Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # [{Ir(C14H11N2O1)2(\m-Cl)]2.2.0(CH2Cl2) P21/n(#14) # Created on Sat Jan 20 13:36:28 2007 #========================================================================== _audit_creation_method 'from SHELXL97 CIF and IUCr SHELXL97-template' _audit_creation_date ' 2007-01-20T13:36:28 ' _publ_contact_author_name 'Prof. Kazushi Mashima' _publ_contact_author_address ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; _publ_contact_author_phone ' +81 6 6850 6245' _publ_contact_author_fax ' +81 6 6850 6245' _publ_contact_author_email mashima@chem.es.osaka-u.ac.jp _publ_section_title ; Stepwise and One-pot Syntheses of Ir(III) Complexes with Imdazolium-based Carbene Ligands ; loop_ _publ_author_name 'Chih-Hsien Chien' 'Singo Fujita' 'Suguru Yamoto' 'Takeshi Hara' 'Tsuneaki Yamagata' 'Masami Watanabe' ; K.Mashima ; data_CCDC656909(compd2b) _database_code_depnum_ccdc_archive 'CCDC 656909' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_properties_physical ' air-stable ' _chemical_temperature_decomposition_gt 553 # in capillary under vacuo _chemical_formula_moiety '(C56, H44, Cl2, Ir2, N8, O4), 2.0(C H2 Cl2)' _chemical_formula_sum 'C58 H48 Cl6 Ir2 N8 O4' _chemical_formula_weight 1518.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ' -P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.2338(6) _cell_length_b 21.0211(7) _cell_length_c 25.5914(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.2230(10) _cell_angle_gamma 90.00 _cell_volume 11241.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 88758 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.45 _exptl_crystal_preparation 'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(1) K' _exptl_crystal_recrystallization_method 'Crystallized from a solution of CH2Cl2/hexane at ambient temperature under Ar' _exptl_crystal_description ' yellow ' _exptl_crystal_colour ' platelet ' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5920 _exptl_absorpt_coefficient_mu 5.071 _exptl_absorpt_correction_type multi-scan # Higashi, T. (1995). ABSCOR - Program for Absorption # Correction, Rigaku Corporation, Tokyo, Japan. _exptl_absorpt_correction_T_min 0.221 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_process_details ; Higashi, H. (1995), ABSCOR: Program for Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; Indexing was performed from 3 oscillations which were exposed for 4.5 minutes. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. #1 Phi=0.0, chi=54.0, omega=0.0 to 180.0 with 2.0deg step #2 Phi=180.0, chi=50.0, omega=0.0 to 180.0 with 2.0deg step #4 Phi=90.0, chi=20.0, omega=90.0 to 180.0 with 2.0deg step #4 Phi=0.0, chi=-10.0, omega=0.0 to 90.0 with 2.0deg step A total of 270 images, corresponding to 540.0 deg. osillation angles, were collected with 4 different goniometer setting. Exposure time was 6.0 minutes per degree. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. ; #========================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ' 0.5 mm double pinhole ' _diffrn_source_power 50 _diffrn_source_current 40 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_radiation_detector 'imaging plate' _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_device_details ; RAPID: Eulerian 3-circle ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 241575 _diffrn_reflns_av_R_equivalents 0.2027 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.47 _reflns_number_total 25625 _reflns_number_gt 16874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_cell_refinement 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'teXan (Rigaku/MSC, 2004)' _computing_structure_solution 'SIR2004 (Maria et al., 2005)' # SIR2004: an improved tool for crystal structure # determination and refinement # Maria C. Burla, Rocco Caliandro, Mercedes Camalli, Benedetta Carrozzini, # Giovanni L. Cascarano, Liberato De Caro, Carmelo Giacovazzo,* Giampiero # Polidoria and Riccardo Spagna, J. Appl. Cryst. (2005). 38, 381-388. _computing_publication_material 'SHELXL-97 (Sheldrick, 1997) and modified' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' # Carroll K. Johnson and M. N. Burnett, ORNL-6895, ORTEP-III(version 1.0.8), # A FORTRAN Thermal-Ellipsoid Plot Program, Oak Ridge National Labratory, # Oak Ridge, Tennessee. # Ortep-3 for Windows, Version 1.08 Louis J. Farrugia, _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25625 _refine_ls_number_parameters 1405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.982402(15) 0.094465(15) 0.814543(12) 0.02583(9) Uani 1 1 d . . . Ir2 Ir 0.972173(15) 0.089058(15) 0.667797(12) 0.02545(9) Uani 1 1 d . . . Ir3 Ir 1.040634(15) 0.574060(15) 0.813514(12) 0.02513(9) Uani 1 1 d . . . Ir4 Ir 0.989351(15) 0.592451(15) 0.666430(12) 0.02514(9) Uani 1 1 d . . . Cl1 Cl 0.97781(9) 0.17063(9) 0.73910(7) 0.0262(4) Uani 1 1 d . . . Cl2 Cl 0.97172(9) 0.01122(9) 0.74254(8) 0.0298(4) Uani 1 1 d . . . Cl3 Cl 1.09123(9) 0.59351(9) 0.73410(8) 0.0265(4) Uani 1 1 d . . . Cl4 Cl 0.93969(9) 0.59568(9) 0.74870(8) 0.0281(4) Uani 1 1 d . . . Cl5 Cl 0.77213(17) -0.1601(2) 0.87467(18) 0.1105(14) Uani 1 1 d . . . Cl6 Cl 0.8747(2) -0.2453(3) 0.9174(2) 0.165(2) Uani 1 1 d . . . Cl7 Cl 0.7394(4) -0.1712(3) 0.6836(3) 0.258(5) Uani 1 1 d . . . Cl8 Cl 0.7658(2) -0.1230(2) 0.58804(14) 0.1192(16) Uani 1 1 d . . . Cl9 Cl 0.74932(13) 0.18958(16) 0.17255(11) 0.0710(9) Uani 1 1 d . . . Cl10 Cl 0.71796(12) 0.20944(14) 0.05839(10) 0.0586(7) Uani 1 1 d . . . Cl11 Cl 0.74079(18) 0.1375(2) 0.31578(14) 0.1052(13) Uani 1 1 d . . . Cl12 Cl 0.7779(3) 0.2224(2) 0.4037(2) 0.187(3) Uani 1 1 d . . . O1 O 1.0678(3) -0.0792(3) 0.9680(2) 0.0373(14) Uani 1 1 d . . . O2 O 0.9211(3) 0.2855(3) 0.9395(2) 0.0438(16) Uani 1 1 d . . . O3 O 0.8787(3) -0.0908(3) 0.5226(3) 0.0452(17) Uani 1 1 d . . . O4 O 1.0570(3) 0.2734(3) 0.5479(2) 0.0387(15) Uani 1 1 d . . . O5 O 0.9170(3) 0.6081(3) 0.9798(2) 0.0445(16) Uani 1 1 d . . . O6 O 1.2442(3) 0.4570(3) 0.9352(2) 0.0346(14) Uani 1 1 d . . . O7 O 0.7685(2) 0.5198(3) 0.5376(2) 0.0365(14) Uani 1 1 d . . . O8 O 1.1572(3) 0.6500(3) 0.5355(2) 0.0358(14) Uani 1 1 d . . . N1 N 0.8310(3) 0.1260(3) 0.7936(2) 0.0289(16) Uani 1 1 d . . . N2 N 0.8663(3) 0.0527(3) 0.8491(3) 0.0315(16) Uani 1 1 d . . . N3 N 1.1322(3) 0.0588(3) 0.8248(3) 0.0298(16) Uani 1 1 d . . . N4 N 1.1055(3) 0.1386(3) 0.8687(3) 0.0356(17) Uani 1 1 d . . . N5 N 1.1252(3) 0.1067(3) 0.6951(3) 0.0279(15) Uani 1 1 d . . . N6 N 1.0866(3) 0.0348(3) 0.6388(3) 0.0286(15) Uani 1 1 d . . . N7 N 0.8189(3) 0.0752(3) 0.6578(3) 0.0340(17) Uani 1 1 d . . . N8 N 0.8552(3) 0.1411(3) 0.6072(3) 0.0358(17) Uani 1 1 d . . . N9 N 1.0580(3) 0.4298(3) 0.7755(3) 0.0327(16) Uani 1 1 d . . . N10 N 1.0061(3) 0.4459(3) 0.8389(3) 0.0334(17) Uani 1 1 d . . . N11 N 1.0291(3) 0.7268(3) 0.8277(3) 0.0279(15) Uani 1 1 d . . . N12 N 1.1069(3) 0.6769(3) 0.8762(3) 0.0290(16) Uani 1 1 d . . . N13 N 1.0173(3) 0.7445(3) 0.6750(2) 0.0278(15) Uani 1 1 d . . . N14 N 0.9266(3) 0.7119(3) 0.6329(3) 0.0321(16) Uani 1 1 d . . . N15 N 0.9497(3) 0.4455(3) 0.6727(3) 0.0298(16) Uani 1 1 d . . . N16 N 1.0071(3) 0.4722(3) 0.6152(3) 0.0320(16) Uani 1 1 d . . . C1 C 0.8247(4) 0.1742(4) 0.7564(3) 0.034(2) Uani 1 1 d . . . H1 H 0.8607 0.1889 0.7425 0.041 Uiso 1 1 calc R . . C2 C 0.7660(4) 0.2001(5) 0.7401(4) 0.043(2) Uani 1 1 d . . . H2 H 0.7611 0.2332 0.7143 0.052 Uiso 1 1 calc R . . C3 C 0.7116(4) 0.1789(5) 0.7607(4) 0.042(2) Uani 1 1 d . . . H3 H 0.6709 0.1976 0.7484 0.051 Uiso 1 1 calc R . . C4 C 0.7175(4) 0.1327(5) 0.7975(4) 0.041(2) Uani 1 1 d . . . H4 H 0.6811 0.1184 0.8109 0.049 Uiso 1 1 calc R . . C5 C 0.7790(4) 0.1051(4) 0.8165(3) 0.032(2) Uani 1 1 d . . . C6 C 0.8026(4) 0.0575(4) 0.8507(3) 0.036(2) Uani 1 1 d . . . H6 H 0.7791 0.0325 0.8716 0.043 Uiso 1 1 calc R . . C7 C 0.8867(4) 0.0943(4) 0.8142(3) 0.0304(19) Uani 1 1 d . . . C8 C 0.9151(4) 0.0155(4) 0.8804(3) 0.033(2) Uani 1 1 d . . . C9 C 0.9015(4) -0.0284(4) 0.9172(3) 0.037(2) Uani 1 1 d . . . H9 H 0.8585 -0.0360 0.9211 0.044 Uiso 1 1 calc R . . C10 C 0.9515(4) -0.0616(4) 0.9485(3) 0.036(2) Uani 1 1 d . . . H10 H 0.9432 -0.0916 0.9742 0.043 Uiso 1 1 calc R . . C11 C 1.0146(4) -0.0494(4) 0.9409(3) 0.033(2) Uani 1 1 d . . . C12 C 1.0267(4) -0.0045(4) 0.9035(3) 0.0299(19) Uani 1 1 d . . . H12 H 1.0697 0.0028 0.8993 0.036 Uiso 1 1 calc R . . C13 C 0.9772(4) 0.0303(4) 0.8717(3) 0.0285(19) Uani 1 1 d . . . C14 C 1.0572(4) -0.1262(4) 1.0053(4) 0.044(2) Uani 1 1 d . . . H14A H 1.0983 -0.1445 1.0221 0.066 Uiso 1 1 calc R . . H14B H 1.0298 -0.1599 0.9870 0.066 Uiso 1 1 calc R . . H14C H 1.0362 -0.1068 1.0325 0.066 Uiso 1 1 calc R . . C15 C 1.1322(4) 0.0053(4) 0.7932(3) 0.034(2) Uani 1 1 d . . . H15 H 1.0933 -0.0115 0.7742 0.041 Uiso 1 1 calc R . . C16 C 1.1884(4) -0.0223(5) 0.7901(4) 0.048(3) Uani 1 1 d . . . H16 H 1.1890 -0.0583 0.7677 0.058 Uiso 1 1 calc R . . C17 C 1.2472(4) 0.0008(5) 0.8194(4) 0.053(3) Uani 1 1 d . . . H17 H 1.2860 -0.0202 0.8167 0.064 Uiso 1 1 calc R . . C18 C 1.2482(4) 0.0511(5) 0.8502(4) 0.054(3) Uani 1 1 d . . . H18 H 1.2879 0.0672 0.8684 0.064 Uiso 1 1 calc R . . C19 C 1.1890(4) 0.0819(4) 0.8565(3) 0.037(2) Uani 1 1 d . . . C20 C 1.1718(4) 0.1317(4) 0.8842(4) 0.041(2) Uani 1 1 d . . . H20 H 1.1992 0.1571 0.9092 0.049 Uiso 1 1 calc R . . C21 C 1.0797(4) 0.0944(4) 0.8322(3) 0.0286(19) Uani 1 1 d . . . C22 C 1.0619(4) 0.1784(4) 0.8896(3) 0.0278(18) Uani 1 1 d . . . C23 C 1.0809(4) 0.2252(4) 0.9275(3) 0.038(2) Uani 1 1 d . . . H23 H 1.1250 0.2324 0.9408 0.046 Uiso 1 1 calc R . . C24 C 1.0346(4) 0.2611(5) 0.9456(3) 0.045(2) Uani 1 1 d . . . H24 H 1.0466 0.2921 0.9726 0.054 Uiso 1 1 calc R . . C25 C 0.9706(4) 0.2518(4) 0.9242(3) 0.036(2) Uani 1 1 d . . . C26 C 0.9517(4) 0.2045(4) 0.8857(3) 0.0299(19) Uani 1 1 d . . . H26 H 0.9075 0.1983 0.8719 0.036 Uiso 1 1 calc R . . C27 C 0.9973(4) 0.1666(4) 0.8675(3) 0.0296(19) Uani 1 1 d . . . C28 C 0.9342(5) 0.3160(4) 0.9905(3) 0.048(3) Uani 1 1 d . . . H28A H 0.8959 0.3385 0.9969 0.073 Uiso 1 1 calc R . . H28B H 0.9693 0.3465 0.9911 0.073 Uiso 1 1 calc R . . H28C H 0.9466 0.2839 1.0182 0.073 Uiso 1 1 calc R . . C29 C 1.1336(4) 0.1568(4) 0.7309(3) 0.0306(19) Uani 1 1 d . . . H29 H 1.0980 0.1756 0.7427 0.037 Uiso 1 1 calc R . . C30 C 1.1939(4) 0.1785(4) 0.7486(3) 0.034(2) Uani 1 1 d . . . H30 H 1.2002 0.2136 0.7723 0.041 Uiso 1 1 calc R . . C31 C 1.2484(4) 0.1489(4) 0.7319(4) 0.040(2) Uani 1 1 d . . . H31 H 1.2903 0.1636 0.7457 0.048 Uiso 1 1 calc R . . C32 C 1.2403(4) 0.1005(4) 0.6968(4) 0.036(2) Uani 1 1 d . . . H32 H 1.2765 0.0815 0.6858 0.044 Uiso 1 1 calc R . . C33 C 1.1782(4) 0.0779(4) 0.6764(3) 0.0310(19) Uani 1 1 d . . . C34 C 1.1532(4) 0.0327(4) 0.6421(3) 0.033(2) Uani 1 1 d . . . H34 H 1.1762 0.0044 0.6235 0.039 Uiso 1 1 calc R . . C35 C 1.0679(4) 0.0790(4) 0.6708(3) 0.0284(19) Uani 1 1 d . . . C36 C 1.0356(4) 0.0007(4) 0.6065(3) 0.0308(19) Uani 1 1 d . . . C37 C 1.0472(4) -0.0461(4) 0.5709(3) 0.033(2) Uani 1 1 d . . . H37 H 1.0896 -0.0567 0.5671 0.039 Uiso 1 1 calc R . . C38 C 0.9948(4) -0.0771(4) 0.5410(3) 0.034(2) Uani 1 1 d . . . H38 H 1.0008 -0.1087 0.5158 0.040 Uiso 1 1 calc R . . C39 C 0.9336(4) -0.0606(4) 0.5486(3) 0.0306(19) Uani 1 1 d . . . C40 C 0.9237(4) -0.0132(4) 0.5835(3) 0.0292(19) Uani 1 1 d . . . H40 H 0.8812 -0.0026 0.5871 0.035 Uiso 1 1 calc R . . C41 C 0.9743(4) 0.0194(4) 0.6136(3) 0.0263(18) Uani 1 1 d . . . C42 C 0.8856(4) -0.1418(5) 0.4881(4) 0.057(3) Uani 1 1 d . . . H42A H 0.8433 -0.1580 0.4722 0.086 Uiso 1 1 calc R . . H42B H 0.9105 -0.1759 0.5082 0.086 Uiso 1 1 calc R . . H42C H 0.9079 -0.1269 0.4600 0.086 Uiso 1 1 calc R . . C43 C 0.8112(4) 0.0294(5) 0.6947(4) 0.044(2) Uani 1 1 d . . . H43 H 0.8477 0.0089 0.7145 0.053 Uiso 1 1 calc R . . C44 C 0.7509(5) 0.0132(5) 0.7031(4) 0.057(3) Uani 1 1 d . . . H44 H 0.7455 -0.0172 0.7294 0.069 Uiso 1 1 calc R . . C45 C 0.6953(4) 0.0438(6) 0.6704(5) 0.064(4) Uani 1 1 d . . . H45 H 0.6533 0.0320 0.6746 0.077 Uiso 1 1 calc R . . C46 C 0.7036(5) 0.0891(5) 0.6342(5) 0.061(3) Uani 1 1 d . . . H46 H 0.6673 0.1099 0.6144 0.074 Uiso 1 1 calc R . . C47 C 0.7663(4) 0.1058(5) 0.6256(4) 0.044(2) Uani 1 1 d . . . C48 C 0.7898(4) 0.1462(5) 0.5944(4) 0.042(2) Uani 1 1 d . . . H48 H 0.7662 0.1733 0.5683 0.050 Uiso 1 1 calc R . . C49 C 0.8764(4) 0.0983(4) 0.6472(3) 0.0269(18) Uani 1 1 d . . . C50 C 0.9047(4) 0.1735(4) 0.5859(3) 0.033(2) Uani 1 1 d . . . C51 C 0.8920(5) 0.2178(4) 0.5443(3) 0.045(2) Uani 1 1 d . . . H51 H 0.8494 0.2255 0.5267 0.054 Uiso 1 1 calc R . . C52 C 0.9432(4) 0.2505(4) 0.5294(3) 0.043(2) Uani 1 1 d . . . H52 H 0.9364 0.2797 0.5007 0.051 Uiso 1 1 calc R . . C53 C 1.0037(4) 0.2395(4) 0.5571(3) 0.035(2) Uani 1 1 d . . . C54 C 1.0154(4) 0.1937(4) 0.5974(3) 0.0309(19) Uani 1 1 d . . . H54 H 1.0581 0.1867 0.6150 0.037 Uiso 1 1 calc R . . C55 C 0.9670(4) 0.1587(4) 0.6120(3) 0.0293(19) Uani 1 1 d . . . C56 C 1.0491(5) 