# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. #=================================================================== _journal_coden_Cambridge 1145 _publ_contact_author_name 'Yoshiro Yamashita' _publ_contact_author_address ; Yoshiro Yamashita Department of Electronic Chemistry Interdisciplinary Graduate School of Science and Engineering Tokyo Institute of Technology, Nagatsuta, Midori-ku, Yokohama 226-8502, Japan ; _publ_contact_author_phone +81-45-924-5571 _publ_contact_author_fax +81-45-924-5489 _publ_contact_author_email yoshiro@echem.titech.ac.jp _publ_section_title ; Synthesis, Characterization and Electroluminescence Properties of New Iridium Complexes Based on Cyclic Phenylvinylpyridine Derivatives: Tuning of Emission Colour and Efficiency by Structural Control ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? loop_ _publ_author_name 'Yoshiro Yamashita' 'M. Akhtaruzzaman' 'Hidenori Echizen' 'Takeshi Iwata' 'Jun-ichi Nishida' ; Y.Sasaki ; 'Shin-ya Takizawa' 'Shizuo Tokito' #------------------------------------------------------------------------------ data_4a _database_code_depnum_ccdc_archive 'CCDC 616850' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C35 H31 Ir N2 O2 ' _chemical_formula_moiety ? _chemical_formula_weight 703.86 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.91(2) _cell_length_b 13.05(2) _cell_length_c 18.42(4) _cell_angle_alpha 94.85(6) _cell_angle_beta 97.12(6) _cell_angle_gamma 94.57(6) _cell_volume 2820(27) _cell_formula_units_Z 4 _cell_measurement_reflns_used 21254 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.500 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.028 _exptl_absorpt_correction_T_max 0.092 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 24537 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9250 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9250 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11929 _reflns_number_gt 8369 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0899 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11929 _refine_ls_number_parameters 721 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0030 _refine_diff_density_max 1.14 _refine_diff_density_min -0.85 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.22831(1) 0.26980(1) 0.010467(9) 0.01327(5) Uani 1.00 d . . . Ir(2) Ir -0.27396(1) 0.27365(1) -0.489670(9) 0.01233(5) Uani 1.00 d . . . O(1) O 0.0719(2) 0.2525(2) 0.0538(2) 0.0183(8) Uani 1.00 d . . . O(2) O 0.2342(3) 0.4318(2) 0.0351(2) 0.0211(9) Uani 1.00 d . . . O(3) O -0.2504(3) 0.4129(2) -0.4188(2) 0.0204(9) Uani 1.00 d . . . O(4) O -0.4524(2) 0.2807(2) -0.4975(2) 0.0178(8) Uani 1.00 d . . . N(1) N 0.1398(3) 0.2770(2) -0.0907(2) 0.0155(9) Uani 1.00 d . . . N(2) N 0.3185(3) 0.2565(2) 0.1102(2) 0.0174(10) Uani 1.00 d . . . N(3) N -0.2808(3) 0.1927(2) -0.4007(2) 0.0144(9) Uani 1.00 d . . . N(4) N -0.2676(3) 0.3561(2) -0.5780(2) 0.0138(9) Uani 1.00 d . . . C(1) C 0.0948(4) 0.1820(3) -0.1189(2) 0.018(1) Uani 1.00 d . . . C(2) C 0.1186(4) 0.3553(3) -0.1328(3) 0.020(1) Uani 1.00 d . . . C(3) C 0.0523(4) 0.3382(3) -0.2000(3) 0.020(1) Uani 1.00 d . . . C(4) C 0.0087(4) 0.2393(3) -0.2296(3) 0.020(1) Uani 1.00 d . . . C(5) C 0.0283(4) 0.1588(3) -0.1868(2) 0.018(1) Uani 1.00 d . . . C(6) C 0.0005(4) 0.0427(3) -0.1985(3) 0.027(1) Uani 1.00 d . . . C(7) C 0.0614(4) -0.0007(3) -0.1287(2) 0.020(1) Uani 1.00 d . . . C(8) C 0.1216(3) 0.0947(3) -0.0810(2) 0.016(1) Uani 1.00 d . . . C(9) C 0.2008(4) 0.1167(3) -0.0203(2) 0.018(1) Uani 1.00 d . . . C(10) C 0.2482(3) 0.0310(3) 0.0186(2) 0.013(1) Uani 1.00 d . . . C(11) C 0.3641(4) 0.0329(3) 0.0413(2) 0.019(1) Uani 1.00 d . . . C(12) C 0.4117(4) -0.0464(3) 0.0761(2) 0.021(1) Uani 1.00 d . . . C(13) C 0.3408(4) -0.1304(3) 0.0905(2) 0.021(1) Uani 1.00 d . . . C(14) C 0.2249(4) -0.1333(3) 0.0692(3) 0.021(1) Uani 1.00 d . . . C(15) C 0.1793(4) -0.0535(3) 0.0336(2) 0.020(1) Uani 1.00 d . . . C(16) C 0.4298(4) 0.2794(3) 0.1092(2) 0.017(1) Uani 1.00 d . . . C(17) C 0.2864(4) 0.2244(3) 0.1737(2) 0.018(1) Uani 1.00 d . . . C(18) C 0.3669(4) 0.2148(3) 0.2332(2) 0.023(1) Uani 1.00 d . . . C(19) C 0.4836(4) 0.2364(3) 0.2304(2) 0.020(1) Uani 1.00 d . . . C(20) C 0.5136(4) 0.2696(3) 0.1667(2) 0.020(1) Uani 1.00 d . . . C(21) C 0.6268(4) 0.2921(3) 0.1384(3) 0.025(1) Uani 1.00 d . . . C(22) C 0.5971(4) 0.3265(3) 0.0600(3) 0.022(1) Uani 1.00 d . . . C(23) C 0.4682(4) 0.3071(3) 0.0428(2) 0.016(1) Uani 1.00 d . . . C(24) C 0.3870(4) 0.2968(3) -0.0169(2) 0.016(1) Uani 1.00 d . . . C(25) C 0.4179(3) 0.3158(3) -0.0901(2) 0.014(1) Uani 1.00 d . . . C(26) C 0.4927(4) 0.4010(3) -0.0996(3) 0.019(1) Uani 1.00 d . . . C(27) C 0.5242(4) 0.4168(3) -0.1676(3) 0.028(1) Uani 1.00 d . . . C(28) C 0.4851(4) 0.3478(3) -0.2283(3) 0.025(1) Uani 1.00 d . . . C(29) C 0.4115(4) 0.2624(3) -0.2201(3) 0.025(1) Uani 1.00 d . . . C(30) C 0.3770(4) 0.2470(3) -0.1524(2) 0.018(1) Uani 1.00 d . . . C(31) C -0.0777(4) 0.2943(3) 0.1183(3) 0.031(1) Uani 1.00 d . . . C(32) C 0.0267(4) 0.3258(3) 0.0859(3) 0.023(1) Uani 1.00 d . . . C(33) C 0.0668(4) 0.4312(3) 0.0939(3) 0.026(1) Uani 1.00 d . . . C(34) C 0.1617(4) 0.4774(3) 0.0676(3) 0.020(1) Uani 1.00 d . . . C(35) C 0.1796(4) 0.5935(3) 0.0770(3) 0.029(1) Uani 1.00 d . . . C(36) C -0.3112(4) 0.0917(3) -0.4208(2) 0.018(1) Uani 1.00 d . . . C(37) C -0.2652(4) 0.2215(3) -0.3272(2) 0.019(1) Uani 1.00 d . . . C(38) C -0.2780(4) 0.1509(3) -0.2771(2) 0.021(1) Uani 1.00 d . . . C(39) C -0.3050(4) 0.0455(3) -0.2992(3) 0.021(1) Uani 1.00 d . . . C(40) C -0.3214(4) 0.0155(3) -0.3735(3) 0.019(1) Uani 1.00 d . . . C(41) C -0.3453(4) -0.0873(3) -0.4202(3) 0.021(1) Uani 1.00 d . . . C(42) C -0.3563(4) -0.0598(3) -0.5015(3) 0.021(1) Uani 1.00 d . . . C(43) C -0.3282(4) 0.0562(3) -0.4973(2) 0.015(1) Uani 1.00 d . . . C(44) C -0.3057(4) 0.1300(3) -0.5435(2) 0.016(1) Uani 1.00 d . . . C(45) C -0.3080(4) 0.1025(3) -0.6240(2) 0.014(1) Uani 1.00 d . . . C(46) C -0.3956(4) 0.0334(3) -0.6629(2) 0.018(1) Uani 1.00 d . . . C(47) C -0.3996(4) 0.0072(3) -0.7380(2) 0.021(1) Uani 1.00 d . . . C(48) C -0.3153(4) 0.0488(3) -0.7749(2) 0.025(1) Uani 1.00 d . . . C(49) C -0.2281(4) 0.1172(3) -0.7365(3) 0.022(1) Uani 1.00 d . . . C(50) C -0.2253(4) 0.1444(3) -0.6625(2) 0.016(1) Uani 1.00 d . . . C(51) C -0.1609(4) 0.3854(3) -0.5870(2) 0.015(1) Uani 1.00 d . . . C(52) C -0.3505(4) 0.3861(3) -0.6272(2) 0.014(1) Uani 1.00 d . . . C(53) C -0.3254(4) 0.4429(3) -0.6832(2) 0.020(1) Uani 1.00 d . . . C(54) C -0.2130(4) 0.4699(3) -0.6928(3) 0.022(1) Uani 1.00 d . . . C(55) C -0.1281(4) 0.4389(3) -0.6434(2) 0.019(1) Uani 1.00 d . . . C(56) C 0.0002(4) 0.4462(3) -0.6372(3) 0.024(1) Uani 1.00 d . . . C(57) C 0.0393(4) 0.3892(3) -0.5678(3) 0.022(1) Uani 1.00 d . . . C(58) C -0.0700(4) 0.3489(3) -0.5402(2) 0.016(1) Uani 1.00 d . . . C(59) C -0.1029(4) 0.2834(3) -0.4917(2) 0.017(1) Uani 1.00 d . . . C(60) C -0.0183(4) 0.2300(3) -0.4466(2) 0.015(1) Uani 1.00 d . . . C(61) C 0.0817(4) 0.2846(3) -0.4104(2) 0.019(1) Uani 1.00 d . . . C(62) C 0.1624(4) 0.2359(3) -0.3688(2) 0.022(1) Uani 1.00 d . . . C(63) C 0.1449(4) 0.1297(3) -0.3630(3) 0.023(1) Uani 1.00 d . . . C(64) C 0.0474(4) 0.0747(3) -0.3994(3) 0.022(1) Uani 1.00 d . . . C(65) C -0.0343(4) 0.1243(3) -0.4399(2) 0.019(1) Uani 1.00 d . . . C(66) C -0.2937(4) 0.5432(3) -0.3327(3) 0.027(1) Uani 1.00 d . . . C(67) C -0.3303(4) 0.4555(3) -0.3930(2) 0.021(1) Uani 1.00 d . . . C(68) C -0.4463(4) 0.4316(3) -0.4123(3) 0.019(1) Uani 1.00 d . . . C(69) C -0.5006(4) 0.3511(3) -0.4645(2) 0.017(1) Uani 1.00 d . . . C(70) C -0.6268(4) 0.3441(3) -0.4813(3) 0.025(1) Uani 1.00 d . . . H(1) H 0.1511 0.4238 -0.1146 0.0242 Uiso 1.00 calc . . . H(2) H 0.0358 0.3950 -0.2273 0.0254 Uiso 1.00 calc . . . H(3) H -0.0331 0.2281 -0.2773 0.0278 Uiso 1.00 calc . . . H(4) H -0.0789 0.0263 -0.2035 0.0319 Uiso 1.00 calc . . . H(5) H 0.0293 0.0152 -0.2414 0.0319 Uiso 1.00 calc . . . H(6) H 0.0059 -0.0339 -0.1033 0.0216 Uiso 1.00 calc . . . H(7) H 0.1131 -0.0472 -0.1419 0.0216 Uiso 1.00 calc . . . H(8) H 0.4132 0.0908 0.0322 0.0222 Uiso 1.00 calc . . . H(9) H 0.4915 -0.0445 0.0904 0.0238 Uiso 1.00 calc . . . H(10) H 0.3717 -0.1855 0.1145 0.0271 Uiso 1.00 calc . . . H(11) H 0.1768 -0.1888 0.0812 0.0263 Uiso 1.00 calc . . . H(12) H 0.0995 -0.0590 0.0171 0.0211 Uiso 1.00 calc . . . H(13) H 0.2081 0.2086 0.1768 0.0230 Uiso 1.00 calc . . . H(14) H 0.3415 0.1939 0.2775 0.0254 Uiso 1.00 calc . . . H(15) H 0.5387 0.2265 0.2703 0.0255 Uiso 1.00 calc . . . H(16) H 0.6711 0.3464 0.1696 0.0288 Uiso 1.00 calc . . . H(17) H 0.6661 0.2324 0.1367 0.0288 Uiso 1.00 calc . . . H(18) H 0.6194 0.3979 0.0590 0.0258 Uiso 1.00 calc . . . H(19) H 0.6330 0.2873 0.0254 0.0258 Uiso 1.00 calc . . . H(20) H 0.5204 0.4500 -0.0579 0.0257 Uiso 1.00 calc . . . H(21) H 0.5763 0.4757 -0.1725 0.0308 Uiso 1.00 calc . . . H(22) H 0.5087 0.3581 -0.2753 0.0306 Uiso 1.00 calc . . . H(23) H 0.3841 0.2139 -0.2620 0.0286 Uiso 1.00 calc . . . H(24) H 0.3236 0.1891 -0.1480 0.0227 Uiso 1.00 calc . . . H(25) H -0.1306 0.2524 0.0817 0.0387 Uiso 1.00 calc . . . H(26) H -0.0597 0.2548 0.1585 0.0387 Uiso 1.00 calc . . . H(27) H -0.1130 0.3532 0.1344 0.0387 Uiso 1.00 calc . . . H(28) H 0.0226 0.4763 0.1199 0.0317 Uiso 1.00 calc . . . H(29) H 0.1297 0.6215 0.0409 0.0348 Uiso 1.00 calc . . . H(30) H 0.1632 0.6182 0.1248 0.0348 Uiso 1.00 calc . . . H(31) H 0.2557 0.6156 0.0725 0.0348 Uiso 1.00 calc . . . H(32) H -0.2454 0.2932 -0.3109 0.0228 Uiso 1.00 calc . . . H(33) H -0.2673 0.1734 -0.2260 0.0262 Uiso 1.00 calc . . . H(34) H -0.3120 -0.0034 -0.2644 0.0265 Uiso 1.00 calc . . . H(35) H -0.2852 -0.1295 -0.4103 0.0248 Uiso 1.00 calc . . . H(36) H -0.4145 -0.1218 -0.4104 0.0248 Uiso 1.00 calc . . . H(37) H -0.3040 -0.0958 -0.5276 0.0243 Uiso 1.00 calc . . . H(38) H -0.4312 -0.0793 -0.5256 0.0243 Uiso 1.00 calc . . . H(39) H -0.4530 0.0027 -0.6376 0.0219 Uiso 1.00 calc . . . H(40) H -0.4598 -0.0390 -0.7636 0.0258 Uiso 1.00 calc . . . H(41) H -0.3154 0.0301 -0.8260 0.0260 Uiso 1.00 calc . . . H(42) H -0.1713 0.1461 -0.7622 0.0254 Uiso 1.00 calc . . . H(43) H -0.1656 0.1918 -0.6370 0.0191 Uiso 1.00 calc . . . H(44) H -0.4270 0.3655 -0.6231 0.0180 Uiso 1.00 calc . . . H(45) H -0.3858 0.4636 -0.7160 0.0234 Uiso 1.00 calc . . . H(46) H -0.1952 0.5076 -0.7327 0.0252 Uiso 1.00 calc . . . H(47) H 0.0238 0.4138 -0.6801 0.0277 Uiso 1.00 calc . . . H(48) H 0.0312 0.5166 -0.6302 0.0277 Uiso 1.00 calc . . . H(49) H 0.0821 0.3331 -0.5818 0.0277 Uiso 1.00 calc . . . H(50) H 0.0855 0.4351 -0.5316 0.0277 Uiso 1.00 calc . . . H(51) H 0.0950 0.3566 -0.4149 0.0204 Uiso 1.00 calc . . . H(52) H 0.2297 0.2734 -0.3438 0.0258 Uiso 1.00 calc . . . H(53) H 0.2003 0.0965 -0.3338 0.0292 Uiso 1.00 calc . . . H(54) H 0.0378 0.0021 -0.3971 0.0276 Uiso 1.00 calc . . . H(55) H -0.1028 0.0862 -0.4629 0.0214 Uiso 1.00 calc . . . H(56) H -0.3578 0.5766 -0.3211 0.0322 Uiso 1.00 calc . . . H(57) H -0.2583 0.5163 -0.2900 0.0322 Uiso 1.00 calc . . . H(58) H -0.2407 0.5915 -0.3493 0.0322 Uiso 1.00 calc . . . H(59) H -0.4959 0.4732 -0.3876 0.0211 Uiso 1.00 calc . . . H(60) H -0.6605 0.2897 -0.4569 0.0312 Uiso 1.00 calc . . . H(61) H -0.6547 0.4075 -0.4640 0.0312 Uiso 1.00 calc . . . H(62) H -0.6500 0.3311 -0.5325 0.0312 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) 0.0121(1) 0.01317(9) 0.0152(1) 0.00232(6) 0.00359(7) 0.00180(7) Ir(2) 0.0116(1) 0.01230(9) 0.01309(10) 0.00134(6) 0.00171(7) 0.00096(6) O(1) 0.011(2) 0.016(1) 0.029(2) 0.000(1) 0.007(1) 0.002(1) O(2) 0.024(2) 0.019(2) 0.020(2) 0.001(1) 0.003(1) 0.001(1) O(3) 0.025(2) 0.014(1) 0.022(2) 0.001(1) 0.003(1) 0.003(1) O(4) 0.014(2) 0.016(1) 0.023(2) -0.001(1) 0.005(1) 0.001(1) N(1) 0.007(2) 0.022(2) 0.018(2) 0.004(1) 0.004(1) 0.000(1) N(2) 0.022(2) 0.015(2) 0.014(2) 0.003(1) 0.004(2) -0.001(1) N(3) 0.011(2) 0.014(2) 0.018(2) 0.000(1) 0.001(1) -0.001(1) N(4) 0.009(2) 0.016(2) 0.018(2) 0.002(1) 0.004(1) 0.002(1) C(1) 0.014(2) 0.026(2) 0.017(2) 0.005(2) 0.004(2) 0.002(2) C(2) 0.014(2) 0.027(2) 0.022(3) 0.007(2) 0.007(2) 0.004(2) C(3) 0.015(2) 0.023(2) 0.026(3) 0.004(2) 0.005(2) 0.010(2) C(4) 0.010(2) 0.030(2) 0.021(3) 0.003(2) 0.002(2) 0.005(2) C(5) 0.016(2) 0.014(2) 0.021(2) -0.003(2) 0.000(2) -0.003(2) C(6) 0.023(3) 0.034(3) 0.024(3) 0.006(2) 0.001(2) 0.004(2) C(7) 0.027(3) 0.013(2) 0.018(2) -0.001(2) 0.000(2) -0.004(2) C(8) 0.003(2) 0.029(2) 0.018(2) 0.002(2) 0.005(2) 0.003(2) C(9) 0.024(3) 0.015(2) 0.017(2) 0.002(2) 0.006(2) 0.001(2) C(10) 0.013(2) 0.009(2) 0.016(2) 0.000(1) 0.004(2) -0.005(2) C(11) 0.023(3) 0.022(2) 0.014(2) 0.005(2) 0.005(2) 0.001(2) C(12) 0.019(3) 0.028(2) 0.016(2) 0.009(2) 0.001(2) -0.001(2) C(13) 0.025(3) 0.024(2) 0.017(2) 0.012(2) 0.005(2) 0.004(2) C(14) 0.028(3) 0.012(2) 0.024(3) 0.001(2) 0.012(2) 0.002(2) C(15) 0.022(3) 0.019(2) 0.019(2) 0.003(2) 0.002(2) -0.001(2) C(16) 0.018(2) 0.014(2) 0.017(2) 0.001(2) 0.000(2) -0.004(2) C(17) 0.020(2) 0.012(2) 0.024(3) 0.002(2) 0.011(2) 0.004(2) C(18) 0.042(3) 0.016(2) 0.012(2) 0.002(2) 0.006(2) 0.001(2) C(19) 0.024(3) 0.015(2) 0.019(3) -0.001(2) 0.000(2) -0.002(2) C(20) 0.019(3) 0.022(2) 0.016(2) 0.001(2) 0.000(2) -0.004(2) C(21) 0.018(3) 0.032(2) 0.023(3) -0.003(2) 0.000(2) 0.000(2) C(22) 0.022(3) 0.025(2) 0.019(3) 0.004(2) 0.001(2) 0.000(2) C(23) 0.015(2) 0.009(2) 0.022(2) -0.004(1) 0.000(2) -0.002(2) C(24) 0.014(2) 0.015(2) 0.019(2) 0.004(2) 0.003(2) 0.001(2) C(25) 0.007(2) 0.014(2) 0.020(2) 0.004(1) 0.002(2) 0.003(2) C(26) 0.019(3) 0.018(2) 0.021(3) 0.003(2) 0.004(2) 0.001(2) C(27) 0.030(3) 0.026(2) 0.028(3) 0.002(2) 0.007(2) 0.008(2) C(28) 0.024(3) 0.038(3) 0.018(3) 0.012(2) 0.007(2) 0.009(2) C(29) 0.030(3) 0.030(2) 0.016(2) 0.013(2) 0.001(2) 0.002(2) C(30) 0.016(2) 0.017(2) 0.023(3) 0.004(2) 0.002(2) 0.003(2) C(31) 0.020(3) 0.025(2) 0.052(4) 0.002(2) 0.021(2) 0.002(2) C(32) 0.020(3) 0.026(2) 0.027(3) 0.009(2) 0.008(2) 0.008(2) C(33) 0.029(3) 0.013(2) 0.039(3) 0.002(2) 0.018(2) -0.002(2) C(34) 0.020(3) 0.012(2) 0.026(3) 0.002(2) 0.005(2) 0.001(2) C(35) 0.037(3) 0.011(2) 0.042(3) 0.001(2) 0.016(3) 0.002(2) C(36) 0.009(2) 0.025(2) 0.020(2) 0.004(2) 0.002(2) 0.005(2) C(37) 0.019(3) 0.017(2) 0.018(2) -0.004(2) 0.000(2) -0.002(2) C(38) 0.018(3) 0.027(2) 0.018(2) 0.002(2) 0.002(2) 0.001(2) C(39) 0.010(2) 0.029(2) 0.026(3) -0.001(2) 0.004(2) 0.010(2) C(40) 0.009(2) 0.023(2) 0.023(3) -0.002(2) 0.004(2) 0.003(2) C(41) 0.020(3) 0.023(2) 0.022(3) 0.001(2) 0.007(2) 0.005(2) C(42) 0.018(3) 0.017(2) 0.027(3) -0.003(2) 0.002(2) 0.002(2) C(43) 0.013(2) 0.011(2) 0.021(2) -0.001(1) 0.001(2) 0.001(2) C(44) 0.016(2) 0.007(2) 0.022(2) -0.004(1) -0.001(2) -0.003(2) C(45) 0.011(2) 0.016(2) 0.018(2) 0.007(2) 0.003(2) 0.003(2) C(46) 0.011(2) 0.023(2) 0.020(2) 0.004(2) 0.004(2) 0.002(2) C(47) 0.020(3) 0.025(2) 0.018(2) 0.003(2) -0.003(2) -0.002(2) C(48) 0.031(3) 0.029(2) 0.014(2) 0.010(2) 0.000(2) -0.001(2) C(49) 0.020(3) 0.028(2) 0.021(3) 0.009(2) 0.009(2) 0.008(2) C(50) 0.017(2) 0.015(2) 0.017(2) 0.007(2) 0.003(2) 0.001(2) C(51) 0.012(2) 0.015(2) 0.018(2) 0.000(2) 0.002(2) -0.001(2) C(52) 0.011(2) 0.013(2) 0.018(2) -0.003(1) 0.000(2) -0.001(2) C(53) 0.022(3) 0.018(2) 0.018(2) 0.005(2) -0.003(2) 0.001(2) C(54) 0.024(3) 0.021(2) 0.020(3) -0.001(2) 0.004(2) 0.006(2) C(55) 0.024(3) 0.008(2) 0.023(3) -0.003(2) 0.001(2) 0.000(2) C(56) 0.018(3) 0.032(2) 0.024(3) 0.002(2) 0.007(2) 0.009(2) C(57) 0.019(3) 0.019(2) 0.027(3) -0.003(2) 0.001(2) 0.003(2) C(58) 0.009(2) 0.020(2) 0.019(2) 0.001(2) 0.002(2) 0.001(2) C(59) 0.013(2) 0.019(2) 0.017(2) 0.002(2) -0.001(2) -0.003(2) C(60) 0.022(2) 0.010(2) 0.015(2) 0.002(2) 0.005(2) 0.000(2) C(61) 0.023(3) 0.013(2) 0.021(3) -0.002(2) 0.004(2) 0.002(2) C(62) 0.010(2) 0.039(3) 0.018(2) 0.006(2) -0.001(2) 0.004(2) C(63) 0.018(3) 0.034(2) 0.021(3) 0.013(2) 0.006(2) 0.008(2) C(64) 0.019(3) 0.024(2) 0.023(3) 0.008(2) 0.003(2) 0.003(2) C(65) 0.018(2) 0.024(2) 0.017(2) 0.005(2) 0.005(2) 0.005(2) C(66) 0.020(3) 0.033(3) 0.026(3) 0.001(2) 0.007(2) -0.009(2) C(67) 0.027(3) 0.023(2) 0.015(2) 0.008(2) 0.005(2) 0.005(2) C(68) 0.023(3) 0.011(2) 0.023(3) 0.001(2) 0.005(2) -0.001(2) C(69) 0.015(2) 0.017(2) 0.022(3) 0.002(2) 0.005(2) 0.008(2) C(70) 0.018(3) 0.019(2) 0.039(3) -0.001(2) 0.007(2) 0.001(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; For all methyl groups of the complex, even if it is the lowest, one of H atoms was localized in the Fourier maps, respectively, and H atoms of the rest were placed in geometrically calculated positions. ; 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) O(1) 2.119(4) . . yes Ir(1) O(2) 2.118(3) . . yes Ir(1) N(1) 2.038(4) . . yes Ir(1) N(2) 2.038(4) . . yes Ir(1) C(9) 2.021(4) . . yes Ir(1) C(24) 2.029(5) . . yes Ir(2) O(3) 2.124(3) . . yes Ir(2) O(4) 2.122(4) . . yes Ir(2) N(3) 2.029(4) . . yes Ir(2) N(4) 2.031(4) . . yes Ir(2) C(44) 2.030(4) . . yes Ir(2) C(59) 2.037(6) . . yes O(1) C(32) 1.273(5) . . yes O(2) C(34) 1.268(5) . . yes O(3) C(67) 1.263(6) . . yes O(4) C(69) 1.274(5) . . yes N(1) C(1) 1.346(5) . . yes N(1) C(2) 1.355(5) . . yes N(2) C(16) 1.339(6) . . yes N(2) C(17) 1.364(6) . . yes N(3) C(36) 1.347(5) . . yes N(3) C(37) 1.361(5) . . yes N(4) C(51) 1.332(6) . . yes N(4) C(52) 1.359(5) . . yes C(1) C(5) 1.391(6) . . yes C(1) C(8) 1.424(6) . . yes C(2) C(3) 1.373(6) . . yes C(2) H(1) 0.961 . . no C(3) C(4) 1.392(6) . . yes C(3) H(2) 0.951 . . no C(4) C(5) 1.383(6) . . yes C(4) H(3) 0.948 . . no C(5) C(6) 1.516(6) . . yes C(6) C(7) 1.568(6) . . yes C(6) H(4) 0.944 . . no C(6) H(5) 0.954 . . no C(7) C(8) 1.534(5) . . yes C(7) H(6) 0.953 . . no C(7) H(7) 0.938 . . no C(8) C(9) 1.364(6) . . yes C(9) C(10) 1.490(6) . . yes C(10) C(11) 1.390(6) . . yes C(10) C(15) 1.389(6) . . yes C(11) C(12) 1.385(6) . . yes C(11) H(8) 0.957 . . no C(12) C(13) 1.394(6) . . yes C(12) H(9) 0.953 . . no C(13) C(14) 1.384(7) . . yes C(13) H(10) 0.950 . . no C(14) C(15) 1.390(6) . . yes C(14) H(11) 0.945 . . no C(15) H(12) 0.956 . . no C(16) C(20) 1.384(6) . . yes C(16) C(23) 1.422(6) . . yes C(17) C(18) 1.385(6) . . yes C(17) H(13) 0.948 . . no C(18) C(19) 1.404(7) . . yes C(18) H(14) 0.958 . . no C(19) C(20) 1.363(6) . . yes C(19) H(15) 0.947 . . no C(20) C(21) 1.521(7) . . yes C(21) C(22) 1.557(6) . . yes C(21) H(16) 0.952 . . no C(21) H(17) 0.940 . . no C(22) C(23) 1.524(7) . . yes C(22) H(18) 0.951 . . no C(22) H(19) 0.948 . . no C(23) C(24) 1.362(6) . . yes C(24) C(25) 1.476(6) . . yes C(25) C(26) 1.405(6) . . yes C(25) C(30) 1.406(5) . . yes C(26) C(27) 1.378(7) . . yes C(26) H(20) 0.963 . . no C(27) C(28) 1.383(6) . . yes C(27) H(21) 0.967 . . no C(28) C(29) 1.392(7) . . yes C(28) H(22) 0.960 . . no C(29) C(30) 1.385(7) . . yes C(29) H(23) 0.961 . . no C(30) H(24) 0.964 . . no C(31) C(32) 1.489(7) . . yes C(31) H(25) 0.964 . . no C(31) H(26) 0.950 . . no C(31) H(27) 0.948 . . no C(32) C(33) 1.410(6) . . yes C(33) C(34) 1.398(7) . . yes C(33) H(28) 0.958 . . no C(34) C(35) 1.506(5) . . yes C(35) H(29) 0.951 . . no C(35) H(30) 0.959 . . no C(35) H(31) 0.946 . . no C(36) C(40) 1.385(6) . . yes C(36) C(43) 1.429(6) . . yes C(37) C(38) 1.371(6) . . yes C(37) H(32) 0.960 . . no C(38) C(39) 1.403(6) . . yes C(38) H(33) 0.951 . . no C(39) C(40) 1.376(6) . . yes C(39) H(34) 0.948 . . no C(40) C(41) 1.520(6) . . yes C(41) C(42) 1.561(6) . . yes C(41) H(35) 0.946 . . no C(41) H(36) 0.953 . . no C(42) C(43) 1.518(5) . . yes C(42) H(37) 0.961 . . no C(42) H(38) 0.951 . . no C(43) C(44) 1.371(6) . . yes C(44) C(45) 1.493(6) . . yes C(45) C(46) 1.403(6) . . yes C(45) C(50) 1.387(6) . . yes C(46) C(47) 1.391(6) . . yes C(46) H(39) 0.956 . . no C(47) C(48) 1.382(7) . . yes C(47) H(40) 0.947 . . no C(48) C(49) 1.393(6) . . yes C(48) H(41) 0.952 . . no C(49) C(50) 1.377(6) . . yes C(49) H(42) 0.945 . . no C(50) H(43) 0.952 . . no C(51) C(55) 1.379(6) . . yes C(51) C(58) 1.435(6) . . yes C(52) C(53) 1.369(6) . . yes C(52) H(44) 0.944 . . no C(53) C(54) 1.394(7) . . yes C(53) H(45) 0.952 . . no C(54) C(55) 1.383(6) . . yes C(54) H(46) 0.955 . . no C(55) C(56) 1.513(7) . . yes C(56) C(57) 1.572(6) . . yes C(56) H(47) 0.949 . . no C(56) H(48) 0.955 . . no C(57) C(58) 1.526(6) . . yes C(57) H(49) 0.962 . . no C(57) H(50) 0.946 . . no C(58) C(59) 1.359(6) . . yes C(59) C(60) 1.482(6) . . yes C(60) C(61) 1.400(6) . . yes C(60) C(65) 1.396(5) . . yes C(61) C(62) 1.383(6) . . yes C(61) H(51) 0.953 . . no C(62) C(63) 1.400(6) . . yes C(62) H(52) 0.950 . . no C(63) C(64) 1.380(6) . . yes C(63) H(53) 0.953 . . no C(64) C(65) 1.389(6) . . yes C(64) H(54) 0.950 . . no C(65) H(55) 0.951 . . no C(66) C(67) 1.522(6) . . yes C(66) H(56) 0.946 . . no C(66) H(57) 0.953 . . no C(66) H(58) 0.952 . . no C(67) C(68) 1.387(7) . . yes C(68) C(69) 1.419(6) . . yes C(68) H(59) 0.963 . . no C(69) C(70) 1.490(7) . . yes C(70) H(60) 0.959 . . no C(70) H(61) 0.961 . . no C(70) H(62) 0.947 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ir(1) O(2) 89.6(1) . . . yes O(1) Ir(1) N(1) 88.9(1) . . . yes O(1) Ir(1) N(2) 91.8(2) . . . yes O(1) Ir(1) C(9) 85.6(2) . . . yes O(1) Ir(1) C(24) 171.9(1) . . . yes O(2) Ir(1) N(1) 91.8(1) . . . yes O(2) Ir(1) N(2) 90.5(1) . . . yes O(2) Ir(1) C(9) 172.0(1) . . . yes O(2) Ir(1) C(24) 86.0(1) . . . yes N(1) Ir(1) N(2) 177.6(1) . . . yes N(1) Ir(1) C(9) 81.8(2) . . . yes N(1) Ir(1) C(24) 98.0(2) . . . yes N(2) Ir(1) C(9) 96.0(2) . . . yes N(2) Ir(1) C(24) 81.5(2) . . . yes C(9) Ir(1) C(24) 99.6(2) . . . yes O(3) Ir(2) O(4) 89.4(1) . . . yes O(3) Ir(2) N(3) 89.3(1) . . . yes O(3) Ir(2) N(4) 90.1(1) . . . yes O(3) Ir(2) C(44) 170.8(2) . . . yes O(3) Ir(2) C(59) 88.4(1) . . . yes O(4) Ir(2) N(3) 89.1(1) . . . yes O(4) Ir(2) N(4) 90.6(1) . . . yes O(4) Ir(2) C(44) 87.6(1) . . . yes O(4) Ir(2) C(59) 171.8(1) . . . yes N(3) Ir(2) N(4) 179.3(1) . . . yes N(3) Ir(2) C(44) 81.9(2) . . . yes N(3) Ir(2) C(59) 98.7(2) . . . yes N(4) Ir(2) C(44) 98.7(2) . . . yes N(4) Ir(2) C(59) 81.5(2) . . . yes C(44) Ir(2) C(59) 95.7(2) . . . yes Ir(1) O(1) C(32) 124.5(3) . . . yes Ir(1) O(2) C(34) 124.6(3) . . . yes Ir(2) O(3) C(67) 123.9(3) . . . yes Ir(2) O(4) C(69) 124.6(3) . . . yes Ir(1) N(1) C(1) 109.9(3) . . . yes Ir(1) N(1) C(2) 133.5(3) . . . yes C(1) N(1) C(2) 116.6(4) . . . yes Ir(1) N(2) C(16) 111.2(3) . . . yes Ir(1) N(2) C(17) 131.9(3) . . . yes C(16) N(2) C(17) 116.9(4) . . . yes Ir(2) N(3) C(36) 111.4(3) . . . yes Ir(2) N(3) C(37) 132.7(3) . . . yes C(36) N(3) C(37) 115.9(4) . . . yes Ir(2) N(4) C(51) 111.5(3) . . . yes Ir(2) N(4) C(52) 132.0(3) . . . yes C(51) N(4) C(52) 116.5(4) . . . yes N(1) C(1) C(5) 125.2(4) . . . yes N(1) C(1) C(8) 119.8(4) . . . yes C(5) C(1) C(8) 114.8(4) . . . yes N(1) C(2) C(3) 121.3(4) . . . yes N(1) C(2) H(1) 118.4 . . . no C(3) C(2) H(1) 120.3 . . . no C(2) C(3) C(4) 121.7(4) . . . yes C(2) C(3) H(2) 119.6 . . . no C(4) C(3) H(2) 118.7 . . . no C(3) C(4) C(5) 117.6(4) . . . yes C(3) C(4) H(3) 120.8 . . . no C(5) C(4) H(3) 121.6 . . . no C(1) C(5) C(4) 117.5(4) . . . yes C(1) C(5) C(6) 107.9(4) . . . yes C(4) C(5) C(6) 134.4(4) . . . yes C(5) C(6) C(7) 105.6(3) . . . yes C(5) C(6) H(4) 110.1 . . . no C(5) C(6) H(5) 110.4 . . . no C(7) C(6) H(4) 111.1 . . . no C(7) C(6) H(5) 109.9 . . . no H(4) C(6) H(5) 109.6 . . . no C(6) C(7) C(8) 105.0(3) . . . yes C(6) C(7) H(6) 109.4 . . . no C(6) C(7) H(7) 110.7 . . . no C(8) C(7) H(6) 109.9 . . . no C(8) C(7) H(7) 111.6 . . . no H(6) C(7) H(7) 110.2 . . . no C(1) C(8) C(7) 106.7(4) . . . yes C(1) C(8) C(9) 114.3(4) . . . yes C(7) C(8) C(9) 138.4(4) . . . yes Ir(1) C(9) C(8) 112.3(3) . . . yes Ir(1) C(9) C(10) 127.7(3) . . . yes C(8) C(9) C(10) 119.8(4) . . . yes C(9) C(10) C(11) 120.8(4) . . . yes C(9) C(10) C(15) 121.8(4) . . . yes C(11) C(10) C(15) 117.4(4) . . . yes C(10) C(11) C(12) 122.5(4) . . . yes C(10) C(11) H(8) 118.9 . . . no C(12) C(11) H(8) 118.6 . . . no C(11) C(12) C(13) 119.1(4) . . . yes C(11) C(12) H(9) 121.3 . . . no C(13) C(12) H(9) 119.6 . . . no C(12) C(13) C(14) 119.4(4) . . . yes C(12) C(13) H(10) 120.4 . . . no C(14) C(13) H(10) 120.2 . . . no C(13) C(14) C(15) 120.5(4) . . . yes C(13) C(14) H(11) 119.2 . . . no C(15) C(14) H(11) 120.3 . . . no C(10) C(15) C(14) 121.1(4) . . . yes C(10) C(15) H(12) 119.9 . . . no C(14) C(15) H(12) 118.9 . . . no N(2) C(16) C(20) 124.8(4) . . . yes N(2) C(16) C(23) 119.0(4) . . . yes C(20) C(16) C(23) 116.0(4) . . . yes N(2) C(17) C(18) 120.5(4) . . . yes N(2) C(17) H(13) 119.3 . . . no C(18) C(17) H(13) 120.2 . . . no C(17) C(18) C(19) 121.8(4) . . . yes C(17) C(18) H(14) 118.5 . . . no C(19) C(18) H(14) 119.7 . . . no C(18) C(19) C(20) 116.7(4) . . . yes C(18) C(19) H(15) 121.6 . . . no C(20) C(19) H(15) 121.7 . . . no C(16) C(20) C(19) 119.4(5) . . . yes C(16) C(20) C(21) 106.7(4) . . . yes C(19) C(20) C(21) 133.7(4) . . . yes C(20) C(21) C(22) 105.7(4) . . . yes C(20) C(21) H(16) 109.6 . . . no C(20) C(21) H(17) 110.2 . . . no C(22) C(21) H(16) 110.2 . . . no C(22) C(21) H(17) 110.9 . . . no H(16) C(21) H(17) 110.1 . . . no C(21) C(22) C(23) 105.3(4) . . . yes C(21) C(22) H(18) 110.9 . . . no C(21) C(22) H(19) 110.6 . . . no C(23) C(22) H(18) 109.7 . . . no C(23) C(22) H(19) 110.8 . . . no H(18) C(22) H(19) 109.5 . . . no C(16) C(23) C(22) 105.7(4) . . . yes C(16) C(23) C(24) 115.1(4) . . . yes C(22) C(23) C(24) 138.5(4) . . . yes Ir(1) C(24) C(23) 112.3(3) . . . yes Ir(1) C(24) C(25) 127.1(3) . . . yes C(23) C(24) C(25) 120.3(4) . . . yes C(24) C(25) C(26) 121.2(4) . . . yes C(24) C(25) C(30) 121.1(4) . . . yes C(26) C(25) C(30) 117.6(4) . . . yes C(25) C(26) C(27) 121.1(4) . . . yes C(25) C(26) H(20) 119.1 . . . no C(27) C(26) H(20) 119.8 . . . no C(26) C(27) C(28) 120.9(4) . . . yes C(26) C(27) H(21) 119.5 . . . no C(28) C(27) H(21) 119.6 . . . no C(27) C(28) C(29) 119.0(4) . . . yes C(27) C(28) H(22) 120.7 . . . no C(29) C(28) H(22) 120.3 . . . no C(28) C(29) C(30) 120.7(4) . . . yes C(28) C(29) H(23) 119.5 . . . no C(30) C(29) H(23) 119.8 . . . no C(25) C(30) C(29) 120.7(4) . . . yes C(25) C(30) H(24) 119.5 . . . no C(29) C(30) H(24) 119.8 . . . no C(32) C(31) H(25) 109.4 . . . no C(32) C(31) H(26) 110.4 . . . no C(32) C(31) H(27) 110.5 . . . no H(25) C(31) H(26) 108.3 . . . no H(25) C(31) H(27) 108.5 . . . no H(26) C(31) H(27) 109.7 . . . no O(1) C(32) C(31) 115.3(4) . . . yes O(1) C(32) C(33) 126.4(5) . . . yes C(31) C(32) C(33) 118.3(4) . . . yes C(32) C(33) C(34) 127.8(4) . . . yes C(32) C(33) H(28) 115.6 . . . no C(34) C(33) H(28) 116.6 . . . no O(2) C(34) C(33) 126.8(4) . . . yes O(2) C(34) C(35) 115.9(4) . . . yes C(33) C(34) C(35) 117.3(4) . . . yes C(34) C(35) H(29) 109.9 . . . no C(34) C(35) H(30) 109.4 . . . no C(34) C(35) H(31) 110.1 . . . no H(29) C(35) H(30) 108.6 . . . no H(29) C(35) H(31) 109.7 . . . no H(30) C(35) H(31) 109.0 . . . no N(3) C(36) C(40) 125.8(4) . . . yes N(3) C(36) C(43) 118.8(4) . . . yes C(40) C(36) C(43) 115.3(4) . . . yes N(3) C(37) C(38) 121.5(4) . . . yes N(3) C(37) H(32) 118.2 . . . no C(38) C(37) H(32) 120.3 . . . no C(37) C(38) C(39) 121.5(4) . . . yes C(37) C(38) H(33) 119.6 . . . no C(39) C(38) H(33) 118.9 . . . no C(38) C(39) C(40) 117.5(4) . . . yes C(38) C(39) H(34) 121.4 . . . no C(40) C(39) H(34) 121.2 . . . no C(36) C(40) C(39) 117.7(4) . . . yes C(36) C(40) C(41) 107.3(4) . . . yes C(39) C(40) C(41) 134.9(4) . . . yes C(40) C(41) C(42) 105.3(3) . . . yes C(40) C(41) H(35) 110.6 . . . no C(40) C(41) H(36) 109.8 . . . no C(42) C(41) H(35) 111.1 . . . no C(42) C(41) H(36) 110.4 . . . no H(35) C(41) H(36) 109.5 . . . no C(41) C(42) C(43) 105.7(3) . . . yes C(41) C(42) H(37) 109.8 . . . no C(41) C(42) H(38) 110.7 . . . no C(43) C(42) H(37) 111.1 . . . no C(43) C(42) H(38) 111.0 . . . no H(37) C(42) H(38) 108.5 . . . no C(36) C(43) C(42) 106.0(4) . . . yes C(36) C(43) C(44) 115.0(4) . . . yes C(42) C(43) C(44) 138.6(4) . . . yes Ir(2) C(44) C(43) 112.3(3) . . . yes Ir(2) C(44) C(45) 126.5(3) . . . yes C(43) C(44) C(45) 121.2(4) . . . yes C(44) C(45) C(46) 120.2(4) . . . yes C(44) C(45) C(50) 121.5(4) . . . yes C(46) C(45) C(50) 118.3(4) . . . yes C(45) C(46) C(47) 121.1(4) . . . yes C(45) C(46) H(39) 120.0 . . . no C(47) C(46) H(39) 118.9 . . . no C(46) C(47) C(48) 119.5(4) . . . yes C(46) C(47) H(40) 120.1 . . . no C(48) C(47) H(40) 120.4 . . . no C(47) C(48) C(49) 119.6(4) . . . yes C(47) C(48) H(41) 120.7 . . . no C(49) C(48) H(41) 119.7 . . . no C(48) C(49) C(50) 120.8(5) . . . yes C(48) C(49) H(42) 119.2 . . . no C(50) C(49) H(42) 120.0 . . . no C(45) C(50) C(49) 120.7(4) . . . yes C(45) C(50) H(43) 119.5 . . . no C(49) C(50) H(43) 119.9 . . . no N(4) C(51) C(55) 125.6(4) . . . yes N(4) C(51) C(58) 118.8(4) . . . yes C(55) C(51) C(58) 115.2(4) . . . yes N(4) C(52) C(53) 121.7(4) . . . yes N(4) C(52) H(44) 118.8 . . . no C(53) C(52) H(44) 119.5 . . . no C(52) C(53) C(54) 120.7(4) . . . yes C(52) C(53) H(45) 119.3 . . . no C(54) C(53) H(45) 120.0 . . . no C(53) C(54) C(55) 118.0(4) . . . yes C(53) C(54) H(46) 120.9 . . . no C(55) C(54) H(46) 121.1 . . . no C(51) C(55) C(54) 117.5(4) . . . yes C(51) C(55) C(56) 108.2(4) . . . yes C(54) C(55) C(56) 134.3(5) . . . yes C(55) C(56) C(57) 105.1(4) . . . yes C(55) C(56) H(47) 110.6 . . . no C(55) C(56) H(48) 110.8 . . . no C(57) C(56) H(47) 111.0 . . . no C(57) C(56) H(48) 110.1 . . . no H(47) C(56) H(48) 109.2 . . . no C(56) C(57) C(58) 105.5(4) . . . yes C(56) C(57) H(49) 109.5 . . . no C(56) C(57) H(50) 110.7 . . . no C(58) C(57) H(49) 110.7 . . . no C(58) C(57) H(50) 111.6 . . . no H(49) C(57) H(50) 108.8 . . . no C(51) C(58) C(57) 105.8(4) . . . yes C(51) C(58) C(59) 115.2(4) . . . yes C(57) C(58) C(59) 138.5(4) . . . yes Ir(2) C(59) C(58) 112.0(3) . . . yes Ir(2) C(59) C(60) 127.1(3) . . . yes C(58) C(59) C(60) 120.9(4) . . . yes C(59) C(60) C(61) 120.4(3) . . . yes C(59) C(60) C(65) 121.5(4) . . . yes C(61) C(60) C(65) 118.1(4) . . . yes C(60) C(61) C(62) 121.2(4) . . . yes C(60) C(61) H(51) 119.5 . . . no C(62) C(61) H(51) 119.3 . . . no C(61) C(62) C(63) 119.8(4) . . . yes C(61) C(62) H(52) 121.0 . . . no C(63) C(62) H(52) 119.3 . . . no C(62) C(63) C(64) 119.5(4) . . . yes C(62) C(63) H(53) 119.5 . . . no C(64) C(63) H(53) 120.9 . . . no C(63) C(64) C(65) 120.5(4) . . . yes C(63) C(64) H(54) 119.1 . . . no C(65) C(64) H(54) 120.4 . . . no C(60) C(65) C(64) 120.8(4) . . . yes C(60) C(65) H(55) 119.4 . . . no C(64) C(65) H(55) 119.8 . . . no C(67) C(66) H(56) 109.9 . . . no C(67) C(66) H(57) 109.5 . . . no C(67) C(66) H(58) 109.2 . . . no H(56) C(66) H(57) 109.5 . . . no H(56) C(66) H(58) 109.6 . . . no H(57) C(66) H(58) 109.1 . . . no O(3) C(67) C(66) 115.5(4) . . . yes O(3) C(67) C(68) 128.0(4) . . . yes C(66) C(67) C(68) 116.6(4) . . . yes C(67) C(68) C(69) 126.9(4) . . . yes C(67) C(68) H(59) 117.1 . . . no C(69) C(68) H(59) 115.9 . . . no O(4) C(69) C(68) 126.3(4) . . . yes O(4) C(69) C(70) 115.5(4) . . . yes C(68) C(69) C(70) 118.1(4) . . . yes C(69) C(70) H(60) 110.3 . . . no C(69) C(70) H(61) 110.1 . . . no C(69) C(70) H(62) 110.8 . . . no H(60) C(70) H(61) 107.8 . . . no H(60) C(70) H(62) 108.9 . . . no H(61) C(70) H(62) 108.