# 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 'Barbara Messerle' _publ_contact_author_email B.MESSERLE@UNSW.EDU.AU _publ_section_title ; Weakly Coordinating Counter-Ions for Highly Efficient Catalysis of Intramolecular Hydroamination ; loop_ _publ_author_name 'Barbara Messerle' 'Serin L. Dabb' 'Joanne H. H. Ho' 'Richard Hodgeson' 'Jorg Wagler' # Attachment 'jh00101.cif' data_jh00101 _database_code_depnum_ccdc_archive 'CCDC 697500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C15 H20 Ir N4' _chemical_formula_sum 'C47 H32 B F24 Ir N4' _chemical_formula_weight 1311.78 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' B B 0.0013 0.0007 '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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9389(3) _cell_length_b 15.8085(2) _cell_length_c 20.8606(4) _cell_angle_alpha 107.5120(10) _cell_angle_beta 92.1280(10) _cell_angle_gamma 91.1660(10) _cell_volume 4692.34(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 130305 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 30.034 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 2.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_T_max 0.436 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 90419 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 30.00 _reflns_number_total 27296 _reflns_number_gt 20484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+1.8161P] 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 27296 _refine_ls_number_parameters 1475 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.145 _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 0.078967(10) 0.796600(10) 0.001080(7) 0.02221(5) Uani 1 1 d . . . N1 N 0.0800(2) 0.6936(2) -0.08897(17) 0.0203(6) Uani 1 1 d . . . N2 N 0.1587(2) 0.6693(2) -0.11999(17) 0.0209(7) Uani 1 1 d . . . N3 N 0.2517(2) 0.7978(2) -0.06945(18) 0.0268(7) Uani 1 1 d . . . N4 N 0.1929(2) 0.8504(2) -0.02960(18) 0.0258(7) Uani 1 1 d . . . C1 C 0.1170(3) 0.8626(3) 0.1030(2) 0.0364(11) Uani 1 1 d . . . H1 H 0.1770 0.8633 0.0895 0.044 Uiso 1 1 calc R . . C2 C 0.0563(4) 0.9142(4) 0.0802(3) 0.0481(15) Uani 1 1 d . . . H2 H 0.0766 0.9460 0.0511 0.058 Uiso 1 1 calc R . . C3 C -0.0411(4) 0.9219(4) 0.1000(3) 0.0582(18) Uani 1 1 d . . . H3A H -0.0610 0.9824 0.1033 0.070 Uiso 1 1 calc R . . H3B H -0.0453 0.9135 0.1449 0.070 Uiso 1 1 calc R . . C4 C -0.1034(4) 0.8541(4) 0.0497(3) 0.0569(18) Uani 1 1 d . . . H4A H -0.1546 0.8393 0.0736 0.068 Uiso 1 1 calc R . . H4B H -0.1275 0.8808 0.0157 0.068 Uiso 1 1 calc R . . C5 C -0.0575(3) 0.7703(4) 0.0146(2) 0.0386(12) Uani 1 1 d . . . H5 H -0.0649 0.7484 -0.0331 0.046 Uiso 1 1 calc R . . C6 C -0.0042(3) 0.7218(3) 0.0471(2) 0.0328(10) Uani 1 1 d . . . H6 H 0.0246 0.6710 0.0203 0.039 Uiso 1 1 calc R . . C7 C 0.0095(3) 0.7469(4) 0.1232(2) 0.0417(12) Uani 1 1 d . . . H7A H 0.0137 0.6923 0.1369 0.050 Uiso 1 1 calc R . . H7B H -0.0428 0.7795 0.1445 0.050 Uiso 1 1 calc R . . C8 C 0.0950(3) 0.8049(4) 0.1479(2) 0.0411(12) Uani 1 1 d . . . H8A H 0.0874 0.8437 0.1943 0.049 Uiso 1 1 calc R . . H8B H 0.1459 0.7662 0.1492 0.049 Uiso 1 1 calc R . . C9 C 0.0162(3) 0.6446(3) -0.1315(2) 0.0261(8) Uani 1 1 d . . . H9 H -0.0462 0.6483 -0.1243 0.031 Uiso 1 1 calc R . . C10 C 0.0537(3) 0.5871(3) -0.1881(2) 0.0302(9) Uani 1 1 d . . . H10 H 0.0229 0.5447 -0.2250 0.036 Uiso 1 1 calc R . . C11 C 0.1447(3) 0.6050(3) -0.1789(2) 0.0281(9) Uani 1 1 d . . . H11 H 0.1893 0.5770 -0.2087 0.034 Uiso 1 1 calc R . . C12 C 0.2429(3) 0.7024(3) -0.0837(2) 0.0259(8) Uani 1 1 d . . . H12A H 0.2932 0.6738 -0.1108 0.031 Uiso 1 1 calc R . . H12B H 0.2457 0.6873 -0.0409 0.031 Uiso 1 1 calc R . . C13 C 0.3169(3) 0.8473(4) -0.0867(3) 0.0396(12) Uani 1 1 d . . . H13 H 0.3660 0.8253 -0.1137 0.048 Uiso 1 1 calc R . . C14 C 0.2987(4) 0.9333(3) -0.0582(3) 0.0460(14) Uani 1 1 d . . . H14 H 0.3322 0.9834 -0.0615 0.055 Uiso 1 1 calc R . . C15 C 0.2213(4) 0.9340(3) -0.0230(3) 0.0372(11) Uani 1 1 d . . . H15 H 0.1927 0.9860 0.0020 0.045 Uiso 1 1 calc R . . Ir2 Ir 0.567675(10) 0.293009(9) 0.505806(7) 0.02102(5) Uani 1 1 d . . . N5 N 0.5761(2) 0.1933(2) 0.41443(17) 0.0190(6) Uani 1 1 d . . . N6 N 0.6566(2) 0.1743(2) 0.38513(17) 0.0216(7) Uani 1 1 d . . . N7 N 0.7384(2) 0.3099(2) 0.43754(18) 0.0268(8) Uani 1 1 d . . . N8 N 0.6745(3) 0.3566(2) 0.47715(19) 0.0290(8) Uani 1 1 d . . . C16 C 0.6027(3) 0.3594(3) 0.6086(2) 0.0332(10) Uani 1 1 d . . . H16 H 0.6619 0.3667 0.5955 0.040 Uiso 1 1 calc R . . C17 C 0.5338(4) 0.4056(3) 0.5869(2) 0.0394(12) Uani 1 1 d . . . H17 H 0.5493 0.4403 0.5585 0.047 Uiso 1 1 calc R . . C18 C 0.4369(4) 0.4035(4) 0.6057(3) 0.0475(14) Uani 1 1 d . . . H18A H 0.4110 0.4620 0.6098 0.057 Uiso 1 1 calc R . . H18B H 0.4346 0.3931 0.6501 0.057 Uiso 1 1 calc R . . C19 C 0.3802(3) 0.3317(4) 0.5541(3) 0.0433(13) Uani 1 1 d . . . H19A H 0.3315 0.3110 0.5772 0.052 Uiso 1 1 calc R . . H19B H 0.3522 0.3575 0.5208 0.052 Uiso 1 1 calc R . . C20 C 0.4341(3) 0.2533(3) 0.5178(2) 0.0286(9) Uani 1 1 d . . . H20 H 0.4277 0.2325 0.4700 0.034 Uiso 1 1 calc R . . C21 C 0.4934(3) 0.2088(3) 0.5500(2) 0.0257(8) Uani 1 1 d . . . H21 H 0.5262 0.1614 0.5228 0.031 Uiso 1 1 calc R . . C22 C 0.5074(3) 0.2331(3) 0.6260(2) 0.0315(10) Uani 1 1 d . . . H22A H 0.5178 0.1787 0.6389 0.038 Uiso 1 1 calc R . . H22B H 0.4526 0.2602 0.6475 0.038 Uiso 1 1 calc R . . C23 C 0.5878(3) 0.2988(3) 0.6518(2) 0.0339(10) Uani 1 1 d . . . H23A H 0.5779 0.3355 0.6984 0.041 Uiso 1 1 calc R . . H23B H 0.6426 0.2649 0.6528 0.041 Uiso 1 1 calc R . . C24 C 0.5160(3) 0.1406(3) 0.3704(2) 0.0243(8) Uani 1 1 d . . . H24 H 0.4532 0.1403 0.3763 0.029 Uiso 1 1 calc R . . C25 C 0.5575(3) 0.0861(3) 0.3148(2) 0.0279(9) Uani 1 1 d . . . H25 H 0.5298 0.0423 0.2773 0.034 Uiso 1 1 calc R . . C26 C 0.6468(3) 0.1096(3) 0.3260(2) 0.0265(9) Uani 1 1 d . . . H26 H 0.6934 0.0847 0.2971 0.032 Uiso 1 1 calc R . . C27 C 0.7376(3) 0.2143(3) 0.4227(2) 0.0279(9) Uani 1 1 d . . . H27A H 0.7901 0.1904 0.3964 0.033 Uiso 1 1 calc R . . H27B H 0.7420 0.1989 0.4653 0.033 Uiso 1 1 calc R . . C28 C 0.7975(3) 0.3649(4) 0.4209(3) 0.0390(12) Uani 1 1 d . . . H28 H 0.8482 0.3476 0.3944 0.047 Uiso 1 1 calc R . . C29 C 0.7711(4) 0.4496(4) 0.4490(3) 0.0480(15) Uani 1 1 d . . . H29 H 0.7988 0.5026 0.4456 0.058 Uiso 1 1 calc R . . C30 C 0.6950(4) 0.4421(3) 0.4837(2) 0.0374(11) Uani 1 1 d . . . H30 H 0.6620 0.4909 0.5087 0.045 Uiso 1 1 calc R . . B1 B 0.6108(3) 0.6926(3) 0.9280(2) 0.0151(7) Uani 1 1 d . . . C31 C 0.6530(2) 0.7763(2) 0.90620(18) 0.0161(7) Uani 1 1 d . . . C32 C 0.7362(2) 0.7744(2) 0.87678(19) 0.0193(7) Uani 1 1 d . . . H32 H 0.7722 0.7243 0.8720 0.023 Uiso 1 1 calc R . . C33 C 0.7676(2) 0.8438(2) 0.85430(19) 0.0179(7) Uani 1 1 d . . . C34 C 0.7167(3) 0.9175(2) 0.85913(19) 0.0201(7) Uani 1 1 d . . . H34 H 0.7373 0.9640 0.8427 0.024 Uiso 1 1 calc R . . C35 C 0.6344(3) 0.9212(2) 0.88882(19) 0.0194(7) Uani 1 1 d . . . C36 C 0.6042(2) 0.8532(2) 0.91265(18) 0.0178(7) Uani 1 1 d . . . H36 H 0.5486 0.8588 0.9340 0.021 Uiso 1 1 calc R . . C37 C 0.8595(3) 0.8374(3) 0.8259(2) 0.0254(8) Uani 1 1 d . . . F37A F 0.87396(19) 0.75779(18) 0.78376(16) 0.0406(7) Uani 1 1 d . . . F37B F 0.92318(17) 0.8525(2) 0.87562(16) 0.0392(7) Uani 1 1 d . . . F37C F 0.87500(18) 0.89759(19) 0.79392(15) 0.0374(7) Uani 1 1 d . . . C38 C 0.5772(3) 0.9997(3) 0.8927(2) 0.0269(9) Uani 1 1 d . . . F38A F 0.5337(2) 1.02554(19) 0.94884(14) 0.0396(7) Uani 1 1 d . . . F38B F 0.5181(2) 0.9833(2) 0.84248(16) 0.0526(9) Uani 1 1 d . . . F38C F 0.6253(2) 1.07085(19) 0.8905(2) 0.0564(10) Uani 1 1 d . . . C39 C 0.5306(2) 0.6409(2) 0.87419(17) 0.0156(7) Uani 1 1 d . . . C40 C 0.4983(2) 0.5563(2) 0.87518(18) 0.0171(7) Uani 1 1 d . . . H40 H 0.5239 0.5309 0.9072 0.021 Uiso 1 1 calc R . . C41 C 0.4302(2) 0.5095(2) 0.83067(18) 0.0166(7) Uani 1 1 d . . . C42 C 0.3912(2) 0.5433(2) 0.78240(18) 0.0174(7) Uani 1 1 d . . . H42 H 0.3451 0.5109 0.7517 0.021 Uiso 1 1 calc R . . C43 C 0.4219(2) 0.6261(3) 0.78051(18) 0.0183(7) Uani 1 1 d . . . C44 C 0.4905(2) 0.6734(3) 0.82501(19) 0.0175(7) Uani 1 1 d . . . H44 H 0.5105 0.7293 0.8218 0.021 Uiso 1 1 calc R . . C45 C 0.3998(3) 0.4182(3) 0.8322(2) 0.0244(8) Uani 1 1 d . . . F45A F 0.40852(18) 0.41035(16) 0.89435(13) 0.0283(5) Uani 1 1 d . . . F45B F 0.3154(2) 0.3985(2) 0.81100(16) 0.0422(7) Uani 1 1 d . . . F45C F 0.4500(2) 0.35563(17) 0.79291(16) 0.0468(8) Uani 1 1 d . . . C46 C 0.3793(3) 0.6650(3) 0.7295(2) 0.0247(8) Uani 1 1 d . . . F46A F 0.4197(2) 0.6431(3) 0.67214(16) 0.0644(11) Uani 1 1 d . . . F46B F 0.29606(19) 0.6371(3) 0.71281(19) 0.0631(11) Uani 1 1 d . . . F46C F 0.3803(3) 0.7513(2) 0.75011(19) 0.0803(15) Uani 1 1 d . . . C47 C 0.5716(2) 0.7322(2) 1.00372(18) 0.0159(7) Uani 1 1 d . . . C48 C 0.4880(2) 0.7090(2) 1.02234(18) 0.0177(7) Uani 1 1 d . . . H48 H 0.4484 0.6707 0.9890 0.021 Uiso 1 1 calc R . . C49 C 0.4609(2) 0.7402(2) 1.08849(19) 0.0188(7) Uani 1 1 d . . . C50 C 0.5167(3) 0.7949(2) 1.13930(19) 0.0193(7) Uani 1 1 d . . . H50 H 0.4984 0.8151 1.1844 0.023 Uiso 1 1 calc R . . C51 C 0.5996(3) 0.8192(2) 1.12229(19) 0.0197(7) Uani 1 1 d . . . C52 C 0.6260(2) 0.7901(2) 1.05617(19) 0.0177(7) Uani 1 1 d . . . H52 H 0.6827 0.8099 1.0459 0.021 Uiso 1 1 calc R . . C53 C 0.3711(3) 0.7098(3) 1.1047(2) 0.0291(9) Uani 1 1 d . . . F53A F 0.3528(2) 0.7399(3) 1.16853(15) 0.0585(10) Uani 1 1 d . . . F53B F 0.3631(3) 0.6224(2) 1.0875(2) 0.0844(16) Uani 1 1 d . . . F53C F 0.3041(2) 0.7345(3) 1.07200(18) 0.0646(11) Uani 1 1 d . . . C54 C 0.6649(3) 0.8741(3) 1.1752(2) 0.0287(9) Uani 1 1 d . . . F54A F 0.6367(2) 0.8907(2) 1.23715(13) 0.0437(7) Uani 1 1 d . . . F54B F 0.7435(2) 0.8366(3) 1.17391(16) 0.0616(11) Uani 1 1 d . . . F54C F 0.6816(3) 0.9545(2) 1.16757(19) 0.0700(12) Uani 1 1 d . . . C55 C 0.6884(2) 0.6206(2) 0.92837(18) 0.0160(7) Uani 1 1 d . C . C56 C 0.7295(2) 0.6095(2) 0.98671(19) 0.0184(7) Uani 1 1 d . . . H56 H 0.7114 0.6447 1.0294 0.022 Uiso 1 1 calc R . . C57 C 0.7968(3) 0.5478(3) 0.9839(2) 0.0221(8) Uani 1 1 d . C . C58 C 0.8254(3) 0.4949(3) 0.9230(2) 0.0223(8) Uani 1 1 d . . . H58 H 0.8712 0.4536 0.9212 0.027 Uiso 1 1 calc R A 1 C60 C 0.7175(2) 0.5652(2) 0.86680(19) 0.0186(7) Uani 1 1 d . . . H60 H 0.6909 0.5695 0.8259 0.022 Uiso 1 1 calc R B 1 C61 C 0.8331(3) 0.5346(3) 1.0478(2) 0.0286(9) Uani 1 1 d . . . F61A F 0.7792(2) 0.47890(19) 1.06825(15) 0.0453(8) Uani 1 1 d . C . F61B F 0.9144(2) 0.5003(2) 1.04225(16) 0.0554(10) Uani 1 1 d . C . F61C F 0.84031(18) 0.60966(17) 1.09877(13) 0.0316(6) Uani 1 1 d . C . C59A C 0.7847(3) 0.5042(3) 0.8645(2) 0.0213(8) Uani 0.70 1 d PD C 1 C62A C 0.8138(2) 0.4533(2) 0.79632(12) 0.0328(11) Uani 0.70 1 d PGD C 1 F62A F 0.7490(2) 0.4215(2) 0.75117(12) 0.0623(15) Uani 0.70 1 d PRU C 1 F62B F 0.8743(2) 0.3949(2) 0.79626(12) 0.083(2) Uani 0.70 1 d PRU C 1 F62C F 0.8524(2) 0.5042(2) 0.76574(12) 0.0589(14) Uani 0.70 1 d PRU C 1 C59B C 0.7847(3) 0.5042(3) 0.8645(2) 0.0213(8) Uani 0.30 1 d PD C 2 C62B C 0.8116(5) 0.4431(4) 0.7988(2) 0.0328(11) Uani 0.30 1 d PGD C 2 F62D F 0.7691(5) 0.3662(4) 0.7833(2) 0.066(3) Uani 0.30 1 d PRU C 2 F62E F 0.8958(5) 0.4226(4) 0.7991(2) 0.048(3) Uani 0.30 1 d PRU C 2 F62F F 0.8068(5) 0.4754(4) 0.7481(2) 0.108(6) Uani 0.30 1 d PRU C 2 B2 B 0.1041(3) 0.1935(3) 0.4311(2) 0.0153(7) Uani 1 1 d . . . C63 C 0.0242(2) 0.1420(2) 0.37642(18) 0.0159(7) Uani 1 1 d . F . C64 C -0.0060(2) 0.0564(2) 0.37488(18) 0.0164(7) Uani 1 1 d . . . H64 H 0.0201 0.0302 0.4062 0.020 Uiso 1 1 calc R . . C65 C -0.0724(2) 0.0091(2) 0.32926(18) 0.0165(7) Uani 1 1 d . F . C66 C -0.1134(2) 0.0442(2) 0.28228(18) 0.0171(7) Uani 1 1 d . . . H66 H -0.1586 0.0116 0.2508 0.021 Uiso 1 1 calc R D 1 C68 C -0.0180(2) 0.1768(2) 0.32871(18) 0.0166(7) Uani 1 1 d . . . H68 H -0.0002 0.2343 0.3274 0.020 Uiso 1 1 calc R E 1 C69 C -0.0993(3) -0.0842(3) 0.3282(2) 0.0231(8) Uani 1 1 d . . . F69A F -0.08947(18) -0.09444(16) 0.38977(13) 0.0275(5) Uani 1 1 d . F . F69B F -0.0479(2) -0.14374(17) 0.28805(15) 0.0455(8) Uani 1 1 d . F . F69C F -0.1840(2) -0.10537(19) 0.30756(16) 0.0419(7) Uani 1 1 d . F . C67A C -0.0853(2) 0.1288(2) 0.28346(18) 0.0169(7) Uani 0.50 1 d PD F 1 C70A C -0.1296(2) 0.1700(2) 0.23526(16) 0.0235(8) Uani 0.50 1 d PGD F 1 F70A F -0.1597(2) 0.2486(2) 0.26666(16) 0.0523(18) Uani 0.50 1 d PRU F 1 F70B F -0.0788(2) 0.1787(2) 0.18735(16) 0.0457(17) Uani 0.50 1 d PRU F 1 F70C F -0.1996(2) 0.1218(2) 0.20332(16) 0.0488(18) Uani 0.50 1 d PRU F 1 C67B C -0.0853(2) 0.1288(2) 0.28346(18) 0.0169(7) Uani 0.50 1 d PD F 2 C70B C -0.1284(2) 0.1707(3) 0.23524(17) 0.0235(8) Uani 0.50 1 d PGD F 2 F70D F -0.1103(2) 0.2562(3) 0.24855(17) 0.0557(19) Uani 0.50 1 d PRU F 2 F70E F -0.1004(2) 0.1383(3) 0.17391(17) 0.0499(19) Uani 0.50 1 d PRU F 2 F70F F -0.2157(2) 0.1578(3) 0.22527(17) 0.0455(17) Uani 0.50 1 d PRU F 2 C71 C 0.0645(2) 0.2312(2) 0.50639(18) 0.0158(7) Uani 1 1 d . I . C72 C -0.0195(2) 0.2079(2) 0.52462(19) 0.0183(7) Uani 1 1 d . . . H72 H -0.0593 0.1706 0.4908 0.022 Uiso 1 1 calc R G 1 C74 C 0.0093(3) 0.2913(2) 0.64211(19) 0.0194(7) Uani 1 1 d . . . H74 H -0.0088 0.3104 0.6872 0.023 Uiso 1 1 calc R H 1 C75 C 0.0924(2) 0.3162(2) 0.62540(19) 0.0177(7) Uani 1 1 d . I . C76 C 0.1187(2) 0.2881(2) 0.55919(19) 0.0192(7) Uani 1 1 d . . . H76 H 0.1754 0.3082 0.5492 0.023 Uiso 1 1 calc R I . C73A C -0.0468(2) 0.2375(3) 0.5907(2) 0.0200(7) Uani 0.42 1 d PDU I 1 C77A C -0.1408(2) 0.2184(3) 0.6061(3) 0.0318(12) Uani 0.42 1 d PGD I 1 F77A F -0.1564(2) 0.2210(3) 0.6686(3) 0.078(5) Uani 0.42 1 d PRU I 1 F77B F -0.1800(2) 0.1470(3) 0.5630(3) 0.0491(19) Uani 0.42 1 d PRU I 1 F77C F -0.1976(2) 0.2764(3) 0.5955(3) 0.060(2) Uani 0.42 1 d PRU I 1 C73B C -0.0468(2) 0.2375(3) 0.5907(2) 0.0200(7) Uani 0.58 1 d PD I 2 C77B C -0.13444(18) 0.2013(2) 0.60551(19) 0.0318(12) Uani 0.58 1 d PGD I 2 F77D F -0.14962(18) 0.2305(2) 0.67038(19) 0.048(2) Uani 0.58 1 d PRU I 2 F77E F -0.13600(18) 0.1140(2) 0.59135(19) 0.0664(19) Uani 0.58 1 d PRU I 2 F77F F -0.20394(18) 0.2261(2) 0.57521(19) 0.0585(17) Uani 0.58 1 d PRU I 2 C78 C 0.1583(3) 0.3688(3) 0.6791(2) 0.0280(9) Uani 1 1 d . . . F78A F 0.1266(2) 0.3915(2) 0.74044(13) 0.0409(7) Uani 1 1 d . I . F78B F 0.2327(2) 0.3259(3) 0.68163(16) 0.0564(10) Uani 1 1 d . I . F78C F 0.1842(3) 0.4459(2) 0.66850(17) 0.0613(11) Uani 1 1 d . I . C79 C 0.1823(2) 0.1219(2) 0.43034(18) 0.0151(7) Uani 1 1 d . . . C80 C 0.2221(2) 0.1079(2) 0.48808(19) 0.0184(7) Uani 1 1 d . . . H80 H 0.2024 0.1406 0.5310 0.022 Uiso 1 1 calc R . . C81 C 0.2901(3) 0.0471(2) 0.48419(19) 0.0189(7) Uani 1 1 d . . . C82 C 0.3215(3) -0.0023(3) 0.4226(2) 0.0210(8) Uani 1 1 d . . . H82 H 0.3681 -0.0430 0.4201 0.025 Uiso 1 1 calc R . . C83 C 0.2819(2) 0.0102(2) 0.36476(19) 0.0186(7) Uani 1 1 d . . . C84 C 0.2142(2) 0.0701(2) 0.36843(19) 0.0177(7) Uani 1 1 d . . . H84 H 0.1884 0.0765 0.3279 0.021 Uiso 1 1 calc R . . C85 C 0.3253(3) 0.0310(3) 0.5475(2) 0.0248(8) Uani 1 1 d . . . F85A F 0.4061(2) -0.0049(2) 0.54173(15) 0.0487(8) Uani 1 1 d . . . F85B F 0.33288(18) 0.10465(17) 0.59972(12) 0.0283(5) Uani 1 1 d . . . F85C F 0.2699(2) -0.02527(18) 0.56640(14) 0.0413(7) Uani 1 1 d . . . C86 C 0.3136(3) -0.0395(3) 0.2965(2) 0.0302(10) Uani 1 1 d . . . F86A F 0.2491(2) -0.0725(3) 0.25205(16) 0.0638(11) Uani 1 1 d . . . F86B F 0.3549(2) 0.0156(2) 0.26825(16) 0.0615(10) Uani 1 1 d . . . F86C F 0.3737(3) -0.0976(3) 0.29780(17) 0.0839(16) Uani 1 1 d . . . C87 C 0.1455(2) 0.2780(2) 0.40992(18) 0.0177(7) Uani 1 1 d . L . C88 C 0.2290(2) 0.2789(2) 0.38209(19) 0.0188(7) Uani 1 1 d . . . H88 H 0.2670 0.2304 0.3783 0.023 Uiso 1 1 calc R . . C89 C 0.2583(3) 0.3493(3) 0.3597(2) 0.0232(8) Uani 1 1 d . L . C90 C 0.2058(3) 0.4214(3) 0.3642(2) 0.0270(9) Uani 1 1 d . . . H90 H 0.2254 0.4685 0.3482 0.032 Uiso 1 1 calc R J 1 C92 C 0.0942(3) 0.3535(2) 0.41630(19) 0.0206(7) Uani 1 1 d . . . H92 H 0.0383 0.3572 0.4370 0.025 Uiso 1 1 calc R K 1 C93 C 0.3508(3) 0.3454(3) 0.3330(2) 0.0289(9) Uani 1 1 d . . . F93A F 0.41340(19) 0.3630(2) 0.38415(16) 0.0452(7) Uani 1 1 d . L . F93B F 0.3685(2) 0.26637(19) 0.29163(16) 0.0447(8) Uani 1 1 d . L . F93C F 0.3664(2) 0.4053(2) 0.30109(17) 0.0460(8) Uani 1 1 d . L . C91A C 0.1232(3) 0.4229(3) 0.3931(2) 0.0259(9) Uani 0.60 1 d PD L 1 C94A C 0.0709(2) 0.50381(19) 0.3980(2) 0.0352(12) Uani 0.60 1 d PGD L 1 F94A F 0.0187(2) 0.48984(19) 0.3444(2) 0.079(2) Uani 0.60 1 d PRU L 1 F94B F 0.0289(2) 0.52767(19) 0.4537(2) 0.0527(15) Uani 0.60 1 d PRU L 1 F94C F 0.1183(2) 0.57452(19) 0.4000(2) 0.0692(18) Uani 0.60 1 d PRU L 1 C91B C 0.1232(3) 0.4229(3) 0.3931(2) 0.0259(9) Uani 0.40 1 d PD L 2 C94B C 0.0596(3) 0.4956(3) 0.3966(3) 0.0352(12) Uani 0.40 1 d PGD L 2 F94D F 0.0454(3) 0.5179(3) 0.3421(3) 0.054(2) Uani 0.40 1 d PRU L 2 F94E F 0.0748(3) 0.5669(3) 0.4470(3) 0.0426(18) Uani 0.40 1 d PRU L 2 F94F F -0.0236(3) 0.4810(3) 0.4075(3) 0.067(2) Uani 0.40 1 d PRU L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02315(8) 0.02100(9) 0.01898(9) 0.00083(6) -0.00201(6) 0.00472(6) N1 0.0190(15) 0.0186(16) 0.0218(17) 0.0041(13) -0.0024(13) 0.0008(12) N2 0.0235(16) 0.0185(16) 0.0206(16) 0.0055(13) 0.0015(13) 0.0018(12) N3 0.0266(17) 0.0302(19) 0.0251(18) 0.0115(15) -0.0038(14) -0.0051(14) N4 0.0309(18) 0.0212(17) 0.0253(18) 0.0083(14) -0.0067(15) -0.0061(14) C1 0.035(2) 0.044(3) 0.020(2) -0.007(2) -0.0016(18) -0.003(2) C2 0.059(3) 0.034(3) 0.036(3) -0.014(2) -0.003(3) 0.017(2) C3 0.054(4) 0.060(4) 0.044(3) -0.012(3) -0.001(3) 0.029(3) C4 0.035(3) 0.083(5) 0.040(3) -0.003(3) 0.001(2) 0.030(3) C5 0.024(2) 0.059(3) 0.026(2) 0.000(2) 0.0034(18) 0.008(2) C6 0.0225(19) 0.047(3) 0.025(2) 0.004(2) 0.0039(17) -0.0022(18) C7 0.030(2) 0.066(4) 0.026(2) 0.010(2) 0.0065(19) -0.007(2) C8 0.028(2) 0.071(4) 0.020(2) 0.009(2) -0.0005(18) -0.002(2) C9 0.0253(19) 0.023(2) 0.027(2) 0.0037(17) -0.0017(16) 0.0003(15) C10 0.035(2) 0.027(2) 0.024(2) 0.0024(18) -0.0017(18) -0.0019(18) C11 0.033(2) 0.026(2) 0.021(2) 0.0008(17) -0.0004(17) 0.0030(17) C12 0.0255(19) 0.028(2) 0.025(2) 0.0088(17) -0.0007(16) 0.0010(16) C13 0.036(2) 0.054(3) 0.031(2) 0.018(2) -0.006(2) -0.021(2) C14 0.067(4) 0.038(3) 0.035(3) 0.019(2) -0.011(3) -0.029(3) C15 0.058(3) 0.020(2) 0.032(2) 0.0085(19) -0.015(2) -0.009(2) Ir2 0.02549(9) 0.01793(9) 0.01781(9) 0.00288(6) -0.00217(6) 0.00262(6) N5 0.0187(14) 0.0184(15) 0.0195(16) 0.0050(13) -0.0007(12) 0.0017(12) N6 0.0202(15) 0.0255(17) 0.0193(16) 0.0068(14) 0.0005(13) 0.0038(13) N7 0.0284(17) 0.031(2) 0.0224(17) 0.0123(15) -0.0054(14) -0.0090(15) N8 0.040(2) 0.0212(18) 0.0252(19) 0.0069(15) -0.0067(16) -0.0007(15) C16 0.042(3) 0.034(2) 0.018(2) 0.0008(18) -0.0072(19) -0.008(2) C17 0.063(3) 0.026(2) 0.022(2) -0.0049(18) 0.001(2) 0.009(2) C18 0.060(4) 0.043(3) 0.035(3) 0.005(2) 0.006(3) 0.025(3) C19 0.039(3) 0.059(3) 0.028(2) 0.005(2) 0.002(2) 0.030(2) C20 0.0190(18) 0.041(3) 0.021(2) 0.0021(18) 0.0012(15) 0.0071(17) C21 0.0237(19) 0.028(2) 0.024(2) 0.0064(17) 0.0055(16) -0.0014(16) C22 0.029(2) 0.037(2) 0.028(2) 0.0085(19) 0.0034(18) 0.0030(18) C23 0.027(2) 0.052(3) 0.022(2) 0.010(2) 0.0010(17) 0.003(2) C24 0.0252(19) 0.023(2) 0.022(2) 0.0037(16) 0.0003(16) 0.0013(15) C25 0.034(2) 0.027(2) 0.0182(19) -0.0004(16) -0.0006(17) 0.0016(17) C26 0.028(2) 0.029(2) 0.021(2) 0.0040(17) 0.0029(16) 0.0068(16) C27 0.0234(19) 0.037(2) 0.027(2) 0.0166(19) -0.0057(17) -0.0025(17) C28 0.038(2) 0.052(3) 0.033(3) 0.025(2) -0.012(2) -0.025(2) C29 0.066(4) 0.043(3) 0.038(3) 0.020(2) -0.015(3) -0.031(3) C30 0.057(3) 0.028(2) 0.027(2) 0.0107(19) -0.008(2) -0.016(2) B1 0.0171(17) 0.0162(18) 0.0140(18) 0.0074(15) -0.0001(14) 0.0012(14) C31 0.0171(15) 0.0167(17) 0.0136(16) 0.0037(13) -0.0017(13) 0.0000(13) C32 0.0199(17) 0.0183(18) 0.0210(18) 0.0077(15) -0.0001(14) 0.0013(13) C33 0.0188(16) 0.0194(18) 0.0163(17) 0.0061(14) 0.0025(14) 0.0010(13) C34 0.0262(18) 0.0167(18) 0.0191(18) 0.0081(15) 0.0000(15) -0.0015(14) C35 0.0257(18) 0.0178(18) 0.0161(17) 0.0072(14) 0.0009(15) 0.0037(14) C36 0.0191(16) 0.0179(17) 0.0164(17) 0.0048(14) 0.0022(14) 0.0020(13) C37 0.0240(19) 0.027(2) 0.029(2) 0.0129(18) 0.0061(16) -0.0001(16) F37A 0.0362(15) 0.0298(14) 0.0511(18) 0.0030(13) 0.0217(14) 0.0000(11) F37B 0.0196(12) 0.0558(18) 0.0466(17) 0.0226(15) -0.0011(12) -0.0030(12) F37C 0.0341(14) 0.0416(16) 0.0483(17) 0.0292(14) 0.0187(13) 0.0026(12) C38 0.036(2) 0.026(2) 0.023(2) 0.0133(18) 0.0072(18) 0.0100(17) F38A 0.0470(17) 0.0425(16) 0.0364(16) 0.0187(13) 0.0199(14) 0.0275(13) F38B 0.056(2) 0.057(2) 0.0403(18) 0.0079(16) -0.0138(15) 0.0304(16) F38C 0.0471(18) 0.0329(16) 0.103(3) 0.0375(18) 0.0270(19) 0.0118(14) C39 0.0180(16) 0.0176(17) 0.0117(16) 0.0051(13) 0.0019(13) 0.0025(13) C40 0.0217(17) 0.0167(17) 0.0137(16) 0.0055(14) 0.0022(13) 0.0035(13) C41 0.0202(16) 0.0176(17) 0.0121(16) 0.0043(13) 0.0012(13) 0.0021(13) C42 0.0170(15) 0.0204(18) 0.0134(16) 0.0026(14) 0.0002(13) 0.0040(13) C43 0.0176(16) 0.0247(19) 0.0131(16) 0.0063(14) -0.0008(13) 0.0065(14) C44 0.0167(16) 0.0201(18) 0.0166(17) 0.0071(15) -0.0008(13) 0.0032(13) C45 0.031(2) 0.024(2) 0.0193(19) 0.0088(16) -0.0019(16) -0.0037(16) F45A 0.0370(14) 0.0263(13) 0.0246(13) 0.0129(10) -0.0007(11) -0.0057(10) F45B 0.0417(16) 0.0441(17) 0.0438(17) 0.0217(14) -0.0197(14) -0.0239(13) F45C 0.083(2) 0.0158(13) 0.0408(17) 0.0043(12) 0.0263(17) 0.0088(13) C46 0.0245(19) 0.028(2) 0.026(2) 0.0144(17) -0.0024(16) 0.0023(15) F46A 0.065(2) 0.112(3) 0.0396(18) 0.054(2) 0.0199(17) 0.039(2) F46B 0.0285(15) 0.110(3) 0.078(3) 0.074(2) -0.0224(16) -0.0153(17) F46C 0.147(4) 0.0300(17) 0.060(2) 0.0122(17) -0.057(3) 0.023(2) C47 0.0193(16) 0.0147(16) 0.0147(16) 0.0062(13) -0.0011(13) 0.0032(13) C48 0.0188(16) 0.0196(18) 0.0139(17) 0.0042(14) -0.0006(13) 0.0015(13) C49 0.0170(16) 0.0207(18) 0.0202(18) 0.0078(15) 0.0034(14) 0.0043(13) C50 0.0233(17) 0.0188(18) 0.0147(17) 0.0031(14) 0.0007(14) 0.0072(14) C51 0.0273(18) 0.0153(17) 0.0155(17) 0.0031(14) -0.0017(15) 0.0034(14) C52 0.0188(16) 0.0166(17) 0.0179(17) 0.0058(14) -0.0016(14) 0.0007(13) C53 0.026(2) 0.035(2) 0.022(2) 0.0018(18) 0.0084(17) -0.0048(17) F53A 0.0358(16) 0.104(3) 0.0250(16) 0.0039(17) 0.0099(13) -0.0159(18) F53B 0.072(3) 0.044(2) 0.127(4) 0.005(2) 0.063(3) -0.0195(18) F53C 0.0236(15) 0.125(3) 0.054(2) 0.041(2) -0.0007(14) 0.0018(18) C54 0.029(2) 0.035(2) 0.019(2) 0.0032(18) -0.0010(17) -0.0021(18) F54A 0.0440(16) 0.0592(19) 0.0163(13) -0.0051(13) -0.0005(12) -0.0102(14) F54B 0.0342(16) 0.092(3) 0.0336(17) -0.0171(17) -0.0163(13) 0.0169(17) F54C 0.102(3) 0.053(2) 0.054(2) 0.0224(18) -0.032(2) -0.048(2) C55 0.0189(16) 0.0157(17) 0.0149(17) 0.0069(14) 0.0012(13) -0.0005(13) C56 0.0206(17) 0.0172(17) 0.0201(18) 0.0096(15) -0.0005(14) 0.0023(13) C57 0.0219(18) 0.025(2) 0.0220(19) 0.0106(16) 0.0003(15) 0.0022(15) C58 0.0201(17) 0.0216(19) 0.027(2) 0.0102(16) 0.0001(15) 0.0062(14) C60 0.0201(17) 0.0209(18) 0.0166(17) 0.0085(15) 0.0010(14) 0.0006(14) C61 0.033(2) 0.029(2) 0.027(2) 0.0127(18) -0.0010(18) 0.0124(17) F61A 0.077(2) 0.0323(15) 0.0353(16) 0.0249(13) -0.0099(15) -0.0067(14) F61B 0.057(2) 0.077(2) 0.0344(17) 0.0182(16) -0.0024(15) 0.0464(18) F61C 0.0400(14) 0.0318(14) 0.0222(13) 0.0077(11) -0.0072(11) 0.0052(11) C59A 0.0228(18) 0.024(2) 0.0174(18) 0.0060(15) 0.0053(15) 0.0052(15) C62A 0.029(2) 0.047(3) 0.023(2) 0.010(2) 0.0078(18) 0.017(2) F62A 0.041(2) 0.084(3) 0.031(2) -0.029(2) -0.0074(19) 0.017(2) F62B 0.094(4) 0.088(4) 0.054(3) 0.000(3) -0.001(3) 0.056(3) F62C 0.062(3) 0.072(3) 0.036(2) 0.005(2) 0.020(2) -0.004(2) C59B 0.0228(18) 0.024(2) 0.0174(18) 0.0060(15) 0.0053(15) 0.0052(15) C62B 0.029(2) 0.047(3) 0.023(2) 0.010(2) 0.0078(18) 0.017(2) F62D 0.063(5) 0.061(5) 0.054(5) -0.013(4) 0.032(4) -0.027(4) F62E 0.029(4) 0.062(5) 0.034(4) -0.017(3) 0.010(3) 0.018(4) F62F 0.121(8) 0.112(7) 0.096(7) 0.038(5) 0.001(5) 0.025(5) B2 0.0179(17) 0.0144(18) 0.0124(17) 0.0022(14) -0.0008(14) 0.0048(14) C63 0.0169(15) 0.0172(17) 0.0150(16) 0.0064(14) 0.0025(13) 0.0032(13) C64 0.0185(16) 0.0178(17) 0.0144(16) 0.0069(14) 0.0021(13) 0.0038(13) C65 0.0197(16) 0.0155(17) 0.0139(16) 0.0034(13) 0.0017(13) 0.0031(13) C66 0.0141(15) 0.0224(18) 0.0154(17) 0.0064(14) 0.0005(13) 0.0030(13) C68 0.0197(16) 0.0151(17) 0.0161(17) 0.0059(14) 0.0025(14) 0.0039(13) C69 0.0254(19) 0.0224(19) 0.0208(19) 0.0059(16) -0.0012(16) -0.0041(15) F69A 0.0377(14) 0.0255(13) 0.0229(13) 0.0131(10) -0.0014(11) -0.0043(10) F69B 0.079(2) 0.0190(13) 0.0375(16) 0.0045(12) 0.0277(16) 0.0081(13) F69C 0.0435(16) 0.0397(16) 0.0463(18) 0.0229(14) -0.0184(14) -0.0210(13) C67A 0.0157(15) 0.0216(18) 0.0146(16) 0.0072(14) 0.0003(13) 0.0037(13) C70A 0.0199(17) 0.028(2) 0.025(2) 0.0124(17) -0.0008(15) 0.0050(15) F70A 0.064(4) 0.048(3) 0.040(3) 0.007(3) -0.010(3) 0.038(3) F70B 0.036(3) 0.072(4) 0.053(3) 0.052(3) 0.017(3) 0.009(3) F70C 0.052(3) 0.038(3) 0.061(4) 0.026(3) -0.030(3) -0.007(3) C67B 0.0157(15) 0.0216(18) 0.0146(16) 0.0072(14) 0.0003(13) 0.0037(13) C70B 0.0199(17) 0.028(2) 0.025(2) 0.0124(17) -0.0008(15) 0.0050(15) F70D 0.072(4) 0.040(3) 0.062(4) 0.030(3) -0.033(3) -0.005(3) F70E 0.067(4) 0.061(4) 0.031(3) 0.027(3) 0.005(3) 0.025(3) F70F 0.025(2) 0.065(4) 0.066(4) 0.051(3) -0.003(3) 0.008(3) C71 0.0195(16) 0.0136(16) 0.0149(16) 0.0050(13) 0.0003(13) 0.0044(12) C72 0.0234(17) 0.0165(17) 0.0146(17) 0.0042(14) -0.0008(14) 0.0036(13) C74 0.0263(18) 0.0171(17) 0.0144(17) 0.0036(14) 0.0015(14) 0.0072(14) C75 0.0212(17) 0.0158(17) 0.0148(17) 0.0028(14) -0.0020(14) 0.0027(13) C76 0.0209(17) 0.0190(18) 0.0163(17) 0.0031(14) 0.0015(14) 0.0034(14) C73A 0.0181(16) 0.0229(18) 0.0197(17) 0.0071(14) 0.0025(14) 0.0027(13) C77A 0.028(2) 0.039(3) 0.021(2) -0.001(2) 0.0062(19) -0.007(2) F77A 0.069(6) 0.103(7) 0.065(7) 0.030(5) 0.016(4) -0.014(4) F77B 0.042(3) 0.055(4) 0.040(3) 0.000(3) 0.019(3) -0.028(3) F77C 0.034(3) 0.068(4) 0.077(5) 0.019(4) 0.001(3) 0.000(3) C73B 0.0181(16) 0.0229(18) 0.0197(17) 0.0071(14) 0.0025(14) 0.0027(13) C77B 0.028(2) 0.039(3) 0.021(2) -0.001(2) 0.0062(19) -0.007(2) F77D 0.031(3) 0.088(4) 0.019(3) 0.007(3) 0.011(2) -0.015(3) F77E 0.058(3) 0.046(3) 0.092(4) 0.014(3) 0.031(3) -0.017(2) F77F 0.034(3) 0.093(4) 0.048(3) 0.020(3) -0.006(2) -0.004(3) C78 0.030(2) 0.030(2) 0.0175(19) -0.0016(17) -0.0015(16) -0.0004(17) F78A 0.0426(16) 0.0510(18) 0.0165(13) -0.0085(12) 0.0026(11) -0.0089(13) F78B 0.0346(16) 0.081(3) 0.0323(17) -0.0140(16) -0.0148(13) 0.0146(16) F78C 0.086(3) 0.053(2) 0.0411(19) 0.0141(16) -0.0189(18) -0.047(2) C79 0.0156(15) 0.0147(16) 0.0159(17) 0.0059(13) -0.0007(13) 0.0006(12) C80 0.0199(17) 0.0210(18) 0.0153(17) 0.0067(14) 0.0025(14) 0.0050(14) C81 0.0231(17) 0.0187(18) 0.0168(17) 0.0086(15) -0.0024(14) 0.0023(14) C82 0.0227(18) 0.0184(18) 0.0214(19) 0.0052(15) 0.0002(15) 0.0048(14) C83 0.0211(17) 0.0197(18) 0.0142(17) 0.0032(14) 0.0038(14) 0.0045(14) C84 0.0205(17) 0.0161(17) 0.0166(17) 0.0049(14) 0.0028(14) 0.0022(13) C85 0.035(2) 0.0203(19) 0.0195(19) 0.0068(16) -0.0005(16) 0.0082(16) F85A 0.0512(18) 0.066(2) 0.0308(16) 0.0150(15) -0.0014(14) 0.0397(16) F85B 0.0372(14) 0.0295(13) 0.0175(12) 0.0066(10) -0.0048(10) 0.0049(10) F85C 0.070(2) 0.0280(14) 0.0319(15) 0.0204(12) -0.0063(14) -0.0073(13) C86 0.025(2) 0.042(3) 0.019(2) 0.0007(18) 0.0046(16) 0.0100(18) F86A 0.0426(18) 0.090(3) 0.0328(17) -0.0213(18) 0.0019(14) -0.0004(18) F86B 0.064(2) 0.082(3) 0.0362(18) 0.0114(17) 0.0236(17) -0.0051(19) F86C 0.121(4) 0.099(3) 0.0349(19) 0.017(2) 0.021(2) 0.091(3) C87 0.0226(17) 0.0170(17) 0.0136(16) 0.0054(14) -0.0032(14) 0.0017(13) C88 0.0217(17) 0.0198(18) 0.0167(17) 0.0090(14) -0.0025(14) -0.0009(14) C89 0.030(2) 0.0216(19) 0.0181(18) 0.0060(15) -0.0003(16) -0.0050(15) C90 0.044(2) 0.0182(19) 0.0198(19) 0.0080(16) -0.0023(18) -0.0053(17) C92 0.0288(19) 0.0161(17) 0.0173(18) 0.0055(14) -0.0008(15) 0.0055(14) C93 0.033(2) 0.027(2) 0.030(2) 0.0134(18) 0.0046(18) -0.0050(17) F93A 0.0288(14) 0.064(2) 0.0475(19) 0.0243(16) -0.0008(13) -0.0097(13) F93B 0.0425(16) 0.0355(16) 0.0515(19) 0.0040(14) 0.0228(15) -0.0061(12) F93C 0.0467(17) 0.0505(18) 0.0535(19) 0.0345(16) 0.0101(15) -0.0101(14) C91A 0.046(2) 0.0137(18) 0.0195(19) 0.0069(15) 0.0025(18) 0.0087(16) C94A 0.055(3) 0.021(2) 0.033(3) 0.012(2) 0.008(3) 0.012(2) F94A 0.098(4) 0.071(4) 0.058(4) 0.006(3) -0.029(3) 0.048(3) F94B 0.063(3) 0.053(3) 0.041(3) 0.010(2) 0.010(3) 0.032(3) F94C 0.072(3) 0.036(3) 0.107(4) 0.032(3) 0.005(3) 0.012(2) C91B 0.046(2) 0.0137(18) 0.0195(19) 0.0069(15) 0.0025(18) 0.0087(16) C94B 0.055(3) 0.021(2) 0.033(3) 0.012(2) 0.008(3) 0.012(2) F94D 0.085(5) 0.042(4) 0.036(4) 0.011(3) -0.007(3) 0.035(4) F94E 0.051(4) 0.036(3) 0.037(3) 0.003(3) -0.001(3) 0.022(3) F94F 0.058(4) 0.045(4) 0.116(5) 0.050(4) 0.009(4) 0.016(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 Ir1 N1 2.084(3) . ? Ir1 N4 2.093(4) . ? Ir1 C1 2.117(4) . ? Ir1 C5 2.118(4) . ? Ir1 C2 2.125(5) . ? Ir1 C6 2.139(5) . ? N1 C9 1.337(5) . ? N1 N2 1.370(4) . ? N2 C11 1.345(5) . ? N2 C12 1.447(5) . ? N3 N4 1.350(5) . ? N3 C13 1.361(5) . ? N3 C12 1.449(5) . ? N4 C15 1.346(5) . ? C1 C2 1.394(8) . ? C1 C8 1.532(7) . ? C1 H1 0.9500 . ? C2 C3 1.524(8) . ? C2 H2 0.9500 . ? C3 C4 1.526(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.500(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.407(7) . ? C5 H5 0.9500 . ? C6 C7 1.521(6) . ? C6 H6 0.9500 . ? C7 C8 1.535(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.399(6) . ? C9 H9 0.9500 . ? C10 C11 1.378(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.348(8) . