# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JM566b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C153 H154 Cl14 Ir4 N8 O12' _chemical_formula_weight 3561.94 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 24.9384(19) _cell_length_b 12.5149(9) _cell_length_c 26.260(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.146(2) _cell_angle_gamma 90.00 _cell_volume 7643.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7644 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.47 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3540 _exptl_absorpt_coefficient_mu 3.775 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38674 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13225 _reflns_number_gt 8362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0891P)^2^+70.6726P] 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 13225 _refine_ls_number_parameters 832 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.005 _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 C2 C 0.6908(8) 0.7216(13) 0.0964(6) 0.058(4) Uani 1 1 d . . . C3 C 0.6260(6) 0.7365(11) 0.0748(6) 0.045(3) Uani 1 1 d . . . H3 H 0.6128 0.7698 0.1020 0.054 Uiso 1 1 calc R . . C4 C 0.6229(6) 0.6119(12) 0.0765(6) 0.050(4) Uani 1 1 d . . . H4 H 0.6161 0.5815 0.0403 0.060 Uiso 1 1 calc R . . C5 C 0.7269(6) 0.5331(11) 0.1271(6) 0.041(3) Uani 1 1 d . . . C6 C 0.7130(6) 0.4383(13) 0.0968(7) 0.056(4) Uani 1 1 d . . . H6 H 0.6781 0.4329 0.0678 0.068 Uiso 1 1 calc R . . C7 C 0.7498(6) 0.3544(12) 0.1090(6) 0.054(4) Uani 1 1 d . . . H7 H 0.7397 0.2919 0.0886 0.065 Uiso 1 1 calc R . . C8 C 0.8035(6) 0.3610(11) 0.1526(7) 0.053(4) Uani 1 1 d . . . H8 H 0.8279 0.3022 0.1627 0.064 Uiso 1 1 calc R . . C9 C 0.8191(5) 0.4586(10) 0.1804(6) 0.044(4) Uani 1 1 d . . . C10 C 0.8715(6) 0.6854(13) 0.2920(6) 0.056(4) Uani 1 1 d . . . H10 H 0.9095 0.6784 0.3155 0.067 Uiso 1 1 calc R . . C11 C 0.8403(7) 0.7642(14) 0.3004(7) 0.066(5) Uani 1 1 d . . . H11 H 0.8558 0.8108 0.3296 0.079 Uiso 1 1 calc R . . C12 C 0.7833(7) 0.7763(13) 0.2643(7) 0.061(4) Uani 1 1 d . . . H12 H 0.7604 0.8312 0.2692 0.073 Uiso 1 1 calc R . . C13 C 0.7618(6) 0.7062(12) 0.2217(6) 0.052(4) Uani 1 1 d . . . H13 H 0.7241 0.7137 0.1976 0.062 Uiso 1 1 calc R . . C14 C 0.7958(6) 0.6236(11) 0.2141(5) 0.041(3) Uani 1 1 d . . . C15 C 0.7773(6) 0.5403(11) 0.1724(6) 0.043(3) Uani 1 1 d . . . C16 C 0.9590(6) 0.3722(13) 0.2293(9) 0.069(5) Uani 1 1 d . . . C17 C 0.9892(7) 0.4271(14) 0.2809(8) 0.064(5) Uani 1 1 d . . . C18 C 0.9892(6) 0.5373(13) 0.2709(7) 0.057(4) Uani 1 1 d . . . C19 C 0.9604(6) 0.5569(12) 0.2144(7) 0.052(4) Uani 1 1 d . . . C20 C 0.9439(6) 0.4564(14) 0.1879(7) 0.058(4) Uani 1 1 d . . . C21 C 0.9535(8) 0.2538(13) 0.2253(12) 0.132(11) Uani 1 1 d . . . H21A H 0.9895 0.2230 0.2275 0.197 Uiso 1 1 calc R . . H21B H 0.9244 0.2347 0.1910 0.197 Uiso 1 1 calc R . . H21C H 0.9430 0.2272 0.2547 0.197 Uiso 1 1 calc R . . C22 C 1.0162(9) 0.369(2) 0.3359(9) 0.115(9) Uani 1 1 d . . . H22A H 1.0514 0.3358 0.3376 0.173 Uiso 1 1 calc R . . H22B H 0.9900 0.3162 0.3393 0.173 Uiso 1 1 calc R . . H22C H 1.0240 0.4202 0.3651 0.173 Uiso 1 1 calc R . . C23 C 1.0220(8) 0.6215(17) 0.3116(8) 0.089(6) Uani 1 1 d . . . H23A H 1.0247 0.6006 0.3476 0.133 Uiso 1 1 calc R . . H23B H 1.0023 0.6887 0.3024 0.133 Uiso 1 1 calc R . . H23C H 1.0600 0.6287 0.3106 0.133 Uiso 1 1 calc R . . C24 C 0.9532(9) 0.6594(15) 0.1842(9) 0.100(7) Uani 1 1 d . . . H24A H 0.9897 0.6826 0.1839 0.150 Uiso 1 1 calc R . . H24B H 0.9381 0.7123 0.2018 0.150 Uiso 1 1 calc R . . H24C H 0.9270 0.6494 0.1474 0.150 Uiso 1 1 calc R . . C25 C 0.9210(9) 0.4356(19) 0.1276(7) 0.096(7) Uani 1 1 d . . . H25A H 0.8847 0.4709 0.1111 0.144 Uiso 1 1 calc R . . H25B H 0.9161 0.3601 0.1212 0.144 Uiso 1 1 calc R . . H25C H 0.9477 0.4624 0.1120 0.144 Uiso 1 1 calc R . . C26 C 0.5462(7) 0.8120(14) 0.0042(7) 0.061(4) Uani 1 1 d . . . C27 C 0.5285(9) 0.8833(14) -0.0388(7) 0.072(5) Uani 1 1 d . . . H27 H 0.5558 0.9116 -0.0515 0.086 Uiso 1 1 calc R . . C28 C 0.4720(11) 0.9141(17) -0.0637(9) 0.100(7) Uani 1 1 d . . . H28 H 0.4610 0.9624 -0.0925 0.120 Uiso 1 1 calc R . . C29 C 0.4312(10) 0.869(2) -0.0434(10) 0.103(7) Uani 1 1 d . . . H29 H 0.3924 0.8864 -0.0590 0.124 Uiso 1 1 calc R . . C30 C 0.4502(9) 0.802(2) -0.0018(10) 0.101(7) Uani 1 1 d . . . H30 H 0.4231 0.7731 0.0111 0.121 Uiso 1 1 calc R . . C31 C 0.5072(9) 0.7711(16) 0.0244(9) 0.087(6) Uani 1 1 d . . . H31 H 0.5182 0.7249 0.0541 0.104 Uiso 1 1 calc R . . C32 C 0.5888(6) 0.5533(11) 0.1042(6) 0.046(3) Uani 1 1 d . . . C33 C 0.5538(7) 0.4678(12) 0.0778(7) 0.058(4) Uani 1 1 d . . . H33 H 0.5515 0.4470 0.0430 0.069 Uiso 1 1 calc R . . C34 C 0.5219(7) 0.4133(13) 0.1047(7) 0.067(5) Uani 1 1 d . . . H34 H 0.5002 0.3539 0.0881 0.080 Uiso 1 1 calc R . . C35 C 0.5223(6) 0.4447(12) 0.1526(8) 0.056(4) Uani 1 1 d . . . C36 C 0.5574(8) 0.5291(14) 0.1802(7) 0.065(5) Uani 1 1 d . . . H36 H 0.5589 0.5486 0.2149 0.078 Uiso 1 1 calc R . . C37 C 0.5899(7) 0.5837(13) 0.1555(7) 0.058(4) Uani 1 1 d . . . H37 H 0.6126 0.6410 0.1734 0.070 Uiso 1 1 calc R . . C38 C 0.4820(10) 0.4235(19) 0.2224(9) 0.109(8) Uani 1 1 d . . . H38A H 0.5197 0.4369 0.2488 0.164 Uiso 1 1 calc R . . H38B H 0.4635 0.3692 0.2360 0.164 Uiso 1 1 calc R . . H38C H 0.4597 0.4880 0.2161 0.164 Uiso 1 1 calc R . . C39 C 0.4046(6) 0.3213(13) 0.3194(6) 0.047(4) Uani 1 1 d . . . C40 C 0.4191(6) 0.3110(13) 0.3805(6) 0.058(4) Uani 1 1 d . . . H40 H 0.3886 0.2744 0.3890 0.069 Uiso 1 1 calc R . . C41 C 0.4132(7) 0.4337(13) 0.3819(7) 0.061(4) Uani 1 1 d . . . H41 H 0.4511 0.4678 0.3950 0.073 Uiso 1 1 calc R . . C42 C 0.3751(6) 0.5104(11) 0.2817(6) 0.044(3) Uani 1 1 d . . . C43 C 0.4064(6) 0.6069(12) 0.2981(6) 0.052(4) Uani 1 1 d . . . H43 H 0.4329 0.6150 0.3335 0.062 Uiso 1 1 calc R . . C44 C 0.3970(7) 0.6871(12) 0.2613(7) 0.058(4) Uani 1 1 d . . . H44 H 0.4154 0.7525 0.2720 0.069 Uiso 1 1 calc R . . C45 C 0.3596(6) 0.6725(11) 0.2067(6) 0.047(3) Uani 1 1 d . . . H45 H 0.3536 0.7281 0.1818 0.056 Uiso 1 1 calc R . . C46 C 0.3314(6) 0.5744(11) 0.1899(5) 0.043(3) Uani 1 1 d . . . C47 C 0.2177(7) 0.3513(14) 0.1337(6) 0.064(5) Uani 1 1 d . . . H47 H 0.1952 0.3587 0.0969 0.077 Uiso 1 1 calc R . . C48 C 0.2050(7) 0.2704(13) 0.1613(6) 0.059(4) Uani 1 1 d . . . H48 H 0.1760 0.2224 0.1430 0.071 Uiso 1 1 calc R . . C49 C 0.2347(6) 0.2587(12) 0.2163(7) 0.054(4) Uani 1 1 d . . . H49 H 0.2264 0.2046 0.2366 0.065 Uiso 1 1 calc R . . C50 C 0.2779(6) 0.3330(11) 0.2396(6) 0.045(3) Uani 1 1 d . . . H50 H 0.2981 0.3308 0.2771 0.054 Uiso 1 1 calc R . . C51 C 0.2923(6) 0.4117(10) 0.2085(6) 0.040(3) Uani 1 1 d . . . C52 C 0.3347(5) 0.4976(10) 0.2286(6) 0.039(3) Uani 1 1 d . . . C53 C 0.2899(7) 0.6565(10) 0.0548(6) 0.053(4) Uani 1 1 d . . . C54 C 0.3354(7) 0.5761(12) 0.0720(7) 0.057(4) Uani 1 1 d . . . C55 C 0.3067(7) 0.4733(13) 0.0550(6) 0.055(4) Uani 1 1 d . . . C56 C 0.2461(8) 0.4930(14) 0.0249(6) 0.061(5) Uani 1 1 d . . . C57 C 0.2372(7) 0.6045(12) 0.0257(6) 0.052(4) Uani 1 1 d . . . C58 C 0.3004(9) 0.7739(15) 0.0591(8) 0.090(6) Uani 1 1 d . . . H58A H 0.3091 0.7980 0.0283 0.134 Uiso 1 1 calc R . . H58B H 0.3321 0.7895 0.0921 0.134 Uiso 1 1 calc R . . H58C H 0.2666 0.8099 0.0596 0.134 Uiso 1 1 calc R . . C59 C 0.3978(7) 0.5940(16) 0.0982(8) 0.079(6) Uani 1 1 d . . . H59A H 0.4150 0.5342 0.1212 0.119 Uiso 1 1 calc R . . H59B H 0.4045 0.6579 0.1199 0.119 Uiso 1 1 calc R . . H59C H 0.4144 0.6016 0.0707 0.119 Uiso 1 1 calc R . . C60 C 0.3374(8) 0.3660(13) 0.0646(8) 0.079(6) Uani 1 1 d . . . H60A H 0.3360 0.3370 0.0303 0.118 Uiso 1 1 calc R . . H60B H 0.3188 0.3178 0.0814 0.118 Uiso 1 1 calc R . . H60C H 0.3767 0.3756 0.0881 0.118 Uiso 1 1 calc R . . C61 C 0.2045(9) 0.4117(16) -0.0057(7) 0.085(6) Uani 1 1 d . . . H61A H 0.1674 0.4279 -0.0044 0.127 Uiso 1 1 calc R . . H61B H 0.2167 0.3427 0.0103 0.127 Uiso 1 1 calc R . . H61C H 0.2021 0.4112 -0.0430 0.127 Uiso 1 1 calc R . . C62 C 0.1817(7) 0.6629(17) 0.0004(7) 0.085(6) Uani 1 1 d . . . H62A H 0.1849 0.7326 0.0165 0.128 Uiso 1 1 calc R . . H62B H 0.1515 0.6238 0.0065 0.128 Uiso 1 1 calc R . . H62C H 0.1731 0.6700 -0.0382 0.128 Uiso 1 1 calc R . . C63 C 0.4879(8) 0.2347(16) 0.4601(9) 0.080(6) Uani 1 1 d . . . C64 C 0.5350(8) 0.158(2) 0.4791(9) 0.112(9) Uani 1 1 d . . . H64 H 0.5522 0.1292 0.4562 0.134 Uiso 1 1 calc R . . C65 C 0.5529(11) 0.130(2) 0.5363(12) 0.126(10) Uani 1 1 d . . . H65 H 0.5825 0.0811 0.5509 0.152 Uiso 1 1 calc R . . C66 C 0.5272(12) 0.175(3) 0.5695(11) 0.130(11) Uani 1 1 d . . . H66 H 0.5395 0.1573 0.6063 0.156 Uiso 1 1 calc R . . C67 C 0.4828(11) 0.248(2) 0.5475(10) 0.121(9) Uani 1 1 d . . . H67 H 0.4658 0.2775 0.5704 0.145 Uiso 1 1 calc R . . C68 C 0.4629(9) 0.278(2) 0.4943(9) 0.095(7) Uani 1 1 d . . . H68 H 0.4329 0.3267 0.4813 0.114 Uiso 1 1 calc R . . C69 C 0.3746(7) 0.4847(12) 0.4071(6) 0.052(4) Uani 1 1 d . . . C70 C 0.3185(8) 0.4568(13) 0.3945(7) 0.070(5) Uani 1 1 d . . . H70 H 0.3044 0.4061 0.3670 0.085 Uiso 1 1 calc R . . C71 C 0.2783(7) 0.4951(14) 0.4179(6) 0.063(5) Uani 1 1 d . . . H71 H 0.2412 0.4689 0.4095 0.075 Uiso 1 1 calc R . . C72 C 0.3033(13) 0.5797(15) 0.4563(10) 0.110(9) Uani 1 1 d . . . C73 C 0.3610(12) 0.6118(15) 0.4697(8) 0.099(8) Uani 1 1 d . . . H73 H 0.3752 0.6675 0.4944 0.119 Uiso 1 1 calc R . . C74 C 0.3972(9) 0.5636(14) 0.4474(8) 0.080(6) Uani 1 1 d . . . H74 H 0.4358 0.5828 0.4588 0.097 Uiso 1 1 calc R . . C75 C 0.2157(12) 0.5929(18) 0.4724(11) 0.129(10) Uani 1 1 d . . . H75A H 0.1919 0.6083 0.4353 0.194 Uiso 1 1 calc R . . H75B H 0.1999 0.6271 0.4967 0.194 Uiso 1 1 calc R . . H75C H 0.2168 0.5170 0.4782 0.194 Uiso 1 1 calc R . . C76 C 0.3483(6) 1.0334(17) 0.2660(4) 0.111(8) Uani 1 1 d D . . H76A H 0.3476 1.1106 0.2625 0.133 Uiso 1 1 calc R . . H76B H 0.3169 1.0115 0.2772 0.133 Uiso 1 1 calc R . . C77 C 0.7433(8) 0.004(3) 0.1653(6) 0.201 Uani 1 1 d D . . H77A H 0.7152 0.0295 0.1800 0.241 Uiso 1 1 calc R . . H77B H 0.7409 -0.0733 0.1627 0.241 Uiso 1 1 calc R . . C78 C 0.8667(8) -0.024(2) 0.1080(17) 0.100(14) Uani 0.50 1 d PD . . H78A H 0.8591 -0.0135 0.1414 0.120 Uiso 0.50 1 calc PR . . H78B H 0.8392 -0.0754 0.0854 0.120 Uiso 0.50 1 calc PR . . Cl1 Cl 0.86666(18) 0.3927(4) 0.30703(18) 0.0695(12) Uani 1 1 d . . . Cl2 Cl 0.20408(18) 0.6410(4) 0.13832(18) 0.0688(12) Uani 1 1 d . . . Cl3 Cl 0.4144(3) 0.9909(6) 0.3138(4) 0.159 Uani 1 1 d D . . Cl4 Cl 0.3421(6) 0.9728(9) 0.2038(4) 0.200 Uani 1 1 d D . . Cl5 Cl 0.8128(4) 0.0440(9) 0.2071(5) 0.193 Uani 1 1 d D . . Cl6 Cl 0.7309(5) 0.0606(8) 0.1008(5) 0.206 Uani 1 1 d D . . Cl7 Cl 0.8611(7) 0.0976(10) 0.0731(6) 0.131 Uani 0.50 1 d PD . . Cl8 Cl 0.9372(6) -0.0711(18) 0.1232(7) 0.181 Uani 0.50 1 d PD . . Ir1 Ir 0.89727(2) 0.48163(4) 0.24107(2) 0.04133(18) Uani 1 1 d . . . Ir2 Ir 0.27497(2) 0.54955(4) 0.11274(2) 0.03954(17) Uani 1 1 d . . . N1 N 0.6862(5) 0.6176(9) 0.1092(5) 0.045(3) Uani 1 1 d . . . N2 N 0.8500(4) 0.6135(8) 0.2499(4) 0.039(3) Uani 1 1 d . . . N3 N 0.3900(5) 0.4283(10) 0.3217(5) 0.048(3) Uani 1 1 d . . . N4 N 0.2593(4) 0.4204(8) 0.1546(4) 0.039(3) Uani 1 1 d . . . O1 O 0.6032(5) 0.7881(9) 0.0239(4) 0.066(3) Uani 1 1 d . . . O2 O 0.7323(5) 0.7795(9) 0.1015(5) 0.069(3) Uani 1 1 d . . . O3 O 0.4867(5) 0.3889(10) 0.1730(6) 0.089(4) Uani 1 1 d . . . O4 O 0.4049(4) 0.2672(9) 0.2824(5) 0.060(3) Uani 1 1 d . . . O5 O 0.4728(4) 0.2596(10) 0.4049(5) 0.066(3) Uani 1 1 d . . . O6 O 0.2734(8) 0.6323(10) 0.4832(7) 0.118(6) Uani 1 1 d . . . 