# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Adam Veige' _publ_contact_author_email VEIGE@CHEM.UFL.EDU _publ_section_title ; New iridium and rhodium chiral di-N-heterocyclic carbene (NHC) complexes and their application in enantioselective catalysis. ; loop_ _publ_author_name 'Adam Veige' 'Khalil Abboud' 'Ion Ghiviriga' 'Muhammed T. Jan' 'Matthew S. Jeletic' # Attachment 'mj25.cif' data_mj25 _database_code_depnum_ccdc_archive 'CCDC 707708' _audit_update_record ; 2008-06-30 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C119 H117 Cl6 F6 Ir2 N8 O6 S2' _chemical_formula_weight 2530.43 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 13.2280(13) _cell_length_b 20.306(2) _cell_length_c 18.9627(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.224(2) _cell_angle_gamma 90.00 _cell_volume 5053.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 114 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2554 _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7405 _exptl_absorpt_correction_T_max 0.9442 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)' _diffrn_ambient_temperature 173(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 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 34294 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19094 _reflns_number_gt 15086 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.14 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The asymmetric unit consists of two Ir complex cations, two triflate anions, two toluene solvent molecules and two chloroform solvent molecules. The solvent molecules were disordered and could not be modeled properly, thus program SQUEEZE, a part of the PLATON package of crystallographic software, was used to calculate the solvent disorder area and remove its contribution to the overall intensity data. Space group P2/n was checked to confirm the correct space group. The complexes can be clearly seen to not be related by a two-fold rotation symmetry or an inversion center. Thus the correct space group is the reported one, Pn. ; _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^)+(0.0454P)] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(7) _refine_ls_number_reflns 19094 _refine_ls_number_parameters 1064 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.80990(2) 0.700869(19) 0.625431(18) 0.02813(9) Uani 1 1 d . . . Ir2 Ir 0.85666(2) 0.102571(18) 0.656430(18) 0.02467(9) Uani 1 1 d . . . N1 N 0.6115(6) 0.6244(4) 0.6029(4) 0.0276(18) Uani 1 1 d . . . N2 N 0.6870(6) 0.6200(4) 0.5088(4) 0.0310(18) Uani 1 1 d . . . N3 N 0.6793(5) 0.8173(4) 0.5562(4) 0.032(2) Uani 1 1 d . . . N4 N 0.8304(6) 0.8166(4) 0.5204(4) 0.0321(19) Uani 1 1 d . . . N5 N 0.6593(5) 0.1183(4) 0.5552(4) 0.0288(18) Uani 1 1 d . . . N6 N 0.7893(5) 0.1418(4) 0.5009(4) 0.0291(19) Uani 1 1 d . . . N7 N 0.8322(5) 0.2491(4) 0.6938(4) 0.0277(17) Uani 1 1 d . . . N8 N 0.9917(5) 0.2252(4) 0.6944(4) 0.0242(17) Uani 1 1 d . . . O1 O 0.4140(7) 0.5464(6) 0.7643(7) 0.097(4) Uani 1 1 d . . . F1 F 0.306(1) 0.5737(5) 0.8831(5) 0.129(4) Uani 1 1 d . . . S1 S 0.3069(2) 0.54488(17) 0.74822(18) 0.0536(8) Uani 1 1 d . . . O2 O 0.2666(9) 0.5815(7) 0.6885(6) 0.117(5) Uani 1 1 d . . . F2 F 0.2799(9) 0.6540(4) 0.8171(6) 0.122(4) Uani 1 1 d . . . O3 O 0.2616(8) 0.4832(5) 0.7518(6) 0.085(3) Uani 1 1 d . . . F3 F 0.1657(7) 0.5824(5) 0.8233(6) 0.117(4) Uani 1 1 d . . . C93 C 0.2630(9) 0.5907(6) 0.8203(6) 0.050(3) Uani 1 1 d . . . S2 S 0.25082(17) 0.07431(14) 0.55432(13) 0.0307(5) Uani 1 1 d . . . O4 O 0.1491(5) 0.0789(4) 0.5158(5) 0.051(2) Uani 1 1 d . . . F4 F 0.3093(5) 0.0156(4) 0.4435(3) 0.0638(19) Uani 1 1 d . . . O5 O 0.3188(5) 0.1277(4) 0.5410(4) 0.0407(17) Uani 1 1 d . . . F5 F 0.2488(6) -0.0506(3) 0.5174(4) 0.0578(18) Uani 1 1 d . . . O6 O 0.2553(5) 0.0563(3) 0.6279(3) 0.0387(16) Uani 1 1 d . . . F6 F 0.3995(5) -0.0083(4) 0.5428(4) 0.066(2) Uani 1 1 d . . . C94 C 0.3030(8) 0.0030(6) 0.5129(6) 0.047(3) Uani 1 1 d . . . C1 C 0.6059(6) 0.8012(5) 0.7820(5) 0.036(2) Uani 1 1 d . . . C2 C 0.6801(7) 0.8266(7) 0.8323(6) 0.055(3) Uani 1 1 d . . . H2A H 0.7157 0.8657 0.8229 0.066 Uiso 1 1 calc R . . C3 C 0.7021(8) 0.7934(8) 0.8984(6) 0.063(4) Uani 1 1 d . . . H3A H 0.7513 0.8110 0.9342 0.076 Uiso 1 1 calc R . . C4 C 0.6534(7) 0.7369(7) 0.9105(6) 0.054(3) Uani 1 1 d . . . H4A H 0.6708 0.7139 0.9539 0.065 Uiso 1 1 calc R . . C5 C 0.5779(7) 0.7122(6) 0.8597(5) 0.041(3) Uani 1 1 d . . . H5A H 0.5421 0.6735 0.8698 0.049 Uiso 1 1 calc R . . C6 C 0.5545(7) 0.7425(5) 0.7963(5) 0.036(2) Uani 1 1 d . . . C7 C 0.4590(6) 0.8383(5) 0.7011(4) 0.028(2) Uani 1 1 d . . . C8 C 0.4086(9) 0.8964(5) 0.6828(5) 0.041(2) Uani 1 1 d . . . H8A H 0.4457 0.9346 0.6729 0.049 Uiso 1 1 calc R . . C9 C 0.3038(8) 0.8987(5) 0.6791(7) 0.047(3) Uani 1 1 d . . . H9A H 0.2684 0.9382 0.6650 0.056 Uiso 1 1 calc R . . C10 C 0.2505(6) 0.8438(5) 0.6958(5) 0.034(2) Uani 1 1 d . . . H10G H 0.1786 0.8464 0.6947 0.041 Uiso 1 1 calc R . . C11 C 0.3004(6) 0.7839(5) 0.7144(5) 0.027(2) Uani 1 1 d . . . H11A H 0.2624 0.7458 0.7237 0.033 Uiso 1 1 calc R . . C12 C 0.4043(6) 0.7813(5) 0.7188(5) 0.029(2) Uani 1 1 d . . . C13 C 0.5737(7) 0.8264(5) 0.7072(5) 0.033(2) Uani 1 1 d . . . H13E H 0.6113 0.8674 0.6974 0.040 Uiso 1 1 calc R . . C14 C 0.4737(6) 0.7220(5) 0.7368(4) 0.0208(18) Uani 1 1 d . . . H14A H 0.4349 0.6824 0.7496 0.025 Uiso 1 1 calc R . . C15 C 0.5944(6) 0.7706(4) 0.6564(4) 0.0231(18) Uani 1 1 d . . . H15A H 0.6663 0.7560 0.6704 0.028 Uiso 1 1 calc R . . C16 C 0.5250(6) 0.7110(4) 0.6684(5) 0.026(2) Uani 1 1 d . . . H16A H 0.4698 0.7091 0.6273 0.032 Uiso 1 1 calc R . . C17 C 0.5812(7) 0.6441(5) 0.6722(5) 0.034(2) Uani 1 1 d . . . H17D H 0.6428 0.6471 0.7076 0.041 Uiso 1 1 calc R . . H17E H 0.5363 0.6098 0.6885 0.041 Uiso 1 1 calc R . . C18 C 0.5493(7) 0.5867(5) 0.5549(6) 0.034(2) Uani 1 1 d . . . C19 C 0.4570(7) 0.5544(5) 0.5603(6) 0.040(2) Uani 1 1 d . . . H19D H 0.4230 0.5585 0.6014 0.048 Uiso 1 1 calc R . . C20 C 0.4182(8) 0.5165(6) 0.5034(7) 0.052(3) Uani 1 1 d . . . H20C H 0.3562 0.4933 0.5054 0.062 Uiso 1 1 calc R . . C21 C 0.4667(9) 0.5112(6) 0.4438(7) 0.061(3) Uani 1 1 d . . . H21A H 0.4365 0.4844 0.4058 0.074 Uiso 1 1 calc R . . C22 C 0.5592(9) 0.5435(6) 0.4360(6) 0.050(3) Uani 1 1 d . . . H22A H 0.5922 0.5398 0.3945 0.060 Uiso 1 1 calc R . . C23 C 0.5971(7) 0.5809(5) 0.4940(5) 0.033(2) Uani 1 1 d . . . C24 C 0.6943(7) 0.6448(5) 0.5735(5) 0.029(2) Uani 1 1 d . . . C25 C 0.7618(8) 0.6334(6) 0.4571(5) 0.047(3) Uani 1 1 d . . . H25A H 0.8162 0.6626 0.4815 0.056 Uiso 1 1 calc R . . C26 C 0.7058(9) 0.6724(7) 0.3940(6) 0.062(4) Uani 1 1 d . . . H26B H 0.7534 0.6822 0.3597 0.093 Uiso 1 1 calc R . . H26C H 0.6795 0.7136 0.4114 0.093 Uiso 1 1 calc R . . H26D H 0.6491 0.6460 0.3708 0.093 Uiso 1 1 calc R . . C27 C 0.8114(10) 0.5727(7) 0.4361(8) 0.075(4) Uani 1 1 d . . . H27D H 0.8460 0.5509 0.4785 0.113 Uiso 1 1 calc R . . H27E H 0.8614 0.5838 0.4039 0.113 Uiso 1 1 calc R . . H27F H 0.7599 0.5431 0.4118 0.113 Uiso 1 1 calc R . . C28 C 0.5857(6) 0.7899(5) 0.5790(5) 0.029(2) Uani 1 1 d . . . H28A H 0.5655 0.7506 0.5497 0.034 Uiso 1 1 calc R . . H28B H 0.5306 0.8229 0.5694 0.034 Uiso 1 1 calc R . . C29 C 0.6823(6) 0.8686(5) 0.5110(5) 0.031(2) Uani 1 1 d . . . C30 C 0.6080(7) 0.9167(5) 0.4888(6) 0.039(2) Uani 1 1 d . . . H30B H 0.5434 0.9168 0.5058 0.047 Uiso 1 1 calc R . . C31 C 0.6340(8) 0.9644(6) 0.4404(6) 0.051(3) Uani 1 1 d . . . H31B H 0.5853 0.9966 0.4225 0.061 Uiso 1 1 calc R . . C32 C 0.7308(8) 0.9648(6) 0.4181(6) 0.051(3) Uani 1 1 d . . . H32A H 0.7477 0.9989 0.3874 0.062 Uiso 1 1 calc R . . C33 C 0.8027(8) 0.9172(6) 0.4394(5) 0.050(3) Uani 1 1 d . . . H33B H 0.8670 0.9167 0.4220 0.060 Uiso 1 1 calc R . . C34 C 0.7774(7) 0.8700(5) 0.4873(5) 0.035(2) Uani 1 1 d . . . C35 C 0.7713(6) 0.7837(5) 0.5633(5) 0.027(2) Uani 1 1 d . . . C36 C 0.9333(7) 0.7950(6) 0.5082(5) 0.041(3) Uani 1 1 d . . . H36A H 0.9508 0.7546 0.5373 0.049 Uiso 1 1 calc R . . C37 C 1.0142(8) 0.8474(6) 0.5308(7) 0.058(3) Uani 1 1 d . . . H37B H 1.0122 0.8590 0.5807 0.086 Uiso 1 1 calc R . . H37C H 1.0005 0.8867 0.5011 0.086 Uiso 1 1 calc R . . H37D H 1.0818 0.8301 0.5248 0.086 Uiso 1 1 calc R . . C38 C 0.9350(9) 0.7774(6) 0.4302(6) 0.054(3) Uani 1 1 d . . . H38D H 0.8818 0.7447 0.4157 0.081 Uiso 1 1 calc R . . H38E H 1.0017 0.7590 0.4238 0.081 Uiso 1 1 calc R . . H38F H 0.9224 0.8170 0.4010 0.081 Uiso 1 1 calc R . . C39 C 0.9077(8) 0.6152(5) 0.6397(6) 0.043(3) Uani 1 1 d . . . H39A H 0.8877 0.5803 0.6033 0.052 Uiso 1 1 calc R . . C40 C 0.8469(8) 0.6140(6) 0.6957(6) 0.044(3) Uani 1 1 d . . . H40A H 0.7935 0.5788 0.6919 0.053 Uiso 1 1 calc R . . C41 C 0.8886(8) 0.6337(6) 0.7712(6) 0.050(3) Uani 1 1 d . . . H41D H 0.9630 0.6256 0.7791 0.059 Uiso 1 1 calc R . . H41E H 0.8563 0.6064 0.8054 0.059 Uiso 1 1 calc R . . C42 C 0.8675(8) 0.7064(6) 0.7838(6) 0.047(3) Uani 1 1 d . . . H42A H 0.7981 0.7104 0.7979 0.057 Uiso 1 1 calc R . . H42B H 0.9162 0.7220 0.8244 0.057 Uiso 1 1 calc R . . C43 C 0.8750(6) 0.7511(5) 0.7217(5) 0.032(2) Uani 1 1 d . . . H43B H 0.8449 0.7957 0.7274 0.038 Uiso 1 1 calc R . . C44 C 0.9510(8) 0.7508(7) 0.6756(6) 0.057(3) Uani 1 1 d . . . H44B H 0.9657 0.7945 0.6547 0.069 Uiso 1 1 calc R . . C45 C 1.0412(7) 0.7015(7) 0.6840(7) 0.055(4) Uani 1 1 d . . . H45A H 1.0604 0.6922 0.7352 0.066 Uiso 1 1 calc R . . H45B H 1.1006 0.7223 0.6659 0.066 Uiso 1 1 calc R . . C46 C 