Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_date '2002-01-20' _journal_coden_Cambridge 186 loop_ _publ_author_name 'Fusao Takagi' 'Hidetake Seino' 'Masanobu Hidai' 'Yasushi Mizobe' _publ_contact_author_name 'Dr Yasushu Mizobe' _publ_contact_author_address ; Institute of Industrial Science The University of Tokyo Komaba Meguro-ku Tokyo 153-8505 JAPAN ; _publ_contact_author_email 'ymizobe@iis.u-tokyo.ac.jp' _publ_contact_author_fax '+81-3-5452-6361' _publ_contact_author_phone '+81-3-5452-6360' _publ_requested_journal 'Dalton Transactions' # TITLE AND AUTHOR LIST _publ_section_title ; Nucleophilic addition and substitution reactions on the sulfur atoms bound to two Ir atoms. Conversion of a hydrosulfido complex [(eta5-C5Me5)2Ir2(mu-SH)3]Cl into a series of diiridium complexes with bridging thiolate ligands ; data_[(Cp*Ir)2(SCH2CH2SO2Ph)3]Cl.2MeCN_(4b.2MeCN) _database_code_CSD 178526 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Feb 24 15:10:08 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1376.29 _chemical_formula_analytical ? _chemical_formula_sum 'C48 H63 Cl Ir2 N2 O6 S6 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.943(2) _cell_length_b 22.055(2) _cell_length_c 20.508(2) _cell_angle_alpha 90 _cell_angle_beta 90.01(1) _cell_angle_gamma 90 _cell_volume 5401(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.2 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'lemon yellow' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720.00 _exptl_absorpt_coefficient_mu 5.263 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 2 1 1 3 1 3 -2 _diffrn_reflns_number 12996 _reflns_number_total 12409 _reflns_number_gt 7996 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_sigmaI/netI 0.055 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01651 _diffrn_orient_matrix_UB_12 0.04444 _diffrn_orient_matrix_UB_13 -0.00077 _diffrn_orient_matrix_UB_21 -0.07155 _diffrn_orient_matrix_UB_22 0.00815 _diffrn_orient_matrix_UB_23 0.02376 _diffrn_orient_matrix_UB_31 0.04024 _diffrn_orient_matrix_UB_32 -0.00375 _diffrn_orient_matrix_UB_33 0.04257 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.04782(2) 0.22056(1) 0.45025(1) 0.03564(7) Uani 1.00 d . . . Ir(2) Ir 0.21600(2) 0.31968(1) 0.37670(1) 0.03640(7) Uani 1.00 d . . . Cl Cl 0.3590(2) 0.0582(1) 0.5900(1) 0.0936(9) Uani 1.00 d . . . S(1) S 0.0671(1) 0.25512(8) 0.33993(8) 0.0397(5) Uani 1.00 d . . . S(2) S 0.2511(2) 0.1110(1) 0.2340(1) 0.0724(8) Uani 1.00 d . . . S(3) S 0.0776(1) 0.32756(8) 0.46006(8) 0.0393(5) Uani 1.00 d . . . S(4) S -0.2300(1) 0.43310(9) 0.4252(1) 0.0541(6) Uani 1.00 d . . . S(5) S 0.2467(1) 0.22897(8) 0.43852(8) 0.0385(4) Uani 1.00 d . . . S(6) S 0.4935(2) 0.2441(1) 0.59479(10) 0.0597(6) Uani 1.00 d . . . O(1) O 0.2747(6) 0.1416(3) 0.1768(4) 0.100(3) Uani 1.00 d . . . O(2) O 0.3364(5) 0.0763(3) 0.2642(3) 0.092(2) Uani 1.00 d . . . O(3) O -0.2977(4) 0.4627(3) 0.4740(3) 0.074(2) Uani 1.00 d . . . O(4) O -0.2806(4) 0.3889(2) 0.3828(3) 0.071(2) Uani 1.00 d . . . O(5) O 0.5216(5) 0.3050(3) 0.5770(3) 0.081(2) Uani 1.00 d . . . O(6) O 0.5816(4) 0.2024(3) 0.6109(3) 0.084(2) Uani 1.00 d . . . N(1) N 0.5493(8) 0.1529(4) 0.3606(4) 0.102(4) Uani 1.00 d . . . N(2) N 0.8331(8) 0.0693(4) 0.6004(4) 0.100(4) Uani 1.00 d . . . C(1) C -0.0716(6) 0.2070(3) 0.5293(3) 0.050(2) Uani 1.00 d . . . C(2) C 0.0197(6) 0.1669(3) 0.5383(4) 0.055(2) Uani 1.00 d . . . C(3) C 0.0221(6) 0.1268(3) 0.4825(4) 0.054(2) Uani 1.00 d . . . C(4) C -0.0684(6) 0.1439(3) 0.4409(4) 0.056(2) Uani 1.00 d . . . C(5) C -0.1245(6) 0.1948(3) 0.4685(4) 0.050(2) Uani 1.00 d . . . C(6) C -0.1088(7) 0.2546(4) 0.5783(4) 0.075(3) Uani 1.00 d . . . C(7) C 0.0921(7) 0.1603(4) 0.5983(4) 0.077(3) Uani 1.00 d . . . C(8) C 0.0984(8) 0.0741(4) 0.4733(5) 0.080(3) Uani 1.00 d . . . C(9) C -0.1048(8) 0.1121(4) 0.3801(5) 0.090(4) Uani 1.00 d . . . C(10) C -0.2300(6) 0.2245(4) 0.4448(5) 0.079(3) Uani 1.00 d . . . C(11) C 0.2472(6) 0.4171(3) 0.3606(3) 0.044(2) Uani 1.00 d . . . C(12) C 0.2310(7) 0.3879(3) 0.2994(3) 0.058(2) Uani 1.00 d . . . C(13) C 0.3152(7) 0.3439(4) 0.2916(4) 0.066(3) Uani 1.00 d . . . C(14) C 0.3868(6) 0.3447(3) 0.3497(4) 0.061(3) Uani 1.00 d . . . C(15) C 0.3427(6) 0.3894(3) 0.3930(4) 0.049(2) Uani 1.00 d . . . C(16) C 0.1825(7) 0.4697(4) 0.3856(4) 0.063(3) Uani 1.00 d . . . C(17) C 0.1446(9) 0.4031(4) 0.2491(4) 0.090(4) Uani 1.00 d . . . C(18) C 0.339(1) 0.3068(5) 0.2320(5) 0.125(5) Uani 1.00 d . . . C(19) C 0.4889(7) 0.3087(4) 0.3622(6) 0.107(4) Uani 1.00 d . . . C(20) C 0.3908(7) 0.4111(4) 0.4559(4) 0.067(3) Uani 1.00 d . . . C(21) C 0.1126(6) 0.1980(4) 0.2826(4) 0.066(3) Uani 1.00 d . . . C(22) C 0.2055(7) 0.1618(4) 0.3009(4) 0.068(3) Uani 1.00 d . . . C(23) C 0.1352(6) 0.0632(3) 0.2195(4) 0.058(2) Uani 1.00 d . . . C(24) C 0.1140(7) 0.0194(4) 0.2656(4) 0.066(3) Uani 1.00 d . . . C(25) C 0.0257(9) -0.0196(4) 0.2557(6) 0.087(4) Uani 1.00 d . . . C(26) C -0.0362(9) -0.0140(5) 0.2011(7) 0.107(5) Uani 1.00 d . . . C(27) C -0.0158(9) 0.0290(5) 0.1546(6) 0.106(5) Uani 1.00 d . . . C(28) C 0.0712(8) 0.0693(4) 0.1631(5) 0.077(3) Uani 1.00 d . . . C(29) C -0.0431(6) 0.3654(3) 0.4183(3) 0.051(2) Uani 1.00 d . . . C(30) C -0.1164(6) 0.3975(3) 0.4663(4) 0.055(2) Uani 1.00 d . . . C(31) C -0.1676(5) 0.4887(3) 0.3755(4) 0.051(2) Uani 1.00 d . . . C(32) C -0.1371(7) 0.5440(4) 0.4039(4) 0.068(3) Uani 1.00 d . . . C(33) C -0.0900(8) 0.5875(4) 0.3652(6) 0.086(4) Uani 1.00 d . . . C(34) C -0.0713(8) 0.5774(5) 0.3008(6) 0.095(4) Uani 1.00 d . . . C(35) C -0.1024(8) 0.5240(5) 0.2708(5) 0.088(4) Uani 1.00 d . . . C(36) C -0.1495(7) 0.4796(4) 0.3095(4) 0.073(3) Uani 1.00 d . . . C(37) C 0.3095(5) 0.2516(3) 0.5169(3) 0.048(2) Uani 1.00 d . . . C(38) C 0.4127(6) 0.2125(3) 0.5300(3) 0.050(2) Uani 1.00 d . . . C(39) C 0.3970(6) 0.2474(4) 0.6603(3) 0.053(2) Uani 1.00 d . . . C(40) C 0.3622(8) 0.1938(4) 0.6908(4) 0.070(3) Uani 1.00 d . . . C(41) C 0.2830(9) 0.1983(5) 0.7394(5) 0.087(4) Uani 1.00 d . . . C(42) C 0.2428(9) 0.2541(7) 0.7586(5) 0.097(4) Uani 1.00 d . . . C(43) C 0.2770(8) 0.3048(5) 0.7283(5) 0.088(4) Uani 1.00 d . . . C(44) C 0.3535(7) 0.3027(4) 0.6790(4) 0.068(3) Uani 1.00 d . . . C(45) C 0.4986(8) 0.1151(4) 0.3810(4) 0.067(3) Uani 1.00 d . . . C(46) C 0.4376(8) 0.0645(4) 0.4083(5) 0.088(4) Uani 1.00 d . . . C(47) C 0.7565(9) 0.0716(4) 0.5678(5) 0.070(3) Uani 1.00 d . . . C(48) C 0.6620(8) 0.0746(4) 0.5261(5) 0.083(3) Uani 1.00 d . . . H(1) H -0.0492 0.2824 0.5857 0.0897 Uiso 1.00 calc . . . H(2) H -0.1718 0.2758 0.5616 0.0897 Uiso 1.00 calc . . . H(3) H -0.1282 0.2355 0.6182 0.0897 Uiso 1.00 calc . . . H(4) H 0.0469 0.1484 0.6342 0.0946 Uiso 1.00 calc . . . H(5) H 0.1476 0.1303 0.5906 0.0946 Uiso 1.00 calc . . . H(6) H 0.1272 0.1979 0.6078 0.0946 Uiso 1.00 calc . . . H(7) H 0.0559 0.0376 0.4728 0.0963 Uiso 1.00 calc . . . H(8) H 0.1371 0.0782 0.4330 0.0963 Uiso 1.00 calc . . . H(9) H 0.1509 0.0727 0.5080 0.0963 Uiso 1.00 calc . . . H(10) H -0.1781 0.0962 0.3860 0.1080 Uiso 1.00 calc . . . H(11) H -0.1047 0.1397 0.3447 0.1080 Uiso 1.00 calc . . . H(12) H -0.0545 0.0796 0.3710 0.1080 Uiso 1.00 calc . . . H(13) H -0.2185 0.2669 0.4413 0.0968 Uiso 1.00 calc . . . H(14) H -0.2494 0.2084 0.4033 0.0968 Uiso 1.00 calc . . . H(15) H -0.2888 0.2167 0.4749 0.0968 Uiso 1.00 calc . . . H(16) H 0.2098 0.4809 0.4274 0.0759 Uiso 1.00 calc . . . H(17) H 0.1909 0.5031 0.3565 0.0759 Uiso 1.00 calc . . . H(18) H 0.1056 0.4593 0.3887 0.0759 Uiso 1.00 calc . . . H(19) H 0.0968 0.4337 0.2651 0.1081 Uiso 1.00 calc . . . H(20) H 0.1808 0.4166 0.2105 0.1081 Uiso 1.00 calc . . . H(21) H 0.1019 0.3676 0.2395 0.1081 Uiso 1.00 calc . . . H(22) H 0.3411 0.2647 0.2438 0.1516 Uiso 1.00 calc . . . H(23) H 0.2833 0.3129 0.2002 0.1516 Uiso 1.00 calc . . . H(24) H 0.4105 0.3176 0.2147 0.1516 Uiso 1.00 calc . . . H(25) H 0.4789 0.2855 0.4010 0.1288 Uiso 1.00 calc . . . H(26) H 0.5015 0.2818 0.3266 0.1288 Uiso 1.00 calc . . . H(27) H 0.5512 0.3347 0.3672 0.1288 Uiso 1.00 calc . . . H(28) H 0.4518 0.3860 0.4681 0.0797 Uiso 1.00 calc . . . H(29) H 0.4165 0.4517 0.4508 0.0797 Uiso 1.00 calc . . . H(30) H 0.3349 0.4099 0.4888 0.0797 Uiso 1.00 calc . . . H(31) H 0.0514 0.1709 0.2757 0.0788 Uiso 1.00 calc . . . H(32) H 0.1309 0.2175 0.2430 0.0788 Uiso 1.00 calc . . . H(33) H 0.1859 0.1383 0.3376 0.0816 Uiso 1.00 calc . . . H(34) H 0.2659 0.1882 0.3119 0.0816 Uiso 1.00 calc . . . H(35) H 0.1594 0.0162 0.3034 0.0798 Uiso 1.00 calc . . . H(36) H 0.0088 -0.0502 0.2870 0.1034 Uiso 1.00 calc . . . H(37) H -0.0968 -0.0414 0.1947 0.1278 Uiso 1.00 calc . . . H(38) H -0.0613 0.0310 0.1167 0.1286 Uiso 1.00 calc . . . H(39) H 0.0866 0.1000 0.1318 0.0912 Uiso 1.00 calc . . . H(40) H -0.0152 0.3937 0.3876 0.0609 Uiso 1.00 calc . . . H(41) H -0.0862 0.3354 0.3963 0.0609 Uiso 1.00 calc . . . H(42) H -0.0736 0.4276 0.4884 0.0665 Uiso 1.00 calc . . . H(43) H -0.1448 0.3693 0.4970 0.0665 Uiso 1.00 calc . . . H(44) H -0.1493 0.5514 0.4491 0.0830 Uiso 1.00 calc . . . H(45) H -0.0695 0.6252 0.3839 0.1021 Uiso 1.00 calc . . . H(46) H -0.0358 0.6081 0.2757 0.1116 Uiso 1.00 calc . . . H(47) H -0.0916 0.5181 0.2254 0.1059 Uiso 1.00 calc . . . H(48) H -0.1700 0.4420 0.2904 0.0870 Uiso 1.00 calc . . . H(49) H 0.3310 0.2931 0.5150 0.0577 Uiso 1.00 calc . . . H(50) H 0.2565 0.2462 0.5510 0.0577 Uiso 1.00 calc . . . H(51) H 0.4572 0.2103 0.4917 0.0592 Uiso 1.00 calc . . . H(52) H 0.3893 0.1726 0.5419 0.0592 Uiso 1.00 calc . . . H(53) H 0.3921 0.1558 0.6785 0.0835 Uiso 1.00 calc . . . H(54) H 0.2560 0.1630 0.7600 0.1051 Uiso 1.00 calc . . . H(55) H 0.1903 0.2562 0.7934 0.1167 Uiso 1.00 calc . . . H(56) H 0.2475 0.3432 0.7415 0.1048 Uiso 1.00 calc . . . H(57) H 0.3768 0.3391 0.6577 0.0820 Uiso 1.00 calc . . . H(58) H 0.3596 0.0726 0.4065 0.1057 Uiso 1.00 calc . . . H(59) H 0.4535 0.0288 0.3838 0.1057 Uiso 1.00 calc . . . H(60) H 0.4596 0.0585 0.4523 0.1057 Uiso 1.00 calc . . . H(61) H 0.6532 0.1149 0.5107 0.1012 Uiso 1.00 calc . . . H(62) H 0.6727 0.0481 0.4901 0.1012 Uiso 1.00 calc . . . H(63) H 0.5970 0.0627 0.5495 0.1012 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0291(1) 0.0418(2) 0.0360(1) -0.0021(1) 0.00274(10) 0.0028(1) Ir(2) 0.0320(1) 0.0418(2) 0.0354(1) -0.0066(1) 0.00733(10) -0.0069(1) Cl 0.097(2) 0.071(2) 0.113(2) 0.021(1) -0.001(2) -0.008(1) S(1) 0.0367(9) 0.049(1) 0.0330(9) -0.0060(7) 0.0002(7) -0.0021(7) S(2) 0.048(1) 0.061(1) 0.109(2) -0.005(1) 0.016(1) -0.032(1) S(3) 0.0350(8) 0.0440(10) 0.0390(9) 0.0021(7) 0.0080(7) -0.0051(7) S(4) 0.0393(10) 0.049(1) 0.074(1) 0.0045(8) 0.0037(9) -0.0015(10) S(5) 0.0310(8) 0.049(1) 0.0351(8) 0.0025(7) -0.0005(6) -0.0060(7) S(6) 0.043(1) 0.084(2) 0.052(1) 0.001(1) -0.0147(9) -0.006(1) O(1) 0.097(5) 0.093(5) 0.111(6) 0.006(4) 0.002(4) 0.014(5) O(2) 0.046(3) 0.128(6) 0.103(5) 0.008(4) -0.007(3) -0.042(4) O(3) 0.067(4) 0.072(4) 0.084(4) 0.018(3) 0.025(3) -0.001(3) O(4) 0.053(3) 0.058(3) 0.101(4) -0.007(3) -0.014(3) -0.010(3) O(5) 0.075(4) 0.087(4) 0.080(4) -0.037(3) -0.014(3) 0.001(3) O(6) 0.051(3) 0.127(5) 0.073(4) 0.030(3) -0.021(3) -0.005(4) N(1) 0.120(8) 0.079(6) 0.107(7) -0.028(5) 0.004(6) -0.005(5) N(2) 0.100(7) 0.107(7) 0.093(7) -0.002(6) 0.002(5) 0.010(5) C(1) 0.052(4) 0.052(5) 0.047(4) -0.004(3) 0.020(3) 0.014(3) C(2) 0.048(4) 0.063(5) 0.053(5) -0.003(4) 0.005(3) 0.012(4) C(3) 0.050(4) 0.039(4) 0.073(5) -0.004(3) 0.009(4) 0.013(4) C(4) 0.045(4) 0.054(5) 0.068(5) -0.020(4) 0.006(4) 0.005(4) C(5) 0.037(4) 0.052(5) 0.060(5) -0.011(3) 0.001(3) 0.012(4) C(6) 0.087(6) 0.083(6) 0.055(5) 0.013(5) 0.036(5) 0.019(5) C(7) 0.061(5) 0.110(8) 0.059(5) 0.006(5) -0.001(4) 0.036(5) C(8) 0.088(7) 0.043(5) 0.109(8) 0.004(4) 0.024(6) 0.011(5) C(9) 0.083(7) 0.080(7) 0.107(8) -0.033(5) 0.005(6) -0.013(6) C(10) 0.039(4) 0.098(7) 0.100(7) 0.002(4) 0.002(4) 0.032(6) C(11) 0.044(4) 0.045(4) 0.044(4) -0.005(3) 0.003(3) 0.001(3) C(12) 0.082(6) 0.052(5) 0.039(4) -0.027(4) 0.016(4) 0.002(4) C(13) 0.074(6) 0.069(6) 0.055(5) -0.036(5) 0.030(4) -0.023(4) C(14) 0.037(4) 0.043(4) 0.104(7) -0.020(3) 0.034(4) -0.012(4) C(15) 0.044(4) 0.044(4) 0.059(5) -0.010(3) 0.004(3) -0.011(4) C(16) 0.066(5) 0.062(5) 0.063(5) 0.005(4) 0.001(4) 0.006(4) C(17) 0.134(9) 0.092(7) 0.044(5) -0.046(6) -0.009(5) 0.017(5) C(18) 0.18(1) 0.100(8) 0.100(8) -0.067(8) 0.095(8) -0.051(6) C(19) 0.045(5) 0.048(6) 0.23(1) -0.001(4) 0.048(7) -0.009(7) C(20) 0.062(5) 0.059(5) 0.080(6) -0.013(4) -0.016(4) -0.003(4) C(21) 0.052(5) 0.061(5) 0.085(6) -0.015(4) 0.005(4) -0.027(4) C(22) 0.080(6) 0.058(5) 0.066(6) -0.012(5) -0.011(5) -0.013(4) C(23) 0.045(4) 0.044(5) 0.084(6) 0.006(3) -0.014(4) -0.020(4) C(24) 0.077(6) 0.052(5) 0.069(6) 0.002(4) -0.004(5) -0.016(4) C(25) 0.087(7) 0.058(6) 0.116(9) -0.010(5) 0.005(6) 0.000(6) C(26) 0.069(7) 0.077(8) 0.18(1) 0.002(6) -0.031(8) -0.033(8) C(27) 0.090(8) 0.087(8) 0.14(1) 0.013(7) -0.072(8) -0.018(7) C(28) 0.072(6) 0.059(6) 0.100(7) 0.017(5) -0.012(5) -0.001(5) C(29) 0.042(4) 0.054(5) 0.056(5) 0.012(3) 0.003(3) -0.003(4) C(30) 0.050(4) 0.050(5) 0.066(5) 0.003(4) 0.012(4) -0.002(4) C(31) 0.035(4) 0.062(5) 0.057(5) 0.005(3) 0.001(3) -0.002(4) C(32) 0.066(6) 0.063(6) 0.076(6) -0.010(4) -0.006(5) 0.008(5) C(33) 0.089(7) 0.068(6) 0.101(8) -0.016(5) -0.006(6) 0.013(6) C(34) 0.054(6) 0.099(8) 0.13(1) 0.005(6) 0.014(6) 0.047(8) C(35) 0.091(8) 0.102(8) 0.070(6) 0.016(6) 0.019(5) 0.026(6) C(36) 0.068(6) 0.077(6) 0.074(6) 0.005(5) 0.003(5) -0.003(5) C(37) 0.041(4) 0.063(5) 0.040(4) 0.008(3) -0.006(3) -0.009(3) C(38) 0.043(4) 0.061(5) 0.044(4) 0.000(3) -0.007(3) -0.012(4) C(39) 0.054(4) 0.066(5) 0.039(4) 0.010(4) -0.021(3) -0.013(4) C(40) 0.091(7) 0.063(6) 0.055(5) 0.012(5) -0.009(5) 0.012(4) C(41) 0.091(8) 0.111(9) 0.060(6) -0.010(6) -0.004(5) 0.014(6) C(42) 0.086(8) 0.15(1) 0.055(6) 0.010(8) 0.006(5) -0.017(7) C(43) 0.074(7) 0.101(8) 0.088(8) 0.022(6) -0.002(6) -0.023(6) C(44) 0.061(5) 0.070(6) 0.073(6) 0.008(4) -0.012(4) -0.005(5) C(45) 0.080(6) 0.060(6) 0.060(6) 0.003(5) -0.008(5) -0.012(5) C(46) 0.091(7) 0.086(7) 0.088(7) -0.003(6) -0.006(6) 0.010(6) C(47) 0.084(7) 0.057(6) 0.070(6) -0.003(5) 0.014(5) 0.009(5) C(48) 0.082(7) 0.074(7) 0.093(7) -0.007(5) -0.006(6) 0.012(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00047(7) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7996 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0364 _refine_ls_wR_factor_gt 0.0364 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.349 _refine_ls_shift/su_max 0.0300 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -1.34 _refine_diff_density_max 1.59 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) S(1) 2.398(2) 1_555 1_555 yes Ir(1) S(3) 2.395(2) 1_555 1_555 yes Ir(1) S(5) 2.395(2) 1_555 1_555 yes Ir(1) C(1) 2.179(6) 1_555 1_555 yes Ir(1) C(2) 2.185(7) 1_555 1_555 yes Ir(1) C(3) 2.193(7) 1_555 1_555 yes Ir(1) C(4) 2.196(7) 1_555 1_555 yes Ir(1) C(5) 2.167(6) 1_555 1_555 yes Ir(2) S(1) 2.400(2) 1_555 1_555 yes Ir(2) S(3) 2.384(2) 1_555 1_555 yes Ir(2) S(5) 2.397(2) 1_555 1_555 yes Ir(2) C(11) 2.205(7) 1_555 1_555 yes Ir(2) C(12) 2.193(7) 1_555 1_555 yes Ir(2) C(13) 2.177(7) 1_555 1_555 yes Ir(2) C(14) 2.184(6) 1_555 1_555 yes Ir(2) C(15) 2.183(6) 1_555 1_555 yes S(1) C(21) 1.807(8) 1_555 1_555 yes S(2) O(1) 1.381(7) 1_555 1_555 yes S(2) O(2) 1.417(6) 1_555 1_555 yes S(2) C(22) 1.854(8) 1_555 1_555 yes S(2) C(23) 1.765(7) 1_555 1_555 yes S(3) C(29) 1.873(7) 1_555 1_555 yes S(4) O(3) 1.444(5) 1_555 1_555 yes S(4) O(4) 1.439(5) 1_555 1_555 yes S(4) C(30) 1.780(8) 1_555 1_555 yes S(4) C(31) 1.759(8) 1_555 1_555 yes S(5) C(37) 1.843(6) 1_555 1_555 yes S(6) O(5) 1.432(6) 1_555 1_555 yes S(6) O(6) 1.436(6) 1_555 1_555 yes S(6) C(38) 1.783(7) 1_555 1_555 yes S(6) C(39) 1.771(8) 1_555 1_555 yes N(1) C(45) 1.11(1) 1_555 1_555 yes N(2) C(47) 1.13(1) 1_555 1_555 yes C(1) C(2) 1.416(10) 1_555 1_555 yes C(1) C(5) 1.423(10) 1_555 1_555 yes C(1) C(6) 1.52(1) 1_555 1_555 yes C(2) C(3) 1.45(1) 1_555 1_555 yes C(2) C(7) 1.51(1) 1_555 1_555 yes C(3) C(4) 1.427(10) 1_555 1_555 yes C(3) C(8) 1.49(1) 1_555 1_555 yes C(4) C(5) 1.42(1) 1_555 1_555 yes C(4) C(9) 1.50(1) 1_555 1_555 yes C(5) C(10) 1.500(10) 1_555 1_555 yes C(11) C(12) 1.423(9) 1_555 1_555 yes C(11) C(15) 1.453(9) 1_555 1_555 yes C(11) C(16) 1.49(1) 1_555 1_555 yes C(12) C(13) 1.41(1) 1_555 1_555 yes C(12) C(17) 1.50(1) 1_555 1_555 yes C(13) C(14) 1.47(1) 1_555 1_555 yes C(13) C(18) 1.50(1) 1_555 1_555 yes C(14) C(15) 1.428(9) 1_555 1_555 yes C(14) C(19) 1.48(1) 1_555 1_555 yes C(15) C(20) 1.491(10) 1_555 1_555 yes C(21) C(22) 1.42(1) 1_555 1_555 yes C(23) C(24) 1.38(1) 1_555 1_555 yes C(23) C(28) 1.39(1) 1_555 1_555 yes C(24) C(25) 1.38(1) 1_555 1_555 yes C(25) C(26) 1.35(1) 1_555 1_555 yes C(26) C(27) 1.37(2) 1_555 1_555 yes C(27) C(28) 1.38(1) 1_555 1_555 yes C(29) C(30) 1.495(9) 1_555 1_555 yes C(31) C(32) 1.40(1) 1_555 1_555 yes C(31) C(36) 1.39(1) 1_555 1_555 yes C(32) C(33) 1.37(1) 1_555 1_555 yes C(33) C(34) 1.36(1) 1_555 1_555 yes C(34) C(35) 1.38(1) 