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? Ir2 N8 2.068(4) . ? Ir2 N5 2.086(3) . ? Ir2 C16 2.125(4) . ? Ir2 C20 2.126(4) . ? Ir2 C17 2.138(4) . ? Ir2 C21 2.146(4) . ? N5 C24 1.339(5) . ? N5 N6 1.366(4) . ? N6 C26 1.346(5) . ? N6 C27 1.442(5) . ? N7 C28 1.351(5) . ? N7 N8 1.364(5) . ? N7 C27 1.449(6) . ? N8 C30 1.345(5) . ? C16 C17 1.412(7) . ? C16 C23 1.517(7) . ? C16 H16 0.9500 . ? C17 C18 1.517(8) . ? C17 H17 0.9500 . ? C18 C19 1.523(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.510(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.414(6) . ? C20 H20 0.9500 . ? C21 C22 1.521(6) . ? C21 H21 0.9500 . ? C22 C23 1.541(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.395(5) . ? C24 H24 0.9500 . ? C25 C26 1.369(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.363(8) . ? C28 H28 0.9500 . ? C29 C30 1.392(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? B1 C39 1.635(5) . ? B1 C55 1.642(5) . ? B1 C31 1.646(5) . ? B1 C47 1.648(5) . ? C31 C32 1.402(5) . ? C31 C36 1.403(5) . ? C32 C33 1.396(5) . ? C32 H32 0.9500 . ? C33 C34 1.384(5) . ? C33 C37 1.509(5) . ? C34 C35 1.392(5) . ? C34 H34 0.9500 . ? C35 C36 1.388(5) . ? C35 C38 1.505(5) . ? C36 H36 0.9500 . ? C37 F37A 1.328(5) . ? C37 F37C 1.336(5) . ? C37 F37B 1.344(5) . ? C38 F38B 1.305(5) . ? C38 F38A 1.318(4) . ? C38 F38C 1.337(5) . ? C39 C44 1.400(5) . ? C39 C40 1.418(5) . ? C40 C41 1.389(5) . ? C40 H40 0.9500 . ? C41 C42 1.390(5) . ? C41 C45 1.515(5) . ? C42 C43 1.390(5) . ? C42 H42 0.9500 . ? C43 C44 1.397(5) . ? C43 C46 1.507(5) . ? C44 H44 0.9500 . ? C45 F45B 1.321(5) . ? C45 F45A 1.341(5) . ? C45 F45C 1.342(5) . ? C46 F46C 1.301(5) . ? C46 F46B 1.310(5) . ? C46 F46A 1.315(5) . ? C47 C48 1.395(5) . ? C47 C52 1.413(5) . ? C48 C49 1.397(5) . ? C48 H48 0.9500 . ? C49 C50 1.386(5) . ? C49 C53 1.499(5) . ? C50 C51 1.379(5) . ? C50 H50 0.9500 . ? C51 C52 1.392(5) . ? C51 C54 1.495(6) . ? C52 H52 0.9500 . ? C53 F53A 1.313(5) . ? C53 F53B 1.321(5) . ? C53 F53C 1.321(5) . ? C54 F54B 1.323(5) . ? C54 F54A 1.326(5) . ? C54 F54C 1.347(6) . ? C55 C56 1.402(5) . ? C55 C60 1.409(5) . ? C56 C57 1.405(5) . ? C56 H56 0.9500 . ? C57 C58 1.382(5) . ? C57 C61 1.493(6) . ? C58 C59A 1.393(6) . ? C58 H58 0.9500 . ? C60 C59A 1.398(5) . ? C60 H60 0.9500 . ? C61 F61C 1.334(5) . ? C61 F61B 1.335(5) . ? C61 F61A 1.351(5) . ? C59A C62A 1.493(4) . ? C62A F62A 1.3054 . ? C62A F62B 1.3055 . ? C62A F62C 1.3063 . ? C62B F62E 1.3055 . ? C62B F62F 1.3058 . ? C62B F62D 1.3058 . ? B2 C79 1.639(5) . ? B2 C63 1.640(5) . ? B2 C71 1.641(5) . ? B2 C87 1.645(5) . ? C63 C64 1.408(5) . ? C63 C68 1.410(5) . ? C64 C65 1.386(5) . ? C64 H64 0.9500 . ? C65 C66 1.393(5) . ? C65 C69 1.513(5) . ? C66 C67A 1.387(5) . ? C66 H66 0.9500 . ? C68 C67A 1.394(5) . ? C68 H68 0.9500 . ? C69 F69C 1.325(5) . ? C69 F69B 1.335(5) . ? C69 F69A 1.345(5) . ? C67A C70A 1.495(4) . ? C70A F70B 1.3145 . ? C70A F70A 1.3149 . ? C70A F70C 1.3149 . ? C70B F70F 1.3148 . ? C70B F70E 1.3148 . ? C70B F70D 1.3150 . ? C71 C72 1.399(5) . ? C71 C76 1.409(5) . ? C72 C73A 1.395(5) . ? C72 H72 0.9500 . ? C74 C75 1.383(5) . ? C74 C73A 1.391(5) . ? C74 H74 0.9500 . ? C75 C76 1.392(5) . ? C75 C78 1.497(6) . ? C76 H76 0.9500 . ? C73A C77A 1.498(4) . ? C77A F77B 1.3216 . ? C77A F77A 1.3217 . ? C77A F77C 1.3220 . ? C77B F77D 1.3216 . ? C77B F77F 1.3217 . ? C77B F77E 1.3221 . ? C78 F78B 1.320(5) . ? C78 F78A 1.328(5) . ? C78 F78C 1.355(5) . ? C79 C80 1.402(5) . ? C79 C84 1.411(5) . ? C80 C81 1.401(5) . ? C80 H80 0.9500 . ? C81 C82 1.392(5) . ? C81 C85 1.498(5) . ? C82 C83 1.394(5) . ? C82 H82 0.9500 . ? C83 C84 1.388(5) . ? C83 C86 1.505(5) . ? C84 H84 0.9500 . ? C85 F85B 1.332(5) . ? C85 F85A 1.339(5) . ? C85 F85C 1.356(5) . ? C86 F86A 1.297(5) . ? C86 F86C 1.302(5) . ? C86 F86B 1.342(6) . ? C87 C88 1.396(5) . ? C87 C92 1.406(5) . ? C88 C89 1.398(5) . ? C88 H88 0.9500 . ? C89 C90 1.379(6) . ? C89 C93 1.504(6) . ? C90 C91A 1.390(6) . ? C90 H90 0.9500 . ? C92 C91A 1.394(5) . ? C92 H92 0.9500 . ? C93 F93B 1.326(5) . ? C93 F93C 1.333(5) . ? C93 F93A 1.351(6) . ? C91A C94A 1.492(4) . ? C94A F94A 1.2982 . ? C94A F94B 1.2983 . ? C94A F94C 1.3003 . ? C94B F94E 1.2986 . ? C94B F94D 1.2989 . ? C94B F94F 1.3003 . ? 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 Ir1 N4 87.56(13) . . ? N1 Ir1 C1 154.92(18) . . ? N4 Ir1 C1 90.19(17) . . ? N1 Ir1 C5 92.45(16) . . ? N4 Ir1 C5 160.28(19) . . ? C1 Ir1 C5 97.88(19) . . ? N1 Ir1 C2 166.70(19) . . ? N4 Ir1 C2 93.7(2) . . ? C1 Ir1 C2 38.4(2) . . ? C5 Ir1 C2 81.9(2) . . ? N1 Ir1 C6 92.85(15) . . ? N4 Ir1 C6 161.11(17) . . ? C1 Ir1 C6 81.46(19) . . ? C5 Ir1 C6 38.61(19) . . ? C2 Ir1 C6 90.2(2) . . ? C9 N1 N2 105.0(3) . . ? C9 N1 Ir1 134.2(3) . . ? N2 N1 Ir1 120.4(2) . . ? C11 N2 N1 111.4(3) . . ? C11 N2 C12 128.5(4) . . ? N1 N2 C12 119.4(3) . . ? N4 N3 C13 110.9(4) . . ? N4 N3 C12 119.5(3) . . ? C13 N3 C12 129.5(4) . . ? C15 N4 N3 105.4(4) . . ? C15 N4 Ir1 133.1(3) . . ? N3 N4 Ir1 121.2(3) . . ? C2 C1 C8 125.4(5) . . ? C2 C1 Ir1 71.1(3) . . ? C8 C1 Ir1 111.1(3) . . ? C2 C1 H1 117.3 . . ? C8 C1 H1 117.3 . . ? Ir1 C1 H1 87.7 . . ? C1 C2 C3 122.9(6) . . ? C1 C2 Ir1 70.5(3) . . ? C3 C2 Ir1 112.9(4) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? Ir1 C2 H2 86.7 . . ? C2 C3 C4 112.5(4) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 112.8(4) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 124.7(5) . . ? C6 C5 Ir1 71.5(3) . . ? C4 C5 Ir1 111.1(4) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? Ir1 C5 H5 87.3 . . ? C5 C6 C7 123.0(4) . . ? C5 C6 Ir1 69.9(3) . . ? C7 C6 Ir1 114.2(3) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? Ir1 C6 H6 86.1 . . ? C6 C7 C8 111.4(4) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C1 C8 C7 112.5(4) . . ? C1 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C1 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C10 110.9(4) . . ? N1 C9 H9 124.5 . . ? C10 C9 H9 124.5 . . ? C11 C10 C9 105.3(4) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 107.3(4) . . ? N2 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? N2 C12 N3 110.5(3) . . ? N2 C12 H12A 109.6 . . ? N3 C12 H12A 109.6 . . ? N2 C12 H12B 109.6 . . ? N3 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 N3 107.3(5) . . ? C14 C13 H13 126.4 . . ? N3 C13 H13 126.4 . . ? C13 C14 C15 106.4(4) . . ? C13 C14 H14 126.8 . . ? C15 C14 H14 126.8 . . ? N4 C15 C14 110.0(4) . . ? N4 C15 H15 125.0 . . ? C14 C15 H15 125.0 . . ? N8 Ir2 N5 87.16(13) . . ? N8 Ir2 C16 90.16(17) . . ? N5 Ir2 C16 154.96(17) . . ? N8 Ir2 C20 160.67(17) . . ? N5 Ir2 C20 92.39(15) . . ? C16 Ir2 C20 98.13(18) . . ? N8 Ir2 C17 94.91(19) . . ? N5 Ir2 C17 166.34(18) . . ? C16 Ir2 C17 38.7(2) . . ? C20 Ir2 C17 81.2(2) . . ? N8 Ir2 C21 160.68(16) . . ? N5 Ir2 C21 93.06(14) . . ? C16 Ir2 C21 81.50(17) . . ? C20 Ir2 C21 38.66(17) . . ? C17 Ir2 C21 89.43(19) . . ? C24 N5 N6 104.9(3) . . ? C24 N5 Ir2 134.3(3) . . ? N6 N5 Ir2 120.7(2) . . ? C26 N6 N5 111.1(3) . . ? C26 N6 C27 129.3(4) . . ? N5 N6 C27 119.1(3) . . ? C28 N7 N8 111.1(4) . . ? C28 N7 C27 130.0(4) . . ? N8 N7 C27 118.8(3) . . ? C30 N8 N7 104.8(4) . . ? C30 N8 Ir2 133.5(3) . . ? N7 N8 Ir2 121.4(3) . . ? C17 C16 C23 123.9(5) . . ? C17 C16 Ir2 71.2(3) . . ? C23 C16 Ir2 111.0(3) . . ? C17 C16 H16 118.1 . . ? C23 C16 H16 118.1 . . ? Ir2 C16 H16 87.8 . . ? C16 C17 C18 124.4(5) . . ? C16 C17 Ir2 70.2(3) . . ? C18 C17 Ir2 113.5(4) . . ? C16 C17 H17 117.8 . . ? C18 C17 H17 117.8 . . ? Ir2 C17 H17 86.3 . . ? C17 C18 C19 112.5(4) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 112.7(4) . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 124.3(4) . . ? C21 C20 Ir2 71.4(2) . . ? C19 C20 Ir2 111.4(3) . . ? C21 C20 H20 117.8 . . ? C19 C20 H20 117.8 . . ? Ir2 C20 H20 87.1 . . ? C20 C21 C22 123.2(4) . . ? C20 C21 Ir2 69.9(2) . . ? C22 C21 Ir2 113.8(3) . . ? C20 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? Ir2 C21 H21 86.3 . . ? C21 C22 C23 111.4(4) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C16 C23 C22 113.0(4) . . ? C16 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C16 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N5 C24 C25 111.1(4) . . ? N5 C24 H24 124.4 . . ? C25 C24 H24 124.4 . . ? C26 C25 C24 105.1(4) . . ? C26 C25 H25 127.4 . . ? C24 C25 H25 127.4 . . ? N6 C26 C25 107.8(4) . . ? N6 C26 H26 126.1 . . ? C25 C26 H26 126.1 . . ? N6 C27 N7 110.9(3) . . ? N6 C27 H27A 109.5 . . ? N7 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? N7 C27 H27B 109.5 . . ? H27A C27 H27B 108.0 . . ? N7 C28 C29 107.6(5) . . ? N7 C28 H28 126.2 . . ? C29 C28 H28 126.2 . . ? C28 C29 C30 105.6(4) . . ? C28 C29 H29 127.2 . . ? C30 C29 H29 127.2 . . ? N8 C30 C29 110.9(5) . . ? N8 C30 H30 124.5 . . ? C29 C30 H30 124.5 . . ? C39 B1 C55 107.5(3) . . ? C39 B1 C31 110.5(3) . . ? C55 B1 C31 110.3(3) . . ? C39 B1 C47 110.2(3) . . ? C55 B1 C47 110.3(3) . . ? C31 B1 C47 108.1(3) . . ? C32 C31 C36 115.7(3) . . ? C32 C31 B1 123.2(3) . . ? C36 C31 B1 120.9(3) . . ? C33 C32 C31 122.1(3) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C34 C33 C32 121.0(3) . . ? C34 C33 C37 120.7(3) . . ? C32 C33 C37 118.3(3) . . ? C33 C34 C35 117.8(3) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C36 C35 C34 121.1(3) . . ? C36 C35 C38 120.4(3) . . ? C34 C35 C38 118.4(3) . . ? C35 C36 C31 122.2(3) . . ? C35 C36 H36 118.9 . . ? C31 C36 H36 118.9 . . ? F37A C37 F37C 108.0(3) . . ? F37A C37 F37B 106.4(4) . . ? F37C C37 F37B 106.1(3) . . ? F37A C37 C33 112.9(3) . . ? F37C C37 C33 112.7(3) . . ? F37B C37 C33 110.3(3) . . ? F38B C38 F38A 107.7(4) . . ? F38B C38 F38C 105.8(4) . . ? F38A C38 F38C 105.7(4) . . ? F38B C38 C35 111.9(4) . . ? F38A C38 C35 113.0(3) . . ? F38C C38 C35 112.4(4) . . ? C44 C39 C40 115.8(3) . . ? C44 C39 B1 124.7(3) . . ? C40 C39 B1 119.5(3) . . ? C41 C40 C39 121.9(3) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 121.3(3) . . ? C40 C41 C45 120.0(3) . . ? C42 C41 C45 118.7(3) . . ? C41 C42 C43 117.8(3) . . ? C41 C42 H42 121.1 . . ? C43 C42 H42 121.1 . . ? C42 C43 C44 121.2(3) . . ? C42 C43 C46 118.8(3) . . ? C44 C43 C46 120.0(3) . . ? C43 C44 C39 122.0(3) . . ? C43 C44 H44 119.0 . . ? C39 C44 H44 119.0 . . ? F45B C45 F45A 107.5(3) . . ? F45B C45 F45C 107.5(4) . . ? F45A C45 F45C 106.7(3) . . ? F45B C45 C41 112.7(4) . . ? F45A C45 C41 111.7(3) . . ? F45C C45 C41 110.5(3) . . ? F46C C46 F46B 107.5(4) . . ? F46C C46 F46A 105.8(4) . . ? F46B C46 F46A 104.3(4) . . ? F46C C46 C43 112.8(4) . . ? F46B C46 C43 112.9(3) . . ? F46A C46 C43 112.9(3) . . ? C48 C47 C52 115.3(3) . . ? C48 C47 B1 124.7(3) . . ? C52 C47 B1 119.9(3) . . ? C47 C48 C49 122.1(3) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C50 C49 C48 121.3(3) . . ? C50 C49 C53 119.9(3) . . ? C48 C49 C53 118.7(4) . . ? C51 C50 C49 117.8(3) . . ? C51 C50 H50 121.1 . . ? C49 C50 H50 121.1 . . ? C50 C51 C52 121.1(4) . . ? C50 C51 C54 120.6(3) . . ? C52 C51 C54 118.3(4) . . ? C51 C52 C47 122.3(3) . . ? C51 C52 H52 118.8 . . ? C47 C52 H52 118.8 . . ? F53A C53 F53B 106.9(4) . . ? F53A C53 F53C 105.2(4) . . ? F53B C53 F53C 105.3(4) . . ? F53A C53 C49 114.3(4) . . ? F53B C53 C49 111.8(3) . . ? F53C C53 C49 112.7(4) . . ? F54B C54 F54A 107.2(4) . . ? F54B C54 F54C 106.1(4) . . ? F54A C54 F54C 105.1(4) . . ? F54B C54 C51 112.3(4) . . ? F54A C54 C51 113.5(4) . . ? F54C C54 C51 112.1(4) . . ? C56 C55 C60 116.0(3) . . ? C56 C55 B1 124.5(3) . . ? C60 C55 B1 119.5(3) . . ? C55 C56 C57 122.0(4) . . ? C55 C56 H56 119.0 . . ? C57 C56 H56 119.0 . . ? C58 C57 C56 121.2(4) . . ? C58 C57 C61 119.4(4) . . ? C56 C57 C61 119.2(4) . . ? C57 C58 C59A 117.8(4) . . ? C57 C58 H58 121.1 . . ? C59A C58 H58 121.1 . . ? C59A C60 C55 121.6(4) . . ? C59A C60 H60 119.2 . . ? C55 C60 H60 119.2 . . ? F61C C61 F61B 106.1(4) . . ? F61C C61 F61A 106.0(4) . . ? F61B C61 F61A 106.8(4) . . ? F61C C61 C57 113.0(3) . . ? F61B C61 C57 113.1(4) . . ? F61A C61 C57 111.4(4) . . ? C58 C59A C60 121.4(4) . . ? C58 C59A C62A 121.9(3) . . ? C60 C59A C62A 116.6(3) . . ? F62A C62A F62B 112.4 . . ? F62A C62A F62C 97.2 . . ? F62B C62A F62C 102.9 . . ? F62A C62A C59A 115.3(2) . . ? F62B C62A C59A 114.7(2) . . ? F62C C62A C59A 112.4(2) . . ? F62E C62B F62F 101.2 . . ? F62E C62B F62D 103.3 . . ? F62F C62B F62D 110.3 . . ? C79 B2 C63 107.5(3) . . ? C79 B2 C71 110.6(3) . . ? C63 B2 C71 110.3(3) . . ? C79 B2 C87 110.1(3) . . ? C63 B2 C87 110.0(3) . . ? C71 B2 C87 108.4(3) . . ? C64 C63 C68 115.6(3) . . ? C64 C63 B2 119.6(3) . . ? C68 C63 B2 124.7(3) . . ? C65 C64 C63 122.3(3) . . ? C65 C64 H64 118.8 . . ? C63 C64 H64 118.8 . . ? C64 C65 C66 121.4(3) . . ? C64 C65 C69 119.9(3) . . ? C66 C65 C69 118.7(3) . . ? C67A C66 C65 117.1(3) . . ? C67A C66 H66 121.4 . . ? C65 C66 H66 121.4 . . ? C67A C68 C63 121.5(3) . . ? C67A C68 H68 119.3 . . ? C63 C68 H68 119.3 . . ? F69C C69 F69B 108.1(4) . . ? F69C C69 F69A 106.8(3) . . ? F69B C69 F69A 106.6(3) . . ? F69C C69 C65 112.6(3) . . ? F69B C69 C65 111.0(3) . . ? F69A C69 C65 111.4(3) . . ? C66 C67A C68 122.0(3) . . ? C66 C67A C70A 118.8(3) . . ? C68 C67A C70A 119.2(3) . . ? F70B C70A F70A 107.9 . . ? F70B C70A F70C 104.7 . . ? F70A C70A F70C 106.1 . . ? F70B C70A C67A 114.84(19) . . ? F70A C70A C67A 111.4(2) . . ? F70C C70A C67A 111.3(2) . . ? F70F C70B F70E 101.9 . . ? F70F C70B F70D 108.0 . . ? F70E C70B F70D 102.4 . . ? C72 C71 C76 115.2(3) . . ? C72 C71 B2 125.1(3) . . ? C76 C71 B2 119.6(3) . . ? C73A C72 C71 122.3(4) . . ? C73A C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? C75 C74 C73A 117.8(3) . . ? C75 C74 H74 121.1 . . ? C73A C74 H74 121.1 . . ? C74 C75 C76 120.9(3) . . ? C74 C75 C78 120.3(3) . . ? C76 C75 C78 118.7(3) . . ? C75 C76 C71 122.6(3) . . ? C75 C76 H76 118.7 . . ? C71 C76 H76 118.7 . . ? C74 C73A C72 121.1(3) . . ? C74 C73A C77A 118.7(4) . . ? C72 C73A C77A 120.0(4) . . ? F77B C77A F77A 110.5 . . ? F77B C77A F77C 96.9 . . ? F77A C77A F77C 102.1 . . ? F77B C77A C73A 114.6(2) . . ? F77A C77A C73A 117.6(3) . . ? F77C C77A C73A 112.4(3) . . ? F77D C77B F77F 105.0 . . ? F77D C77B F77E 104.5 . . ? F77F C77B F77E 110.0 . . ? F78B C78 F78A 107.1(4) . . ? F78B C78 F78C 105.8(4) . . ? F78A C78 F78C 105.7(4) . . ? F78B C78 C75 112.3(4) . . ? F78A C78 C75 113.7(4) . . ? F78C C78 C75 111.7(4) . . ? C80 C79 C84 115.8(3) . . ? C80 C79 B2 124.5(3) . . ? C84 C79 B2 119.7(3) . . ? C81 C80 C79 121.8(3) . . ? C81 C80 H80 119.1 . . ? C79 C80 H80 119.1 . . ? C82 C81 C80 121.4(4) . . ? C82 C81 C85 119.5(3) . . ? C80 C81 C85 118.9(3) . . ? C81 C82 C83 117.4(3) . . ? C81 C82 H82 121.3 . . ? C83 C82 H82 121.3 . . ? C84 C83 C82 121.3(3) . . ? C84 C83 C86 118.3(4) . . ? C82 C83 C86 120.4(3) . . ? C83 C84 C79 122.3(4) . . ? C83 C84 H84 118.9 . . ? C79 C84 H84 118.9 . . ? F85B C85 F85A 106.4(4) . . ? F85B C85 F85C 105.9(3) . . ? F85A C85 F85C 106.5(3) . . ? F85B C85 C81 113.1(3) . . ? F85A C85 C81 113.2(3) . . ? F85C C85 C81 111.2(4) . . ? F86A C86 F86C 112.3(4) . . ? F86A C86 F86B 100.9(4) . . ? F86C C86 F86B 103.8(4) . . ? F86A C86 C83 113.7(3) . . ? F86C C86 C83 113.8(4) . . ? F86B C86 C83 111.0(4) . . ? C88 C87 C92 116.0(3) . . ? C88 C87 B2 123.9(3) . . ? C92 C87 B2 120.0(3) . . ? C87 C88 C89 121.9(4) . . ? C87 C88 H88 119.0 . . ? C89 C88 H88 119.0 . . ? C90 C89 C88 121.3(4) . . ? C90 C89 C93 121.0(4) . . ? C88 C89 C93 117.7(4) . . ? C89 C90 C91A 117.9(4) . . ? C89 C90 H90 121.1 . . ? C91A C90 H90 121.1 . . ? C91A C92 C87 121.8(4) . . ? C91A C92 H92 119.1 . . ? C87 C92 H92 119.1 . . ? F93B C93 F93C 107.6(4) . . ? F93B C93 F93A 106.4(4) . . ? F93C C93 F93A 105.6(4) . . ? F93B C93 C89 113.1(3) . . ? F93C C93 C89 113.3(4) . . ? F93A C93 C89 110.3(4) . . ? C90 C91A C92 121.0(4) . . ? C90 C91A C94A 115.1(3) . . ? C92 C91A C94A 123.9(4) . . ? F94A C94A F94B 113.8 . . ? F94A C94A F94C 104.2 . . ? F94B C94A F94C 103.4 . . ? F94A C94A C91A 109.2(2) . . ? F94B C94A C91A 110.9(2) . . ? F94C C94A C91A 115.3(2) . . ? F94E C94B F94D 109.1 . . ? F94E C94B F94F 97.9 . . ? F94D C94B F94F 97.7 . . ? 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 N4 Ir1 N1 C9 -145.0(4) . . . . ? C1 Ir1 N1 C9 129.8(5) . . . . ? C5 Ir1 N1 C9 15.3(4) . . . . ? C2 Ir1 N1 C9 -49.2(10) . . . . ? C6 Ir1 N1 C9 53.9(4) . . . . ? N4 Ir1 N1 N2 27.9(3) . . . . ? C1 Ir1 N1 N2 -57.3(5) . . . . ? C5 Ir1 N1 N2 -171.8(3) . . . . ? C2 Ir1 N1 N2 123.7(8) . . . . ? C6 Ir1 N1 N2 -133.2(3) . . . . ? C9 N1 N2 C11 -2.1(4) . . . . ? Ir1 N1 N2 C11 -176.8(3) . . . . ? C9 N1 N2 C12 -172.7(3) . . . . ? Ir1 N1 N2 C12 12.6(5) . . . . ? C13 N3 N4 C15 1.1(5) . . . . ? C12 N3 N4 C15 176.6(4) . . . . ? C13 N3 N4 Ir1 175.8(3) . . . . ? C12 N3 N4 Ir1 -8.7(5) . . . . ? N1 Ir1 N4 C15 142.9(4) . . . . ? C1 Ir1 N4 C15 -62.1(4) . . . . ? C5 Ir1 N4 C15 52.4(7) . . . . ? C2 Ir1 N4 C15 -23.9(5) . . . . ? C6 Ir1 N4 C15 -125.5(6) . . . . ? N1 Ir1 N4 N3 -30.1(3) . . . . ? C1 Ir1 N4 N3 124.9(3) . . . . ? C5 Ir1 N4 N3 -120.6(5) . . . . ? C2 Ir1 N4 N3 163.1(3) . . . . ? C6 Ir1 N4 N3 61.5(6) . . . . ? N1 Ir1 C1 C2 -179.6(4) . . . . ? N4 Ir1 C1 C2 95.7(4) . . . . ? C5 Ir1 C1 C2 -66.2(4) . . . . ? C6 Ir1 C1 C2 -101.3(4) . . . . ? N1 Ir1 C1 C8 -58.0(6) . . . . ? N4 Ir1 C1 C8 -142.6(3) . . . . ? C5 Ir1 C1 C8 55.4(4) . . . . ? C2 Ir1 C1 C8 121.6(5) . . . . ? C6 Ir1 C1 C8 20.3(3) . . . . ? C8 C1 C2 C3 2.3(8) . . . . ? Ir1 C1 C2 C3 105.2(5) . . . . ? C8 C1 C2 Ir1 -102.9(5) . . . . ? N1 Ir1 C2 C1 179.3(7) . . . . ? N4 Ir1 C2 C1 -85.6(3) . . . . ? C5 Ir1 C2 C1 113.7(4) . . . . ? C6 Ir1 C2 C1 75.9(3) . . . . ? N1 Ir1 C2 C3 60.9(11) . . . . ? N4 Ir1 C2 C3 156.0(5) . . . . ? C1 Ir1 C2 C3 -118.4(6) . . . . ? C5 Ir1 C2 C3 -4.7(5) . . . . ? C6 Ir1 C2 C3 -42.5(5) . . . . ? C1 C2 C3 C4 -92.6(7) . . . . ? Ir1 C2 C3 C4 -11.7(7) . . . . ? C2 C3 C4 C5 29.2(8) . . . . ? C3 C4 C5 C6 48.9(8) . . . . ? C3 C4 C5 Ir1 -32.7(7) . . . . ? N1 Ir1 C5 C6 91.5(3) . . . . ? N4 Ir1 C5 C6 -178.9(4) . . . . ? C1 Ir1 C5 C6 -65.6(3) . . . . ? C2 Ir1 C5 C6 -100.6(3) . . . . ? N1 Ir1 C5 C4 -147.5(4) . . . . ? N4 Ir1 C5 C4 -57.9(7) . . . . ? C1 Ir1 C5 C4 55.4(4) . . . . ? C2 Ir1 C5 C4 20.4(4) . . . . ? C6 Ir1 C5 C4 121.0(5) . . . . ? C4 C5 C6 C7 3.1(8) . . . . ? Ir1 C5 C6 C7 106.4(4) . . . . ? C4 C5 C6 Ir1 -103.3(5) . . . . ? N1 Ir1 C6 C5 -90.4(3) . . . . ? N4 Ir1 C6 C5 178.9(4) . . . . ? C1 Ir1 C6 C5 114.2(3) . . . . ? C2 Ir1 C6 C5 76.7(3) . . . . ? N1 Ir1 C6 C7 151.5(4) . . . . ? N4 Ir1 C6 C7 60.7(7) . . . . ? C1 Ir1 C6 C7 -3.9(4) . . . . ? C5 Ir1 C6 C7 -118.1(5) . . . . ? C2 Ir1 C6 C7 -41.4(4) . . . . ? C5 C6 C7 C8 -94.2(6) . . . . ? Ir1 C6 C7 C8 -13.3(6) . . . . ? C2 C1 C8 C7 47.5(7) . . . . ? Ir1 C1 C8 C7 -33.8(5) . . . . ? C6 C7 C8 C1 30.5(6) . . . . ? N2 N1 C9 C10 2.2(5) . . . . ? Ir1 N1 C9 C10 175.8(3) . . . . ? N1 C9 C10 C11 -1.5(5) . . . . ? N1 N2 C11 C10 1.2(5) . . . . ? C12 N2 C11 C10 170.7(4) . . . . ? C9 C10 C11 N2 0.2(5) . . . . ? C11 N2 C12 N3 125.8(4) . . . . ? N1 N2 C12 N3 -65.5(5) . . . . ? N4 N3 C12 N2 63.1(5) . . . . ? C13 N3 C12 N2 -122.3(5) . . . . ? N4 N3 C13 C14 -1.0(5) . . . . ? C12 N3 C13 C14 -176.0(4) . . . . ? N3 C13 C14 C15 0.5(6) . . . . ? N3 N4 C15 C14 -0.8(5) . . . . ? Ir1 N4 C15 C14 -174.6(3) . . . . ? C13 C14 C15 N4 0.2(6) . . . . ? N8 Ir2 N5 C24 -144.4(4) . . . . ? C16 Ir2 N5 C24 131.3(4) . . . . ? C20 Ir2 N5 C24 16.2(4) . . . . ? C17 Ir2 N5 C24 -45.3(9) . . . . ? C21 Ir2 N5 C24 54.9(4) . . . . ? N8 Ir2 N5 N6 30.6(3) . . . . ? C16 Ir2 N5 N6 -53.6(5) . . . . ? C20 Ir2 N5 N6 -168.7(3) . . . . ? C17 Ir2 N5 N6 129.7(7) . . . . ? C21 Ir2 N5 N6 -130.0(3) . . . . ? C24 N5 N6 C26 -2.2(4) . . . . ? Ir2 N5 N6 C26 -178.5(3) . . . . ? C24 N5 N6 C27 -174.2(3) . . . . ? Ir2 N5 N6 C27 9.4(5) . . . . ? C28 N7 N8 C30 0.9(5) . . . . ? C27 N7 N8 C30 177.6(4) . . . . ? C28 N7 N8 Ir2 175.2(3) . . . . ? C27 N7 N8 Ir2 -8.1(5) . . . . ? N5 Ir2 N8 C30 141.1(4) . . . . ? C16 Ir2 N8 C30 -63.8(5) . . . . ? C20 Ir2 N8 C30 52.0(7) . . . . ? C17 Ir2 N8 C30 -25.3(5) . . . . ? C21 Ir2 N8 C30 -127.7(5) . . . . ? N5 Ir2 N8 N7 -31.2(3) . . . . ? C16 Ir2 N8 N7 123.8(3) . . . . ? C20 Ir2 N8 N7 -120.4(5) . . . . ? C17 Ir2 N8 N7 162.3(3) . . . . ? C21 Ir2 N8 N7 59.9(6) . . . . ? N8 Ir2 C16 C17 97.7(3) . . . . ? N5 Ir2 C16 C17 -178.7(3) . . . . ? C20 Ir2 C16 C17 -64.8(3) . . . . ? C21 Ir2 C16 C17 -99.8(3) . . . . ? N8 Ir2 C16 C23 -142.3(3) . . . . ? N5 Ir2 C16 C23 -58.7(6) . . . . ? C20 Ir2 C16 C23 55.2(4) . . . . ? C17 Ir2 C16 C23 120.0(5) . . . . ? C21 Ir2 C16 C23 20.2(3) . . . . ? C23 C16 C17 C18 2.3(7) . . . . ? Ir2 C16 C17 C18 105.5(5) . . . . ? C23 C16 C17 Ir2 -103.2(4) . . . . ? N8 Ir2 C17 C16 -84.1(3) . . . . ? N5 Ir2 C17 C16 177.7(6) . . . . ? C20 Ir2 C17 C16 115.0(3) . . . . ? C21 Ir2 C17 C16 77.0(3) . . . . ? N8 Ir2 C17 C18 156.1(4) . . . . ? N5 Ir2 C17 C18 57.9(9) . . . . ? C16 Ir2 C17 C18 -119.8(5) . . . . ? C20 Ir2 C17 C18 -4.9(4) . . . . ? C21 Ir2 C17 C18 -42.8(4) . . . . ? C16 C17 C18 C19 -92.8(6) . . . . ? Ir2 C17 C18 C19 -11.4(6) . . . . ? C17 C18 C19 C20 28.7(7) . . . . ? C18 C19 C20 C21 49.0(7) . . . . ? C18 C19 C20 Ir2 -32.6(6) . . . . ? N8 Ir2 C20 C21 -179.9(4) . . . . ? N5 Ir2 C20 C21 91.9(3) . . . . ? C16 Ir2 C20 C21 -65.3(3) . . . . ? C17 Ir2 C20 C21 -100.2(3) . . . . ? N8 Ir2 C20 C19 -59.4(6) . . . . ? N5 Ir2 C20 C19 -147.6(3) . . . . ? C16 Ir2 C20 C19 55.2(4) . . . . ? C17 Ir2 C20 C19 20.3(3) . . . . ? C21 Ir2 C20 C19 120.5(4) . . . . ? C19 C20 C21 C22 2.3(7) . . . . ? Ir2 C20 C21 C22 106.0(4) . . . . ? C19 C20 C21 Ir2 -103.7(5) . . . . ? N8 Ir2 C21 C20 179.9(4) . . . . ? N5 Ir2 C21 C20 -90.0(3) . . . . ? C16 Ir2 C21 C20 114.6(3) . . . . ? C17 Ir2 C21 C20 76.6(3) . . . . ? N8 Ir2 C21 C22 61.5(6) . . . . ? N5 Ir2 C21 C22 151.6(3) . . . . ? C16 Ir2 C21 C22 -3.8(3) . . . . ? C20 Ir2 C21 C22 -118.4(4) . . . . ? C17 Ir2 C21 C22 -41.8(3) . . . . ? C20 C21 C22 C23 -93.9(5) . . . . ? Ir2 C21 C22 C23 -13.1(5) . . . . ? C17 C16 C23 C22 47.4(6) . . . . ? Ir2 C16 C23 C22 -33.5(5) . . . . ? C21 C22 C23 C16 30.4(5) . . . . ? N6 N5 C24 C25 2.2(5) . . . . ? Ir2 N5 C24 C25 177.8(3) . . . . ? N5 C24 C25 C26 -1.5(5) . . . . ? N5 N6 C26 C25 1.3(5) . . . . ? C27 N6 C26 C25 172.3(4) . . . . ? C24 C25 C26 N6 0.1(5) . . . . ? C26 N6 C27 N7 125.8(4) . . . . ? N5 N6 C27 N7 -63.8(5) . . . . ? C28 N7 C27 N6 -120.9(5) . . . . ? N8 N7 C27 N6 63.1(5) . . . . ? N8 N7 