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) O(1) C(32) C(31) -174.4(3) . . . . yes Ir(1) O(1) C(32) C(33) 4.8(7) . . . . yes Ir(1) O(2) C(34) C(33) 0.9(7) . . . . yes Ir(1) O(2) C(34) C(35) -177.7(3) . . . . yes Ir(1) N(1) C(1) C(5) 179.3(4) . . . . yes Ir(1) N(1) C(1) C(8) -5.7(5) . . . . yes Ir(1) N(1) C(2) C(3) -178.5(3) . . . . yes Ir(1) N(2) C(16) C(20) -174.6(3) . . . . yes Ir(1) N(2) C(16) C(23) -0.6(4) . . . . yes Ir(1) N(2) C(17) C(18) 174.9(3) . . . . yes Ir(1) C(9) C(8) C(1) 13.5(5) . . . . yes Ir(1) C(9) C(8) C(7) -177.4(5) . . . . yes Ir(1) C(9) C(10) C(11) -50.5(6) . . . . yes Ir(1) C(9) C(10) C(15) 129.4(4) . . . . yes Ir(1) C(24) C(23) C(16) 10.6(4) . . . . yes Ir(1) C(24) C(23) C(22) 179.5(4) . . . . yes Ir(1) C(24) C(25) C(26) 129.2(4) . . . . yes Ir(1) C(24) C(25) C(30) -53.3(5) . . . . yes Ir(2) O(3) C(67) C(66) 169.3(3) . . . . yes Ir(2) O(3) C(67) C(68) -10.2(7) . . . . yes Ir(2) O(4) C(69) C(68) -5.8(6) . . . . yes Ir(2) O(4) C(69) C(70) 176.7(3) . . . . yes Ir(2) N(3) C(36) C(40) 178.7(4) . . . . yes Ir(2) N(3) C(36) C(43) 2.8(5) . . . . yes Ir(2) N(3) C(37) C(38) 178.0(3) . . . . yes Ir(2) N(4) C(51) C(55) 177.4(3) . . . . yes Ir(2) N(4) C(51) C(58) 5.5(5) . . . . yes Ir(2) N(4) C(52) C(53) 179.7(3) . . . . yes Ir(2) C(44) C(43) C(36) -7.4(5) . . . . yes Ir(2) C(44) C(43) C(42) -179.5(4) . . . . yes Ir(2) C(44) C(45) C(46) -135.4(3) . . . . yes Ir(2) C(44) C(45) C(50) 44.1(5) . . . . yes Ir(2) C(59) C(58) C(51) -8.7(5) . . . . yes Ir(2) C(59) C(58) C(57) -179.7(4) . . . . yes Ir(2) C(59) C(60) C(61) -132.6(4) . . . . yes Ir(2) C(59) C(60) C(65) 48.7(6) . . . . yes O(1) Ir(1) O(2) C(34) 3.2(3) . . . . yes O(1) Ir(1) N(1) C(1) -75.8(3) . . . . yes O(1) Ir(1) N(1) C(2) 104.1(4) . . . . yes O(1) Ir(1) N(2) C(16) -170.5(3) . . . . yes O(1) Ir(1) N(2) C(17) 13.3(3) . . . . yes O(1) Ir(1) C(9) C(8) 76.6(4) . . . . yes O(1) Ir(1) C(9) C(10) -97.7(4) . . . . yes O(1) Ir(1) C(24) C(23) 25(1) . . . . yes O(1) Ir(1) C(24) C(25) -147.6(8) . . . . yes O(1) C(32) C(33) C(34) 1.4(9) . . . . yes O(2) Ir(1) O(1) C(32) -5.9(3) . . . . yes O(2) Ir(1) N(1) C(1) -165.3(3) . . . . yes O(2) Ir(1) N(1) C(2) 14.5(4) . . . . yes O(2) Ir(1) N(2) C(16) -80.9(3) . . . . yes O(2) Ir(1) N(2) C(17) 103.0(3) . . . . yes O(2) Ir(1) C(9) C(8) 23(1) . . . . yes O(2) Ir(1) C(9) C(10) -150.3(9) . . . . yes O(2) Ir(1) C(24) C(23) 82.6(3) . . . . yes O(2) Ir(1) C(24) C(25) -90.8(3) . . . . yes O(2) C(34) C(33) C(32) -4.7(9) . . . . yes O(3) Ir(2) O(4) C(69) -0.8(3) . . . . yes O(3) Ir(2) N(3) C(36) 171.9(3) . . . . yes O(3) Ir(2) N(3) C(37) -5.2(4) . . . . yes O(3) Ir(2) N(4) C(51) 80.6(3) . . . . yes O(3) Ir(2) N(4) C(52) -98.7(3) . . . . yes O(3) Ir(2) C(44) C(43) -11(1) . . . . yes O(3) Ir(2) C(44) C(45) 167.7(7) . . . . yes O(3) Ir(2) C(59) C(58) -81.3(3) . . . . yes O(3) Ir(2) C(59) C(60) 97.4(3) . . . . yes O(3) C(67) C(68) C(69) 2.0(8) . . . . yes O(4) Ir(2) O(3) C(67) 8.4(3) . . . . yes O(4) Ir(2) N(3) C(36) 82.5(3) . . . . yes O(4) Ir(2) N(3) C(37) -94.6(4) . . . . yes O(4) Ir(2) N(4) C(51) 170.0(3) . . . . yes O(4) Ir(2) N(4) C(52) -9.3(3) . . . . yes O(4) Ir(2) C(44) C(43) -82.5(3) . . . . yes O(4) Ir(2) C(44) C(45) 96.4(4) . . . . yes O(4) Ir(2) C(59) C(58) -6(1) . . . . yes O(4) Ir(2) C(59) C(60) 171.9(7) . . . . yes O(4) C(69) C(68) C(67) 7.2(8) . . . . yes N(1) Ir(1) O(1) C(32) -97.8(4) . . . . yes N(1) Ir(1) O(2) C(34) 92.1(4) . . . . yes N(1) Ir(1) N(2) C(16) 82(3) . . . . yes N(1) Ir(1) N(2) C(17) -93(3) . . . . yes N(1) Ir(1) C(9) C(8) -13.0(3) . . . . yes N(1) Ir(1) C(9) C(10) 172.8(4) . . . . yes N(1) Ir(1) C(24) C(23) 173.9(3) . . . . yes N(1) Ir(1) C(24) C(25) 0.5(3) . . . . yes N(1) C(1) C(5) C(4) 1.4(7) . . . . yes N(1) C(1) C(5) C(6) 177.2(4) . . . . yes N(1) C(1) C(8) C(7) -177.7(4) . . . . yes N(1) C(1) C(8) C(9) -5.2(6) . . . . yes N(1) C(2) C(3) C(4) -3.2(7) . . . . yes N(2) Ir(1) O(1) C(32) 84.5(4) . . . . yes N(2) Ir(1) O(2) C(34) -88.6(4) . . . . yes N(2) Ir(1) N(1) C(1) 31(3) . . . . yes N(2) Ir(1) N(1) C(2) -148(3) . . . . yes N(2) Ir(1) C(9) C(8) 167.9(3) . . . . yes N(2) Ir(1) C(9) C(10) -6.3(4) . . . . yes N(2) Ir(1) C(24) C(23) -8.5(3) . . . . yes N(2) Ir(1) C(24) C(25) 178.1(3) . . . . yes N(2) C(16) C(20) C(19) -1.4(6) . . . . yes N(2) C(16) C(20) C(21) 173.6(4) . . . . yes N(2) C(16) C(23) C(22) -179.2(3) . . . . yes N(2) C(16) C(23) C(24) -6.8(5) . . . . yes N(2) C(17) C(18) C(19) -0.7(6) . . . . yes N(3) Ir(2) O(3) C(67) -80.8(3) . . . . yes N(3) Ir(2) O(4) C(69) 88.5(3) . . . . yes N(3) Ir(2) N(4) C(51) 103(10) . . . . yes N(3) Ir(2) N(4) C(52) -75(10) . . . . yes N(3) Ir(2) C(44) C(43) 6.9(3) . . . . yes N(3) Ir(2) C(44) C(45) -174.2(4) . . . . yes N(3) Ir(2) C(59) C(58) -170.4(3) . . . . yes N(3) Ir(2) C(59) C(60) 8.4(4) . . . . yes N(3) C(36) C(40) C(39) 3.5(7) . . . . yes N(3) C(36) C(40) C(41) -174.2(4) . . . . yes N(3) C(36) C(43) C(42) 177.7(4) . . . . yes N(3) C(36) C(43) C(44) 3.1(6) . . . . yes N(3) C(37) C(38) C(39) 1.7(7) . . . . yes N(4) Ir(2) O(3) C(67) 99.0(3) . . . . yes N(4) Ir(2) O(4) C(69) -90.9(3) . . . . yes N(4) Ir(2) N(3) C(36) 148(10) . . . . yes N(4) Ir(2) N(3) C(37) -28(11) . . . . yes N(4) Ir(2) C(44) C(43) -172.8(3) . . . . yes N(4) Ir(2) C(44) C(45) 6.1(4) . . . . yes N(4) Ir(2) C(59) C(58) 9.0(3) . . . . yes N(4) Ir(2) C(59) C(60) -172.3(4) . . . . yes N(4) C(51) C(55) C(54) 3.8(6) . . . . yes N(4) C(51) C(55) C(56) -174.0(4) . . . . yes N(4) C(51) C(58) C(57) 176.0(4) . . . . yes N(4) C(51) C(58) C(59) 2.2(6) . . . . yes N(4) C(52) C(53) C(54) 1.6(6) . . . . yes C(1) N(1) Ir(1) C(9) 9.9(3) . . . . yes C(1) N(1) Ir(1) C(24) 108.5(3) . . . . yes C(1) N(1) C(2) C(3) 1.4(6) . . . . yes C(1) C(5) C(4) C(3) -3.0(7) . . . . yes C(1) C(5) C(6) C(7) -0.9(5) . . . . yes C(1) C(8) C(7) C(6) 1.4(5) . . . . yes C(1) C(8) C(9) C(10) -171.8(4) . . . . yes C(2) N(1) Ir(1) C(9) -170.2(4) . . . . yes C(2) N(1) Ir(1) C(24) -71.6(4) . . . . yes C(2) N(1) C(1) C(5) -0.6(7) . . . . yes C(2) N(1) C(1) C(8) 174.4(4) . . . . yes C(2) C(3) C(4) C(5) 4.0(7) . . . . yes C(3) C(4) C(5) C(6) -177.4(5) . . . . yes C(4) C(5) C(1) C(8) -173.8(4) . . . . yes C(4) C(5) C(6) C(7) 173.8(5) . . . . yes C(5) C(1) C(8) C(7) -2.2(5) . . . . yes C(5) C(1) C(8) C(9) 170.3(4) . . . . yes C(5) C(6) C(7) C(8) -0.3(5) . . . . yes C(6) C(5) C(1) C(8) 2.0(6) . . . . yes C(6) C(7) C(8) C(9) -168.2(6) . . . . yes C(7) C(8) C(9) C(10) -2.6(9) . . . . yes C(8) C(9) Ir(1) C(24) -109.7(4) . . . . yes C(8) C(9) C(10) C(11) 135.6(5) . . . . yes C(8) C(9) C(10) C(15) -44.5(6) . . . . yes C(9) Ir(1) O(1) C(32) -179.6(4) . . . . yes C(9) Ir(1) O(2) C(34) 55(1) . . . . yes C(9) Ir(1) N(2) C(16) 103.8(3) . . . . yes C(9) Ir(1) N(2) C(17) -72.4(4) . . . . yes C(9) Ir(1) C(24) C(23) -103.2(3) . . . . yes C(9) Ir(1) C(24) C(25) 83.5(3) . . . . yes C(9) C(10) C(11) C(12) -178.4(4) . . . . yes C(9) C(10) C(15) C(14) 179.3(4) . . . . yes C(10) C(9) Ir(1) C(24) 76.0(4) . . . . yes C(10) C(11) C(12) C(13) -1.6(7) . . . . yes C(10) C(15) C(14) C(13) -0.1(7) . . . . yes C(11) C(10) C(15) C(14) -0.7(6) . . . . yes C(11) C(12) C(13) C(14) 0.7(7) . . . . yes C(12) C(11) C(10) C(15) 1.6(6) . . . . yes C(12) C(13) C(14) C(15) 0.2(7) . . . . yes C(16) N(2) Ir(1) C(24) 4.9(3) . . . . yes C(16) N(2) C(17) C(18) -1.1(5) . . . . yes C(16) C(20) C(19) C(18) -0.4(6) . . . . yes C(16) C(20) C(21) C(22) 5.4(4) . . . . yes C(16) C(23) C(22) C(21) 7.7(4) . . . . yes C(16) C(23) C(24) C(25) -175.5(3) . . . . yes C(17) N(2) Ir(1) C(24) -171.2(4) . . . . yes C(17) N(2) C(16) C(20) 2.2(6) . . . . yes C(17) N(2) C(16) C(23) 176.1(3) . . . . yes C(17) C(18) C(19) C(20) 1.5(6) . . . . yes C(18) C(19) C(20) C(21) -173.9(4) . . . . yes C(19) C(20) C(16) C(23) -175.6(4) . . . . yes C(19) C(20) C(21) C(22) 179.4(4) . . . . yes C(20) C(16) C(23) C(22) -4.7(5) . . . . yes C(20) C(16) C(23) C(24) 167.7(4) . . . . yes C(20) C(21) C(22) C(23) -8.0(4) . . . . yes C(21) C(20) C(16) C(23) -0.5(5) . . . . yes C(21) C(22) C(23) C(24) -161.9(5) . . . . yes C(22) C(23) C(24) C(25) -6.6(7) . . . . yes C(23) C(24) C(25) C(26) -43.7(6) . . . . yes C(23) C(24) C(25) C(30) 133.8(4) . . . . yes C(24) Ir(1) O(1) C(32) 50(1) . . . . yes C(24) Ir(1) O(2) C(34) -170.0(4) . . . . yes C(24) C(25) C(26) C(27) 177.9(4) . . . . yes C(24) C(25) C(30) C(29) -176.4(4) . . . . yes C(25) C(26) C(27) C(28) -1.5(7) . . . . yes C(25) C(30) C(29) C(28) -1.6(7) . . . . yes C(26) C(25) C(30) C(29) 1.2(6) . . . . yes C(26) C(27) C(28) C(29) 1.0(7) . . . . yes C(27) C(26) C(25) C(30) 0.4(6) . . . . yes C(27) C(28) C(29) C(30) 0.5(7) . . . . yes C(31) C(32) C(33) C(34) -179.4(5) . . . . yes C(32) C(33) C(34) C(35) 173.9(5) . . . . yes C(36) N(3) Ir(2) C(44) -5.2(3) . . . . yes C(36) N(3) Ir(2) C(59) -99.8(3) . . . . yes C(36) N(3) C(37) C(38) 1.0(6) . . . . yes C(36) C(40) C(39) C(38) -0.6(6) . . . . yes C(36) C(40) C(41) C(42) -4.0(5) . . . . yes C(36) C(43) C(42) C(41) -3.9(5) . . . . yes C(36) C(43) C(44) C(45) 173.7(4) . . . . yes C(37) N(3) Ir(2) C(44) 177.6(4) . . . . yes C(37) N(3) Ir(2) C(59) 83.1(4) . . . . yes C(37) N(3) C(36) C(40) -3.7(6) . . . . yes C(37) N(3) C(36) C(43) -179.5(4) . . . . yes C(37) C(38) C(39) C(40) -1.8(7) . . . . yes C(38) C(39) C(40) C(41) 176.4(5) . . . . yes C(39) C(40) C(36) C(43) 179.5(4) . . . . yes C(39) C(40) C(41) C(42) 178.8(5) . . . . yes C(40) C(36) C(43) C(42) 1.4(5) . . . . yes C(40) C(36) C(43) C(44) -173.2(4) . . . . yes C(40) C(41) C(42) C(43) 4.8(5) . . . . yes C(41) C(40) C(36) C(43) 1.7(5) . . . . yes C(41) C(42) C(43) C(44) 168.7(5) . . . . yes C(42) C(43) C(44) C(45) 1.5(8) . . . . yes C(43) C(44) Ir(2) C(59) 105.0(3) . . . . yes C(43) C(44) C(45) C(46) 43.4(6) . . . . yes C(43) C(44) C(45) C(50) -137.1(4) . . . . yes C(44) Ir(2) O(3) C(67) -62.8(9) . . . . yes C(44) Ir(2) O(4) C(69) 170.4(3) . . . . yes C(44) Ir(2) N(4) C(51) -102.3(3) . . . . yes C(44) Ir(2) N(4) C(52) 78.4(4) . . . . yes C(44) Ir(2) C(59) C(58) 107.0(3) . . . . yes C(44) Ir(2) C(59) C(60) -74.3(4) . . . . yes C(44) C(45) C(46) C(47) 179.6(4) . . . . yes C(44) C(45) C(50) C(49) 179.2(4) . . . . yes C(45) C(44) Ir(2) C(59) -76.1(4) . . . . yes C(45) C(46) C(47) C(48) 0.9(6) . . . . yes C(45) C(50) C(49) C(48) 1.4(6) . . . . yes C(46) C(45) C(50) C(49) -1.3(6) . . . . yes C(46) C(47) C(48) C(49) -0.7(6) . . . . yes C(47) C(46) C(45) C(50) 0.1(6) . . . . yes C(47) C(48) C(49) C(50) -0.4(6) . . . . yes C(51) N(4) Ir(2) C(59) -7.8(3) . . . . yes C(51) N(4) C(52) C(53) 0.4(6) . . . . yes C(51) C(55) C(54) C(53) -1.6(6) . . . . yes C(51) C(55) C(56) C(57) -0.4(5) . . . . yes C(51) C(58) C(57) C(56) -3.2(4) . . . . yes C(51) C(58) C(59) C(60) 172.5(3) . . . . yes C(52) N(4) Ir(2) C(59) 172.9(4) . . . . yes C(52) N(4) C(51) C(55) -3.2(6) . . . . yes C(52) N(4) C(51) C(58) -175.1(3) . . . . yes C(52) C(53) C(54) C(55) -0.9(6) . . . . yes C(53) C(54) C(55) C(56) 175.5(4) . . . . yes C(54) C(55) C(51) C(58) 176.0(4) . . . . yes C(54) C(55) C(56) C(57) -177.7(4) . . . . yes C(55) C(51) C(58) C(57) 3.3(5) . . . . yes C(55) C(51) C(58) C(59) -170.5(4) . . . . yes C(55) C(56) C(57) C(58) 2.2(4) . . . . yes C(56) C(55) C(51) C(58) -1.8(5) . . . . yes C(56) C(57) C(58) C(59) 168.3(5) . . . . yes C(57) C(58) C(59) C(60) 1.5(8) . . . . yes C(58) C(59) C(60) C(61) 46.0(6) . . . . yes C(58) C(59) C(60) C(65) -132.7(5) . . . . yes C(59) Ir(2) O(3) C(67) -179.5(4) . . . . yes C(59) Ir(2) O(4) C(69) -75(1) . . . . yes C(59) C(60) C(61) C(62) -179.1(4) . . . . yes C(59) C(60) C(65) C(64) 177.9(4) . . . . yes C(60) C(61) C(62) C(63) 0.6(7) . . . . yes C(60) C(65) C(64) C(63) 1.8(7) . . . . yes C(61) C(60) C(65) C(64) -0.8(7) . . . . yes C(61) C(62) C(63) C(64) 0.4(7) . . . . yes C(62) C(61) C(60) C(65) -0.4(7) . . . . yes C(62) C(63) C(64) C(65) -1.6(7) . . . . yes C(66) C(67) C(68) C(69) -177.4(4) . . . . yes C(67) C(68) C(69) C(70) -175.3(4) . . . . yes C(67) C(68) C(69) C(70) -175.3(4) . . . . 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 O(3) C(56) 3.372(7) . 2_564 ? O(3) C(57) 3.505(6) . 2_564 ? O(4) C(41) 3.457(6) . 2_454 ? O(4) C(42) 3.527(5) . 2_454 ? C(4) C(62) 3.331(7) . . ? C(4) C(63) 3.390(7) . . ? C(4) C(38) 3.496(8) . . ? C(4) C(37) 3.505(7) . . ? C(14) C(35) 3.581(6) . 1_545 ? C(19) C(52) 3.441(6) . 1_656 ? C(19) C(47) 3.462(6) . 1_656 ? C(19) C(53) 3.517(6) . 1_656 ? C(19) C(48) 3.564(7) . 1_656 ? C(21) C(31) 3.583(9) . 1_655 ? C(29) C(47) 3.527(6) . 2_554 ? C(39) C(46) 3.598(8) . 2_454 ? C(40) C(46) 3.537(8) . 2_454 ? #===END #------------------------------------------------------------------------------ data_4b _database_code_depnum_ccdc_archive 'CCDC 616851' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C37 H35 Ir N2 O2 ' _chemical_formula_moiety ? _chemical_formula_weight 731.92 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.73(2) _cell_length_b 14.00(2) _cell_length_c 16.84(3) _cell_angle_alpha 101.66(6) _cell_angle_beta 101.76(6) _cell_angle_gamma 103.76(6) _cell_volume 2969(25) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25326 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.350 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.028 _exptl_absorpt_correction_T_max 0.204 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27059 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9415 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9415 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12816 _reflns_number_gt 10471 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.1167 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 12816 _refine_ls_number_parameters 757 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0013 _refine_diff_density_max 1.65 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ir Ir -1.444 7.990 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.19549(2) 0.03682(2) 0.25099(1) 0.01504(6) Uani 1.00 d . . . Ir(2) Ir -0.32550(2) 0.46842(2) 0.22403(1) 0.01535(6) Uani 1.00 d . . . O(1) O 0.2117(3) 0.1945(3) 0.3037(3) 0.021(1) Uani 1.00 d . . . O(2) O 0.2861(3) 0.0811(3) 0.1676(2) 0.018(1) Uani 1.00 d . . . O(3) O -0.4922(3) 0.4372(3) 0.1780(3) 0.021(1) Uani 1.00 d . . . O(4) O -0.3116(3) 0.5802(3) 0.1535(3) 0.020(1) Uani 1.00 d . . . N(1) N 0.0651(3) 0.0147(4) 0.1594(3) 0.018(1) Uani 1.00 d . . . N(2) N 0.3199(3) 0.0593(3) 0.3504(3) 0.017(1) Uani 1.00 d . . . N(3) N -0.3171(4) 0.5778(4) 0.3272(3) 0.018(1) Uani 1.00 d . . . N(4) N -0.3218(3) 0.3555(4) 0.1275(3) 0.020(1) Uani 1.00 d . . . C(1) C 0.0184(5) 0.0854(4) 0.1470(4) 0.022(2) Uani 1.00 d . . . C(2) C -0.0725(4) 0.0642(4) 0.0851(4) 0.022(2) Uani 1.00 d . . . C(3) C -0.1177(4) -0.0329(4) 0.0353(4) 0.022(2) Uani 1.00 d . . . C(4) C -0.0718(4) -0.1089(4) 0.0473(4) 0.019(1) Uani 1.00 d . . . C(5) C -0.1149(4) -0.2184(4) -0.0043(4) 0.023(2) Uani 1.00 d . . . C(6) C -0.0760(5) -0.2918(5) 0.0399(4) 0.028(2) Uani 1.00 d . . . C(7) C 0.0433(4) -0.2581(4) 0.0684(4) 0.022(2) Uani 1.00 d . . . C(8) C 0.0827(4) -0.1515(4) 0.1278(4) 0.018(1) Uani 1.00 d . . . C(9) C 0.0236(4) -0.0833(4) 0.1096(4) 0.017(1) Uani 1.00 d . . . C(10) C 0.1683(4) -0.1082(4) 0.1931(4) 0.017(1) Uani 1.00 d . . . C(11) C 0.2413(5) -0.1685(5) 0.2184(4) 0.024(2) Uani 1.00 d . . . C(12) C 0.3464(5) -0.1328(5) 0.2205(4) 0.025(2) Uani 1.00 d . . . C(13) C 0.4137(5) -0.1900(6) 0.2442(5) 0.039(2) Uani 1.00 d . . . C(14) C 0.3797(6) -0.2771(6) 0.2663(5) 0.041(2) Uani 1.00 d . . . C(15) C 0.2780(6) -0.3114(5) 0.2656(5) 0.039(2) Uani 1.00 d . . . C(16) C 0.2076(5) -0.2586(5) 0.2419(4) 0.030(2) Uani 1.00 d . . . C(17) C 0.4199(4) 0.1073(5) 0.3559(4) 0.023(2) Uani 1.00 d . . . C(18) C 0.4963(4) 0.1327(5) 0.4304(4) 0.024(2) Uani 1.00 d . . . C(19) C 0.4722(4) 0.1046(5) 0.4992(4) 0.023(2) Uani 1.00 d . . . C(20) C 0.3686(4) 0.0526(4) 0.4943(4) 0.022(2) Uani 1.00 d . . . C(21) C 0.3361(5) 0.0211(5) 0.5665(4) 0.025(2) Uani 1.00 d . . . C(22) C 0.2377(5) -0.0699(5) 0.5349(4) 0.030(2) Uani 1.00 d . . . C(23) C 0.1503(5) -0.0414(5) 0.4804(4) 0.026(2) Uani 1.00 d . . . C(24) C 0.1837(4) -0.0099(4) 0.4072(4) 0.020(2) Uani 1.00 d . . . C(25) C 0.2950(4) 0.0330(4) 0.4185(4) 0.019(1) Uani 1.00 d . . . C(26) C 0.1225(4) -0.0119(4) 0.3334(4) 0.021(2) Uani 1.00 d . . . C(27) C 0.0084(5) -0.0538(4) 0.3126(4) 0.021(2) Uani 1.00 d . . . C(28) C -0.0392(5) -0.1578(5) 0.2955(4) 0.027(2) Uani 1.00 d . . . C(29) C -0.1473(5) -0.1974(5) 0.2746(4) 0.031(2) Uani 1.00 d . . . C(30) C -0.2100(5) -0.1350(5) 0.2674(5) 0.032(2) Uani 1.00 d . . . C(31) C -0.1640(5) -0.0300(5) 0.2828(4) 0.031(2) Uani 1.00 d . . . C(32) C -0.0569(4) 0.0097(4) 0.3048(4) 0.022(2) Uani 1.00 d . . . C(33) C 0.2883(5) 0.3726(4) 0.3410(4) 0.027(2) Uani 1.00 d . . . C(34) C 0.2741(4) 0.2667(4) 0.2870(4) 0.021(2) Uani 1.00 d . . . C(35) C 0.3293(4) 0.2591(4) 0.2271(4) 0.022(2) Uani 1.00 d . . . C(36) C 0.3316(4) 0.1724(4) 0.1704(4) 0.019(1) Uani 1.00 d . . . C(37) C 0.3918(4) 0.1847(4) 0.1059(4) 0.023(2) Uani 1.00 d . . . C(38) C -0.3972(4) 0.6117(4) 0.3439(4) 0.021(2) Uani 1.00 d . . . C(39) C -0.3830(4) 0.6850(4) 0.4145(4) 0.024(2) Uani 1.00 d . . . C(40) C -0.2874(5) 0.7270(5) 0.4729(4) 0.026(2) Uani 1.00 d . . . C(41) C -0.2038(5) 0.6929(5) 0.4562(4) 0.024(2) Uani 1.00 d . . . C(42) C -0.0967(5) 0.7366(5) 0.5159(4) 0.033(2) Uani 1.00 d . . . C(43) C -0.0334(5) 0.6626(6) 0.5036(4) 0.037(2) Uani 1.00 d . . . C(44) C -0.0329(4) 0.6255(5) 0.4127(4) 0.027(2) Uani 1.00 d . . . C(45) C -0.1411(5) 0.5817(5) 0.3554(4) 0.022(2) Uani 1.00 d . . . C(46) C -0.2220(4) 0.6199(4) 0.3818(4) 0.019(1) Uani 1.00 d . . . C(47) C -0.1733(4) 0.5108(4) 0.2807(4) 0.019(1) Uani 1.00 d . . . C(48) C -0.0961(4) 0.4696(4) 0.2454(4) 0.021(2) Uani 1.00 d . . . C(49) C -0.0606(5) 0.5030(5) 0.1812(5) 0.031(2) Uani 1.00 d . . . C(50) C 0.0163(6) 0.4677(5) 0.1530(5) 0.037(2) Uani 1.00 d . . . C(51) C 0.0518(6) 0.3941(6) 0.1818(5) 0.040(2) Uani 1.00 d . . . C(52) C 0.0123(5) 0.3557(5) 0.2416(5) 0.033(2) Uani 1.00 d . . . C(53) C -0.0614(5) 0.3929(5) 0.2733(4) 0.031(2) Uani 1.00 d . . . C(54) C -0.3108(5) 0.3665(5) 0.0527(4) 0.025(2) Uani 1.00 d . . . C(55) C -0.3062(5) 0.2852(5) -0.0073(4) 0.029(2) Uani 1.00 d . . . C(56) C -0.3127(5) 0.1921(5) 0.0098(4) 0.034(2) Uani 1.00 d . . . C(57) C -0.3251(5) 0.1802(5) 0.0873(4) 0.027(2) Uani 1.00 d . . . C(58) C -0.3331(5) 0.0788(5) 0.1118(5) 0.037(2) Uani 1.00 d . . . C(59) C -0.3867(5) 0.0723(5) 0.1819(5) 0.033(2) Uani 1.00 d . . . C(60) C -0.3366(5) 0.1656(5) 0.2561(4) 0.028(2) Uani 1.00 d . . . C(61) C -0.3348(4) 0.2631(4) 0.2305(4) 0.019(2) Uani 1.00 d . . . C(62) C -0.3259(4) 0.2637(5) 0.1464(4) 0.023(2) Uani 1.00 d . . . C(63) C -0.3366(4) 0.3541(4) 0.2792(4) 0.015(1) Uani 1.00 d . . . C(64) C -0.3398(4) 0.3643(4) 0.3675(4) 0.019(1) Uani 1.00 d . . . C(65) C -0.4230(4) 0.3901(4) 0.3935(4) 0.020(1) Uani 1.00 d . . . C(66) C -0.4291(5) 0.4000(4) 0.4757(4) 0.025(2) Uani 1.00 d . . . C(67) C -0.3499(5) 0.3872(5) 0.5340(4) 0.026(2) Uani 1.00 d . . . C(68) C -0.2670(5) 0.3619(5) 0.5109(4) 0.026(2) Uani 1.00 d . . . C(69) C -0.2625(5) 0.3512(5) 0.4277(4) 0.028(2) Uani 1.00 d . . . C(70) C -0.6524(5) 0.4674(5) 0.1301(4) 0.029(2) Uani 1.00 d . . . C(71) C -0.5366(5) 0.4936(5) 0.1432(4) 0.022(2) Uani 1.00 d . . . C(72) C -0.4893(5) 0.5762(5) 0.1151(4) 0.024(2) Uani 1.00 d . . . C(73) C -0.3841(5) 0.6108(4) 0.1180(4) 0.021(2) Uani 1.00 d . . . C(74) C -0.3543(5) 0.6928(5) 0.0742(4) 0.032(2) Uani 1.00 d . . . H(1) H 0.0490 0.1531 0.1821 0.0264 Uiso 1.00 calc . . . H(2) H -0.1036 0.1167 0.0771 0.0263 Uiso 1.00 calc . . . H(3) H -0.1803 -0.0482 -0.0077 0.0256 Uiso 1.00 calc . . . H(4) H -0.0950 -0.2235 -0.0554 0.0280 Uiso 1.00 calc . . . H(5) H -0.1884 -0.2370 -0.0159 0.0280 Uiso 1.00 calc . . . H(6) H -0.0991 -0.3580 0.0021 0.0334 Uiso 1.00 calc . . . H(7) H -0.1024 -0.2935 0.0875 0.0334 Uiso 1.00 calc . . . H(8) H 0.0701 -0.2581 0.0207 0.0265 Uiso 1.00 calc . . . H(9) H 0.0661 -0.3044 0.0967 0.0265 Uiso 1.00 calc . . . H(10) H 0.3719 -0.0709 0.2062 0.0301 Uiso 1.00 calc . . . H(11) H 0.4848 -0.1668 0.2443 0.0465 Uiso 1.00 calc . . . H(12) H 0.4265 -0.3145 0.2820 0.0497 Uiso 1.00 calc . . . H(13) H 0.2541 -0.3730 0.2811 0.0466 Uiso 1.00 calc . . . H(14) H 0.1369 -0.2835 0.2420 0.0359 Uiso 1.00 calc . . . H(15) H 0.4379 0.1238 0.3079 0.0275 Uiso 1.00 calc . . . H(16) H 0.5655 0.1696 0.4340 0.0282 Uiso 1.00 calc . . . H(17) H 0.5247 0.1197 0.5499 0.0276 Uiso 1.00 calc . . . H(18) H 0.3222 0.0762 0.6005 0.0308 Uiso 1.00 calc . . . H(19) H 0.3905 0.0025 0.5985 0.0308 Uiso 1.00 calc . . . H(20) H 0.2170 -0.0880 0.5816 0.0357 Uiso 1.00 calc . . . H(21) H 0.2521 -0.1264 0.5022 0.0357 Uiso 1.00 calc . . . H(22) H 0.1350 0.0137 0.5137 0.0311 Uiso 1.00 calc . . . H(23) H 0.0899 -0.0984 0.4597 0.0311 Uiso 1.00 calc . . . H(24) H 0.0023 -0.2030 0.2978 0.0324 Uiso 1.00 calc . . . H(25) H -0.1777 -0.2688 0.2655 0.0366 Uiso 1.00 calc . . . H(26) H -0.2834 -0.1626 0.2525 0.0379 Uiso 1.00 calc . . . H(27) H -0.2066 0.0144 0.2780 0.0365 Uiso 1.00 calc . . . H(28) H -0.0270 0.0810 0.3148 0.0265 Uiso 1.00 calc . . . H(29) H 0.3091 0.3721 0.3998 0.0350 Uiso 1.00 calc . . . H(30) H 0.3400 0.4208 0.3302 0.0350 Uiso 1.00 calc . . . H(31) H 0.2244 0.3883 0.3317 0.0350 Uiso 1.00 calc . . . H(32) H 0.3721 0.3215 0.2241 0.0266 Uiso 1.00 calc . . . H(33) H 0.3518 0.2030 0.0604 0.0282 Uiso 1.00 calc . . . H(34) H 0.4558 0.2358 0.1297 0.0282 Uiso 1.00 calc . . . H(35) H 0.4039 0.1216 0.0829 0.0282 Uiso 1.00 calc . . . H(36) H -0.4645 0.5836 0.3056 0.0246 Uiso 1.00 calc . . . H(37) H -0.4401 0.7080 0.4241 0.0289 Uiso 1.00 calc . . . H(38) H -0.2790 0.7780 0.5227 0.0318 Uiso 1.00 calc . . . H(39) H -0.0627 0.7986 0.5055 0.0398 Uiso 1.00 calc . . . H(40) H -0.1024 0.7495 0.5720 0.0398 Uiso 1.00 calc . . . H(41) H 0.0363 0.6958 0.5362 0.0444 Uiso 1.00 calc . . . H(42) H -0.0616 0.6055 0.5226 0.0444 Uiso 1.00 calc . . . H(43) H 0.0032 0.6814 0.3954 0.0323 Uiso 1.00 calc . . . H(44) H 0.0020 0.5746 0.4082 0.0323 Uiso 1.00 calc . . . H(45) H -0.0887 0.5493 0.1564 0.0375 Uiso 1.00 calc . . . H(46) H 0.0460 0.4960 0.1134 0.0451 Uiso 1.00 calc . . . H(47) H 0.1030 0.3695 0.1604 0.0476 Uiso 1.00 calc . . . H(48) H 0.0359 0.3037 0.2617 0.0396 Uiso 1.00 calc . . . H(49) H -0.0888 0.3652 0.3142 0.0369 Uiso 1.00 calc . . . H(50) H -0.3065 0.4306 0.0405 0.0299 Uiso 1.00 calc . . . H(51) H -0.2989 0.2935 -0.0610 0.0341 Uiso 1.00 calc . . . H(52) H -0.3089 0.1365 -0.0312 0.0410 Uiso 1.00 calc . . . H(53) H -0.3719 0.0240 0.0639 0.0437 Uiso 1.00 calc . . . H(54) H -0.2653 0.0731 0.1301 0.0437 Uiso 1.00 calc . . . H(55) H -0.4580 0.0678 0.1611 0.0392 Uiso 1.00 calc . . . H(56) H -0.3819 0.0131 0.1998 0.0392 Uiso 1.00 calc . . . H(57) H -0.3747 0.1615 0.2971 0.0340 Uiso 1.00 calc . . . H(58) H -0.2672 0.1667 0.2797 0.0340 Uiso 1.00 calc . . . H(59) H -0.4763 0.4011 0.3541 0.0240 Uiso 1.00 calc . . . H(60) H -0.4870 0.4159 0.4917 0.0291 Uiso 1.00 calc . . . H(61) H -0.3533 0.3967 0.5905 0.0310 Uiso 1.00 calc . . . H(62) H -0.2139 0.3513 0.5514 0.0318 Uiso 1.00 calc . . . H(63) H -0.2046 0.3345 0.4118 0.0338 Uiso 1.00 calc . . . H(64) H -0.6695 0.4607 0.1816 0.0346 Uiso 1.00 calc . . . H(65) H -0.6858 0.4037 0.0886 0.0346 Uiso 1.00 calc . . . H(66) H -0.6782 0.5187 0.1124 0.0346 Uiso 1.00 calc . . . H(67) H -0.5336 0.6122 0.0921 0.0286 Uiso 1.00 calc . . . H(68) H -0.3782 0.6642 0.0142 0.0388 Uiso 1.00 calc . . . H(69) H -0.3880 0.7444 0.0881 0.0388 Uiso 1.00 calc . . . H(70) H -0.2821 0.7228 0.0895 0.0388 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) 0.0149(1) 0.0155(1) 0.0121(1) 0.00330(9) -0.00005(9) 0.00290(9) Ir(2) 0.0150(1) 0.0162(1) 0.0136(1) 0.00528(9) 0.00081(10) 0.00316(9) O(1) 0.021(2) 0.017(2) 0.022(2) 0.006(2) 0.000(2) 0.005(2) O(2) 0.021(2) 0.020(2) 0.013(2) 0.003(2) 0.003(2) 0.005(2) O(3) 0.016(2) 0.021(2) 0.022(2) 0.004(2) -0.001(2) 0.007(2) O(4) 0.021(2) 0.014(2) 0.018(2) 0.002(2) 0.000(2) 0.003(2) N(1) 0.014(2) 0.023(3) 0.010(2) -0.002(2) 0.000(2) 0.004(2) N(2) 0.017(2) 0.011(2) 0.016(3) 0.004(2) -0.003(2) -0.001(2) N(3) 0.018(2) 0.021(3) 0.015(3) 0.004(2) 0.001(2) 0.007(2) N(4) 0.012(2) 0.025(3) 0.018(3) 0.007(2) -0.002(2) 0.001(2) C(1) 0.027(3) 0.021(3) 0.018(3) 0.008(2) 0.004(3) 0.006(3) C(2) 0.022(3) 0.025(3) 0.023(3) 0.013(2) 0.008(3) 0.009(3) C(3) 0.016(3) 0.028(3) 0.021(3) 0.005(2) 0.002(3) 0.009(3) C(4) 0.020(3) 0.020(3) 0.014(3) 0.002(2) -0.001(3) 0.004(2) C(5) 0.016(3) 0.022(3) 0.021(3) 0.000(2) -0.004(3) 0.001(3) C(6) 0.027(3) 0.031(4) 0.016(3) -0.002(3) 0.002(3) 0.004(3) C(7) 0.024(3) 0.017(3) 0.018(3) 0.001(2) 0.001(3) 0.000(2) C(8) 0.018(3) 0.018(3) 0.017(3) 0.004(2) 0.004(3) 0.002(2) C(9) 0.018(3) 0.016(3) 0.019(3) 0.005(2) 0.007(3) 0.004(2) C(10) 0.023(3) 0.014(3) 0.012(3) 0.003(2) 0.003(3) 0.006(2) C(11) 0.032(3) 0.025(3) 0.014(3) 0.012(3) 0.000(3) 0.003(3) C(12) 0.026(3) 0.029(3) 0.017(3) 0.011(3) 0.001(3) -0.002(3) C(13) 0.034(4) 0.049(5) 0.025(4) 0.019(3) -0.006(3) -0.005(3) C(14) 0.055(5) 0.037(4) 0.030(4) 0.031(4) -0.012(4) 0.006(3) C(15) 0.056(5) 0.030(4) 0.028(4) 0.018(3) -0.002(4) 0.007(3) C(16) 0.037(4) 0.023(3) 0.025(4) 0.011(3) -0.003(3) 0.004(3) C(17) 0.014(3) 0.032(3) 0.020(3) 0.011(2) 0.000(3) 0.002(3) C(18) 0.019(3) 0.024(3) 0.023(4) 0.003(2) 0.000(3) 0.005(3) C(19) 0.020(3) 0.025(3) 0.019(3) 0.013(2) -0.005(3) -0.003(3) C(20) 0.022(3) 0.023(3) 0.020(3) 0.013(2) -0.002(3) 0.001(3) C(21) 0.033(3) 0.029(3) 0.017(3) 0.016(3) 0.003(3) 0.007(3) C(22) 0.039(4) 0.035(4) 0.017(3) 0.009(3) 0.007(3) 0.012(3) C(23) 0.028(3) 0.031(4) 0.016(3) 0.004(3) 0.002(3) 0.009(3) C(24) 0.020(3) 0.024(3) 0.016(3) 0.008(2) 0.003(3) 0.005(2) C(25) 0.023(3) 0.020(3) 0.016(3) 0.011(2) 0.007(3) 0.002(2) C(26) 0.024(3) 0.015(3) 0.016(3) 0.000(2) -0.002(3) -0.001(2) C(27) 0.027(3) 0.023(3) 0.009(3) 0.005(2) 0.000(3) 0.002(2) C(28) 0.026(3) 0.035(4) 0.025(4) 0.011(3) 0.006(3) 0.015(3) C(29) 0.033(4) 0.028(4) 0.023(4) -0.006(3) 0.009(3) 0.004(3) C(30) 0.020(3) 0.037(4) 0.033(4) 0.008(3) 0.004(3) 0.001(3) C(31) 0.028(3) 0.045(4) 0.023(4) 0.018(3) 0.010(3) 0.006(3) C(32) 0.022(3) 0.025(3) 0.016(3) -0.001(2) 0.007(3) 0.004(3) C(33) 0.032(3) 0.016(3) 0.029(4) 0.006(3) 0.002(3) 0.000(3) C(34) 0.023(3) 0.018(3) 0.016(3) 0.003(2) -0.007(3) 0.004(2) C(35) 0.019(3) 0.018(3) 0.018(3) -0.006(2) -0.005(3) 0.003(2) C(36) 0.017(3) 0.020(3) 0.017(3) 0.003(2) -0.004(2) 0.008(2) C(37) 0.017(3) 0.021(3) 0.029(4) 0.004(2) 0.001(3) 0.009(3) C(38) 0.020(3) 0.021(3) 0.022(3) 0.009(2) 0.001(3) 0.007(3) C(39) 0.022(3) 0.024(3) 0.027(4) 0.009(2) 0.007(3) 0.006(3) C(40) 0.034(3) 0.030(3) 0.017(3) 0.010(3) 0.010(3) 0.007(3) C(41) 0.021(3) 0.029(3) 0.018(3) 0.003(2) 0.001(3) 0.009(3) C(42) 0.026(3) 0.036(4) 0.027(4) 0.004(3) 0.000(3) -0.001(3) C(43) 0.022(3) 0.057(5) 0.021(4) 0.008(3) -0.004(3) 0.002(3) C(44) 0.017(3) 0.034(4) 0.026(4) 0.011(3) 0.000(3) -0.001(3) C(45) 0.021(3) 0.024(3) 0.017(3) 0.003(2) 0.000(3) 0.006(3) C(46) 0.014(3) 0.022(3) 0.018(3) 0.005(2) -0.001(2) 0.004(2) C(47) 0.015(3) 0.018(3) 0.022(3) 0.005(2) 0.001(3) 0.003(2) C(48) 0.018(3) 0.008(3) 0.030(4) 0.003(2) 0.001(3) -0.006(2) C(49) 0.035(4) 0.029(4) 0.035(4) 0.008(3) 0.017(3) 0.013(3) C(50) 0.042(4) 0.036(4) 0.044(5) 0.015(3) 0.028(4) 0.012(3) C(51) 0.038(4) 0.040(4) 0.038(5) 0.014(3) 0.010(4) 0.001(4) C(52) 0.025(3) 0.036(4) 0.036(4) 0.020(3) 0.002(3) -0.002(3) C(53) 0.033(4) 0.046(4) 0.026(4) 0.020(3) 0.015(3) 0.014(3) C(54) 0.031(3) 0.026(3) 0.020(3) 0.008(3) 0.005(3) 0.009(3) C(55) 0.036(4) 0.029(4) 0.018(3) 0.013(3) 0.002(3) 0.002(3) C(56) 0.039(4) 0.035(4) 0.021(4) 0.011(3) 0.003(3) -0.004(3) C(57) 0.021(3) 0.028(3) 0.025(4) 0.006(3) 0.000(3) -0.006(3) C(58) 0.045(4) 0.026(4) 0.043(5) 0.018(3) 0.018(4) 0.003(3) C(59) 0.039(4) 0.021(3) 0.042(5) 0.015(3) 0.007(4) 0.010(3) C(60) 0.034(4) 0.022(3) 0.031(4) 0.011(3) 0.012(3) 0.007(3) C(61) 0.014(3) 0.017(3) 0.029(4) 0.009(2) 0.003(3) 0.006(3) C(62) 0.020(3) 0.027(3) 0.020(3) 0.005(2) 0.004(3) 0.006(3) C(63) 0.013(3) 0.016(3) 0.018(3) 0.007(2) 0.003(2) 0.006(2) C(64) 0.020(3) 0.012(3) 0.023(3) 0.002(2) 0.001(3) 0.005(2) C(65) 0.016(3) 0.018(3) 0.023(3) 0.006(2) 0.001(3) 0.002(2) C(66) 0.030(3) 0.021(3) 0.030(4) 0.013(3) 0.013(3) 0.011(3) C(67) 0.033(3) 0.024(3) 0.019(3) 0.007(3) 0.007(3) 0.005(3) C(68) 0.023(3) 0.035(4) 0.019(3) 0.007(3) 0.001(3) 0.010(3) C(69) 0.025(3) 0.034(4) 0.021(4) 0.007(3) 0.002(3) 0.006(3) C(70) 0.023(3) 0.029(4) 0.031(4) 0.002(3) 0.000(3) 0.010(3) C(71) 0.022(3) 0.030(3) 0.013(3) 0.007(3) 0.000(3) 0.006(3) C(72) 0.023(3) 0.027(3) 0.020(3) 0.007(3) -0.002(3) 0.009(3) C(73) 0.029(3) 0.016(3) 0.010(3) 0.002(2) 0.001(3) -0.001(2) C(74) 0.039(4) 0.026(4) 0.025(4) 0.003(3) 0.000(3) 0.011(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; For all methyl groups of the complex, even if it is the lowest, one of H atoms was localized in the Fourier maps, respectively, and H atoms of the rest were placed in geometrically calculated positions. ; 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) O(1) 2.146(4) . . yes Ir(1) O(2) 2.145(4) . . yes Ir(1) N(1) 2.025(5) . . yes Ir(1) N(2) 2.045(5) . . yes Ir(1) C(10) 1.976(5) . . yes Ir(1) C(26) 2.004(6) . . yes Ir(2) O(3) 2.167(5) . . yes Ir(2) O(4) 2.144(4) . . yes Ir(2) N(3) 2.034(4) . . yes Ir(2) N(4) 2.045(4) . . yes Ir(2) C(47) 2.000(6) . . yes Ir(2) C(63) 1.998(6) . . yes O(1) C(34) 1.279(7) . . yes O(2) C(36) 1.269(6) . . yes O(3) C(71) 1.269(7) . . yes O(4) C(73) 1.264(7) . . yes N(1) C(1) 1.329(8) . . yes N(1) C(9) 1.370(7) . . yes N(2) C(17) 1.353(7) . . yes N(2) C(25) 1.357(7) . . yes N(3) C(38) 1.355(7) . . yes N(3) C(46) 1.350(7) . . yes N(4) C(54) 1.333(8) . . yes N(4) C(62) 1.376(8) . . yes C(1) C(2) 1.378(9) . . yes C(1) H(1) 0.952 . . no C(2) C(3) 1.366(8) . . yes C(2) H(2) 0.952 . . no C(3) C(4) 1.387(8) . . yes C(3) H(3) 0.951 . . no C(4) C(5) 1.508(8) . . yes C(4) C(9) 1.417(8) . . yes C(5) C(6) 1.518(9) . . yes C(5) H(4) 0.949 . . no C(5) H(5) 0.947 . . no C(6) C(7) 1.535(8) . . yes C(6) H(6) 0.951 . . no C(6) H(7) 0.947 . . no C(7) C(8) 1.521(7) . . yes C(7) H(8) 0.950 . . no C(7) H(9) 0.950 . . no C(8) C(9) 1.432(8) . . yes C(8) C(10) 1.350(8) . . yes C(10) C(11) 1.507(8) . . yes C(11) C(12) 1.401(8) . . yes C(11) C(16) 1.400(9) . . yes C(12) C(13) 1.409(10) . . yes C(12) H(10) 0.952 . . no C(13) C(14) 1.35(1) . . yes C(13) H(11) 0.952 . . no C(14) C(15) 1.36(1) . . yes C(14) H(12) 0.951 . . no C(15) C(16) 1.394(10) . . yes C(15) H(13) 0.954 . . no C(16) H(14) 0.951 . . no C(17) C(18) 1.381(9) . . yes C(17) H(15) 0.947 . . no C(18) C(19) 1.372(9) . . yes C(18) H(16) 0.951 . . no C(19) C(20) 1.412(8) . . yes C(19) H(17) 0.948 . . no C(20) C(21) 1.487(9) . . yes C(20) C(25) 1.388(9) . . yes C(21) C(22) 1.532(9) . . yes C(21) H(18) 0.947 . . no C(21) H(19) 0.949 . . no C(22) C(23) 1.538(10) . . yes C(22) H(20) 0.950 . . no C(22) H(21) 0.955 . . no C(23) C(24) 1.510(8) . . yes C(23) H(22) 0.951 . . no C(23) H(23) 0.950 . . no C(24) C(25) 1.460(8) . . yes C(24) C(26) 1.342(9) . . yes C(26) C(27) 1.476(8) . . yes C(27) C(28) 1.390(8) . . yes C(27) C(32) 1.411(9) . . yes C(28) C(29) 1.397(9) . . yes C(28) H(24) 0.948 . . no C(29) C(30) 1.371(10) . . yes C(29) H(25) 0.954 . . no C(30) C(31) 1.401(9) . . yes C(30) H(26) 0.949 . . no C(31) C(32) 1.384(8) . . yes C(31) H(27) 0.953 . . no C(32) H(28) 0.949 . . no C(33) C(34) 1.519(8) . . yes C(33) H(29) 0.975 . . no C(33) H(30) 0.931 . . no C(33) H(31) 0.945 . . no C(34) C(35) 1.382(8) . . yes C(35) C(36) 1.395(8) . . yes C(35) H(32) 0.947 . . no C(36) C(37) 1.505(8) . . yes C(37) H(33) 0.965 . . no C(37) H(34) 0.942 . . no C(37) H(35) 0.956 . . no C(38) C(39) 1.350(8) . . yes C(38) H(36) 0.951 . . no C(39) C(40) 1.381(9) . . yes C(39) H(37) 0.946 . . no C(40) C(41) 1.401(8) . . yes C(40) H(38) 0.951 . . no C(41) C(42) 1.507(9) . . yes C(41) C(46) 1.382(8) . . yes C(42) C(43) 1.512(10) . . yes C(42) H(39) 0.950 . . no C(42) H(40) 0.949 . . no C(43) C(44) 1.516(9) . . yes C(43) H(41) 0.952 . . no C(43) H(42) 0.947 . . no C(44) C(45) 1.502(9) . . yes C(44) H(43) 0.954 . . no C(44) H(44) 0.948 . . no C(45) C(46) 1.451(8) . . yes C(45) C(47) 1.350(8) . . yes C(47) C(48) 1.490(7) . . yes C(48) C(49) 1.391(9) . . yes C(48) C(53) 1.400(9) . . yes C(49) C(50) 1.394(9) . . yes C(49) H(45) 0.953 . . no C(50) C(51) 1.37(1) . . yes C(50) H(46) 0.953 . . no C(51) C(52) 1.38(1) . . yes C(51) H(47) 0.955 . . no C(52) C(53) 1.392(8) . . yes C(52) H(48) 0.956 . . no C(53) H(49) 0.955 . . no C(54) C(55) 1.385(8) . . yes C(54) H(50) 0.951 . . no C(55) C(56) 1.378(10) . . yes C(55) H(51) 0.956 . . no C(56) C(57) 1.387(10) . . yes C(56) H(52) 0.949 . . no C(57) C(58) 1.542(10) . . yes C(57) C(62) 1.379(8) . . yes C(58) C(59) 1.520(9) . . yes C(58) H(53) 0.951 . . no C(58) H(54) 0.948 . . no C(59) C(60) 1.517(9) . . yes C(59) H(55) 0.952 . . no C(59) H(56) 0.950 . . no C(60) C(61) 1.508(8) . . yes C(60) H(57) 0.951 . . no C(60) H(58) 0.950 . . no C(61) C(62) 1.448(8) . . yes C(61) C(63) 1.377(7) . . yes C(63) C(64) 1.475(8) . . yes C(64) C(65) 1.402(8) . . yes C(64) C(69) 1.385(9) . . yes C(65) C(66) 1.384(9) . . yes C(65) H(59) 0.947 . . no C(66) C(67) 1.382(9) . . yes C(66) H(60) 0.949 . . no C(67) C(68) 1.374(8) . . yes C(67) H(61) 0.946 . . no C(68) C(69) 1.395(9) . . yes C(68) H(62) 0.953 . . no C(69) H(63) 0.952 . . no C(70) C(71) 1.503(8) . . yes C(70) H(64) 0.961 . . no C(70) H(65) 0.957 . . no C(70) H(66) 0.946 . . no C(71) C(72) 1.404(8) . . yes C(72) C(73) 1.397(8) . . yes C(72) H(67) 0.951 . . no C(73) C(74) 1.507(9) . . yes C(74) H(68) 0.963 . . no C(74) H(69) 0.963 . . no C(74) H(70) 0.938 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ir(1) O(2) 89.1(1) . . . yes O(1) Ir(1) N(1) 94.7(2) . . . yes O(1) Ir(1) N(2) 84.0(2) . . . yes O(1) Ir(1) C(10) 174.0(2) . . . yes O(1) Ir(1) C(26) 94.2(2) . . . yes O(2) Ir(1) N(1) 88.8(2) . . . yes O(2) Ir(1) N(2) 95.7(2) . . . yes O(2) Ir(1) C(10) 90.2(2) . . . yes O(2) Ir(1) C(26) 173.8(2) . . . yes N(1) Ir(1) N(2) 175.3(2) . . . yes N(1) Ir(1) C(10) 79.3(2) . . . yes N(1) Ir(1) C(26) 96.1(2) . . . yes N(2) Ir(1) C(10) 102.0(2) . . . yes N(2) Ir(1) C(26) 79.5(2) . . . yes C(10) Ir(1) C(26) 87.1(2) . . . yes O(3) Ir(2) O(4) 86.5(1) . . . yes O(3) Ir(2) N(3) 92.8(2) . . . yes O(3) Ir(2) N(4) 92.1(2) . . . yes O(3) Ir(2) C(47) 171.9(2) . . . yes O(3) Ir(2) C(63) 94.2(2) . . . yes O(4) Ir(2) N(3) 89.7(2) . . . yes O(4) Ir(2) N(4) 93.5(2) . . . yes O(4) Ir(2) C(47) 94.0(2) . . . yes O(4) Ir(2) C(63) 173.9(2) . . . yes N(3) Ir(2) N(4) 174.3(2) . . . yes N(3) Ir(2) C(47) 79.2(2) . . . yes N(3) Ir(2) C(63) 96.3(2) . . . yes N(4) Ir(2) C(47) 95.9(2) . . . yes N(4) Ir(2) C(63) 80.4(2) . . . yes C(47) Ir(2) C(63) 86.2(2) . . . yes Ir(1) O(1) C(34) 122.4(4) . . . yes Ir(1) O(2) C(36) 124.9(3) . . . yes Ir(2) O(3) C(71) 124.9(4) . . . yes Ir(2) O(4) C(73) 126.6(4) . . . yes Ir(1) N(1) C(1) 125.3(4) . . . yes Ir(1) N(1) C(9) 114.4(4) . . . yes C(1) N(1) C(9) 120.3(5) . . . yes Ir(1) N(2) C(17) 125.4(4) . . . yes Ir(1) N(2) C(25) 114.9(4) . . . yes C(17) N(2) C(25) 119.3(5) . . . yes Ir(2) N(3) C(38) 125.7(4) . . . yes Ir(2) N(3) C(46) 115.5(4) . . . yes C(38) N(3) C(46) 118.8(5) . . . yes Ir(2) N(4) C(54) 125.4(4) . . . yes Ir(2) N(4) C(62) 114.4(4) . . . yes C(54) N(4) C(62) 120.2(5) . . . yes N(1) C(1) C(2) 122.2(5) . . . yes N(1) C(1) H(1) 118.7 . . . no C(2) C(1) H(1) 119.0 . . . no C(1) C(2) C(3) 119.5(6) . . . yes C(1) C(2) H(2) 120.4 . . . no C(3) C(2) H(2) 120.1 . . . no C(2) C(3) C(4) 119.7(6) . . . yes C(2) C(3) H(3) 119.9 . . . no C(4) C(3) H(3) 120.3 . . . no C(3) C(4) C(5) 124.1(6) . . . yes C(3) C(4) C(9) 119.1(5) . . . yes C(5) C(4) C(9) 116.8(5) . . . yes C(4) C(5) C(6) 113.0(5) . . . yes C(4) C(5) H(4) 108.4 . . . no C(4) C(5) H(5) 108.5 . . . no C(6) C(5) H(4) 108.7 . . . no C(6) C(5) H(5) 108.5 . . . no H(4) C(5) H(5) 109.7 . . . no C(5) C(6) C(7) 110.5(5) . . . yes C(5) C(6) H(6) 109.2 . . . no C(5) C(6) H(7) 109.6 . . . no C(7) C(6) H(6) 108.8 . . . no C(7) C(6) H(7) 109.1 . . . no H(6) C(6) H(7) 109.6 . . . no C(6) C(7) C(8) 110.0(5) . . . yes C(6) C(7) H(8) 109.3 . . . no C(6) C(7) H(9) 109.3 . . . no C(8) C(7) H(8) 109.4 . . . no C(8) C(7) H(9) 109.4 . . . no H(8) C(7) H(9) 109.4 . . . no C(7) C(8) C(9) 115.7(5) . . . yes C(7) C(8) C(10) 130.4(6) . . . yes C(9) C(8) C(10) 113.8(5) . . . yes N(1) C(9) C(4) 119.1(5) . . . yes N(1) C(9) C(8) 114.9(5) . . . yes C(4) C(9) C(8) 126.0(5) . . . yes Ir(1) C(10) C(8) 117.5(4) . . . yes Ir(1) C(10) C(11) 121.9(4) . . . yes C(8) C(10) C(11) 120.6(5) . . . yes C(10) C(11) C(12) 119.5(6) . . . yes C(10) C(11) C(16) 121.9(6) . . . yes C(12) C(11) C(16) 118.6(6) . . . yes C(11) C(12) C(13) 118.9(6) . . . yes C(11) C(12) H(10) 120.6 . . . no C(13) C(12) H(10) 120.5 . . . no C(12) C(13) C(14) 121.6(7) . . . yes C(12) C(13) H(11) 119.1 . . . no C(14) C(13) H(11) 119.3 . . . no C(13) C(14) C(15) 119.8(7) . . . yes C(13) C(14) H(12) 120.2 . . . no C(15) C(14) H(12) 120.0 . . . no C(14) C(15) C(16) 121.1(7) . . . yes C(14) C(15) H(13) 119.7 . . . no C(16) C(15) H(13) 119.2 . . . no C(11) C(16) C(15) 119.9(6) . . . yes C(11) C(16) H(14) 120.1 . . . no C(15) C(16) H(14) 120.0 . . . no N(2) C(17) C(18) 121.1(6) . . . yes N(2) C(17) H(15) 119.4 . . . no C(18) C(17) H(15) 119.5 . . . no C(17) C(18) C(19) 119.9(5) . . . yes C(17) C(18) H(16) 119.9 . . . no C(19) C(18) H(16) 120.2 . . . no C(18) C(19) C(20) 119.9(6) . . . yes C(18) C(19) H(17) 120.4 . . . no C(20) C(19) H(17) 119.7 . . . no C(19) C(20) C(21) 123.1(6) . . . yes C(19) C(20) C(25) 117.1(6) . . . yes C(21) C(20) C(25) 119.8(5) . . . yes C(20) C(21) C(22) 110.4(5) . . . yes C(20) C(21) H(18) 109.2 . . . no C(20) C(21) H(19) 109.2 . . . no C(22) C(21) H(18) 109.0 . . . no C(22) C(21) H(19) 109.3 . . . no H(18) C(21) H(19) 109.8 . . . no C(21) C(22) C(23) 109.6(5) . . . yes C(21) C(22) H(20) 109.4 . . . no C(21) C(22) H(21) 109.3 . . . no C(23) C(22) H(20) 109.9 . . . no C(23) C(22) H(21) 109.6 . . . no H(20) C(22) H(21) 109.0 . . . no C(22) C(23) C(24) 110.3(5) . . . yes C(22) C(23) H(22) 109.2 . . . no C(22) C(23) H(23) 109.5 . . . no C(24) C(23) H(22) 109.2 . . . no C(24) C(23) H(23) 109.3 . . . no H(22) C(23) H(23) 109.4 . . . no C(23) C(24) C(25) 117.1(5) . . . yes C(23) C(24) C(26) 127.6(5) . . . yes C(25) C(24) C(26) 115.3(5) . . . yes N(2) C(25) C(20) 122.6(5) . . . yes N(2) C(25) C(24) 114.1(5) . . . yes C(20) C(25) C(24) 123.1(5) . . . yes Ir(1) C(26) C(24) 116.2(4) . . . yes Ir(1) C(26) C(27) 122.3(5) . . . yes C(24) C(26) C(27) 121.5(5) . . . yes C(26) C(27) C(28) 121.5(5) . . . yes C(26) C(27) C(32) 121.1(5) . . . yes C(28) C(27) C(32) 117.4(5) . . . yes C(27) C(28) C(29) 121.3(6) . . . yes C(27) C(28) H(24) 119.5 . . . no C(29) C(28) H(24) 119.2 . . . no C(28) C(29) C(30) 120.9(6) . . . yes C(28) C(29) H(25) 119.4 . . . no C(30) C(29) H(25) 119.8 . . . no C(29) C(30) C(31) 119.0(6) . . . yes C(29) C(30) H(26) 120.3 . . . no C(31) C(30) H(26) 120.7 . . . no C(30) C(31) C(32) 120.3(6) . . . yes C(30) C(31) H(27) 120.0 . . . no C(32) C(31) H(27) 119.6 . . . no C(27) C(32) C(31) 121.2(6) . . . yes C(27) C(32) H(28) 119.6 . . . no C(31) C(32) H(28) 119.3 . . . no C(34) C(33) H(29) 108.0 . . . no C(34) C(33) H(30) 110.6 . . . no C(34) C(33) H(31) 109.9 . . . no H(29) C(33) H(30) 108.9 . . . no H(29) C(33) H(31) 107.8 . . . no H(30) C(33) H(31) 111.5 . . . no O(1) C(34) C(33) 114.7(5) . . . yes O(1) C(34) C(35) 127.8(5) . . . yes C(33) C(34) C(35) 117.5(5) . . . yes C(34) C(35) C(36) 129.3(5) . . . yes C(34) C(35) H(32) 115.5 . . . no C(36) C(35) H(32) 115.2 . . . no O(2) C(36) C(35) 125.5(5) . . . yes O(2) C(36) C(37) 115.3(5) . . . yes C(35) C(36) C(37) 119.3(5) . . . yes C(36) C(37) H(33) 109.5 . . . no C(36) C(37) H(34) 111.0 . . . no C(36) C(37) H(35) 110.1 . . . no H(33) C(37) H(34) 108.9 . . . no H(33) C(37) H(35) 107.7 . . . no H(34) C(37) H(35) 109.6 . . . no N(3) C(38) C(39) 120.8(6) . . . yes N(3) C(38) H(36) 119.8 . . . no C(39) C(38) H(36) 119.4 . . . no C(38) C(39) C(40) 121.7(5) . . . yes C(38) C(39) H(37) 118.9 . . . no C(40) C(39) H(37) 119.4 . . . no C(39) C(40) C(41) 118.0(5) . . . yes C(39) C(40) H(38) 120.5 . . . no C(41) C(40) H(38) 121.4 . . . no C(40) C(41) C(42) 121.2(6) . . . yes C(40) C(41) C(46) 117.9(6) . . . yes C(42) C(41) C(46) 120.9(5) . . . yes C(41) C(42) C(43) 110.3(5) . . . yes C(41) C(42) H(39) 109.2 . . . no C(41) C(42) H(40) 109.3 . . . no C(43) C(42) H(39) 109.2 . . . no C(43) C(42) H(40) 109.2 . . . no H(39) C(42) H(40) 109.5 . . . no C(42) C(43) C(44) 113.1(6) . . . yes C(42) C(43) H(41) 108.3 . . . no C(42) C(43) H(42) 108.6 . . . no C(44) C(43) H(41) 108.6 . . . no C(44) C(43) H(42) 108.7 . . . no H(41) C(43) H(42) 109.5 . . . no C(43) C(44) C(45) 111.9(5) . . . yes C(43) C(44) H(43) 108.9 . . . no C(43) C(44) H(44) 109.1 . . . no C(45) C(44) H(43) 108.8 . . . no C(45) C(44) H(44) 108.9 . . . no H(43) C(44) H(44) 109.2 . . . no C(44) C(45) C(46) 117.2(5) . . . yes C(44) C(45) C(47) 127.9(5) . . . yes C(46) C(45) C(47) 114.9(5) . . . yes N(3) C(46) C(41) 122.7(5) . . . yes N(3) C(46) C(45) 114.1(5) . . . yes C(41) C(46) C(45) 123.2(5) . . . yes Ir(2) C(47) C(45) 116.3(4) . . . yes Ir(2) C(47) C(48) 124.1(4) . . . yes C(45) C(47) C(48) 119.6(5) . . . yes C(47) C(48) C(49) 120.9(6) . . . yes C(47) C(48) C(53) 120.7(6) . . . yes C(49) C(48) C(53) 118.4(5) . . . yes C(48) C(49) C(50) 119.5(7) . . . yes C(48) C(49) H(45) 120.4 . . . no C(50) C(49) H(45) 120.0 . . . no C(49) C(50) C(51) 121.6(7) . . . yes C(49) C(50) H(46) 119.5 . . . no C(51) C(50) H(46) 118.9 . . . no C(50) C(51) C(52) 119.3(6) . . . yes C(50) C(51) H(47) 120.4 . . . no C(52) C(51) H(47) 120.3 . . . no C(51) C(52) C(53) 120.1(7) . . . yes C(51) C(52) H(48) 120.1 . . . no C(53) C(52) H(48) 119.8 . . . no C(48) C(53) C(52) 120.8(6) . . . yes C(48) C(53) H(49) 119.7 . . . no C(52) C(53) H(49) 119.5 . . . no N(4) C(54) C(55) 120.4(6) . . . yes N(4) C(54) H(50) 119.7 . . . no C(55) C(54) H(50) 119.9 . . . no C(54) C(55) C(56) 120.2(6) . . . yes C(54) C(55) H(51) 120.0 . . . no C(56) C(55) H(51) 119.8 . . . no C(55) C(56) C(57) 119.5(6) . . . yes C(55) C(56) H(52) 120.1 . . . no C(57) C(56) H(52) 120.4 . . . no C(56) C(57) C(58) 123.0(5) . . . yes C(56) C(57) C(62) 118.7(6) . . . yes C(58) C(57) C(62) 118.3(6) . . . yes C(57) C(58) C(59) 112.1(5) . . . yes C(57) C(58) H(53) 108.9 . . . no C(57) C(58) H(54) 109.0 . . . no C(59) C(58) H(53) 108.6 . . . no C(59) C(58) H(54) 108.7 . . . no H(53) C(58) H(54) 109.6 . . . no C(58) C(59) C(60) 111.0(5) . . . yes C(58) C(59) H(55) 109.1 . . . no C(58) C(59) H(56) 109.1 . . . no C(60) C(59) H(55) 109.1 . . . no C(60) C(59) H(56) 109.2 . . . no H(55) C(59) H(56) 109.3 . . . no C(59) C(60) C(61) 111.9(6) . . . yes C(59) C(60) H(57) 108.9 . . . no C(59) C(60) H(58) 108.9 . . . no C(61) C(60) H(57) 108.8 . . . no C(61) C(60) H(58) 108.9 . . . no H(57) C(60) H(58) 109.4 . . . no C(60) C(61) C(62) 117.1(5) . . . yes C(60) C(61) C(63) 127.5(6) . . . yes C(62) C(61) C(63) 115.4(5) . . . yes N(4) C(62) C(57) 120.9(6) . . . yes N(4) C(62) C(61) 114.5(5) . . . yes C(57) C(62) C(61) 124.5(6) . . . yes Ir(2) C(63) C(61) 115.4(4) . . . yes Ir(2) C(63) C(64) 124.2(4) . . . yes C(61) C(63) C(64) 120.3(5) . . . yes C(63) C(64) C(65) 119.7(6) . . . yes C(63) C(64) C(69) 122.9(5) . . . yes C(65) C(64) C(69) 117.4(6) . . . yes C(64) C(65) C(66) 121.5(6) . . . yes C(64) C(65) H(59) 119.3 . . . no C(66) C(65) H(59) 119.2 . . . no C(65) C(66) C(67) 119.4(5) . . . yes C(65) C(66) H(60) 120.1 . . . no C(67) C(66) H(60) 120.5 . . . no C(66) C(67) C(68) 120.8(6) . . . yes C(66) C(67) H(61) 118.9 . . . no C(68) C(67) H(61) 120.3 . . . no C(67) C(68) C(69) 119.2(6) . . . yes C(67) C(68) H(62) 120.0 . . . no C(69) C(68) H(62) 120.8 . . . no C(64) C(69) C(68) 121.7(6) . . . yes C(64) C(69) H(63) 119.0 . . . no C(68) C(69) H(63) 119.2 . . . no C(71) C(70) H(64) 109.9 . . . no C(71) C(70) H(65) 110.1 . . . no C(71) C(70) H(66) 110.8 . . . no H(64) C(70) H(65) 107.9 . . . no H(64) C(70) H(66) 108.8 . . . no H(65) C(70) H(66) 109.2 . . . no O(3) C(71) C(70) 115.7(5) . . . yes O(3) C(71) C(72) 127.0(6) . . . yes C(70) C(71) C(72) 117.2(6) . . . yes C(71) C(72) C(73) 126.6(6) . . . yes C(71) C(72) H(67) 116.4 . . . no C(73) C(72) H(67) 117.0 . . . no O(4) C(73) C(72) 126.6(6) . . . yes O(4) C(73) C(74) 116.8(5) . . . yes C(72) C(73) C(74) 116.7(6) . . . yes C(73) C(74) H(68) 109.7 . . . no C(73) C(74) H(69) 109.6 . . . no C(73) C(74) H(70) 111.4 . . . no H(68) C(74) H(69) 107.3 . . . no H(68) C(74) H(70) 109.4 . . . no H(69) C(74) H(70) 109.3 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) O(1) C(34) C(33) -170.2(4) . . . . yes Ir(1) O(1) C(34) C(35) 9.2(9) . . . . yes Ir(1) O(2) C(36) C(35) -1.0(9) . . . . yes Ir(1) O(2) C(36) C(37) 179.3(4) . . . . yes Ir(1) N(1) C(1) C(2) -177.6(4) . . . . yes Ir(1) N(1) C(9) C(4) 175.5(4) . . . . yes Ir(1) N(1) C(9) C(8) -3.4(6) . . . . yes Ir(1) N(2) C(17) C(18) 169.8(4) . . . . yes Ir(1) N(2) C(25) C(20) -173.3(4) . . . . yes Ir(1) N(2) C(25) C(24) 2.0(6) . . . . yes Ir(1) C(10) C(8) C(7) 176.7(5) . . . . yes Ir(1) C(10) C(8) C(9) 0.6(7) . . . . yes Ir(1) C(10) C(11) C(12) -55.3(7) . . . . yes Ir(1) C(10) C(11) C(16) 123.2(6) . . . . yes Ir(1) C(26) C(24) C(23) 179.7(5) . . . . yes Ir(1) C(26) C(24) C(25) 3.3(7) . . . . yes Ir(1) C(26) C(27) C(28) 104.8(6) . . . . yes Ir(1) C(26) C(27) C(32) -71.7(6) . . . . yes Ir(2) O(3) C(71) C(70) -169.6(4) . . . . yes Ir(2) O(3) C(71) C(72) 11.3(9) . . . . yes Ir(2) O(4) C(73) C(72) -2.1(8) . . . . yes Ir(2) O(4) C(73) C(74) 178.2(4) . . . . yes Ir(2) N(3) C(38) C(39) -180.0(5) . . . . yes Ir(2) N(3) C(46) C(41) -177.9(5) . . . . yes Ir(2) N(3) C(46) C(45) 2.0(7) . . . . yes Ir(2) N(4) C(54) C(55) 178.0(4) . . . . yes Ir(2) N(4) C(62) C(57) 179.4(4) . . . . yes Ir(2) N(4) C(62) C(61) 1.5(6) . . . . yes Ir(2) C(47) C(45) C(44) 178.2(5) . . . . yes Ir(2) C(47) C(45) C(46) -2.5(8) . . . . yes Ir(2) C(47) C(48) C(49) 77.3(7) . . . . yes Ir(2) C(47) C(48) C(53) -99.6(7) . . . . yes Ir(2) C(63) C(61) C(60) 176.8(4) . . . . yes Ir(2) C(63) C(61) C(62) -0.4(6) . . . . yes Ir(2) C(63) C(64) C(65) 63.6(6) . . . . yes Ir(2) C(63) C(64) C(69) -115.2(6) . . . . yes O(1) Ir(1) O(2) C(36) 6.5(5) . . . . yes O(1) Ir(1) N(1) C(1) 0.4(5) . . . . yes O(1) Ir(1) N(1) C(9) -177.7(4) . . . . yes O(1) Ir(1) N(2) C(17) -77.1(4) . . . . yes O(1) Ir(1) N(2) C(25) 95.2(4) . . . . yes O(1) Ir(1) C(10) C(8) -7(1) . . . . yes O(1) Ir(1) C(10) C(11) 170(1) . . . . yes O(1) Ir(1) C(26) C(24) -84.8(5) . . . . yes O(1) Ir(1) C(26) C(27) 99.0(4) . . . . yes O(1) C(34) C(35) C(36) 0(1) . . . . yes O(2) Ir(1) O(1) C(34) -10.2(5) . . . . yes O(2) Ir(1) N(1) C(1) -88.7(5) . . . . yes O(2) Ir(1) N(1) C(9) 93.2(4) . . . . yes O(2) Ir(1) N(2) C(17) 11.5(4) . . . . yes O(2) Ir(1) N(2) C(25) -176.3(4) . . . . yes O(2) Ir(1) C(10) C(8) -90.7(4) . . . . yes O(2) Ir(1) C(10) C(11) 87.6(5) . . . . yes O(2) Ir(1) C(26) C(24) 37(1) . . . . yes O(2) Ir(1) C(26) C(27) -138(1) . . . . yes O(2) C(36) C(35) C(34) -4(1) . . . . yes O(3) Ir(2) O(4) C(73) 9.7(4) . . . . yes O(3) Ir(2) N(3) C(38) -4.4(5) . . . . yes O(3) Ir(2) N(3) C(46) 176.8(4) . . . . yes O(3) Ir(2) N(4) C(54) 88.2(5) . . . . yes O(3) Ir(2) N(4) C(62) -95.2(4) . . . . yes O(3) Ir(2) C(47) C(45) -1(1) . . . . yes O(3) Ir(2) C(47) C(48) 178(1) . . . . yes O(3) Ir(2) C(63) C(61) 92.4(4) . . . . yes O(3) Ir(2) C(63) C(64) -91.5(5) . . . . yes O(3) C(71) C(72) C(73) 1(1) . . . . yes O(4) Ir(2) O(3) C(71) -13.9(4) . . . . yes O(4) Ir(2) N(3) C(38) 82.0(5) . . . . yes O(4) Ir(2) N(3) C(46) -96.8(4) . . . . yes O(4) Ir(2) N(4) C(54) 1.6(5) . . . . yes O(4) Ir(2) N(4) C(62) 178.2(4) . . . . yes O(4) Ir(2) C(47) C(45) 91.7(5) . . . . yes O(4) Ir(2) C(47) C(48) -87.9(5) . . . . yes O(4) Ir(2) C(63) C(61) -3(1) . . . . yes O(4) Ir(2) C(63) C(64) 172(1) . . . . yes O(4) C(73) C(72) C(71) -7.1(10) . . . . yes N(1) Ir(1) O(1) C(34) -99.0(5) . . . . yes N(1) Ir(1) O(2) C(36) 101.3(5) . . . . yes N(1) Ir(1) N(2) C(17) -151(2) . . . . yes N(1) Ir(1) N(2) C(25) 20(2) . . . . yes N(1) Ir(1) C(10) C(8) -1.9(4) . . . . yes N(1) Ir(1) C(10) C(11) 176.4(5) . . . . yes N(1) Ir(1) C(26) C(24) 180.0(5) . . . . yes N(1) Ir(1) C(26) C(27) 3.8(5) . . . . yes N(1) C(1) C(2) C(3) 1.0(9) . . . . yes N(1) C(9) C(4) C(3) 3.6(8) . . . . yes N(1) C(9) C(4) C(5) -178.7(5) . . . . yes N(1) C(9) C(8) C(7) -174.8(5) . . . . yes N(1) C(9) C(8) C(10) 1.9(7) . . . . yes N(2) Ir(1) O(1) C(34) 85.5(5) . . . . yes N(2) Ir(1) O(2) C(36) -77.3(5) . . . . yes N(2) Ir(1) N(1) C(1) 74(2) . . . . yes N(2) Ir(1) N(1) C(9) -103(2) . . . . yes N(2) Ir(1) C(10) C(8) 173.5(4) . . . . yes N(2) Ir(1) C(10) C(11) -8.2(5) . . . . yes N(2) Ir(1) C(26) C(24) -1.7(4) . . . . yes N(2) Ir(1) C(26) C(27) -177.9(5) . . . . yes N(2) C(17) C(18) C(19) 3.4(9) . . . . yes N(2) C(25) C(20) C(19) 1.8(8) . . . . yes N(2) C(25) C(20) C(21) -179.6(5) . . . . yes N(2) C(25) C(24) C(23) 179.7(5) . . . . yes N(2) C(25) C(24) C(26) -3.4(7) . . . . yes N(3) Ir(2) O(3) C(71) 75.6(5) . . . . yes N(3) Ir(2) O(4) C(73) -83.1(4) . . . . yes N(3) Ir(2) N(4) C(54) -123(1) . . . . yes N(3) Ir(2) N(4) C(62) 53(1) . . . . yes N(3) Ir(2) C(47) C(45) 2.7(5) . . . . yes N(3) Ir(2) C(47) C(48) -176.9(6) . . . . yes N(3) Ir(2) C(63) C(61) -174.4(4) . . . . yes N(3) Ir(2) C(63) C(64) 1.7(5) . . . . yes N(3) C(38) C(39) C(40) -0.9(10) . . . . yes N(3) C(46) C(41) C(40) -2.9(9) . . . . yes N(3) C(46) C(41) C(42) 179.0(6) . . . . yes N(3) C(46) C(45) C(44) 179.6(5) . . . . yes N(3) C(46) C(45) C(47) 0.3(8) . . . . yes N(4) Ir(2) O(3) C(71) -107.3(5) . . . . yes N(4) Ir(2) O(4) C(73) 101.6(4) . . . . yes N(4) Ir(2) N(3) C(38) -153(1) . . . . yes N(4) Ir(2) N(3) C(46) 28(1) . . . . yes N(4) Ir(2) C(47) C(45) -174.3(5) . . . . yes N(4) Ir(2) C(47) C(48) 6.1(5) . . . . yes N(4) Ir(2) C(63) C(61) 1.0(4) . . . . yes N(4) Ir(2) C(63) C(64) 177.1(5) . . . . yes N(4) C(54) C(55) C(56) 0.0(10) . . . . yes N(4) C(62) C(57) C(56) 4.4(9) . . . . yes N(4) C(62) C(57) C(58) -178.3(5) . . . . yes N(4) C(62) C(61) C(60) -178.3(5) . . . . yes N(4) C(62) C(61) C(63) -0.7(7) . . . . yes C(1) N(1) Ir(1) C(10) -179.0(5) . . . . yes