1_555 1_555 yes C(35) C(36) 1.38(1) 1_555 1_555 yes C(37) C(38) 1.528(9) 1_555 1_555 yes C(39) C(40) 1.40(1) 1_555 1_555 yes C(39) C(44) 1.38(1) 1_555 1_555 yes C(40) C(41) 1.38(1) 1_555 1_555 yes C(41) C(42) 1.38(1) 1_555 1_555 yes C(42) C(43) 1.34(1) 1_555 1_555 yes C(43) C(44) 1.36(1) 1_555 1_555 yes C(45) C(46) 1.45(1) 1_555 1_555 yes C(47) C(48) 1.42(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(3) 75.63(6) 1_555 1_555 1_555 yes S(1) Ir(1) S(5) 77.61(5) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 143.9(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 165.1(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 126.7(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 102.9(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 109.7(2) 1_555 1_555 1_555 yes S(3) Ir(1) S(5) 77.57(5) 1_555 1_555 1_555 yes S(3) Ir(1) C(1) 99.8(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(2) 119.2(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(3) 157.6(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(4) 149.3(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(5) 112.6(2) 1_555 1_555 1_555 yes S(5) Ir(1) C(1) 137.3(2) 1_555 1_555 1_555 yes S(5) Ir(1) C(2) 106.1(2) 1_555 1_555 1_555 yes S(5) Ir(1) C(3) 104.0(2) 1_555 1_555 1_555 yes S(5) Ir(1) C(4) 132.7(2) 1_555 1_555 1_555 yes S(5) Ir(1) C(5) 168.4(2) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 37.9(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 63.6(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 63.0(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 38.2(3) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 38.6(3) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 63.8(3) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 64.5(3) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 38.0(3) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 64.4(3) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38.1(3) 1_555 1_555 1_555 yes S(1) Ir(2) S(3) 75.80(6) 1_555 1_555 1_555 yes S(1) Ir(2) S(5) 77.55(6) 1_555 1_555 1_555 yes S(1) Ir(2) C(11) 131.0(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(12) 104.0(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(13) 107.3(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(14) 139.6(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(15) 168.4(2) 1_555 1_555 1_555 yes S(3) Ir(2) S(5) 77.75(5) 1_555 1_555 1_555 yes S(3) Ir(2) C(11) 98.8(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(12) 121.7(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(13) 159.2(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(14) 144.2(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(15) 108.6(2) 1_555 1_555 1_555 yes S(5) Ir(2) C(11) 150.0(2) 1_555 1_555 1_555 yes S(5) Ir(2) C(12) 160.5(2) 1_555 1_555 1_555 yes S(5) Ir(2) C(13) 123.1(3) 1_555 1_555 1_555 yes S(5) Ir(2) C(14) 101.7(2) 1_555 1_555 1_555 yes S(5) Ir(2) C(15) 113.7(2) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 37.8(2) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 63.2(3) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 63.8(3) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 38.7(2) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 37.6(3) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 64.3(3) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 64.5(3) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 39.3(3) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 64.7(3) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38.2(3) 1_555 1_555 1_555 yes Ir(1) S(1) Ir(2) 87.90(5) 1_555 1_555 1_555 yes Ir(1) S(1) C(21) 114.9(3) 1_555 1_555 1_555 yes Ir(2) S(1) C(21) 113.3(2) 1_555 1_555 1_555 yes O(1) S(2) O(2) 119.2(4) 1_555 1_555 1_555 yes O(1) S(2) C(22) 113.1(4) 1_555 1_555 1_555 yes O(1) S(2) C(23) 108.0(4) 1_555 1_555 1_555 yes O(2) S(2) C(22) 102.4(4) 1_555 1_555 1_555 yes O(2) S(2) C(23) 108.3(4) 1_555 1_555 1_555 yes C(22) S(2) C(23) 104.8(4) 1_555 1_555 1_555 yes Ir(1) S(3) Ir(2) 88.34(5) 1_555 1_555 1_555 yes Ir(1) S(3) C(29) 106.6(2) 1_555 1_555 1_555 yes Ir(2) S(3) C(29) 103.8(2) 1_555 1_555 1_555 yes O(3) S(4) O(4) 119.4(3) 1_555 1_555 1_555 yes O(3) S(4) C(30) 107.3(3) 1_555 1_555 1_555 yes O(3) S(4) C(31) 108.8(3) 1_555 1_555 1_555 yes O(4) S(4) C(30) 107.9(3) 1_555 1_555 1_555 yes O(4) S(4) C(31) 107.5(4) 1_555 1_555 1_555 yes C(30) S(4) C(31) 105.0(3) 1_555 1_555 1_555 yes Ir(1) S(5) Ir(2) 88.04(5) 1_555 1_555 1_555 yes Ir(1) S(5) C(37) 109.7(2) 1_555 1_555 1_555 yes Ir(2) S(5) C(37) 107.3(2) 1_555 1_555 1_555 yes O(5) S(6) O(6) 119.2(4) 1_555 1_555 1_555 yes O(5) S(6) C(38) 107.7(3) 1_555 1_555 1_555 yes O(5) S(6) C(39) 107.9(4) 1_555 1_555 1_555 yes O(6) S(6) C(38) 108.5(4) 1_555 1_555 1_555 yes O(6) S(6) C(39) 109.2(4) 1_555 1_555 1_555 yes C(38) S(6) C(39) 103.2(3) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 71.3(4) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 70.4(4) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 126.1(5) 1_555 1_555 1_555 yes C(2) C(1) C(5) 109.7(7) 1_555 1_555 1_555 yes C(2) C(1) C(6) 124.8(7) 1_555 1_555 1_555 yes C(5) C(1) C(6) 125.5(7) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 70.8(4) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 71.0(4) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 129.6(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 107.1(7) 1_555 1_555 1_555 yes C(1) C(2) C(7) 127.4(7) 1_555 1_555 1_555 yes C(3) C(2) C(7) 125.1(7) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 70.4(4) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 71.1(4) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 127.8(5) 1_555 1_555 1_555 yes C(2) C(3) C(4) 107.2(7) 1_555 1_555 1_555 yes C(2) C(3) C(8) 126.1(8) 1_555 1_555 1_555 yes C(4) C(3) C(8) 126.5(8) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 70.9(4) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 69.9(4) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 128.1(6) 1_555 1_555 1_555 yes C(3) C(4) C(5) 109.1(7) 1_555 1_555 1_555 yes C(3) C(4) C(9) 126.4(8) 1_555 1_555 1_555 yes C(5) C(4) C(9) 124.4(7) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 71.3(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 72.0(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 128.8(5) 1_555 1_555 1_555 yes C(1) C(5) C(4) 106.7(6) 1_555 1_555 1_555 yes C(1) C(5) C(10) 125.0(7) 1_555 1_555 1_555 yes C(4) C(5) C(10) 127.6(7) 1_555 1_555 1_555 yes Ir(2) C(11) C(12) 70.7(4) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 69.8(4) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 128.5(5) 1_555 1_555 1_555 yes C(12) C(11) C(15) 108.6(6) 1_555 1_555 1_555 yes C(12) C(11) C(16) 125.9(7) 1_555 1_555 1_555 yes C(15) C(11) C(16) 125.3(6) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 71.6(4) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 70.6(4) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 126.5(5) 1_555 1_555 1_555 yes C(11) C(12) C(13) 108.4(7) 1_555 1_555 1_555 yes C(11) C(12) C(17) 126.9(8) 1_555 1_555 1_555 yes C(13) C(12) C(17) 124.5(8) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 71.8(4) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 70.6(4) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 128.7(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 108.3(7) 1_555 1_555 1_555 yes C(12) C(13) C(18) 127.4(10) 1_555 1_555 1_555 yes C(14) C(13) C(18) 123.8(9) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 70.1(4) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 70.9(4) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 126.2(6) 1_555 1_555 1_555 yes C(13) C(14) C(15) 107.4(7) 1_555 1_555 1_555 yes C(13) C(14) C(19) 128.0(8) 1_555 1_555 1_555 yes C(15) C(14) C(19) 124.6(9) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 71.5(4) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 71.0(4) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 128.7(5) 1_555 1_555 1_555 yes C(11) C(15) C(14) 107.2(6) 1_555 1_555 1_555 yes C(11) C(15) C(20) 124.3(6) 1_555 1_555 1_555 yes C(14) C(15) C(20) 128.1(7) 1_555 1_555 1_555 yes S(1) C(21) C(22) 117.1(6) 1_555 1_555 1_555 yes S(2) C(22) C(21) 112.0(6) 1_555 1_555 1_555 yes S(2) C(23) C(24) 116.7(6) 1_555 1_555 1_555 yes S(2) C(23) C(28) 120.8(7) 1_555 1_555 1_555 yes C(24) C(23) C(28) 122.4(8) 1_555 1_555 1_555 yes C(23) C(24) C(25) 118.7(8) 1_555 1_555 1_555 yes C(24) C(25) C(26) 119.0(10) 1_555 1_555 1_555 yes C(25) C(26) C(27) 123.1(10) 1_555 1_555 1_555 yes C(26) C(27) C(28) 119.6(9) 1_555 1_555 1_555 yes C(23) C(28) C(27) 117.2(9) 1_555 1_555 1_555 yes S(3) C(29) C(30) 111.1(5) 1_555 1_555 1_555 yes S(4) C(30) C(29) 110.1(5) 1_555 1_555 1_555 yes S(4) C(31) C(32) 118.5(6) 1_555 1_555 1_555 yes S(4) C(31) C(36) 122.1(6) 1_555 1_555 1_555 yes C(32) C(31) C(36) 119.4(8) 1_555 1_555 1_555 yes C(31) C(32) C(33) 118.6(9) 1_555 1_555 1_555 yes C(32) C(33) C(34) 121.0(10) 1_555 1_555 1_555 yes C(33) C(34) C(35) 122.1(10) 1_555 1_555 1_555 yes C(34) C(35) C(36) 117.3(9) 1_555 1_555 1_555 yes C(31) C(36) C(35) 121.6(9) 1_555 1_555 1_555 yes S(5) C(37) C(38) 109.2(5) 1_555 1_555 1_555 yes S(6) C(38) C(37) 110.3(5) 1_555 1_555 1_555 yes S(6) C(39) C(40) 119.8(6) 1_555 1_555 1_555 yes S(6) C(39) C(44) 119.5(7) 1_555 1_555 1_555 yes C(40) C(39) C(44) 120.7(8) 1_555 1_555 1_555 yes C(39) C(40) C(41) 117.8(8) 1_555 1_555 1_555 yes C(40) C(41) C(42) 120.7(10) 1_555 1_555 1_555 yes C(41) C(42) C(43) 120.3(10) 1_555 1_555 1_555 yes C(42) C(43) C(44) 121.3(10) 1_555 1_555 1_555 yes C(39) C(44) C(43) 119.2(9) 1_555 1_555 1_555 yes N(1) C(45) C(46) 177(1) 1_555 1_555 1_555 yes N(2) C(47) C(48) 178(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir(1) Ir(2) 3.3300(4) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END data_[(Cp*Ir)2(SCH2CH2CN)2(SCH2CH2Cl)][PF6] _database_code_CSD 178527 #------------------------------------------------------------------------------ _audit_creation_date 'Tue May 28 11:35:43 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1067.69 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H42 Cl F6 Ir2 N2 P S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 20.655(4) _cell_length_b 11.025(5) _cell_length_c 31.223(4) _cell_angle_alpha 90 _cell_angle_beta 89 _cell_angle_gamma 89 _cell_volume 7110(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.7 _cell_measurement_theta_max 19.7 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'lemonyel' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096.00 _exptl_absorpt_coefficient_mu 7.849 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.270 _exptl_absorpt_correction_T_max 0.980 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -12.27 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -6 -2 0 -5 2 0 -5 _diffrn_reflns_number 10553 _reflns_number_total 10539 _reflns_number_gt 5440 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.197 _diffrn_reflns_av_sigmaI/netI 0.126 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00883 _diffrn_orient_matrix_UB_12 -0.00525 _diffrn_orient_matrix_UB_13 -0.03144 _diffrn_orient_matrix_UB_21 -0.04700 _diffrn_orient_matrix_UB_22 -0.01529 _diffrn_orient_matrix_UB_23 -0.00546 _diffrn_orient_matrix_UB_31 -0.00753 _diffrn_orient_matrix_UB_32 0.08925 _diffrn_orient_matrix_UB_33 -0.00278 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.03337(3) 0.37617(6) 0.4908 0.0371(2) Uani 1.00 d . . . Ir(2) Ir 0.07115(3) 0.08216(6) 0.49370(4) 0.0385(2) Uani 1.00 d . . . Ir(3) Ir 0.25957(3) 0.39251(6) 0.23226(4) 0.0388(2) Uani 1.00 d . . . Ir(4) Ir 0.29866(3) 0.10017(7) 0.23445(3) 0.0358(2) Uani 1.00 d . . . Cl(1) Cl -0.0373(6) 0.172(2) 0.6586(3) 0.168(6) Uani 1.00 d . . . Cl(2) Cl 0.1961(6) 0.165(2) 0.0675(4) 0.165(6) Uani 1.00 d . . . S(1) S 0.1236(2) 0.2616(5) 0.5181(2) 0.041(1) Uani 1.00 d . . . S(2) S 0.0492(2) 0.2233(4) 0.4367(2) 0.041(1) Uani 1.00 d . . . S(3) S -0.0174(3) 0.1997(5) 0.5208(2) 0.049(2) Uani 1.00 d . . . S(4) S 0.3501(2) 0.2786(4) 0.2058(2) 0.038(1) Uani 1.00 d . . . S(5) S 0.2811(2) 0.2509(5) 0.2880(2) 0.044(1) Uani 1.00 d . . . S(6) S 0.2087(3) 0.2122(5) 0.2077(3) 0.052(2) Uani 1.00 d . . . P(1) P 0.3068(3) 0.6335(10) 0.4284(3) 0.081(3) Uani 1.00 d . . . P(2) P 0.0314(4) -0.1694(9) 0.2929(3) 0.079(3) Uani 1.00 d . . . F(1) F 0.3489(9) 0.739(2) 0.442(1) 0.17(1) Uani 1.00 d . . . F(2) F 0.2635(8) 0.522(2) 0.4184(8) 0.128(8) Uani 1.00 d . . . F(3) F 0.2671(9) 0.708(2) 0.3963(8) 0.159(9) Uani 1.00 d . . . F(4) F 0.3473(8) 0.547(2) 0.4593(7) 0.130(8) Uani 1.00 d . . . F(5) F 0.2586(8) 0.666(3) 0.4648(6) 0.163(9) Uani 1.00 d . . . F(6) F 0.3582(8) 0.597(2) 0.3936(6) 0.164(10) Uani 1.00 d . . . F(7) F 0.0789(9) -0.154(3) 0.3302(7) 0.22(1) Uani 1.00 d . . . F(8) F -0.0176(9) -0.199(3) 0.2571(7) 0.19(1) Uani 1.00 d . . . F(9a) F 0.055(3) -0.043(5) 0.286(4) 0.22(4) Uani 0.50 d P . . F(9b) F -0.015(2) -0.052(3) 0.294(2) 0.13(1) Uani 0.50 d P . . F(10a) F 0.023(2) -0.317(4) 0.306(2) 0.19(2) Uani 0.50 d P . . F(10b) F 0.074(3) -0.260(4) 0.278(2) 0.15(2) Uani 0.50 d P . . F(11a) F 0.091(2) -0.221(4) 0.261(1) 0.09(1) Uani 0.50 d P . . F(11b) F 0.072(4) -0.074(6) 0.260(2) 0.16(3) Uani 0.50 d P . . F(12a) F -0.016(2) -0.129(4) 0.325(1) 0.10(1) Uani 0.50 d P . . F(12b) F -0.014(3) -0.222(5) 0.324(2) 0.17(2) Uani 0.50 d P . . N(1) N 0.287(2) 0.271(4) 0.575(1) 0.15(2) Uani 1.00 d . . . N(2) N 0.033(1) 0.298(3) 0.3186(10) 0.10(1) Uani 1.00 d . . . N(3) N 0.518(1) 0.261(4) 0.151(1) 0.16(2) Uani 1.00 d . . . N(4) N 0.306(1) 0.161(3) 0.408(1) 0.13(1) Uani 1.00 d . . . C(1) C -0.012(1) 0.523(2) 0.4525(8) 0.049(5) Uani 1.00 d . . . C(2) C 0.053(1) 0.545(2) 0.4605(9) 0.053(5) Uani 1.00 d . . . C(3) C 0.064(1) 0.562(2) 0.5073(8) 0.057(5) Uani 1.00 d . . . C(4) C 0.003(1) 0.529(2) 0.5271(8) 0.055(6) Uani 1.00 d . . . C(5) C -0.0424(9) 0.517(2) 0.496(1) 0.060(5) Uani 1.00 d . . . C(6) C -0.044(1) 0.520(3) 0.4105(9) 0.074(9) Uani 1.00 d . . . C(7) C 0.103(1) 0.573(2) 0.425(1) 0.079(9) Uani 1.00 d . . . C(8) C 0.126(1) 0.596(2) 0.525(1) 0.10(1) Uani 1.00 d . . . C(9) C -0.006(3) 0.542(3) 0.576(1) 0.17(2) Uani 1.00 d . . . C(10) C -0.111(1) 0.491(2) 0.502(1) 0.10(1) Uani 1.00 d . . . C(11) C 0.053(1) -0.098(2) 0.4664(8) 0.045(4) Uani 1.00 d . . . C(12) C 0.120(1) -0.070(2) 0.4581(8) 0.047(5) Uani 1.00 d . . . C(13) C 0.1464(9) -0.058(2) 0.5028(8) 0.051(5) Uani 1.00 d . . . C(14) C 0.097(1) -0.071(2) 0.5357(9) 0.060(6) Uani 1.00 d . . . C(15) C 0.039(1) -0.104(2) 0.5119(9) 0.060(5) Uani 1.00 d . . . C(16) C 0.008(1) -0.132(2) 0.4315(8) 0.058(7) Uani 1.00 d . . . C(17) C 0.157(1) -0.065(2) 0.4200(9) 0.067(8) Uani 1.00 d . . . C(18) C 0.218(1) -0.035(2) 0.512(1) 0.089(10) Uani 1.00 d . . . C(19) C 0.106(2) -0.076(2) 0.5832(10) 0.090(9) Uani 1.00 d . . . C(20) C -0.025(1) -0.135(2) 0.529(1) 0.072(9) Uani 1.00 d . . . C(21) C 0.1950(9) 0.287(2) 0.4845(6) 0.051(6) Uani 1.00 d . . . C(22) C 0.248(1) 0.351(3) 0.5031(9) 0.11(1) Uani 1.00 d . . . C(23) C 0.274(1) 0.299(3) 0.5437(9) 0.085(10) Uani 1.00 d . . . C(24) C -0.0304(9) 0.189(2) 0.4154(8) 0.053(5) Uani 1.00 d . . . C(25) C -0.026(1) 0.145(2) 0.3681(9) 0.074(7) Uani 1.00 d . . . C(26) C 0.007(1) 0.236(3) 0.3392(8) 0.074(9) Uani 1.00 d . . . C(27) C -0.005(1) 0.213(3) 0.5830(9) 0.098(9) Uani 1.00 d . . . C(28) C -0.054(2) 0.161(5) 0.6010(9) 0.17(2) Uani 1.00 d . . . C(29) C 0.229(2) 0.546(2) 0.1920(9) 0.088(9) Uani 1.00 d . . . C(30) C 0.286(2) 0.573(3) 0.214(1) 0.096(8) Uani 1.00 d . . . C(31) C 0.283(2) 0.578(3) 0.257(1) 0.083(7) Uani 1.00 d . . . C(32) C 0.214(1) 0.544(2) 0.2647(9) 0.056(6) Uani 1.00 d . . . C(33) C 0.181(1) 0.522(2) 0.2277(10) 0.054(5) Uani 1.00 d . . . C(34) C 0.212(2) 0.550(3) 0.146(1) 0.12(1) Uani 1.00 d . . . C(35) C 0.349(2) 0.614(3) 0.188(1) 0.12(1) Uani 1.00 d . . . C(36) C 0.329(2) 0.609(3) 0.289(1) 0.11(1) Uani 1.00 d . . . C(37) C 0.180(1) 0.539(3) 0.3084(10) 0.071(9) Uani 1.00 d . . . C(38) C 0.110(1) 0.493(3) 0.220(2) 0.14(1) Uani 1.00 d . . . C(39) C 0.268(1) -0.085(2) 0.2206(7) 0.045(4) Uani 1.00 d . . . C(40) C 0.325(1) -0.056(2) 0.1971(8) 0.049(5) Uani 1.00 d . . . C(41) C 0.3760(9) -0.039(2) 0.231(1) 0.057(5) Uani 1.00 d . . . C(42) C 0.3478(10) -0.046(2) 0.2691(8) 0.044(5) Uani 1.00 d . . . C(43) C 0.277(1) -0.079(2) 0.2647(7) 0.040(4) Uani 1.00 d . . . C(44) C 0.205(1) -0.121(2) 0.197(1) 0.074(10) Uani 1.00 d . . . C(45) C 0.339(1) -0.066(2) 0.1494(9) 0.075(8) Uani 1.00 d . . . C(46) C 0.446(1) -0.017(2) 0.219(1) 0.10(1) Uani 1.00 d . . . C(47) C 0.381(1) -0.028(3) 0.3131(10) 0.082(10) Uani 1.00 d . . . C(48) C 0.232(1) -0.101(2) 0.2997(8) 0.083(9) Uani 1.00 d . . . C(49) C 0.4188(9) 0.310(2) 0.239(1) 0.076(8) Uani 1.00 d . . . C(50) C 0.477(1) 0.372(2) 0.217(1) 0.076(8) Uani 1.00 d . . . C(51) C 0.4978(10) 0.304(3) 0.178(1) 0.071(8) Uani 1.00 d . . . C(52) C 0.208(1) 0.223(2) 0.3180(8) 0.061(7) Uani 