1.00 1 c R . . H(27) H 0.5365 0.1086 0.9914 0.045 Uiso 1.00 1 c R . . H(28) H 0.6486 0.0917 1.0567 0.045 Uiso 1.00 1 c R . . H(29) H 0.6176 0.0460 0.9791 0.045 Uiso 1.00 1 c R . . H(30) H 0.5073 0.2857 0.8880 0.039 Uiso 1.00 1 c R . . H(31) H 0.4978 0.2434 0.9634 0.039 Uiso 1.00 1 c R . . H(32) H 0.4617 0.2061 0.8807 0.039 Uiso 1.00 1 c R . . H(33) H 0.7995 0.3438 0.8708 0.043 Uiso 1.00 1 c R . . H(34) H 0.6996 0.3623 0.9097 0.043 Uiso 1.00 1 c R . . H(35) H 0.6722 0.3289 0.8250 0.043 Uiso 1.00 1 c R . . H(36) H 0.5796 -0.0833 0.9104 0.051 Uiso 1.00 1 c R . . H(37) H 0.6376 -0.1247 0.8529 0.051 Uiso 1.00 1 c R . . H(38) H 0.7864 -0.1545 0.9462 0.061 Uiso 1.00 1 c R . . H(39) H 0.6960 -0.1519 0.9964 0.061 Uiso 1.00 1 c R . . H(40) H 0.7763 -0.0855 0.9956 0.061 Uiso 1.00 1 c R . . H(41) H 0.6184 -0.0960 0.7183 0.054 Uiso 1.00 1 c R . . H(42) H 0.4937 -0.0657 0.7052 0.054 Uiso 1.00 1 c R . . H(43) H 0.4811 -0.0404 0.5821 0.063 Uiso 1.00 1 c R . . H(44) H 0.5650 -0.1061 0.5899 0.063 Uiso 1.00 1 c R . . H(45) H 0.6131 -0.0272 0.5968 0.063 Uiso 1.00 1 c R . . H(46) H 0.4003 0.1096 0.8035 0.052 Uiso 1.00 1 c R . . H(47) H 0.3904 0.0571 0.7321 0.052 Uiso 1.00 1 c R . . H(48) H 0.2682 -0.0121 0.7706 0.141 Uiso 1.00 1 c R . . H(49) H 0.2349 0.0604 0.8051 0.140 Uiso 1.00 1 c R . . H(50) H 0.3186 0.0063 0.8598 0.140 Uiso 1.00 1 c R . . 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) 0.01745(11) 0.01562(11) 0.01743(11) -0.00001(6) 0.00377(7) 0.00027(6) S(1) 0.0187(5) 0.0311(6) 0.0348(6) 0.0024(4) 0.0071(4) -0.0009(4) S(2) 0.0252(5) 0.0204(5) 0.0228(5) 0.0015(4) 0.0032(4) 0.0041(4) P(1) 0.0194(5) 0.0190(5) 0.0216(5) -0.0017(4) 0.0063(4) 0.0012(4) Si(1) 0.0247(6) 0.0283(6) 0.0244(6) -0.0034(5) 0.0096(5) 0.0034(5) O(1) 0.0290(19) 0.045(2) 0.041(2) 0.0079(16) -0.0029(16) -0.0078(17) O(2) 0.031(2) 0.042(2) 0.057(2) -0.0030(17) 0.0239(18) -0.0023(18) O(3) 0.042(2) 0.0259(18) 0.035(2) 0.0097(15) 0.0014(16) -0.0021(15) O(4) 0.035(2) 0.038(2) 0.0281(18) -0.0028(15) 0.0038(15) 0.0128(15) O(5) 0.0229(16) 0.0169(15) 0.0353(18) -0.0029(12) 0.0073(14) 0.0057(13) O(6) 0.0336(18) 0.0197(16) 0.0307(18) -0.0099(13) 0.0127(14) -0.0040(13) O(7) 0.0195(16) 0.0329(18) 0.0281(17) -0.0012(13) 0.0045(13) 0.0059(14) N(1) 0.0155(18) 0.0265(19) 0.029(2) 0.0022(15) 0.0062(15) -0.0002(16) N(2) 0.0232(19) 0.024(2) 0.0198(19) 0.0043(15) 0.0066(15) 0.0063(15) C(1) 0.042(3) 0.042(3) 0.059(4) -0.014(2) 0.017(2) 0.014(2) C(2) 0.042(3) 0.055(3) 0.027(2) 0.011(2) 0.017(2) 0.002(2) C(3) 0.020(2) 0.028(2) 0.034(2) 0.0078(18) 0.0084(19) 0.0003(19) C(4) 0.053(3) 0.037(3) 0.032(2) 0.006(2) 0.015(2) 0.003(2) C(5) 0.043(3) 0.041(3) 0.034(3) 0.007(2) 0.011(2) -0.000(2) C(6) 0.026(2) 0.030(2) 0.048(3) 0.008(2) 0.014(2) -0.001(2) C(7) 0.031(2) 0.033(2) 0.036(2) 0.006(2) 0.010(2) 0.007(2) C(8) 0.021(2) 0.034(2) 0.030(2) 0.008(2) 0.0056(18) 0.003(2) C(9) 0.044(3) 0.042(3) 0.062(4) -0.004(2) 0.021(3) -0.009(2) C(10) 0.026(2) 0.033(2) 0.022(2) -0.0005(19) 0.0040(18) 0.0059(19) C(11) 0.034(2) 0.043(3) 0.038(3) 0.003(2) 0.014(2) 0.005(2) C(12) 0.028(2) 0.063(3) 0.040(3) 0.002(2) 0.013(2) 0.004(2) C(13) 0.027(2) 0.058(3) 0.030(2) -0.013(2) 0.005(2) 0.006(2) C(14) 0.040(3) 0.059(3) 0.034(3) -0.011(2) 0.012(2) -0.014(2) C(15) 0.029(2) 0.046(3) 0.031(2) -0.002(2) 0.013(2) -0.005(2) C(16) 0.041(3) 0.105(6) 0.048(3) -0.039(3) 0.011(3) -0.001(3) C(17) 0.029(2) 0.029(2) 0.020(2) -0.0043(19) 0.0005(18) -0.0069(18) C(18) 0.027(2) 0.027(2) 0.023(2) 0.0022(18) -0.0003(19) -0.0017(18) C(19) 0.030(2) 0.027(2) 0.021(2) 0.0006(18) 0.0090(19) -0.0029(17) C(20) 0.034(2) 0.021(2) 0.020(2) 0.0041(19) 0.0064(19) -0.0010(17) C(21) 0.029(2) 0.024(2) 0.024(2) -0.0006(18) 0.0052(19) -0.0079(18) C(22) 0.031(2) 0.047(3) 0.047(3) -0.006(2) 0.000(2) -0.009(2) C(23) 0.045(3) 0.040(3) 0.031(2) 0.014(2) -0.006(2) 0.002(2) C(24) 0.054(3) 0.031(2) 0.027(2) -0.006(2) 0.021(2) -0.000(2) C(25) 0.039(2) 0.026(2) 0.033(2) 0.004(2) 0.013(2) -0.003(2) C(26) 0.045(3) 0.020(2) 0.041(3) -0.009(2) 0.009(2) -0.008(2) C(27) 0.043(3) 0.030(2) 0.055(3) -0.011(2) 0.001(2) 0.019(2) C(28) 0.068(4) 0.036(3) 0.048(3) -0.004(3) 0.004(3) 0.013(2) C(29) 0.069(4) 0.030(2) 0.036(3) -0.024(2) 0.018(2) -0.011(2) C(30) 0.080(4) 0.043(3) 0.034(3) -0.011(3) 0.022(3) -0.013(2) C(31) 0.030(2) 0.053(3) 0.047(3) 0.010(2) 0.010(2) 0.016(2) C(32) 0.021(3) 0.204(11) 0.126(8) 0.011(5) 0.015(4) 0.110(8) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) P(1) 2.2296(11) yes . . Ir(1) N(1) 2.146(4) yes . . Ir(1) N(2) 2.166(3) yes . . Ir(1) C(17) 2.288(4) yes . . Ir(1) C(18) 2.163(4) yes . . Ir(1) C(19) 2.184(5) yes . . Ir(1) C(20) 2.185(5) yes . . Ir(1) C(21) 2.282(4) yes . . S(1) O(1) 1.437(3) yes . . S(1) O(2) 1.447(4) yes . . S(1) N(1) 1.573(4) yes . . S(1) C(3) 1.804(4) yes . . S(2) O(3) 1.442(4) yes . . S(2) O(4) 1.456(4) yes . . S(2) N(2) 1.563(3) yes . . S(2) C(10) 1.773(4) yes . . P(1) O(5) 1.582(3) yes . . P(1) O(6) 1.576(3) yes . . P(1) O(7) 1.596(3) yes . . Si(1) N(1) 1.745(4) yes . . Si(1) N(2) 1.744(4) yes . . Si(1) C(1) 1.855(6) yes . . Si(1) C(2) 1.852(5) yes . . O(5) C(27) 1.452(6) yes . . O(6) C(29) 1.454(6) yes . . O(7) C(31) 1.446(6) yes . . C(3) C(4) 1.371(7) yes . . C(3) C(8) 1.377(7) yes . . C(4) C(5) 1.378(7) yes . . C(5) C(6) 1.386(8) yes . . C(6) C(7) 1.391(8) yes . . C(6) C(9) 1.509(8) yes . . C(7) C(8) 1.400(6) yes . . C(10) C(11) 1.389(8) yes . . C(10) C(15) 1.384(7) yes . . C(11) C(12) 1.389(8) yes . . C(12) C(13) 1.372(9) yes . . C(13) C(14) 1.395(9) yes . . C(13) C(16) 1.506(9) yes . . C(14) C(15) 1.381(8) yes . . C(17) C(18) 1.458(7) yes . . C(17) C(21) 1.410(6) yes . . C(17) C(22) 1.472(7) yes . . C(18) C(19) 1.435(7) yes . . C(18) C(23) 1.508(7) yes . . C(19) C(20) 1.419(6) yes . . C(19) C(24) 1.506(8) yes . . C(20) C(21) 1.466(7) yes . . C(20) C(25) 1.489(7) yes . . C(21) C(26) 1.503(7) yes . . C(27) C(28) 1.468(8) yes . . C(29) C(30) 1.476(8) yes . . C(31) C(32) 1.481(11) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(2) H(5) 0.950 no . . C(2) H(6) 0.950 no . . C(4) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(7) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(11) H(14) 0.950 no . . C(12) H(15) 0.950 no . . C(14) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(22) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(25) H(30) 0.950 no . . C(25) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(26) H(33) 0.950 no . . C(26) H(34) 0.950 no . . C(26) H(35) 0.950 no . . C(27) H(36) 0.950 no . . C(27) H(37) 0.950 no . . C(28) H(38) 0.950 no . . C(28) H(39) 0.950 no . . C(28) H(40) 0.950 no . . C(29) H(41) 0.950 no . . C(29) H(42) 0.950 no . . C(30) H(43) 0.950 no . . C(30) H(44) 0.950 no . . C(30) H(45) 0.950 no . . C(31) H(46) 0.950 no . . C(31) H(47) 0.950 no . . C(32) H(48) 0.950 no . . C(32) H(49) 0.950 no . . C(32) H(50) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 P(1) Ir(1) N(1) 91.63(11) yes . . . P(1) Ir(1) N(2) 95.40(10) yes . . . P(1) Ir(1) C(17) 144.12(12) yes . . . P(1) Ir(1) C(18) 106.41(12) yes . . . P(1) Ir(1) C(19) 92.27(12) yes . . . P(1) Ir(1) C(20) 113.63(13) yes . . . P(1) Ir(1) C(21) 151.64(14) yes . . . N(1) Ir(1) N(2) 69.82(14) yes . . . N(1) Ir(1) C(17) 96.17(16) yes . . . N(1) Ir(1) C(18) 108.56(17) yes . . . N(1) Ir(1) C(19) 146.14(16) yes . . . N(1) Ir(1) C(20) 154.71(16) yes . . . N(1) Ir(1) C(21) 116.47(17) yes . . . N(2) Ir(1) C(17) 120.17(15) yes . . . N(2) Ir(1) C(18) 158.19(15) yes . . . N(2) Ir(1) C(19) 143.00(16) yes . . . N(2) Ir(1) C(20) 107.15(15) yes . . . N(2) Ir(1) C(21) 97.83(15) yes . . . C(17) Ir(1) C(18) 38.10(17) yes . . . C(17) Ir(1) C(19) 62.81(18) yes . . . C(17) Ir(1) C(20) 62.88(18) yes . . . C(17) Ir(1) C(21) 35.93(16) yes . . . C(18) Ir(1) C(19) 38.5(2) yes . . . C(18) Ir(1) C(20) 64.50(18) yes . . . C(18) Ir(1) C(21) 62.74(16) yes . . . C(19) Ir(1) C(20) 37.91(16) yes . . . C(19) Ir(1) C(21) 62.56(17) yes . . . C(20) Ir(1) C(21) 38.24(19) yes . . . O(1) S(1) O(2) 117.4(2) yes . . . O(1) S(1) N(1) 111.6(2) yes . . . O(1) S(1) C(3) 105.5(2) yes . . . O(2) S(1) N(1) 108.1(2) yes . . . O(2) S(1) C(3) 105.0(2) yes . . . N(1) S(1) C(3) 108.7(2) yes . . . O(3) S(2) O(4) 116.5(2) yes . . . O(3) S(2) N(2) 112.8(2) yes . . . O(3) S(2) C(10) 104.6(2) yes . . . O(4) S(2) N(2) 108.3(2) yes . . . O(4) S(2) C(10) 105.0(2) yes . . . N(2) S(2) C(10) 108.9(2) yes . . . Ir(1) P(1) O(5) 110.11(12) yes . . . Ir(1) P(1) O(6) 112.41(13) yes . . . Ir(1) P(1) O(7) 120.38(13) yes . . . O(5) P(1) O(6) 108.92(18) yes . . . O(5) P(1) O(7) 98.15(18) yes . . . O(6) P(1) O(7) 105.63(18) yes . . . N(1) Si(1) N(2) 90.03(19) yes . . . N(1) Si(1) C(1) 113.5(2) yes . . . N(1) Si(1) C(2) 115.6(2) yes . . . N(2) Si(1) C(1) 113.9(2) yes . . . N(2) Si(1) C(2) 114.3(2) yes . . . C(1) Si(1) C(2) 108.7(3) yes . . . P(1) O(5) C(27) 126.9(3) yes . . . P(1) O(6) C(29) 124.3(3) yes . . . P(1) O(7) C(31) 122.4(3) yes . . . Ir(1) N(1) S(1) 136.9(2) yes . . . Ir(1) N(1) Si(1) 99.44(18) yes . . . S(1) N(1) Si(1) 123.5(2) yes . . . Ir(1) N(2) S(2) 136.1(2) yes . . . Ir(1) N(2) Si(1) 98.72(16) yes . . . S(2) N(2) Si(1) 122.5(2) yes . . . S(1) C(3) C(4) 120.0(4) yes . . . S(1) C(3) C(8) 119.7(3) yes . . . C(4) C(3) C(8) 120.4(4) yes . . . C(3) C(4) C(5) 119.9(5) yes . . . C(4) C(5) C(6) 121.9(5) yes . . . C(5) C(6) C(7) 117.4(4) yes . . . C(5) C(6) C(9) 121.1(5) yes . . . C(7) C(6) C(9) 121.5(5) yes . . . C(6) C(7) C(8) 121.2(5) yes . . . C(3) C(8) C(7) 119.3(5) yes . . . S(2) C(10) C(11) 120.4(4) yes . . . S(2) C(10) C(15) 120.8(4) yes . . . C(11) C(10) C(15) 118.8(4) yes . . . C(10) C(11) C(12) 120.4(5) yes . . . C(11) C(12) C(13) 121.1(6) yes . . . C(12) C(13) C(14) 118.2(5) yes . . . C(12) C(13) C(16) 121.5(5) yes . . . C(14) C(13) C(16) 120.2(5) yes . . . C(13) C(14) C(15) 121.1(5) yes . . . C(10) C(15) C(14) 120.3(5) yes . . . Ir(1) C(17) C(18) 66.3(2) yes . . . Ir(1) C(17) C(21) 71.8(2) yes . . . Ir(1) C(17) C(22) 127.5(3) yes . . . C(18) C(17) C(21) 107.7(4) yes . . . C(18) C(17) C(22) 125.5(4) yes . . . C(21) C(17) C(22) 126.8(4) yes . . . Ir(1) C(18) C(17) 75.6(2) yes . . . Ir(1) C(18) C(19) 71.5(2) yes . . . Ir(1) C(18) C(23) 129.3(3) yes . . . C(17) C(18) C(19) 107.4(4) yes . . . C(17) C(18) C(23) 125.2(4) yes . . . C(19) C(18) C(23) 125.9(4) yes . . . Ir(1) C(19) C(18) 69.9(3) yes . . . Ir(1) C(19) C(20) 71.1(3) yes . . . Ir(1) C(19) C(24) 129.6(3) yes . . . C(18) C(19) C(20) 108.8(4) yes . . . C(18) C(19) C(24) 125.1(4) yes . . . C(20) C(19) C(24) 125.8(4) yes . . . Ir(1) C(20) C(19) 71.0(3) yes . . . Ir(1) C(20) C(21) 74.4(3) yes . . . Ir(1) C(20) C(25) 130.2(3) yes . . . C(19) C(20) C(21) 107.0(4) yes . . . C(19) C(20) C(25) 125.5(4) yes . . . C(21) C(20) C(25) 126.1(4) yes . . . Ir(1) C(21) C(17) 72.3(2) yes . . . Ir(1) C(21) C(20) 67.3(2) yes . . . Ir(1) C(21) C(26) 127.8(3) yes . . . C(17) C(21) C(20) 108.6(4) yes . . . C(17) C(21) C(26) 126.4(4) yes . . . C(20) C(21) C(26) 125.0(4) yes . . . O(5) C(27) C(28) 110.1(4) yes . . . O(6) C(29) C(30) 109.5(4) yes . . . O(7) C(31) C(32) 108.1(5) yes . . . Si(1) C(1) H(1) 109.2 no . . . Si(1) C(1) H(2) 109.8 no . . . Si(1) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . Si(1) C(2) H(4) 109.5 no . . . Si(1) C(2) H(5) 109.8 no . . . Si(1) C(2) H(6) 109.1 no . . . H(4) C(2) H(5) 109.5 no . . . H(4) C(2) H(6) 109.5 no . . . H(5) C(2) H(6) 109.5 no . . . C(3) C(4) H(7) 119.7 no . . . C(5) C(4) H(7) 120.4 no . . . C(4) C(5) H(8) 119.4 no . . . C(6) C(5) H(8) 118.7 no . . . C(6) C(7) H(9) 119.2 no . . . C(8) C(7) H(9) 119.6 no . . . C(3) C(8) H(10) 120.3 no . . . C(7) C(8) H(10) 120.5 no . . . C(6) C(9) H(11) 109.6 no . . . C(6) C(9) H(12) 108.7 no . . . C(6) C(9) H(13) 110.2 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . C(10) C(11) H(14) 119.8 no . . . C(12) C(11) H(14) 119.9 no . . . C(11) C(12) H(15) 119.4 no . . . C(13) C(12) H(15) 119.4 no . . . C(13) C(14) H(16) 119.2 no . . . C(15) C(14) H(16) 119.6 no . . . C(10) C(15) H(17) 119.7 no . . . C(14) C(15) H(17) 120.0 no . . . C(13) C(16) H(18) 110.7 no . . . C(13) C(16) H(19) 109.5 no . . . C(13) C(16) H(20) 108.2 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(17) C(22) H(21) 109.6 no . . . C(17) C(22) H(22) 109.8 no . . . C(17) C(22) H(23) 109.0 no . . . H(21) C(22) H(22) 109.5 no . . . H(21) C(22) H(23) 109.5 no . . . H(22) C(22) H(23) 109.5 no . . . C(18) C(23) H(24) 109.4 no . . . C(18) C(23) H(25) 109.7 no . . . C(18) C(23) H(26) 109.3 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . C(19) C(24) H(27) 109.1 no . . . C(19) C(24) H(28) 109.7 no . . . C(19) C(24) H(29) 109.6 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . C(20) C(25) H(30) 109.3 no . . . C(20) C(25) H(31) 110.1 no . . . C(20) C(25) H(32) 109.0 no . . . H(30) C(25) H(31) 109.5 no . . . H(30) C(25) H(32) 109.5 no . . . H(31) C(25) H(32) 109.5 no . . . C(21) C(26) H(33) 109.5 no . . . C(21) C(26) H(34) 110.0 no . . . C(21) C(26) H(35) 108.8 no . . . H(33) C(26) H(34) 109.5 no . . . H(33) C(26) H(35) 109.5 no . . . H(34) C(26) H(35) 109.5 no . . . O(5) C(27) H(36) 109.0 no . . . O(5) C(27) H(37) 109.9 no . . . C(28) C(27) H(36) 109.3 no . . . C(28) C(27) H(37) 109.1 no . . . H(36) C(27) H(37) 109.5 no . . . C(27) C(28) H(38) 109.6 no . . . C(27) C(28) H(39) 110.7 no . . . C(27) C(28) H(40) 108.1 no . . . H(38) C(28) H(39) 109.5 no . . . H(38) C(28) H(40) 109.5 no . . . H(39) C(28) H(40) 109.5 no . . . O(6) C(29) H(41) 109.2 no . . . O(6) C(29) H(42) 110.0 no . . . C(30) C(29) H(41) 108.6 no . . . C(30) C(29) H(42) 110.2 no . . . H(41) C(29) H(42) 109.5 no . . . C(29) C(30) H(43) 108.6 no . . . C(29) C(30) H(44) 110.9 no . . . C(29) C(30) H(45) 109.0 no . . . H(43) C(30) H(44) 109.5 no . . . H(43) C(30) H(45) 109.5 no . . . H(44) C(30) H(45) 109.5 no . . . O(7) C(31) H(46) 110.1 no . . . O(7) C(31) H(47) 109.8 no . . . C(32) C(31) H(46) 108.2 no . . . C(32) C(31) H(47) 111.0 no . . . H(46) C(31) H(47) 109.5 no . . . C(31) C(32) H(48) 107.8 no . . . C(31) C(32) H(49) 111.6 no . . . C(31) C(32) H(50) 109.0 no . . . H(48) C(32) H(49) 109.5 no . . . H(48) C(32) H(50) 109.5 no . . . H(49) C(32) H(50) 109.5 no . . . #===END data___3c.