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 C2 0.081(12) 0.051(10) 0.054(10) -0.005(8) 0.039(9) 0.002(9) C3 0.049(9) 0.045(8) 0.036(8) 0.004(6) 0.009(7) 0.005(6) C4 0.045(8) 0.053(9) 0.046(9) -0.009(7) 0.009(7) 0.005(7) C5 0.036(7) 0.048(8) 0.043(8) 0.008(7) 0.019(7) 0.001(6) C6 0.041(8) 0.064(10) 0.072(11) -0.007(9) 0.030(8) -0.001(7) C7 0.053(9) 0.051(9) 0.061(10) -0.011(8) 0.021(8) -0.010(7) C8 0.049(9) 0.040(8) 0.084(12) -0.001(8) 0.040(9) -0.003(7) C9 0.010(5) 0.033(7) 0.082(11) -0.030(7) 0.008(6) -0.007(5) C10 0.041(8) 0.069(10) 0.056(10) -0.024(8) 0.016(8) -0.001(7) C11 0.060(11) 0.076(12) 0.055(11) -0.032(9) 0.016(9) -0.003(9) C12 0.063(11) 0.053(10) 0.072(12) -0.011(9) 0.030(9) 0.020(8) C13 0.050(9) 0.062(10) 0.040(9) 0.000(8) 0.013(7) 0.013(7) C14 0.042(8) 0.049(8) 0.039(8) -0.006(6) 0.023(7) -0.001(6) C15 0.046(8) 0.050(8) 0.043(9) -0.009(7) 0.027(7) -0.012(6) C16 0.025(8) 0.054(10) 0.136(17) -0.021(11) 0.038(10) -0.001(7) C17 0.046(9) 0.071(12) 0.076(12) 0.016(10) 0.021(9) 0.016(8) C18 0.039(8) 0.057(10) 0.064(11) -0.003(8) 0.007(8) -0.004(7) C19 0.025(7) 0.056(9) 0.067(11) -0.003(8) 0.006(7) 0.004(6) C20 0.042(9) 0.075(12) 0.069(11) -0.002(9) 0.035(8) 0.007(8) C21 0.076(14) 0.036(10) 0.31(4) -0.001(15) 0.097(19) 0.010(9) C22 0.086(15) 0.14(2) 0.125(19) 0.063(17) 0.042(14) 0.051(15) C23 0.084(14) 0.099(16) 0.085(14) -0.020(12) 0.033(12) -0.008(12) C24 0.114(17) 0.067(13) 0.131(19) 0.040(13) 0.060(15) -0.018(12) C25 0.098(16) 0.14(2) 0.057(12) -0.012(12) 0.031(12) -0.008(14) C26 0.059(11) 0.063(11) 0.051(10) -0.001(8) 0.010(9) 0.017(8) C27 0.096(14) 0.059(11) 0.052(11) 0.015(9) 0.017(10) 0.003(10) C28 0.108(18) 0.073(14) 0.102(18) 0.024(13) 0.017(15) 0.047(13) C29 0.087(17) 0.100(18) 0.102(19) 0.006(15) 0.008(15) 0.026(14) C30 0.069(14) 0.12(2) 0.113(19) 0.011(16) 0.033(13) 0.024(13) C31 0.092(15) 0.079(14) 0.098(16) 0.004(12) 0.044(13) 0.005(12) C32 0.043(8) 0.039(8) 0.057(10) -0.004(7) 0.020(7) 0.008(6) C33 0.072(11) 0.057(10) 0.055(10) -0.009(8) 0.036(9) 0.001(8) C34 0.065(11) 0.055(10) 0.077(13) -0.015(9) 0.022(10) -0.019(8) C35 0.041(8) 0.051(9) 0.085(13) 0.008(9) 0.032(9) 0.002(7) C36 0.078(12) 0.080(12) 0.049(10) 0.007(9) 0.037(9) -0.006(10) C37 0.063(10) 0.050(9) 0.059(11) 0.000(8) 0.020(9) -0.001(8) C38 0.14(2) 0.114(18) 0.119(19) 0.026(15) 0.099(17) 0.005(16) C39 0.032(8) 0.069(10) 0.037(9) 0.007(8) 0.010(7) -0.004(7) C40 0.043(9) 0.068(11) 0.054(10) 0.021(8) 0.007(8) -0.004(8) C41 0.056(10) 0.064(10) 0.055(11) 0.006(8) 0.011(8) -0.018(8) C42 0.047(8) 0.047(8) 0.044(9) -0.001(7) 0.023(7) -0.004(7) C43 0.040(8) 0.059(10) 0.050(10) -0.011(8) 0.008(7) -0.013(7) C44 0.058(10) 0.045(9) 0.076(12) 0.000(8) 0.032(9) -0.013(7) C45 0.053(9) 0.039(8) 0.049(9) -0.004(7) 0.019(8) -0.009(7) C46 0.053(8) 0.055(9) 0.034(8) -0.006(6) 0.032(7) -0.022(7) C47 0.069(11) 0.075(12) 0.041(10) -0.010(8) 0.010(9) -0.018(9) C48 0.066(10) 0.065(10) 0.044(10) -0.005(8) 0.016(8) -0.033(8) C49 0.059(10) 0.051(9) 0.060(11) 0.003(8) 0.030(9) -0.012(8) C50 0.049(8) 0.046(8) 0.048(9) 0.011(7) 0.026(7) 0.002(7) C51 0.041(8) 0.038(7) 0.044(9) -0.006(6) 0.020(7) -0.001(6) C52 0.020(6) 0.038(7) 0.058(10) -0.003(7) 0.012(7) 0.000(5) C53 0.086(11) 0.026(7) 0.062(10) 0.020(7) 0.045(9) 0.004(7) C54 0.081(11) 0.043(9) 0.072(11) 0.015(8) 0.057(10) 0.007(8) C55 0.071(11) 0.064(10) 0.049(10) -0.006(8) 0.044(9) 0.002(8) C56 0.083(12) 0.072(11) 0.024(8) -0.024(8) 0.015(8) -0.024(9) C57 0.062(10) 0.049(9) 0.044(9) 0.018(7) 0.018(8) 0.010(8) C58 0.127(18) 0.059(12) 0.091(15) 0.007(11) 0.050(14) -0.005(11) C59 0.068(12) 0.089(13) 0.109(15) 0.009(12) 0.065(12) -0.004(10) C60 0.104(15) 0.047(10) 0.103(15) -0.008(10) 0.059(13) 0.014(10) C61 0.111(16) 0.085(14) 0.070(13) -0.012(11) 0.045(12) -0.006(12) C62 0.068(12) 0.103(15) 0.073(13) 0.026(11) 0.013(10) 0.044(11) C63 0.053(11) 0.083(13) 0.086(15) 0.037(12) 0.003(11) -0.022(9) C64 0.057(12) 0.17(2) 0.096(17) 0.072(17) 0.008(12) 0.003(14) C65 0.074(16) 0.13(2) 0.14(3) 0.06(2) -0.004(17) 0.008(15) C66 0.088(19) 0.19(3) 0.081(19) 0.06(2) -0.003(16) -0.02(2) C67 0.12(2) 0.16(3) 0.079(17) 0.036(17) 0.023(16) -0.030(18) C68 0.076(14) 0.13(2) 0.072(14) 0.029(14) 0.024(12) -0.020(13) C69 0.060(10) 0.058(9) 0.036(8) 0.014(7) 0.016(8) -0.012(8) C70 0.089(13) 0.059(11) 0.075(12) -0.019(9) 0.043(11) -0.028(9) C71 0.053(9) 0.093(13) 0.040(9) -0.025(9) 0.013(8) 0.013(9) C72 0.21(3) 0.043(11) 0.13(2) -0.004(12) 0.13(2) -0.012(14) C73 0.17(2) 0.055(12) 0.070(14) -0.034(10) 0.036(15) -0.042(14) C74 0.104(15) 0.055(11) 0.090(14) -0.033(10) 0.044(13) -0.046(10) C75 0.20(3) 0.072(14) 0.19(3) -0.010(16) 0.15(2) 0.010(17) C76 0.082(15) 0.110(18) 0.14(2) -0.023(16) 0.044(16) -0.002(13) C77 0.178 0.304 0.070 0.021 -0.019 -0.044 C78 0.09(3) 0.13(4) 0.08(3) 0.01(3) 0.03(3) 0.02(3) Cl1 0.064(3) 0.080(3) 0.078(3) 0.027(2) 0.042(2) 0.009(2) Cl2 0.062(3) 0.084(3) 0.068(3) 0.010(2) 0.034(2) 0.033(2) Cl3 0.094 0.138 0.209 0.072 0.011 0.011 Cl4 0.263 0.176 0.135 -0.024 0.039 -0.024 Cl5 0.151 0.227 0.194 -0.049 0.052 -0.027 Cl6 0.221 0.144 0.230 0.023 0.054 0.056 Cl7 0.183 0.070 0.139 0.003 0.055 0.014 Cl8 0.096 0.313 0.163 0.126 0.081 0.106 Ir1 0.0363(3) 0.0390(3) 0.0525(4) 0.0024(3) 0.0207(3) 0.0033(2) Ir2 0.0434(3) 0.0377(3) 0.0415(3) 0.0039(2) 0.0201(3) 0.0048(2) N1 0.046(7) 0.042(7) 0.052(8) 0.000(6) 0.023(6) 0.000(5) N2 0.037(6) 0.040(6) 0.041(7) -0.007(5) 0.014(6) 0.000(5) N3 0.045(7) 0.053(8) 0.039(7) 0.005(6) 0.007(6) 0.000(6) N4 0.038(6) 0.037(6) 0.041(7) 0.009(5) 0.013(6) 0.000(5) O1 0.081(8) 0.076(8) 0.048(7) 0.025(6) 0.029(6) 0.017(6) O2 0.063(7) 0.072(8) 0.074(8) 0.012(6) 0.026(6) -0.016(6) O3 0.091(9) 0.071(8) 0.128(12) 0.011(8) 0.069(9) -0.006(7) O4 0.061(7) 0.059(7) 0.067(8) -0.004(6) 0.029(6) 0.001(5) O5 0.044(6) 0.085(8) 0.060(8) 0.015(6) 0.008(6) 0.005(6) O6 0.200(18) 0.055(8) 0.146(14) -0.034(9) 0.118(14) -0.020(10) _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 C2 O2 1.232(18) . ? C2 N1 1.359(19) . ? C2 C3 1.52(2) . ? C3 O1 1.405(16) . ? C3 C4 1.564(19) . ? C3 H3 0.9800 . ? C4 C32 1.50(2) . ? C4 N1 1.500(17) . ? C4 H4 0.9800 . ? C5 C15 1.39(2) . ? C5 C6 1.40(2) . ? C5 N1 1.423(17) . ? C6 C7 1.35(2) . ? C6 H6 0.9300 . ? C7 C8 1.42(2) . ? C7 H7 0.9300 . ? C8 C9 1.403(18) . ? C8 H8 0.9300 . ? C9 C15 1.421(18) . ? C9 Ir1 2.045(12) . ? C10 C11 1.32(2) . ? C10 N2 1.376(17) . ? C10 H10 0.9300 . ? C11 C12 1.40(2) . ? C11 H11 0.9300 . ? C12 C13 1.37(2) . ? C12 H12 0.9300 . ? C13 C14 1.397(19) . ? C13 H13 0.9300 . ? C14 N2 1.345(17) . ? C14 C15 1.460(18) . ? C16 C17 1.46(2) . ? C16 C20 1.46(2) . ? C16 C21 1.49(2) . ? C16 Ir1 2.165(14) . ? C17 C18 1.40(2) . ? C17 C22 1.54(2) . ? C17 Ir1 2.255(15) . ? C18 C19 1.42(2) . ? C18 C23 1.51(2) . ? C18 Ir1 2.248(15) . ? C19 C20 1.42(2) . ? C19 C24 1.48(2) . ? C19 Ir1 2.158(15) . ? C20 C25 1.50(2) . ? C20 Ir1 2.137(14) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O1 1.359(18) . ? C26 C27 1.38(2) . ? C26 C31 1.36(2) . ? C27 C28 1.38(3) . ? C27 H27 0.9300 . ? C28 C29 1.42(3) . ? C28 H28 0.9300 . ? C29 C30 1.32(3) . ? C29 H29 0.9300 . ? C30 C31 1.39(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.39(2) . ? C32 C33 1.40(2) . ? C33 C34 1.42(2) . ? C33 H33 0.9300 . ? C34 C35 1.31(2) . ? C34 H34 0.9300 . ? C35 O3 1.381(18) . ? C35 C36 1.40(2) . ? C36 C37 1.39(2) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O3 1.41(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O4 1.187(17) . ? C39 N3 1.395(19) . ? C39 C40 1.52(2) . ? C40 O5 1.414(17) . ? C40 C41 1.55(2) . ? C40 H40 0.9800 . ? C41 N3 1.474(19) . ? C41 C69 1.49(2) . ? C41 H41 0.9800 . ? C42 C52 1.40(2) . ? C42 C43 1.419(19) . ? C42 N3 1.420(18) . ? C43 C44 1.35(2) . ? C43 H43 0.9300 . ? C44 C45 1.41(2) . ? C44 H44 0.9300 . ? C45 C46 1.404(18) . ? C45 H45 0.9300 . ? C46 C52 1.380(19) . ? C46 Ir2 2.031(14) . ? C47 N4 1.310(18) . ? C47 C48 1.35(2) . ? C47 H47 0.9300 . ? C48 C49 1.37(2) . ? C48 H48 0.9300 . ? C49 C50 1.388(19) . ? C49 H49 0.9300 . ? C50 C51 1.407(18) . ? C50 H50 0.9300 . ? C51 N4 1.359(17) . ? C51 C52 1.466(18) . ? C53 C57 1.42(2) . ? C53 C54 1.46(2) . ? C53 C58 1.49(2) . ? C53 Ir2 2.157(12) . ? C54 C55 1.46(2) . ? C54 C59 1.47(2) . ? C54 Ir2 2.166(13) . ? C55 C56 1.45(2) . ? C55 C60 1.52(2) . ? C55 Ir2 2.168(13) . ? C56 C57 1.42(2) . ? C56 C61 1.47(2) . ? C56 Ir2 2.269(13) . ? C57 C62 1.49(2) . ? C57 Ir2 2.244(14) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C68 1.38(3) . ? C63 O5 1.40(2) . ? C63 C64 1.46(3) . ? C64 C65 1.45(3) . ? C64 H64 0.9300 . ? C65 C66 1.38(4) . ? C65 H65 0.9300 . ? C66 C67 1.39(4) . ? C66 H66 0.9300 . ? C67 C68 1.35(3) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.36(2) . ? C69 C74 1.41(2) . ? C70 C71 1.43(2) . ? C70 H70 0.9300 . ? C71 C72 1.44(3) . ? C71 H71 0.9300 . ? C72 C73 1.41(3) . ? C72 O6 1.36(2) . ? C73 C74 1.38(3) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 O6 1.45(3) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 Cl3 1.755(5) . ? C76 Cl4 1.757(5) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 Cl5 1.756(5) . ? C77 Cl6 1.757(5) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 Cl8 1.757(5) . ? C78 Cl7 1.759(5) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? Cl1 Ir1 2.403(4) . ? Cl2 Ir2 2.396(4) . ? Ir1 N2 2.090(10) . ? Ir2 N4 2.070(10) . ? 