1.00 d . . . C(53) C 0.208(1) 0.264(3) 0.3616(9) 0.085(9) Uani 1.00 d . . . C(54) C 0.262(1) 0.203(2) 0.3866(8) 0.073(8) Uani 1.00 d . . . C(55) C 0.218(2) 0.219(2) 0.1498(5) 0.107(9) Uani 1.00 d . . . C(56a) C 0.168(3) 0.159(7) 0.123(1) 0.1627 Uiso 0.60 d P . . C(56b) C 0.191(5) 0.120(6) 0.124(1) 0.16(2) Uiso 0.40 d P . . H(1) H -0.0409 0.5962 0.3966 0.0909 Uiso 1.00 calc . . . H(2) H -0.0261 0.4587 0.3926 0.0909 Uiso 1.00 calc . . . H(3) H -0.0896 0.5017 0.4144 0.0909 Uiso 1.00 calc . . . H(4) H 0.1459 0.5852 0.4359 0.1131 Uiso 1.00 calc . . . H(5) H 0.1056 0.5057 0.4048 0.1131 Uiso 1.00 calc . . . H(6) H 0.0910 0.6433 0.4089 0.1131 Uiso 1.00 calc . . . H(7) H 0.1576 0.5344 0.5183 0.1208 Uiso 1.00 calc . . . H(8) H 0.1401 0.6705 0.5135 0.1208 Uiso 1.00 calc . . . H(9) H 0.1228 0.6018 0.5553 0.1208 Uiso 1.00 calc . . . H(10) H -0.0001 0.6244 0.5840 0.2110 Uiso 1.00 calc . . . H(11) H -0.0471 0.5146 0.5841 0.2110 Uiso 1.00 calc . . . H(12) H 0.0267 0.4941 0.5901 0.2110 Uiso 1.00 calc . . . H(13) H -0.1299 0.5538 0.5185 0.1240 Uiso 1.00 calc . . . H(14) H -0.1323 0.4856 0.4751 0.1240 Uiso 1.00 calc . . . H(15) H -0.1158 0.4157 0.5168 0.1240 Uiso 1.00 calc . . . H(16) H -0.0338 -0.1470 0.4426 0.0717 Uiso 1.00 calc . . . H(17) H 0.0057 -0.0678 0.4109 0.0717 Uiso 1.00 calc . . . H(18) H 0.0234 -0.2033 0.4173 0.0717 Uiso 1.00 calc . . . H(19) H 0.1885 -0.1266 0.4210 0.0878 Uiso 1.00 calc . . . H(20) H 0.1300 -0.0722 0.3965 0.0878 Uiso 1.00 calc . . . H(21) H 0.1786 0.0128 0.4196 0.0878 Uiso 1.00 calc . . . H(22) H 0.2350 -0.1013 0.5282 0.1114 Uiso 1.00 calc . . . H(23) H 0.2414 -0.0280 0.4860 0.1114 Uiso 1.00 calc . . . H(24) H 0.2227 0.0375 0.5282 0.1114 Uiso 1.00 calc . . . H(25) H 0.0958 -0.1553 0.5935 0.1117 Uiso 1.00 calc . . . H(26) H 0.1463 -0.0513 0.5917 0.1117 Uiso 1.00 calc . . . H(27) H 0.0732 -0.0213 0.5959 0.1117 Uiso 1.00 calc . . . H(28) H -0.0232 -0.1308 0.5593 0.0851 Uiso 1.00 calc . . . H(29) H -0.0561 -0.0793 0.5185 0.0851 Uiso 1.00 calc . . . H(30) H -0.0353 -0.2144 0.5201 0.0851 Uiso 1.00 calc . . . H(31) H 0.2100 0.2090 0.4760 0.0579 Uiso 1.00 calc . . . H(32) H 0.1805 0.3301 0.4599 0.0579 Uiso 1.00 calc . . . H(33) H 0.2809 0.3548 0.4825 0.1384 Uiso 1.00 calc . . . H(34) H 0.2325 0.4311 0.5093 0.1384 Uiso 1.00 calc . . . H(35) H -0.0487 0.1249 0.4320 0.0663 Uiso 1.00 calc . . . H(36) H -0.0564 0.2582 0.4169 0.0663 Uiso 1.00 calc . . . H(37) H -0.0028 0.0711 0.3669 0.0899 Uiso 1.00 calc . . . H(38) H -0.0686 0.1335 0.3575 0.0899 Uiso 1.00 calc . . . H(39) H 0.0334 0.1758 0.5920 0.1140 Uiso 1.00 calc . . . H(40) H -0.0048 0.2970 0.5915 0.1140 Uiso 1.00 calc . . . H(41) H -0.0564 0.0790 0.5914 0.2107 Uiso 1.00 calc . . . H(42) H -0.0931 0.2016 0.5932 0.2107 Uiso 1.00 calc . . . H(43) H 0.2170 0.6275 0.1353 0.1421 Uiso 1.00 calc . . . H(44) H 0.2389 0.4934 0.1310 0.1421 Uiso 1.00 calc . . . H(45) H 0.1680 0.5234 0.1435 0.1421 Uiso 1.00 calc . . . H(46) H 0.3832 0.6277 0.2075 0.1501 Uiso 1.00 calc . . . H(47) H 0.3597 0.5488 0.1695 0.1501 Uiso 1.00 calc . . . H(48) H 0.3394 0.6840 0.1724 0.1501 Uiso 1.00 calc . . . H(49) H 0.3657 0.5559 0.2872 0.1335 Uiso 1.00 calc . . . H(50) H 0.3435 0.6901 0.2847 0.1335 Uiso 1.00 calc . . . H(51) H 0.3108 0.6021 0.3169 0.1335 Uiso 1.00 calc . . . H(52) H 0.2099 0.5612 0.3306 0.0801 Uiso 1.00 calc . . . H(53) H 0.1450 0.5986 0.3093 0.0801 Uiso 1.00 calc . . . H(54) H 0.1627 0.4625 0.3140 0.0801 Uiso 1.00 calc . . . H(55) H 0.0829 0.5557 0.2307 0.1886 Uiso 1.00 calc . . . H(56) H 0.1014 0.4789 0.1910 0.1886 Uiso 1.00 calc . . . H(57) H 0.0988 0.4190 0.2359 0.1886 Uiso 1.00 calc . . . H(58) H 0.1730 -0.1378 0.2166 0.0948 Uiso 1.00 calc . . . H(59) H 0.1931 -0.0570 0.1782 0.0948 Uiso 1.00 calc . . . H(60) H 0.2142 -0.1919 0.1797 0.0948 Uiso 1.00 calc . . . H(61) H 0.3354 -0.1476 0.1403 0.0862 Uiso 1.00 calc . . . H(62) H 0.3104 -0.0164 0.1333 0.0862 Uiso 1.00 calc . . . H(63) H 0.3826 -0.0388 0.1445 0.0862 Uiso 1.00 calc . . . H(64) H 0.4720 -0.0790 0.2313 0.1161 Uiso 1.00 calc . . . H(65) H 0.4510 -0.0185 0.1886 0.1161 Uiso 1.00 calc . . . H(66) H 0.4592 0.0596 0.2296 0.1161 Uiso 1.00 calc . . . H(67) H 0.4124 -0.0907 0.3166 0.1044 Uiso 1.00 calc . . . H(68) H 0.3985 0.0475 0.3151 0.1044 Uiso 1.00 calc . . . H(69) H 0.3478 -0.0403 0.3346 0.1044 Uiso 1.00 calc . . . H(70) H 0.2537 -0.0886 0.3262 0.0974 Uiso 1.00 calc . . . H(71) H 0.1972 -0.0450 0.2973 0.0974 Uiso 1.00 calc . . . H(72) H 0.2167 -0.1809 0.2978 0.0974 Uiso 1.00 calc . . . H(73) H 0.4052 0.3636 0.2612 0.0929 Uiso 1.00 calc . . . H(74) H 0.4336 0.2367 0.2508 0.0929 Uiso 1.00 calc . . . H(75) H 0.4653 0.4514 0.2081 0.0849 Uiso 1.00 calc . . . H(76) H 0.5125 0.3751 0.2358 0.0849 Uiso 1.00 calc . . . H(77) H 0.1723 0.2618 0.3042 0.0746 Uiso 1.00 calc . . . H(78) H 0.1995 0.1372 0.3186 0.0746 Uiso 1.00 calc . . . H(79) H 0.2150 0.3490 0.3615 0.0998 Uiso 1.00 calc . . . H(80) H 0.1689 0.2446 0.3749 0.0998 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0408(4) 0.0369(4) 0.0337(5) 0.0019(3) -0.0028(5) -0.0037(4) Ir(2) 0.0405(3) 0.0364(3) 0.0386(4) 0.0008(3) -0.0044(4) -0.0022(5) Ir(3) 0.0426(4) 0.0348(4) 0.0391(4) 0.0058(3) 0.0015(4) 0.0002(4) Ir(4) 0.0369(4) 0.0338(4) 0.0367(5) 0.0032(3) 0.0043(4) 0.0021(5) Cl(1) 0.17(1) 0.30(2) 0.037(5) 0.02(1) 0.020(5) 0.013(9) Cl(2) 0.19(1) 0.23(2) 0.077(9) 0.019(10) 0.025(7) 0.00(1) S(1) 0.045(3) 0.040(2) 0.038(3) 0.002(2) -0.004(2) -0.002(2) S(2) 0.053(3) 0.036(2) 0.034(3) 0.007(2) -0.007(2) -0.008(1) S(3) 0.049(3) 0.043(3) 0.054(4) 0.004(2) 0.012(2) 0.003(2) S(4) 0.044(2) 0.034(2) 0.035(3) 0.003(2) 0.007(2) 0.005(2) S(5) 0.057(3) 0.046(2) 0.029(2) 0.002(2) 0.003(2) 0.001(1) S(6) 0.043(3) 0.044(3) 0.070(5) 0.007(2) -0.018(3) -0.006(3) P(1) 0.052(4) 0.125(7) 0.066(5) -0.017(3) 0.001(3) -0.007(5) P(2) 0.066(4) 0.107(6) 0.065(5) 0.013(4) 0.007(3) -0.020(5) F(1) 0.11(1) 0.10(1) 0.30(4) -0.06(1) -0.01(2) -0.03(2) F(2) 0.09(1) 0.12(1) 0.17(2) -0.027(9) -0.03(1) -0.03(2) F(3) 0.13(1) 0.21(2) 0.14(2) 0.09(1) 0.00(1) 0.11(2) F(4) 0.08(1) 0.17(2) 0.14(2) -0.04(1) -0.05(1) 0.11(1) F(5) 0.09(1) 0.33(3) 0.07(1) -0.05(2) 0.032(8) -0.10(2) F(6) 0.09(1) 0.32(3) 0.08(1) 0.04(2) 0.038(9) -0.03(2) F(7) 0.09(1) 0.48(5) 0.08(1) -0.03(2) -0.021(9) -0.09(2) F(8) 0.11(1) 0.32(3) 0.14(2) 0.04(2) -0.09(1) -0.14(2) F(9a) 0.14(3) 0.09(2) 0.4(2) 0.03(2) -0.02(6) 0.05(5) F(9b) 0.12(2) 0.05(2) 0.23(5) -0.01(1) -0.10(3) 0.04(2) F(10a) 0.16(4) 0.11(2) 0.30(7) -0.07(3) 0.06(4) 0.01(3) F(10b) 0.17(4) 0.11(4) 0.17(6) 0.09(3) 0.09(3) 0.02(3) F(11a) 0.07(2) 0.12(3) 0.08(3) -0.02(2) 0.05(2) 0.00(2) F(11b) 0.21(8) 0.10(3) 0.16(5) -0.02(4) 0.11(5) 0.03(4) F(12a) 0.09(2) 0.19(3) 0.04(2) 0.06(3) -0.02(1) -0.04(2) F(12b) 0.14(4) 0.18(3) 0.19(5) -0.01(4) 0.10(3) 0.10(4) N(1) 0.18(3) 0.22(4) 0.07(2) -0.02(3) -0.05(2) 0.04(3) N(2) 0.09(2) 0.14(2) 0.07(2) -0.01(1) 0.02(1) 0.04(2) N(3) 0.11(2) 0.26(5) 0.10(3) 0.02(2) 0.05(2) -0.09(3) N(4) 0.12(2) 0.20(3) 0.08(2) 0.06(2) 0.01(1) 0.05(2) C(1) 0.061(10) 0.031(9) 0.06(1) 0.000(9) -0.027(8) 0.000(8) C(2) 0.060(9) 0.030(9) 0.07(1) 0.000(9) -0.023(9) 0.004(9) C(3) 0.08(1) 0.027(6) 0.07(1) 0.002(9) -0.02(1) 0.017(10) C(4) 0.08(1) 0.04(1) 0.05(1) 0.03(1) -0.001(9) -0.007(8) C(5) 0.046(8) 0.06(1) 0.07(1) 0.028(6) 0.005(10) 0.00(2) C(6) 0.10(2) 0.08(2) 0.05(1) 0.02(1) -0.03(1) 0.02(1) C(7) 0.08(2) 0.03(1) 0.12(3) 0.00(1) 0.05(2) 0.01(2) C(8) 0.10(2) 0.06(2) 0.15(3) -0.02(1) -0.07(2) -0.04(2) C(9) 0.35(6) 0.11(3) 0.06(1) 0.14(4) 0.07(3) 0.00(2) C(10) 0.056(10) 0.06(1) 0.17(4) 0.02(1) 0.07(2) 0.04(2) C(11) 0.049(8) 0.024(6) 0.06(1) 0.017(8) -0.019(8) 0.008(8) C(12) 0.053(9) 0.04(1) 0.043(9) 0.008(8) -0.007(7) -0.013(9) C(13) 0.047(8) 0.05(1) 0.05(1) 0.019(6) -0.030(8) -0.01(1) C(14) 0.07(1) 0.05(1) 0.06(1) -0.01(1) -0.015(8) 0.03(1) C(15) 0.07(1) 0.046(9) 0.06(1) -0.03(1) -0.013(9) 0.02(1) C(16) 0.08(2) 0.04(1) 0.05(1) 0.01(1) -0.03(1) 0.00(1) C(17) 0.08(2) 0.06(2) 0.06(2) 0.00(1) 0.04(1) -0.02(1) C(18) 0.050(10) 0.07(2) 0.15(3) -0.01(1) -0.03(2) -0.03(2) C(19) 0.16(3) 0.05(2) 0.06(1) 0.02(2) -0.04(2) -0.02(1) C(20) 0.06(1) 0.08(2) 0.07(2) 0.01(1) 0.00(1) 0.00(2) C(21) 0.062(8) 0.07(1) 0.02(1) 0.015(8) 0.005(6) 0.020(10) C(22) 0.08(2) 0.21(3) 0.05(2) -0.10(2) -0.01(1) 0.03(2) C(23) 0.06(2) 0.14(3) 0.05(1) -0.05(2) 0.01(1) -0.01(2) C(24) 0.043(8) 0.06(1) 0.06(1) 0.016(9) -0.003(9) 0.02(1) C(25) 0.10(2) 0.06(1) 0.07(1) -0.02(1) -0.02(1) -0.02(1) C(26) 0.08(2) 0.10(2) 0.04(2) 0.01(1) -0.02(1) 0.02(1) C(27) 0.09(2) 0.16(3) 0.050(6) 0.03(2) 0.02(1) 0.02(2) C(28) 0.13(3) 0.35(6) 0.041(7) -0.15(3) 0.01(2) 0.02(3) C(29) 0.17(2) 0.05(2) 0.04(1) 0.06(2) 0.03(1) 0.024(9) C(30) 0.13(2) 0.030(9) 0.12(2) 0.03(1) 0.07(2) 0.03(2) C(31) 0.09(1) 0.04(1) 0.12(2) -0.02(1) 0.01(2) -0.03(2) C(32) 0.08(1) 0.04(1) 0.05(1) 0.036(10) -0.005(8) -0.005(8) C(33) 0.079(9) 0.012(7) 0.07(1) 0.022(6) -0.019(9) -0.02(1) C(34) 0.24(4) 0.09(3) 0.05(2) 0.01(3) -0.02(2) 0.01(2) C(35) 0.15(3) 0.06(2) 0.15(3) -0.01(2) 0.11(3) 0.00(2) C(36) 0.09(2) 0.07(2) 0.17(4) 0.00(2) -0.03(2) -0.08(2) C(37) 0.06(1) 0.08(2) 0.07(2) 0.00(1) 0.02(1) -0.01(2) C(38) 0.06(1) 0.10(2) 0.25(5) 0.05(1) -0.03(2) 0.06(3) C(39) 0.07(1) 0.025(5) 0.037(9) 0.019(7) 0.005(7) 0.005(8) C(40) 0.08(1) 0.027(9) 0.04(1) 0.015(10) 0.012(8) 0.013(6) C(41) 0.052(8) 0.05(1) 0.07(1) 0.026(6) 0.009(9) 0.00(1) C(42) 0.046(8) 0.024(9) 0.06(1) 0.020(7) -0.016(8) -0.018(7) C(43) 0.052(8) 0.030(7) 0.038(9) -0.005(8) -0.004(8) -0.002(8) C(44) 0.09(2) 0.03(1) 0.10(3) -0.01(1) -0.04(2) -0.02(1) C(45) 0.13(2) 0.06(2) 0.04(1) 0.04(2) 0.02(2) -0.01(1) C(46) 0.06(1) 0.06(2) 0.19(4) 0.02(1) 0.06(2) 0.03(2) C(47) 0.08(2) 0.11(2) 0.06(2) 0.01(2) -0.03(1) 0.01(2) C(48) 0.12(2) 0.08(2) 0.04(2) -0.03(2) 0.06(1) -0.02(1) C(49) 0.043(10) 0.04(1) 0.14(2) -0.012(8) -0.06(1) 0.01(2) C(50) 0.07(1) 0.04(1) 0.12(2) -0.01(1) -0.01(1) -0.02(1) C(51) 0.03(1) 0.08(2) 0.11(2) 0.01(1) 0.01(1) 0.00(1) C(52) 0.07(1) 0.08(2) 0.04(1) 0.01(1) 0.03(1) 0.01(1) C(53) 0.12(2) 0.10(2) 0.04(1) 0.02(2) 0.02(1) 0.01(1) C(54) 0.10(2) 0.08(2) 0.04(1) 0.01(1) 0.05(1) 0.00(1) C(55) 0.22(3) 0.04(2) 0.062(6) 0.03(2) -0.08(2) -0.02(1) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00031(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.28(3) _refine_ls_number_reflns 5440 _refine_ls_number_parameters 810 _refine_ls_number_restraints 6 _refine_ls_number_constraints 1 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.504 _refine_ls_shift/su_max 0.9290 _refine_ls_shift/su_mean 0.0560 _refine_diff_density_min -1.94 _refine_diff_density_max 3.76 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) S(1) 2.407(6) 1_555 1_555 yes Ir(1) S(2) 2.409(7) 1_555 1_555 yes Ir(1) S(3) 2.400(7) 1_555 1_555 yes Ir(1) C(1) 2.22(3) 1_555 1_555 yes Ir(1) C(2) 2.13(3) 1_555 1_555 yes Ir(1) C(3) 2.21(3) 1_555 1_555 yes Ir(1) C(4) 2.13(3) 1_555 1_555 yes Ir(1) C(5) 2.21(2) 1_555 1_555 yes Ir(2) S(1) 2.380(6) 1_555 1_555 yes Ir(2) S(2) 2.408(7) 1_555 1_555 yes Ir(2) S(3) 2.395(7) 1_555 1_555 yes Ir(2) C(11) 2.19(3) 1_555 1_555 yes Ir(2) C(12) 2.25(3) 1_555 1_555 yes Ir(2) C(13) 2.21(2) 1_555 1_555 yes Ir(2) C(14) 2.21(3) 1_555 1_555 yes Ir(2) C(15) 2.23(3) 1_555 1_555 yes Ir(3) S(4) 2.399(6) 1_555 1_555 yes Ir(3) S(5) 2.380(7) 1_555 1_555 yes Ir(3) S(6) 2.375(7) 1_555 1_555 yes Ir(3) C(29) 2.20(3) 1_555 1_555 yes Ir(3) C(30) 2.15(4) 1_555 1_555 yes Ir(3) C(31) 2.24(3) 1_555 1_555 yes Ir(3) C(32) 2.18(3) 1_555 1_555 yes Ir(3) C(33) 2.18(2) 1_555 1_555 yes Ir(4) S(4) 2.408(6) 1_555 1_555 yes Ir(4) S(5) 2.386(7) 1_555 1_555 yes Ir(4) S(6) 2.382(7) 1_555 1_555 yes Ir(4) C(39) 2.18(3) 1_555 1_555 yes Ir(4) C(40) 2.14(3) 1_555 1_555 yes Ir(4) C(41) 2.22(2) 1_555 1_555 yes Ir(4) C(42) 2.19(3) 1_555 1_555 yes Ir(4) C(43) 2.24(3) 1_555 1_555 yes Cl(1) C(28) 1.83(4) 1_555 1_555 yes Cl(2) C(56a) 1.82(5) 1_555 1_555 yes Cl(2) C(56b) 1.82(5) 1_555 1_555 yes S(1) C(21) 1.83(2) 1_555 1_555 yes S(2) C(24) 1.81(3) 1_555 1_555 yes S(3) C(27) 1.96(4) 1_555 1_555 yes S(4) C(49) 1.79(2) 1_555 1_555 yes S(5) C(52) 1.81(3) 1_555 1_555 yes S(6) C(55) 1.82(3) 1_555 1_555 yes P(1) F(1) 1.51(2) 1_555 1_555 yes P(1) F(2) 1.55(2) 1_555 1_555 yes P(1) F(3) 1.54(2) 1_555 1_555 yes P(1) F(4) 1.59(2) 1_555 1_555 yes P(1) F(5) 1.55(2) 1_555 1_555 yes P(1) F(6) 1.57(2) 1_555 1_555 yes P(2) F(7) 1.53(2) 1_555 1_555 yes P(2) F(8) 1.54(2) 1_555 1_555 yes P(2) F(9a) 1.49(7) 1_555 1_555 yes P(2) F(9b) 1.62(4) 1_555 1_555 yes P(2) F(10a) 1.69(6) 1_555 1_555 yes P(2) F(10b) 1.41(5) 1_555 1_555 yes P(2) F(11a) 1.69(4) 1_555 1_555 yes P(2) F(11b) 1.69(7) 1_555 1_555 yes P(2) F(12a) 1.48(4) 1_555 1_555 yes P(2) F(12b) 1.47(5) 1_555 1_555 yes N(1) C(23) 1.07(5) 1_555 1_555 yes N(2) C(26) 1.08(4) 1_555 1_555 yes N(3) C(51) 1.06(5) 1_555 1_555 yes N(4) C(54) 1.21(4) 1_555 1_555 yes C(1) C(2) 1.40(4) 1_555 1_555 yes C(1) C(5) 1.49(5) 1_555 1_555 yes C(1) C(6) 1.47(4) 1_555 1_555 yes C(2) C(3) 1.49(4) 1_555 1_555 yes C(2) C(7) 1.55(4) 1_555 1_555 yes C(3) C(4) 1.45(4) 1_555 1_555 yes C(3) C(8) 1.44(4) 1_555 1_555 yes C(4) C(5) 1.37(4) 1_555 1_555 yes C(4) C(9) 1.53(5) 1_555 1_555 yes C(5) C(10) 1.46(3) 1_555 1_555 yes C(11) C(12) 1.44(4) 1_555 1_555 yes C(11) C(15) 1.45(4) 1_555 1_555 yes C(11) C(16) 1.49(4) 1_555 1_555 yes C(12) C(13) 1.50(4) 1_555 1_555 yes C(12) C(17) 1.41(4) 1_555 1_555 yes C(13) C(14) 1.45(4) 1_555 1_555 yes C(13) C(18) 1.53(3) 1_555 1_555 yes C(14) C(15) 1.46(4) 1_555 1_555 yes C(14) C(19) 1.50(5) 1_555 1_555 yes C(15) C(20) 1.45(4) 1_555 1_555 yes C(21) C(22) 1.42(4) 1_555 1_555 yes C(22) C(23) 1.50(5) 1_555 1_555 yes C(24) C(25) 1.56(4) 1_555 1_555 yes C(25) C(26) 1.51(4) 1_555 1_555 yes C(27) C(28) 1.29(4) 1_555 1_555 yes C(29) C(30) 1.39(6) 1_555 1_555 yes C(29) C(33) 1.52(5) 1_555 1_555 yes C(29) C(34) 1.47(5) 1_555 1_555 yes C(30) C(31) 1.37(6) 1_555 1_555 yes C(30) C(35) 1.58(5) 1_555 1_555 yes C(31) C(32) 1.50(5) 1_555 1_555 yes C(31) C(36) 1.41(5) 1_555 1_555 yes C(32) C(33) 1.36(4) 1_555 1_555 yes C(32) C(37) 1.54(4) 1_555 1_555 yes C(33) C(38) 1.52(4) 1_555 1_555 yes C(39) C(40) 1.41(4) 1_555 1_555 yes C(39) C(43) 1.39(4) 1_555 1_555 yes C(39) C(44) 1.55(4) 1_555 1_555 yes C(40) C(41) 1.51(4) 1_555 1_555 yes C(40) C(45) 1.52(4) 1_555 1_555 yes C(41) C(42) 1.33(5) 1_555 1_555 yes C(41) C(46) 1.52(4) 1_555 1_555 yes C(42) C(43) 1.52(3) 1_555 1_555 yes C(42) C(47) 1.54(4) 1_555 1_555 yes C(43) C(48) 1.45(4) 1_555 1_555 yes C(49) C(50) 1.54(4) 1_555 1_555 yes C(50) C(51) 1.50(5) 1_555 1_555 yes C(52) C(53) 1.43(4) 1_555 1_555 yes C(53) C(54) 1.52(4) 1_555 1_555 yes C(55) C(56a) 1.48(4) 1_555 1_555 yes C(55) C(56b) 1.47(5) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 77.1(2) 1_555 1_555 1_555 yes S(1) Ir(1) S(3) 77.0(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 154.2(8) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 117.7(8) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 100.5(7) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 117.0(9) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 153(1) 1_555 1_555 1_555 yes S(2) Ir(1) S(3) 76.4(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(1) 100.9(8) 1_555 1_555 1_555 yes S(2) Ir(1) C(2) 105.9(9) 1_555 1_555 1_555 yes S(2) Ir(1) C(3) 140.7(8) 1_555 1_555 1_555 yes S(2) Ir(1) C(4) 165.7(9) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 129(1) 1_555 1_555 1_555 yes S(3) Ir(1) C(1) 128.1(7) 1_555 1_555 1_555 yes S(3) Ir(1) C(2) 165.3(8) 1_555 1_555 1_555 yes S(3) Ir(1) C(3) 142.0(8) 1_555 1_555 1_555 yes S(3) Ir(1) C(4) 107.9(9) 1_555 1_555 1_555 yes S(3) Ir(1) C(5) 103.5(8) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 37.4(10) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 64(1) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 65.5(10) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 39(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 40(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 66(1) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 63(1) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 38(1) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 62(1) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 36(1) 1_555 1_555 1_555 yes S(1) Ir(2) S(2) 77.6(2) 1_555 1_555 1_555 yes S(1) Ir(2) S(3) 77.6(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(11) 162.5(7) 1_555 1_555 1_555 yes S(1) Ir(2) C(12) 124.8(7) 1_555 1_555 1_555 yes S(1) Ir(2) C(13) 102.7(6) 1_555 1_555 1_555 yes S(1) Ir(2) C(14) 109.6(9) 1_555 1_555 1_555 yes S(1) Ir(2) C(15) 145.0(9) 1_555 1_555 1_555 yes S(2) Ir(2) S(3) 76.6(2) 1_555 1_555 1_555 yes S(2) Ir(2) C(11) 105.4(8) 1_555 1_555 1_555 yes S(2) Ir(2) C(12) 101.6(8) 1_555 1_555 1_555 yes S(2) Ir(2) C(13) 132.8(8) 1_555 1_555 1_555 yes S(2) Ir(2) C(14) 168.7(10) 1_555 1_555 1_555 yes S(2) Ir(2) C(15) 136.5(8) 1_555 1_555 1_555 yes S(3) Ir(2) C(11) 119.9(7) 1_555 1_555 1_555 yes S(3) Ir(2) C(12) 157.1(7) 1_555 1_555 1_555 yes S(3) Ir(2) C(13) 150.5(8) 