C(1) N(1) Ir(1) C(26) 95.1(5) . . . . yes C(1) N(1) C(9) C(4) -2.7(8) . . . . yes C(1) N(1) C(9) C(8) 178.4(5) . . . . yes C(1) C(2) C(3) C(4) -0.1(9) . . . . yes C(2) C(1) N(1) C(9) 0.4(8) . . . . yes C(2) C(3) C(4) C(5) -179.8(5) . . . . yes C(2) C(3) C(4) C(9) -2.2(8) . . . . yes C(3) C(4) C(5) C(6) -158.5(5) . . . . yes C(3) C(4) C(9) C(8) -177.6(5) . . . . yes C(4) C(5) C(6) C(7) -53.6(6) . . . . yes C(4) C(9) C(8) C(7) 6.4(8) . . . . yes C(4) C(9) C(8) C(10) -177.0(5) . . . . yes C(5) C(4) C(9) C(8) 0.1(9) . . . . yes C(5) C(6) C(7) C(8) 59.1(6) . . . . yes C(6) C(5) C(4) C(9) 23.9(7) . . . . yes C(6) C(7) C(8) C(9) -35.4(7) . . . . yes C(6) C(7) C(8) C(10) 148.5(6) . . . . yes C(7) C(8) C(10) C(11) -1.6(9) . . . . yes C(8) C(10) Ir(1) C(26) 94.9(5) . . . . yes C(8) C(10) C(11) C(12) 122.9(6) . . . . yes C(8) C(10) C(11) C(16) -58.6(8) . . . . yes C(9) N(1) Ir(1) C(10) 2.8(4) . . . . yes C(9) N(1) Ir(1) C(26) -83.0(4) . . . . yes C(9) C(8) C(10) C(11) -177.7(5) . . . . yes C(10) Ir(1) O(1) C(34) -93(1) . . . . yes C(10) Ir(1) O(2) C(36) -179.4(5) . . . . yes C(10) Ir(1) N(2) C(17) 102.8(4) . . . . yes C(10) Ir(1) N(2) C(25) -84.9(4) . . . . yes C(10) Ir(1) C(26) C(24) 101.0(5) . . . . yes C(10) Ir(1) C(26) C(27) -75.1(5) . . . . yes C(10) C(11) C(12) C(13) -179.9(6) . . . . yes C(10) C(11) C(16) C(15) -179.4(6) . . . . yes C(11) C(10) Ir(1) C(26) -86.8(5) . . . . yes C(11) C(12) C(13) C(14) -1(1) . . . . yes C(11) C(16) C(15) C(14) 0(1) . . . . yes C(12) C(11) C(16) C(15) -0.9(10) . . . . yes C(12) C(13) C(14) C(15) 0(1) . . . . yes C(13) C(12) C(11) C(16) 1.5(9) . . . . yes C(13) C(14) C(15) C(16) 0(1) . . . . yes C(17) N(2) Ir(1) C(26) -172.5(5) . . . . yes C(17) N(2) C(25) C(20) -0.6(8) . . . . yes C(17) N(2) C(25) C(24) 174.7(5) . . . . yes C(17) C(18) C(19) C(20) -2.1(9) . . . . yes C(18) C(17) N(2) C(25) -2.1(8) . . . . yes C(18) C(19) C(20) C(21) -179.0(5) . . . . yes C(18) C(19) C(20) C(25) -0.4(8) . . . . yes C(19) C(20) C(21) C(22) -155.0(5) . . . . yes C(19) C(20) C(25) C(24) -173.1(5) . . . . yes C(20) C(21) C(22) C(23) -58.0(6) . . . . yes C(20) C(25) C(24) C(23) -5.0(8) . . . . yes C(20) C(25) C(24) C(26) 171.8(5) . . . . yes C(21) C(20) C(25) C(24) 5.5(8) . . . . yes C(21) C(22) C(23) C(24) 58.3(6) . . . . yes C(22) C(21) C(20) C(25) 26.5(7) . . . . yes C(22) C(23) C(24) C(25) -27.2(7) . . . . yes C(22) C(23) C(24) C(26) 156.4(6) . . . . yes C(23) C(24) C(26) C(27) -4.1(9) . . . . yes C(24) C(26) C(27) C(28) -71.1(8) . . . . yes C(24) C(26) C(27) C(32) 112.4(7) . . . . yes C(25) N(2) Ir(1) C(26) -0.2(4) . . . . yes C(25) C(24) C(26) C(27) 179.5(5) . . . . yes C(26) Ir(1) O(1) C(34) 164.5(5) . . . . yes C(26) Ir(1) O(2) C(36) -115(1) . . . . yes C(26) C(27) C(28) C(29) -179.0(6) . . . . yes C(26) C(27) C(32) C(31) 178.0(6) . . . . yes C(27) C(28) C(29) C(30) 2(1) . . . . yes C(27) C(32) C(31) C(30) -0.2(10) . . . . yes C(28) C(27) C(32) C(31) 1.3(9) . . . . yes C(28) C(29) C(30) C(31) -1(1) . . . . yes C(29) C(28) C(27) C(32) -2.4(9) . . . . yes C(29) C(30) C(31) C(32) 0(1) . . . . yes C(33) C(34) C(35) C(36) 179.3(6) . . . . yes C(34) C(35) C(36) C(37) 175.0(6) . . . . yes C(38) N(3) Ir(2) C(47) 176.2(5) . . . . yes C(38) N(3) Ir(2) C(63) -99.0(5) . . . . yes C(38) N(3) C(46) C(41) 3.2(9) . . . . yes C(38) N(3) C(46) C(45) -176.8(5) . . . . yes C(38) C(39) C(40) C(41) 1.2(10) . . . . yes C(39) C(38) N(3) C(46) -1.3(9) . . . . yes C(39) C(40) C(41) C(42) 178.7(6) . . . . yes C(39) C(40) C(41) C(46) 0.6(9) . . . . yes C(40) C(41) C(42) C(43) 157.5(6) . . . . yes C(40) C(41) C(46) C(45) 177.2(6) . . . . yes C(41) C(42) C(43) C(44) 51.6(8) . . . . yes C(41) C(46) C(45) C(44) -0.4(9) . . . . yes C(41) C(46) C(45) C(47) -179.8(6) . . . . yes C(42) C(41) C(46) C(45) -0.9(10) . . . . yes C(42) C(43) C(44) C(45) -53.8(8) . . . . yes C(43) C(42) C(41) C(46) -24.5(9) . . . . yes C(43) C(44) C(45) C(46) 27.3(8) . . . . yes C(43) C(44) C(45) C(47) -153.5(7) . . . . yes C(44) C(45) C(47) C(48) -2(1) . . . . yes C(45) C(47) Ir(2) C(63) -94.5(5) . . . . yes C(45) C(47) C(48) C(49) -102.3(8) . . . . yes C(45) C(47) C(48) C(53) 80.9(8) . . . . yes C(46) N(3) Ir(2) C(47) -2.6(4) . . . . yes C(46) N(3) Ir(2) C(63) 82.3(4) . . . . yes C(46) C(45) C(47) C(48) 177.1(5) . . . . yes C(47) Ir(2) O(3) C(71) 79(1) . . . . yes C(47) Ir(2) O(4) C(73) -162.2(4) . . . . yes C(47) Ir(2) N(4) C(54) -92.8(5) . . . . yes C(47) Ir(2) N(4) C(62) 83.7(4) . . . . yes C(47) Ir(2) C(63) C(61) -95.7(4) . . . . yes C(47) Ir(2) C(63) C(64) 80.4(5) . . . . yes C(47) C(48) C(49) C(50) 176.1(6) . . . . yes C(47) C(48) C(53) C(52) -178.7(6) . . . . yes C(48) C(47) Ir(2) C(63) 85.9(5) . . . . yes C(48) C(49) C(50) C(51) 5(1) . . . . yes C(48) C(53) C(52) C(51) 0(1) . . . . yes C(49) C(48) C(53) C(52) 4.3(10) . . . . yes C(49) C(50) C(51) C(52) -1(1) . . . . yes C(50) C(49) C(48) C(53) -6.9(10) . . . . yes C(50) C(51) C(52) C(53) -1(1) . . . . yes C(54) N(4) Ir(2) C(63) -177.9(5) . . . . yes C(54) N(4) C(62) C(57) -3.9(8) . . . . yes C(54) N(4) C(62) C(61) 178.2(5) . . . . yes C(54) C(55) C(56) C(57) 0.6(10) . . . . yes C(55) C(54) N(4) C(62) 1.6(9) . . . . yes C(55) C(56) C(57) C(58) -180.0(6) . . . . yes C(55) C(56) C(57) C(62) -2.8(10) . . . . yes C(56) C(57) C(58) C(59) -157.8(6) . . . . yes C(56) C(57) C(62) C(61) -178.0(6) . . . . yes C(57) C(58) C(59) C(60) -52.1(8) . . . . yes C(57) C(62) C(61) C(60) 4.0(9) . . . . yes C(57) C(62) C(61) C(63) -178.5(5) . . . . yes C(58) C(57) C(62) C(61) -0.6(9) . . . . yes C(58) C(59) C(60) C(61) 55.7(7) . . . . yes C(59) C(58) C(57) C(62) 25.0(8) . . . . yes C(59) C(60) C(61) C(62) -31.6(7) . . . . yes C(59) C(60) C(61) C(63) 151.2(6) . . . . yes C(60) C(61) C(63) C(64) 0.5(9) . . . . yes C(61) C(63) C(64) C(65) -120.5(6) . . . . yes C(61) C(63) C(64) C(69) 60.7(8) . . . . yes C(62) N(4) Ir(2) C(63) -1.3(4) . . . . yes C(62) C(61) C(63) C(64) -176.7(5) . . . . yes C(63) Ir(2) O(3) C(71) 172.2(5) . . . . yes C(63) Ir(2) O(4) C(73) 106(1) . . . . yes C(63) C(64) C(65) C(66) 179.7(5) . . . . yes C(63) C(64) C(69) C(68) 179.6(6) . . . . yes C(64) C(65) C(66) C(67) 2.0(9) . . . . yes C(64) C(69) C(68) C(67) -0.6(10) . . . . yes C(65) C(64) C(69) C(68) 0.7(9) . . . . yes C(65) C(66) C(67) C(68) -1.9(9) . . . . yes C(66) C(65) C(64) C(69) -1.4(8) . . . . yes C(66) C(67) C(68) C(69) 1.2(10) . . . . yes C(70) C(71) C(72) C(73) -177.4(6) . . . . yes C(71) C(72) C(73) C(74) 172.6(6) . . . . yes C(71) C(72) C(73) C(74) 172.6(6) . . . . 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 O(1) C(40) 3.555(8) . 2_566 ? O(2) C(3) 3.546(8) . 2_555 ? O(3) C(37) 3.363(7) . 1_455 ? O(3) C(35) 3.414(7) . 1_455 ? O(4) C(29) 3.341(7) . 1_565 ? N(1) C(3) 3.542(8) . 2_555 ? C(1) C(4) 3.557(8) . 2_555 ? C(1) C(5) 3.595(9) . 2_555 ? C(2) C(4) 3.327(8) . 2_555 ? C(2) C(9) 3.527(8) . 2_555 ? C(3) C(9) 3.486(8) . 2_555 ? C(3) C(4) 3.575(8) . 2_555 ? C(18) C(21) 3.506(9) . 2_656 ? C(18) C(66) 3.513(8) . 1_655 ? C(18) C(67) 3.550(8) . 1_655 ? C(19) C(19) 3.20(1) . 2_656 ? C(19) C(20) 3.453(8) . 2_656 ? C(20) C(40) 3.502(9) . 2_566 ? C(22) C(31) 3.551(9) . 2_556 ? C(25) C(40) 3.523(8) . 2_566 ? C(29) C(46) 3.496(9) . 1_545 ? C(30) C(74) 3.501(10) . 1_545 ? C(33) C(67) 3.394(8) . 2_566 ? C(39) C(66) 3.587(8) . 2_466 ? #===END #------------------------------------------------------------------------------ data_4c _database_code_depnum_ccdc_archive 'CCDC 616852' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C39 H39 Ir N2 O2 ' _chemical_formula_moiety ? _chemical_formula_weight 759.97 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.04(2) _cell_length_b 14.11(2) _cell_length_c 17.34(2) _cell_angle_alpha 101.53(6) _cell_angle_beta 103.15(6) _cell_angle_gamma 102.54(5) _cell_volume 3150(24) _cell_formula_units_Z 4 _cell_measurement_reflns_used 26928 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.274 _exptl_absorpt_correction_T_max 0.651 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 29064 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9607 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9607 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 13865 _reflns_number_gt 11464 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0761 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 13865 _refine_ls_number_parameters 793 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0014 _refine_diff_density_max 1.05 _refine_diff_density_min -0.77 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.042274(9) 0.19279(1) 0.250406(8) 0.01380(4) Uani 1.00 d . . . Ir(2) Ir -0.46449(1) 0.34169(1) -0.220520(8) 0.01512(4) Uani 1.00 d . . . O(1) O 0.0842(2) 0.2822(2) 0.1701(2) 0.0201(7) Uani 1.00 d . . . O(2) O 0.1993(2) 0.2007(2) 0.2976(2) 0.0211(7) Uani 1.00 d . . . O(3) O -0.5789(2) 0.3236(2) -0.1557(2) 0.0204(7) Uani 1.00 d . . . O(4) O -0.4406(2) 0.5025(2) -0.1776(2) 0.0216(7) Uani 1.00 d . . . N(1) N 0.0678(2) 0.3101(2) 0.3498(2) 0.0151(7) Uani 1.00 d . . . N(2) N 0.0119(2) 0.0696(2) 0.1562(2) 0.0154(8) Uani 1.00 d . . . N(3) N -0.3489(2) 0.3429(2) -0.1250(2) 0.0192(8) Uani 1.00 d . . . N(4) N -0.5764(2) 0.3277(2) -0.3232(2) 0.0175(8) Uani 1.00 d . . . C(1) C 0.1125(2) 0.4063(3) 0.3539(2) 0.0162(9) Uani 1.00 d . . . C(2) C 0.1333(3) 0.4821(3) 0.4233(3) 0.0198(10) Uani 1.00 d . . . C(3) C 0.1000(3) 0.4598(3) 0.4894(2) 0.0192(9) Uani 1.00 d . . . C(4) C 0.0543(2) 0.3616(3) 0.4867(2) 0.0149(8) Uani 1.00 d . . . C(5) C 0.0410(2) 0.2851(3) 0.4162(2) 0.0149(9) Uani 1.00 d . . . C(6) C 0.0135(3) 0.3405(3) 0.5573(2) 0.024(1) Uani 1.00 d . . . C(7) C -0.0949(3) 0.2710(3) 0.5287(3) 0.026(1) Uani 1.00 d . . . C(8) C -0.1021(3) 0.1582(3) 0.5045(2) 0.026(1) Uani 1.00 d . . . C(9) C -0.0144(3) 0.1350(3) 0.4748(2) 0.024(1) Uani 1.00 d . . . C(10) C 0.0061(3) 0.1771(3) 0.4040(2) 0.0167(9) Uani 1.00 d . . . C(11) C 0.0003(3) 0.1197(3) 0.3299(2) 0.0170(9) Uani 1.00 d . . . C(12) C -0.0373(3) 0.0082(3) 0.3087(2) 0.0173(9) Uani 1.00 d . . . C(13) C 0.0281(3) -0.0524(3) 0.2998(2) 0.024(1) Uani 1.00 d . . . C(14) C -0.0081(4) -0.1566(3) 0.2814(3) 0.034(1) Uani 1.00 d . . . C(15) C -0.1096(3) -0.2015(3) 0.2711(3) 0.028(1) Uani 1.00 d . . . C(16) C -0.1771(3) -0.1434(3) 0.2780(3) 0.029(1) Uani 1.00 d . . . C(17) C -0.1387(3) -0.0389(3) 0.2965(2) 0.024(1) Uani 1.00 d . . . C(18) C 0.0817(3) 0.0227(3) 0.1410(2) 0.0186(9) Uani 1.00 d . . . C(19) C 0.0564(3) -0.0662(3) 0.0802(2) 0.022(1) Uani 1.00 d . . . C(20) C -0.0461(3) -0.1094(3) 0.0374(2) 0.026(1) Uani 1.00 d . . . C(21) C -0.1192(3) -0.0624(3) 0.0528(2) 0.0205(9) Uani 1.00 d . . . C(22) C -0.0889(3) 0.0308(3) 0.1107(2) 0.0183(9) Uani 1.00 d . . . C(23) C -0.2314(3) -0.1170(3) 0.0099(3) 0.028(1) Uani 1.00 d . . . C(24) C -0.2989(3) -0.1089(3) 0.0678(3) 0.034(1) Uani 1.00 d . . . C(25) C -0.3356(3) -0.0139(3) 0.0775(3) 0.030(1) Uani 1.00 d . . . C(26) C -0.2561(3) 0.0775(3) 0.0751(3) 0.024(1) Uani 1.00 d . . . C(27) C -0.1502(3) 0.0972(3) 0.1328(2) 0.0196(9) Uani 1.00 d . . . C(28) C -0.1047(3) 0.1754(3) 0.1984(2) 0.0178(9) Uani 1.00 d . . . C(29) C -0.1582(3) 0.2496(3) 0.2274(2) 0.024(1) Uani 1.00 d . . . C(30) C -0.2386(4) 0.2215(4) 0.2599(3) 0.036(1) Uani 1.00 d . . . C(31) C -0.2887(4) 0.2898(5) 0.2864(3) 0.049(2) Uani 1.00 d . . . C(32) C -0.2590(4) 0.3877(4) 0.2815(3) 0.048(2) Uani 1.00 d . . . C(33) C -0.1797(3) 0.4162(3) 0.2501(3) 0.035(1) Uani 1.00 d . . . C(34) C -0.1265(3) 0.3495(3) 0.2245(3) 0.026(1) Uani 1.00 d . . . C(35) C 0.1862(3) 0.3801(3) 0.1083(3) 0.024(1) Uani 1.00 d . . . C(36) C 0.1746(3) 0.3195(3) 0.1698(2) 0.0203(9) Uani 1.00 d . . . C(37) C 0.2641(3) 0.3110(3) 0.2216(3) 0.025(1) Uani 1.00 d . . . C(38) C 0.2721(3) 0.2570(3) 0.2802(2) 0.0233(10) Uani 1.00 d . . . C(39) C 0.3777(3) 0.2622(4) 0.3301(3) 0.035(1) Uani 1.00 d . . . C(40) C -0.3605(3) 0.3405(3) -0.0505(2) 0.023(1) Uani 1.00 d . . . C(41) C -0.2807(3) 0.3317(3) 0.0110(2) 0.029(1) Uani 1.00 d . . . C(42) C -0.1929(3) 0.3233(3) -0.0064(3) 0.027(1) Uani 1.00 d . . . C(43) C -0.1791(3) 0.3270(3) -0.0819(3) 0.0235(10) Uani 1.00 d . . . C(44) C -0.2593(3) 0.3385(3) -0.1424(2) 0.0197(9) Uani 1.00 d . . . C(45) C -0.0817(3) 0.3132(4) -0.1001(3) 0.034(1) Uani 1.00 d . . . C(46) C -0.0197(4) 0.3987(4) -0.1227(3) 0.052(2) Uani 1.00 d . . . C(47) C -0.0689(3) 0.4211(4) -0.2015(3) 0.035(1) Uani 1.00 d . . . C(48) C -0.1679(3) 0.3471(4) -0.2555(3) 0.029(1) Uani 1.00 d . . . C(49) C -0.2605(3) 0.3457(3) -0.2250(2) 0.0177(9) Uani 1.00 d . . . C(50) C -0.3508(3) 0.3510(3) -0.2716(2) 0.0171(9) Uani 1.00 d . . . C(51) C -0.3651(3) 0.3577(3) -0.3577(2) 0.0174(9) Uani 1.00 d . . . C(52) C -0.3642(3) 0.2797(3) -0.4198(3) 0.027(1) Uani 1.00 d . . . C(53) C -0.3790(3) 0.2874(3) -0.5003(3) 0.030(1) Uani 1.00 d . . . C(54) C -0.3937(3) 0.3750(3) -0.5185(3) 0.029(1) Uani 1.00 d . . . C(55) C -0.3959(3) 0.4530(3) -0.4577(3) 0.027(1) Uani 1.00 d . . . C(56) C -0.3812(3) 0.4458(3) -0.3778(3) 0.0211(10) Uani 1.00 d . . . C(57) C -0.6094(3) 0.4047(3) -0.3440(2) 0.0189(9) Uani 1.00 d . . . C(58) C -0.6802(3) 0.3912(3) -0.4164(3) 0.024(1) Uani 1.00 d . . . C(59) C -0.7203(3) 0.2970(3) -0.4698(2) 0.024(1) Uani 1.00 d . . . C(60) C -0.6904(3) 0.2149(3) -0.4503(2) 0.0209(10) Uani 1.00 d . . . C(61) C -0.6200(3) 0.2319(3) -0.3737(2) 0.0171(9) Uani 1.00 d . . . C(62) C -0.7290(3) 0.1150(3) -0.5133(3) 0.030(1) Uani 1.00 d . . . C(63) C -0.6452(3) 0.0650(3) -0.5245(3) 0.033(1) Uani 1.00 d . . . C(64) C -0.6208(3) 0.0028(3) -0.4641(3) 0.028(1) Uani 1.00 d . . . C(65) C -0.6322(3) 0.0464(3) -0.3797(3) 0.023(1) Uani 1.00 d . . . C(66) C -0.5784(3) 0.1565(3) -0.3407(2) 0.0191(10) Uani 1.00 d . . . C(67) C -0.5029(3) 0.1931(3) -0.2706(2) 0.0180(9) Uani 1.00 d . . . C(68) C -0.4482(3) 0.1259(3) -0.2351(2) 0.0197(9) Uani 1.00 d . . . C(69) C -0.3830(3) 0.0861(3) -0.2711(3) 0.029(1) Uani 1.00 d . . . C(70) C -0.3343(4) 0.0207(4) -0.2404(3) 0.037(1) Uani 1.00 d . . . C(71) C -0.3558(4) -0.0102(4) -0.1748(3) 0.043(2) Uani 1.00 d . . . C(72) C -0.4185(4) 0.0297(4) -0.1364(3) 0.042(1) Uani 1.00 d . . . C(73) C -0.4653(3) 0.0979(3) -0.1654(3) 0.031(1) Uani 1.00 d . . . C(74) C -0.6957(3) 0.3620(3) -0.0830(3) 0.028(1) Uani 1.00 d . . . C(75) C -0.6141(3) 0.3932(3) -0.1236(2) 0.0202(9) Uani 1.00 d . . . C(76) C -0.5789(3) 0.4957(3) -0.1193(2) 0.024(1) Uani 1.00 d . . . C(77) C -0.4985(3) 0.5431(3) -0.1437(2) 0.0205(9) Uani 1.00 d . . . C(78) C -0.4759(3) 0.6560(3) -0.1293(3) 0.030(1) Uani 1.00 d . . . H(1) H 0.1298 0.4221 0.3072 0.0196 Uiso 1.00 calc . . . H(2) H 0.1699 0.5487 0.4266 0.0236 Uiso 1.00 calc . . . H(3) H 0.1082 0.5124 0.5361 0.0230 Uiso 1.00 calc . . . H(4) H 0.0565 0.3096 0.5881 0.0287 Uiso 1.00 calc . . . H(5) H 0.0136 0.4023 0.5910 0.0287 Uiso 1.00 calc . . . H(6) H -0.1250 0.2828 0.5723 0.0308 Uiso 1.00 calc . . . H(7) H -0.1317 0.2873 0.4826 0.0308 Uiso 1.00 calc . . . H(8) H -0.1041 0.1328 0.5511 0.0307 Uiso 1.00 calc . . . H(9) H -0.1634 0.1252 0.4619 0.0307 Uiso 1.00 calc . . . H(10) H 0.0453 0.1615 0.5198 0.0281 Uiso 1.00 calc . . . H(11) H -0.0282 0.0639 0.4576 0.0281 Uiso 1.00 calc . . . H(12) H 0.0979 -0.0221 0.3065 0.0292 Uiso 1.00 calc . . . H(13) H 0.0368 -0.1971 0.2752 0.0406 Uiso 1.00 calc . . . H(14) H -0.1331 -0.2725 0.2591 0.0336 Uiso 1.00 calc . . . H(15) H -0.2472 -0.1738 0.2703 0.0347 Uiso 1.00 calc . . . H(16) H -0.1843 0.0016 0.3009 0.0292 Uiso 1.00 calc . . . H(17) H 0.1505 0.0513 0.1729 0.0224 Uiso 1.00 calc . . . H(18) H 0.1071 -0.0967 0.0680 0.0270 Uiso 1.00 calc . . . H(19) H -0.0655 -0.1722 -0.0026 0.0306 Uiso 1.00 calc . . . H(20) H -0.2544 -0.0881 -0.0333 0.0338 Uiso 1.00 calc . . . H(21) H -0.2374 -0.1859 -0.0118 0.0338 Uiso 1.00 calc . . . H(22) H -0.3563 -0.1659 0.0473 0.0404 Uiso 1.00 calc . . . H(23) H -0.2605 -0.1098 0.1205 0.0404 Uiso 1.00 calc . . . H(24) H -0.3955 -0.0255 0.0341 0.0366 Uiso 1.00 calc . . . H(25) H -0.3509 -0.0003 0.1286 0.0366 Uiso 1.00 calc . . . H(26) H -0.2506 0.0681 0.0208 0.0286 Uiso 1.00 calc . . . H(27) H -0.2795 0.1352 0.0892 0.0286 Uiso 1.00 calc . . . H(28) H -0.2585 0.1546 0.2641 0.0432 Uiso 1.00 calc . . . H(29) H -0.3443 0.2694 0.3076 0.0595 Uiso 1.00 calc . . . H(30) H -0.2934 0.4348 0.2996 0.0576 Uiso 1.00 calc . . . H(31) H -0.1603 0.4834 0.2456 0.0416 Uiso 1.00 calc . . . H(32) H -0.0694 0.3715 0.2056 0.0314 Uiso 1.00 calc . . . H(33) H 0.1244 0.3953 0.0876 0.0296 Uiso 1.00 calc . . . H(34) H 0.2052 0.3442 0.0650 0.0296 Uiso 1.00 calc . . . H(35) H 0.2385 0.4424 0.1352 0.0296 Uiso 1.00 calc . . . H(36) H 0.3264 0.3467 0.2156 0.0306 Uiso 1.00 calc . . . H(37) H 0.3899 0.2967 0.3854 0.0423 Uiso 1.00 calc . . . H(38) H 0.4276 0.2964 0.3079 0.0423 Uiso 1.00 calc . . . H(39) H 0.3846 0.1955 0.3271 0.0423 Uiso 1.00 calc . . . H(40) H -0.4228 0.3445 -0.0393 0.0280 Uiso 1.00 calc . . . H(41) H -0.2880 0.3319 0.0642 0.0344 Uiso 1.00 calc . . . H(42) H -0.1399 0.3146 0.0343 0.0325 Uiso 1.00 calc . . . H(43) H -0.0403 0.3030 -0.0525 0.0409 Uiso 1.00 calc . . . H(44) H -0.0992 0.2549 -0.1443 0.0409 Uiso 1.00 calc . . . H(45) H -0.0047 0.4579 -0.0792 0.0616 Uiso 1.00 calc . . . H(46) H 0.0420 0.3839 -0.1271 0.0616 Uiso 1.00 calc . . . H(47) H -0.0814 0.4849 -0.1879 0.0424 Uiso 1.00 calc . . . H(48) H -0.0217 0.4239 -0.2333 0.0424 Uiso 1.00 calc . . . H(49) H -0.1818 0.3621 -0.3072 0.0350 Uiso 1.00 calc . . . H(50) H -0.1584 0.2816 -0.2622 0.0350 Uiso 1.00 calc . . . H(51) H -0.3531 0.2196 -0.4073 0.0318 Uiso 1.00 calc . . . H(52) H -0.3791 0.2326 -0.5424 0.0366 Uiso 1.00 calc . . . H(53) H -0.4026 0.3816 -0.5731 0.0341 Uiso 1.00 calc . . . H(54) H -0.4078 0.5127 -0.4708 0.0324 Uiso 1.00 calc . . . H(55) H -0.3820 0.5005 -0.3361 0.0254 Uiso 1.00 calc . . . H(56) H -0.5828 0.4700 -0.3072 0.0227 Uiso 1.00 calc . . . H(57) H -0.7015 0.4468 -0.4297 0.0284 Uiso 1.00 calc . . . H(58) H -0.7691 0.2879 -0.5207 0.0282 Uiso 1.00 calc . . . H(59) H -0.7774 0.0714 -0.4966 0.0366 Uiso 1.00 calc . . . H(60) H -0.7610 0.1248 -0.5644 0.0366 Uiso 1.00 calc . . . H(61) H -0.6664 0.0222 -0.5787 0.0398 Uiso 1.00 calc . . . H(62) H -0.5854 0.1162 -0.5178 0.0398 Uiso 1.00 calc . . . H(63) H -0.6661 -0.0634 -0.4861 0.0338 Uiso 1.00 calc . . . H(64) H -0.5530 -0.0008 -0.4579 0.0338 Uiso 1.00 calc . . . H(65) H -0.7027 0.0374 -0.3851 0.0277 Uiso 1.00 calc . . . H(66) H -0.6063 0.0093 -0.3438 0.0277 Uiso 1.00 calc . . . H(67) H -0.3714 0.1038 -0.3188 0.0344 Uiso 1.00 calc . . . H(68) H -0.2865 -0.0027 -0.2645 0.0441 Uiso 1.00 calc . . . H(69) H -0.3270 -0.0592 -0.1557 0.0512 Uiso 1.00 calc . . . H(70) H -0.4297 0.0109 -0.0888 0.0504 Uiso 1.00 calc . . . H(71) H -0.5092 0.1247 -0.1385 0.0375 Uiso 1.00 calc . . . H(72) H -0.7353 0.4081 -0.0812 0.0347 Uiso 1.00 calc . . . H(73) H -0.7376 0.2964 -0.1119 0.0347 Uiso 1.00 calc . . . H(74) H -0.6641 0.3614 -0.0277 0.0347 Uiso 1.00 calc . . . H(75) H -0.6152 0.5380 -0.0963 0.0289 Uiso 1.00 calc . . . H(76) H -0.5101 0.6813 -0.0917 0.0365 Uiso 1.00 calc . . . H(77) H -0.4045 0.6856 -0.1063 0.0365 Uiso 1.00 calc . . . H(78) H -0.4981 0.6721 -0.1794 0.0365 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) 0.01410(7) 0.01382(7) 0.01231(8) 0.00319(5) 0.00396(5) 0.00129(6) Ir(2) 0.01532(8) 0.01619(8) 0.01321(8) 0.00547(6) 0.00447(6) 0.00075(6) O(1) 0.021(1) 0.022(1) 0.019(1) 0.006(1) 0.007(1) 0.006(1) O(2) 0.022(1) 0.022(1) 0.019(1) 0.007(1) 0.005(1) 0.003(1) O(3) 0.017(1) 0.025(1) 0.021(1) 0.007(1) 0.008(1) 0.005(1) O(4) 0.031(1) 0.015(1) 0.018(1) 0.007(1) 0.008(1) -0.001(1) N(1) 0.016(1) 0.013(1) 0.013(2) 0.004(1) 0.002(1) 0.001(1) N(2) 0.020(2) 0.015(1) 0.013(2) 0.006(1) 0.007(1) 0.001(1) N(3) 0.026(2) 0.016(2) 0.010(2) 0.006(1) 0.003(1) -0.006(1) N(4) 0.023(2) 0.015(1) 0.014(2) 0.005(1) 0.007(1) -0.001(1) C(1) 0.011(2) 0.016(2) 0.022(2) 0.003(1) 0.005(1) 0.004(2) C(2) 0.011(2) 0.020(2) 0.030(2) 0.006(1) 0.007(2) 0.006(2) C(3) 0.019(2) 0.014(2) 0.018(2) 0.004(1) 0.001(1) -0.007(2) C(4) 0.009(2) 0.017(2) 0.015(2) 0.004(1) 0.003(1) -0.001(2) C(5) 0.010(2) 0.020(2) 0.014(2) 0.007(1) 0.001(1) 0.003(2) C(6) 0.033(2) 0.025(2) 0.018(2) 0.013(2) 0.009(2) 0.006(2) C(7) 0.027(2) 0.026(2) 0.028(2) 0.007(2) 0.017(2) 0.006(2) C(8) 0.041(2) 0.019(2) 0.017(2) 0.005(2) 0.014(2) 0.002(2) C(9) 0.045(2) 0.013(2) 0.011(2) 0.008(2) 0.008(2) 0.000(2) C(10) 0.020(2) 0.016(2) 0.016(2) 0.007(1) 0.006(1) 0.004(2) C(11) 0.014(2) 0.019(2) 0.021(2) 0.008(1) 0.005(1) 0.009(2) C(12) 0.030(2) 0.016(2) 0.009(2) 0.010(2) 0.007(1) 0.002(2) C(13) 0.026(2) 0.027(2) 0.020(2) 0.009(2) 0.006(2) 0.003(2) C(14) 0.051(3) 0.026(2) 0.026(2) 0.021(2) 0.008(2) 0.002(2) C(15) 0.046(3) 0.013(2) 0.022(2) 0.008(2) 0.008(2) 0.001(2) C(16) 0.039(2) 0.023(2) 0.022(2) 0.003(2) 0.011(2) 0.004(2) C(17) 0.035(2) 0.022(2) 0.020(2) 0.009(2) 0.012(2) 0.006(2) C(18) 0.019(2) 0.021(2) 0.017(2) 0.006(1) 0.009(1) 0.002(2) C(19) 0.030(2) 0.021(2) 0.022(2) 0.012(2) 0.014(2) 0.007(2) C(20) 0.041(2) 0.021(2) 0.016(2) 0.008(2) 0.011(2) 0.005(2) C(21) 0.022(2) 0.020(2) 0.016(2) 0.000(2) 0.004(2) 0.004(2) C(22) 0.017(2) 0.021(2) 0.015(2) 0.000(1) 0.006(1) 0.005(2) C(23) 0.031(2) 0.018(2) 0.023(2) -0.002(2) 0.000(2) -0.005(2) C(24) 0.035(2) 0.025(2) 0.029(2) -0.003(2) 0.002(2) 0.000(2) C(25) 0.014(2) 0.038(2) 0.034(2) -0.001(2) 0.000(2) 0.014(2) C(26) 0.013(2) 0.029(2) 0.025(2) 0.003(2) 0.003(2) 0.005(2) C(27) 0.016(2) 0.020(2) 0.022(2) 0.003(1) 0.005(2) 0.007(2) C(28) 0.013(2) 0.023(2) 0.018(2) 0.004(1) 0.005(1) 0.006(2) C(29) 0.032(2) 0.026(2) 0.013(2) 0.012(2) 0.003(2) 0.004(2) C(30) 0.044(3) 0.039(3) 0.037(3) 0.021(2) 0.022(2) 0.012(2) C(31) 0.051(3) 0.073(4) 0.045(3) 0.041(3) 0.028(3) 0.020(3) C(32) 0.044(3) 0.065(4) 0.043(3) 0.042(3) 0.011(2) 0.005(3) C(33) 0.034(2) 0.029(2) 0.034(3) 0.021(2) -0.004(2) -0.006(2) C(34) 0.025(2) 0.025(2) 0.023(2) 0.009(2) 0.001(2) -0.001(2) C(35) 0.022(2) 0.024(2) 0.028(2) 0.002(2) 0.015(2) 0.005(2) C(36) 0.026(2) 0.017(2) 0.015(2) 0.003(2) 0.008(2) -0.002(2) C(37) 0.022(2) 0.025(2) 0.021(2) -0.003(2) 0.007(2) -0.001(2) C(38) 0.020(2) 0.026(2) 0.018(2) 0.006(2) 0.002(2) -0.002(2) C(39) 0.026(2) 0.040(3) 0.030(3) 0.003(2) 0.002(2) 0.005(2) C(40) 0.017(2) 0.035(2) 0.017(2) 0.010(2) 0.007(2) 0.000(2) C(41) 0.034(2) 0.038(2) 0.013(2) 0.015(2) 0.004(2) 0.001(2) C(42) 0.028(2) 0.034(2) 0.020(2) 0.015(2) 0.003(2) 0.007(2) C(43) 0.025(2) 0.017(2) 0.024(2) 0.006(2) 0.000(2) 0.005(2) C(44) 0.018(2) 0.019(2) 0.021(2) 0.005(1) 0.003(1) 0.002(2) C(45) 0.036(2) 0.041(3) 0.031(3) 0.024(2) 0.006(2) 0.016(2) C(46) 0.035(3) 0.066(4) 0.039(3) -0.006(2) -0.004(2) 0.017(3) C(47) 0.017(2) 0.047(3) 0.049(3) 0.011(2) 0.017(2) 0.018(3) C(48) 0.022(2) 0.048(3) 0.023(2) 0.018(2) 0.009(2) 0.007(2) C(49) 0.012(2) 0.017(2) 0.023(2) 0.004(1) 0.005(1) 0.001(2) C(50) 0.020(2) 0.015(2) 0.019(2) 0.008(1) 0.009(1) 0.004(2) C(51) 0.019(2) 0.017(2) 0.016(2) 0.007(1) 0.007(1) 0.001(2) C(52) 0.040(2) 0.020(2) 0.020(2) 0.006(2) 0.009(2) 0.006(2) C(53) 0.045(3) 0.024(2) 0.016(2) 0.003(2) 0.008(2) -0.003(2) C(54) 0.033(2) 0.031(2) 0.017(2) 0.003(2) 0.002(2) 0.010(2) C(55) 0.022(2) 0.032(2) 0.035(2) 0.013(2) 0.010(2) 0.020(2) C(56) 0.019(2) 0.019(2) 0.028(2) 0.008(1) 0.012(2) 0.002(2) C(57) 0.020(2) 0.017(2) 0.023(2) 0.010(1) 0.008(2) 0.005(2) C(58) 0.028(2) 0.021(2) 0.023(2) 0.013(2) 0.006(2) 0.004(2) C(59) 0.023(2) 0.026(2) 0.021(2) 0.009(2) 0.001(2) 0.008(2) C(60) 0.014(2) 0.028(2) 0.023(2) 0.010(2) 0.005(1) 0.006(2) C(61) 0.022(2) 0.015(2) 0.016(2) 0.007(1) 0.008(1) 0.004(2) C(62) 0.035(2) 0.028(2) 0.021(2) 0.011(2) -0.002(2) -0.001(2) C(63) 0.044(3) 0.030(2) 0.024(2) 0.014(2) 0.010(2) -0.001(2) C(64) 0.025(2) 0.028(2) 0.030(2) 0.010(2) 0.009(2) 0.001(2) C(65) 0.029(2) 0.017(2) 0.021(2) 0.008(2) 0.004(2) 0.002(2) C(66) 0.022(2) 0.021(2) 0.021(2) 0.012(2) 0.009(2) 0.009(2) C(67) 0.018(2) 0.019(2) 0.020(2) 0.008(1) 0.008(1) 0.007(2) C(68) 0.019(2) 0.021(2) 0.020(2) 0.004(1) 0.005(1) 0.009(2) C(69) 0.032(2) 0.038(2) 0.028(2) 0.022(2) 0.014(2) 0.015(2) C(70) 0.052(3) 0.040(3) 0.032(3) 0.029(2) 0.017(2) 0.015(2) C(71) 0.056(3) 0.051(3) 0.039(3) 0.036(3) 0.017(2) 0.024(3) C(72) 0.043(3) 0.062(3) 0.036(3) 0.021(2) 0.016(2) 0.031(3) C(73) 0.042(2) 0.037(2) 0.023(2) 0.020(2) 0.014(2) 0.010(2) C(74) 0.032(2) 0.028(2) 0.028(2) 0.009(2) 0.016(2) 0.002(2) C(75) 0.021(2) 0.024(2) 0.013(2) 0.007(2) 0.004(1) -0.002(2) C(76) 0.035(2) 0.017(2) 0.018(2) 0.011(2) 0.009(2) -0.005(2) C(77) 0.026(2) 0.015(2) 0.015(2) 0.006(2) 0.001(2) -0.003(2) C(78) 0.035(2) 0.022(2) 0.032(2) 0.005(2) 0.014(2) 0.000(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; For all methyl groups of the complex, even if it is the lowest, one of H atoms was localized in the Fourier maps, respectively, and H atoms of the rest were placed in geometrically calculated positions. ; 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) O(1) 2.151(2) . . yes Ir(1) O(2) 2.140(4) . . yes Ir(1) N(1) 2.039(3) . . yes Ir(1) N(2) 2.024(3) . . yes Ir(1) C(11) 1.997(3) . . yes Ir(1) C(28) 1.994(4) . . yes Ir(2) O(3) 2.160(3) . . yes Ir(2) O(4) 2.167(3) . . yes Ir(2) N(3) 2.033(3) . . yes Ir(2) N(4) 2.032(3) . . yes Ir(2) C(50) 1.988(4) . . yes Ir(2) C(67) 2.002(4) . . yes O(1) C(36) 1.266(4) . . yes O(2) C(38) 1.285(4) . . yes O(3) C(75) 1.279(5) . . yes O(4) C(77) 1.272(5) . . yes N(1) C(1) 1.347(4) . . yes N(1) C(5) 1.375(4) . . yes N(2) C(18) 1.340(5) . . yes N(2) C(22) 1.381(5) . . yes N(3) C(40) 1.345(5) . . yes N(3) C(44) 1.369(5) . . yes N(4) C(57) 1.350(4) . . yes N(4) C(61) 1.376(5) . . yes C(1) C(2) 1.367(6) . . yes C(1) H(1) 0.950 . . no C(2) C(3) 1.399(5) . . yes C(2) H(2) 0.951 . . no C(3) C(4) 1.380(5) . . yes C(3) H(3) 0.949 . . no C(4) C(5) 1.405(5) . . yes C(4) C(6) 1.519(5) . . yes C(5) C(10) 1.452(5) . . yes C(6) C(7) 1.529(6) . . yes C(6) H(4) 0.949 . . no C(6) H(5) 0.948 . . no C(7) C(8) 1.536(6) . . yes C(7) H(6) 0.951 . . no C(7) H(7) 0.947 . . no C(8) C(9) 1.511(6) . . yes C(8) H(8) 0.951 . . no C(8) H(9) 0.950 . . no C(9) C(10) 1.524(5) . . yes C(9) H(10) 0.948 . . no C(9) H(11) 0.949 . . no C(10) C(11) 1.349(5) . . yes C(11) C(12) 1.486(5) . . yes C(12) C(13) 1.397(5) . . yes C(12) C(17) 1.382(6) . . yes C(13) C(14) 1.391(6) . . yes C(13) H(12) 0.950 . . no C(14) C(15) 1.381(6) . . yes C(14) H(13) 0.948 . . no C(15) C(16) 1.391(6) . . yes C(15) H(14) 0.948 . . no C(16) C(17) 1.398(5) . . yes C(16) H(15) 0.951 . . no C(17) H(16) 0.951 . . no C(18) C(19) 1.386(6) . . yes C(18) H(17) 0.949 . . no C(19) C(20) 1.394(6) . . yes C(19) H(18) 0.950 . . no C(20) C(21) 1.384(6) . . yes C(20) H(19) 0.951 . . no C(21) C(22) 1.398(6) . . yes C(21) C(23) 1.529(6) . . yes C(22) C(27) 1.457(5) . . yes C(23) C(24) 1.536(7) . . yes C(23) H(20) 0.949 . . no C(23) H(21) 0.947 . . no C(24) C(25) 1.529(6) . . yes C(24) H(22) 0.947 . . no C(24) H(23) 0.953 . . no C(25) C(26) 1.525(5) . . yes C(25) H(24) 0.951 . . no C(25) H(25) 0.952 . . no C(26) C(27) 1.524(5) . . yes C(26) H(26) 0.949 . . no C(26) H(27) 0.951 . . no C(27) C(28) 1.334(6) . . yes C(28) C(29) 1.488(6) . . yes C(29) C(30) 1.391(6) . . yes C(29) C(34) 1.397(5) . . yes C(30) C(31) 1.378(7) . . yes C(30) H(28) 0.947 . . no