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 647951' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H37 Cl2 Ir N2 O5 S2 Si ' _chemical_formula_moiety 'C27 H35 Ir N2 O5 S2 Si, C H2 Cl2 ' _chemical_formula_weight 836.94 _chemical_melting_point ? _chemical_absolute_configuration ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.605(3) _cell_length_b 14.305(4) _cell_length_c 18.654(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3363.5(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14676 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664.00 _exptl_absorpt_coefficient_mu 4.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.118 _exptl_absorpt_correction_T_max 0.272 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 31426 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_max 31.41 _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7623 _reflns_number_gt 6648 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0924 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 7623 _refine_ls_number_parameters 408 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0011Fo^2^ + 0.2000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.20 _refine_diff_density_min -1.35 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 3361 Friedel Pairs' _refine_ls_abs_structure_Flack 0.008(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.082 0.070 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.615310(10) -0.007130(10) 0.855150(10) 0.02393(4) Uani 1.00 1 d . . . Cl(1) Cl 1.1291(3) 0.0962(3) 0.6275(2) 0.1421(16) Uani 1.00 1 d . . . Cl(2) Cl 1.0935(3) 0.1165(3) 0.7789(2) 0.1304(15) Uani 1.00 1 d . . . S(1) S 0.66747(12) -0.04608(10) 1.03000(7) 0.0345(3) Uani 1.00 1 d . . . S(2) S 0.55128(13) 0.22025(10) 0.83173(9) 0.0397(3) Uani 1.00 1 d . . . Si(1) Si 0.56327(16) 0.12532(13) 0.97229(9) 0.0410(4) Uani 1.00 1 d . . . O(1) O 0.6340(3) -0.1425(3) 1.0302(2) 0.0421(11) Uani 1.00 1 d . . . O(2) O 0.6542(3) 0.0044(3) 1.0963(2) 0.0503(12) Uani 1.00 1 d . . . O(3) O 0.4858(4) 0.1997(3) 0.7710(2) 0.0496(13) Uani 1.00 1 d . . . O(4) O 0.5164(4) 0.2950(3) 0.8790(2) 0.0554(14) Uani 1.00 1 d . . . O(5) O 0.8445(4) 0.0366(4) 0.8280(3) 0.0615(16) Uani 1.00 1 d . . . N(1) N 0.5691(4) 0.1323(3) 0.8798(2) 0.0352(12) Uani 1.00 1 d . . . N(2) N 0.6141(3) 0.0128(3) 0.9682(2) 0.0319(10) Uani 1.00 1 d . . . C(1) C 0.4230(8) 0.1281(8) 1.0031(5) 0.088(3) Uani 1.00 1 d . . . C(2) C 0.6441(9) 0.2127(5) 1.0202(5) 0.088(3) Uani 1.00 1 d . . . C(3) C 0.8059(5) -0.0481(4) 1.0104(3) 0.0369(15) Uani 1.00 1 d . . . C(4) C 0.8643(5) 0.0339(4) 1.0146(3) 0.0476(18) Uani 1.00 1 d . . . C(5) C 0.9703(6) 0.0327(6) 0.9999(4) 0.056(2) Uani 1.00 1 d . . . C(6) C 1.0228(5) -0.0504(7) 0.9828(4) 0.059(2) Uani 1.00 1 d . . . C(7) C 0.9640(6) -0.1318(6) 0.9793(4) 0.059(2) Uani 1.00 1 d . . . C(8) C 0.8539(5) -0.1307(5) 0.9940(3) 0.0466(18) Uani 1.00 1 d . . . C(9) C 1.1387(6) -0.0503(9) 0.9680(6) 0.095(3) Uani 1.00 1 d . . . C(10) C 0.6764(5) 0.2528(4) 0.7956(3) 0.0421(17) Uani 1.00 1 d . . . C(11) C 0.7061(6) 0.2251(5) 0.7287(4) 0.056(2) Uani 1.00 1 d . . . C(12) C 0.8004(7) 0.2522(5) 0.7005(4) 0.058(2) Uani 1.00 1 d . . . C(13) C 0.8697(8) 0.3084(6) 0.7396(4) 0.069(2) Uani 1.00 1 d . . . C(14) C 0.8396(8) 0.3337(6) 0.8070(4) 0.075(2) Uani 1.00 1 d . . . C(15) C 0.7442(8) 0.3094(6) 0.8357(4) 0.070(2) Uani 1.00 1 d . . . C(16) C 0.9765(9) 0.3399(8) 0.7103(6) 0.089(3) Uani 1.00 1 d . . . C(17) C 0.4591(4) -0.0503(4) 0.8047(3) 0.0325(13) Uani 1.00 1 d . . . C(18) C 0.4877(4) -0.1186(3) 0.8563(3) 0.0314(12) Uani 1.00 1 d . . . C(19) C 0.5905(4) -0.1561(3) 0.8373(3) 0.0335(14) Uani 1.00 1 d . . . C(20) C 0.6207(4) -0.1133(3) 0.7698(3) 0.0333(13) Uani 1.00 1 d . . . C(21) C 0.5423(4) -0.0446(4) 0.7524(3) 0.0326(13) Uani 1.00 1 d . . . C(22) C 0.3580(5) 0.0026(5) 0.8032(3) 0.0488(17) Uani 1.00 1 d . . . C(23) C 0.4256(6) -0.1461(5) 0.9202(3) 0.052(2) Uani 1.00 1 d . . . C(24) C 0.6430(5) -0.2380(4) 0.8717(4) 0.0497(18) Uani 1.00 1 d . . . C(25) C 0.7137(5) -0.1393(4) 0.7252(4) 0.0487(18) Uani 1.00 1 d . . . C(26) C 0.5374(5) 0.0077(4) 0.6839(3) 0.0475(16) Uani 1.00 1 d . . . C(27) C 0.7579(4) 0.0233(4) 0.8419(3) 0.0363(14) Uani 1.00 1 d . . . C(28) C 1.0402(9) 0.0841(9) 0.6979(8) 0.121(5) Uani 1.00 1 d . . . H(1) H 0.4014 0.1908 1.0112 0.106 Uiso 1.00 1 c R . . H(2) H 0.4172 0.0935 1.0464 0.106 Uiso 1.00 1 c R . . H(3) H 0.3789 0.1007 0.9675 0.106 Uiso 1.00 1 c R . . H(4) H 0.7130 0.1881 1.0286 0.106 Uiso 1.00 1 c R . . H(5) H 0.6112 0.2266 1.0647 0.106 Uiso 1.00 1 c R . . H(6) H 0.6496 0.2682 0.9925 0.106 Uiso 1.00 1 c R . . H(7) H 0.8307 0.0908 1.0278 0.057 Uiso 1.00 1 c R . . H(8) H 1.0098 0.0892 1.0014 0.068 Uiso 1.00 1 c R . . H(9) H 0.9979 -0.1890 0.9673 0.071 Uiso 1.00 1 c R . . H(10) H 0.8139 -0.1870 0.9925 0.056 Uiso 1.00 1 c R . . H(11) H 1.1518 -0.0401 0.9184 0.114 Uiso 1.00 1 c R . . H(12) H 1.1658 -0.1098 0.9815 0.114 Uiso 1.00 1 c R . . H(13) H 1.1727 -0.0030 0.9953 0.114 Uiso 1.00 1 c R . . H(14) H 0.6600 0.1863 0.7015 0.067 Uiso 1.00 1 c R . . H(15) H 0.8196 0.2319 0.6538 0.069 Uiso 1.00 1 c R . . H(16) H 0.8868 0.3708 0.8347 0.090 Uiso 1.00 1 c R . . H(17) H 0.7241 0.3307 0.8820 0.084 Uiso 1.00 1 c R . . H(18) H 1.0290 0.2954 0.7232 0.107 Uiso 1.00 1 c R . . H(19) H 0.9947 0.3991 0.7298 0.107 Uiso 1.00 1 c R . . H(20) H 0.9726 0.3444 0.6596 0.107 Uiso 1.00 1 c R . . H(21) H 0.3064 -0.0304 0.7760 0.059 Uiso 1.00 1 c R . . H(22) H 0.3707 0.0618 0.7817 0.059 Uiso 1.00 1 c R . . H(23) H 0.3327 0.0114 0.8507 0.059 Uiso 1.00 1 c R . . H(24) H 0.4447 -0.1078 0.9597 0.062 Uiso 1.00 1 c R . . H(25) H 0.4397 -0.2096 0.9314 0.062 Uiso 1.00 1 c R . . H(26) H 0.3521 -0.1386 0.9103 0.062 Uiso 1.00 1 c R . . H(27) H 0.6849 -0.2176 0.9111 0.060 Uiso 1.00 1 c R . . H(28) H 0.6871 -0.2681 0.8375 0.060 Uiso 1.00 1 c R . . H(29) H 0.5906 -0.2806 0.8882 0.060 Uiso 1.00 1 c R . . H(30) H 0.7735 -0.1033 0.7393 0.059 Uiso 1.00 1 c R . . H(31) H 0.6986 -0.1278 0.6761 0.059 Uiso 1.00 1 c R . . H(32) H 0.7287 -0.2039 0.7318 0.059 Uiso 1.00 1 c R . . H(33) H 0.5102 -0.0314 0.6470 0.057 Uiso 1.00 1 c R . . H(34) H 0.6067 0.0280 0.6713 0.057 Uiso 1.00 1 c R . . H(35) H 0.4925 0.0604 0.6896 0.057 Uiso 1.00 1 c R . . H(36) H 0.9815 0.1240 0.6886 0.145 Uiso 1.00 1 c R . . H(37) H 1.0165 0.0211 0.7003 0.145 Uiso 1.00 1 c R . . 