1.0165(8) 0.6336(7) 0.6432(7) 0.054(3) Uani 1 1 d . . . H46B H 1.0347 0.6374 0.5943 0.065 Uiso 1 1 calc R . . H46C H 1.0589 0.5983 0.6678 0.065 Uiso 1 1 calc R . . C47 C 0.5915(6) 0.1370(5) 0.7983(5) 0.031(2) Uani 1 1 d . . . C48 C 0.6246(6) 0.0974(5) 0.8574(5) 0.033(2) Uani 1 1 d . . . H48A H 0.6810 0.1105 0.8904 0.040 Uiso 1 1 calc R . . C49 C 0.5748(7) 0.0403(5) 0.8667(5) 0.037(2) Uani 1 1 d . . . H49A H 0.5977 0.0136 0.9066 0.044 Uiso 1 1 calc R . . C50 C 0.4918(7) 0.0195(5) 0.8202(6) 0.039(2) Uani 1 1 d . . . H50A H 0.4601 -0.0214 0.8278 0.046 Uiso 1 1 calc R . . C51 C 0.4546(8) 0.0588(6) 0.7619(6) 0.039(3) Uani 1 1 d . . . H51A H 0.3961 0.0459 0.7306 0.046 Uiso 1 1 calc R . . C52 C 0.5053(6) 0.1168(5) 0.7509(5) 0.026(2) Uani 1 1 d . . . C53 C 0.5540(6) 0.2541(5) 0.7682(5) 0.033(2) Uani 1 1 d . . . C54 C 0.5569(7) 0.3148(6) 0.7994(6) 0.042(3) Uani 1 1 d . . . H54A H 0.6142 0.3277 0.8318 0.050 Uiso 1 1 calc R . . C55 C 0.4758(8) 0.3574(6) 0.7832(6) 0.050(3) Uani 1 1 d . . . H55A H 0.4766 0.4003 0.8033 0.060 Uiso 1 1 calc R . . C56 C 0.3926(8) 0.3354(7) 0.7364(6) 0.056(4) Uani 1 1 d . . . H56A H 0.3360 0.3641 0.7257 0.068 Uiso 1 1 calc R . . C57 C 0.3889(7) 0.2748(6) 0.7056(6) 0.038(2) Uani 1 1 d . . . H57A H 0.3311 0.2615 0.6739 0.046 Uiso 1 1 calc R . . C58 C 0.4691(6) 0.2342(5) 0.7209(5) 0.033(2) Uani 1 1 d . . . C59 C 0.6368(6) 0.1995(5) 0.7777(4) 0.0270(19) Uani 1 1 d . . . H59A H 0.6963 0.2128 0.8127 0.032 Uiso 1 1 calc R . . C60 C 0.4777(6) 0.1649(5) 0.6901(5) 0.033(2) Uani 1 1 d . . . H60A H 0.4149 0.1515 0.6584 0.039 Uiso 1 1 calc R . . C61 C 0.6680(6) 0.1892(4) 0.7021(4) 0.0240(19) Uani 1 1 d . . . H61A H 0.7166 0.1513 0.7050 0.029 Uiso 1 1 calc R . . C62 C 0.5736(6) 0.1695(5) 0.6492(4) 0.0242(19) Uani 1 1 d . . . H62A H 0.5611 0.2052 0.6128 0.029 Uiso 1 1 calc R . . C63 C 0.5932(6) 0.1048(5) 0.6104(5) 0.027(2) Uani 1 1 d . . . H63A H 0.6263 0.0723 0.6448 0.033 Uiso 1 1 calc R . . H63B H 0.5277 0.0860 0.5883 0.033 Uiso 1 1 calc R . . C64 C 0.6196(7) 0.1340(5) 0.4859(5) 0.032(2) Uani 1 1 d . . . C65 C 0.5194(7) 0.1346(5) 0.4534(5) 0.034(2) Uani 1 1 d . . . H65A H 0.4637 0.1253 0.4789 0.041 Uiso 1 1 calc R . . C66 C 0.5058(7) 0.1499(6) 0.3813(5) 0.042(3) Uani 1 1 d . . . H66A H 0.4394 0.1479 0.3557 0.050 Uiso 1 1 calc R . . C67 C 0.5890(8) 0.1681(7) 0.3452(6) 0.056(3) Uani 1 1 d . . . H67A H 0.5765 0.1823 0.2971 0.067 Uiso 1 1 calc R . . C68 C 0.6885(7) 0.1657(5) 0.3787(5) 0.037(2) Uani 1 1 d . . . H68A H 0.7447 0.1742 0.3534 0.044 Uiso 1 1 calc R . . C69 C 0.7028(6) 0.1503(5) 0.4502(5) 0.029(2) Uani 1 1 d . . . C70 C 0.7630(6) 0.1258(5) 0.5636(5) 0.028(2) Uani 1 1 d . . . C71 C 0.8947(7) 0.1612(6) 0.4877(5) 0.042(3) Uani 1 1 d . . . H71A H 0.9415 0.1505 0.5319 0.051 Uiso 1 1 calc R . . C72 C 0.9321(7) 0.1242(6) 0.4283(6) 0.049(3) Uani 1 1 d . . . H72A H 0.9285 0.0769 0.4374 0.073 Uiso 1 1 calc R . . H72B H 1.0028 0.1367 0.4247 0.073 Uiso 1 1 calc R . . H72C H 0.8895 0.1349 0.3837 0.073 Uiso 1 1 calc R . . C73 C 0.8975(8) 0.2369(6) 0.4779(6) 0.049(3) Uani 1 1 d . . . H73A H 0.9659 0.2503 0.4691 0.074 Uiso 1 1 calc R . . H73B H 0.8802 0.2586 0.5209 0.074 Uiso 1 1 calc R . . H73C H 0.8480 0.2496 0.4373 0.074 Uiso 1 1 calc R . . C74 C 0.7209(6) 0.2467(4) 0.6743(4) 0.0255(19) Uani 1 1 d . . . H74A H 0.7063 0.2467 0.6218 0.031 Uiso 1 1 calc R . . H74B H 0.6913 0.2875 0.6917 0.031 Uiso 1 1 calc R . . C75 C 0.8844(6) 0.3071(5) 0.7113(5) 0.032(2) Uani 1 1 d . . . C76 C 0.8536(8) 0.3698(6) 0.7276(6) 0.045(3) Uani 1 1 d . . . H76A H 0.7837 0.3801 0.7284 0.054 Uiso 1 1 calc R . . C77 C 0.9299(9) 0.4173(6) 0.7430(6) 0.048(3) Uani 1 1 d . . . H77A H 0.9118 0.4611 0.7537 0.057 Uiso 1 1 calc R . . C78 C 1.0297(7) 0.4012(5) 0.7428(6) 0.037(2) Uani 1 1 d . . . H78A H 1.0789 0.4346 0.7556 0.045 Uiso 1 1 calc R . . C79 C 1.0644(7) 0.3413(6) 0.7257(5) 0.039(2) Uani 1 1 d . . . H79A H 1.1345 0.3327 0.7234 0.047 Uiso 1 1 calc R . . C80 C 0.9871(6) 0.2913(5) 0.7112(5) 0.032(2) Uani 1 1 d . . . C81 C 0.8955(6) 0.1981(5) 0.6812(4) 0.0223(18) Uani 1 1 d . . . C82 C 1.0861(6) 0.1900(5) 0.6783(5) 0.029(2) Uani 1 1 d . . . H82A H 1.0658 0.1440 0.6637 0.034 Uiso 1 1 calc R . . C83 C 1.1281(7) 0.2221(5) 0.6162(6) 0.039(2) Uani 1 1 d . . . H83A H 1.0748 0.2239 0.5753 0.058 Uiso 1 1 calc R . . H83B H 1.1859 0.1964 0.6036 0.058 Uiso 1 1 calc R . . H83C H 1.1508 0.2669 0.6293 0.058 Uiso 1 1 calc R . . C84 C 1.1651(7) 0.1853(6) 0.7435(6) 0.043(3) Uani 1 1 d . . . H84A H 1.1347 0.1642 0.7822 0.065 Uiso 1 1 calc R . . H84B H 1.1883 0.2297 0.7581 0.065 Uiso 1 1 calc R . . H84C H 1.2232 0.1592 0.7321 0.065 Uiso 1 1 calc R . . C85 C 0.9120(7) 0.0150(5) 0.6114(6) 0.042(3) Uani 1 1 d . . . H85A H 0.9106 0.0169 0.5586 0.050 Uiso 1 1 calc R . . C86 C 0.8179(9) 0.0003(5) 0.6332(6) 0.042(3) Uani 1 1 d . . . H86A H 0.7612 -0.0066 0.5938 0.050 Uiso 1 1 calc R . . C87 C 0.8112(9) -0.0420(5) 0.7009(6) 0.047(3) Uani 1 1 d . . . H87A H 0.7495 -0.0700 0.6935 0.056 Uiso 1 1 calc R . . H87B H 0.8713 -0.0713 0.7090 0.056 Uiso 1 1 calc R . . C88 C 0.8069(8) 0.0003(6) 0.7648(6) 0.049(3) Uani 1 1 d . . . H88A H 0.8327 -0.0254 0.8077 0.058 Uiso 1 1 calc R . . H88B H 0.7348 0.0113 0.7682 0.058 Uiso 1 1 calc R . . C89 C 0.8669(7) 0.0633(6) 0.7649(5) 0.036(2) Uani 1 1 d . . . H89A H 0.8508 0.0961 0.8013 0.044 Uiso 1 1 calc R . . C90 C 0.9656(7) 0.0680(6) 0.7470(5) 0.037(2) Uani 1 1 d . . . H90A H 1.0054 0.1047 0.7722 0.044 Uiso 1 1 calc R . . C91 C 1.0312(7) 0.0129(5) 0.7287(6) 0.041(3) Uani 1 1 d . . . H91A H 1.0152 -0.0270 0.7552 0.049 Uiso 1 1 calc R . . H91B H 1.1035 0.0244 0.7436 0.049 Uiso 1 1 calc R . . C92 C 1.0166(8) -0.0017(6) 0.6510(7) 0.051(3) Uani 1 1 d . . . H92A H 1.0295 -0.0492 0.6445 0.061 Uiso 1 1 calc R . . H92B H 1.0687 0.0229 0.6285 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01877(15) 0.0426(2) 0.02291(18) -0.00378(18) 0.00224(12) 0.00016(17) Ir2 0.02024(15) 0.0342(2) 0.01970(17) -0.00094(18) 0.00286(12) -0.00388(17) N1 0.026(4) 0.030(5) 0.026(4) -0.009(3) 0.000(3) -0.004(3) N2 0.031(4) 0.036(5) 0.026(4) -0.006(3) 0.006(3) 0.005(3) N3 0.021(4) 0.047(5) 0.029(4) 0.000(4) 0.008(3) -0.015(4) N4 0.027(4) 0.042(5) 0.028(4) 0.003(4) 0.006(3) -0.005(3) N5 0.016(3) 0.041(5) 0.029(4) -0.004(3) 0.002(3) 0.004(3) N6 0.017(4) 0.049(6) 0.023(4) 0.006(4) 0.005(3) -0.006(3) N7 0.010(3) 0.042(5) 0.031(4) 0.003(4) 0.004(3) -0.002(3) N8 0.016(3) 0.034(5) 0.022(4) 0.000(3) -0.001(3) -0.002(3) O1 0.050(6) 0.097(8) 0.150(11) -0.002(8) 0.037(6) -0.003(5) F1 0.219(13) 0.087(7) 0.072(6) 0.007(5) -0.017(7) 0.027(7) S1 0.0402(15) 0.063(2) 0.060(2) 0.0093(16) 0.0166(14) 0.0009(14) O2 0.115(9) 0.168(13) 0.076(8) 0.033(8) 0.039(7) 0.052(9) F2 0.196(11) 0.049(6) 0.143(9) 0.005(5) 0.107(8) -0.005(6) O3 0.095(7) 0.070(7) 0.096(8) -0.032(6) 0.038(6) -0.023(5) F3 0.079(6) 0.121(8) 0.168(11) -0.007(7) 0.076(7) 0.010(5) C93 0.062(7) 0.041(7) 0.053(7) 0.029(6) 0.025(6) 0.004(5) S2 0.0236(11) 0.0411(15) 0.0270(13) 0.0009(11) 0.0021(10) 0.003(1) O4 0.027(4) 0.060(5) 0.063(6) 0.005(5) -0.003(4) 0.001(4) F4 0.079(5) 0.079(5) 0.037(4) -0.011(3) 0.020(3) -0.006(4) O5 0.032(4) 0.048(4) 0.042(4) -0.005(3) 0.005(3) 0.004(3) F5 0.079(5) 0.041(4) 0.051(4) -0.007(3) -0.002(4) -0.008(4) O6 0.045(4) 0.042(4) 0.028(4) 0.004(3) 0.003(3) -0.001(3) F6 0.040(3) 0.077(5) 0.078(5) -0.008(4) -0.003(3) 0.028(3) C94 0.043(6) 0.055(8) 0.041(6) -0.005(6) 0.005(5) 0.007(6) C1 0.019(4) 0.061(7) 0.030(5) -0.013(5) 0.007(4) -0.001(4) C2 0.028(5) 0.091(10) 0.045(7) -0.043(7) -0.003(5) 0.000(6) C3 0.030(6) 0.125(13) 0.032(6) -0.029(7) -0.003(5) 0.013(7) C4 0.027(5) 0.105(11) 0.026(6) -0.004(6) -0.011(4) 0.021(6) C5 0.041(6) 0.056(7) 0.031(5) 0.004(5) 0.022(4) 0.009(5) C6 0.024(4) 0.051(7) 0.033(5) 0.003(5) 0.011(4) 0.005(4) C7 0.031(4) 0.039(6) 0.016(4) -0.002(4) 0.008(4) -0.012(4) C8 0.059(6) 0.037(6) 0.029(5) -0.004(5) 0.019(5) 0.004(5) C9 0.040(6) 0.035(6) 0.065(8) 0.011(6) 0.005(5) 0.011(5) C10 0.019(4) 0.051(7) 0.033(5) 0.002(5) 0.010(4) 0.012(4) C11 0.019(4) 0.042(6) 0.023(5) -0.008(4) 0.013(3) -0.007(4) C12 0.019(4) 0.043(6) 0.026(5) -0.006(4) 0.003(3) 0.000(4) C13 0.031(5) 0.035(6) 0.037(6) -0.009(4) 0.014(4) 0.005(4) C14 0.017(4) 0.033(5) 0.013(4) -0.004(4) 0.006(3) -0.001(4) C15 0.011(3) 0.036(5) 0.022(4) 0.005(4) 0.000(3) 0.003(3) C16 0.017(4) 0.034(5) 0.028(5) -0.001(4) 0.000(3) -0.006(3) C17 0.034(5) 0.046(6) 0.026(5) -0.006(4) 0.014(4) -0.002(4) C18 0.033(5) 0.031(6) 0.036(6) -0.002(4) -0.001(4) 0.002(4) C19 0.033(5) 0.035(6) 0.052(7) -0.003(5) 0.008(5) -0.006(4) C20 0.042(6) 0.043(7) 0.067(8) 0.003(6) -0.003(6) -0.005(5) C21 0.063(8) 0.058(8) 0.059(8) -0.025(7) -0.011(6) -0.015(6) C22 0.062(7) 0.061(8) 0.026(6) -0.001(5) 0.001(5) -0.013(6) C23 0.032(5) 0.029(5) 0.039(6) -0.005(4) 0.007(4) 0.000(4) C24 0.034(5) 0.033(6) 0.020(5) -0.001(4) 0.006(4) -0.010(4) C25 0.039(6) 0.078(9) 0.025(5) -0.014(5) 0.009(4) -0.013(5) C26 0.061(7) 0.093(10) 0.029(6) 0.016(6) -0.005(5) -0.027(7) C27 0.074(8) 0.090(11) 0.073(9) -0.035(8) 0.049(8) -0.006(7) C28 0.018(4) 0.041(6) 0.029(5) 0.002(4) 0.009(4) -0.012(4) C29 0.018(4) 0.045(6) 0.030(5) 0.002(5) 0.001(4) -0.005(4) C30 0.029(5) 0.040(6) 0.046(6) 0.001(5) -0.001(4) -0.007(4) C31 0.042(6) 0.053(7) 0.056(8) -0.006(6) -0.004(6) -0.005(5) C32 0.051(7) 0.053(8) 0.049(7) 0.018(6) 0.004(5) -0.014(6) C33 0.047(6) 0.076(9) 0.032(6) 0.009(6) 0.023(5) -0.017(6) C34 0.028(5) 0.049(6) 0.028(5) -0.006(5) 