C(31) C(32) 1.379(8) . . yes C(31) H(29) 0.949 . . no C(32) C(33) 1.366(7) . . yes C(32) H(30) 0.948 . . no C(33) C(34) 1.390(6) . . yes C(33) H(31) 0.951 . . no C(34) H(32) 0.949 . . no C(35) C(36) 1.509(5) . . yes C(35) H(33) 0.949 . . no C(35) H(34) 0.943 . . no C(35) H(35) 0.964 . . no C(36) C(37) 1.413(5) . . yes C(37) C(38) 1.385(5) . . yes C(37) H(36) 0.950 . . no C(38) C(39) 1.516(6) . . yes C(39) H(37) 0.942 . . no C(39) H(38) 0.960 . . no C(39) H(39) 0.959 . . no C(40) C(41) 1.406(5) . . yes C(40) H(40) 0.949 . . no C(41) C(42) 1.358(6) . . yes C(41) H(41) 0.951 . . no C(42) C(43) 1.375(6) . . yes C(42) H(42) 0.950 . . no C(43) C(44) 1.416(5) . . yes C(43) C(45) 1.515(6) . . yes C(44) C(49) 1.452(5) . . yes C(45) C(46) 1.501(6) . . yes C(45) H(43) 0.952 . . no C(45) H(44) 0.949 . . no C(46) C(47) 1.511(6) . . yes C(46) H(45) 0.954 . . no C(46) H(46) 0.949 . . no C(47) C(48) 1.512(6) . . yes C(47) H(47) 0.948 . . no C(47) H(48) 0.954 . . no C(48) C(49) 1.509(5) . . yes C(48) H(49) 0.950 . . no C(48) H(50) 0.949 . . no C(49) C(50) 1.366(5) . . yes C(50) C(51) 1.486(5) . . yes C(51) C(52) 1.382(6) . . yes C(51) C(56) 1.405(5) . . yes C(52) C(53) 1.392(5) . . yes C(52) H(51) 0.952 . . no C(53) C(54) 1.382(6) . . yes C(53) H(52) 0.951 . . no C(54) C(55) 1.374(6) . . yes C(54) H(53) 0.952 . . no C(55) C(56) 1.382(6) . . yes C(55) H(54) 0.953 . . no C(56) H(55) 0.951 . . no C(57) C(58) 1.362(5) . . yes C(57) H(56) 0.950 . . no C(58) C(59) 1.373(6) . . yes C(58) H(57) 0.951 . . no C(59) C(60) 1.391(5) . . yes C(59) H(58) 0.951 . . no C(60) C(61) 1.405(5) . . yes C(60) C(62) 1.502(6) . . yes C(61) C(66) 1.470(4) . . yes C(62) C(63) 1.526(6) . . yes C(62) H(59) 0.950 . . no C(62) H(60) 0.950 . . no C(63) C(64) 1.522(6) . . yes C(63) H(61) 0.952 . . no C(63) H(62) 0.949 . . no C(64) C(65) 1.528(6) . . yes C(64) H(63) 0.955 . . no C(64) H(64) 0.948 . . no C(65) C(66) 1.510(5) . . yes C(65) H(65) 0.951 . . no C(65) H(66) 0.951 . . no C(66) C(67) 1.338(5) . . yes C(67) C(68) 1.484(5) . . yes C(68) C(69) 1.372(6) . . yes C(68) C(73) 1.399(5) . . yes C(69) C(70) 1.381(5) . . yes C(69) H(67) 0.948 . . no C(70) C(71) 1.369(6) . . yes C(70) H(68) 0.950 . . no C(71) C(72) 1.366(7) . . yes C(71) H(69) 0.950 . . no C(72) C(73) 1.389(6) . . yes C(72) H(70) 0.950 . . no C(73) H(71) 0.949 . . no C(74) C(75) 1.508(5) . . yes C(74) H(72) 0.945 . . no C(74) H(73) 0.947 . . no C(74) H(74) 0.964 . . no C(75) C(76) 1.405(5) . . yes C(76) C(77) 1.380(6) . . yes C(76) H(75) 0.951 . . no C(77) C(78) 1.512(5) . . yes C(78) H(76) 0.953 . . no C(78) H(77) 0.953 . . no C(78) H(78) 0.943 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ir(1) O(2) 88.84(10) . . . yes O(1) Ir(1) N(1) 96.6(1) . . . yes O(1) Ir(1) N(2) 87.6(1) . . . yes O(1) Ir(1) C(11) 175.2(1) . . . yes O(1) Ir(1) C(28) 90.6(1) . . . yes O(2) Ir(1) N(1) 85.5(1) . . . yes O(2) Ir(1) N(2) 95.4(1) . . . yes O(2) Ir(1) C(11) 93.0(1) . . . yes O(2) Ir(1) C(28) 175.0(1) . . . yes N(1) Ir(1) N(2) 175.7(1) . . . yes N(1) Ir(1) C(11) 79.1(1) . . . yes N(1) Ir(1) C(28) 99.5(1) . . . yes N(2) Ir(1) C(11) 96.7(1) . . . yes N(2) Ir(1) C(28) 79.6(1) . . . yes C(11) Ir(1) C(28) 88.0(1) . . . yes O(3) Ir(2) O(4) 87.00(10) . . . yes O(3) Ir(2) N(3) 95.0(1) . . . yes O(3) Ir(2) N(4) 88.4(1) . . . yes O(3) Ir(2) C(50) 173.5(1) . . . yes O(3) Ir(2) C(67) 91.2(1) . . . yes O(4) Ir(2) N(3) 91.8(1) . . . yes O(4) Ir(2) N(4) 93.5(1) . . . yes O(4) Ir(2) C(50) 95.9(1) . . . yes O(4) Ir(2) C(67) 172.6(1) . . . yes N(3) Ir(2) N(4) 173.8(1) . . . yes N(3) Ir(2) C(50) 79.2(2) . . . yes N(3) Ir(2) C(67) 95.5(1) . . . yes N(4) Ir(2) C(50) 97.2(2) . . . yes N(4) Ir(2) C(67) 79.2(1) . . . yes C(50) Ir(2) C(67) 86.6(1) . . . yes Ir(1) O(1) C(36) 124.8(2) . . . yes Ir(1) O(2) C(38) 123.7(2) . . . yes Ir(2) O(3) C(75) 126.0(2) . . . yes Ir(2) O(4) C(77) 124.6(2) . . . yes Ir(1) N(1) C(1) 123.6(2) . . . yes Ir(1) N(1) C(5) 115.9(2) . . . yes C(1) N(1) C(5) 120.5(3) . . . yes Ir(1) N(2) C(18) 123.6(2) . . . yes Ir(1) N(2) C(22) 115.5(3) . . . yes C(18) N(2) C(22) 120.7(3) . . . yes Ir(2) N(3) C(40) 122.7(3) . . . yes Ir(2) N(3) C(44) 116.0(2) . . . yes C(40) N(3) C(44) 121.1(3) . . . yes Ir(2) N(4) C(57) 124.7(3) . . . yes Ir(2) N(4) C(61) 115.9(2) . . . yes C(57) N(4) C(61) 119.4(3) . . . yes N(1) C(1) C(2) 121.8(3) . . . yes N(1) C(1) H(1) 119.2 . . . no C(2) C(1) H(1) 119.0 . . . no C(1) C(2) C(3) 118.7(3) . . . yes C(1) C(2) H(2) 120.6 . . . no C(3) C(2) H(2) 120.7 . . . no C(2) C(3) C(4) 120.2(4) . . . yes C(2) C(3) H(3) 119.9 . . . no C(4) C(3) H(3) 119.9 . . . no C(3) C(4) C(5) 118.9(3) . . . yes C(3) C(4) C(6) 119.0(3) . . . yes C(5) C(4) C(6) 122.0(3) . . . yes N(1) C(5) C(4) 119.5(3) . . . yes N(1) C(5) C(10) 112.5(3) . . . yes C(4) C(5) C(10) 127.9(3) . . . yes C(4) C(6) C(7) 113.0(3) . . . yes C(4) C(6) H(4) 108.7 . . . no C(4) C(6) H(5) 108.8 . . . no C(7) C(6) H(4) 108.4 . . . no C(7) C(6) H(5) 108.3 . . . no H(4) C(6) H(5) 109.7 . . . no C(6) C(7) C(8) 114.6(3) . . . yes C(6) C(7) H(6) 108.0 . . . no C(6) C(7) H(7) 108.3 . . . no C(8) C(7) H(6) 108.0 . . . no C(8) C(7) H(7) 108.2 . . . no H(6) C(7) H(7) 109.6 . . . no C(7) C(8) C(9) 114.0(3) . . . yes C(7) C(8) H(8) 108.4 . . . no C(7) C(8) H(9) 108.2 . . . no C(9) C(8) H(8) 108.3 . . . no C(9) C(8) H(9) 108.5 . . . no H(8) C(8) H(9) 109.4 . . . no C(8) C(9) C(10) 116.0(3) . . . yes C(8) C(9) H(10) 107.8 . . . no C(8) C(9) H(11) 107.7 . . . no C(10) C(9) H(10) 107.8 . . . no C(10) C(9) H(11) 107.8 . . . no H(10) C(9) H(11) 109.7 . . . no C(5) C(10) C(9) 119.9(3) . . . yes C(5) C(10) C(11) 116.0(3) . . . yes C(9) C(10) C(11) 124.0(3) . . . yes Ir(1) C(11) C(10) 116.4(3) . . . yes Ir(1) C(11) C(12) 122.2(3) . . . yes C(10) C(11) C(12) 121.4(3) . . . yes C(11) C(12) C(13) 121.3(3) . . . yes C(11) C(12) C(17) 120.9(3) . . . yes C(13) C(12) C(17) 117.8(4) . . . yes C(12) C(13) C(14) 120.5(4) . . . yes C(12) C(13) H(12) 119.6 . . . no C(14) C(13) H(12) 119.9 . . . no C(13) C(14) C(15) 120.3(4) . . . yes C(13) C(14) H(13) 119.9 . . . no C(15) C(14) H(13) 119.8 . . . no C(14) C(15) C(16) 120.7(4) . . . yes C(14) C(15) H(14) 119.5 . . . no C(16) C(15) H(14) 119.9 . . . no C(15) C(16) C(17) 117.8(4) . . . yes C(15) C(16) H(15) 121.2 . . . no C(17) C(16) H(15) 121.0 . . . no C(12) C(17) C(16) 122.8(4) . . . yes C(12) C(17) H(16) 118.5 . . . no C(16) C(17) H(16) 118.7 . . . no N(2) C(18) C(19) 122.0(3) . . . yes N(2) C(18) H(17) 119.1 . . . no C(19) C(18) H(17) 119.0 . . . no C(18) C(19) C(20) 117.7(4) . . . yes C(18) C(19) H(18) 121.1 . . . no C(20) C(19) H(18) 121.1 . . . no C(19) C(20) C(21) 120.9(4) . . . yes C(19) C(20) H(19) 119.1 . . . no C(21) C(20) H(19) 120.0 . . . no C(20) C(21) C(22) 119.1(3) . . . yes C(20) C(21) C(23) 119.0(4) . . . yes C(22) C(21) C(23) 121.8(4) . . . yes N(2) C(22) C(21) 119.2(3) . . . yes N(2) C(22) C(27) 111.8(3) . . . yes C(21) C(22) C(27) 129.0(3) . . . yes C(21) C(23) C(24) 112.8(4) . . . yes C(21) C(23) H(20) 108.5 . . . no C(21) C(23) H(21) 108.7 . . . no C(24) C(23) H(20) 108.3 . . . no C(24) C(23) H(21) 108.7 . . . no H(20) C(23) H(21) 109.8 . . . no C(23) C(24) C(25) 114.6(3) . . . yes C(23) C(24) H(22) 107.9 . . . no C(23) C(24) H(23) 107.7 . . . no C(25) C(24) H(22) 108.7 . . . no C(25) C(24) H(23) 108.3 . . . no H(22) C(24) H(23) 109.5 . . . no C(24) C(25) C(26) 112.3(3) . . . yes C(24) C(25) H(24) 108.7 . . . no C(24) C(25) H(25) 108.8 . . . no C(26) C(25) H(24) 108.8 . . . no C(26) C(25) H(25) 108.9 . . . no H(24) C(25) H(25) 109.3 . . . no C(25) C(26) C(27) 115.5(3) . . . yes C(25) C(26) H(26) 108.0 . . . no C(25) C(26) H(27) 108.0 . . . no C(27) C(26) H(26) 108.0 . . . no C(27) C(26) H(27) 107.9 . . . no H(26) C(26) H(27) 109.5 . . . no C(22) C(27) C(26) 117.6(4) . . . yes C(22) C(27) C(28) 116.4(3) . . . yes C(26) C(27) C(28) 125.7(4) . . . yes Ir(1) C(28) C(27) 116.0(3) . . . yes Ir(1) C(28) C(29) 121.8(3) . . . yes C(27) C(28) C(29) 122.0(3) . . . yes C(28) C(29) C(30) 120.7(4) . . . yes C(28) C(29) C(34) 120.5(4) . . . yes C(30) C(29) C(34) 118.8(4) . . . yes C(29) C(30) C(31) 120.9(4) . . . yes C(29) C(30) H(28) 119.2 . . . no C(31) C(30) H(28) 119.9 . . . no C(30) C(31) C(32) 120.2(5) . . . yes C(30) C(31) H(29) 120.1 . . . no C(32) C(31) H(29) 119.8 . . . no C(31) C(32) C(33) 119.4(4) . . . yes C(31) C(32) H(30) 120.4 . . . no C(33) C(32) H(30) 120.2 . . . no C(32) C(33) C(34) 121.6(4) . . . yes C(32) C(33) H(31) 119.4 . . . no C(34) C(33) H(31) 119.0 . . . no C(29) C(34) C(33) 119.0(4) . . . yes C(29) C(34) H(32) 120.4 . . . no C(33) C(34) H(32) 120.5 . . . no C(36) C(35) H(33) 109.9 . . . no C(36) C(35) H(34) 110.3 . . . no C(36) C(35) H(35) 109.0 . . . no H(33) C(35) H(34) 110.2 . . . no H(33) C(35) H(35) 108.4 . . . no H(34) C(35) H(35) 108.9 . . . no O(1) C(36) C(35) 115.8(3) . . . yes O(1) C(36) C(37) 126.5(3) . . . yes C(35) C(36) C(37) 117.7(3) . . . yes C(36) C(37) C(38) 128.0(3) . . . yes C(36) C(37) H(36) 116.0 . . . no C(38) C(37) H(36) 116.0 . . . no O(2) C(38) C(37) 127.5(3) . . . yes O(2) C(38) C(39) 114.5(3) . . . yes C(37) C(38) C(39) 118.0(3) . . . yes C(38) C(39) H(37) 110.7 . . . no C(38) C(39) H(38) 109.7 . . . no C(38) C(39) H(39) 109.8 . . . no H(37) C(39) H(38) 109.3 . . . no H(37) C(39) H(39) 109.4 . . . no H(38) C(39) H(39) 107.9 . . . no N(3) C(40) C(41) 120.2(3) . . . yes N(3) C(40) H(40) 120.0 . . . no C(41) C(40) H(40) 119.8 . . . no C(40) C(41) C(42) 119.3(4) . . . yes C(40) C(41) H(41) 120.4 . . . no C(42) C(41) H(41) 120.3 . . . no C(41) C(42) C(43) 121.3(3) . . . yes C(41) C(42) H(42) 119.5 . . . no C(43) C(42) H(42) 119.2 . . . no C(42) C(43) C(44) 118.6(4) . . . yes C(42) C(43) C(45) 119.7(3) . . . yes C(44) C(43) C(45) 121.5(4) . . . yes N(3) C(44) C(43) 119.4(3) . . . yes N(3) C(44) C(49) 112.9(3) . . . yes C(43) C(44) C(49) 127.8(3) . . . yes C(43) C(45) C(46) 116.2(4) . . . yes C(43) C(45) H(43) 107.7 . . . no C(43) C(45) H(44) 107.7 . . . no C(46) C(45) H(43) 107.9 . . . no C(46) C(45) H(44) 107.8 . . . no H(43) C(45) H(44) 109.4 . . . no C(45) C(46) C(47) 116.1(4) . . . yes C(45) C(46) H(45) 107.7 . . . no C(45) C(46) H(46) 107.9 . . . no C(47) C(46) H(45) 107.6 . . . no C(47) C(46) H(46) 108.2 . . . no H(45) C(46) H(46) 109.2 . . . no C(46) C(47) C(48) 117.2(4) . . . yes C(46) C(47) H(47) 108.1 . . . no C(46) C(47) H(48) 107.5 . . . no C(48) C(47) H(47) 107.5 . . . no C(48) C(47) H(48) 107.1 . . . no H(47) C(47) H(48) 109.3 . . . no C(47) C(48) C(49) 116.8(4) . . . yes C(47) C(48) H(49) 107.7 . . . no C(47) C(48) H(50) 107.6 . . . no C(49) C(48) H(49) 107.7 . . . no C(49) C(48) H(50) 107.5 . . . no H(49) C(48) H(50) 109.5 . . . no C(44) C(49) C(48) 121.6(3) . . . yes C(44) C(49) C(50) 115.0(3) . . . yes C(48) C(49) C(50) 123.5(3) . . . yes Ir(2) C(50) C(49) 116.6(3) . . . yes Ir(2) C(50) C(51) 121.6(2) . . . yes C(49) C(50) C(51) 121.8(3) . . . yes C(50) C(51) C(52) 122.4(3) . . . yes C(50) C(51) C(56) 119.5(3) . . . yes C(52) C(51) C(56) 118.1(3) . . . yes C(51) C(52) C(53) 121.3(3) . . . yes C(51) C(52) H(51) 119.3 . . . no C(53) C(52) H(51) 119.4 . . . no C(52) C(53) C(54) 119.6(4) . . . yes C(52) C(53) H(52) 120.2 . . . no C(54) C(53) H(52) 120.3 . . . no C(53) C(54) C(55) 119.9(4) . . . yes C(53) C(54) H(53) 120.3 . . . no C(55) C(54) H(53) 119.7 . . . no C(54) C(55) C(56) 120.7(3) . . . yes C(54) C(55) H(54) 119.7 . . . no C(56) C(55) H(54) 119.6 . . . no C(51) C(56) C(55) 120.3(4) . . . yes C(51) C(56) H(55) 119.7 . . . no C(55) C(56) H(55) 120.0 . . . no N(4) C(57) C(58) 121.7(4) . . . yes N(4) C(57) H(56) 119.3 . . . no C(58) C(57) H(56) 119.0 . . . no C(57) C(58) C(59) 119.7(3) . . . yes C(57) C(58) H(57) 119.9 . . . no C(59) C(58) H(57) 120.3 . . . no C(58) C(59) C(60) 120.7(3) . . . yes C(58) C(59) H(58) 119.6 . . . no C(60) C(59) H(58) 119.7 . . . no C(59) C(60) C(61) 117.5(4) . . . yes C(59) C(60) C(62) 119.1(3) . . . yes C(61) C(60) C(62) 123.3(3) . . . yes N(4) C(61) C(60) 120.7(3) . . . yes N(4) C(61) C(66) 112.5(3) . . . yes C(60) C(61) C(66) 126.6(4) . . . yes C(60) C(62) C(63) 113.2(3) . . . yes C(60) C(62) H(59) 108.6 . . . no C(60) C(62) H(60) 108.6 . . . no C(63) C(62) H(59) 108.4 . . . no C(63) C(62) H(60) 108.6 . . . no H(59) C(62) H(60) 109.5 . . . no C(62) C(63) C(64) 114.0(4) . . . yes C(62) C(63) H(61) 108.1 . . . no C(62) C(63) H(62) 108.3 . . . no C(64) C(63) H(61) 108.6 . . . no C(64) C(63) H(62) 108.5 . . . no H(61) C(63) H(62) 109.4 . . . no C(63) C(64) C(65) 113.1(3) . . . yes C(63) C(64) H(63) 108.6 . . . no C(63) C(64) H(64) 108.8 . . . no C(65) C(64) H(63) 108.4 . . . no C(65) C(64) H(64) 108.7 . . . no H(63) C(64) H(64) 109.2 . . . no C(64) C(65) C(66) 116.1(3) . . . yes C(64) C(65) H(65) 107.9 . . . no C(64) C(65) H(66) 107.8 . . . no C(66) C(65) H(65) 107.8 . . . no C(66) C(65) H(66) 107.8 . . . no H(65) C(65) H(66) 109.3 . . . no C(61) C(66) C(65) 118.8(3) . . . yes C(61) C(66) C(67) 115.4(3) . . . yes C(65) C(66) C(67) 125.2(3) . . . yes Ir(2) C(67) C(66) 116.8(3) . . . yes Ir(2) C(67) C(68) 122.5(3) . . . yes C(66) C(67) C(68) 120.6(4) . . . yes C(67) C(68) C(69) 121.6(3) . . . yes C(67) C(68) C(73) 120.4(4) . . . yes C(69) C(68) C(73) 118.0(3) . . . yes C(68) C(69) C(70) 122.2(4) . . . yes C(68) C(69) H(67) 118.9 . . . no C(70) C(69) H(67) 118.8 . . . no C(69) C(70) C(71) 119.1(4) . . . yes C(69) C(70) H(68) 120.6 . . . no C(71) C(70) H(68) 120.3 . . . no C(70) C(71) C(72) 120.0(4) . . . yes C(70) C(71) H(69) 120.1 . . . no C(72) C(71) H(69) 119.9 . . . no C(71) C(72) C(73) 121.0(4) . . . yes C(71) C(72) H(70) 119.4 . . . no C(73) C(72) H(70) 119.6 . . . no C(68) C(73) C(72) 119.4(4) . . . yes C(68) C(73) H(71) 120.3 . . . no C(72) C(73) H(71) 120.3 . . . no C(75) C(74) H(72) 110.1 . . . no C(75) C(74) H(73) 110.1 . . . no C(75) C(74) H(74) 109.1 . . . no H(72) C(74) H(73) 110.2 . . . no H(72) C(74) H(74) 108.8 . . . no H(73) C(74) H(74) 108.6 . . . no O(3) C(75) C(74) 116.5(3) . . . yes O(3) C(75) C(76) 125.2(3) . . . yes C(74) C(75) C(76) 118.2(4) . . . yes C(75) C(76) C(77) 128.6(4) . . . yes C(75) C(76) H(75) 115.6 . . . no C(77) C(76) H(75) 115.8 . . . no O(4) C(77) C(76) 127.3(3) . . . yes O(4) C(77) C(78) 115.6(3) . . . yes C(76) C(77) C(78) 117.1(4) . . . yes C(77) C(78) H(76) 109.3 . . . no C(77) C(78) H(77) 109.2 . . . no C(77) C(78) H(78) 109.8 . . . no H(76) C(78) H(77) 109.0 . . . no H(76) C(78) H(78) 109.8 . . . no H(77) C(78) H(78) 109.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) O(1) C(36) C(35) -179.8(2) . . . . yes Ir(1) O(1) C(36) C(37) -0.6(6) . . . . yes Ir(1) O(2) C(38) C(37) -9.4(6) . . . . yes Ir(1) O(2) C(38) C(39) 171.4(3) . . . . yes Ir(1) N(1) C(1) C(2) -176.3(2) . . . . yes Ir(1) N(1) C(5) C(4) -178.8(2) . . . . yes Ir(1) N(1) C(5) C(10) 4.3(3) . . . . yes Ir(1) N(2) C(18) C(19) 174.5(3) . . . . yes Ir(1) N(2) C(22) C(21) -170.3(2) . . . . yes Ir(1) N(2) C(22) C(27) 9.0(4) . . . . yes Ir(1) C(11) C(10) C(5) 0.7(4) . . . . yes Ir(1) C(11) C(10) C(9) -174.9(3) . . . . yes Ir(1) C(11) C(12) C(13) 71.1(4) . . . . yes Ir(1) C(11) C(12) C(17) -108.4(4) . . . . yes Ir(1) C(28) C(27) C(22) 3.8(4) . . . . yes Ir(1) C(28) C(27) C(26) -170.0(3) . . . . yes Ir(1) C(28) C(29) C(30) -117.1(4) . . . . yes Ir(1) C(28) C(29) C(34) 61.0(4) . . . . yes Ir(2) O(3) C(75) C(74) 178.6(2) . . . . yes Ir(2) O(3) C(75) C(76) -5.2(5) . . . . yes Ir(2) O(4) C(77) C(76) 7.9(5) . . . . yes Ir(2) O(4) C(77) C(78) -171.8(2) . . . . yes Ir(2) N(3) C(40) C(41) 173.9(3) . . . . yes Ir(2) N(3) C(44) C(43) -172.5(3) . . . . yes Ir(2) N(3) C(44) C(49) 6.9(4) . . . . yes Ir(2) N(4) C(57) C(58) 175.6(3) . . . . yes Ir(2) N(4) C(61) C(60) -173.3(3) . . . . yes Ir(2) N(4) C(61) C(66) 2.3(4) . . . . yes Ir(2) C(50) C(49) C(44) -2.7(4) . . . . yes Ir(2) C(50) C(49) C(48) 177.3(3) . . . . yes Ir(2) C(50) C(51) C(52) -109.8(4) . . . . yes Ir(2) C(50) C(51) C(56) 69.5(4) . . . . yes Ir(2) C(67) C(66) C(61) 2.8(4) . . . . yes Ir(2) C(67) C(66) C(65) -167.8(3) . . . . yes Ir(2) C(67) C(68) C(69) -106.1(4) . . . . yes Ir(2) C(67) C(68) C(73) 76.7(4) . . . . yes O(1) Ir(1) O(2) C(38) 8.5(3) . . . . yes O(1) Ir(1) N(1) C(1) -8.5(3) . . . . yes O(1) Ir(1) N(1) C(5) 174.6(2) . . . . yes O(1) Ir(1) N(2) C(18) 87.9(3) . . . . yes O(1) Ir(1) N(2) C(22) -96.7(2) . . . . yes O(1) Ir(1) C(11) C(10) -25(1) . . . . yes O(1) Ir(1) C(11) C(12) 152(1) . . . . yes O(1) Ir(1) C(28) C(27) 88.3(3) . . . . yes O(1) Ir(1) C(28) C(29) -87.4(3) . . . . yes O(1) C(36) C(37) C(38) 3.2(7) . . . . yes O(2) Ir(1) O(1) C(36) -3.9(3) . . . . yes O(2) Ir(1) N(1) C(1) 79.8(3) . . . . yes O(2) Ir(1) N(1) C(5) -97.1(2) . . . . yes O(2) Ir(1) N(2) C(18) -0.7(3) . . . . yes O(2) Ir(1) N(2) C(22) 174.7(2) . . . . yes O(2) Ir(1) C(11) C(10) 86.1(3) . . . . yes O(2) Ir(1) C(11) C(12) -95.1(3) . . . . yes O(2) Ir(1) C(28) C(27) 4(1) . . . . yes O(2) Ir(1) C(28) C(29) -170(1) . . . . yes O(2) C(38) C(37) C(36) 2.6(8) . . . . yes O(3) Ir(2) O(4) C(77) -11.2(3) . . . . yes O(3) Ir(2) N(3) C(40) -4.4(3) . . . . yes O(3) Ir(2) N(3) C(44) 170.6(3) . . . . yes O(3) Ir(2) N(4) C(57) 87.8(3) . . . . yes O(3) Ir(2) N(4) C(61) -92.2(3) . . . . yes O(3) Ir(2) C(50) C(49) -21(1) . . . . yes O(3) Ir(2) C(50) C(51) 155.7(10) . . . . yes O(3) Ir(2) C(67) C(66) 87.0(3) . . . . yes O(3) Ir(2) C(67) C(68) -96.0(3) . . . . yes O(3) C(75) C(76) C(77) -3.5(7) . . . . yes O(4) Ir(2) O(3) C(75) 10.0(3) . . . . yes O(4) Ir(2) N(3) C(40) 82.7(3) . . . . yes O(4) Ir(2) N(3) C(44) -102.2(3) . . . . yes O(4) Ir(2) N(4) C(57) 0.9(3) . . . . yes O(4) Ir(2) N(4) C(61) -179.1(3) . . . . yes O(4) Ir(2) C(50) C(49) 95.6(3) . . . . yes O(4) Ir(2) C(50) C(51) -87.6(3) . . . . yes O(4) Ir(2) C(67) C(66) 11(1) . . . . yes O(4) Ir(2) C(67) C(68) -171.6(8) . . . . yes O(4) C(77) C(76) C(75) 1.9(7) . . . . yes N(1) Ir(1) O(1) C(36) 81.4(3) . . . . yes N(1) Ir(1) O(2) C(38) -88.2(3) . . . . yes N(1) Ir(1) N(2) C(18) -102(1) . . . . yes N(1) Ir(1) N(2) C(22) 72(1) . . . . yes N(1) Ir(1) C(11) C(10) 1.3(3) . . . . yes N(1) Ir(1) C(11) C(12) -179.9(3) . . . . yes N(1) Ir(1) C(28) C(27) -174.9(3) . . . . yes N(1) Ir(1) C(28) C(29) 9.4(3) . . . . yes N(1) C(1) C(2) C(3) -5.0(5) . . . . yes N(1) C(5) C(4) C(3) -4.0(5) . . . . yes N(1) C(5) C(4) C(6) 171.7(3) . . . . yes N(1) C(5) C(10) C(9) 172.5(3) . . . . yes N(1) C(5) C(10) C(11) -3.3(4) . . . . yes N(2) Ir(1) O(1) C(36) -99.4(3) . . . . yes N(2) Ir(1) O(2) C(38) 96.0(3) . . . . yes N(2) Ir(1) N(1) C(1) -177(1) . . . . yes N(2) Ir(1) N(1) C(5) 5(1) . . . . yes N(2) Ir(1) C(11) C(10) -178.1(3) . . . . yes N(2) Ir(1) C(11) C(12) 0.7(3) . . . . yes N(2) Ir(1) C(28) C(27) 0.9(3) . . . . yes N(2) Ir(1) C(28) C(29) -174.8(3) . . . . yes N(2) C(18) C(19) C(20) -3.5(5) . . . . yes N(2) C(22) C(21) C(20) -5.7(5) . . . . yes N(2) C(22) C(21) C(23) 170.5(3) . . . . yes N(2) C(22) C(27) C(26) 166.0(3) . . . . yes N(2) C(22) C(27) C(28) -8.4(4) . . . . yes N(3) Ir(2) O(3) C(75) 101.6(3) . . . . yes N(3) Ir(2) O(4) C(77) -106.1(3) . . . . yes N(3) Ir(2) N(4) C(57) -148.6(10) . . . . yes N(3) Ir(2) N(4) C(61) 31(1) . . . . yes N(3) Ir(2) C(50) C(49) 4.9(3) . . . . yes N(3) Ir(2) C(50) C(51) -178.3(3) . . . . yes N(3) Ir(2) C(67) C(66) -177.9(3) . . . . yes N(3) Ir(2) C(67) C(68) -0.8(3) . . . . yes N(3) C(40) C(41) C(42) -1.6(6) . . . . yes N(3) C(44) C(43) C(42) -1.7(6) . . . . yes N(3) C(44) C(43) C(45) 175.0(4) . . . . yes N(3) C(44) C(49) C(48) 177.2(3) . . . . yes N(3) C(44) C(49) C(50) -2.8(5) . . . . yes N(4) Ir(2) O(3) C(75) -83.6(3) . . . . yes N(4) Ir(2) O(4) C(77) 77.0(3) . . . . yes N(4) Ir(2) N(3) C(40) -127.8(10) . . . . yes N(4) Ir(2) N(3) C(44) 47(1) . . . . yes N(4) Ir(2) C(50) C(49) -170.1(3) . . . . yes N(4) Ir(2) C(50) C(51) 6.7(3) . . . . yes N(4) Ir(2) C(67) C(66) -1.2(3) . . . . yes N(4) Ir(2) C(67) C(68) 175.9(3) . . . . yes N(4) C(57) C(58) C(59) 0.6(6) . . . . yes N(4) C(61) C(60) C(59) -5.1(5) . . . . yes N(4) C(61) C(60) C(62) 170.8(4) . . . . yes N(4) C(61) C(66) C(65) 167.9(3) . . . . yes N(4) C(61) C(66) C(67) -3.3(5) . . . . yes C(1) N(1) Ir(1) C(11) 173.7(3) . . . . yes C(1) N(1) Ir(1) C(28) -100.2(3) . . . . yes C(1) N(1) C(5) C(4) 4.2(5) . . . . yes C(1) N(1) C(5) C(10) -172.6(3) . . . . yes C(1) C(2) C(3) C(4) 5.1(5) . . . . yes C(2) C(1) N(1) C(5) 0.4(5) . . . . yes C(2) C(3) C(4) C(5) -0.7(5) . . . . yes C(2) C(3) C(4) C(6) -176.5(3) . . . . yes C(3) C(4) C(5) C(10) 172.3(3) . . . . yes C(3) C(4) C(6) C(7) 131.6(4) . . . . yes C(4) C(5) C(10) C(9) -4.0(5) . . . . yes C(4) C(5) C(10) C(11) -179.8(3) . . . . yes C(4) C(6) C(7) C(8) 83.3(4) . . . . yes C(5) N(1) Ir(1) C(11) -3.2(2) . . . . yes C(5) N(1) Ir(1) C(28) 82.9(2) . . . . yes C(5) C(4) C(6) C(7) -44.0(4) . . . . yes C(5) C(10) C(9) C(8) 66.3(4) . . . . yes C(5) C(10) C(11) C(12) -178.1(3) . . . . yes C(6) C(4) C(5) C(10) -12.1(5) . . . . yes C(6) C(7) C(8) C(9) -27.1(5) . . . . yes C(7) C(8) C(9) C(10) -54.8(5) . . . . yes C(8) C(9) C(10) C(11) -118.3(4) . . . . yes C(9) C(10) C(11) C(12) 6.3(5) . . . . yes C(10) C(11) Ir(1) C(28) -98.9(3) . . . . yes C(10) C(11) C(12) C(13) -110.1(4) . . . . yes C(10) C(11) C(12) C(17) 70.4(5) . . . . yes C(11) Ir(1) O(1) C(36) 108(1) . . . . yes C(11) Ir(1) O(2) C(38) -167.0(3) . . . . yes C(11) Ir(1) N(2) C(18) -94.3(3) . . . . yes C(11) Ir(1) N(2) C(22) 81.0(2) . . . . yes C(11) Ir(1) C(28) C(27) -96.3(3) . . . . yes C(11) Ir(1) C(28) C(29) 88.0(3) . . . . yes C(11) C(12) C(13) C(14) 178.9(4) . . . . yes C(11) C(12) C(17) C(16) -178.7(4) . . . . yes C(12) C(11) Ir(1) C(28) 80.0(3) . . . . yes C(12) C(13) C(14) C(15) 0.4(6) . . . . yes C(12) C(17) C(16) C(15) -0.6(6) . . . . yes C(13) C(12) C(17) C(16) 1.7(6) . . . . yes C(13) C(14) C(15) C(16) 0.8(6) . . . . yes C(14) C(13) C(12) C(17) -1.6(6) . . . . yes C(14) C(15) C(16) C(17) -0.6(6) . . . . yes C(18) N(2) Ir(1) C(28) 179.0(3) . . . . yes C(18) N(2) C(22) C(21) 5.2(5) . . . . yes C(18) N(2) C(22) C(27) -175.5(3) . . . . yes C(18) C(19) C(20) C(21) 2.9(5) . . . . yes C(19) C(18) N(2) C(22) -0.6(5) . . . . yes C(19) C(20) C(21) C(22) 1.6(5) . . . . yes C(19) C(20) C(21) C(23) -174.6(3) . . . . yes C(20) C(21) C(22) C(27) 175.2(3) . . . . yes C(20) C(21) C(23) C(24) 136.1(4) . . . . yes C(21) C(22) C(27) C(26) -14.9(5) . . . . yes C(21) C(22) C(27) C(28) 170.8(3) . . . . yes C(21) C(23) C(24) C(25) 85.5(4) . . . . yes C(22) N(2) Ir(1) C(28) -5.7(2) . . . . yes C(22) C(21) C(23) C(24) -40.1(5) . . . . yes C(22) C(27) C(26) C(25) 74.0(5) . . . . yes C(22) C(27) C(28) C(29) 179.5(3) . . . . yes C(23) C(21) C(22) C(27) -8.7(6) . . . . yes C(23) C(24) C(25) C(26) -35.3(5) . . . . yes C(24) C(25) C(26) C(27) -51.0(5) . . . . yes C(25) C(26) C(27) C(28) -112.3(4) . . . . yes C(26) C(27) C(28) C(29) 5.7(6) . . . . yes C(27) C(28) C(29) C(30) 67.5(5) . . . . yes C(27) C(28) C(29) C(34) -114.4(4) . . . . yes C(28) Ir(1) O(1) C(36) -178.9(3) . . . . yes C(28) Ir(1) O(2) C(38) 91(1) . . . . yes C(28) C(29) C(30) C(31) -179.7(4) . . . . yes C(28) C(29) C(34) C(33) 178.4(4) . . . . yes C(29) C(30) C(31) C(32) -0.5(8) . . . . yes C(29) C(34) C(33) C(32) 3.2(7) . . . . yes C(30) C(29) C(34) C(33) -3.4(6) . . . . yes C(30) C(31) C(32) C(33) 0.1(8) . . . . yes C(31) C(30) C(29) C(34) 2.2(7) . . . . yes C(31) C(32) C(33) C(34) -1.4(7) . . . . yes C(35) C(36) C(37) C(38) -177.6(4) . . . . yes C(36) C(37) C(38) C(39) -178.2(4) . . . . yes C(40) N(3) Ir(2) C(50) 178.4(3) . . . . yes C(40) N(3) Ir(2) C(67) -96.1(3) . . . . yes C(40) N(3) C(44) C(43) 2.6(5) . . . . yes C(40) N(3) C(44) C(49) -178.0(3) . . . . yes C(40) C(41) C(42) C(43) 2.5(7) . . . . yes C(41) C(40) N(3) C(44) -0.9(6) . . . . yes C(41) C(42) C(43) C(44) -0.9(6) . . . . yes C(41) C(42) C(43) C(45) -177.6(4) . . . . yes C(42) C(43) C(44) C(49) 179.0(4) . . . . yes C(42) C(43) C(45) C(46) -121.0(4) . . . . yes C(43) C(44) C(49) C(48) -3.4(6) . . . . yes C(43) C(44) C(49) C(50) 176.6(4) . . . . yes C(43) C(45) C(46) C(47) -64.2(6) . . . . yes C(44) N(3) Ir(2) C(50) -6.5(3) . . . . yes C(44) N(3) Ir(2) C(67) 79.0(3) . . . . yes C(44) C(43) C(45) C(46) 62.3(6) . . . . yes C(44) C(49) C(48) C(47) -50.3(5) . . . . yes C(44) C(49) C(50) C(51) -179.5(3) . . . . yes C(45) C(43) C(44) C(49) -4.3(6) . . . . yes C(45) C(46) C(47) C(48) -8.6(7) . . . . yes C(46) C(47) C(48) C(49) 71.6(5) . . . . yes C(47) C(48) C(49) C(50) 129.7(4) . . . . yes C(48) C(49) C(50) C(51) 0.5(6) . . . . yes C(49) C(50) Ir(2) C(67) -91.4(3) . . . . yes C(49) C(50) C(51) C(52) 66.9(5) . . . . yes C(49) C(50) C(51) C(56) -113.8(4) . . . . yes C(50) Ir(2) O(3) C(75) 127(1) . . . . yes C(50) Ir(2) O(4) C(77) 174.6(3) . . . . yes C(50) Ir(2) N(4) C(57) -95.6(3) . . . . yes C(50) Ir(2) N(4) C(61) 84.4(3) . . . . yes C(50) Ir(2) C(67) C(66) -99.1(3) . . . . yes C(50) Ir(2) C(67) C(68) 77.9(3) . . . . yes C(50) C(51) C(52) C(53) 179.2(4) . . . . yes C(50) C(51) C(56) C(55) -179.2(3) . . . . yes C(51) C(50) Ir(2) C(67) 85.4(3) . . . . yes C(51) C(52) C(53) C(54) 0.8(6) . . . . yes C(51) C(56) C(55) C(54) -0.8(6) . . . . yes C(52) C(51) C(56) C(55) 0.1(5) . . . . yes C(52) C(53) C(54) C(55) -1.4(6) . . . . yes C(53) C(52) C(51) C(56) -0.1(6) . . . . yes C(53) C(54) C(55) C(56) 1.4(6) . . . . yes C(57) N(4) Ir(2) C(67) 179.3(3) . . . . yes C(57) N(4) C(61) C(60) 6.7(5) . . . . yes C(57) N(4) C(61) C(66) -177.7(3) . . . . yes C(57) C(58) C(59) C(60) 0.9(6) . . . . yes C(58) C(57) N(4) C(61) -4.4(5) . . . . yes C(58) C(59) C(60) C(61) 1.4(6) . . . . yes C(58) C(59) C(60) C(62) -174.8(4) . . . . yes C(59) C(60) C(61) C(66) 179.9(4) . . . . yes C(59) C(60) C(62) C(63) 131.4(4) . . . . yes C(60) C(61) C(66) C(65) -16.7(6) . . . . yes C(60) C(61) C(66) C(67) 172.0(4) . . . . yes C(60) C(62) C(63) C(64) 85.9(5) . . . . yes C(61) N(4) Ir(2) C(67) -0.7(3) . . . . yes C(61) C(60) C(62) C(63) -44.4(5) . . . . yes C(61) C(66) C(65) C(64) 72.9(4) . . . . yes C(61) C(66) C(67) C(68) -174.3(3) . . . . yes C(62) C(60) C(61) C(66) -4.2(6) . . . . yes C(62) C(63) C(64) C(65) -33.9(5) . . . . yes C(63) C(64) C(65) C(66) -50.7(5) . . . . yes C(64) C(65) C(66) C(67) -116.8(4) . . . . yes C(65) C(66) C(67) C(68) 15.1(6) . . . . yes C(66) C(67) C(68) C(69) 70.8(5) . . . . yes C(66) C(67) C(68) C(73) -106.4(5) . . . . yes C(67) Ir(2) O(3) C(75) -162.8(3) . . . . yes C(67) Ir(2) O(4) C(77) 64.7(10) . . . . yes C(67) C(68) C(69) C(70) -177.6(4) . . . . yes C(67) C(68) C(73) C(72) 175.7(4) . . . . yes C(68) C(69) C(70) C(71) 3.7(8) . . . . yes C(68) C(73) C(72) C(71) 0.2(8) . . . . yes C(69) C(68) C(73) C(72) -1.6(7) . . . . yes C(69) C(70) C(71) C(72) -5.1(8) . . . . yes C(70) C(69) C(68) C(73) -0.4(7) . . . . yes C(70) C(71) C(72) C(73) 3.2(9) . . . . yes C(74) C(75) C(76) C(77) 172.5(4) . . . . yes C(75) C(76) C(77) C(78) -178.3(4) . . . . yes C(75) C(76) C(77) C(78) -178.3(4) . . . . 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 O(4) C(35) 3.410(6) . 2_565 ? O(4) C(37) 3.533(5) . 2_565 ? C(2) C(55) 3.479(7) . 2_565 ? C(2) C(6) 3.585(6) . 2_566 ? C(2) C(54) 3.589(7) . 2_565 ? C(3) C(3) 3.317(8) . 2_566 ? C(3) C(58) 3.573(6) . 