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 O2 C2 N1 132.8(16) . . ? O2 C2 C3 135.1(15) . . ? N1 C2 C3 92.1(12) . . ? O1 C3 C2 115.1(12) . . ? O1 C3 C4 118.6(12) . . ? C2 C3 C4 85.5(11) . . ? O1 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? C4 C3 H3 111.7 . . ? C32 C4 N1 114.3(12) . . ? C32 C4 C3 123.0(12) . . ? N1 C4 C3 85.3(10) . . ? C32 C4 H4 110.6 . . ? N1 C4 H4 110.6 . . ? C3 C4 H4 110.6 . . ? C15 C5 C6 120.3(13) . . ? C15 C5 N1 123.5(13) . . ? C6 C5 N1 116.2(13) . . ? C7 C6 C5 121.0(15) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.6(15) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 118.3(13) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C15 120.0(12) . . ? C8 C9 Ir1 122.3(10) . . ? C15 C9 Ir1 117.1(9) . . ? C11 C10 N2 122.6(14) . . ? C11 C10 H10 118.7 . . ? N2 C10 H10 118.7 . . ? C10 C11 C12 118.8(15) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 119.0(13) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 120.8(14) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N2 C14 C13 118.6(13) . . ? N2 C14 C15 115.0(12) . . ? C13 C14 C15 126.3(13) . . ? C5 C15 C9 117.9(12) . . ? C5 C15 C14 129.3(13) . . ? C9 C15 C14 112.8(12) . . ? C17 C16 C20 104.9(14) . . ? C17 C16 C21 123(2) . . ? C20 C16 C21 132(2) . . ? C17 C16 Ir1 74.0(9) . . ? C20 C16 Ir1 69.1(8) . . ? C21 C16 Ir1 126.0(11) . . ? C18 C17 C16 108.8(15) . . ? C18 C17 C22 127.5(19) . . ? C16 C17 C22 123.7(18) . . ? C18 C17 Ir1 71.6(9) . . ? C16 C17 Ir1 67.4(8) . . ? C22 C17 Ir1 127.2(12) . . ? C17 C18 C19 109.4(15) . . ? C17 C18 C23 126.0(16) . . ? C19 C18 C23 124.0(15) . . ? C17 C18 Ir1 72.1(9) . . ? C19 C18 Ir1 67.8(8) . . ? C23 C18 Ir1 133.3(12) . . ? C20 C19 C18 107.8(14) . . ? C20 C19 C24 123.0(16) . . ? C18 C19 C24 128.8(16) . . ? C20 C19 Ir1 69.9(8) . . ? C18 C19 Ir1 74.7(9) . . ? C24 C19 Ir1 126.0(11) . . ? C19 C20 C16 108.8(15) . . ? C19 C20 C25 127.0(17) . . ? C16 C20 C25 123.9(17) . . ? C19 C20 Ir1 71.4(8) . . ? C16 C20 Ir1 71.2(8) . . ? C25 C20 Ir1 128.8(12) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 C27 115.9(16) . . ? O1 C26 C31 124.3(16) . . ? C27 C26 C31 119.8(17) . . ? C26 C27 C28 123(2) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C29 117(2) . . ? C27 C28 H28 121.3 . . ? C29 C28 H28 121.3 . . ? C30 C29 C28 118(2) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C29 C30 C31 125(2) . . ? C29 C30 H30 117.3 . . ? C31 C30 H30 117.3 . . ? C26 C31 C30 117(2) . . ? C26 C31 H31 121.7 . . ? C30 C31 H31 121.7 . . ? C37 C32 C33 118.8(14) . . ? C37 C32 C4 121.5(13) . . ? C33 C32 C4 119.7(13) . . ? C32 C33 C34 118.9(14) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 121.5(15) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 O3 115.9(15) . . ? C34 C35 C36 120.6(14) . . ? O3 C35 C36 123.4(16) . . ? C35 C36 C37 119.5(15) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C32 C37 C36 120.5(15) . . ? C32 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? O3 C38 H38A 109.5 . . ? O3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 N3 131.4(14) . . ? O4 C39 C40 138.4(15) . . ? N3 C39 C40 90.1(12) . . ? O5 C40 C39 110.1(13) . . ? O5 C40 C41 121.6(13) . . ? C39 C40 C41 87.2(12) . . ? O5 C40 H40 111.8 . . ? C39 C40 H40 111.8 . . ? C41 C40 H40 111.8 . . ? N3 C41 C69 115.4(13) . . ? N3 C41 C40 86.2(12) . . ? C69 C41 C40 121.1(13) . . ? N3 C41 H41 110.7 . . ? C69 C41 H41 110.7 . . ? C40 C41 H41 110.7 . . ? C52 C42 C43 121.2(13) . . ? C52 C42 N3 123.8(12) . . ? C43 C42 N3 115.0(13) . . ? C44 C43 C42 118.7(14) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C45 120.6(14) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 120.3(13) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C52 C46 C45 119.2(13) . . ? C52 C46 Ir2 117.6(9) . . ? C45 C46 Ir2 122.4(11) . . ? N4 C47 C48 125.1(15) . . ? N4 C47 H47 117.5 . . ? C48 C47 H47 117.5 . . ? C47 C48 C49 120.2(14) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 115.5(13) . . ? C50 C49 H49 122.2 . . ? C48 C49 H49 122.2 . . ? C49 C50 C51 122.2(14) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? N4 C51 C50 118.4(12) . . ? N4 C51 C52 113.8(12) . . ? C50 C51 C52 127.2(13) . . ? C46 C52 C42 118.9(12) . . ? C46 C52 C51 113.7(12) . . ? C42 C52 C51 127.4(13) . . ? C57 C53 C54 108.4(12) . . ? C57 C53 C58 126.6(15) . . ? C54 C53 C58 124.1(16) . . ? C57 C53 Ir2 74.6(8) . . ? C54 C53 Ir2 70.6(7) . . ? C58 C53 Ir2 129.0(12) . . ? C55 C54 C53 105.7(14) . . ? C55 C54 C59 126.5(15) . . ? C53 C54 C59 127.6(15) . . ? C55 C54 Ir2 70.4(7) . . ? C53 C54 Ir2 69.9(7) . . ? C59 C54 Ir2 126.7(12) . . ? C54 C55 C56 108.5(14) . . ? C54 C55 C60 124.4(15) . . ? C56 C55 C60 127.1(16) . . ? C54 C55 Ir2 70.2(8) . . ? C56 C55 Ir2 74.7(8) . . ? C60 C55 Ir2 124.1(11) . . ? C57 C56 C55 107.3(14) . . ? C57 C56 C61 127.5(17) . . ? C55 C56 C61 124.9(17) . . ? C57 C56 Ir2 70.8(8) . . ? C55 C56 Ir2 67.2(8) . . ? C61 C56 Ir2 132.4(12) . . ? C53 C57 C56 109.9(13) . . ? C53 C57 C62 123.1(15) . . ? C56 C57 C62 127.0(16) . . ? C53 C57 Ir2 67.9(8) . . ? C56 C57 Ir2 72.7(8) . . ? C62 C57 Ir2 125.8(11) . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 O5 125.2(18) . . ? C68 C63 C64 122.2(19) . . ? O5 C63 C64 113(2) . . ? C65 C64 C63 115(2) . . ? C65 C64 H64 122.5 . . ? C63 C64 H64 122.5 . . ? C66 C65 C64 121(2) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C65 C66 C67 119(2) . . ? C65 C66 H66 120.4 . . ? C67 C66 H66 120.4 . . ? C68 C67 C66 124(3) . . ? C68 C67 H67 118.2 . . ? C66 C67 H67 118.2 . . ? C67 C68 C63 119(2) . . ? C67 C68 H68 120.7 . . ? C63 C68 H68 120.7 . . ? C70 C69 C74 117.4(16) . . ? C70 C69 C41 123.5(15) . . ? C74 C69 C41 119.1(15) . . ? C69 C70 C71 128.7(16) . . ? C69 C70 H70 115.6 . . ? C71 C70 H70 115.6 . . ? C72 C71 C70 110.7(16) . . ? C72 C71 H71 124.6 . . ? C70 C71 H71 124.6 . . ? C73 C72 O6 116(2) . . ? C73 C72 C71 121.8(18) . . ? O6 C72 C71 123(2) . . ? C74 C73 C72 122.3(17) . . ? C74 C73 H73 118.8 . . ? C72 C73 H73 118.8 . . ? C73 C74 C69 118.7(18) . . ? C73 C74 H74 120.7 . . ? C69 C74 H74 120.7 . . ? O6 C75 H75A 109.5 . . ? O6 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? O6 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? Cl3 C76 Cl4 106.2(8) . . ? Cl3 C76 H76A 110.5 . . ? Cl4 C76 H76A 110.5 . . ? Cl3 C76 H76B 110.5 . . ? Cl4 C76 H76B 110.5 . . ? H76A C76 H76B 108.7 . . ? Cl5 C77 Cl6 106.2(9) . . ? Cl5 C77 H77A 110.5 . . ? Cl6 C77 H77A 110.5 . . ? Cl5 C77 H77B 110.5 . . ? Cl6 C77 H77B 110.5 . . ? H77A C77 H77B 108.7 . . ? Cl8 C78 Cl7 107.0(11) . . ? Cl8 C78 H78A 110.3 . . ? Cl7 C78 H78A 110.3 . . ? Cl8 C78 H78B 110.3 . . ? Cl7 C78 H78B 110.3 . . ? H78A C78 H78B 108.6 . . ? C9 Ir1 N2 77.3(4) . . ? C9 Ir1 C20 93.5(6) . . ? N2 Ir1 C20 130.6(6) . . ? C9 Ir1 C19 114.2(6) . . ? N2 Ir1 C19 101.5(5) . . ? C20 Ir1 C19 38.7(6) . . ? C9 Ir1 C16 109.1(6) . . ? N2 Ir1 C16 167.1(5) . . ? C20 Ir1 C16 39.7(6) . . ? C19 Ir1 C16 65.8(6) . . ? C9 Ir1 C18 151.7(6) . . ? N2 Ir1 C18 105.2(5) . . ? C20 Ir1 C18 63.1(6) . . ? C19 Ir1 C18 37.5(6) . . ? C16 Ir1 C18 63.7(6) . . ? C9 Ir1 C17 147.4(6) . . ? N2 Ir1 C17 135.0(6) . . ? C20 Ir1 C17 63.7(6) . . ? C19 Ir1 C17 62.8(6) . . ? C16 Ir1 C17 38.6(6) . . ? C18 Ir1 C17 36.3(6) . . ? C9 Ir1 Cl1 92.0(4) . . ? N2 Ir1 Cl1 86.9(3) . . ? C20 Ir1 Cl1 142.3(5) . . ? C19 Ir1 Cl1 153.5(4) . . ? C16 Ir1 Cl1 103.7(5) . . ? C18 Ir1 Cl1 116.2(4) . . ? C17 Ir1 Cl1 93.4(4) . . ? C46 Ir2 N4 77.6(5) . . ? C46 Ir2 C53 112.0(6) . . ? N4 Ir2 C53 166.6(5) . . ? C46 Ir2 C54 96.6(6) . . ? N4 Ir2 C54 132.9(5) . . ? C53 Ir2 C54 39.5(5) . . ? C46 Ir2 C55 118.0(6) . . ? N4 Ir2 C55 102.4(5) . . ? C53 Ir2 C55 65.2(6) . . ? C54 Ir2 C55 39.4(6) . . ? C46 Ir2 C57 148.7(5) . . ? N4 Ir2 C57 133.7(5) . . ? C53 Ir2 C57 37.5(6) . . ? C54 Ir2 C57 64.0(6) . . ? C55 Ir2 C57 63.1(6) . . ? C46 Ir2 C56 156.1(6) . . ? N4 Ir2 C56 104.2(5) . . ? C53 Ir2 C56 63.2(6) . . ? C54 Ir2 C56 64.4(6) . . ? C55 Ir2 C56 38.1(6) . . ? C57 Ir2 C56 36.5(6) . . ? C46 Ir2 Cl2 87.9(4) . . ? N4 Ir2 Cl2 85.7(3) . . ? C53 Ir2 Cl2 103.5(4) . . ? C54 Ir2 Cl2 141.3(4) . . ? C55 Ir2 Cl2 153.9(5) . . ? C57 Ir2 Cl2 93.3(4) . . ? C56 Ir2 Cl2 116.0(5) . . ? C2 N1 C5 132.8(12) . . ? C2 N1 C4 94.0(12) . . ? C5 N1 C4 129.1(11) . . ? C14 N2 C10 120.2(11) . . ? C14 N2 Ir1 117.5(9) . . ? C10 N2 Ir1 122.3(9) . . ? C39 N3 C42 131.7(12) . . ? C39 N3 C41 94.8(11) . . ? C42 N3 C41 131.1(12) . . ? C47 N4 C51 118.3(12) . . ? C47 N4 Ir2 124.4(10) . . ? C51 N4 Ir2 117.1(9) . . ? C26 O1 C3 118.2(12) . . ? C35 O3 C38 118.6(15) . . ? C40 O5 C63 115.3(13) . . ? C72 O6 C75 115.1(18) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.491 _refine_diff_density_min -1.577 _refine_diff_density_rms 0.179 _database_code_depnum_ccdc_archive 'CCDC 944670' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2JM603sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H36 Cl N2 O3 Rh' _chemical_formula_weight 695.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 32.2169(10) _cell_length_b 32.2169(10) _cell_length_c 20.2356(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 18189.2(14) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2772 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 16.13 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6444 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46957 _diffrn_reflns_av_R_equivalents 0.1184 _diffrn_reflns_av_sigmaI/netI 0.1758 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7135 _reflns_number_gt 2544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The paper reports that unspecified disordered solvent molecules were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. 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^)+(0.0128P)^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 7135 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _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 0.6115(2) 0.0221(2) -0.1020(3) 0.070(2) Uani 1 1 d . . . H1 H 0.6392 0.0199 -0.1020 0.084 Uiso 1 1 calc R . . C2 C 0.5808(3) 0.0031(2) -0.1553(3) 0.072(2) Uani 1 1 d . . . H2 H 0.5875 -0.0115 -0.1900 0.087 Uiso 1 1 calc R . . C3 C 0.5392(2) 0.0065(2) -0.1554(3) 0.075(2) Uani 1 1 d . . . H3 H 0.5179 -0.0056 -0.1907 0.090 Uiso 1 1 calc R . . C4 C 0.5302(2) 0.0277(2) -0.1036(3) 0.067(2) Uani 1 1 d . . . H4 H 0.5022 0.0293 -0.1023 0.080 Uiso 1 1 calc R . . C5 C 0.5636(2) 0.0469(2) -0.0521(3) 0.0545(18) Uani 1 1 d . . . C6 C 0.5590(2) 0.07119(19) 0.0066(3) 0.0477(17) Uani 1 1 d . . . C7 C 0.5221(2) 0.0800(2) 0.0143(3) 0.0604(18) Uani 1 1 d . . . H7 H 0.4992 0.0711 -0.0188 0.072 Uiso 1 1 calc R . . C8 C 0.5183(3) 0.1019(2) 0.0709(3) 0.0601(19) Uani 1 1 d . . . C9 C 0.5519(2) 0.1130(2) 0.1206(3) 0.069(2) Uani 1 1 d . . . H9 H 0.5492 0.1261 0.1602 0.083 Uiso 1 1 calc R . . C10 C 0.5891(2) 0.1046(2) 0.1109(3) 0.073(2) Uani 1 1 d . . . H10 H 0.6113 0.1128 0.1450 0.088 Uiso 1 1 calc R . . C11 C 0.5964(2) 0.0844(2) 0.0530(3) 0.0549(18) Uani 1 1 d . . . C12 C 0.4456(2) 0.1073(2) 0.0275(3) 0.0664(19) Uani 1 1 d . . . H12 H 0.4296 0.0760 0.0056 0.080 Uiso 1 1 calc R . . C13 C 0.4153(2) 0.1093(2) 0.0859(3) 0.072(2) Uani 1 1 d . . . H13 H 0.3870 0.0778 0.0939 0.087 Uiso 1 1 calc R . . C14 C 0.4576(3) 0.1173(2) 0.1310(4) 0.076(2) Uani 1 1 d . . . C15 C 0.4657(2) 0.1470(3) -0.0208(3) 0.0520(18) Uani 1 1 d . . . C16 C 0.4498(2) 0.1388(2) -0.0846(4) 0.074(2) Uani 1 1 d . . . H16 H 0.4268 0.1080 -0.0975 0.089 Uiso 1 1 calc R . . C17 C 0.4678(3) 0.1760(3) -0.1308(3) 0.083(2) Uani 1 1 d . . . H17 H 0.4560 0.1699 -0.1738 0.100 Uiso 1 1 calc R . . C18 C 0.5019(3) 0.2204(3) -0.1137(5) 0.076(2) Uani 1 1 d . . . C19 C 0.5181(2) 0.2295(3) -0.0483(4) 0.083(2) Uani 1 1 d . . . H19 H 0.5408 0.2604 -0.0354 0.099 Uiso 1 1 calc R . . C20 C 0.5007(3) 0.1930(3) -0.0034(4) 0.082(2) Uani 1 1 d . . . H20 