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) 0.02385(10) 0.02344(9) 0.02450(10) 0.00035(7) -0.00174(6) -0.00021(7) Cl(1) 0.132(3) 0.129(3) 0.165(3) -0.058(2) 0.004(2) 0.005(2) Cl(2) 0.083(2) 0.138(3) 0.170(3) -0.002(2) -0.022(2) 0.017(2) S(1) 0.0394(7) 0.0377(7) 0.0262(6) -0.0035(5) -0.0070(5) 0.0067(5) S(2) 0.0524(9) 0.0261(6) 0.0406(7) 0.0067(6) -0.0063(6) 0.0009(5) Si(1) 0.0526(10) 0.0390(8) 0.0314(8) 0.0129(7) -0.0018(7) -0.0070(6) O(1) 0.045(2) 0.042(2) 0.039(2) -0.0096(18) -0.0074(18) 0.0120(17) O(2) 0.061(2) 0.064(2) 0.0265(17) -0.007(2) -0.0082(17) -0.003(2) O(3) 0.056(2) 0.039(2) 0.054(2) 0.009(2) -0.018(2) 0.009(2) O(4) 0.073(3) 0.030(2) 0.063(3) 0.014(2) -0.004(2) -0.011(2) O(5) 0.036(2) 0.082(3) 0.066(3) -0.017(2) 0.006(2) 0.001(2) N(1) 0.050(2) 0.026(2) 0.030(2) 0.009(2) -0.001(2) 0.0014(18) N(2) 0.038(2) 0.033(2) 0.0250(19) 0.008(2) -0.0052(16) -0.0023(16) C(1) 0.084(6) 0.098(7) 0.083(6) 0.045(6) 0.042(5) 0.014(5) C(2) 0.153(10) 0.040(3) 0.072(5) 0.027(5) -0.057(6) -0.021(3) C(3) 0.043(3) 0.039(3) 0.028(2) -0.004(2) -0.009(2) 0.008(2) C(4) 0.055(4) 0.047(3) 0.041(3) -0.011(3) -0.005(2) 0.002(2) C(5) 0.053(4) 0.067(4) 0.049(4) -0.029(3) -0.006(3) 0.003(3) C(6) 0.035(3) 0.093(6) 0.049(4) -0.006(3) -0.000(3) 0.018(4) C(7) 0.053(4) 0.061(4) 0.064(4) 0.017(3) 0.001(3) 0.010(3) C(8) 0.043(3) 0.044(3) 0.053(3) -0.003(2) -0.008(3) 0.011(2) C(9) 0.033(4) 0.161(11) 0.091(7) -0.007(5) 0.008(4) 0.011(7) C(10) 0.059(4) 0.035(3) 0.032(3) -0.003(2) -0.006(2) 0.008(2) C(11) 0.075(5) 0.039(3) 0.053(4) -0.007(3) -0.003(3) -0.004(3) C(12) 0.069(4) 0.050(4) 0.054(4) 0.001(3) 0.002(3) -0.005(3) C(13) 0.083(6) 0.061(4) 0.062(5) -0.017(4) 0.009(4) 0.006(3) C(14) 0.082(5) 0.083(6) 0.061(5) -0.046(5) -0.004(4) -0.011(4) C(15) 0.098(6) 0.063(5) 0.049(4) -0.028(4) -0.000(4) -0.008(3) C(16) 0.085(7) 0.087(7) 0.096(7) -0.024(6) 0.000(6) 0.002(6) C(17) 0.028(2) 0.033(2) 0.037(2) -0.004(2) -0.009(2) -0.002(2) C(18) 0.023(2) 0.033(2) 0.038(2) -0.0061(18) -0.003(2) -0.002(2) C(19) 0.034(2) 0.022(2) 0.044(3) -0.0043(19) -0.009(2) -0.004(2) C(20) 0.037(2) 0.027(2) 0.036(2) -0.001(2) -0.004(2) -0.006(2) C(21) 0.035(2) 0.034(2) 0.029(2) -0.002(2) -0.005(2) -0.003(2) C(22) 0.038(3) 0.052(3) 0.056(3) 0.007(3) -0.010(2) 0.001(3) C(23) 0.050(3) 0.061(4) 0.045(3) -0.013(3) -0.004(3) 0.009(3) C(24) 0.056(4) 0.032(2) 0.061(4) 0.006(2) -0.018(3) 0.002(2) C(25) 0.050(3) 0.043(3) 0.054(3) -0.009(2) 0.015(3) -0.013(3) C(26) 0.074(4) 0.037(3) 0.031(2) -0.006(3) -0.012(2) 0.001(2) C(27) 0.025(2) 0.041(3) 0.044(3) 0.001(2) -0.003(2) -0.007(2) C(28) 0.055(6) 0.087(8) 0.220(16) -0.018(5) -0.008(8) -0.002(9) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) N(1) 2.129(4) yes . . Ir(1) N(2) 2.128(4) yes . . Ir(1) C(17) 2.267(5) yes . . Ir(1) C(18) 2.265(5) yes . . Ir(1) C(19) 2.179(5) yes . . Ir(1) C(20) 2.201(5) yes . . Ir(1) C(21) 2.193(5) yes . . Ir(1) C(27) 1.866(5) yes . . Cl(1) C(28) 1.735(15) yes . . Cl(2) C(28) 1.718(16) yes . . S(1) O(1) 1.443(4) yes . . S(1) O(2) 1.442(4) yes . . S(1) N(2) 1.579(4) yes . . S(1) C(3) 1.783(6) yes . . S(2) O(3) 1.432(5) yes . . S(2) O(4) 1.453(5) yes . . S(2) N(1) 1.561(4) yes . . S(2) C(10) 1.778(7) yes . . Si(1) N(1) 1.730(4) yes . . Si(1) N(2) 1.734(4) yes . . Si(1) C(1) 1.859(11) yes . . Si(1) C(2) 1.844(9) yes . . O(5) C(27) 1.137(7) yes . . C(3) C(4) 1.387(9) yes . . C(3) C(8) 1.363(9) yes . . C(4) C(5) 1.364(10) yes . . C(5) C(6) 1.397(12) yes . . C(6) C(7) 1.381(12) yes . . C(6) C(9) 1.487(11) yes . . C(7) C(8) 1.415(10) yes . . C(10) C(11) 1.362(10) yes . . C(10) C(15) 1.394(11) yes . . C(11) C(12) 1.357(12) yes . . C(12) C(13) 1.393(12) yes . . C(13) C(14) 1.362(12) yes . . C(13) C(16) 1.521(15) yes . . C(14) C(15) 1.362(14) yes . . C(17) C(18) 1.418(8) yes . . C(17) C(21) 1.435(8) yes . . C(17) C(22) 1.483(8) yes . . C(18) C(19) 1.447(7) yes . . C(18) C(23) 1.479(9) yes . . C(19) C(20) 1.452(8) yes . . C(19) C(24) 1.490(8) yes . . C(20) C(21) 1.431(8) yes . . C(20) C(25) 1.485(9) yes . . C(21) C(26) 1.482(8) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(2) H(5) 0.950 no . . C(2) H(6) 0.950 no . . C(4) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(7) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(11) H(14) 0.950 no . . C(12) H(15) 0.950 no . . C(14) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(22) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(25) H(30) 0.950 no . . C(25) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(26) H(33) 0.950 no . . C(26) H(34) 0.950 no . . C(26) H(35) 0.950 no . . C(28) H(36) 0.950 no . . C(28) H(37) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ir(1) N(2) 70.03(17) yes . . . N(1) Ir(1) C(17) 96.2(2) yes . . . N(1) Ir(1) C(18) 117.62(19) yes . . . N(1) Ir(1) C(19) 155.5(2) yes . . . N(1) Ir(1) C(20) 144.21(19) yes . . . N(1) Ir(1) C(21) 107.6(2) yes . . . N(1) Ir(1) C(27) 94.2(2) yes . . . N(2) Ir(1) C(17) 116.21(19) yes . . . N(2) Ir(1) C(18) 94.59(19) yes . . . N(2) Ir(1) C(19) 106.33(19) yes . . . N(2) Ir(1) C(20) 144.04(18) yes . . . N(2) Ir(1) C(21) 153.65(19) yes . . . N(2) Ir(1) C(27) 96.1(2) yes . . . C(17) Ir(1) C(18) 36.5(2) yes . . . C(17) Ir(1) C(19) 63.0(2) yes . . . C(17) Ir(1) C(20) 62.5(2) yes . . . C(17) Ir(1) C(21) 37.5(2) yes . . . C(17) Ir(1) C(27) 147.7(2) yes . . . C(18) Ir(1) C(19) 37.93(19) yes . . . C(18) Ir(1) C(20) 62.8(2) yes . . . C(18) Ir(1) C(21) 62.5(2) yes . . . C(18) Ir(1) C(27) 148.2(2) yes . . . C(19) Ir(1) C(20) 38.7(2) yes . . . C(19) Ir(1) C(21) 64.4(2) yes . . . C(19) Ir(1) C(27) 110.2(2) yes . . . C(20) Ir(1) C(21) 38.0(2) yes . . . C(20) Ir(1) C(27) 92.0(2) yes . . . C(21) Ir(1) C(27) 110.2(2) yes . . . O(1) S(1) O(2) 116.3(2) yes . . . O(1) S(1) N(2) 112.8(2) yes . . . O(1) S(1) C(3) 105.8(2) yes . . . O(2) S(1) N(2) 108.0(2) yes . . . O(2) S(1) C(3) 107.3(2) yes . . . N(2) S(1) C(3) 