1_656 ? C(4) C(59) 3.443(6) . 1_656 ? C(5) C(59) 3.432(6) . 1_656 ? C(18) C(20) 3.521(5) . 2_555 ? C(19) C(21) 3.360(5) . 2_555 ? C(19) C(20) 3.516(5) . 2_555 ? C(19) C(22) 3.558(5) . 2_555 ? C(25) C(73) 3.573(7) . 2_455 ? C(39) C(54) 3.465(7) . 1_656 ? C(55) C(58) 3.563(5) . 2_464 ? #===END #------------------------------------------------------------------------------ data_5 _database_code_depnum_ccdc_archive 'CCDC 616853' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C27 H31 Ir N2 O2 ' _chemical_formula_moiety 'C27 H31 Ir N2 O2 ' _chemical_formula_weight 607.77 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.89(1) _cell_length_b 11.24(1) _cell_length_c 11.79(1) _cell_angle_alpha 68.15(3) _cell_angle_beta 87.50(4) _cell_angle_gamma 70.81(3) _cell_volume 1143(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11163 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.880 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.097 _exptl_absorpt_correction_T_max 0.250 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11223 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9910 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9910 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5198 _reflns_number_gt 4939 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0513 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5198 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 1.61 _refine_diff_density_min -1.07 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.26212(1) 0.200680(8) 0.235785(8) 0.01714(3) Uani 1.00 d . . . O(1) O 0.3754(2) 0.2683(2) 0.3388(2) 0.0255(5) Uani 1.00 d . . . O(2) O 0.0658(2) 0.3411(2) 0.2625(2) 0.0219(5) Uani 1.00 d . . . N(1) N 0.2972(3) 0.3408(2) 0.0799(2) 0.0185(6) Uani 1.00 d . . . N(2) N 0.2356(3) 0.0473(2) 0.3855(2) 0.0195(6) Uani 1.00 d . . . C(1) C 0.2120(3) 0.4725(3) 0.0244(3) 0.0235(7) Uani 1.00 d . . . C(2) C 0.2450(3) 0.5607(3) -0.0802(3) 0.0260(7) Uani 1.00 d . . . C(3) C 0.3742(3) 0.5149(3) -0.1287(2) 0.0237(7) Uani 1.00 d . . . C(4) C 0.4623(3) 0.3797(3) -0.0753(2) 0.0203(7) Uani 1.00 d . . . C(5) C 0.5986(3) 0.3220(3) -0.1274(3) 0.0255(7) Uani 1.00 d . . . C(6) C 0.7030(3) 0.1926(3) -0.0306(3) 0.0282(7) Uani 1.00 d . . . C(7) C 0.6307(3) 0.0888(3) 0.0357(2) 0.0213(7) Uani 1.00 d . . . C(8) C 0.4998(3) 0.1491(2) 0.0924(2) 0.0184(6) Uani 1.00 d . . . C(9) C 0.4207(3) 0.2934(3) 0.0296(2) 0.0188(6) Uani 1.00 d . . . C(10) C 0.4405(3) 0.0841(3) 0.1928(2) 0.0178(6) Uani 1.00 d . . . C(11) C 0.5025(3) -0.0673(3) 0.2630(2) 0.0231(7) Uani 1.00 d . . . C(12) C 0.2992(3) 0.0028(3) 0.4997(2) 0.0242(7) Uani 1.00 d . . . C(13) C 0.2777(3) -0.1043(3) 0.5956(2) 0.0292(7) Uani 1.00 d . . . C(14) C 0.1894(3) -0.1689(3) 0.5728(3) 0.0277(7) Uani 1.00 d . . . C(15) C 0.1270(3) -0.1274(3) 0.4548(2) 0.0227(7) Uani 1.00 d . . . C(16) C 0.0374(3) -0.1974(3) 0.4236(3) 0.0267(7) Uani 1.00 d . . . C(17) C 0.0382(3) -0.1792(3) 0.2879(3) 0.0282(8) Uani 1.00 d . . . C(18) C -0.0032(3) -0.0278(3) 0.2052(2) 0.0232(7) Uani 1.00 d . . . C(19) C 0.0968(3) 0.0357(2) 0.2344(2) 0.0184(6) Uani 1.00 d . . . C(20) C 0.1515(3) -0.0164(2) 0.3620(2) 0.0186(6) Uani 1.00 d . . . C(21) C 0.1447(3) 0.1342(3) 0.1569(2) 0.0174(6) Uani 1.00 d . . . C(22) C 0.1058(3) 0.1966(3) 0.0198(2) 0.0202(6) Uani 1.00 d . . . C(23) C 0.4199(3) 0.3919(3) 0.4482(3) 0.0278(8) Uani 1.00 d . . . C(24) C 0.3180(3) 0.3619(3) 0.3794(2) 0.0226(7) Uani 1.00 d . . . C(25) C 0.1712(3) 0.4378(3) 0.3669(2) 0.0231(7) Uani 1.00 d . . . C(26) C 0.0571(3) 0.4266(2) 0.3110(2) 0.0193(6) Uani 1.00 d . . . C(27) C -0.0922(3) 0.5244(3) 0.3055(2) 0.0230(7) Uani 1.00 d . . . H(1) H 0.1256 0.5046 0.0595 0.0280 Uiso 1.00 calc . . . H(2) H 0.1815 0.6516 -0.1188 0.0312 Uiso 1.00 calc . . . H(3) H 0.4021 0.5759 -0.1982 0.0285 Uiso 1.00 calc . . . H(4) H 0.7383 0.2173 0.0281 0.0338 Uiso 1.00 calc . . . H(5) H 0.6447 0.3883 -0.1575 0.0307 Uiso 1.00 calc . . . H(6) H 0.7803 0.1530 -0.0698 0.0338 Uiso 1.00 calc . . . H(7) H 0.5750 0.3002 -0.1927 0.0307 Uiso 1.00 calc . . . H(8) H 0.6972 0.0141 0.0986 0.0257 Uiso 1.00 calc . . . H(9) H 0.6027 0.0579 -0.0212 0.0257 Uiso 1.00 calc . . . H(10) H 0.5861 -0.1042 0.2277 0.0276 Uiso 1.00 calc . . . H(11) H 0.4332 -0.1080 0.2595 0.0276 Uiso 1.00 calc . . . H(12) H 0.5270 -0.0849 0.3461 0.0276 Uiso 1.00 calc . . . H(13) H 0.3600 0.0466 0.5146 0.0288 Uiso 1.00 calc . . . H(14) H 0.3223 -0.1336 0.6755 0.0352 Uiso 1.00 calc . . . H(15) H 0.1717 -0.2414 0.6380 0.0334 Uiso 1.00 calc . . . H(16) H -0.0587 -0.1604 0.4405 0.0321 Uiso 1.00 calc . . . H(17) H 0.0744 -0.2919 0.4729 0.0321 Uiso 1.00 calc . . . H(18) H -0.0288 -0.2153 0.2693 0.0336 Uiso 1.00 calc . . . H(19) H 0.1318 -0.2266 0.2724 0.0336 Uiso 1.00 calc . . . H(20) H -0.0988 0.0181 0.2180 0.0277 Uiso 1.00 calc . . . H(21) H 0.0009 -0.0190 0.1221 0.0277 Uiso 1.00 calc . . . H(22) H 0.0518 0.2910 -0.0044 0.0242 Uiso 1.00 calc . . . H(23) H 0.1920 0.1874 -0.0215 0.0242 Uiso 1.00 calc . . . H(24) H 0.0515 0.1521 -0.0019 0.0242 Uiso 1.00 calc . . . H(25) H -0.1586 0.4764 0.3236 0.0275 Uiso 1.00 calc . . . H(26) H -0.0939 0.5641 0.3642 0.0275 Uiso 1.00 calc . . . H(27) H -0.1179 0.5937 0.2259 0.0275 Uiso 1.00 calc . . . H(28) H 0.1463 0.5059 0.4010 0.0277 Uiso 1.00 calc . . . H(29) H 0.4035 0.4878 0.4161 0.0336 Uiso 1.00 calc . . . H(30) H 0.4082 0.3615 0.5322 0.0336 Uiso 1.00 calc . . . H(31) H 0.5176 0.3470 0.4357 0.0336 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) 0.01902(7) 0.01511(6) 0.01664(6) -0.00359(5) 0.00092(4) -0.00710(5) O(1) 0.025(1) 0.0246(10) 0.028(1) -0.0048(9) 0.0005(9) -0.0134(9) O(2) 0.022(1) 0.0213(9) 0.0230(10) -0.0043(8) 0.0022(8) -0.0113(8) N(1) 0.020(1) 0.014(1) 0.020(1) -0.0027(9) 0.0000(10) -0.0075(9) N(2) 0.022(1) 0.020(1) 0.015(1) -0.0027(10) 0.0016(9) -0.0076(9) C(1) 0.025(1) 0.017(1) 0.025(1) -0.002(1) 0.001(1) -0.009(1) C(2) 0.031(2) 0.015(1) 0.026(1) -0.003(1) -0.003(1) -0.006(1) C(3) 0.030(2) 0.021(1) 0.020(1) -0.010(1) -0.001(1) -0.006(1) C(4) 0.022(1) 0.021(1) 0.019(1) -0.009(1) 0.000(1) -0.008(1) C(5) 0.027(2) 0.024(1) 0.026(1) -0.012(1) 0.006(1) -0.007(1) C(6) 0.020(1) 0.028(1) 0.032(2) -0.006(1) 0.005(1) -0.009(1) C(7) 0.019(1) 0.020(1) 0.023(1) -0.004(1) 0.000(1) -0.009(1) C(8) 0.018(1) 0.018(1) 0.021(1) -0.005(1) -0.001(1) -0.009(1) C(9) 0.020(1) 0.019(1) 0.021(1) -0.007(1) 0.000(1) -0.010(1) C(10) 0.019(1) 0.014(1) 0.017(1) -0.002(1) -0.003(1) -0.004(1) C(11) 0.027(2) 0.019(1) 0.021(1) -0.006(1) 0.002(1) -0.008(1) C(12) 0.028(2) 0.026(1) 0.018(1) -0.004(1) -0.001(1) -0.011(1) C(13) 0.031(2) 0.029(1) 0.018(1) 0.000(1) -0.001(1) -0.007(1) C(14) 0.032(2) 0.022(1) 0.019(1) -0.001(1) 0.004(1) -0.004(1) C(15) 0.024(1) 0.020(1) 0.021(1) -0.003(1) 0.006(1) -0.007(1) C(16) 0.030(2) 0.022(1) 0.024(1) -0.011(1) 0.007(1) -0.002(1) C(17) 0.037(2) 0.024(1) 0.027(1) -0.017(1) 0.006(1) -0.008(1) C(18) 0.025(1) 0.020(1) 0.022(1) -0.009(1) 0.002(1) -0.005(1) C(19) 0.019(1) 0.018(1) 0.016(1) -0.004(1) 0.001(1) -0.007(1) C(20) 0.019(1) 0.016(1) 0.017(1) -0.003(1) 0.003(1) -0.006(1) C(21) 0.017(1) 0.014(1) 0.018(1) 0.001(1) 0.000(1) -0.007(1) C(22) 0.024(1) 0.018(1) 0.017(1) -0.007(1) 0.000(1) -0.006(1) C(23) 0.032(2) 0.028(1) 0.027(1) -0.013(1) 0.000(1) -0.012(1) C(24) 0.031(2) 0.019(1) 0.018(1) -0.011(1) 0.003(1) -0.005(1) C(25) 0.030(2) 0.019(1) 0.023(1) -0.010(1) 0.007(1) -0.010(1) C(26) 0.028(1) 0.015(1) 0.014(1) -0.008(1) 0.005(1) -0.004(1) C(27) 0.026(2) 0.020(1) 0.019(1) -0.005(1) 0.005(1) -0.006(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; For all methyl groups of the complex, even if it is the lowest, one of H atoms was localized in the Fourier maps, respectively, and H atoms of the rest were placed in geometrically calculated positions. ; 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) O(1) 2.161(2) . . yes Ir(1) O(2) 2.159(2) . . yes Ir(1) N(1) 2.032(2) . . yes Ir(1) N(2) 2.037(2) . . yes Ir(1) C(10) 1.995(3) . . yes Ir(1) C(21) 1.988(3) . . yes O(1) C(24) 1.271(3) . . yes O(2) C(26) 1.268(3) . . yes N(1) C(1) 1.355(3) . . yes N(1) C(9) 1.368(4) . . yes N(2) C(12) 1.351(3) . . yes N(2) C(20) 1.356(4) . . yes C(1) C(2) 1.371(4) . . yes C(1) H(1) 0.953 . . no C(2) C(3) 1.395(4) . . yes C(2) H(2) 0.950 . . no C(3) C(4) 1.389(4) . . yes C(3) H(3) 0.951 . . no C(4) C(5) 1.505(4) . . yes C(4) C(9) 1.401(4) . . yes C(5) C(6) 1.537(4) . . yes C(5) H(5) 0.949 . . no C(5) H(7) 0.949 . . no C(6) C(7) 1.517(4) . . yes C(6) H(4) 0.952 . . no C(6) H(6) 0.945 . . no C(7) C(8) 1.505(4) . . yes C(7) H(8) 0.950 . . no C(7) H(9) 0.950 . . no C(8) C(9) 1.453(3) . . yes C(8) C(10) 1.362(4) . . yes C(10) C(11) 1.506(4) . . yes C(11) H(10) 0.949 . . no C(11) H(11) 0.950 . . no C(11) H(12) 0.950 . . no C(12) C(13) 1.380(4) . . yes C(12) H(13) 0.950 . . no C(13) C(14) 1.393(5) . . yes C(13) H(14) 0.950 . . no C(14) C(15) 1.392(4) . . yes C(14) H(15) 0.949 . . no C(15) C(16) 1.497(4) . . yes C(15) C(20) 1.404(4) . . yes C(16) C(17) 1.536(4) . . yes C(16) H(16) 0.950 . . no C(16) H(17) 0.950 . . no C(17) C(18) 1.534(4) . . yes C(17) H(18) 0.953 . . no C(17) H(19) 0.952 . . no C(18) C(19) 1.510(4) . . yes C(18) H(20) 0.953 . . no C(18) H(21) 0.948 . . no C(19) C(20) 1.452(3) . . yes C(19) C(21) 1.356(4) . . yes C(21) C(22) 1.513(4) . . yes C(22) H(22) 0.953 . . no C(22) H(23) 0.957 . . no C(22) H(24) 0.942 . . no C(23) C(24) 1.512(4) . . yes C(23) H(29) 0.958 . . no C(23) H(30) 0.936 . . no C(23) H(31) 0.965 . . no C(24) C(25) 1.403(4) . . yes C(25) C(26) 1.393(4) . . yes C(25) H(28) 0.951 . . no C(26) C(27) 1.510(4) . . yes C(27) H(25) 0.950 . . no C(27) H(26) 0.951 . . no C(27) H(27) 0.948 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ir(1) O(2) 87.3(1) . . . yes O(1) Ir(1) N(1) 88.19(9) . . . yes O(1) Ir(1) N(2) 94.79(9) . . . yes O(1) Ir(1) C(10) 94.6(1) . . . yes O(1) Ir(1) C(21) 173.56(9) . . . yes O(2) Ir(1) N(1) 94.28(8) . . . yes O(2) Ir(1) N(2) 90.12(9) . . . yes O(2) Ir(1) C(10) 174.01(8) . . . yes O(2) Ir(1) C(21) 88.9(1) . . . yes N(1) Ir(1) N(2) 174.80(8) . . . yes N(1) Ir(1) C(10) 80.12(10) . . . yes N(1) Ir(1) C(21) 97.3(1) . . . yes N(2) Ir(1) C(10) 95.38(10) . . . yes N(2) Ir(1) C(21) 80.0(1) . . . yes C(10) Ir(1) C(21) 89.7(1) . . . yes Ir(1) O(1) C(24) 125.5(2) . . . yes Ir(1) O(2) C(26) 125.9(2) . . . yes Ir(1) N(1) C(1) 126.4(2) . . . yes Ir(1) N(1) C(9) 114.6(2) . . . yes C(1) N(1) C(9) 119.0(2) . . . yes Ir(1) N(2) C(12) 125.6(2) . . . yes Ir(1) N(2) C(20) 114.4(2) . . . yes C(12) N(2) C(20) 119.9(2) . . . yes N(1) C(1) C(2) 122.5(3) . . . yes N(1) C(1) H(1) 118.6 . . . no C(2) C(1) H(1) 118.9 . . . no C(1) C(2) C(3) 118.8(2) . . . yes C(1) C(2) H(2) 120.7 . . . no C(3) C(2) H(2) 120.5 . . . no C(2) C(3) C(4) 119.9(3) . . . yes C(2) C(3) H(3) 120.2 . . . no C(4) C(3) H(3) 119.9 . . . no C(3) C(4) C(5) 122.4(3) . . . yes C(3) C(4) C(9) 118.6(3) . . . yes C(5) C(4) C(9) 119.0(2) . . . yes C(4) C(5) C(6) 111.9(2) . . . yes C(4) C(5) H(5) 109.0 . . . no C(4) C(5) H(7) 108.8 . . . no C(6) C(5) H(5) 108.8 . . . no C(6) C(5) H(7) 108.7 . . . no H(5) C(5) H(7) 109.7 . . . no C(5) C(6) C(7) 112.2(3) . . . yes C(5) C(6) H(4) 108.6 . . . no C(5) C(6) H(6) 108.9 . . . no C(7) C(6) H(4) 108.6 . . . no C(7) C(6) H(6) 108.9 . . . no H(4) C(6) H(6) 109.7 . . . no C(6) C(7) C(8) 111.5(2) . . . yes C(6) C(7) H(8) 109.0 . . . no C(6) C(7) H(9) 109.0 . . . no C(8) C(7) H(8) 109.0 . . . no C(8) C(7) H(9) 109.0 . . . no H(8) C(7) H(9) 109.5 . . . no C(7) C(8) C(9) 116.8(2) . . . yes C(7) C(8) C(10) 128.2(2) . . . yes C(9) C(8) C(10) 114.9(2) . . . yes N(1) C(9) C(4) 121.1(2) . . . yes N(1) C(9) C(8) 114.4(2) . . . yes C(4) C(9) C(8) 124.5(3) . . . yes Ir(1) C(10) C(8) 115.8(2) . . . yes Ir(1) C(10) C(11) 122.3(2) . . . yes C(8) C(10) C(11) 121.8(2) . . . yes C(10) C(11) H(10) 109.4 . . . no C(10) C(11) H(11) 109.3 . . . no C(10) C(11) H(12) 109.4 . . . no H(10) C(11) H(11) 109.6 . . . no H(10) C(11) H(12) 109.6 . . . no H(11) C(11) H(12) 109.5 . . . no N(2) C(12) C(13) 121.8(3) . . . yes N(2) C(12) H(13) 119.1 . . . no C(13) C(12) H(13) 119.1 . . . no C(12) C(13) C(14) 118.8(3) . . . yes C(12) C(13) H(14) 120.6 . . . no C(14) C(13) H(14) 120.6 . . . no C(13) C(14) C(15) 120.2(3) . . . yes C(13) C(14) H(15) 119.9 . . . no C(15) C(14) H(15) 119.8 . . . no C(14) C(15) C(16) 122.6(3) . . . yes C(14) C(15) C(20) 118.0(3) . . . yes C(16) C(15) C(20) 119.4(2) . . . yes C(15) C(16) C(17) 112.0(2) . . . yes C(15) C(16) H(16) 108.8 . . . no C(15) C(16) H(17) 108.9 . . . no C(17) C(16) H(16) 108.8 . . . no C(17) C(16) H(17) 108.8 . . . no H(16) C(16) H(17) 109.5 . . . no C(16) C(17) C(18) 110.5(2) . . . yes C(16) C(17) H(18) 109.5 . . . no C(16) C(17) H(19) 109.6 . . . no C(18) C(17) H(18) 109.2 . . . no C(18) C(17) H(19) 109.0 . . . no H(18) C(17) H(19) 109.1 . . . no C(17) C(18) C(19) 111.3(2) . . . yes C(17) C(18) H(20) 108.6 . . . no C(17) C(18) H(21) 109.1 . . . no C(19) C(18) H(20) 109.1 . . . no C(19) C(18) H(21) 109.3 . . . no H(20) C(18) H(21) 109.4 . . . no C(18) C(19) C(20) 116.2(2) . . . yes C(18) C(19) C(21) 128.8(2) . . . yes C(20) C(19) C(21) 115.0(2) . . . yes N(2) C(20) C(15) 121.3(2) . . . yes N(2) C(20) C(19) 114.5(2) . . . yes C(15) C(20) C(19) 124.1(3) . . . yes Ir(1) C(21) C(19) 115.7(2) . . . yes Ir(1) C(21) C(22) 121.2(2) . . . yes C(19) C(21) C(22) 123.0(3) . . . yes C(21) C(22) H(22) 109.5 . . . no C(21) C(22) H(23) 109.3 . . . no C(21) C(22) H(24) 109.9 . . . no H(22) C(22) H(23) 108.6 . . . no H(22) C(22) H(24) 109.9 . . . no H(23) C(22) H(24) 109.5 . . . no C(24) C(23) H(29) 109.6 . . . no C(24) C(23) H(30) 111.0 . . . no C(24) C(23) H(31) 109.2 . . . no H(29) C(23) H(30) 110.0 . . . no H(29) C(23) H(31) 107.5 . . . no H(30) C(23) H(31) 109.4 . . . no O(1) C(24) C(23) 115.8(3) . . . yes O(1) C(24) C(25) 126.3(3) . . . yes C(23) C(24) C(25) 117.9(3) . . . yes C(24) C(25) C(26) 128.5(3) . . . yes C(24) C(25) H(28) 115.7 . . . no C(26) C(25) H(28) 115.8 . . . no O(2) C(26) C(25) 126.1(3) . . . yes O(2) C(26) C(27) 115.4(3) . . . yes C(25) C(26) C(27) 118.5(2) . . . yes C(26) C(27) H(25) 109.4 . . . no C(26) C(27) H(26) 109.3 . . . no C(26) C(27) H(27) 109.6 . . . no H(25) C(27) H(26) 109.4 . . . no H(25) C(27) H(27) 109.6 . . . no H(26) C(27) H(27) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) O(1) C(24) C(23) -179.6(2) . . . . yes Ir(1) O(1) C(24) C(25) 0.9(4) . . . . yes Ir(1) O(2) C(26) C(25) -6.5(4) . . . . yes Ir(1) O(2) C(26) C(27) 173.1(2) . . . . yes Ir(1) N(1) C(1) C(2) 179.1(2) . . . . yes Ir(1) N(1) C(9) C(4) -177.4(2) . . . . yes Ir(1) N(1) C(9) C(8) 3.7(3) . . . . yes Ir(1) N(2) C(12) C(13) -178.4(2) . . . . yes Ir(1) N(2) C(20) C(15) 177.7(2) . . . . yes Ir(1) N(2) C(20) C(19) 0.5(3) . . . . yes Ir(1) C(10) C(8) C(7) -178.2(2) . . . . yes Ir(1) C(10) C(8) C(9) -1.9(3) . . . . yes Ir(1) C(21) C(19) C(18) 174.7(2) . . . . yes Ir(1) C(21) C(19) C(20) -6.3(3) . . . . yes O(1) Ir(1) O(2) C(26) 6.3(2) . . . . yes O(1) Ir(1) N(1) C(1) -88.2(3) . . . . yes O(1) Ir(1) N(1) C(9) 91.3(2) . . . . yes O(1) Ir(1) N(2) C(12) -10.2(2) . . . . yes O(1) Ir(1) N(2) C(20) 173.2(2) . . . . yes O(1) Ir(1) C(10) C(8) -84.3(2) . . . . yes O(1) Ir(1) C(10) C(11) 98.3(2) . . . . yes O(1) Ir(1) C(21) C(19) -31.9(8) . . . . yes O(1) Ir(1) C(21) C(22) 144.9(6) . . . . yes O(1) C(24) C(25) C(26) 1.5(5) . . . . yes O(2) Ir(1) O(1) C(24) -3.6(2) . . . . yes O(2) Ir(1) N(1) C(1) -1.0(2) . . . . yes O(2) Ir(1) N(1) C(9) 178.5(2) . . . . yes O(2) Ir(1) N(2) C(12) -97.5(2) . . . . yes O(2) Ir(1) N(2) C(20) 85.9(2) . . . . yes O(2) Ir(1) C(10) C(8) 24.0(10) . . . . yes O(2) Ir(1) C(10) C(11) -153.4(7) . . . . yes O(2) Ir(1) C(21) C(19) -85.2(2) . . . . yes O(2) Ir(1) C(21) C(22) 91.5(2) . . . . yes O(2) C(26) C(25) C(24) 1.7(5) . . . . yes N(1) Ir(1) O(1) C(24) 90.8(2) . . . . yes N(1) Ir(1) O(2) C(26) -81.7(2) . . . . yes N(1) Ir(1) N(2) C(12) 114.6(9) . . . . yes N(1) Ir(1) N(2) C(20) -62.0(10) . . . . yes N(1) Ir(1) C(10) C(8) 3.0(2) . . . . yes N(1) Ir(1) C(10) C(11) -174.3(2) . . . . yes N(1) Ir(1) C(21) C(19) -179.4(2) . . . . yes N(1) Ir(1) C(21) C(22) -2.7(2) . . . . yes N(1) C(1) C(2) C(3) -2.7(5) . . . . yes N(1) C(9) C(4) C(3) -0.9(4) . . . . yes N(1) C(9) C(4) C(5) -179.5(2) . . . . yes N(1) C(9) C(8) C(7) 175.5(2) . . . . yes N(1) C(9) C(8) C(10) -1.2(4) . . . . yes N(2) Ir(1) O(1) C(24) -93.5(2) . . . . yes N(2) Ir(1) O(2) C(26) 101.1(2) . . . . yes N(2) Ir(1) N(1) C(1) 146.7(8) . . . . yes N(2) Ir(1) N(1) C(9) -33.8(10) . . . . yes N(2) Ir(1) C(10) C(8) -179.6(2) . . . . yes N(2) Ir(1) C(10) C(11) 3.1(2) . . . . yes N(2) Ir(1) C(21) C(19) 5.1(2) . . . . yes N(2) Ir(1) C(21) C(22) -178.2(2) . . . . yes N(2) C(12) C(13) C(14) 0.9(4) . . . . yes N(2) C(20) C(15) C(14) 1.2(4) . . . . yes N(2) C(20) C(15) C(16) -178.0(2) . . . . yes N(2) C(20) C(19) C(18) -177.1(2) . . . . yes N(2) C(20) C(19) C(21) 3.8(3) . . . . yes C(1) N(1) Ir(1) C(10) 176.8(3) . . . . yes C(1) N(1) Ir(1) C(21) 88.3(3) . . . . yes C(1) N(1) C(9) C(4) 2.1(4) . . . . yes C(1) N(1) C(9) C(8) -176.7(2) . . . . yes C(1) C(2) C(3) C(4) 3.9(4) . . . . yes C(2) C(1) N(1) C(9) -0.3(4) . . . . yes C(2) C(3) C(4) C(5) 176.5(3) . . . . yes C(2) C(3) C(4) C(9) -2.2(4) . . . . yes C(3) C(4) C(5) C(6) 158.3(3) . . . . yes C(3) C(4) C(9) C(8) 177.9(3) . . . . yes C(4) C(5) C(6) C(7) 51.1(3) . . . . yes C(4) C(9) C(8) C(7) -3.3(4) . . . . yes C(4) C(9) C(8) C(10) 179.9(3) . . . . yes C(5) C(4) C(9) C(8) -0.8(4) . . . . yes C(5) C(6) C(7) C(8) -55.3(3) . . . . yes C(6) C(5) C(4) C(9) -23.0(4) . . . . yes C(6) C(7) C(8) C(9) 31.2(3) . . . . yes C(6) C(7) C(8) C(10) -152.6(3) . . . . yes C(7) C(8) C(10) C(11) -0.8(4) . . . . yes C(8) C(10) Ir(1) C(21) 100.5(2) . . . . yes C(9) N(1) Ir(1) C(10) -3.7(2) . . . . yes C(9) N(1) Ir(1) C(21) -92.2(2) . . . . yes C(9) C(8) C(10) C(11) 175.4(2) . . . . yes C(10) Ir(1) O(1) C(24) 170.7(2) . . . . yes C(10) Ir(1) O(2) C(26) -102.3(8) . . . . yes C(10) Ir(1) N(2) C(12) 84.9(2) . . . . yes C(10) Ir(1) N(2) C(20) -91.7(2) . . . . yes C(10) Ir(1) C(21) C(19) 100.6(2) . . . . yes C(10) Ir(1) C(21) C(22) -82.7(2) . . . . yes C(11) C(10) Ir(1) C(21) -76.9(2) . . . . yes C(12) N(2) Ir(1) C(21) 173.7(2) . . . . yes C(12) N(2) C(20) C(15) 0.9(4) . . . . yes C(12) N(2) C(20) C(19) -176.4(2) . . . . yes C(12) C(13) C(14) C(15) 1.4(4) . . . . yes C(13) C(12) N(2) C(20) -2.0(4) . . . . yes C(13) C(14) C(15) C(16) 176.8(3) . . . . yes C(13) C(14) C(15) C(20) -2.4(4) . . . . yes C(14) C(15) C(16) C(17) -154.3(3) . . . . yes C(14) C(15) C(20) C(19) 178.3(3) . . . . yes C(15) C(16) C(17) C(18) -52.7(3) . . . . yes C(15) C(20) C(19) C(18) 5.6(4) . . . . yes C(15) C(20) C(19) C(21) -173.4(3) . . . . yes C(16) C(15) C(20) C(19) -0.9(4) . . . . yes C(16) C(17) C(18) C(19) 57.5(3) . . . . yes C(17) C(16) C(15) C(20) 24.8(4) . . . . yes C(17) C(18) C(19) C(20) -33.9(3) . . . . yes C(17) C(18) C(19) C(21) 145.0(3) . . . . yes C(18) C(19) C(21) C(22) -1.9(4) . . . . yes C(20) N(2) Ir(1) C(21) -2.9(2) . . . . yes C(20) C(19) C(21) C(22) 177.0(2) . . . . yes C(21) Ir(1) O(1) C(24) -57.0(7) . . . . yes C(21) Ir(1) O(2) C(26) -178.9(2) . . . . yes C(23) C(24) C(25) C(26) -178.1(3) . . . . yes C(24) C(25) C(26) C(27) -177.9(3) . . . . yes C(24) C(25) C(26) C(27) -177.9(3) . . . . 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 O(1) C(13) 3.283(5) . 2_656 ? O(2) C(2) 3.444(5) . 2_565 ? C(14) C(20) 3.555(5) . 2_556 ? C(15) C(15) 3.598(6) . 2_556 ? C(16) C(26) 3.553(4) . 2_556 ? #===END #------------------------------------------------------------------------------ data_6a _database_code_depnum_ccdc_archive 'CCDC 616854' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C49 H43 Cl3 Ir N3 ' _chemical_formula_moiety ? _chemical_formula_weight 972.48 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 15.87(2) _cell_length_b 20.70(2) _cell_length_c 24.37(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8004(51) _cell_formula_units_Z 8 _cell_measurement_reflns_used 57160 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.141 _exptl_absorpt_correction_T_max 0.238 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 65766 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9755 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9755 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8973 _reflns_number_gt 6796 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0479 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8973 _refine_ls_number_parameters 505 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.01800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0041 _refine_diff_density_max 1.30 _refine_diff_density_min -1.00 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; Ir Ir -1.444 7.990 ;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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.240374(6) 0.234090(5) 0.139180(4) 0.01118(3) Uani 1.00 d . . . Cl(1) Cl 0.75626(7) -0.03958(7) 0.15717(5) 0.0727(4) Uani 1.00 d . . . Cl(2) Cl 0.63417(6) 0.05286(5) 0.11911(4) 0.0442(3) Uani 1.00 d . . . Cl(3) Cl 0.61267(5) -0.00922(5) 0.22390(4) 0.0415(3) Uani 1.00 d . . . N(1) N 0.1820(1) 0.1477(1) 0.11344(10) 0.0138(6) Uani 1.00 d . . . N(2) N 0.1263(1) 0.28718(10) 0.13356(9) 0.0126(6) Uani 1.00 d . . . N(3) N 0.2356(1) 0.21546(10) 0.22479(10) 0.0128(6) Uani 1.00 d . . . C(1) C 0.1447(2) 0.1038(1) 0.1458(1) 0.0162(7) Uani 1.00 d . . . C(2) C 0.1031(2) 0.0503(1) 0.1245(1) 0.0174(8) Uani 1.00 d . . . C(3) C 0.1003(2) 0.0428(1) 0.0683(1) 0.0184(8) Uani 1.00 d . . . C(4) C 0.1384(2) 0.0874(1) 0.0339(1) 0.0165(8) Uani 1.00 d . . . C(5) C 0.1795(2) 0.1405(1) 0.0578(1) 0.0136(7) Uani 1.00 d . . . C(6) C 0.1376(2) 0.0816(1) -0.0274(1) 0.0252(9) Uani 1.00 d . . . C(7) C 0.1477(2) 0.1465(1) -0.0560(1) 0.0220(8) Uani 1.00 d . . . C(8) C 0.2251(2) 0.1821(1) -0.0344(1) 0.0184(8) Uani 1.00 d . . . C(9) C 0.2206(2) 0.1909(1) 0.0269(1) 0.0137(7) Uani 1.00 d . . . C(10) C 0.2530(1) 0.2407(1) 0.0568(1) 0.0127(6) Uani 1.00 d . . . C(11) C 0.2966(2) 0.2943(1) 0.0278(1) 0.0140(7) Uani 1.00 d . . . C(12) C 0.3766(2) 0.2867(1) 0.0052(1) 0.0175(8) Uani 1.00 d . . . C(13) C 0.4169(2) 0.3375(1) -0.0206(1) 0.0198(8) Uani 1.00 d . . . C(14) C 0.3777(2) 0.3971(1) -0.0256(1) 0.0216(8) Uani 1.00 d . . . C(15) C 0.2973(2) 0.4052(1) -0.0041(1) 0.0205(8) Uani 1.00 d . . . C(16) C 0.2581(2) 0.3548(1) 0.0229(1) 0.0173(7) Uani 1.00 d . . . C(17) C 0.0504(2) 0.2654(1) 0.1181(1) 0.0176(7) Uani 1.00 d . . . C(18) C -0.0179(2) 0.3050(1) 0.1111(1) 0.0197(8) Uani 1.00 d . . . C(19) C -0.0083(2) 0.3705(1) 0.1193(1) 0.0181(8) Uani 1.00 d . . . C(20) C 0.0686(2) 0.3948(1) 0.1352(1) 0.0182(8) Uani 1.00 d . . . C(21) C 0.1363(2) 0.3516(1) 0.1429(1) 0.0152(7) Uani 1.00 d . . . C(22) C 0.0839(2) 0.4660(1) 0.1452(2) 0.0282(9) Uani 1.00 d . . . C(23) C 0.1731(2) 0.4843(1) 0.1455(2) 0.041(1) Uani 1.00 d . . . C(24) C 0.2318(2) 0.4412(1) 0.1745(2) 0.0318(10) Uani 1.00 d . . . C(25) C 0.2203(2) 0.3711(1) 0.1591(1) 0.0175(8) Uani 1.00 d . . . C(26) C 0.2799(2) 0.3243(1) 0.1581(1) 0.0116(7) Uani 1.00 d . . . C(27) C 0.3683(2) 0.3413(1) 0.1731(1) 0.0139(7) Uani 1.00 d . . . C(28) C 0.4188(2) 0.3771(1) 0.1375(1) 0.0159(7) Uani 1.00 d . . . C(29) C 0.4999(2) 0.3951(1) 0.1527(1) 0.0186(8) Uani 1.00 d . . . C(30) C 0.5330(2) 0.3766(1) 0.2024(1) 0.0202(8) Uani 1.00 d . . . C(31) C 0.4839(2) 0.3400(1) 0.2377(1) 0.0189(8) Uani 1.00 d . . . C(32) C 0.4023(2) 0.3231(1) 0.2232(1) 0.0165(7) Uani 1.00 d . . . C(33) C 0.1784(2) 0.2369(1) 0.2606(1) 0.0187(8) Uani 1.00 d . . . C(34) C 0.1842(2) 0.2266(1) 0.3161(1) 0.0244(9) Uani 1.00 d . . . C(35) C 0.2521(2) 0.1909(1) 0.3361(1) 0.0227(8) Uani 1.00 d . . . C(36) C 0.3120(2) 0.1678(1) 0.3002(1) 0.0188(8) Uani 1.00 d . . . C(37) C 0.3030(2) 0.1814(1) 0.2439(1) 0.0143(7) Uani 1.00 d . . . C(38) C 0.3875(2) 0.1288(2) 0.3186(1) 0.0282(9) Uani 1.00 d . . . C(39) C 0.4205(2) 0.0861(2) 0.2728(1) 0.0290(9) Uani 1.00 d . . . C(40) C 0.4411(2) 0.1267(1) 0.2221(1) 0.0201(8) Uani 1.00 d . . . C(41) C 0.3646(2) 0.1644(1) 0.2029(1) 0.0144(7) Uani 1.00 d . . . C(42) C 0.3499(2) 0.1855(1) 0.1513(1) 0.0144(7) Uani 1.00 d . . . C(43) C 0.4115(2) 0.1697(1) 0.1072(1) 0.0142(7) Uani 1.00 d . . . C(44) C 0.4877(2) 0.2025(1) 0.1026(1) 0.0183(8) Uani 1.00 d . . . C(45) C 0.5449(2) 0.1863(1) 0.0617(1) 0.0214(8) Uani 1.00 d . . . C(46) C 0.5272(2) 0.1376(1) 0.0250(1) 0.0231(9) Uani 1.00 d . . . C(47) C 0.4515(2) 0.1045(1) 0.0289(1) 0.0201(8) Uani 1.00 d . . . C(48) C 0.3945(2) 0.1208(1) 0.0694(1) 0.0164(8) Uani 1.00 d . . . C(49) C 0.6854(2) 0.0210(2) 0.1766(2) 0.0315(10) Uani 1.00 d . . . H(1) H 0.1474 0.1091 0.1849 0.0182 Uiso 1.00 calc . . . H(2) H 0.0751 0.0198 0.1483 0.0216 Uiso 1.00 calc . . . H(3) H 0.0718 0.0060 0.0524 0.0218 Uiso 1.00 calc . . . H(4) H 0.1825 0.0540 -0.0389 0.0300 Uiso 1.00 calc . . . H(5) H 0.0854 0.0626 -0.0385 0.0300 Uiso 1.00 calc . . . H(6) H 0.1522 0.1408 -0.0944 0.0264 Uiso 1.00 calc . . . H(7) H 0.0987 0.1727 -0.0485 0.0264 Uiso 1.00 calc . . . H(8) H 0.2740 0.1573 -0.0435 0.0226 Uiso 1.00 calc . . . H(9) H 0.2292 0.2232 -0.0519 0.0226 Uiso 1.00 calc . . . H(10) H 0.4044 0.2455 0.0077 0.0211 Uiso 1.00 calc . . . H(11) H 0.4723 0.3320 -0.0356 0.0248 Uiso 1.00 calc . . . H(12) H 0.4061 0.4322 -0.0435 0.0249 Uiso 1.00 calc . . . H(13) H 0.2685 0.4459 -0.0082 0.0249 Uiso 1.00 calc . . . H(14) H 0.2035 0.3609 0.0389 0.0209 Uiso 1.00 calc . . . H(15) H 0.0435 0.2196 0.1120 0.0210 Uiso 1.00 calc . . . H(16) H -0.0716 0.2870 0.1008 0.0249 Uiso 1.00 calc . . . H(17) H -0.0553 0.3991 0.1135 0.0225 Uiso 1.00 calc . . . H(18) H 0.0530 0.4907 0.1191 0.0365 Uiso 1.00 calc . . . H(19) H 0.0617 0.4769 0.1814 0.0365 Uiso 1.00 calc . . . H(20) H 0.1923 0.4840 0.1061 0.0423 Uiso 1.00 calc . . . H(21) H 0.1807 0.5277 0.1573 0.0423 Uiso 1.00 calc . . . H(22) H 0.2887 0.4535 0.1696 0.0363 Uiso 1.00 calc . . . H(23) H 0.2191 0.4457 0.2138 0.0363 Uiso 1.00 calc . . . H(24) H 0.3970 0.3898 0.1021 0.0184 Uiso 1.00 calc . . . H(25) H 0.5329 0.4215 0.1279 0.0228 Uiso 1.00 calc . . . H(26) H 0.5893 0.3886 0.2127 0.0235 Uiso 1.00 calc . . . H(27) H 0.5062 0.3259 0.2720 0.0229 Uiso 1.00 calc . . . H(28) H 0.3687 0.2982 0.2485 0.0215 Uiso 1.00 calc . . . H(29) H 0.1306 0.2610 0.2467 0.0223 Uiso 1.00 calc . . . H(30) H 0.1427 0.2436 0.3408 0.0295 Uiso 1.00 calc . . . H(31) H 0.2568 0.1826 0.3745 0.0279 Uiso 1.00 calc . . . H(32) H 0.4310 0.1573 0.3300 0.0338 Uiso 1.00 calc . . . H(33) H 0.3716 0.1023 0.3492 0.0338 Uiso 1.00 calc . . . H(34) H 0.4697 0.0636 0.2848 0.0324 Uiso 1.00 calc . . . H(35) H 0.3785 0.0546 0.2633 0.0324 Uiso 1.00 calc . . . H(36) H 0.4851 0.1560 0.2312 0.0239 Uiso 1.00 calc . . . H(37) H 0.4599 0.0990 0.1933 0.0239 Uiso 1.00 calc . . . H(38) H 0.5000 0.2368 0.1281 0.0234 Uiso 1.00 calc . . . H(39) H 0.5973 0.2095 0.0590 0.0272 Uiso 1.00 calc . . . H(40) H 0.5670 0.1270 -0.0033 0.0268 Uiso 1.00 calc . . . H(41) H 0.4391 0.0702 0.0037 0.0252 Uiso 1.00 calc . . . H(42) H 0.3420 0.0980 0.0714 0.0202 Uiso 1.00 calc . . . H(43) H 0.7172 0.0552 0.1941 