0.3098(4) 0.4997(3) 0.050(3) Uani 1 1 d . . . H56A H 1.0892 0.3318 0.4974 0.075 Uiso 1 1 calc R . . H56B H 1.0149 0.3412 0.4998 0.075 Uiso 1 1 calc R . . H56C H 1.0377 0.2814 0.4692 0.075 Uiso 1 1 calc R . . C57 C 1.0930(4) 0.4357(4) 0.7346(3) 0.034(2) Uani 1 1 d . . . H57 H 1.1064 0.4764 0.7247 0.041 Uiso 1 1 calc R . . C58 C 1.1077(4) 0.3832(4) 0.7094(4) 0.040(2) Uani 1 1 d . . . H58 H 1.1292 0.3871 0.6800 0.048 Uiso 1 1 calc R . . C59 C 1.0913(4) 0.3218(5) 0.7261(4) 0.051(3) Uani 1 1 d . . . H59 H 1.1028 0.2853 0.7081 0.061 Uiso 1 1 calc R . . C60 C 1.0600(4) 0.3142(4) 0.7667(4) 0.047(3) Uani 1 1 d . . . H60 H 1.0493 0.2728 0.7771 0.056 Uiso 1 1 calc R . . C61 C 1.0427(4) 0.3694(4) 0.7942(3) 0.034(2) Uani 1 1 d . . . C62 C 1.0106(4) 0.3801(4) 0.8344(3) 0.038(2) Uani 1 1 d . . . H62 H 0.9944 0.3490 0.8555 0.046 Uiso 1 1 calc R . . C63 C 1.0350(4) 0.4788(4) 0.8040(3) 0.0317(19) Uani 1 1 d . . . C64 C 0.9811(4) 0.4836(4) 0.8766(3) 0.034(2) Uani 1 1 d . . . C65 C 0.9489(4) 0.4577(4) 0.9145(3) 0.041(2) Uani 1 1 d . . . H65 H 0.9423 0.4131 0.9159 0.049 Uiso 1 1 calc R . . C66 C 0.9266(4) 0.4978(4) 0.9501(3) 0.040(2) Uani 1 1 d . . . H66 H 0.9046 0.4812 0.9764 0.048 Uiso 1 1 calc R . . C67 C 0.9371(4) 0.5627(4) 0.9465(3) 0.034(2) Uani 1 1 d . . . C68 C 0.9692(4) 0.5894(4) 0.9079(3) 0.037(2) Uani 1 1 d . . . H68 H 0.9744 0.6342 0.9063 0.044 Uiso 1 1 calc R . . C69 C 0.9936(3) 0.5494(4) 0.8719(3) 0.0271(18) Uani 1 1 d . . . C70 C 0.8807(5) 0.5847(5) 1.0179(4) 0.062(3) Uani 1 1 d . . . H70A H 0.8686 0.6202 1.0388 0.093 Uiso 1 1 calc R . . H70B H 0.9067 0.5543 1.0415 0.093 Uiso 1 1 calc R . . H70C H 0.8420 0.5634 0.9993 0.093 Uiso 1 1 calc R . . C71 C 0.9753(4) 0.7452(4) 0.7910(3) 0.0314(19) Uani 1 1 d . . . H71 H 0.9504 0.7143 0.7693 0.038 Uiso 1 1 calc R . . C72 C 0.9591(4) 0.8073(4) 0.7869(3) 0.038(2) Uani 1 1 d . . . H72 H 0.9226 0.8197 0.7619 0.046 Uiso 1 1 calc R . . C73 C 0.9951(4) 0.8548(4) 0.8187(4) 0.041(2) Uani 1 1 d . . . H73 H 0.9824 0.8981 0.8153 0.050 Uiso 1 1 calc R . . C74 C 1.0475(4) 0.8376(4) 0.8539(4) 0.039(2) Uani 1 1 d . . . H74 H 1.0723 0.8691 0.8748 0.046 Uiso 1 1 calc R . . C75 C 1.0658(4) 0.7722(4) 0.8599(3) 0.0268(18) Uani 1 1 d . . . C76 C 1.1150(4) 0.7403(4) 0.8903(3) 0.033(2) Uani 1 1 d . . . H76 H 1.1482 0.7580 0.9160 0.040 Uiso 1 1 calc R . . C77 C 1.0547(4) 0.6656(4) 0.8379(3) 0.0259(18) Uani 1 1 d . . . C78 C 1.1444(4) 0.6222(4) 0.8941(3) 0.032(2) Uani 1 1 d . . . C79 C 1.1969(4) 0.6254(4) 0.9346(3) 0.035(2) Uani 1 1 d . . . H79 H 1.2089 0.6647 0.9518 0.042 Uiso 1 1 calc R . . C80 C 1.2318(4) 0.5707(4) 0.9502(3) 0.034(2) Uani 1 1 d . . . H80 H 1.2678 0.5719 0.9780 0.041 Uiso 1 1 calc R . . C81 C 1.2127(4) 0.5138(4) 0.9239(3) 0.0282(18) Uani 1 1 d . . . C82 C 1.1588(3) 0.5120(4) 0.8833(3) 0.0278(18) Uani 1 1 d . . . H82 H 1.1472 0.4726 0.8661 0.033 Uiso 1 1 calc R . . C83 C 1.1213(4) 0.5658(4) 0.8671(3) 0.0292(19) Uani 1 1 d . . . C84 C 1.2927(4) 0.4545(4) 0.9824(4) 0.043(2) Uani 1 1 d . . . H84A H 1.3118 0.4120 0.9859 0.064 Uiso 1 1 calc R . . H84B H 1.2733 0.4638 1.0136 0.064 Uiso 1 1 calc R . . H84C H 1.3259 0.4861 0.9798 0.064 Uiso 1 1 calc R . . C85 C 1.0780(4) 0.7498(4) 0.7049(3) 0.034(2) Uani 1 1 d . . . H85 H 1.1020 0.7128 0.7167 0.040 Uiso 1 1 calc R . . C86 C 1.1029(4) 0.8083(4) 0.7174(4) 0.046(2) Uani 1 1 d . . . H86 H 1.1446 0.8123 0.7380 0.055 Uiso 1 1 calc R . . C87 C 1.0661(5) 0.8650(4) 0.6993(4) 0.044(2) Uani 1 1 d . . . H87 H 1.0841 0.9059 0.7076 0.053 Uiso 1 1 calc R . . C88 C 1.0074(4) 0.8596(4) 0.6712(4) 0.040(2) Uani 1 1 d . . . H88 H 0.9831 0.8968 0.6605 0.048 Uiso 1 1 calc R . . C89 C 0.9806(4) 0.7987(4) 0.6571(3) 0.035(2) Uani 1 1 d . . . C90 C 0.9245(4) 0.7777(4) 0.6309(3) 0.035(2) Uani 1 1 d . . . H90 H 0.8897 0.8031 0.6140 0.042 Uiso 1 1 calc R . . C91 C 0.9840(4) 0.6895(4) 0.6603(3) 0.0267(18) Uani 1 1 d . . . C92 C 0.8825(4) 0.6650(4) 0.6088(3) 0.0283(18) Uani 1 1 d . . . C93 C 0.8234(4) 0.6808(4) 0.5795(3) 0.035(2) Uani 1 1 d . . . H93 H 0.8106 0.7241 0.5758 0.042 Uiso 1 1 calc R . . C94 C 0.7835(4) 0.6340(4) 0.5557(3) 0.038(2) Uani 1 1 d . . . H94 H 0.7426 0.6443 0.5359 0.045 Uiso 1 1 calc R . . C95 C 0.8040(4) 0.5704(4) 0.5608(3) 0.0301(19) Uani 1 1 d . . . C96 C 0.8626(4) 0.5553(4) 0.5904(3) 0.0305(19) Uani 1 1 d . . . H96 H 0.8754 0.5120 0.5929 0.037 Uiso 1 1 calc R . . C97 C 0.9050(4) 0.6020(4) 0.6177(3) 0.0293(19) Uani 1 1 d . . . C98 C 0.7137(4) 0.5329(5) 0.4984(4) 0.054(3) Uani 1 1 d . . . H98A H 0.6931 0.4929 0.4854 0.080 Uiso 1 1 calc R . . H98B H 0.7268 0.5559 0.4688 0.080 Uiso 1 1 calc R . . H98C H 0.6836 0.5590 0.5140 0.080 Uiso 1 1 calc R . . C99 C 0.9119(4) 0.4440(4) 0.7127(3) 0.0318(19) Uani 1 1 d . . . H99 H 0.9060 0.4815 0.7319 0.038 Uiso 1 1 calc R . . C100 C 0.8844(4) 0.3894(4) 0.7236(3) 0.037(2) Uani 1 1 d . . . H100 H 0.8584 0.3885 0.7503 0.045 Uiso 1 1 calc R . . C101 C 0.8940(4) 0.3318(4) 0.6949(4) 0.044(2) Uani 1 1 d . . . H101 H 0.8752 0.2930 0.7036 0.053 Uiso 1 1 calc R . . C102 C 0.9294(4) 0.3327(4) 0.6560(4) 0.038(2) Uani 1 1 d . . . H102 H 0.9356 0.2946 0.6376 0.045 Uiso 1 1 calc R . . C103 C 0.9571(4) 0.3894(4) 0.6425(3) 0.035(2) Uani 1 1 d . . . C104 C 0.9935(4) 0.4082(4) 0.6069(4) 0.035(2) Uani 1 1 d . . . H104 H 1.0073 0.3821 0.5808 0.042 Uiso 1 1 calc R . . C105 C 0.9817(4) 0.4972(4) 0.6570(3) 0.0254(17) Uani 1 1 d . . . C106 C 1.0428(4) 0.5159(4) 0.5894(3) 0.034(2) Uani 1 1 d . . . C107 C 1.0778(4) 0.4966(4) 0.5518(3) 0.037(2) Uani 1 1 d . . . H107 H 1.0769 0.4534 0.5408 0.045 Uiso 1 1 calc R . . C108 C 1.1143(4) 0.5408(4) 0.5302(3) 0.036(2) Uani 1 1 d . . . H108 H 1.1368 0.5291 0.5027 0.043 Uiso 1 1 calc R . . C109 C 1.1173(4) 0.6027(4) 0.5497(3) 0.0311(19) Uani 1 1 d . . . C110 C 1.0804(4) 0.6213(4) 0.5878(3) 0.0299(19) Uani 1 1 d . . . H110 H 1.0828 0.6641 0.5999 0.036 Uiso 1 1 calc R . . C111 C 1.0399(4) 0.5781(4) 0.6086(3) 0.0291(19) Uani 1 1 d . . . C112 C 1.1904(5) 0.6341(5) 0.4935(4) 0.050(3) Uani 1 1 d . . . H11A H 1.2172 0.6701 0.4867 0.074 Uiso 1 1 calc R . . H11B H 1.1594 0.6246 0.4613 0.074 Uiso 1 1 calc R . . H11C H 1.2175 0.5968 0.5036 0.074 Uiso 1 1 calc R . . C113 C 0.8483(5) -0.1878(6) 0.8718(5) 0.076(4) Uani 1 1 d . . . H11D H 0.8485 -0.2050 0.8359 0.091 Uiso 1 1 calc R . . H11E H 0.8785 -0.1516 0.8774 0.091 Uiso 1 1 calc R . . C114 C 0.7087(7) -0.1368(10) 0.6255(7) 0.150(8) Uani 1 1 d . . . H11F H 0.6883 -0.0960 0.6323 0.180 Uiso 1 1 calc R . . H11G H 0.6753 -0.1647 0.6056 0.180 Uiso 1 1 calc R . . C115 C 0.7092(5) 0.2394(5) 0.1217(3) 0.055(3) Uani 1 1 d . . . H11H H 0.7270 0.2830 0.1263 0.066 Uiso 1 1 calc R . . H11I H 0.6632 0.2416 0.1241 0.066 Uiso 1 1 calc R . . C116 C 0.734(2) 0.1703(9) 0.3645(8) 0.45(3) Uani 1 1 d . . . H11J H 0.7281 0.1352 0.3889 0.535 Uiso 1 1 calc R . . H11K H 0.6921 0.1913 0.3555 0.535 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02364(17) 0.02386(18) 0.02992(18) -0.00063(13) 0.00452(13) -0.00078(13) Ir2 0.02194(17) 0.02415(18) 0.02994(18) -0.00250(13) 0.00372(13) 0.00072(13) Ir3 0.02351(17) 0.02179(17) 0.02942(18) 0.00052(13) 0.00289(13) -0.00115(13) Ir4 0.02333(17) 0.02286(18) 0.02867(18) -0.00121(13) 0.00308(13) 0.00091(13) Cl1 0.0248(10) 0.0222(10) 0.0314(11) -0.0024(8) 0.0043(8) -0.0020(8) Cl2 0.0316(11) 0.0248(11) 0.0332(11) -0.0026(8) 0.0064(9) -0.0022(8) Cl3 0.0225(10) 0.0260(11) 0.0303(11) -0.0027(8) 0.0022(8) 0.0005(8) Cl4 0.0236(10) 0.0266(11) 0.0332(11) -0.0001(8) 0.0027(8) 0.0015(8) Cl5 0.063(2) 0.121(4) 0.149(4) -0.040(3) 0.024(2) 0.007(2) Cl6 0.142(4) 0.157(5) 0.178(5) 0.088(4) -0.024(4) -0.016(4) Cl7 0.406(11) 0.191(6) 0.244(7) 0.160(6) 0.241(8) 0.184(7) Cl8 0.113(3) 0.182(5) 0.068(2) 0.023(3) 0.030(2) 0.064(3) Cl9 0.0607(18) 0.080(2) 0.0682(19) 0.0237(16) 0.0002(14) -0.0088(16) Cl10 0.0528(16) 0.0669(19) 0.0546(16) -0.0129(13) 0.0054(12) -0.0037(14) Cl11 0.095(3) 0.151(4) 0.072(2) -0.011(2) 0.020(2) -0.035(3) Cl12 0.246(6) 0.081(3) 0.179(5) -0.051(3) -0.110(4) 0.062(4) O1 0.044(4) 0.028(4) 0.038(4) 0.006(3) 0.003(3) -0.003(3) O2 0.051(4) 0.032(4) 0.051(4) -0.015(3) 0.016(3) -0.001(3) O3 0.036(4) 0.040(4) 0.058(4) -0.027(3) 0.003(3) 0.003(3) O4 0.049(4) 0.031(4) 0.038(3) 0.009(3) 0.011(3) 0.004(3) O5 0.043(4) 0.054(4) 0.040(4) -0.001(3) 0.017(3) -0.007(3) O6 0.028(3) 0.035(4) 0.039(3) 0.006(3) 0.002(3) 0.005(3) O7 0.023(3) 0.036(4) 0.045(4) -0.006(3) -0.007(3) 0.001(3) O8 0.037(3) 0.033(4) 0.041(4) 0.004(3) 0.017(3) 0.007(3) N1 0.023(4) 0.032(4) 0.030(4) -0.007(3) 0.001(3) -0.001(3) N2 0.024(4) 0.031(4) 0.040(4) 0.003(3) 0.006(3) -0.005(3) N3 0.029(4) 0.027(4) 0.032(4) 0.004(3) 0.003(3) 0.003(3) N4 0.029(4) 0.036(4) 0.041(4) 0.003(3) 0.002(3) -0.002(3) N5 0.021(4) 0.023(4) 0.038(4) -0.002(3) 0.002(3) -0.002(3) N6 0.027(4) 0.023(4) 0.036(4) -0.003(3) 0.006(3) 0.004(3) N7 0.023(4) 0.045(5) 0.035(4) -0.011(3) 0.007(3) -0.008(3) N8 0.031(4) 0.031(4) 0.043(5) -0.009(3) 0.000(3) 0.010(3) N9 0.028(4) 0.027(4) 0.040(4) 0.002(3) -0.003(3) -0.002(3) N10 0.035(4) 0.020(4) 0.045(5) 0.007(3) 0.006(3) -0.006(3) N11 0.030(4) 0.019(4) 0.036(4) -0.003(3) 0.008(3) -0.002(3) N12 0.021(4) 0.030(4) 0.035(4) -0.004(3) 0.001(3) -0.004(3) N13 0.029(4) 0.023(4) 0.032(4) 0.001(3) 0.005(3) 0.003(3) N14 0.037(4) 0.030(4) 0.029(4) 0.001(3) 0.005(3) 0.010(3) N15 0.021(4) 0.033(4) 0.034(4) -0.004(3) 0.001(3) -0.003(3) N16 0.024(4) 0.028(4) 0.044(4) -0.007(3) 0.006(3) -0.004(3) C1 0.033(5) 0.034(5) 0.037(5) 0.000(4) 0.008(4) -0.003(4) C2 0.031(5) 0.044(6) 0.052(6) 0.006(5) 0.001(4) 0.001(4) C3 0.021(5) 0.045(6) 0.063(7) 0.004(5) 0.014(4) 0.007(4) C4 0.027(5) 0.055(7) 0.042(6) -0.008(5) 0.012(4) -0.001(4) C5 0.020(4) 0.039(5) 0.039(5) -0.004(4) 0.010(4) -0.002(4) C6 0.021(4) 0.041(6) 0.045(5) -0.009(4) 0.008(4) -0.008(4) C7 0.039(5) 0.021(4) 0.031(5) -0.004(3) 0.006(4) -0.009(4) C8 0.040(5) 0.024(5) 0.035(5) -0.007(4) 0.007(4) 0.001(4) C9 0.042(5) 0.030(5) 0.040(5) 0.001(4) 0.012(4) -0.006(4) C10 0.041(5) 0.031(5) 0.035(5) 0.003(4) 0.009(4) -0.012(4) C11 0.042(5) 0.027(5) 0.030(5) -0.004(4) 0.001(4) 0.001(4) C12 0.029(5) 0.028(5) 0.032(5) 0.001(4) 0.004(4) -0.008(4) C13 0.026(4) 0.021(4) 0.040(5) -0.011(4) 0.011(4) -0.009(3) C14 0.042(6) 0.038(6) 0.047(6) 0.017(4) -0.003(4) 0.000(4) C15 0.030(5) 0.028(5) 0.042(5) 0.000(4) 0.003(4) 0.005(4) C16 0.044(6) 0.043(6) 0.056(6) -0.003(5) 0.006(5) 0.024(5) C17 0.028(5) 0.069(8) 0.061(7) -0.005(6) 0.003(5) 0.015(5) C18 0.027(5) 0.060(8) 0.068(7) -0.002(6) -0.006(5) 0.014(5) C19 0.026(5) 0.047(6) 0.035(5) 0.000(4) -0.004(4) -0.001(4) C20 0.028(5) 0.039(6) 0.050(6) 0.000(4) -0.007(4) -0.001(4) C21 0.026(4) 0.024(5) 0.039(5) -0.003(4) 0.015(4) 0.001(4) C22 0.034(5) 0.024(5) 0.024(4) -0.002(3) 0.001(3) -0.006(4) C23 0.040(5) 0.035(5) 0.038(5) -0.012(4) 0.003(4) -0.006(4) C24 0.049(6) 0.051(7) 0.035(5) -0.010(4) 0.008(4) -0.006(5) C25 0.048(6) 0.024(5) 0.037(5) 0.001(4) 0.012(4) -0.003(4) C26 0.032(5) 0.030(5) 0.026(4) 0.006(3) 0.000(3) -0.004(4) C27 0.028(5) 0.031(5) 0.027(5) 0.005(4) 0.000(3) -0.003(4) C28 0.070(7) 0.036(6) 0.044(6) -0.001(4) 0.024(5) 0.012(5) C29 0.034(5) 0.019(4) 0.039(5) 0.002(3) 0.010(4) 0.003(4) C30 0.024(5) 0.038(5) 0.038(5) -0.014(4) -0.001(4) 0.006(4) C31 0.026(5) 0.041(6) 0.049(6) -0.009(4) -0.003(4) -0.004(4) C32 0.028(5) 0.031(5) 0.050(6) 0.000(4) 0.006(4) -0.002(4) C33 0.027(4) 0.028(5) 0.039(5) 0.002(4) 0.007(4) 0.003(4) C34 0.026(5) 0.027(5) 0.047(5) -0.005(4) 0.012(4) -0.002(4) C35 0.037(5) 0.019(4) 0.030(5) 0.004(3) 0.004(4) 0.012(4) C36 0.030(5) 0.026(5) 0.033(5) 0.003(4) -0.004(4) -0.005(4) C37 0.029(5) 0.029(5) 0.040(5) -0.011(4) 0.008(4) 0.001(4) C38 0.033(5) 0.027(5) 0.042(5) -0.006(4) 0.011(4) 0.006(4) C39 0.028(5) 0.028(5) 0.033(5) -0.005(4) -0.003(4) 0.003(4) C40 0.022(4) 0.034(5) 0.031(5) -0.007(4) 0.003(3) 0.001(4) C41 0.026(4) 0.028(5) 0.027(4) 0.005(3) 0.008(3) 0.003(3) C42 0.040(6) 0.054(7) 0.072(7) -0.043(6) -0.005(5) 0.006(5) C43 0.034(5) 0.050(6) 0.048(6) -0.018(5) 0.004(4) -0.010(5) C44 0.052(7) 0.067(8) 0.059(7) -0.026(6) 0.024(5) -0.034(6) C45 0.014(5) 0.096(10) 0.083(9) -0.042(7) 0.016(5) -0.013(5) C46 0.035(6) 0.065(8) 0.084(9) -0.036(7) 0.011(6) -0.010(5) C47 0.021(5) 0.059(7) 0.047(6) -0.024(5) -0.005(4) 0.000(4) C48 0.023(5) 0.045(6) 0.054(6) -0.013(5) -0.003(4) 0.000(4) C49 0.021(4) 0.026(5) 0.033(5) -0.009(3) 0.003(3) 0.007(3) C50 0.029(5) 0.030(5) 0.039(5) -0.009(4) 0.005(4) 0.003(4) C51 0.056(6) 0.035(6) 0.038(5) 0.003(4) -0.010(5) 0.020(5) C52 0.055(6) 0.042(6) 0.031(5) 0.004(4) 0.006(4) 0.011(5) C53 0.046(5) 0.029(5) 0.033(5) -0.004(4) 0.011(4) 0.002(4) C54 0.036(5) 0.025(5) 0.033(5) -0.003(4) 0.012(4) -0.002(4) C55 0.039(5) 0.025(5) 0.024(4) -0.005(3) 0.004(4) 0.008(4) C56 0.075(7) 0.040(6) 0.036(5) 0.011(4) 0.014(5) 0.001(5) C57 0.023(4) 0.032(5) 0.045(5) -0.002(4) 0.003(4) 0.000(4) C58 0.034(5) 0.034(5) 0.052(6) -0.010(4) 0.004(4) 0.004(4) C59 0.036(6) 0.026(6) 0.088(8) -0.012(5) 0.005(5) 0.005(4) C60 