1_555 1_555 1_555 yes S(3) Ir(2) C(14) 113.1(9) 1_555 1_555 1_555 yes S(3) Ir(2) C(15) 100.2(9) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 37.8(9) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 62.3(9) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 64(1) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 38(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 39(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 67(1) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 65(1) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 38(1) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 62(1) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38(1) 1_555 1_555 1_555 yes S(4) Ir(3) S(5) 76.3(2) 1_555 1_555 1_555 yes S(4) Ir(3) S(6) 78.2(2) 1_555 1_555 1_555 yes S(4) Ir(3) C(29) 115.4(10) 1_555 1_555 1_555 yes S(4) Ir(3) C(30) 101(1) 1_555 1_555 1_555 yes S(4) Ir(3) C(31) 115(1) 1_555 1_555 1_555 yes S(4) Ir(3) C(32) 154.6(9) 1_555 1_555 1_555 yes S(4) Ir(3) C(33) 155(1) 1_555 1_555 1_555 yes S(5) Ir(3) S(6) 76.7(3) 1_555 1_555 1_555 yes S(5) Ir(3) C(29) 167.4(9) 1_555 1_555 1_555 yes S(5) Ir(3) C(30) 139(1) 1_555 1_555 1_555 yes S(5) Ir(3) C(31) 107(1) 1_555 1_555 1_555 yes S(5) Ir(3) C(32) 104.2(9) 1_555 1_555 1_555 yes S(5) Ir(3) C(33) 128.3(10) 1_555 1_555 1_555 yes S(6) Ir(3) C(29) 109(1) 1_555 1_555 1_555 yes S(6) Ir(3) C(30) 143(1) 1_555 1_555 1_555 yes S(6) Ir(3) C(31) 166(1) 1_555 1_555 1_555 yes S(6) Ir(3) C(32) 127.0(9) 1_555 1_555 1_555 yes S(6) Ir(3) C(33) 101.5(7) 1_555 1_555 1_555 yes C(29) Ir(3) C(30) 37(1) 1_555 1_555 1_555 yes C(29) Ir(3) C(31) 63(1) 1_555 1_555 1_555 yes C(29) Ir(3) C(32) 63(1) 1_555 1_555 1_555 yes C(29) Ir(3) C(33) 40(1) 1_555 1_555 1_555 yes C(30) Ir(3) C(31) 36(1) 1_555 1_555 1_555 yes C(30) Ir(3) C(32) 61(1) 1_555 1_555 1_555 yes C(30) Ir(3) C(33) 64(1) 1_555 1_555 1_555 yes C(31) Ir(3) C(32) 39(1) 1_555 1_555 1_555 yes C(31) Ir(3) C(33) 65(1) 1_555 1_555 1_555 yes C(32) Ir(3) C(33) 36(1) 1_555 1_555 1_555 yes S(4) Ir(4) S(5) 76.0(2) 1_555 1_555 1_555 yes S(4) Ir(4) S(6) 77.9(2) 1_555 1_555 1_555 yes S(4) Ir(4) C(39) 145.0(7) 1_555 1_555 1_555 yes S(4) Ir(4) C(40) 110.1(8) 1_555 1_555 1_555 yes S(4) Ir(4) C(41) 103.2(8) 1_555 1_555 1_555 yes S(4) Ir(4) C(42) 125.4(7) 1_555 1_555 1_555 yes S(4) Ir(4) C(43) 165.3(7) 1_555 1_555 1_555 yes S(5) Ir(4) S(6) 76.4(3) 1_555 1_555 1_555 yes S(5) Ir(4) C(39) 138.4(7) 1_555 1_555 1_555 yes S(5) Ir(4) C(40) 167.8(8) 1_555 1_555 1_555 yes S(5) Ir(4) C(41) 128(1) 1_555 1_555 1_555 yes S(5) Ir(4) C(42) 103.6(8) 1_555 1_555 1_555 yes S(5) Ir(4) C(43) 106.8(7) 1_555 1_555 1_555 yes S(6) Ir(4) C(39) 101.1(7) 1_555 1_555 1_555 yes S(6) Ir(4) C(40) 114.8(8) 1_555 1_555 1_555 yes S(6) Ir(4) C(41) 154(1) 1_555 1_555 1_555 yes S(6) Ir(4) C(42) 156.4(8) 1_555 1_555 1_555 yes S(6) Ir(4) C(43) 116.7(7) 1_555 1_555 1_555 yes C(39) Ir(4) C(40) 38.1(10) 1_555 1_555 1_555 yes C(39) Ir(4) C(41) 63.2(10) 1_555 1_555 1_555 yes C(39) Ir(4) C(42) 62.8(10) 1_555 1_555 1_555 yes C(39) Ir(4) C(43) 36.7(9) 1_555 1_555 1_555 yes C(40) Ir(4) C(41) 40(1) 1_555 1_555 1_555 yes C(40) Ir(4) C(42) 64.2(10) 1_555 1_555 1_555 yes C(40) Ir(4) C(43) 64(1) 1_555 1_555 1_555 yes C(41) Ir(4) C(42) 35(1) 1_555 1_555 1_555 yes C(41) Ir(4) C(43) 63(1) 1_555 1_555 1_555 yes C(42) Ir(4) C(43) 40.0(9) 1_555 1_555 1_555 yes Ir(1) S(1) Ir(2) 88.3(2) 1_555 1_555 1_555 yes Ir(1) S(1) C(21) 109.8(8) 1_555 1_555 1_555 yes Ir(2) S(1) C(21) 108.2(9) 1_555 1_555 1_555 yes Ir(1) S(2) Ir(2) 87.6(3) 1_555 1_555 1_555 yes Ir(1) S(2) C(24) 106.2(10) 1_555 1_555 1_555 yes Ir(2) S(2) C(24) 107.9(9) 1_555 1_555 1_555 yes Ir(1) S(3) Ir(2) 88.1(2) 1_555 1_555 1_555 yes Ir(1) S(3) C(27) 105(1) 1_555 1_555 1_555 yes Ir(2) S(3) C(27) 107(1) 1_555 1_555 1_555 yes Ir(3) S(4) Ir(4) 87.5(2) 1_555 1_555 1_555 yes Ir(3) S(4) C(49) 108(1) 1_555 1_555 1_555 yes Ir(4) S(4) C(49) 107(1) 1_555 1_555 1_555 yes Ir(3) S(5) Ir(4) 88.4(3) 1_555 1_555 1_555 yes Ir(3) S(5) C(52) 109(1) 1_555 1_555 1_555 yes Ir(4) S(5) C(52) 111(1) 1_555 1_555 1_555 yes Ir(3) S(6) Ir(4) 88.6(2) 1_555 1_555 1_555 yes Ir(3) S(6) C(55) 104(1) 1_555 1_555 1_555 yes Ir(4) S(6) C(55) 106(1) 1_555 1_555 1_555 yes F(1) P(1) F(2) 174(2) 1_555 1_555 1_555 yes F(1) P(1) F(3) 94(1) 1_555 1_555 1_555 yes F(1) P(1) F(4) 88(1) 1_555 1_555 1_555 yes F(1) P(1) F(5) 88(1) 1_555 1_555 1_555 yes F(1) P(1) F(6) 90(1) 1_555 1_555 1_555 yes F(2) P(1) F(3) 89(1) 1_555 1_555 1_555 yes F(2) P(1) F(4) 87(1) 1_555 1_555 1_555 yes F(2) P(1) F(5) 87(1) 1_555 1_555 1_555 yes F(2) P(1) F(6) 92(1) 1_555 1_555 1_555 yes F(3) P(1) F(4) 175(1) 1_555 1_555 1_555 yes F(3) P(1) F(5) 90(1) 1_555 1_555 1_555 yes F(3) P(1) F(6) 92(1) 1_555 1_555 1_555 yes F(4) P(1) F(5) 91(1) 1_555 1_555 1_555 yes F(4) P(1) F(6) 84(1) 1_555 1_555 1_555 yes F(5) P(1) F(6) 176(1) 1_555 1_555 1_555 yes F(7) P(2) F(8) 173(2) 1_555 1_555 1_555 yes F(7) P(2) F(9a) 78(4) 1_555 1_555 1_555 yes F(7) P(2) F(9b) 105(2) 1_555 1_555 1_555 yes F(7) P(2) F(10a) 89(3) 1_555 1_555 1_555 yes F(7) P(2) F(10b) 85(3) 1_555 1_555 1_555 yes F(7) P(2) F(11a) 91(2) 1_555 1_555 1_555 yes F(7) P(2) F(11b) 94(4) 1_555 1_555 1_555 yes F(7) P(2) F(12a) 82(2) 1_555 1_555 1_555 yes F(7) P(2) F(12b) 87(3) 1_555 1_555 1_555 yes F(8) P(2) F(9a) 108(4) 1_555 1_555 1_555 yes F(8) P(2) F(9b) 78(1) 1_555 1_555 1_555 yes F(8) P(2) F(10a) 84(2) 1_555 1_555 1_555 yes F(8) P(2) F(10b) 91(3) 1_555 1_555 1_555 yes F(8) P(2) F(11a) 88(2) 1_555 1_555 1_555 yes F(8) P(2) F(11b) 91(4) 1_555 1_555 1_555 yes F(8) P(2) F(12a) 97(1) 1_555 1_555 1_555 yes F(8) P(2) F(12b) 88(3) 1_555 1_555 1_555 yes F(9a) P(2) F(10a) 166(4) 1_555 1_555 1_555 yes F(9a) P(2) F(11a) 90(4) 1_555 1_555 1_555 yes F(9a) P(2) F(12a) 91(4) 1_555 1_555 1_555 yes F(9b) P(2) F(10b) 162(3) 1_555 1_555 1_555 yes F(9b) P(2) F(11b) 79(3) 1_555 1_555 1_555 yes F(9b) P(2) F(12b) 84(3) 1_555 1_555 1_555 yes F(10a) P(2) F(11a) 83(2) 1_555 1_555 1_555 yes F(10a) P(2) F(12a) 93(3) 1_555 1_555 1_555 yes F(10b) P(2) F(11b) 86(3) 1_555 1_555 1_555 yes F(10b) P(2) F(12b) 109(3) 1_555 1_555 1_555 yes F(11a) P(2) F(12a) 173(2) 1_555 1_555 1_555 yes F(11b) P(2) F(12b) 163(3) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 67(1) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 69(1) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 130(2) 1_555 1_555 1_555 yes C(2) C(1) C(5) 104(2) 1_555 1_555 1_555 yes C(2) C(1) C(6) 127(3) 1_555 1_555 1_555 yes C(5) C(1) C(6) 127(2) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 74(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 72(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 128(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 109(2) 1_555 1_555 1_555 yes C(1) C(2) C(7) 123(3) 1_555 1_555 1_555 yes C(3) C(2) C(7) 125(2) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 67(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 67(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 125(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 105(2) 1_555 1_555 1_555 yes C(2) C(3) C(8) 122(3) 1_555 1_555 1_555 yes C(4) C(3) C(8) 132(3) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 73(1) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 74(1) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 129(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 108(2) 1_555 1_555 1_555 yes C(3) C(4) C(9) 120(3) 1_555 1_555 1_555 yes C(5) C(4) C(9) 129(3) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 70(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 68(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 123(1) 1_555 1_555 1_555 yes C(1) C(5) C(4) 110(2) 1_555 1_555 1_555 yes C(1) C(5) C(10) 123(3) 1_555 1_555 1_555 yes C(4) C(5) C(10) 125(4) 1_555 1_555 1_555 yes C(1) C(6) H(1) 110(3) 1_555 1_555 1_555 no C(1) C(6) H(2) 111(2) 1_555 1_555 1_555 no C(1) C(6) H(3) 109(3) 1_555 1_555 1_555 no H(1) C(6) H(2) 109(3) 1_555 1_555 1_555 no H(1) C(6) H(3) 108(2) 1_555 1_555 1_555 no H(2) C(6) H(3) 107(3) 1_555 1_555 1_555 no C(2) C(7) H(4) 112(3) 1_555 1_555 1_555 no C(2) C(7) H(5) 110(2) 1_555 1_555 1_555 no C(2) C(7) H(6) 110(2) 1_555 1_555 1_555 no H(4) C(7) H(5) 107(2) 1_555 1_555 1_555 no H(4) C(7) H(6) 108(2) 1_555 1_555 1_555 no H(5) C(7) H(6) 107(4) 1_555 1_555 1_555 no C(3) C(8) H(7) 109(2) 1_555 1_555 1_555 no C(3) C(8) H(8) 110(3) 1_555 1_555 1_555 no C(3) C(8) H(9) 109(3) 1_555 1_555 1_555 no H(7) C(8) H(8) 108(4) 1_555 1_555 1_555 no H(7) C(8) H(9) 108(3) 1_555 1_555 1_555 no H(8) C(8) H(9) 109(3) 1_555 1_555 1_555 no C(4) C(9) H(10) 109(4) 1_555 1_555 1_555 no C(4) C(9) H(11) 111(5) 1_555 1_555 1_555 no C(4) C(9) H(12) 108(3) 1_555 1_555 1_555 no H(10) C(9) H(11) 110(3) 1_555 1_555 1_555 no H(10) C(9) H(12) 107(6) 1_555 1_555 1_555 no H(11) C(9) H(12) 109(4) 1_555 1_555 1_555 no C(5) C(10) H(13) 109(3) 1_555 1_555 1_555 no C(5) C(10) H(14) 109(3) 1_555 1_555 1_555 no C(5) C(10) H(15) 110(2) 1_555 1_555 1_555 no H(13) C(10) H(14) 108(2) 1_555 1_555 1_555 no H(13) C(10) H(15) 110(4) 1_555 1_555 1_555 no H(14) C(10) H(15) 108(3) 1_555 1_555 1_555 no Ir(2) C(11) C(12) 73(1) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 72(1) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 128(1) 1_555 1_555 1_555 yes C(12) C(11) C(15) 112(2) 1_555 1_555 1_555 yes C(12) C(11) C(16) 121(2) 1_555 1_555 1_555 yes C(15) C(11) C(16) 125(2) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 68(1) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 68(1) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 128(2) 1_555 1_555 1_555 yes C(11) C(12) C(13) 101(2) 1_555 1_555 1_555 yes C(11) C(12) C(17) 132(2) 1_555 1_555 1_555 yes C(13) C(12) C(17) 126(2) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 71(1) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 70(1) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 125(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 113(2) 1_555 1_555 1_555 yes C(12) C(13) C(18) 122(2) 1_555 1_555 1_555 yes C(14) C(13) C(18) 123(2) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 70(1) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 71(1) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 129(2) 1_555 1_555 1_555 yes C(13) C(14) C(15) 104(2) 1_555 1_555 1_555 yes C(13) C(14) C(19) 128(2) 1_555 1_555 1_555 yes C(15) C(14) C(19) 126(3) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 69(1) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 69(1) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 125(2) 1_555 1_555 1_555 yes C(11) C(15) C(14) 108(2) 1_555 1_555 1_555 yes C(11) C(15) C(20) 124(2) 1_555 1_555 1_555 yes C(14) C(15) C(20) 127(3) 1_555 1_555 1_555 yes C(11) C(16) H(16) 110(2) 1_555 1_555 1_555 no C(11) C(16) H(17) 109(2) 1_555 1_555 1_555 no C(11) C(16) H(18) 109(2) 1_555 1_555 1_555 no H(16) C(16) H(17) 108(2) 1_555 1_555 1_555 no H(16) C(16) H(18) 109(2) 1_555 1_555 1_555 no H(17) C(16) H(18) 108(3) 1_555 1_555 1_555 no C(12) C(17) H(19) 108(3) 1_555 1_555 1_555 no C(12) C(17) H(20) 110(2) 1_555 1_555 1_555 no C(12) C(17) H(21) 107(2) 1_555 1_555 1_555 no H(19) C(17) H(20) 112(3) 1_555 1_555 1_555 no H(19) C(17) H(21) 107(2) 1_555 1_555 1_555 no H(20) C(17) H(21) 110(3) 1_555 1_555 1_555 no C(13) C(18) H(22) 109(2) 1_555 1_555 1_555 no C(13) C(18) H(23) 109(3) 1_555 1_555 1_555 no C(13) C(18) H(24) 110(2) 1_555 1_555 1_555 no H(22) C(18) H(23) 108(2) 1_555 1_555 1_555 no H(22) C(18) H(24) 110(3) 1_555 1_555 1_555 no H(23) C(18) H(24) 109(3) 1_555 1_555 1_555 no C(14) C(19) H(25) 109(2) 1_555 1_555 1_555 no C(14) C(19) H(26) 112(4) 1_555 1_555 1_555 no C(14) C(19) H(27) 107(3) 1_555 1_555 1_555 no H(25) C(19) H(26) 111(3) 1_555 1_555 1_555 no H(25) C(19) H(27) 105(4) 1_555 1_555 1_555 no H(26) C(19) H(27) 109(3) 1_555 1_555 1_555 no C(15) C(20) H(28) 109(2) 1_555 1_555 1_555 no C(15) C(20) H(29) 109(3) 1_555 1_555 1_555 no C(15) C(20) H(30) 108(3) 1_555 1_555 1_555 no H(28) C(20) H(29) 109(3) 1_555 1_555 1_555 no H(28) C(20) H(30) 110(3) 1_555 1_555 1_555 no H(29) C(20) H(30) 109(3) 1_555 1_555 1_555 no S(1) C(21) C(22) 117(2) 1_555 1_555 1_555 yes S(1) C(21) H(31) 106(1) 1_555 1_555 1_555 no S(1) C(21) H(32) 106(1) 1_555 1_555 1_555 no C(22) C(21) H(31) 108(2) 1_555 1_555 1_555 no C(22) C(21) H(32) 109(2) 1_555 1_555 1_555 no H(31) C(21) H(32) 108(2) 1_555 1_555 1_555 no C(21) C(22) C(23) 115(2) 1_555 1_555 1_555 yes C(21) C(22) H(33) 107(3) 1_555 1_555 1_555 no C(21) C(22) H(34) 106(3) 1_555 1_555 1_555 no C(23) C(22) H(33) 109(3) 1_555 1_555 1_555 no C(23) C(22) H(34) 107(3) 1_555 1_555 1_555 no H(33) C(22) H(34) 110(3) 1_555 1_555 1_555 no N(1) C(23) C(22) 171(5) 1_555 1_555 1_555 yes S(2) C(24) C(25) 111(1) 1_555 1_555 1_555 yes S(2) C(24) H(35) 108(2) 1_555 1_555 1_555 no S(2) C(24) H(36) 109(2) 1_555 1_555 1_555 no C(25) C(24) H(35) 107(2) 1_555 1_555 1_555 no C(25) C(24) H(36) 109(2) 1_555 1_555 1_555 no H(35) C(24) H(36) 110(2) 1_555 1_555 1_555 no C(24) C(25) C(26) 112(2) 1_555 1_555 1_555 yes C(24) C(25) H(37) 109(2) 1_555 1_555 1_555 no C(24) C(25) H(38) 108(2) 1_555 1_555 1_555 no C(26) C(25) H(37) 108(3) 1_555 1_555 1_555 no C(26) C(25) H(38) 107(3) 1_555 1_555 1_555 no H(37) C(25) H(38) 109(2) 1_555 1_555 1_555 no N(2) C(26) C(25) 177(4) 1_555 1_555 1_555 yes S(3) C(27) C(28) 107(3) 1_555 1_555 1_555 yes S(3) C(27) H(39) 111(2) 1_555 1_555 1_555 no S(3) C(27) H(40) 110(2) 1_555 1_555 1_555 no C(28) C(27) H(39) 109(4) 1_555 1_555 1_555 no C(28) C(27) H(40) 108(3) 1_555 1_555 1_555 no H(39) C(27) H(40) 108(4) 1_555 1_555 1_555 no Cl(1) C(28) C(27) 104(2) 1_555 1_555 1_555 yes Cl(1) C(28) H(41) 112(4) 1_555 1_555 1_555 no Cl(1) C(28) H(42) 111(3) 1_555 1_555 1_555 no C(27) C(28) H(41) 109(4) 1_555 1_555 1_555 no C(27) C(28) H(42) 109(5) 1_555 1_555 1_555 no H(41) C(28) H(42) 108(3) 1_555 1_555 1_555 no Ir(3) C(29) C(30) 69(2) 1_555 1_555 1_555 yes Ir(3) C(29) C(33) 68(1) 1_555 1_555 1_555 yes Ir(3) C(29) C(34) 130(2) 1_555 1_555 1_555 yes C(30) C(29) C(33) 103(3) 1_555 1_555 1_555 yes C(30) C(29) C(34) 131(4) 1_555 1_555 1_555 yes C(33) C(29) C(34) 123(4) 1_555 1_555 1_555 yes Ir(3) C(30) C(29) 73(2) 1_555 1_555 1_555 yes Ir(3) C(30) C(31) 75(2) 1_555 1_555 1_555 yes Ir(3) C(30) C(35) 127(2) 1_555 1_555 1_555 yes C(29) C(30) C(31) 117(4) 1_555 1_555 1_555 yes C(29) C(30) C(35) 120(4) 1_555 1_555 1_555 yes C(31) C(30) C(35) 121(5) 1_555 1_555 1_555 yes Ir(3) C(31) C(30) 68(2) 1_555 1_555 1_555 yes Ir(3) C(31) C(32) 67(1) 1_555 1_555 1_555 yes Ir(3) C(31) C(36) 128(2) 1_555 1_555 1_555 yes C(30) C(31) C(32) 100(3) 1_555 1_555 1_555 yes C(30) C(31) C(36) 132(4) 1_555 1_555 1_555 yes C(32) C(31) C(36) 126(4) 1_555 1_555 1_555 yes Ir(3) C(32) C(31) 72(1) 1_555 1_555 1_555 yes Ir(3) C(32) C(33) 71(1) 1_555 1_555 1_555 yes Ir(3) C(32) C(37) 125(2) 1_555 1_555 1_555 yes C(31) C(32) C(33) 113(3) 1_555 1_555 1_555 yes C(31) C(32) C(37) 125(3) 1_555 1_555 1_555 yes C(33) C(32) C(37) 121(2) 1_555 1_555 1_555 yes Ir(3) C(33) C(29) 70(1) 1_555 1_555 1_555 yes Ir(3) C(33) C(32) 71(1) 1_555 1_555 1_555 yes Ir(3) C(33) C(38) 126(1) 1_555 1_555 1_555 yes C(29) C(33) C(32) 105(2) 1_555 1_555 1_555 yes C(29) C(33) C(38) 124(3) 1_555 1_555 1_555 yes C(32) C(33) C(38) 130(3) 1_555 1_555 1_555 yes C(29) C(34) H(43) 111(4) 1_555 1_555 1_555 no C(29) C(34) H(44) 108(3) 1_555 1_555 1_555 no C(29) C(34) H(45) 107(4) 1_555 1_555 1_555 no H(43) C(34) H(44) 110(4) 1_555 1_555 1_555 no H(43) C(34) H(45) 110(4) 1_555 1_555 1_555 no H(44) C(34) H(45) 107(4) 1_555 1_555 1_555 no C(30) C(35) H(46) 110(4) 1_555 1_555 1_555 no C(30) C(35) H(47) 106(3) 1_555 1_555 1_555 no C(30) C(35) H(48) 109(3) 1_555 1_555 1_555 no H(46) C(35) H(47) 109(4) 1_555 1_555 1_555 no H(46) C(35) H(48) 111(3) 1_555 1_555 1_555 no H(47) C(35) H(48) 109(5) 1_555 1_555 1_555 no C(31) C(36) H(49) 109(3) 1_555 1_555 1_555 no C(31) C(36) H(50) 110(4) 1_555 1_555 1_555 no C(31) C(36) H(51) 110(3) 1_555 1_555 1_555 no H(49) C(36) H(50) 109(3) 1_555 1_555 1_555 no H(49) C(36) H(51) 108(4) 1_555 1_555 1_555 no H(50) C(36) H(51) 109(3) 1_555 1_555 1_555 no C(32) C(37) H(52) 109(2) 1_555 1_555 1_555 no C(32) C(37) H(53) 109(3) 1_555 1_555 1_555 no C(32) C(37) H(54) 112(3) 1_555 1_555 1_555 no H(52) C(37) H(53) 106(3) 1_555 1_555 1_555 no H(52) C(37) H(54) 110(3) 1_555 1_555 1_555 no H(53) C(37) H(54) 109(2) 1_555 1_555 1_555 no C(33) C(38) H(55) 110(3) 1_555 1_555 1_555 no C(33) C(38) H(56) 110(4) 1_555 1_555 1_555 no C(33) C(38) H(57) 108(2) 1_555 1_555 1_555 no H(55) C(38) H(56) 110(3) 1_555 1_555 1_555 no H(55) C(38) H(57) 107(4) 1_555 1_555 1_555 no H(56) C(38) H(57) 108(4) 1_555 1_555 1_555 no Ir(4) C(39) C(40) 69(1) 1_555 1_555 1_555 yes Ir(4) C(39) C(43) 74(1) 1_555 1_555 1_555 yes Ir(4) C(39) C(44) 125(1) 1_555 1_555 1_555 yes C(40) C(39) C(43) 113(2) 1_555 1_555 1_555 yes C(40) C(39) C(44) 120(2) 1_555 1_555 1_555 yes C(43) C(39) C(44) 