106.0(2) yes . . . O(3) S(2) O(4) 117.1(3) yes . . . O(3) S(2) N(1) 111.8(2) yes . . . O(3) S(2) C(10) 105.4(3) yes . . . O(4) S(2) N(1) 106.7(2) yes . . . O(4) S(2) C(10) 107.8(3) yes . . . N(1) S(2) C(10) 107.5(3) yes . . . N(1) Si(1) N(2) 89.7(2) yes . . . N(1) Si(1) C(1) 110.3(3) yes . . . N(1) Si(1) C(2) 114.9(3) yes . . . N(2) Si(1) C(1) 112.6(4) yes . . . N(2) Si(1) C(2) 116.5(3) yes . . . C(1) Si(1) C(2) 111.2(5) yes . . . Ir(1) N(1) S(2) 132.1(2) yes . . . Ir(1) N(1) Si(1) 99.9(2) yes . . . S(2) N(1) Si(1) 127.9(3) yes . . . Ir(1) N(2) S(1) 130.5(2) yes . . . Ir(1) N(2) Si(1) 99.8(2) yes . . . S(1) N(2) Si(1) 128.3(2) yes . . . S(1) C(3) C(4) 119.6(5) yes . . . S(1) C(3) C(8) 119.6(5) yes . . . C(4) C(3) C(8) 120.7(6) yes . . . C(3) C(4) C(5) 119.8(6) yes . . . C(4) C(5) C(6) 121.4(7) yes . . . C(5) C(6) C(7) 118.3(7) yes . . . C(5) C(6) C(9) 120.5(9) yes . . . C(7) C(6) C(9) 121.2(9) yes . . . C(6) C(7) C(8) 120.5(7) yes . . . C(3) C(8) C(7) 119.2(6) yes . . . S(2) C(10) C(11) 121.0(5) yes . . . S(2) C(10) C(15) 119.5(5) yes . . . C(11) C(10) C(15) 119.5(7) yes . . . C(10) C(11) C(12) 120.9(7) yes . . . C(11) C(12) C(13) 120.7(7) yes . . . C(12) C(13) C(14) 117.6(8) yes . . . C(12) C(13) C(16) 122.5(8) yes . . . C(14) C(13) C(16) 119.9(8) yes . . . C(13) C(14) C(15) 122.7(9) yes . . . C(10) C(15) C(14) 118.6(7) yes . . . Ir(1) C(17) C(18) 71.7(3) yes . . . Ir(1) C(17) C(21) 68.4(3) yes . . . Ir(1) C(17) C(22) 128.0(4) yes . . . C(18) C(17) C(21) 108.4(4) yes . . . C(18) C(17) C(22) 125.7(5) yes . . . C(21) C(17) C(22) 125.9(5) yes . . . Ir(1) C(18) C(17) 71.9(3) yes . . . Ir(1) C(18) C(19) 67.8(2) yes . . . Ir(1) C(18) C(23) 124.8(4) yes . . . C(17) C(18) C(19) 108.5(4) yes . . . C(17) C(18) C(23) 126.6(5) yes . . . C(19) C(18) C(23) 124.9(5) yes . . . Ir(1) C(19) C(18) 74.3(2) yes . . . Ir(1) C(19) C(20) 71.5(2) yes . . . Ir(1) C(19) C(24) 129.7(4) yes . . . C(18) C(19) C(20) 106.9(4) yes . . . C(18) C(19) C(24) 125.7(5) yes . . . C(20) C(19) C(24) 126.1(5) yes . . . Ir(1) C(20) C(19) 69.8(3) yes . . . Ir(1) C(20) C(21) 70.7(3) yes . . . Ir(1) C(20) C(25) 127.1(4) yes . . . C(19) C(20) C(21) 107.8(4) yes . . . C(19) C(20) C(25) 125.9(5) yes . . . C(21) C(20) C(25) 126.2(5) yes . . . Ir(1) C(21) C(17) 74.1(3) yes . . . Ir(1) C(21) C(20) 71.3(3) yes . . . Ir(1) C(21) C(26) 130.4(4) yes . . . C(17) C(21) C(20) 108.1(4) yes . . . C(17) C(21) C(26) 125.8(5) yes . . . C(20) C(21) C(26) 124.8(5) yes . . . Ir(1) C(27) O(5) 173.3(5) yes . . . Cl(1) C(28) Cl(2) 112.8(6) yes . . . Si(1) C(1) H(1) 110.0 no . . . Si(1) C(1) H(2) 109.0 no . . . Si(1) C(1) H(3) 109.4 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . Si(1) C(2) H(4) 109.5 no . . . Si(1) C(2) H(5) 108.9 no . . . Si(1) C(2) H(6) 110.1 no . . . H(4) C(2) H(5) 109.5 no . . . H(4) C(2) H(6) 109.5 no . . . H(5) C(2) H(6) 109.5 no . . . C(3) C(4) H(7) 120.2 no . . . C(5) C(4) H(7) 120.0 no . . . C(4) C(5) H(8) 119.8 no . . . C(6) C(5) H(8) 118.9 no . . . C(6) C(7) H(9) 119.8 no . . . C(8) C(7) H(9) 119.7 no . . . C(3) C(8) H(10) 120.4 no . . . C(7) C(8) H(10) 120.4 no . . . C(6) C(9) H(11) 110.6 no . . . C(6) C(9) H(12) 107.7 no . . . C(6) C(9) H(13) 110.1 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . C(10) C(11) H(14) 119.4 no . . . C(12) C(11) H(14) 119.7 no . . . C(11) C(12) H(15) 119.4 no . . . C(13) C(12) H(15) 119.9 no . . . C(13) C(14) H(16) 118.5 no . . . C(15) C(14) H(16) 118.8 no . . . C(10) C(15) H(17) 120.7 no . . . C(14) C(15) H(17) 120.7 no . . . C(13) C(16) H(18) 109.1 no . . . C(13) C(16) H(19) 109.9 no . . . C(13) C(16) H(20) 109.4 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(17) C(22) H(21) 110.2 no . . . C(17) C(22) H(22) 108.5 no . . . C(17) C(22) H(23) 109.7 no . . . H(21) C(22) H(22) 109.5 no . . . H(21) C(22) H(23) 109.5 no . . . H(22) C(22) H(23) 109.5 no . . . C(18) C(23) H(24) 109.7 no . . . C(18) C(23) H(25) 109.4 no . . . C(18) C(23) H(26) 109.2 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . C(19) C(24) H(27) 109.8 no . . . C(19) C(24) H(28) 109.0 no . . . C(19) C(24) H(29) 109.6 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . C(20) C(25) H(30) 109.5 no . . . C(20) C(25) H(31) 109.7 no . . . C(20) C(25) H(32) 109.2 no . . . H(30) C(25) H(31) 109.5 no . . . H(30) C(25) H(32) 109.5 no . . . H(31) C(25) H(32) 109.5 no . . . C(21) C(26) H(33) 110.0 no . . . C(21) C(26) H(34) 109.2 no . . . C(21) C(26) H(35) 109.2 no . . . H(33) C(26) H(34) 109.5 no . . . H(33) C(26) H(35) 109.5 no . . . H(34) C(26) H(35) 109.5 no . . . Cl(1) C(28) H(36) 107.8 no . . . Cl(1) C(28) H(37) 109.4 no . . . Cl(2) C(28) H(36) 107.7 no . . . Cl(2) C(28) H(37) 109.7 no . . . H(36) C(28) H(37) 109.5 no . . . #===END data___5.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 647952' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C43 H48 Cl2 Ir N2 O4 P S2 ' _chemical_formula_moiety 'C42 H46 Ir N2 O4 P S2, C H2 Cl2 ' _chemical_formula_weight 1015.08 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,1/2-Y,1/2+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,1/2+Y,1/2-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 14.832(5) _cell_length_b 19.130(7) _cell_length_c 30.389(11) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 8623(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 17674 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 29.1 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080.00 _exptl_absorpt_coefficient_mu 3.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.506 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 88525 _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_theta_max 29.23 _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). The two amido hydrogen atoms were not included in the refinement. ; _reflns_number_total 9870 _reflns_number_gt 5836 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1386 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9869 _refine_ls_number_parameters 542 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0009Fo^2^ + 0.6000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 3.68 _refine_diff_density_min -2.16 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.68517(2) 0.245810(10) 0.075080(10) 0.01909(6) Uani 1.00 1 d . . . Cl(1) Cl 1.07706(19) 0.2942(2) 0.15911(10) 0.0843(10) Uani 1.00 1 d . . . Cl(2) Cl 0.9293(2) 0.22686(17) 0.20651(9) 0.0801(10) Uani 1.00 1 d . . . S(1) S 0.50760(11) 0.33095(9) 0.03451(6) 0.0249(4) Uani 1.00 1 d . . . S(2) S 0.75048(12) 0.38050(9) 0.13876(5) 0.0259(4) Uani 1.00 1 d . . . P(1) P 