0.033(5) 0.019(5) 0.078(8) 0.006(5) -0.019(5) 0.002(4) C61 0.030(5) 0.023(5) 0.043(5) 0.003(4) -0.006(4) -0.002(4) C62 0.047(6) 0.024(5) 0.041(5) 0.005(4) -0.001(4) 0.002(4) C63 0.032(5) 0.030(5) 0.033(5) -0.003(4) 0.005(4) -0.006(4) C64 0.041(5) 0.029(5) 0.032(5) -0.001(4) 0.004(4) -0.009(4) C65 0.045(6) 0.034(6) 0.043(6) 0.009(4) 0.003(4) -0.011(4) C66 0.041(5) 0.044(6) 0.037(5) 0.010(4) 0.011(4) -0.006(5) C67 0.024(4) 0.042(6) 0.034(5) 0.002(4) -0.004(4) -0.013(4) C68 0.030(5) 0.039(6) 0.037(5) 0.013(4) -0.004(4) 0.001(4) C69 0.016(4) 0.030(5) 0.029(5) 0.002(4) -0.010(3) 0.002(3) C70 0.055(7) 0.079(9) 0.060(7) -0.002(6) 0.032(6) -0.022(6) C71 0.027(4) 0.031(5) 0.034(5) -0.004(4) 0.000(3) -0.002(4) C72 0.041(5) 0.033(5) 0.039(5) 0.004(4) 0.004(4) 0.004(4) C73 0.043(6) 0.023(5) 0.057(6) -0.004(4) 0.008(5) -0.001(4) C74 0.046(6) 0.023(5) 0.049(6) -0.012(4) 0.014(5) -0.002(4) C75 0.028(4) 0.024(5) 0.028(4) -0.007(3) 0.004(3) 0.002(4) C76 0.030(5) 0.026(5) 0.043(5) -0.008(4) 0.006(4) -0.004(4) C77 0.021(4) 0.019(4) 0.040(5) 0.003(3) 0.014(3) 0.000(3) C78 0.030(5) 0.025(5) 0.044(5) 0.006(4) 0.013(4) 0.002(4) C79 0.031(5) 0.027(5) 0.045(5) -0.001(4) 0.002(4) -0.003(4) C80 0.027(5) 0.038(5) 0.034(5) 0.000(4) 0.001(4) 0.000(4) C81 0.022(4) 0.028(5) 0.035(5) 0.006(4) 0.004(3) 0.005(3) C82 0.020(4) 0.026(5) 0.038(5) 0.001(4) 0.007(3) -0.008(3) C83 0.028(4) 0.026(5) 0.035(5) 0.005(4) 0.009(4) 0.000(4) C84 0.034(5) 0.037(6) 0.053(6) 0.011(4) -0.005(4) 0.003(4) C85 0.023(4) 0.024(5) 0.052(6) -0.002(4) -0.001(4) 0.005(4) C86 0.037(5) 0.038(6) 0.057(6) -0.003(5) -0.006(4) -0.012(5) C87 0.051(6) 0.024(5) 0.055(6) 0.002(4) 0.001(5) -0.006(4) C88 0.045(6) 0.027(5) 0.049(6) 0.006(4) 0.008(5) 0.004(4) C89 0.032(5) 0.034(5) 0.039(5) 0.000(4) 0.006(4) 0.008(4) C90 0.033(5) 0.032(5) 0.039(5) 0.013(4) 0.005(4) 0.007(4) C91 0.024(4) 0.030(5) 0.029(4) -0.005(3) 0.011(3) 0.000(4) C92 0.024(4) 0.032(5) 0.028(5) -0.006(4) 0.003(3) -0.005(4) C93 0.027(5) 0.034(5) 0.046(6) 0.008(4) 0.009(4) 0.000(4) C94 0.025(5) 0.044(6) 0.041(5) 0.006(4) -0.004(4) 0.001(4) C95 0.023(4) 0.036(5) 0.030(5) -0.005(4) 0.003(3) -0.006(4) C96 0.039(5) 0.024(5) 0.030(5) 0.002(3) 0.011(4) 0.007(4) C97 0.025(4) 0.028(5) 0.038(5) -0.004(4) 0.015(4) 0.001(4) C98 0.036(6) 0.057(7) 0.058(7) 0.006(5) -0.018(5) 0.001(5) C99 0.023(4) 0.031(5) 0.042(5) -0.003(4) 0.007(4) 0.005(4) C100 0.033(5) 0.037(6) 0.042(5) 0.003(4) 0.008(4) -0.003(4) C101 0.034(5) 0.025(5) 0.069(7) -0.002(5) 0.000(5) -0.008(4) C102 0.034(5) 0.028(5) 0.052(6) -0.012(4) 0.013(4) -0.008(4) C103 0.035(5) 0.024(5) 0.047(6) -0.009(4) 0.008(4) 0.002(4) C104 0.033(5) 0.030(5) 0.044(5) -0.007(4) 0.010(4) 0.001(4) C105 0.023(4) 0.021(4) 0.032(5) -0.004(3) 0.004(3) 0.000(3) C106 0.025(5) 0.033(5) 0.042(5) -0.009(4) 0.007(4) -0.005(4) C107 0.040(5) 0.029(5) 0.047(6) -0.015(4) 0.019(4) -0.005(4) C108 0.040(5) 0.036(5) 0.034(5) -0.005(4) 0.014(4) 0.003(4) C109 0.033(5) 0.025(5) 0.036(5) 0.003(4) 0.006(4) 0.007(4) C110 0.022(4) 0.033(5) 0.034(5) 0.003(4) 0.003(3) 0.007(4) C111 0.024(4) 0.028(5) 0.032(5) -0.006(4) -0.004(3) -0.001(4) C112 0.054(6) 0.048(6) 0.053(6) 0.006(5) 0.027(5) 0.000(5) C113 0.061(8) 0.080(9) 0.089(9) -0.008(7) 0.021(7) -0.008(7) C114 0.065(10) 0.21(2) 0.180(19) -0.084(17) 0.033(11) -0.059(12) C115 0.079(8) 0.054(7) 0.033(5) 0.001(5) 0.014(5) 0.008(6) C116 1.14(10) 0.085(15) 0.084(15) -0.029(11) 0.02(3) -0.25(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 1.6289 (0.0360)x - 14.1561 (0.0230)y + 18.8661 (0.0279)z = 9.7230 (0.0254) * -0.0008 (0.0068) C29 * -0.0712 (0.0074) C30 * -0.0563 (0.0080) C31 * -0.0195 (0.0074) C32 * 0.0151 (0.0077) C33 * 0.0495 (0.0075) C34 * 0.0750 (0.0070) C35 * 0.0225 (0.0076) C36 * -0.0052 (0.0075) C37 * -0.0466 (0.0072) C38 * -0.0352 (0.0072) C39 * -0.0314 (0.0068) C40 * -0.0083 (0.0068) C41 * 0.0474 (0.0064) N5 * 0.0649 (0.0064) N6 Rms deviation of fitted atoms = 0.0435 - 4.6924 (0.0352)x - 13.3516 (0.0225)y + 19.6431 (0.0268)z = 10.1536 (0.0608) Angle to previous plane (with approximate esd) = 8.56 ( 0.21 ) * 0.0440 (0.0071) C15 * 0.0875 (0.0081) C16 * 0.0789 (0.0092) C17 * 0.0088 (0.0090) C18 * -0.0027 (0.0084) C19 * -0.0428 (0.0081) C20 * -0.1343 (0.0074) C21 * -0.0439 (0.0074) C22 * -0.0134 (0.0078) C23 * 0.0800 (0.0078) C24 * 0.0843 (0.0073) C25 * 0.0477 (0.0065) C26 * -0.0173 (0.0069) C27 * -0.0489 (0.0063) N3 * -0.1279 (0.0068) N4 Rms deviation of fitted atoms = 0.0696 0.4412 (0.0373)x + 14.6628 (0.0202)y + 17.9447 (0.0312)z = 16.5045 (0.0164) Angle to previous plane (with approximate esd) = 85.27 ( 0.09 ) * -0.0136 (0.0072) C1 * 0.0482 (0.0079) C2 * 0.0834 (0.0083) C3 * 0.0687 (0.0076) C4 * 0.0324 (0.0079) C5 * -0.0414 (0.0075) C6 * -0.1194 (0.0072) C7 * -0.0739 (0.0075) C8 * -0.0655 (0.0074) C9 * 0.0321 (0.0070) C10 * 0.1027 (0.0071) C11 * 0.0949 (0.0067) C12 * 0.0138 (0.0067) C13 * -0.0494 (0.0063) N1 * -0.1129 (0.0067) N2 Rms deviation of fitted atoms = 0.0716 - 2.9410 (0.0314)x + 15.1704 (0.0231)y + 17.7105 (0.0301)z = 10.4242 (0.0399) Angle to previous plane (with approximate esd) = 9.50 ( 0.21 ) * -0.0602 (0.0073) C43 * 0.0189 (0.0079) C44 * 0.0690 (0.0090) C45 * 0.0907 (0.0084) C46 * 0.0071 (0.0082) C47 * -0.0027 (0.0079) C48 * -0.0478 (0.0069) C49 * -0.0761 (0.0077) C50 * -0.1020 (0.0077) C51 * -0.0214 (0.0074) C52 * 0.1243 (0.0072) C53 * 0.1081 (0.0066) C54 * -0.0210 (0.0068) C55 * -0.0415 (0.0066) N7 * -0.0453 (0.0066) N8 Rms deviation of fitted atoms = 0.0670 21.1220 (0.0017)x - 0.8536 (0.0163)y - 2.1481 (0.0185)z = 18.9200 (0.0139) Angle to previous plane (with approximate esd) = 84.07 ( 0.10 ) * 0.0000 (0.0000) Ir1 * 0.0000 (0.0000) Cl1 * 0.0000 (0.0000) Cl2 Rms deviation of fitted atoms = 0.0000 20.9790 (0.0025)x - 0.8174 (0.0163)y - 0.7230 (0.0187)z = 19.8396 (0.0104) Angle to previous plane (with approximate esd) = 3.20 ( 0.03 ) * 0.0000 (0.0000) Ir2 * 0.0000 (0.0000) Cl1 * 0.0000 (0.0000) Cl2 Rms deviation of fitted atoms = 0.0000 16.2051 (0.0186)x - 1.1523 (0.0374)y + 12.7494 (0.0272)z = 26.5554 (0.0159) Angle to previous plane (with approximate esd) = 31.53 ( 0.09 ) * 0.0209 (0.0067) C57 * -0.0032 (0.0073) C58 * 0.0156 (0.0082) C59 * 0.0340 (0.0072) C60 * 0.0411 (0.0075) C61 * 0.0230 (0.0076) C62 * -0.0843 (0.0075) C63 * -0.0376 (0.0080) C64 * -0.0468 (0.0075) C65 * -0.0002 (0.0074) C66 * 0.0483 (0.0070) C67 * 0.0474 (0.0066) C68 * 0.0292 (0.0064) C69 * -0.0185 (0.0063) N9 * -0.0688 (0.0066) N10 Rms deviation of fitted atoms = 0.0410 15.1704 (0.0272)x - 4.8270 (0.0496)y + 13.4008 (0.0483)z = 21.2589 (0.0348) Angle to previous plane (with approximate esd) = 10.46 ( 0.25 ) * -0.0164 (0.0062) C99 * -0.0249 (0.0066) C100 * 0.0145 (0.0071) C101 * 0.0251 (0.0070) C102 * -0.0095 (0.0079) C103 * -0.0243 (0.0067) C104 * 0.0380 (0.0059) C105 * 0.0123 (0.0060) N15 * -0.0147 (0.0058) N16 Rms deviation of fitted atoms = 0.0216 15.0010 (0.0220)x + 3.2164 (0.0281)y - 20.6118 (0.0279)z = 0.7528 (0.0641) Angle to previous plane (with approximate esd) = 89.26 ( 0.11 ) * -0.0298 (0.0067) C71 * 0.0128 (0.0073) C72 * 0.0485 (0.0077) C73 * 0.0537 (0.0072) C74 * -0.0047 (0.0071) C75 * 0.0039 (0.0071) C76 * -0.0612 (0.0067) C77 * -0.0123 (0.0074) C78 * -0.0518 (0.0072) C79 * -0.0241 (0.0068) C80 * 0.0483 (0.0067) C81 * 0.0707 (0.0062) C82 * 0.0152 (0.0067) C83 * -0.0376 (0.0060) N11 * -0.0314 (0.0063) N12 Rms deviation of fitted atoms = 0.0395 - 11.6327 (0.0269)x - 0.5785 (0.0343)y + 23.5463 (0.0141)z = 3.6243 (0.0220) Angle to previous plane (with approximate esd) = 14.30 ( 0.18 ) * 0.0001 (0.0071) C85 * -0.0303 (0.0080) C86 * -0.0603 (0.0081) C87 * -0.0352 (0.0074) C88 * -0.0209 (0.0078) C89 * 0.0259 (0.0074) C90 * 0.0794 (0.0067) C91 * 0.0610 (0.0073) C92 * 0.0473 (0.0072) C93 * -0.0218 (0.0072) C94 * -0.1016 (0.0068) C95 * -0.0776 (0.0063) C96 * 0.0440 (0.0068) C97 * 0.0038 (0.0060) N13 * 0.0862 (0.0063) N14 Rms deviation of fitted atoms = 0.0550 0.8265 (0.0173)x + 20.4566 (0.0037)y + 5.5372 (0.0186)z = 17.1080 (0.0193) Angle to previous plane (with approximate esd) = 81.86 ( 0.10 ) * 0.0000 (0.0000) Ir3 * 0.0000 (0.0000) Cl3 * 0.0000 (0.0000) Cl4 Rms deviation of fitted atoms = 0.0000 0.2352 (0.0173)x + 21.0132 (0.0008)y - 0.6832 (0.0191)z = 12.2267 (0.0189) Angle to previous plane (with approximate esd) = 14.65 ( 0.03 ) * 0.0000 (0.0000) Ir4 * 0.0000 (0.0000) Cl3 * 0.0000 (0.0000) Cl4 Rms deviation of fitted atoms = 0.0000 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C13 2.007(8) . ? Ir1 C27 2.021(8) . ? Ir1 C7 2.030(9) . ? Ir1 C21 2.036(8) . ? Ir1 Cl1 2.4967(19) . ? Ir1 Cl2 2.5220(19) . ? Ir1 Ir2 3.7248(4) . ? Ir2 C49 2.019(8) . ? Ir2 C41 2.024(8) . ? Ir2 C35 2.031(8) . ? Ir2 C55 2.033(8) . ? Ir2 Cl1 2.4914(19) . ? Ir2 Cl2 2.519(2) . ? Ir3 C83 2.003(8) . ? Ir3 C69 2.007(8) . ? Ir3 C63 2.017(8) . ? Ir3 C77 2.028(8) . ? Ir3 Cl3 2.4954(19) . ? Ir3 Cl4 2.5080(19) . ? Ir3 Ir4 3.7482(4) . ? Ir4 C111 1.999(8) . ? Ir4 C97 2.003(8) . ? Ir4 C105 2.020(8) . ? Ir4 C91 2.047(8) . ? Ir4 Cl4 2.517(2) . ? Ir4 Cl3 2.5199(19) . ? Cl5 C113 1.732(11) . ? Cl6 C113 1.703(13) . ? Cl7 C114 1.68(2) . ? Cl8 C114 1.699(15) . ? Cl9 C115 1.767(10) . ? Cl10 C115 1.779(9) . ? Cl11 C116 1.45(2) . ? Cl12 C116 1.65(2) . ? O1 C11 1.368(10) . ? O1 C14 1.421(9) . ? O2 C25 1.380(10) . ? O2 C28 1.436(10) . ? O3 C39 1.389(9) . ? O3 C42 1.414(9) . ? O4 C53 1.393(10) . ? O4 C56 1.436(9) . ? O5 C67 1.397(10) . ? O5 C70 1.431(10) . ? O6 C81 1.374(9) . ? O6 C84 1.442(9) . ? O7 C95 1.376(9) . ? O7 C98 1.422(9) . ? O8 C109 1.396(9) . ? O8 C112 1.427(10) . ? N1 C7 1.379(10) . ? N1 C1 1.382(10) . ? N1 C5 1.408(10) . ? N2 C6 1.364(10) . ? N2 C7 1.375(10) . ? N2 C8 1.425(10) . ? N3 C21 1.381(10) . ? N3 C15 1.385(10) . ? N3 C19 1.414(10) . ? N4 C21 1.362(10) . ? N4 C20 1.400(10) . ? N4 C22 1.422(10) . ? N5 C29 1.385(10) . ? N5 C35 1.391(10) . ? N5 C33 1.435(10) . ? N6 C35 1.346(9) . ? N6 C34 1.401(9) . ? N6 C36 1.433(10) . ? N7 C43 1.378(11) . ? N7 C49 1.385(10) . ? N7 C47 1.420(11) . ? N8 C48 1.372(10) . ? N8 C49 1.376(10) . ? N8 C50 1.441(11) . ? N9 C57 1.392(10) . ? N9 C63 1.400(10) . ? N9 C61 1.414(10) . ? N10 C63 1.361(10) . ? N10 C62 1.391(11) . ? N10 C64 1.421(10) . ? N11 C71 1.400(9) . ? N11 C75 1.401(9) . ? N11 C77 1.404(9) . ? N12 C77 1.364(10) . ? N12 C76 1.383(10) . ? N12 C78 1.426(10) . ? N13 C91 1.373(10) . ? N13 C85 1.381(10) . ? N13 C89 1.410(10) . ? N14 C91 1.377(10) . ? N14 C90 1.385(10) . ? N14 C92 1.422(10) . ? N15 C105 1.380(10) . ? N15 C99 1.408(10) . ? N15 C103 1.435(10) . ? N16 C105 1.382(9) . ? N16 C104 1.383(10) . ? N16 C106 1.427(10) . ? C1 C2 1.356(11) . ? C1 H1 0.9500 . ? C2 C3 1.424(12) . ? C2 H2 0.9500 . ? C3 C4 1.344(12) . ? C3 H3 0.9500 . ? C4 C5 1.432(12) . ? C4 H4 0.9500 . ? C5 C6 1.365(12) . ? C6 H6 0.9500 . ? C8 C9 1.384(11) . ? C8 C13 1.411(11) . ? C9 C10 1.396(12) . ? C9 H9 0.9500 . ? C10 C11 1.412(11) . ? C10 H10 0.9500 . ? C11 C12 1.400(11) . ? C12 C13 1.414(11) . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.342(11) . ? C15 H15 0.9500 . ? C16 C17 1.422(13) . ? C16 H16 0.9500 . ? C17 C18 1.316(13) . ? C17 H17 0.9500 . ? C18 C19 1.449(12) . ? C18 H18 0.9500 . ? C19 C20 1.350(12) . ? C20 H20 0.9500 . ? C22 C23 1.392(11) . ? C22 C27 1.408(10) . ? C23 C24 1.383(12) . ? C23 H23 0.9500 . ? C24 C25 1.386(12) . ? C24 H24 0.9500 . ? C25 C26 1.408(11) . ? C26 C27 1.397(11) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.358(11) . ? C29 H29 0.9500 . ? C30 C31 1.446(11) . ? C30 H30 0.9500 . ? C31 C32 1.347(12) . ? C31 H31 0.9500 . ? C32 C33 1.412(11) . ? C32 H32 0.9500 . ? C33 C34 1.337(11) . ? C34 H34 0.9500 . ? C36 C37 1.391(11) . ? C36 C41 1.402(11) . ? C37 C38 1.394(11) . ? C37 H37 0.9500 . ? C38 C39 1.392(11) . ? C38 H38 0.9500 . ? C39 C40 1.379(10) . ? C40 C41 1.386(10) . ? C40 H40 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.378(12) . ? C43 H43 0.9500 . ? C44 C45 1.470(15) . ? C44 H44 0.9500 . ? C45 C46 1.362(16) . ? C45 H45 0.9500 . ? C46 C47 1.431(13) . ? C46 H46 0.9500 . ? C47 C48 1.323(13) . ? C48 H48 0.9500 . ? C50 C51 1.403(12) . ? C50 C55 1.407(11) . ? C51 C52 1.396(13) . ? C51 H51 0.9500 . ? C52 C53 1.371(12) . ? C52 H52 0.9500 . ? C53 C54 1.401(11) . ? C54 C55 1.369(11) . ? C54 H54 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.343(11) . ? C57 H57 0.9500 . ? C58 C59 1.422(13) . ? C58 H58 0.9500 . ? C59 C60 1.336(13) . ? C59 H59 0.9500 . ? C60 C61 1.439(12) . ? C60 H60 0.9500 . ? C61 C62 1.350(12) . ? C62 H62 0.9500 . ? C64 C65 1.395(11) . ? C64 C69 1.416(11) . ? C65 C66 1.384(12) . ? C65 H65 0.9500 . ? C66 C67 1.389(12) . ? C66 H66 0.9500 . ? C67 C68 1.411(11) . ? C68 C69 1.414(11) . ? C68 H68 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.349(11) . ? C71 H71 0.9500 . ? C72 C73 1.424(12) . ? C72 H72 0.9500 . ? C73 C74 1.350(12) . ? C73 H73 0.9500 . ? C74 C75 1.430(11) . ? C74 H74 0.9500 . ? C75 C76 1.363(11) . ? C76 H76 0.9500 . ? C78 C79 1.382(11) . ? C78 C83 1.415(11) . ? C79 C80 1.388(11) . ? C79 H79 0.9500 . ? C80 C81 1.396(11) . ? C80 H80 0.9500 . ? C81 C82 1.401(10) . ? C82 C83 1.403(11) . ? C82 H82 0.9500 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.354(12) . ? C85 H85 0.9500 . ? C86 C87 1.454(12) . ? C86 H86 0.9500 . ? C87 C88 1.328(12) . ? C87 H87 0.9500 . ? C88 C89 1.422(12) . ? C88 H88 0.9500 . ? C89 C90 1.335(11) . ? C90 H90 0.9500 . ? C92 C93 1.383(11) . ? C92 C97 1.412(11) . ? C93 C94 1.370(12) . ? C93 H93 0.9500 . ? C94 C95 1.403(12) . ? C94 H94 0.9500 . ? C95 C96 1.375(11) . ? C96 C97 1.428(11) . ? C96 H96 0.9500 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.339(11) . ? C99 H99 0.9500 . ? C100 C101 1.451(12) . ? C100 H100 0.9500 . ? C101 C102 1.351(12) . ? C101 H101 0.9500 . ? C102 C103 1.398(11) . ? C102 H102 0.9500 . ? C103 C104 1.355(12) . ? C104 H104 0.9500 . ? C106 C107 1.375(11) . ? C106 C111 1.402(11) . ? C107 C108 1.387(11) . ? C107 H107 0.9500 . ? C108 C109 1.390(11) . ? C108 H108 0.9500 . ? C109 C110 1.409(11) . ? C110 C111 1.418(11) . ? C110 H110 0.9500 . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C113 H11D 0.9900 . ? C113 H11E 0.9900 . ? C114 H11F 0.9900 . ? C114 H11G 0.9900 . ? C115 H11H 0.9900 . ? C115 H11I 0.9900 . ? C116 H11J 0.9900 . ? C116 H11K 0.9900 . ? 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_3 _geom_angle_publ_flag C13 Ir1 C27 92.2(3) . . ? C13 Ir1 C7 79.5(3) . . ? C27 Ir1 C7 92.4(3) . . ? C13 Ir1 C21 91.3(3) . . ? C27 Ir1 C21 79.6(3) . . ? C7 Ir1 C21 167.6(3) . . ? C13 Ir1 Cl1 174.2(2) . . ? C27 Ir1 Cl1 91.0(2) . . ? C7 Ir1 Cl1 95.5(2) . . ? C21 Ir1 Cl1 94.0(2) . . ? C13 Ir1 Cl2 93.3(2) . . ? C27 Ir1 Cl2 173.5(2) . . ? C7 Ir1 Cl2 92.1(2) . . ? C21 Ir1 Cl2 96.7(2) . . ? Cl1 Ir1 Cl2 83.91(6) . . ? C13 Ir1 Ir2 135.5(2) . . ? C27 Ir1 Ir2 132.3(2) . . ? C7 Ir1 Ir2 96.7(2) . . ? C21 Ir1 Ir2 95.6(2) . . ? Cl1 Ir1 Ir2 41.64(4) . . ? Cl2 Ir1 Ir2 42.32(5) . . ? C49 Ir2 C41 92.0(3) . . ? C49 Ir2 C35 167.3(3) . . ? C41 Ir2 C35 78.9(3) . . ? C49 Ir2 C55 79.7(3) . . ? C41 Ir2 C55 92.6(3) . . ? C35 Ir2 C55 91.8(3) . . ? C49 Ir2 Cl1 92.3(2) . . ? C41 Ir2 Cl1 175.1(2) . . ? C35 Ir2 Cl1 97.2(2) . . ? C55 Ir2 Cl1 90.5(2) . . ? C49 Ir2 Cl2 97.0(2) . . ? C41 Ir2 Cl2 93.1(2) . . ? C35 Ir2 Cl2 92.4(2) . . ? C55 Ir2 Cl2 173.5(2) . . ? Cl1 Ir2 Cl2 84.09(6) . . ? C49 Ir2 Ir1 97.8(2) . . ? C41 Ir2 Ir1 135.1(2) . . ? C35 Ir2 Ir1 94.9(2) . . ? C55 Ir2 Ir1 132.2(2) . . ? Cl1 Ir2 Ir1 41.75(4) . . ? Cl2 Ir2 Ir1 42.39(4) . . ? C83 Ir3 C69 86.9(3) . . ? C83 Ir3 C63 91.3(3) . . ? C69 Ir3 C63 78.9(3) . . ? C83 Ir3 C77 79.0(3) . . ? C69 Ir3 C77 94.7(3) . . ? C63 Ir3 C77 168.7(3) . . ? C83 Ir3 Cl3 97.6(2) . . ? C69 Ir3 Cl3 172.6(2) . . ? C63 Ir3 Cl3 95.1(2) . . ? C77 Ir3 Cl3 91.9(2) . . ? C83 Ir3 Cl4 174.4(2) . . ? C69 Ir3 Cl4 93.4(2) . . ? C63 Ir3 Cl4 94.3(2) . . ? C77 Ir3 Cl4 95.4(2) . . ? Cl3 Ir3 Cl4 82.68(6) . . ? C83 Ir3 Ir4 139.2(2) . . ? C69 Ir3 Ir4 132.8(2) . . ? C63 Ir3 Ir4 88.9(2) . . ? C77 Ir3 Ir4 102.2(2) . . ? Cl3 Ir3 Ir4 41.89(4) . . ? Cl4 Ir3 Ir4 41.86(4) . . ? C111 Ir4 C97 95.3(3) . . ? C111 Ir4 C105 78.7(3) . . ? C97 Ir4 C105 88.9(3) . . ? C111 Ir4 C91 97.2(3) . . ? C97 Ir4 C91 79.7(3) . . ? C105 Ir4 C91 167.5(3) . . ? C111 Ir4 Cl4 169.3(2) . . ? C97 Ir4 Cl4 93.3(2) . . ? C105 Ir4 Cl4 95.2(2) . . ? C91 Ir4 Cl4 90.6(2) . . ? C111 Ir4 Cl3 90.1(2) . . ? C97 Ir4 Cl3 172.3(2) . . ? C105 Ir4 Cl3 97.6(2) . . ? C91 Ir4 Cl3 94.2(2) . . ? Cl4 Ir4 Cl3 82.01(6) . . ? C111 Ir4 Ir3 129.0(2) . . ? C97 Ir4 Ir3 134.8(2) . . ? C105 Ir4 Ir3 91.2(2) . . ? C91 Ir4 Ir3 100.5(2) . . ? Cl4 Ir4 Ir3 41.67(4) . . ? Cl3 Ir4 Ir3 41.39(4) . . ? Ir2 Cl1 Ir1 96.62(7) . . ? Ir2 Cl2 Ir1 95.29(7) . . ? Ir3 Cl3 Ir4 96.72(6) . . ? Ir3 Cl4 Ir4 96.46(6) . . ? C11 O1 C14 116.4(7) . . ? C25 O2 C28 116.8(7) . . ? C39 O3 C42 118.3(7) . . ? C53 O4 C56 116.3(7) . . ? C67 O5 C70 116.1(7) . . ? C81 O6 C84 117.2(7) . . ? C95 O7 C98 118.1(7) . . ? C109 O8 C112 115.7(7) . . ? C7 N1 C1 126.1(7) . . ? C7 N1 C5 112.0(7) . . ? C1 N1 C5 121.9(7) . . ? C6 N2 C7 113.7(7) . . ? C6 N2 C8 130.5(7) . . ? C7 N2 C8 115.6(7) . . ? C21 N3 C15 127.1(7) . . ? C21 N3 C19 111.2(7) . . ? C15 N3 C19 121.6(7) . . ? C21 N4 C20 112.6(7) . . ? C21 N4 C22 116.8(7) . . ? C20 N4 C22 130.1(7) . . ? C29 N5 C35 127.9(7) . . ? C29 N5 C33 121.6(7) . . ? C35 N5 C33 110.5(6) . . ? C35 N6 C34 112.9(7) . . ? C35 N6 C36 115.0(7) . . ? C34 N6 C36 132.1(7) . . ? C43 N7 C49 126.6(7) . . ? C43 N7 C47 122.6(8) . . ? C49 N7 C47 110.8(7) . . ? C48 N8 C49 114.3(8) . . ? C48 N8 C50 130.4(8) . . ? C49 N8 C50 115.3(7) . . ? C57 N9 C63 127.4(7) . . ? C57 N9 C61 121.4(7) . . ? C63 N9 C61 111.2(7) . . ? C63 N10 C62 114.0(7) . . ? C63 N10 C64 115.3(7) . . ? C62 N10 C64 130.5(7) . . ? C71 N11 C75 120.6(7) . . ? C71 N11 C77 128.3(7) . . ? C75 N11 C77 111.0(6) . . ? C77 N12 C76 113.8(7) . . ? C77 N12 C78 115.3(7) . . ? C76 N12 C78 131.0(7) . . ? C91 N13 C85 127.2(7) . . ? C91 N13 C89 111.3(7) . . ? C85 N13 C89 121.4(7) . . ? C91 N14 C90 112.4(7) . . ? C91 N14 C92 116.0(7) . . ? C90 N14 C92 131.4(7) . . ? C105 N15 C99 127.2(7) . . ? C105 N15 C103 112.5(7) . . ? C99 N15 C103 120.3(7) . . ? C105 N16 C104 112.9(7) . . ? C105 N16 C106 115.2(7) . . ? C104 N16 C106 131.9(7) . . ? C2 C1 N1 118.6(8) . . ? C2 C1 H1 120.7 . . ? N1 C1 H1 120.7 . . ? C1 C2 C3 121.5(9) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 120.3(8) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.8(8) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 N1 105.7(7) . . ? C6 C5 C4 136.3(8) . . ? N1 C5 C4 117.8(8) . . ? C5 C6 N2 106.7(7) . . ? C5 C6 H6 126.6 . . ? N2 C6 H6 126.6 . . ? N2 C7 N1 101.9(7) . . ? N2 C7 Ir1 115.5(6) . . ? N1 C7 Ir1 142.4(6) . . ? C9 C8 C13 124.5(8) . . ? C9 C8 N2 122.0(8) . . ? C13 C8 N2 113.4(7) . . ? C8 C9 C10 119.7(8) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 118.3(8) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? O1 C11 C12 114.8(8) . . ? O1 C11 C10 124.5(8) . . ? C12 C11 C10 120.7(8) . . ? C11 C12 C13 122.3(8) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C8 C13 C12 114.5(7) . . ? C8 C13 Ir1 116.0(6) . . ? C12 C13 Ir1 129.5(6) . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N3 118.6(8) . . ? C16 C15 H15 120.7 . . ? N3 C15 H15 120.7 . . ? C15 C16 C17 121.8(9) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 120.7(9) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.2(9) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 N3 106.5(7) . . ? C20 C19 C18 136.5(9) . . ? N3 C19 C18 116.8(8) . . ? C19 C20 N4 106.4(8) . . ? C19 C20 H20 126.8 . . ? N4 C20 H20 126.8 . . ? N4 C21 N3 103.2(7) . . ? N4 C21 Ir1 114.8(5) . . ? N3 C21 Ir1 141.4(6) . . ? C23 C22 C27 123.1(8) . . ? C23 C22 N4 123.4(7) . . ? C27 C22 N4 113.5(7) . . ? C24 C23 C22 118.9(8) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 119.8(8) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? O2 C25 C24 124.0(8) . . ? O2 C25 C26 115.0(8) . . ? C24 C25 C26 120.9(8) . . ? C27 C26 C25 120.5(8) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C22 116.7(7) . . ? C26 C27 Ir1 128.0(6) . . ? C22 C27 Ir1 115.2(6) . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N5 118.7(7) . . ? C30 C29 H29 120.6 . . ? N5 C29 H29 120.6 . . ? C29 C30 C31 120.8(8) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 120.6(8) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 120.1(8) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 135.9(8) . . ? C34 C33 N5 105.9(7) . . ? C32 C33 N5 118.1(7) . . ? C33 C34 N6 107.3(7) . . ? C33 C34 H34 126.3 . . ? N6 C34 H34 126.3 . . ? N6 C35 N5 103.4(7) . . ? N6 C35 Ir2 116.8(6) . . ? N5 C35 Ir2 139.7(6) . . ? C37 C36 C41 124.0(8) . . ? C37 C36 N6 121.9(7) . . ? C41 C36 N6 114.1(7) . . ? C36 C37 C38 118.2(7) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C39 C38 C37 118.7(8) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C40 C39 O3 115.4(7) . . ? C40 C39 C38 121.6(8) . . ? O3 C39 C38 123.0(7) . . ? C39 C40 C41 121.6(7) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C40 C41 C36 115.8(7) . . ? C40 C41 Ir2 128.9(6) . . ? C36 C41 Ir2 115.2(6) . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N7 120.4(9) . . ? C44 C43 H43 119.8 . . ? N7 C43 H43 119.8 . . ? C43 C44 C45 118.6(10) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C46 C45 C44 120.3(9) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 120.8(11) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 N7 107.5(8) . . ? C48 C47 C46 135.3(10) . . ? N7 C47 C46 117.2(10) . . ? C47 C48 N8 106.2(9) . . ? C47 C48 H48 126.9 . . ? N8 C48 H48 126.9 . . ? N8 C49 N7 101.1(7) . . ? N8 C49 Ir2 116.0(6) . . ? N7 C49 Ir2 142.9(6) . . ? C51 C50 C55 123.2(8) . . ? C51 C50 N8 123.1(8) . . ? C55 C50 N8 113.7(8) . . ? C52 C51 C50 118.6(8) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 118.7(8) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C52 C53 O4 122.8(8) . . ? C52 C53 C54 121.6(8) . . ? O4 C53 C54 115.6(7) . . ? C55 C54 C53 121.8(8) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C54 C55 C50 116.0(8) . . ? C54 C55 Ir2 129.0(6) . . ? C50 C55 Ir2 115.0(6) . . ? O4 C56 H56A 109.5 . . ? O4 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O4 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N9 119.2(8) . . ? C58 C57 H57 120.4 . . ? N9 C57 H57 120.4 . . ? C57 C58 C59 120.7(9) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C60 C59 C58 121.7(9) . . ? C60 C59 H59 119.2 . . ? C58 C59 H59 119.2 . . ? C59 C60 C61 119.2(9) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 N9 106.7(8) . . ? C62 C61 C60 135.6(9) . . ? N9 C61 C60 117.6(8) . . ? C61 C62 N10 106.2(8) . . ? C61 C62 H62 126.9 . . ? N10 C62 H62 126.9 . . ? N10 C63 N9 101.9(7) . . ? N10 C63 Ir3 116.7(6) . . ? N9 C63 Ir3 140.9(6) . . ? C65 C64 C69 124.2(8) . . ? C65 C64 N10 122.8(8) . . ? C69 C64 N10 112.9(7) . . ? C66 C65 C64 119.2(8) . . ? C66 C65 H65 120.4 . . ? C64 C65 H65 120.4 . . ? C65 C66 C67 118.4(8) . . ? C65 C66 H66 120.8 . . ? C67 C66 H66 120.8 . . ? C66 C67 O5 124.1(8) . . ? C66 C67 C68 122.8(9) . . ? O5 C67 C68 113.1(8) . . ? C67 C68 C69 119.8(8) . . ? C67 C68 H68 120.1 . . ? C69 C68 H68 120.1 . . ? C68 C69 C64 115.5(8) . . ? C68 C69 Ir3 128.3(6) . . ? C64 C69 Ir3 116.1(6) . . ? O5 C70 H70A 109.5 . . ? O5 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O5 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 N11 119.0(8) . . ? C72 C71 H71 120.5 . . ? N11 C71 H71 120.5 . . ? C71 C72 C73 122.1(8) . . ? C71 C72 H72 119.0 . . ? C73 C72 H72 119.0 . . ? C74 C73 C72 119.3(9) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C75 120.3(8) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C76 C75 N11 106.9(7) . . ? C76 C75 C74 134.4(8) . . ? N11 C75 C74 118.6(7) . . ? C75 C76 N12 106.1(7) . . ? C75 C76 H76 126.9 . . ? N12 C76 H76 126.9 . . ? N12 C77 N11 102.2(6) . . ? N12 C77 Ir3 116.3(5) . . ? N11 C77 Ir3 141.4(6) . . ? C79 C78 C83 124.7(8) . . ? C79 C78 N12 122.1(8) . . ? C83 C78 N12 113.1(7) . . ? C78 C79 C80 119.5(8) . . ? C78 C79 H79 120.2 . . ? C80 C79 H79 120.2 . . ? C79 C80 C81 118.5(8) . . ? C79 C80 H80 120.8 . . ? C81 C80 H80 120.8 . . ? O6 C81 C80 123.6(7) . . ? O6 C81 C82 115.8(7) . . ? C80 C81 C82 120.6(7) . . ? C81 C82 C83 122.9(8) . . ? C81 C82 H82 118.6 . . ? C83 C82 H82 118.6 . . ? C82 C83 C78 113.7(7) . . ? C82 C83 Ir3 130.1(6) . . ? C78 C83 Ir3 116.2(6) . . ? O6 C84 H84A 109.5 . . ? O6 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? O6 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 N13 119.4(8) . . ? C86 C85 H85 120.3 . . ? N13 C85 H85 120.3 . . ? C85 C86 C87 120.2(8) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C88 C87 C86 120.1(9) . . ? C88 C87 H87 119.9 . . ? C86 C87 H87 119.9 . . ? C87 C88 C89 120.5(9) . . ? C87 C88 H88 119.7 . . ? C89 C88 H88 119.7 . . ? C90 C89 N13 106.9(8) . . ? C90 C89 C88 134.9(8) . . ? N13 C89 C88 118.2(8) . . ? C89 C90 N14 106.9(7) . . ? C89 C90 H90 126.6 . . ? N14 C90 H90 126.6 . . ? N13 C91 N14 102.6(7) . . ? N13 C91 Ir4 143.0(6) . . ? N14 C91 Ir4 114.4(6) . . ? C93 C92 C97 124.1(8) . . ? C93 C92 N14 122.2(8) . . ? C97 C92 N14 113.7(7) . . ? C94 C93 C92 120.0(8) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 119.0(8) . . ? C93 C94 H94 120.5 . . ? C95 C94 H94 120.5 . . ? C96 C95 O7 115.6(8) . . ? C96 C95 C94 120.4(8) . . ? O7 C95 C94 124.0(7) . . ? C95 C96 C97 122.8(8) . . ? C95 C96 H96 118.6 . . ? C97 C96 H96 118.6 . . ? C92 C97 C96 113.6(7) . . ? C92 C97 Ir4 115.7(6) . . ? C96 C97 Ir4 130.7(6) . . ? O7 C98 H98A 109.5 . . ? O7 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O7 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C100 C99 N15 119.8(8) . . ? C100 C99 H99 120.1 . . ? N15 C99 H99 120.1 . . ? C99 C100 C101 120.3(8) . . ? C99 C100 H100 119.9 . . ? C101 C100 H100 119.9 . . ? C102 C101 C100 120.5(8) . . ? C102 C101 H101 119.7 . . ? C100 C101 H101 119.7 . . ? C101 C102 C103 120.5(8) . . ? C101 C102 H102 119.7 . . ? C103 C102 H102 119.7 . . ? C104 C103 C102 136.9(8) . . ? C104 C103 N15 104.6(7) . . ? C102 C103 N15 118.5(8) . . ? C103 C104 N16 108.0(7) . . ? C103 C104 H104 126.0 . . ? N16 C104 H104 126.0 . . ? N15 C105 N16 101.9(6) . . ? N15 C105 Ir4 141.1(6) . . ? N16 C105 Ir4 115.9(5) . . ? C107 C106 C111 125.7(8) . . ? C107 C106 N16 122.1(8) . . ? C111 C106 N16 112.2(7) . . ? C106 C107 C108 119.4(8) . . ? C106 C107 H107 120.3 . . ? C108 C107 H107 120.3 . . ? C107 C108 C109 118.4(8) . . ? C107 C108 H108 120.8 . . ? C109 C108 H108 120.8 . . ? C108 C109 O8 124.3(7) . . ? C108 C109 C110 120.8(8) . . ? O8 C109 C110 114.8(7) . . ? C109 C110 C111 122.0(8) . . ? C109 C110 H110 119.0 . . ? C111 C110 H110 119.0 . . ? C106 C111 C110 113.4(7) . . ? C106 C111 Ir4 117.7(6) . . ? C110 C111 Ir4 128.5(6) . . ? O8 C112 H11A 109.5 . . ? O8 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? O8 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? Cl6 C113 Cl5 114.0(7) . . ? Cl6 C113 H11D 108.8 . . ? Cl5 C113 H11D 108.8 . . ? Cl6 C113 H11E 108.8 . . ? Cl5 C113 H11E 108.8 . . ? H11D C113 H11E 107.6 . . ? Cl7 C114 Cl8 111.7(10) . . ? Cl7 C114 H11F 109.3 . . ? Cl8 C114 H11F 109.3 . . ? Cl7 C114 H11G 109.3 . . ? Cl8 C114 H11G 109.3 . . ? H11F C114 H11G 107.9 . . ? Cl9 C115 Cl10 110.2(5) . . ? Cl9 C115 H11H 109.6 . . ? Cl10 C115 H11H 109.6 . . ? Cl9 C115 H11I 109.6 . . ? Cl10 C115 H11I 109.6 . . ? H11H C115 H11I 108.1 . . ? Cl11 C116 Cl12 135(3) . . ? Cl11 C116 H11J 103.4 . . ? Cl12 C116 H11J 103.4 . . ? Cl11 C116 H11K 103.4 . . ? Cl12 C116 H11K 103.4 . . ? H11J C116 H11K 105.2 . . ? 