0.003(4) -0.007(4) C35 0.021(4) 0.040(6) 0.022(5) -0.004(4) 0.011(4) -0.012(4) C36 0.032(5) 0.061(7) 0.035(6) -0.010(5) 0.019(4) -0.002(5) C37 0.041(6) 0.070(9) 0.064(8) 0.001(7) 0.015(6) -0.023(6) C38 0.060(7) 0.062(8) 0.044(7) -0.010(6) 0.024(6) -0.012(6) C39 0.040(6) 0.046(7) 0.044(7) -0.018(5) 0.007(5) 0.012(5) C40 0.033(6) 0.048(7) 0.048(7) 0.010(5) -0.002(5) 0.003(5) C41 0.035(6) 0.074(9) 0.037(6) 0.019(6) -0.004(5) 0.013(6) C42 0.045(6) 0.068(8) 0.029(6) -0.007(5) 0.005(5) 0.009(6) C43 0.019(4) 0.052(7) 0.023(5) -0.009(5) 0.000(4) -0.003(4) C44 0.029(5) 0.09(1) 0.048(7) -0.012(7) -0.011(5) -0.017(6) C45 0.015(5) 0.105(11) 0.044(7) -0.014(7) 0.001(4) -0.003(5) C46 0.028(5) 0.079(9) 0.054(8) -0.003(7) 0.004(5) 0.021(5) C47 0.026(4) 0.046(6) 0.024(5) 0.001(4) 0.008(4) -0.002(4) C48 0.021(4) 0.048(6) 0.032(5) 0.007(5) 0.008(4) -0.002(4) C49 0.036(5) 0.061(7) 0.015(5) 0.016(5) 0.015(4) 0.008(5) C50 0.037(5) 0.038(6) 0.044(6) -0.001(5) 0.013(5) 0.002(4) C51 0.030(5) 0.050(7) 0.036(6) 0.006(5) 0.005(4) -0.005(5) C52 0.018(4) 0.047(6) 0.016(4) 0.008(4) 0.009(3) 0.000(4) C53 0.024(4) 0.045(6) 0.031(5) -0.004(4) 0.010(4) -0.005(4) C54 0.028(5) 0.059(8) 0.039(6) 0.005(5) 0.008(4) -0.011(5) C55 0.051(7) 0.047(7) 0.057(7) 0.008(6) 0.031(6) 0.016(5) C56 0.027(6) 0.095(11) 0.050(7) 0.013(7) 0.015(5) 0.001(6) C57 0.025(5) 0.050(7) 0.041(6) 0.009(5) 0.009(4) 0.000(4) C58 0.023(4) 0.048(6) 0.033(5) -0.006(5) 0.017(4) -0.003(4) C59 0.020(4) 0.040(5) 0.020(4) -0.012(4) 0.002(3) 0.001(4) C60 0.017(4) 0.058(7) 0.025(5) 0.011(5) 0.011(4) -0.010(4) C61 0.014(4) 0.038(5) 0.020(4) -0.006(4) 0.000(3) -0.003(3) C62 0.020(4) 0.041(5) 0.014(4) 0.008(4) 0.011(3) -0.005(4) C63 0.014(4) 0.049(6) 0.019(4) 0.005(4) 0.005(3) -0.011(4) C64 0.027(5) 0.046(6) 0.023(5) -0.011(4) -0.001(4) 0.007(4) C65 0.025(4) 0.041(6) 0.037(6) -0.002(5) 0.009(4) 0.001(4) C66 0.026(5) 0.066(8) 0.033(6) 0.005(5) -0.003(4) 0.007(5) C67 0.042(6) 0.085(10) 0.039(7) 0.015(6) 0.003(5) 0.010(6) C68 0.023(4) 0.059(7) 0.030(5) -0.002(5) 0.007(4) -0.004(4) C69 0.017(4) 0.049(6) 0.023(5) -0.006(4) 0.005(3) 0.000(4) C70 0.028(5) 0.040(6) 0.018(4) 0.006(4) 0.006(4) -0.006(4) C71 0.025(5) 0.081(9) 0.021(5) 0.015(5) 0.000(4) -0.010(5) C72 0.026(5) 0.076(8) 0.046(7) -0.011(6) 0.010(5) -0.001(5) C73 0.046(6) 0.047(7) 0.054(7) 0.010(6) 0.003(5) -0.002(5) C74 0.027(4) 0.033(5) 0.017(4) -0.002(4) 0.006(3) -0.004(4) C75 0.017(4) 0.040(6) 0.037(5) 0.000(5) 0.002(4) 0.002(4) C76 0.028(5) 0.051(7) 0.051(7) 0.010(6) -0.013(5) -0.012(5) C77 0.072(8) 0.033(6) 0.036(6) -0.001(5) 0.000(6) 0.004(6) C78 0.036(5) 0.029(6) 0.046(6) 0.003(5) 0.001(5) -0.007(4) C79 0.021(4) 0.063(8) 0.030(5) -0.001(5) -0.003(4) -0.010(5) C80 0.022(4) 0.046(6) 0.029(5) 0.003(4) 0.007(4) -0.002(4) C81 0.013(4) 0.036(5) 0.019(4) 0.009(4) 0.005(3) -0.003(4) C82 0.014(4) 0.034(6) 0.039(6) -0.002(4) 0.007(4) -0.002(4) C83 0.018(4) 0.051(7) 0.049(7) 0.000(5) 0.006(4) -0.001(4) C84 0.033(5) 0.047(7) 0.053(7) -0.003(5) 0.018(5) 0.005(5) C85 0.042(6) 0.044(7) 0.042(6) 0.010(5) 0.014(5) 0.005(5) C86 0.047(6) 0.038(6) 0.041(7) 0.004(5) 0.006(5) -0.014(5) C87 0.059(7) 0.028(6) 0.058(7) -0.007(5) 0.027(6) -0.012(5) C88 0.039(6) 0.066(8) 0.043(6) 0.021(6) 0.010(5) -0.006(6) C89 0.044(6) 0.054(7) 0.012(4) -0.012(4) 0.006(4) -0.012(5) C90 0.028(5) 0.061(7) 0.020(5) -0.014(5) -0.006(4) 0.000(5) C91 0.031(5) 0.047(7) 0.045(6) 0.003(5) 0.006(5) -0.002(5) C92 0.042(6) 0.048(7) 0.064(8) -0.001(6) 0.008(6) 0.003(5) _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 Ir1 C24 2.056(9) . ? Ir1 C35 2.081(10) . ? Ir1 C39 2.165(10) . ? Ir1 C43 2.172(9) . ? Ir1 C40 2.228(11) . ? Ir1 C44 2.229(10) . ? Ir2 C81 2.046(9) . ? Ir2 C70 2.075(9) . ? Ir2 C85 2.142(11) . ? Ir2 C86 2.17(1) . ? Ir2 C89 2.195(9) . ? Ir2 C90 2.212(9) . ? N1 C24 1.355(11) . ? N1 C18 1.379(12) . ? N1 C17 1.477(11) . ? N2 C24 1.318(11) . ? N2 C23 1.428(12) . ? N2 C25 1.503(12) . ? N3 C29 1.354(12) . ? N3 C35 1.386(12) . ? N3 C28 1.47(1) . ? N4 C35 1.370(11) . ? N4 C34 1.396(13) . ? N4 C36 1.475(11) . ? N5 C70 1.369(11) . ? N5 C64 1.390(12) . ? N5 C63 1.47(1) . ? N6 C70 1.321(11) . ? N6 C69 1.409(11) . ? N6 C71 1.500(11) . ? N7 C81 1.372(11) . ? N7 C75 1.384(12) . ? N7 C74 1.472(10) . ? N8 C81 1.381(10) . ? N8 C80 1.382(12) . ? N8 C82 1.503(11) . ? O1 S1 1.412(10) . ? F1 C93 1.301(14) . ? S1 O3 1.394(10) . ? S1 O2 1.403(12) . ? S1 C93 1.809(13) . ? F2 C93 1.307(13) . ? F3 C93 1.307(14) . ? S2 O6 1.436(7) . ? S2 O5 1.451(8) . ? S2 O4 1.452(8) . ? S2 C94 1.824(11) . ? F4 C94 1.354(12) . ? F5 C94 1.313(13) . ? F6 C94 1.349(12) . ? C1 C2 1.380(13) . ? C1 C6 1.415(14) . ? C1 C13 1.517(14) . ? C2 C3 1.421(18) . ? C2 H2A 0.9500 . ? C3 C4 1.349(18) . ? C3 H3A 0.9500 . ? C4 C5 1.392(15) . ? C4 H4A 0.9500 . ? C5 C6 1.350(14) . ? C5 H5A 0.9500 . ? C6 C14 1.512(13) . ? C7 C8 1.378(14) . ? C7 C12 1.427(13) . ? C7 C13 1.527(12) . ? C8 C9 1.379(14) . ? C8 H8A 0.9500 . ? C9 C10 1.377(14) . ? C9 H9A 0.9500 . ? C10 C11 1.408(13) . ? C10 H10G 0.9500 . ? C11 C12 1.367(11) . ? C11 H11A 0.9500 . ? C12 C14 1.527(12) . ? C13 C15 1.534(12) . ? C13 H13E 1.0000 . ? C14 C16 1.554(11) . ? C14 H14A 1.0000 . ? C15 C28 1.509(12) . ? C15 C16 1.553(12) . ? C15 H15A 1.0000 . ? C16 C17 1.545(13) . ? C16 H16A 1.0000 . ? C17 H17D 0.9900 . ? C17 H17E 0.9900 . ? C18 C23 1.390(14) . ? C18 C19 1.402(13) . ? C19 C20 1.371(16) . ? C19 H19D 0.9500 . ? C20 C21 1.373(16) . ? C20 H20C 0.9500 . ? C21 C22 1.412(16) . ? C21 H21A 0.9500 . ? C22 C23 1.378(14) . ? C22 H22A 0.9500 . ? C25 C27 1.475(17) . ? C25 C26 1.544(16) . ? C25 H25A 1.0000 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.388(12) . ? C29 C30 1.412(14) . ? C30 C31 1.407(15) . ? C30 H30B 0.9500 . ? C31 C32 1.397(15) . ? C31 H31B 0.9500 . ? C32 C33 1.381(16) . ? C32 H32A 0.9500 . ? C33 C34 1.389(14) . ? C33 H33B 0.9500 . ? C36 C38 1.525(14) . ? C36 C37 1.532(15) . ? C36 H36A 1.0000 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C37 H37D 0.9800 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? C39 C40 1.410(15) . ? C39 C46 1.481(15) . ? C39 H39A 1.0000 . ? C40 C41 1.522(16) . ? C40 H40A 1.0000 . ? C41 C42 1.528(17) . ? C41 H41D 0.9900 . ? C41 H41E 0.9900 . ? C42 C43 1.501(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.414(14) . ? C43 H43B 1.0000 . ? C44 C45 1.549(17) . ? C44 H44B 1.0000 . ? C45 C46 1.594(17) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46B 0.9900 . ? C46 H46C 0.9900 . ? C47 C48 1.403(13) . ? C47 C52 1.420(13) . ? C47 C59 1.478(13) . ? C48 C49 1.356(14) . ? C48 H48A 0.9500 . ? C49 C50 1.385(14) . ? C49 H49A 0.9500 . ? C50 C51 1.402(14) . ? C50 H50A 0.9500 . ? C51 C52 1.385(14) . ? C51 H51A 0.9500 . ? C52 C60 1.520(13) . ? C53 C54 1.366(14) . ? C53 C58 1.406(13) . ? C53 C59 1.552(13) . ? C54 C55 1.381(15) . ? C54 H54A 0.9500 . ? C55 C56 1.398(17) . ? C55 H55A 0.9500 . ? C56 C57 1.361(16) . ? C56 H56A 0.9500 . ? C57 C58 1.346(14) . ? C57 H57A 0.9500 . ? C58 C60 1.534(14) . ? C59 C61 1.556(11) . ? C59 H59A 1.0000 . ? C60 C62 1.57(1) . ? C60 H60A 1.0000 . ? C61 C74 1.491(12) . ? C61 C62 1.552(11) . ? C61 H61A 1.0000 . ? C62 C63 1.545(13) . ? C62 H62A 1.0000 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.389(12) . ? C64 C69 1.403(12) . ? C65 C66 1.392(14) . ? C65 H65A 0.9500 . ? C66 C67 1.417(14) . ? C66 H66A 0.9500 . ? C67 C68 1.389(14) . ? C67 H67A 0.9500 . ? C68 C69 1.381(13) . ? C68 H68A 0.9500 . ? C71 C72 1.489(14) . ? C71 C73 1.550(16) . ? C71 H71A 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.383(15) . ? C75 C80 1.395(12) . ? C76 C77 1.400(15) . ? C76 H76A 0.9500 . ? C77 C78 1.360(15) . ? C77 H77A 0.9500 . ? C78 C79 1.355(15) . ? C78 H78A 0.9500 . ? C79 C80 1.442(13) . ? C79 H79A 0.9500 . ? C82 C83 1.512(13) . ? C82 C84 1.518(15) . ? C82 H82A 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.392(14) . ? C85 C92 1.527(15) . ? C85 H85A 1.0000 . ? C86 C87 1.557(15) . ? C86 H86A 1.0000 . ? C87 C88 1.492(15) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.506(15) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.393(13) . ? C89 H89A 1.0000 . ? C90 C91 1.483(14) . ? C90 H90A 1.0000 . ? C91 C92 1.491(15) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Ir1 C35 93.5(4) . . ? C24 Ir1 C39 90.6(4) . . ? C35 Ir1 C39 145.2(4) . . ? C24 Ir1 C43 148.8(3) . . ? C35 Ir1 C43 98.0(4) . . ? C39 Ir1 C43 96.0(4) . . ? C24 Ir1 C40 86.7(4) . . ? C35 Ir1 C40 177.4(4) . . ? C39 Ir1 C40 37.4(4) . . ? C43 Ir1 C40 80.6(4) . . ? C24 Ir1 C44 171.4(4) . . ? C35 Ir1 C44 90.4(4) . . ? C39 Ir1 C44 81.8(5) . . ? C43 Ir1 C44 37.4(4) . . ? C40 Ir1 C44 89.8(5) . . ? C81 Ir2 C70 94.9(4) . . ? C81 Ir2 C85 142.2(3) . . ? C70 Ir2 C85 92.7(4) . . ? C81 Ir2 C86 178.3(4) . . ? C70 Ir2 C86 86.8(4) . . ? C85 Ir2 C86 37.6(4) . . ? C81 Ir2 C89 98.4(4) . . ? C70 Ir2 C89 146.9(3) . . ? C85 Ir2 C89 95.1(4) . . ? C86 Ir2 C89 80.1(4) . . ? C81 Ir2 C90 90.2(4) . . ? C70 Ir2 C90 172.4(4) . . ? C85 Ir2 C90 79.9(4) . . ? C86 Ir2 C90 88.1(4) . . ? C89 Ir2 C90 36.9(3) . . ? C24 N1 C18 110.1(8) . . ? C24 N1 C17 127.4(8) . . ? C18 N1 C17 122.1(8) . . ? C24 N2 C23 110.9(7) . . ? C24 N2 C25 124.1(8) . . ? C23 N2 C25 124.9(8) . . ? C29 N3 C35 110.1(7) . . ? C29 N3 C28 124.7(8) . . ? C35 N3 C28 123.2(8) . . ? C35 N4 C34 110.7(8) . . ? C35 N4 C36 123.6(9) . . ? C34 N4 C36 125.6(8) . . ? C70 N5 C64 109.8(7) . . ? C70 N5 C63 128.0(7) . . ? C64 N5 C63 121.8(7) . . ? C70 N6 C69 111.2(7) . . ? C70 