0.58615(11) 0.18463(9) 0.11957(5) 0.0211(4) Uani 1.00 1 d . . . O(1) O 0.5308(3) 0.3587(2) -0.00818(16) 0.0384(15) Uani 1.00 1 d . . . O(2) O 0.4611(3) 0.2645(2) 0.03457(17) 0.0319(13) Uani 1.00 1 d . . . O(3) O 0.8376(3) 0.3866(2) 0.16029(18) 0.0396(15) Uani 1.00 1 d . . . O(4) O 0.7383(3) 0.4166(2) 0.09774(15) 0.0323(14) Uani 1.00 1 d . . . N(1) N 0.5895(3) 0.3281(2) 0.06785(17) 0.0246(14) Uani 1.00 1 d . . . N(2) N 0.7230(3) 0.3012(2) 0.13376(17) 0.0237(14) Uani 1.00 1 d . . . C(1) C 0.4339(4) 0.3936(3) 0.0579(2) 0.0249(17) Uani 1.00 1 d . . . C(2) C 0.4544(5) 0.4649(4) 0.0554(2) 0.039(2) Uani 1.00 1 d . . . C(3) C 0.3985(6) 0.5130(4) 0.0754(2) 0.043(2) Uani 1.00 1 d . . . C(4) C 0.3212(5) 0.4925(4) 0.0976(2) 0.038(2) Uani 1.00 1 d . . . C(5) C 0.3006(5) 0.4225(4) 0.0984(2) 0.042(2) Uani 1.00 1 d . . . C(6) C 0.3563(5) 0.3725(4) 0.0787(2) 0.036(2) Uani 1.00 1 d . . . C(7) C 0.2626(6) 0.5457(5) 0.1206(3) 0.063(3) Uani 1.00 1 d . . . C(8) C 0.6734(5) 0.4190(4) 0.1763(2) 0.032(2) Uani 1.00 1 d . . . C(9) C 0.6864(6) 0.4112(4) 0.2208(2) 0.050(2) Uani 1.00 1 d . . . C(10) C 0.6226(10) 0.4401(5) 0.2496(3) 0.078(4) Uani 1.00 1 d . . . C(11) C 0.5487(9) 0.4763(5) 0.2343(4) 0.080(4) Uani 1.00 1 d . . . C(12) C 0.5372(6) 0.4835(4) 0.1905(4) 0.062(3) Uani 1.00 1 d . . . C(13) C 0.5992(5) 0.4544(4) 0.1609(3) 0.042(2) Uani 1.00 1 d . . . C(14) C 0.4817(11) 0.5051(7) 0.2686(5) 0.161(7) Uani 1.00 1 d . . . C(15) C 0.7587(4) 0.2737(3) 0.0133(2) 0.0266(17) Uani 1.00 1 d . . . C(16) C 0.7045(4) 0.2110(3) 0.0074(2) 0.0276(18) Uani 1.00 1 d . . . C(17) C 0.7391(4) 0.1580(3) 0.0352(2) 0.0281(18) Uani 1.00 1 d . . . C(18) C 0.8111(4) 0.1877(4) 0.0612(2) 0.0318(19) Uani 1.00 1 d . . . C(19) C 0.8231(4) 0.2586(4) 0.0463(2) 0.0289(18) Uani 1.00 1 d . . . C(20) C 0.7513(5) 0.3409(4) -0.0118(2) 0.043(2) Uani 1.00 1 d . . . C(21) C 0.6369(5) 0.2009(4) -0.0290(2) 0.035(2) Uani 1.00 1 d . . . C(22) C 0.7161(5) 0.0817(4) 0.0329(2) 0.042(2) Uani 1.00 1 d . . . C(23) C 0.8774(5) 0.1497(5) 0.0895(2) 0.047(2) Uani 1.00 1 d . . . C(24) C 0.8963(5) 0.3073(5) 0.0615(2) 0.049(2) Uani 1.00 1 d . . . C(25) C 0.5414(4) 0.1024(3) 0.0975(2) 0.0243(17) Uani 1.00 1 d . . . C(26) C 0.4891(4) 0.1062(3) 0.0595(2) 0.0295(19) Uani 1.00 1 d . . . C(27) C 0.4502(5) 0.0468(3) 0.0431(2) 0.036(2) Uani 1.00 1 d . . . C(28) C 0.4622(6) -0.0177(4) 0.0636(2) 0.043(2) Uani 1.00 1 d . . . C(29) C 0.5144(5) -0.0219(4) 0.1008(3) 0.043(2) Uani 1.00 1 d . . . C(30) C 0.5548(5) 0.0383(3) 0.1180(2) 0.033(2) Uani 1.00 1 d . . . C(31) C 0.4833(4) 0.2275(3) 0.1402(2) 0.0230(16) Uani 1.00 1 d . . . C(32) C 0.4902(4) 0.2939(3) 0.1592(2) 0.0274(18) Uani 1.00 1 d . . . C(33) C 0.4169(5) 0.3233(4) 0.1800(2) 0.034(2) Uani 1.00 1 d . . . C(34) C 0.3344(5) 0.2894(4) 0.1805(2) 0.039(2) Uani 1.00 1 d . . . C(35) C 0.3263(5) 0.2249(4) 0.1608(2) 0.039(2) Uani 1.00 1 d . . . C(36) C 0.4014(4) 0.1935(4) 0.1410(2) 0.033(2) Uani 1.00 1 d . . . C(37) C 0.6414(4) 0.1590(3) 0.1712(2) 0.0246(17) Uani 1.00 1 d . . . C(38) C 0.6124(6) 0.1806(4) 0.2123(2) 0.054(2) Uani 1.00 1 d . . . C(39) C 0.6612(8) 0.1619(5) 0.2497(3) 0.075(3) Uani 1.00 1 d . . . C(40) C 0.7386(7) 0.1224(4) 0.2465(2) 0.057(2) Uani 1.00 1 d . . . C(41) C 0.7663(5) 0.1004(4) 0.2066(2) 0.038(2) Uani 1.00 1 d . . . C(42) C 0.7188(5) 0.1187(4) 0.1691(2) 0.037(2) Uani 1.00 1 d . . . C(43) C 0.9961(6) 0.3006(5) 0.2010(3) 0.064(3) Uani 1.00 1 d . . . H(1) H 0.5059 0.4801 0.0395 0.046 Uiso 1.00 1 c R . . H(2) H 0.4140 0.5611 0.0744 0.052 Uiso 1.00 1 c R . . H(3) H 0.2471 0.4076 0.1128 0.051 Uiso 1.00 1 c R . . H(4) H 0.3403 0.3244 0.0795 0.043 Uiso 1.00 1 c R . . H(5) H 0.2824 0.5505 0.1501 0.075 Uiso 1.00 1 c R . . H(6) H 0.2016 0.5307 0.1203 0.075 Uiso 1.00 1 c R . . H(7) H 0.2675 0.5894 0.1060 0.075 Uiso 1.00 1 c R . . H(8) H 0.7372 0.3866 0.2319 0.060 Uiso 1.00 1 c R . . H(9) H 0.6304 0.4346 0.2804 0.094 Uiso 1.00 1 c R . . H(10) H 0.4868 0.5087 0.1796 0.075 Uiso 1.00 1 c R . . H(11) H 0.5897 0.4593 0.1302 0.050 Uiso 1.00 1 c R . . H(12) H 0.4365 0.4710 0.2741 0.193 Uiso 1.00 1 c R . . H(13) H 0.4545 0.5464 0.2576 0.193 Uiso 1.00 1 c R . . H(14) H 0.5124 0.5154 0.2953 0.193 Uiso 1.00 1 c R . . H(15) H 0.7950 0.3731 -0.0012 0.052 Uiso 1.00 1 c R . . H(16) H 0.7618 0.3320 -0.0422 0.052 Uiso 1.00 1 c R . . H(17) H 0.6927 0.3601 -0.0082 0.052 Uiso 1.00 1 c R . . H(18) H 0.6307 0.2431 -0.0452 0.043 Uiso 1.00 1 c R . . H(19) H 0.6573 0.1649 -0.0481 0.043 Uiso 1.00 1 c R . . H(20) H 0.5801 0.1881 -0.0169 0.043 Uiso 1.00 1 c R . . H(21) H 0.6706 0.0746 0.0114 0.050 Uiso 1.00 1 c R . . H(22) H 0.7684 0.0560 0.0251 0.050 Uiso 1.00 1 c R . . H(23) H 0.6947 0.0662 0.0607 0.050 Uiso 1.00 1 c R . . H(24) H 0.8595 0.1022 0.0915 0.056 Uiso 1.00 1 c R . . H(25) H 0.9359 0.1524 0.0768 0.056 Uiso 1.00 1 c R . . H(26) H 0.8784 0.1699 0.1180 0.056 Uiso 1.00 1 c R . . H(27) H 0.9327 0.2837 0.0825 0.058 Uiso 1.00 1 c R . . H(28) H 0.9325 0.3210 0.0372 0.058 Uiso 1.00 1 c R . . H(29) H 0.8703 0.3475 0.0747 0.058 Uiso 1.00 1 c R . . H(30) H 0.4799 0.1498 0.0451 0.035 Uiso 1.00 1 c R . . H(31) H 0.4157 0.0492 0.0168 0.044 Uiso 1.00 1 c R . . H(32) H 0.4335 -0.0583 0.0523 0.052 Uiso 1.00 1 c R . . H(33) H 0.5236 -0.0659 0.1147 0.052 Uiso 1.00 1 c R . . H(34) H 0.5910 0.0353 0.1437 0.040 Uiso 1.00 1 c R . . H(35) H 0.5456 0.3188 0.1577 0.033 Uiso 1.00 1 c R . . H(36) H 0.4231 0.3673 0.1942 0.041 Uiso 1.00 1 c R . . H(37) H 0.2837 0.3105 0.1942 0.047 Uiso 1.00 1 c R . . H(38) H 0.2696 0.2018 0.1606 0.047 Uiso 1.00 1 c R . . H(39) H 0.3957 0.1485 0.1281 0.040 Uiso 1.00 1 c R . . H(40) H 0.5596 0.2084 0.2151 0.065 Uiso 1.00 1 c R . . H(41) H 0.6404 0.1765 0.2778 0.090 Uiso 1.00 1 c R . . H(42) H 0.7716 0.1106 0.2722 0.068 Uiso 1.00 1 c R . . H(43) H 0.8187 0.0721 0.2041 0.045 Uiso 1.00 1 c R . . H(44) H 0.7401 0.1036 0.1412 0.044 Uiso 1.00 1 c R . . H(45) H 1.0267 0.3083 0.2280 0.076 Uiso 1.00 1 c R . . H(46) H 0.9585 0.3396 0.1948 0.076 Uiso 1.00 1 c R . . 