H 0.5124 0.1991 0.0396 0.099 Uiso 1 1 calc R . . C21 C 0.5102(3) 0.2530(3) -0.2207(4) 0.165(4) Uani 1 1 d . . . H21A H 0.5214 0.2332 -0.2402 0.248 Uiso 1 1 calc R . . H21B H 0.5248 0.2834 -0.2427 0.248 Uiso 1 1 calc R . . H21C H 0.4760 0.2376 -0.2252 0.248 Uiso 1 1 calc R . . C22 C 0.3607(3) 0.1342(3) 0.0584(4) 0.071(2) Uani 1 1 d . . . C23 C 0.3434(4) 0.1635(3) 0.0761(4) 0.111(3) Uani 1 1 d . . . H23 H 0.3609 0.1891 0.1046 0.133 Uiso 1 1 calc R . . C24 C 0.3009(4) 0.1554(3) 0.0524(6) 0.135(4) Uani 1 1 d . . . H24 H 0.2903 0.1764 0.0645 0.162 Uiso 1 1 calc R . . C25 C 0.2724(3) 0.1178(4) 0.0113(5) 0.122(4) Uani 1 1 d . . . H25 H 0.2420 0.1114 -0.0015 0.146 Uiso 1 1 calc R . . C26 C 0.2917(3) 0.0903(3) -0.0098(3) 0.098(3) Uani 1 1 d . . . H26 H 0.2755 0.0669 -0.0417 0.118 Uiso 1 1 calc R . . C27 C 0.3350(3) 0.0967(3) 0.0155(4) 0.088(2) Uani 1 1 d . . . H27 H 0.3461 0.0761 0.0036 0.105 Uiso 1 1 calc R . . C28 C 0.7135(2) 0.1268(3) -0.0132(4) 0.069(2) Uani 1 1 d . . . C29 C 0.7210(2) 0.0872(3) -0.0030(4) 0.072(2) Uani 1 1 d . . . C30 C 0.7161(2) 0.0762(3) 0.0636(4) 0.071(2) Uani 1 1 d . . . C31 C 0.7059(2) 0.1094(3) 0.0971(3) 0.070(2) Uani 1 1 d . . . C32 C 0.7061(2) 0.1410(3) 0.0492(4) 0.071(2) Uani 1 1 d . . . C33 C 0.7198(2) 0.1515(2) -0.0775(3) 0.102(2) Uani 1 1 d . . . H33A H 0.7015 0.1676 -0.0776 0.152 Uiso 1 1 calc R . . H33B H 0.7090 0.1284 -0.1127 0.152 Uiso 1 1 calc R . . H33C H 0.7531 0.1746 -0.0839 0.152 Uiso 1 1 calc R . . C34 C 0.7364(2) 0.0638(2) -0.0549(3) 0.110(3) Uani 1 1 d . . . H34A H 0.7700 0.0751 -0.0504 0.165 Uiso 1 1 calc R . . H34B H 0.7302 0.0719 -0.0981 0.165 Uiso 1 1 calc R . . H34C H 0.7187 0.0297 -0.0493 0.165 Uiso 1 1 calc R . . C35 C 0.7220(2) 0.0384(2) 0.0972(3) 0.126(3) Uani 1 1 d . . . H35A H 0.7145 0.0127 0.0668 0.190 Uiso 1 1 calc R . . H35B H 0.7007 0.0263 0.1344 0.190 Uiso 1 1 calc R . . H35C H 0.7545 0.0517 0.1120 0.190 Uiso 1 1 calc R . . C36 C 0.7038(2) 0.1129(2) 0.1718(3) 0.115(3) Uani 1 1 d . . . H36A H 0.7338 0.1191 0.1906 0.172 Uiso 1 1 calc R . . H36B H 0.6784 0.0832 0.1889 0.172 Uiso 1 1 calc R . . H36C H 0.6980 0.1385 0.1830 0.172 Uiso 1 1 calc R . . C37 C 0.7045(2) 0.1858(2) 0.0635(3) 0.112(3) Uani 1 1 d . . . H37A H 0.7361 0.2131 0.0590 0.167 Uiso 1 1 calc R . . H37B H 0.6932 0.1845 0.1077 0.167 Uiso 1 1 calc R . . H37C H 0.6833 0.1886 0.0328 0.167 Uiso 1 1 calc R . . Cl1 Cl 0.60096(6) -0.00525(5) 0.08613(7) 0.0796(5) Uani 1 1 d . . . N1 N 0.60386(18) 0.04346(16) -0.0507(2) 0.0529(14) Uani 1 1 d . . . N2 N 0.4798(2) 0.10999(17) 0.0780(3) 0.0679(16) Uani 1 1 d . . . O1 O 0.46701(16) 0.12414(17) 0.1881(2) 0.0998(17) Uani 1 1 d . . . O2 O 0.52242(18) 0.25978(17) -0.1538(3) 0.1071(18) Uani 1 1 d . . . O3 O 0.40347(17) 0.14526(16) 0.0885(2) 0.0780(14) Uani 1 1 d . . . Rh1 Rh 0.647817(17) 0.070395(17) 0.03103(2) 0.05842(18) Uani 1 1 d . . . 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 0.077(5) 0.085(6) 0.054(5) -0.013(4) -0.005(4) 0.045(5) C2 0.091(6) 0.072(5) 0.051(5) -0.011(4) 0.000(4) 0.038(5) C3 0.065(6) 0.093(6) 0.067(6) -0.011(4) -0.018(4) 0.040(5) C4 0.078(5) 0.083(5) 0.048(5) -0.018(4) -0.004(4) 0.048(5) C5 0.055(5) 0.053(5) 0.045(5) 0.005(4) -0.009(4) 0.019(4) C6 0.054(5) 0.052(4) 0.039(4) -0.003(3) -0.003(4) 0.027(4) C7 0.064(5) 0.063(5) 0.049(5) -0.007(4) -0.006(4) 0.027(4) C8 0.077(6) 0.072(5) 0.038(5) 0.004(4) -0.004(4) 0.042(5) C9 0.078(6) 0.077(5) 0.046(5) -0.014(4) -0.004(4) 0.033(5) C10 0.058(5) 0.090(6) 0.071(6) -0.003(4) 0.000(4) 0.036(5) C11 0.062(5) 0.062(5) 0.038(4) -0.003(3) -0.003(4) 0.029(4) C12 0.072(5) 0.063(5) 0.069(5) 0.005(4) 0.008(5) 0.038(4) C13 0.079(6) 0.079(6) 0.063(5) -0.001(4) 0.015(5) 0.042(5) C14 0.080(6) 0.092(6) 0.053(5) 0.002(5) 0.015(5) 0.040(5) C15 0.044(5) 0.058(5) 0.048(5) -0.005(4) 0.006(4) 0.021(4) C16 0.075(5) 0.068(6) 0.067(6) 0.012(5) 0.004(5) 0.026(4) C17 0.088(6) 0.075(6) 0.076(6) 0.006(5) -0.009(5) 0.032(5) C18 0.078(6) 0.055(6) 0.099(8) 0.013(6) 0.024(5) 0.035(5) C19 0.094(6) 0.075(7) 0.073(6) -0.024(5) -0.007(5) 0.039(5) C20 0.097(7) 0.087(7) 0.064(6) -0.007(5) -0.001(5) 0.047(6) C21 0.225(11) 0.115(8) 0.106(8) 0.042(7) 0.018(8) 0.048(7) C22 0.077(7) 0.068(6) 0.071(6) 0.009(5) 0.015(5) 0.038(6) C23 0.102(9) 0.087(8) 0.136(8) 0.023(6) 0.011(7) 0.041(7) C24 0.122(11) 0.059(7) 0.214(13) 0.012(7) 0.000(9) 0.038(8) C25 0.099(9) 0.146(10) 0.144(10) 0.084(8) 0.055(8) 0.080(9) C26 0.085(7) 0.152(9) 0.052(5) 0.017(5) 0.005(5) 0.056(7) C27 0.091(7) 0.104(7) 0.060(6) -0.002(5) 0.008(5) 0.042(6) C28 0.079(5) 0.067(6) 0.065(6) 0.015(5) -0.002(4) 0.039(5) C29 0.066(5) 0.081(6) 0.059(6) -0.002(5) -0.008(4) 0.030(5) C30 0.066(5) 0.069(6) 0.067(6) 0.016(5) -0.015(4) 0.026(4) C31 0.061(5) 0.090(6) 0.050(5) 0.003(5) -0.002(4) 0.031(5) C32 0.076(5) 0.055(5) 0.068(6) 0.005(5) 0.007(4) 0.023(4) C33 0.103(6) 0.105(6) 0.077(5) 0.043(5) 0.006(5) 0.037(5) C34 0.093(6) 0.137(7) 0.113(7) -0.026(6) -0.008(5) 0.067(6) C35 0.124(7) 0.121(7) 0.142(7) 0.043(6) -0.030(6) 0.068(6) C36 0.079(6) 0.182(8) 0.056(5) -0.003(5) -0.019(4) 0.045(5) C37 0.104(6) 0.058(5) 0.149(7) 0.005(5) 0.014(5) 0.023(5) Cl1 0.0873(13) 0.0641(12) 0.0696(12) 0.0041(9) -0.0082(10) 0.0246(11) N1 0.066(4) 0.059(4) 0.040(3) 0.003(3) 0.003(3) 0.036(3) N2 0.066(4) 0.085(4) 0.054(4) -0.009(3) 0.003(4) 0.039(4) O1 0.105(4) 0.139(5) 0.054(3) -0.016(3) 0.000(3) 0.060(3) O2 0.134(5) 0.071(4) 0.104(5) 0.021(4) 0.008(4) 0.043(4) O3 0.067(4) 0.081(4) 0.082(4) -0.012(3) 0.008(3) 0.035(3) Rh1 0.0634(4) 0.0576(4) 0.0494(3) 0.0018(3) -0.0096(3) 0.0266(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. ; 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 N1 1.335(6) . ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.395(7) . ? C2 H2 0.9300 . ? C3 C4 1.360(7) . ? C3 H3 0.9300 . ? C4 C5 1.401(7) . ? C4 H4 0.9300 . ? C5 N1 1.355(6) . ? C5 C6 1.470(7) . ? C6 C11 1.417(7) . ? C6 C7 1.361(7) . ? C7 C8 1.383(7) . ? C7 H7 0.9300 . ? C8 N2 1.395(7) . ? C8 C9 1.389(7) . ? C9 C10 1.369(7) . ? C9 H9 0.9300 . ? C10 C11 1.417(7) . ? C10 H10 0.9300 . ? C11 Rh1 1.972(6) . ? C12 N2 1.473(7) . ? C12 C15 1.479(7) . ? C12 C13 1.555(7) . ? C12 H12 0.9800 . ? C13 O3 1.390(6) . ? C13 C14 1.551(8) . ? C13 H13 0.9800 . ? C14 O1 1.188(7) . ? C14 N2 1.373(7) . ? C15 C16 1.366(7) . ? C15 C20 1.386(7) . ? C16 C17 1.397(7) . ? C16 H16 0.9300 . ? C17 C18 1.343(8) . ? C17 H17 0.9300 . ? C18 O2 1.365(7) . ? C18 C19 1.399(8) . ? C19 C20 1.366(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 O2 1.397(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.378(8) . ? C22 C23 1.363(9) . ? C22 O3 1.381(8) . ? C23 C24 1.345(10) . ? C23 H23 0.9300 . ? C24 C25 1.375(10) . ? C24 H24 0.9300 . ? C25 C26 1.381(9) . ? C25 H25 0.9300 . ? C26 C27 1.401(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C32 1.404(8) . ? C28 C29 1.427(8) . ? C28 C33 1.487(7) . ? C28 Rh1 2.175(6) . ? C29 C30 1.381(7) . ? C29 C34 1.513(7) . ? C29 Rh1 2.247(7) . ? C30 C31 1.439(8) . ? C30 C35 1.487(7) . ? C30 Rh1 2.213(6) . ? C31 C32 1.403(8) . ? C31 C36 1.518(7) . ? C31 Rh1 2.125(6) . ? C32 C37 1.498(7) . ? C32 Rh1 2.135(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? Cl1 Rh1 2.4046(16) . ? N1 Rh1 2.064(5) . ? 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 N1 C1 C2 124.0(6) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 118.0(6) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.3(6) . . ? N1 C5 C6 112.5(6) . . ? C4 C5 C6 125.1(7) . . ? C11 C6 C7 124.3(6) . . ? C11 C6 C5 113.4(6) . . ? C7 C6 C5 122.4(6) . . ? C8 C7 C6 120.7(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? N2 C8 C7 119.7(7) . . ? N2 C8 C9 121.9(7) . . ? C7 C8 C9 118.4(7) . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 124.9(6) . . ? C9 C10 H10 117.5 . . ? C11 C10 H10 117.5 . . ? C6 C11 C10 112.0(6) . . ? C6 C11 Rh1 118.0(5) . . ? C10 C11 Rh1 130.0(5) . . ? N2 C12 C15 114.6(6) . . ? N2 C12 C13 86.5(5) . . ? C15 C12 C13 118.6(5) . . ? N2 C12 H12 111.6 . . ? C15 C12 H12 111.6 . . ? C13 C12 H12 111.6 . . ? O3 C13 C14 115.0(6) . . ? O3 C13 C12 120.2(6) . . ? C14 C13 C12 86.3(5) . . ? O3 C13 H13 111.0 . . ? C14 C13 H13 111.0 . . ? C12 C13 H13 111.0 . . ? O1 C14 N2 133.2(8) . . ? O1 C14 C13 136.5(7) . . ? N2 C14 C13 90.2(6) . . ? C16 C15 C20 118.2(7) . . ? C16 C15 C12 119.9(7) . . ? C20 C15 C12 121.9(7) . . ? C17 C16 C15 120.8(7) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.6(7) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 O2 126.5(9) . . ? C17 C18 C19 119.2(7) . . ? O2 C18 C19 114.2(8) . . ? C20 C19 C18 119.9(7) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 121.1(7) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? O2 C21 H21A 109.5 . . ? O2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.9(9) . . ? C27 C22 O3 126.0(9) . . ? C23 C22 O3 114.0(10) . . ? C24 C23 C22 120.0(11) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 123.7(12) . . ? C23 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C24 C25 C26 115.8(11) . . ? C24 C25 H25 122.1 . . ? C26 C25 H25 122.1 . . ? C27 C26 C25 121.9(9) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C22 C27 C26 118.4(8) . . ? C22 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C32 C28 C29 107.1(6) . . ? C32 C28 C33 127.7(7) . . ? C29 C28 C33 124.6(7) . . ? C32 C28 Rh1 69.5(4) . . ? C29 C28 Rh1 73.9(4) . . ? C33 C28 Rh1 128.6(4) . . ? C30 C29 C28 108.8(7) . . ? C30 C29 C34 125.0(8) . . ? C28 C29 C34 125.9(7) . . ? C30 C29 Rh1 70.6(4) . . ? C28 C29 Rh1 68.5(4) . . ? C34 C29 Rh1 131.1(4) . . ? C29 C30 C31 108.0(7) . . ? C29 C30 C35 127.6(8) . . ? C31 C30 C35 124.4(8) . . ? C29 C30 Rh1 73.3(4) . . ? C31 C30 Rh1 67.4(4) . . ? C35 C30 Rh1 126.6(4) . . ? C32 C31 C30 107.1(6) . . ? C32 C31 C36 128.3(8) . . ? C30 C31 C36 123.9(7) . . ? C32 C31 Rh1 71.2(4) . . ? C30 C31 Rh1 74.0(4) . . ? C36 C31 Rh1 127.7(4) . . ? C28 C32 C31 109.0(7) . . ? C28 C32 C37 125.6(7) . . ? C31 C32 C37 125.1(7) . . ? C28 C32 Rh1 72.5(4) . . ? C31 C32 Rh1 70.4(4) . . ? C37 C32 Rh1 128.7(5) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C5 N1 C1 117.1(6) . . ? C5 N1 Rh1 117.8(4) . . ? C1 N1 Rh1 125.1(5) . . ? C14 N2 C8 134.5(7) . . ? C14 N2 C12 96.5(6) . . ? C8 N2 C12 128.7(6) . . ? C18 O2 C21 117.5(7) . . ? C13 O3 C22 115.0(6) . . ? C11 Rh1 N1 78.4(2) . . ? C11 Rh1 C31 108.3(3) . . ? N1 Rh1 C31 165.6(2) . . ? C11 Rh1 C32 96.2(3) . . ? N1 Rh1 C32 129.7(2) . . ? C31 Rh1 C32 38.5(2) . . ? C11 Rh1 C28 118.6(3) . . ? N1 Rh1 C28 101.4(2) . . ? C31 Rh1 C28 64.2(2) . . ? C32 Rh1 C28 38.0(2) . . ? C11 Rh1 C30 145.7(3) . . ? N1 Rh1 C30 135.9(3) . . ? C31 Rh1 C30 38.7(2) . . ? C32 Rh1 C30 63.4(2) . . ? C28 Rh1 C30 62.7(2) . . ? C11 Rh1 C29 156.0(3) . . ? N1 Rh1 C29 105.8(2) . . ? C31 Rh1 C29 62.8(2) . . ? C32 Rh1 C29 62.6(3) . . ? C28 Rh1 C29 37.6(2) . . ? C30 Rh1 C29 36.08(19) . . ? C11 Rh1 Cl1 87.36(16) . . ? N1 Rh1 