C28 C29 -1.2(5) . . . . ? C27 N7 C28 C29 -177.4(4) . . . . ? N7 C28 C29 C30 1.0(6) . . . . ? N7 N8 C30 C29 -0.2(5) . . . . ? Ir2 N8 C30 C29 -173.5(3) . . . . ? C28 C29 C30 N8 -0.5(6) . . . . ? C39 B1 C31 C32 -104.5(4) . . . . ? C55 B1 C31 C32 14.2(5) . . . . ? C47 B1 C31 C32 134.8(4) . . . . ? C39 B1 C31 C36 71.7(4) . . . . ? C55 B1 C31 C36 -169.6(3) . . . . ? C47 B1 C31 C36 -49.0(4) . . . . ? C36 C31 C32 C33 -1.1(6) . . . . ? B1 C31 C32 C33 175.3(4) . . . . ? C31 C32 C33 C34 -1.1(6) . . . . ? C31 C32 C33 C37 177.6(4) . . . . ? C32 C33 C34 C35 1.7(6) . . . . ? C37 C33 C34 C35 -176.9(4) . . . . ? C33 C34 C35 C36 -0.1(6) . . . . ? C33 C34 C35 C38 -178.4(4) . . . . ? C34 C35 C36 C31 -2.2(6) . . . . ? C38 C35 C36 C31 176.0(4) . . . . ? C32 C31 C36 C35 2.7(6) . . . . ? B1 C31 C36 C35 -173.8(4) . . . . ? C34 C33 C37 F37A -136.7(4) . . . . ? C32 C33 C37 F37A 44.6(5) . . . . ? C34 C33 C37 F37C -13.9(6) . . . . ? C32 C33 C37 F37C 167.3(4) . . . . ? C34 C33 C37 F37B 104.5(4) . . . . ? C32 C33 C37 F37B -74.2(5) . . . . ? C36 C35 C38 F38B -83.1(5) . . . . ? C34 C35 C38 F38B 95.1(5) . . . . ? C36 C35 C38 F38A 38.6(6) . . . . ? C34 C35 C38 F38A -143.2(4) . . . . ? C36 C35 C38 F38C 158.1(4) . . . . ? C34 C35 C38 F38C -23.7(6) . . . . ? C55 B1 C39 C44 -132.9(3) . . . . ? C31 B1 C39 C44 -12.5(5) . . . . ? C47 B1 C39 C44 106.8(4) . . . . ? C55 B1 C39 C40 46.2(4) . . . . ? C31 B1 C39 C40 166.6(3) . . . . ? C47 B1 C39 C40 -74.0(4) . . . . ? C44 C39 C40 C41 -0.9(5) . . . . ? B1 C39 C40 C41 179.9(3) . . . . ? C39 C40 C41 C42 0.7(5) . . . . ? C39 C40 C41 C45 178.1(3) . . . . ? C40 C41 C42 C43 -0.7(5) . . . . ? C45 C41 C42 C43 -178.1(3) . . . . ? C41 C42 C43 C44 0.8(5) . . . . ? C41 C42 C43 C46 -178.7(3) . . . . ? C42 C43 C44 C39 -1.0(5) . . . . ? C46 C43 C44 C39 178.5(3) . . . . ? C40 C39 C44 C43 1.0(5) . . . . ? B1 C39 C44 C43 -179.8(3) . . . . ? C40 C41 C45 F45B 152.4(4) . . . . ? C42 C41 C45 F45B -30.2(5) . . . . ? C40 C41 C45 F45A 31.2(5) . . . . ? C42 C41 C45 F45A -151.3(3) . . . . ? C40 C41 C45 F45C -87.3(4) . . . . ? C42 C41 C45 F45C 90.1(4) . . . . ? C42 C43 C46 F46C 149.9(4) . . . . ? C44 C43 C46 F46C -29.6(5) . . . . ? C42 C43 C46 F46B 27.8(5) . . . . ? C44 C43 C46 F46B -151.8(4) . . . . ? C42 C43 C46 F46A -90.1(5) . . . . ? C44 C43 C46 F46A 90.3(5) . . . . ? C39 B1 C47 C48 13.0(5) . . . . ? C55 B1 C47 C48 -105.6(4) . . . . ? C31 B1 C47 C48 133.8(3) . . . . ? C39 B1 C47 C52 -171.0(3) . . . . ? C55 B1 C47 C52 70.4(4) . . . . ? C31 B1 C47 C52 -50.2(4) . . . . ? C52 C47 C48 C49 -0.7(5) . . . . ? B1 C47 C48 C49 175.5(3) . . . . ? C47 C48 C49 C50 -1.1(6) . . . . ? C47 C48 C49 C53 -178.2(4) . . . . ? C48 C49 C50 C51 1.2(6) . . . . ? C53 C49 C50 C51 178.3(4) . . . . ? C49 C50 C51 C52 0.5(5) . . . . ? C49 C50 C51 C54 -176.7(4) . . . . ? C50 C51 C52 C47 -2.3(6) . . . . ? C54 C51 C52 C47 175.0(4) . . . . ? C48 C47 C52 C51 2.3(5) . . . . ? B1 C47 C52 C51 -174.0(3) . . . . ? C50 C49 C53 F53A 0.4(6) . . . . ? C48 C49 C53 F53A 177.6(4) . . . . ? C50 C49 C53 F53B -121.2(4) . . . . ? C48 C49 C53 F53B 56.0(6) . . . . ? C50 C49 C53 F53C 120.4(4) . . . . ? C48 C49 C53 F53C -62.4(5) . . . . ? C50 C51 C54 F54B 125.6(4) . . . . ? C52 C51 C54 F54B -51.7(5) . . . . ? C50 C51 C54 F54A 3.8(6) . . . . ? C52 C51 C54 F54A -173.5(4) . . . . ? C50 C51 C54 F54C -115.1(4) . . . . ? C52 C51 C54 F54C 67.6(5) . . . . ? C39 B1 C55 C56 -133.6(3) . . . . ? C31 B1 C55 C56 105.8(4) . . . . ? C47 B1 C55 C56 -13.4(5) . . . . ? C39 B1 C55 C60 46.7(4) . . . . ? C31 B1 C55 C60 -73.9(4) . . . . ? C47 B1 C55 C60 166.9(3) . . . . ? C60 C55 C56 C57 0.9(5) . . . . ? B1 C55 C56 C57 -178.8(3) . . . . ? C55 C56 C57 C58 -0.1(6) . . . . ? C55 C56 C57 C61 -175.5(4) . . . . ? C56 C57 C58 C59A -0.5(6) . . . . ? C61 C57 C58 C59A 174.9(4) . . . . ? C56 C55 C60 C59A -1.1(5) . . . . ? B1 C55 C60 C59A 178.6(3) . . . . ? C58 C57 C61 F61C 147.2(4) . . . . ? C56 C57 C61 F61C -37.3(5) . . . . ? C58 C57 C61 F61B 26.6(6) . . . . ? C56 C57 C61 F61B -157.9(4) . . . . ? C58 C57 C61 F61A -93.6(5) . . . . ? C56 C57 C61 F61A 81.9(5) . . . . ? C57 C58 C59A C60 0.3(6) . . . . ? C57 C58 C59A C62A 177.1(4) . . . . ? C55 C60 C59A C58 0.5(6) . . . . ? C55 C60 C59A C62A -176.4(3) . . . . ? C58 C59A C62A F62A 138.3(3) . . . . ? C60 C59A C62A F62A -44.8(4) . . . . ? C58 C59A C62A F62B 5.4(4) . . . . ? C60 C59A C62A F62B -177.7(3) . . . . ? C58 C59A C62A F62C -111.6(3) . . . . ? C60 C59A C62A F62C 65.3(4) . . . . ? C79 B2 C63 C64 45.0(4) . . . . ? C71 B2 C63 C64 -75.7(4) . . . . ? C87 B2 C63 C64 164.8(3) . . . . ? C79 B2 C63 C68 -134.4(3) . . . . ? C71 B2 C63 C68 104.9(4) . . . . ? C87 B2 C63 C68 -14.6(5) . . . . ? C68 C63 C64 C65 0.4(5) . . . . ? B2 C63 C64 C65 -179.1(3) . . . . ? C63 C64 C65 C66 -0.2(5) . . . . ? C63 C64 C65 C69 177.5(3) . . . . ? C64 C65 C66 C67A -0.4(5) . . . . ? C69 C65 C66 C67A -178.2(3) . . . . ? C64 C63 C68 C67A 0.2(5) . . . . ? B2 C63 C68 C67A 179.6(3) . . . . ? C64 C65 C69 F69C 151.0(4) . . . . ? C66 C65 C69 F69C -31.2(5) . . . . ? C64 C65 C69 F69B -87.7(4) . . . . ? C66 C65 C69 F69B 90.1(4) . . . . ? C64 C65 C69 F69A 31.0(5) . . . . ? C66 C65 C69 F69A -151.2(3) . . . . ? C65 C66 C67A C68 1.0(5) . . . . ? C65 C66 C67A C70A -178.1(3) . . . . ? C63 C68 C67A C66 -0.9(5) . . . . ? C63 C68 C67A C70A 178.2(3) . . . . ? C66 C67A C70A F70B -110.3(3) . . . . ? C68 C67A C70A F70B 70.5(3) . . . . ? C66 C67A C70A F70A 126.6(3) . . . . ? C68 C67A C70A F70A -52.6(3) . . . . ? C66 C67A C70A F70C 8.4(4) . . . . ? C68 C67A C70A F70C -170.8(2) . . . . ? C79 B2 C71 C72 -106.5(4) . . . . ? C63 B2 C71 C72 12.2(5) . . . . ? C87 B2 C71 C72 132.7(4) . . . . ? C79 B2 C71 C76 70.1(4) . . . . ? C63 B2 C71 C76 -171.2(3) . . . . ? C87 B2 C71 C76 -50.7(4) . . . . ? C76 C71 C72 C73A -1.3(5) . . . . ? B2 C71 C72 C73A 175.4(3) . . . . ? C73A C74 C75 C76 0.1(5) . . . . ? C73A C74 C75 C78 -175.7(4) . . . . ? C74 C75 C76 C71 -2.2(6) . . . . ? C78 C75 C76 C71 173.6(4) . . . . ? C72 C71 C76 C75 2.8(5) . . . . ? B2 C71 C76 C75 -174.2(3) . . . . ? C75 C74 C73A C72 1.4(6) . . . . ? C75 C74 C73A C77A -173.0(4) . . . . ? C71 C72 C73A C74 -0.7(6) . . . . ? C71 C72 C73A C77A 173.6(4) . . . . ? C74 C73A C77A F77B -159.5(3) . . . . ? C72 C73A C77A F77B 26.1(4) . . . . ? C74 C73A C77A F77A -27.0(4) . . . . ? C72 C73A C77A F77A 158.6(3) . . . . ? C74 C73A C77A F77C 91.2(4) . . . . ? C72 C73A C77A F77C -83.2(4) . . . . ? C74 C75 C78 F78B 118.1(4) . . . . ? C76 C75 C78 F78B -57.7(5) . . . . ? C74 C75 C78 F78A -3.6(6) . . . . ? C76 C75 C78 F78A -179.5(4) . . . . ? C74 C75 C78 F78C -123.2(4) . . . . ? C76 C75 C78 F78C 61.0(5) . . . . ? C63 B2 C79 C80 -132.0(4) . . . . ? C71 B2 C79 C80 -11.6(5) . . . . ? C87 B2 C79 C80 108.2(4) . . . . ? C63 B2 C79 C84 48.6(4) . . . . ? C71 B2 C79 C84 169.0(3) . . . . ? C87 B2 C79 C84 -71.2(4) . . . . ? C84 C79 C80 C81 0.8(5) . . . . ? B2 C79 C80 C81 -178.6(3) . . . . ? C79 C80 C81 C82 0.1(6) . . . . ? C79 C80 C81 C85 -175.9(3) . . . . ? C80 C81 C82 C83 -0.7(6) . . . . ? C85 C81 C82 C83 175.3(4) . . . . ? C81 C82 C83 C84 0.4(6) . . . . ? C81 C82 C83 C86 178.8(4) . . . . ? C82 C83 C84 C79 0.6(6) . . . . ? C86 C83 C84 C79 -177.8(4) . . . . ? C80 C79 C84 C83 -1.2(5) . . . . ? B2 C79 C84 C83 178.3(3) . . . . ? C82 C81 C85 F85B 144.8(4) . . . . ? C80 C81 C85 F85B -39.1(5) . . . . ? C82 C81 C85 F85A 23.7(6) . . . . ? C80 C81 C85 F85A -160.2(4) . . . . ? C82 C81 C85 F85C -96.2(4) . . . . ? C80 C81 C85 F85C 79.9(5) . . . . ? C84 C83 C86 F86A -46.1(6) . . . . ? C82 C83 C86 F86A 135.5(4) . . . . ? C84 C83 C86 F86C -176.5(4) . . . . ? C82 C83 C86 F86C 5.1(6) . . . . ? C84 C83 C86 F86B 66.8(5) . . . . ? C82 C83 C86 F86B -111.6(4) . . . . ? C79 B2 C87 C88 12.3(5) . . . . ? C63 B2 C87 C88 -106.0(4) . . . . ? C71 B2 C87 C88 133.4(4) . . . . ? C79 B2 C87 C92 -171.0(3) . . . . ? C63 B2 C87 C92 70.7(4) . . . . ? C71 B2 C87 C92 -49.9(4) . . . . ? C92 C87 C88 C89 -2.3(6) . . . . ? B2 C87 C88 C89 174.6(4) . . . . ? C87 C88 C89 C90 0.2(6) . . . . ? C87 C88 C89 C93 177.7(4) . . . . ? C88 C89 C90 C91A 1.2(6) . . . . ? C93 C89 C90 C91A -176.2(4) . . . . ? C88 C87 C92 C91A 3.1(6) . . . . ? B2 C87 C92 C91A -173.8(4) . . . . ? C90 C89 C93 F93B -137.6(4) . . . . ? C88 C89 C93 F93B 44.9(6) . . . . ? C90 C89 C93 F93C -14.8(6) . . . . ? C88 C89 C93 F93C 167.7(4) . . . . ? C90 C89 C93 F93A 103.3(5) . . . . ? C88 C89 C93 F93A -74.2(5) . . . . ? C89 C90 C91A C92 -0.3(6) . . . . ? C89 C90 C91A C94A 178.5(4) . . . . ? C87 C92 C91A C90 -1.9(6) . . . . ? C87 C92 C91A C94A 179.3(4) . . . . ? C90 C91A C94A F94A 91.5(4) . . . . ? C92 C91A C94A F94A -89.7(4) . . . . ? C90 C91A C94A F94B -142.3(3) . . . . ? C92 C91A C94A F94B 36.5(5) . . . . ? C90 C91A C94A F94C -25.3(4) . . . . ? C92 C91A C94A F94C 153.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.519 _refine_diff_density_min -3.693 _refine_diff_density_rms 0.167 # Attachment 'rh00301.cif' data_rh00301 _database_code_depnum_ccdc_archive 'CCDC 697501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C15 H20 N4 Rh ' _chemical_formula_sum 'C47 H32 B F24 N4 Rh' _chemical_formula_weight 1222.49 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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0057(2) _cell_length_b 13.6112(2) _cell_length_c 15.8258(3) _cell_angle_alpha 68.9120(10) _cell_angle_beta 69.2710(10) _cell_angle_gamma 68.3680(10) _cell_volume 2349.38(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 70707 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 30.034 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 55288 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13658 _reflns_number_gt 11594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+2.8888P] 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 13658 _refine_ls_number_parameters 730 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.004 _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 0.923145(16) 0.565496(16) 0.711410(13) 0.02469(6) Uani 1 1 d . . . N1 N 1.01054(16) 0.66307(16) 0.71932(13) 0.0216(4) Uani 1 1 d . . . N2 N 0.95991(17) 0.77205(16) 0.71099(13) 0.0224(4) Uani 1 1 d . . . N3 N 0.82144(19) 0.8066(2) 0.62995(15) 0.0320(5) Uani 1 1 d . . . N4 N 0.84365(19) 0.7051(2) 0.62033(15) 0.0328(5) Uani 1 1 d . . . C1 C 0.7834(2) 0.4985(3) 0.7491(2) 0.0380(6) Uani 1 1 d . . . H1 H 0.7369 0.5707 0.7298 0.046 Uiso 1 1 calc R . . C2 C 0.8693(3) 0.4542(3) 0.6804(2) 0.0498(9) Uani 1 1 d . . . H2 H 0.8801 0.4991 0.6178 0.060 Uiso 1 1 calc R . . C3 C 0.9479(4) 0.3376(3) 0.6987(3) 0.0619(11) Uani 1 1 d . . . H3A H 0.9072 0.2905 0.7543 0.074 Uiso 1 1 calc R . . H3B H 0.9663 0.3087 0.6444 0.074 Uiso 1 1 calc R . . C4 C 1.0588(3) 0.3316(3) 0.7152(3) 0.0598(11) Uani 1 1 d . . . H4A H 1.0872 0.2583 0.7559 0.072 Uiso 1 1 calc R . . H4B H 1.1171 0.3403 0.6545 0.072 Uiso 1 1 calc R . . C5 C 1.0449(2) 0.4181(2) 0.7604(2) 0.0373(6) Uani 1 1 d . . . H5 H 1.1004 0.4579 0.7345 0.045 Uiso 1 1 calc R . . C6 C 0.9566(2) 0.4438(2) 0.8370(2) 0.0308(5) Uani 1 1 d . . . H6 H 0.9534 0.5023 0.8580 0.037 Uiso 1 1 calc R . . C7 C 0.8651(2) 0.3834(2) 0.8892(2) 0.0359(6) Uani 1 1 d . . . H7A H 0.8448 0.3786 0.9568 0.043 Uiso 1 1 calc R . . H7B H 0.8958 0.3079 0.8819 0.043 Uiso 1 1 calc R . . C8 C 0.7575(2) 0.4413(2) 0.8528(2) 0.0377(6) Uani 1 1 d . . . H8A H 0.7171 0.3868 0.8647 0.045 Uiso 1 1 calc R . . H8B H 0.7057 0.4960 0.8880 0.045 Uiso 1 1 calc R . . C9 C 1.1154(2) 0.6470(2) 0.72588(18) 0.0264(5) Uani 1 1 d . . . H9 H 1.1720 0.5783 0.7313 0.032 Uiso 1 1 calc R . . C10 C 1.1312(2) 0.7436(2) 0.7238(2) 0.0309(5) Uani 1 1 d . . . H10 H 1.1979 0.7533 0.7279 0.037 Uiso 1 1 calc R . . C11 C 1.0302(2) 0.8218(2) 0.71451(18) 0.0277(5) Uani 1 1 d . . . H11 H 1.0128 0.8971 0.7112 0.033 Uiso 1 1 calc R . . C12 C 0.8401(2) 0.8167(2) 0.71108(18) 0.0289(5) Uani 1 1 d . . . H12A H 0.8147 0.8950 0.7107 0.035 Uiso 1 1 calc R . . H12B H 0.7940 0.7773 0.7688 0.035 Uiso 1 1 calc R . . C13 C 0.7789(3) 0.8852(3) 0.5603(2) 0.0474(8) Uani 1 1 d . . . H13 H 0.7563 0.9620 0.5528 0.057 Uiso 1 1 calc R . . C14 C 0.7744(3) 0.8331(4) 0.5023(2) 0.0584(11) Uani 1 1 d . . . H14 H 0.7488 0.8662 0.4466 0.070 Uiso 1 1 calc R . . C15 C 0.8146(3) 0.7232(3) 0.5417(2) 0.0484(9) Uani 1 1 d . . . H15 H 0.8209 0.6669 0.5164 0.058 Uiso 1 1 calc R . . B1 B 0.4623(2) 0.17676(19) 0.73657(16) 0.0172(4) Uani 1 1 d . . . C16 C 0.59707(17) 0.15134(17) 0.73401(14) 0.0173(4) Uani 1 1 d . . . C17 C 0.62779(18) 0.12102(17) 0.81839(14) 0.0181(4) Uani 1 1 d . . . H17 H 0.5699 0.1158 0.8756 0.022 Uiso 1 1 calc R . . C18 C 0.74048(18) 0.09837(17) 0.82090(14) 0.0182(4) Uani 1 1 d . . . C19 C 0.82800(18) 0.10542(17) 0.73894(15) 0.0188(4) Uani 1 1 d . . . H19 H 0.9048 0.0904 0.7405 0.023 Uiso 1 1 calc R . . C20 C 0.79956(18) 0.13503(17) 0.65501(15) 0.0192(4) Uani 1 1 d . . . C21 C 0.68648(18) 0.15831(17) 0.65185(14) 0.0184(4) Uani 1 1 d . . . H21 H 0.6699 0.1793 0.5929 0.022 Uiso 1 1 calc R . . C22 C 0.7678(2) 0.0701(2) 0.91275(16) 0.0245(4) Uani 1 1 d . . . F22A F 0.69731(13) 0.01807(13) 0.98402(9) 0.0285(3) Uani 1 1 d . . . F22B F 0.87401(14) 0.00597(17) 0.91296(12) 0.0433(4) Uani 1 1 d . . . F22C F 0.75815(19) 0.16058(15) 0.93431(12) 0.0461(5) Uani 1 1 d . . . C23 C 0.8917(2) 0.1426(2) 0.56494(16) 0.0256(4) Uani 1 1 d . . . F23A F 0.99333(16) 0.0811(2) 0.57649(15) 0.0807(9) Uani 1 1 d . . . F23B F 0.9045(2) 0.24034(17) 0.52400(17) 0.0832(10) Uani 1 1 d . . . F23C F 0.8738(2) 0.1125(4) 0.50338(18) 0.1081(14) Uani 1 1 d . . . C24 C 0.44252(18) 0.24017(18) 0.63135(14) 0.0182(4) Uani 1 1 d . C . C25 C 0.38767(18) 0.35166(19) 0.60310(15) 0.0205(4) Uani 1 1 d . . . H25 H 0.3548 0.3930 0.6481 0.025 Uiso 1 1 calc R . . C26 C 0.3795(2) 0.4046(2) 0.51110(16) 0.0235(4) Uani 1 1 d . C . C27 C 0.4267(2) 0.3486(2) 0.44282(16) 0.0264(5) Uani 1 1 d . . . H27 H 0.4229 0.3851 0.3798 0.032 Uiso 1 1 calc R A 1 C29 C 0.48657(19) 0.18364(19) 0.56141(15) 0.0222(4) Uani 1 1 d . . . H29 H 0.5219 0.1070 0.5774 0.027 Uiso 1 1 calc R B 1 C30 C 0.3140(2) 0.5232(2) 0.48901(17) 0.0304(5) Uani 1 1 d . . . F30A F 0.20055(15) 0.53553(15) 0.52172(13) 0.0451(4) Uani 1 1 d . C . F30B F 0.33175(17) 0.57218(15) 0.39690(11) 0.0440(4) Uani 1 1 d . C . F30C F 0.33855(18) 0.58215(14) 0.52752(14) 0.0445(4) Uani 1 1 d . C . C28A C 0.4797(2) 0.2373(2) 0.46910(16) 0.0266(5) Uani 0.73 1 d PD C 1 C31A C 0.53419(15) 0.17428(13) 0.39713(10) 0.0369(6) Uani 0.73 1 d PGD C 1 F31A F 0.51284(15) 0.08151(13) 0.42476(10) 0.0456(7) Uani 0.73 1 d PR C 1 F31B F 0.48395(15) 0.23068(13) 0.32083(10) 0.0669(9) Uani 0.73 1 d PR C 1 F31C F 0.63796(15) 0.17178(13) 0.35625(10) 0.0584(9) Uani 0.73 1 d PR C 1 C28B C 0.4797(2) 0.2373(2) 0.46910(16) 0.0266(5) Uani 0.27 1 d PD C 2 C31B C 0.5299(4) 0.1771(3) 0.3952(2) 0.0369(6) Uani 0.27 1 d PGD C 2 F31D F 0.6418(4) 0.0842(3) 0.4179(2) 0.0669(9) Uani 0.27 1 d PR C 2 F31E F 0.4750(4) 0.1279(3) 0.3784(2) 0.054(2) Uani 0.27 1 d PR C 2 F31F F 0.5984(4) 0.2216(3) 0.3184(2) 0.0427(18) Uani 0.27 1 d PR C 2 C32 C 0.38507(17) 0.25501(17) 0.80798(14) 0.0167(4) Uani 1 1 d . F . C33 C 0.28704(18) 0.23774(17) 0.87910(14) 0.0181(4) Uani 1 1 d . . . H33 H 0.2629 0.1758 0.8886 0.022 Uiso 1 1 calc R . . C34 C 0.22356(18) 0.30873(18) 0.93651(15) 0.0201(4) Uani 1 1 d . F . C35 C 0.25502(19) 0.40043(19) 0.92554(16) 0.0220(4) Uani 1 1 d . . . H35 H 0.2114 0.4490 0.9642 0.026 Uiso 1 1 calc R D 1 C37 C 0.41643(18) 0.34751(17) 0.79952(15) 0.0190(4) Uani 1 1 d . . . H37 H 0.4836 0.3617 0.7536 0.023 Uiso 1 1 calc R E 1 C38 C 0.1242(2) 0.2807(2) 1.01495(17) 0.0279(5) Uani 1 1 d . . . F38A F 0.06501(13) 0.23607(13) 0.99279(10) 0.0303(3) Uani 1 1 d . F . F38B F 0.04877(16) 0.36823(16) 1.04395(14) 0.0518(5) Uani 1 1 d . F . F38C F 0.15906(16) 0.20693(17) 1.09057(10) 0.0441(4) Uani 1 1 d . F . C36A C 0.35258(19) 0.41863(18) 0.85601(16) 0.0211(4) Uani 0.80 1 d PD F 1 C39A C 0.39234(13) 0.51559(11) 0.84306(12) 0.0336(6) Uani 0.80 1 d PGD F 1 F39A F 0.32970(13) 0.57401(11) 0.89833(12) 0.0806(12) Uani 0.80 1 d PR F 1 F39B F 0.38017(13) 0.58744(11) 0.75305(12) 0.0559(6) Uani 0.80 1 d PR F 1 F39C F 0.50014(13) 0.49922(11) 0.82291(12) 0.0684(10) Uani 0.80 1 d PR F 1 C36B C 0.35258(19) 0.41863(18) 0.85601(16) 0.0211(4) Uani 0.20 1 d PD F 2 C39B C 0.3853(5) 0.5177(3) 0.8482(5) 0.0336(6) Uani 0.20 1 d PGD F 2 F39D F 0.4127(5) 0.4998(3) 0.9380(5) 0.0559(6) Uani 0.20 1 d PR F 2 F39E F 0.3225(5) 0.6035(3) 0.8279(5) 0.049(2) Uani 0.20 1 d PRU F 2 F39F F 0.4770(5) 0.5298(3) 0.7843(5) 0.0806(12) Uani 0.20 1 d PRU F 2 C40 C 0.42618(17) 0.06179(17) 0.77357(14) 0.0170(4) Uani 1 1 d . I . C41 C 0.49160(18) -0.03994(18) 0.81532(15) 0.0197(4) Uani 1 1 d . . . H41 H 0.5649 -0.0456 0.8192 0.024 Uiso 1 1 calc R G 1 C43 C 0.34587(19) -0.12921(18) 0.84843(15) 0.0208(4) Uani 1 1 d . . . H43 H 0.3190 -0.1926 0.8738 0.025 Uiso 1 1 calc R H 1 C44 C 0.27976(18) -0.02947(19) 0.80719(15) 0.0208(4) Uani 1 1 d . I . C45 C 0.31953(18) 0.06333(18) 0.76928(15) 0.0201(4) Uani 1 1 d . . . H45 H 0.2729 0.1300 0.7395 0.024 Uiso 1 1 calc R I . C42A C 0.45294(19) -0.13371(18) 0.85158(16) 0.0210(4) Uani 0.73 1 d PD I 1 C46A C 0.52768(15) -0.23813(11) 0.89440(13) 0.0374(6) Uani 0.73 1 d PGD I 1 F46A F 0.47728(15) -0.31924(11) 0.93685(13) 0.0510(8) Uani 0.73 1 d PR I 1 F46B F 0.62184(15) -0.27670(11) 0.84020(13) 0.0627(9) Uani 0.73 1 d PR I 1 F46C F 0.55497(15) -0.22672(11) 0.96379(13) 0.0862(14) Uani 0.73 1 d PR I 1 C42B C 0.45294(19) -0.13371(18) 0.85158(16) 0.0210(4) Uani 0.27 1 d PD I 2 C46B C 0.5285(4) -0.2402(2) 0.8904(4) 0.0374(6) Uani 0.27 1 d PGD I 2 F46D F 0.4767(4) -0.3110(2) 0.9654(4) 0.0510(8) Uani 0.27 1 d PR I 2 F46E F 0.6081(4) -0.2903(2) 0.8043(4) 0.0862(14) Uani 0.27 1 d PR I 2 F46F F 0.6180(4) -0.2420(2) 0.9063(4) 0.064(3) Uani 0.27 1 d PR I 2 C47 C 0.1609(2) -0.0180(2) 0.8070(2) 0.0311(5) Uani 1 1 d . . . F47A F 0.14698(19) 0.0135(2) 0.72034(16) 0.0681(7) Uani 1 1 d . I . F47B F 0.12891(15) -0.10934(14) 0.84928(15) 0.0436(4) Uani 1 1 d . I . F47C F 0.08360(15) 0.05787(18) 0.8491(2) 0.0674(7) Uani 1 1 d . I . 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 0.02151(9) 0.03337(11) 0.02548(10) -0.01405(7) -0.00181(7) -0.01237(7) N1 0.0197(9) 0.0247(9) 0.0220(9) -0.0082(7) -0.0046(7) -0.0068(7) N2 0.0214(9) 0.0241(9) 0.0219(9) -0.0072(7) -0.0044(7) -0.0064(7) N3 0.0228(10) 0.0433(12) 0.0260(10) 0.0001(9) -0.0084(8) -0.0118(9) N4 0.0282(11) 0.0546(14) 0.0219(9) -0.0070(9) -0.0058(8) -0.0218(10) C1 0.0310(13) 0.0469(16) 0.0460(16) -0.0117(13) -0.0091(12) -0.0229(12) C2 0.057(2) 0.071(2) 0.0473(17) -0.0298(16) -0.0010(15) -0.0438(18) C3 0.066(2) 0.067(2) 0.073(3) -0.051(2) 0.0151(19) -0.039(2) C4 0.0402(17) 0.0477(18) 0.093(3) -0.049(2) 0.0193(18) -0.0193(14) C5 0.0232(12) 0.0254(12) 0.0628(19) -0.0208(12) -0.0018(12) -0.0062(9) C6 0.0265(12) 0.0212(10) 0.0429(14) -0.0068(10) -0.0112(10) -0.0040(9) C7 0.0289(13) 0.0268(12) 0.0452(15) -0.0080(11) -0.0040(11) -0.0071(10) C8 0.0247(12) 0.0345(13) 0.0468(16) -0.0058(12) -0.0017(11) -0.0122(10) C9 0.0218(11) 0.0292(11) 0.0303(11) -0.0093(9) -0.0082(9) -0.0065(9) C10 0.0260(12) 0.0336(12) 0.0394(14) -0.0119(11) -0.0089(10) -0.0123(10) C11 0.0294(12) 0.0278(11) 0.0298(12) -0.0090(9) -0.0059(9) -0.0124(9) C12 0.0216(11) 0.0327(12) 0.0272(11) -0.0081(9) -0.0038(9) -0.0042(9) C13 0.0278(13) 0.064(2) 0.0375(15) 0.0136(14) -0.0149(12) -0.0192(13) C14 0.0446(18) 0.102(3) 0.0300(14) 0.0162(17) -0.0209(13) -0.044(2) C15 0.0423(16) 0.093(3) 0.0234(12) -0.0063(14) -0.0076(11) -0.0431(18) B1 0.0164(10) 0.0206(10) 0.0150(9) -0.0053(8) -0.0016(8) -0.0073(8) C16 0.0166(9) 0.0187(9) 0.0174(9) -0.0065(7) -0.0006(7) -0.0076(7) C17 0.0168(9) 0.0215(9) 0.0165(9) -0.0066(7) -0.0002(7) -0.0082(7) C18 0.0196(9) 0.0177(9) 0.0182(9) -0.0049(7) -0.0041(7) -0.0067(7) C19 0.0166(9) 0.0179(9) 0.0226(10) -0.0072(7) -0.0028(7) -0.0057(7) C20 0.0162(9) 0.0201(9) 0.0194(9) -0.0072(7) 0.0011(7) -0.0064(7) C21 0.0173(9) 0.0209(9) 0.0169(9) -0.0067(7) -0.0008(7) -0.0072(7) C22 0.0239(11) 0.0308(11) 0.0232(10) -0.0062(9) -0.0067(8) -0.0124(9) F22A 0.0291(7) 0.0378(8) 0.0185(6) -0.0019(6) -0.0054(5) -0.0152(6) F22B 0.0230(7) 0.0674(12) 0.0322(8) -0.0025(8) -0.0121(6) -0.0102(7) F22C 0.0845(14) 0.0433(9) 0.0316(8) -0.0080(7) -0.0231(9) -0.0347(10) C23 0.0182(10) 0.0329(12) 0.0216(10) -0.0086(9) 0.0015(8) -0.0075(9) F23A 0.0244(9) 0.1054(19) 0.0387(11) 0.0122(11) 0.0104(8) 0.0145(10) F23B 0.0886(18) 0.0384(11) 0.0585(13) -0.0023(10) 0.0452(13) -0.0188(11) F23C 0.0674(16) 0.251(4) 0.0621(15) -0.108(2) 0.0450(13) -0.099(2) C24 0.0159(9) 0.0250(10) 0.0160(9) -0.0072(7) -0.0015(7) -0.0089(7) C25 0.0169(9) 0.0284(10) 0.0167(9) -0.0079(8) -0.0029(7) -0.0064(8) C26 0.0215(10) 0.0302(11) 0.0199(10) -0.0034(8) -0.0053(8) -0.0114(8) C27 0.0293(12) 0.0378(13) 0.0166(9) -0.0044(9) -0.0047(8) -0.0179(10) C29 0.0219(10) 0.0278(11) 0.0204(10) -0.0096(8) -0.0009(8) -0.0117(8) C30 0.0328(13) 0.0329(12) 0.0226(11) -0.0006(9) -0.0103(9) -0.0094(10) F30A 0.0292(8) 0.0446(10) 0.0476(10) -0.0040(8) -0.0106(7) -0.0021(7) F30B 0.0559(11) 0.0406(9) 0.0249(8) 0.0063(7) -0.0156(8) -0.0110(8) F30C 0.0615(12) 0.0288(8) 0.0511(10) -0.0062(7) -0.0322(9) -0.0083(8) C28A 0.0307(12) 0.0389(13) 0.0169(9) -0.0122(9) 0.0019(8) -0.0197(10) C31A 0.0512(17) 0.0481(16) 0.0195(11) -0.0158(11) 0.0031(11) -0.0272(14) F31A 0.0651(18) 0.0394(13) 0.0388(14) -0.0262(11) 0.0076(12) -0.0257(12) F31B 0.101(2) 0.0591(16) 0.0357(13) -0.0301(12) -0.0330(15) 0.0155(16) F31C 0.0363(15) 0.075(2) 0.071(2) -0.0522(19) 0.0214(14) -0.0250(15) C28B 0.0307(12) 0.0389(13) 0.0169(9) -0.0122(9) 0.0019(8) -0.0197(10) C31B 0.0512(17) 0.0481(16) 0.0195(11) -0.0158(11) 0.0031(11) -0.0272(14) F31D 0.101(2) 0.0591(16) 0.0357(13) -0.0301(12) -0.0330(15) 0.0155(16) F31E 0.057(5) 0.088(6) 0.045(4) -0.051(4) 0.014(3) -0.043(4) F31F 0.050(5) 0.037(4) 0.031(3) -0.016(3) 0.016(3) -0.019(3) C32 0.0167(9) 0.0199(9) 0.0139(8) -0.0039(7) -0.0036(7) -0.0064(7) C33 0.0192(9) 0.0217(9) 0.0143(8) -0.0059(7) -0.0014(7) -0.0082(7) C34 0.0184(9) 0.0246(10) 0.0166(9) -0.0082(8) 0.0001(7) -0.0067(8) C35 0.0205(10) 0.0257(10) 0.0215(10) -0.0115(8) -0.0036(8) -0.0049(8) C37 0.0176(9) 0.0214(9) 0.0182(9) -0.0046(7) -0.0031(7) -0.0076(7) C38 0.0287(12) 0.0351(12) 0.0217(10) -0.0147(9) 0.0053(9) -0.0150(10) F38A 0.0239(7) 0.0415(8) 0.0285(7) -0.0126(6) 0.0024(6) -0.0177(6) F38B 0.0410(10) 0.0535(11) 0.0580(12) -0.0407(10) 0.0287(9) -0.0240(8) F38C 0.0486(10) 0.0717(12) 0.0159(7) -0.0031(7) -0.0014(7) -0.0359(9) C36A 0.0221(10) 0.0199(9) 0.0235(10) -0.0071(8) -0.0052(8) -0.0074(8) C39A 0.0253(12) 0.0259(11) 0.0507(16) -0.0194(11) 0.0018(11) -0.0102(9) F39A 0.089(2) 0.0775(19) 0.090(2) -0.0700(18) 0.0512(18) -0.0629(18) F39B 0.0713(18) 0.0373(12) 0.0596(16) 0.0034(11) -0.0188(14) -0.0293(12) F39C 0.0308(12) 0.0431(13) 0.149(3) -0.0381(17) -0.0282(16) -0.0124(10) C36B 0.0221(10) 0.0199(9) 0.0235(10) -0.0071(8) -0.0052(8) -0.0074(8) C39B 0.0253(12) 0.0259(11) 0.0507(16) -0.0194(11) 0.0018(11) -0.0102(9) F39D 0.0713(18) 0.0373(12) 0.0596(16) 0.0034(11) -0.0188(14) -0.0293(12) F39E 0.032(4) 0.017(3) 0.095(6) -0.008(4) -0.025(4) -0.004(3) F39F 0.089(2) 0.0775(19) 0.090(2) -0.0700(18) 0.0512(18) -0.0629(18) C40 0.0163(9) 0.0212(9) 0.0145(8) -0.0084(7) 0.0007(7) -0.0072(7) C41 0.0165(9) 0.0234(10) 0.0202(9) -0.0087(8) -0.0004(7) -0.0080(7) C43 0.0211(10) 0.0243(10) 0.0205(9) -0.0105(8) 0.0009(8) -0.0113(8) C44 0.0178(9) 0.0279(10) 0.0211(9) -0.0108(8) -0.0016(8) -0.0101(8) C45 0.0174(9) 0.0243(10) 0.0210(9) -0.0096(8) -0.0027(7) -0.0069(8) C42A 0.0203(10) 0.0204(9) 0.0230(10) -0.0083(8) -0.0029(8) -0.0064(8) C46A 0.0328(14) 0.0250(12) 0.0562(18) -0.0009(11) -0.0195(13) -0.0117(10) F46A 0.0431(11) 0.0265(9) 0.077(2) 0.0073(11) -0.0221(13) -0.0166(8) F46B 0.0249(12) 0.0463(16) 0.076(2) -0.0068(14) 0.0039(13) 0.0099(11) F46C 0.140(4) 0.0349(14) 0.112(3) -0.0105(17) -0.106(3) 0.0075(18) C42B 0.0203(10) 0.0204(9) 0.0230(10) -0.0083(8) -0.0029(8) -0.0064(8) C46B 0.0328(14) 0.0250(12) 0.0562(18) -0.0009(11) -0.0195(13) -0.0117(10) F46D 0.0431(11) 0.0265(9) 0.077(2) 0.0073(11) -0.0221(13) -0.0166(8) F46E 0.140(4) 0.0349(14) 0.112(3) -0.0105(17) -0.106(3) 0.0075(18) F46F 0.030(4) 0.029(4) 0.123(9) 0.015(4) -0.044(5) -0.009(3) C47 0.0225(11) 0.0330(12) 0.0429(14) -0.0106(11) -0.0084(10) -0.0127(9) F47A 0.0520(12) 0.1067(19) 0.0546(12) 0.0120(12) -0.0345(11) -0.0442(13) F47B 0.0342(9) 0.0384(9) 0.0671(12) -0.0053(8) -0.0181(8) -0.0233(7) F47C 0.0174(8) 0.0612(13) 0.135(2) -0.0581(14) 0.0000(10) -0.0108(8) _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 N4 2.096(2) . ? Rh1 N1 2.0987(19) . ? Rh1 C5 2.130(3) . ? Rh1 C1 2.133(3) . ? Rh1 C2 2.141(3) . ? Rh1 C6 2.144(3) . ? N1 C9 1.335(3) . ? N1 N2 1.361(3) . ? N2 C11 1.348(3) . ? N2 C12 1.449(3) . ? N3 C13 1.346(4) . ? N3 N4 1.357(4) . ? N3 C12 1.449(3) . ? N4 C15 1.340(3) . ? C1 C2 1.382(5) . ? C1 C8 1.514(4) . ? C1 H1 0.9500 . ? C2 C3 1.526(6) . ? C2 H2 0.9500 . ? C3 C4 1.523(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C7 1.521(4) . ? C6 H6 0.9500 . ? C7 C8 1.531(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.369(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.372(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? B1 C24 1.640(3) . ? B1 C32 1.641(3) . ? B1 C40 1.643(3) . ? B1 C16 1.645(3) . ? C16 C17 1.405(3) . ? C16 C21 1.405(3) . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 C19 1.390(3) . ? C18 C22 1.500(3) . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.401(3) . ? C20 C23 1.502(3) . ? C21 H21 0.9500 . ? C22 F22B 1.335(3) . ? C22 F22A 1.336(3) . ? C22 F22C 1.344(3) . ? C23 F23B 1.298(3) . ? C23 F23C 1.299(3) . ? C23 F23A 1.314(3) . ? C24 C25 1.397(3) . ? C24 C29 1.409(3) . ? C25 C26 1.396(3) . ? C25 H25 0.9500 . ? C26 C27 1.380(3) . ? C26 C30 1.499(4) . ? C27 C28A 1.386(4) . ? C27 H27 0.9500 . ? C29 C28A 1.397(3) . ? C29 H29 0.9500 . ? C30 F30C 1.340(3) . ? C30 F30B 1.341(3) . ? C30 F30A 1.346(3) . ? C28A C31A 1.490(3) . ? C31A F31C 1.2670 . ? C31A F31A 1.2798 . ? C31A F31B 1.4128 . ? C31B F31E 1.2825 . ? C31B F31F 1.3195 . ? C31B F31D 1.5911 . ? C32 C33 1.401(3) . ? C32 C37 1.410(3) . ? C33 C34 1.398(3) . ? C33 H33 0.9500 . ? C34 C35 1.388(3) . ? C34 C38 1.498(3) . ? C35 C36A 1.389(3) . ? C35 H35 0.9500 . ? C37 C36A 1.389(3) . ? C37 H37 0.9500 . ? C38 F38A 1.332(3) . ? C38 F38B 1.343(3) . ? C38 F38C 1.353(3) . ? C36A C39A 1.512(2) . ? C39A F39A 1.2568 . ? C39A F39C 1.2733 . ? C39A F39B 1.4331 . ? C39B F39E 1.1603 . ? C39B F39F 1.2824 . ? C39B F39D 1.4995 . ? C40 C41 1.396(3) . ? C40 C45 1.405(3) . ? C41 C42A 1.398(3) . ? C41 H41 0.9500 . ? C43 C44 1.381(3) . ? C43 C42A 1.389(3) . ? C43 H43 0.9500 . ? C44 C45 1.393(3) . ? C44 C47 1.496(3) . ? C45 H45 0.9500 . ? C42A C46A 1.476(2) . ? C46A F46B 1.2718 . ? C46A F46A 1.3371 . ? C46A F46C 1.3399 . ? C46B F46F 1.2653 . ? C46B F46D 1.3715 . ? C46B F46E 1.5947 . ? C47 F47B 1.323(3) . ? C47 F47C 1.333(3) . ? C47 F47A 1.340(3) . ? 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 N4 Rh1 N1 87.02(8) . . ? N4 Rh1 C5 160.65(11) . . ? N1 Rh1 C5 92.20(9) . . ? N4 Rh1 C1 90.64(11) . . ? N1 Rh1 C1 155.34(10) . . ? C5 Rh1 C1 97.87(12) . . ? N4 Rh1 C2 94.76(13) . . ? N1 Rh1 C2 166.91(11) . . ? C5 Rh1 C2 81.83(14) . . ? C1 Rh1 C2 37.74(13) . . ? N4 Rh1 C6 161.38(10) . . ? N1 Rh1 C6 93.09(9) . . ? C5 Rh1 C6 37.97(11) . . ? C1 Rh1 C6 81.52(11) . . ? C2 Rh1 C6 89.34(13) . . ? C9 N1 N2 104.65(19) . . ? C9 N1 Rh1 135.26(17) . . ? N2 N1 Rh1 119.95(14) . . ? C11 N2 N1 111.53(19) . . ? C11 N2 C12 128.4(2) . . ? N1 N2 C12 119.56(19) . . ? C13 N3 N4 111.5(3) . . ? C13 N3 C12 129.5(3) . . ? N4 N3 C12 119.0(2) . . ? C15 N4 N3 104.6(3) . . ? C15 N4 Rh1 134.4(3) . . ? N3 N4 Rh1 120.76(16) . . ? C2 C1 C8 125.3(3) . . ? C2 C1 Rh1 71.45(16) . . ? C8 C1 Rh1 110.00(19) . . ? C2 C1 H1 117.3 . . ? C8 C1 H1 117.3 . . ? Rh1 C1 H1 88.5 . . ? C1 C2 C3 124.0(3) . . ? C1 C2 Rh1 70.81(16) . . ? C3 C2 Rh1 112.6(2) . . ? C1 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? Rh1 C2 H2 86.6 . . ? C4 C3 C2 112.5(3) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 112.9(3) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 124.8(3) . . ? C6 C5 Rh1 71.56(15) . . ? C4 C5 Rh1 110.2(3) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? Rh1 C5 H5 88.2 . . ? C5 C6 C7 123.7(2) . . ? C5 C6 Rh1 70.47(17) . . ? C7 C6 Rh1 113.30(18) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? Rh1 C6 H6 86.3 . . ? C6 C7 C8 111.6(2) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C1 C8 C7 112.9(2) . . ? C1 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C1 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C10 111.4(2) . . ? N1 C9 H9 124.3 . . ? C10 C9 H9 124.3 . . ? C11 C10 C9 105.2(2) . . ? C11 C10 H10 127.4 . . ? C9 C10 H10 127.4 . . ? N2 C11 C10 107.2(2) . . ? N2 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? N2 C12 N3 110.8(2) . . ? N2 C12 H12A 109.5 . . ? N3 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C14 106.9(3) . . ? N3 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? C15 C14 C13 105.6(3) . . ? C15 C14 H14 127.2 . . ? C13 C14 H14 127.2 . . ? N4 C15 C14 111.5(3) . . ? N4 C15 H15 124.3 . . ? C14 C15 H15 124.3 . . ? C24 B1 C32 110.06(17) . . ? C24 B1 C40 108.68(16) . . ? C32 B1 C40 110.55(16) . . ? C24 B1 C16 110.07(16) . . ? C32 B1 C16 107.20(16) . . ? C40 B1 C16 110.28(17) . . ? C17 C16 C21 116.14(19) . . ? C17 C16 B1 119.39(17) . . ? C21 C16 B1 124.47(18) . . ? C18 C17 C16 122.13(19) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 121.00(19) . . ? C19 C18 C22 119.12(19) . . ? C17 C18 C22 119.84(19) . . ? C20 C19 C18 117.78(19) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C19 C20 C21 121.58(19) . . ? C19 C20 C23 119.5(2) . . ? C21 C20 C23 118.9(2) . . ? C20 C21 C16 121.4(2) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? F22B C22 F22A 106.8(2) . . ? F22B C22 F22C 106.8(2) . . ? F22A C22 F22C 106.3(2) . . ? F22B C22 C18 112.8(2) . . ? F22A C22 C18 112.53(18) . . ? F22C C22 C18 111.29(19) . . ? F23B C23 F23C 106.1(3) . . ? F23B C23 F23A 104.5(3) . . ? F23C C23 F23A 106.1(3) . . ? F23B C23 C20 113.9(2) . . ? F23C C23 C20 112.8(2) . . ? F23A C23 C20 112.8(2) . . ? C25 C24 C29 115.61(19) . . ? C25 C24 B1 123.97(18) . . ? C29 C24 B1 120.36(19) . . ? C26 C25 C24 122.4(2) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C27 C26 C25 121.1(2) . . ? C27 C26 C30 120.6(2) . . ? C25 C26 C30 118.2(2) . . ? C26 C27 C28A 117.8(2) . . ? C26 C27 H27 121.1 . . ? C28A C27 H27 121.1 . . ? C28A C29 C24 121.7(2) . . ? C28A C29 H29 119.1 . . ? C24 C29 H29 119.1 . . ? F30C C30 F30B 106.9(2) . . ? F30C C30 F30A 106.5(2) . . ? F30B C30 F30A 105.8(2) . . ? F30C C30 C26 112.8(2) . . ? F30B C30 C26 113.4(2) . . ? F30A C30 C26 110.9(2) . . ? C27 C28A C29 121.3(2) . . ? C27 C28A C31A 119.6(2) . . ? C29 C28A C31A 119.1(2) . . ? F31C C31A F31A 114.7 . . ? F31C C31A F31B 100.6 . . ? F31A C31A F31B 102.9 . . ? F31C C31A C28A 114.87(11) . . ? F31A C31A C28A 113.19(11) . . ? F31B C31A C28A 108.84(12) . . ? F31E C31B F31F 112.2 . . ? F31E C31B F31D 104.4 . . ? F31F C31B F31D 86.7 . . ? C33 C32 C37 115.48(19) . . ? C33 C32 B1 124.85(18) . . ? C37 C32 B1 119.67(18) . . ? C34 C33 C32 122.12(19) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C35 C34 C33 121.3(2) . . ? C35 C34 C38 119.75(19) . . ? C33 C34 C38 118.9(2) . . ? C34 C35 C36A 117.6(2) . . ? C34 C35 H35 121.2 . . ? C36A C35 H35 121.2 . . ? C36A C37 C32 122.31(19) . . ? C36A C37 H37 118.8 . . ? C32 C37 H37 118.8 . . ? F38A C38 F38B 106.3(2) . . ? F38A C38 F38C 105.8(2) . . ? F38B C38 F38C 106.8(2) . . ? F38A C38 C34 113.24(19) . . ? F38B C38 C34 112.9(2) . . ? F38C C38 C34 111.3(2) . . ? C35 C36A C37 121.2(2) . . ? C35 C36A C39A 119.66(19) . . ? C37 C36A C39A 119.13(18) . . ? F39A C39A F39C 118.2 . . ? F39A C39A F39B 103.4 . . ? F39C C39A F39B 94.9 . . ? F39A C39A C36A 114.24(10) . . ? F39C C39A C36A 115.91(10) . . ? F39B C39A C36A 106.42(11) . . ? F39E C39B F39F 100.8 . . ? F39E C39B F39D 111.4 . . ? F39F C39B F39D 104.9 . . ? C41 C40 C45 115.55(19) . . ? C41 C40 B1 124.70(18) . . ? C45 C40 B1 119.65(18) . . ? C40 C41 C42A 122.2(2) . . ? C40 C41 H41 118.9 . . ? C42A C41 H41 118.9 . . ? C44 C43 C42A 117.8(2) . . ? C44 C43 H43 121.1 . . ? C42A C43 H43 121.1 . . ? C43 C44 C45 121.1(2) . . ? C43 C44 C47 120.2(2) . . ? C45 C44 C47 118.6(2) . . ? C44 C45 C40 122.3(2) . . ? C44 C45 H45 118.9 . . ? C40 C45 H45 118.9 . . ? C43 C42A C41 121.0(2) . . ? C43 C42A C46A 120.27(19) . . ? C41 C42A C46A 118.76(19) . . ? F46B C46A F46A 105.9 . . ? F46B C46A F46C 106.2 . . ? F46A C46A F46C 103.5 . . ? F46B C46A C42A 116.40(12) . . ? F46A C46A C42A 113.79(11) . . ? F46C C46A C42A 110.03(11) . . ? F46F C46B F46D 108.1 . . ? F46F C46B F46E 88.4 . . ? F46D C46B F46E 114.7 . . ? F47B C47 F47C 106.6(2) . . ? F47B C47 F47A 105.8(2) . . ? F47C C47 F47A 105.5(3) . . ? F47B C47 C44 114.0(2) . . ? F47C C47 C44 111.8(2) . . ? F47A C47 C44 112.6(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 N4 Rh1 N1 C9 -143.9(2) . . . . ? C5 Rh1 N1 C9 16.7(2) . . . . ? C1 Rh1 N1 C9 131.0(3) . . . . ? C2 Rh1 N1 C9 -45.7(6) . . . . ? C6 Rh1 N1 C9 54.7(2) . . . . ? N4 Rh1 N1 N2 31.10(17) . . . . ? C5 Rh1 N1 N2 -168.26(18) . . . . ? C1 Rh1 N1 N2 -53.9(3) . . . . ? C2 Rh1 N1 N2 129.3(5) . . . . ? C6 Rh1 N1 N2 -130.26(17) . . . . ? C9 N1 N2 C11 -1.4(3) . . . . ? Rh1 N1 N2 C11 -177.81(16) . . . . ? C9 N1 N2 C12 -174.2(2) . . . . ? Rh1 N1 N2 C12 9.4(3) . . . . ? C13 N3 N4 C15 0.6(3) . . . . ? C12 N3 N4 C15 177.9(2) . . . . ? C13 N3 N4 Rh1 174.95(18) . . . . ? C12 N3 N4 Rh1 -7.7(3) . . . . ? N1 Rh1 N4 C15 140.3(3) . . . . ? C5 Rh1 N4 C15 52.1(4) . . . . ? C1 Rh1 N4 C15 -64.3(3) . . . . ? C2 Rh1 N4 C15 -26.7(3) . . . . ? C6 Rh1 N4 C15 -128.9(3) . . . . ? N1 Rh1 N4 N3 -32.08(18) . . . . ? C5 Rh1 N4 N3 -120.2(3) . . . . ? C1 Rh1 N4 N3 123.4(2) . . . . ? C2 Rh1 N4 N3 160.9(2) . . . . ? C6 Rh1 N4 N3 58.7(4) . . . . ? N4 Rh1 C1 C2 97.0(2) . . . . ? N1 Rh1 C1 C2 -178.8(2) . . . . ? C5 Rh1 C1 C2 -65.6(2) . . . . ? C6 Rh1 C1 C2 -100.0(2) . . . . ? N4 Rh1 C1 C8 -141.2(2) . . . . ? N1 Rh1 C1 C8 -57.0(4) . . . . ? C5 Rh1 C1 C8 56.2(2) . . . . ? C2 Rh1 C1 C8 121.8(3) . . . . ? C6 Rh1 C1 C8 21.8(2) . . . . ? C8 C1 C2 C3 3.1(5) . . . . ? Rh1 C1 C2 C3 104.8(3) . . . . ? C8 C1 C2 Rh1 -101.8(3) . . . . ? N4 Rh1 C2 C1 -84.9(2) . . . . ? N1 Rh1 C2 C1 177.8(4) . . . . ? C5 Rh1 C2 C1 114.3(2) . . . . ? C6 Rh1 C2 C1 76.9(2) . . . . ? N4 Rh1 C2 C3 155.3(2) . . . . ? N1 Rh1 C2 C3 58.0(7) . . . . ? C5 Rh1 C2 C3 -5.5(2) . . . . ? C1 Rh1 C2 C3 -119.8(4) . . . . ? C6 Rh1 C2 C3 -42.9(3) . . . . ? C1 C2 C3 C4 -93.3(4) . . . . ? Rh1 C2 C3 C4 -11.9(4) . . . . ? C2 C3 C4 C5 30.8(5) . . . . ? C3 C4 C5 C6 46.3(5) . . . . ? C3 C4 C5 Rh1 -34.8(4) . . . . ? N4 Rh1 C5 C6 179.5(2) . . . . ? N1 Rh1 C5 C6 92.21(16) . . . . ? C1 Rh1 C5 C6 -65.22(18) . . . . ? C2 Rh1 C5 C6 -99.50(18) . . . . ? N4 Rh1 C5 C4 -59.3(4) . . . . ? N1 Rh1 C5 C4 -146.6(2) . . . . ? C1 Rh1 C5 C4 56.0(2) . . . . ? C2 Rh1 C5 C4 21.7(2) . . . . ? C6 Rh1 C5 C4 121.2(3) . . . . ? C4 C5 C6 C7 3.3(5) . . . . ? Rh1 C5 C6 C7 105.5(3) . . . . ? C4 C5 C6 Rh1 -102.2(4) . . . . ? N4 Rh1 C6 C5 -179.4(3) . . . . ? N1 Rh1 C6 C5 -89.61(16) . . . . ? C1 Rh1 C6 C5 114.58(18) . . . . ? C2 Rh1 C6 C5 77.52(18) . . . . ? N4 Rh1 C6 C7 61.3(4) . . . . ? N1 Rh1 C6 C7 151.14(19) . . . . ? C5 Rh1 C6 C7 -119.2(3) . . . . ? C1 Rh1 C6 C7 -4.7(2) . . . . ? C2 Rh1 C6 C7 -41.7(2) . . . . ? C5 C6 C7 C8 -94.8(3) . . . . ? Rh1 C6 C7 C8 -13.4(3) . . . . ? C2 C1 C8 C7 45.0(4) . . . . ? Rh1 C1 C8 C7 -35.9(3) . . . . ? C6 C7 C8 C1 32.5(4) . . . . ? N2 N1 C9 C10 1.2(3) . . . . ? Rh1 N1 C9 C10 176.77(18) . . . . ? N1 C9 C10 C11 -0.6(3) . . . . ? N1 N2 C11 C10 1.1(3) . . . . ? C12 N2 C11 C10 173.1(2) . . . . ? C9 C10 C11 N2 -0.3(3) . . . . ? C11 N2 C12 N3 124.0(3) . . . . ? N1 N2 C12 N3 -64.6(3) . . . . ? C13 N3 C12 N2 -119.8(3) . . . . ? N4 N3 C12 N2 63.4(3) . . . . ? N4 N3 C13 C14 -0.7(3) . . . . ? C12 N3 C13 C14 -177.7(3) . . . . ? N3 C13 C14 C15 0.5(3) . . . . ? N3 N4 C15 C14 -0.3(3) . . . . ? Rh1 N4 C15 C14 -173.5(2) . . . . ? C13 C14 C15 N4 -0.2(4) . . . . ? C24 B1 C16 C17 165.33(18) . . . . ? C32 B1 C16 C17 45.6(2) . . . . ? C40 B1 C16 C17 -74.8(2) . . . . ? C24 B1 C16 C21 -14.3(3) . . . . ? C32 B1 C16 C21 -134.0(2) . . . . ? C40 B1 C16 C21 105.6(2) . . . . ? C21 C16 C17 C18 -0.4(3) . . . . ? B1 C16 C17 C18 179.96(19) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C16 C17 C18 C22 177.9(2) . . . . ? C17 C18 C19 C20 -0.4(3) . . . . ? C22 C18 C19 C20 -178.01(19) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? C18 C19 C20 C23 -179.44(19) . . . . ? C19 C20 C21 C16 -0.8(3) . . . . ? C23 C20 C21 C16 179.3(2) . . . . ? C17 C16 C21 C20 0.6(3) . . . . ? B1 C16 C21 C20 -179.75(19) . . . . ? C19 C18 C22 F22B -30.3(3) . . . . ? C17 C18 C22 F22B 152.1(2) . . . . ? C19 C18 C22 F22A -151.1(2) . . . . ? C17 C18 C22 F22A 31.2(3) . . . . ? C19 C18 C22 F22C 89.7(3) . . . . ? C17 C18 C22 F22C -88.0(3) . . . . ? C19 C20 C23 F23B -93.9(3) . . . . ? C21 C20 C23 F23B 86.0(3) . . . . ? C19 C20 C23 F23C 145.1(3) . . . . ? C21 C20 C23 F23C -34.9(4) . . . . ? C19 C20 C23 F23A 24.9(3) . . . . ? C21 C20 C23 F23A -155.1(3) . . . . ? C32 B1 C24 C25 12.4(3) . . . . ? C40 B1 C24 C25 133.6(2) . . . . ? C16 B1 C24 C25 -105.5(2) . . . . ? C32 B1 C24 C29 -170.72(18) . . . . ? C40 B1 C24 C29 -49.5(2) . . . . ? C16 B1 C24 C29 71.3(2) . . . . ? C29 C24 C25 C26 -1.6(3) . . . . ? B1 C24 C25 C26 175.4(2) . . . . ? C24 C25 C26 C27 -0.6(3) . . . . ? C24 C25 C26 C30 177.1(2) . . . . ? C25 C26 C27 C28A 1.8(3) . . . . ? C30 C26 C27 C28A -175.9(2) . . . . ? C25 C24 C29 C28A 2.6(3) . . . . ? B1 C24 C29 C28A -174.5(2) . . . . ? C27 C26 C30 F30C -137.8(2) . . . . ? C25 C26 C30 F30C 44.5(3) . . . . ? C27 C26 C30 F30B -16.0(3) . . . . ? C25 C26 C30 F30B 166.3(2) . . . . ? C27 C26 C30 F30A 102.9(3) . . . . ? C25 C26 C30 F30A -74.9(3) . . . . ? C26 C27 C28A C29 -0.8(4) . . . . ? C26 C27 C28A C31A -178.6(2) . . . . ? C24 C29 C28A C27 -1.5(4) . . . . ? C24 C29 C28A C31A 176.30(19) . . . . ? C27 C28A C31A F31C 89.0(2) . . . . ? C29 C28A C31A F31C -88.9(2) . . . . ? C27 C28A C31A F31A -136.56(18) . . . . ? C29 C28A C31A F31A 45.6(2) . . . . ? C27 C28A C31A F31B -22.8(2) . . . . ? C29 C28A C31A F31B 159.33(17) . . . . ? C24 B1 C32 C33 107.9(2) . . . . ? C40 B1 C32 C33 -12.2(3) . . . . ? C16 B1 C32 C33 -132.4(2) . . . . ? C24 B1 C32 C37 -72.0(2) . . . . ? C40 B1 C32 C37 167.95(18) . . . . ? C16 B1 C32 C37 47.7(2) . . . . ? C37 C32 C33 C34 1.2(3) . . . . ? B1 C32 C33 C34 -178.7(2) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C32 C33 C34 C38 -176.1(2) . . . . ? C33 C34 C35 C36A -0.6(3) . . . . ? C38 C34 C35 C36A 175.5(2) . . . . ? C33 C32 C37 C36A -1.8(3) . . . . ? B1 C32 C37 C36A 178.0(2) . . . . ? C35 C34 C38 F38A 145.8(2) . . . . ? C33 C34 C38 F38A -38.0(3) . . . . ? C35 C34 C38 F38B 25.0(3) . . . . ? C33 C34 C38 F38B -158.8(2) . . . . ? C35 C34 C38 F38C -95.1(3) . . . . ? C33 C34 C38 F38C 81.1(3) . . . . ? C34 C35 C36A C37 -0.1(3) . . . . ? C34 C35 C36A C39A -178.27(19) . . . . ? C32 C37 C36A C35 1.3(3) . . . . ? C32 C37 C36A C39A 179.57(18) . . . . ? C35 C36A C39A F39A -0.8(2) . . . . ? C37 C36A C39A F39A -179.06(15) . . . . ? C35 C36A C39A F39C 141.81(17) . . . . ? C37 C36A C39A F39C -36.4(2) . . . . ? C35 C36A C39A F39B -114.24(19) . . . . ? C37 C36A C39A F39B 67.5(2) . . . . ? C24 B1 C40 C41 133.2(2) . . . . ? C32 B1 C40 C41 -105.9(2) . . . . ? C16 B1 C40 C41 12.5(3) . . . . ? C24 B1 C40 C45 -50.8(2) . . . . ? C32 B1 C40 C45 70.1(2) . . . . ? C16 B1 C40 C45 -171.51(18) . . . . ? C45 C40 C41 C42A -0.8(3) . . . . ? B1 C40 C41 C42A 175.30(19) . . . . ? C42A C43 C44 C45 0.6(3) . . . . ? C42A C43 C44 C47 -176.2(2) . . . . ? C43 C44 C45 C40 -2.2(3) . . . . ? C47 C44 C45 C40 174.6(2) . . . . ? C41 C40 C45 C44 2.3(3) . . . . ? B1 C40 C45 C44 -174.07(19) . . . . ? C44 C43 C42A C41 0.9(3) . . . . ? C44 C43 C42A C46A -179.73(19) . . . . ? C40 C41 C42A C43 -0.7(3) . . . . ? C40 C41 C42A C46A 179.87(19) . . . . ? C43 C42A C46A F46B 116.50(18) . . . . ? C41 C42A C46A F46B -64.1(2) . . . . ? C43 C42A C46A F46A -7.1(2) . . . . ? C41 C42A C46A F46A 172.29(15) . . . . ? C43 C42A C46A F46C -122.71(18) . . . . ? C41 C42A C46A F46C 56.7(2) . . . . ? C43 C44 C47 F47B 0.5(3) . . . . ? C45 C44 C47 F47B -176.4(2) . . . . ? C43 C44 C47 F47C 121.4(3) . . . . ? C45 C44 C47 F47C -55.4(3) . . . . ? C43 C44 C47 F47A -120.0(3) . . . . ? C45 C44 C47 F47A 63.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.343 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.091 # Attachment 'rh00401.cif' data_rh00401 _database_code_depnum_ccdc_archive 'CCDC 697502' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C11 H12 Ir N4 O2' _chemical_formula_sum 'C43 H24 B F24 Ir N4 O2' _chemical_formula_weight 1287.67 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' B B 0.0013 0.0007 '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' 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 P21/n _symmetry_space_group_name_Hall -P2yn 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 12.40560(10) _cell_length_b 24.5181(3) _cell_length_c 16.1804(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.5840(10) _cell_angle_gamma 90.00 _cell_volume 4576.36(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 197743 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 30.034 _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 3.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 74647 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13330 _reflns_number_gt 10589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+10.5637P] 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 13330 _refine_ls_number_parameters 727 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.104 _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 0.967886(14) 0.012115(7) 0.585760(10) 0.02534(6) Uani 1 1 d . . . O1 O 0.7589(4) 0.08296(18) 0.5047(3) 0.0505(10) Uani 1 1 d . . . O2 O 1.1050(4) 0.11555(15) 0.6326(2) 0.0414(8) Uani 1 1 d . . . N1 N 1.1129(3) -0.03626(17) 0.6490(2) 0.0267(7) Uani 1 1 d . . . N2 N 1.2294(3) -0.10603(18) 0.6967(3) 0.0317(8) Uani 1 1 d . . . N3 N 0.8161(3) -0.14461(17) 0.5341(3) 0.0309(8) Uani 1 1 d . . . N4 N 0.8707(3) -0.05891(17) 0.5530(2) 0.0272(8) Uani 1 1 d . . . C1 C 1.2261(4) -0.0172(2) 0.6893(4) 0.0385(12) Uani 1 1 d . . . H1 H 1.2491 0.0200 0.6951 0.046 Uiso 1 1 calc R . . C2 C 1.2978(4) -0.0604(2) 0.7187(3) 0.0392(12) Uani 1 1 d . . . H2 H 1.3795 -0.0593 0.7487 0.047 Uiso 1 1 calc R . . C3 C 1.1186(4) -0.0903(2) 0.6552(3) 0.0265(9) Uani 1 1 d . . . C4 C 1.2713(5) -0.1625(2) 0.7137(4) 0.0387(11) Uani 1 1 d . . . H4A H 1.2193 -0.1838 0.7344 0.058 Uiso 1 1 calc R . . H4B H 1.3496 -0.1629 0.7592 0.058 Uiso 1 1 calc R . . H4C H 1.2729 -0.1786 0.6587 0.058 Uiso 1 1 calc R . . C5 C 1.0231(4) -0.1311(2) 0.6262(3) 0.0312(9) Uani 1 1 d . . . H5A H 1.0442 -0.1597 0.5917 0.037 Uiso 1 1 calc R . . H5B H 1.0187 -0.1488 0.6799 0.037 Uiso 1 1 calc R . . C6 C 0.8196(5) -0.2042(2) 0.5393(4) 0.0434(12) Uani 1 1 d . . . H6A H 0.8833 -0.2177 0.5229 0.065 Uiso 1 1 calc R . . H6B H 0.7461 -0.2191 0.4983 0.065 Uiso 1 1 calc R . . H6C H 0.8317 -0.2156 0.6001 0.065 Uiso 1 1 calc R . . C7 C 0.9057(4) -0.1106(2) 0.5717(3) 0.0270(9) Uani 1 1 d . . . C8 C 0.7196(4) -0.1139(2) 0.4887(3) 0.0366(11) Uani 1 1 d . . . H8 H 0.6442 -0.1273 0.4555 0.044 Uiso 1 1 calc R . . C9 C 0.7526(4) -0.0614(2) 0.5002(3) 0.0323(10) Uani 1 1 d . . . H9 H 0.7037 -0.0309 0.4765 0.039 Uiso 1 1 calc R . . C10 C 0.8375(5) 0.0558(2) 0.5350(3) 0.0343(10) Uani 1 1 d . . . C11 C 1.0547(4) 0.0758(2) 0.6165(3) 0.0306(10) Uani 1 1 d . . . B1 B 0.9728(4) 0.14920(18) 0.8572(3) 0.0186(8) Uani 1 1 d . . . C12 C 1.1116(3) 0.13824(16) 0.8818(2) 0.0190(7) Uani 1 1 d . . . C13 C 1.1751(3) 0.10346(16) 0.9523(3) 0.0202(7) Uani 1 1 d . . . H13 H 1.1386 0.0895 0.9902 0.024 Uiso 1 1 calc R . . C14 C 1.2894(3) 0.08890(18) 0.9682(3) 0.0229(8) Uani 1 1 d . . . C15 C 1.3474(3) 0.10995(19) 0.9160(3) 0.0252(8) Uani 1 1 d . . . H15 H 1.4252 0.0998 0.9262 0.030 Uiso 1 1 calc R . . C16 C 1.2881(3) 0.14605(18) 0.8487(3) 0.0236(8) Uani 1 1 d . . . C17 C 1.1727(3) 0.15986(17) 0.8318(3) 0.0205(7) Uani 1 1 d . . . H17 H 1.1346 0.1846 0.7850 0.025 Uiso 1 1 calc R . . C18 C 1.3527(4) 0.0495(2) 1.0403(3) 0.0295(9) Uani 1 1 d . . . F18A F 1.2941(3) 0.0342(2) 1.0894(3) 0.0631(12) Uani 1 1 d . . . F18B F 1.4530(3) 0.07125(16) 1.0975(2) 0.0537(9) Uani 1 1 d . . . F18C F 1.3869(4) 0.00534(15) 1.0095(3) 0.0653(12) Uani 1 1 d . . . C19 C 1.3516(4) 0.1711(2) 0.7949(3) 0.0295(9) Uani 1 1 d . . . F19A F 1.4395(4) 0.2012(3) 0.8426(3) 0.097(2) Uani 1 1 d . . . F19B F 1.3928(5) 0.13387(18) 0.7553(3) 0.0844(16) Uani 1 1 d . . . F19C F 1.2858(3) 0.20249(17) 0.7288(2) 0.0544(9) Uani 1 1 d . . . C20 C 0.8996(3) 0.09542(16) 0.8052(2) 0.0189(7) Uani 1 1 d . C . C21 C 0.9445(3) 0.04230(16) 0.8223(3) 0.0209(7) Uani 1 1 d . . . H21 H 1.0225 0.0376 0.8619 0.025 Uiso 1 1 calc R . . C22 C 0.8804(4) -0.00333(18) 0.7841(3) 0.0257(8) Uani 1 1 d . C . C23 C 0.7653(4) 0.00085(18) 0.7268(3) 0.0260(9) Uani 1 1 d . . . H23 H 0.7204 -0.0306 0.7016 0.031 Uiso 1 1 calc R A 1 C25 C 0.7831(3) 0.09871(17) 0.7468(3) 0.0220(8) Uani 1 1 d . . . H25 H 0.7473 0.1335 0.7335 0.026 Uiso 1 1 calc R B 1 C26 C 0.9340(4) -0.05845(19) 0.8099(3) 0.0320(10) Uani 1 1 d . . . F26A F 1.0416(3) -0.06088(14) 0.8094(3) 0.0506(9) Uani 1 1 d . C . F26B F 0.9438(4) -0.07299(15) 0.8902(2) 0.0618(11) Uani 1 1 d . C . F26C F 0.8779(4) -0.09795(14) 0.7528(3) 0.0711(13) Uani 1 1 d . C . C24A C 0.7189(3) 0.05289(18) 0.7081(3) 0.0247(8) Uani 0.24 1 d PD C 1 C27A C 0.5973(5) 0.0614(5) 0.6413(7) 0.0380(13) Uani 0.24 1 d PGD C 1 F27A F 0.5249(5) 0.0822(5) 0.6835(7) 0.084(2) Uani 0.24 1 d PR C 1 F27B F 0.5829(5) 0.0872(5) 0.5753(7) 0.082(6) Uani 0.24 1 d PRU C 1 F27C F 0.5476(5) 0.0164(5) 0.6058(7) 0.0680(16) Uani 0.24 1 d PRU C 1 C24B C 0.7189(3) 0.05289(18) 0.7081(3) 0.0247(8) Uani 0.76 1 d PD C 2 C27B C 0.5914(2) 0.06081(13) 0.6540(2) 0.0380(13) Uani 0.76 1 d PGD C 2 F27D F 0.5203(2) 0.04611(13) 0.6877(2) 0.084(2) Uani 0.76 1 d PR C 2 F27E F 0.5750(2) 0.11008(13) 0.6067(2) 0.0702(16) Uani 0.76 1 d PRU C 2 F27F F 0.5627(2) 0.01878(13) 0.5793(2) 0.0680(16) Uani 0.76 1 d PRU C 2 C28 C 0.9366(3) 0.20281(16) 0.7921(3) 0.0192(7) Uani 1 1 d . F . C29 C 0.9373(4) 0.25557(17) 0.8231(3) 0.0242(8) Uani 1 1 d . . . H29 H 0.9504 0.2607 0.8842 0.029 Uiso 1 1 calc R . . C30 C 0.9197(4) 0.30124(17) 0.7691(3) 0.0292(9) Uani 1 1 d . F . C31 C 0.8982(4) 0.29625(18) 0.6791(3) 0.0278(9) Uani 1 1 d . . . H31 H 0.8853 0.3274 0.6418 0.033 Uiso 1 1 calc R D 1 C33 C 0.9142(3) 0.19855(17) 0.6998(3) 0.0210(7) Uani 1 1 d . . . H33 H 0.9117 0.1634 0.6746 0.025 Uiso 1 1 calc R E 1 C34 C 0.9258(5) 0.3563(2) 0.8110(4) 0.0418(12) Uani 1 1 d . . . F34A F 0.8515(3) 0.36079(13) 0.8530(2) 0.0481(8) Uani 1 1 d . F . F34B F 0.9069(6) 0.39724(14) 0.7559(3) 0.0945(19) Uani 1 1 d . F . F34C F 1.0311(4) 0.36630(18) 0.8739(4) 0.0847(16) Uani 1 1 d . F . C32A C 0.8960(3) 0.24355(18) 0.6455(3) 0.0246(8) Uani 0.75 1 d PD F 1 C35A C 0.8723(3) 0.23624(13) 0.54932(15) 0.0292(9) Uani 0.75 1 d PGD F 1 F35A F 0.9081(3) 0.18859(13) 0.52789(15) 0.0709(16) Uani 0.75 1 d PRU F 1 F35B F 0.7634(3) 0.23728(13) 0.49793(15) 0.0710(16) Uani 0.75 1 d PRU F 1 F35C F 0.9228(3) 0.27153(13) 0.51501(15) 0.0794(18) Uani 0.75 1 d PRU F 1 C32B C 0.8960(3) 0.24355(18) 0.6455(3) 0.0246(8) Uani 0.25 1 d PD F 2 C35B C 0.8680(7) 0.2380(3) 0.54848(18) 0.0292(9) Uani 0.25 1 d PGD F 2 F35D F 0.8418(7) 0.1844(3) 0.52106(18) 0.048(3) Uani 0.25 1 d PRU F 2 F35E F 0.7815(7) 0.2675(3) 0.49716(18) 0.049(3) Uani 0.25 1 d PRU F 2 F35F F 0.9728(7) 0.2356(3) 0.53787(18) 0.067(4) Uani 0.25 1 d PRU F 2 C36 C 0.9432(3) 0.16101(16) 0.9459(3) 0.0192(7) Uani 1 1 d . I . C37 C 0.8410(3) 0.14282(16) 0.9548(3) 0.0204(7) Uani 1 1 d . . . H37 H 0.7899 0.1200 0.9099 0.025 Uiso 1 1 calc R . . C38 C 0.8119(3) 0.15709(17) 1.0271(3) 0.0227(8) Uani 1 1 d . I . C39 C 0.8839(3) 0.19030(18) 1.0944(3) 0.0244(8) Uani 1 1 d . . . H39 H 0.8634 0.2005 1.1433 0.029 Uiso 1 1 calc R G 1 C41 C 1.0164(3) 0.19363(16) 1.0161(3) 0.0206(7) Uani 1 1 d . . . H41 H 1.0880 0.2060 1.0142 0.025 Uiso 1 1 calc R H 1 C42 C 0.7021(4) 0.1368(2) 1.0350(3) 0.0317(10) Uani 1 1 d . . . F42A F 0.7213(3) 0.10119(16) 1.1014(2) 0.0511(9) Uani 1 1 d . I . F42B F 0.6326(3) 0.11121(16) 0.9617(2) 0.0490(9) Uani 1 1 d . I . F42C F 0.6407(3) 0.17696(15) 1.0518(3) 0.0566(10) Uani 1 1 d . I . C40A C 0.9866(3) 0.20817(17) 1.0879(3) 0.0221(8) Uani 0.77 1 d PD I 1 C43A C 1.0628(2) 0.24450(11) 1.15997(17) 0.0289(9) Uani 0.77 1 d PGD I 1 F43A F 1.1462(2) 0.26759(11) 1.14301(17) 0.0512(12) Uani 0.77 1 d PRU I 1 F43B F 1.1089(2) 0.21974(11) 1.23617(17) 0.0766(17) Uani 0.77 1 d PRU I 1 F43C F 1.0033(2) 0.28723(11) 1.17571(17) 0.0493(12) Uani 0.77 1 d PRU I 1 C40B C 0.9866(3) 0.20817(17) 1.0879(3) 0.0221(8) Uani 0.23 1 d PD I 2 C43B C 1.0703(8) 0.2422(4) 1.1597(6) 0.0289(9) Uani 0.23 1 d PGD I 2 F43D F 1.1343(8) 0.2818(4) 1.1180(6) 0.0512(12) Uani 0.23 1 d PRU I 2 F43E F 1.1651(8) 0.2120(4) 1.2201(6) 0.069(5) Uani 0.23 1 d PRU I 2 F43F F 1.0261(8) 0.2682(4) 1.2075(6) 0.071(6) Uani 0.23 1 d PRU I 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02692(9) 0.02818(10) 0.01853(9) 0.00003(6) 0.00555(6) 0.00373(7) O1 0.048(2) 0.051(2) 0.048(2) 0.0062(19) 0.0122(19) 0.021(2) O2 0.052(2) 0.0323(19) 0.0381(19) -0.0105(16) 0.0149(17) -0.0032(17) N1 0.0228(16) 0.034(2) 0.0185(15) 0.0021(15) 0.0018(13) 0.0029(15) N2 0.0272(18) 0.039(2) 0.0242(18) 0.0087(16) 0.0043(15) 0.0052(17) N3 0.0283(19) 0.033(2) 0.0310(19) -0.0022(16) 0.0104(16) -0.0036(16) N4 0.0222(17) 0.034(2) 0.0224(17) 0.0026(15) 0.0045(14) 0.0011(15) C1 0.028(2) 0.046(3) 0.031(2) 0.007(2) -0.0009(19) -0.008(2) C2 0.022(2) 0.050(3) 0.033(2) 0.008(2) -0.0040(18) -0.001(2) C3 0.026(2) 0.034(2) 0.0168(18) 0.0041(16) 0.0056(15) 0.0034(18) C4 0.034(2) 0.042(3) 0.037(3) 0.009(2) 0.008(2) 0.016(2) C5 0.028(2) 0.029(2) 0.033(2) -0.0020(18) 0.0060(18) 0.0037(18) C6 0.041(3) 0.032(3) 0.054(3) -0.005(2) 0.014(3) -0.005(2) C7 0.023(2) 0.035(2) 0.0233(19) -0.0017(17) 0.0100(16) 0.0000(17) C8 0.023(2) 0.048(3) 0.034(2) 0.002(2) 0.0052(18) -0.005(2) C9 0.021(2) 0.042(3) 0.030(2) 0.004(2) 0.0038(17) 0.0026(19) C10 0.040(3) 0.034(2) 0.029(2) 0.0003(19) 0.013(2) 0.009(2) C11 0.033(2) 0.034(2) 0.022(2) -0.0045(17) 0.0066(17) 0.0028(19) B1 0.0158(18) 0.0167(18) 0.0215(19) -0.0003(15) 0.0047(15) 0.0008(15) C12 0.0165(16) 0.0203(17) 0.0185(16) -0.0013(14) 0.0045(13) -0.0025(14) C13 0.0175(17) 0.0211(18) 0.0212(17) 0.0000(14) 0.0062(14) 0.0004(14) C14 0.0153(16) 0.027(2) 0.0227(18) -0.0027(15) 0.0021(14) 0.0009(15) C15 0.0160(17) 0.032(2) 0.027(2) -0.0011(17) 0.0063(15) 0.0012(16) C16 0.0193(18) 0.030(2) 0.0233(19) -0.0042(16) 0.0095(15) -0.0036(16) C17 0.0184(17) 0.0234(19) 0.0180(17) -0.0015(14) 0.0047(14) -0.0021(14) C18 0.0204(19) 0.034(2) 0.030(2) 0.0040(18) 0.0042(16) 0.0028(17) F18A 0.0332(16) 0.096(3) 0.061(2) 0.052(2) 0.0189(16) 0.0193(19) F18B 0.0341(16) 0.057(2) 0.0462(19) 0.0121(16) -0.0131(14) -0.0016(15) F18C 0.102(3) 0.0364(18) 0.049(2) 0.0054(16) 0.017(2) 0.033(2) C19 0.0208(19) 0.039(3) 0.030(2) 0.0030(19) 0.0115(17) -0.0040(18) F19A 0.075(3) 0.172(5) 0.040(2) -0.008(3) 0.0169(19) -0.091(3) F19B 0.132(4) 0.062(3) 0.115(4) 0.024(3) 0.110(4) 0.027(3) F19C 0.0375(16) 0.072(2) 0.061(2) 0.0327(19) 0.0256(16) 0.0034(16) C20 0.0184(17) 0.0178(17) 0.0182(16) -0.0006(14) 0.0041(14) 0.0003(14) C21 