125(2) 1_555 1_555 1_555 yes Ir(4) C(40) C(39) 72(1) 1_555 1_555 1_555 yes Ir(4) C(40) C(41) 72(1) 1_555 1_555 1_555 yes Ir(4) C(40) C(45) 129(1) 1_555 1_555 1_555 yes C(39) C(40) C(41) 104(2) 1_555 1_555 1_555 yes C(39) C(40) C(45) 130(3) 1_555 1_555 1_555 yes C(41) C(40) C(45) 123(2) 1_555 1_555 1_555 yes Ir(4) C(41) C(40) 67(1) 1_555 1_555 1_555 yes Ir(4) C(41) C(42) 71(1) 1_555 1_555 1_555 yes Ir(4) C(41) C(46) 126(1) 1_555 1_555 1_555 yes C(40) C(41) C(42) 108(2) 1_555 1_555 1_555 yes C(40) C(41) C(46) 121(3) 1_555 1_555 1_555 yes C(42) C(41) C(46) 130(3) 1_555 1_555 1_555 yes Ir(4) C(42) C(41) 73(1) 1_555 1_555 1_555 yes Ir(4) C(42) C(43) 71(1) 1_555 1_555 1_555 yes Ir(4) C(42) C(47) 123(2) 1_555 1_555 1_555 yes C(41) C(42) C(43) 110(2) 1_555 1_555 1_555 yes C(41) C(42) C(47) 126(2) 1_555 1_555 1_555 yes C(43) C(42) C(47) 122(2) 1_555 1_555 1_555 yes Ir(4) C(43) C(39) 69(1) 1_555 1_555 1_555 yes Ir(4) C(43) C(42) 68(1) 1_555 1_555 1_555 yes Ir(4) C(43) C(48) 126(2) 1_555 1_555 1_555 yes C(39) C(43) C(42) 102(2) 1_555 1_555 1_555 yes C(39) C(43) C(48) 131(2) 1_555 1_555 1_555 yes C(42) C(43) C(48) 126(2) 1_555 1_555 1_555 yes C(39) C(44) H(58) 110(3) 1_555 1_555 1_555 no C(39) C(44) H(59) 109(2) 1_555 1_555 1_555 no C(39) C(44) H(60) 107(2) 1_555 1_555 1_555 no H(58) C(44) H(59) 112(3) 1_555 1_555 1_555 no H(58) C(44) H(60) 110(2) 1_555 1_555 1_555 no H(59) C(44) H(60) 106(4) 1_555 1_555 1_555 no C(40) C(45) H(61) 110(3) 1_555 1_555 1_555 no C(40) C(45) H(62) 110(2) 1_555 1_555 1_555 no C(40) C(45) H(63) 108(3) 1_555 1_555 1_555 no H(61) C(45) H(62) 109(3) 1_555 1_555 1_555 no H(61) C(45) H(63) 108(2) 1_555 1_555 1_555 no H(62) C(45) H(63) 108(3) 1_555 1_555 1_555 no C(41) C(46) H(64) 108(2) 1_555 1_555 1_555 no C(41) C(46) H(65) 109(3) 1_555 1_555 1_555 no C(41) C(46) H(66) 108(2) 1_555 1_555 1_555 no H(64) C(46) H(65) 109(3) 1_555 1_555 1_555 no H(64) C(46) H(66) 109(4) 1_555 1_555 1_555 no H(65) C(46) H(66) 110(3) 1_555 1_555 1_555 no C(42) C(47) H(67) 108(3) 1_555 1_555 1_555 no C(42) C(47) H(68) 111(3) 1_555 1_555 1_555 no C(42) C(47) H(69) 106(2) 1_555 1_555 1_555 no H(67) C(47) H(68) 112(3) 1_555 1_555 1_555 no H(67) C(47) H(69) 107(3) 1_555 1_555 1_555 no H(68) C(47) H(69) 111(4) 1_555 1_555 1_555 no C(43) C(48) H(70) 109(2) 1_555 1_555 1_555 no C(43) C(48) H(71) 108(2) 1_555 1_555 1_555 no C(43) C(48) H(72) 108(2) 1_555 1_555 1_555 no H(70) C(48) H(71) 109(2) 1_555 1_555 1_555 no H(70) C(48) H(72) 110(3) 1_555 1_555 1_555 no H(71) C(48) H(72) 110(3) 1_555 1_555 1_555 no S(4) C(49) C(50) 116(2) 1_555 1_555 1_555 yes S(4) C(49) H(73) 107(1) 1_555 1_555 1_555 no S(4) C(49) H(74) 108(1) 1_555 1_555 1_555 no C(50) C(49) H(73) 106(2) 1_555 1_555 1_555 no C(50) C(49) H(74) 107(2) 1_555 1_555 1_555 no H(73) C(49) H(74) 109(4) 1_555 1_555 1_555 no C(49) C(50) C(51) 111(2) 1_555 1_555 1_555 yes C(49) C(50) H(75) 110(2) 1_555 1_555 1_555 no C(49) C(50) H(76) 110(3) 1_555 1_555 1_555 no C(51) C(50) H(75) 106(3) 1_555 1_555 1_555 no C(51) C(50) H(76) 106(2) 1_555 1_555 1_555 no H(75) C(50) H(76) 110(2) 1_555 1_555 1_555 no N(3) C(51) C(50) 173(4) 1_555 1_555 1_555 yes S(5) C(52) C(53) 115(2) 1_555 1_555 1_555 yes S(5) C(52) H(77) 109(2) 1_555 1_555 1_555 no S(5) C(52) H(78) 108(2) 1_555 1_555 1_555 no C(53) C(52) H(77) 107(2) 1_555 1_555 1_555 no C(53) C(52) H(78) 107(2) 1_555 1_555 1_555 no H(77) C(52) H(78) 108(3) 1_555 1_555 1_555 no C(52) C(53) C(54) 110(2) 1_555 1_555 1_555 yes C(52) C(53) H(79) 108(3) 1_555 1_555 1_555 no C(52) C(53) H(80) 109(3) 1_555 1_555 1_555 no C(54) C(53) H(79) 109(3) 1_555 1_555 1_555 no C(54) C(53) H(80) 107(2) 1_555 1_555 1_555 no H(79) C(53) H(80) 110(3) 1_555 1_555 1_555 no N(4) C(54) C(53) 176(4) 1_555 1_555 1_555 yes S(6) C(55) C(56a) 118(3) 1_555 1_555 1_555 yes S(6) C(55) C(56b) 119(3) 1_555 1_555 1_555 yes Cl(2) C(56a) C(55) 107(2) 1_555 1_555 1_555 yes Cl(2) C(56b) C(55) 108(3) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir(1) Ir(2) 3.335(1) 1_555 1_555 ? Ir(3) Ir(4) 3.323(1) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END data_[(Cp*Ir)2(SCH2CH2S)(SCH2CH2Cl)][PF6]_(7') _database_code_CSD 178528 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Aug 7 12:32:16 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 987.60 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H38 Cl F6 Ir2 P S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.039(2) _cell_length_b 11.287(1) _cell_length_c 12.663(3) _cell_angle_alpha 92.26(1) _cell_angle_beta 95.68(2) _cell_angle_gamma 100.85(1) _cell_volume 1539.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'lemonyel' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 2.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940.00 _exptl_absorpt_coefficient_mu 9.053 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.63 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 3 -1 0 2 -2 0 2 0 _diffrn_reflns_number 7433 _reflns_number_total 7064 _reflns_number_gt 5412 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.048 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02253 _diffrn_orient_matrix_UB_12 0.08271 _diffrn_orient_matrix_UB_13 0.03621 _diffrn_orient_matrix_UB_21 0.03632 _diffrn_orient_matrix_UB_22 0.03212 _diffrn_orient_matrix_UB_23 -0.06483 _diffrn_orient_matrix_UB_31 -0.08235 _diffrn_orient_matrix_UB_32 0.01713 _diffrn_orient_matrix_UB_33 -0.02839 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.14461(2) 0.22453(2) 0.27355(2) 0.03040(7) Uani 1.00 d . . . Ir(2) Ir -0.13508(2) 0.28933(2) 0.28734(2) 0.03251(7) Uani 1.00 d . . . Cl Cl 0.0703(3) 0.6987(2) 0.0811(2) 0.0797(8) Uani 1.00 d . . . S(1) S -0.0133(2) 0.1709(2) 0.3898(1) 0.0404(5) Uani 1.00 d . . . S(2) S -0.0475(2) 0.1748(2) 0.1635(1) 0.0371(4) Uani 1.00 d . . . S(3) S 0.0694(2) 0.4069(1) 0.2957(1) 0.0369(4) Uani 1.00 d . . . P P 0.4850(2) 0.2489(2) 0.7931(2) 0.0589(7) Uani 1.00 d . . . F(1) F 0.6169(7) 0.3182(8) 0.820(1) 0.230(5) Uani 1.00 d . . . F(2) F 0.3550(6) 0.1780(7) 0.7512(8) 0.166(4) Uani 1.00 d . . . F(3) F 0.454(1) 0.304(1) 0.8921(6) 0.244(6) Uani 1.00 d . . . F(4) F 0.5255(8) 0.1944(9) 0.6912(6) 0.173(4) Uani 1.00 d . . . F(5) F 0.518(1) 0.1412(6) 0.8504(6) 0.185(4) Uani 1.00 d . . . F(6) F 0.4483(6) 0.3556(6) 0.7331(7) 0.142(3) Uani 1.00 d . . . C(1) C 0.3083(6) 0.1785(7) 0.3613(6) 0.044(2) Uani 1.00 d . . . C(2) C 0.2582(6) 0.0849(6) 0.2802(6) 0.045(2) Uani 1.00 d . . . C(3) C 0.2658(6) 0.1400(7) 0.1802(6) 0.046(2) Uani 1.00 d . . . C(4) C 0.3170(6) 0.2652(7) 0.1992(6) 0.043(2) Uani 1.00 d . . . C(5) C 0.3448(6) 0.2884(6) 0.3134(6) 0.042(2) Uani 1.00 d . . . C(6) C 0.3239(8) 0.1620(10) 0.4780(7) 0.077(3) Uani 1.00 d . . . C(7) C 0.2220(8) -0.0458(8) 0.2989(9) 0.083(3) Uani 1.00 d . . . C(8) C 0.2307(9) 0.0748(10) 0.0730(7) 0.082(3) Uani 1.00 d . . . C(9) C 0.3503(8) 0.3554(9) 0.1173(7) 0.078(3) Uani 1.00 d . . . C(10) C 0.4051(7) 0.4073(8) 0.3689(8) 0.072(3) Uani 1.00 d . . . C(11) C -0.2724(6) 0.3266(6) 0.3908(6) 0.040(2) Uani 1.00 d . . . C(12) C -0.3267(6) 0.2233(7) 0.3187(6) 0.044(2) Uani 1.00 d . . . C(13) C -0.3264(6) 0.2632(7) 0.2124(6) 0.048(2) Uani 1.00 d . . . C(14) C -0.2720(6) 0.3881(7) 0.2170(6) 0.043(2) Uani 1.00 d . . . C(15) C -0.2408(6) 0.4281(6) 0.3282(6) 0.043(2) Uani 1.00 d . . . C(16) C -0.2599(8) 0.3280(8) 0.5099(6) 0.063(3) Uani 1.00 d . . . C(17) C -0.3860(7) 0.1009(7) 0.3514(8) 0.067(3) Uani 1.00 d . . . C(18) C -0.3763(7) 0.1836(9) 0.1144(7) 0.068(3) Uani 1.00 d . . . C(19) C -0.2670(8) 0.4659(8) 0.1241(7) 0.068(3) Uani 1.00 d . . . C(20) C -0.1907(8) 0.5546(8) 0.3726(8) 0.067(3) Uani 1.00 d . . . C(21) C -0.0842(7) 0.0210(6) 0.3273(6) 0.050(2) Uani 1.00 d . . . C(22) C -0.1016(7) 0.0231(6) 0.2070(7) 0.053(2) Uani 1.00 d . . . C(23) C 0.0817(7) 0.4886(6) 0.1733(6) 0.049(2) Uani 1.00 d . . . C(24) C 0.0851(9) 0.6183(7) 0.1986(6) 0.064(3) Uani 1.00 d . . . H(1) H 0.2910 0.0805 0.4910 0.0921 Uiso 1.00 calc . . . H(2) H 0.4095 0.1809 0.5036 0.0921 Uiso 1.00 calc . . . H(3) H 0.2809 0.2142 0.5138 0.0921 Uiso 1.00 calc . . . H(4) H 0.1592 -0.0567 0.3457 0.0998 Uiso 1.00 calc . . . H(5) H 0.1914 -0.0899 0.2332 0.0998 Uiso 1.00 calc . . . H(6) H 0.2923 -0.0744 0.3297 0.0998 Uiso 1.00 calc . . . H(7) H 0.1697 0.1098 0.0340 0.0989 Uiso 1.00 calc . . . H(8) H 0.3020 0.0812 0.0357 0.0989 Uiso 1.00 calc . . . H(9) H 0.1980 -0.0080 0.0814 0.0989 Uiso 1.00 calc . . . H(10) H 0.3832 0.4327 0.1519 0.0932 Uiso 1.00 calc . . . H(11) H 0.4107 0.3310 0.0773 0.0932 Uiso 1.00 calc . . . H(12) H 0.2782 0.3597 0.0712 0.0932 Uiso 1.00 calc . . . H(13) H 0.4815 0.3999 0.4073 0.0869 Uiso 1.00 calc . . . H(14) H 0.4202 0.4664 0.3180 0.0869 Uiso 1.00 calc . . . H(15) H 0.3519 0.4312 0.4168 0.0869 Uiso 1.00 calc . . . H(16) H -0.2875 0.2487 0.5316 0.0751 Uiso 1.00 calc . . . H(17) H -0.1754 0.3556 0.5369 0.0751 Uiso 1.00 calc . . . H(18) H -0.3089 0.3806 0.5368 0.0751 Uiso 1.00 calc . . . H(19) H -0.4533 0.1086 0.3907 0.0803 Uiso 1.00 calc . . . H(20) H -0.4157 0.0488 0.2898 0.0803 Uiso 1.00 calc . . . H(21) H -0.3265 0.0679 0.3942 0.0803 Uiso 1.00 calc . . . H(22) H -0.4620 0.1521 0.1169 0.0818 Uiso 1.00 calc . . . H(23) H -0.3661 0.2294 0.0534 0.0818 Uiso 1.00 calc . . . H(24) H -0.3326 0.1190 0.1106 0.0818 Uiso 1.00 calc . . . H(25) H -0.2258 0.5457 0.1470 0.0816 Uiso 1.00 calc . . . H(26) H -0.2230 0.4341 0.0723 0.0816 Uiso 1.00 calc . . . H(27) H -0.3489 0.4672 0.0938 0.0816 Uiso 1.00 calc . . . H(28) H -0.1144 0.5571 0.4153 0.0799 Uiso 1.00 calc . . . H(29) H -0.1773 0.6066 0.3159 0.0799 Uiso 1.00 calc . . . H(30) H -0.2486 0.5804 0.4147 0.0799 Uiso 1.00 calc . . . H(31) H -0.0321 -0.0344 0.3466 0.0604 Uiso 1.00 calc . . . H(32) H -0.1629 -0.0044 0.3522 0.0604 Uiso 1.00 calc . . . H(33) H -0.1872 -0.0023 0.1828 0.0636 Uiso 1.00 calc . . . H(34) H -0.0558 -0.0309 0.1773 0.0636 Uiso 1.00 calc . . . H(35) H 0.1555 0.4791 0.1440 0.0588 Uiso 1.00 calc . . . H(36) H 0.0119 0.4571 0.1232 0.0588 Uiso 1.00 calc . . . H(37) H 0.1618 0.6522 0.2391 0.0763 Uiso 1.00 calc . . . H(38) H 0.0187 0.6260 0.2391 0.0763 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0318(1) 0.0304(1) 0.0305(1) 0.0085(1) 0.0050(1) 0.0034(1) Ir(2) 0.0329(1) 0.0342(2) 0.0321(1) 0.0107(1) 0.0035(1) 0.0025(1) Cl 0.124(2) 0.051(1) 0.061(1) 0.012(1) -0.003(1) 0.017(1) S(1) 0.0412(9) 0.050(1) 0.0354(9) 0.0167(8) 0.0101(7) 0.0129(8) S(2) 0.0389(9) 0.0388(9) 0.0329(8) 0.0081(7) 0.0014(7) -0.0022(7) S(3) 0.0389(9) 0.0303(8) 0.0411(9) 0.0073(7) 0.0025(7) -0.0004(7) P 0.072(2) 0.049(1) 0.052(1) 0.004(1) 0.002(1) 0.002(1) F(1) 0.099(6) 0.133(7) 0.42(2) -0.002(6) -0.091(8) -0.029(9) F(2) 0.085(5) 0.116(6) 0.28(1) -0.029(4) -0.003(6) 0.015(7) F(3) 0.43(2) 0.28(1) 0.093(6) 0.23(1) 0.060(9) -0.023(7) F(4) 0.166(8) 0.29(1) 0.095(6) 0.114(8) 0.040(5) 0.015(7) F(5) 0.35(1) 0.084(5) 0.111(6) 0.052(7) -0.056(7) 0.029(4) F(6) 0.125(6) 0.084(5) 0.207(8) 0.011(4) -0.038(5) 0.060(5) C(1) 0.038(4) 0.056(5) 0.042(4) 0.018(3) 0.005(3) 0.010(4) C(2) 0.038(4) 0.039(4) 0.063(5) 0.015(3) 0.014(4) 0.008(4) C(3) 0.039(4) 0.053(5) 0.048(4) 0.015(3) 0.009(3) -0.012(4) C(4) 0.037(4) 0.050(4) 0.045(4) 0.014(3) 0.015(3) 0.011(3) C(5) 0.028(3) 0.042(4) 0.056(4) 0.006(3) 0.005(3) -0.002(3) C(6) 0.068(6) 0.125(9) 0.051(5) 0.049(6) 0.006(4) 0.029(6) C(7) 0.067(6) 0.043(5) 0.15(1) 0.025(4) 0.028(6) 0.015(6) C(8) 0.076(6) 0.108(8) 0.060(6) 0.017(6) 0.007(5) -0.030(6) C(9) 0.074(6) 0.092(7) 0.082(7) 0.030(5) 0.041(5) 0.046(6) C(10) 0.041(4) 0.066(6) 0.105(8) 0.004(4) 0.008(5) -0.020(5) C(11) 0.040(4) 0.043(4) 0.044(4) 0.019(3) 0.012(3) 0.001(3) C(12) 0.028(3) 0.054(5) 0.054(5) 0.015(3) 0.007(3) 0.005(4) C(13) 0.036(4) 0.060(5) 0.050(5) 0.021(4) -0.006(3) -0.005(4) C(14) 0.038(4) 0.055(5) 0.043(4) 0.022(3) 0.006(3) 0.009(4) C(15) 0.041(4) 0.039(4) 0.052(4) 0.016(3) 0.007(3) 0.001(3) C(16) 0.074(6) 0.075(6) 0.046(5) 0.025(5) 0.020(4) 0.005(4) C(17) 0.043(4) 0.052(5) 0.108(8) 0.007(4) 0.020(5) 0.011(5) C(18) 0.049(5) 0.090(7) 0.060(5) 0.019(5) -0.019(4) -0.027(5) C(19) 0.071(6) 0.074(6) 0.073(6) 0.039(5) 0.015(5) 0.029(5) C(20) 0.063(5) 0.054(5) 0.088(7) 0.019(4) 0.023(5) 0.003(5) C(21) 0.046(4) 0.041(4) 0.070(5) 0.014(3) 0.019(4) 0.017(4) C(22) 0.049(4) 0.034(4) 0.074(6) 0.004(3) 0.005(4) -0.003(4) C(23) 0.060(5) 0.041(4) 0.050(4) 0.010(4) 0.015(4) 0.011(4) C(24) 0.106(7) 0.039(4) 0.043(4) 0.009(5) 0.001(5) 0.005(4) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0042(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5412 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0307 _refine_ls_wR_factor_gt 0.0307 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.545 _refine_ls_shift/su_max 0.0280 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -1.47 _refine_diff_density_max 1.45 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) S(1) 2.398(2) 1_555 1_555 yes Ir(1) S(2) 2.380(2) 1_555 1_555 yes Ir(1) S(3) 2.376(2) 1_555 1_555 yes Ir(1) C(1) 2.184(7) 1_555 1_555 yes Ir(1) C(2) 2.190(7) 1_555 1_555 yes Ir(1) C(3) 2.192(7) 1_555 1_555 yes Ir(1) C(4) 2.186(6) 1_555 1_555 yes Ir(1) C(5) 2.193(6) 1_555 1_555 yes Ir(2) S(1) 2.397(2) 1_555 1_555 yes Ir(2) S(2) 2.383(2) 1_555 1_555 yes Ir(2) S(3) 2.383(2) 1_555 1_555 yes Ir(2) C(11) 2.186(6) 1_555 1_555 yes Ir(2) C(12) 2.187(6) 1_555 1_555 yes Ir(2) C(13) 2.190(7) 1_555 1_555 yes Ir(2) C(14) 2.184(6) 1_555 1_555 yes Ir(2) C(15) 2.197(7) 1_555 1_555 yes Cl C(24) 1.783(7) 1_555 1_555 yes S(1) C(21) 1.837(8) 1_555 1_555 yes S(2) C(22) 1.829(7) 1_555 1_555 yes S(3) C(23) 1.839(7) 1_555 1_555 yes P F(1) 1.516(7) 1_555 1_555 yes P F(2) 1.539(7) 1_555 1_555 yes P F(3) 1.474(8) 1_555 1_555 yes P F(4) 1.548(8) 1_555 1_555 yes P F(5) 1.525(6) 1_555 1_555 yes P F(6) 1.546(6) 1_555 1_555 yes C(1) C(2) 1.44(1) 1_555 1_555 yes C(1) C(5) 1.411(9) 1_555 1_555 yes C(1) C(6) 1.494(10) 1_555 1_555 yes C(2) C(3) 1.436(10) 1_555 1_555 yes C(2) C(7) 1.49(1) 1_555 1_555 yes C(3) C(4) 1.421(10) 1_555 1_555 yes C(3) C(8) 1.50(1) 1_555 1_555 yes C(4) C(5) 1.451(10) 1_555 1_555 yes C(4) C(9) 1.505(9) 1_555 1_555 yes C(5) C(10) 1.50(1) 1_555 1_555 yes C(11) C(12) 1.45(1) 1_555 1_555 yes C(11) C(15) 1.428(9) 1_555 1_555 yes C(11) C(16) 1.501(10) 1_555 1_555 yes C(12) C(13) 1.437(10) 1_555 1_555 yes C(12) C(17) 1.507(10) 1_555 1_555 yes C(13) C(14) 1.42(1) 1_555 1_555 yes C(13) C(18) 1.50(1) 1_555 1_555 yes C(14) C(15) 1.449(10) 1_555 1_555 yes C(14) C(19) 1.494(9) 1_555 1_555 yes C(15) C(20) 1.50(1) 1_555 1_555 yes C(21) C(22) 1.52(1) 1_555 1_555 yes C(23) C(24) 1.48(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 73.43(6) 1_555 1_555 1_555 yes S(1) Ir(1) S(3) 77.31(6) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 103.0(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 107.2(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 140.0(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 166.7(2) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 129.2(2) 1_555 1_555 1_555 yes S(2) Ir(1) S(3) 79.71(6) 1_555 1_555 1_555 yes S(2) Ir(1) C(1) 152.9(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(2) 116.0(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(3) 101.4(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(4) 119.1(2) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 157.3(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(1) 126.4(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(2) 164.3(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(3) 142.0(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(4) 108.2(2) 1_555 1_555 1_555 yes S(3) Ir(1) C(5) 101.3(2) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 38.3(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 63.5(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 63.9(2) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 37.6(2) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 38.3(3) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 64.2(2) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 63.9(3) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 37.9(3) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 63.7(3) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38.7(3) 1_555 1_555 1_555 yes S(1) Ir(2) S(2) 73.41(6) 1_555 1_555 1_555 yes S(1) Ir(2) S(3) 77.20(6) 1_555 1_555 1_555 yes S(1) Ir(2) C(11) 104.6(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(12) 105.5(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(13) 135.9(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(14) 168.7(2) 1_555 1_555 1_555 yes S(1) Ir(2) C(15) 133.9(2) 1_555 1_555 1_555 yes S(2) Ir(2) S(3) 79.51(6) 1_555 1_555 1_555 yes S(2) Ir(2) C(11) 156.5(2) 1_555 1_555 1_555 yes S(2) Ir(2) C(12) 118.4(2) 1_555 1_555 1_555 yes S(2) Ir(2) C(13) 100.3(2) 1_555 1_555 1_555 yes S(2) Ir(2) C(14) 115.0(2) 1_555 1_555 1_555 yes S(2) Ir(2) C(15) 152.4(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(11) 123.4(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(12) 