Cl1 89.67(13) . . ? C31 Rh1 Cl1 103.2(2) . . ? C32 Rh1 Cl1 140.5(2) . . ? C28 Rh1 Cl1 153.2(2) . . ? C30 Rh1 Cl1 92.35(18) . . ? C29 Rh1 Cl1 115.9(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 N1 C1 C2 C3 0.1(10) . . . . ? C1 C2 C3 C4 -0.7(9) . . . . ? C2 C3 C4 C5 1.9(9) . . . . ? C3 C4 C5 N1 -2.7(9) . . . . ? C3 C4 C5 C6 179.3(5) . . . . ? N1 C5 C6 C11 -2.0(7) . . . . ? C4 C5 C6 C11 176.1(5) . . . . ? N1 C5 C6 C7 177.7(5) . . . . ? C4 C5 C6 C7 -4.2(9) . . . . ? C11 C6 C7 C8 -1.9(9) . . . . ? C5 C6 C7 C8 178.4(5) . . . . ? C6 C7 C8 N2 -179.2(5) . . . . ? C6 C7 C8 C9 -2.5(9) . . . . ? N2 C8 C9 C10 -179.6(6) . . . . ? C7 C8 C9 C10 3.7(9) . . . . ? C8 C9 C10 C11 -0.7(10) . . . . ? C7 C6 C11 C10 4.5(8) . . . . ? C5 C6 C11 C10 -175.8(5) . . . . ? C7 C6 C11 Rh1 -177.9(4) . . . . ? C5 C6 C11 Rh1 1.8(6) . . . . ? C9 C10 C11 C6 -3.2(9) . . . . ? C9 C10 C11 Rh1 179.6(5) . . . . ? N2 C12 C13 O3 122.5(6) . . . . ? C15 C12 C13 O3 6.3(10) . . . . ? N2 C12 C13 C14 5.6(5) . . . . ? C15 C12 C13 C14 -110.6(7) . . . . ? O3 C13 C14 O1 56.1(12) . . . . ? C12 C13 C14 O1 177.9(9) . . . . ? O3 C13 C14 N2 -127.8(6) . . . . ? C12 C13 C14 N2 -6.0(5) . . . . ? N2 C12 C15 C16 146.3(6) . . . . ? C13 C12 C15 C16 -113.7(7) . . . . ? N2 C12 C15 C20 -33.5(9) . . . . ? C13 C12 C15 C20 66.4(9) . . . . ? C20 C15 C16 C17 -1.2(10) . . . . ? C12 C15 C16 C17 178.9(6) . . . . ? C15 C16 C17 C18 1.7(10) . . . . ? C16 C17 C18 O2 -179.9(6) . . . . ? C16 C17 C18 C19 -2.4(10) . . . . ? C17 C18 C19 C20 2.7(11) . . . . ? O2 C18 C19 C20 -179.5(6) . . . . ? C18 C19 C20 C15 -2.3(11) . . . . ? C16 C15 C20 C19 1.5(10) . . . . ? C12 C15 C20 C19 -178.6(6) . . . . ? C27 C22 C23 C24 0.8(12) . . . . ? O3 C22 C23 C24 -177.3(8) . . . . ? C22 C23 C24 C25 1.5(15) . . . . ? C23 C24 C25 C26 -5.5(15) . . . . ? C24 C25 C26 C27 7.5(12) . . . . ? C23 C22 C27 C26 1.2(11) . . . . ? O3 C22 C27 C26 179.0(6) . . . . ? C25 C26 C27 C22 -5.5(11) . . . . ? C32 C28 C29 C30 2.6(7) . . . . ? C33 C28 C29 C30 174.6(6) . . . . ? Rh1 C28 C29 C30 -59.3(5) . . . . ? C32 C28 C29 C34 -172.1(6) . . . . ? C33 C28 C29 C34 -0.1(10) . . . . ? Rh1 C28 C29 C34 126.0(6) . . . . ? C32 C28 C29 Rh1 61.9(4) . . . . ? C33 C28 C29 Rh1 -126.1(6) . . . . ? C28 C29 C30 C31 -0.7(7) . . . . ? C34 C29 C30 C31 174.1(6) . . . . ? Rh1 C29 C30 C31 -58.7(5) . . . . ? C28 C29 C30 C35 -178.4(6) . . . . ? C34 C29 C30 C35 -3.6(11) . . . . ? Rh1 C29 C30 C35 123.6(7) . . . . ? C28 C29 C30 Rh1 58.0(5) . . . . ? C34 C29 C30 Rh1 -127.3(6) . . . . ? C29 C30 C31 C32 -1.5(8) . . . . ? C35 C30 C31 C32 176.3(6) . . . . ? Rh1 C30 C31 C32 -63.9(4) . . . . ? C29 C30 C31 C36 -172.5(6) . . . . ? C35 C30 C31 C36 5.3(10) . . . . ? Rh1 C30 C31 C36 125.1(6) . . . . ? C29 C30 C31 Rh1 62.4(5) . . . . ? C35 C30 C31 Rh1 -119.8(6) . . . . ? C29 C28 C32 C31 -3.6(8) . . . . ? C33 C28 C32 C31 -175.2(6) . . . . ? Rh1 C28 C32 C31 61.3(5) . . . . ? C29 C28 C32 C37 169.7(6) . . . . ? C33 C28 C32 C37 -2.0(11) . . . . ? Rh1 C28 C32 C37 -125.5(7) . . . . ? C29 C28 C32 Rh1 -64.8(5) . . . . ? C33 C28 C32 Rh1 123.5(7) . . . . ? C30 C31 C32 C28 3.1(8) . . . . ? C36 C31 C32 C28 173.6(6) . . . . ? Rh1 C31 C32 C28 -62.7(5) . . . . ? C30 C31 C32 C37 -170.1(6) . . . . ? C36 C31 C32 C37 0.4(11) . . . . ? Rh1 C31 C32 C37 124.1(7) . . . . ? C30 C31 C32 Rh1 65.8(5) . . . . ? C36 C31 C32 Rh1 -123.7(7) . . . . ? C4 C5 N1 C1 2.2(8) . . . . ? C6 C5 N1 C1 -179.7(5) . . . . ? C4 C5 N1 Rh1 -176.8(4) . . . . ? C6 C5 N1 Rh1 1.4(6) . . . . ? C2 C1 N1 C5 -0.8(9) . . . . ? C2 C1 N1 Rh1 178.0(4) . . . . ? O1 C14 N2 C8 9.4(14) . . . . ? C13 C14 N2 C8 -166.9(7) . . . . ? O1 C14 N2 C12 -177.3(9) . . . . ? C13 C14 N2 C12 6.4(5) . . . . ? C7 C8 N2 C14 157.8(7) . . . . ? C9 C8 N2 C14 -18.8(11) . . . . ? C7 C8 N2 C12 -13.6(10) . . . . ? C9 C8 N2 C12 169.8(6) . . . . ? C15 C12 N2 C14 113.6(6) . . . . ? C13 C12 N2 C14 -6.4(5) . . . . ? C15 C12 N2 C8 -72.6(8) . . . . ? C13 C12 N2 C8 167.5(6) . . . . ? C17 C18 O2 C21 -6.2(11) . . . . ? C19 C18 O2 C21 176.2(7) . . . . ? C14 C13 O3 C22 -168.5(5) . . . . ? C12 C13 O3 C22 90.6(7) . . . . ? C27 C22 O3 C13 -14.7(9) . . . . ? C23 C22 O3 C13 163.3(6) . . . . ? C6 C11 Rh1 N1 -0.8(4) . . . . ? C10 C11 Rh1 N1 176.3(6) . . . . ? C6 C11 Rh1 C31 166.0(4) . . . . ? C10 C11 Rh1 C31 -17.0(6) . . . . ? C6 C11 Rh1 C32 128.5(5) . . . . ? C10 C11 Rh1 C32 -54.5(6) . . . . ? C6 C11 Rh1 C28 96.0(5) . . . . ? C10 C11 Rh1 C28 -87.0(6) . . . . ? C6 C11 Rh1 C30 178.7(4) . . . . ? C10 C11 Rh1 C30 -4.2(8) . . . . ? C6 C11 Rh1 C29 102.1(7) . . . . ? C10 C11 Rh1 C29 -80.8(8) . . . . ? C6 C11 Rh1 Cl1 -91.0(4) . . . . ? C10 C11 Rh1 Cl1 86.1(5) . . . . ? C5 N1 Rh1 C11 -0.4(4) . . . . ? C1 N1 Rh1 C11 -179.2(5) . . . . ? C5 N1 Rh1 C31 -119.5(11) . . . . ? C1 N1 Rh1 C31 61.6(13) . . . . ? C5 N1 Rh1 C32 -88.9(5) . . . . ? C1 N1 Rh1 C32 92.3(5) . . . . ? C5 N1 Rh1 C28 -117.6(4) . . . . ? C1 N1 Rh1 C28 63.5(5) . . . . ? C5 N1 Rh1 C30 -180.0(4) . . . . ? C1 N1 Rh1 C30 1.2(6) . . . . ? C5 N1 Rh1 C29 -156.1(4) . . . . ? C1 N1 Rh1 C29 25.1(5) . . . . ? C5 N1 Rh1 Cl1 87.0(4) . . . . ? C1 N1 Rh1 Cl1 -91.9(5) . . . . ? C32 C31 Rh1 C11 -76.6(5) . . . . ? C30 C31 Rh1 C11 168.5(4) . . . . ? C36 C31 Rh1 C11 47.7(8) . . . . ? C32 C31 Rh1 N1 39.1(14) . . . . ? C30 C31 Rh1 N1 -75.8(13) . . . . ? C36 C31 Rh1 N1 163.4(8) . . . . ? C30 C31 Rh1 C32 -114.9(6) . . . . ? C36 C31 Rh1 C32 124.3(10) . . . . ? C32 C31 Rh1 C28 37.0(4) . . . . ? C30 C31 Rh1 C28 -77.8(4) . . . . ? C36 C31 Rh1 C28 161.4(9) . . . . ? C32 C31 Rh1 C30 114.9(6) . . . . ? C36 C31 Rh1 C30 -120.8(10) . . . . ? C32 C31 Rh1 C29 79.2(4) . . . . ? C30 C31 Rh1 C29 -35.6(4) . . . . ? C36 C31 Rh1 C29 -156.4(9) . . . . ? C32 C31 Rh1 Cl1 -168.2(4) . . . . ? C30 C31 Rh1 Cl1 76.9(4) . . . . ? C36 C31 Rh1 Cl1 -43.9(7) . . . . ? C28 C32 Rh1 C11 -130.0(4) . . . . ? C31 C32 Rh1 C11 111.7(5) . . . . ? C37 C32 Rh1 C11 -8.0(7) . . . . ? C28 C32 Rh1 N1 -49.9(5) . . . . ? C31 C32 Rh1 N1 -168.2(4) . . . . ? C37 C32 Rh1 N1 72.0(8) . . . . ? C28 C32 Rh1 C31 118.3(6) . . . . ? C37 C32 Rh1 C31 -119.7(9) . . . . ? C31 C32 Rh1 C28 -118.3(6) . . . . ? C37 C32 Rh1 C28 122.0(9) . . . . ? C28 C32 Rh1 C30 78.9(4) . . . . ? C31 C32 Rh1 C30 -39.3(4) . . . . ? C37 C32 Rh1 C30 -159.1(8) . . . . ? C28 C32 Rh1 C29 38.3(4) . . . . ? C31 C32 Rh1 C29 -80.0(4) . . . . ? C37 C32 Rh1 C29 160.2(8) . . . . ? C28 C32 Rh1 Cl1 136.5(4) . . . . ? C31 C32 Rh1 Cl1 18.3(6) . . . . ? C37 C32 Rh1 Cl1 -101.5(7) . . . . ? C32 C28 Rh1 C11 60.2(5) . . . . ? C29 C28 Rh1 C11 175.9(4) . . . . ? C33 C28 Rh1 C11 -62.4(8) . . . . ? C32 C28 Rh1 N1 143.0(4) . . . . ? C29 C28 Rh1 N1 -101.2(4) . . . . ? C33 C28 Rh1 N1 20.5(7) . . . . ? C32 C28 Rh1 C31 -37.5(4) . . . . ? C29 C28 Rh1 C31 78.3(4) . . . . ? C33 C28 Rh1 C31 -160.0(8) . . . . ? C29 C28 Rh1 C32 115.8(6) . . . . ? C33 C28 Rh1 C32 -122.5(9) . . . . ? C32 C28 Rh1 C30 -80.9(4) . . . . ? C29 C28 Rh1 C30 34.9(4) . . . . ? C33 C28 Rh1 C30 156.6(8) . . . . ? C32 C28 Rh1 C29 -115.8(6) . . . . ? C33 C28 Rh1 C29 121.7(9) . . . . ? C32 C28 Rh1 Cl1 -104.2(6) . . . . ? C29 C28 Rh1 Cl1 11.6(7) . . . . ? C33 C28 Rh1 Cl1 133.3(5) . . . . ? C29 C30 Rh1 C11 -137.9(5) . . . . ? C31 C30 Rh1 C11 -19.6(7) . . . . ? C35 C30 Rh1 C11 97.3(8) . . . . ? C29 C30 Rh1 N1 41.4(6) . . . . ? C31 C30 Rh1 N1 159.7(4) . . . . ? C35 C30 Rh1 N1 -83.4(7) . . . . ? C29 C30 Rh1 C31 -118.3(6) . . . . ? C35 C30 Rh1 C31 116.9(9) . . . . ? C29 C30 Rh1 C32 -79.2(4) . . . . ? C31 C30 Rh1 C32 39.1(4) . . . . ? C35 C30 Rh1 C32 156.0(9) . . . . ? C29 C30 Rh1 C28 -36.3(4) . . . . ? C31 C30 Rh1 C28 82.0(4) . . . . ? C35 C30 Rh1 C28 -161.2(9) . . . . ? C31 C30 Rh1 C29 118.3(6) . . . . ? C35 C30 Rh1 C29 -124.8(10) . . . . ? C29 C30 Rh1 Cl1 133.4(5) . . . . ? C31 C30 Rh1 Cl1 -108.3(4) . . . . ? C35 C30 Rh1 Cl1 8.5(7) . . . . ? C30 C29 Rh1 C11 111.5(7) . . . . ? C28 C29 Rh1 C11 -8.8(9) . . . . ? C34 C29 Rh1 C11 -128.4(7) . . . . ? C30 C29 Rh1 N1 -151.4(4) . . . . ? C28 C29 Rh1 N1 88.2(4) . . . . ? C34 C29 Rh1 N1 -31.3(8) . . . . ? C30 C29 Rh1 C31 38.2(4) . . . . ? C28 C29 Rh1 C31 -82.2(4) . . . . ? C34 C29 Rh1 C31 158.3(9) . . . . ? C30 C29 Rh1 C32 81.7(4) . . . . ? C28 C29 Rh1 C32 -38.6(4) . . . . ? C34 C29 Rh1 C32 -158.2(9) . . . . ? C30 C29 Rh1 C28 120.4(6) . . . . ? C34 C29 Rh1 C28 -119.6(9) . . . . ? C28 C29 Rh1 C30 -120.4(6) . . . . ? C34 C29 Rh1 C30 120.1(10) . . . . ? C30 C29 Rh1 Cl1 -53.9(5) . . . . ? C28 C29 Rh1 Cl1 -174.2(4) . . . . ? C34 C29 Rh1 Cl1 66.2(7) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.001 1535 351 ' ' 2 0.333 0.667 0.670 1541 352 ' ' 3 0.667 0.333 0.336 1541 352 ' ' _platon_squeeze_details ; The final refinement show high values of residual non-modelled electronic density.Therefore, the Squeeze program was used to remove its contribution to the overal intensity data.An improvement was observed in all refinement parameters and residual when this procedure is applied ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.452 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 944671' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JM542 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H53 Cl4 Ir2 N3 O2' _chemical_formula_weight 1278.17 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 19.8758(13) _cell_length_b 12.6780(9) _cell_length_c 23.5977(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.2220(10) _cell_angle_gamma 90.00 _cell_volume 5930.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7656 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.33 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 4.