0.0202(17) 0.0173(18) 0.0232(18) 0.0016(14) 0.0058(14) 0.0012(14) C22 0.026(2) 0.0202(18) 0.028(2) 0.0016(16) 0.0069(17) 0.0026(16) C23 0.024(2) 0.0221(19) 0.030(2) -0.0025(16) 0.0071(17) -0.0019(15) C25 0.0215(18) 0.0179(17) 0.0249(19) 0.0005(15) 0.0066(15) 0.0027(15) C26 0.034(2) 0.0195(19) 0.039(2) -0.0003(18) 0.010(2) 0.0016(18) F26A 0.0523(19) 0.0383(17) 0.074(2) 0.0170(17) 0.0380(18) 0.0236(15) F26B 0.101(3) 0.049(2) 0.060(2) 0.0343(18) 0.058(2) 0.042(2) F26C 0.074(3) 0.0238(16) 0.085(3) -0.0110(18) -0.006(2) 0.0066(17) C24A 0.0176(17) 0.026(2) 0.0256(19) -0.0028(16) 0.0017(15) 0.0013(15) C27A 0.023(2) 0.032(2) 0.045(3) -0.004(2) -0.004(2) -0.0034(19) F27A 0.0183(17) 0.139(7) 0.089(4) 0.002(5) 0.011(2) 0.001(3) F27B 0.074(7) 0.079(7) 0.082(7) 0.009(5) 0.017(5) -0.011(5) F27C 0.052(2) 0.072(2) 0.058(3) -0.030(2) -0.0068(18) 0.0125(18) C24B 0.0176(17) 0.026(2) 0.0256(19) -0.0028(16) 0.0017(15) 0.0013(15) C27B 0.023(2) 0.032(2) 0.045(3) -0.004(2) -0.004(2) -0.0034(19) F27D 0.0183(17) 0.139(7) 0.089(4) 0.002(5) 0.011(2) 0.001(3) F27E 0.043(2) 0.040(2) 0.082(3) -0.001(2) -0.031(2) 0.0116(19) F27F 0.052(2) 0.072(2) 0.058(3) -0.030(2) -0.0068(18) 0.0125(18) C28 0.0158(16) 0.0192(17) 0.0221(18) 0.0029(14) 0.0067(14) 0.0022(14) C29 0.0254(19) 0.0226(19) 0.027(2) 0.0013(16) 0.0119(16) 0.0010(16) C30 0.036(2) 0.0166(18) 0.040(2) 0.0018(17) 0.020(2) 0.0050(17) C31 0.027(2) 0.0215(19) 0.038(2) 0.0097(18) 0.0163(18) 0.0070(17) C33 0.0182(17) 0.0187(17) 0.0245(18) 0.0023(14) 0.0060(14) 0.0017(14) C34 0.061(3) 0.026(2) 0.044(3) 0.002(2) 0.025(3) 0.004(2) F34A 0.067(2) 0.0343(16) 0.058(2) -0.0088(15) 0.0410(18) 0.0044(15) F34B 0.215(6) 0.0223(16) 0.082(3) 0.0083(18) 0.097(4) 0.017(3) F34C 0.062(3) 0.052(2) 0.131(4) -0.051(3) 0.025(3) -0.013(2) C32A 0.0188(18) 0.029(2) 0.0255(19) 0.0064(16) 0.0081(15) 0.0065(16) C35A 0.032(2) 0.030(2) 0.027(2) 0.0076(17) 0.0121(18) 0.0078(18) F35A 0.103(4) 0.068(3) 0.042(2) 0.007(2) 0.027(2) 0.040(3) F35B 0.053(3) 0.114(4) 0.043(2) -0.009(3) 0.014(2) 0.012(3) F35C 0.115(4) 0.086(3) 0.048(3) -0.001(2) 0.043(3) -0.052(3) C32B 0.0188(18) 0.029(2) 0.0255(19) 0.0064(16) 0.0081(15) 0.0065(16) C35B 0.032(2) 0.030(2) 0.027(2) 0.0076(17) 0.0121(18) 0.0078(18) F35D 0.053(5) 0.047(5) 0.042(5) 0.002(4) 0.016(4) -0.012(4) F35E 0.059(5) 0.038(5) 0.040(5) 0.008(4) 0.006(4) 0.022(4) F35F 0.063(6) 0.082(6) 0.060(6) 0.000(5) 0.028(4) 0.006(5) C36 0.0190(17) 0.0168(17) 0.0200(17) 0.0025(14) 0.0048(14) 0.0033(14) C37 0.0153(16) 0.0209(18) 0.0229(18) 0.0011(14) 0.0044(14) 0.0004(14) C38 0.0166(17) 0.025(2) 0.0255(19) 0.0043(16) 0.0072(15) 0.0032(15) C39 0.0206(18) 0.031(2) 0.0235(19) -0.0001(16) 0.0101(15) 0.0059(16) C41 0.0183(17) 0.0191(17) 0.0235(18) -0.0001(15) 0.0065(14) -0.0002(14) C42 0.023(2) 0.040(3) 0.036(2) 0.003(2) 0.0154(18) -0.0008(19) F42A 0.0356(16) 0.067(2) 0.0522(19) 0.0247(17) 0.0184(15) -0.0063(16) F42B 0.0258(14) 0.078(3) 0.0441(18) -0.0110(17) 0.0139(13) -0.0183(15) F42C 0.0361(17) 0.053(2) 0.096(3) -0.005(2) 0.0419(19) 0.0041(15) C40A 0.0196(18) 0.0208(18) 0.0239(19) -0.0001(15) 0.0055(15) 0.0017(14) C43A 0.030(2) 0.030(2) 0.026(2) -0.0083(18) 0.0093(17) -0.0015(18) F43A 0.0458(18) 0.063(2) 0.051(2) -0.025(2) 0.0247(17) -0.0250(18) F43B 0.103(4) 0.051(3) 0.040(2) 0.001(2) -0.016(2) -0.018(3) F43C 0.039(2) 0.039(2) 0.071(3) -0.030(2) 0.020(2) -0.0045(18) C40B 0.0196(18) 0.0208(18) 0.0239(19) -0.0001(15) 0.0055(15) 0.0017(14) C43B 0.030(2) 0.030(2) 0.026(2) -0.0083(18) 0.0093(17) -0.0015(18) F43D 0.0458(18) 0.063(2) 0.051(2) -0.025(2) 0.0247(17) -0.0250(18) F43E 0.058(6) 0.068(7) 0.072(7) -0.010(5) 0.014(5) 0.004(5) F43F 0.064(7) 0.074(8) 0.076(7) -0.018(5) 0.027(5) 0.007(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 C11 1.857(5) . ? Ir1 C10 1.861(5) . ? Ir1 N4 2.073(4) . ? Ir1 N1 2.082(4) . ? Ir1 Ir1 3.2120(3) 3_756 ? O1 C10 1.132(6) . ? O2 C11 1.135(6) . ? N1 C3 1.329(6) . ? N1 C1 1.393(6) . ? N2 C3 1.345(6) . ? N2 C2 1.369(7) . ? N2 C4 1.469(7) . ? N3 C7 1.344(6) . ? N3 C8 1.375(7) . ? N3 C6 1.462(7) . ? N4 C7 1.337(6) . ? N4 C9 1.400(6) . ? C1 C2 1.352(8) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C5 1.488(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.486(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.343(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? B1 C36 1.632(6) . ? B1 C28 1.641(6) . ? B1 C12 1.642(6) . ? B1 C20 1.646(6) . ? C12 C17 1.400(5) . ? C12 C13 1.410(5) . ? C13 C14 1.392(5) . ? C13 H13 0.9500 . ? C14 C15 1.394(6) . ? C14 C18 1.495(6) . ? C15 C16 1.386(6) . ? C15 H15 0.9500 . ? C16 C17 1.396(5) . ? C16 C19 1.503(6) . ? C17 H17 0.9500 . ? C18 F18A 1.313(6) . ? C18 F18C 1.326(6) . ? C18 F18B 1.356(5) . ? C19 F19A 1.308(6) . ? C19 F19B 1.321(6) . ? C19 F19C 1.327(6) . ? C20 C21 1.404(5) . ? C20 C25 1.407(5) . ? C21 C22 1.380(6) . ? C21 H21 0.9500 . ? C22 C23 1.391(6) . ? C22 C26 1.496(6) . ? C23 C24A 1.386(6) . ? C23 H23 0.9500 . ? C25 C24A 1.386(6) . ? C25 H25 0.9500 . ? C26 F26B 1.310(6) . ? C26 F26A 1.339(6) . ? C26 F26C 1.342(6) . ? C24A C27A 1.513(5) . ? C27A F27B 1.1980 . ? C27A F27C 1.2912 . ? C27A F27A 1.4084 . ? C27B F27D 1.2492 . ? C27B F27E 1.4043 . ? C27B F27F 1.5270 . ? C28 C29 1.386(6) . ? C28 C33 1.419(6) . ? C29 C30 1.387(6) . ? C29 H29 0.9500 . ? C30 C31 1.385(7) . ? C30 C34 1.501(7) . ? C31 C32A 1.399(6) . ? C31 H31 0.9500 . ? C33 C32A 1.376(6) . ? C33 H33 0.9500 . ? C34 F34B 1.304(6) . ? C34 F34A 1.337(6) . ? C34 F34C 1.350(7) . ? C32A C35A 1.485(5) . ? C35A F35B 1.3007 . ? C35A F35C 1.3056 . ? C35A F35A 1.3398 . ? C35B F35E 1.3083 . ? C35B F35F 1.3728 . ? C35B F35D 1.3859 . ? C36 C37 1.401(5) . ? C36 C41 1.413(5) . ? C37 C38 1.391(6) . ? C37 H37 0.9500 . ? C38 C39 1.389(6) . ? C38 C42 1.499(6) . ? C39 C40A 1.387(6) . ? C39 H39 0.9500 . ? C41 C40A 1.388(6) . ? C41 H41 0.9500 . ? C42 F42C 1.332(6) . ? C42 F42A 1.336(6) . ? C42 F42B 1.339(6) . ? C40A C43A 1.496(4) . ? C43A F43A 1.2942 . ? C43A F43B 1.3028 . ? C43A F43C 1.3589 . ? C43B F43F 1.2726 . ? C43B F43E 1.4281 . ? C43B F43D 1.5556 . ? 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 C11 Ir1 C10 87.6(2) . . ? C11 Ir1 N4 179.26(17) . . ? C10 Ir1 N4 92.4(2) . . ? C11 Ir1 N1 92.07(18) . . ? C10 Ir1 N1 177.00(18) . . ? N4 Ir1 N1 87.89(15) . . ? C11 Ir1 Ir1 94.79(14) . 3_756 ? C10 Ir1 Ir1 100.18(15) . 3_756 ? N4 Ir1 Ir1 85.94(10) . 3_756 ? N1 Ir1 Ir1 82.81(10) . 3_756 ? C3 N1 C1 106.4(4) . . ? C3 N1 Ir1 128.1(3) . . ? C1 N1 Ir1 125.4(3) . . ? C3 N2 C2 108.5(4) . . ? C3 N2 C4 126.1(4) . . ? C2 N2 C4 125.3(4) . . ? C7 N3 C8 108.4(4) . . ? C7 N3 C6 126.3(4) . . ? C8 N3 C6 125.3(4) . . ? C7 N4 C9 106.1(4) . . ? C7 N4 Ir1 128.9(3) . . ? C9 N4 Ir1 125.0(3) . . ? C2 C1 N1 108.8(5) . . ? C2 C1 H1 125.6 . . ? N1 C1 H1 125.6 . . ? C1 C2 N2 106.5(4) . . ? C1 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? N1 C3 N2 109.9(4) . . ? N1 C3 C5 129.3(4) . . ? N2 C3 C5 120.8(4) . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C3 116.8(4) . . ? C7 C5 H5A 108.1 . . ? C3 C5 H5A 108.1 . . ? C7 C5 H5B 108.1 . . ? C3 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N3 109.9(4) . . ? N4 C7 C5 128.5(4) . . ? N3 C7 C5 121.7(4) . . ? C9 C8 N3 106.8(4) . . ? C9 C8 H8 126.6 . . ? N3 C8 H8 126.6 . . ? C8 C9 N4 108.9(4) . . ? C8 C9 H9 125.6 . . ? N4 C9 H9 125.6 . . ? O1 C10 Ir1 179.1(6) . . ? O2 C11 Ir1 177.5(5) . . ? C36 B1 C28 109.0(3) . . ? C36 B1 C12 111.8(3) . . ? C28 B1 C12 107.5(3) . . ? C36 B1 C20 109.4(3) . . ? C28 B1 C20 110.1(3) . . ? C12 B1 C20 109.0(3) . . ? C17 C12 C13 115.9(4) . . ? C17 C12 B1 122.8(3) . . ? C13 C12 B1 121.2(3) . . ? C14 C13 C12 122.1(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 120.7(4) . . ? C13 C14 C18 121.1(4) . . ? C15 C14 C18 118.2(4) . . ? C16 C15 C14 118.0(4) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C17 121.2(4) . . ? C15 C16 C19 118.4(4) . . ? C17 C16 C19 120.4(4) . . ? C16 C17 C12 121.9(4) . . ? C16 C17 H17 119.0 . . ? C12 C17 H17 119.0 . . ? F18A C18 F18C 108.6(5) . . ? F18A C18 F18B 105.8(4) . . ? F18C C18 F18B 103.7(4) . . ? F18A C18 C14 114.1(4) . . ? F18C C18 C14 112.5(4) . . ? F18B C18 C14 111.4(4) . . ? F19A C19 F19B 106.8(5) . . ? F19A C19 F19C 106.2(5) . . ? F19B C19 F19C 104.0(4) . . ? F19A C19 C16 113.0(4) . . ? F19B C19 C16 112.2(4) . . ? F19C C19 C16 113.9(4) . . ? C21 C20 C25 114.9(4) . . ? C21 C20 B1 122.5(3) . . ? C25 C20 B1 122.3(3) . . ? C22 C21 C20 122.8(4) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C21 C22 C23 121.3(4) . . ? C21 C22 C26 118.9(4) . . ? C23 C22 C26 119.6(4) . . ? C24A C23 C22 117.0(4) . . ? C24A C23 H23 121.5 . . ? C22 C23 H23 121.5 . . ? C24A C25 C20 122.3(4) . . ? C24A C25 H25 118.9 . . ? C20 C25 H25 118.9 . . ? F26B C26 F26A 105.3(4) . . ? F26B C26 F26C 108.8(4) . . ? F26A C26 F26C 103.3(4) . . ? F26B C26 C22 113.1(4) . . ? F26A C26 C22 112.3(4) . . ? F26C C26 C22 113.3(4) . . ? C23 C24A C25 121.6(4) . . ? C23 C24A C27A 120.5(6) . . ? C25 C24A C27A 117.8(6) . . ? F27B C27A F27C 99.5 . . ? F27B C27A F27A 109.2 . . ? F27C C27A F27A 103.8 . . ? F27B C27A C24A 119.5(6) . . ? F27C C27A C24A 112.8(5) . . ? F27A C27A C24A 110.5(5) . . ? F27D C27B F27E 120.2 . . ? F27D C27B F27F 98.9 . . ? F27E C27B F27F 101.8 . . ? C29 C28 C33 115.0(4) . . ? C29 C28 B1 123.5(4) . . ? C33 C28 B1 121.2(3) . . ? C28 C29 C30 123.2(4) . . ? C28 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C31 C30 C29 121.0(4) . . ? C31 C30 C34 120.8(4) . . ? C29 C30 C34 118.2(4) . . ? C30 C31 C32A 117.3(4) . . ? C30 C31 H31 121.3 . . ? C32A C31 H31 121.3 . . ? C32A C33 C28 122.4(4) . . ? C32A C33 H33 118.8 . . ? C28 C33 H33 118.8 . . ? F34B C34 F34A 107.5(5) . . ? F34B C34 F34C 104.9(6) . . ? F34A C34 F34C 105.0(5) . . ? F34B C34 C30 114.6(5) . . ? F34A C34 C30 111.9(4) . . ? F34C C34 C30 112.2(5) . . ? C33 C32A C31 121.2(4) . . ? C33 C32A C35A 119.7(4) . . ? C31 C32A C35A 119.2(4) . . ? F35B C35A F35C 105.3 . . ? F35B C35A F35A 102.5 . . ? F35C C35A F35A 102.2 . . ? F35B C35A C32A 115.26(19) . . ? F35C C35A C32A 115.1(2) . . ? F35A C35A C32A 114.8(2) . . ? F35E C35B F35F 122.5 . . ? F35E C35B F35D 106.3 . . ? F35F C35B F35D 92.4 . . ? C37 C36 C41 115.8(4) . . ? C37 C36 B1 122.6(3) . . ? C41 C36 B1 121.5(3) . . ? C38 C37 C36 122.1(4) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C39 C38 C37 121.0(4) . . ? C39 C38 C42 118.1(4) . . ? C37 C38 C42 120.9(4) . . ? C40A C39 C38 118.0(4) . . ? C40A C39 H39 121.0 . . ? C38 C39 H39 121.0 . . ? C40A C41 C36 121.9(4) . . ? C40A C41 H41 119.1 . . ? C36 C41 H41 119.1 . . ? F42C C42 F42A 105.4(4) . . ? F42C C42 F42B 107.3(4) . . ? F42A C42 F42B 105.8(4) . . ? F42C C42 C38 112.3(4) . . ? F42A C42 C38 112.7(4) . . ? F42B C42 C38 112.9(4) . . ? C39 C40A C41 121.1(4) . . ? C39 C40A C43A 117.6(3) . . ? C41 C40A C43A 121.2(3) . . ? F43A C43A F43B 107.3 . . ? F43A C43A F43C 103.6 . . ? F43B C43A F43C 105.2 . . ? F43A C43A C40A 114.88(19) . . ? F43B C43A C40A 113.1(2) . . ? F43C C43A C40A 111.95(19) . . ? F43F C43B F43E 105.9 . . ? F43F C43B F43D 110.7 . . ? F43E C43B F43D 101.4 . . ? 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 C11 Ir1 N1 C3 -179.8(4) . . . . ? N4 Ir1 N1 C3 0.9(4) . . . . ? Ir1 Ir1 N1 C3 -85.3(4) 3_756 . . . ? C11 Ir1 N1 C1 -3.8(4) . . . . ? N4 Ir1 N1 C1 177.0(4) . . . . ? Ir1 Ir1 N1 C1 90.8(4) 3_756 . . . ? C10 Ir1 N4 C7 -177.2(4) . . . . ? N1 Ir1 N4 C7 -0.2(4) . . . . ? Ir1 Ir1 N4 C7 82.7(4) 3_756 . . . ? C10 Ir1 N4 C9 7.1(4) . . . . ? N1 Ir1 N4 C9 -175.9(4) . . . . ? Ir1 Ir1 N4 C9 -93.0(4) 3_756 . . . ? C3 N1 C1 C2 0.3(6) . . . . ? Ir1 N1 C1 C2 -176.5(3) . . . . ? N1 C1 C2 N2 0.0(6) . . . . ? C3 N2 C2 C1 -0.3(6) . . . . ? C4 N2 C2 C1 178.1(5) . . . . ? C1 N1 C3 N2 -0.5(5) . . . . ? Ir1 N1 C3 N2 176.2(3) . . . . ? C1 N1 C3 C5 177.6(5) . . . . ? Ir1 N1 C3 C5 -5.7(7) . . . . ? C2 N2 C3 N1 0.5(5) . . . . ? C4 N2 C3 N1 -177.9(4) . . . . ? C2 N2 C3 C5 -177.8(4) . . . . ? C4 N2 C3 C5 3.8(7) . . . . ? N1 C3 C5 C7 9.1(7) . . . . ? N2 C3 C5 C7 -173.0(4) . . . . ? C9 N4 C7 N3 -0.4(5) . . . . ? Ir1 N4 C7 N3 -176.7(3) . . . . ? C9 N4 C7 C5 -179.4(4) . . . . ? Ir1 N4 C7 C5 4.2(7) . . . . ? C8 N3 C7 N4 0.6(5) . . . . ? C6 N3 C7 N4 179.9(5) . . . . ? C8 N3 C7 C5 179.7(4) . . . . ? C6 N3 C7 C5 -1.0(7) . . . . ? C3 C5 C7 N4 -8.3(7) . . . . ? C3 C5 C7 N3 172.8(4) . . . . ? C7 N3 C8 C9 -0.5(6) . . . . ? C6 N3 C8 C9 -179.9(5) . . . . ? N3 C8 C9 N4 0.3(6) . . . . ? C7 N4 C9 C8 0.1(5) . . . . ? Ir1 N4 C9 C8 176.6(3) . . . . ? C36 B1 C12 C17 -138.4(4) . . . . ? C28 B1 C12 C17 -18.8(5) . . . . ? C20 B1 C12 C17 100.6(4) . . . . ? C36 B1 C12 C13 45.4(5) . . . . ? C28 B1 C12 C13 165.0(3) . . . . ? C20 B1 C12 C13 -75.7(4) . . . . ? C17 C12 C13 C14 -3.6(6) . . . . ? B1 C12 C13 C14 172.8(4) . . . . ? C12 C13 C14 C15 2.2(6) . . . . ? C12 C13 C14 C18 -176.6(4) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C18 C14 C15 C16 179.5(4) . . . . ? C14 C15 C16 C17 -1.8(6) . . . . ? C14 C15 C16 C19 177.1(4) . . . . ? C15 C16 C17 C12 0.2(6) . . . . ? C19 C16 C17 C12 -178.6(4) . . . . ? C13 C12 C17 C16 2.4(6) . . . . ? B1 C12 C17 C16 -174.0(4) . . . . ? C13 C14 C18 F18A -4.9(6) . . . . ? C15 C14 C18 F18A 176.3(4) . . . . ? C13 C14 C18 F18C 119.4(5) . . . . ? C15 C14 C18 F18C -59.5(6) . . . . ? C13 C14 C18 F18B -124.6(4) . . . . ? C15 C14 C18 F18B 56.5(6) . . . . ? C15 C16 C19 F19A -62.5(6) . . . . ? C17 C16 C19 F19A 116.4(5) . . . . ? C15 C16 C19 F19B 58.3(6) . . . . ? C17 C16 C19 F19B -122.8(5) . . . . ? C15 C16 C19 F19C 176.2(4) . . . . ? C17 C16 C19 F19C -4.9(6) . . . . ? C36 B1 C20 C21 -91.0(4) . . . . ? C28 B1 C20 C21 149.2(4) . . . . ? C12 B1 C20 C21 31.5(5) . . . . ? C36 B1 C20 C25 82.5(4) . . . . ? C28 B1 C20 C25 -37.3(5) . . . . ? C12 B1 C20 C25 -155.0(4) . . . . ? C25 C20 C21 C22 0.9(6) . . . . ? B1 C20 C21 C22 174.8(4) . . . . ? C20 C21 C22 C23 -1.2(7) . . . . ? C20 C21 C22 C26 -177.0(4) . . . . ? C21 C22 C23 C24A 1.6(7) . . . . ? C26 C22 C23 C24A 177.4(4) . . . . ? C21 C20 C25 C24A -1.2(6) . . . . ? B1 C20 C25 C24A -175.1(4) . . . . ? C21 C22 C26 F26B 72.5(6) . . . . ? C23 C22 C26 F26B -103.4(6) . . . . ? C21 C22 C26 F26A -46.6(6) . . . . ? C23 C22 C26 F26A 137.5(5) . . . . ? C21 C22 C26 F26C -163.1(5) . . . . ? C23 C22 C26 F26C 21.0(7) . . . . ? C22 C23 C24A C25 -2.0(7) . . . . ? C22 C23 C24A C27A 175.5(7) . . . . ? C20 C25 C24A C23 1.8(7) . . . . ? C20 C25 C24A C27A -175.7(7) . . . . ? C23 C24A C27A F27B -117.3(5) . . . . ? C25 C24A C27A F27B 60.2(6) . . . . ? C23 C24A C27A F27C -1.1(7) . . . . ? C25 C24A C27A F27C 176.5(3) . . . . ? C23 C24A C27A F27A 114.7(5) . . . . ? C25 C24A C27A F27A -67.8(6) . . . . ? C36 B1 C28 C29 29.0(5) . . . . ? C12 B1 C28 C29 -92.4(4) . . . . ? C20 B1 C28 C29 149.0(4) . . . . ? C36 B1 C28 C33 -157.9(3) . . . . ? C12 B1 C28 C33 80.7(4) . . . . ? C20 B1 C28 C33 -37.9(5) . . . . ? C33 C28 C29 C30 -1.2(6) . . . . ? B1 C28 C29 C30 172.3(4) . . . . ? C28 C29 C30 C31 1.1(7) . . . . ? C28 C29 C30 C34 -178.3(4) . . . . ? C29 C30 C31 C32A -0.6(7) . . . . ? C34 C30 C31 C32A 178.8(4) . . . . ? C29 C28 C33 C32A 0.8(6) . . . . ? B1 C28 C33 C32A -172.8(4) . . . . ? C31 C30 C34 F34B 1.5(8) . . . . ? C29 C30 C34 F34B -179.2(5) . . . . ? C31 C30 C34 F34A 124.2(5) . . . . ? C29 C30 C34 F34A -56.4(7) . . . . ? C31 C30 C34 F34C -118.1(6) . . . . ? C29 C30 C34 F34C 61.3(7) . . . . ? C28 C33 C32A C31 -0.4(6) . . . . ? C28 C33 C32A C35A -179.6(3) . . . . ? C30 C31 C32A C33 0.2(6) . . . . ? C30 C31 C32A C35A 179.5(4) . . . . ? C33 C32A C35A F35B 97.3(3) . . . . ? C31 C32A C35A F35B -81.9(4) . . . . ? C33 C32A C35A F35C -139.8(3) . . . . ? C31 C32A C35A F35C 40.9(4) . . . . ? C33 C32A C35A F35A -21.5(4) . . . . ? C31 C32A C35A F35A 159.3(3) . . . . ? C28 B1 C36 C37 97.3(4) . . . . ? C12 B1 C36 C37 -143.9(4) . . . . ? C20 B1 C36 C37 -23.1(5) . . . . ? C28 B1 C36 C41 -78.3(4) . . . . ? C12 B1 C36 C41 40.5(5) . . . . ? C20 B1 C36 C41 161.3(3) . . . . ? C41 C36 C37 C38 1.5(6) . . . . ? B1 C36 C37 C38 -174.3(4) . . . . ? C36 C37 C38 C39 0.0(6) . . . . ? C36 C37 C38 C42 -179.8(4) . . . . ? C37 C38 C39 C40A -1.0(6) . . . . ? C42 C38 C39 C40A 178.8(4) . . . . ? C37 C36 C41 C40A -2.1(6) . . . . ? B1 C36 C41 C40A 173.8(4) . . . . ? C39 C38 C42 F42C 50.5(6) . . . . ? C37 C38 C42 F42C -129.8(5) . . . . ? C39 C38 C42 F42A -68.3(6) . . . . ? C37 C38 C42 F42A 111.4(5) . . . . ? C39 C38 C42 F42B 171.9(4) . . . . ? C37 C38 C42 F42B -8.3(6) . . . . ? C38 C39 C40A C41 0.4(6) . . . . ? C38 C39 C40A C43A 179.2(4) . . . . ? C36 C41 C40A C39 1.2(6) . . . . ? C36 C41 C40A C43A -177.6(3) . . . . ? C39 C40A C43A F43A -168.3(3) . . . . ? C41 C40A C43A F43A 10.5(4) . . . . ? C39 C40A C43A F43B 68.0(4) . . . . ? C41 C40A C43A F43B -113.1(3) . . . . ? C39 C40A C43A F43C -50.6(4) . . . . ? C41 C40A C43A F43C 128.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.018 _refine_diff_density_min -1.898 _refine_diff_density_rms 0.150 # Attachment 'rh00502.cif' data_rh00502 _database_code_depnum_ccdc_archive 'CCDC 697503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C11 H12 N4 O2 Rh, 0.5(C H2 Cl2)' _chemical_formula_sum 'C43.50 H25 B Cl F24 N4 O2 Rh' _chemical_formula_weight 1240.84 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' B B 0.0013 0.0007 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 13.1291(3) _cell_length_b 25.6224(6) _cell_length_c 15.3207(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.0720(10) _cell_angle_gamma 90.00 _cell_volume 4741.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 124517 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 30.034 _exptl_crystal_description piece _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 75612 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13785 _reflns_number_gt 10960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; The structure bears 0.5 dichloromethane in the asymmetric unit, which is situated in the close proximity of a centre of inversion and is twofold disordered with s.o.f. 0.23 and 0.27. 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^)+(0.0498P)^2^+4.2011P] 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 13785 _refine_ls_number_parameters 702 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.054 _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 Rh1 Rh 0.466728(13) 0.246922(6) 0.105592(11) 0.02314(5) Uani 1 1 d . . . O1 O 0.26109(17) 0.23768(10) 0.14480(15) 0.0547(6) Uani 1 1 d . . . O2 O 0.56338(16) 0.32854(9) 0.25497(14) 0.0502(5) Uani 1 1 d . . . N1 N 0.60899(14) 0.24933(7) 0.07860(13) 0.0225(3) Uani 1 1 d . . . N2 N 0.75372(14) 0.21982(7) 0.05620(12) 0.0227(3) Uani 1 1 d . . . N3 N 0.42569(14) 0.12178(7) -0.08034(12) 0.0228(3) Uani 1 1 d . . . N4 N 0.41573(14) 0.18938(7) 0.00367(13) 0.0227(3) Uani 1 1 d . . . C1 C 0.67944(18) 0.29067(9) 0.08551(16) 0.0274(4) Uani 1 1 d . . . H1 H 0.6672 0.3259 0.0980 0.033 Uiso 1 1 calc R . . C2 C 0.76886(18) 0.27259(9) 0.07157(15) 0.0270(4) Uani 1 1 d . . . H2 H 0.8302 0.2925 0.0723 0.032 Uiso 1 1 calc R . . C3 C 0.65564(15) 0.20711(8) 0.06013(14) 0.0204(4) Uani 1 1 d . . . C4 C 0.83435(17) 0.18420(9) 0.04380(17) 0.0291(4) Uani 1 1 d . . . H4A H 0.8538 0.1569 0.0924 0.044 Uiso 1 1 calc R . . H4B H 0.9011 0.2037 0.0500 0.044 Uiso 1 1 calc R . . H4C H 0.8021 0.1682 -0.0193 0.044 Uiso 1 1 calc R . . C5 C 0.60630(16) 0.15345(8) 0.04487(15) 0.0228(4) Uani 1 1 d . . . H5A H 0.6219 0.1368 0.1071 0.027 Uiso 1 1 calc R . . H5B H 0.6412 0.1320 0.0104 0.027 Uiso 1 1 calc R . . C6 C 0.46741(18) 0.07613(8) -0.11344(17) 0.0289(4) Uani 1 1 d . . . H6A H 0.5358 0.0854 -0.1212 0.043 Uiso 1 1 calc R . . H6B H 0.4118 0.0645 -0.1745 0.043 Uiso 1 1 calc R . . H6C H 0.4825 0.0479 -0.0668 0.043 Uiso 1 1 calc R . . C7 C 0.48341(16) 0.15516(8) -0.01088(14) 0.0210(4) Uani 1 1 d . . . C8 C 0.31547(17) 0.13550(8) -0.11183(16) 0.0270(4) Uani 1 1 d . . . H8 H 0.2552 0.1189 -0.1606 0.032 Uiso 1 1 calc R . . C9 C 0.30972(16) 0.17716(8) -0.05991(16) 0.0259(4) Uani 1 1 d . . . H9 H 0.2440 0.1951 -0.0660 0.031 Uiso 1 1 calc R . . C10 C 0.3386(2) 0.24185(11) 0.13014(18) 0.0352(5) Uani 1 1 d . . . C11 C 0.52354(19) 0.29774(11) 0.19881(17) 0.0354(5) Uani 1 1 d . . . B1 B 0.13402(17) 0.10146(9) 0.28111(15) 0.0183(4) Uani 1 1 d . . . C12 C 0.06787(15) 0.15300(8) 0.29478(13) 0.0190(4) Uani 1 1 d . . . C13 C -0.02785(15) 0.14682(8) 0.31398(14) 0.0214(4) Uani 1 1 d . . . H13 H -0.0487 0.1127 0.3249 0.026 Uiso 1 1 calc R . . C14 C -0.09299(16) 0.18891(9) 0.31755(14) 0.0236(4) Uani 1 1 d . . . C15 C -0.06572(17) 0.23965(9) 0.30338(15) 0.0250(4) Uani 1 1 d . . . H15 H -0.1093 0.2684 0.3074 0.030 Uiso 1 1 calc R . . C16 C 0.02767(17) 0.24678(8) 0.28313(14) 0.0226(4) Uani 1 1 d . . . C17 C 0.09198(15) 0.20442(8) 0.27796(14) 0.0206(4) Uani 1 1 d . . . H17 H 0.1543 0.2107 0.2625 0.025 Uiso 1 1 calc R . . C18 C -0.19459(17) 0.17845(9) 0.33721(16) 0.0293(4) Uani 1 1 d . . . F18A F -0.17177(14) 0.16799(10) 0.42662(11) 0.0652(6) Uani 1 1 d . . . F18B F -0.25209(12) 0.13791(7) 0.28793(13) 0.0525(5) Uani 1 1 d . . . F18C F -0.26508(14) 0.21841(8) 0.31369(17) 0.0641(6) Uani 1 1 d . . . C19 C 0.06106(18) 0.30104(9) 0.26856(15) 0.0267(4) Uani 1 1 d . . . F19A F -0.02648(13) 0.33370(6) 0.23097(15) 0.0581(5) Uani 1 1 d . . . F19B F 0.1134(2) 0.30356(6) 0.21217(15) 0.0652(6) Uani 1 1 d . . . F19C F 0.12358(14) 0.32413(6) 0.35018(11) 0.0476(4) Uani 1 1 d . . . C20 C 0.25986(15) 0.11422(7) 0.28911(13) 0.0182(3) Uani 1 1 d . . . C21 C 0.32690(15) 0.15220(8) 0.35087(14) 0.0198(4) Uani 1 1 d . . . H21 H 0.2971 0.1726 0.3870 0.024 Uiso 1 1 calc R . . C22 C 0.43573(15) 0.16121(8) 0.36117(14) 0.0202(4) Uani 1 1 d . . . C23 C 0.48479(15) 0.13105(8) 0.31343(14) 0.0211(4) Uani 1 1 d . . . H23 H 0.5590 0.1371 0.3206 0.025 Uiso 1 1 calc R . . C24 C 0.42167(15) 0.09162(8) 0.25464(14) 0.0199(4) Uani 1 1 d . . . C25 C 0.31136(15) 0.08419(8) 0.24138(14) 0.0201(4) Uani 1 1 d . . . H25 H 0.2696 0.0579 0.1986 0.024 Uiso 1 1 calc R . . C26 C 0.49696(17) 0.20556(9) 0.42296(17) 0.0278(4) Uani 1 1 d . . . F26A F 0.50068(15) 0.20199(8) 0.51099(12) 0.0574(5) Uani 1 1 d . . . F26B F 0.44709(16) 0.25098(6) 0.39049(17) 0.0671(7) Uani 1 1 d . . . F26C F 0.60110(11) 0.21022(6) 0.43131(12) 0.0441(4) Uani 1 1 d . . . C27 C 0.47272(17) 0.05715(9) 0.20384(16) 0.0260(4) Uani 1 1 d . . . F27A F 0.42862(12) 0.00947(5) 0.18755(11) 0.0346(3) Uani 1 1 d . . . F27B F 0.45875(14) 0.07588(6) 0.11765(11) 0.0435(4) Uani 1 1 d . . . F27C F 0.58155(11) 0.05127(7) 0.25084(13) 0.0521(5) Uani 1 1 d . . . C28 C 0.05299(15) 0.08049(7) 0.17498(13) 0.0174(3) Uani 1 1 d . . . C29 C 0.05951(15) 0.10035(8) 0.09211(14) 0.0190(4) Uani 1 1 d . . . H29 H 0.1183 0.1234 0.0974 0.023 Uiso 1 1 calc R . . C30 C -0.01753(15) 0.08729(7) 0.00225(13) 0.0189(3) Uani 1 1 d . . . C31 C -0.10502(15) 0.05370(8) -0.00849(14) 0.0206(4) Uani 1 1 d . . . H31 H -0.1574 0.0446 -0.0697 0.025 Uiso 1 1 calc R . . C32 C -0.11347(15) 0.03397(7) 0.07266(14) 0.0193(4) Uani 1 1 d . . . C33 C -0.03576(15) 0.04686(7) 0.16249(13) 0.0184(3) Uani 1 1 d . . . H33 H -0.0432 0.0324 0.2168 0.022 Uiso 1 1 calc R . . C34 C -0.01080(17) 0.11066(8) -0.08496(14) 0.0234(4) Uani 1 1 d . . . F34A F -0.00642(14) 0.07451(6) -0.14646(10) 0.0392(3) Uani 1 1 d . . . F34B F -0.10017(11) 0.13980(5) -0.13358(9) 0.0315(3) Uani 1 1 d . . . F34C F 0.07642(12) 0.14193(7) -0.06523(10) 0.0439(4) Uani 1 1 d . . . C35 C -0.21020(16) 0.00002(8) 0.06171(15) 0.0230(4) Uani 1 1 d . . . F35A F -0.20215(11) -0.02297(6) 0.14256(9) 0.0328(3) Uani 1 1 d . . . F35B F -0.22588(11) -0.03837(5) -0.00197(10) 0.0342(3) Uani 1 1 d . . . F35C F -0.30549(11) 0.02743(6) 0.03070(13) 0.0439(4) Uani 1 1 d . . . C36 C 0.14973(15) 0.05647(8) 0.36151(13) 0.0206(4) Uani 1 1 d . . . C37 C 0.17631(16) 0.00503(8) 0.34637(14) 0.0233(4) Uani 1 1 d . . . H37 H 0.1784 -0.0036 0.2868 0.028 Uiso 1 1 calc R . . C38 C 0.19962(17) -0.03363(9) 0.41474(15) 0.0266(4) Uani 1 1 d . . . C39 C 0.19392(19) -0.02296(10) 0.50221(16) 0.0315(5) Uani 1 1 d . . . H39 H 0.2083 -0.0494 0.5491 0.038 Uiso 1 1 calc R . . C40 C 0.16691(19) 0.02699(10) 0.51830(15) 0.0303(5) Uani 1 1 d . . . C41 C 0.14660(17) 0.06625(9) 0.45025(14) 0.0256(4) Uani 1 1 d . . . H41 H 0.1302 0.1005 0.4646 0.031 Uiso 1 1 calc R . . C42 C 0.2275(2) -0.08774(9) 0.39500(18) 0.0350(5) Uani 1 1 d . . . F42A F 0.26196(17) -0.08992(6) 0.32375(13) 0.0537(4) Uani 1 1 d . . . F42B F 0.14205(15) -0.12013(7) 0.37181(16) 0.0650(6) Uani 1 1 d . . . F42C F 0.30772(15) -0.10911(7) 0.47068(12) 0.0536(4) Uani 1 1 d . . . C43 C 0.1599(3) 0.03990(12) 0.61102(18) 0.0437(6) Uani 1 1 d . . . F43A F 0.07596(18) 0.07137(10) 0.60207(13) 0.0742(6) Uani 1 1 d . . . F43B F 0.24540(18) 0.06752(12) 0.66799(13) 0.0869(8) Uani 1 1 d . . . F43C F 0.1507(3) -0.00095(9) 0.65846(17) 0.1199(13) Uani 1 1 d . . . Cl1 Cl 0.5129(5) 0.9621(4) 0.3980(5) 0.1142(15) Uani 0.23 1 d PD . 1 C1S C 0.521(4) 0.9765(11) 0.5092(18) 0.1142(15) Uani 0.23 1 d PD A 1 H1S1 H 0.5996 0.9759 0.5543 0.137 Uiso 0.23 1 calc PR A 1 H1S2 H 0.4806 0.9498 0.5296 0.137 Uiso 0.23 1 calc PR A 1 Cl2 Cl 0.4662(7) 1.0366(4) 0.5110(7) 0.1142(15) Uani 0.23 1 d PD . 