162.1(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(13) 145.9(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(14) 111.0(2) 1_555 1_555 1_555 yes S(3) Ir(2) C(15) 101.1(2) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 38.6(3) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 64.3(3) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 64.6(2) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 38.0(2) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 38.3(3) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 64.3(2) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 63.9(3) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 37.9(3) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 63.7(3) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38.6(3) 1_555 1_555 1_555 yes Ir(1) S(1) Ir(2) 87.75(5) 1_555 1_555 1_555 yes Ir(1) S(1) C(21) 98.3(2) 1_555 1_555 1_555 yes Ir(2) S(1) C(21) 98.7(2) 1_555 1_555 1_555 yes Ir(1) S(2) Ir(2) 88.50(6) 1_555 1_555 1_555 yes Ir(1) S(2) C(22) 98.8(3) 1_555 1_555 1_555 yes Ir(2) S(2) C(22) 99.5(3) 1_555 1_555 1_555 yes Ir(1) S(3) Ir(2) 88.56(6) 1_555 1_555 1_555 yes Ir(1) S(3) C(23) 109.0(3) 1_555 1_555 1_555 yes Ir(2) S(3) C(23) 108.1(3) 1_555 1_555 1_555 yes F(1) P F(2) 172.7(7) 1_555 1_555 1_555 yes F(1) P F(3) 88.1(7) 1_555 1_555 1_555 yes F(1) P F(4) 88.7(6) 1_555 1_555 1_555 yes F(1) P F(5) 90.3(5) 1_555 1_555 1_555 yes F(1) P F(6) 91.1(5) 1_555 1_555 1_555 yes F(2) P F(3) 98.6(7) 1_555 1_555 1_555 yes F(2) P F(4) 84.6(5) 1_555 1_555 1_555 yes F(2) P F(5) 92.3(5) 1_555 1_555 1_555 yes F(2) P F(6) 86.2(4) 1_555 1_555 1_555 yes F(3) P F(4) 176.8(7) 1_555 1_555 1_555 yes F(3) P F(5) 91.8(5) 1_555 1_555 1_555 yes F(3) P F(6) 89.0(5) 1_555 1_555 1_555 yes F(4) P F(5) 87.8(5) 1_555 1_555 1_555 yes F(4) P F(6) 91.5(5) 1_555 1_555 1_555 yes F(5) P F(6) 178.4(4) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 71.1(4) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 71.5(4) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 125.3(5) 1_555 1_555 1_555 yes C(2) C(1) C(5) 109.2(6) 1_555 1_555 1_555 yes C(2) C(1) C(6) 125.7(7) 1_555 1_555 1_555 yes C(5) C(1) C(6) 125.0(8) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 70.6(4) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 71.0(4) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 129.4(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 106.7(6) 1_555 1_555 1_555 yes C(1) C(2) C(7) 125.0(7) 1_555 1_555 1_555 yes C(3) C(2) C(7) 127.9(8) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 70.8(4) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 70.8(4) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 126.5(6) 1_555 1_555 1_555 yes C(2) C(3) C(4) 109.1(7) 1_555 1_555 1_555 yes C(2) C(3) C(8) 125.4(8) 1_555 1_555 1_555 yes C(4) C(3) C(8) 125.5(7) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 71.3(4) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 70.9(3) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 128.2(5) 1_555 1_555 1_555 yes C(3) C(4) C(5) 107.2(6) 1_555 1_555 1_555 yes C(3) C(4) C(9) 127.1(8) 1_555 1_555 1_555 yes C(5) C(4) C(9) 125.4(7) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 70.9(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 70.4(4) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 125.6(5) 1_555 1_555 1_555 yes C(1) C(5) C(4) 107.8(6) 1_555 1_555 1_555 yes C(1) C(5) C(10) 126.6(7) 1_555 1_555 1_555 yes C(4) C(5) C(10) 125.6(7) 1_555 1_555 1_555 yes Ir(2) C(11) C(12) 70.7(4) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 71.4(4) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 126.5(5) 1_555 1_555 1_555 yes C(12) C(11) C(15) 107.6(6) 1_555 1_555 1_555 yes C(12) C(11) C(16) 125.9(6) 1_555 1_555 1_555 yes C(15) C(11) C(16) 126.3(7) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 70.7(4) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 71.0(4) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 129.2(5) 1_555 1_555 1_555 yes C(11) C(12) C(13) 107.6(6) 1_555 1_555 1_555 yes C(11) C(12) C(17) 125.3(7) 1_555 1_555 1_555 yes C(13) C(12) C(17) 126.7(8) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 70.7(4) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 70.8(4) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 124.6(5) 1_555 1_555 1_555 yes C(12) C(13) C(14) 108.8(7) 1_555 1_555 1_555 yes C(12) C(13) C(18) 124.4(8) 1_555 1_555 1_555 yes C(14) C(13) C(18) 126.8(7) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 71.3(4) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 71.2(4) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 129.9(5) 1_555 1_555 1_555 yes C(13) C(14) C(15) 107.5(6) 1_555 1_555 1_555 yes C(13) C(14) C(19) 125.1(7) 1_555 1_555 1_555 yes C(15) C(14) C(19) 126.9(7) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 70.6(4) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 70.2(4) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 127.6(5) 1_555 1_555 1_555 yes C(11) C(15) C(14) 108.4(6) 1_555 1_555 1_555 yes C(11) C(15) C(20) 124.6(7) 1_555 1_555 1_555 yes C(14) C(15) C(20) 126.9(7) 1_555 1_555 1_555 yes S(1) C(21) C(22) 111.6(5) 1_555 1_555 1_555 yes S(2) C(22) C(21) 111.2(5) 1_555 1_555 1_555 yes S(3) C(23) C(24) 109.2(5) 1_555 1_555 1_555 yes Cl C(24) C(23) 111.5(6) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir(1) Ir(2) 3.3233(6) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END data_[(Cp*Ir)2(S){SCHPhCH2CH(OH)S}].THF_(9.THF) _database_code_CSD 178529 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Apr 13 02:41:26 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 957.36 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H48 Ir2 O2 S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 22.375(3) _cell_length_b 22.375(3) _cell_length_c 27.148(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13591(3) _cell_formula_units_Z 16 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.5 _cell_measurement_theta_max 19.6 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_Int_Tables_number 88 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2-y,z 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z -x,-y,-z x,1/2+y,-z 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z 1/2-x,-y,1/2+z 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z 1/2+x,y,1/2-z 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7424.00 _exptl_absorpt_coefficient_mu 8.059 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 -2 2 0 -4 -2 0 -4 _diffrn_reflns_number 8354 _reflns_number_total 8354 _reflns_number_gt 4602 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.097 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00781 _diffrn_orient_matrix_UB_12 -0.00059 _diffrn_orient_matrix_UB_13 -0.03627 _diffrn_orient_matrix_UB_21 0.04397 _diffrn_orient_matrix_UB_22 0.00166 _diffrn_orient_matrix_UB_23 -0.00645 _diffrn_orient_matrix_UB_31 0.00173 _diffrn_orient_matrix_UB_32 -0.04466 _diffrn_orient_matrix_UB_33 0.00024 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.19465(2) 0.13145(2) 0.03557(1) 0.0355(1) Uani 1.00 d . . . Ir(2) Ir 0.31961(2) 0.11714(2) -0.03020(1) 0.0407(1) Uani 1.00 d . . . S(1) S 0.2181(1) 0.0898(1) -0.04314(8) 0.0398(7) Uani 1.00 d . . . S(2) S 0.2669(1) 0.1985(1) 0.00352(9) 0.0438(7) Uani 1.00 d . . . S(3) S 0.2872(1) 0.0804(1) 0.04787(9) 0.0469(8) Uani 1.00 d . . . O(1) O 0.1355(3) 0.1218(4) -0.1094(3) 0.061(3) Uani 1.00 d . . . O(2) O 0.414(3) 0.308(4) 0.074(1) 0.37(3) Uani 0.88 d P . . O(3) O 0.355(2) 0.263(1) 0.130(1) 0.30(2) Uani 0.88 d P . . C(1) C 0.1341(5) 0.1890(5) 0.0780(4) 0.055(4) Uani 1.00 d . . . C(2) C 0.1648(5) 0.1475(5) 0.1102(3) 0.055(4) Uani 1.00 d . . . C(3) C 0.1451(5) 0.0882(5) 0.0945(3) 0.049(3) Uani 1.00 d . . . C(4) C 0.1066(5) 0.0937(5) 0.0538(4) 0.049(3) Uani 1.00 d . . . C(5) C 0.0997(5) 0.1571(5) 0.0437(4) 0.051(3) Uani 1.00 d . . . C(6) C 0.1391(7) 0.2551(6) 0.0852(5) 0.091(5) Uani 1.00 d . . . C(7) C 0.2024(6) 0.1611(7) 0.1536(4) 0.085(5) Uani 1.00 d . . . C(8) C 0.1636(6) 0.0324(6) 0.1195(4) 0.075(4) Uani 1.00 d . . . C(9) C 0.0760(5) 0.0456(6) 0.0265(5) 0.071(4) Uani 1.00 d . . . C(10) C 0.0543(5) 0.1827(7) 0.0085(5) 0.091(5) Uani 1.00 d . . . C(11) C 0.3968(5) 0.1604(6) -0.0651(5) 0.067(4) Uani 1.00 d . . . C(12) C 0.4171(5) 0.1226(8) -0.0280(5) 0.073(5) Uani 1.00 d . . . C(13) C 0.3981(5) 0.0622(6) -0.0402(5) 0.064(4) Uani 1.00 d . . . C(14) C 0.3677(5) 0.0635(5) -0.0846(4) 0.053(4) Uani 1.00 d . . . C(15) C 0.3655(5) 0.1246(6) -0.1013(4) 0.059(4) Uani 1.00 d . . . C(16) C 0.4084(7) 0.2258(7) -0.0682(7) 0.122(7) Uani 1.00 d . . . C(17) C 0.4557(7) 0.137(1) 0.0160(6) 0.150(8) Uani 1.00 d . . . C(18) C 0.4120(7) 0.0061(7) -0.0113(6) 0.110(6) Uani 1.00 d . . . C(19) C 0.3412(6) 0.0107(7) -0.1111(5) 0.097(5) Uani 1.00 d . . . C(20) C 0.3421(6) 0.1448(8) -0.1502(4) 0.115(6) Uani 1.00 d . . . C(21) C 0.1914(4) 0.1410(5) -0.0912(3) 0.042(3) Uani 1.00 d . . . C(22) C 0.1815(5) 0.2046(5) -0.0740(4) 0.052(4) Uani 1.00 d . . . C(23) C 0.2352(5) 0.2377(5) -0.0513(4) 0.047(3) Uani 1.00 d . . . C(24) C 0.2213(6) 0.3013(5) -0.0354(4) 0.053(3) Uani 1.00 d . . . C(25) C 0.2679(6) 0.3376(6) -0.0198(4) 0.066(4) Uani 1.00 d . . . C(26) C 0.2576(8) 0.3977(6) -0.0064(5) 0.085(5) Uani 1.00 d . . . C(27) C 0.2018(9) 0.4204(6) -0.0088(5) 0.090(6) Uani 1.00 d . . . C(28) C 0.1576(8) 0.3864(6) -0.0243(5) 0.086(5) Uani 1.00 d . . . C(29) C 0.1652(6) 0.3265(5) -0.0380(4) 0.067(4) Uani 1.00 d . . . C(30) C 0.437(5) 0.304(7) 0.105(2) 0.46(6) Uani 1.00 d . . . C(31) C 0.424(2) 0.262(2) 0.134(2) 0.27(2) Uani 1.00 d . . . C(32) C 0.344(2) 0.317(2) 0.103(1) 0.21(2) Uani 1.00 d . . . H(1) H 0.1797 0.2669 0.0822 0.1093 Uiso 1.00 calc . . . H(2) H 0.1159 0.2751 0.0609 0.1093 Uiso 1.00 calc . . . H(3) H 0.1248 0.2654 0.1170 0.1093 Uiso 1.00 calc . . . H(4) H 0.1829 0.1474 0.1825 0.1019 Uiso 1.00 calc . . . H(5) H 0.2398 0.1415 0.1503 0.1019 Uiso 1.00 calc . . . H(6) H 0.2085 0.2030 0.1557 0.1019 Uiso 1.00 calc . . . H(7) H 0.1509 0.0334 0.1529 0.0904 Uiso 1.00 calc . . . H(8) H 0.1459 -0.0009 0.1034 0.0904 Uiso 1.00 calc . . . H(9) H 0.2059 0.0288 0.1183 0.0904 Uiso 1.00 calc . . . H(10) H 0.0340 0.0500 0.0299 0.0855 Uiso 1.00 calc . . . H(11) H 0.0865 0.0478 -0.0074 0.0855 Uiso 1.00 calc . . . H(12) H 0.0879 0.0079 0.0394 0.0855 Uiso 1.00 calc . . . H(13) H 0.0242 0.2030 0.0266 0.1098 Uiso 1.00 calc . . . H(14) H 0.0735 0.2100 -0.0132 0.1098 Uiso 1.00 calc . . . H(15) H 0.0368 0.1513 -0.0101 0.1098 Uiso 1.00 calc . . . H(16) H 0.4502 0.2327 -0.0700 0.1464 Uiso 1.00 calc . . . H(17) H 0.3896 0.2415 -0.0968 0.1464 Uiso 1.00 calc . . . H(18) H 0.3927 0.2450 -0.0398 0.1464 Uiso 1.00 calc . . . H(19) H 0.4359 0.1252 0.0453 0.1798 Uiso 1.00 calc . . . H(20) H 0.4927 0.1166 0.0133 0.1798 Uiso 1.00 calc . . . H(21) H 0.4629 0.1790 0.0170 0.1798 Uiso 1.00 calc . . . H(22) H 0.3758 -0.0135 -0.0028 0.1315 Uiso 1.00 calc . . . H(23) H 0.4358 -0.0198 -0.0308 0.1315 Uiso 1.00 calc . . . H(24) H 0.4331 0.0163 0.0179 0.1315 Uiso 1.00 calc . . . H(25) H 0.3123 -0.0079 -0.0906 0.1164 Uiso 1.00 calc . . . H(26) H 0.3228 0.0238 -0.1407 0.1164 Uiso 1.00 calc . . . H(27) H 0.3720 -0.0171 -0.1187 0.1164 Uiso 1.00 calc . . . H(28) H 0.3451 0.1871 -0.1525 0.1384 Uiso 1.00 calc . . . H(29) H 0.3649 0.1270 -0.1758 0.1384 Uiso 1.00 calc . . . H(30) H 0.3014 0.1333 -0.1534 0.1384 Uiso 1.00 calc . . . H(31) H 0.213(3) 0.138(3) -0.120(2) 0.01(1) Uiso 1.00 calc . . . H(32) H 0.139(4) 0.081(4) -0.124(3) 0.043(10) Uiso 1.00 calc . . . H(33) H 0.151(4) 0.208(4) -0.048(3) 0.056(8) Uiso 1.00 calc . . . H(34) H 0.171(5) 0.232(5) -0.104(4) 0.089(7) Uiso 1.00 calc . . . H(35) H 0.266(4) 0.236(4) -0.072(3) 0.03(1) Uiso 1.00 calc . . . H(36) H 0.3072 0.3218 -0.0181 0.0787 Uiso 1.00 calc . . . H(37) H 0.2899 0.4221 0.0042 0.1022 Uiso 1.00 calc . . . H(38) H 0.1945 0.4606 0.0007 0.1076 Uiso 1.00 calc . . . H(39) H 0.1188 0.4033 -0.0263 0.1030 Uiso 1.00 calc . . . H(40) H 0.1321 0.3035 -0.0490 0.0802 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0397(2) 0.0363(2) 0.0305(2) 0.0052(2) 0.0030(2) -0.0028(2) Ir(2) 0.0336(2) 0.0512(3) 0.0372(2) -0.0015(2) 0.0011(2) -0.0047(2) S(1) 0.038(1) 0.048(2) 0.034(1) -0.001(1) 0.001(1) -0.007(1) S(2) 0.047(2) 0.042(2) 0.042(1) -0.007(1) 0.000(1) -0.004(1) S(3) 0.045(2) 0.058(2) 0.038(1) 0.012(1) -0.001(1) 0.004(1) O(1) 0.053(5) 0.068(6) 0.062(5) 0.009(5) -0.015(4) -0.020(4) O(2) 0.37(5) 0.54(6) 0.19(3) -0.22(5) 0.13(4) 0.02(5) O(3) 0.25(3) 0.23(3) 0.42(4) -0.01(3) -0.02(3) 0.11(3) C(1) 0.068(8) 0.045(7) 0.053(6) 0.008(7) 0.019(6) 0.005(6) C(2) 0.069(8) 0.066(8) 0.030(5) -0.014(7) 0.017(5) -0.014(5) C(3) 0.048(7) 0.061(8) 0.039(5) 0.017(6) 0.015(5) 0.011(5) C(4) 0.050(7) 0.040(7) 0.059(7) 0.007(6) 0.016(5) -0.005(5) C(5) 0.049(7) 0.059(8) 0.044(6) 0.016(6) 0.007(5) 0.003(5) C(6) 0.12(1) 0.054(8) 0.10(1) 0.011(9) 0.049(9) -0.016(8) C(7) 0.09(1) 0.12(1) 0.042(7) -0.013(10) -0.005(7) -0.022(7) C(8) 0.09(1) 0.071(9) 0.064(8) 0.021(8) 0.018(7) 0.025(7) C(9) 0.047(7) 0.067(8) 0.100(10) -0.010(7) 0.013(7) -0.023(8) C(10) 0.053(8) 0.14(1) 0.086(10) 0.048(9) 0.002(7) 0.026(9) C(11) 0.045(8) 0.065(9) 0.090(9) -0.017(7) 0.020(7) 0.000(8) C(12) 0.028(6) 0.13(1) 0.062(8) -0.013(8) 0.003(6) -0.015(9) C(13) 0.040(7) 0.079(10) 0.074(8) 0.015(7) 0.007(6) 0.013(8) C(14) 0.031(6) 0.065(8) 0.063(7) -0.002(6) 0.021(5) -0.016(6) C(15) 0.045(7) 0.088(10) 0.044(6) 0.004(7) 0.019(5) 0.008(6) C(16) 0.09(1) 0.08(1) 0.20(2) -0.04(1) 0.06(1) -0.01(1) C(17) 0.06(1) 0.27(3) 0.12(1) -0.01(1) -0.037(10) -0.06(2) C(18) 0.09(1) 0.11(1) 0.13(1) 0.03(1) 0.03(1) 0.03(1) C(19) 0.08(1) 0.10(1) 0.10(1) -0.039(9) 0.048(9) -0.065(9) C(20) 0.08(1) 0.21(2) 0.052(8) 0.05(1) 0.030(8) 0.036(10) C(21) 0.027(6) 0.060(8) 0.040(5) 0.000(5) -0.004(4) -0.008(5) C(22) 0.055(8) 0.060(8) 0.039(6) 0.017(7) -0.009(5) 0.010(6) C(23) 0.054(7) 0.041(7) 0.046(6) 0.007(6) 0.006(5) 0.009(5) C(24) 0.074(8) 0.038(6) 0.046(6) -0.005(6) 0.021(6) 0.006(5) C(25) 0.09(1) 0.054(8) 0.055(7) -0.010(8) 0.016(7) 0.002(6) C(26) 0.14(2) 0.056(9) 0.057(8) -0.01(1) 0.013(9) 0.018(7) C(27) 0.16(2) 0.058(10) 0.048(8) 0.00(1) 0.008(10) -0.010(7) C(28) 0.13(1) 0.058(9) 0.070(9) 0.029(10) 0.009(9) 0.003(8) C(29) 0.087(10) 0.058(8) 0.055(7) 0.018(8) 0.005(7) 0.011(6) C(30) 0.6(2) 0.6(1) 0.16(5) -0.3(1) 0.10(6) -0.02(7) C(31) 0.20(4) 0.28(4) 0.31(5) -0.03(3) -0.02(3) 0.16(3) C(32) 0.20(3) 0.24(3) 0.20(3) 0.10(3) -0.05(3) 0.00(3) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00014|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.000030(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4602 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0389 _refine_ls_wR_factor_gt 0.0389 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.319 _refine_ls_shift/su_max 0.4300 _refine_ls_shift/su_mean 0.0240 _refine_diff_density_min -1.38 _refine_diff_density_max 1.29 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) S(1) 2.389(2) 1_555 1_555 yes Ir(1) S(2) 2.371(3) 1_555 1_555 yes Ir(1) S(3) 2.388(3) 1_555 1_555 yes Ir(1) C(1) 2.20(1) 1_555 1_555 yes Ir(1) C(2) 2.164(9) 1_555 1_555 yes Ir(1) C(3) 2.175(10) 1_555 1_555 yes Ir(1) C(4) 2.20(1) 1_555 1_555 yes Ir(1) C(5) 2.21(1) 1_555 1_555 yes Ir(2) S(1) 2.378(3) 1_555 1_555 yes Ir(2) S(2) 2.354(3) 1_555 1_555 yes Ir(2) S(3) 2.386(3) 1_555 1_555 yes Ir(2) C(11) 2.19(1) 1_555 1_555 yes Ir(2) C(12) 2.19(1) 1_555 1_555 yes Ir(2) C(13) 2.16(1) 1_555 1_555 yes Ir(2) C(14) 2.185(10) 1_555 1_555 yes Ir(2) C(15) 2.192(10) 1_555 1_555 yes S(1) C(21) 1.83(1) 1_555 1_555 yes S(2) C(23) 1.87(1) 1_555 1_555 yes O(1) C(21) 1.41(1) 1_555 1_555 yes O(2) C(30) 1.0(1) 1_555 1_555 yes O(2) C(32) 1.77(7) 1_555 1_555 yes O(3) C(31) 1.53(4) 1_555 1_555 yes O(3) C(32) 1.45(3) 1_555 1_555 yes C(1) C(2) 1.45(1) 1_555 1_555 yes C(1) C(5) 1.40(1) 1_555 1_555 yes C(1) C(6) 1.50(2) 1_555 1_555 yes C(2) C(3) 1.46(1) 1_555 1_555 yes C(2) C(7) 1.48(1) 1_555 1_555 yes C(3) C(4) 1.41(1) 1_555 1_555 yes C(3) C(8) 1.48(1) 1_555 1_555 yes C(4) C(5) 1.45(1) 1_555 1_555 yes C(4) C(9) 1.48(1) 1_555 1_555 yes C(5) C(10) 1.51(1) 1_555 1_555 yes C(11) C(12) 1.39(2) 1_555 1_555 yes C(11) C(15) 1.45(2) 1_555 1_555 yes C(11) C(16) 1.49(2) 1_555 1_555 yes C(12) C(13) 1.45(2) 1_555 1_555 yes C(12) C(17) 1.51(2) 1_555 1_555 yes C(13) C(14) 1.39(1) 1_555 1_555 yes C(13) C(18) 1.51(2) 1_555 1_555 yes C(14) C(15) 1.44(2) 1_555 1_555 yes C(14) C(19) 1.51(2) 1_555 1_555 yes C(15) C(20) 1.50(2) 1_555 1_555 yes C(21) C(22) 1.51(1) 1_555 1_555 yes C(22) C(23) 1.54(2) 1_555 1_555 yes C(23) C(24) 1.52(1) 1_555 1_555 yes C(24) C(25) 1.39(2) 1_555 1_555 yes C(24) C(29) 1.38(2) 1_555 1_555 yes C(25) C(26) 1.41(2) 1_555 1_555 yes C(26) C(27) 1.35(2) 1_555 1_555 yes C(27) C(28) 1.32(2) 1_555 1_555 yes C(28) C(29) 1.40(2) 1_555 1_555 yes C(30) C(31) 