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 C13 Ir1 Ir2 C49 87.9(4) . . . . ? C27 Ir1 Ir2 C49 -93.3(4) . . . . ? C7 Ir1 Ir2 C49 6.1(3) . . . . ? C21 Ir1 Ir2 C49 -174.4(3) . . . . ? Cl1 Ir1 Ir2 C49 -84.7(2) . . . . ? Cl2 Ir1 Ir2 C49 91.8(2) . . . . ? C13 Ir1 Ir2 C41 -13.0(4) . . . . ? C27 Ir1 Ir2 C41 165.8(4) . . . . ? C7 Ir1 Ir2 C41 -94.7(4) . . . . ? C21 Ir1 Ir2 C41 84.7(4) . . . . ? Cl1 Ir1 Ir2 C41 174.5(3) . . . . ? Cl2 Ir1 Ir2 C41 -9.1(3) . . . . ? C13 Ir1 Ir2 C35 -92.1(4) . . . . ? C27 Ir1 Ir2 C35 86.7(4) . . . . ? C7 Ir1 Ir2 C35 -173.9(3) . . . . ? C21 Ir1 Ir2 C35 5.6(3) . . . . ? Cl1 Ir1 Ir2 C35 95.3(2) . . . . ? Cl2 Ir1 Ir2 C35 -88.2(2) . . . . ? C13 Ir1 Ir2 C55 171.0(4) . . . . ? C27 Ir1 Ir2 C55 -10.2(5) . . . . ? C7 Ir1 Ir2 C55 89.2(4) . . . . ? C21 Ir1 Ir2 C55 -91.3(4) . . . . ? Cl1 Ir1 Ir2 C55 -1.5(3) . . . . ? Cl2 Ir1 Ir2 C55 174.9(3) . . . . ? C13 Ir1 Ir2 Cl1 172.6(3) . . . . ? C27 Ir1 Ir2 Cl1 -8.6(3) . . . . ? C7 Ir1 Ir2 Cl1 90.8(2) . . . . ? C21 Ir1 Ir2 Cl1 -89.7(2) . . . . ? Cl2 Ir1 Ir2 Cl1 176.45(9) . . . . ? C13 Ir1 Ir2 Cl2 -3.9(3) . . . . ? C27 Ir1 Ir2 Cl2 174.9(3) . . . . ? C7 Ir1 Ir2 Cl2 -85.7(2) . . . . ? C21 Ir1 Ir2 Cl2 93.8(2) . . . . ? Cl1 Ir1 Ir2 Cl2 -176.45(9) . . . . ? C83 Ir3 Ir4 C111 15.5(5) . . . . ? C69 Ir3 Ir4 C111 -148.8(4) . . . . ? C63 Ir3 Ir4 C111 -75.1(4) . . . . ? C77 Ir3 Ir4 C111 102.8(4) . . . . ? Cl3 Ir3 Ir4 C111 23.8(3) . . . . ? Cl4 Ir3 Ir4 C111 -172.8(3) . . . . ? C83 Ir3 Ir4 C97 -178.5(5) . . . . ? C69 Ir3 Ir4 C97 17.3(5) . . . . ? C63 Ir3 Ir4 C97 90.9(4) . . . . ? C77 Ir3 Ir4 C97 -91.1(4) . . . . ? Cl3 Ir3 Ir4 C97 -170.2(3) . . . . ? Cl4 Ir3 Ir4 C97 -6.8(3) . . . . ? C83 Ir3 Ir4 C105 91.9(4) . . . . ? C69 Ir3 Ir4 C105 -72.4(4) . . . . ? C63 Ir3 Ir4 C105 1.2(3) . . . . ? C77 Ir3 Ir4 C105 179.2(3) . . . . ? Cl3 Ir3 Ir4 C105 100.1(2) . . . . ? Cl4 Ir3 Ir4 C105 -96.5(2) . . . . ? C83 Ir3 Ir4 C91 -92.7(4) . . . . ? C69 Ir3 Ir4 C91 103.0(4) . . . . ? C63 Ir3 Ir4 C91 176.7(3) . . . . ? C77 Ir3 Ir4 C91 -5.4(3) . . . . ? Cl3 Ir3 Ir4 C91 -84.4(2) . . . . ? Cl4 Ir3 Ir4 C91 79.0(2) . . . . ? C83 Ir3 Ir4 Cl4 -171.7(4) . . . . ? C69 Ir3 Ir4 Cl4 24.0(3) . . . . ? C63 Ir3 Ir4 Cl4 97.7(2) . . . . ? C77 Ir3 Ir4 Cl4 -84.3(2) . . . . ? Cl3 Ir3 Ir4 Cl4 -163.42(9) . . . . ? C83 Ir3 Ir4 Cl3 -8.3(4) . . . . ? C69 Ir3 Ir4 Cl3 -172.6(3) . . . . ? C63 Ir3 Ir4 Cl3 -98.9(2) . . . . ? C77 Ir3 Ir4 Cl3 79.1(2) . . . . ? Cl4 Ir3 Ir4 Cl3 163.42(9) . . . . ? C49 Ir2 Cl1 Ir1 99.2(2) . . . . ? C41 Ir2 Cl1 Ir1 -53(3) . . . . ? C35 Ir2 Cl1 Ir1 -89.3(2) . . . . ? C55 Ir2 Cl1 Ir1 178.9(2) . . . . ? Cl2 Ir2 Cl1 Ir1 2.41(6) . . . . ? C13 Ir1 Cl1 Ir2 -64(2) . . . . ? C27 Ir1 Cl1 Ir2 173.6(2) . . . . ? C7 Ir1 Cl1 Ir2 -93.9(2) . . . . ? C21 Ir1 Cl1 Ir2 94.0(2) . . . . ? Cl2 Ir1 Cl1 Ir2 -2.40(6) . . . . ? C49 Ir2 Cl2 Ir1 -94.0(2) . . . . ? C41 Ir2 Cl2 Ir1 173.6(2) . . . . ? C35 Ir2 Cl2 Ir1 94.6(2) . . . . ? C55 Ir2 Cl2 Ir1 -35(2) . . . . ? Cl1 Ir2 Cl2 Ir1 -2.38(6) . . . . ? C13 Ir1 Cl2 Ir2 177.3(2) . . . . ? C27 Ir1 Cl2 Ir2 -36(2) . . . . ? C7 Ir1 Cl2 Ir2 97.7(2) . . . . ? C21 Ir1 Cl2 Ir2 -91.0(2) . . . . ? Cl1 Ir1 Cl2 Ir2 2.37(6) . . . . ? C83 Ir3 Cl3 Ir4 174.6(2) . . . . ? C69 Ir3 Cl3 Ir4 47.4(17) . . . . ? C63 Ir3 Cl3 Ir4 82.6(2) . . . . ? C77 Ir3 Cl3 Ir4 -106.2(2) . . . . ? Cl4 Ir3 Cl3 Ir4 -11.07(6) . . . . ? C111 Ir4 Cl3 Ir3 -161.7(2) . . . . ? C97 Ir4 Cl3 Ir3 63.9(17) . . . . ? C105 Ir4 Cl3 Ir3 -83.2(2) . . . . ? C91 Ir4 Cl3 Ir3 101.1(2) . . . . ? Cl4 Ir4 Cl3 Ir3 11.05(6) . . . . ? C83 Ir3 Cl4 Ir4 104(2) . . . . ? C69 Ir3 Cl4 Ir4 -162.6(2) . . . . ? C63 Ir3 Cl4 Ir4 -83.5(2) . . . . ? C77 Ir3 Cl4 Ir4 102.4(2) . . . . ? Cl3 Ir3 Cl4 Ir4 11.08(6) . . . . ? C111 Ir4 Cl4 Ir3 31.7(12) . . . . ? C97 Ir4 Cl4 Ir3 175.2(2) . . . . ? C105 Ir4 Cl4 Ir3 86.0(2) . . . . ? C91 Ir4 Cl4 Ir3 -105.1(2) . . . . ? Cl3 Ir4 Cl4 Ir3 -10.99(6) . . . . ? C7 N1 C1 C2 179.6(8) . . . . ? C5 N1 C1 C2 -2.7(12) . . . . ? N1 C1 C2 C3 0.3(14) . . . . ? C1 C2 C3 C4 0.6(15) . . . . ? C2 C3 C4 C5 0.7(15) . . . . ? C7 N1 C5 C6 -2.4(9) . . . . ? C1 N1 C5 C6 179.7(7) . . . . ? C7 N1 C5 C4 -178.1(7) . . . . ? C1 N1 C5 C4 3.9(12) . . . . ? C3 C4 C5 C6 -176.9(10) . . . . ? C3 C4 C5 N1 -2.9(13) . . . . ? N1 C5 C6 N2 2.1(9) . . . . ? C4 C5 C6 N2 176.7(10) . . . . ? C7 N2 C6 C5 -1.3(10) . . . . ? C8 N2 C6 C5 173.0(8) . . . . ? C6 N2 C7 N1 -0.1(9) . . . . ? C8 N2 C7 N1 -175.4(6) . . . . ? C6 N2 C7 Ir1 175.1(5) . . . . ? C8 N2 C7 Ir1 -0.1(9) . . . . ? C1 N1 C7 N2 179.4(7) . . . . ? C5 N1 C7 N2 1.5(9) . . . . ? C1 N1 C7 Ir1 6.4(14) . . . . ? C5 N1 C7 Ir1 -171.5(8) . . . . ? C13 Ir1 C7 N2 -1.7(6) . . . . ? C27 Ir1 C7 N2 -93.5(6) . . . . ? C21 Ir1 C7 N2 -44.2(18) . . . . ? Cl1 Ir1 C7 N2 175.3(6) . . . . ? Cl2 Ir1 C7 N2 91.2(6) . . . . ? Ir2 Ir1 C7 N2 133.4(6) . . . . ? C13 Ir1 C7 N1 170.7(10) . . . . ? C27 Ir1 C7 N1 79.0(10) . . . . ? C21 Ir1 C7 N1 128.2(14) . . . . ? Cl1 Ir1 C7 N1 -12.3(10) . . . . ? Cl2 Ir1 C7 N1 -96.3(9) . . . . ? Ir2 Ir1 C7 N1 -54.1(10) . . . . ? C6 N2 C8 C9 5.9(13) . . . . ? C7 N2 C8 C9 -179.9(8) . . . . ? C6 N2 C8 C13 -171.5(8) . . . . ? C7 N2 C8 C13 2.8(10) . . . . ? C13 C8 C9 C10 -0.1(13) . . . . ? N2 C8 C9 C10 -177.2(7) . . . . ? C8 C9 C10 C11 -0.8(12) . . . . ? C14 O1 C11 C12 -178.4(7) . . . . ? C14 O1 C11 C10 1.3(12) . . . . ? C9 C10 C11 O1 -178.7(8) . . . . ? C9 C10 C11 C12 0.9(12) . . . . ? O1 C11 C12 C13 179.5(7) . . . . ? C10 C11 C12 C13 -0.2(13) . . . . ? C9 C8 C13 C12 0.9(12) . . . . ? N2 C8 C13 C12 178.2(7) . . . . ? C9 C8 C13 Ir1 178.5(7) . . . . ? N2 C8 C13 Ir1 -4.2(9) . . . . ? C11 C12 C13 C8 -0.7(11) . . . . ? C11 C12 C13 Ir1 -177.9(6) . . . . ? C27 Ir1 C13 C8 95.3(6) . . . . ? C7 Ir1 C13 C8 3.2(6) . . . . ? C21 Ir1 C13 C8 174.9(6) . . . . ? Cl1 Ir1 C13 C8 -27(3) . . . . ? Cl2 Ir1 C13 C8 -88.2(6) . . . . ? Ir2 Ir1 C13 C8 -85.6(6) . . . . ? C27 Ir1 C13 C12 -87.5(7) . . . . ? C7 Ir1 C13 C12 -179.6(8) . . . . ? C21 Ir1 C13 C12 -7.9(7) . . . . ? Cl1 Ir1 C13 C12 149.7(18) . . . . ? Cl2 Ir1 C13 C12 88.9(7) . . . . ? Ir2 Ir1 C13 C12 91.6(7) . . . . ? C21 N3 C15 C16 178.5(8) . . . . ? C19 N3 C15 C16 -4.6(12) . . . . ? N3 C15 C16 C17 1.8(14) . . . . ? C15 C16 C17 C18 -0.9(16) . . . . ? C16 C17 C18 C19 2.7(17) . . . . ? C21 N3 C19 C20 0.7(10) . . . . ? C15 N3 C19 C20 -176.7(8) . . . . ? C21 N3 C19 C18 -176.5(8) . . . . ? C15 N3 C19 C18 6.1(12) . . . . ? C17 C18 C19 C20 178.7(11) . . . . ? C17 C18 C19 N3 -5.1(15) . . . . ? N3 C19 C20 N4 -0.7(10) . . . . ? C18 C19 C20 N4 175.7(11) . . . . ? C21 N4 C20 C19 0.4(10) . . . . ? C22 N4 C20 C19 171.9(8) . . . . ? C20 N4 C21 N3 0.0(9) . . . . ? C22 N4 C21 N3 -172.6(6) . . . . ? C20 N4 C21 Ir1 172.8(6) . . . . ? C22 N4 C21 Ir1 0.1(9) . . . . ? C15 N3 C21 N4 176.8(7) . . . . ? C19 N3 C21 N4 -0.5(9) . . . . ? C15 N3 C21 Ir1 7.3(14) . . . . ? C19 N3 C21 Ir1 -169.9(8) . . . . ? C13 Ir1 C21 N4 -91.0(6) . . . . ? C27 Ir1 C21 N4 1.0(6) . . . . ? C7 Ir1 C21 N4 -49.4(18) . . . . ? Cl1 Ir1 C21 N4 91.2(6) . . . . ? Cl2 Ir1 C21 N4 175.6(6) . . . . ? Ir2 Ir1 C21 N4 133.0(6) . . . . ? C13 Ir1 C21 N3 77.7(10) . . . . ? C27 Ir1 C21 N3 169.6(10) . . . . ? C7 Ir1 C21 N3 119.3(15) . . . . ? Cl1 Ir1 C21 N3 -100.1(9) . . . . ? Cl2 Ir1 C21 N3 -15.8(10) . . . . ? Ir2 Ir1 C21 N3 -58.3(9) . . . . ? C21 N4 C22 C23 179.3(8) . . . . ? C20 N4 C22 C23 8.2(14) . . . . ? C21 N4 C22 C27 -1.7(10) . . . . ? C20 N4 C22 C27 -172.9(8) . . . . ? C27 C22 C23 C24 1.6(13) . . . . ? N4 C22 C23 C24 -179.5(8) . . . . ? C22 C23 C24 C25 -2.7(14) . . . . ? C28 O2 C25 C24 -20.5(12) . . . . ? C28 O2 C25 C26 157.4(7) . . . . ? C23 C24 C25 O2 -179.7(8) . . . . ? C23 C24 C25 C26 2.5(14) . . . . ? O2 C25 C26 C27 -179.1(7) . . . . ? C24 C25 C26 C27 -1.1(12) . . . . ? C25 C26 C27 C22 0.0(11) . . . . ? C25 C26 C27 Ir1 178.0(6) . . . . ? C23 C22 C27 C26 -0.2(12) . . . . ? N4 C22 C27 C26 -179.2(7) . . . . ? C23 C22 C27 Ir1 -178.5(7) . . . . ? N4 C22 C27 Ir1 2.5(9) . . . . ? C13 Ir1 C27 C26 -89.0(7) . . . . ? C7 Ir1 C27 C26 -9.4(7) . . . . ? C21 Ir1 C27 C26 -180.0(8) . . . . ? Cl1 Ir1 C27 C26 86.1(7) . . . . ? Cl2 Ir1 C27 C26 123.9(18) . . . . ? Ir2 Ir1 C27 C26 91.8(7) . . . . ? C13 Ir1 C27 C22 89.1(6) . . . . ? C7 Ir1 C27 C22 168.6(6) . . . . ? C21 Ir1 C27 C22 -1.9(6) . . . . ? Cl1 Ir1 C27 C22 -95.8(6) . . . . ? Cl2 Ir1 C27 C22 -58(2) . . . . ? Ir2 Ir1 C27 C22 -90.1(6) . . . . ? C35 N5 C29 C30 -177.6(8) . . . . ? C33 N5 C29 C30 -0.5(12) . . . . ? N5 C29 C30 C31 -1.8(13) . . . . ? C29 C30 C31 C32 2.3(14) . . . . ? C30 C31 C32 C33 -0.5(14) . . . . ? C31 C32 C33 C34 179.7(10) . . . . ? C31 C32 C33 N5 -1.7(13) . . . . ? C29 N5 C33 C34 -178.8(7) . . . . ? C35 N5 C33 C34 -1.2(9) . . . . ? C29 N5 C33 C32 2.2(11) . . . . ? C35 N5 C33 C32 179.8(7) . . . . ? C32 C33 C34 N6 -179.7(9) . . . . ? N5 C33 C34 N6 1.6(9) . . . . ? C35 N6 C34 C33 -1.6(10) . . . . ? C36 N6 C34 C33 175.8(8) . . . . ? C34 N6 C35 N5 0.8(9) . . . . ? C36 N6 C35 N5 -177.1(6) . . . . ? C34 N6 C35 Ir2 177.9(5) . . . . ? C36 N6 C35 Ir2 0.1(9) . . . . ? C29 N5 C35 N6 177.6(7) . . . . ? C33 N5 C35 N6 0.2(8) . . . . ? C29 N5 C35 Ir2 1.6(14) . . . . ? C33 N5 C35 Ir2 -175.8(7) . . . . ? C49 Ir2 C35 N6 -45.2(17) . . . . ? C41 Ir2 C35 N6 -0.3(6) . . . . ? C55 Ir2 C35 N6 -92.6(6) . . . . ? Cl1 Ir2 C35 N6 176.7(6) . . . . ? Cl2 Ir2 C35 N6 92.4(6) . . . . ? Ir1 Ir2 C35 N6 134.8(6) . . . . ? C49 Ir2 C35 N5 130.5(13) . . . . ? C41 Ir2 C35 N5 175.4(9) . . . . ? C55 Ir2 C35 N5 83.1(9) . . . . ? Cl1 Ir2 C35 N5 -7.6(9) . . . . ? Cl2 Ir2 C35 N5 -91.9(9) . . . . ? Ir1 Ir2 C35 N5 -49.5(9) . . . . ? C35 N6 C36 C37 179.4(8) . . . . ? C34 N6 C36 C37 2.1(13) . . . . ? C35 N6 C36 C41 0.3(10) . . . . ? C34 N6 C36 C41 -177.0(8) . . . . ? C41 C36 C37 C38 -1.0(13) . . . . ? N6 C36 C37 C38 -180.0(7) . . . . ? C36 C37 C38 C39 -1.1(12) . . . . ? C42 O3 C39 C40 -177.1(8) . . . . ? C42 O3 C39 C38 2.1(13) . . . . ? C37 C38 C39 C40 2.3(13) . . . . ? C37 C38 C39 O3 -176.8(8) . . . . ? O3 C39 C40 C41 177.7(7) . . . . ? C38 C39 C40 C41 -1.5(13) . . . . ? C39 C40 C41 C36 -0.5(12) . . . . ? C39 C40 C41 Ir2 -178.9(6) . . . . ? C37 C36 C41 C40 1.8(12) . . . . ? N6 C36 C41 C40 -179.2(7) . . . . ? C37 C36 C41 Ir2 -179.6(7) . . . . ? N6 C36 C41 Ir2 -0.5(9) . . . . ? C49 Ir2 C41 C40 -10.1(8) . . . . ? C35 Ir2 C41 C40 178.8(8) . . . . ? C55 Ir2 C41 C40 -89.9(8) . . . . ? Cl1 Ir2 C41 C40 142(2) . . . . ? Cl2 Ir2 C41 C40 87.0(7) . . . . ? Ir1 Ir2 C41 C40 93.1(7) . . . . ? C49 Ir2 C41 C36 171.5(6) . . . . ? C35 Ir2 C41 C36 0.4(6) . . . . ? C55 Ir2 C41 C36 91.8(6) . . . . ? Cl1 Ir2 C41 C36 -37(3) . . . . ? Cl2 Ir2 C41 C36 -91.4(6) . . . . ? Ir1 Ir2 C41 C36 -85.3(6) . . . . ? C49 N7 C43 C44 176.6(8) . . . . ? C47 N7 C43 C44 -2.4(13) . . . . ? N7 C43 C44 C45 2.4(13) . . . . ? C43 C44 C45 C46 -2.6(15) . . . . ? C44 C45 C46 C47 2.7(16) . . . . ? C43 N7 C47 C48 -179.3(8) . . . . ? C49 N7 C47 C48 1.5(10) . . . . ? C43 N7 C47 C46 2.4(12) . . . . ? C49 N7 C47 C46 -176.8(8) . . . . ? C45 C46 C47 C48 179.7(11) . . . . ? C45 C46 C47 N7 -2.6(14) . . . . ? N7 C47 C48 N8 -0.5(10) . . . . ? C46 C47 C48 N8 177.4(10) . . . . ? C49 N8 C48 C47 -0.8(10) . . . . ? C50 N8 C48 C47 179.8(8) . . . . ? C48 N8 C49 N7 1.6(9) . . . . ? C50 N8 C49 N7 -178.9(6) . . . . ? C48 N8 C49 Ir2 -179.9(6) . . . . ? C50 N8 C49 Ir2 -0.4(9) . . . . ? C43 N7 C49 N8 179.0(8) . . . . ? C47 N7 C49 N8 -1.8(8) . . . . ? C43 N7 C49 Ir2 1.2(14) . . . . ? C47 N7 C49 Ir2 -179.6(7) . . . . ? C41 Ir2 C49 N8 -89.5(6) . . . . ? C35 Ir2 C49 N8 -45.6(17) . . . . ? C55 Ir2 C49 N8 2.8(6) . . . . ? Cl1 Ir2 C49 N8 92.8(6) . . . . ? Cl2 Ir2 C49 N8 177.2(5) . . . . ? Ir1 Ir2 C49 N8 134.4(5) . . . . ? C41 Ir2 C49 N7 88.1(9) . . . . ? C35 Ir2 C49 N7 132.0(13) . . . . ? C55 Ir2 C49 N7 -179.6(10) . . . . ? Cl1 Ir2 C49 N7 -89.6(9) . . . . ? Cl2 Ir2 C49 N7 -5.2(9) . . . . ? Ir1 Ir2 C49 N7 -48.0(9) . . . . ? C48 N8 C50 C51 -1.8(14) . . . . ? C49 N8 C50 C51 178.8(8) . . . . ? C48 N8 C50 C55 175.7(8) . . . . ? C49 N8 C50 C55 -3.7(10) . . . . ? C55 C50 C51 C52 -2.4(13) . . . . ? N8 C50 C51 C52 174.9(8) . . . . ? C50 C51 C52 C53 -2.1(13) . . . . ? C51 C52 C53 O4 -174.8(8) . . . . ? C51 C52 C53 C54 4.1(13) . . . . ? C56 O4 C53 C52 -14.5(12) . . . . ? C56 O4 C53 C54 166.5(7) . . . . ? C52 C53 C54 C55 -1.6(13) . . . . ? O4 C53 C54 C55 177.4(7) . . . . ? C53 C54 C55 C50 -2.7(12) . . . . ? C53 C54 C55 Ir2 178.7(6) . . . . ? C51 C50 C55 C54 4.7(12) . . . . ? N8 C50 C55 C54 -172.7(7) . . . . ? C51 C50 C55 Ir2 -176.5(7) . . . . ? N8 C50 C55 Ir2 6.0(9) . . . . ? C49 Ir2 C55 C54 173.7(8) . . . . ? C41 Ir2 C55 C54 -94.7(7) . . . . ? C35 Ir2 C55 C54 -15.8(7) . . . . ? Cl1 Ir2 C55 C54 81.5(7) . . . . ? Cl2 Ir2 C55 C54 114(2) . . . . ? Ir1 Ir2 C55 C54 82.5(8) . . . . ? C49 Ir2 C55 C50 -4.8(6) . . . . ? C41 Ir2 C55 C50 86.8(6) . . . . ? C35 Ir2 C55 C50 165.7(6) . . . . ? Cl1 Ir2 C55 C50 -97.1(6) . . . . ? Cl2 Ir2 C55 C50 -64(2) . . . . ? Ir1 Ir2 C55 C50 -96.0(6) . . . . ? C63 N9 C57 C58 -175.8(8) . . . . ? C61 N9 C57 C58 5.9(12) . . . . ? N9 C57 C58 C59 -3.9(13) . . . . ? C57 C58 C59 C60 1.2(14) . . . . ? C58 C59 C60 C61 -0.3(14) . . . . ? C57 N9 C61 C62 178.2(7) . . . . ? C63 N9 C61 C62 -0.4(9) . . . . ? C57 N9 C61 C60 -5.0(11) . . . . ? C63 N9 C61 C60 176.5(7) . . . . ? C59 C60 C61 C62 177.9(10) . . . . ? C59 C60 C61 N9 2.1(12) . . . . ? N9 C61 C62 N10 1.0(9) . . . . ? C60 C61 C62 N10 -175.1(9) . . . . ? C63 N10 C62 C61 -1.3(10) . . . . ? C64 N10 C62 C61 -175.4(8) . . . . ? C62 N10 C63 N9 1.0(9) . . . . ? C64 N10 C63 N9 176.0(6) . . . . ? C62 N10 C63 Ir3 -172.6(5) . . . . ? C64 N10 C63 Ir3 2.5(9) . . . . ? C57 N9 C63 N10 -178.8(7) . . . . ? C61 N9 C63 N10 -0.3(9) . . . . ? C57 N9 C63 Ir3 -8.0(14) . . . . ? C61 N9 C63 Ir3 170.5(7) . . . . ? C83 Ir3 C63 N10 85.3(6) . . . . ? C69 Ir3 C63 N10 -1.3(6) . . . . ? C77 Ir3 C63 N10 54.7(18) . . . . ? Cl3 Ir3 C63 N10 -177.0(6) . . . . ? Cl4 Ir3 C63 N10 -94.0(6) . . . . ? Ir4 Ir3 C63 N10 -135.5(6) . . . . ? C83 Ir3 C63 N9 -84.6(10) . . . . ? C69 Ir3 C63 N9 -171.2(10) . . . . ? C77 Ir3 C63 N9 -115.2(16) . . . . ? Cl3 Ir3 C63 N9 13.1(10) . . . . ? Cl4 Ir3 C63 N9 96.1(9) . . . . ? Ir4 Ir3 C63 N9 54.6(9) . . . . ? C63 N10 C64 C65 178.6(8) . . . . ? C62 N10 C64 C65 -7.3(14) . . . . ? C63 N10 C64 C69 -2.5(10) . . . . ? C62 N10 C64 C69 171.5(8) . . . . ? C69 C64 C65 C66 0.6(14) . . . . ? N10 C64 C65 C66 179.3(8) . . . . ? C64 C65 C66 C67 0.3(13) . . . . ? C65 C66 C67 O5 179.9(8) . . . . ? C65 C66 C67 C68 0.2(13) . . . . ? C70 O5 C67 C66 -3.3(12) . . . . ? C70 O5 C67 C68 176.4(8) . . . . ? C66 C67 C68 C69 -1.6(13) . . . . ? O5 C67 C68 C69 178.7(7) . . . . ? C67 C68 C69 C64 2.3(11) . . . . ? C67 C68 C69 Ir3 179.8(6) . . . . ? C65 C64 C69 C68 -1.9(12) . . . . ? N10 C64 C69 C68 179.3(7) . . . . ? C65 C64 C69 Ir3 -179.7(7) . . . . ? N10 C64 C69 Ir3 1.4(9) . . . . ? C83 Ir3 C69 C68 90.4(7) . . . . ? C63 Ir3 C69 C68 -177.7(7) . . . . ? C77 Ir3 C69 C68 11.7(7) . . . . ? Cl3 Ir3 C69 C68 -141.9(14) . . . . ? Cl4 Ir3 C69 C68 -84.0(7) . . . . ? Ir4 Ir3 C69 C68 -99.8(7) . . . . ? C83 Ir3 C69 C64 -92.0(6) . . . . ? C63 Ir3 C69 C64 -0.1(6) . . . . ? C77 Ir3 C69 C64 -170.8(6) . . . . ? Cl3 Ir3 C69 C64 36(2) . . . . ? Cl4 Ir3 C69 C64 93.6(6) . . . . ? Ir4 Ir3 C69 C64 77.8(6) . . . . ? C75 N11 C71 C72 0.1(11) . . . . ? C77 N11 C71 C72 -179.1(8) . . . . ? N11 C71 C72 C73 -0.1(13) . . . . ? C71 C72 C73 C74 0.7(14) . . . . ? C72 C73 C74 C75 -1.3(13) . . . . ? C71 N11 C75 C76 -178.9(7) . . . . ? C77 N11 C75 C76 0.5(9) . . . . ? C71 N11 C75 C74 -0.8(11) . . . . ? C77 N11 C75 C74 178.6(7) . . . . ? C73 C74 C75 C76 178.8(9) . . . . ? C73 C74 C75 N11 1.4(12) . . . . ? N11 C75 C76 N12 -0.3(8) . . . . ? C74 C75 C76 N12 -178.0(9) . . . . ? C77 N12 C76 C75 0.1(9) . . . . ? C78 N12 C76 C75 178.5(8) . . . . ? C76 N12 C77 N11 0.2(8) . . . . ? C78 N12 C77 N11 -178.5(6) . . . . ? C76 N12 C77 Ir3 178.4(5) . . . . ? C78 N12 C77 Ir3 -0.3(8) . . . . ? C71 N11 C77 N12 178.9(7) . . . . ? C75 N11 C77 N12 -0.4(8) . . . . ? C71 N11 C77 Ir3 1.4(13) . . . . ? C75 N11 C77 Ir3 -177.8(7) . . . . ? C83 Ir3 C77 N12 -0.9(5) . . . . ? C69 Ir3 C77 N12 85.0(6) . . . . ? C63 Ir3 C77 N12 30.3(19) . . . . ? Cl3 Ir3 C77 N12 -98.3(5) . . . . ? Cl4 Ir3 C77 N12 178.9(5) . . . . ? Ir4 Ir3 C77 N12 -139.3(5) . . . . ? C83 Ir3 C77 N11 176.3(9) . . . . ? C69 Ir3 C77 N11 -97.8(9) . . . . ? C63 Ir3 C77 N11 -152.5(14) . . . . ? Cl3 Ir3 C77 N11 78.9(9) . . . . ? Cl4 Ir3 C77 N11 -3.9(9) . . . . ? Ir4 Ir3 C77 N11 37.9(9) . . . . ? C77 N12 C78 C79 -176.6(7) . . . . ? C76 N12 C78 C79 5.0(13) . . . . ? C77 N12 C78 C83 1.9(10) . . . . ? C76 N12 C78 C83 -176.5(7) . . . . ? C83 C78 C79 C80 2.0(13) . . . . ? N12 C78 C79 C80 -179.7(7) . . . . ? C78 C79 C80 C81 0.2(12) . . . . ? C84 O6 C81 C80 10.6(11) . . . . ? C84 O6 C81 C82 -169.6(7) . . . . ? C79 C80 C81 O6 178.8(7) . . . . ? C79 C80 C81 C82 -1.0(12) . . . . ? O6 C81 C82 C83 179.8(7) . . . . ? C80 C81 C82 C83 -0.4(12) . . . . ? C81 C82 C83 C78 2.3(11) . . . . ? C81 C82 C83 Ir3 -176.4(6) . . . . ? C79 C78 C83 C82 -3.2(12) . . . . ? N12 C78 C83 C82 178.4(6) . . . . ? C79 C78 C83 Ir3 175.7(6) . . . . ? N12 C78 C83 Ir3 -2.7(9) . . . . ? C69 Ir3 C83 C82 85.3(8) . . . . ? C63 Ir3 C83 C82 6.5(8) . . . . ? C77 Ir3 C83 C82 -179.3(8) . . . . ? Cl3 Ir3 C83 C82 -88.8(7) . . . . ? Cl4 Ir3 C83 C82 179(25) . . . . ? Ir4 Ir3 C83 C82 -83.2(8) . . . . ? C69 Ir3 C83 C78 -93.4(6) . . . . ? C63 Ir3 C83 C78 -172.2(6) . . . . ? C77 Ir3 C83 C78 2.0(6) . . . . ? Cl3 Ir3 C83 C78 92.5(6) . . . . ? Cl4 Ir3 C83 C78 0(3) . . . . ? Ir4 Ir3 C83 C78 98.1(6) . . . . ? C91 N13 C85 C86 -177.5(8) . . . . ? C89 N13 C85 C86 -0.1(12) . . . . ? N13 C85 C86 C87 -0.1(14) . . . . ? C85 C86 C87 C88 1.1(15) . . . . ? C86 C87 C88 C89 -2.0(14) . . . . ? C91 N13 C89 C90 -0.6(9) . . . . ? C85 N13 C89 C90 -178.4(7) . . . . ? C91 N13 C89 C88 177.1(7) . . . . ? C85 N13 C89 C88 -0.7(11) . . . . ? C87 C88 C89 C90 178.7(10) . . . . ? C87 C88 C89 N13 1.7(13) . . . . ? N13 C89 C90 N14 0.3(9) . . . . ? C88 C89 C90 N14 -176.8(9) . . . . ? C91 N14 C90 C89 0.0(9) . . . . ? C92 N14 C90 C89 -175.1(8) . . . . ? C85 N13 C91 N14 178.2(7) . . . . ? C89 N13 C91 N14 0.6(8) . . . . ? C85 N13 C91 Ir4 0.0(14) . . . . ? C89 N13 C91 Ir4 -177.7(7) . . . . ? C90 N14 C91 N13 -0.4(8) . . . . ? C92 N14 C91 N13 175.6(6) . . . . ? C90 N14 C91 Ir4 178.5(5) . . . . ? C92 N14 C91 Ir4 -5.6(8) . . . . ? C111 Ir4 C91 N13 -81.4(9) . . . . ? C97 Ir4 C91 N13 -175.5(9) . . . . ? C105 Ir4 C91 N13 -150.9(12) . . . . ? Cl4 Ir4 C91 N13 91.3(9) . . . . ? Cl3 Ir4 C91 N13 9.2(9) . . . . ? Ir3 Ir4 C91 N13 50.5(9) . . . . ? C111 Ir4 C91 N14 100.5(6) . . . . ? C97 Ir4 C91 N14 6.4(5) . . . . ? C105 Ir4 C91 N14 31.0(17) . . . . ? Cl4 Ir4 C91 N14 -86.9(5) . . . . ? Cl3 Ir4 C91 N14 -168.9(5) . . . . ? Ir3 Ir4 C91 N14 -127.6(5) . . . . ? C91 N14 C92 C93 -179.2(7) . . . . ? C90 N14 C92 C93 -4.2(13) . . . . ? C91 N14 C92 C97 0.5(10) . . . . ? C90 N14 C92 C97 175.5(8) . . . . ? C97 C92 C93 C94 -1.8(13) . . . . ? N14 C92 C93 C94 177.8(7) . . . . ? C92 C93 C94 C95 -1.1(13) . . . . ? C98 O7 C95 C96 -167.8(7) . . . . ? C98 O7 C95 C94 12.3(12) . . . . ? C93 C94 C95 C96 1.6(12) . . . . ? C93 C94 C95 O7 -178.5(7) . . . . ? O7 C95 C96 C97 -179.2(7) . . . . ? C94 C95 C96 C97 0.8(12) . . . . ? C93 C92 C97 C96 3.9(11) . . . . ? N14 C92 C97 C96 -175.8(6) . . . . ? C93 C92 C97 Ir4 -175.3(6) . . . . ? N14 C92 C97 Ir4 5.0(9) . . . . ? C95 C96 C97 C92 -3.3(11) . . . . ? C95 C96 C97 Ir4 175.7(6) . . . . ? C111 Ir4 C97 C92 -102.5(6) . . . . ? C105 Ir4 C97 C92 179.0(6) . . . . ? C91 Ir4 C97 C92 -6.2(6) . . . . ? Cl4 Ir4 C97 C92 83.9(6) . . . . ? Cl3 Ir4 C97 C92 32(2) . . . . ? Ir3 Ir4 C97 C92 88.4(6) . . . . ? C111 Ir4 C97 C96 78.5(8) . . . . ? C105 Ir4 C97 C96 0.0(7) . . . . ? C91 Ir4 C97 C96 174.8(8) . . . . ? Cl4 Ir4 C97 C96 -95.2(7) . . . . ? Cl3 Ir4 C97 C96 -147.4(13) . . . . ? Ir3 Ir4 C97 C96 -90.7(7) . . . . ? C105 N15 C99 C100 -179.3(8) . . . . ? C103 N15 C99 C100 1.9(11) . . . . ? N15 C99 C100 C101 0.9(12) . . . . ? C99 C100 C101 C102 -1.7(14) . . . . ? C100 C101 C102 C103 -0.4(14) . . . . ? C101 C102 C103 C104 -179.2(10) . . . . ? C101 C102 C103 N15 3.1(13) . . . . ? C105 N15 C103 C104 -1.2(9) . . . . ? C99 N15 C103 C104 177.7(7) . . . . ? C105 N15 C103 C102 177.1(7) . . . . ? C99 N15 C103 C102 -4.0(12) . . . . ? C102 C103 C104 N16 -178.0(10) . . . . ? N15 C103 C104 N16 -0.1(9) . . . . ? C105 N16 C104 C103 1.4(10) . . . . ? C106 N16 C104 C103 -179.5(8) . . . . ? C99 N15 C105 N16 -176.9(7) . . . . ? C103 N15 C105 N16 2.0(8) . . . . ? C99 N15 C105 Ir4 -10.5(14) . . . . ? C103 N15 C105 Ir4 168.3(7) . . . . ? C104 N16 C105 N15 -2.0(9) . . . . ? C106 N16 C105 N15 178.7(6) . . . . ? C104 N16 C105 Ir4 -172.6(5) . . . . ? C106 N16 C105 Ir4 8.2(9) . . . . ? C111 Ir4 C105 N15 -171.1(9) . . . . ? C97 Ir4 C105 N15 -75.5(9) . . . . ? C91 Ir4 C105 N15 -99.7(15) . . . . ? Cl4 Ir4 C105 N15 17.7(9) . . . . ? Cl3 Ir4 C105 N15 100.3(9) . . . . ? Ir3 Ir4 C105 N15 59.2(9) . . . . ? C111 Ir4 C105 N16 -6.0(6) . . . . ? C97 Ir4 C105 N16 89.6(6) . . . . ? C91 Ir4 C105 N16 65.5(16) . . . . ? Cl4 Ir4 C105 N16 -177.2(5) . . . . ? Cl3 Ir4 C105 N16 -94.6(6) . . . . ? Ir3 Ir4 C105 N16 -135.6(6) . . . . ? C105 N16 C106 C107 171.5(8) . . . . ? C104 N16 C106 C107 -7.6(14) . . . . ? C105 N16 C106 C111 -5.6(10) . . . . ? C104 N16 C106 C111 175.3(8) . . . . ? C111 C106 C107 C108 0.3(14) . . . . ? N16 C106 C107 C108 -176.4(8) . . . . ? C106 C107 C108 C109 3.8(13) . . . . ? C107 C108 C109 O8 173.1(8) . . . . ? C107 C108 C109 C110 -4.5(13) . . . . ? C112 O8 C109 C108 7.9(12) . . . . ? C112 O8 C109 C110 -174.3(7) . . . . ? C108 C109 C110 C111 1.2(12) . . . . ? O8 C109 C110 C111 -176.7(7) . . . . ? C107 C106 C111 C110 -3.5(13) . . . . ? N16 C106 C111 C110 173.5(7) . . . . ? C107 C106 C111 Ir4 -176.4(7) . . . . ? N16 C106 C111 Ir4 0.6(9) . . . . ? C109 C110 C111 C106 2.7(11) . . . . ? C109 C110 C111 Ir4 174.7(6) . . . . ? C97 Ir4 C111 C106 -85.0(7) . . . . ? C105 Ir4 C111 C106 2.9(6) . . . . ? C91 Ir4 C111 C106 -165.2(6) . . . . ? Cl4 Ir4 C111 C106 58.4(15) . . . . ? Cl3 Ir4 C111 C106 100.6(6) . . . . ? Ir3 Ir4 C111 C106 85.1(7) . . . . ? C97 Ir4 C111 C110 103.3(7) . . . . ? C105 Ir4 C111 C110 -168.9(8) . . . . ? C91 Ir4 C111 C110 23.1(7) . . . . ? Cl4 Ir4 C111 C110 -113.3(12) . . . . ? Cl3 Ir4 C111 C110 -71.1(7) . . . . ? Ir3 Ir4 C111 C110 -86.6(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 Cl1 0.95 2.53 3.359(9) 145.5 . C29 H29 Cl1 0.95 2.54 3.365(8) 145.5 . C15 H15 Cl2 0.95 2.61 3.427(9) 144.5 . C43 H43 Cl2 0.95 2.60 3.432(9) 145.8 . C57 H57 Cl3 0.95 2.50 3.318(9) 144.2 . C85 H85 Cl3 0.95 2.56 3.370(9) 142.9 . C99 H99 Cl4 0.95 2.52 3.343(9) 145.1 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.703 _refine_diff_density_min -2.402 _refine_diff_density_rms 0.207 # end of cif #===END data_CCDC656910(mer-3a) _database_code_depnum_ccdc_archive 'CCDC 656910' _audit_creation_date ' 2006-02-24T19:18:14 ' _audit_update_record ' 2006-04-19T15:24:35 ' _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution DIRDIF-99 _chemical_name_common ; racemic-mer-tris(kappa$2!C3,C2'-2-phenyl-pyrido(1,2-c) imidazo-3-ylidene)iridium(iii) ; _chemical_melting_point ? _chemical_temperature_decomposition_gt 509 _chemical_properties_physical ' emission luminescence ' _chemical_name_systematic ; racemic-mer-tris(\k^2^C3,C2'-2-phenyl-pyrido[1,2-c] imidazo-3-ylidene)iridium(III) ; _chemical_formula_structural ' (C13 H9 N2)3 Ir ' _chemical_formula_iupac ' [Ir (C13 H9 N2)3] ' _chemical_formula_moiety 'Ir, 3(C13 H9 N2)' _chemical_formula_sum 'C39 H27 Ir N6' _chemical_formula_weight 771.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M ' I41/a ' _symmetry_Int_Tables_number 88 _symmetry_space_group_name_Hall ' -I 4ad ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.109(2) _cell_length_b 19.109(2) _cell_length_c 35.200(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12853(3) _cell_formula_units_Z 16 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 69903 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.47 _exptl_crystal_preparation 'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(2) K' _exptl_crystal_recrystallization_method 'crystallized from a solution of CHCl3/hexsan at ambient temperature' _exptl_crystal_description ' needle ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6080 _exptl_absorpt_coefficient_mu 4.