N6 C71 124.7(8) . . ? C69 N6 C71 123.1(7) . . ? C81 N7 C75 112.7(7) . . ? C81 N7 C74 123.0(7) . . ? C75 N7 C74 122.8(7) . . ? C81 N8 C80 111.3(7) . . ? C81 N8 C82 122.9(8) . . ? C80 N8 C82 124.8(7) . . ? O3 S1 O2 113.2(8) . . ? O3 S1 O1 115.8(7) . . ? O2 S1 O1 115.6(7) . . ? O3 S1 C93 104.1(5) . . ? O2 S1 C93 102.3(6) . . ? O1 S1 C93 103.5(7) . . ? F1 C93 F3 104.2(11) . . ? F1 C93 F2 104.3(12) . . ? F3 C93 F2 107.7(10) . . ? F1 C93 S1 114.3(9) . . ? F3 C93 S1 112.2(10) . . ? F2 C93 S1 113.4(7) . . ? O6 S2 O5 114.1(4) . . ? O6 S2 O4 115.3(4) . . ? O5 S2 O4 114.8(5) . . ? O6 S2 C94 104.2(5) . . ? O5 S2 C94 104.0(5) . . ? O4 S2 C94 102.2(5) . . ? F5 C94 F6 109.1(10) . . ? F5 C94 F4 108.8(9) . . ? F6 C94 F4 105.6(8) . . ? F5 C94 S2 113.0(7) . . ? F6 C94 S2 110.1(8) . . ? F4 C94 S2 110.0(8) . . ? C2 C1 C6 120.0(11) . . ? C2 C1 C13 127.7(10) . . ? C6 C1 C13 112.2(8) . . ? C1 C2 C3 118.7(12) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 120.3(11) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 120.3(11) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 121.1(11) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C1 119.5(10) . . ? C5 C6 C14 126.9(10) . . ? C1 C6 C14 113.6(8) . . ? C8 C7 C12 120.7(8) . . ? C8 C7 C13 126.8(9) . . ? C12 C7 C13 112.5(8) . . ? C7 C8 C9 119.5(10) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 120.1(9) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 121.3(8) . . ? C9 C10 H10G 119.3 . . ? C11 C10 H10G 119.3 . . ? C12 C11 C10 118.9(9) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C7 119.4(9) . . ? C11 C12 C14 128.0(8) . . ? C7 C12 C14 112.5(7) . . ? C1 C13 C7 106.5(7) . . ? C1 C13 C15 106.7(8) . . ? C7 C13 C15 108.9(7) . . ? C1 C13 H13E 111.5 . . ? C7 C13 H13E 111.5 . . ? C15 C13 H13E 111.5 . . ? C6 C14 C12 107.4(8) . . ? C6 C14 C16 108.7(6) . . ? C12 C14 C16 104.0(7) . . ? C6 C14 H14A 112.1 . . ? C12 C14 H14A 112.1 . . ? C16 C14 H14A 112.1 . . ? C28 C15 C13 114.9(8) . . ? C28 C15 C16 111.8(7) . . ? C13 C15 C16 109.1(7) . . ? C28 C15 H15A 106.8 . . ? C13 C15 H15A 106.8 . . ? C16 C15 H15A 106.8 . . ? C17 C16 C15 113.7(7) . . ? C17 C16 C14 110.2(7) . . ? C15 C16 C14 109.8(7) . . ? C17 C16 H16A 107.6 . . ? C15 C16 H16A 107.6 . . ? C14 C16 H16A 107.6 . . ? N1 C17 C16 112.3(8) . . ? N1 C17 H17D 109.1 . . ? C16 C17 H17D 109.1 . . ? N1 C17 H17E 109.1 . . ? C16 C17 H17E 109.1 . . ? H17D C17 H17E 107.9 . . ? N1 C18 C23 107.4(8) . . ? N1 C18 C19 131.6(10) . . ? C23 C18 C19 120.9(9) . . ? C20 C19 C18 116.6(10) . . ? C20 C19 H19D 121.7 . . ? C18 C19 H19D 121.7 . . ? C19 C20 C21 121.7(11) . . ? C19 C20 H20C 119.2 . . ? C21 C20 H20C 119.2 . . ? C20 C21 C22 123.3(11) . . ? C20 C21 H21A 118.3 . . ? C22 C21 H21A 118.3 . . ? C23 C22 C21 114(1) . . ? C23 C22 H22A 123.0 . . ? C21 C22 H22A 123.0 . . ? C22 C23 C18 123.5(9) . . ? C22 C23 N2 132.4(9) . . ? C18 C23 N2 104.1(8) . . ? N2 C24 N1 107.3(8) . . ? N2 C24 Ir1 128.4(6) . . ? N1 C24 Ir1 124.3(6) . . ? C27 C25 N2 112.1(10) . . ? C27 C25 C26 113.9(10) . . ? N2 C25 C26 107.9(8) . . ? C27 C25 H25A 107.5 . . ? N2 C25 H25A 107.5 . . ? C26 C25 H25A 107.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26D 109.5 . . ? H26B C26 H26D 109.5 . . ? H26C C26 H26D 109.5 . . ? C25 C27 H27D 109.5 . . ? C25 C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? C25 C27 H27F 109.5 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? N3 C28 C15 114.8(7) . . ? N3 C28 H28A 108.6 . . ? C15 C28 H28A 108.6 . . ? N3 C28 H28B 108.6 . . ? C15 C28 H28B 108.6 . . ? H28A C28 H28B 107.5 . . ? N3 C29 C34 108.7(8) . . ? N3 C29 C30 130.3(8) . . ? C34 C29 C30 121.0(9) . . ? C31 C30 C29 116.9(9) . . ? C31 C30 H30B 121.6 . . ? C29 C30 H30B 121.6 . . ? C32 C31 C30 120.7(11) . . ? C32 C31 H31B 119.7 . . ? C30 C31 H31B 119.7 . . ? C33 C32 C31 122.1(10) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 117.4(9) . . ? C32 C33 H33B 121.3 . . ? C34 C33 H33B 121.3 . . ? C29 C34 C33 121.9(10) . . ? C29 C34 N4 105.3(8) . . ? C33 C34 N4 132.8(9) . . ? N4 C35 N3 105.3(8) . . ? N4 C35 Ir1 127.8(7) . . ? N3 C35 Ir1 126.9(6) . . ? N4 C36 C38 110.3(9) . . ? N4 C36 C37 112.1(9) . . ? C38 C36 C37 109.8(8) . . ? N4 C36 H36A 108.2 . . ? C38 C36 H36A 108.2 . . ? C37 C36 H36A 108.2 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C37 H37D 109.5 . . ? H37B C37 H37D 109.5 . . ? H37C C37 H37D 109.5 . . ? C36 C38 H38D 109.5 . . ? C36 C38 H38E 109.5 . . ? H38D C38 H38E 109.5 . . ? C36 C38 H38F 109.5 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C40 C39 C46 127.9(11) . . ? C40 C39 Ir1 73.7(6) . . ? C46 C39 Ir1 111.4(8) . . ? C40 C39 H39A 112.4 . . ? C46 C39 H39A 112.4 . . ? Ir1 C39 H39A 112.4 . . ? C39 C40 C41 122.0(11) . . ? C39 C40 Ir1 68.9(6) . . ? C41 C40 Ir1 112.4(8) . . ? C39 C40 H40A 115.0 . . ? C41 C40 H40A 115.0 . . ? Ir1 C40 H40A 115.0 . . ? C40 C41 C42 110.5(9) . . ? C40 C41 H41D 109.6 . . ? C42 C41 H41D 109.6 . . ? C40 C41 H41E 109.6 . . ? C42 C41 H41E 109.6 . . ? H41D C41 H41E 108.1 . . ? C43 C42 C41 115.5(9) . . ? C43 C42 H42A 108.4 . . ? C41 C42 H42A 108.4 . . ? C43 C42 H42B 108.4 . . ? C41 C42 H42B 108.4 . . ? H42A C42 H42B 107.5 . . ? C44 C43 C42 127.2(10) . . ? C44 C43 Ir1 73.5(6) . . ? C42 C43 Ir1 108.5(7) . . ? C44 C43 H43B 113.3 . . ? C42 C43 H43B 113.3 . . ? Ir1 C43 H43B 113.3 . . ? C43 C44 C45 122.5(12) . . ? C43 C44 Ir1 69.1(5) . . ? C45 C44 Ir1 110.1(8) . . ? C43 C44 H44B 115.4 . . ? C45 C44 H44B 115.4 . . ? Ir1 C44 H44B 115.4 . . ? C44 C45 C46 113.6(9) . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C39 C46 C45 112.3(9) . . ? C39 C46 H46B 109.1 . . ? C45 C46 H46B 109.1 . . ? C39 C46 H46C 109.1 . . ? C45 C46 H46C 109.1 . . ? H46B C46 H46C 107.9 . . ? C48 C47 C52 119.1(9) . . ? C48 C47 C59 127.3(8) . . ? C52 C47 C59 113.6(8) . . ? C49 C48 C47 119.0(9) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C48 C49 C50 122.6(9) . . ? C48 C49 H49A 118.7 . . ? C50 C49 H49A 118.7 . . ? C49 C50 C51 120(1) . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C52 C51 C50 118.3(10) . . ? C52 C51 H51A 120.8 . . ? C50 C51 H51A 120.8 . . ? C51 C52 C47 121.0(9) . . ? C51 C52 C60 125.9(9) . . ? C47 C52 C60 113.1(8) . . ? C54 C53 C58 120.8(9) . . ? C54 C53 C59 127.8(8) . . ? C58 C53 C59 111.4(8) . . ? C53 C54 C55 119.4(10) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C54 C55 C56 118.0(12) . . ? C54 C55 H55A 121.0 . . ? C56 C55 H55A 121.0 . . ? C57 C56 C55 123.0(11) . . ? C57 C56 H56A 118.5 . . ? C55 C56 H56A 118.5 . . ? C58 C57 C56 118.4(10) . . ? C58 C57 H57A 120.8 . . ? C56 C57 H57A 120.8 . . ? C57 C58 C53 120.5(10) . . ? C57 C58 C60 125.0(9) . . ? C53 C58 C60 114.5(8) . . ? C47 C59 C53 109.9(7) . . ? C47 C59 C61 106.9(7) . . ? C53 C59 C61 104.7(7) . . ? C47 C59 H59A 111.6 . . ? C53 C59 H59A 111.6 . . ? C61 C59 H59A 111.6 . . ? C52 C60 C58 108.8(8) . . ? C52 C60 C62 106.4(7) . . ? C58 C60 C62 103.7(7) . . ? C52 C60 H60A 112.5 . . ? C58 C60 H60A 112.5 . . ? C62 C60 H60A 112.5 . . ? C74 C61 C62 110.4(7) . . ? C74 C61 C59 114.3(7) . . ? C62 C61 C59 110.2(6) . . ? C74 C61 H61A 107.2 . . ? C62 C61 H61A 107.2 . . ? C59 C61 H61A 107.2 . . ? C63 C62 C61 111.0(7) . . ? C63 C62 C60 112.3(7) . . ? C61 C62 C60 109.3(7) . . ? C63 C62 H62A 108.0 . . ? C61 C62 H62A 108.0 . . ? C60 C62 H62A 108.0 . . ? N5 C63 C62 109.3(7) . . ? N5 C63 H63A 109.8 . . ? C62 C63 H63A 109.8 . . ? N5 C63 H63B 109.8 . . ? C62 C63 H63B 109.8 . . ? H63A C63 H63B 108.3 . . ? C65 C64 N5 130.4(9) . . ? C65 C64 C69 123.1(9) . . ? N5 C64 C69 106.5(7) . . ? C64 C65 C66 115.9(8) . . ? C64 C65 H65A 122.1 . . ? C66 C65 H65A 122.1 . . ? C65 C66 C67 121.4(9) . . ? C65 C66 H66A 119.3 . . ? C67 C66 H66A 119.3 . . ? C68 C67 C66 121.3(10) . . ? C68 C67 H67A 119.4 . . ? C66 C67 H67A 119.4 . . ? C69 C68 C67 117.5(8) . . ? C69 C68 H68A 121.2 . . ? C67 C68 H68A 121.2 . . ? C68 C69 C64 120.6(8) . . ? C68 C69 N6 134.1(7) . . ? C64 C69 N6 105.1(8) . . ? N6 C70 N5 107.2(8) . . ? N6 C70 Ir2 128.5(6) . . ? N5 C70 Ir2 123.7(6) . . ? C72 C71 N6 113.4(9) . . ? C72 C71 C73 113.1(9) . . ? N6 C71 C73 108.5(8) . . ? C72 C71 H71A 107.1 . . ? N6 C71 H71A 107.1 . . ? C73 C71 H71A 107.1 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N7 C74 C61 115.8(7) . . ? N7 C74 H74A 108.3 . . ? C61 C74 H74A 108.3 . . ? N7 C74 H74B 108.3 . . ? C61 C74 H74B 108.3 . . ? H74A C74 H74B 107.4 . . ? C76 C75 N7 133.2(8) . . ? C76 C75 C80 121.7(9) . . ? N7 C75 C80 105.1(8) . . ? C75 C76 C77 117.1(10) . . ? C75 C76 H76A 121.4 . . ? C77 C76 H76A 121.4 . . ? C78 C77 C76 120.6(11) . . ? C78 C77 H77A 119.7 . . ? C76 C77 H77A 119.7 . . ? C79 C78 C77 125(1) . . ? C79 C78 H78A 117.5 . . ? C77 C78 H78A 117.5 . . ? C78 C79 C80 115.1(9) . . ? C78 C79 H79A 122.4 . . ? C80 C79 H79A 122.4 . . ? N8 C80 C75 107.1(8) . . ? N8 C80 C79 132.5(8) . . ? C75 C80 C79 120.3(9) . . ? N7 C81 N8 103.7(7) . . ? N7 C81 Ir2 127.9(5) . . ? N8 C81 Ir2 128.2(6) . . ? N8 C82 C83 110.4(8) . . ? N8 C82 C84 111.6(8) . . ? C83 C82 C84 112.2(7) . . ? N8 C82 H82A 107.4 . . ? C83 C82 H82A 107.4 . . ? C84 C82 H82A 107.4 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 C92 126.5(10) . . ? C86 C85 Ir2 72.3(6) . . ? C92 C85 Ir2 108.8(8) . . ? C86 C85 H85A 113.7 . . ? C92 C85 H85A 113.7 . . ? Ir2 C85 H85A 113.7 . . ? C85 C86 C87 120.6(10) . . ? C85 C86 Ir2 70.1(6) . . ? C87 C86 Ir2 113.4(7) . . ? C85 C86 H86A 115.0 . . ? C87 C86 H86A 115.0 . . ? Ir2 C86 H86A 115.0 . . ? C88 C87 C86 111.3(9) . . ? C88 C87 H87A 109.4 . . ? C86 C87 H87A 109.4 . . ? C88 C87 H87B 109.4 . . ? C86 C87 H87B 109.4 . . ? H87A C87 H87B 108.0 . . ? C87 C88 C89 114.7(8) . . ? C87 C88 H88A 108.6 . . ? C89 C88 H88A 108.6 . . ? C87 C88 H88B 108.6 . . ? C89 C88 H88B 108.6 . . ? H88A C88 H88B 107.6 . . ? C90 C89 C88 124.5(10) . . ? C90 C89 Ir2 72.2(6) . . ? C88 C89 Ir2 109.7(6) . . ? C90 C89 H89A 114.2 . . ? C88 C89 H89A 114.2 . . ? Ir2 C89 H89A 114.2 . . ? C89 C90 C91 126.9(10) . . ? C89 C90 Ir2 70.9(5) . . ? C91 C90 Ir2 113.6(6) . . ? C89 C90 H90A 112.7 . . ? C91 C90 H90A 112.7 . . ? Ir2 C90 H90A 112.7 . . ? C90 C91 C92 112.0(9) . . ? C90 C91 H91A 109.2 . . ? C92 C91 H91A 109.2 . . ? C90 C91 H91B 109.2 . . ? C92 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? C91 C92 C85 116.0(9) . . ? C91 C92 H92A 108.3 . . ? C85 C92 H92A 108.3 . . ? C91 C92 H92B 108.3 . . ? C85 C92 H92B 108.3 . . ? H92A C92 H92B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.551 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.123 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 1 -0.020 0.500 0.109 1170.6 464.1 _platon_squeeze_details ; # e- is matched to the Diff Four map to decide amount of solv to remove. ; # Attachment 'tj01.cif' data_tj01 _database_code_depnum_ccdc_archive 'CCDC 707709' _audit_update_record ; 2007-08-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H64 B2 Cl12 F8 N8 O4 Rh2' _chemical_formula_weight 1958.19 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.039(2) _cell_length_b 20.668(3) _cell_length_c 20.407(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.533(2) _cell_angle_gamma 90.00 _cell_volume 8379.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 359 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8348 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)' _diffrn_ambient_temperature 173(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 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 56208 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19074 _reflns_number_gt 11647 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.14 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. . The asymmetric unit consists of two chemically equivalent but crystallographically independent complex cations, two tetrafluoroborate anions and four chloroform molecules of crystallization. Both borate anions are disordered by rotation around one of the B-F bonds. Two of the chloroform molecules are disordered. One of them is disordered in the position of one Chlorine atom and the other was disordered and its Chlorine atoms were refined in four parts. ; _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^)+(0.0611P)^2^] 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 19074 _refine_ls_number_parameters 1077 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.007 _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 Rh1 Rh 0.427352(14) 0.585150(15) 0.243733(14) 0.03639(9) Uani 1 1 d . . . O1 O 0.34598(17) 0.6187(2) 0.35401(17) 0.0860(12) Uani 1 1 d . . . O2 O 0.31127(18) 0.5929(3) 0.13553(18) 0.1123(17) Uani 1 1 d . . . N1 N 0.57076(14) 0.58731(12) 0.32380(13) 0.0285(6) Uani 1 1 d . . . N2 N 0.50779(16) 0.51378(13) 0.36037(14) 0.0345(7) Uani 1 1 d . . . N3 N 0.50930(14) 0.61558(13) 0.13065(13) 0.0288(6) Uani 1 1 d . . . N4 N 0.50684(15) 0.51262(13) 0.14792(13) 0.0339(7) Uani 1 1 d . . . C1 C 0.47799(17) 0.78265(16) 0.28215(17) 0.0306(8) Uani 1 1 d . . . C2 C 0.42167(19) 0.79289(18) 0.3123(2) 0.0434(10) Uani 1 1 d . . . H2A H 0.4191 0.7763 0.3553 0.052 Uiso 1 1 calc R . . C3 C 0.3683(2) 0.8280(2) 0.2789(2) 0.0577(12) Uani 1 1 d . . . H3A H 0.3291 0.8353 0.2995 0.069 Uiso 1 1 calc R . . C4 C 0.3715(2) 0.8520(2) 0.2173(2) 0.0574(12) Uani 1 1 d . . . H4A H 0.3348 0.8762 0.1956 0.069 Uiso 1 1 calc R . . C5 C 0.4278(2) 0.84153(18) 0.1859(2) 0.0454(10) Uani 1 1 d . . . H5A H 0.4296 0.8577 0.1426 0.054 Uiso 1 1 calc R . . C6 C 0.48128(18) 0.80721(16) 0.21846(17) 0.0336(8) Uani 1 1 d . . . C7 C 0.59925(17) 0.79024(15) 0.30682(17) 0.0306(8) Uani 1 1 d . . . C8 C 0.64456(18) 0.80973(17) 0.36003(19) 0.0394(9) Uani 1 1 d . . . H8A H 0.6422 0.7924 0.4028 0.047 Uiso 1 1 calc R . . C9 C 0.6936(2) 0.85491(19) 0.3503(2) 0.0477(10) Uani 1 1 d . . . H9A H 0.7241 0.8697 0.3868 0.057 Uiso 1 1 calc R . . C10 C 0.6979(2) 0.87848(19) 0.2873(2) 0.0512(11) Uani 1 1 d . . . H10A H 0.7320 0.9089 0.2809 0.061 Uiso 1 1 calc R . . C11 C 0.65313(19) 0.85802(17) 0.2338(2) 0.0424(10) Uani 1 1 d . . . H11A H 0.6570 0.8735 0.1907 0.051 Uiso 1 1 calc R . . C12 C 0.60276(17) 0.81491(15) 0.24366(18) 0.0326(8) Uani 1 1 d . . . C13 C 0.53986(17) 0.74576(15) 0.30954(16) 0.0289(7) Uani 1 1 d . . . H13A H 0.5372 0.7297 0.3553 0.035 Uiso 1 1 calc R . . C14 C 0.54725(18) 0.79106(16) 0.19232(17) 0.0331(8) Uani 1 1 d . . . H14A H 0.5497 0.8109 0.1480 0.040 Uiso 1 1 calc R . . C15 C 0.54467(17) 0.68930(15) 0.25987(16) 0.0278(7) Uani 1 1 d . . . H15A H 0.4998 0.6673 0.2550 0.033 Uiso 1 1 calc R . . C16 C 0.55294(17) 0.71591(15) 0.19042(16) 0.0288(7) Uani 1 1 d . . . H16A H 0.5991 0.7045 0.1805 0.035 Uiso 1 1 calc R . . C17 C 0.59633(17) 0.63693(16) 0.28229(17) 0.0326(8) Uani 1 1 d . . . H17A H 0.6106 0.6159 0.2428 0.039 Uiso 1 1 calc R . . H17B H 0.6365 0.6575 0.3073 0.039 Uiso 1 1 calc R . . C18 C 0.61016(18) 0.55637(16) 0.37572(17) 0.0332(8) Uani 1 1 d . . . C19 C 0.6767(2) 0.56413(18) 0.40333(19) 0.0432(9) Uani 1 1 d . . . H19A H 0.7052 0.5955 0.3874 0.052 Uiso 1 1 calc R . . C20 C 0.6990(2) 0.5236(2) 0.4553(2) 0.0568(12) Uani 1 1 d . . . H20A H 0.7443 0.5274 0.4756 0.068 Uiso 1 1 calc R . . C21 C 0.6583(3) 0.4780(2) 0.4790(2) 0.0613(13) Uani 1 1 d . . . H21A H 0.6763 0.4517 0.5153 0.074 Uiso 1 1 calc R . . C22 C 0.5924(2) 0.46913(18) 0.45213(19) 0.0501(11) Uani 1 1 d . . . H22A H 0.5644 0.4375 0.4683 0.060 Uiso 1 1 calc R . . C23 C 0.5694(2) 0.51011(15) 0.39902(17) 0.0364(9) Uani 1 1 d . . . C24 C 0.4508(2) 0.47364(19) 0.3701(2) 0.0530(11) Uani 1 1 d . . . H24A H 0.4125 0.4846 0.3370 0.080 Uiso 1 1 calc R . . H24B H 0.4387 0.4811 0.4145 0.080 Uiso 1 1 calc R . . H24C H 0.4626 0.4280 0.3654 0.080 Uiso 1 1 calc R . . C25 C 0.50828(18) 0.56099(16) 0.31387(16) 0.0313(8) Uani 1 1 d . . . C26 C 0.50155(19) 0.68623(15) 0.13682(16) 0.0340(8) Uani 1 1 d . . . H26A H 0.4556 0.6957 0.1472 0.041 Uiso 1 1 calc R . . H26B H 0.5064 0.7068 0.0939 0.041 Uiso 1 1 calc R . . C27 C 0.54584(17) 0.58715(16) 0.08425(16) 0.0302(7) Uani 1 1 d . . . C28 C 0.57816(18) 0.61258(17) 0.03405(17) 0.0358(8) Uani 1 1 d . . . H28A H 0.5796 0.6578 0.0262 0.043 Uiso 1 1 calc R . . C29 C 0.60819(19) 0.56883(19) -0.00400(19) 0.0433(9) Uani 1 1 d . . . H29A H 0.6301 0.5844 -0.0394 0.052 Uiso 1 1 calc R . . C30 C 0.6073(2) 0.50242(19) 0.00798(19) 0.0464(10) Uani 1 1 d . . . H30A H 0.6294 0.4740 -0.0188 0.056 Uiso 1 1 calc R . . C31 C 0.5751(2) 0.47707(18) 0.05794(18) 0.0432(10) Uani 1 1 d . . . H31A H 0.5739 0.4318 0.0659 0.052 Uiso 1 1 calc R . . C32 C 0.54447(18) 0.52107(16) 0.09607(17) 0.0335(8) Uani 1 1 d . . . C33 C 0.4917(2) 0.44932(17) 0.17511(19) 0.0474(10) Uani 1 1 d . . . H33A H 0.4645 0.4554 0.2112 0.071 Uiso 1 1 calc R . . H33B H 0.5338 0.4274 0.1920 0.071 Uiso 1 1 calc R . . H33C H 0.4666 0.4230 0.1403 0.071 Uiso 1 1 calc R . . C34 C 0.48583(17) 0.56971(16) 0.16918(16) 0.0323(8) Uani 1 1 d . . . C35 C 0.3760(2) 0.6046(2) 0.3130(2) 0.0555(12) Uani 1 1 d . . . C36 C 0.3540(2) 0.5925(3) 0.1770(2) 0.0653(14) Uani 1 1 d . . . Rh2 Rh -0.086672(15) 0.244481(13) 0.965077(15) 0.03690(9) Uani 1 1 d . . . O3 O -0.17643(18) 0.35876(15) 0.9257(2) 0.0907(12) Uani 1 1 d . . . O4 O -0.19560(16) 0.14709(16) 0.9227(2) 0.0851(12) Uani 1 1 d . . . N5 N 0.05260(15) 0.31026(13) 0.96473(14) 0.0352(7) Uani 1 1 d . . . N6 N -0.00482(18) 0.36072(15) 1.03122(14) 0.0454(8) Uani 1 1 d . . . N7 N -0.00051(14) 0.12360(12) 0.94806(13) 0.0283(6) Uani 1 1 d . . . N8 N 0.00178(15) 0.14851(13) 1.05169(13) 0.0330(7) Uani 1 1 d . . . C37 C -0.04999(17) 0.26693(15) 0.76875(16) 0.0276(7) Uani 1 1 d . . . C38 C -0.10839(18) 0.30291(17) 0.75958(18) 0.0380(9) Uani 1 1 d . . . H38A H -0.1079 0.3468 0.7736 0.046 Uiso 1 1 calc R . . C39 C -0.1675(2) 0.2755(2) 0.7301(2) 0.0516(11) Uani 1 1 d . . . H39A H -0.2074 0.3007 0.7227 0.062 Uiso 1 1 calc R . . C40 C -0.1686(2) 0.2111(2) 0.7112(2) 0.0535(11) Uani 1 1 d . . . H40A H -0.2095 0.1922 0.6914 0.064 Uiso 1 1 calc R . . C41 C -0.1108(2) 0.17408(18) 0.72077(17) 0.0401(9) Uani 1 1 d . . . H41A H -0.1120 0.1299 0.7078 0.048 Uiso 1 1 calc R . . C42 C -0.05127(17) 0.20162(15) 0.74925(15) 0.0290(8) Uani 1 1 d . . . C43 C 0.07123(18) 0.27240(17) 0.76496(16) 0.0331(8) Uani 1 1 d . . . C44 C 0.11989(19) 0.31482(19) 0.7487(2) 0.0462(10) Uani 1 1 d . . . H44A H 0.1228 0.3574 0.7663 0.055 Uiso 1 1 calc R . . C45 C 0.1644(2) 0.2942(2) 0.7062(2) 0.0639(13) Uani 1 1 d . . . H45A H 0.1974 0.3233 0.6941 0.077 Uiso 1 1 calc R . . C46 C 0.1613(2) 0.2330(2) 0.6820(3) 0.0707(15) Uani 1 1 d . . . H46A H 0.1920 0.2200 0.6527 0.085 Uiso 1 1 calc R . . C47 C 0.1141(2) 0.1889(2) 0.69923(19) 0.0510(11) Uani 1 1 d . . . H47A H 0.1128 0.1460 0.6825 0.061 Uiso 1 1 calc R . . C48 C 0.06909(18) 0.20871(17) 0.74108(17) 0.0345(8) Uani 1 1 d . . . C49 C 0.01636(16) 0.28703(15) 0.80663(16) 0.0275(7) Uani 1 1 d . . . H49A H 0.0165 0.3334 0.8206 0.033 Uiso 1 1 calc R . . C50 C 0.01533(17) 0.16796(15) 0.76659(15) 0.0303(8) Uani 1 1 d . . . H50A H 0.0146 0.1227 