1 Cl3 Cl 0.5465(4) 0.9230(3) 0.4070(4) 0.1142(15) Uani 0.27 1 d PD B 2 C2S C 0.5235(18) 0.9809(8) 0.4369(15) 0.1142(15) Uani 0.27 1 d PD B 2 H2S1 H 0.5836 1.0043 0.4373 0.137 Uiso 0.27 1 calc PR B 2 H2S2 H 0.4533 0.9940 0.3882 0.137 Uiso 0.27 1 calc PR B 2 Cl4 Cl 0.5154(6) 0.9840(3) 0.5393(5) 0.1142(15) Uani 0.27 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02159(8) 0.02837(9) 0.02143(8) -0.00091(6) 0.01055(6) 0.00712(6) O1 0.0394(10) 0.0856(16) 0.0517(13) 0.0092(11) 0.0315(10) 0.0141(10) O2 0.0370(10) 0.0703(14) 0.0381(10) -0.0283(10) 0.0091(8) 0.0078(9) N1 0.0224(8) 0.0220(8) 0.0239(8) -0.0032(6) 0.0100(7) 0.0020(6) N2 0.0191(7) 0.0262(9) 0.0234(8) -0.0015(7) 0.0091(6) 0.0004(6) N3 0.0213(8) 0.0186(8) 0.0267(8) -0.0004(7) 0.0075(7) 0.0003(6) N4 0.0195(7) 0.0223(8) 0.0279(9) 0.0001(7) 0.0110(7) 0.0014(6) C1 0.0295(10) 0.0233(10) 0.0290(10) -0.0036(8) 0.0112(8) -0.0011(8) C2 0.0250(10) 0.0281(11) 0.0271(10) -0.0017(8) 0.0095(8) -0.0053(8) C3 0.0177(8) 0.0234(9) 0.0199(9) -0.0017(7) 0.0073(7) 0.0013(7) C4 0.0192(9) 0.0367(12) 0.0333(11) -0.0013(9) 0.0123(8) 0.0051(8) C5 0.0194(8) 0.0215(9) 0.0262(10) -0.0007(8) 0.0077(7) 0.0027(7) C6 0.0291(10) 0.0193(10) 0.0339(11) -0.0046(8) 0.0076(9) 0.0017(8) C7 0.0202(9) 0.0192(9) 0.0241(9) 0.0015(7) 0.0092(7) -0.0001(7) C8 0.0192(9) 0.0222(10) 0.0350(11) 0.0033(8) 0.0058(8) -0.0025(7) C9 0.0184(9) 0.0251(10) 0.0342(11) 0.0030(8) 0.0104(8) -0.0008(7) C10 0.0319(11) 0.0481(15) 0.0303(11) 0.0048(10) 0.0172(9) 0.0139(10) C11 0.0274(11) 0.0497(15) 0.0284(11) -0.0058(10) 0.0101(9) 0.0143(10) B1 0.0155(9) 0.0202(10) 0.0196(9) -0.0022(8) 0.0073(7) -0.0021(7) C12 0.0152(8) 0.0251(9) 0.0164(8) -0.0031(7) 0.0057(7) -0.0017(7) C13 0.0186(8) 0.0245(9) 0.0213(9) -0.0039(7) 0.0081(7) -0.0031(7) C14 0.0171(8) 0.0328(11) 0.0220(9) -0.0050(8) 0.0088(7) -0.0017(7) C15 0.0209(9) 0.0298(11) 0.0239(10) -0.0057(8) 0.0085(8) 0.0033(8) C16 0.0233(9) 0.0251(10) 0.0186(8) -0.0032(7) 0.0074(7) -0.0007(7) C17 0.0175(8) 0.0248(10) 0.0201(9) -0.0032(7) 0.0079(7) -0.0010(7) C18 0.0217(9) 0.0361(12) 0.0329(11) -0.0077(9) 0.0137(8) -0.0021(8) F18A 0.0368(8) 0.1337(19) 0.0320(8) -0.0018(10) 0.0209(7) -0.0203(10) F18B 0.0310(7) 0.0638(11) 0.0732(11) -0.0333(9) 0.0319(8) -0.0210(7) F18C 0.0401(9) 0.0553(11) 0.1165(17) 0.0114(11) 0.0518(11) 0.0146(8) C19 0.0304(10) 0.0251(10) 0.0248(10) -0.0035(8) 0.0109(8) 0.0008(8) F19A 0.0376(8) 0.0250(8) 0.0883(14) 0.0034(8) -0.0007(8) 0.0041(6) F19B 0.1310(18) 0.0264(8) 0.0797(13) 0.0073(8) 0.0860(14) 0.0058(9) F19C 0.0558(10) 0.0420(9) 0.0332(8) -0.0021(7) 0.0048(7) -0.0225(7) C20 0.0169(8) 0.0204(9) 0.0169(8) 0.0000(7) 0.0062(7) -0.0010(7) C21 0.0175(8) 0.0217(9) 0.0207(9) -0.0018(7) 0.0080(7) -0.0006(7) C22 0.0157(8) 0.0206(9) 0.0229(9) -0.0024(7) 0.0060(7) -0.0020(7) C23 0.0161(8) 0.0228(9) 0.0254(9) 0.0001(8) 0.0092(7) -0.0004(7) C24 0.0180(8) 0.0215(9) 0.0212(9) -0.0002(7) 0.0088(7) 0.0013(7) C25 0.0174(8) 0.0211(9) 0.0214(9) -0.0012(7) 0.0073(7) -0.0016(7) C26 0.0185(9) 0.0259(10) 0.0389(12) -0.0096(9) 0.0112(8) -0.0038(7) F26A 0.0565(10) 0.0795(13) 0.0443(9) -0.0368(9) 0.0286(8) -0.0370(9) F26B 0.0470(10) 0.0235(8) 0.0993(16) -0.0162(8) -0.0052(10) 0.0022(7) F26C 0.0240(6) 0.0471(9) 0.0657(10) -0.0272(8) 0.0224(7) -0.0174(6) C27 0.0209(9) 0.0273(10) 0.0326(11) -0.0061(8) 0.0137(8) -0.0017(8) F27A 0.0396(7) 0.0240(6) 0.0480(8) -0.0086(6) 0.0256(7) -0.0002(5) F27B 0.0627(10) 0.0423(9) 0.0433(8) -0.0032(7) 0.0400(8) -0.0021(7) F27C 0.0192(6) 0.0658(11) 0.0663(11) -0.0334(9) 0.0112(7) 0.0066(7) C28 0.0155(8) 0.0182(8) 0.0186(8) -0.0006(7) 0.0070(6) 0.0002(6) C29 0.0163(8) 0.0197(9) 0.0225(9) -0.0008(7) 0.0092(7) -0.0006(6) C30 0.0197(8) 0.0194(9) 0.0187(8) 0.0014(7) 0.0086(7) 0.0022(7) C31 0.0180(8) 0.0226(9) 0.0187(8) -0.0020(7) 0.0046(7) -0.0005(7) C32 0.0159(8) 0.0175(8) 0.0238(9) -0.0018(7) 0.0072(7) -0.0012(6) C33 0.0174(8) 0.0193(9) 0.0190(8) 0.0007(7) 0.0077(7) 0.0003(7) C34 0.0239(9) 0.0257(10) 0.0210(9) 0.0018(8) 0.0091(7) 0.0010(8) F34A 0.0651(10) 0.0335(7) 0.0276(7) 0.0041(6) 0.0272(7) 0.0170(7) F34B 0.0347(7) 0.0327(7) 0.0277(6) 0.0098(5) 0.0128(5) 0.0112(5) F34C 0.0356(7) 0.0656(11) 0.0280(7) 0.0113(7) 0.0097(6) -0.0213(7) C35 0.0186(9) 0.0225(9) 0.0259(10) -0.0005(8) 0.0065(7) -0.0023(7) F35A 0.0327(7) 0.0385(8) 0.0285(7) -0.0006(6) 0.0134(5) -0.0166(6) F35B 0.0354(7) 0.0339(7) 0.0325(7) -0.0117(6) 0.0126(6) -0.0158(6) F35C 0.0172(6) 0.0359(8) 0.0732(11) 0.0051(7) 0.0119(6) 0.0011(5) C36 0.0142(8) 0.0265(10) 0.0190(9) -0.0003(7) 0.0042(7) -0.0036(7) C37 0.0192(9) 0.0282(10) 0.0201(9) 0.0000(8) 0.0052(7) -0.0024(7) C38 0.0225(9) 0.0265(10) 0.0260(10) 0.0028(8) 0.0044(8) -0.0033(8) C39 0.0325(11) 0.0338(12) 0.0238(10) 0.0064(9) 0.0063(9) -0.0058(9) C40 0.0334(11) 0.0385(12) 0.0182(9) 0.0006(9) 0.0092(8) -0.0060(9) C41 0.0256(10) 0.0302(11) 0.0205(9) -0.0016(8) 0.0085(8) -0.0044(8) C42 0.0363(12) 0.0275(11) 0.0332(12) 0.0052(9) 0.0051(10) 0.0000(9) F42A 0.0845(13) 0.0339(8) 0.0515(10) 0.0048(7) 0.0363(9) 0.0174(8) F42B 0.0519(10) 0.0309(9) 0.1005(16) -0.0095(9) 0.0174(10) -0.0128(7) F42C 0.0591(10) 0.0409(9) 0.0428(9) 0.0073(7) 0.0003(8) 0.0178(8) C43 0.0550(16) 0.0533(17) 0.0250(12) 0.0016(11) 0.0180(11) -0.0004(13) F43A 0.0772(14) 0.1165(19) 0.0425(10) 0.0008(11) 0.0381(10) 0.0196(13) F43B 0.0712(14) 0.150(2) 0.0354(10) -0.0394(12) 0.0164(9) -0.0224(14) F43C 0.275(4) 0.0611(14) 0.0682(15) 0.0106(12) 0.116(2) -0.0034(19) Cl1 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) C1S 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) Cl2 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) Cl3 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) C2S 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) Cl4 0.0613(14) 0.152(4) 0.106(2) 0.053(2) 0.0072(16) -0.0325(18) _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 C11 1.859(3) . ? Rh1 C10 1.867(2) . ? Rh1 N4 2.0594(18) . ? Rh1 N1 2.0661(17) . ? O1 C10 1.129(3) . ? O2 C11 1.133(3) . ? N1 C3 1.327(2) . ? N1 C1 1.383(3) . ? N2 C3 1.352(2) . ? N2 C2 1.373(3) . ? N2 C4 1.465(3) . ? N3 C7 1.344(3) . ? N3 C8 1.380(3) . ? N3 C6 1.464(3) . ? N4 C7 1.328(3) . ? N4 C9 1.386(3) . ? C1 C2 1.355(3) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C5 1.499(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.502(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.351(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? B1 C12 1.639(3) . ? B1 C36 1.640(3) . ? B1 C20 1.641(3) . ? B1 C28 1.646(3) . ? C12 C17 1.402(3) . ? C12 C13 1.407(3) . ? C13 C14 1.391(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(3) . ? C14 C18 1.502(3) . ? C15 C16 1.390(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 C19 1.500(3) . ? C17 H17 0.9500 . ? C18 F18A 1.310(3) . ? C18 F18B 1.331(3) . ? C18 F18C 1.332(3) . ? C19 F19B 1.299(3) . ? C19 F19C 1.335(3) . ? C19 F19A 1.354(3) . ? C20 C21 1.402(3) . ? C20 C25 1.404(3) . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C22 C26 1.496(3) . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 C25 1.394(3) . ? C24 C27 1.498(3) . ? C25 H25 0.9500 . ? C26 F26C 1.328(2) . ? C26 F26B 1.332(3) . ? C26 F26A 1.334(3) . ? C27 F27C 1.333(2) . ? C27 F27A 1.333(3) . ? C27 F27B 1.348(3) . ? C28 C33 1.401(3) . ? C28 C29 1.401(3) . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 C31 1.393(3) . ? C30 C34 1.498(3) . ? C31 C32 1.386(3) . ? C31 H31 0.9500 . ? C32 C33 1.394(3) . ? C32 C35 1.494(3) . ? C33 H33 0.9500 . ? C34 F34C 1.332(2) . ? C34 F34A 1.338(2) . ? C34 F34B 1.343(2) . ? C35 F35A 1.338(2) . ? C35 F35B 1.343(2) . ? C35 F35C 1.348(2) . ? C36 C41 1.399(3) . ? C36 C37 1.406(3) . ? C37 C38 1.386(3) . ? C37 H37 0.9500 . ? C38 C39 1.398(3) . ? C38 C42 1.495(3) . ? C39 C40 1.376(4) . ? C39 H39 0.9500 . ? C40 C41 1.397(3) . ? C40 C43 1.496(3) . ? C41 H41 0.9500 . ? C42 F42B 1.327(3) . ? C42 F42A 1.337(3) . ? C42 F42C 1.340(3) . ? C43 F43C 1.307(4) . ? C43 F43B 1.325(4) . ? C43 F43A 1.328(4) . ? Cl1 C1S 1.704(16) . ? C1S Cl2 1.704(16) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? Cl3 C2S 1.615(13) . ? C2S Cl4 1.615(13) . ? C2S H2S1 0.9900 . ? C2S H2S2 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 C11 Rh1 C10 90.91(11) . . ? C11 Rh1 N4 175.74(8) . . ? C10 Rh1 N4 92.98(10) . . ? C11 Rh1 N1 90.62(9) . . ? C10 Rh1 N1 177.72(9) . . ? N4 Rh1 N1 85.43(7) . . ? C3 N1 C1 106.86(17) . . ? C3 N1 Rh1 123.18(14) . . ? C1 N1 Rh1 129.61(14) . . ? C3 N2 C2 107.81(17) . . ? C3 N2 C4 127.19(18) . . ? C2 N2 C4 124.90(17) . . ? C7 N3 C8 107.67(17) . . ? C7 N3 C6 127.69(17) . . ? C8 N3 C6 124.47(18) . . ? C7 N4 C9 106.66(17) . . ? C7 N4 Rh1 124.05(14) . . ? C9 N4 Rh1 129.28(14) . . ? C2 C1 N1 108.72(19) . . ? C2 C1 H1 125.6 . . ? N1 C1 H1 125.6 . . ? C1 C2 N2 106.72(18) . . ? C1 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? N1 C3 N2 109.89(18) . . ? N1 C3 C5 125.01(17) . . ? N2 C3 C5 125.10(17) . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 C7 111.37(16) . . ? C3 C5 H5A 109.4 . . ? C7 C5 H5A 109.4 . . ? C3 C5 H5B 109.4 . . ? C7 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N3 110.26(17) . . ? N4 C7 C5 124.36(18) . . ? N3 C7 C5 125.35(18) . . ? C9 C8 N3 106.76(18) . . ? C9 C8 H8 126.6 . . ? N3 C8 H8 126.6 . . ? C8 C9 N4 108.65(18) . . ? C8 C9 H9 125.7 . . ? N4 C9 H9 125.7 . . ? O1 C10 Rh1 178.6(3) . . ? O2 C11 Rh1 176.3(2) . . ? C12 B1 C36 112.80(16) . . ? C12 B1 C20 113.48(15) . . ? C36 B1 C20 104.92(15) . . ? C12 B1 C28 102.69(15) . . ? C36 B1 C28 110.79(15) . . ? C20 B1 C28 112.39(15) . . ? C17 C12 C13 115.37(18) . . ? C17 C12 B1 124.38(16) . . ? C13 C12 B1 119.84(17) . . ? C14 C13 C12 122.30(19) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C13 121.32(18) . . ? C15 C14 C18 120.15(19) . . ? C13 C14 C18 118.5(2) . . ? C14 C15 C16 117.54(19) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? C15 C16 C17 121.10(19) . . ? C15 C16 C19 119.34(19) . . ? C17 C16 C19 119.56(19) . . ? C16 C17 C12 122.33(18) . . ? C16 C17 H17 118.8 . . ? C12 C17 H17 118.8 . . ? F18A C18 F18B 106.3(2) . . ? F18A C18 F18C 106.9(2) . . ? F18B C18 F18C 105.48(19) . . ? F18A C18 C14 112.88(18) . . ? F18B C18 C14 112.11(18) . . ? F18C C18 C14 112.7(2) . . ? F19B C19 F19C 108.0(2) . . ? F19B C19 F19A 105.6(2) . . ? F19C C19 F19A 103.42(18) . . ? F19B C19 C16 113.99(18) . . ? F19C C19 C16 112.29(18) . . ? F19A C19 C16 112.77(18) . . ? C21 C20 C25 115.40(17) . . ? C21 C20 B1 122.44(16) . . ? C25 C20 B1 121.88(16) . . ? C22 C21 C20 122.42(18) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C23 C22 C21 121.08(18) . . ? C23 C22 C26 120.83(17) . . ? C21 C22 C26 118.06(17) . . ? C22 C23 C24 117.72(17) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? C23 C24 C25 120.98(18) . . ? C23 C24 C27 119.37(17) . . ? C25 C24 C27 119.64(18) . . ? C24 C25 C20 122.28(18) . . ? C24 C25 H25 118.9 . . ? C20 C25 H25 118.9 . . ? F26C C26 F26B 107.1(2) . . ? F26C C26 F26A 106.29(18) . . ? F26B C26 F26A 104.8(2) . . ? F26C C26 C22 114.02(17) . . ? F26B C26 C22 111.33(18) . . ? F26A C26 C22 112.67(19) . . ? F27C C27 F27A 107.00(18) . . ? F27C C27 F27B 105.96(18) . . ? F27A C27 F27B 105.09(17) . . ? F27C C27 C24 112.91(18) . . ? F27A C27 C24 112.81(17) . . ? F27B C27 C24 112.47(18) . . ? C33 C28 C29 116.27(17) . . ? C33 C28 B1 121.12(16) . . ? C29 C28 B1 122.09(16) . . ? C30 C29 C28 122.00(17) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 120.75(17) . . ? C29 C30 C34 120.80(17) . . ? C31 C30 C34 118.41(17) . . ? C32 C31 C30 118.14(17) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 120.94(17) . . ? C31 C32 C35 118.37(17) . . ? C33 C32 C35 120.66(18) . . ? C32 C33 C28 121.90(17) . . ? C32 C33 H33 119.1 . . ? C28 C33 H33 119.1 . . ? F34C C34 F34A 107.81(18) . . ? F34C C34 F34B 106.14(17) . . ? F34A C34 F34B 105.28(16) . . ? F34C C34 C30 112.58(17) . . ? F34A C34 C30 112.65(17) . . ? F34B C34 C30 111.88(16) . . ? F35A C35 F35B 106.51(16) . . ? F35A C35 F35C 106.33(17) . . ? F35B C35 F35C 105.57(16) . . ? F35A C35 C32 113.41(16) . . ? F35B C35 C32 112.93(17) . . ? F35C C35 C32 111.52(17) . . ? C41 C36 C37 115.60(19) . . ? C41 C36 B1 124.14(19) . . ? C37 C36 B1 120.09(17) . . ? C38 C37 C36 122.76(19) . . ? C38 C37 H37 118.6 . . ? C36 C37 H37 118.6 . . ? C37 C38 C39 120.4(2) . . ? C37 C38 C42 120.6(2) . . ? C39 C38 C42 119.0(2) . . ? C40 C39 C38 117.9(2) . . ? C40 C39 H39 121.0 . . ? C38 C39 H39 121.0 . . ? C39 C40 C41 121.5(2) . . ? C39 C40 C43 119.5(2) . . ? C41 C40 C43 119.0(2) . . ? C40 C41 C36 121.8(2) . . ? C40 C41 H41 119.1 . . ? C36 C41 H41 119.1 . . ? F42B C42 F42A 106.0(2) . . ? F42B C42 F42C 105.7(2) . . ? F42A C42 F42C 106.7(2) . . ? F42B C42 C38 112.7(2) . . ? F42A C42 C38 113.1(2) . . ? F42C C42 C38 112.1(2) . . ? F43C C43 F43B 107.5(3) . . ? F43C C43 F43A 106.9(3) . . ? F43B C43 F43A 101.4(3) . . ? F43C C43 C40 113.9(3) . . ? F43B C43 C40 113.1(2) . . ? F43A C43 C40 113.2(2) . . ? Cl1 C1S Cl2 110.4(15) . . ? Cl1 C1S H1S1 109.6 . . ? Cl2 C1S H1S1 109.6 . . ? Cl1 C1S H1S2 109.6 . . ? Cl2 C1S H1S2 109.6 . . ? H1S1 C1S H1S2 108.1 . . ? Cl4 C2S Cl3 114.3(16) . . ? Cl4 C2S H2S1 108.7 . . ? Cl3 C2S H2S1 108.7 . . ? Cl4 C2S H2S2 108.7 . . ? Cl3 C2S H2S2 108.7 . . ? H2S1 C2S H2S2 107.6 . . ? 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 C11 Rh1 N1 C3 140.85(18) . . . . ? N4 Rh1 N1 C3 -37.53(16) . . . . ? C11 Rh1 N1 C1 -31.4(2) . . . . ? N4 Rh1 N1 C1 150.18(19) . . . . ? C10 Rh1 N4 C7 -144.53(18) . . . . ? N1 Rh1 N4 C7 33.82(17) . . . . ? C10 Rh1 N4 C9 33.70(19) . . . . ? N1 Rh1 N4 C9 -147.95(18) . . . . ? C3 N1 C1 C2 -0.4(2) . . . . ? Rh1 N1 C1 C2 172.88(15) . . . . ? N1 C1 C2 N2 -0.1(2) . . . . ? C3 N2 C2 C1 0.6(2) . . . . ? C4 N2 C2 C1 -176.0(2) . . . . ? C1 N1 C3 N2 0.8(2) . . . . ? Rh1 N1 C3 N2 -173.03(13) . . . . ? C1 N1 C3 C5 -178.62(19) . . . . ? Rh1 N1 C3 C5 7.6(3) . . . . ? C2 N2 C3 N1 -0.9(2) . . . . ? C4 N2 C3 N1 175.63(19) . . . . ? C2 N2 C3 C5 178.52(19) . . . . ? C4 N2 C3 C5 -5.0(3) . . . . ? N1 C3 C5 C7 38.8(3) . . . . ? N2 C3 C5 C7 -140.5(2) . . . . ? C9 N4 C7 N3 -0.1(2) . . . . ? Rh1 N4 C7 N3 178.45(13) . . . . ? C9 N4 C7 C5 -178.41(19) . . . . ? Rh1 N4 C7 C5 0.2(3) . . . . ? C8 N3 C7 N4 0.1(2) . . . . ? C6 N3 C7 N4 -175.25(19) . . . . ? C8 N3 C7 C5 178.38(19) . . . . ? C6 N3 C7 C5 3.0(3) . . . . ? C3 C5 C7 N4 -43.1(3) . . . . ? C3 C5 C7 N3 138.8(2) . . . . ? C7 N3 C8 C9 0.0(2) . . . . ? C6 N3 C8 C9 175.5(2) . . . . ? N3 C8 C9 N4 0.0(2) . . . . ? C7 N4 C9 C8 0.1(2) . . . . ? Rh1 N4 C9 C8 -178.38(15) . . . . ? C36 B1 C12 C17 143.12(18) . . . . ? C20 B1 C12 C17 24.0(3) . . . . ? C28 B1 C12 C17 -97.6(2) . . . . ? C36 B1 C12 C13 -44.6(2) . . . . ? C20 B1 C12 C13 -163.78(17) . . . . ? C28 B1 C12 C13 74.7(2) . . . . ? C17 C12 C13 C14 -1.0(3) . . . . ? B1 C12 C13 C14 -173.93(18) . . . . ? C12 C13 C14 C15 -0.8(3) . . . . ? C12 C13 C14 C18 179.16(18) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C18 C14 C15 C16 -178.43(19) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C14 C15 C16 C19 -179.21(19) . . . . ? C15 C16 C17 C12 -1.5(3) . . . . ? C19 C16 C17 C12 177.30(18) . . . . ? C13 C12 C17 C16 2.1(3) . . . . ? B1 C12 C17 C16 174.68(18) . . . . ? C15 C14 C18 F18A -104.0(3) . . . . ? C13 C14 C18 F18A 76.0(3) . . . . ? C15 C14 C18 F18B 136.1(2) . . . . ? C13 C14 C18 F18B -43.9(3) . . . . ? C15 C14 C18 F18C 17.2(3) . . . . ? C13 C14 C18 F18C -162.8(2) . . . . ? C15 C16 C19 F19B -151.3(2) . . . . ? C17 C16 C19 F19B 29.9(3) . . . . ? C15 C16 C19 F19C 85.4(2) . . . . ? C17 C16 C19 F19C -93.4(2) . . . . ? C15 C16 C19 F19A -30.9(3) . . . . ? C17 C16 C19 F19A 150.3(2) . . . . ? C12 B1 C20 C21 34.8(2) . . . . ? C36 B1 C20 C21 -88.7(2) . . . . ? C28 B1 C20 C21 150.80(18) . . . . ? C12 B1 C20 C25 -151.64(18) . . . . ? C36 B1 C20 C25 84.8(2) . . . . ? C28 B1 C20 C25 -35.7(2) . . . . ? C25 C20 C21 C22 2.7(3) . . . . ? B1 C20 C21 C22 176.66(18) . . . . ? C20 C21 C22 C23 -3.0(3) . . . . ? C20 C21 C22 C26 175.09(19) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C26 C22 C23 C24 -177.79(19) . . . . ? C22 C23 C24 C25 2.6(3) . . . . ? C22 C23 C24 C27 -178.31(19) . . . . ? C23 C24 C25 C20 -2.8(3) . . . . ? C27 C24 C25 C20 178.10(19) . . . . ? C21 C20 C25 C24 0.1(3) . . . . ? B1 C20 C25 C24 -173.88(18) . . . . ? C23 C22 C26 F26C -4.1(3) . . . . ? C21 C22 C26 F26C 177.84(19) . . . . ? C23 C22 C26 F26B 117.3(2) . . . . ? C21 C22 C26 F26B -60.8(3) . . . . ? C23 C22 C26 F26A -125.3(2) . . . . ? C21 C22 C26 F26A 56.6(3) . . . . ? C23 C24 C27 F27C 29.4(3) . . . . ? C25 C24 C27 F27C -151.4(2) . . . . ? C23 C24 C27 F27A 150.90(19) . . . . ? C25 C24 C27 F27A -30.0(3) . . . . ? C23 C24 C27 F27B -90.4(2) . . . . ? C25 C24 C27 F27B 88.7(2) . . . . ? C12 B1 C28 C33 -86.3(2) . . . . ? C36 B1 C28 C33 34.4(2) . . . . ? C20 B1 C28 C33 151.44(17) . . . . ? C12 B1 C28 C29 85.1(2) . . . . ? C36 B1 C28 C29 -154.17(17) . . . . ? C20 B1 C28 C29 -37.2(2) . . . . ? C33 C28 C29 C30 -0.3(3) . . . . ? B1 C28 C29 C30 -172.06(17) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? C28 C29 C30 C34 177.76(18) . . . . ? C29 C30 C31 C32 0.4(3) . . . . ? C34 C30 C31 C32 -177.28(18) . . . . ? C30 C31 C32 C33 -0.8(3) . . . . ? C30 C31 C32 C35 177.05(17) . . . . ? C31 C32 C33 C28 0.7(3) . . . . ? C35 C32 C33 C28 -177.09(18) . . . . ? C29 C28 C33 C32 -0.2(3) . . . . ? B1 C28 C33 C32 171.71(17) . . . . ? C29 C30 C34 F34C 2.4(3) . . . . ? C31 C30 C34 F34C -179.91(18) . . . . ? C29 C30 C34 F34A 124.6(2) . . . . ? C31 C30 C34 F34A -57.7(2) . . . . ? C29 C30 C34 F34B -117.0(2) . . . . ? C31 C30 C34 F34B 60.6(2) . . . . ? C31 C32 C35 F35A 170.80(18) . . . . ? C33 C32 C35 F35A -11.3(3) . . . . ? C31 C32 C35 F35B 49.5(2) . . . . ? C33 C32 C35 F35B -132.61(19) . . . . ? C31 C32 C35 F35C -69.2(2) . . . . ? C33 C32 C35 F35C 108.7(2) . . . . ? C12 B1 C36 C41 -22.5(2) . . . . ? C20 B1 C36 C41 101.5(2) . . . . ? C28 B1 C36 C41 -136.98(18) . . . . ? C12 B1 C36 C37 162.52(16) . . . . ? C20 B1 C36 C37 -73.5(2) . . . . ? C28 B1 C36 C37 48.0(2) . . . . ? C41 C36 C37 C38 -0.9(3) . . . . ? B1 C36 C37 C38 174.50(18) . . . . ? C36 C37 C38 C39 2.1(3) . . . . ? C36 C37 C38 C42 -179.95(19) . . . . ? C37 C38 C39 C40 -1.3(3) . . . . ? C42 C38 C39 C40 -179.3(2) . . . . ? C38 C39 C40 C41 -0.6(3) . . . . ? C38 C39 C40 C43 179.9(2) . . . . ? C39 C40 C41 C36 1.8(3) . . . . ? C43 C40 C41 C36 -178.7(2) . . . . ? C37 C36 C41 C40 -1.0(3) . . . . ? B1 C36 C41 C40 -176.19(19) . . . . ? C37 C38 C42 F42B -99.8(3) . . . . ? C39 C38 C42 F42B 78.2(3) . . . . ? C37 C38 C42 F42A 20.5(3) . . . . ? C39 C38 C42 F42A -161.6(2) . . . . ? C37 C38 C42 F42C 141.1(2) . . . . ? C39 C38 C42 F42C -40.9(3) . . . . ? C39 C40 C43 F43C -17.8(4) . . . . ? C41 C40 C43 F43C 162.7(3) . . . . ? C39 C40 C43 F43B 105.3(3) . . . . ? C41 C40 C43 F43B -74.3(3) . . . . ? C39 C40 C43 F43A -140.1(3) . . . . ? C41 C40 C43 F43A 40.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.861 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.096 # Attachment 'rh00701.cif' data_rh00701 _database_code_depnum_ccdc_archive 'CCDC 697504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C17 H24 Ir N4' _chemical_formula_sum 'C49 H36 B F24 Ir N4' _chemical_formula_weight 1339.85 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' B B 0.0013 0.0007 '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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0661(2) _cell_length_b 18.5517(2) _cell_length_c 19.3024(2) _cell_angle_alpha 65.8340(10) _cell_angle_beta 64.3060(10) _cell_angle_gamma 75.4040(10) _cell_volume 5003.69(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 130100 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 30.034 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 2.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.486 _exptl_absorpt_correction_T_max 0.560 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 135754 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 30.00 _reflns_number_total 29145 _reflns_number_gt 24977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+37.8737P] 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 29145 _refine_ls_number_parameters 1445 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.277 _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 Ir1 Ir 0.413993(12) 0.417213(11) 0.109236(11) 0.01679(5) Uani 1 1 d . . . N1 N 0.3243(3) 0.5050(2) 0.0683(3) 0.0195(8) Uani 1 1 d . . . N2 N 0.2012(3) 0.5827(3) 0.0827(3) 0.0232(9) Uani 1 1 d . . . N3 N 0.3682(3) 0.5692(3) 0.2385(3) 0.0206(8) Uani 1 1 d . . . N4 N 0.4127(3) 0.4845(2) 0.1732(2) 0.0190(8) Uani 1 1 d . . . C1 C 0.3760(3) 0.3322(3) 0.0850(3) 0.0206(9) Uani 1 1 d . . . H1 H 0.3208 0.3624 0.0945 0.025 Uiso 1 1 calc R . . C2 C 0.4491(4) 0.3671(3) 0.0167(3) 0.0228(10) Uani 1 1 d . . . H2 H 0.4399 0.4190 -0.0191 0.027 Uiso 1 1 calc R . . C3 C 0.5407(4) 0.3270(3) -0.0026(3) 0.0287(12) Uani 1 1 d . . . H3A H 0.5815 0.3660 -0.0479 0.034 Uiso 1 1 calc R . . H3B H 0.5445 0.2838 -0.0218 0.034 Uiso 1 1 calc R . . C4 C 0.5696(4) 0.2925(4) 0.0702(4) 0.0298(12) Uani 1 1 d . . . H4A H 0.5570 0.2362 0.0994 0.036 Uiso 1 1 calc R . . H4B H 0.6334 0.2944 0.0501 0.036 Uiso 1 1 calc R . . C5 C 0.5234(3) 0.3377(3) 0.1294(3) 0.0227(10) Uani 1 1 d . . . H5 H 0.5477 0.3831 0.1203 0.027 Uiso 1 1 calc R . . C6 C 0.4456(3) 0.3147(3) 0.1974(3) 0.0209(9) Uani 1 1 d . . . H6 H 0.4217 0.3446 0.2330 0.025 Uiso 1 1 calc R . . C7 C 0.3972(4) 0.2463(3) 0.2182(3) 0.0260(11) Uani 1 1 d . . . H7A H 0.3399 0.2482 0.2630 0.031 Uiso 1 1 calc R . . H7B H 0.4308 0.1957 0.2379 0.031 Uiso 1 1 calc R . . C8 C 0.3826(4) 0.2483(3) 0.1435(3) 0.0256(11) Uani 1 1 d . . . H8A H 0.4318 0.2168 0.1141 0.031 Uiso 1 1 calc R . . H8B H 0.3283 0.2237 0.1629 0.031 Uiso 1 1 calc R . . C9 C 0.2972(4) 0.5153(3) 0.0065(3) 0.0276(11) Uani 1 1 d . . . H9 H 0.3271 0.4928 -0.0355 0.033 Uiso 1 1 calc R . . C10 C 0.2212(4) 0.5627(4) 0.0153(4) 0.0313(12) Uani 1 1 d . . . H10 H 0.1882 0.5789 -0.0184 0.038 Uiso 1 1 calc R . . C11 C 0.2646(3) 0.5475(3) 0.1129(3) 0.0188(9) Uani 1 1 d . . . C12 C 0.1191(4) 0.6256(4) 0.1205(4) 0.0314(12) Uani 1 1 d . . . H12A H 0.0859 0.5899 0.1746 0.047 Uiso 1 1 calc R . . H12B H 0.0847 0.6444 0.0858 0.047 Uiso 1 1 calc R . . H12C H 0.1320 0.6709 0.1263 0.047 Uiso 1 1 calc R . . C13 C 0.2635(3) 0.5565(3) 0.1869(3) 0.0242(10) Uani 1 1 d . . . H13A H 0.2424 0.6120 0.1844 0.029 Uiso 1 1 calc R . . H13B H 0.2208 0.5220 0.2361 0.029 Uiso 1 1 calc R . . C14 C 0.3178(4) 0.6322(3) 0.2719(3) 0.0256(11) Uani 1 1 d . . . H14A H 0.3059 0.6788 0.2283 0.038 Uiso 1 1 calc R . . H14B H 0.3513 0.6465 0.2939 0.038 Uiso 1 1 calc R . . H14C H 0.2625 0.6133 0.3157 0.038 Uiso 1 1 calc R . . C15 C 0.3482(3) 0.5372(3) 0.1973(3) 0.0179(9) Uani 1 1 d . . . C16 C 0.4494(4) 0.5349(3) 0.2407(3) 0.0233(10) Uani 1 1 d . . . H16 H 0.4803 0.5454 0.2657 0.028 Uiso 1 1 calc R . . C17 C 0.4760(4) 0.4830(3) 0.1999(3) 0.0232(10) Uani 1 1 d . . . H17 H 0.5298 0.4508 0.1912 0.028 Uiso 1 1 calc R . . Ir2 Ir 0.504580(14) 0.130479(13) 0.47610(1) 0.01953(5) Uani 0.8878(5) 1 d P A 1 Ir2A Ir 0.48542(11) 0.08576(11) 0.51052(11) 0.01953(5) Uani 0.1122(5) 1 d P A 2 N5 N 0.4835(3) 0.0939(3) 0.6004(3) 0.0302(10) Uani 1 1 d . . . N6 N 0.4237(3) 0.0868(3) 0.7292(3) 0.0354(12) Uani 1 1 d . . . N7 N 0.2294(3) 0.1586(3) 0.5857(3) 0.0266(10) Uani 1 1 d . A . N8 N 0.3682(3) 0.1332(3) 0.5160(3) 0.0235(9) Uani 1 1 d . . . C18 C 0.6242(4) 0.1769(4) 0.4424(4) 0.0380(15) Uani 1 1 d . . . H18 H 0.6032 0.1809 0.4952 0.046 Uiso 1 1 calc R A 1 C19 C 0.6420(4) 0.0987(4) 0.4372(4) 0.0394(15) Uani 1 1 d . A . H19 H 0.6294 0.0540 0.4864 0.047 Uiso 1 1 calc R B 1 C20 C 0.6803(6) 0.0855(6) 0.3557(5) 0.058(2) Uani 1 1 d . . . H20A H 0.7270 0.1214 0.3172 0.070 Uiso 1 1 calc R A . H20B H 0.7077 0.0304 0.3639 0.070 Uiso 1 1 calc R . . C21 C 0.6189(6) 0.0982(8) 0.3182(7) 0.082(4) Uani 1 1 d . A . H21A H 0.6121 0.0464 0.3190 0.099 Uiso 1 1 calc R . . H21B H 0.6442 0.1322 0.2601 0.099 Uiso 1 1 calc R . . C22 C 0.5302(5) 0.1354(5) 0.3562(4) 0.0423(16) Uani 1 1 d . . . H22 H 0.4819 0.1049 0.3805 0.051 Uiso 1 1 calc R A 1 C23 C 0.5143(5) 0.2113(4) 0.3581(4) 0.0440(17) Uani 1 1 d . A . H23 H 0.4557 0.2301 0.3837 0.053 Uiso 1 1 calc R C 1 C24 C 0.5849(7) 0.2664(6) 0.3216(6) 0.080(4) Uani 1 1 d . . . H24A H 0.6250 0.2626 0.2676 0.096 Uiso 1 1 calc R A . H24B H 0.5572 0.3215 0.3122 0.096 Uiso 1 1 calc R . . C25 C 0.6365(5) 0.2513(5) 0.3710(5) 0.055(2) Uani 1 1 d . A . H25A H 0.6225 0.2962 0.3910 0.066 Uiso 1 1 calc R . . H25B H 0.6990 0.2511 0.3349 0.066 Uiso 1 1 calc R . . C26 C 0.5423(5) 0.0515(4) 0.6377(4) 0.0425(16) Uani 1 1 d . A . H26 H 0.5992 0.0298 0.6118 0.051 Uiso 1 1 calc R . . C27 C 0.5058(4) 0.0461(5) 0.7167(4) 0.0439(17) Uani 1 1 d . A . H27 H 0.5316 0.0193 0.7565 0.053 Uiso 1 1 calc R . . C28 C 0.4128(4) 0.1149(3) 0.6561(3) 0.0283(12) Uani 1 1 d . A . C29 C 0.3627(5) 0.0985(5) 0.8053(4) 0.0447(17) Uani 1 1 d . A . H29A H 0.3216 0.1450 0.7936 0.067 Uiso 1 1 calc R . . H29B H 0.3949 0.1068 0.8324 0.067 Uiso 1 1 calc R . . H29C H 0.3305 0.0514 0.8412 0.067 Uiso 1 1 calc R . . C30 C 0.3317(4) 0.1617(4) 0.6451(4) 0.0301(12) Uani 1 1 d . . . H30A H 0.3378 0.2188 0.6281 0.036 Uiso 1 1 calc R A . H30B H 0.2821 0.1471 0.6984 0.036 Uiso 1 1 calc R . . C31 C 0.1502(4) 0.1813(5) 0.6465(4) 0.0383(15) Uani 1 1 d . . . H31A H 0.1029 0.1991 0.6258 0.058 Uiso 1 1 calc R . . H31B H 0.1608 0.2246 0.6573 0.058 Uiso 1 1 calc R . . H31C H 0.1339 0.1356 0.6973 0.058 Uiso 1 1 calc R . . C32 C 0.3110(4) 0.1493(3) 0.5831(3) 0.0236(10) Uani 1 1 d . A . C33 C 0.2335(4) 0.1472(4) 0.5180(4) 0.0360(14) Uani 1 1 d . . . H33 H 0.1857 0.1501 0.5038 0.043 Uiso 1 1 calc R A . C34 C 0.3181(4) 0.1311(4) 0.4761(4) 0.0312(12) Uani 1 1 d . A . H34 H 0.3405 0.1200 0.4267 0.037 Uiso 1 1 calc R . . B1 B 0.1842(3) 0.0996(3) 0.1038(3) 0.0160(9) Uani 1 1 d . . . C35 C 0.1805(3) 0.0391(3) 0.0627(3) 0.0167(9) Uani 1 1 d . . . C36 C 0.1546(3) 0.0655(3) -0.0044(3) 0.0186(9) Uani 1 1 d . . . H36 H 0.1373 0.1203 -0.0261 0.022 Uiso 1 1 calc R . . C37 C 0.1536(4) 0.0142(3) -0.0402(3) 0.0234(10) Uani 1 1 d . . . C38 C 0.1796(4) -0.0663(3) -0.0111(3) 0.0245(10) Uani 1 1 d . . . H38 H 0.1784 -0.1015 -0.0350 0.029 Uiso 1 1 calc R . . C39 C 0.2075(3) -0.0938(3) 0.0538(3) 0.0211(10) Uani 1 1 d . . . C40 C 0.2083(3) -0.0416(3) 0.0889(3) 0.0185(9) Uani 1 1 d . . . H40 H 0.2287 -0.0619 0.1326 0.022 Uiso 1 1 calc R . . C41 C 0.1235(5) 0.0436(4) -0.1101(4) 0.0338(13) Uani 1 1 d . . . F41A F 0.0563(3) 0.0086(3) -0.0947(3) 0.0487(10) Uani 