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.239 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details ; Higashi, T. (1995). ABSCOR - Program for Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; Indexing was performed from 3 oscillations which were exposed for 3.0 minutes. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. #1 Phi= 0.0, chi=45.0, omega=0.0 to 180.0 with 3.0deg step #2 Phi=135.0, chi=45.0, omega=0.0 to 180.0 with 3.0deg step A total of 120 images, corresponding to 360.0 deg. osillation angles, were collected with 2 different goniometer setting. Exposure time was 150 seconds per degree. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ' 0.8 mm double pinhole ' _diffrn_source_power 50 _diffrn_source_current 40 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_radiation_detector 'imaging plate' _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_device_details ; RAPID: Eulerian 3-circle ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123986 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9323 _reflns_number_gt 7082 _reflns_threshold_expression >2sigma(I) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+624.0211P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9323 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.1137 _refine_ls_wR_factor_ref 0.2301 _refine_ls_wR_factor_gt 0.2202 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2451(8) 0.3716(7) 0.0260(3) 0.053(3) Uani 1 1 d . . . C2 C 0.2570(9) 0.2671(10) 0.0597(5) 0.085(5) Uani 1 1 d . A . H2 H 0.2744 0.2337 0.0773 0.102 Uiso 1 1 calc R . . C3 C 0.2041(8) 0.2585(8) 0.0357(5) 0.075(5) Uani 1 1 d . A . C4 C 0.1578(11) 0.2033(9) 0.0259(7) 0.097(7) Uani 1 1 d . . . H4 H 0.1610 0.1602 0.0393 0.116 Uiso 1 1 calc R . . C5 C 0.1100(11) 0.2096(10) -0.0016(6) 0.094(6) Uani 1 1 d . . . H5 H 0.0814 0.1711 -0.0086 0.113 Uiso 1 1 calc R . . C6 C 0.1031(9) 0.2759(8) -0.0200(5) 0.078(5) Uani 1 1 d . . . H6 H 0.0670 0.2826 -0.0382 0.093 Uiso 1 1 calc R . . C7 C 0.1467(10) 0.3286(8) -0.0120(4) 0.076(5) Uani 1 1 d . . . H7 H 0.1429 0.3713 -0.0257 0.091 Uiso 1 1 calc R . . C8 C 0.3373(9) 0.3724(9) 0.0703(4) 0.069(4) Uani 1 1 d . A . C9 C 0.3451(8) 0.4404(8) 0.0564(4) 0.059(3) Uani 1 1 d . A . C10 C 0.4026(8) 0.4776(8) 0.0706(4) 0.065(4) Uani 1 1 d . . . H10 H 0.4112 0.5237 0.0615 0.078 Uiso 1 1 calc R . . C11 C 0.4475(9) 0.4489(10) 0.0977(5) 0.080(5) Uani 1 1 d . . . H11 H 0.4858 0.4758 0.1068 0.096 Uiso 1 1 calc R . . C12 C 0.4376(10) 0.3829(12) 0.1115(6) 0.099(7) Uani 1 1 d . . . H12 H 0.4682 0.3641 0.1302 0.119 Uiso 1 1 calc R . . C13 C 0.3829(9) 0.3444(11) 0.0979(6) 0.091(6) Uani 1 1 d . . . H13 H 0.3754 0.2982 0.1071 0.109 Uiso 1 1 calc R . . C14 C 0.2931(12) 0.5702(9) 0.0226(5) 0.099(7) Uani 1 1 d . . . C15 C 0.2805(11) 0.6772(11) 0.0529(8) 0.131(11) Uani 1 1 d . A . H15 H 0.2637 0.7119 0.0699 0.157 Uiso 1 1 calc R . . C16 C 0.3302(9) 0.6869(8) 0.0265(7) 0.090(7) Uani 1 1 d . A . C17 C 0.3681(11) 0.7429(10) 0.0149(8) 0.109(8) Uani 1 1 d . . . H17 H 0.3629 0.7871 0.0269 0.131 Uiso 1 1 calc R . . C18 C 0.4111(11) 0.7344(9) -0.0127(7) 0.092(6) Uani 1 1 d . . . H18 H 0.4379 0.7735 -0.0208 0.110 Uiso 1 1 calc R . . C19 C 0.4208(9) 0.6675(9) -0.0322(5) 0.080(5) Uani 1 1 d . . . H19 H 0.4543 0.6619 -0.0520 0.096 Uiso 1 1 calc R . . C20 C 0.3795(9) 0.6142(8) -0.0205(5) 0.072(5) Uani 1 1 d . . . H20 H 0.3826 0.5702 -0.0330 0.086 Uiso 1 1 calc R . . C21 C 0.2087(8) 0.5653(12) 0.0747(5) 0.088(6) Uani 1 1 d . A . C22 C 0.2033(7) 0.5014(9) 0.0617(4) 0.061(4) Uani 1 1 d . A . C23 C 0.1591(8) 0.4616(11) 0.0842(4) 0.078(5) Uani 1 1 d . . . H23 H 0.1541 0.4131 0.0792 0.093 Uiso 1 1 calc R . . C24 C 0.1216(11) 0.4918(15) 0.1144(6) 0.120(9) Uani 1 1 d . . . H24 H 0.0904 0.4626 0.1282 0.145 Uiso 1 1 calc R . . C25 C 0.1268(12) 0.5584(17) 0.1249(9) 0.152(13) Uani 1 1 d . . . H25 H 0.1013 0.5762 0.1460 0.182 Uiso 1 1 calc R . . C26 C 0.1701(11) 0.5996(12) 0.1044(7) 0.114(8) Uani 1 1 d . . . H26 H 0.1747 0.6483 0.1094 0.137 Uiso 1 1 calc R . . Ir1 Ir 0.26927(4) 0.47067(3) 0.017278(13) 0.0604(2) Uani 1 1 d . . . N1 N 0.2823(6) 0.3357(7) 0.0539(4) 0.065(3) Uani 1 1 d . . . N2 N 0.1966(7) 0.3217(6) 0.0155(3) 0.061(3) Uani 1 1 d . . . N3 N 0.2575(7) 0.6082(7) 0.0513(4) 0.078(4) Uani 1 1 d . . . N4 N 0.3340(7) 0.6218(6) 0.0084(4) 0.064(3) Uani 1 1 d . . . N5 N 0.2474(11) 0.4605(11) -0.0677(6) 0.030(5) Uiso 0.50 1 d P A 1 C36 C 0.4204(15) 0.4154(15) -0.0239(8) 0.038(6) Uiso 0.50 1 d P A 1 H36 H 0.4438 0.4177 -0.0001 0.045 Uiso 0.50 1 calc PR A 1 C39 C 0.345(2) 0.4080(19) -0.0939(11) 0.054(9) Uiso 0.50 1 d P A 1 H39 H 0.3177 0.4048 -0.1165 0.065 Uiso 0.50 1 calc PR A 1 C37 C 0.4576(17) 0.3928(17) -0.0548(9) 0.043(7) Uiso 0.50 1 d P A 1 H37 H 0.5059 0.3817 -0.0523 0.051 Uiso 0.50 1 calc PR A 1 C29 C 0.1483(19) 0.4905(19) -0.0820(10) 0.058(9) Uiso 0.50 1 d P A 1 N6 N 0.1592(9) 0.5020(9) -0.0414(5) 0.031(3) Uiso 0.50 1 d P A 1 C27 C 0.2226(12) 0.4791(12) -0.0304(6) 0.039(4) Uiso 0.50 1 d P A 1 C35 C 0.3490(11) 0.4354(11) -0.0252(6) 0.033(4) Uiso 0.50 1 d P A 1 C34 C 0.3200(11) 0.4311(11) -0.0622(6) 0.034(4) Uiso 0.50 1 d P A 1 C38 C 0.4234(19) 0.3858(18) -0.0916(10) 0.066(8) Uiso 0.50 1 d P A 1 H38 H 0.4477 0.3686 -0.1132 0.079 Uiso 0.50 1 calc PR A 1 C28 C 0.2066(15) 0.4670(15) -0.0957(8) 0.058(7) Uiso 0.50 1 d P A 1 H28 H 0.2167 0.4568 -0.1215 0.069 Uiso 0.50 1 calc PR A 1 C33 C 0.105(2) 0.527(2) -0.0187(10) 0.047(9) Uiso 0.50 1 d P A 1 H33 H 0.1114 0.5270 0.0081 0.056 Uiso 0.50 1 calc PR A 1 C32 C 0.0452(15) 0.5502(16) -0.0325(8) 0.040(6) Uiso 0.50 1 d P A 1 H32 H 0.0110 0.5700 -0.0162 0.048 Uiso 0.50 1 calc PR A 1 C30 C 0.086(2) 0.515(2) -0.0945(12) 0.080(10) Uiso 0.50 1 d P A 1 H30 H 0.0776 0.5116 -0.1210 0.096 Uiso 0.50 1 calc PR A 1 C31 C 0.0328(18) 0.5450(16) -0.0729(9) 0.064(8) Uiso 0.50 1 d P A 1 H31 H -0.0094 0.5611 -0.0841 0.077 Uiso 0.50 1 calc PR A 1 N7 N 0.2626(12) 0.4638(11) -0.0608(6) 0.033(5) Uiso 0.50 1 d P A 2 C47 C 0.4221(17) 0.4077(17) -0.0341(9) 0.046(8) Uiso 0.50 1 d P A 2 H47 H 0.4300 0.4142 -0.0077 0.055 Uiso 0.50 1 calc PR A 2 C42 C 0.360(2) 0.4202(19) -0.0923(10) 0.052(9) Uiso 0.50 1 d P A 2 C46 C 0.471(2) 0.379(2) -0.0553(13) 0.066(12) Uiso 0.50 1 d P A 2 H46 H 0.5120 0.3618 -0.0432 0.079 Uiso 0.50 1 calc PR A 2 C53 C 0.1413(16) 0.5110(16) -0.0847(9) 0.045(7) Uiso 0.50 1 d P A 2 H53 H 0.1545 0.5061 -0.1106 0.053 Uiso 0.50 1 calc PR A 2 C50 C 0.1071(18) 0.5249(18) -0.0097(10) 0.042(8) Uiso 0.50 1 d P A 2 H50 H 0.0939 0.5320 0.0161 0.050 Uiso 0.50 1 calc PR A 2 C51 C 0.059(2) 0.538(2) -0.0390(11) 0.066(11) Uiso 0.50 1 d P A 2 H51 H 0.0120 0.5493 -0.0324 0.079 Uiso 0.50 1 calc PR A 2 N8 N 0.3574(10) 0.4294(9) -0.0505(5) 0.037(4) Uiso 0.50 1 d P A 2 C49 C 0.1761(12) 0.5012(11) -0.0186(6) 0.038(4) Uiso 0.50 1 d P A 2 C40 C 0.3000(13) 0.4580(13) -0.0319(7) 0.045(5) Uiso 0.50 1 d P A 2 C52 C 0.076(2) 0.534(2) -0.0759(12) 0.081(10) Uiso 0.50 1 d P A 2 H52 H 0.0441 0.5470 -0.0951 0.097 Uiso 0.50 1 calc PR A 2 C41 C 0.2866(16) 0.4462(16) -0.0991(9) 0.064(7) Uiso 0.50 1 d P A 2 H41 H 0.2620 0.4501 -0.1225 0.077 Uiso 0.50 1 calc PR A 2 C48 C 0.1877(13) 0.4948(13) -0.0569(7) 0.043(5) Uiso 0.50 1 d P A 2 C43 C 0.4058(18) 0.3919(18) -0.1113(11) 0.073(9) Uiso 0.50 1 d P A 2 H43 H 0.3992 0.3848 -0.1377 0.088 Uiso 0.50 1 calc PR A 2 C45 C 0.465(2) 0.371(2) -0.0946(11) 0.085(11) Uiso 0.50 1 d P A 2 H45 H 0.5022 0.3519 -0.1092 0.102 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.072(9) 0.048(7) 0.039(6) 0.003(5) 0.006(6) -0.014(6) C2 0.067(10) 0.087(12) 0.100(13) 0.040(10) 0.008(10) -0.027(9) C3 0.058(9) 0.061(9) 0.106(13) 0.038(9) 0.005(9) -0.002(7) C4 0.098(14) 0.051(9) 0.141(19) 0.025(11) 0.026(13) -0.027(9) C5 0.103(15) 0.076(12) 0.104(15) 0.025(11) -0.016(12) -0.036(11) C6 0.081(11) 0.061(9) 0.091(12) 0.014(9) -0.012(9) -0.027(8) C7 0.113(14) 0.054(8) 0.060(9) 0.015(7) -0.019(9) -0.041(9) C8 0.067(10) 0.072(10) 0.066(9) 0.023(8) 0.007(8) 0.006(8) C9 0.062(8) 0.070(9) 0.043(7) 0.004(6) 0.007(6) -0.004(7) C10 0.071(10) 0.067(9) 0.057(8) 0.008(7) 0.011(7) 0.000(8) C11 0.057(9) 0.096(13) 0.088(12) 0.011(10) -0.008(9) -0.006(9) C12 0.073(12) 0.122(17) 0.102(15) 0.049(13) -0.009(11) -0.008(12) C13 0.056(10) 0.109(15) 0.109(14) 0.043(12) -0.007(10) -0.012(10) C14 0.154(19) 0.077(11) 0.065(10) 0.024(9) -0.044(11) -0.067(12) C15 0.075(13) 0.103(16) 0.22(3) -0.094(18) -0.054(16) -0.013(12) C16 0.049(9) 0.049(9) 0.17(2) -0.015(11) -0.030(11) -0.007(7) C17 0.067(12) 0.069(12) 0.19(3) -0.023(15) -0.011(15) -0.017(10) C18 0.080(13) 0.046(9) 0.15(2) 0.011(11) -0.014(13) -0.010(9) C19 0.066(10) 0.074(11) 0.100(13) 0.026(9) -0.012(9) -0.030(8) C20 0.084(11) 0.051(8) 0.080(11) 0.021(8) -0.029(9) -0.026(8) C21 0.041(8) 0.137(17) 0.087(12) -0.052(12) 0.004(8) -0.024(9) C22 0.049(8) 0.092(11) 0.043(7) -0.017(7) -0.014(6) 0.000(7) C23 0.051(8) 0.123(15) 0.060(9) -0.004(9) 0.006(7) 0.000(9) C24 0.074(13) 0.18(3) 0.107(17) -0.046(17) 0.043(12) -0.018(15) C25 0.079(15) 0.20(3) 0.18(3) -0.11(2) 0.042(17) -0.018(18) C26 0.084(14) 0.105(16) 0.15(2) -0.071(16) 0.014(14) -0.016(12) Ir1 0.1079(5) 0.0440(3) 0.0295(2) -0.0009(2) -0.0074(3) -0.0220(3) N1 0.058(7) 0.067(8) 0.069(8) 0.028(6) 0.005(6) -0.018(6) N2 0.074(8) 0.051(6) 0.059(7) 0.011(5) 0.011(6) -0.016(6) N3 0.079(9) 0.061(8) 0.094(10) -0.038(7) -0.037(8) -0.010(7) N4 0.069(8) 0.051(7) 0.073(8) 0.003(6) -0.016(7) -0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.380(17) . ? C1 N1 1.396(17) . ? C1 Ir1 1.973(12) . ? C2 C3 1.33(2) . ? C2 N1 1.411(19) . ? C2 H2 0.9500 . ? C3 N2 1.409(17) . ? C3 C4 1.42(2) . ? C4 C5 1.33(3) . ? C4 H4 0.9500 . ? C5 C6 1.43(2) . ? C5 H5 0.9500 . ? C6 C7 1.335(19) . ? C6 H6 0.9500 . ? C7 N2 1.366(19) . ? C7 H7 0.9500 . ? C8 N1 1.39(2) . ? C8 C9 1.40(2) . ? C8 C13 1.41(2) . ? C9 C10 1.40(2) . ? C9 Ir1 2.080(14) . ? C10 C11 1.40(2) . ? C10 H10 0.9500 . ? C11 C12 1.36(2) . ? C11 H11 0.9500 . ? C12 C13 1.37(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N4 1.354(19) . ? C14 N3 1.42(3) . ? C14 Ir1 1.965(16) . ? C15 C16 1.34(3) . ? C15 N3 1.39(2) . ? C15 H15 0.9500 . ? C16 C17 1.35(3) . ? C16 N4 1.40(2) . ? C17 C18 1.28(3) . ? C17 H17 0.9500 . ? C18 C19 1.46(3) . ? C18 H18 0.9500 . ? C19 C20 1.354(19) . ? C19 H19 0.9500 . ? C20 N4 1.35(2) . ? C20 H20 0.9500 . ? C21 C22 1.31(2) . ? C21 C26 1.44(2) . ? C21 N3 1.49(2) . ? C22 C23 1.38(2) . ? C22 Ir1 2.094(14) . ? C23 C24 1.40(2) . ? C23 H23 0.9500 . ? C24 C25 1.33(3) . ? C24 H24 0.9500 . ? C25 C26 1.35(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Ir1 C40 1.84(2) . ? Ir1 C27 1.91(2) . ? Ir1 C35 2.24(2) . ? Ir1 C49 2.26(2) . ? N5 C28 1.26(3) . ? N5 C27 1.44(3) . ? N5 C34 1.51(3) . ? C36 C37 1.37(4) . ? C36 C35 1.42(3) . ? C36 H36 0.9500 . ? C39 C34 1.29(4) . ? C39 C38 1.56(5) . ? C39 H39 0.9500 . ? C37 C38 1.46(5) . ? C37 H37 0.9500 . ? C29 C28 1.29(4) . ? C29 C30 1.35(5) . ? C29 N6 1.46(4) . ? N6 C27 1.35(3) . ? N6 C33 1.39(4) . ? C35 C34 1.42(3) . ? C38 H38 0.9500 . ? C28 H28 0.9500 . ? C33 C32 1.32(5) . ? C33 H33 0.9500 . ? C32 C31 1.45(4) . ? C32 H32 0.9500 . ? C30 C31 1.39(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? N7 C40 1.25(3) . ? N7 C41 1.46(4) . ? N7 C48 1.55(3) . ? C47 C46 1.32(5) . ? C47 N8 1.43(4) . ? C47 H47 0.9500 . ? C42 C43 1.23(5) . ? C42 N8 1.48(4) . ? C42 C41 1.50(5) . ? C46 C45 1.40(6) . ? C46 H46 0.9500 . ? C53 C52 1.35(5) . ? C53 C48 1.36(4) . ? C53 H53 0.9500 . ? C50 C51 1.41(5) . ? C50 C49 1.43(4) . ? C50 H50 0.9500 . ? C51 C52 1.34(5) . ? C51 H51 0.9500 . ? N8 C40 1.39(3) . ? C49 C48 1.37(3) . ? C52 H52 0.9500 . ? C41 H41 0.9500 . ? C43 C45 1.33(5) . ? C43 H43 0.9500 . ? C45 H45 0.9500 . ? 