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3862 _exptl_absorpt_correction_T_max 0.5022 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32593 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11556 _reflns_number_gt 7353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; After modeling of one solvent molecules of CH2Cl2 the residual the disordered electron density was taken into account using the SQUEEZE/PLATON procedure. ; _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^)+(0.0827P)^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 11556 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.006 _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 C53 C 0.7961(8) 0.7685(11) 0.1052(6) 0.125(5) Uiso 1 1 d . . . H53A H 0.7609 0.7380 0.0796 0.149 Uiso 1 1 calc R . . H53B H 0.8283 0.7134 0.1161 0.149 Uiso 1 1 calc R . . Cl3 Cl 0.7608(3) 0.8166(5) 0.1656(3) 0.200(2) Uiso 1 1 d . . . Cl4 Cl 0.8354(3) 0.8663(5) 0.0712(3) 0.190(2) Uiso 1 1 d . . . N1 N 0.1086(3) 0.1799(5) 0.1424(3) 0.0510(17) Uani 1 1 d . . . O1 O 0.0675(4) 0.1439(7) 0.2314(3) 0.102(3) Uani 1 1 d . . . N2 N -0.1376(3) 0.4440(5) 0.0442(2) 0.0460(16) Uani 1 1 d . . . C2 C 0.1075(5) 0.1347(8) 0.1950(4) 0.064(3) Uani 1 1 d . . . O2 O 0.2202(3) 0.0948(6) 0.2303(3) 0.085(2) Uani 1 1 d . . . N3 N 0.4389(3) 0.3862(5) 0.0809(3) 0.0496(17) Uani 1 1 d . . . C3 C 0.1712(4) 0.0733(8) 0.1875(4) 0.063(2) Uani 1 1 d . . . H3 H 0.1631 -0.0024 0.1820 0.075 Uiso 1 1 calc R . . C4 C 0.1744(4) 0.1355(7) 0.1297(3) 0.052(2) Uani 1 1 d . . . H4 H 0.1709 0.0887 0.0966 0.063 Uiso 1 1 calc R . . C5 C 0.0608(4) 0.2407(6) 0.1089(3) 0.0442(19) Uani 1 1 d . . . C6 C 0.0063(4) 0.2828(7) 0.1331(3) 0.048(2) Uani 1 1 d . . . H6 H 0.0027 0.2745 0.1719 0.057 Uiso 1 1 calc R . . C7 C -0.0437(3) 0.3377(6) 0.1011(3) 0.0412(18) Uani 1 1 d . . . C8 C -0.1880(4) 0.5044(7) 0.0209(4) 0.056(2) Uani 1 1 d . . . H8 H -0.2215 0.5262 0.0437 0.067 Uiso 1 1 calc R . . C9 C -0.1924(5) 0.5354(8) -0.0351(4) 0.069(3) Uani 1 1 d . . . H9 H -0.2280 0.5764 -0.0504 0.083 Uiso 1 1 calc R . . C10 C -0.1406(5) 0.5021(8) -0.0679(4) 0.065(3) Uani 1 1 d . . . H10 H -0.1421 0.5197 -0.1063 0.078 Uiso 1 1 calc R . . C11 C -0.0900(5) 0.4465(7) -0.0453(3) 0.060(2) Uani 1 1 d . . . H11 H -0.0552 0.4271 -0.0675 0.072 Uiso 1 1 calc R . . C12 C -0.0876(4) 0.4158(6) 0.0117(3) 0.0446(19) Uani 1 1 d . . . C13 C -0.0340(4) 0.3536(6) 0.0428(3) 0.0415(18) Uani 1 1 d . . . C14 C 0.0215(4) 0.3118(8) 0.0188(3) 0.059(2) Uani 1 1 d . . . H14 H 0.0271 0.3225 -0.0195 0.071 Uiso 1 1 calc R . . C15 C 0.0687(4) 0.2541(6) 0.0520(3) 0.049(2) Uani 1 1 d . . . H15 H 0.1056 0.2246 0.0358 0.059 Uiso 1 1 calc R . . C16 C -0.1770(5) 0.4263(7) 0.2119(4) 0.109(4) Uani 1 1 d G . . C17 C -0.2292(4) 0.4208(8) 0.1675(4) 0.109(4) Uani 1 1 d G . . C18 C -0.2246(4) 0.3214(9) 0.1403(3) 0.110(4) Uani 1 1 d G . . C19 C -0.1696(5) 0.2655(6) 0.1679(4) 0.110(4) Uani 1 1 d G . . C20 C -0.1402(3) 0.3303(8) 0.2121(3) 0.087(4) Uani 1 1 d G . . C22 C -0.2835(7) 0.4941(11) 0.1585(6) 0.121 Uani 1 1 d . . . H22A H -0.3210 0.4709 0.1787 0.181 Uiso 1 1 calc R . . H22B H -0.2968 0.4982 0.1186 0.181 Uiso 1 1 calc R . . H22C H -0.2691 0.5623 0.1722 0.181 Uiso 1 1 calc R . . C23 C -0.2626(10) 0.2608(14) 0.0929(8) 0.170 Uani 1 1 d . . . H23A H -0.2316 0.2182 0.0736 0.254 Uiso 1 1 calc R . . H23B H -0.2847 0.3095 0.0665 0.254 Uiso 1 1 calc R . . H23C H -0.2957 0.2163 0.1086 0.254 Uiso 1 1 calc R . . C24 C -0.1444(9) 0.1483(13) 0.1611(7) 0.152 Uani 1 1 d . . . H24A H -0.1055 0.1362 0.1868 0.228 Uiso 1 1 calc R . . H24B H -0.1327 0.1371 0.1228 0.228 Uiso 1 1 calc R . . H24C H -0.1796 0.1003 0.1696 0.228 Uiso 1 1 calc R . . C25 C -0.0892(7) 0.2816(11) 0.2549(6) 0.124 Uani 1 1 d . . . H25A H -0.0725 0.3345 0.2814 0.186 Uiso 1 1 calc R . . H25B H -0.0524 0.2532 0.2355 0.186 Uiso 1 1 calc R . . H25C H -0.1102 0.2260 0.2749 0.186 Uiso 1 1 calc R . . C32 C 0.2305(4) 0.2141(6) 0.1272(3) 0.0395(18) Uani 1 1 d . . . C33 C 0.2357(4) 0.2978(7) 0.1638(3) 0.054(2) Uani 1 1 d . . . H33 H 0.2030 0.3086 0.1895 0.064 Uiso 1 1 calc R . . C34 C 0.2903(5) 0.3669(7) 0.1626(3) 0.053(2) Uani 1 1 d . . . H34 H 0.2933 0.4250 0.1867 0.064 Uiso 1 1 calc R . . C35 C 0.3407(4) 0.3491(7) 0.1252(3) 0.0437(19) Uani 1 1 d . . . C36 C 0.3983(4) 0.4152(6) 0.1219(3) 0.0442(19) Uani 1 1 d . . . C37 C 0.4146(5) 0.5045(7) 0.1549(3) 0.058(2) Uani 1 1 d . . . H37 H 0.3863 0.5257 0.1825 0.069 Uiso 1 1 calc R . . C38 C 0.4722(5) 0.5613(8) 0.1470(4) 0.069(3) Uani 1 1 d . . . H38 H 0.4838 0.6198 0.1694 0.083 Uiso 1 1 calc R . . C39 C 0.5127(5) 0.5286(9) 0.1044(4) 0.075(3) Uani 1 1 d . . . H39 H 0.5520 0.5654 0.0984 0.090 Uiso 1 1 calc R . . C40 C 0.4954(5) 0.4452(8) 0.0725(4) 0.062(2) Uani 1 1 d . . . H40 H 0.5223 0.4261 0.0436 0.074 Uiso 1 1 calc R . . C41 C 0.3366(4) 0.2642(6) 0.0875(3) 0.0426(19) Uani 1 1 d . . . C42 C 0.2785(4) 0.1970(7) 0.0881(3) 0.0465(19) Uani 1 1 d . . . H42 H 0.2729 0.1418 0.0622 0.056 Uiso 1 1 calc R . . C43 C 0.4350(5) 0.0851(7) 0.0564(4) 0.062(3) Uani 1 1 d . . . C44 C 0.4105(4) 0.0916(7) -0.0015(4) 0.058(2) Uani 1 1 d . . . C45 C 0.4967(5) 0.1468(7) 0.0628(3) 0.058(2) Uani 1 1 d . . . C46 C 0.5119(4) 0.1854(7) 0.0064(4) 0.055(2) Uani 1 1 d . . . C47 C 0.4578(4) 0.1508(7) -0.0317(3) 0.050(2) Uani 1 1 d . . . C48 C 0.3504(5) 0.0347(8) -0.0282(5) 0.083(3) Uani 1 1 d . . . H48A H 0.3650 -0.0200 -0.0527 0.125 Uiso 1 1 calc R . . H48B H 0.3221 0.0834 -0.0501 0.125 Uiso 1 1 calc R . . H48C H 0.3254 0.0039 0.0009 0.125 Uiso 1 1 calc R . . C49 C 0.4067(6) 0.0225(8) 0.1028(4) 0.083(3) Uani 1 1 d . . . H49A H 0.3616 0.0005 0.0910 0.124 Uiso 1 1 calc R . . H49B H 0.4059 0.0653 0.1364 0.124 Uiso 1 1 calc R . . H49C H 0.4344 -0.0385 0.1110 0.124 Uiso 1 1 calc R . . C50 C 0.5426(5) 0.1652(11) 0.1156(4) 0.101(4) Uani 1 1 d . . . H50A H 0.5804 0.1179 0.1158 0.152 Uiso 1 1 calc R . . H50B H 0.5182 0.1526 0.1486 0.152 Uiso 1 1 calc R . . H50C H 0.5585 0.2367 0.1161 0.152 Uiso 1 1 calc R . . C51 C 0.5743(5) 0.2428(9) -0.0082(5) 0.085(3) Uani 1 1 d . . . H51A H 0.5812 0.3031 0.0161 0.128 Uiso 1 1 calc R . . H51B H 0.5691 0.2655 -0.0471 0.128 Uiso 1 1 calc R . . H51C H 0.6125 0.1965 -0.0030 0.128 Uiso 1 1 calc R . . C52 C 0.4501(6) 0.1736(9) -0.0933(3) 0.079(3) Uani 1 1 d . . . H52A H 0.4458 0.1086 -0.1141 0.119 Uiso 1 1 calc R . . H52B H 0.4890 0.2113 -0.1042 0.119 Uiso 1 1 calc R . . H52C H 0.4105 0.2157 -0.1016 0.119 Uiso 1 1 calc R . . Cl1 Cl -0.06670(13) 0.5672(2) 0.14088(10) 0.0714(7) Uani 1 1 d . . . Ir1 Ir -0.128305(16) 0.40413(3) 0.130470(13) 0.04962(12) Uani 1 1 d . . . Cl2 Cl 0.34939(11) 0.3605(2) -0.03032(9) 0.0632(6) Uani 1 1 d . . . Ir2 Ir 0.413142(15) 0.24860(2) 0.035816(11) 0.04170(11) Uani 1 1 d . . . C26 C 0.2801(4) 0.0341(8) 0.2305(4) 0.095(4) Uiso 1 1 d G . . C27 C 0.2863(5) -0.0610(8) 0.2020(4) 0.123(5) Uiso 1 1 d G . . H27 H 0.2503 -0.0869 0.1787 0.148 Uiso 1 1 calc R . . C28 C 0.3464(6) -0.1173(7) 0.2084(4) 0.153(4) Uiso 1 1 d G . . H28 H 0.3506 -0.1809 0.1894 0.184 Uiso 1 1 calc R . . C29 C 0.4002(4) -0.0785(9) 0.2433(5) 0.153(4) Uiso 1 1 d G . . H29 H 0.4404 -0.1162 0.2476 0.184 Uiso 1 1 calc R . . C30 C 0.3939(5) 0.0165(10) 0.2717(4) 0.153(4) Uiso 1 1 d G . . H30 H 0.4299 0.0425 0.2951 0.184 Uiso 1 1 calc R . . C31 C 0.3339(6) 0.0729(7) 0.2654(4) 0.170(7) Uiso 1 1 d G . . H31 H 0.3297 0.1365 0.2844 0.204 Uiso 1 1 calc R . . C21 C -0.1629(11) 0.5179(18) 0.2518(10) 0.215 Uiso 1 1 d . . . H21A H -0.1616 0.5821 0.2303 0.323 Uiso 1 1 calc R . . H21B H -0.1202 0.5074 0.2728 0.323 Uiso 1 1 calc R . . H21C H -0.1978 0.5225 0.2777 0.323 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 N1 0.031(4) 0.067(5) 0.055(4) 0.017(3) 0.000(3) 0.003(3) O1 0.072(5) 0.142(7) 0.096(5) 0.058(5) 0.040(4) 0.044(5) N2 0.040(4) 0.059(4) 0.039(3) 0.012(3) -0.004(3) 0.007(3) C2 0.038(5) 0.071(6) 0.085(7) 0.034(5) 0.005(5) 0.003(5) O2 0.049(4) 0.123(6) 0.081(4) 0.052(4) -0.002(3) 0.010(4) N3 0.041(4) 0.055(4) 0.053(4) -0.004(3) 0.004(3) 0.003(3) C3 0.042(5) 0.064(6) 0.082(6) 0.014(5) 0.004(5) -0.001(5) C4 0.040(5) 0.059(5) 0.058(5) 0.008(4) 0.007(4) 0.016(4) C5 0.030(4) 0.050(5) 0.052(4) 0.003(4) -0.002(3) 0.000(4) C6 0.029(5) 0.070(6) 0.044(4) 0.010(4) 0.000(3) 0.002(4) C7 0.020(4) 0.051(5) 0.051(4) 0.004(4) -0.004(3) 0.000(3) C8 0.032(5) 0.061(6) 0.072(5) 0.005(4) -0.007(4) 0.014(4) C9 0.062(7) 0.086(7) 0.058(5) 0.024(5) -0.005(5) 0.014(6) C10 0.064(7) 0.079(7) 0.052(5) 0.016(5) 0.000(5) 0.015(5) C11 0.056(6) 0.074(6) 0.049(5) 0.017(4) 0.005(4) 0.005(5) C12 0.037(5) 0.061(5) 0.035(4) 0.002(4) -0.003(3) 0.001(4) C13 0.030(4) 0.053(5) 0.041(4) -0.002(3) 0.000(3) 0.003(4) C14 0.046(6) 0.087(7) 0.047(4) -0.002(4) 0.012(4) -0.001(5) C15 0.029(4) 0.069(6) 0.050(4) 0.003(4) 0.005(3) 0.010(4) C16 0.090(8) 0.129(8) 0.115(8) 0.055(7) 0.056(5) 0.025(7) C17 0.090(8) 0.129(8) 0.115(8) 0.055(7) 0.056(5) 0.025(7) C18 0.083(7) 0.169(11) 0.080(6) 0.022(6) 0.024(5) -0.045(7) C19 0.083(7) 0.169(11) 0.080(6) 0.022(6) 0.024(5) -0.045(7) C20 0.034(5) 0.166(12) 0.064(6) 0.058(7) 0.016(4) 0.001(7) C22 0.121 0.121 0.121 0.000 0.009 0.000 C23 0.170 0.170 0.170 0.000 0.012 0.000 C24 0.152 0.152 0.152 0.000 0.011 0.000 C25 0.124 0.124 0.124 0.000 0.009 0.000 C32 0.033(4) 0.048(4) 0.038(4) 0.007(3) 0.004(3) 0.006(4) C33 0.038(5) 0.075(6) 0.049(4) 0.003(4) 0.012(4) -0.006(5) C34 0.057(6) 0.058(5) 0.046(4) -0.009(4) 0.009(4) 0.011(5) C35 0.034(5) 0.057(5) 0.040(4) 0.005(4) 0.006(3) 0.005(4) C36 0.035(5) 0.063(5) 0.035(4) 0.006(4) 0.005(3) -0.003(4) C37 0.064(6) 0.061(6) 0.050(4) -0.013(4) 0.018(4) -0.011(5) C38 0.077(7) 0.066(6) 0.064(6) -0.020(5) 0.008(5) -0.016(6) C39 0.059(7) 0.084(8) 0.086(7) 0.000(6) 0.022(5) -0.017(6) C40 0.049(6) 0.062(6) 0.075(6) -0.002(5) 0.016(5) -0.014(5) C41 0.043(5) 0.051(5) 0.034(3) 0.002(3) 0.003(3) 0.013(4) C42 0.034(5) 0.051(5) 0.055(4) 0.001(4) 0.005(4) 0.012(4) C43 0.066(7) 0.056(6) 0.068(6) 0.009(4) 0.028(5) 0.023(5) C44 0.038(5) 0.057(5) 0.078(6) -0.022(5) 0.008(4) 0.019(4) C45 0.048(6) 0.073(6) 0.053(5) 0.003(4) 0.007(4) 0.028(5) C46 0.047(5) 0.061(6) 0.060(5) 0.007(4) 0.023(4) 0.021(5) C47 0.040(5) 0.063(6) 0.047(4) -0.009(4) 0.009(4) 0.013(4) C48 0.078(8) 0.060(7) 0.114(8) -0.030(6) 0.012(6) -0.007(6) C49 0.087(8) 0.068(7) 0.097(8) 0.021(6) 0.032(6) 0.014(6) C50 0.072(8) 0.168(12) 0.060(6) 0.005(7) -0.017(5) 0.043(8) C51 0.045(6) 0.112(10) 0.100(8) -0.010(6) 0.019(6) -0.007(6) C52 0.094(8) 0.093(8) 0.049(5) -0.013(5) 0.002(5) 0.018(7) Cl1 0.0597(16) 0.0838(18) 0.0710(14) -0.0127(12) 0.0070(12) -0.0035(13) Ir1 0.02992(19) 0.0778(3) 0.04116(16) 0.00943(16) 0.00265(12) 0.00754(17) Cl2 0.0521(14) 0.0797(16) 0.0584(12) 0.0153(11) 0.0086(10) 0.0220(12) Ir2 0.03201(19) 0.0526(2) 0.04129(16) 0.00046(13) 0.00785(12) 0.00852(15) _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 C53 Cl3 1.744(15) . ? C53 Cl4 1.697(15) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? N1 C2 1.370(11) . ? N1 C4 1.475(10) . ? N1 C5 1.417(9) . ? O1 C2 1.217(11) . ? N2 C12 1.348(10) . ? N2 C8 1.346(9) . ? N2 Ir1 2.093(6) . ? C2 C3 1.508(13) . ? O2 C26 1.417(10) . ? O2 C3 1.378(11) . ? N3 C36 1.354(10) . ? N3 C40 1.377(11) . ? N3 Ir2 2.087(6) . ? C3 C4 1.581(12) . ? C3 H3 0.9800 . ? C4 C32 1.499(11) . ? C4 H4 0.9800 . ? C5 C6 1.369(11) . ? C5 C15 1.375(11) . ? C6 C7 1.391(10) . ? C6 H6 0.9300 . ? C7 C13 1.417(10) . ? C7 Ir1 2.047(8) . ? C8 C9 1.375(11) . ? C8 H8 0.9300 . ? C9 C10 1.398(13) . ? C9 H9 0.9300 . ? C10 C11 1.310(12) . ? C10 H10 0.9300 . ? C11 C12 1.397(10) . ? C11 H11 0.9300 . ? C12 C13 1.478(10) . ? C13 C14 1.381(11) . ? C14 C15 1.386(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.4200 . ? C16 C20 1.4200 . ? C16 C21 1.51(2) . ? C16 Ir1 2.231(8) . ? C17 C18 1.4200 . ? C17 C22 1.427(15) . ? C17 Ir1 2.255(8) . ? C18 C19 1.4200 . ? C18 C23 1.512(19) . ? C18 Ir1 2.210(8) . ? C19 C20 1.4200 . ? C19 C24 1.580(17) . ? C19 Ir1 2.156(8) . ? C20 C25 1.509(15) . ? C20 Ir1 2.170(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C32 C33 1.368(11) . ? C32 C42 1.392(10) . ? C33 C34 1.397(12) . ? C33 H33 0.9300 . ? C34 C35 1.400(11) . ? C34 H34 0.9300 . ? C35 C41 