1.26(10) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 76.62(9) 1_555 1_555 1_555 yes S(1) Ir(1) S(3) 75.42(9) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 146.5(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 166.0(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 126.7(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 104.4(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 113.7(3) 1_555 1_555 1_555 yes S(2) Ir(1) S(3) 76.26(10) 1_555 1_555 1_555 yes S(2) Ir(1) C(1) 104.0(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(2) 116.7(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(3) 154.1(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(4) 159.4(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 121.9(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(1) 137.9(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(2) 102.5(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(3) 97.3(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(4) 124.2(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(5) 160.6(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 38.8(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 63.9(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 63.6(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 37.2(4) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 39.4(4) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 65.0(4) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 64.4(4) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 37.5(4) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 63.4(4) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38.4(4) 1_555 1_555 1_555 yes S(1) Ir(2) S(2) 77.16(9) 1_555 1_555 1_555 yes S(1) Ir(2) S(3) 75.65(9) 1_555 1_555 1_555 yes S(1) Ir(2) C(11) 143.3(4) 1_555 1_555 1_555 yes S(1) Ir(2) C(12) 166.3(4) 1_555 1_555 1_555 yes S(1) Ir(2) C(13) 127.7(4) 1_555 1_555 1_555 yes S(1) Ir(2) C(14) 103.3(3) 1_555 1_555 1_555 yes S(1) Ir(2) C(15) 109.7(3) 1_555 1_555 1_555 yes S(2) Ir(2) S(3) 76.61(9) 1_555 1_555 1_555 yes S(2) Ir(2) C(11) 102.8(4) 1_555 1_555 1_555 yes S(2) Ir(2) C(12) 116.5(4) 1_555 1_555 1_555 yes S(2) Ir(2) C(13) 153.6(4) 1_555 1_555 1_555 yes S(2) Ir(2) C(14) 159.0(3) 1_555 1_555 1_555 yes S(2) Ir(2) C(15) 121.2(4) 1_555 1_555 1_555 yes S(3) Ir(2) C(11) 140.8(4) 1_555 1_555 1_555 yes S(3) Ir(2) C(12) 107.3(4) 1_555 1_555 1_555 yes S(3) Ir(2) C(13) 99.4(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(14) 124.1(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(15) 161.9(3) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 37.0(5) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 63.7(5) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 64.1(4) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 38.5(4) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 39.0(5) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 63.8(4) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 63.4(4) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 37.2(4) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 63.4(4) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38.4(4) 1_555 1_555 1_555 yes Ir(1) S(1) Ir(2) 88.71(8) 1_555 1_555 1_555 yes Ir(1) S(1) C(21) 108.7(3) 1_555 1_555 1_555 yes Ir(2) S(1) C(21) 104.8(3) 1_555 1_555 1_555 yes Ir(1) S(2) Ir(2) 89.73(9) 1_555 1_555 1_555 yes Ir(1) S(2) C(23) 109.3(4) 1_555 1_555 1_555 yes Ir(2) S(2) C(23) 104.1(3) 1_555 1_555 1_555 yes Ir(1) S(3) Ir(2) 88.56(9) 1_555 1_555 1_555 yes C(21) O(1) H(32) 110(5) 1_555 1_555 1_555 no C(30) O(2) C(32) 95(7) 1_555 1_555 1_555 yes C(31) O(3) C(32) 102(3) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 69.4(6) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 72.0(6) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 127.1(9) 1_555 1_555 1_555 yes C(2) C(1) C(5) 109.5(10) 1_555 1_555 1_555 yes C(2) C(1) C(6) 121(1) 1_555 1_555 1_555 yes C(5) C(1) C(6) 129(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 71.8(6) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 70.7(5) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 127.2(9) 1_555 1_555 1_555 yes C(1) C(2) C(3) 105.2(9) 1_555 1_555 1_555 yes C(1) C(2) C(7) 128(1) 1_555 1_555 1_555 yes C(3) C(2) C(7) 126(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 69.9(6) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 72.2(6) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 124.7(8) 1_555 1_555 1_555 yes C(2) C(3) C(4) 109.6(10) 1_555 1_555 1_555 yes C(2) C(3) C(8) 123(1) 1_555 1_555 1_555 yes C(4) C(3) C(8) 127(1) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 70.3(6) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 71.2(6) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 125.7(7) 1_555 1_555 1_555 yes C(3) C(4) C(5) 107.4(10) 1_555 1_555 1_555 yes C(3) C(4) C(9) 127(1) 1_555 1_555 1_555 yes C(5) C(4) C(9) 124(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 70.9(6) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 70.4(6) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 133.1(8) 1_555 1_555 1_555 yes C(1) C(5) C(4) 108.3(10) 1_555 1_555 1_555 yes C(1) C(5) C(10) 126(1) 1_555 1_555 1_555 yes C(4) C(5) C(10) 124(1) 1_555 1_555 1_555 yes Ir(2) C(11) C(12) 71.1(7) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 70.6(6) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 126.5(9) 1_555 1_555 1_555 yes C(12) C(11) C(15) 108(1) 1_555 1_555 1_555 yes C(12) C(11) C(16) 125(1) 1_555 1_555 1_555 yes C(15) C(11) C(16) 126(1) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 71.8(7) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 69.6(6) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 127.3(9) 1_555 1_555 1_555 yes C(11) C(12) C(13) 107(1) 1_555 1_555 1_555 yes C(11) C(12) C(17) 128(1) 1_555 1_555 1_555 yes C(13) C(12) C(17) 123(1) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 71.4(7) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 72.3(6) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 125.0(9) 1_555 1_555 1_555 yes C(12) C(13) C(14) 108(1) 1_555 1_555 1_555 yes C(12) C(13) C(18) 126(1) 1_555 1_555 1_555 yes C(14) C(13) C(18) 124(1) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 70.5(6) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 71.1(6) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 124.1(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 108(1) 1_555 1_555 1_555 yes C(13) C(14) C(19) 126(1) 1_555 1_555 1_555 yes C(15) C(14) C(19) 125(1) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 70.8(6) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 70.5(6) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 129.8(8) 1_555 1_555 1_555 yes C(11) C(15) C(14) 107(1) 1_555 1_555 1_555 yes C(11) C(15) C(20) 127(1) 1_555 1_555 1_555 yes C(14) C(15) C(20) 125(1) 1_555 1_555 1_555 yes S(1) C(21) O(1) 110.4(7) 1_555 1_555 1_555 yes S(1) C(21) C(22) 114.5(7) 1_555 1_555 1_555 yes S(1) C(21) H(31) 112(4) 1_555 1_555 1_555 no O(1) C(21) C(22) 105.3(9) 1_555 1_555 1_555 yes O(1) C(21) H(31) 98(4) 1_555 1_555 1_555 no C(22) C(21) H(31) 114(4) 1_555 1_555 1_555 no C(21) C(22) C(23) 117.5(9) 1_555 1_555 1_555 yes C(21) C(22) H(33) 112(6) 1_555 1_555 1_555 no C(21) C(22) H(34) 109(5) 1_555 1_555 1_555 no C(23) C(22) H(33) 103(5) 1_555 1_555 1_555 no C(23) C(22) H(34) 101(6) 1_555 1_555 1_555 no H(33) C(22) H(34) 111(8) 1_555 1_555 1_555 no S(2) C(23) C(22) 112.8(7) 1_555 1_555 1_555 yes S(2) C(23) C(24) 106.9(7) 1_555 1_555 1_555 yes S(2) C(23) H(35) 100(5) 1_555 1_555 1_555 no C(22) C(23) C(24) 114.0(10) 1_555 1_555 1_555 yes C(22) C(23) H(35) 108(5) 1_555 1_555 1_555 no C(24) C(23) H(35) 112(5) 1_555 1_555 1_555 no C(23) C(24) C(25) 118(1) 1_555 1_555 1_555 yes C(23) C(24) C(29) 123(1) 1_555 1_555 1_555 yes C(25) C(24) C(29) 117(1) 1_555 1_555 1_555 yes C(24) C(25) C(26) 120(1) 1_555 1_555 1_555 yes C(25) C(26) C(27) 119(1) 1_555 1_555 1_555 yes C(26) C(27) C(28) 119(1) 1_555 1_555 1_555 yes C(27) C(28) C(29) 123(1) 1_555 1_555 1_555 yes C(24) C(29) C(28) 119(1) 1_555 1_555 1_555 yes O(2) C(30) C(31) 118(12) 1_555 1_555 1_555 yes O(3) C(31) C(30) 100(6) 1_555 1_555 1_555 yes O(2) C(32) O(3) 87(3) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir(1) Ir(2) 3.3328(6) 1_555 1_555 ? S(3) O(1) 3.240(8) 1_555 4_555 ? S(3) H(32) 2.43(9) 1_555 4_555 ? #------------------------------------------------------------------------------ #===END data_[Cp*Ir(S2C2H4)]2_(10) _database_code_CSD 178530 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Dec 23 01:14:01 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 839.24 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H38 Ir2 S4 ' _chemical_formula_moiety 'C24 H38 Ir2 S4 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 8.4984(7) _cell_length_b 17.147(2) _cell_length_c 18.213(2) _cell_angle_alpha 90 _cell_angle_beta 98.384(9) _cell_angle_gamma 90 _cell_volume 2625.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.2 _cell_measurement_theta_max 19.4 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600.00 _exptl_absorpt_coefficient_mu 10.483 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.464 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.28 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 2 -2 0 -2 -1 1 2 _diffrn_reflns_number 3217 _reflns_number_total 3019 _reflns_number_gt 2359 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.11342 _diffrn_orient_matrix_UB_12 -0.01536 _diffrn_orient_matrix_UB_13 0.00029 _diffrn_orient_matrix_UB_21 0.01967 _diffrn_orient_matrix_UB_22 -0.00311 _diffrn_orient_matrix_UB_23 0.05541 _diffrn_orient_matrix_UB_31 -0.02994 _diffrn_orient_matrix_UB_32 0.05618 _diffrn_orient_matrix_UB_33 0.00313 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.10949(2) 0.11203(1) 0.34411(1) 0.02679(5) Uani 1.00 d . . . S(1) S 0.1559(1) 0.10532(8) 0.21953(7) 0.0341(3) Uani 1.00 d . . . S(2) S 0.1661(2) -0.02255(8) 0.35167(9) 0.0500(4) Uani 1.00 d . . . C(1) C 0.2629(6) 0.2135(3) 0.3776(3) 0.039(2) Uani 1.00 d . . . C(2) C 0.1044(6) 0.2315(3) 0.3892(3) 0.039(1) Uani 1.00 d . . . C(3) C 0.0600(6) 0.1780(3) 0.4421(3) 0.036(1) Uani 1.00 d . . . C(4) C 0.1898(6) 0.1277(3) 0.4639(3) 0.034(1) Uani 1.00 d . . . C(5) C 0.3169(6) 0.1484(3) 0.4232(3) 0.037(1) Uani 1.00 d . . . C(6) C 0.3616(8) 0.2563(4) 0.3280(4) 0.062(2) Uani 1.00 d . . . C(7) C 0.0041(8) 0.2990(3) 0.3554(4) 0.061(2) Uani 1.00 d . . . C(8) C -0.0937(6) 0.1790(4) 0.4722(4) 0.055(2) Uani 1.00 d . . . C(9) C 0.1998(7) 0.0651(4) 0.5230(3) 0.053(2) Uani 1.00 d . . . C(10) C 0.4776(7) 0.1109(4) 0.4328(4) 0.059(2) Uani 1.00 d . . . C(11) C 0.2453(9) 0.0092(5) 0.2130(4) 0.074(3) Uani 1.00 d . . . C(12a) C 0.293(2) -0.0326(7) 0.2805(7) 0.060(4) Uani 0.60 d P . . C(12b) C 0.195(2) -0.046(1) 0.257(1) 0.062(5) Uani 0.40 d P . . H(1) H 0.4540 0.2769 0.3571 0.0746 Uiso 1.00 calc . . . H(2) H 0.3922 0.2211 0.2923 0.0746 Uiso 1.00 calc . . . H(3) H 0.3009 0.2975 0.3033 0.0746 Uiso 1.00 calc . . . H(4) H -0.0174 0.3334 0.3936 0.0735 Uiso 1.00 calc . . . H(5) H 0.0600 0.3262 0.3218 0.0735 Uiso 1.00 calc . . . H(6) H -0.0933 0.2797 0.3295 0.0735 Uiso 1.00 calc . . . H(7) H -0.1045 0.2271 0.4967 0.0658 Uiso 1.00 calc . . . H(8) H -0.1790 0.1731 0.4326 0.0658 Uiso 1.00 calc . . . H(9) H -0.0957 0.1373 0.5063 0.0658 Uiso 1.00 calc . . . H(10) H 0.1012 0.0619 0.5416 0.0632 Uiso 1.00 calc . . . H(11) H 0.2225 0.0163 0.5021 0.0632 Uiso 1.00 calc . . . H(12) H 0.2820 0.0777 0.5623 0.0632 Uiso 1.00 calc . . . H(13) H 0.4665 0.0569 0.4215 0.0704 Uiso 1.00 calc . . . H(14) H 0.5410 0.1348 0.4002 0.0704 Uiso 1.00 calc . . . H(15) H 0.5273 0.1172 0.4826 0.0704 Uiso 1.00 calc . . . H(16a) H 0.1694 -0.0224 0.1830 0.0894 Uiso 0.60 calc P . . H(16b) H 0.2208 -0.0082 0.1630 0.0894 Uiso 0.40 calc P . . H(17a) H 0.3363 0.0157 0.1889 0.0894 Uiso 0.60 calc P . . H(17b) H 0.3571 0.0144 0.2256 0.0894 Uiso 0.40 calc P . . H(18) H 0.3004 -0.0865 0.2693 0.0702 Uiso 1.00 calc . . . H(19a) H 0.3976 -0.0145 0.3013 0.0702 Uiso 0.60 calc P . . H(19b) H 0.0960 -0.0642 0.2327 0.0747 Uiso 0.40 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir 0.02892(10) 0.0285(1) 0.0221(1) 0.00180(9) 0.00072(6) -0.00120(9) S(1) 0.0297(6) 0.0481(7) 0.0241(6) 0.0024(6) 0.0030(5) -0.0019(6) S(2) 0.0681(10) 0.0333(7) 0.0449(9) 0.0102(7) -0.0044(8) 0.0031(7) C(1) 0.043(3) 0.038(3) 0.035(3) -0.012(2) 0.004(2) -0.006(2) C(2) 0.048(3) 0.029(3) 0.035(3) 0.001(2) -0.003(2) -0.008(2) C(3) 0.033(3) 0.041(3) 0.034(3) -0.002(2) 0.004(2) -0.013(2) C(4) 0.039(3) 0.040(3) 0.023(3) -0.008(2) 0.001(2) -0.005(2) C(5) 0.033(3) 0.044(3) 0.030(3) 0.000(2) -0.003(2) -0.003(2) C(6) 0.079(5) 0.063(4) 0.047(4) -0.033(4) 0.017(4) -0.001(3) C(7) 0.087(5) 0.040(3) 0.053(4) 0.016(3) -0.005(4) -0.007(3) C(8) 0.043(3) 0.076(5) 0.049(4) -0.003(3) 0.017(3) -0.021(3) C(9) 0.068(4) 0.055(4) 0.032(3) -0.010(3) -0.005(3) 0.002(3) C(10) 0.039(3) 0.088(5) 0.046(4) 0.004(3) -0.004(3) -0.015(4) C(11) 0.083(5) 0.098(6) 0.043(4) 0.062(5) 0.011(4) -0.005(4) C(12a) 0.085(9) 0.055(7) 0.043(7) 0.044(7) 0.016(6) 0.000(6) C(12b) 0.07(1) 0.05(1) 0.05(1) 0.041(9) -0.042(9) -0.026(9) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00080(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2359 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0222 _refine_ls_wR_factor_gt 0.0222 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_shift/su_max 0.0480 _refine_ls_shift/su_mean 0.0040 _refine_diff_density_min -0.71 _refine_diff_density_max 0.68 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir S(1) 2.362(1) 1_555 1_555 yes Ir S(1) 2.383(1) 1_555 2_555 yes Ir S(2) 2.357(1) 1_555 1_555 yes Ir C(1) 2.207(5) 1_555 1_555 yes Ir C(2) 2.210(5) 1_555 1_555 yes Ir C(3) 2.204(5) 1_555 1_555 yes Ir C(4) 2.205(5) 1_555 1_555 yes Ir C(5) 2.197(5) 1_555 1_555 yes S(1) C(11) 1.827(7) 1_555 1_555 yes S(2) C(12a) 1.81(1) 1_555 1_555 yes S(2) C(12b) 1.82(2) 1_555 1_555 yes C(1) C(2) 1.428(7) 1_555 1_555 yes C(1) C(5) 1.427(7) 1_555 1_555 yes C(1) C(6) 1.510(8) 1_555 1_555 yes C(2) C(3) 1.420(7) 1_555 1_555 yes C(2) C(7) 1.513(8) 1_555 1_555 yes C(3) C(4) 1.411(7) 1_555 1_555 yes C(3) C(8) 1.489(7) 1_555 1_555 yes C(4) C(5) 1.441(7) 1_555 1_555 yes C(4) C(9) 1.513(7) 1_555 1_555 yes C(5) C(10) 1.496(7) 1_555 1_555 yes C(11) C(12a) 1.43(1) 1_555 1_555 yes C(11) C(12b) 1.36(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir S(1) 78.99(4) 1_555 1_555 2_555 yes S(1) Ir S(2) 86.97(5) 1_555 1_555 1_555 yes S(1) Ir C(1) 97.4(1) 1_555 1_555 1_555 yes S(1) Ir C(2) 114.7(2) 1_555 1_555 1_555 yes S(1) Ir C(3) 151.8(1) 1_555 1_555 1_555 yes S(1) Ir C(4) 152.3(1) 1_555 1_555 1_555 yes S(1) Ir C(5) 114.4(1) 1_555 1_555 1_555 yes S(1) Ir S(2) 98.73(5) 2_555 1_555 1_555 yes S(1) Ir C(1) 130.7(1) 2_555 1_555 1_555 yes S(1) Ir C(2) 99.0(1) 2_555 1_555 1_555 yes S(1) Ir C(3) 98.0(1) 2_555 1_555 1_555 yes S(1) Ir C(4) 128.4(1) 2_555 1_555 1_555 yes S(1) Ir C(5) 160.8(1) 2_555 1_555 1_555 yes S(2) Ir C(1) 130.4(1) 1_555 1_555 1_555 yes S(2) Ir C(2) 154.3(1) 1_555 1_555 1_555 yes S(2) Ir C(3) 121.1(1) 1_555 1_555 1_555 yes S(2) Ir C(4) 91.7(1) 1_555 1_555 1_555 yes S(2) Ir C(5) 95.8(1) 1_555 1_555 1_555 yes C(1) Ir C(2) 37.7(2) 1_555 1_555 1_555 yes C(1) Ir C(3) 63.0(2) 1_555 1_555 1_555 yes C(1) Ir C(4) 63.0(2) 1_555 1_555 1_555 yes C(1) Ir C(5) 37.8(2) 1_555 1_555 1_555 yes C(2) Ir C(3) 37.5(2) 1_555 1_555 1_555 yes C(2) Ir C(4) 62.6(2) 1_555 1_555 1_555 yes C(2) Ir C(5) 63.3(2) 1_555 1_555 1_555 yes C(3) Ir C(4) 37.3(2) 1_555 1_555 1_555 yes C(3) Ir C(5) 63.5(2) 1_555 1_555 1_555 yes C(4) Ir C(5) 38.2(2) 1_555 1_555 1_555 yes Ir S(1) Ir 100.74(4) 1_555 1_555 2_555 yes Ir S(1) C(11) 103.7(2) 1_555 1_555 1_555 yes Ir S(1) C(11) 112.7(3) 2_555 1_555 1_555 yes Ir S(2) C(12a) 100.9(4) 1_555 1_555 1_555 yes Ir S(2) C(12b) 102.7(6) 1_555 1_555 1_555 yes Ir C(1) C(2) 71.3(3) 1_555 1_555 1_555 yes Ir C(1) C(5) 70.7(3) 1_555 1_555 1_555 yes Ir C(1) C(6) 125.1(4) 1_555 1_555 1_555 yes C(2) C(1) C(5) 108.3(5) 1_555 1_555 1_555 yes C(2) C(1) C(6) 127.0(5) 1_555 1_555 1_555 yes C(5) C(1) C(6) 124.7(5) 1_555 1_555 1_555 yes Ir C(2) C(1) 71.0(3) 1_555 1_555 1_555 yes Ir C(2) C(3) 71.0(3) 1_555 1_555 1_555 yes Ir C(2) C(7) 126.7(4) 1_555 1_555 1_555 yes C(1) C(2) C(3) 108.1(5) 1_555 1_555 1_555 yes C(1) C(2) C(7) 126.3(5) 1_555 1_555 1_555 yes C(3) C(2) C(7) 125.5(5) 1_555 1_555 1_555 yes Ir C(3) C(2) 71.4(3) 1_555 1_555 1_555 yes Ir C(3) C(4) 71.4(3) 1_555 1_555 1_555 yes Ir C(3) C(8) 125.8(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 108.2(4) 1_555 1_555 1_555 yes C(2) C(3) C(8) 125.2(5) 1_555 1_555 1_555 yes C(4) C(3) C(8) 126.5(5) 1_555 1_555 1_555 yes Ir C(4) C(3) 71.3(3) 1_555 1_555 1_555 yes Ir C(4) C(5) 70.6(3) 1_555 1_555 1_555 yes Ir C(4) C(9) 126.5(4) 1_555 1_555 1_555 yes C(3) C(4) C(5) 108.5(5) 1_555 1_555 1_555 yes C(3) C(4) C(9) 