0.7492 0.036 Uiso 1 1 calc R . . C51 C 0.02321(17) 0.24010(14) 0.86633(15) 0.0268(7) Uani 1 1 d . . . H51A H -0.0207 0.2417 0.8846 0.032 Uiso 1 1 calc R . . C52 C 0.03150(17) 0.17018(15) 0.84310(15) 0.0275(7) Uani 1 1 d . . . H52A H 0.0793 0.1566 0.8560 0.033 Uiso 1 1 calc R . . C53 C 0.07706(18) 0.25981(16) 0.92253(17) 0.0336(8) Uani 1 1 d . . . H53A H 0.0911 0.2214 0.9498 0.040 Uiso 1 1 calc R . . H53B H 0.1170 0.2762 0.9038 0.040 Uiso 1 1 calc R . . C54 C 0.0914(2) 0.36372(17) 0.98811(17) 0.0419(10) Uani 1 1 d . . . C55 C 0.1539(2) 0.3863(2) 0.9752(2) 0.0521(11) Uani 1 1 d . . . H55A H 0.1790 0.3644 0.9456 0.062 Uiso 1 1 calc R . . C56 C 0.1775(3) 0.4419(2) 1.0078(2) 0.0603(12) Uani 1 1 d . . . H56A H 0.2201 0.4588 1.0009 0.072 Uiso 1 1 calc R . . C57 C 0.1400(3) 0.4737(2) 1.0504(2) 0.0694(15) Uani 1 1 d . . . H57A H 0.1575 0.5122 1.0715 0.083 Uiso 1 1 calc R . . C58 C 0.0794(3) 0.4520(2) 1.0629(2) 0.0636(14) Uani 1 1 d . . . H58A H 0.0546 0.4740 1.0927 0.076 Uiso 1 1 calc R . . C59 C 0.0547(2) 0.39591(18) 1.03040(18) 0.0467(10) Uani 1 1 d . . . C60 C -0.0571(3) 0.3789(2) 1.0717(2) 0.0635(13) Uani 1 1 d . . . H60A H -0.0942 0.3478 1.0647 0.095 Uiso 1 1 calc R . . H60B H -0.0739 0.4223 1.0591 0.095 Uiso 1 1 calc R . . H60C H -0.0381 0.3789 1.1185 0.095 Uiso 1 1 calc R . . C61 C -0.0062(2) 0.30822(16) 0.99078(17) 0.0378(9) Uani 1 1 d . . . C62 C -0.01449(18) 0.12433(15) 0.87583(15) 0.0306(8) Uani 1 1 d . . . H62A H -0.0619 0.1375 0.8628 0.037 Uiso 1 1 calc R . . H62B H -0.0092 0.0799 0.8591 0.037 Uiso 1 1 calc R . . C63 C 0.04273(17) 0.07952(15) 0.98375(16) 0.0281(7) Uani 1 1 d . . . C64 C 0.07849(18) 0.02723(16) 0.96341(18) 0.0347(8) Uani 1 1 d . . . H64A H 0.0777 0.0165 0.9181 0.042 Uiso 1 1 calc R . . C65 C 0.11541(18) -0.00842(17) 1.01340(18) 0.0379(9) Uani 1 1 d . . . H65A H 0.1408 -0.0446 1.0020 0.046 Uiso 1 1 calc R . . C66 C 0.11609(19) 0.00771(18) 1.07983(19) 0.0424(9) Uani 1 1 d . . . H66A H 0.1421 -0.0179 1.1124 0.051 Uiso 1 1 calc R . . C67 C 0.08041(18) 0.05954(17) 1.09997(18) 0.0377(9) Uani 1 1 d . . . H67A H 0.0809 0.0701 1.1453 0.045 Uiso 1 1 calc R . . C68 C 0.04361(18) 0.09544(16) 1.04983(17) 0.0320(8) Uani 1 1 d . . . C69 C -0.0125(2) 0.18131(18) 1.11184(17) 0.0461(10) Uani 1 1 d . . . H69A H -0.0437 0.2172 1.1000 0.069 Uiso 1 1 calc R . . H69B H 0.0295 0.1981 1.1358 0.069 Uiso 1 1 calc R . . H69C H -0.0329 0.1506 1.1400 0.069 Uiso 1 1 calc R . . C70 C -0.02475(17) 0.16607(16) 0.99018(16) 0.0309(8) Uani 1 1 d . . . C71 C -0.1435(2) 0.3162(2) 0.9413(2) 0.0537(11) Uani 1 1 d . . . C72 C -0.1565(2) 0.1851(2) 0.9399(2) 0.0543(11) Uani 1 1 d . . . F1 F 0.51475(18) 0.14824(15) 0.06445(13) 0.0967(10) Uani 1 1 d . A . B1 B 0.4820(3) 0.1804(2) 0.0132(2) 0.0518(13) Uani 1 1 d . . . F2 F 0.5268(3) 0.1830(4) -0.0337(4) 0.074(2) Uani 0.527(8) 1 d P A 1 F3 F 0.4267(3) 0.1419(4) -0.0225(4) 0.107(3) Uani 0.527(8) 1 d P A 1 F4 F 0.4523(6) 0.2362(4) 0.0210(3) 0.116(5) Uani 0.527(8) 1 d P A 1 F2A F 0.4784(9) 0.1569(5) -0.0418(4) 0.160(8) Uani 0.473(8) 1 d P A 2 F3A F 0.4192(3) 0.1842(4) 0.0419(4) 0.087(3) Uani 0.473(8) 1 d P A 2 F4A F 0.5062(4) 0.2454(4) 0.0202(4) 0.082(3) Uani 0.473(8) 1 d P A 2 B2 B 0.02972(15) 0.47772(14) 0.78070(14) 0.0422(11) Uani 1 1 d D . . F5 F -0.00219(11) 0.43377(11) 0.73667(11) 0.0585(6) Uani 1 1 d D B . F6 F 0.07422(14) 0.51358(13) 0.74812(14) 0.0629(11) Uani 0.856(6) 1 d PD B 3 F7 F 0.06690(16) 0.44618(13) 0.83234(13) 0.0674(11) Uani 0.856(6) 1 d PD B 3 F8 F -0.01617(16) 0.51931(13) 0.80148(14) 0.0723(12) Uani 0.856(6) 1 d PD B 3 F6' F -0.0020(17) 0.4773(19) 0.8370(10) 0.26(3) Uiso 0.144(6) 1 d PD B 4 F7' F 0.0959(7) 0.4602(14) 0.797(2) 0.29(3) Uiso 0.144(6) 1 d PD B 4 F8' F 0.026(2) 0.5384(4) 0.7534(11) 0.50(6) Uiso 0.144(6) 1 d PD B 4 C73 C 0.2762(2) 0.3043(2) 0.4684(3) 0.0715(14) Uani 1 1 d . . . H73A H 0.3198 0.3238 0.4883 0.086 Uiso 1 1 calc R C 5 Cl1 Cl 0.2297(3) 0.2896(3) 0.5339(3) 0.0554(11) Uiso 0.413(11) 1 d P D 5 Cl2 Cl 0.2323(2) 0.3656(3) 0.4196(2) 0.0554(11) Uiso 0.413(11) 1 d P D 5 Cl3 Cl 0.2955(2) 0.2369(2) 0.4299(4) 0.0554(11) Uiso 0.413(11) 1 d P D 5 Cl1A Cl 0.2062(7) 0.3407(7) 0.4885(7) 0.116(4) Uiso 0.140(3) 1 d P D 6 Cl2A Cl 0.2353(7) 0.2925(7) 0.3722(7) 0.116(4) Uiso 0.140(3) 1 d P D 6 Cl3A Cl 0.2610(7) 0.2183(7) 0.4882(7) 0.116(4) Uiso 0.140(3) 1 d P D 6 Cl1B Cl 0.2393(5) 0.2758(5) 0.5253(5) 0.0581(19) Uiso 0.192(8) 1 d P D 7 Cl2B Cl 0.2503(5) 0.3693(5) 0.4160(5) 0.0581(19) Uiso 0.192(8) 1 d P D 7 Cl3B Cl 0.2813(5) 0.2404(3) 0.4012(7) 0.0581(19) Uiso 0.192(8) 1 d P D 7 Cl1C Cl 0.2210(5) 0.3038(4) 0.5364(5) 0.0635(17) Uiso 0.238(9) 1 d P D 8 Cl2C Cl 0.2348(4) 0.3478(5) 0.4051(4) 0.0635(17) Uiso 0.238(9) 1 d P D 8 Cl3C Cl 0.2921(3) 0.2213(4) 0.4536(6) 0.0635(17) Uiso 0.238(9) 1 d P D 8 Cl4 Cl 0.18477(7) 0.57038(6) 0.36496(6) 0.0739(4) Uani 1 1 d . E . Cl5 Cl 0.20643(6) 0.54936(5) 0.22962(6) 0.0576(3) Uani 1 1 d . E . Cl6A Cl 0.176(3) 0.4435(6) 0.324(3) 0.108(10) Uani 0.27(4) 1 d P E 9 Cl6 Cl 0.1521(3) 0.4472(3) 0.2985(3) 0.0575(14) Uani 0.73(4) 1 d P E 10 C74 C 0.1568(2) 0.52915(18) 0.2918(2) 0.0462(10) Uani 1 1 d . . . H74A H 0.1102 0.5449 0.2764 0.055 Uiso 1 1 calc R E 10 Cl7 Cl 0.25030(11) 0.50295(11) 0.73744(8) 0.1307(7) Uani 1 1 d . . . Cl8 Cl 0.23956(8) 0.55285(6) 0.86741(7) 0.0854(4) Uani 1 1 d . . . Cl9 Cl 0.27088(7) 0.41914(6) 0.84923(7) 0.0747(4) Uani 1 1 d . . . C75 C 0.2266(2) 0.4863(2) 0.8149(2) 0.0631(13) Uani 1 1 d . . . H75A H 0.1775 0.4756 0.8089 0.076 Uiso 1 1 calc R . . Cl10 Cl 0.73366(9) 0.22808(12) 0.06191(8) 0.1332(8) Uani 1 1 d . . . Cl11 Cl 0.64941(16) 0.33405(8) 0.02163(11) 0.1895(14) Uani 1 1 d . . . Cl12 Cl 0.67432(9) 0.24124(10) -0.07149(8) 0.1207(7) Uani 1 1 d . . . C76 C 0.6634(2) 0.2532(2) 0.0107(3) 0.0685(14) Uani 1 1 d . . . H76A H 0.6234 0.2280 0.0209 0.082 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 Rh1 0.03215(16) 0.04595(18) 0.03211(17) 0.00313(13) 0.00810(12) -0.00462(14) O1 0.059(2) 0.136(3) 0.070(2) -0.025(2) 0.0337(19) -0.004(2) O2 0.046(2) 0.228(5) 0.060(2) 0.041(3) -0.0044(19) -0.002(3) N1 0.0359(16) 0.0252(14) 0.0252(15) 0.0039(12) 0.0067(12) 0.0004(13) N2 0.051(2) 0.0280(15) 0.0262(16) 0.0014(12) 0.0112(14) -0.0070(14) N3 0.0344(16) 0.0287(14) 0.0240(15) 0.0029(12) 0.0056(12) 0.0014(13) N4 0.0432(18) 0.0311(15) 0.0273(16) 0.0020(12) 0.0044(14) -0.0050(14) C1 0.0323(19) 0.0279(17) 0.033(2) -0.0042(15) 0.0091(16) -0.0007(15) C2 0.044(2) 0.044(2) 0.046(2) -0.0067(18) 0.0167(19) 0.0005(19) C3 0.040(3) 0.067(3) 0.068(3) -0.015(3) 0.015(2) 0.009(2) C4 0.042(3) 0.059(3) 0.069(3) -0.012(2) -0.002(2) 0.016(2) C5 0.053(3) 0.039(2) 0.043(2) -0.0042(18) 0.000(2) 0.0102(19) C6 0.038(2) 0.0281(17) 0.035(2) -0.0035(15) 0.0064(16) 0.0036(16) C7 0.035(2) 0.0251(16) 0.034(2) 0.0026(15) 0.0104(16) 0.0043(15) C8 0.040(2) 0.036(2) 0.042(2) -0.0042(17) 0.0062(18) 0.0029(17) C9 0.036(2) 0.043(2) 0.063(3) -0.013(2) 0.003(2) -0.0010(18) C10 0.035(2) 0.039(2) 0.083(3) -0.002(2) 0.020(2) -0.0083(18) C11 0.045(2) 0.0316(19) 0.055(3) 0.0032(18) 0.020(2) 0.0018(17) C12 0.036(2) 0.0223(16) 0.042(2) 0.0000(15) 0.0144(17) 0.0068(15) C13 0.039(2) 0.0272(17) 0.0221(17) 0.0011(14) 0.0089(15) -0.0014(15) C14 0.047(2) 0.0270(17) 0.0282(19) 0.0051(15) 0.0153(16) 0.0031(16) C15 0.0294(18) 0.0265(16) 0.0281(19) 0.0029(14) 0.0063(14) -0.0009(14) C16 0.0357(19) 0.0251(16) 0.0278(19) 0.0025(14) 0.0120(15) 0.0038(15) C17 0.035(2) 0.0285(17) 0.036(2) 0.0071(15) 0.0092(16) -0.0017(15) C18 0.042(2) 0.0278(17) 0.030(2) 0.0002(15) 0.0062(17) 0.0071(16) C19 0.044(2) 0.045(2) 0.040(2) 0.0060(18) 0.0032(19) 0.0089(19) C20 0.051(3) 0.068(3) 0.047(3) 0.004(2) -0.008(2) 0.021(2) C21 0.086(4) 0.056(3) 0.041(3) 0.017(2) 0.005(3) 0.023(3) C22 0.083(3) 0.034(2) 0.034(2) 0.0079(17) 0.006(2) 0.006(2) C23 0.060(3) 0.0224(16) 0.028(2) 0.0011(15) 0.0107(18) 0.0016(17) C24 0.075(3) 0.045(2) 0.041(2) 0.0044(19) 0.018(2) -0.019(2) C25 0.043(2) 0.0291(17) 0.0239(18) -0.0037(14) 0.0111(16) -0.0008(16) C26 0.050(2) 0.0268(17) 0.0263(19) 0.0030(14) 0.0075(17) 0.0058(16) C27 0.0337(19) 0.0321(18) 0.0236(18) 0.0015(15) -0.0010(15) 0.0012(15) C28 0.040(2) 0.0376(19) 0.031(2) -0.0004(16) 0.0072(16) -0.0037(17) C29 0.044(2) 0.052(2) 0.037(2) 0.0018(18) 0.0155(18) 0.0003(19) C30 0.053(3) 0.049(2) 0.039(2) -0.0067(19) 0.013(2) 0.009(2) C31 0.058(3) 0.0340(19) 0.038(2) -0.0014(17) 0.007(2) 0.0074(19) C32 0.039(2) 0.0341(18) 0.0272(19) -0.0005(15) 0.0043(16) -0.0007(16) C33 0.067(3) 0.0278(18) 0.047(3) 0.0044(17) 0.008(2) -0.0079(19) C34 0.034(2) 0.0337(18) 0.0277(19) 0.0041(15) -0.0012(15) -0.0013(15) C35 0.039(2) 0.077(3) 0.053(3) -0.009(2) 0.014(2) -0.010(2) C36 0.036(2) 0.116(4) 0.045(3) 0.024(3) 0.011(2) -0.001(3) Rh2 0.04319(18) 0.02870(15) 0.04043(18) 0.00517(13) 0.01157(14) 0.00638(13) O3 0.064(2) 0.0430(18) 0.159(4) 0.007(2) -0.006(2) 0.0183(17) O4 0.045(2) 0.0481(19) 0.161(4) -0.004(2) 0.008(2) 0.0027(17) N5 0.0462(19) 0.0332(15) 0.0251(16) -0.0027(13) 0.0007(14) -0.0019(14) N6 0.074(2) 0.0378(17) 0.0265(17) -0.0028(14) 0.0155(16) -0.0011(17) N7 0.0384(17) 0.0238(13) 0.0227(15) 0.0042(12) 0.0040(13) 0.0024(12) N8 0.0457(18) 0.0295(15) 0.0246(16) 0.0036(12) 0.0079(13) 0.0034(14) C37 0.0348(19) 0.0275(16) 0.0208(17) 0.0044(13) 0.0045(14) 0.0036(15) C38 0.040(2) 0.0322(19) 0.042(2) 0.0052(17) 0.0052(18) 0.0053(17) C39 0.038(2) 0.045(2) 0.069(3) 0.009(2) -0.005(2) 0.0063(19) C40 0.043(2) 0.054(3) 0.059(3) 