0.0374 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) 0.01118(5) 0.01126(5) 0.01111(6) -0.00055(4) -0.00021(5) -0.00035(5) Cl(1) 0.0634(7) 0.1084(10) 0.0461(7) 0.0542(7) 0.0022(6) -0.0082(7) Cl(2) 0.0401(5) 0.0518(6) 0.0408(6) -0.0067(4) -0.0063(4) 0.0214(5) Cl(3) 0.0326(5) 0.0627(6) 0.0292(5) -0.0002(4) -0.0022(4) 0.0107(5) N(1) 0.012(1) 0.013(1) 0.017(1) -0.0005(9) 0.001(1) 0.002(1) N(2) 0.014(1) 0.013(1) 0.011(1) -0.0013(8) 0.001(1) -0.0002(10) N(3) 0.012(1) 0.013(1) 0.014(1) -0.0003(8) -0.0005(10) -0.0014(9) C(1) 0.016(1) 0.016(1) 0.017(2) 0.003(1) 0.000(1) 0.000(1) C(2) 0.017(1) 0.013(1) 0.022(2) -0.002(1) 0.002(1) 0.003(1) C(3) 0.019(1) 0.014(1) 0.022(2) -0.001(1) -0.003(1) -0.002(1) C(4) 0.019(1) 0.014(1) 0.016(2) 0.002(1) -0.004(1) -0.002(1) C(5) 0.012(1) 0.012(1) 0.017(2) 0.002(1) -0.002(1) 0.002(1) C(6) 0.039(2) 0.020(2) 0.016(2) -0.006(1) -0.007(1) -0.001(1) C(7) 0.032(2) 0.019(2) 0.015(2) -0.005(1) -0.007(1) 0.000(1) C(8) 0.025(2) 0.018(1) 0.013(2) 0.001(1) -0.002(1) 0.002(1) C(9) 0.013(1) 0.013(1) 0.015(2) 0.001(1) -0.001(1) 0.002(1) C(10) 0.005(1) 0.015(1) 0.017(1) 0.001(1) -0.003(1) 0.006(1) C(11) 0.015(1) 0.016(1) 0.011(2) 0.000(1) -0.005(1) -0.002(1) C(12) 0.021(1) 0.017(1) 0.014(2) 0.001(1) 0.000(1) 0.000(1) C(13) 0.021(1) 0.024(2) 0.015(2) 0.000(1) 0.004(1) -0.001(1) C(14) 0.034(2) 0.018(2) 0.013(2) -0.010(1) 0.001(1) 0.003(1) C(15) 0.027(2) 0.014(1) 0.020(2) 0.003(1) -0.001(1) 0.003(1) C(16) 0.017(1) 0.019(1) 0.016(2) 0.001(1) -0.001(1) 0.002(1) C(17) 0.018(1) 0.019(1) 0.016(2) -0.004(1) 0.000(1) -0.003(1) C(18) 0.013(1) 0.028(2) 0.018(2) 0.001(1) -0.003(1) -0.004(1) C(19) 0.017(1) 0.024(2) 0.014(2) 0.006(1) 0.001(1) 0.001(1) C(20) 0.019(1) 0.019(1) 0.017(2) 0.000(1) 0.001(1) 0.003(1) C(21) 0.013(1) 0.017(1) 0.016(2) 0.002(1) 0.003(1) 0.001(1) C(22) 0.018(2) 0.016(1) 0.051(3) 0.008(1) -0.001(2) 0.001(2) C(23) 0.035(2) 0.018(2) 0.069(3) 0.005(1) -0.022(2) -0.008(2) C(24) 0.021(2) 0.017(2) 0.058(3) 0.000(1) -0.008(2) -0.005(2) C(25) 0.017(1) 0.014(1) 0.022(2) 0.000(1) -0.002(1) -0.001(1) C(26) 0.009(1) 0.014(1) 0.012(1) -0.002(1) 0.000(1) 0.005(1) C(27) 0.012(1) 0.011(1) 0.018(2) 0.003(1) 0.000(1) -0.004(1) C(28) 0.016(1) 0.013(1) 0.018(2) 0.001(1) -0.001(1) -0.003(1) C(29) 0.015(1) 0.017(1) 0.024(2) -0.002(1) 0.005(1) 0.000(1) C(30) 0.011(1) 0.020(2) 0.029(2) -0.001(1) -0.003(1) -0.007(1) C(31) 0.019(1) 0.020(1) 0.018(2) 0.003(1) -0.005(1) -0.003(1) C(32) 0.019(1) 0.014(1) 0.016(2) -0.001(1) 0.002(1) -0.002(1) C(33) 0.013(1) 0.021(1) 0.022(2) 0.000(1) 0.003(1) 0.000(1) C(34) 0.027(2) 0.029(2) 0.017(2) 0.003(1) 0.007(1) -0.003(1) C(35) 0.028(2) 0.025(2) 0.015(2) -0.003(1) 0.000(1) 0.001(1) C(36) 0.023(2) 0.019(1) 0.015(2) -0.003(1) -0.001(1) -0.001(1) C(37) 0.018(1) 0.011(1) 0.014(2) -0.004(1) 0.001(1) 0.000(1) C(38) 0.033(2) 0.038(2) 0.014(2) 0.010(1) -0.003(1) 0.004(2) C(39) 0.029(2) 0.038(2) 0.020(2) 0.009(1) -0.003(1) 0.005(2) C(40) 0.019(1) 0.026(2) 0.016(2) 0.004(1) -0.002(1) -0.002(1) C(41) 0.016(1) 0.013(1) 0.015(2) -0.003(1) 0.000(1) -0.001(1) C(42) 0.018(1) 0.007(1) 0.018(2) -0.003(1) 0.000(1) -0.003(1) C(43) 0.014(1) 0.016(1) 0.014(2) 0.003(1) -0.001(1) 0.004(1) C(44) 0.018(1) 0.018(1) 0.019(2) 0.000(1) -0.001(1) -0.001(1) C(45) 0.013(1) 0.027(2) 0.024(2) 0.000(1) 0.003(1) 0.005(1) C(46) 0.021(2) 0.034(2) 0.015(2) 0.008(1) 0.006(1) 0.004(1) C(47) 0.022(2) 0.022(2) 0.015(2) 0.005(1) 0.000(1) -0.001(1) C(48) 0.015(1) 0.016(1) 0.018(2) -0.002(1) 0.000(1) 0.006(1) C(49) 0.024(2) 0.035(2) 0.035(2) -0.003(1) -0.004(2) 0.002(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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) N(1) 2.109(2) . . yes Ir(1) N(2) 2.122(3) . . yes Ir(1) N(3) 2.123(2) . . yes Ir(1) C(10) 2.022(3) . . yes Ir(1) C(26) 2.023(3) . . yes Ir(1) C(42) 2.029(3) . . yes Cl(1) C(49) 1.750(3) . . yes Cl(2) C(49) 1.748(4) . . yes Cl(3) C(49) 1.747(4) . . yes N(1) C(1) 1.341(3) . . yes N(1) C(5) 1.364(4) . . yes N(2) C(17) 1.339(3) . . yes N(2) C(21) 1.362(3) . . yes N(3) C(33) 1.336(3) . . yes N(3) C(37) 1.363(3) . . yes C(1) C(2) 1.388(4) . . yes C(1) H(1) 0.961 . . no C(2) C(3) 1.379(4) . . yes C(2) H(2) 0.965 . . no C(3) C(4) 1.385(4) . . yes C(3) H(3) 0.968 . . no C(4) C(5) 1.406(4) . . yes C(4) C(6) 1.497(4) . . yes C(5) C(9) 1.442(4) . . yes C(6) C(7) 1.521(4) . . yes C(6) H(4) 0.956 . . no C(6) H(5) 0.957 . . no C(7) C(8) 1.527(4) . . yes C(7) H(6) 0.946 . . no C(7) H(7) 0.964 . . no C(8) C(9) 1.505(4) . . yes C(8) H(8) 0.957 . . no C(8) H(9) 0.953 . . no C(9) C(10) 1.364(4) . . yes C(10) C(11) 1.486(4) . . yes C(11) C(12) 1.393(4) . . yes C(11) C(16) 1.399(4) . . yes C(12) C(13) 1.383(4) . . yes C(12) H(10) 0.962 . . no C(13) C(14) 1.385(4) . . yes C(13) H(11) 0.959 . . no C(14) C(15) 1.391(4) . . yes C(14) H(12) 0.960 . . no C(15) C(16) 1.381(4) . . yes C(15) H(13) 0.963 . . no C(16) H(14) 0.958 . . no C(17) C(18) 1.371(4) . . yes C(17) H(15) 0.964 . . no C(18) C(19) 1.378(4) . . yes C(18) H(16) 0.963 . . no C(19) C(20) 1.376(4) . . yes C(19) H(17) 0.963 . . no C(20) C(21) 1.411(4) . . yes C(20) C(22) 1.513(4) . . yes C(21) C(25) 1.447(4) . . yes C(22) C(23) 1.465(4) . . yes C(22) H(18) 0.954 . . no C(22) H(19) 0.975 . . no C(23) C(24) 1.470(4) . . yes C(23) H(20) 1.007 . . no C(23) H(21) 0.950 . . no C(24) C(25) 1.509(4) . . yes C(24) H(22) 0.946 . . no C(24) H(23) 0.982 . . no C(25) C(26) 1.355(4) . . yes C(26) C(27) 1.492(4) . . yes C(27) C(28) 1.394(4) . . yes C(27) C(32) 1.387(4) . . yes C(28) C(29) 1.390(4) . . yes C(28) H(24) 0.966 . . no C(29) C(30) 1.374(4) . . yes C(29) H(25) 0.966 . . no C(30) C(31) 1.387(4) . . yes C(30) H(26) 0.962 . . no C(31) C(32) 1.387(4) . . yes C(31) H(27) 0.954 . . no C(32) H(28) 0.964 . . no C(33) C(34) 1.371(4) . . yes C(33) H(29) 0.968 . . no C(34) C(35) 1.394(4) . . yes C(34) H(30) 0.961 . . no C(35) C(36) 1.377(4) . . yes C(35) H(31) 0.955 . . no C(36) C(37) 1.408(4) . . yes C(36) C(38) 1.513(4) . . yes C(37) C(41) 1.441(4) . . yes C(38) C(39) 1.518(4) . . yes C(38) H(32) 0.950 . . no C(38) H(33) 0.960 . . no C(39) C(40) 1.529(4) . . yes C(39) H(34) 0.955 . . no C(39) H(35) 0.961 . . no C(40) C(41) 1.518(4) . . yes C(40) H(36) 0.951 . . no C(40) H(37) 0.953 . . no C(41) C(42) 1.350(4) . . yes C(42) C(43) 1.491(4) . . yes C(43) C(44) 1.391(4) . . yes C(43) C(48) 1.395(4) . . yes C(44) C(45) 1.390(4) . . yes C(44) H(38) 0.964 . . no C(45) C(46) 1.375(4) . . yes C(45) H(39) 0.962 . . no C(46) C(47) 1.387(4) . . yes C(46) H(40) 0.961 . . no C(47) C(48) 1.380(4) . . yes C(47) H(41) 0.961 . . no C(48) H(42) 0.959 . . no C(49) H(43) 0.970 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ir(1) N(2) 92.60(9) . . . yes N(1) Ir(1) N(3) 97.05(8) . . . yes N(1) Ir(1) C(10) 78.79(10) . . . yes N(1) Ir(1) C(26) 170.56(9) . . . yes N(1) Ir(1) C(42) 90.0(1) . . . yes N(2) Ir(1) N(3) 97.31(8) . . . yes N(2) Ir(1) C(10) 89.17(9) . . . yes N(2) Ir(1) C(26) 78.53(10) . . . yes N(2) Ir(1) C(42) 175.1(1) . . . yes N(3) Ir(1) C(10) 172.49(9) . . . yes N(3) Ir(1) C(26) 87.40(9) . . . yes N(3) Ir(1) C(42) 78.27(10) . . . yes C(10) Ir(1) C(26) 97.7(1) . . . yes C(10) Ir(1) C(42) 95.4(1) . . . yes C(26) Ir(1) C(42) 99.1(1) . . . yes Ir(1) N(1) C(1) 126.4(2) . . . yes Ir(1) N(1) C(5) 113.6(2) . . . yes C(1) N(1) C(5) 119.8(2) . . . yes Ir(1) N(2) C(17) 127.6(2) . . . yes Ir(1) N(2) C(21) 113.4(2) . . . yes C(17) N(2) C(21) 118.8(2) . . . yes Ir(1) N(3) C(33) 127.3(2) . . . yes Ir(1) N(3) C(37) 113.7(2) . . . yes C(33) N(3) C(37) 118.9(2) . . . yes N(1) C(1) C(2) 122.1(3) . . . yes N(1) C(1) H(1) 119.0 . . . no C(2) C(1) H(1) 118.9 . . . no C(1) C(2) C(3) 118.3(3) . . . yes C(1) C(2) H(2) 121.1 . . . no C(3) C(2) H(2) 120.5 . . . no C(2) C(3) C(4) 120.9(3) . . . yes C(2) C(3) H(3) 120.2 . . . no C(4) C(3) H(3) 118.9 . . . no C(3) C(4) C(5) 118.1(3) . . . yes C(3) C(4) C(6) 123.3(3) . . . yes C(5) C(4) C(6) 118.7(3) . . . yes N(1) C(5) C(4) 120.8(3) . . . yes N(1) C(5) C(9) 115.3(2) . . . yes C(4) C(5) C(9) 123.9(3) . . . yes C(4) C(6) C(7) 112.7(2) . . . yes C(4) C(6) H(4) 109.5 . . . no C(4) C(6) H(5) 108.8 . . . no C(7) C(6) H(4) 108.4 . . . no C(7) C(6) H(5) 108.9 . . . no H(4) C(6) H(5) 108.4 . . . no C(6) C(7) C(8) 110.6(2) . . . yes C(6) C(7) H(6) 110.6 . . . no C(6) C(7) H(7) 108.9 . . . no C(8) C(7) H(6) 109.9 . . . no C(8) C(7) H(7) 108.1 . . . no H(6) C(7) H(7) 108.6 . . . no C(7) C(8) C(9) 111.2(2) . . . yes C(7) C(8) H(8) 108.2 . . . no C(7) C(8) H(9) 109.4 . . . no C(9) C(8) H(8) 109.5 . . . no C(9) C(8) H(9) 109.8 . . . no H(8) C(8) H(9) 108.6 . . . no C(5) C(9) C(8) 116.9(2) . . . yes C(5) C(9) C(10) 115.9(3) . . . yes C(8) C(9) C(10) 127.1(2) . . . yes Ir(1) C(10) C(9) 116.3(2) . . . yes Ir(1) C(10) C(11) 124.7(2) . . . yes C(9) C(10) C(11) 119.0(2) . . . yes C(10) C(11) C(12) 121.9(2) . . . yes C(10) C(11) C(16) 120.4(2) . . . yes C(12) C(11) C(16) 117.7(3) . . . yes C(11) C(12) C(13) 121.0(3) . . . yes C(11) C(12) H(10) 119.6 . . . no C(13) C(12) H(10) 119.4 . . . no C(12) C(13) C(14) 120.6(3) . . . yes C(12) C(13) H(11) 120.4 . . . no C(14) C(13) H(11) 119.0 . . . no C(13) C(14) C(15) 119.1(3) . . . yes C(13) C(14) H(12) 120.3 . . . no C(15) C(14) H(12) 120.6 . . . no C(14) C(15) C(16) 120.1(3) . . . yes C(14) C(15) H(13) 120.2 . . . no C(16) C(15) H(13) 119.7 . . . no C(11) C(16) C(15) 121.4(3) . . . yes C(11) C(16) H(14) 118.5 . . . no C(15) C(16) H(14) 120.1 . . . no N(2) C(17) C(18) 123.0(3) . . . yes N(2) C(17) H(15) 118.5 . . . no C(18) C(17) H(15) 118.6 . . . no C(17) C(18) C(19) 118.9(2) . . . yes C(17) C(18) H(16) 120.1 . . . no C(19) C(18) H(16) 121.0 . . . no C(18) C(19) C(20) 120.0(2) . . . yes C(18) C(19) H(17) 119.9 . . . no C(20) C(19) H(17) 120.1 . . . no C(19) C(20) C(21) 118.7(3) . . . yes C(19) C(20) C(22) 123.0(2) . . . yes C(21) C(20) C(22) 118.2(2) . . . yes N(2) C(21) C(20) 120.6(2) . . . yes N(2) C(21) C(25) 115.3(2) . . . yes C(20) C(21) C(25) 124.1(2) . . . yes C(20) C(22) C(23) 114.1(2) . . . yes C(20) C(22) H(18) 109.4 . . . no C(20) C(22) H(19) 108.3 . . . no C(23) C(22) H(18) 111.2 . . . no C(23) C(22) H(19) 106.5 . . . no H(18) C(22) H(19) 107.0 . . . no C(22) C(23) C(24) 117.1(3) . . . yes C(22) C(23) H(20) 106.6 . . . no C(22) C(23) H(21) 111.7 . . . no C(24) C(23) H(20) 105.2 . . . no C(24) C(23) H(21) 110.4 . . . no H(20) C(23) H(21) 104.8 . . . no C(23) C(24) C(25) 112.8(3) . . . yes C(23) C(24) H(22) 112.4 . . . no C(23) C(24) H(23) 106.3 . . . no C(25) C(24) H(22) 110.0 . . . no C(25) C(24) H(23) 108.0 . . . no H(22) C(24) H(23) 107.1 . . . no C(21) C(25) C(24) 116.6(2) . . . yes C(21) C(25) C(26) 116.0(2) . . . yes C(24) C(25) C(26) 127.5(3) . . . yes Ir(1) C(26) C(25) 116.6(2) . . . yes Ir(1) C(26) C(27) 124.4(2) . . . yes C(25) C(26) C(27) 118.9(2) . . . yes C(26) C(27) C(28) 120.9(3) . . . yes C(26) C(27) C(32) 121.1(2) . . . yes C(28) C(27) C(32) 118.0(2) . . . yes C(27) C(28) C(29) 120.6(3) . . . yes C(27) C(28) H(24) 119.6 . . . no C(29) C(28) H(24) 119.8 . . . no C(28) C(29) C(30) 120.9(3) . . . yes C(28) C(29) H(25) 119.1 . . . no C(30) C(29) H(25) 120.0 . . . no C(29) C(30) C(31) 119.1(3) . . . yes C(29) C(30) H(26) 120.9 . . . no C(31) C(30) H(26) 120.1 . . . no C(30) C(31) C(32) 120.2(3) . . . yes C(30) C(31) H(27) 120.3 . . . no C(32) C(31) H(27) 119.5 . . . no C(27) C(32) C(31) 121.3(3) . . . yes C(27) C(32) H(28) 119.6 . . . no C(31) C(32) H(28) 119.1 . . . no N(3) C(33) C(34) 123.1(3) . . . yes N(3) C(33) H(29) 118.4 . . . no C(34) C(33) H(29) 118.6 . . . no C(33) C(34) C(35) 118.7(3) . . . yes C(33) C(34) H(30) 121.1 . . . no C(35) C(34) H(30) 120.2 . . . no C(34) C(35) C(36) 119.6(3) . . . yes C(34) C(35) H(31) 120.0 . . . no C(36) C(35) H(31) 120.4 . . . no C(35) C(36) C(37) 118.7(3) . . . yes C(35) C(36) C(38) 122.9(3) . . . yes C(37) C(36) C(38) 118.4(3) . . . yes N(3) C(37) C(36) 121.0(3) . . . yes N(3) C(37) C(41) 114.9(3) . . . yes C(36) C(37) C(41) 124.0(2) . . . yes C(36) C(38) C(39) 111.5(3) . . . yes C(36) C(38) H(32) 109.4 . . . no C(36) C(38) H(33) 109.1 . . . no C(39) C(38) H(32) 109.0 . . . no C(39) C(38) H(33) 109.2 . . . no H(32) C(38) H(33) 108.7 . . . no C(38) C(39) C(40) 110.3(2) . . . yes C(38) C(39) H(34) 109.9 . . . no C(38) C(39) H(35) 109.4 . . . no C(40) C(39) H(34) 109.9 . . . no C(40) C(39) H(35) 109.2 . . . no H(34) C(39) H(35) 108.1 . . . no C(39) C(40) C(41) 111.1(2) . . . yes C(39) C(40) H(36) 108.6 . . . no C(39) C(40) H(37) 109.2 . . . no C(41) C(40) H(36) 109.4 . . . no C(41) C(40) H(37) 109.4 . . . no H(36) C(40) H(37) 109.1 . . . no C(37) C(41) C(40) 117.0(3) . . . yes C(37) C(41) C(42) 116.7(2) . . . yes C(40) C(41) C(42) 126.3(3) . . . yes Ir(1) C(42) C(41) 116.4(2) . . . yes Ir(1) C(42) C(43) 124.4(2) . . . yes C(41) C(42) C(43) 119.1(2) . . . yes C(42) C(43) C(44) 121.4(3) . . . yes C(42) C(43) C(48) 120.6(2) . . . yes C(44) C(43) C(48) 118.0(3) . . . yes C(43) C(44) C(45) 120.5(3) . . . yes C(43) C(44) H(38) 119.0 . . . no C(45) C(44) H(38) 120.5 . . . no C(44) C(45) C(46) 120.6(3) . . . yes C(44) C(45) H(39) 119.4 . . . no C(46) C(45) H(39) 120.0 . . . no C(45) C(46) C(47) 119.6(3) . . . yes C(45) C(46) H(40) 120.1 . . . no C(47) C(46) H(40) 120.3 . . . no C(46) C(47) C(48) 119.8(3) . . . yes C(46) C(47) H(41) 120.0 . . . no C(48) C(47) H(41) 120.2 . . . no C(43) C(48) C(47) 121.5(2) . . . yes C(43) C(48) H(42) 119.5 . . . no C(47) C(48) H(42) 119.1 . . . no Cl(1) C(49) Cl(2) 110.7(2) . . . yes Cl(1) C(49) Cl(3) 110.3(2) . . . yes Cl(1) C(49) H(43) 108.0 . . . no Cl(2) C(49) Cl(3) 110.9(2) . . . yes Cl(2) C(49) H(43) 108.7 . . . no Cl(3) C(49) H(43) 108.3 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) N(1) C(1) C(2) 175.7(2) . . . . yes Ir(1) N(1) C(5) C(4) -176.3(2) . . . . yes Ir(1) N(1) C(5) C(9) 3.2(3) . . . . yes Ir(1) N(2) C(17) C(18) -173.9(2) . . . . yes Ir(1) N(2) C(21) C(20) 173.3(2) . . . . yes Ir(1) N(2) C(21) C(25) -4.7(3) . . . . yes Ir(1) N(3) C(33) C(34) -174.6(2) . . . . yes Ir(1) N(3) C(37) C(36) 176.7(2) . . . . yes Ir(1) N(3) C(37) C(41) 0.0(3) . . . . yes Ir(1) C(10) C(9) C(5) 1.5(3) . . . . yes Ir(1) C(10) C(9) C(8) -176.8(2) . . . . yes Ir(1) C(10) C(11) C(12) 104.5(3) . . . . yes Ir(1) C(10) C(11) C(16) -74.9(3) . . . . yes Ir(1) C(26) C(25) C(21) -4.0(4) . . . . yes Ir(1) C(26) C(25) C(24) 176.9(3) . . . . yes Ir(1) C(26) C(27) C(28) 109.5(3) . . . . yes Ir(1) C(26) C(27) C(32) -71.7(3) . . . . yes Ir(1) C(42) C(41) C(37) -2.9(3) . . . . yes Ir(1) C(42) C(41) C(40) 179.5(2) . . . . yes Ir(1) C(42) C(43) C(44) 106.2(3) . . . . yes Ir(1) C(42) C(43) C(48) -74.4(3) . . . . yes N(1) Ir(1) N(2) C(17) -0.2(2) . . . . yes N(1) Ir(1) N(2) C(21) -174.6(2) . . . . yes N(1) Ir(1) N(3) C(33) -97.5(2) . . . . yes N(1) Ir(1) N(3) C(37) 87.4(2) . . . . yes N(1) Ir(1) C(10) C(9) 0.2(2) . . . . yes N(1) Ir(1) C(10) C(11) -178.0(2) . . . . yes N(1) Ir(1) C(26) C(25) 21.5(7) . . . . yes N(1) Ir(1) C(26) C(27) -161.3(5) . . . . yes N(1) Ir(1) C(42) C(41) -95.0(2) . . . . yes N(1) Ir(1) C(42) C(43) 82.1(2) . . . . yes N(1) C(1) C(2) C(3) -0.1(4) . . . . yes N(1) C(5) C(4) C(3) 0.3(4) . . . . yes N(1) C(5) C(4) C(6) -179.8(2) . . . . yes N(1) C(5) C(9) C(8) 175.3(2) . . . . yes N(1) C(5) C(9) C(10) -3.1(3) . . . . yes N(2) Ir(1) N(1) C(1) -89.0(2) . . . . yes N(2) Ir(1) N(1) C(5) 86.8(2) . . . . yes N(2) Ir(1) N(3) C(33) -4.0(2) . . . . yes N(2) Ir(1) N(3) C(37) -179.1(2) . . . . yes N(2) Ir(1) C(10) C(9) -92.6(2) . . . . yes N(2) Ir(1) C(10) C(11) 89.1(2) . . . . yes N(2) Ir(1) C(26) C(25) 1.1(2) . . . . yes N(2) Ir(1) C(26) C(27) 178.3(2) . . . . yes N(2) Ir(1) C(42) C(41) 26(1) . . . . yes N(2) Ir(1) C(42) C(43) -156.0(9) . . . . yes N(2) C(17) C(18) C(19) 1.2(5) . . . . yes N(2) C(21) C(20) C(19) 1.6(5) . . . . yes N(2) C(21) C(20) C(22) -178.9(3) . . . . yes N(2) C(21) C(25) C(24) -175.0(3) . . . . yes N(2) C(21) C(25) C(26) 5.8(4) . . . . yes N(3) Ir(1) N(1) C(1) 8.7(2) . . . . yes N(3) Ir(1) N(1) C(5) -175.5(2) . . . . yes N(3) Ir(1) N(2) C(17) -97.7(2) . . . . yes N(3) Ir(1) N(2) C(21) 87.9(2) . . . . yes N(3) Ir(1) C(10) C(9) 57.1(7) . . . . yes N(3) Ir(1) C(10) C(11) -121.2(6) . . . . yes N(3) Ir(1) C(26) C(25) -96.9(2) . . . . yes N(3) Ir(1) C(26) C(27) 80.3(2) . . . . yes N(3) Ir(1) C(42) C(41) 2.2(2) . . . . yes N(3) Ir(1) C(42) C(43) 179.3(2) . . . . yes N(3) C(33) C(34) C(35) -1.3(5) . . . . yes N(3) C(37) C(36) C(35) -1.5(4) . . . . yes N(3) C(37) C(36) C(38) 179.0(2) . . . . yes N(3) C(37) C(41) C(40) 179.7(2) . . . . yes N(3) C(37) C(41) C(42) 1.8(3) . . . . yes C(1) N(1) Ir(1) C(10) -177.6(2) . . . . yes C(1) N(1) Ir(1) C(26) -109.0(6) . . . . yes C(1) N(1) Ir(1) C(42) 86.9(2) . . . . yes C(1) N(1) C(5) C(4) -0.2(4) . . . . yes C(1) N(1) C(5) C(9) 179.2(2) . . . . yes C(1) C(2) C(3) C(4) 0.2(4) . . . . yes C(2) C(1) N(1) C(5) 0.1(4) . . . . yes C(2) C(3) C(4) C(5) -0.3(4) . . . . yes C(2) C(3) C(4) C(6) 179.8(3) . . . . yes C(3) C(4) C(5) C(9) -179.1(2) . . . . yes C(3) C(4) C(6) C(7) 155.0(3) . . . . yes C(4) C(5) C(9) C(8) -5.2(4) . . . . yes C(4) C(5) C(9) C(10) 176.3(2) . . . . yes C(4) C(6) C(7) C(8) 52.5(3) . . . . yes C(5) N(1) Ir(1) C(10) -1.9(2) . . . . yes C(5) N(1) Ir(1) C(26) 66.8(6) . . . . yes C(5) N(1) Ir(1) C(42) -97.3(2) . . . . yes C(5) C(4) C(6) C(7) -24.9(4) . . . . yes C(5) C(9) C(8) C(7) 33.1(3) . . . . yes C(5) C(9) C(10) C(11) 179.8(2) . . . . yes C(6) C(4) C(5) C(9) 0.8(4) . . . . yes C(6) C(7) C(8) C(9) -56.5(3) . . . . yes C(7) C(8) C(9) C(10) -148.7(3) . . . . yes C(8) C(9) C(10) C(11) 1.5(4) . . . . yes C(9) C(10) Ir(1) C(26) -171.0(2) . . . . yes C(9) C(10) Ir(1) C(42) 89.1(2) . . . . yes C(9) C(10) C(11) C(12) -73.6(3) . . . . yes C(9) C(10) C(11) C(16) 107.0(3) . . . . yes C(10) Ir(1) N(2) C(17) 78.5(2) . . . . yes C(10) Ir(1) N(2) C(21) -95.9(2) . . . . yes C(10) Ir(1) N(3) C(33) -153.4(6) . . . . yes C(10) Ir(1) N(3) C(37) 31.5(7) . . . . yes C(10) Ir(1) C(26) C(25) 88.7(2) . . . . yes C(10) Ir(1) C(26) C(27) -94.1(2) . . . . yes C(10) Ir(1) C(42) C(41) -173.8(2) . . . . yes C(10) Ir(1) C(42) C(43) 3.4(2) . . . . yes C(10) C(11) C(12) C(13) -178.6(3) . . . . yes C(10) C(11) C(16) C(15) -179.8(3) . . . . yes C(11) C(10) Ir(1) C(26) 10.8(2) . . . . yes C(11) C(10) Ir(1) C(42) -89.1(2) . . . . yes C(11) C(12) C(13) C(14) -1.4(5) . . . . yes C(11) C(16) C(15) C(14) -1.9(5) . . . . yes C(12) C(11) C(16) C(15) 0.8(4) . . . . yes C(12) C(13) C(14) C(15) 0.3(5) . . . . yes C(13) C(12) C(11) C(16) 0.8(4) . . . . yes C(13) C(14) C(15) C(16) 1.4(5) . . . . yes C(17) N(2) Ir(1) C(26) 176.5(3) . . . . yes C(17) N(2) Ir(1) C(42) -122(1) . . . . yes C(17) N(2) C(21) C(20) -1.6(4) . . . . yes C(17) N(2) C(21) C(25) -179.7(3) . . . . yes C(17) C(18) C(19) C(20) -1.2(5) . . . . yes C(18) C(17) N(2) C(21) 0.2(4) . . . . yes C(18) C(19) C(20) C(21) -0.2(5) . . . . yes C(18) C(19) C(20) C(22) -179.7(3) . . . . yes C(19) C(20) C(21) C(25) 179.5(3) . . . . yes C(19) C(20) C(22) C(23) -162.6(3) . . . . yes C(20) C(21) C(25) C(24) 7.1(5) . . . . yes C(20) C(21) C(25) C(26) -172.2(3) . . . . yes C(20) C(22) C(23) C(24) -42.6(5) . . . . yes C(21) N(2) Ir(1) C(26) 2.1(2) . . . . yes C(21) N(2) Ir(1) C(42) 63(1) . . . . yes C(21) C(20) C(22) C(23) 17.9(5) . . . . yes C(21) C(25) C(24) C(23) -29.5(4) . . . . yes C(21) C(25) C(26) C(27) 178.6(3) . . . . yes C(22) C(20) C(21) C(25) -1.0(5) . . . . yes C(22) C(23) C(24) C(25) 48.5(5) . . . . yes C(23) C(24) C(25) C(26) 149.7(3) . . . . yes C(24) C(25) C(26) C(27) -0.5(5) . . . . yes C(25) C(26) Ir(1) C(42) -174.6(2) . . . . yes C(25) C(26) C(27) C(28) -73.3(4) . . . . yes C(25) C(26) C(27) C(32) 105.5(3) . . . . yes C(26) Ir(1) N(3) C(33) 74.1(2) . . . . yes C(26) Ir(1) N(3) C(37) -101.0(2) . . . . yes C(26) Ir(1) C(42) C(41) 87.6(2) . . . . yes C(26) Ir(1) C(42) C(43) -95.3(2) . . . . yes C(26) C(27) C(28) C(29) 177.4(2) . . . . yes C(26) C(27) C(32) C(31) -178.8(2) . . . . yes C(27) C(26) Ir(1) C(42) 2.6(2) . . . . yes C(27) C(28) C(29) C(30) 1.7(4) . . . . yes C(27) C(32) C(31) C(30) 1.1(4) . . . . yes C(28) C(27) C(32) C(31) 0.1(4) . . . . yes C(28) C(29) C(30) C(31) -0.5(4) . . . . yes C(29) C(28) C(27) C(32) -1.5(4) . . . . yes C(29) C(30) C(31) C(32) -0.9(4) . . . . yes C(33) N(3) Ir(1) C(42) 174.0(2) . . . . yes C(33) N(3) C(37) C(36) 1.1(4) . . . . yes C(33) N(3) C(37) C(41) -175.5(2) . . . . yes C(33) C(34) C(35) C(36) 0.8(4) . . . . yes C(34) C(33) N(3) C(37) 0.3(4) . . . . yes C(34) C(35) C(36) C(37) 0.5(4) . . . . yes C(34) C(35) C(36) C(38) 180.0(3) . . . . yes C(35) C(36) C(37) C(41) 174.9(3) . . . . yes C(35) C(36) C(38) C(39) 155.2(3) . . . . yes C(36) C(37) C(41) C(40) 3.2(4) . . . . yes C(36) C(37) C(41) C(42) -174.7(3) . . . . yes C(36) C(38) C(39) C(40) 55.8(3) . . . . yes C(37) N(3) Ir(1) C(42) -1.1(2) . . . . yes C(37) C(36) C(38) C(39) -25.3(4) . . . . yes C(37) C(41) C(40) C(39) 27.9(3) . . . . yes C(37) C(41) C(42) C(43) 179.8(2) . . . . yes C(38) C(36) C(37) C(41) -4.7(4) . . . . yes C(38) C(39) C(40) C(41) -57.2(3) . . . . yes C(39) C(40) C(41) C(42) -154.5(3) . . . . yes C(40) C(41) C(42) C(43) 2.1(4) . . . . yes C(41) C(42) C(43) C(44) -76.7(3) . . . . yes C(41) C(42) C(43) C(48) 102.7(3) . . . . yes C(42) C(43) C(44) C(45) 179.0(3) . . . . yes C(42) C(43) C(48) C(47) -178.7(3) . . . . yes C(43) C(44) C(45) C(46) 0.1(4) . . . . yes C(43) C(48) C(47) C(46) -0.6(4) . . . . yes C(44) C(43) C(48) C(47) 0.8(4) . . . . yes C(44) C(45) C(46) C(47) 0.1(5) . . . . yes C(45) C(44) C(43) C(48) -0.5(4) . . . . yes C(45) C(46) C(47) C(48) 0.2(4) . . . . yes C(45) C(46) C(47) C(48) 0.2(4) . . . . 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 Cl(2) C(46) 3.349(3) . . ? Cl(2) C(45) 3.405(3) . . ? Cl(2) C(35) 3.587(3) . 8_555 ? C(7) C(29) 3.433(4) . 2_455 ? C(18) C(46) 3.596(4) . 2_455 ? C(19) C(31) 3.544(4) . 8_455 ? C(19) C(46) 3.565(4) . 2_455 ? C(20) C(31) 3.563(4) . 8_455 ? C(23) C(48) 3.546(4) . 6_555 ? #===END #------------------------------------------------------------------------------ data_6b _database_code_depnum_ccdc_archive 'CCDC 616855' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H42 Ir N3 ' _chemical_formula_moiety 'C48 H42 Ir N3 ' _chemical_formula_weight 853.10 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.09(1) _cell_length_b 12.19(2) _cell_length_c 13.86(2) _cell_angle_alpha 82.93(5) _cell_angle_beta 78.73(4) _cell_angle_gamma 88.53(5) _cell_volume 1822(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 16919 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.283 _exptl_absorpt_correction_T_max 0.573 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 17514 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9887 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9887 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). A structural disorder was observed in a ligand unit of complex 6b owing to another conformer with a pseudo-half-chair six-membered alkyl bridge, and the structural analysis containing the disorder unit could be converged by assuming 35% contribution of the minor conformer. C atoms of the disorder unit were refined isotropically and H atoms on their C atoms were not added for the refinement. ; _reflns_number_total 8254 _reflns_number_gt 7427 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0747 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8254 _refine_ls_number_parameters 462 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 1.67 _refine_diff_density_min -0.93 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.23106(1) 0.21452(1) 0.211285(9) 0.01577(4) Uani 1.00 d . . . N(1) N 0.0899(3) 0.1330(3) 0.3068(2) 0.0187(7) Uani 1.00 d . . . N(2) N 0.3566(2) 0.3000(2) 0.1008(2) 0.0156(7) Uani 1.00 d . . . N(3) N 0.3257(3) 0.0703(2) 0.1617(2) 0.0185(7) Uani 1.00 d . . . C(1) C 0.0688(3) 0.0232(3) 0.3158(3) 0.0254(10) Uani 1.00 d . . . C(2) C -0.0357(4) -0.0250(3) 0.3733(3) 0.030(1) Uani 1.00 d . . . C(3) C -0.1241(3) 0.0421(4) 0.4247(3) 0.029(1) Uani 1.00 d . . . C(4) C -0.1045(3) 0.1552(3) 0.4167(3) 0.0234(9) Uani 1.00 d . . . C(5) C -0.1945(3) 0.2327(4) 0.4710(3) 0.032(1) Uani 1.00 d . . . C(6) C -0.1823(3) 0.3512(4) 0.4204(3) 0.030(1) Uani 1.00 d . . . C(7) C -0.0492(3) 0.3914(3) 0.4018(3) 0.0275(10) Uani 1.00 d . . . C(8) C 0.0359(3) 0.3150(3) 0.3409(3) 0.0211(9) Uani 1.00 d . . . C(9) C 0.0053(3) 0.1992(3) 0.3569(2) 0.0193(9) Uani 1.00 d . . . C(10) C 0.1413(3) 0.3424(3) 0.2745(2) 0.0174(8) Uani 1.00 d . . . C(11) C 0.1796(3) 0.4595(3) 0.2535(3) 0.0194(9) Uani 1.00 d . . . C(12) C 0.1455(3) 0.5297(3) 0.1750(3) 0.0263(10) Uani 1.00 d . . . C(13) C 0.1694(3) 0.6428(3) 0.1635(3) 0.029(1) Uani 1.00 d . . . C(14) C 0.2293(3) 0.6881(3) 0.2283(3) 0.030(1) Uani 1.00 d . . . C(15) C 0.2666(4) 0.6191(3) 0.3030(3) 0.028(1) Uani 1.00 d . . . C(16) C 0.2419(3) 0.5066(3) 0.3163(3) 0.0232(9) Uani 1.00 d . . . C(17) C 0.4769(3) 0.3133(3) 0.1026(3) 0.0181(8) Uani 1.00 d . . . C(18) C 0.5595(3) 0.3589(3) 0.0210(3) 0.0191(9) Uani 1.00 d . . . C(19) C 0.5188(3) 0.3974(3) -0.0656(2) 0.0197(9) Uani 1.00 d . . . C(20) C 0.3961(3) 0.3863(3) -0.0686(3) 0.0213(9) Uani 1.00 d . . . C(21) C 0.3459(3) 0.4267(3) -0.1608(3) 0.0272(8) Uiso 1.00 d . . . C(22) C 0.2258(5) 0.3642(5) -0.1667(4) 0.024(1) Uiso 0.65 d P . . C(23) C 0.1297(6) 0.3612(6) -0.0697(5) 0.026(2) Uiso 0.65 d P . . C(24) C 0.1886(3) 0.3090(3) 0.0164(3) 0.0251(10) Uani 1.00 d . . . C(25) C 0.3165(3) 0.3347(3) 0.0144(2) 0.0193(9) Uani 1.00 d . . . C(26) C 0.1304(3) 0.2475(3) 0.0985(3) 0.0222(9) Uani 1.00 d . . . C(27) C 0.0001(3) 0.2131(3) 0.1120(3) 0.0238(9) Uani 1.00 d . . . C(28) C -0.0947(3) 0.2844(3) 0.1458(3) 0.028(1) Uani 1.00 d . . . C(29) C -0.2173(3) 0.2498(3) 0.1651(3) 0.028(1) Uani 1.00 d . . . C(30) C -0.2464(3) 0.1449(4) 0.1527(3) 0.028(1) Uani 1.00 d . . . C(31) C -0.1529(4) 0.0729(4) 0.1187(3) 0.035(1) Uani 1.00 d . . . C(32) C -0.0308(3) 0.1063(4) 0.0987(3) 0.032(1) Uani 1.00 d . . . C(33) C 0.3109(3) 0.0212(3) 0.0830(3) 0.0231(9) Uani 1.00 d . . . C(34) C 0.3733(3) -0.0723(3) 0.0575(3) 0.0257(10) Uani 1.00 d . . . C(35) C 0.4567(3) -0.1177(3) 0.1136(3) 0.0262(10) Uani 1.00 d . . . C(36) C 0.4748(3) -0.0686(3) 0.1949(3) 0.0211(9) Uani 1.00 d . . . C(37) C 0.5602(4) -0.1170(3) 0.2615(3) 0.028(1) Uani 1.00 d . . . C(38) C 0.5201(4) -0.0874(3) 0.3666(3) 0.031(1) Uani 1.00 d . . . C(39) C 0.5078(4) 0.0373(3) 0.3658(3) 0.0264(10) Uani 1.00 d . . . C(40) C 0.4202(3) 0.0858(3) 0.3004(2) 0.0182(8) Uani 1.00 d . . . C(41) C 0.4082(3) 0.0272(3) 0.2175(2) 0.0183(8) Uani 1.00 d . . . C(42) C 0.3480(3) 0.1769(3) 0.3129(2) 0.0175(8) Uani 1.00 d . . . C(43) C 0.3536(3) 0.2403(3) 0.3976(2) 0.0163(8) Uani 1.00 d . . . C(44) C 0.2513(3) 0.2450(3) 0.4732(2) 0.0193(8) Uani 1.00 d . . . C(45) C 0.2551(3) 0.3055(3) 0.5519(3) 0.0229(9) Uani 1.00 d . . . C(46) C 0.3601(4) 0.3634(3) 0.5557(3) 0.0244(9) Uani 1.00 d . . . C(47) C 0.4621(3) 0.3588(3) 0.4795(3) 0.0256(10) Uani 1.00 d . . . C(48) C 0.4594(3) 0.2976(3) 0.4023(3) 0.0210(9) Uani 1.00 d . . . C(49) C 0.217(1) 0.437(1) -0.1419(9) 0.038(3) Uiso 0.35 d P . . C(50) C 