1 1 d . . . F41B F 0.1872(3) 0.0285(3) -0.1775(2) 0.0561(12) Uani 1 1 d . . . F41C F 0.1043(5) 0.1220(3) -0.1357(4) 0.088(2) Uani 1 1 d . . . C42 C 0.2338(4) -0.1799(3) 0.0886(3) 0.0265(11) Uani 1 1 d . . . F42A F 0.2435(3) -0.2214(2) 0.0429(3) 0.0446(10) Uani 1 1 d . . . F42B F 0.1754(3) -0.2151(2) 0.1631(2) 0.0494(11) Uani 1 1 d . . . F42C F 0.3091(3) -0.1930(2) 0.1001(3) 0.0450(10) Uani 1 1 d . . . C43 C 0.2828(3) 0.1295(3) 0.0519(3) 0.0160(8) Uani 1 1 d . . . C44 C 0.3029(3) 0.1948(3) -0.0218(3) 0.0190(9) Uani 1 1 d . . . H44 H 0.2573 0.2249 -0.0402 0.023 Uiso 1 1 calc R . . C45 C 0.3876(3) 0.2161(3) -0.0681(3) 0.0211(10) Uani 1 1 d . . . C46 C 0.4571(3) 0.1741(3) -0.0459(3) 0.0194(9) Uani 1 1 d . . . H46 H 0.5149 0.1891 -0.0783 0.023 Uiso 1 1 calc R . . C47 C 0.4388(3) 0.1085(3) 0.0264(3) 0.0169(9) Uani 1 1 d . . . C48 C 0.3541(3) 0.0871(3) 0.0737(3) 0.0168(9) Uani 1 1 d . . . H48 H 0.3441 0.0422 0.1226 0.020 Uiso 1 1 calc R . . C49 C 0.4036(4) 0.2879(3) -0.1451(4) 0.0311(12) Uani 1 1 d . . . F49A F 0.3649(3) 0.3547(2) -0.1288(2) 0.0428(9) Uani 1 1 d . . . F49B F 0.4882(2) 0.2984(2) -0.1887(2) 0.0399(9) Uani 1 1 d . . . F49C F 0.3710(3) 0.2839(2) -0.1954(2) 0.0458(10) Uani 1 1 d . . . C50 C 0.5129(3) 0.0620(3) 0.0518(3) 0.0211(10) Uani 1 1 d . . . F50A F 0.4966(2) -0.01412(18) 0.0999(2) 0.0264(7) Uani 1 1 d . . . F50B F 0.5310(2) 0.0919(2) 0.0956(2) 0.0354(8) Uani 1 1 d . . . F50C F 0.5874(2) 0.0578(2) -0.0113(2) 0.0333(8) Uani 1 1 d . . . C51 C 0.1075(3) 0.1733(3) 0.0995(3) 0.0168(9) Uani 1 1 d . . . C52 C 0.1169(3) 0.2482(3) 0.0951(3) 0.0209(9) Uani 1 1 d . . . H52 H 0.1714 0.2582 0.0901 0.025 Uiso 1 1 calc R . . C53 C 0.0490(4) 0.3083(3) 0.0980(3) 0.0250(10) Uani 1 1 d . . . C54 C -0.0317(4) 0.2962(3) 0.1063(3) 0.0249(11) Uani 1 1 d . . . H54 H -0.0780 0.3374 0.1079 0.030 Uiso 1 1 calc R . . C55 C -0.0432(3) 0.2225(3) 0.1122(3) 0.0195(9) Uani 1 1 d . . . C56 C 0.0245(3) 0.1624(3) 0.1091(3) 0.0189(9) Uani 1 1 d . . . H56 H 0.0143 0.1123 0.1137 0.023 Uiso 1 1 calc R . . C57 C 0.0628(4) 0.3893(4) 0.0888(5) 0.0364(14) Uani 1 1 d . . . F57A F 0.1316(4) 0.3885(3) 0.1042(4) 0.081(2) Uani 1 1 d . . . F57B F -0.0041(3) 0.4211(3) 0.1377(4) 0.0745(17) Uani 1 1 d . . . F57C F 0.0757(4) 0.4405(3) 0.0130(3) 0.0705(15) Uani 1 1 d . . . C58 C -0.1288(4) 0.2078(3) 0.1193(4) 0.0266(11) Uani 1 1 d . . . F58A F -0.1960(2) 0.2559(3) 0.1496(3) 0.0566(13) Uani 1 1 d . . . F58B F -0.1509(2) 0.1338(2) 0.1664(3) 0.0420(9) Uani 1 1 d . . . F58C F -0.1289(3) 0.2170(3) 0.0462(3) 0.0538(12) Uani 1 1 d . . . C59 C 0.1655(3) 0.0549(3) 0.2018(3) 0.0164(8) Uani 1 1 d . F . C60 C 0.1995(3) 0.0787(3) 0.2421(3) 0.0174(9) Uani 1 1 d . . . H60 H 0.2370 0.1203 0.2112 0.021 Uiso 1 1 calc R . . C61 C 0.1804(3) 0.0436(3) 0.3264(3) 0.0185(9) Uani 1 1 d . F . C62 C 0.1252(3) -0.0164(3) 0.3741(3) 0.0229(10) Uani 1 1 d . . . H62 H 0.1120 -0.0403 0.4313 0.027 Uiso 1 1 calc R D 1 C64 C 0.1087(3) -0.0053(3) 0.2516(3) 0.0200(9) Uani 1 1 d . . . H64 H 0.0823 -0.0226 0.2275 0.024 Uiso 1 1 calc R E 1 C65 C 0.2212(4) 0.0712(3) 0.3649(3) 0.0230(10) Uani 1 1 d . . . F65A F 0.2200(3) 0.0195(3) 0.4377(2) 0.0470(11) Uani 1 1 d . F . F65B F 0.1871(3) 0.1412(3) 0.3724(3) 0.0542(12) Uani 1 1 d . F . F65C F 0.3070(2) 0.0810(2) 0.3189(2) 0.0388(9) Uani 1 1 d . F . C63 C 0.0900(4) -0.0402(3) 0.3353(3) 0.0238(10) Uani 0.50 1 d PD F 1 C66 C 0.0348(4) -0.1086(3) 0.3831(5) 0.0364(17) Uani 0.50 1 d PGD F 1 F66A F 0.0594(4) -0.1732(3) 0.3664(5) 0.067(2) Uani 0.50 1 d PRU F 1 F66B F -0.0438(4) -0.0835(3) 0.3790(5) 0.088(2) Uani 0.50 1 d PR F 1 F66C F 0.0343(4) -0.1437(3) 0.4589(5) 0.062(2) Uani 0.50 1 d PRU F 1 C63A C 0.0900(4) -0.0402(3) 0.3353(3) 0.0238(10) Uani 0.50 1 d PD F 2 C66A C 0.0248(4) -0.1005(3) 0.3857(5) 0.0364(17) Uani 0.50 1 d PGD F 2 F66D F 0.0472(4) -0.1525(3) 0.3487(5) 0.067(2) Uani 0.50 1 d PR F 2 F66E F -0.0539(4) -0.0755(3) 0.3817(5) 0.088(2) Uani 0.50 1 d PR F 2 F66F F -0.0132(4) -0.1153(3) 0.4664(5) 0.062(2) Uani 0.50 1 d PR F 2 B2 B 0.1972(4) 0.6024(3) 0.5521(3) 0.0179(10) Uani 1 1 d . . . C67 C 0.2077(3) 0.5351(3) 0.6363(3) 0.0169(9) Uani 1 1 d . . . C68 C 0.1780(3) 0.4590(3) 0.6734(3) 0.0204(9) Uani 1 1 d . . . H68 H 0.1577 0.4413 0.6449 0.025 Uiso 1 1 calc R . . C69 C 0.1774(3) 0.4091(3) 0.7503(3) 0.0212(10) Uani 1 1 d . . . C70 C 0.2060(4) 0.4320(3) 0.7950(3) 0.0227(10) Uani 1 1 d . . . H70 H 0.2053 0.3978 0.8477 0.027 Uiso 1 1 calc R . . C71 C 0.2357(3) 0.5067(3) 0.7596(3) 0.0219(10) Uani 1 1 d . . . C72 C 0.2377(3) 0.5566(3) 0.6815(3) 0.0202(9) Uani 1 1 d . . . H72 H 0.2603 0.6067 0.6584 0.024 Uiso 1 1 calc R . . C73 C 0.1489(4) 0.3277(3) 0.7848(4) 0.0288(12) Uani 1 1 d . . . F73A F 0.0792(3) 0.3252(2) 0.7705(3) 0.0515(11) Uani 1 1 d . . . F73B F 0.2104(3) 0.2779(2) 0.7519(3) 0.0543(12) Uani 1 1 d . . . F73C F 0.1270(4) 0.2941(3) 0.8649(3) 0.0755(18) Uani 1 1 d . . . C74 C 0.2670(4) 0.5353(3) 0.8042(4) 0.0269(11) Uani 1 1 d . . . F74A F 0.2348(3) 0.6091(2) 0.8024(3) 0.0418(10) Uani 1 1 d . . . F74B F 0.3544(2) 0.5366(3) 0.7715(3) 0.0425(9) Uani 1 1 d . . . F74C F 0.2475(3) 0.4902(2) 0.8829(2) 0.0447(10) Uani 1 1 d . . . C75 C 0.2850(3) 0.6484(3) 0.4877(3) 0.0193(9) Uani 1 1 d . . . C76 C 0.2791(4) 0.7182(3) 0.4233(3) 0.0225(10) Uani 1 1 d . . . H76 H 0.2233 0.7397 0.4208 0.027 Uiso 1 1 calc R . . C77 C 0.3515(4) 0.7572(3) 0.3630(3) 0.0260(11) Uani 1 1 d . . . C78 C 0.4339(4) 0.7285(3) 0.3644(4) 0.0310(12) Uani 1 1 d . . . H78 H 0.4836 0.7555 0.3236 0.037 Uiso 1 1 calc R . . C79 C 0.4419(4) 0.6592(3) 0.4269(4) 0.0298(12) Uani 1 1 d . . . C80 C 0.3686(3) 0.6194(3) 0.4880(3) 0.0244(10) Uani 1 1 d . . . H80 H 0.3762 0.5719 0.5302 0.029 Uiso 1 1 calc R . . C81 C 0.3395(4) 0.8313(3) 0.2955(4) 0.0349(14) Uani 1 1 d . . . F81A F 0.3120(3) 0.8952(2) 0.3183(3) 0.0417(9) Uani 1 1 d . . . F81B F 0.4140(3) 0.8488(2) 0.2296(3) 0.0678(16) Uani 1 1 d . . . F81C F 0.2810(4) 0.8266(3) 0.2693(3) 0.0626(14) Uani 1 1 d . . . C82 C 0.5311(4) 0.6230(4) 0.4265(5) 0.0471(18) Uani 1 1 d . . . F82A F 0.5323(3) 0.5798(3) 0.5003(3) 0.0647(14) Uani 1 1 d . . . F82B F 0.5666(3) 0.5736(3) 0.3823(3) 0.0693(15) Uani 1 1 d . . . F82C F 0.5887(3) 0.6777(3) 0.3887(4) 0.086(2) Uani 1 1 d . . . C83 C 0.1162(3) 0.6622(3) 0.5891(3) 0.0178(9) Uani 1 1 d . I . C84 C 0.0302(3) 0.6429(3) 0.6273(3) 0.0221(10) Uani 1 1 d . . . H84 H 0.0170 0.5979 0.6241 0.026 Uiso 1 1 calc R . . C85 C -0.0373(3) 0.6875(3) 0.6702(3) 0.0243(10) Uani 1 1 d . I . C86 C -0.0208(3) 0.7537(3) 0.6763(3) 0.0241(10) Uani 1 1 d . . . H86 H -0.0666 0.7839 0.7058 0.029 Uiso 1 1 calc R G 1 C88 C 0.1309(3) 0.7306(3) 0.5949(3) 0.0189(9) Uani 1 1 d . . . H88 H 0.1882 0.7473 0.5682 0.023 Uiso 1 1 calc R H 1 C89 C -0.1278(4) 0.6642(4) 0.7066(5) 0.0395(15) Uani 1 1 d . . . F89A F -0.1838(2) 0.6987(3) 0.7604(3) 0.0458(10) Uani 1 1 d . I . F89B F -0.1616(3) 0.6809(3) 0.6498(3) 0.0629(14) Uani 1 1 d . I . F89C F -0.1315(3) 0.5848(3) 0.7474(3) 0.0619(14) Uani 1 1 d . I . C87 C 0.0637(3) 0.7745(3) 0.6385(3) 0.0201(9) Uani 0.517(7) 1 d PD I 1 C90 C 0.0910(5) 0.8428(3) 0.6424(5) 0.0269(13) Uani 0.517(7) 1 d PGD I 1 F90A F 0.0301(5) 0.8677(3) 0.7008(5) 0.0467(12) Uani 0.517(7) 1 d PR I 1 F90B F 0.1513(5) 0.8129(3) 0.6755(5) 0.068(2) Uani 0.517(7) 1 d PRU I 1 F90C F 0.1181(5) 0.8984(3) 0.5800(5) 0.051(2) Uani 0.517(7) 1 d PRU I 1 C87A C 0.0637(3) 0.7745(3) 0.6385(3) 0.0201(9) Uani 0.483(7) 1 d PD I 2 C90A C 0.0790(5) 0.8463(3) 0.6462(5) 0.0269(13) Uani 0.483(7) 1 d PGD I 2 F90D F 0.0180(5) 0.8712(3) 0.7046(5) 0.0467(12) Uani 0.483(7) 1 d PR I 2 F90E F 0.1550(5) 0.8428(3) 0.6545(5) 0.068(2) Uani 0.483(7) 1 d PR I 2 F90F F 0.0756(5) 0.9127(3) 0.5766(5) 0.051(2) Uani 0.483(7) 1 d PR I 2 C91 C 0.1774(3) 0.5624(3) 0.5008(3) 0.0184(9) Uani 1 1 d . L . C92 C 0.1150(3) 0.5936(3) 0.4644(3) 0.0203(9) Uani 1 1 d . . . H92 H 0.0797 0.6409 0.4707 0.024 Uiso 1 1 calc R . . C93 C 0.1034(3) 0.5575(3) 0.4194(3) 0.0224(10) Uani 1 1 d . L . C94 C 0.1529(4) 0.4882(3) 0.4087(3) 0.0267(11) Uani 1 1 d . . . H94 H 0.1426 0.4621 0.3805 0.032 Uiso 1 1 calc R J 1 C96 C 0.2300(3) 0.4947(3) 0.4855(3) 0.0216(10) Uani 1 1 d . . . H96 H 0.2753 0.4731 0.5064 0.026 Uiso 1 1 calc R K 1 C97 C 0.0396(4) 0.5968(3) 0.3776(3) 0.0255(11) Uani 1 1 d . . . F97A F -0.0319(3) 0.6318(3) 0.4206(2) 0.0475(10) Uani 1 1 d . L . F97B F 0.0752(2) 0.6538(2) 0.3054(2) 0.0385(9) Uani 1 1 d . L . F97C F 0.0141(3) 0.5464(3) 0.3588(3) 0.0523(12) Uani 1 1 d . L . C95 C 0.2184(4) 0.4581(3) 0.4411(3) 0.0245(11) Uani 0.531(8) 1 d PD L 1 C98 C 0.2771(4) 0.3874(3) 0.4216(4) 0.0269(17) Uani 0.531(8) 1 d PGDU L 1 F98A F 0.3025(4) 0.3862(3) 0.3472(4) 0.0393(13) Uani 0.531(8) 1 d PRU L 1 F98B F 0.2390(4) 0.3219(3) 0.4795(4) 0.097(2) Uani 0.531(8) 1 d PRU L 1 F98C F 0.3618(4) 0.3908(3) 0.4254(4) 0.0602(19) Uani 0.531(8) 1 d PRU L 1 C95A C 0.2184(4) 0.4581(3) 0.4411(3) 0.0245(11) Uani 0.469(8) 1 d PD L 2 C98A C 0.2672(4) 0.3777(3) 0.4431(4) 0.0269(17) Uani 0.469(8) 1 d PGD L 2 F98D F 0.2926(4) 0.3764(3) 0.3687(4) 0.0393(13) Uani 0.469(8) 1 d PR L 2 F98E F 0.2167(4) 0.3185(3) 0.4767(4) 0.097(2) Uani 0.469(8) 1 d PR L 2 F98F F 0.3255(4) 0.3526(3) 0.4624(4) 0.0602(19) Uani 0.469(8) 1 d PR L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02084(9) 0.01568(9) 0.01518(8) -0.00549(7) -0.00682(7) -0.00332(7) N1 0.025(2) 0.0170(19) 0.0177(19) -0.0046(15) -0.0106(17) -0.0023(16) N2 0.023(2) 0.024(2) 0.024(2) -0.0068(18) -0.0132(18) 0.0006(17) N3 0.025(2) 0.022(2) 0.0175(19) -0.0082(16) -0.0075(17) -0.0055(17) N4 0.026(2) 0.0180(19) 0.0160(18) -0.0053(15) -0.0102(16) -0.0034(16) C1 0.025(2) 0.019(2) 0.022(2) -0.0106(19) -0.009(2) -0.0019(19) C2 0.033(3) 0.021(2) 0.017(2) -0.0105(19) -0.006(2) -0.006(2) C3 0.029(3) 0.029(3) 0.022(3) -0.015(2) 0.002(2) -0.005(2) C4 0.024(3) 0.029(3) 0.037(3) -0.018(2) -0.007(2) 0.000(2) C5 0.020(2) 0.021(2) 0.029(3) -0.010(2) -0.010(2) -0.0001(19) C6 0.025(2) 0.016(2) 0.020(2) -0.0041(18) -0.011(2) 0.0006(18) C7 0.030(3) 0.019(2) 0.023(2) -0.002(2) -0.008(2) -0.006(2) C8 0.028(3) 0.021(2) 0.027(3) -0.009(2) -0.007(2) -0.006(2) C9 0.037(3) 0.029(3) 0.024(3) -0.011(2) -0.017(2) -0.002(2) C10 0.043(3) 0.030(3) 0.032(3) -0.012(2) -0.027(3) 0.005(2) C11 0.021(2) 0.018(2) 0.018(2) -0.0030(18) -0.0095(18) -0.0052(18) C12 0.031(3) 0.029(3) 0.033(3) -0.009(2) -0.017(2) 0.003(2) C13 0.024(3) 0.030(3) 0.021(2) -0.012(2) -0.008(2) -0.002(2) C14 0.032(3) 0.022(2) 0.027(3) -0.013(2) -0.010(2) -0.006(2) C15 0.023(2) 0.016(2) 0.015(2) -0.0042(17) -0.0076(18) -0.0042(18) C16 0.027(3) 0.024(2) 0.027(3) -0.009(2) -0.015(2) -0.005(2) C17 0.026(3) 0.022(2) 0.028(3) -0.009(2) -0.015(2) -0.0028(19) Ir2 0.02101(11) 0.01920(11) 0.01699(10) -0.00284(8) -0.00796(8) -0.00384(8) Ir2A 0.02101(11) 0.01920(11) 0.01699(10) -0.00284(8) -0.00796(8) -0.00384(8) N5 0.032(3) 0.033(3) 0.025(2) -0.003(2) -0.017(2) -0.001(2) N6 0.033(3) 0.051(3) 0.019(2) -0.001(2) -0.014(2) -0.011(2) N7 0.030(2) 0.030(2) 0.023(2) -0.0070(19) -0.0104(19) -0.0107(19) N8 0.028(2) 0.022(2) 0.025(2) -0.0068(18) -0.0150(19) -0.0040(17) C18 0.026(3) 0.050(4) 0.029(3) 0.000(3) -0.011(2) -0.009(3) C19 0.029(3) 0.048(4) 0.026(3) -0.006(3) -0.008(2) 0.007(3) C20 0.056(5) 0.065(5) 0.030(4) -0.011(4) -0.011(3) 0.013(4) C21 0.039(5) 0.156(11) 0.078(7) -0.085(8) -0.012(4) 0.009(6) C22 0.038(4) 0.067(5) 0.033(3) -0.024(3) -0.010(3) -0.017(3) C23 0.051(4) 0.048(4) 0.028(3) 0.014(3) -0.023(3) -0.025(3) C24 0.099(8) 0.068(6) 0.074(6) 0.034(5) -0.061(6) -0.055(6) C25 0.051(4) 0.046(4) 0.058(5) 0.017(4) -0.030(4) -0.029(4) C26 0.034(3) 0.051(4) 0.033(3) 0.000(3) -0.022(3) 0.003(3) C27 0.032(3) 0.062(5) 0.028(3) -0.001(3) -0.018(3) -0.001(3) C28 0.037(3) 0.029(3) 0.025(3) -0.004(2) -0.021(2) -0.004(2) C29 0.042(4) 0.068(5) 0.028(3) -0.013(3) -0.021(3) -0.002(3) C30 0.038(3) 0.028(3) 0.032(3) -0.011(2) -0.022(3) 0.002(2) C31 0.025(3) 0.064(5) 0.032(3) -0.021(3) -0.008(2) -0.009(3) C32 0.031(3) 0.019(2) 0.023(2) -0.0016(19) -0.016(2) -0.006(2) C33 0.037(3) 0.055(4) 0.028(3) -0.014(3) -0.014(3) -0.022(3) C34 0.034(3) 0.040(3) 0.029(3) -0.013(3) -0.014(2) -0.011(3) B1 0.016(2) 0.018(2) 0.016(2) -0.0053(19) -0.0069(19) -0.0022(18) C35 0.015(2) 0.019(2) 0.016(2) -0.0060(17) -0.0047(17) -0.0024(17) C36 0.020(2) 0.017(2) 0.018(2) -0.0042(18) -0.0063(18) -0.0055(17) C37 0.032(3) 0.023(2) 0.020(2) -0.0053(19) -0.012(2) -0.008(2) C38 0.031(3) 0.026(3) 0.021(2) -0.011(2) -0.009(2) -0.006(2) C39 0.018(2) 0.020(2) 0.025(2) -0.010(2) -0.0045(19) -0.0028(18) C40 0.018(2) 0.020(2) 0.017(2) -0.0061(18) -0.0060(18) -0.0020(18) C41 0.049(4) 0.032(3) 0.031(3) -0.009(2) -0.023(3) -0.010(3) F41A 0.048(2) 0.069(3) 0.041(2) -0.014(2) -0.0266(19) -0.016(2) F41B 0.072(3) 0.082(3) 0.0206(18) -0.013(2) -0.0157(19) -0.027(3) F41C 0.201(7) 0.027(2) 0.091(4) -0.013(2) -0.121(5) 0.012(3) C42 0.031(3) 0.020(2) 0.027(3) -0.011(2) -0.007(2) -0.003(2) F42A 0.070(3) 0.0263(18) 0.051(2) -0.0234(18) -0.032(2) 0.0095(18) F42B 0.057(3) 0.0215(18) 0.037(2) -0.0002(15) 0.0040(19) -0.0070(17) F42C 0.047(2) 0.0242(18) 0.067(3) -0.0071(18) -0.035(2) 0.0027(16) C43 0.020(2) 0.015(2) 0.014(2) -0.0053(16) -0.0064(17) -0.0010(17) C44 0.022(2) 0.015(2) 0.018(2) -0.0017(17) -0.0102(19) -0.0019(18) C45 0.025(2) 0.016(2) 0.020(2) -0.0023(18) -0.0086(19) -0.0047(18) C46 0.020(2) 0.017(2) 0.020(2) -0.0059(18) -0.0052(18) -0.0052(18) C47 0.018(2) 0.016(2) 0.018(2) -0.0068(17) -0.0063(18) -0.0023(17) C48 0.020(2) 0.016(2) 0.014(2) -0.0042(17) -0.0060(17) -0.0023(17) C49 0.027(3) 0.024(3) 0.029(3) 0.004(2) -0.007(2) -0.008(2) F49A 0.044(2) 0.0182(16) 0.046(2) 0.0041(15) -0.0133(18) -0.0020(15) F49B 0.0272(18) 0.0314(19) 0.036(2) 0.0085(15) -0.0043(15) -0.0110(15) F49C 0.056(3) 0.047(2) 0.0246(18) 0.0099(16) -0.0200(18) -0.0180(19) C50 0.019(2) 0.021(2) 0.025(2) -0.010(2) -0.0090(19) 0.0002(18) F50A 0.0291(17) 0.0199(15) 0.0286(16) -0.0022(12) -0.0160(14) -0.0008(12) F50B 0.043(2) 0.0322(18) 0.055(2) -0.0244(17) -0.0359(19) 0.0082(15) F50C 0.0179(15) 0.039(2) 0.0290(17) -0.0082(15) -0.0033(13) 0.0033(14) C51 0.020(2) 0.018(2) 0.015(2) -0.0060(17) -0.0076(17) -0.0013(17) C52 0.024(2) 0.017(2) 0.025(2) -0.0069(19) -0.012(2) -0.0018(18) C53 0.028(3) 0.020(2) 0.030(3) -0.009(2) -0.014(2) -0.001(2) C54 0.026(3) 0.024(3) 0.028(3) -0.012(2) -0.013(2) 0.003(2) C55 0.018(2) 0.023(2) 0.018(2) -0.0079(19) -0.0063(18) -0.0014(18) C56 0.022(2) 0.017(2) 0.019(2) -0.0070(18) -0.0079(19) -0.0027(18) C57 0.037(3) 0.025(3) 0.055(4) -0.016(3) -0.023(3) 0.000(2) F57A 0.084(4) 0.032(2) 0.181(6) -0.045(3) -0.099(4) 0.013(2) F57B 0.066(3) 0.044(3) 0.117(5) -0.059(3) -0.005(3) -0.009(2) F57C 0.113(5) 0.025(2) 0.069(3) 0.003(2) -0.037(3) -0.027(2) C58 0.024(3) 0.025(3) 0.034(3) -0.013(2) -0.012(2) -0.001(2) F58A 0.0227(19) 0.051(3) 0.113(4) -0.053(3) -0.023(2) 0.0099(17) F58B 0.0278(18) 0.0309(19) 0.058(2) -0.0031(17) -0.0144(18) -0.0111(15) F58C 0.054(3) 0.078(3) 0.046(2) -0.015(2) -0.029(2) -0.023(2) C59 0.017(2) 0.015(2) 0.016(2) -0.0055(17) -0.0059(17) -0.0003(16) C60 0.017(2) 0.017(2) 0.020(2) -0.0063(18) -0.0071(18) -0.0020(17) C61 0.019(2) 0.021(2) 0.016(2) -0.0064(18) -0.0063(18) -0.0047(18) C62 0.022(2) 0.027(3) 0.018(2) -0.005(2) -0.0066(19) -0.006(2) C64 0.021(2) 0.021(2) 0.020(2) -0.0071(19) -0.0065(19) -0.0063(18) C65 0.028(3) 0.024(2) 0.023(2) -0.008(2) -0.014(2) -0.002(2) F65A 0.070(3) 0.054(2) 0.0263(18) 0.0084(17) -0.0312(19) -0.035(2) F65B 0.066(3) 0.050(2) 0.090(3) -0.051(3) -0.057(3) 0.024(2) F65C 0.0319(19) 0.057(2) 0.037(2) -0.0152(18) -0.0147(16) -0.0182(17) C63 0.024(3) 0.025(3) 0.021(2) -0.004(2) -0.006(2) -0.011(2) C66 0.041(4) 0.044(4) 0.021(3) 0.000(3) -0.006(3) -0.028(3) F66A 0.064(3) 0.022(3) 0.085(4) -0.009(3) -0.002(3) -0.022(3) F66B 0.035(3) 0.066(4) 0.137(6) -0.027(4) -0.003(3) -0.031(3) F66C 0.065(4) 0.077(4) 0.043(3) 0.004(3) -0.022(3) -0.045(3) C63A 0.024(3) 0.025(3) 0.021(2) -0.004(2) -0.006(2) -0.011(2) C66A 0.041(4) 0.044(4) 0.021(3) 0.000(3) -0.006(3) -0.028(3) F66D 0.064(3) 0.022(3) 0.085(4) -0.009(3) -0.002(3) -0.022(3) F66E 0.035(3) 0.066(4) 0.137(6) -0.027(4) -0.003(3) -0.031(3) F66F 0.065(4) 0.077(4) 0.043(3) 0.004(3) -0.022(3) -0.045(3) B2 0.019(2) 0.018(2) 0.018(2) -0.005(2) -0.009(2) -0.0015(19) C67 0.016(2) 0.017(2) 0.017(2) -0.0059(17) -0.0056(17) -0.0015(17) C68 0.023(2) 0.021(2) 0.021(2) -0.0074(19) -0.0105(19) -0.0026(19) C69 0.026(3) 0.018(2) 0.021(2) -0.0063(19) -0.010(2) -0.0013(19) C70 0.029(3) 0.022(2) 0.016(2) -0.0040(19) -0.010(2) -0.001(2) C71 0.022(2) 0.024(2) 0.025(2) -0.011(2) -0.013(2) 0.0011(19) C72 0.019(2) 0.022(2) 0.023(2) -0.0094(19) -0.0094(19) -0.0027(18) C73 0.040(3) 0.023(3) 0.026(3) -0.004(2) -0.017(2) -0.007(2) F73A 0.044(2) 0.036(2) 0.076(3) -0.003(2) -0.033(2) -0.0156(18) F73B 0.046(2) 0.027(2) 0.084(3) -0.023(2) -0.015(2) -0.0040(17) F73C 0.159(6) 0.044(3) 0.028(2) 0.0124(18) -0.036(3) -0.058(3) C74 0.030(3) 0.028(3) 0.031(3) -0.015(2) -0.017(2) 0.001(2) F74A 0.061(3) 0.0300(19) 0.061(3) -0.0298(19) -0.042(2) 0.0142(17) F74B 0.033(2) 0.055(2) 0.063(3) -0.033(2) -0.0267(19) -0.0012(17) F74C 0.077(3) 0.039(2) 0.0315(19) -0.0080(16) -0.031(2) -0.015(2) C75 0.020(2) 0.018(2) 0.018(2) -0.0069(18) -0.0053(18) -0.0019(18) C76 0.026(3) 0.019(2) 0.022(2) -0.0107(19) -0.007(2) 0.0011(19) C77 0.033(3) 0.016(2) 0.021(2) -0.0079(19) -0.002(2) -0.002(2) C78 0.026(3) 0.023(3) 0.034(3) -0.009(2) 0.000(2) -0.009(2) C79 0.021(3) 0.024(3) 0.038(3) -0.009(2) -0.006(2) -0.003(2) C80 0.021(2) 0.020(2) 0.028(3) -0.008(2) -0.007(2) 0.0003(19) C81 0.043(4) 0.020(3) 0.027(3) -0.002(2) -0.004(3) -0.005(2) F81A 0.044(2) 0.0204(17) 0.053(2) -0.0133(16) -0.0159(19) 0.0055(15) F81B 0.067(3) 0.031(2) 0.037(2) 0.0075(18) 0.018(2) 0.001(2) F81C 0.108(4) 0.045(2) 0.044(2) 0.0154(19) -0.050(3) -0.033(3) C82 0.026(3) 0.037(4) 0.061(5) 0.000(3) -0.012(3) -0.013(3) F82A 0.031(2) 0.084(4) 0.071(3) -0.011(3) -0.029(2) -0.003(2) F82B 0.039(3) 0.059(3) 0.078(4) -0.022(3) -0.007(2) 0.016(2) F82C 0.031(2) 0.052(3) 0.149(6) -0.006(3) -0.029(3) -0.021(2) C83 0.018(2) 0.018(2) 0.017(2) -0.0059(17) -0.0070(18) -0.0002(17) C84 0.022(2) 0.022(2) 0.023(2) -0.007(2) -0.009(2) -0.0038(19) C85 0.018(2) 0.028(3) 0.025(3) -0.011(2) -0.005(2) -0.003(2) C86 0.019(2) 0.030(3) 0.026(3) -0.016(2) -0.007(2) 0.003(2) C88 0.019(2) 0.020(2) 0.018(2) -0.0064(18) -0.0077(18) -0.0018(18) C89 0.022(3) 0.048(4) 0.050(4) -0.028(3) -0.003(3) -0.006(3) F89A 0.0231(18) 0.057(3) 0.052(2) -0.033(2) 0.0054(17) -0.0064(17) F89B 0.026(2) 0.107(4) 0.084(4) -0.062(3) -0.019(2) -0.005(2) F89C 0.035(2) 0.043(2) 0.086(4) -0.030(2) 0.012(2) -0.0197(19) C87 0.021(2) 0.021(2) 0.020(2) -0.0087(19) -0.0082(19) 0.0003(18) C90 0.019(3) 0.034(3) 0.031(3) -0.021(3) -0.006(3) 0.001(2) F90A 0.049(3) 0.042(2) 0.047(2) -0.035(2) 0.003(2) -0.005(2) F90B 0.053(3) 0.034(4) 0.155(5) -0.059(4) -0.055(3) 0.009(3) F90C 0.093(5) 0.036(3) 0.033(2) -0.001(2) -0.028(3) -0.032(3) C87A 0.021(2) 0.021(2) 0.020(2) -0.0087(19) -0.0082(19) 0.0003(18) C90A 0.019(3) 0.034(3) 0.031(3) -0.021(3) -0.006(3) 0.001(2) F90D 0.049(3) 0.042(2) 0.047(2) -0.035(2) 0.003(2) -0.005(2) F90E 0.053(3) 0.034(4) 0.155(5) -0.059(4) -0.055(3) 0.009(3) F90F 0.093(5) 0.036(3) 0.033(2) -0.001(2) -0.028(3) -0.032(3) C91 0.019(2) 0.018(2) 0.018(2) -0.0066(18) -0.0061(18) -0.0027(17) C92 0.021(2) 0.022(2) 0.015(2) -0.0029(18) -0.0044(18) -0.0073(18) C93 0.025(2) 0.024(2) 0.017(2) -0.0018(19) -0.0089(19) -0.007(2) C94 0.041(3) 0.025(3) 0.020(2) -0.005(2) -0.014(2) -0.013(2) C96 0.027(3) 0.020(2) 0.020(2) -0.0079(19) -0.010(2) 0.0008(19) C97 0.027(3) 0.034(3) 0.014(2) -0.001(2) -0.008(2) -0.014(2) F97A 0.031(2) 0.075(3) 0.032(2) -0.017(2) -0.0167(16) 0.0074(19) F97B 0.037(2) 0.047(2) 0.0199(16) 0.0101(15) -0.0148(15) -0.0134(17) F97C 0.071(3) 0.045(2) 0.067(3) -0.008(2) -0.053(3) -0.017(2) C95 0.039(3) 0.019(2) 0.017(2) -0.0058(19) -0.012(2) 0.000(2) C98 0.045(3) 0.022(3) 0.009(3) -0.006(2) -0.008(3) 0.002(2) F98A 0.049(2) 0.044(2) 0.015(3) -0.016(2) -0.003(2) 0.0039(19) F98B 0.105(4) 0.041(2) 0.085(3) -0.022(2) 0.016(3) -0.004(3) F98C 0.067(3) 0.053(3) 0.086(4) -0.040(3) -0.048(3) 0.017(2) C95A 0.039(3) 0.019(2) 0.017(2) -0.0058(19) -0.012(2) 0.000(2) C98A 0.045(3) 0.022(3) 0.009(3) -0.006(2) -0.008(3) 0.002(2) F98D 0.049(2) 0.044(2) 0.015(3) -0.016(2) -0.003(2) 0.0039(19) F98E 0.105(4) 0.041(2) 0.085(3) -0.022(2) 0.016(3) -0.004(3) F98F 0.067(3) 0.053(3) 0.086(4) -0.040(3) -0.048(3) 0.017(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 Ir1 N4 2.076(4) . ? Ir1 N1 2.087(4) . ? Ir1 C6 2.106(5) . ? Ir1 C1 2.123(5) . ? Ir1 C2 2.135(5) . ? Ir1 C5 2.141(5) . ? N1 C11 1.339(6) . ? N1 C9 1.386(6) . ? N2 C11 1.348(6) . ? N2 C10 1.376(7) . ? N2 C12 1.467(7) . ? N3 C15 1.351(6) . ? N3 C16 1.382(7) . ? N3 C14 1.466(7) . ? N4 C15 1.330(6) . ? N4 C17 1.374(6) . ? C1 C2 1.412(7) . ? C1 C8 1.514(7) . ? C1 H1 0.9500 . ? C2 C3 1.508(8) . ? C2 H2 0.9500 . ? C3 C4 1.528(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.517(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.408(7) . ? C5 H5 0.9500 . ? C6 C7 1.509(7) . ? C6 H6 0.9500 . ? C7 C8 1.549(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.357(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C13 1.496(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.481(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C17 1.356(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? Ir2 N5 2.095(5) . ? Ir2 N8 2.104(5) . ? Ir2 C23 2.113(6) . ? Ir2 C22 2.127(6) . ? Ir2 C19 2.133(6) . ? Ir2 C18 2.146(6) . ? Ir2A N5 1.787(5) . ? Ir2A N8 1.947(5) . ? Ir2A C19 2.442(7) . ? Ir2A C22 2.538(7) . ? N5 C28 1.321(8) . ? N5 C26 1.382(7) . ? N6 C28 1.369(7) . ? N6 C27 1.384(9) . ? N6 C29 1.451(8) . ? N7 C32 1.341(7) . ? N7 C33 1.378(7) . ? N7 C31 1.457(8) . ? N8 C32 1.339(7) . ? N8 C34 1.393(7) . ? C18 C19 1.441(10) . ? C18 C25 1.479(9) . ? C18 H18 0.9500 . ? C19 C20 1.519(10) . ? C19 H19 0.9500 . ? C20 C21 1.438(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.493(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.379(11) . ? C22 H22 0.9500 . ? C23 C24 1.512(10) . ? C23 H23 0.9500 . ? C24 C25 1.467(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.343(9) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C30 1.488(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.498(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.339(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? B1 C51 1.640(7) . ? B1 C59 1.640(7) . ? B1 C43 1.642(7) . ? B1 C35 1.645(7) . ? C35 C40 1.397(7) . ? C35 C36 1.407(7) . ? C36 C37 1.393(7) . ? C36 H36 0.9500 . ? C37 C38 1.392(8) . ? C37 C41 1.497(8) . ? C38 C39 1.388(7) . ? C38 H38 0.9500 . ? C39 C40 1.396(7) . ? C39 C42 1.492(7) . ? C40 H40 0.9500 . ? C41 F41A 1.323(7) . ? C41 F41C 1.334(7) . ? C41 F41B 1.369(8) . ? C42 F42A 1.328(6) . ? C42 F42B 1.343(7) . ? C42 F42C 1.343(7) . ? C43 C48 1.403(7) . ? C43 C44 1.408(6) . ? C44 C45 1.386(7) . ? C44 H44 0.9500 . ? C45 C46 1.380(7) . ? C45 C49 1.507(7) . ? C46 C47 1.395(7) . ? C46 H46 0.9500 . ? C47 C48 1.389(7) . ? C47 C50 1.492(7) . ? C48 H48 0.9500 . ? C49 F49B 1.336(7) . ? C49 F49A 1.341(7) . ? C49 F49C 1.344(7) . ? C50 F50C 1.338(6) . ? C50 F50B 1.346(6) . ? C50 F50A 1.354(6) . ? C51 C56 1.402(7) . ? C51 C52 1.403(7) . ? C52 C53 1.389(7) . ? C52 H52 0.9500 . ? C53 C54 1.382(8) . ? C53 C57 1.505(8) . ? C54 C55 1.382(7) . ? C54 H54 0.9500 . ? C55 C56 1.388(7) . ? C55 C58 1.492(7) . ? C56 H56 0.9500 . ? C57 F57B 1.313(8) . ? C57 F57A 1.326(7) . ? C57 F57C 1.333(8) . ? C58 F58A 1.335(6) . ? C58 F58B 1.340(7) . ? C58 F58C 1.351(7) . ? C59 C60 1.393(6) . ? C59 C64 1.402(7) . ? C60 C61 1.399(7) . ? C60 H60 0.9500 . ? C61 C62 1.382(7) . ? C61 C65 1.496(7) . ? C62 C63 1.384(7) . ? C62 H62 0.9500 . ? C64 C63 1.389(7) . ? C64 H64 0.9500 . ? C65 F65B 1.322(6) . ? C65 F65A 1.333(6) . ? C65 F65C 1.357(6) . ? C63 C66 1.495(6) . ? C66 F66A 1.2894 . ? C66 F66B 1.3311 . ? C66 F66C 1.3327 . ? C66A F66D 1.3131 . ? C66A F66E 1.3311 . ? C66A F66F 1.3366 . ? B2 C91 1.632(7) . ? B2 C83 1.635(7) . ? B2 C75 1.636(7) . ? B2 C67 1.646(7) . ? C67 C72 1.399(7) . ? C67 C68 1.406(7) . ? C68 C69 1.388(7) . ? C68 H68 0.9500 . ? C69 C70 1.390(7) . ? C69 C73 1.493(7) . ? C70 C71 1.387(7) . ? C70 H70 0.9500 . ? C71 C72 1.400(7) . ? C71 C74 1.492(7) . ? C72 H72 0.9500 . ? C73 F73C 1.321(7) . ? C73 F73B 1.331(7) . ? C73 F73A 1.347(7) . ? C74 F74A 1.333(6) . ? C74 F74C 1.335(7) . ? C74 F74B 1.346(7) . ? C75 C80 1.395(7) . ? C75 C76 1.399(7) . ? C76 C77 1.386(7) . ? C76 H76 0.9500 . ? C77 C78 1.379(8) . ? C77 C81 1.501(8) . ? C78 C79 1.383(8) . ? C78 H78 0.9500 . ? C79 C80 1.405(8) . ? C79 C82 1.498(9) . ? C80 H80 0.9500 . ? C81 F81C 1.333(8) . ? C81 F81A 1.337(7) . ? C81 F81B 1.344(7) . ? C82 F82A 1.324(9) . ? C82 F82C 1.344(7) . ? C82 F82B 1.360(10) . ? C83 C84 1.392(7) . ? C83 C88 1.407(7) . ? C84 C85 1.396(7) . ? C84 H84 0.9500 . ? C85 C86 1.386(7) . ? C85 C89 1.488(8) . ? C86 C87 1.379(7) . ? C86 H86 0.9500 . ? C88 C87 1.393(7) . ? C88 H88 0.9500 . ? C89 F89A 1.333(7) . ? C89 F89B 1.346(9) . ? C89 F89C 1.359(8) . ? C87 C90 1.495(6) . ? C90 F90C 1.2113 . ? C90 F90A 1.3169 . ? C90 F90B 1.3303 . ? C90A F90D 1.3169 . ? C90A F90E 1.3578 . ? C90A F90F 1.4142 . ? C91 C92 1.402(7) . ? C91 C96 1.406(7) . ? C92 C93 1.392(7) . ? C92 H92 0.9500 . ? C93 C94 1.388(8) . ? C93 C97 1.499(7) . ? C94 C95 1.399(8) . ? C94 H94 0.9500 . ? C96 C95 1.390(7) . ? C96 H96 0.9500 . ? C97 F97A 1.329(7) . ? C97 F97C 1.347(6) . ? C97 F97B 1.347(6) . ? C95 C98 1.509(6) . ? C98 F98A 1.3164 . ? C98 F98B 1.3427 . ? C98 F98C 1.4977 . ? C98A F98F 1.1370 . ? C98A F98D 1.3164 . ? C98A F98E 1.3328 . ? 