0.003(2) -0.011(2) -0.009(2) C41 0.053(2) 0.0328(19) 0.032(2) -0.0007(16) -0.0029(18) -0.0016(18) C42 0.039(2) 0.0298(17) 0.0174(17) 0.0032(14) 0.0027(15) 0.0045(15) C43 0.037(2) 0.0342(18) 0.0279(19) 0.0089(15) 0.0045(16) 0.0039(16) C44 0.042(2) 0.041(2) 0.057(3) 0.0136(19) 0.013(2) 0.0019(19) C45 0.052(3) 0.059(3) 0.088(4) 0.030(3) 0.037(3) 0.007(2) C46 0.071(3) 0.069(3) 0.083(4) 0.028(3) 0.051(3) 0.031(3) C47 0.068(3) 0.043(2) 0.047(3) 0.0111(19) 0.027(2) 0.020(2) C48 0.041(2) 0.0335(18) 0.029(2) 0.0066(15) 0.0078(17) 0.0097(16) C49 0.0318(19) 0.0232(16) 0.0276(18) 0.0029(14) 0.0049(15) 0.0006(14) C50 0.046(2) 0.0222(16) 0.0226(18) -0.0013(14) 0.0047(15) 0.0063(15) C51 0.0341(19) 0.0241(16) 0.0220(17) 0.0002(13) 0.0029(14) 0.0026(14) C52 0.0350(19) 0.0238(16) 0.0227(18) 0.0024(13) -0.0002(14) 0.0038(14) C53 0.042(2) 0.0318(18) 0.0262(19) -0.0027(15) -0.0004(16) -0.0018(16) C54 0.062(3) 0.037(2) 0.024(2) 0.0010(16) -0.0035(18) -0.0058(19) C55 0.065(3) 0.048(2) 0.041(2) -0.0005(19) -0.001(2) -0.016(2) C56 0.075(3) 0.053(3) 0.050(3) -0.005(2) -0.003(2) -0.026(2) C57 0.113(5) 0.042(2) 0.051(3) -0.004(2) 0.004(3) -0.029(3) C58 0.115(4) 0.038(2) 0.037(3) -0.0120(19) 0.010(3) -0.011(3) C59 0.081(3) 0.0332(19) 0.026(2) -0.0003(16) 0.007(2) -0.006(2) C60 0.093(4) 0.055(3) 0.049(3) -0.010(2) 0.030(3) 0.006(3) C61 0.059(3) 0.0305(18) 0.0233(19) 0.0033(15) 0.0045(18) 0.0017(18) C62 0.043(2) 0.0255(16) 0.0225(18) 0.0004(14) 0.0027(15) -0.0001(15) C63 0.0350(19) 0.0251(16) 0.0242(18) 0.0059(14) 0.0035(15) -0.0053(15) C64 0.037(2) 0.0329(18) 0.034(2) 0.0069(16) 0.0060(16) -0.0003(16) C65 0.037(2) 0.0343(19) 0.043(2) 0.0127(17) 0.0062(17) 0.0044(17) C66 0.038(2) 0.044(2) 0.043(2) 0.0127(18) -0.0051(18) -0.0009(18) C67 0.043(2) 0.041(2) 0.027(2) 0.0084(16) -0.0020(17) -0.0032(18) C68 0.036(2) 0.0314(18) 0.0293(19) 0.0059(15) 0.0057(15) -0.0042(15) C69 0.072(3) 0.044(2) 0.025(2) 0.0023(17) 0.0135(19) 0.005(2) C70 0.039(2) 0.0277(17) 0.0266(19) 0.0049(15) 0.0081(16) -0.0027(15) C71 0.048(3) 0.037(2) 0.076(3) 0.004(2) 0.006(2) 0.006(2) C72 0.038(2) 0.036(2) 0.090(4) 0.007(2) 0.012(2) 0.009(2) F1 0.145(3) 0.092(2) 0.0527(18) 0.0259(16) 0.0113(18) 0.040(2) B1 0.084(4) 0.042(3) 0.033(3) 0.011(2) 0.020(3) 0.016(3) F2 0.067(4) 0.099(5) 0.059(5) 0.016(4) 0.025(3) -0.015(3) F3 0.074(5) 0.148(7) 0.105(7) -0.038(5) 0.031(4) -0.026(4) F4 0.225(12) 0.070(5) 0.055(4) 0.004(3) 0.027(6) 0.087(8) F2A 0.34(2) 0.110(9) 0.028(4) -0.015(5) 0.009(10) 0.126(13) F3A 0.059(4) 0.116(7) 0.084(5) -0.009(5) 0.002(3) -0.004(4) F4A 0.089(6) 0.064(4) 0.098(6) 0.022(4) 0.032(5) -0.004(4) B2 0.052(3) 0.034(2) 0.041(3) -0.006(2) 0.006(2) 0.005(2) F5 0.0571(15) 0.0577(15) 0.0598(16) -0.0218(12) 0.0044(12) -0.0022(12) F6 0.062(2) 0.0570(19) 0.070(2) 0.0034(15) 0.0099(16) -0.0196(15) F7 0.085(2) 0.0516(18) 0.057(2) 0.0118(14) -0.0244(17) -0.0055(16) F8 0.113(3) 0.0526(19) 0.056(2) -0.0109(15) 0.0285(18) 0.0293(18) C73 0.052(3) 0.065(3) 0.096(4) 0.017(3) 0.005(3) 0.005(2) Cl4 0.0910(10) 0.0758(8) 0.0551(7) -0.0002(6) 0.0104(7) -0.0347(7) Cl5 0.0614(7) 0.0496(6) 0.0675(7) 0.0071(5) 0.0299(6) 0.0033(5) Cl6A 0.146(18) 0.048(3) 0.15(2) 0.033(6) 0.093(18) 0.028(6) Cl6 0.068(2) 0.0320(15) 0.073(2) 0.0116(10) 0.0129(19) -0.0083(12) C74 0.045(2) 0.039(2) 0.057(3) 0.0031(19) 0.015(2) -0.0022(18) Cl7 0.1511(17) 0.1710(19) 0.0698(11) 0.0447(11) 0.0141(11) -0.0128(14) Cl8 0.0899(10) 0.0595(7) 0.0996(11) 0.0047(7) -0.0148(8) 0.0009(7) Cl9 0.0757(9) 0.0674(8) 0.0818(9) 0.0142(7) 0.0140(7) 0.0102(7) C75 0.047(3) 0.073(3) 0.067(3) 0.006(3) -0.002(2) -0.012(2) Cl10 0.0971(13) 0.229(2) 0.0693(11) 0.0391(12) -0.0046(9) -0.0123(14) Cl11 0.368(4) 0.0599(10) 0.177(2) -0.0140(11) 0.172(2) 0.0347(16) Cl12 0.1011(12) 0.1681(17) 0.0800(11) -0.0656(11) -0.0369(9) 0.0706(12) C76 0.059(3) 0.055(3) 0.092(4) -0.013(3) 0.012(3) 0.001(2) _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 Rh1 C36 1.874(5) . ? Rh1 C35 1.897(4) . ? Rh1 C34 2.063(3) . ? Rh1 C25 2.078(4) . ? O1 C35 1.132(5) . ? O2 C36 1.122(5) . ? N1 C25 1.356(4) . ? N1 C18 1.391(4) . ? N1 C17 1.465(4) . ? N2 C25 1.362(4) . ? N2 C23 1.377(5) . ? N2 C24 1.446(5) . ? N3 C34 1.355(4) . ? N3 C27 1.400(4) . ? N3 C26 1.475(4) . ? N4 C34 1.344(4) . ? N4 C32 1.388(4) . ? N4 C33 1.468(4) . ? C1 C2 1.371(5) . ? C1 C6 1.405(5) . ? C1 C13 1.500(5) . ? C2 C3 1.395(6) . ? C2 H2A 0.9500 . ? C3 C4 1.360(6) . ? C3 H3A 0.9500 . ? C4 C5 1.386(6) . ? C4 H4A 0.9500 . ? C5 C6 1.380(5) . ? C5 H5A 0.9500 . ? C6 C14 1.526(5) . ? C7 C8 1.381(5) . ? C7 C12 1.396(5) . ? C7 C13 1.511(5) . ? C8 C9 1.388(5) . ? C8 H8A 0.9500 . ? C9 C10 1.387(6) . ? C9 H9A 0.9500 . ? C10 C11 1.386(6) . ? C10 H10A 0.9500 . ? C11 C12 1.381(5) . ? C11 H11A 0.9500 . ? C12 C14 1.507(5) . ? C13 C15 1.557(4) . ? C13 H13A 1.0000 . ? C14 C16 1.558(4) . ? C14 H14A 1.0000 . ? C15 C17 1.526(4) . ? C15 C16 1.549(4) . ? C15 H15A 1.0000 . ? C16 C26 1.529(5) . ? C16 H16A 1.0000 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.382(5) . ? C18 C19 1.387(5) . ? C19 C20 1.380(5) . ? C19 H19A 0.9500 . ? C20 C21 1.376(6) . ? C20 H20A 0.9500 . ? C21 C22 1.373(6) . ? C21 H21A 0.9500 . ? C22 C23 1.405(5) . ? C22 H22A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.385(5) . ? C27 C32 1.388(4) . ? C28 C29 1.380(5) . ? C28 H28A 0.9500 . ? C29 C30 1.395(5) . ? C29 H29A 0.9500 . ? C30 C31 1.380(5) . ? C30 H30A 0.9500 . ? C31 C32 1.391(5) . ? C31 H31A 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Rh2 C72 1.882(5) . ? Rh2 C71 1.893(4) . ? Rh2 C70 2.064(3) . ? Rh2 C61 2.095(4) . ? O3 C71 1.121(5) . ? O4 C72 1.131(5) . ? N5 C61 1.355(4) . ? N5 C54 1.398(4) . ? N5 C53 1.476(4) . ? N6 C61 1.361(4) . ? N6 C59 1.399(5) . ? N6 C60 1.466(5) . ? N7 C70 1.362(4) . ? N7 C63 1.395(4) . ? N7 C62 1.464(4) . ? N8 C70 1.347(4) . ? N8 C68 1.384(4) . ? N8 C69 1.463(4) . ? C37 C38 1.379(5) . ? C37 C42 1.407(4) . ? C37 C49 1.506(5) . ? C38 C39 1.379(5) . ? C38 H38A 0.9500 . ? C39 C40 1.384(6) . ? C39 H39A 0.9500 . ? C40 C41 1.381(5) . ? C40 H40A 0.9500 . ? C41 C42 1.379(5) . ? C41 H41A 0.9500 . ? C42 C50 1.505(4) . ? C43 C44 1.384(5) . ? C43 C48 1.402(5) . ? C43 C49 1.506(4) . ? C44 C45 1.389(5) . ? C44 H44A 0.9500 . ? C45 C46 1.357(7) . ? C45 H45A 0.9500 . ? C46 C47 1.391(6) . ? C46 H46A 0.9500 . ? C47 C48 1.383(5) . ? C47 H47A 0.9500 . ? C48 C50 1.513(5) . ? C49 C51 1.549(4) . ? C49 H49A 1.0000 . ? C50 C52 1.553(4) . ? C50 H50A 1.0000 . ? C51 C53 1.524(5) . ? C51 C52 1.537(4) . ? C51 H51A 1.0000 . ? C52 C62 1.535(4) . ? C52 H52A 1.0000 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C59 1.376(5) . ? C54 C55 1.394(6) . ? C55 C56 1.381(5) . ? C55 H55A 0.9500 . ? C56 C57 1.387(7) . ? C56 H56A 0.9500 . ? C57 C58 1.350(7) . ? C57 H57A 0.9500 . ? C58 C59 1.394(5) . ? C58 H58A 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C68 1.386(4) . ? C63 C64 1.390(5) . ? C64 C65 1.390(5) . ? C64 H64A 0.9500 . ? C65 C66 1.394(5) . ? C65 H65A 0.9500 . ? C66 C67 1.380(5) . ? C66 H66A 0.9500 . ? C67 C68 1.394(5) . ? C67 H67A 0.9500 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? F1 B1 1.336(5) . ? B1 F2A 1.216(8) . ? B1 F4 1.319(7) . ? B1 F2 1.396(8) . ? B1 F4A 1.430(9) . ? B1 F3A 1.460(8) . ? B1 F3 1.477(9) . ? B2 F8 1.366(3) . ? B2 F8' 1.371(4) . ? B2 F7 1.373(3) . ? B2 F7' 1.373(4) . ? B2 F5 1.375(3) . ? B2 F6' 1.384(4) . ? B2 F6 1.393(3) . ? C73 Cl1B 1.570(10) . ? C73 Cl3 1.670(6) . ? C73 Cl1A 1.689(14) . ? C73 Cl2C 1.698(8) . ? C73 Cl2B 1.752(10) . ? C73 Cl1 1.754(8) . ? C73 Cl2 1.772(6) . ? C73 Cl3C 1.779(9) . ? C73 Cl3A 1.857(15) . ? C73 Cl1C 1.884(10) . ? C73 Cl3B 1.916(11) . ? C73 Cl2A 2.040(15) . ? C73 H73A 1.0000 . ? Cl4 C74 1.747(4) . ? Cl5 C74 1.761(4) . ? Cl6A C74 1.91(2) . ? Cl6 C74 1.703(7) . ? C74 H74A 1.0000 . ? Cl7 C75 1.742(5) . ? Cl8 C75 1.742(5) . ? Cl9 C75 1.744(5) . ? C75 H75A 1.0000 . ? Cl10 C76 1.719(5) . ? Cl11 C76 1.715(5) . ? Cl12 C76 1.737(5) . ? C76 H76A 1.0000 . ? 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 C36 Rh1 C35 94.23(19) . . ? C36 Rh1 C34 86.77(16) . . ? C35 Rh1 C34 176.40(17) . . ? C36 Rh1 C25 170.64(19) . . ? C35 Rh1 C25 89.34(16) . . ? C34 Rh1 C25 90.19(13) . . ? C25 N1 C18 110.5(3) . . ? C25 N1 C17 125.5(3) . . ? C18 N1 C17 123.8(3) . . ? C25 N2 C23 110.5(3) . . ? C25 N2 C24 125.8(3) . . ? C23 N2 C24 123.7(3) . . ? C34 N3 C27 110.6(3) . . ? C34 N3 C26 126.5(3) . . ? C27 N3 C26 122.9(3) . . ? C34 N4 C32 111.1(3) . . ? C34 N4 C33 124.8(3) . . ? C32 N4 C33 124.1(3) . . ? C2 C1 C6 120.1(3) . . ? C2 C1 C13 126.9(3) . . ? C6 C1 C13 113.1(3) . . ? C1 C2 C3 119.0(4) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 120.7(4) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 119.0(4) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C14 126.7(3) . . ? C1 C6 C14 113.1(3) . . ? C8 C7 C12 120.8(3) . . ? C8 C7 C13 126.1(3) . . ? C12 C7 C13 113.0(3) . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 119.5(4) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C7 119.8(4) . . ? C11 C12 C14 126.6(3) . . ? C7 C12 C14 113.6(3) . . ? C1 C13 C7 107.1(3) . . ? C1 C13 C15 104.9(3) . . ? C7 C13 C15 108.4(3) . . ? C1 C13 H13A 112.0 . . ? C7 C13 H13A 112.0 . . ? C15 C13 H13A 112.0 . . ? C12 C14 C6 106.2(3) . . ? C12 C14 C16 107.1(3) . . ? C6 C14 C16 107.2(3) . . ? C12 C14 H14A 112.0 . . ? C6 C14 H14A 112.0 . . ? C16 C14 H14A 112.0 . . ? C17 C15 C16 112.1(3) . . ? C17 C15 C13 115.7(3) . . ? C16 C15 C13 110.6(3) . . ? C17 C15 H15A 105.9 . . ? C16 C15 H15A 105.9 . . ? C13 C15 H15A 105.9 . . ? C26 C16 C15 111.7(3) . . ? C26 C16 C14 111.9(3) . . ? C15 C16 C14 108.3(2) . . ? C26 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C14 C16 H16A 108.3 . . ? N1 C17 C15 113.3(3) . . ? N1 C17 H17A 108.9 . . ? C15 C17 H17A 108.9 . . ? N1 C17 H17B 108.9 . . ? C15 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C23 C18 C19 121.4(3) . . ? C23 C18 N1 106.1(3) . . ? C19 C18 N1 132.5(3) . . ? C20 C19 C18 116.1(4) . . ? C20 C19 H19A 121.9 . . ? C18 C19 H19A 121.9 . . ? C21 C20 C19 122.6(4) . . ? C21 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? C22 C21 C20 122.3(4) . . ? C22 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C21 C22 C23 115.5(4) . . ? C21 C22 H22A 122.3 . . ? C23 C22 H22A 122.3 . . ? N2 C23 C18 106.9(3) . . ? N2 C23 C22 130.9(4) . . ? C18 C23 C22 122.2(4) . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 N2 105.9(3) . . ? N1 C25 Rh1 128.9(2) . . ? N2 C25 Rh1 125.1(3) . . ? N3 C26 C16 112.9(3) . . ? N3 C26 H26A 109.0 . . ? C16 C26 H26A 109.0 . . ? N3 C26 H26B 109.0 . . ? C16 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C32 121.6(3) . . ? C28 C27 N3 132.7(3) . . ? C32 C27 N3 105.7(3) . . ? C29 C28 C27 116.6(3) . . ? C29 C28 H28A 121.7 . . ? C27 C28 H28A 121.7 . . ? C28 C29 C30 122.0(3) . . ? C28 C29 H29A 119.0 . . ? C30 C29 H29A 119.0 . . ? C31 C30 C29 121.4(3) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 116.7(3) . . ? C30 C31 H31A 121.7 . . ? C32 C31 H31A 121.7 . . ? C27 C32 N4 106.3(3) . . ? C27 C32 C31 121.7(3) . . ? N4 C32 C31 131.9(3) . . ? N4 C33 H33A 109.5 . . ? N4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 N3 106.3(3) . . ? N4 C34 Rh1 127.3(2) . . ? N3 C34 Rh1 126.4(2) . . ? O1 C35 Rh1 177.3(4) . . ? O2 C36 Rh1 175.2(6) . . ? C72 Rh2 C71 92.33(17) . . ? C72 Rh2 C70 87.53(15) . . ? C71 Rh2 C70 179.54(17) . . ? C72 Rh2 C61 177.52(16) . . ? C71 Rh2 C61 89.35(16) . . ? C70 Rh2 C61 90.78(14) . . ? C61 N5 C54 111.3(3) . . ? C61 N5 C53 125.4(3) . . ? C54 N5 C53 123.0(3) . . ? C61 N6 C59 110.9(3) . . ? C61 N6 C60 126.0(4) . . ? C59 N6 C60 123.1(3) . . ? C70 N7 C63 109.9(3) . . ? C70 N7 C62 126.3(3) . . ? C63 N7 C62 123.8(3) . . ? C70 N8 C68 110.8(3) . . ? C70 N8 C69 124.1(3) . . ? C68 N8 C69 125.2(3) . . ? C38 C37 C42 119.7(3) . . ? C38 C37 C49 126.7(3) . . ? C42 C37 C49 113.1(3) . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C38 C39 C40 119.9(4) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C41 C40 C39 120.8(4) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C42 C41 C40 119.6(3) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? C41 C42 C37 119.9(3) . . ? C41 C42 C50 126.8(3) . . ? C37 C42 C50 113.2(3) . . ? C44 C43 C48 120.1(3) . . ? C44 C43 C49 126.7(3) . . ? C48 C43 C49 113.2(3) . . ? C43 C44 C45 119.1(4) . . ? C43 C44 H44A 120.5 . . ? C45 C44 H44A 120.5 . . ? C46 C45 C44 120.7(4) . . ? C46 C45 H45A 119.6 . . ? C44 C45 H45A 119.6 . . ? C45 C46 C47 121.2(4) . . ? C45 C46 H46A 119.4 . . ? C47 C46 H46A 119.4 . . ? C48 C47 C46 118.9(4) . . ? C48 C47 H47A 120.6 . . ? C46 C47 H47A 120.6 . . ? C47 C48 C43 120.0(3) . . ? C47 C48 C50 126.9(3) . . ? C43 C48 C50 113.2(3) . . ? C43 C49 C37 108.4(3) . . ? C43 C49 C51 108.8(3) . . ? C37 C49 C51 102.2(2) . . ? C43 C49 H49A 112.3 . . ? C37 C49 H49A 112.3 . . ? C51 C49 H49A 112.3 . . ? C42 C50 C48 108.1(3) . . ? C42 C50 C52 106.5(3) . . ? C48 C50 C52 105.4(3) . . ? C42 C50 H50A 112.1 . . ? C48 C50 H50A 112.1 . . ? C52 C50 H50A 112.1 . . ? C53 C51 C52 112.9(3) . . ? C53 C51 C49 113.9(3) . . ? C52 C51 C49 110.4(3) . . ? C53 C51 H51A 106.3 . . ? C52 C51 H51A 106.3 . . ? C49 C51 H51A 106.3 . . ? C62 C52 C51 110.6(3) . . ? C62 C52 C50 111.2(3) . . ? C51 C52 C50 108.7(2) . . ? C62 C52 H52A 108.8 . . ? C51 C52 H52A 108.8 . . ? C50 C52 H52A 108.8 . . ? N5 C53 C51 111.8(3) . . ? N5 C53 H53A 109.3 . . ? C51 C53 H53A 109.3 . . ? N5 C53 H53B 109.3 . . ? C51 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C59 C54 C55 121.6(4) . . ? C59 C54 N5 106.1(3) . . ? C55 C54 N5 132.3(4) . . ? C56 C55 C54 116.5(4) . . ? C56 C55 H55A 121.7 . . ? C54 C55 H55A 121.7 . . ? C55 C56 C57 121.1(5) . . ? C55 C56 H56A 119.4 . . ? C57 C56 H56A 119.4 . . ? C58 C57 C56 122.4(4) . . ? C58 C57 H57A 118.8 . . ? C56 C57 H57A 118.8 . . ? C57 C58 C59 117.3(4) . . ? C57 C58 H58A 121.4 . . ? C59 C58 H58A 121.4 . . ? C54 C59 C58 121.0(4) . . ? C54 C59 N6 106.4(3) . . ? C58 C59 N6 132.6(4) . . ? N6 C60 H60A 109.5 . . ? N6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N5 C61 N6 105.3(3) . . ? N5 C61 Rh2 127.0(2) . . ? N6 C61 Rh2 127.4(3) . . ? N7 C62 C52 113.5(3) . . ? N7 C62 H62A 108.9 . . ? C52 C62 H62A 108.9 . . ? N7 C62 H62B 108.9 . . ? C52 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? C68 C63 C64 122.3(3) . . ? C68 C63 N7 106.3(3) . . ? C64 C63 N7 131.4(3) . . ? C63 C64 C65 116.0(3) . . ? C63 C64 H64A 122.0 . . ? C65 C64 H64A 122.0 . . ? C64 C65 C66 121.5(3) . . ? C64 C65 H65A 119.2 . . ? C66 C65 H65A 119.2 . . ? C67 C66 C65 122.4(3) . . ? C67 C66 H66A 118.8 . . ? C65 C66 H66A 118.8 . . ? C66 C67 C68 116.1(3) . . ? C66 C67 H67A 122.0 . . ? C68 C67 H67A 122.0 . . ? N8 C68 C63 106.5(3) . . ? N8 C68 C67 131.7(3) . . ? C63 C68 C67 121.7(3) . . ? N8 C69 H69A 109.5 . . ? N8 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N8 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N8 C70 N7 106.5(3) . . ? N8 C70 Rh2 126.4(2) . . ? N7 C70 Rh2 127.0(2) . . ? O3 C71 Rh2 178.1(4) . . ? O4 C72 Rh2 175.4(4) . . ? F2A B1 F4 119.2(6) . . ? F2A B1 F1 119.3(6) . . ? F4 B1 F1 121.6(5) . . ? F2A B1 F2 49.4(9) . . ? F4 B1 F2 113.0(7) . . ? F1 B1 F2 105.3(5) . . ? F2A B1 F4A 116.5(9) . . ? F4 B1 F4A 47.0(5) . . ? F1 B1 F4A 105.3(5) . . ? F2 B1 F4A 78.1(5) . . ? F2A B1 F3A 116.2(11) . . ? F4 B1 F3A 58.4(6) . . ? F1 B1 F3A 94.2(4) . . ? F2 B1 F3A 159.9(6) . . ? F4A B1 F3A 102.0(6) . . ? F2A B1 F3 51.7(9) . . ? F4 B1 F3 102.0(8) . . ? F1 B1 F3 112.2(5) . . ? F2 B1 F3 101.0(5) . . ? F4A B1 F3 141.1(6) . . ? F3A B1 F3 66.1(5) . . ? F8 B2 F8' 63(2) . . ? F8 B2 F7 112.3(3) . . ? F8' B2 F7 138.1(8) . . ? F8 B2 F7' 139.3(7) . . ? F8' B2 F7' 110.2(4) . . ? F7 B2 F7' 44(2) . . ? F8 B2 F5 110.1(2) . . ? F8' B2 F5 109.9(4) . . ? F7 B2 F5 110.3(2) . . ? F7' B2 F5 109.7(3) . . ? F8 B2 F6' 49(2) . . ? F8' B2 F6' 109.4(3) . . ? F7 B2 F6' 68(2) . . ? F7' B2 F6' 109.2(3) . . ? F5 B2 F6' 108.3(3) . . ? F8 B2 F6 108.2(2) . . ? F8' B2 F6 48(2) . . ? F7 B2 F6 107.6(2) . . ? F7' B2 F6 66(2) . . ? F5 B2 F6 108.1(2) . . ? F6' B2 F6 142.3(7) . . ? Cl1B C73 Cl3 101.2(5) . . ? Cl1B C73 Cl1A 60.1(6) . . ? Cl3 C73 Cl1A 137.5(6) . . ? Cl1B C73 Cl2C 122.1(6) . . ? Cl3 C73 Cl2C 101.8(4) . . ? Cl1A C73 Cl2C 67.1(6) . . ? Cl1B C73 Cl2B 127.5(7) . . ? Cl3 C73 Cl2B 115.0(6) . . ? Cl1A C73 Cl2B 67.5(6) . . ? Cl2C C73 Cl2B 18.9(4) . . ? Cl1B C73 Cl1 12.2(4) . . ? Cl3 C73 Cl1 113.1(3) . . ? Cl1A C73 Cl1 49.5(6) . . ? Cl2C C73 Cl1 114.6(4) . . ? Cl2B C73 Cl1 116.9(5) . . ? Cl1B C73 Cl2 115.9(5) . . ? Cl3 C73 Cl2 117.5(4) . . ? Cl1A C73 Cl2 56.7(5) . . ? Cl2C C73 Cl2 15.7(3) . . ? Cl2B C73 Cl2 12.5(3) . . ? Cl1 C73 Cl2 106.1(3) . . ? Cl1B C73 Cl3C 82.8(6) . . ? Cl3 C73 Cl3C 19.5(3) . . ? Cl1A C73 Cl3C 130.1(6) . . ? Cl2C C73 Cl3C 117.6(4) . . ? Cl2B C73 Cl3C 133.0(6) . . ? Cl1 C73 Cl3C 95.0(4) . . ? Cl2 C73 Cl3C 133.0(4) . . ? Cl1B C73 Cl3A 51.2(6) . . ? Cl3 C73 Cl3A 50.0(5) . . ? Cl1A C73 Cl3A 102.0(7) . . ? Cl2C C73 Cl3A 126.5(6) . . ? Cl2B C73 Cl3A 145.4(7) . . ? Cl1 C73 Cl3A 63.2(6) . . ? Cl2 C73 Cl3A 136.4(6) . . ? Cl3C C73 Cl3A 31.9(5) . . ? Cl1B C73 Cl1C 22.3(4) . . ? Cl3 C73 Cl1C 122.4(4) . . ? Cl1A C73 Cl1C 40.3(5) . . ? Cl2C C73 Cl1C 106.7(5) . . ? Cl2B C73 Cl1C 107.3(5) . . ? Cl1 C73 Cl1C 10.1(3) . . ? Cl2 C73 Cl1C 97.0(4) . . ? Cl3C C73 Cl1C 104.7(4) . . ? Cl3A C73 Cl1C 72.9(6) . . ? Cl1B C73 Cl3B 110.2(5) . . ? Cl3 C73 Cl3B 18.4(3) . . ? Cl1A C73 Cl3B 127.2(6) . . ? Cl2C C73 Cl3B 83.5(6) . . ? Cl2B C73 Cl3B 97.6(6) . . ? Cl1 C73 Cl3B 120.7(4) . . ? Cl2 C73 Cl3B 99.2(5) . . ? Cl3C C73 Cl3B 35.6(5) . . ? Cl3A C73 Cl3B 61.4(6) . . ? Cl1C C73 Cl3B 127.9(4) . . ? Cl1B C73 Cl2A 119.9(6) . . ? Cl3 C73 Cl2A 62.4(5) . . ? Cl1A C73 Cl2A 92.6(6) . . ? Cl2C C73 Cl2A 40.3(5) . . ? Cl2B C73 Cl2A 57.0(6) . . ? Cl1 C73 Cl2A 121.8(5) . . ? Cl2 C73 Cl2A 55.8(5) . . ? Cl3C C73 Cl2A 77.3(6) . . ? Cl3A C73 Cl2A 92.2(6) . . ? Cl1C C73 Cl2A 120.5(5) . . ? Cl3B C73 Cl2A 44.1(5) . . ? Cl1B C73 H73A 108.7 . . ? Cl3 C73 H73A 106.5 . . ? Cl1A C73 H73A 115.6 . . ? Cl2C C73 H73A 114.2 . . ? Cl2B C73 H73A 96.4 . . ? Cl1 C73 H73A 106.5 . . ? Cl2 C73 H73A 106.5 . . ? Cl3C C73 H73A 106.9 . . ? Cl3A C73 H73A 117.2 . . ? Cl1C C73 H73A 105.6 . . ? Cl3B C73 H73A 116.3 . . ? Cl2A C73 H73A 131.2 . . ? Cl6 C74 Cl4 115.5(3) . . ? Cl6 C74 Cl5 109.7(3) . . ? Cl4 C74 Cl5 110.6(2) . . ? Cl6 C74 Cl6A 20.1(19) . . ? Cl4 C74 Cl6A 97.7(19) . . ? Cl5 C74 Cl6A 110.9(4) . . ? Cl6 C74 H74A 106.9 . . ? Cl4 C74 H74A 106.9 . . ? Cl5 C74 H74A 106.9 . . ? Cl6A C74 H74A 123.3 . . ? Cl7 C75 Cl8 111.5(3) . . ? Cl7 C75 Cl9 109.7(3) . . ? Cl8 C75 Cl9 110.7(3) . . ? Cl7 C75 H75A 108.3 . . ? Cl8 C75 H75A 108.3 . . ? Cl9 C75 H75A 108.3 . . ? Cl11 C76 Cl10 110.5(3) . . ? Cl11 C76 Cl12 107.9(3) . . ? Cl10 C76 Cl12 110.3(3) . . ? Cl11 C76 H76A 109.4 . . ? Cl10 C76 H76A 109.4 . . ? Cl12 C76 H76A 109.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.142 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.078