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) 0.01559(12) 0.02282(14) 0.01886(13) -0.00018(11) 0.00057(9) -0.00254(11) Cl(1) 0.0540(17) 0.119(2) 0.0796(19) 0.0048(17) 0.0012(14) 0.0245(19) Cl(2) 0.085(2) 0.091(2) 0.0642(16) -0.0350(17) -0.0167(15) 0.0072(15) S(1) 0.0216(8) 0.0261(8) 0.0269(8) 0.0016(6) -0.0023(6) -0.0006(6) S(2) 0.0233(8) 0.0276(9) 0.0269(8) -0.0052(7) -0.0001(7) -0.0035(6) P(1) 0.0200(8) 0.0210(8) 0.0225(8) -0.0016(6) 0.0011(6) -0.0027(6) O(1) 0.034(3) 0.050(3) 0.031(2) 0.008(2) -0.002(2) 0.005(2) O(2) 0.023(2) 0.028(2) 0.045(3) 0.001(2) -0.008(2) -0.004(2) O(3) 0.028(2) 0.041(3) 0.049(3) -0.013(2) -0.009(2) -0.003(2) O(4) 0.035(3) 0.034(2) 0.028(2) -0.007(2) 0.003(2) 0.001(2) N(1) 0.022(2) 0.028(3) 0.023(2) 0.004(2) -0.003(2) 0.004(2) N(2) 0.024(2) 0.022(2) 0.024(2) -0.002(2) -0.002(2) -0.002(2) C(1) 0.023(3) 0.025(3) 0.026(3) 0.003(2) -0.004(2) 0.001(2) C(2) 0.036(4) 0.038(4) 0.042(4) 0.003(3) 0.003(3) 0.007(3) C(3) 0.052(5) 0.023(3) 0.053(5) 0.006(3) -0.001(4) 0.000(3) C(4) 0.039(4) 0.040(4) 0.036(4) 0.019(3) -0.005(3) -0.006(3) C(5) 0.023(4) 0.053(5) 0.051(5) 0.007(3) 0.008(3) 0.006(4) C(6) 0.028(3) 0.035(4) 0.045(4) 0.005(3) 0.000(3) 0.002(3) C(7) 0.059(6) 0.060(6) 0.069(6) 0.029(5) 0.004(5) -0.011(5) C(8) 0.040(4) 0.028(3) 0.030(3) -0.009(3) 0.011(3) -0.010(2) C(9) 0.078(7) 0.036(4) 0.036(4) -0.003(4) 0.013(4) -0.002(3) C(10) 0.129(11) 0.061(7) 0.044(5) -0.031(7) 0.036(6) -0.012(5) C(11) 0.093(9) 0.043(6) 0.105(10) -0.015(6) 0.058(8) -0.026(6) C(12) 0.047(6) 0.032(5) 0.107(8) -0.004(4) 0.021(5) -0.024(5) C(13) 0.033(4) 0.035(4) 0.057(5) 0.001(3) 0.009(3) -0.011(3) C(14) 0.208(18) 0.106(12) 0.168(15) 0.009(12) 0.156(14) -0.024(11) C(15) 0.019(3) 0.032(3) 0.029(3) 0.001(2) 0.006(2) -0.005(2) C(16) 0.024(3) 0.029(3) 0.029(3) 0.000(2) 0.007(2) -0.004(2) C(17) 0.024(3) 0.037(4) 0.024(3) 0.007(3) 0.006(2) -0.004(2) C(18) 0.022(3) 0.048(4) 0.026(3) 0.008(3) 0.007(2) -0.007(3) C(19) 0.015(2) 0.047(4) 0.025(3) -0.002(3) 0.007(2) -0.009(3) C(20) 0.038(4) 0.040(4) 0.051(4) -0.007(3) 0.007(4) 0.012(3) C(21) 0.033(4) 0.049(4) 0.025(3) 0.007(3) 0.001(3) -0.011(3) C(22) 0.043(4) 0.035(4) 0.047(4) 0.008(3) 0.011(3) -0.015(3) C(23) 0.028(4) 0.082(6) 0.030(4) 0.022(4) 0.004(3) 0.005(4) C(24) 0.018(3) 0.081(6) 0.047(4) -0.012(4) 0.009(3) -0.023(4) C(25) 0.022(3) 0.019(3) 0.032(3) -0.001(2) 0.004(2) -0.004(2) C(26) 0.027(3) 0.026(3) 0.036(3) 0.004(3) -0.002(3) -0.004(3) C(27) 0.039(4) 0.028(4) 0.042(4) 0.001(3) -0.005(3) -0.009(3) C(28) 0.052(5) 0.022(3) 0.056(5) -0.001(3) -0.013(4) -0.008(3) C(29) 0.044(5) 0.022(3) 0.064(5) -0.002(3) -0.001(4) -0.001(3) C(30) 0.035(4) 0.025(3) 0.040(4) -0.001(3) -0.000(3) -0.003(3) C(31) 0.021(3) 0.024(3) 0.024(3) -0.001(2) 0.006(2) -0.001(2) C(32) 0.021(3) 0.026(3) 0.036(3) -0.001(2) 0.002(2) -0.001(3) C(33) 0.036(4) 0.029(4) 0.038(4) 0.002(3) 0.004(3) -0.011(3) C(34) 0.021(3) 0.048(5) 0.047(4) 0.005(3) 0.012(3) -0.008(3) C(35) 0.025(4) 0.042(4) 0.051(4) -0.007(3) 0.016(3) -0.009(3) C(36) 0.026(3) 0.033(4) 0.041(4) -0.008(3) 0.007(3) -0.007(3) C(37) 0.026(3) 0.016(3) 0.032(3) -0.002(2) -0.005(2) -0.002(2) C(38) 0.067(6) 0.064(6) 0.032(4) 0.041(5) -0.003(4) -0.005(4) C(39) 0.104(9) 0.092(8) 0.029(4) 0.049(7) -0.003(5) -0.012(5) C(40) 0.084(7) 0.053(5) 0.035(4) 0.027(5) -0.019(4) -0.007(4) C(41) 0.035(4) 0.037(4) 0.042(4) 0.007(3) -0.007(3) 0.008(3) C(42) 0.033(4) 0.044(4) 0.034(4) 0.004(3) 0.003(3) -0.003(3) C(43) 0.049(6) 0.076(7) 0.066(6) -0.003(5) -0.011(5) -0.007(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) P(1) 2.3140(16) yes . . Ir(1) N(1) 2.130(5) yes . . Ir(1) N(2) 2.148(5) yes . . Ir(1) C(15) 2.237(6) yes . . Ir(1) C(16) 2.181(7) yes . . Ir(1) C(17) 2.220(7) yes . . Ir(1) C(18) 2.214(7) yes . . Ir(1) C(19) 2.238(6) yes . . Cl(1) C(43) 1.754(10) yes . . Cl(2) C(43) 1.733(10) yes . . S(1) O(1) 1.443(5) yes . . S(1) O(2) 1.446(4) yes . . S(1) N(1) 1.583(5) yes . . S(1) C(1) 1.770(7) yes . . S(2) O(3) 1.453(5) yes . . S(2) O(4) 1.436(4) yes . . S(2) N(2) 1.579(5) yes . . S(2) C(8) 1.776(7) yes . . P(1) C(25) 1.834(6) yes . . P(1) C(31) 1.842(6) yes . . P(1) C(37) 1.836(6) yes . . C(1) C(2) 1.400(10) yes . . C(1) C(6) 1.375(10) yes . . C(2) C(3) 1.379(11) yes . . C(3) C(4) 1.386(12) yes . . C(4) C(5) 1.373(12) yes . . C(4) C(7) 1.510(12) yes . . C(5) C(6) 1.399(11) yes . . C(8) C(9) 1.375(10) yes . . C(8) C(13) 1.374(11) yes . . C(9) C(10) 1.403(15) yes . . C(10) C(11) 1.376(19) yes . . C(11) C(12) 1.349(19) yes . . C(11) C(14) 1.54(2) yes . . C(12) C(13) 1.399(13) yes . . C(15) C(16) 1.454(9) yes . . C(15) C(19) 1.415(9) yes . . C(15) C(20) 1.500(10) yes . . C(16) C(17) 1.417(9) yes . . C(16) C(21) 1.506(9) yes . . C(17) C(18) 1.444(9) yes . . C(17) C(22) 1.501(10) yes . . C(18) C(19) 1.442(11) yes . . C(18) C(23) 1.494(10) yes . . C(19) C(24) 1.503(10) yes . . C(25) C(26) 1.395(9) yes . . C(25) C(30) 1.389(9) yes . . C(26) C(27) 1.369(10) yes . . C(27) C(28) 1.392(10) yes . . C(28) C(29) 1.372(12) yes . . C(29) C(30) 1.400(10) yes . . C(31) C(32) 1.399(9) yes . . C(31) C(36) 1.378(9) yes . . C(32) C(33) 1.378(10) yes . . C(33) C(34) 1.386(11) yes . . C(34) C(35) 1.376(12) yes . . C(35) C(36) 1.401(10) yes . . C(37) C(38) 1.386(10) yes . . C(37) C(42) 1.384(10) yes . . C(38) C(39) 1.393(13) yes . . C(39) C(40) 1.378(15) yes . . C(40) C(41) 1.348(11) yes . . C(41) C(42) 1.383(11) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(7) H(7) 0.950 no . . C(9) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(12) H(10) 0.950 no . . C(13) H(11) 0.950 no . . C(14) H(12) 0.950 no . . C(14) H(13) 0.950 no . . C(14) H(14) 0.950 no . . C(20) H(15) 0.950 no . . C(20) H(16) 0.950 no . . C(20) H(17) 0.950 no . . C(21) H(18) 0.950 no . . C(21) H(19) 0.950 no . . C(21) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(22) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(29) 0.950 no . . C(26) H(30) 0.950 no . . C(27) H(31) 0.950 no . . C(28) H(32) 0.950 no . . C(29) H(33) 0.950 no . . C(30) H(34) 0.950 no . . C(32) H(35) 0.950 no . . C(33) H(36) 0.950 no . . C(34) H(37) 0.950 no . . C(35) H(38) 0.950 no . . C(36) H(39) 0.950 no . . C(38) H(40) 0.950 no . . C(39) H(41) 0.950 no . . C(40) H(42) 0.950 no . . C(41) H(43) 0.950 no . . C(42) H(44) 0.950 no . . C(43) H(45) 0.950 no . . C(43) H(46) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 P(1) Ir(1) N(1) 90.65(15) yes . . . P(1) Ir(1) N(2) 85.99(14) yes . . . P(1) Ir(1) C(15) 157.03(18) yes . . . P(1) Ir(1) C(16) 118.71(19) yes . . . P(1) Ir(1) C(17) 99.49(18) yes . . . P(1) Ir(1) C(18) 113.1(2) yes . . . P(1) Ir(1) C(19) 149.75(19) yes . . . N(1) Ir(1) N(2) 84.0(2) yes . . . N(1) Ir(1) C(15) 93.6(2) yes . . . N(1) Ir(1) C(16) 102.4(2) yes . . . N(1) Ir(1) C(17) 138.0(2) yes . . . N(1) Ir(1) C(18) 155.9(2) yes . . . N(1) Ir(1) C(19) 119.2(2) yes . . . N(2) Ir(1) C(15) 116.9(2) yes . . . N(2) Ir(1) C(16) 154.0(2) yes . . . N(2) Ir(1) C(17) 137.0(2) yes . . . N(2) Ir(1) C(18) 100.7(2) yes . . . N(2) Ir(1) C(19) 91.8(2) yes . . . C(15) Ir(1) C(16) 38.4(2) yes . . . C(15) Ir(1) C(17) 63.0(2) yes . . . C(15) Ir(1) C(18) 63.2(2) yes . . . C(15) Ir(1) C(19) 36.9(2) yes . . . C(16) Ir(1) C(17) 37.6(2) yes . . . C(16) Ir(1) C(18) 