1.395(10) . ? C35 C36 1.426(11) . ? C36 C37 1.400(11) . ? C37 C38 1.376(12) . ? C37 H37 0.9300 . ? C38 C39 1.397(13) . ? C38 H38 0.9300 . ? C39 C40 1.329(13) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.436(11) . ? C41 Ir2 2.029(8) . ? C42 H42 0.9300 . ? C43 C44 1.420(13) . ? C43 C45 1.453(13) . ? C43 C49 1.495(12) . ? C43 Ir2 2.166(9) . ? C44 C47 1.433(12) . ? C44 C48 1.496(12) . ? C44 Ir2 2.175(8) . ? C45 C46 1.469(11) . ? C45 C50 1.508(12) . ? C45 Ir2 2.162(8) . ? C46 C47 1.420(12) . ? C46 C51 1.500(13) . ? C46 Ir2 2.275(8) . ? C47 C52 1.478(11) . ? C47 Ir2 2.253(8) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? Cl1 Ir1 2.407(3) . ? Cl2 Ir2 2.400(2) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Cl3 C53 Cl4 110.9(9) . . ? Cl3 C53 H53A 109.5 . . ? Cl4 C53 H53A 109.5 . . ? Cl3 C53 H53B 109.5 . . ? Cl4 C53 H53B 109.5 . . ? H53A C53 H53B 108.0 . . ? C2 N1 C4 95.6(6) . . ? C2 N1 C5 132.7(7) . . ? C4 N1 C5 131.5(6) . . ? C12 N2 C8 118.4(7) . . ? C12 N2 Ir1 118.3(5) . . ? C8 N2 Ir1 123.0(6) . . ? O1 C2 N1 130.8(9) . . ? O1 C2 C3 136.9(8) . . ? N1 C2 C3 92.3(8) . . ? C26 O2 C3 116.3(8) . . ? C36 N3 C40 119.3(7) . . ? C36 N3 Ir2 117.1(5) . . ? C40 N3 Ir2 123.6(6) . . ? O2 C3 C2 111.4(8) . . ? O2 C3 C4 117.6(7) . . ? C2 C3 C4 86.1(6) . . ? O2 C3 H3 113.0 . . ? C2 C3 H3 113.0 . . ? C4 C3 H3 113.0 . . ? N1 C4 C32 115.3(7) . . ? N1 C4 C3 85.6(6) . . ? C32 C4 C3 116.4(7) . . ? N1 C4 H4 112.3 . . ? C32 C4 H4 112.3 . . ? C3 C4 H4 112.3 . . ? C6 C5 C15 120.7(7) . . ? C6 C5 N1 119.8(7) . . ? C15 C5 N1 119.4(7) . . ? C5 C6 C7 121.6(7) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C13 117.1(7) . . ? C6 C7 Ir1 126.4(6) . . ? C13 C7 Ir1 116.4(5) . . ? N2 C8 C9 123.2(9) . . ? N2 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C8 C9 C10 116.7(8) . . ? C8 C9 H9 121.7 . . ? C10 C9 H9 121.7 . . ? C11 C10 C9 120.8(8) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.9(9) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? N2 C12 C11 120.0(7) . . ? N2 C12 C13 113.2(6) . . ? C11 C12 C13 126.8(8) . . ? C14 C13 C7 120.9(7) . . ? C14 C13 C12 124.7(7) . . ? C7 C13 C12 114.4(7) . . ? C13 C14 C15 120.0(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C5 C15 C14 119.6(8) . . ? C5 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C20 108.0 . . ? C17 C16 C21 126.2(12) . . ? C20 C16 C21 125.8(12) . . ? C17 C16 Ir1 72.5(3) . . ? C20 C16 Ir1 68.9(3) . . ? C21 C16 Ir1 124.2(10) . . ? C16 C17 C18 108.0 . . ? C16 C17 C22 125.5(11) . . ? C18 C17 C22 125.7(11) . . ? C16 C17 Ir1 70.6(3) . . ? C18 C17 Ir1 69.7(3) . . ? C22 C17 Ir1 133.4(8) . . ? C19 C18 C17 108.0 . . ? C19 C18 C23 114.2(11) . . ? C17 C18 C23 137.7(11) . . ? C19 C18 Ir1 69.0(3) . . ? C17 C18 Ir1 73.2(3) . . ? C23 C18 Ir1 123.6(9) . . ? C18 C19 C20 108.0 . . ? C18 C19 C24 131.5(10) . . ? C20 C19 C24 120.1(10) . . ? C18 C19 Ir1 73.1(3) . . ? C20 C19 Ir1 71.4(3) . . ? C24 C19 Ir1 126.3(8) . . ? C19 C20 C16 108.0 . . ? C19 C20 C25 118.3(9) . . ? C16 C20 C25 132.4(9) . . ? C19 C20 Ir1 70.3(3) . . ? C16 C20 Ir1 73.5(3) . . ? C25 C20 Ir1 131.2(7) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C33 C32 C42 121.0(8) . . ? C33 C32 C4 120.8(7) . . ? C42 C32 C4 118.1(7) . . ? C32 C33 C34 119.7(8) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.3(8) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C41 121.0(8) . . ? C34 C35 C36 123.7(8) . . ? C41 C35 C36 115.3(7) . . ? N3 C36 C37 119.5(7) . . ? N3 C36 C35 113.7(7) . . ? C37 C36 C35 126.8(8) . . ? C36 C37 C38 120.6(8) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 118.2(9) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C40 C39 C38 120.3(9) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 N3 122.1(9) . . ? C39 C40 H40 119.0 . . ? N3 C40 H40 119.0 . . ? C35 C41 C42 117.4(7) . . ? C35 C41 Ir2 116.6(6) . . ? C42 C41 Ir2 126.0(6) . . ? C41 C42 C32 120.4(7) . . ? C41 C42 H42 119.8 . . ? C32 C42 H42 119.8 . . ? C44 C43 C45 107.2(8) . . ? C44 C43 C49 128.0(10) . . ? C45 C43 C49 124.7(9) . . ? C44 C43 Ir2 71.3(5) . . ? C45 C43 Ir2 70.2(5) . . ? C49 C43 Ir2 126.3(6) . . ? C43 C44 C47 108.6(8) . . ? C43 C44 C48 125.8(10) . . ? C47 C44 C48 125.2(9) . . ? C43 C44 Ir2 70.6(5) . . ? C47 C44 Ir2 74.1(5) . . ? C48 C44 Ir2 127.4(6) . . ? C46 C45 C43 108.3(8) . . ? C46 C45 C50 123.0(9) . . ? C43 C45 C50 128.6(9) . . ? C46 C45 Ir2 74.9(5) . . ? C43 C45 Ir2 70.6(5) . . ? C50 C45 Ir2 123.8(7) . . ? C45 C46 C47 105.9(8) . . ? C45 C46 C51 126.8(9) . . ? C47 C46 C51 127.1(8) . . ? C45 C46 Ir2 66.6(4) . . ? C47 C46 Ir2 70.9(5) . . ? C51 C46 Ir2 130.2(7) . . ? C44 C47 C46 109.9(7) . . ? C44 C47 C52 124.5(8) . . ? C46 C47 C52 125.6(8) . . ? C44 C47 Ir2 68.2(4) . . ? C46 C47 Ir2 72.6(4) . . ? C52 C47 Ir2 124.8(6) . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C43 C49 H49A 109.5 . . ? C43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C7 Ir1 N2 77.6(3) . . ? C7 Ir1 C20 105.6(3) . . ? N2 Ir1 C20 163.8(3) . . ? C7 Ir1 C19 98.6(3) . . ? N2 Ir1 C19 125.9(3) . . ? C20 Ir1 C19 38.32(11) . . ? C7 Ir1 C16 139.7(3) . . ? N2 Ir1 C16 142.6(3) . . ? C20 Ir1 C16 37.61(11) . . ? C19 Ir1 C16 63.13(13) . . ? C7 Ir1 C18 125.4(4) . . ? N2 Ir1 C18 101.6(3) . . ? C20 Ir1 C18 63.28(14) . . ? C19 Ir1 C18 37.94(12) . . ? C16 Ir1 C18 62.31(14) . . ? C7 Ir1 C17 161.1(3) . . ? N2 Ir1 C17 109.7(3) . . ? C20 Ir1 C17 62.52(13) . . ? C19 Ir1 C17 62.73(14) . . ? C16 Ir1 C17 36.90(12) . . ? C18 Ir1 C17 37.07(11) . . ? C7 Ir1 Cl1 87.9(2) . . ? N2 Ir1 Cl1 84.24(19) . . ? C20 Ir1 Cl1 111.6(3) . . ? C19 Ir1 Cl1 149.9(3) . . ? C16 Ir1 Cl1 93.1(2) . . ? C18 Ir1 Cl1 146.6(3) . . ? C17 Ir1 Cl1 109.9(3) . . ? C41 Ir2 N3 77.2(3) . . ? C41 Ir2 C43 96.0(3) . . ? N3 Ir2 C43 130.4(3) . . ? C41 Ir2 C45 118.3(3) . . ? N3 Ir2 C45 101.2(3) . . ? C43 Ir2 C45 39.2(4) . . ? C41 Ir2 C44 109.6(3) . . ? N3 Ir2 C44 165.6(3) . . ? C43 Ir2 C44 38.2(3) . . ? C45 Ir2 C44 64.4(3) . . ? C41 Ir2 C47 146.2(3) . . ? N3 Ir2 C47 136.6(3) . . ? C43 Ir2 C47 63.2(3) . . ? C45 Ir2 C47 63.0(3) . . ? C44 Ir2 C47 37.7(3) . . ? C41 Ir2 C46 156.9(3) . . ? N3 Ir2 C46 105.4(3) . . ? C43 Ir2 C46 64.4(3) . . ? C45 Ir2 C46 38.6(3) . . ? C44 Ir2 C46 63.3(3) . . ? C47 Ir2 C46 36.6(3) . . ? C41 Ir2 Cl2 87.1(2) . . ? N3 Ir2 Cl2 86.30(18) . . ? C43 Ir2 Cl2 143.0(3) . . ? C45 Ir2 Cl2 154.4(2) . . ? C44 Ir2 Cl2 106.3(3) . . ? C47 Ir2 Cl2 94.7(2) . . ? C46 Ir2 Cl2 115.8(2) . . ? O2 C26 C27 125.1(8) . . ? O2 C26 C31 114.8(8) . . ? C27 C26 C31 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 C4 N1 C2 O1 175.3(12) . . . . ? C5 N1 C2 O1 -9.5(19) . . . . ? C4 N1 C2 C3 -5.6(8) . . . . ? C5 N1 C2 C3 169.5(9) . . . . ? C26 O2 C3 C2 174.4(7) . . . . ? C26 O2 C3 C4 -88.6(10) . . . . ? O1 C2 C3 O2 -57.7(17) . . . . ? N1 C2 C3 O2 123.3(8) . . . . ? O1 C2 C3 C4 -175.8(14) . . . . ? N1 C2 C3 C4 5.2(7) . . . . ? C2 N1 C4 C32 -111.8(8) . . . . ? C5 N1 C4 C32 73.0(11) . . . . ? C2 N1 C4 C3 5.3(7) . . . . ? C5 N1 C4 C3 -169.9(8) . . . . ? O2 C3 C4 N1 -117.0(8) . . . . ? C2 C3 C4 N1 -4.8(7) . . . . ? O2 C3 C4 C32 -0.9(12) . . . . ? C2 C3 C4 C32 111.3(8) . . . . ? C2 N1 C5 C6 14.0(14) . . . . ? C4 N1 C5 C6 -172.5(8) . . . . ? C2 N1 C5 C15 -164.1(9) . . . . ? C4 N1 C5 C15 9.4(13) . . . . ? C15 C5 C6 C7 1.9(13) . . . . ? N1 C5 C6 C7 -176.2(7) . . . . ? C5 C6 C7 C13 -3.6(12) . . . . ? C5 C6 C7 Ir1 179.5(6) . . . . ? C12 N2 C8 C9 2.6(13) . . . . ? Ir1 N2 C8 C9 176.5(7) . . . . ? N2 C8 C9 C10 -0.8(14) . . . . ? C8 C9 C10 C11 -1.6(15) . . . . ? C9 C10 C11 C12 2.2(15) . . . . ? C8 N2 C12 C11 -2.0(12) . . . . ? Ir1 N2 C12 C11 -176.1(6) . . . . ? C8 N2 C12 C13 177.5(7) . . . . ? Ir1 N2 C12 C13 3.3(9) . . . . ? C10 C11 C12 N2 -0.4(14) . . . . ? C10 C11 C12 C13 -179.8(9) . . . . ? C6 C7 C13 C14 2.9(12) . . . . ? Ir1 C7 C13 C14 -179.9(6) . . . . ? C6 C7 C13 C12 -177.8(7) . . . . ? Ir1 C7 C13 C12 -0.6(9) . . . . ? N2 C12 C13 C14 177.5(8) . . . . ? C11 C12 C13 C14 -3.0(14) . . . . ? N2 C12 C13 C7 -1.8(10) . . . . ? C11 C12 C13 C7 177.7(8) . . . . ? C7 C13 C14 C15 -0.4(13) . . . . ? C12 C13 C14 C15 -179.7(8) . . . . ? C6 C5 C15 C14 0.7(13) . . . . ? N1 C5 C15 C14 178.8(8) . . . . ? C13 C14 C15 C5 -1.4(13) . . . . ? C20 C16 C17 C18 0.0 . . . . ? C21 C16 C17 C18 179.9(14) . . . . ? Ir1 C16 C17 C18 60.0(3) . . . . ? C20 C16 C17 C22 169.9(10) . . . . ? C21 C16 C17 C22 -10.2(15) . . . . ? Ir1 C16 C17 C22 -130.1(10) . . . . ? C20 C16 C17 Ir1 -60.0(3) . . . . ? C21 C16 C17 Ir1 119.9(13) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C22 C17 C18 C19 -169.9(10) . . . . ? Ir1 C17 C18 C19 60.5(3) . . . . ? C16 C17 C18 C23 177.7(14) . . . . ? C22 C17 C18 C23 7.7(17) . . . . ? Ir1 C17 C18 C23 -121.8(14) . . . . ? C16 C17 C18 Ir1 -60.5(3) . . . . ? C22 C17 C18 Ir1 129.5(10) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C23 C18 C19 C20 -178.3(11) . . . . ? Ir1 C18 C19 C20 63.2(3) . . . . ? C17 C18 C19 C24 172.9(12) . . . . ? C23 C18 C19 C24 -5.4(14) . . . . ? Ir1 C18 C19 C24 -123.9(11) . . . . ? C17 C18 C19 Ir1 -63.2(3) . . . . ? C23 C18 C19 Ir1 118.5(10) . . . . ? C18 C19 C20 C16 0.0 . . . . ? C24 C19 C20 C16 -173.9(10) . . . . ? Ir1 C19 C20 C16 64.4(3) . . . . ? C18 C19 C20 C25 168.6(9) . . . . ? C24 C19 C20 C25 -5.2(12) . . . . ? Ir1 C19 C20 C25 -127.0(8) . . . . ? C18 C19 C20 Ir1 -64.4(3) . . . . ? C24 C19 C20 Ir1 121.8(9) . . . . ? C17 C16 C20 C19 0.0 . . . . ? C21 C16 C20 C19 -179.9(13) . . . . ? Ir1 C16 C20 C19 -62.3(3) . . . . ? C17 C16 C20 C25 -166.4(11) . . . . ? C21 C16 C20 C25 13.7(16) . . . . ? Ir1 C16 C20 C25 131.3(10) . . . . ? C17 C16 C20 Ir1 62.3(3) . . . . ? C21 C16 C20 Ir1 -117.6(13) . . . . ? N1 C4 C32 C33 37.6(10) . . . . ? C3 C4 C32 C33 -60.4(10) . . . . ? N1 C4 C32 C42 -145.1(7) . . . . ? C3 C4 C32 C42 116.9(8) . . . . ? C42 C32 C33 C34 -0.6(12) . . . . ? C4 C32 C33 C34 176.7(7) . . . . ? C32 C33 C34 C35 -2.0(12) . . . . ? C33 C34 C35 C41 1.8(12) . . . . ? C33 C34 C35 C36 -179.3(7) . . . . ? C40 N3 C36 C37 -0.1(11) . . . . ? Ir2 N3 C36 C37 177.5(6) . . . . ? C40 N3 C36 C35 178.5(7) . . . . ? Ir2 N3 C36 C35 -3.9(8) . . . . ? C34 C35 C36 N3 -177.0(7) . . . . ? C41 C35 C36 N3 2.0(10) . . . . ? C34 C35 C36 C37 1.5(13) . . . . ? C41 C35 C36 C37 -179.5(8) . . . . ? N3 C36 C37 C38 -1.6(13) . . . . ? C35 C36 C37 C38 -179.9(8) . . . . ? C36 C37 C38 C39 1.4(14) . . . . ? C37 C38 C39 C40 0.3(16) . . . . ? C38 C39 C40 N3 -2.0(16) . . . . ? C36 N3 C40 C39 1.9(13) . . . . ? Ir2 N3 C40 C39 -175.6(8) . . . . ? C34 C35 C41 C42 0.8(11) . . . . ? C36 C35 C41 C42 -178.2(6) . . . . ? C34 C35 C41 Ir2 179.8(6) . . . . ? C36 C35 C41 Ir2 0.8(9) . . . . ? C35 C41 C42 C32 -3.3(10) . . . . ? Ir2 C41 C42 C32 177.8(5) . . . . ? C33 C32 C42 C41 3.2(11) . . . . ? C4 C32 C42 C41 -174.1(6) . . . . ? C45 C43 C44 C47 3.4(9) . . . . ? C49 C43 C44 C47 -173.3(9) . . . . ? Ir2 C43 C44 C47 64.8(6) . . . . ? C45 C43 C44 C48 176.0(8) . . . . ? C49 C43 C44 C48 -0.8(14) . . . . ? Ir2 C43 C44 C48 -122.7(8) . . . . ? C45 C43 C44 Ir2 -61.4(6) . . . . ? C49 C43 C44 Ir2 121.9(9) . . . . ? C44 C43 C45 C46 -3.8(9) . . . . ? C49 C43 C45 C46 173.0(8) . . . . ? Ir2 C43 C45 C46 -65.9(6) . . . . ? C44 C43 C45 C50 -179.7(9) . . . . ? C49 C43 C45 C50 -2.8(15) . . . . ? Ir2 C43 C45 C50 118.2(10) . . . . ? C44 C43 C45 Ir2 62.1(6) . . . . ? C49 C43 C45 Ir2 -121.1(9) . . . . ? C43 C45 C46 C47 2.8(9) . . . . ? C50 C45 C46 C47 178.9(9) . . . . ? Ir2 C45 C46 C47 -60.3(6) . . . . ? C43 C45 C46 C51 -173.2(9) . . . . ? C50 C45 C46 C51 2.9(15) . . . . ? Ir2 C45 C46 C51 123.7(9) . . . . ? C43 C45 C46 Ir2 63.1(6) . . . . ? C50 C45 C46 Ir2 -120.8(9) . . . . ? C43 C44 C47 C46 -1.7(9) . . . . ? C48 C44 C47 C46 -174.3(8) . . . . ? Ir2 C44 C47 C46 60.8(6) . . . . ? C43 C44 C47 C52 179.4(8) . . . . ? C48 C44 C47 C52 6.8(14) . . . . ? Ir2 C44 C47 C52 -118.1(8) . . . . ? C43 C44 C47 Ir2 -62.5(6) . . . . ? C48 C44 C47 Ir2 124.9(9) . . . . ? C45 C46 C47 C44 -0.7(9) . . . . ? C51 C46 C47 C44 175.3(9) . . . . ? Ir2 C46 C47 C44 -58.2(6) . . . . ? C45 C46 C47 C52 178.2(8) . . . . ? C51 C46 C47 C52 -5.8(14) . . . . ? Ir2 C46 C47 C52 120.7(9) . . . . ? C45 C46 C47 Ir2 57.5(6) . . . . ? C51 C46 C47 Ir2 -126.5(9) . . . . ? C6 C7 Ir1 N2 178.7(8) . . . . ? C13 C7 Ir1 N2 1.7(6) . . . . ? C6 C7 Ir1 C20 -17.7(8) . . . . ? C13 C7 Ir1 C20 165.3(6) . . . . ? C6 C7 Ir1 C19 -56.3(8) . . . . ? C13 C7 Ir1 C19 126.7(6) . . . . ? C6 C7 Ir1 C16 1.8(10) . . . . ? C13 C7 Ir1 C16 -175.1(5) . . . . ? C6 C7 Ir1 C18 -85.8(7) . . . . ? C13 C7 Ir1 C18 97.3(6) . . . . ? C6 C7 Ir1 C17 -66.3(13) . . . . ? C13 C7 Ir1 C17 116.7(10) . . . . ? C6 C7 Ir1 Cl1 94.1(7) . . . . ? C13 C7 Ir1 Cl1 -82.8(6) . . . . ? C12 N2 Ir1 C7 -2.9(6) . . . . ? C8 N2 Ir1 C7 -176.8(7) . . . . ? C12 N2 Ir1 C20 -106.3(11) . . . . ? C8 N2 Ir1 C20 79.8(13) . . . . ? C12 N2 Ir1 C19 -94.7(6) . . . . ? C8 N2 Ir1 C19 91.4(7) . . . . ? C12 N2 Ir1 C16 173.8(5) . . . . ? C8 N2 Ir1 C16 -0.1(9) . . . . ? C12 N2 Ir1 C18 -127.0(6) . . . . ? C8 N2 Ir1 C18 59.1(7) . . . . ? C12 N2 Ir1 C17 -164.7(6) . . . . ? C8 N2 Ir1 C17 21.4(8) . . . . ? C12 N2 Ir1 Cl1 86.3(6) . . . . ? C8 N2 Ir1 Cl1 -87.6(6) . . . . ? C19 C20 Ir1 C7 -84.1(4) . . . . ? C16 C20 Ir1 C7 159.2(4) . . . . ? C25 C20 Ir1 C7 26.8(11) . . . . ? C19 C20 Ir1 N2 15.3(13) . . . . ? C16 C20 Ir1 N2 -101.4(13) . . . . ? C25 C20 Ir1 N2 126.2(11) . . . . ? C16 C20 Ir1 C19 -116.61(15) . . . . ? C25 C20 Ir1 C19 110.9(13) . . . . ? C19 C20 Ir1 C16 116.61(15) . . . . ? C25 C20 Ir1 C16 -132.5(13) . . . . ? C19 C20 Ir1 C18 38.09(13) . . . . ? C16 C20 Ir1 C18 -78.52(18) . . . . ? C25 C20 Ir1 C18 149.0(13) . . . . ? C19 C20 Ir1 C17 79.92(18) . . . . ? C16 C20 Ir1 C17 -36.69(13) . . . . ? C25 C20 Ir1 C17 -169.2(13) . . . . ? C19 C20 Ir1 Cl1 -178.2(4) . . . . ? C16 C20 Ir1 Cl1 65.2(4) . . . . ? C25 C20 Ir1 Cl1 -67.2(11) . . . . ? C18 C19 Ir1 C7 -139.4(4) . . . . ? C20 C19 Ir1 C7 104.3(4) . . . . ? C24 C19 Ir1 C7 -9.9(11) . . . . ? C18 C19 Ir1 N2 -58.5(4) . . . . ? C20 C19 Ir1 N2 -174.8(4) . . . . ? C24 C19 Ir1 N2 71.1(11) . . . . ? C18 C19 Ir1 C20 116.33(16) . . . . ? C24 C19 Ir1 C20 -114.2(13) . . . . ? C18 C19 Ir1 C16 78.62(17) . . . . ? C20 C19 Ir1 C16 -37.71(11) . . . . ? C24 C19 Ir1 C16 -151.9(13) . . . . ? C20 C19 Ir1 C18 -116.33(16) . . . . ? C24 C19 Ir1 C18 129.5(13) . . . . ? C18 C19 Ir1 C17 36.98(11) . . . . ? C20 C19 Ir1 C17 -79.35(18) . . . . ? C24 C19 Ir1 C17 166.5(13) . . . . ? C18 C19 Ir1 Cl1 119.7(7) . . . . ? C20 C19 Ir1 Cl1 3.4(7) . . . . ? C24 C19 Ir1 Cl1 -110.7(10) . . . . ? C17 C16 Ir1 C7 -149.9(6) . . . . ? C20 C16 Ir1 C7 -31.9(6) . . . . ? C21 C16 Ir1 C7 87.8(13) . . . . ? C17 C16 Ir1 N2 35.2(5) . . . . ? C20 C16 Ir1 N2 153.2(5) . . . . ? C21 C16 Ir1 N2 -87.1(14) . . . . ? C17 C16 Ir1 C20 -118.01(17) . . . . ? C21 C16 Ir1 C20 119.7(15) . . . . ? C17 C16 Ir1 C19 -79.59(19) . . . . ? C20 C16 Ir1 C19 38.42(13) . . . . ? C21 C16 Ir1 C19 158.1(15) . . . . ? C17 C16 Ir1 C18 -36.70(12) . . . . ? C20 C16 Ir1 C18 81.3(2) . . . . ? C21 C16 Ir1 C18 -159.0(15) . . . . ? C20 C16 Ir1 C17 118.01(17) . . . . ? C21 C16 Ir1 C17 -122.3(15) . . . . ? C17 C16 Ir1 Cl1 119.7(4) . . . . ? C20 C16 Ir1 Cl1 -122.3(4) . . . . ? C21 C16 Ir1 Cl1 -2.6(13) . . . . ? C19 C18 Ir1 C7 52.2(4) . . . . ? C17 C18 Ir1 C7 169.7(4) . . . . ? C23 C18 Ir1 C7 -53.7(12) . . . . ? C19 C18 Ir1 N2 135.2(4) . . . . ? C17 C18 Ir1 N2 -107.3(4) . . . . ? C23 C18 Ir1 N2 29.3(12) . . . . ? C19 C18 Ir1 C20 -38.48(13) . . . . ? C17 C18 Ir1 C20 79.0(2) . . . . ? C23 C18 Ir1 C20 -144.3(13) . . . . ? C17 C18 Ir1 C19 117.49(15) . . . . ? C23 C18 Ir1 C19 -105.8(13) . . . . ? C19 C18 Ir1 C16 -80.97(17) . . . . ? C17 C18 Ir1 C16 36.53(13) . . . . ? C23 C18 Ir1 C16 173.2(13) . . . . ? C19 C18 Ir1 C17 -117.49(15) . . . . ? C23 C18 Ir1 C17 136.7(14) . . . . ? C19 C18 Ir1 Cl1 -127.6(6) . . . . ? C17 C18 Ir1 Cl1 -10.1(6) . . . . ? C23 C18 Ir1 Cl1 126.6(11) . . . . ? C16 C17 Ir1 C7 91.9(12) . . . . ? C18 C17 Ir1 C7 -26.7(12) . . . . ? C22 C17 Ir1 C7 -147.1(10) . . . . ? C16 C17 Ir1 N2 -158.2(4) . . . . ? C18 C17 Ir1 N2 83.2(4) . . . . ? C22 C17 Ir1 N2 -37.2(14) . . . . ? C16 C17 Ir1 C20 37.40(13) . . . . ? C18 C17 Ir1 C20 -81.2(2) . . . . ? C22 C17 Ir1 C20 158.4(15) . . . . ? C16 C17 Ir1 C19 80.78(18) . . . . ? C18 C17 Ir1 C19 -37.85(14) . . . . ? C22 C17 Ir1 C19 -158.2(15) . . . . ? C18 C17 Ir1 C16 -118.62(16) . . . . ? C22 C17 Ir1 C16 121.0(15) . . . . ? C16 C17 Ir1 C18 118.62(16) . . . . ? C22 C17 Ir1 C18 -120.4(15) . . . . ? C16 C17 Ir1 Cl1 -67.3(3) . . . . ? C18 C17 Ir1 Cl1 174.1(4) . . . . ? C22 C17 Ir1 Cl1 53.7(13) . . . . ? C35 C41 Ir2 N3 -2.1(5) . . . . ? C42 C41 Ir2 N3 176.8(7) . . . . ? C35 C41 Ir2 C43 128.0(6) . . . . ? C42 C41 Ir2 C43 -53.1(7) . . . . ? C35 C41 Ir2 C45 93.8(6) . . . . ? C42 C41 Ir2 C45 -87.2(7) . . . . ? C35 C41 Ir2 C44 164.7(5) . . . . ? C42 C41 Ir2 C44 -16.4(7) . . . . ? C35 C41 Ir2 C47 176.8(5) . . . . ? C42 C41 Ir2 C47 -4.2(9) . . . . ? C35 C41 Ir2 C46 97.1(9) . . . . ? C42 C41 Ir2 C46 -84.0(10) . . . . ? C35 C41 Ir2 Cl2 -89.0(5) . . . . ? C42 C41 Ir2 Cl2 89.9(6) . . . . ? C36 N3 Ir2 C41 3.3(5) . . . . ? C40 N3 Ir2 C41 -179.2(7) . . . . ? C36 N3 Ir2 C43 -83.7(7) . . . . ? C40 N3 Ir2 C43 93.8(7) . . . . ? C36 N3 Ir2 C45 -113.5(6) . . . . ? C40 N3 Ir2 C45 64.0(7) . . . . ? C36 N3 Ir2 C44 -116.7(13) . . . . ? C40 N3 Ir2 C44 60.8(15) . . . . ? C36 N3 Ir2 C47 -175.8(5) . . . . ? C40 N3 Ir2 C47 1.7(8) . . . . ? C36 N3 Ir2 C46 -153.0(5) . . . . ? C40 N3 Ir2 C46 24.6(7) . . . . ? C36 N3 Ir2 Cl2 91.2(5) . . . . ? C40 N3 Ir2 Cl2 -91.3(6) . . . . ? C44 C43 Ir2 C41 114.3(5) . . . . ? C45 C43 Ir2 C41 -128.7(5) . . . . ? C49 C43 Ir2 C41 -9.6(10) . . . . ? C44 C43 Ir2 N3 -167.4(5) . . . . ? C45 C43 Ir2 N3 -50.4(6) . . . . ? C49 C43 Ir2 N3 68.7(11) . . . . ? C44 C43 Ir2 C45 -116.9(7) . . . . ? C49 C43 Ir2 C45 119.2(11) . . . . ? C45 C43 Ir2 C44 116.9(7) . . . . ? C49 C43 Ir2 C44 -123.9(12) . . . . ? C44 C43 Ir2 C47 -37.7(5) . . . . ? C45 C43 Ir2 C47 79.3(5) . . . . ? C49 C43 Ir2 C47 -161.6(11) . . . . ? C44 C43 Ir2 C46 -78.6(6) . . . . ? C45 C43 Ir2 C46 38.4(5) . . . . ? C49 C43 Ir2 C46 157.5(11) . . . . ? C44 C43 Ir2 Cl2 21.1(8) . . . . ? C45 C43 Ir2 Cl2 138.0(5) . . . . ? C49 C43 Ir2 Cl2 -102.8(9) . . . . ? C46 C45 Ir2 C41 178.0(5) . . . . ? C43 C45 Ir2 C41 61.8(6) . . . . ? C50 C45 Ir2 C41 -62.2(10) . . . . ? C46 C45 Ir2 N3 -100.6(5) . . . . ? C43 C45 Ir2 N3 143.2(5) . . . . ? C50 C45 Ir2 N3 19.2(9) . . . . ? C46 C45 Ir2 C43 116.1(7) . . . . ? C50 C45 Ir2 C43 -124.0(11) . . . . ? C46 C45 Ir2 C44 78.5(6) . . . . ? C43 C45 Ir2 C44 -37.6(5) . . . . ? C50 C45 Ir2 C44 -161.7(10) . . . . ? C46 C45 Ir2 C47 36.2(5) . . . . ? C43 C45 Ir2 C47 -79.9(5) . . . . ? C50 C45 Ir2 C47 156.1(10) . . . . ? C43 C45 Ir2 C46 -116.1(7) . . . . ? C50 C45 Ir2 C46 119.9(12) . . . . ? C46 C45 Ir2 Cl2 4.5(10) . . . . ? C43 C45 Ir2 Cl2 -111.6(7) . . . . ? C50 C45 Ir2 Cl2 124.4(8) . . . . ? C43 C44 Ir2 C41 -74.2(6) . . . . ? C47 C44 Ir2 C41 169.0(4) . . . . ? C48 C44 Ir2 C41 46.5(10) . . . . ? C43 C44 Ir2 N3 42.2(15) . . . . ? C47 C44 Ir2 N3 -74.7(14) . . . . ? C48 C44 Ir2 N3 162.9(10) . . . . ? C47 C44 Ir2 C43 -116.9(7) . . . . ? C48 C44 Ir2 C43 120.7(12) . . . . ? C43 C44 Ir2 C45 38.7(5) . . . . ? C47 C44 Ir2 C45 -78.2(5) . . . . ? C48 C44 Ir2 C45 159.4(10) . . . . ? C43 C44 Ir2 C47 116.9(7) . . . . ? C48 C44 Ir2 C47 -122.4(11) . . . . ? C43 C44 Ir2 C46 81.9(6) . . . . ? C47 C44 Ir2 C46 -35.0(5) . . . . ? C48 C44 Ir2 C46 -157.4(10) . . . . ? C43 C44 Ir2 Cl2 -167.0(5) . . . . ? C47 C44 Ir2 Cl2 76.1(5) . . . . ? C48 C44 Ir2 Cl2 -46.3(10) . . . . ? C44 C47 Ir2 C41 -18.9(8) . . . . ? C46 C47 Ir2 C41 -139.5(6) . . . . ? C52 C47 Ir2 C41 98.8(9) . . . . ? C44 C47 Ir2 N3 159.6(5) . . . . ? C46 C47 Ir2 N3 39.0(7) . . . . ? C52 C47 Ir2 N3 -82.6(9) . . . . ? C44 C47 Ir2 C43 38.1(5) . . . . ? C46 C47 Ir2 C43 -82.5(6) . . . . ? C52 C47 Ir2 C43 155.9(9) . . . . ? C44 C47 Ir2 C45 82.4(6) . . . . ? C46 C47 Ir2 C45 -38.2(5) . . . . ? C52 C47 Ir2 C45 -159.8(9) . . . . ? C46 C47 Ir2 C44 -120.6(7) . . . . ? C52 C47 Ir2 C44 117.8(10) . . . . ? C44 C47 Ir2 C46 120.6(7) . . . . ? C52 C47 Ir2 C46 -121.6(10) . . . . ? C44 C47 Ir2 Cl2 -110.8(5) . . . . ? C46 C47 Ir2 Cl2 128.6(5) . . . . ? C52 C47 Ir2 Cl2 7.0(8) . . . . ? C45 C46 Ir2 C41 -4.6(11) . . . . ? C47 C46 Ir2 C41 113.3(9) . . . . ? C51 C46 Ir2 C41 -123.8(10) . . . . ? C45 C46 Ir2 N3 88.8(6) . . . . ? C47 C46 Ir2 N3 -153.4(5) . . . . ? C51 C46 Ir2 N3 -30.4(9) . . . . ? C45 C46 Ir2 C43 -39.0(5) . . . . ? C47 C46 Ir2 C43 78.8(6) . . . . ? C51 C46 Ir2 C43 -158.2(10) . . . . ? C47 C46 Ir2 C45 117.9(8) . . . . ? C51 C46 Ir2 C45 -119.2(11) . . . . ? C45 C46 Ir2 C44 -81.7(6) . . . . ? C47 C46 Ir2 C44 36.1(5) . . . . ? C51 C46 Ir2 C44 159.0(10) . . . . ? C45 C46 Ir2 C47 -117.9(8) . . . . ? C51 C46 Ir2 C47 122.9(11) . . . . ? C45 C46 Ir2 Cl2 -177.8(5) . . . . ? C47 C46 Ir2 Cl2 -60.0(5) . . . . ? C51 C46 Ir2 Cl2 63.0(9) . . . . ? C3 O2 C26 C27 -18.3(11) . . . . ? C3 O2 C26 C31 165.9(7) . . . . ? O2 C26 C27 C28 -175.6(9) . . . . ? C31 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C26 0.0 . . . . ? O2 C26 C31 C30 176.0(8) . . . . ? C27 C26 C31 C30 0.0 . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 671 248 ' ' 2 0.500 0.500 0.500 672 249 ' ' _platon_squeeze_details ; The final refinement show high values of residual non-modelled electronic density.Therefore, the SQUEEZE/PLATON program was used to remove its contribution to the overal intensity data.An improvement was observed in all refinement parameters and residual when this procedure is applied. ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.783 _refine_diff_density_min -1.475 _refine_diff_density_rms 0.150 #========================================================================END _database_code_depnum_ccdc_archive 'CCDC 944672'