126.5(5) 1_555 1_555 1_555 yes C(5) C(4) C(9) 124.9(5) 1_555 1_555 1_555 yes Ir C(5) C(1) 71.4(3) 1_555 1_555 1_555 yes Ir C(5) C(4) 71.2(3) 1_555 1_555 1_555 yes Ir C(5) C(10) 125.9(4) 1_555 1_555 1_555 yes C(1) C(5) C(4) 106.9(4) 1_555 1_555 1_555 yes C(1) C(5) C(10) 127.9(5) 1_555 1_555 1_555 yes C(4) C(5) C(10) 125.0(5) 1_555 1_555 1_555 yes S(1) C(11) C(12a) 117.6(6) 1_555 1_555 1_555 yes S(1) C(11) C(12b) 115.2(8) 1_555 1_555 1_555 yes S(2) C(12a) C(11) 116.5(7) 1_555 1_555 1_555 yes S(2) C(12b) C(11) 119(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir Ir 3.6544(4) 1_555 2_555 ? #------------------------------------------------------------------------------ #===END data_[(Cp*Ir)2(S)(SCH2CH2CN)2]_(3) _database_code_CSD 172894 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Aug 26 13:06:20 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 859.22 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H38 Ir2 N2 S3 ' _chemical_formula_moiety 'C26 H38 Ir2 N2 S3 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.384(4) _cell_length_b 16.097(3) _cell_length_c 16.368(2) _cell_angle_alpha 90 _cell_angle_beta 104.93(2) _cell_angle_gamma 90 _cell_volume 2898(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.7 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640.00 _exptl_absorpt_coefficient_mu 9.433 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.221 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.26 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 -2 1 -2 -3 1 -2 -1 _diffrn_reflns_number 6977 _reflns_number_total 6650 _reflns_number_gt 5510 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08110 _diffrn_orient_matrix_UB_12 -0.02705 _diffrn_orient_matrix_UB_13 0.00715 _diffrn_orient_matrix_UB_21 0.00004 _diffrn_orient_matrix_UB_22 -0.01657 _diffrn_orient_matrix_UB_23 0.05889 _diffrn_orient_matrix_UB_31 -0.04109 _diffrn_orient_matrix_UB_32 -0.05341 _diffrn_orient_matrix_UB_33 -0.02189 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ir' 'Ir' -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.34319(3) 0.27137(2) 0.29011(2) 0.03382(10) Uani 1.00 d . . . Ir(2) Ir 0.06997(3) 0.20656(2) 0.29996(2) 0.03255(10) Uani 1.00 d . . . S(1) S 0.2269(2) 0.1485(1) 0.2457(1) 0.0393(6) Uani 1.00 d . . . S(2) S 0.2477(2) 0.2523(1) 0.4032(1) 0.0374(6) Uani 1.00 d . . . S(3) S 0.1401(2) 0.3158(2) 0.2262(2) 0.0431(6) Uani 1.00 d . . . N(1) N 0.374(1) -0.0891(7) 0.4619(8) 0.091(4) Uani 1.00 d . . . N(2) N 0.180(2) 0.5162(9) 0.5572(9) 0.137(7) Uani 1.00 d . . . C(1) C 0.4342(9) 0.3515(8) 0.2187(7) 0.055(3) Uani 1.00 d . . . C(2) C 0.4754(8) 0.2700(7) 0.2144(6) 0.047(3) Uani 1.00 d . . . C(3) C 0.5358(9) 0.2420(7) 0.3007(6) 0.048(3) Uani 1.00 d . . . C(4) C 0.5295(10) 0.3102(7) 0.3556(6) 0.047(3) Uani 1.00 d . . . C(5) C 0.4653(9) 0.3774(6) 0.3059(6) 0.048(3) Uani 1.00 d . . . C(6) C 0.369(1) 0.404(1) 0.1442(9) 0.093(5) Uani 1.00 d . . . C(7) C 0.468(1) 0.217(1) 0.1383(8) 0.084(5) Uani 1.00 d . . . C(8) C 0.601(1) 0.1605(8) 0.3240(8) 0.066(4) Uani 1.00 d . . . C(9) C 0.584(1) 0.3111(8) 0.4477(7) 0.063(4) Uani 1.00 d . . . C(10) C 0.448(1) 0.4617(8) 0.3386(9) 0.079(5) Uani 1.00 d . . . C(11) C -0.118(1) 0.2042(10) 0.2280(8) 0.070(4) Uani 1.00 d . . . C(12) C -0.078(1) 0.1215(8) 0.2439(7) 0.062(4) Uani 1.00 d . . . C(13) C -0.045(1) 0.1071(7) 0.3324(8) 0.060(4) Uani 1.00 d . . . C(14) C -0.0644(9) 0.1828(9) 0.3722(6) 0.058(3) Uani 1.00 d . . . C(15) C -0.108(1) 0.2440(8) 0.3088(9) 0.062(4) Uani 1.00 d . . . C(16) C -0.168(2) 0.247(2) 0.146(1) 0.164(9) Uani 1.00 d . . . C(17) C -0.077(2) 0.060(1) 0.176(1) 0.146(9) Uani 1.00 d . . . C(18) C -0.010(2) 0.025(1) 0.375(1) 0.128(8) Uani 1.00 d . . . C(19) C -0.050(2) 0.189(2) 0.4671(10) 0.146(9) Uani 1.00 d . . . C(20) C -0.150(1) 0.3296(10) 0.322(2) 0.145(8) Uani 1.00 d . . . C(21) C 0.289(1) 0.0536(6) 0.3009(7) 0.052(3) Uani 1.00 d . . . C(22) C 0.323(1) 0.0582(7) 0.3957(7) 0.056(3) Uani 1.00 d . . . C(23) C 0.353(1) -0.0247(8) 0.4337(8) 0.070(4) Uani 1.00 d . . . C(24) C 0.230(1) 0.3589(6) 0.4347(6) 0.051(3) Uani 1.00 d . . . C(25) C 0.159(1) 0.3671(7) 0.5015(7) 0.060(4) Uani 1.00 d . . . C(26) C 0.169(1) 0.4516(9) 0.5340(8) 0.079(5) Uani 1.00 d . . . H(1) H 0.3491 0.4566 0.1641 0.1116 Uiso 1.00 calc . . . H(2) H 0.4200 0.4123 0.1074 0.1116 Uiso 1.00 calc . . . H(3) H 0.2963 0.3769 0.1147 0.1116 Uiso 1.00 calc . . . H(4) H 0.4217 0.1689 0.1415 0.1002 Uiso 1.00 calc . . . H(5) H 0.4302 0.2478 0.0889 0.1002 Uiso 1.00 calc . . . H(6) H 0.5477 0.2016 0.1362 0.1002 Uiso 1.00 calc . . . H(7) H 0.5469 0.1160 0.3027 0.0794 Uiso 1.00 calc . . . H(8) H 0.6687 0.1579 0.3002 0.0794 Uiso 1.00 calc . . . H(9) H 0.6284 0.1563 0.3838 0.0794 Uiso 1.00 calc . . . H(10) H 0.6221 0.2591 0.4648 0.0761 Uiso 1.00 calc . . . H(11) H 0.6432 0.3541 0.4612 0.0761 Uiso 1.00 calc . . . H(12) H 0.5227 0.3207 0.4762 0.0761 Uiso 1.00 calc . . . H(13) H 0.5244 0.4868 0.3617 0.0943 Uiso 1.00 calc . . . H(14) H 0.4018 0.4950 0.2936 0.0943 Uiso 1.00 calc . . . H(15) H 0.4049 0.4570 0.3812 0.0943 Uiso 1.00 calc . . . H(16) H -0.1197 0.2943 0.1430 0.1965 Uiso 1.00 calc . . . H(17) H -0.1655 0.2098 0.1012 0.1965 Uiso 1.00 calc . . . H(18) H -0.2491 0.2631 0.1417 0.1965 Uiso 1.00 calc . . . H(19) H -0.1586 0.0495 0.1446 0.1758 Uiso 1.00 calc . . . H(20) H -0.0319 0.0811 0.1396 0.1758 Uiso 1.00 calc . . . H(21) H -0.0416 0.0095 0.2009 0.1758 Uiso 1.00 calc . . . H(22) H -0.0702 0.0079 0.4016 0.1534 Uiso 1.00 calc . . . H(23) H -0.0031 -0.0152 0.3334 0.1534 Uiso 1.00 calc . . . H(24) H 0.0661 0.0301 0.4154 0.1534 Uiso 1.00 calc . . . H(25) H -0.1022 0.1504 0.4836 0.1767 Uiso 1.00 calc . . . H(26) H 0.0319 0.1780 0.4963 0.1767 Uiso 1.00 calc . . . H(27) H -0.0709 0.2440 0.4806 0.1767 Uiso 1.00 calc . . . H(28) H -0.0850 0.3591 0.3594 0.1738 Uiso 1.00 calc . . . H(29) H -0.1738 0.3578 0.2699 0.1738 Uiso 1.00 calc . . . H(30) H -0.2166 0.3264 0.3471 0.1738 Uiso 1.00 calc . . . H(31) H 0.2305 0.0109 0.2840 0.0628 Uiso 1.00 calc . . . H(32) H 0.3606 0.0396 0.2840 0.0628 Uiso 1.00 calc . . . H(33) H 0.3910 0.0936 0.4142 0.0674 Uiso 1.00 calc . . . H(34) H 0.2558 0.0801 0.4134 0.0674 Uiso 1.00 calc . . . H(35) H 0.3085 0.3820 0.4566 0.0607 Uiso 1.00 calc . . . H(36) H 0.1883 0.3892 0.3860 0.0607 Uiso 1.00 calc . . . H(37) H 0.0760 0.3544 0.4770 0.0724 Uiso 1.00 calc . . . H(38) H 0.1913 0.3296 0.5465 0.0724 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0312(2) 0.0401(2) 0.0324(2) -0.0029(1) 0.0123(1) 0.0030(1) Ir(2) 0.0313(2) 0.0348(2) 0.0340(2) -0.0025(1) 0.0128(1) 0.0007(1) S(1) 0.042(1) 0.041(1) 0.039(1) -0.0017(10) 0.0168(10) -0.0053(9) S(2) 0.044(1) 0.037(1) 0.035(1) -0.0021(10) 0.0177(9) -0.0017(8) S(3) 0.037(1) 0.044(1) 0.049(1) 0.002(1) 0.012(1) 0.015(1) N(1) 0.11(1) 0.057(7) 0.101(9) 0.011(7) 0.018(7) 0.025(6) N(2) 0.23(2) 0.076(10) 0.13(1) -0.02(1) 0.10(1) -0.041(9) C(1) 0.031(5) 0.082(8) 0.056(6) -0.008(5) 0.020(4) 0.024(5) C(2) 0.014(4) 0.086(8) 0.040(5) -0.012(5) 0.006(3) 0.000(5) C(3) 0.035(5) 0.068(7) 0.047(5) -0.015(5) 0.019(4) -0.014(5) C(4) 0.042(6) 0.058(6) 0.043(5) -0.012(5) 0.013(4) 0.004(4) C(5) 0.043(6) 0.048(6) 0.057(6) -0.011(4) 0.020(5) 0.005(4) C(6) 0.09(1) 0.11(1) 0.084(9) -0.006(9) 0.025(8) 0.055(9) C(7) 0.063(9) 0.14(1) 0.052(7) 0.002(9) 0.031(6) -0.016(7) C(8) 0.037(6) 0.073(8) 0.091(8) -0.002(6) 0.021(6) -0.003(7) C(9) 0.049(7) 0.088(9) 0.049(6) -0.021(6) 0.004(5) -0.002(6) C(10) 0.08(1) 0.053(7) 0.108(10) -0.021(7) 0.040(8) -0.005(7) C(11) 0.036(6) 0.12(1) 0.056(7) -0.025(7) 0.011(5) 0.016(7) C(12) 0.059(8) 0.069(8) 0.067(7) -0.022(6) 0.030(6) -0.024(6) C(13) 0.041(6) 0.060(7) 0.083(8) -0.021(5) 0.023(6) 0.012(6) C(14) 0.027(5) 0.111(10) 0.041(5) -0.035(6) 0.018(4) -0.014(6) C(15) 0.034(6) 0.063(7) 0.098(9) -0.012(5) 0.033(6) -0.013(7) C(16) 0.06(1) 0.33(3) 0.08(1) -0.07(2) -0.025(8) 0.10(2) C(17) 0.13(2) 0.16(2) 0.17(2) -0.09(1) 0.08(1) -0.12(2) C(18) 0.09(1) 0.09(1) 0.20(2) -0.006(10) 0.04(1) 0.07(1) C(19) 0.15(2) 0.25(3) 0.063(9) -0.09(2) 0.06(1) -0.01(1) C(20) 0.06(1) 0.055(9) 0.34(3) -0.010(7) 0.09(1) -0.06(1) C(21) 0.055(7) 0.042(5) 0.064(6) 0.006(5) 0.021(5) 0.002(5) C(22) 0.063(8) 0.045(6) 0.058(6) 0.005(5) 0.012(5) 0.008(5) C(23) 0.071(9) 0.060(8) 0.078(8) 0.012(6) 0.017(7) 0.018(6) C(24) 0.065(7) 0.039(5) 0.052(5) -0.003(5) 0.022(5) -0.010(4) C(25) 0.073(8) 0.054(7) 0.064(7) -0.003(6) 0.037(6) -0.016(5) C(26) 0.11(1) 0.059(8) 0.075(8) 0.002(8) 0.047(8) -0.016(6) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0036(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5510 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.982 _refine_ls_shift/su_max 0.0270 _refine_ls_shift/su_mean 0.0040 _refine_diff_density_min -3.79 _refine_diff_density_max 2.38 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir(1) S(1) 2.387(2) 1_555 1_555 yes Ir(1) S(2) 2.395(2) 1_555 1_555 yes Ir(1) S(3) 2.388(3) 1_555 1_555 yes Ir(1) C(1) 2.175(9) 1_555 1_555 yes Ir(1) C(2) 2.182(9) 1_555 1_555 yes Ir(1) C(3) 2.21(1) 1_555 1_555 yes Ir(1) C(4) 2.21(1) 1_555 1_555 yes Ir(1) C(5) 2.174(10) 1_555 1_555 yes Ir(2) S(1) 2.382(2) 1_555 1_555 yes Ir(2) S(2) 2.394(2) 1_555 1_555 yes Ir(2) S(3) 2.384(2) 1_555 1_555 yes Ir(2) C(11) 2.16(1) 1_555 1_555 yes Ir(2) C(12) 2.18(1) 1_555 1_555 yes Ir(2) C(13) 2.214(10) 1_555 1_555 yes Ir(2) C(14) 2.194(8) 1_555 1_555 yes Ir(2) C(15) 2.16(1) 1_555 1_555 yes S(1) C(21) 1.82(1) 1_555 1_555 yes S(2) C(24) 1.817(10) 1_555 1_555 yes N(1) C(23) 1.14(2) 1_555 1_555 yes N(2) C(26) 1.10(2) 1_555 1_555 yes C(1) C(2) 1.40(2) 1_555 1_555 yes C(1) C(5) 1.44(1) 1_555 1_555 yes C(1) C(6) 1.51(2) 1_555 1_555 yes C(2) C(3) 1.47(1) 1_555 1_555 yes C(2) C(7) 1.49(2) 1_555 1_555 yes C(3) C(4) 1.43(1) 1_555 1_555 yes C(3) C(8) 1.51(2) 1_555 1_555 yes C(4) C(5) 1.43(1) 1_555 1_555 yes C(4) C(9) 1.47(1) 1_555 1_555 yes C(5) C(10) 1.49(2) 1_555 1_555 yes C(11) C(12) 1.41(2) 1_555 1_555 yes C(11) C(15) 1.45(2) 1_555 1_555 yes C(11) C(16) 1.48(2) 1_555 1_555 yes C(12) C(13) 1.42(2) 1_555 1_555 yes C(12) C(17) 1.49(2) 1_555 1_555 yes C(13) C(14) 1.43(2) 1_555 1_555 yes C(13) C(18) 1.50(2) 1_555 1_555 yes C(14) C(15) 1.43(2) 1_555 1_555 yes C(14) C(19) 1.52(2) 1_555 1_555 yes C(15) C(20) 1.49(2) 1_555 1_555 yes C(21) C(22) 1.50(1) 1_555 1_555 yes C(22) C(23) 1.47(2) 1_555 1_555 yes C(24) C(25) 1.52(1) 1_555 1_555 yes C(25) C(26) 1.45(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ir(1) S(2) 78.65(7) 1_555 1_555 1_555 yes S(1) Ir(1) S(3) 73.53(9) 1_555 1_555 1_555 yes S(1) Ir(1) C(1) 129.1(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(2) 103.2(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(3) 107.9(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(4) 140.5(3) 1_555 1_555 1_555 yes S(1) Ir(1) C(5) 166.9(3) 1_555 1_555 1_555 yes S(2) Ir(1) S(3) 78.25(8) 1_555 1_555 1_555 yes S(2) Ir(1) C(1) 149.9(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(2) 162.6(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(3) 123.5(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(4) 103.4(3) 1_555 1_555 1_555 yes S(2) Ir(1) C(5) 114.3(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(1) 97.4(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(2) 119.0(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(3) 158.3(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(4) 146.0(3) 1_555 1_555 1_555 yes S(3) Ir(1) C(5) 109.5(3) 1_555 1_555 1_555 yes C(1) Ir(1) C(2) 37.5(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(3) 64.4(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(4) 64.0(4) 1_555 1_555 1_555 yes C(1) Ir(1) C(5) 38.7(4) 1_555 1_555 1_555 yes C(2) Ir(1) C(3) 39.2(4) 1_555 1_555 1_555 yes C(2) Ir(1) C(4) 64.0(3) 1_555 1_555 1_555 yes C(2) Ir(1) C(5) 64.0(4) 1_555 1_555 1_555 yes C(3) Ir(1) C(4) 37.9(4) 1_555 1_555 1_555 yes C(3) Ir(1) C(5) 64.3(4) 1_555 1_555 1_555 yes C(4) Ir(1) C(5) 38.2(4) 1_555 1_555 1_555 yes S(1) Ir(2) S(2) 78.76(8) 1_555 1_555 1_555 yes S(1) Ir(2) S(3) 73.67(8) 1_555 1_555 1_555 yes S(1) Ir(2) C(11) 121.5(4) 1_555 1_555 1_555 yes S(1) Ir(2) C(12) 99.6(3) 1_555 1_555 1_555 yes S(1) Ir(2) C(13) 110.5(3) 1_555 1_555 1_555 yes S(1) Ir(2) C(14) 145.7(4) 1_555 1_555 1_555 yes S(1) Ir(2) C(15) 160.7(4) 1_555 1_555 1_555 yes S(2) Ir(2) S(3) 78.35(8) 1_555 1_555 1_555 yes S(2) Ir(2) C(11) 158.2(4) 1_555 1_555 1_555 yes S(2) Ir(2) C(12) 155.6(4) 1_555 1_555 1_555 yes S(2) Ir(2) C(13) 119.8(3) 1_555 1_555 1_555 yes S(2) Ir(2) C(14) 104.7(3) 1_555 1_555 1_555 yes S(2) Ir(2) C(15) 120.4(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(11) 98.7(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(12) 124.9(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(13) 161.7(3) 1_555 1_555 1_555 yes S(3) Ir(2) C(14) 140.6(4) 1_555 1_555 1_555 yes S(3) Ir(2) C(15) 105.7(4) 1_555 1_555 1_555 yes C(11) Ir(2) C(12) 37.9(5) 1_555 1_555 1_555 yes C(11) Ir(2) C(13) 63.6(5) 1_555 1_555 1_555 yes C(11) Ir(2) C(14) 63.9(4) 1_555 1_555 1_555 yes C(11) Ir(2) C(15) 39.2(5) 1_555 1_555 1_555 yes C(12) Ir(2) C(13) 37.7(4) 1_555 1_555 1_555 yes C(12) Ir(2) C(14) 63.2(4) 1_555 1_555 1_555 yes C(12) Ir(2) C(15) 64.4(5) 1_555 1_555 1_555 yes C(13) Ir(2) C(14) 37.8(4) 1_555 1_555 1_555 yes C(13) Ir(2) C(15) 64.2(5) 1_555 1_555 1_555 yes C(14) Ir(2) C(15) 38.2(5) 1_555 1_555 1_555 yes Ir(1) S(1) Ir(2) 88.36(8) 1_555 1_555 1_555 yes Ir(1) S(1) C(21) 115.4(4) 1_555 1_555 1_555 yes Ir(2) S(1) C(21) 112.2(3) 1_555 1_555 1_555 yes Ir(1) S(2) Ir(2) 87.90(7) 1_555 1_555 1_555 yes Ir(1) S(2) C(24) 101.8(3) 1_555 1_555 1_555 yes Ir(2) S(2) C(24) 110.8(4) 1_555 1_555 1_555 yes Ir(1) S(3) Ir(2) 88.28(8) 1_555 1_555 1_555 yes Ir(1) C(1) C(2) 71.5(6) 1_555 1_555 1_555 yes Ir(1) C(1) C(5) 70.6(5) 1_555 1_555 1_555 yes Ir(1) C(1) C(6) 124.1(8) 1_555 1_555 1_555 yes C(2) C(1) C(5) 108.7(9) 1_555 1_555 1_555 yes C(2) C(1) C(6) 125(1) 1_555 1_555 1_555 yes C(5) C(1) C(6) 125(1) 1_555 1_555 1_555 yes Ir(1) C(2) C(1) 71.0(5) 1_555 1_555 1_555 yes Ir(1) C(2) C(3) 71.3(5) 1_555 1_555 1_555 yes Ir(1) C(2) C(7) 125.5(8) 1_555 1_555 1_555 yes C(1) C(2) C(3) 108.6(9) 1_555 1_555 1_555 yes C(1) C(2) C(7) 128(1) 1_555 1_555 1_555 yes C(3) C(2) C(7) 122(1) 1_555 1_555 1_555 yes Ir(1) C(3) C(2) 69.5(5) 1_555 1_555 1_555 yes Ir(1) C(3) C(4) 71.1(6) 1_555 1_555 1_555 yes Ir(1) C(3) C(8) 128.4(7) 1_555 1_555 1_555 yes C(2) C(3) C(4) 106.3(10) 1_555 1_555 1_555 yes C(2) C(3) C(8) 126.0(10) 1_555 1_555 1_555 yes C(4) C(3) C(8) 127.5(10) 1_555 1_555 1_555 yes Ir(1) C(4) C(3) 71.0(6) 1_555 1_555 1_555 yes Ir(1) C(4) C(5) 69.7(6) 1_555 1_555 1_555 yes Ir(1) C(4) C(9) 126.8(7) 1_555 1_555 1_555 yes C(3) C(4) C(5) 108.8(9) 1_555 1_555 1_555 yes C(3) C(4) C(9) 124(1) 1_555 1_555 1_555 yes C(5) C(4) C(9) 126(1) 1_555 1_555 1_555 yes Ir(1) C(5) C(1) 70.7(6) 1_555 1_555 1_555 yes Ir(1) C(5) C(4) 72.1(6) 1_555 1_555 1_555 yes Ir(1) C(5) C(10) 127.9(8) 1_555 1_555 1_555 yes C(1) C(5) C(4) 107.6(9) 1_555 1_555 1_555 yes C(1) C(5) C(10) 126(1) 1_555 1_555 1_555 yes C(4) C(5) C(10) 125(1) 1_555 1_555 1_555 yes Ir(2) C(11) C(12) 71.5(7) 1_555 1_555 1_555 yes Ir(2) C(11) C(15) 70.1(7) 1_555 1_555 1_555 yes Ir(2) C(11) C(16) 125.1(9) 1_555 1_555 1_555 yes C(12) C(11) C(15) 107(1) 1_555 1_555 1_555 yes C(12) C(11) C(16) 129(1) 1_555 1_555 1_555 yes C(15) C(11) C(16) 122(1) 1_555 1_555 1_555 yes Ir(2) C(12) C(11) 70.5(7) 1_555 1_555 1_555 yes Ir(2) C(12) C(13) 72.6(6) 1_555 1_555 1_555 yes Ir(2) C(12) C(17) 125.8(9) 1_555 1_555 1_555 yes C(11) C(12) C(13) 109(1) 1_555 1_555 1_555 yes C(11) C(12) C(17) 123(1) 1_555 1_555 1_555 yes C(13) C(12) C(17) 126(1) 1_555 1_555 1_555 yes Ir(2) C(13) C(12) 69.7(6) 1_555 1_555 1_555 yes Ir(2) C(13) C(14) 70.4(5) 1_555 1_555 1_555 yes Ir(2) C(13) C(18) 130.3(10) 1_555 1_555 1_555 yes C(12) C(13) C(14) 107(1) 1_555 1_555 1_555 yes C(12) C(13) C(18) 125(1) 1_555 1_555 1_555 yes C(14) C(13) C(18) 126(1) 1_555 1_555 1_555 yes Ir(2) C(14) C(13) 71.9(5) 1_555 1_555 1_555 yes Ir(2) C(14) C(15) 69.4(5) 1_555 1_555 1_555 yes Ir(2) C(14) C(19) 129.1(9) 1_555 1_555 1_555 yes C(13) C(14) C(15) 109.0(9) 1_555 1_555 1_555 yes C(13) C(14) C(19) 122(1) 1_555 1_555 1_555 yes C(15) C(14) C(19) 128(1) 1_555 1_555 1_555 yes Ir(2) C(15) C(11) 70.7(6) 1_555 1_555 1_555 yes Ir(2) C(15) C(14) 72.3(6) 1_555 1_555 1_555 yes Ir(2) C(15) C(20) 127.5(9) 1_555 1_555 1_555 yes C(11) C(15) C(14) 106(1) 1_555 1_555 1_555 yes C(11) C(15) C(20) 126(1) 1_555 1_555 1_555 yes C(14) C(15) C(20) 126(1) 1_555 1_555 1_555 yes S(1) C(21) C(22) 115.7(7) 1_555 1_555 1_555 yes C(21) C(22) C(23) 111.2(9) 1_555 1_555 1_555 yes N(1) C(23) C(22) 178(1) 1_555 1_555 1_555 yes S(2) C(24) C(25) 113.9(7) 1_555 1_555 1_555 yes C(24) C(25) C(26) 109.7(10) 1_555 1_555 1_555 yes N(2) C(26) C(25) 177(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ir(1) Ir(2) 3.324(1) 1_555 1_555 ? #------------------------------------------------------------------------------ #===END