63.7(2) yes . . . C(16) Ir(1) C(19) 62.9(2) yes . . . C(17) Ir(1) C(18) 38.0(2) yes . . . C(17) Ir(1) C(19) 62.6(2) yes . . . C(18) Ir(1) C(19) 37.8(2) yes . . . O(1) S(1) O(2) 116.0(3) yes . . . O(1) S(1) N(1) 113.9(3) yes . . . O(1) S(1) C(1) 105.0(3) yes . . . O(2) S(1) N(1) 109.6(2) yes . . . O(2) S(1) C(1) 107.5(3) yes . . . N(1) S(1) C(1) 103.9(3) yes . . . O(3) S(2) O(4) 117.7(3) yes . . . O(3) S(2) N(2) 110.5(3) yes . . . O(3) S(2) C(8) 104.5(3) yes . . . O(4) S(2) N(2) 110.2(2) yes . . . O(4) S(2) C(8) 106.1(3) yes . . . N(2) S(2) C(8) 107.1(3) yes . . . Ir(1) P(1) C(25) 116.8(2) yes . . . Ir(1) P(1) C(31) 120.0(2) yes . . . Ir(1) P(1) C(37) 110.5(2) yes . . . C(25) P(1) C(31) 101.9(3) yes . . . C(25) P(1) C(37) 104.2(3) yes . . . C(31) P(1) C(37) 101.4(3) yes . . . Ir(1) N(1) S(1) 127.1(3) yes . . . Ir(1) N(2) S(2) 128.4(3) yes . . . S(1) C(1) C(2) 120.3(5) yes . . . S(1) C(1) C(6) 120.2(5) yes . . . C(2) C(1) C(6) 119.6(6) yes . . . C(1) C(2) C(3) 119.7(7) yes . . . C(2) C(3) C(4) 121.6(7) yes . . . C(3) C(4) C(5) 117.9(7) yes . . . C(3) C(4) C(7) 120.7(7) yes . . . C(5) C(4) C(7) 121.4(7) yes . . . C(4) C(5) C(6) 121.9(7) yes . . . C(1) C(6) C(5) 119.4(7) yes . . . S(2) C(8) C(9) 119.8(6) yes . . . S(2) C(8) C(13) 120.1(5) yes . . . C(9) C(8) C(13) 120.1(7) yes . . . C(8) C(9) C(10) 118.3(8) yes . . . C(9) C(10) C(11) 121.7(10) yes . . . C(10) C(11) C(12) 119.0(11) yes . . . C(10) C(11) C(14) 117.6(12) yes . . . C(12) C(11) C(14) 123.4(12) yes . . . C(11) C(12) C(13) 120.6(9) yes . . . C(8) C(13) C(12) 120.2(8) yes . . . Ir(1) C(15) C(16) 68.7(3) yes . . . Ir(1) C(15) C(19) 71.6(3) yes . . . Ir(1) C(15) C(20) 126.6(5) yes . . . C(16) C(15) C(19) 107.0(6) yes . . . C(16) C(15) C(20) 127.2(6) yes . . . C(19) C(15) C(20) 125.8(6) yes . . . Ir(1) C(16) C(15) 72.9(3) yes . . . Ir(1) C(16) C(17) 72.7(3) yes . . . Ir(1) C(16) C(21) 130.1(4) yes . . . C(15) C(16) C(17) 108.4(5) yes . . . C(15) C(16) C(21) 124.4(6) yes . . . C(17) C(16) C(21) 126.0(6) yes . . . Ir(1) C(17) C(16) 69.8(4) yes . . . Ir(1) C(17) C(18) 70.8(4) yes . . . Ir(1) C(17) C(22) 132.8(5) yes . . . C(16) C(17) C(18) 108.2(6) yes . . . C(16) C(17) C(22) 125.9(6) yes . . . C(18) C(17) C(22) 125.2(6) yes . . . Ir(1) C(18) C(17) 71.2(3) yes . . . Ir(1) C(18) C(19) 72.0(3) yes . . . Ir(1) C(18) C(23) 133.6(5) yes . . . C(17) C(18) C(19) 106.8(6) yes . . . C(17) C(18) C(23) 127.6(7) yes . . . C(19) C(18) C(23) 123.8(6) yes . . . Ir(1) C(19) C(15) 71.5(3) yes . . . Ir(1) C(19) C(18) 70.2(3) yes . . . Ir(1) C(19) C(24) 127.5(5) yes . . . C(15) C(19) C(18) 109.3(6) yes . . . C(15) C(19) C(24) 125.5(6) yes . . . C(18) C(19) C(24) 125.1(6) yes . . . P(1) C(25) C(26) 117.3(5) yes . . . P(1) C(25) C(30) 122.8(5) yes . . . C(26) C(25) C(30) 119.8(6) yes . . . C(25) C(26) C(27) 119.5(6) yes . . . C(26) C(27) C(28) 121.3(7) yes . . . C(27) C(28) C(29) 119.5(7) yes . . . C(28) C(29) C(30) 120.0(7) yes . . . C(25) C(30) C(29) 119.9(7) yes . . . P(1) C(31) C(32) 118.9(5) yes . . . P(1) C(31) C(36) 121.8(5) yes . . . C(32) C(31) C(36) 119.0(6) yes . . . C(31) C(32) C(33) 120.1(6) yes . . . C(32) C(33) C(34) 120.7(7) yes . . . C(33) C(34) C(35) 119.5(7) yes . . . C(34) C(35) C(36) 120.1(7) yes . . . C(31) C(36) C(35) 120.5(6) yes . . . P(1) C(37) C(38) 123.6(5) yes . . . P(1) C(37) C(42) 118.8(5) yes . . . C(38) C(37) C(42) 117.6(6) yes . . . C(37) C(38) C(39) 119.9(8) yes . . . C(38) C(39) C(40) 121.0(8) yes . . . C(39) C(40) C(41) 119.3(8) yes . . . C(40) C(41) C(42) 120.4(7) yes . . . C(37) C(42) C(41) 121.8(7) yes . . . Cl(1) C(43) Cl(2) 113.8(6) yes . . . C(1) C(2) H(1) 120.0 no . . . C(3) C(2) H(1) 120.3 no . . . C(2) C(3) H(2) 119.1 no . . . C(4) C(3) H(2) 119.3 no . . . C(4) C(5) H(3) 119.1 no . . . C(6) C(5) H(3) 119.0 no . . . C(1) C(6) H(4) 120.3 no . . . C(5) C(6) H(4) 120.3 no . . . C(4) C(7) H(5) 109.0 no . . . C(4) C(7) H(6) 109.9 no . . . C(4) C(7) H(7) 109.5 no . . . H(5) C(7) H(6) 109.5 no . . . H(5) C(7) H(7) 109.5 no . . . H(6) C(7) H(7) 109.5 no . . . C(8) C(9) H(8) 120.9 no . . . C(10) C(9) H(8) 120.7 no . . . C(9) C(10) H(9) 119.2 no . . . C(11) C(10) H(9) 119.1 no . . . C(11) C(12) H(10) 119.6 no . . . C(13) C(12) H(10) 119.8 no . . . C(8) C(13) H(11) 120.1 no . . . C(12) C(13) H(11) 119.6 no . . . C(11) C(14) H(12) 109.1 no . . . C(11) C(14) H(13) 109.3 no . . . C(11) C(14) H(14) 110.0 no . . . H(12) C(14) H(13) 109.5 no . . . H(12) C(14) H(14) 109.5 no . . . H(13) C(14) H(14) 109.5 no . . . C(15) C(20) H(15) 109.5 no . . . C(15) C(20) H(16) 109.1 no . . . C(15) C(20) H(17) 109.8 no . . . H(15) C(20) H(16) 109.5 no . . . H(15) C(20) H(17) 109.5 no . . . H(16) C(20) H(17) 109.5 no . . . C(16) C(21) H(18) 109.4 no . . . C(16) C(21) H(19) 109.2 no . . . C(16) C(21) H(20) 109.8 no . . . H(18) C(21) H(19) 109.5 no . . . H(18) C(21) H(20) 109.5 no . . . H(19) C(21) H(20) 109.5 no . . . C(17) C(22) H(21) 109.4 no . . . C(17) C(22) H(22) 109.3 no . . . C(17) C(22) H(23) 109.7 no . . . H(21) C(22) H(22) 109.5 no . . . H(21) C(22) H(23) 109.5 no . . . H(22) C(22) H(23) 109.5 no . . . C(18) C(23) H(24) 108.6 no . . . C(18) C(23) H(25) 110.0 no . . . C(18) C(23) H(26) 109.8 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . C(19) C(24) H(27) 108.9 no . . . C(19) C(24) H(28) 109.9 no . . . C(19) C(24) H(29) 109.7 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(29) 109.5 no . . . H(28) C(24) H(29) 109.5 no . . . C(25) C(26) H(30) 120.4 no . . . C(27) C(26) H(30) 120.1 no . . . C(26) C(27) H(31) 119.4 no . . . C(28) C(27) H(31) 119.2 no . . . C(27) C(28) H(32) 120.3 no . . . C(29) C(28) H(32) 120.2 no . . . C(28) C(29) H(33) 119.9 no . . . C(30) C(29) H(33) 120.1 no . . . C(25) C(30) H(34) 120.1 no . . . C(29) C(30) H(34) 120.0 no . . . C(31) C(32) H(35) 119.9 no . . . C(33) C(32) H(35) 119.9 no . . . C(32) C(33) H(36) 119.6 no . . . C(34) C(33) H(36) 119.7 no . . . C(33) C(34) H(37) 120.3 no . . . C(35) C(34) H(37) 120.2 no . . . C(34) C(35) H(38) 119.8 no . . . C(36) C(35) H(38) 120.1 no . . . C(31) C(36) H(39) 119.9 no . . . C(35) C(36) H(39) 119.7 no . . . C(37) C(38) H(40) 120.1 no . . . C(39) C(38) H(40) 120.0 no . . . C(38) C(39) H(41) 119.2 no . . . C(40) C(39) H(41) 119.8 no . . . C(39) C(40) H(42) 120.1 no . . . C(41) C(40) H(42) 120.6 no . . . C(40) C(41) H(43) 119.9 no . . . C(42) C(41) H(43) 119.7 no . . . C(37) C(42) H(44) 118.9 no . . . C(41) C(42) H(44) 119.3 no . . . Cl(1) C(43) H(45) 108.1 no . . . Cl(1) C(43) H(46) 108.3 no . . . Cl(2) C(43) H(45) 108.3 no . . . Cl(2) C(43) H(46) 108.8 no . . . H(45) C(43) H(46) 109.5 no . . . #===END