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_3 _geom_angle_publ_flag N2 C1 N1 101.0(11) . . ? N2 C1 Ir1 141.2(11) . . ? N1 C1 Ir1 117.5(10) . . ? C3 C2 N1 106.6(15) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 107.0(15) . . ? C2 C3 C4 136.2(17) . . ? N2 C3 C4 116.8(16) . . ? C5 C4 C3 122.3(17) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 118.2(17) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C7 C6 C5 121.0(17) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 N2 120.8(14) . . ? C6 C7 H7 119.6 . . ? N2 C7 H7 119.6 . . ? N1 C8 C9 113.9(13) . . ? N1 C8 C13 124.1(15) . . ? C9 C8 C13 122.0(17) . . ? C8 C9 C10 115.5(14) . . ? C8 C9 Ir1 114.7(11) . . ? C10 C9 Ir1 129.9(11) . . ? C11 C10 C9 121.7(15) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C12 C11 C10 121.5(17) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.7(18) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C8 120.6(18) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? N4 C14 N3 99.7(15) . . ? N4 C14 Ir1 143.4(18) . . ? N3 C14 Ir1 116.9(12) . . ? C16 C15 N3 109.0(19) . . ? C16 C15 H15 125.5 . . ? N3 C15 H15 125.5 . . ? C15 C16 C17 134(2) . . ? C15 C16 N4 103.2(15) . . ? C17 C16 N4 123(2) . . ? C18 C17 C16 118(2) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C19 123.2(18) . . ? C17 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C20 C19 C18 116.2(19) . . ? C20 C19 H19 121.9 . . ? C18 C19 H19 121.9 . . ? N4 C20 C19 121.6(17) . . ? N4 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C26 129.8(19) . . ? C22 C21 N3 111.6(14) . . ? C26 C21 N3 118.2(18) . . ? C21 C22 C23 111.1(15) . . ? C21 C22 Ir1 118.4(13) . . ? C23 C22 Ir1 129.8(13) . . ? C22 C23 C24 121(2) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 124(2) . . ? C25 C24 H24 117.8 . . ? C23 C24 H24 117.8 . . ? C24 C25 C26 117(2) . . ? C24 C25 H25 121.5 . . ? C26 C25 H25 121.5 . . ? C25 C26 C21 116(2) . . ? C25 C26 H26 122.1 . . ? C21 C26 H26 122.1 . . ? C40 Ir1 C27 48.2(10) . . ? C40 Ir1 C14 98.2(10) . . ? C27 Ir1 C14 96.3(8) . . ? C40 Ir1 C1 95.4(8) . . ? C27 Ir1 C1 96.2(8) . . ? C14 Ir1 C1 165.6(6) . . ? C40 Ir1 C9 111.3(9) . . ? C27 Ir1 C9 158.6(8) . . ? C14 Ir1 C9 92.6(7) . . ? C1 Ir1 C9 78.1(6) . . ? C40 Ir1 C22 158.5(8) . . ? C27 Ir1 C22 110.7(8) . . ? C14 Ir1 C22 78.3(8) . . ? C1 Ir1 C22 90.7(6) . . ? C9 Ir1 C22 90.2(5) . . ? C40 Ir1 C35 27.9(9) . . ? C27 Ir1 C35 75.8(9) . . ? C14 Ir1 C35 101.4(9) . . ? C1 Ir1 C35 88.5(6) . . ? C9 Ir1 C35 83.3(6) . . ? C22 Ir1 C35 173.5(6) . . ? C40 Ir1 C49 76.1(9) . . ? C27 Ir1 C49 28.1(8) . . ? C14 Ir1 C49 89.2(8) . . ? C1 Ir1 C49 98.6(7) . . ? C9 Ir1 C49 172.1(7) . . ? C22 Ir1 C49 82.6(7) . . ? C35 Ir1 C49 103.9(8) . . ? C8 N1 C1 115.5(11) . . ? C8 N1 C2 132.0(14) . . ? C1 N1 C2 112.5(13) . . ? C7 N2 C1 126.3(12) . . ? C7 N2 C3 120.8(13) . . ? C1 N2 C3 112.9(13) . . ? C15 N3 C14 111.3(18) . . ? C15 N3 C21 134.1(18) . . ? C14 N3 C21 114.4(13) . . ? C20 N4 C14 124.9(15) . . ? C20 N4 C16 118.3(15) . . ? C14 N4 C16 116.7(17) . . ? C28 N5 C27 119(2) . . ? C28 N5 C34 135(2) . . ? C27 N5 C34 106.2(18) . . ? C37 C36 C35 124(3) . . ? C37 C36 H36 118.0 . . ? C35 C36 H36 118.0 . . ? C34 C39 C38 114(3) . . ? C34 C39 H39 123.2 . . ? C38 C39 H39 123.2 . . ? C36 C37 C38 120(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C28 C29 C30 139(4) . . ? C28 C29 N6 107(3) . . ? C30 C29 N6 113(3) . . ? C27 N6 C33 128(2) . . ? C27 N6 C29 111(2) . . ? C33 N6 C29 120(2) . . ? N6 C27 N5 96.6(18) . . ? N6 C27 Ir1 134.6(17) . . ? N5 C27 Ir1 128.8(17) . . ? C36 C35 C34 113(2) . . ? C36 C35 Ir1 135.5(17) . . ? C34 C35 Ir1 111.4(14) . . ? C39 C34 C35 132(3) . . ? C39 C34 N5 111(2) . . ? C35 C34 N5 117.1(18) . . ? C37 C38 C39 117(3) . . ? C37 C38 H38 121.5 . . ? C39 C38 H38 121.5 . . ? N5 C28 C29 106(3) . . ? N5 C28 H28 127.0 . . ? C29 C28 H28 127.0 . . ? C32 C33 N6 123(3) . . ? C32 C33 H33 118.4 . . ? N6 C33 H33 118.4 . . ? C33 C32 C31 119(3) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C29 C30 C31 127(4) . . ? C29 C30 H30 116.3 . . ? C31 C30 H30 116.3 . . ? C30 C31 C32 117(3) . . ? C30 C31 H31 121.7 . . ? C32 C31 H31 121.7 . . ? C40 N7 C41 123(2) . . ? C40 N7 C48 119(2) . . ? C41 N7 C48 117(2) . . ? C46 C47 N8 120(3) . . ? C46 C47 H47 119.8 . . ? N8 C47 H47 119.8 . . ? C43 C42 N8 128(4) . . ? C43 C42 C41 136(4) . . ? N8 C42 C41 95(3) . . ? C47 C46 C45 123(4) . . ? C47 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? C52 C53 C48 121(3) . . ? C52 C53 H53 119.7 . . ? C48 C53 H53 119.7 . . ? C51 C50 C49 120(3) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 123(4) . . ? C52 C51 H51 118.7 . . ? C50 C51 H51 118.7 . . ? C40 N8 C47 127(2) . . ? C40 N8 C42 123(2) . . ? C47 N8 C42 110(2) . . ? C48 C49 C50 113(2) . . ? C48 C49 Ir1 113.5(17) . . ? C50 C49 Ir1 133(2) . . ? N7 C40 N8 96(2) . . ? N7 C40 Ir1 124.8(19) . . ? N8 C40 Ir1 138.2(18) . . ? C51 C52 C53 118(4) . . ? C51 C52 H52 121.1 . . ? C53 C52 H52 121.1 . . ? N7 C41 C42 103(3) . . ? N7 C41 H41 128.6 . . ? C42 C41 H41 128.6 . . ? C53 C48 C49 126(3) . . ? C53 C48 N7 129(2) . . ? C49 C48 N7 105.6(19) . . ? C42 C43 C45 120(4) . . ? C42 C43 H43 120.0 . . ? C45 C43 H43 120.0 . . ? C43 C45 C46 118(4) . . ? C43 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? 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 N1 C2 C3 N2 0(2) . . . . ? N1 C2 C3 C4 178(2) . . . . ? C2 C3 C4 C5 -177(2) . . . . ? N2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C6 -4(3) . . . . ? C4 C5 C6 C7 5(3) . . . . ? C5 C6 C7 N2 -4(3) . . . . ? N1 C8 C9 C10 -176.4(13) . . . . ? C13 C8 C9 C10 2(2) . . . . ? N1 C8 C9 Ir1 3.4(18) . . . . ? C13 C8 C9 Ir1 -178.0(14) . . . . ? C8 C9 C10 C11 -2(2) . . . . ? Ir1 C9 C10 C11 178.4(12) . . . . ? C9 C10 C11 C12 0(3) . . . . ? C10 C11 C12 C13 1(3) . . . . ? C11 C12 C13 C8 0(3) . . . . ? N1 C8 C13 C12 177.3(18) . . . . ? C9 C8 C13 C12 -1(3) . . . . ? N3 C15 C16 C17 177(2) . . . . ? N3 C15 C16 N4 2(2) . . . . ? C15 C16 C17 C18 -178(2) . . . . ? N4 C16 C17 C18 -3(3) . . . . ? C16 C17 C18 C19 0(3) . . . . ? C17 C18 C19 C20 2(3) . . . . ? C18 C19 C20 N4 -2(2) . . . . ? C26 C21 C22 C23 -9(3) . . . . ? N3 C21 C22 C23 178.7(13) . . . . ? C26 C21 C22 Ir1 179.5(19) . . . . ? N3 C21 C22 Ir1 7(2) . . . . ? C21 C22 C23 C24 6(2) . . . . ? Ir1 C22 C23 C24 176.3(15) . . . . ? C22 C23 C24 C25 -3(4) . . . . ? C23 C24 C25 C26 2(5) . . . . ? C24 C25 C26 C21 -3(4) . . . . ? C22 C21 C26 C25 8(4) . . . . ? N3 C21 C26 C25 -180(2) . . . . ? N4 C14 Ir1 C40 -21(2) . . . . ? N3 C14 Ir1 C40 159.0(14) . . . . ? N4 C14 Ir1 C27 -70(2) . . . . ? N3 C14 Ir1 C27 110.4(14) . . . . ? N4 C14 Ir1 C1 140(3) . . . . ? N3 C14 Ir1 C1 -40(4) . . . . ? N4 C14 Ir1 C9 91(2) . . . . ? N3 C14 Ir1 C9 -89.1(14) . . . . ? N4 C14 Ir1 C22 -180(2) . . . . ? N3 C14 Ir1 C22 0.6(12) . . . . ? N4 C14 Ir1 C35 7(2) . . . . ? N3 C14 Ir1 C35 -172.8(13) . . . . ? N4 C14 Ir1 C49 -97(2) . . . . ? N3 C14 Ir1 C49 83.2(14) . . . . ? N2 C1 Ir1 C40 -71.3(18) . . . . ? N1 C1 Ir1 C40 116.4(13) . . . . ? N2 C1 Ir1 C27 -22.8(18) . . . . ? N1 C1 Ir1 C27 164.9(12) . . . . ? N2 C1 Ir1 C14 128(3) . . . . ? N1 C1 Ir1 C14 -45(4) . . . . ? N2 C1 Ir1 C9 178.1(17) . . . . ? N1 C1 Ir1 C9 5.8(10) . . . . ? N2 C1 Ir1 C22 88.1(16) . . . . ? N1 C1 Ir1 C22 -84.3(11) . . . . ? N2 C1 Ir1 C35 -98.4(17) . . . . ? N1 C1 Ir1 C35 89.3(11) . . . . ? N2 C1 Ir1 C49 5.4(17) . . . . ? N1 C1 Ir1 C49 -166.9(11) . . . . ? C8 C9 Ir1 C40 -96.2(13) . . . . ? C10 C9 Ir1 C40 83.6(16) . . . . ? C8 C9 Ir1 C27 -81(2) . . . . ? C10 C9 Ir1 C27 98(2) . . . . ? C8 C9 Ir1 C14 164.0(13) . . . . ? C10 C9 Ir1 C14 -16.2(15) . . . . ? C8 C9 Ir1 C1 -4.9(11) . . . . ? C10 C9 Ir1 C1 174.8(14) . . . . ? C8 C9 Ir1 C22 85.7(12) . . . . ? C10 C9 Ir1 C22 -94.5(14) . . . . ? C8 C9 Ir1 C35 -94.8(12) . . . . ? C10 C9 Ir1 C35 84.9(14) . . . . ? C8 C9 Ir1 C49 61(5) . . . . ? C10 C9 Ir1 C49 -119(5) . . . . ? C21 C22 Ir1 C40 -87(3) . . . . ? C23 C22 Ir1 C40 103(3) . . . . ? C21 C22 Ir1 C27 -96.8(15) . . . . ? C23 C22 Ir1 C27 93.1(15) . . . . ? C21 C22 Ir1 C14 -4.4(14) . . . . ? C23 C22 Ir1 C14 -174.5(15) . . . . ? C21 C22 Ir1 C1 166.3(14) . . . . ? C23 C22 Ir1 C1 -3.8(14) . . . . ? C21 C22 Ir1 C9 88.2(14) . . . . ? C23 C22 Ir1 C9 -81.9(14) . . . . ? C21 C22 Ir1 C35 83(6) . . . . ? C23 C22 Ir1 C35 -87(6) . . . . ? C21 C22 Ir1 C49 -95.1(14) . . . . ? C23 C22 Ir1 C49 94.8(14) . . . . ? C9 C8 N1 C1 1(2) . . . . ? C13 C8 N1 C1 -177.3(16) . . . . ? C9 C8 N1 C2 179.9(16) . . . . ? C13 C8 N1 C2 1(3) . . . . ? N2 C1 N1 C8 179.1(13) . . . . ? Ir1 C1 N1 C8 -5.8(17) . . . . ? N2 C1 N1 C2 0.2(16) . . . . ? Ir1 C1 N1 C2 175.4(11) . . . . ? C3 C2 N1 C8 -178.5(17) . . . . ? C3 C2 N1 C1 0(2) . . . . ? C6 C7 N2 C1 179.0(16) . . . . ? C6 C7 N2 C3 1(3) . . . . ? N1 C1 N2 C7 -178.6(15) . . . . ? Ir1 C1 N2 C7 8(3) . . . . ? N1 C1 N2 C3 -0.5(16) . . . . ? Ir1 C1 N2 C3 -173.6(13) . . . . ? C2 C3 N2 C7 178.8(16) . . . . ? C4 C3 N2 C7 0(2) . . . . ? C2 C3 N2 C1 1(2) . . . . ? C4 C3 N2 C1 -177.9(15) . . . . ? C16 C15 N3 C14 0(2) . . . . ? C16 C15 N3 C21 174.1(18) . . . . ? N4 C14 N3 C15 -1.8(19) . . . . ? Ir1 C14 N3 C15 178.1(13) . . . . ? N4 C14 N3 C21 -177.2(13) . . . . ? Ir1 C14 N3 C21 2.7(19) . . . . ? C22 C21 N3 C15 179.8(18) . . . . ? C26 C21 N3 C15 6(3) . . . . ? C22 C21 N3 C14 -6(2) . . . . ? C26 C21 N3 C14 -179.8(17) . . . . ? C19 C20 N4 C14 -177.2(16) . . . . ? C19 C20 N4 C16 0(2) . . . . ? N3 C14 N4 C20 -179.6(14) . . . . ? Ir1 C14 N4 C20 1(3) . . . . ? N3 C14 N4 C16 3.2(19) . . . . ? Ir1 C14 N4 C16 -176.7(18) . . . . ? C15 C16 N4 C20 179.2(16) . . . . ? C17 C16 N4 C20 3(3) . . . . ? C15 C16 N4 C14 -3(2) . . . . ? C17 C16 N4 C14 -179.6(19) . . . . ? C35 C36 C37 C38 -2(5) . . . . ? C28 C29 N6 C27 -6(3) . . . . ? C30 C29 N6 C27 -178(3) . . . . ? C28 C29 N6 C33 -179(3) . . . . ? C30 C29 N6 C33 8(4) . . . . ? C33 N6 C27 N5 178(3) . . . . ? C29 N6 C27 N5 5(2) . . . . ? C33 N6 C27 Ir1 -1(4) . . . . ? C29 N6 C27 Ir1 -175(2) . . . . ? C28 N5 C27 N6 -3(3) . . . . ? C34 N5 C27 N6 -178.9(17) . . . . ? C28 N5 C27 Ir1 176(2) . . . . ? C34 N5 C27 Ir1 1(3) . . . . ? C40 Ir1 C27 N6 -173(3) . . . . ? C14 Ir1 C27 N6 -77(2) . . . . ? C1 Ir1 C27 N6 96(2) . . . . ? C9 Ir1 C27 N6 168.7(16) . . . . ? C22 Ir1 C27 N6 3(2) . . . . ? C35 Ir1 C27 N6 -177(2) . . . . ? C49 Ir1 C27 N6 -1.1(17) . . . . ? C40 Ir1 C27 N5 8.1(18) . . . . ? C14 Ir1 C27 N5 104(2) . . . . ? C1 Ir1 C27 N5 -84(2) . . . . ? C9 Ir1 C27 N5 -11(4) . . . . ? C22 Ir1 C27 N5 -176.7(19) . . . . ? C35 Ir1 C27 N5 3(2) . . . . ? C49 Ir1 C27 N5 180(3) . . . . ? C37 C36 C35 C34 -1(4) . . . . ? C37 C36 C35 Ir1 177(2) . . . . ? C40 Ir1 C35 C36 167(4) . . . . ? C27 Ir1 C35 C36 175(3) . . . . ? C14 Ir1 C35 C36 81(2) . . . . ? C1 Ir1 C35 C36 -88(2) . . . . ? C9 Ir1 C35 C36 -10(2) . . . . ? C22 Ir1 C35 C36 -5(8) . . . . ? C49 Ir1 C35 C36 173(2) . . . . ? C40 Ir1 C35 C34 -14.2(19) . . . . ? C27 Ir1 C35 C34 -6.5(15) . . . . ? C14 Ir1 C35 C34 -100.2(15) . . . . ? C1 Ir1 C35 C34 90.3(15) . . . . ? C9 Ir1 C35 C34 168.4(15) . . . . ? C22 Ir1 C35 C34 174(5) . . . . ? C49 Ir1 C35 C34 -8.3(16) . . . . ? C38 C39 C34 C35 -5(5) . . . . ? C38 C39 C34 N5 172(2) . . . . ? C36 C35 C34 C39 6(4) . . . . ? Ir1 C35 C34 C39 -173(3) . . . . ? C36 C35 C34 N5 -172(2) . . . . ? Ir1 C35 C34 N5 9(2) . . . . ? C28 N5 C34 C39 0(4) . . . . ? C27 N5 C34 C39 175(2) . . . . ? C28 N5 C34 C35 178(3) . . . . ? C27 N5 C34 C35 -7(3) . . . . ? C36 C37 C38 C39 2(5) . . . . ? C34 C39 C38 C37 1(4) . . . . ? C27 N5 C28 C29 0(4) . . . . ? C34 N5 C28 C29 174(3) . . . . ? C30 C29 C28 N5 172(5) . . . . ? N6 C29 C28 N5 3(4) . . . . ? C27 N6 C33 C32 178(3) . . . . ? C29 N6 C33 C32 -9(5) . . . . ? N6 C33 C32 C31 5(5) . . . . ? C28 C29 C30 C31 -172(4) . . . . ? N6 C29 C30 C31 -4(6) . . . . ? C29 C30 C31 C32 0(6) . . . . ? C33 C32 C31 C30 0(5) . . . . ? N8 C47 C46 C45 4(6) . . . . ? C49 C50 C51 C52 -5(6) . . . . ? C46 C47 N8 C40 177(3) . . . . ? C46 C47 N8 C42 -5(4) . . . . ? C43 C42 N8 C40 -175(4) . . . . ? C41 C42 N8 C40 -3(3) . . . . ? C43 C42 N8 C47 7(5) . . . . ? C41 C42 N8 C47 179(2) . . . . ? C51 C50 C49 C48 1(4) . . . . ? C51 C50 C49 Ir1 -178(2) . . . . ? C40 Ir1 C49 C48 0.6(17) . . . . ? C27 Ir1 C49 C48 -5.8(18) . . . . ? C14 Ir1 C49 C48 99.3(18) . . . . ? C1 Ir1 C49 C48 -92.8(17) . . . . ? C9 Ir1 C49 C48 -158(4) . . . . ? C22 Ir1 C49 C48 177.6(18) . . . . ? C35 Ir1 C49 C48 -2.2(18) . . . . ? C40 Ir1 C49 C50 180(3) . . . . ? C27 Ir1 C49 C50 173(4) . . . . ? C14 Ir1 C49 C50 -82(3) . . . . ? C1 Ir1 C49 C50 86(3) . . . . ? C9 Ir1 C49 C50 21(7) . . . . ? C22 Ir1 C49 C50 -4(3) . . . . ? C35 Ir1 C49 C50 177(3) . . . . ? C41 N7 C40 N8 -3(3) . . . . ? C48 N7 C40 N8 -179.9(19) . . . . ? C41 N7 C40 Ir1 -173(2) . . . . ? C48 N7 C40 Ir1 10(3) . . . . ? C47 N8 C40 N7 -179(2) . . . . ? C42 N8 C40 N7 4(3) . . . . ? C47 N8 C40 Ir1 -11(4) . . . . ? C42 N8 C40 Ir1 172(2) . . . . ? C27 Ir1 C40 N7 -2(2) . . . . ? C14 Ir1 C40 N7 -93(2) . . . . ? C1 Ir1 C40 N7 92(2) . . . . ? C9 Ir1 C40 N7 171(2) . . . . ? C22 Ir1 C40 N7 -14(4) . . . . ? C35 Ir1 C40 N7 168(4) . . . . ? C49 Ir1 C40 N7 -6(2) . . . . ? C27 Ir1 C40 N8 -167(3) . . . . ? C14 Ir1 C40 N8 102(3) . . . . ? C1 Ir1 C40 N8 -73(3) . . . . ? C9 Ir1 C40 N8 6(3) . . . . ? C22 Ir1 C40 N8 -179.3(17) . . . . ? C35 Ir1 C40 N8 3.1(19) . . . . ? C49 Ir1 C40 N8 -171(3) . . . . ? C50 C51 C52 C53 6(6) . . . . ? C48 C53 C52 C51 -2(5) . . . . ? C40 N7 C41 C42 2(4) . . . . ? C48 N7 C41 C42 178(2) . . . . ? C43 C42 C41 N7 172(5) . . . . ? N8 C42 C41 N7 1(3) . . . . ? C52 C53 C48 C49 -2(5) . . . . ? C52 C53 C48 N7 176(3) . . . . ? C50 C49 C48 C53 2(4) . . . . ? Ir1 C49 C48 C53 -179(2) . . . . ? C50 C49 C48 N7 -176(2) . . . . ? Ir1 C49 C48 N7 3(2) . . . . ? C40 N7 C48 C53 174(3) . . . . ? C41 N7 C48 C53 -3(4) . . . . ? C40 N7 C48 C49 -8(3) . . . . ? C41 N7 C48 C49 175(2) . . . . ? N8 C42 C43 C45 -7(6) . . . . ? C41 C42 C43 C45 -175(4) . . . . ? C42 C43 C45 C46 4(6) . . . . ? C47 C46 C45 C43 -3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.151 _refine_diff_density_min -2.679 _refine_diff_density_rms 0.190 # end of file