0.150(1) 0.333(1) -0.0859(10) 0.030(3) Uiso 0.35 d P . . H(1) H -0.0754 0.3585 0.1563 0.0328 Uiso 1.00 calc . . . H(2) H -0.2818 0.3006 0.1864 0.0324 Uiso 1.00 calc . . . H(3) H -0.3315 0.1221 0.1669 0.0352 Uiso 1.00 calc . . . H(4) H -0.1743 -0.0013 0.1090 0.0418 Uiso 1.00 calc . . . H(5) H 0.0350 0.0542 0.0764 0.0400 Uiso 1.00 calc . . . H(6) H 0.1778 0.2063 0.4711 0.0229 Uiso 1.00 calc . . . H(7) H 0.1841 0.3069 0.6038 0.0270 Uiso 1.00 calc . . . H(8) H 0.3617 0.4056 0.6091 0.0280 Uiso 1.00 calc . . . H(9) H 0.5360 0.3983 0.4813 0.0310 Uiso 1.00 calc . . . H(10) H 0.5319 0.2926 0.3515 0.0263 Uiso 1.00 calc . . . H(11) H 0.1063 0.4989 0.1288 0.0310 Uiso 1.00 calc . . . H(12) H 0.1437 0.6887 0.1091 0.0365 Uiso 1.00 calc . . . H(13) H 0.2439 0.7664 0.2213 0.0352 Uiso 1.00 calc . . . H(14) H 0.3115 0.6489 0.3467 0.0351 Uiso 1.00 calc . . . H(15) H 0.2679 0.4606 0.3699 0.0276 Uiso 1.00 calc . . . H(16) H 0.2536 0.0537 0.0442 0.0274 Uiso 1.00 calc . . . H(17) H 0.3589 -0.1056 0.0016 0.0300 Uiso 1.00 calc . . . H(18) H 0.5021 -0.1832 0.0972 0.0300 Uiso 1.00 calc . . . H(19) H 0.5056 0.2900 0.1636 0.0231 Uiso 1.00 calc . . . H(20) H 0.6451 0.3641 0.0237 0.0226 Uiso 1.00 calc . . . H(21) H 0.5759 0.4297 -0.1235 0.0250 Uiso 1.00 calc . . . H(22) H 0.1293 -0.0223 0.2808 0.0289 Uiso 1.00 calc . . . H(23) H -0.0477 -0.1037 0.3785 0.0360 Uiso 1.00 calc . . . H(24) H -0.1980 0.0102 0.4651 0.0342 Uiso 1.00 calc . . . H(25) H -0.2752 0.2063 0.4758 0.0392 Uiso 1.00 calc . . . H(26) H -0.1780 0.2311 0.5370 0.0392 Uiso 1.00 calc . . . H(27) H -0.2080 0.3553 0.3578 0.0381 Uiso 1.00 calc . . . H(28) H -0.2345 0.3993 0.4603 0.0381 Uiso 1.00 calc . . . H(29) H -0.0421 0.4653 0.3688 0.0327 Uiso 1.00 calc . . . H(30) H -0.0242 0.3923 0.4649 0.0327 Uiso 1.00 calc . . . H(31) H 0.5616 -0.1956 0.2622 0.0329 Uiso 1.00 calc . . . H(32) H 0.6414 -0.0895 0.2345 0.0329 Uiso 1.00 calc . . . H(33) H 0.4424 -0.1209 0.3959 0.0383 Uiso 1.00 calc . . . H(34) H 0.5789 -0.1147 0.4058 0.0383 Uiso 1.00 calc . . . H(35) H 0.4793 0.0544 0.4317 0.0341 Uiso 1.00 calc . . . H(36) H 0.5875 0.0698 0.3414 0.0341 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) 0.01567(8) 0.01515(8) 0.01626(8) 0.00036(5) -0.00274(5) -0.00160(5) N(1) 0.019(1) 0.019(2) 0.018(1) 0.001(1) -0.004(1) -0.002(1) N(2) 0.016(1) 0.015(1) 0.017(1) 0.002(1) -0.005(1) -0.004(1) N(3) 0.023(1) 0.017(2) 0.015(1) -0.002(1) -0.003(1) -0.003(1) C(1) 0.028(2) 0.021(2) 0.025(2) -0.002(2) -0.001(1) -0.003(2) C(2) 0.036(2) 0.019(2) 0.032(2) -0.006(2) -0.003(2) 0.002(2) C(3) 0.024(2) 0.033(2) 0.026(2) -0.009(2) 0.000(1) 0.003(2) C(4) 0.021(2) 0.026(2) 0.022(2) 0.001(2) -0.003(1) -0.001(2) C(5) 0.021(2) 0.033(2) 0.037(2) 0.003(2) 0.006(2) 0.001(2) C(6) 0.022(2) 0.032(2) 0.033(2) 0.008(2) 0.000(2) -0.001(2) C(7) 0.025(2) 0.023(2) 0.031(2) 0.003(2) 0.003(2) -0.003(2) C(8) 0.023(2) 0.018(2) 0.023(2) -0.001(1) -0.004(1) -0.001(1) C(9) 0.018(2) 0.022(2) 0.018(2) 0.003(1) -0.007(1) -0.001(1) C(10) 0.018(2) 0.019(2) 0.018(2) 0.005(1) -0.011(1) -0.002(1) C(11) 0.017(2) 0.017(2) 0.022(2) 0.004(1) 0.001(1) -0.002(1) C(12) 0.021(2) 0.025(2) 0.032(2) 0.000(2) -0.006(1) 0.003(2) C(13) 0.022(2) 0.022(2) 0.040(2) 0.004(2) -0.004(2) 0.008(2) C(14) 0.025(2) 0.016(2) 0.041(2) 0.000(2) 0.008(2) -0.001(2) C(15) 0.032(2) 0.022(2) 0.028(2) -0.003(2) 0.001(2) -0.005(2) C(16) 0.030(2) 0.020(2) 0.019(2) -0.001(2) -0.003(1) -0.002(1) C(17) 0.016(2) 0.017(2) 0.021(2) 0.003(1) -0.005(1) -0.004(1) C(18) 0.018(2) 0.016(2) 0.023(2) 0.002(1) -0.002(1) -0.006(1) C(19) 0.024(2) 0.014(2) 0.020(2) 0.003(1) 0.000(1) -0.005(1) C(20) 0.029(2) 0.015(2) 0.019(2) 0.001(1) -0.002(1) -0.002(1) C(24) 0.020(2) 0.029(2) 0.027(2) 0.003(2) -0.010(1) 0.001(2) C(25) 0.026(2) 0.018(2) 0.015(2) 0.001(1) -0.005(1) -0.004(1) C(26) 0.020(2) 0.026(2) 0.022(2) 0.002(2) -0.009(1) -0.001(1) C(27) 0.020(2) 0.026(2) 0.027(2) 0.001(2) -0.010(1) 0.000(2) C(28) 0.027(2) 0.024(2) 0.035(2) -0.003(2) -0.012(2) 0.001(2) C(29) 0.024(2) 0.031(2) 0.029(2) 0.003(2) -0.009(2) -0.003(2) C(30) 0.020(2) 0.041(2) 0.027(2) -0.004(2) -0.009(1) -0.002(2) C(31) 0.028(2) 0.034(2) 0.046(3) -0.005(2) -0.009(2) -0.011(2) C(32) 0.023(2) 0.035(2) 0.043(2) 0.003(2) -0.009(2) -0.015(2) C(33) 0.026(2) 0.024(2) 0.020(2) -0.006(2) -0.004(1) -0.004(1) C(34) 0.030(2) 0.025(2) 0.023(2) -0.005(2) -0.003(1) -0.009(2) C(35) 0.030(2) 0.016(2) 0.030(2) 0.000(2) 0.003(2) -0.006(2) C(36) 0.019(2) 0.017(2) 0.025(2) 0.001(1) 0.000(1) 0.001(1) C(37) 0.030(2) 0.020(2) 0.031(2) 0.011(2) -0.002(2) -0.003(2) C(38) 0.038(2) 0.025(2) 0.028(2) 0.015(2) -0.007(2) 0.002(2) C(39) 0.033(2) 0.027(2) 0.022(2) 0.016(2) -0.010(2) -0.006(2) C(40) 0.021(2) 0.017(2) 0.016(2) 0.002(1) -0.004(1) 0.000(1) C(41) 0.020(2) 0.017(2) 0.016(2) -0.002(1) 0.001(1) -0.001(1) C(42) 0.019(2) 0.015(2) 0.017(2) 0.000(1) -0.001(1) 0.000(1) C(43) 0.019(2) 0.015(2) 0.015(2) 0.005(1) -0.008(1) 0.002(1) C(44) 0.022(2) 0.017(2) 0.018(2) 0.001(1) -0.004(1) 0.001(1) C(45) 0.030(2) 0.021(2) 0.017(2) 0.004(2) -0.002(1) -0.002(1) C(46) 0.036(2) 0.019(2) 0.021(2) 0.003(2) -0.009(1) -0.005(1) C(47) 0.025(2) 0.022(2) 0.031(2) -0.001(2) -0.008(2) -0.003(2) C(48) 0.018(2) 0.021(2) 0.024(2) 0.006(1) -0.003(1) -0.002(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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) N(1) 2.033(3) . . yes Ir(1) N(2) 2.053(3) . . yes Ir(1) N(3) 2.141(3) . . yes Ir(1) C(10) 2.026(3) . . yes Ir(1) C(26) 2.086(4) . . yes Ir(1) C(42) 2.097(4) . . yes N(1) C(1) 1.351(5) . . yes N(1) C(9) 1.363(4) . . yes N(2) C(17) 1.353(4) . . yes N(2) C(25) 1.373(4) . . yes N(3) C(33) 1.344(4) . . yes N(3) C(41) 1.365(4) . . yes C(1) C(2) 1.372(5) . . yes C(1) H(22) 0.955 . . no C(2) C(3) 1.403(6) . . yes C(2) H(23) 0.963 . . no C(3) C(4) 1.388(6) . . yes C(3) H(24) 0.959 . . no C(4) C(5) 1.512(5) . . yes C(4) C(9) 1.410(5) . . yes C(5) C(6) 1.522(6) . . yes C(5) H(25) 0.946 . . no C(5) H(26) 0.964 . . no C(6) C(7) 1.530(6) . . yes C(6) H(27) 0.960 . . no C(6) H(28) 0.960 . . no C(7) C(8) 1.519(5) . . yes C(7) H(29) 0.957 . . no C(7) H(30) 0.968 . . no C(8) C(9) 1.440(5) . . yes C(8) C(10) 1.359(5) . . yes C(10) C(11) 1.478(5) . . yes C(11) C(12) 1.405(5) . . yes C(11) C(16) 1.392(5) . . yes C(12) C(13) 1.393(6) . . yes C(12) H(11) 0.957 . . no C(13) C(14) 1.388(6) . . yes C(13) H(12) 0.967 . . no C(14) C(15) 1.373(6) . . yes C(14) H(13) 0.962 . . no C(15) C(16) 1.388(5) . . yes C(15) H(14) 0.963 . . no C(16) H(15) 0.960 . . no C(17) C(18) 1.376(5) . . yes C(17) H(19) 0.968 . . no C(18) C(19) 1.388(5) . . yes C(18) H(20) 0.961 . . no C(19) C(20) 1.380(5) . . yes C(19) H(21) 0.967 . . no C(20) C(21) 1.514(5) . . yes C(20) C(25) 1.397(5) . . yes C(21) C(22) 1.571(7) . . yes C(21) C(49) 1.41(1) . . yes C(22) C(23) 1.541(9) . . yes C(22) C(49) 0.99(1) . . yes C(22) C(50) 1.28(1) . . yes C(23) C(24) 1.533(7) . . yes C(23) C(49) 1.49(2) . . yes C(23) C(50) 0.47(1) . . yes C(24) C(25) 1.454(5) . . yes C(24) C(26) 1.343(5) . . yes C(24) C(50) 1.55(1) . . yes C(26) C(27) 1.485(5) . . yes C(27) C(28) 1.393(5) . . yes C(27) C(32) 1.398(6) . . yes C(28) C(29) 1.399(6) . . yes C(28) H(1) 0.968 . . no C(29) C(30) 1.364(6) . . yes C(29) H(2) 0.961 . . no C(30) C(31) 1.390(6) . . yes C(30) H(3) 0.967 . . no C(31) C(32) 1.388(6) . . yes C(31) H(4) 0.972 . . no C(32) H(5) 0.983 . . no C(33) C(34) 1.365(5) . . yes C(33) H(16) 0.959 . . no C(34) C(35) 1.384(6) . . yes C(34) H(17) 0.960 . . no C(35) C(36) 1.389(5) . . yes C(35) H(18) 0.960 . . no C(36) C(37) 1.508(5) . . yes C(36) C(41) 1.400(5) . . yes C(37) C(38) 1.522(5) . . yes C(37) H(31) 0.957 . . no C(37) H(32) 0.957 . . no C(38) C(39) 1.521(6) . . yes C(38) H(33) 0.956 . . no C(38) H(34) 0.956 . . no C(39) C(40) 1.515(5) . . yes C(39) H(35) 0.952 . . no C(39) H(36) 0.960 . . no C(40) C(41) 1.455(5) . . yes C(40) C(42) 1.360(5) . . yes C(42) C(43) 1.495(5) . . yes C(43) C(44) 1.391(5) . . yes C(43) C(48) 1.397(5) . . yes C(44) C(45) 1.397(5) . . yes C(44) H(6) 0.959 . . no C(45) C(46) 1.390(6) . . yes C(45) H(7) 0.959 . . no C(46) C(47) 1.394(5) . . yes C(46) H(8) 0.954 . . no C(47) C(48) 1.383(5) . . yes C(47) H(9) 0.967 . . no C(48) H(10) 0.966 . . no C(49) C(50) 1.53(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ir(1) N(2) 171.8(1) . . . yes N(1) Ir(1) N(3) 96.4(1) . . . yes N(1) Ir(1) C(10) 79.4(1) . . . yes N(1) Ir(1) C(26) 93.5(1) . . . yes N(1) Ir(1) C(42) 90.9(1) . . . yes N(2) Ir(1) N(3) 84.9(1) . . . yes N(2) Ir(1) C(10) 100.0(1) . . . yes N(2) Ir(1) C(26) 78.2(1) . . . yes N(2) Ir(1) C(42) 97.3(1) . . . yes N(3) Ir(1) C(10) 173.3(1) . . . yes N(3) Ir(1) C(26) 97.8(1) . . . yes N(3) Ir(1) C(42) 77.5(1) . . . yes C(10) Ir(1) C(26) 87.7(1) . . . yes C(10) Ir(1) C(42) 97.3(1) . . . yes C(26) Ir(1) C(42) 173.9(1) . . . yes Ir(1) N(1) C(1) 125.3(2) . . . yes Ir(1) N(1) C(9) 115.0(2) . . . yes C(1) N(1) C(9) 119.3(3) . . . yes Ir(1) N(2) C(17) 125.4(2) . . . yes Ir(1) N(2) C(25) 115.9(2) . . . yes C(17) N(2) C(25) 118.3(3) . . . yes Ir(1) N(3) C(33) 126.3(2) . . . yes Ir(1) N(3) C(41) 114.4(2) . . . yes C(33) N(3) C(41) 119.3(3) . . . yes N(1) C(1) C(2) 122.5(3) . . . yes N(1) C(1) H(22) 118.4 . . . no C(2) C(1) H(22) 119.1 . . . no C(1) C(2) C(3) 118.8(4) . . . yes C(1) C(2) H(23) 120.5 . . . no C(3) C(2) H(23) 120.7 . . . no C(2) C(3) C(4) 119.8(4) . . . yes C(2) C(3) H(24) 120.2 . . . no C(4) C(3) H(24) 120.0 . . . no C(3) C(4) C(5) 122.9(3) . . . yes C(3) C(4) C(9) 118.4(3) . . . yes C(5) C(4) C(9) 118.7(4) . . . yes C(4) C(5) C(6) 112.4(3) . . . yes C(4) C(5) H(25) 108.7 . . . no C(4) C(5) H(26) 107.8 . . . no C(6) C(5) H(25) 110.4 . . . no C(6) C(5) H(26) 108.9 . . . no H(25) C(5) H(26) 108.6 . . . no C(5) C(6) C(7) 111.3(3) . . . yes C(5) C(6) H(27) 109.6 . . . no C(5) C(6) H(28) 110.1 . . . no C(7) C(6) H(27) 108.4 . . . no C(7) C(6) H(28) 109.6 . . . no H(27) C(6) H(28) 107.8 . . . no C(6) C(7) C(8) 110.6(3) . . . yes C(6) C(7) H(29) 110.7 . . . no C(6) C(7) H(30) 109.0 . . . no C(8) C(7) H(29) 109.9 . . . no C(8) C(7) H(30) 109.1 . . . no H(29) C(7) H(30) 107.4 . . . no C(7) C(8) C(9) 117.1(3) . . . yes C(7) C(8) C(10) 127.5(3) . . . yes C(9) C(8) C(10) 115.3(3) . . . yes N(1) C(9) C(4) 121.1(3) . . . yes N(1) C(9) C(8) 114.8(3) . . . yes C(4) C(9) C(8) 124.0(3) . . . yes Ir(1) C(10) C(8) 115.2(3) . . . yes Ir(1) C(10) C(11) 125.9(2) . . . yes C(8) C(10) C(11) 118.9(3) . . . yes C(10) C(11) C(12) 121.4(3) . . . yes C(10) C(11) C(16) 120.9(3) . . . yes C(12) C(11) C(16) 117.5(3) . . . yes C(11) C(12) C(13) 120.7(4) . . . yes C(11) C(12) H(11) 119.2 . . . no C(13) C(12) H(11) 120.1 . . . no C(12) C(13) C(14) 120.7(4) . . . yes C(12) C(13) H(12) 118.4 . . . no C(14) C(13) H(12) 120.9 . . . no C(13) C(14) C(15) 118.7(4) . . . yes C(13) C(14) H(13) 120.7 . . . no C(15) C(14) H(13) 120.6 . . . no C(14) C(15) C(16) 121.2(4) . . . yes C(14) C(15) H(14) 119.7 . . . no C(16) C(15) H(14) 119.2 . . . no C(11) C(16) C(15) 121.2(3) . . . yes C(11) C(16) H(15) 119.6 . . . no C(15) C(16) H(15) 119.3 . . . no N(2) C(17) C(18) 122.3(3) . . . yes N(2) C(17) H(19) 118.7 . . . no C(18) C(17) H(19) 119.0 . . . no C(17) C(18) C(19) 119.7(3) . . . yes C(17) C(18) H(20) 120.4 . . . no C(19) C(18) H(20) 119.9 . . . no C(18) C(19) C(20) 119.0(3) . . . yes C(18) C(19) H(21) 120.6 . . . no C(20) C(19) H(21) 120.4 . . . no C(19) C(20) C(21) 121.5(3) . . . yes C(19) C(20) C(25) 119.4(3) . . . yes C(21) C(20) C(25) 119.0(3) . . . yes C(20) C(21) C(22) 112.8(4) . . . yes C(20) C(21) C(49) 112.9(6) . . . yes C(22) C(21) C(49) 38.2(6) . . . yes C(21) C(22) C(23) 111.8(5) . . . yes C(21) C(22) C(49) 61.9(8) . . . yes C(21) C(22) C(50) 118.7(7) . . . yes C(23) C(22) C(49) 68.4(9) . . . yes C(23) C(22) C(50) 15.9(7) . . . yes C(49) C(22) C(50) 83(1) . . . yes C(22) C(23) C(24) 108.8(5) . . . yes C(22) C(23) C(49) 37.9(5) . . . yes C(22) C(23) C(50) 48(2) . . . yes C(24) C(23) C(49) 111.5(7) . . . yes C(24) C(23) C(50) 83(2) . . . yes C(49) C(23) C(50) 85(2) . . . yes C(23) C(24) C(25) 118.2(4) . . . yes C(23) C(24) C(26) 125.9(4) . . . yes C(23) C(24) C(50) 17.4(5) . . . yes C(25) C(24) C(26) 115.7(3) . . . yes C(25) C(24) C(50) 113.9(6) . . . yes C(26) C(24) C(50) 128.5(6) . . . yes N(2) C(25) C(20) 121.2(3) . . . yes N(2) C(25) C(24) 114.6(3) . . . yes C(20) C(25) C(24) 124.1(3) . . . yes Ir(1) C(26) C(24) 115.3(3) . . . yes Ir(1) C(26) C(27) 122.0(3) . . . yes C(24) C(26) C(27) 122.5(3) . . . yes C(26) C(27) C(28) 120.4(4) . . . yes C(26) C(27) C(32) 121.3(3) . . . yes C(28) C(27) C(32) 118.1(4) . . . yes C(27) C(28) C(29) 120.7(4) . . . yes C(27) C(28) H(1) 119.5 . . . no C(29) C(28) H(1) 119.8 . . . no C(28) C(29) C(30) 120.7(3) . . . yes C(28) C(29) H(2) 119.6 . . . no C(30) C(29) H(2) 119.7 . . . no C(29) C(30) C(31) 119.4(4) . . . yes C(29) C(30) H(3) 119.7 . . . no C(31) C(30) H(3) 121.0 . . . no C(30) C(31) C(32) 120.6(4) . . . yes C(30) C(31) H(4) 118.9 . . . no C(32) C(31) H(4) 120.5 . . . no C(27) C(32) C(31) 120.6(4) . . . yes C(27) C(32) H(5) 119.3 . . . no C(31) C(32) H(5) 120.1 . . . no N(3) C(33) C(34) 122.6(3) . . . yes N(3) C(33) H(16) 117.8 . . . no C(34) C(33) H(16) 119.6 . . . no C(33) C(34) C(35) 119.0(3) . . . yes C(33) C(34) H(17) 120.1 . . . no C(35) C(34) H(17) 121.0 . . . no C(34) C(35) C(36) 119.8(3) . . . yes C(34) C(35) H(18) 120.7 . . . no C(36) C(35) H(18) 119.5 . . . no C(35) C(36) C(37) 122.3(3) . . . yes C(35) C(36) C(41) 118.7(3) . . . yes C(37) C(36) C(41) 119.0(3) . . . yes C(36) C(37) C(38) 111.8(3) . . . yes C(36) C(37) H(31) 108.6 . . . no C(36) C(37) H(32) 108.7 . . . no C(38) C(37) H(31) 109.9 . . . no C(38) C(37) H(32) 109.5 . . . no H(31) C(37) H(32) 108.3 . . . no C(37) C(38) C(39) 110.4(3) . . . yes C(37) C(38) H(33) 109.6 . . . no C(37) C(38) H(34) 109.8 . . . no C(39) C(38) H(33) 108.9 . . . no C(39) C(38) H(34) 109.6 . . . no H(33) C(38) H(34) 108.5 . . . no C(38) C(39) C(40) 111.8(3) . . . yes C(38) C(39) H(35) 109.5 . . . no C(38) C(39) H(36) 108.4 . . . no C(40) C(39) H(35) 109.5 . . . no C(40) C(39) H(36) 109.1 . . . no H(35) C(39) H(36) 108.4 . . . no C(39) C(40) C(41) 117.0(3) . . . yes C(39) C(40) C(42) 126.8(3) . . . yes C(41) C(40) C(42) 116.1(3) . . . yes N(3) C(41) C(36) 120.6(3) . . . yes N(3) C(41) C(40) 116.0(3) . . . yes C(36) C(41) C(40) 123.4(3) . . . yes Ir(1) C(42) C(40) 116.1(2) . . . yes Ir(1) C(42) C(43) 124.7(2) . . . yes C(40) C(42) C(43) 119.2(3) . . . yes C(42) C(43) C(44) 120.1(3) . . . yes C(42) C(43) C(48) 121.5(3) . . . yes C(44) C(43) C(48) 118.4(3) . . . yes C(43) C(44) C(45) 120.5(3) . . . yes C(43) C(44) H(6) 119.4 . . . no C(45) C(44) H(6) 120.1 . . . no C(44) C(45) C(46) 121.0(3) . . . yes C(44) C(45) H(7) 119.2 . . . no C(46) C(45) H(7) 119.8 . . . no C(45) C(46) C(47) 118.3(3) . . . yes C(45) C(46) H(8) 120.6 . . . no C(47) C(46) H(8) 121.1 . . . no C(46) C(47) C(48) 121.0(4) . . . yes C(46) C(47) H(9) 119.3 . . . no C(48) C(47) H(9) 119.8 . . . no C(43) C(48) C(47) 120.9(3) . . . yes C(43) C(48) H(10) 119.1 . . . no C(47) C(48) H(10) 120.0 . . . no C(21) C(49) C(22) 79.9(9) . . . yes C(21) C(49) C(23) 125.3(10) . . . yes C(21) C(49) C(50) 113(1) . . . yes C(22) C(49) C(23) 73.7(10) . . . yes C(22) C(49) C(50) 56.4(9) . . . yes C(23) C(49) C(50) 17.7(5) . . . yes C(22) C(50) C(23) 115(2) . . . yes C(22) C(50) C(24) 123(1) . . . yes C(22) C(50) C(49) 39.8(6) . . . yes C(23) C(50) C(24) 79(2) . . . yes C(23) C(50) C(49) 76(2) . . . yes C(24) C(50) C(49) 108.5(10) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir(1) N(1) C(1) C(2) -172.3(3) . . . . yes Ir(1) N(1) C(9) C(4) 172.6(3) . . . . yes Ir(1) N(1) C(9) C(8) -5.6(4) . . . . yes Ir(1) N(2) C(17) C(18) 171.2(2) . . . . yes Ir(1) N(2) C(25) C(20) -175.1(3) . . . . yes Ir(1) N(2) C(25) C(24) 2.5(4) . . . . yes Ir(1) N(3) C(33) C(34) -178.6(3) . . . . yes Ir(1) N(3) C(41) C(36) 178.6(3) . . . . yes Ir(1) N(3) C(41) C(40) -0.6(4) . . . . yes Ir(1) C(10) C(8) C(7) 178.3(3) . . . . yes Ir(1) C(10) C(8) C(9) 0.8(4) . . . . yes Ir(1) C(10) C(11) C(12) 86.5(4) . . . . yes Ir(1) C(10) C(11) C(16) -99.1(4) . . . . yes Ir(1) C(26) C(24) C(23) -169.2(4) . . . . yes Ir(1) C(26) C(24) C(25) 5.5(4) . . . . yes Ir(1) C(26) C(24) C(50) 169.2(7) . . . . yes Ir(1) C(26) C(27) C(28) 91.3(4) . . . . yes Ir(1) C(26) C(27) C(32) -83.6(4) . . . . yes Ir(1) C(42) C(40) C(39) -176.8(3) . . . . yes Ir(1) C(42) C(40) C(41) 0.8(4) . . . . yes Ir(1) C(42) C(43) C(44) 63.2(4) . . . . yes Ir(1) C(42) C(43) C(48) -115.6(3) . . . . yes N(1) Ir(1) N(2) C(17) -172.2(6) . . . . yes N(1) Ir(1) N(2) C(25) -0.1(8) . . . . yes N(1) Ir(1) N(3) C(33) 91.5(3) . . . . yes N(1) Ir(1) N(3) C(41) -88.7(3) . . . . yes N(1) Ir(1) C(10) C(8) -2.9(2) . . . . yes N(1) Ir(1) C(10) C(11) 178.0(3) . . . . yes N(1) Ir(1) C(26) C(24) 176.7(3) . . . . yes N(1) Ir(1) C(26) C(27) 1.6(3) . . . . yes N(1) Ir(1) C(42) C(40) 95.5(3) . . . . yes N(1) Ir(1) C(42) C(43) -82.6(3) . . . . yes N(1) C(1) C(2) C(3) 0.1(6) . . . . yes N(1) C(9) C(4) C(3) 0.9(5) . . . . yes N(1) C(9) C(4) C(5) 179.6(3) . . . . yes N(1) C(9) C(8) C(7) -174.6(3) . . . . yes N(1) C(9) C(8) C(10) 3.2(4) . . . . yes N(2) Ir(1) N(1) C(1) 91.1(8) . . . . yes N(2) Ir(1) N(1) C(9) -81.9(8) . . . . yes N(2) Ir(1) N(3) C(33) -80.3(3) . . . . yes N(2) Ir(1) N(3) C(41) 99.5(3) . . . . yes N(2) Ir(1) C(10) C(8) 168.8(2) . . . . yes N(2) Ir(1) C(10) C(11) -10.4(3) . . . . yes N(2) Ir(1) C(26) C(24) -3.2(3) . . . . yes N(2) Ir(1) C(26) C(27) -178.3(3) . . . . yes N(2) Ir(1) C(42) C(40) -84.0(3) . . . . yes N(2) Ir(1) C(42) C(43) 98.0(3) . . . . yes N(2) C(17) C(18) C(19) 2.8(5) . . . . yes N(2) C(25) C(20) C(19) 3.5(5) . . . . yes N(2) C(25) C(20) C(21) -177.8(3) . . . . yes N(2) C(25) C(24) C(23) 169.8(4) . . . . yes N(2) C(25) C(24) C(26) -5.3(5) . . . . yes N(2) C(25) C(24) C(50) -171.3(6) . . . . yes N(3) Ir(1) N(1) C(1) -7.6(3) . . . . yes N(3) Ir(1) N(1) C(9) 179.4(2) . . . . yes N(3) Ir(1) N(2) C(17) -72.7(3) . . . . yes N(3) Ir(1) N(2) C(25) 99.4(2) . . . . yes N(3) Ir(1) C(10) C(8) -54(1) . . . . yes N(3) Ir(1) C(10) C(11) 126.4(10) . . . . yes N(3) Ir(1) C(26) C(24) -86.4(3) . . . . yes N(3) Ir(1) C(26) C(27) 98.5(3) . . . . yes N(3) Ir(1) C(42) C(40) -0.9(3) . . . . yes N(3) Ir(1) C(42) C(43) -178.9(3) . . . . yes N(3) C(33) C(34) C(35) -1.1(6) . . . . yes N(3) C(41) C(36) C(35) 1.2(5) . . . . yes N(3) C(41) C(36) C(37) -176.8(3) . . . . yes N(3) C(41) C(40) C(39) 177.8(3) . . . . yes N(3) C(41) C(40) C(42) -0.1(5) . . . . yes C(1) N(1) Ir(1) C(10) 177.7(3) . . . . yes C(1) N(1) Ir(1) C(26) 90.7(3) . . . . yes C(1) N(1) Ir(1) C(42) -85.1(3) . . . . yes C(1) N(1) C(9) C(4) -0.9(5) . . . . yes C(1) N(1) C(9) C(8) -179.0(3) . . . . yes C(1) C(2) C(3) C(4) -0.1(6) . . . . yes C(2) C(1) N(1) C(9) 0.4(5) . . . . yes C(2) C(3) C(4) C(5) -179.0(4) . . . . yes C(2) C(3) C(4) C(9) -0.4(6) . . . . yes C(3) C(4) C(5) C(6) -156.2(4) . . . . yes C(3) C(4) C(9) C(8) 178.8(3) . . . . yes C(4) C(5) C(6) C(7) -52.4(5) . . . . yes C(4) C(9) C(8) C(7) 7.3(5) . . . . yes C(4) C(9) C(8) C(10) -174.9(3) . . . . yes C(5) C(4) C(9) C(8) -2.5(5) . . . . yes C(5) C(6) C(7) C(8) 56.6(4) . . . . yes C(6) C(5) C(4) C(9) 25.1(5) . . . . yes C(6) C(7) C(8) C(9) -34.0(4) . . . . yes C(6) C(7) C(8) C(10) 148.5(4) . . . . yes C(7) C(8) C(10) C(11) -2.5(5) . . . . yes C(8) C(10) Ir(1) C(26) 91.2(3) . . . . yes C(8) C(10) Ir(1) C(42) -92.4(3) . . . . yes C(8) C(10) C(11) C(12) -92.6(4) . . . . yes C(8) C(10) C(11) C(16) 81.8(4) . . . . yes C(9) N(1) Ir(1) C(10) 4.6(2) . . . . yes C(9) N(1) Ir(1) C(26) -82.4(3) . . . . yes C(9) N(1) Ir(1) C(42) 101.9(2) . . . . yes C(9) C(8) C(10) C(11) 180.0(3) . . . . yes C(10) Ir(1) N(2) C(17) 102.7(3) . . . . yes C(10) Ir(1) N(2) C(25) -85.2(2) . . . . yes C(10) Ir(1) N(3) C(33) 142.3(10) . . . . yes C(10) Ir(1) N(3) C(41) -37(1) . . . . yes C(10) Ir(1) C(26) C(24) 97.4(3) . . . . yes C(10) Ir(1) C(26) C(27) -77.7(3) . . . . yes C(10) Ir(1) C(42) C(40) 174.9(3) . . . . yes C(10) Ir(1) C(42) C(43) -3.1(3) . . . . yes C(10) C(11) C(12) C(13) 172.1(3) . . . . yes C(10) C(11) C(16) C(15) -173.1(3) . . . . yes C(11) C(10) Ir(1) C(26) -88.0(3) . . . . yes C(11) C(10) Ir(1) C(42) 88.4(3) . . . . yes C(11) C(12) C(13) C(14) 1.2(6) . . . . yes C(11) C(16) C(15) C(14) 0.8(6) . . . . yes C(12) C(11) C(16) C(15) 1.5(5) . . . . yes C(12) C(13) C(14) C(15) 1.2(5) . . . . yes C(13) C(12) C(11) C(16) -2.5(5) . . . . yes C(13) C(14) C(15) C(16) -2.1(5) . . . . yes C(17) N(2) Ir(1) C(26) -171.8(3) . . . . yes C(17) N(2) Ir(1) C(42) 3.9(3) . . . . yes C(17) N(2) C(25) C(20) -2.5(5) . . . . yes C(17) N(2) C(25) C(24) 175.1(3) . . . . yes C(17) C(18) C(19) C(20) -1.7(5) . . . . yes C(18) C(17) N(2) C(25) -0.7(5) . . . . yes C(18) C(19) C(20) C(21) 179.9(3) . . . . yes C(18) C(19) C(20) C(25) -1.3(5) . . . . yes C(19) C(20) C(21) C(22) 155.3(4) . . . . yes C(19) C(20) C(21) C(49) -163.2(7) . . . . yes C(19) C(20) C(25) C(24) -173.8(3) . . . . yes C(20) C(21) C(22) C(23) 50.0(6) . . . . yes C(20) C(21) C(22) C(49) 98.5(10) . . . . yes C(20) C(21) C(22) C(50) 34.1(9) . . . . yes C(20) C(21) C(49) C(22) -98.2(8) . . . . yes C(20) C(21) C(49) C(23) -36(1) . . . . yes C(20) C(21) C(49) C(50) -51(1) . . . . yes C(20) C(25) C(24) C(23) -12.7(6) . . . . yes C(20) C(25) C(24) C(26) 172.2(3) . . . . yes C(20) C(25) C(24) C(50) 6.1(8) . . . . yes C(21) C(20) C(25) C(24) 4.9(5) . . . . yes C(21) C(22) C(23) C(24) -55.9(6) . . . . yes C(21) C(22) C(23) C(49) 45.3(9) . . . . yes C(21) C(22) C(23) C(50) -118(2) . . . . yes C(21) C(22) C(49) C(23) -131.6(7) . . . . yes C(21) C(22) C(49) C(50) -127.3(8) . . . . yes C(21) C(22) C(50) C(23) 68(2) . . . . yes C(21) C(22) C(50) C(24) -25(1) . . . . yes C(21) C(22) C(50) C(49) 53.2(9) . . . . yes C(21) C(49) C(22) C(23) 131.6(7) . . . . yes C(21) C(49) C(22) C(50) 127.3(8) . . . . yes C(21) C(49) C(23) C(22) -64(1) . . . . yes C(21) C(49) C(23) C(24) 28(1) . . . . yes C(21) C(49) C(23) C(50) -52(2) . . . . yes C(21) C(49) C(50) C(22) -58.7(9) . . . . yes C(21) C(49) C(50) C(23) 135(2) . . . . yes C(21) C(49) C(50) C(24) 61(1) . . . . yes C(22) C(21) C(20) C(25) -23.4(5) . . . . yes C(22) C(21) C(49) C(23) 61(1) . . . . yes C(22) C(21) C(49) C(50) 46.3(9) . . . . yes C(22) C(23) C(24) C(25) 37.7(7) . . . . yes C(22) C(23) C(24) C(26) -147.7(5) . . . . yes C(22) C(23) C(24) C(50) -42(2) . . . . yes C(22) C(23) C(49) C(50) -11(2) . . . . yes C(22) C(23) C(50) C(24) 121(1) . . . . yes C(22) C(23) C(50) C(49) 9(1) . . . . yes C(22) C(49) C(23) C(24) 93.3(9) . . . . yes C(22) C(49) C(23) C(50) 11(2) . . . . yes C(22) C(49) C(50) C(23) -166(2) . . . . yes C(22) C(49) C(50) C(24) 120(1) . . . . yes C(22) C(50) C(23) C(24) -121(1) . . . . yes C(22) C(50) C(23) C(49) -9(1) . . . . yes C(22) C(50) C(24) C(23) 113(2) . . . . yes C(22) C(50) C(24) C(25) 4(1) . . . . yes C(22) C(50) C(24) C(26) -158.9(9) . . . . yes C(22) C(50) C(49) C(23) 166(2) . . . . yes C(23) C(22) C(21) C(49) -48.5(9) . . . . yes C(23) C(22) C(49) C(50) 4.3(8) . . . . yes C(23) C(22) C(50) C(24) -93(2) . . . . yes C(23) C(22) C(50) C(49) -14(2) . . . . yes C(23) C(24) C(26) C(27) 5.9(7) . . . . yes C(23) C(24) C(50) C(49) 71(2) . . . . yes C(23) C(49) C(22) C(50) -4.3(8) . . . . yes C(23) C(49) C(50) C(24) -73(2) . . . . yes C(23) C(50) C(22) C(49) 14(2) . . . . yes C(23) C(50) C(24) C(25) -108(2) . . . . yes C(23) C(50) C(24) C(26) 88(2) . . . . yes C(24) C(23) C(22) C(49) -101.2(9) . . . . yes C(24) C(23) C(22) C(50) 62(2) . . . . yes C(24) C(23) C(49) C(50) 81(2) . . . . yes C(24) C(23) C(50) C(49) -112.2(6) . . . . yes C(24) C(26) Ir(1) C(42) -47(1) . . . . yes C(24) C(26) C(27) C(28) -83.4(5) . . . . yes C(24) C(26) C(27) C(32) 101.7(5) . . . . yes C(24) C(50) C(22) C(49) -78(1) . . . . yes C(24) C(50) C(23) C(49) 112.2(6) . . . . yes C(25) N(2) Ir(1) C(26) 0.3(2) . . . . yes C(25) N(2) Ir(1) C(42) 176.0(2) . . . . yes C(25) C(20) C(21) C(49) 18.1(8) . . . . yes C(25) C(24) C(23) C(49) -2.6(8) . . . . yes C(25) C(24) C(23) C(50) 80(2) . . . . yes C(25) C(24) C(26) C(27) -179.4(3) . . . . yes C(25) C(24) C(50) C(49) -36(1) . . . . yes C(26) Ir(1) N(3) C(33) -3.0(3) . . . . yes C(26) Ir(1) N(3) C(41) 176.8(3) . . . . yes C(26) Ir(1) C(42) C(40) -40(1) . . . . yes C(26) Ir(1) C(42) C(43) 141(1) . . . . yes C(26) C(24) C(23) C(49) 172.0(7) . . . . yes C(26) C(24) C(23) C(50) -105(2) . . . . yes C(26) C(24) C(50) C(49) 159.7(7) . . . . yes C(26) C(27) C(28) C(29) -175.6(4) . . . . yes C(26) C(27) C(32) C(31) 175.1(4) . . . . yes C(27) C(26) Ir(1) C(42) 137(1) . . . . yes C(27) C(26) C(24) C(50) -15.8(9) . . . . yes C(27) C(28) C(29) C(30) 1.1(6) . . . . yes C(27) C(32) C(31) C(30) -0.3(7) . . . . yes C(28) C(27) C(32) C(31) 0.1(6) . . . . yes C(28) C(29) C(30) C(31) -1.3(6) . . . . yes C(29) C(28) C(27) C(32) -0.5(6) . . . . yes C(29) C(30) C(31) C(32) 0.9(7) . . . . yes C(33) N(3) Ir(1) C(42) -179.0(3) . . . . yes C(33) N(3) C(41) C(36) -1.6(5) . . . . yes C(33) N(3) C(41) C(40) 179.2(3) . . . . yes C(33) C(34) C(35) C(36) 0.6(6) . . . . yes C(34) C(33) N(3) C(41) 1.6(6) . . . . yes C(34) C(35) C(36) C(37) 177.2(4) . . . . yes C(34) C(35) C(36) C(41) -0.7(6) . . . . yes C(35) C(36) C(37) C(38) -151.7(4) . . . . yes C(35) C(36) C(41) C(40) -179.7(3) . . . . yes C(36) C(37) C(38) C(39) -55.0(5) . . . . yes C(36) C(41) C(40) C(39) -1.4(5) . . . . yes C(36) C(41) C(40) C(42) -179.3(3) . . . . yes C(37) C(36) C(41) C(40) 2.4(5) . . . . yes C(37) C(38) C(39) C(40) 56.0(4) . . . . yes C(38) C(37) C(36) C(41) 26.2(5) . . . . yes C(38) C(39) C(40) C(41) -28.1(5) . . . . yes C(38) C(39) C(40) C(42) 149.5(4) . . . . yes C(39) C(40) C(42) C(43) 1.3(6) . . . . yes C(40) C(42) C(43) C(44) -114.8(4) . . . . yes C(40) C(42) C(43) C(48) 66.4(5) . . . . yes C(41) N(3) Ir(1) C(42) 0.8(2) . . . . yes C(41) C(40) C(42) C(43) 179.0(3) . . . . yes C(42) C(43) C(44) C(45) -179.0(3) . . . . yes C(42) C(43) C(48) C(47) 177.9(3) . . . . yes C(43) C(44) C(45) C(46) 1.0(5) . . . . yes C(43) C(48) C(47) C(46) 1.3(6) . . . . yes C(44) C(43) C(48) C(47) -0.9(5) . . . . yes C(44) C(45) C(46) C(47) -0.6(5) . . . . yes C(45) C(44) C(43) C(48) -0.2(5) . . . . yes C(45) C(46) C(47) C(48) -0.5(6) . . . . yes C(49) C(21) C(22) C(50) -64(1) . . . . yes C(49) C(22) C(23) C(50) -164(2) . . . . yes C(49) C(23) C(22) C(50) 164(2) . . . . yes C(49) C(23) C(24) C(50) -82(2) . . . . yes C(49) C(23) C(24) C(50) -82(2) . . . . 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 C(2) C(3) 3.577(6) . 2_556 ? C(13) C(19) 3.504(6) . 2_665 ? C(13) C(18) 3.547(6) . 2_665 ? C(14) C(19) 3.455(5) . 2_665 ? C(14) C(35) 3.507(6) . 1_565 ? C(17) C(19) 3.500(5) . 2_665 ? C(18) C(19) 3.173(5) . 2_665 ? C(18) C(20) 3.321(5) . 2_665 ? C(19) C(19) 3.241(6) . 2_665 ? C(19) C(35) 3.546(5) . 2_655 ? C(33) C(35) 3.475(6) . 2_655 ? C(34) C(34) 3.369(8) . 2_655 ? C(34) C(35) 3.415(6) . 2_655 ? #===END #------------------------------------------------------------------------------ # END of CIF #------------------------------------------------------------------------------