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 N4 Ir1 N1 87.28(16) . . ? N4 Ir1 C6 89.01(18) . . ? N1 Ir1 C6 151.89(19) . . ? N4 Ir1 C1 158.70(18) . . ? N1 Ir1 C1 91.70(18) . . ? C6 Ir1 C1 81.9(2) . . ? N4 Ir1 C2 162.56(18) . . ? N1 Ir1 C2 94.16(19) . . ? C6 Ir1 C2 97.6(2) . . ? C1 Ir1 C2 38.73(19) . . ? N4 Ir1 C5 94.60(18) . . ? N1 Ir1 C5 169.37(19) . . ? C6 Ir1 C5 38.7(2) . . ? C1 Ir1 C5 90.3(2) . . ? C2 Ir1 C5 80.9(2) . . ? C11 N1 C9 105.9(4) . . ? C11 N1 Ir1 123.4(3) . . ? C9 N1 Ir1 128.3(4) . . ? C11 N2 C10 107.9(4) . . ? C11 N2 C12 126.6(5) . . ? C10 N2 C12 125.0(5) . . ? C15 N3 C16 107.6(4) . . ? C15 N3 C14 128.0(4) . . ? C16 N3 C14 124.3(4) . . ? C15 N4 C17 106.8(4) . . ? C15 N4 Ir1 125.6(3) . . ? C17 N4 Ir1 127.6(4) . . ? C2 C1 C8 122.2(5) . . ? C2 C1 Ir1 71.1(3) . . ? C8 C1 Ir1 113.7(3) . . ? C2 C1 H1 118.9 . . ? C8 C1 H1 118.9 . . ? Ir1 C1 H1 85.4 . . ? C1 C2 C3 123.9(5) . . ? C1 C2 Ir1 70.2(3) . . ? C3 C2 Ir1 111.8(4) . . ? C1 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? Ir1 C2 H2 88.0 . . ? C2 C3 C4 113.5(4) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 111.7(5) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 122.1(5) . . ? C6 C5 Ir1 69.3(3) . . ? C4 C5 Ir1 114.4(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? Ir1 C5 H5 86.5 . . ? C5 C6 C7 125.2(5) . . ? C5 C6 Ir1 72.0(3) . . ? C7 C6 Ir1 111.5(3) . . ? C5 C6 H6 117.4 . . ? C7 C6 H6 117.4 . . ? Ir1 C6 H6 86.5 . . ? C6 C7 C8 112.0(4) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C1 C8 C7 111.9(4) . . ? C1 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? C1 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 N1 109.3(5) . . ? C10 C9 H9 125.3 . . ? N1 C9 H9 125.3 . . ? C9 C10 N2 106.5(5) . . ? C9 C10 H10 126.7 . . ? N2 C10 H10 126.7 . . ? N1 C11 N2 110.4(4) . . ? N1 C11 C13 127.4(4) . . ? N2 C11 C13 122.2(5) . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C11 115.7(4) . . ? C15 C13 H13A 108.3 . . ? C11 C13 H13A 108.3 . . ? C15 C13 H13B 108.3 . . ? C11 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 N3 110.0(4) . . ? N4 C15 C13 126.9(4) . . ? N3 C15 C13 122.9(4) . . ? C17 C16 N3 106.3(4) . . ? C17 C16 H16 126.8 . . ? N3 C16 H16 126.8 . . ? C16 C17 N4 109.3(5) . . ? C16 C17 H17 125.4 . . ? N4 C17 H17 125.4 . . ? N5 Ir2 N8 85.56(18) . . ? N5 Ir2 C23 157.0(3) . . ? N8 Ir2 C23 92.1(2) . . ? N5 Ir2 C22 165.1(3) . . ? N8 Ir2 C22 94.9(2) . . ? C23 Ir2 C22 37.9(3) . . ? N5 Ir2 C19 95.2(2) . . ? N8 Ir2 C19 165.7(2) . . ? C23 Ir2 C19 92.6(3) . . ? C22 Ir2 C19 80.7(3) . . ? N5 Ir2 C18 90.7(2) . . ? N8 Ir2 C18 154.9(2) . . ? C23 Ir2 C18 81.7(2) . . ? C22 Ir2 C18 94.9(3) . . ? C19 Ir2 C18 39.4(3) . . ? N5 Ir2A N8 99.5(2) . . ? N5 Ir2A C19 93.9(2) . . ? N8 Ir2A C19 146.4(2) . . ? N5 Ir2A C22 150.4(3) . . ? N8 Ir2A C22 87.0(2) . . ? C19 Ir2A C22 67.2(2) . . ? C28 N5 C26 107.4(5) . . ? C28 N5 Ir2A 124.4(4) . . ? C26 N5 Ir2A 123.8(5) . . ? C28 N5 Ir2 124.9(4) . . ? C26 N5 Ir2 127.4(4) . . ? C28 N6 C27 106.8(5) . . ? C28 N6 C29 127.4(6) . . ? C27 N6 C29 125.8(5) . . ? C32 N7 C33 108.0(5) . . ? C32 N7 C31 126.4(5) . . ? C33 N7 C31 125.5(5) . . ? C32 N8 C34 105.5(5) . . ? C32 N8 Ir2A 119.9(4) . . ? C34 N8 Ir2A 130.9(4) . . ? C32 N8 Ir2 124.3(3) . . ? C34 N8 Ir2 129.6(4) . . ? C19 C18 C25 124.4(7) . . ? C19 C18 Ir2 69.8(4) . . ? C25 C18 Ir2 111.0(4) . . ? C19 C18 H18 117.8 . . ? C25 C18 H18 117.8 . . ? Ir2 C18 H18 89.2 . . ? C18 C19 C20 122.1(6) . . ? C18 C19 Ir2 70.8(3) . . ? C20 C19 Ir2 112.8(5) . . ? C18 C19 Ir2A 87.2(4) . . ? C20 C19 Ir2A 114.7(5) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? Ir2 C19 H19 86.5 . . ? Ir2A C19 H19 67.6 . . ? C21 C20 C19 115.2(7) . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 116.4(7) . . ? C20 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? C20 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C23 C22 C21 123.9(8) . . ? C23 C22 Ir2 70.5(4) . . ? C21 C22 Ir2 112.6(5) . . ? C23 C22 Ir2A 87.5(4) . . ? C21 C22 Ir2A 109.9(6) . . ? C23 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? Ir2 C22 H22 86.9 . . ? Ir2A C22 H22 71.6 . . ? C22 C23 C24 123.7(8) . . ? C22 C23 Ir2 71.6(4) . . ? C24 C23 Ir2 112.2(5) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? Ir2 C23 H23 86.2 . . ? C25 C24 C23 115.5(6) . . ? C25 C24 H24A 108.4 . . ? C23 C24 H24A 108.4 . . ? C25 C24 H24B 108.4 . . ? C23 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C18 116.4(6) . . ? C24 C25 H25A 108.2 . . ? C18 C25 H25A 108.2 . . ? C24 C25 H25B 108.2 . . ? C18 C25 H25B 108.2 . . ? H25A C25 H25B 107.3 . . ? C27 C26 N5 108.8(6) . . ? C27 C26 H26 125.6 . . ? N5 C26 H26 125.6 . . ? C26 C27 N6 107.3(5) . . ? C26 C27 H27 126.3 . . ? N6 C27 H27 126.3 . . ? N5 C28 N6 109.7(5) . . ? N5 C28 C30 127.4(5) . . ? N6 C28 C30 122.8(6) . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 C32 113.6(5) . . ? C28 C30 H30A 108.9 . . ? C32 C30 H30A 108.9 . . ? C28 C30 H30B 108.9 . . ? C32 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? N7 C31 H31A 109.5 . . ? N7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C32 N7 110.4(5) . . ? N8 C32 C30 126.9(5) . . ? N7 C32 C30 122.6(5) . . ? C34 C33 N7 106.6(5) . . ? C34 C33 H33 126.7 . . ? N7 C33 H33 126.7 . . ? C33 C34 N8 109.6(5) . . ? C33 C34 H34 125.2 . . ? N8 C34 H34 125.2 . . ? C51 B1 C59 104.8(4) . . ? C51 B1 C43 112.6(4) . . ? C59 B1 C43 111.9(4) . . ? C51 B1 C35 111.5(4) . . ? C59 B1 C35 111.4(4) . . ? C43 B1 C35 104.8(4) . . ? C40 C35 C36 115.4(4) . . ? C40 C35 B1 121.9(4) . . ? C36 C35 B1 122.6(4) . . ? C37 C36 C35 122.2(5) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C38 C37 C36 120.8(5) . . ? C38 C37 C41 118.1(5) . . ? C36 C37 C41 121.1(5) . . ? C39 C38 C37 118.2(5) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C38 C39 C40 120.3(5) . . ? C38 C39 C42 120.2(5) . . ? C40 C39 C42 119.4(5) . . ? C39 C40 C35 122.9(5) . . ? C39 C40 H40 118.5 . . ? C35 C40 H40 118.5 . . ? F41A C41 F41C 108.9(6) . . ? F41A C41 F41B 104.4(5) . . ? F41C C41 F41B 104.7(6) . . ? F41A C41 C37 113.6(5) . . ? F41C C41 C37 113.2(5) . . ? F41B C41 C37 111.4(5) . . ? F42A C42 F42B 106.1(5) . . ? F42A C42 F42C 106.7(5) . . ? F42B C42 F42C 104.5(5) . . ? F42A C42 C39 113.8(5) . . ? F42B C42 C39 112.3(5) . . ? F42C C42 C39 112.8(4) . . ? C48 C43 C44 115.6(4) . . ? C48 C43 B1 122.0(4) . . ? C44 C43 B1 122.1(4) . . ? C45 C44 C43 121.6(5) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C46 C45 C44 122.3(5) . . ? C46 C45 C49 119.1(5) . . ? C44 C45 C49 118.6(5) . . ? C45 C46 C47 117.0(5) . . ? C45 C46 H46 121.5 . . ? C47 C46 H46 121.5 . . ? C48 C47 C46 121.2(4) . . ? C48 C47 C50 120.7(4) . . ? C46 C47 C50 118.0(4) . . ? C47 C48 C43 122.3(4) . . ? C47 C48 H48 118.9 . . ? C43 C48 H48 118.9 . . ? F49B C49 F49A 107.0(5) . . ? F49B C49 F49C 106.6(5) . . ? F49A C49 F49C 105.8(5) . . ? F49B C49 C45 113.3(5) . . ? F49A C49 C45 111.7(5) . . ? F49C C49 C45 112.0(5) . . ? F50C C50 F50B 106.3(4) . . ? F50C C50 F50A 105.7(4) . . ? F50B C50 F50A 105.6(4) . . ? F50C C50 C47 113.5(4) . . ? F50B C50 C47 112.7(4) . . ? F50A C50 C47 112.4(4) . . ? C56 C51 C52 115.6(4) . . ? C56 C51 B1 121.4(4) . . ? C52 C51 B1 122.7(4) . . ? C53 C52 C51 122.2(5) . . ? C53 C52 H52 118.9 . . ? C51 C52 H52 118.9 . . ? C54 C53 C52 120.9(5) . . ? C54 C53 C57 118.3(5) . . ? C52 C53 C57 120.7(5) . . ? C55 C54 C53 118.1(5) . . ? C55 C54 H54 121.0 . . ? C53 C54 H54 121.0 . . ? C54 C55 C56 121.2(5) . . ? C54 C55 C58 119.6(5) . . ? C56 C55 C58 119.2(5) . . ? C55 C56 C51 122.0(4) . . ? C55 C56 H56 119.0 . . ? C51 C56 H56 119.0 . . ? F57B C57 F57A 106.3(6) . . ? F57B C57 F57C 106.0(6) . . ? F57A C57 F57C 106.4(6) . . ? F57B C57 C53 113.1(6) . . ? F57A C57 C53 112.6(5) . . ? F57C C57 C53 111.8(5) . . ? F58A C58 F58B 106.0(5) . . ? F58A C58 F58C 105.9(5) . . ? F58B C58 F58C 104.2(5) . . ? F58A C58 C55 114.0(5) . . ? F58B C58 C55 113.7(5) . . ? F58C C58 C55 112.2(5) . . ? C60 C59 C64 115.6(4) . . ? C60 C59 B1 121.9(4) . . ? C64 C59 B1 122.3(4) . . ? C59 C60 C61 122.4(4) . . ? C59 C60 H60 118.8 . . ? C61 C60 H60 118.8 . . ? C62 C61 C60 120.9(4) . . ? C62 C61 C65 119.8(4) . . ? C60 C61 C65 119.3(4) . . ? C61 C62 C63 117.5(5) . . ? C61 C62 H62 121.2 . . ? C63 C62 H62 121.2 . . ? C63 C64 C59 121.9(5) . . ? C63 C64 H64 119.0 . . ? C59 C64 H64 119.0 . . ? F65B C65 F65A 108.5(5) . . ? F65B C65 F65C 104.0(5) . . ? F65A C65 F65C 104.5(4) . . ? F65B C65 C61 114.0(4) . . ? F65A C65 C61 113.4(4) . . ? F65C C65 C61 111.6(4) . . ? C62 C63 C64 121.6(5) . . ? C62 C63 C66 119.6(5) . . ? C64 C63 C66 118.7(5) . . ? F66A C66 F66B 106.6 . . ? F66A C66 F66C 94.2 . . ? F66B C66 F66C 114.6 . . ? F66A C66 C63 121.0(4) . . ? F66B C66 C63 108.5(3) . . ? F66C C66 C63 111.7(4) . . ? F66D C66A F66E 97.8 . . ? F66D C66A F66F 126.4 . . ? F66E C66A F66F 88.2 . . ? C91 B2 C83 113.8(4) . . ? C91 B2 C75 105.0(4) . . ? C83 B2 C75 111.8(4) . . ? C91 B2 C67 111.2(4) . . ? C83 B2 C67 101.4(4) . . ? C75 B2 C67 113.8(4) . . ? C72 C67 C68 115.6(4) . . ? C72 C67 B2 119.0(4) . . ? C68 C67 B2 124.9(4) . . ? C69 C68 C67 122.2(5) . . ? C69 C68 H68 118.9 . . ? C67 C68 H68 118.9 . . ? C68 C69 C70 121.5(5) . . ? C68 C69 C73 119.6(5) . . ? C70 C69 C73 118.8(5) . . ? C71 C70 C69 117.4(5) . . ? C71 C70 H70 121.3 . . ? C69 C70 H70 121.3 . . ? C70 C71 C72 121.2(5) . . ? C70 C71 C74 120.3(5) . . ? C72 C71 C74 118.5(5) . . ? C67 C72 C71 122.2(5) . . ? C67 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? F73C C73 F73B 106.3(5) . . ? F73C C73 F73A 105.4(5) . . ? F73B C73 F73A 104.5(5) . . ? F73C C73 C69 114.2(5) . . ? F73B C73 C69 112.3(5) . . ? F73A C73 C69 113.3(5) . . ? F74A C74 F74C 106.6(5) . . ? F74A C74 F74B 105.5(5) . . ? F74C C74 F74B 105.8(5) . . ? F74A C74 C71 113.0(5) . . ? F74C C74 C71 113.4(5) . . ? F74B C74 C71 111.9(5) . . ? C80 C75 C76 116.1(5) . . ? C80 C75 B2 124.3(4) . . ? C76 C75 B2 119.3(4) . . ? C77 C76 C75 122.6(5) . . ? C77 C76 H76 118.7 . . ? C75 C76 H76 118.7 . . ? C78 C77 C76 120.7(5) . . ? C78 C77 C81 120.1(5) . . ? C76 C77 C81 119.1(5) . . ? C77 C78 C79 118.1(5) . . ? C77 C78 H78 121.0 . . ? C79 C78 H78 121.0 . . ? C78 C79 C80 121.3(5) . . ? C78 C79 C82 119.3(5) . . ? C80 C79 C82 119.2(5) . . ? C75 C80 C79 121.1(5) . . ? C75 C80 H80 119.4 . . ? C79 C80 H80 119.4 . . ? F81C C81 F81A 106.1(5) . . ? F81C C81 F81B 106.7(6) . . ? F81A C81 F81B 105.7(5) . . ? F81C C81 C77 112.7(5) . . ? F81A C81 C77 112.6(5) . . ? F81B C81 C77 112.5(5) . . ? F82A C82 F82C 109.4(7) . . ? F82A C82 F82B 105.6(6) . . ? F82C C82 F82B 103.3(6) . . ? F82A C82 C79 113.7(6) . . ? F82C C82 C79 112.1(6) . . ? F82B C82 C79 112.0(6) . . ? C84 C83 C88 115.9(4) . . ? C84 C83 B2 122.0(4) . . ? C88 C83 B2 121.5(4) . . ? C83 C84 C85 122.2(5) . . ? C83 C84 H84 118.9 . . ? C85 C84 H84 118.9 . . ? C86 C85 C84 120.7(5) . . ? C86 C85 C89 120.7(5) . . ? C84 C85 C89 118.5(5) . . ? C87 C86 C85 118.2(5) . . ? C87 C86 H86 120.9 . . ? C85 C86 H86 120.9 . . ? C87 C88 C83 121.9(5) . . ? C87 C88 H88 119.1 . . ? C83 C88 H88 119.1 . . ? F89A C89 F89B 106.7(6) . . ? F89A C89 F89C 105.8(6) . . ? F89B C89 F89C 105.2(6) . . ? F89A C89 C85 113.7(5) . . ? F89B C89 C85 112.6(6) . . ? F89C C89 C85 112.1(5) . . ? C86 C87 C88 121.0(5) . . ? C86 C87 C90 123.8(5) . . ? C88 C87 C90 115.2(5) . . ? F90C C90 F90A 110.6 . . ? F90C C90 F90B 109.1 . . ? F90A C90 F90B 98.5 . . ? F90C C90 C87 119.1(3) . . ? F90A C90 C87 110.9(4) . . ? F90B C90 C87 106.5(3) . . ? F90D C90A F90E 105.1 . . ? F90D C90A F90F 100.0 . . ? F90E C90A F90F 108.5 . . ? C92 C91 C96 115.7(4) . . ? C92 C91 B2 125.0(4) . . ? C96 C91 B2 119.1(4) . . ? C93 C92 C91 121.9(5) . . ? C93 C92 H92 119.1 . . ? C91 C92 H92 119.1 . . ? C94 C93 C92 121.5(5) . . ? C94 C93 C97 119.3(5) . . ? C92 C93 C97 119.1(5) . . ? C93 C94 C95 117.6(5) . . ? C93 C94 H94 121.2 . . ? C95 C94 H94 121.2 . . ? C95 C96 C91 122.6(5) . . ? C95 C96 H96 118.7 . . ? C91 C96 H96 118.7 . . ? F97A C97 F97C 107.5(5) . . ? F97A C97 F97B 105.9(5) . . ? F97C C97 F97B 104.7(4) . . ? F97A C97 C93 113.7(4) . . ? F97C C97 C93 112.9(5) . . ? F97B C97 C93 111.4(4) . . ? C96 C95 C94 120.6(5) . . ? C96 C95 C98 122.7(5) . . ? C94 C95 C98 116.7(5) . . ? F98A C98 F98B 112.3 . . ? F98A C98 F98C 101.9 . . ? F98B C98 F98C 110.8 . . ? F98A C98 C95 118.0(3) . . ? F98B C98 C95 107.5(3) . . ? F98C C98 C95 106.0(3) . . ? F98F C98A F98D 106.7 . . ? F98F C98A F98E 106.5 . . ? F98D C98A F98E 93.2 . . ? 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 N4 Ir1 N1 C11 -32.4(4) . . . . ? C6 Ir1 N1 C11 50.4(6) . . . . ? C1 Ir1 N1 C11 126.3(4) . . . . ? C2 Ir1 N1 C11 165.1(4) . . . . ? C5 Ir1 N1 C11 -132.9(9) . . . . ? N4 Ir1 N1 C9 167.8(5) . . . . ? C6 Ir1 N1 C9 -109.4(5) . . . . ? C1 Ir1 N1 C9 -33.5(5) . . . . ? C2 Ir1 N1 C9 5.2(5) . . . . ? C5 Ir1 N1 C9 67.3(11) . . . . ? N1 Ir1 N4 C15 23.8(4) . . . . ? C6 Ir1 N4 C15 -128.4(4) . . . . ? C1 Ir1 N4 C15 -63.9(7) . . . . ? C2 Ir1 N4 C15 119.0(7) . . . . ? C5 Ir1 N4 C15 -166.7(4) . . . . ? N1 Ir1 N4 C17 -157.3(4) . . . . ? C6 Ir1 N4 C17 50.6(4) . . . . ? C1 Ir1 N4 C17 115.0(6) . . . . ? C2 Ir1 N4 C17 -62.1(8) . . . . ? C5 Ir1 N4 C17 12.2(4) . . . . ? N4 Ir1 C1 C2 -178.6(4) . . . . ? N1 Ir1 C1 C2 94.5(3) . . . . ? C6 Ir1 C1 C2 -113.0(3) . . . . ? C5 Ir1 C1 C2 -75.0(3) . . . . ? N4 Ir1 C1 C8 -60.9(7) . . . . ? N1 Ir1 C1 C8 -147.7(4) . . . . ? C6 Ir1 C1 C8 4.8(4) . . . . ? C2 Ir1 C1 C8 117.7(5) . . . . ? C5 Ir1 C1 C8 42.7(4) . . . . ? C8 C1 C2 C3 -3.1(8) . . . . ? Ir1 C1 C2 C3 103.5(5) . . . . ? C8 C1 C2 Ir1 -106.6(5) . . . . ? N4 Ir1 C2 C1 178.3(5) . . . . ? N1 Ir1 C2 C1 -87.5(3) . . . . ? C6 Ir1 C2 C1 66.9(3) . . . . ? C5 Ir1 C2 C1 102.0(3) . . . . ? N4 Ir1 C2 C3 58.6(8) . . . . ? N1 Ir1 C2 C3 152.8(4) . . . . ? C6 Ir1 C2 C3 -52.8(4) . . . . ? C1 Ir1 C2 C3 -119.7(5) . . . . ? C5 Ir1 C2 C3 -17.7(4) . . . . ? C1 C2 C3 C4 -49.9(7) . . . . ? Ir1 C2 C3 C4 30.3(6) . . . . ? C2 C3 C4 C5 -28.1(7) . . . . ? C3 C4 C5 C6 92.8(6) . . . . ? C3 C4 C5 Ir1 12.8(6) . . . . ? N4 Ir1 C5 C6 82.6(3) . . . . ? N1 Ir1 C5 C6 -177.5(9) . . . . ? C1 Ir1 C5 C6 -76.6(3) . . . . ? C2 Ir1 C5 C6 -114.3(3) . . . . ? N4 Ir1 C5 C4 -160.4(4) . . . . ? N1 Ir1 C5 C4 -60.6(11) . . . . ? C6 Ir1 C5 C4 116.9(5) . . . . ? C1 Ir1 C5 C4 40.3(4) . . . . ? C2 Ir1 C5 C4 2.6(4) . . . . ? C4 C5 C6 C7 -2.5(8) . . . . ? Ir1 C5 C6 C7 104.0(5) . . . . ? C4 C5 C6 Ir1 -106.5(5) . . . . ? N4 Ir1 C6 C5 -98.6(3) . . . . ? N1 Ir1 C6 C5 179.0(3) . . . . ? C1 Ir1 C6 C5 100.7(3) . . . . ? C2 Ir1 C6 C5 65.2(3) . . . . ? N4 Ir1 C6 C7 139.8(4) . . . . ? N1 Ir1 C6 C7 57.4(6) . . . . ? C1 Ir1 C6 C7 -20.9(4) . . . . ? C2 Ir1 C6 C7 -56.4(4) . . . . ? C5 Ir1 C6 C7 -121.6(5) . . . . ? C5 C6 C7 C8 -49.4(7) . . . . ? Ir1 C6 C7 C8 33.2(5) . . . . ? C2 C1 C8 C7 93.7(6) . . . . ? Ir1 C1 C8 C7 11.9(6) . . . . ? C6 C7 C8 C1 -29.3(6) . . . . ? C11 N1 C9 C10 -0.9(6) . . . . ? Ir1 N1 C9 C10 161.6(4) . . . . ? N1 C9 C10 N2 0.6(7) . . . . ? C11 N2 C10 C9 -0.1(7) . . . . ? C12 N2 C10 C9 -172.3(5) . . . . ? C9 N1 C11 N2 0.9(6) . . . . ? Ir1 N1 C11 N2 -162.8(3) . . . . ? C9 N1 C11 C13 -179.9(5) . . . . ? Ir1 N1 C11 C13 16.5(7) . . . . ? C10 N2 C11 N1 -0.5(6) . . . . ? C12 N2 C11 N1 171.5(5) . . . . ? C10 N2 C11 C13 -179.8(5) . . . . ? C12 N2 C11 C13 -7.8(8) . . . . ? N1 C11 C13 C15 19.7(8) . . . . ? N2 C11 C13 C15 -161.1(5) . . . . ? C17 N4 C15 N3 -0.1(6) . . . . ? Ir1 N4 C15 N3 179.0(3) . . . . ? C17 N4 C15 C13 -176.4(5) . . . . ? Ir1 N4 C15 C13 2.7(7) . . . . ? C16 N3 C15 N4 -0.1(6) . . . . ? C14 N3 C15 N4 176.6(5) . . . . ? C16 N3 C15 C13 176.4(5) . . . . ? C14 N3 C15 C13 -6.9(8) . . . . ? C11 C13 C15 N4 -30.5(8) . . . . ? C11 C13 C15 N3 153.6(5) . . . . ? C15 N3 C16 C17 0.3(6) . . . . ? C14 N3 C16 C17 -176.6(5) . . . . ? N3 C16 C17 N4 -0.3(6) . . . . ? C15 N4 C17 C16 0.3(6) . . . . ? Ir1 N4 C17 C16 -178.8(4) . . . . ? N8 Ir2A N5 C28 9.6(5) . . . . ? C19 Ir2A N5 C28 158.6(5) . . . . ? C22 Ir2A N5 C28 110.5(6) . . . . ? N8 Ir2A N5 C26 163.1(5) . . . . ? C19 Ir2A N5 C26 -47.9(6) . . . . ? C22 Ir2A N5 C26 -96.0(7) . . . . ? N8 Ir2A N5 Ir2 -89.8(2) . . . . ? C19 Ir2A N5 Ir2 59.3(2) . . . . ? C22 Ir2A N5 Ir2 11.1(4) . . . . ? N8 Ir2 N5 C28 -31.2(5) . . . . ? C23 Ir2 N5 C28 53.7(9) . . . . ? C22 Ir2 N5 C28 -123.6(9) . . . . ? C19 Ir2 N5 C28 163.1(5) . . . . ? C18 Ir2 N5 C28 123.9(5) . . . . ? N8 Ir2 N5 C26 156.3(6) . . . . ? C23 Ir2 N5 C26 -118.8(7) . . . . ? C22 Ir2 N5 C26 63.9(11) . . . . ? C19 Ir2 N5 C26 -9.4(6) . . . . ? C18 Ir2 N5 C26 -48.6(6) . . . . ? N8 Ir2 N5 Ir2A 66.2(2) . . . . ? C23 Ir2 N5 Ir2A 151.2(6) . . . . ? C22 Ir2 N5 Ir2A -26.2(9) . . . . ? C19 Ir2 N5 Ir2A -99.5(3) . . . . ? C18 Ir2 N5 Ir2A -138.6(3) . . . . ? N5 Ir2A N8 C32 -9.4(5) . . . . ? C19 Ir2A N8 C32 -121.5(5) . . . . ? C22 Ir2A N8 C32 -160.4(4) . . . . ? N5 Ir2A N8 C34 -164.0(5) . . . . ? C19 Ir2A N8 C34 83.9(7) . . . . ? C22 Ir2A N8 C34 45.0(5) . . . . ? N5 Ir2A N8 Ir2 98.5(2) . . . . ? C19 Ir2A N8 Ir2 -13.6(4) . . . . ? C22 Ir2A N8 Ir2 -52.50(19) . . . . ? N5 Ir2 N8 C32 30.6(4) . . . . ? C23 Ir2 N8 C32 -126.4(5) . . . . ? C22 Ir2 N8 C32 -164.4(5) . . . . ? C19 Ir2 N8 C32 124.3(8) . . . . ? C18 Ir2 N8 C32 -51.6(7) . . . . ? N5 Ir2 N8 C34 -159.8(5) . . . . ? C23 Ir2 N8 C34 43.1(5) . . . . ? C22 Ir2 N8 C34 5.2(5) . . . . ? C19 Ir2 N8 C34 -66.1(10) . . . . ? C18 Ir2 N8 C34 118.0(6) . . . . ? N5 Ir2 N8 Ir2A -56.6(2) . . . . ? C23 Ir2 N8 Ir2A 146.4(3) . . . . ? C22 Ir2 N8 Ir2A 108.4(3) . . . . ? C19 Ir2 N8 Ir2A 37.1(9) . . . . ? C18 Ir2 N8 Ir2A -138.8(5) . . . . ? N5 Ir2 C18 C19 97.3(4) . . . . ? N8 Ir2 C18 C19 178.4(4) . . . . ? C23 Ir2 C18 C19 -104.5(4) . . . . ? C22 Ir2 C18 C19 -68.8(4) . . . . ? N5 Ir2 C18 C25 -142.5(6) . . . . ? N8 Ir2 C18 C25 -61.4(8) . . . . ? C23 Ir2 C18 C25 15.7(6) . . . . ? C22 Ir2 C18 C25 51.3(6) . . . . ? C19 Ir2 C18 C25 120.2(7) . . . . ? C25 C18 C19 C20 3.3(10) . . . . ? Ir2 C18 C19 C20 105.5(7) . . . . ? C25 C18 C19 Ir2 -102.2(6) . . . . ? C25 C18 C19 Ir2A -114.3(6) . . . . ? Ir2 C18 C19 Ir2A -12.08(10) . . . . ? N5 Ir2 C19 C18 -84.8(4) . . . . ? N8 Ir2 C19 C18 -177.2(7) . . . . ? C23 Ir2 C19 C18 73.5(4) . . . . ? C22 Ir2 C19 C18 109.7(4) . . . . ? N5 Ir2 C19 C20 157.6(6) . . . . ? N8 Ir2 C19 C20 65.1(11) . . . . ? C23 Ir2 C19 C20 -44.1(6) . . . . ? C22 Ir2 C19 C20 -7.9(6) . . . . ? C18 Ir2 C19 C20 -117.6(7) . . . . ? N5 Ir2 C19 Ir2A 57.90(19) . . . . ? N8 Ir2 C19 Ir2A -34.6(8) . . . . ? C23 Ir2 C19 Ir2A -143.8(2) . . . . ? C22 Ir2 C19 Ir2A -107.6(2) . . . . ? C18 Ir2 C19 Ir2A 142.7(3) . . . . ? N5 Ir2A C19 C18 -62.7(4) . . . . ? N8 Ir2A C19 C18 50.9(6) . . . . ? C22 Ir2A C19 C18 93.8(4) . . . . ? N5 Ir2A C19 C20 173.0(5) . . . . ? N8 Ir2A C19 C20 -73.3(7) . . . . ? C22 Ir2A C19 C20 -30.5(5) . . . . ? N5 Ir2A C19 Ir2 -97.7(2) . . . . ? N8 Ir2A C19 Ir2 15.9(4) . . . . ? C22 Ir2A C19 Ir2 58.8(2) . . . . ? C18 C19 C20 C21 -79.6(11) . . . . ? Ir2 C19 C20 C21 1.4(11) . . . . ? Ir2A C19 C20 C21 23.3(11) . . . . ? C19 C20 C21 C22 9.9(15) . . . . ? C20 C21 C22 C23 64.6(14) . . . . ? C20 C21 C22 Ir2 -16.5(13) . . . . ? C20 C21 C22 Ir2A -36.2(12) . . . . ? N5 Ir2 C22 C23 178.3(8) . . . . ? N8 Ir2 C22 C23 87.1(4) . . . . ? C19 Ir2 C22 C23 -106.6(5) . . . . ? C18 Ir2 C22 C23 -69.8(4) . . . . ? N5 Ir2 C22 C21 -62.2(12) . . . . ? N8 Ir2 C22 C21 -153.3(7) . . . . ? C23 Ir2 C22 C21 119.6(9) . . . . ? C19 Ir2 C22 C21 13.0(7) . . . . ? C18 Ir2 C22 C21 49.8(7) . . . . ? N5 Ir2 C22 Ir2A 23.2(8) . . . . ? N8 Ir2 C22 Ir2A -68.01(18) . . . . ? C23 Ir2 C22 Ir2A -155.1(4) . . . . ? C19 Ir2 C22 Ir2A 98.3(3) . . . . ? C18 Ir2 C22 Ir2A 135.1(2) . . . . ? N5 Ir2A C22 C23 -37.3(7) . . . . ? N8 Ir2A C22 C23 66.8(4) . . . . ? C19 Ir2A C22 C23 -91.0(5) . . . . ? N5 Ir2A C22 C21 88.0(8) . . . . ? N8 Ir2A C22 C21 -167.9(6) . . . . ? C19 Ir2A C22 C21 34.3(6) . . . . ? N5 Ir2A C22 Ir2 -13.9(5) . . . . ? N8 Ir2A C22 Ir2 90.2(2) . . . . ? C19 Ir2A C22 Ir2 -67.6(2) . . . . ? C21 C22 C23 C24 0.2(11) . . . . ? Ir2 C22 C23 C24 104.9(7) . . . . ? Ir2A C22 C23 C24 112.6(6) . . . . ? C21 C22 C23 Ir2 -104.7(8) . . . . ? Ir2A C22 C23 Ir2 7.72(11) . . . . ? N5 Ir2 C23 C22 -178.9(5) . . . . ? N8 Ir2 C23 C22 -95.3(4) . . . . ? C19 Ir2 C23 C22 71.2(4) . . . . ? C18 Ir2 C23 C22 109.2(5) . . . . ? N5 Ir2 C23 C24 61.5(11) . . . . ? N8 Ir2 C23 C24 145.1(7) . . . . ? C22 Ir2 C23 C24 -119.7(9) . . . . ? C19 Ir2 C23 C24 -48.4(8) . . . . ? C18 Ir2 C23 C24 -10.5(7) . . . . ? C22 C23 C24 C25 -78.5(12) . . . . ? Ir2 C23 C24 C25 3.5(13) . . . . ? C23 C24 C25 C18 10.2(15) . . . . ? C19 C18 C25 C24 60.7(12) . . . . ? Ir2 C18 C25 C24 -18.6(11) . . . . ? C28 N5 C26 C27 1.1(8) . . . . ? Ir2A N5 C26 C27 -156.2(5) . . . . ? Ir2 N5 C26 C27 174.7(5) . . . . ? N5 C26 C27 N6 -1.2(9) . . . . ? C28 N6 C27 C26 0.9(8) . . . . ? C29 N6 C27 C26 -177.6(7) . . . . ? C26 N5 C28 N6 -0.5(7) . . . . ? Ir2A N5 C28 N6 156.6(4) . . . . ? Ir2 N5 C28 N6 -174.3(4) . . . . ? C26 N5 C28 C30 179.7(6) . . . . ? Ir2A N5 C28 C30 -23.2(9) . . . . ? Ir2 N5 C28 C30 5.9(9) . . . . ? C27 N6 C28 N5 -0.2(7) . . . . ? C29 N6 C28 N5 178.3(6) . . . . ? C27 N6 C28 C30 179.6(6) . . . . ? C29 N6 C28 C30 -1.9(10) . . . . ? N5 C28 C30 C32 31.5(9) . . . . ? N6 C28 C30 C32 -148.3(6) . . . . ? C34 N8 C32 N7 -1.2(6) . . . . ? Ir2A N8 C32 N7 -161.6(4) . . . . ? Ir2 N8 C32 N7 170.5(3) . . . . ? C34 N8 C32 C30 -176.9(5) . . . . ? Ir2A N8 C32 C30 22.8(7) . . . . ? Ir2 N8 C32 C30 -5.2(8) . . . . ? C33 N7 C32 N8 0.8(6) . . . . ? C31 N7 C32 N8 -176.0(6) . . . . ? C33 N7 C32 C30 176.7(5) . . . . ? C31 N7 C32 C30 -0.2(9) . . . . ? C28 C30 C32 N8 -31.7(8) . . . . ? C28 C30 C32 N7 153.2(5) . . . . ? C32 N7 C33 C34 -0.1(7) . . . . ? C31 N7 C33 C34 176.8(6) . . . . ? N7 C33 C34 N8 -0.7(7) . . . . ? C32 N8 C34 C33 1.2(7) . . . . ? Ir2A N8 C34 C33 158.5(5) . . . . ? Ir2 N8 C34 C33 -169.9(4) . . . . ? C51 B1 C35 C40 -150.8(4) . . . . ? C59 B1 C35 C40 -34.1(6) . . . . ? C43 B1 C35 C40 87.1(5) . . . . ? C51 B1 C35 C36 33.5(6) . . . . ? C59 B1 C35 C36 150.2(4) . . . . ? C43 B1 C35 C36 -88.6(5) . . . . ? C40 C35 C36 C37 2.4(7) . . . . ? B1 C35 C36 C37 178.4(5) . . . . ? C35 C36 C37 C38 -0.9(8) . . . . ? C35 C36 C37 C41 178.3(5) . . . . ? C36 C37 C38 C39 -0.7(8) . . . . ? C41 C37 C38 C39 -179.9(5) . . . . ? C37 C38 C39 C40 0.6(8) . . . . ? C37 C38 C39 C42 178.4(5) . . . . ? C38 C39 C40 C35 1.2(8) . . . . ? C42 C39 C40 C35 -176.7(5) . . . . ? C36 C35 C40 C39 -2.6(7) . . . . ? B1 C35 C40 C39 -178.6(4) . . . . ? C38 C37 C41 F41A 58.3(8) . . . . ? C36 C37 C41 F41A -120.8(6) . . . . ? C38 C37 C41 F41C -176.8(6) . . . . ? C36 C37 C41 F41C 4.0(9) . . . . ? C38 C37 C41 F41B -59.2(7) . . . . ? C36 C37 C41 F41B 121.7(6) . . . . ? C38 C39 C42 F42A 12.1(7) . . . . ? C40 C39 C42 F42A -170.1(5) . . . . ? C38 C39 C42 F42B -108.6(6) . . . . ? C40 C39 C42 F42B 69.3(7) . . . . ? C38 C39 C42 F42C 133.7(5) . . . . ? C40 C39 C42 F42C -48.4(7) . . . . ? C51 B1 C43 C48 151.0(4) . . . . ? C59 B1 C43 C48 33.3(6) . . . . ? C35 B1 C43 C48 -87.5(5) . . . . ? C51 B1 C43 C44 -35.2(6) . . . . ? C59 B1 C43 C44 -152.9(4) . . . . ? C35 B1 C43 C44 86.2(5) . . . . ? C48 C43 C44 C45 -1.3(7) . . . . ? B1 C43 C44 C45 -175.5(4) . . . . ? C43 C44 C45 C46 1.2(8) . . . . ? C43 C44 C45 C49 -178.5(5) . . . . ? C44 C45 C46 C47 -0.4(7) . . . . ? C49 C45 C46 C47 179.3(5) . . . . ? C45 C46 C47 C48 -0.3(7) . . . . ? C45 C46 C47 C50 179.9(4) . . . . ? C46 C47 C48 C43 0.2(7) . . . . ? C50 C47 C48 C43 179.9(4) . . . . ? C44 C43 C48 C47 0.6(7) . . . . ? B1 C43 C48 C47 174.8(4) . . . . ? C46 C45 C49 F49B 6.3(8) . . . . ? C44 C45 C49 F49B -174.0(5) . . . . ? C46 C45 C49 F49A -114.6(6) . . . . ? C44 C45 C49 F49A 65.1(7) . . . . ? C46 C45 C49 F49C 126.9(5) . . . . ? C44 C45 C49 F49C -53.4(7) . . . . ? C48 C47 C50 F50C 145.3(5) . . . . ? C46 C47 C50 F50C -34.9(6) . . . . ? C48 C47 C50 F50B -93.7(6) . . . . ? C46 C47 C50 F50B 86.1(6) . . . . ? C48 C47 C50 F50A 25.5(6) . . . . ? C46 C47 C50 F50A -154.7(4) . . . . ? C59 B1 C51 C56 -84.4(5) . . . . ? C43 B1 C51 C56 153.8(4) . . . . ? C35 B1 C51 C56 36.3(6) . . . . ? C59 B1 C51 C52 88.3(5) . . . . ? C43 B1 C51 C52 -33.5(6) . . . . ? C35 B1 C51 C52 -151.0(4) . . . . ? C56 C51 C52 C53 -1.7(7) . . . . ? B1 C51 C52 C53 -174.8(5) . . . . ? C51 C52 C53 C54 0.8(8) . . . . ? C51 C52 C53 C57 -176.8(5) . . . . ? C52 C53 C54 C55 0.4(8) . . . . ? C57 C53 C54 C55 178.1(5) . . . . ? C53 C54 C55 C56 -0.6(8) . . . . ? C53 C54 C55 C58 -178.6(5) . . . . ? C54 C55 C56 C51 -0.4(8) . . . . ? C58 C55 C56 C51 177.6(5) . . . . ? C52 C51 C56 C55 1.5(7) . . . . ? B1 C51 C56 C55 174.7(4) . . . . ? C54 C53 C57 F57B 41.7(8) . . . . ? C52 C53 C57 F57B -140.7(6) . . . . ? C54 C53 C57 F57A 162.3(6) . . . . ? C52 C53 C57 F57A -20.1(9) . . . . ? C54 C53 C57 F57C -77.9(7) . . . . ? C52 C53 C57 F57C 99.7(7) . . . . ? C54 C55 C58 F58A -23.9(8) . . . . ? C56 C55 C58 F58A 158.1(5) . . . . ? C54 C55 C58 F58B -145.7(5) . . . . ? C56 C55 C58 F58B 36.3(7) . . . . ? C54 C55 C58 F58C 96.4(6) . . . . ? C56 C55 C58 F58C -81.6(6) . . . . ? C51 B1 C59 C60 -87.0(5) . . . . ? C43 B1 C59 C60 35.4(6) . . . . ? C35 B1 C59 C60 152.3(4) . . . . ? C51 B1 C59 C64 87.7(5) . . . . ? C43 B1 C59 C64 -150.0(4) . . . . ? C35 B1 C59 C64 -33.1(6) . . . . ? C64 C59 C60 C61 1.7(7) . . . . ? B1 C59 C60 C61 176.7(4) . . . . ? C59 C60 C61 C62 -0.8(8) . . . . ? C59 C60 C61 C65 178.5(5) . . . . ? C60 C61 C62 C63 0.1(8) . . . . ? C65 C61 C62 C63 -179.3(5) . . . . ? C60 C59 C64 C63 -1.9(7) . . . . ? B1 C59 C64 C63 -176.9(5) . . . . ? C62 C61 C65 F65B -106.4(6) . . . . ? C60 C61 C65 F65B 74.2(7) . . . . ? C62 C61 C65 F65A 18.4(7) . . . . ? C60 C61 C65 F65A -161.0(5) . . . . ? C62 C61 C65 F65C 136.1(5) . . . . ? C60 C61 C65 F65C -43.3(7) . . . . ? C61 C62 C63 C64 -0.3(8) . . . . ? C61 C62 C63 C66 175.8(5) . . . . ? C59 C64 C63 C62 1.2(8) . . . . ? C59 C64 C63 C66 -174.9(5) . . . . ? C62 C63 C66 F66A -115.6(5) . . . . ? C64 C63 C66 F66A 60.6(6) . . . . ? C62 C63 C66 F66B 120.9(5) . . . . ? C64 C63 C66 F66B -62.9(5) . . . . ? C62 C63 C66 F66C -6.4(6) . . . . ? C64 C63 C66 F66C 169.9(4) . . . . ? C91 B2 C67 C72 170.5(4) . . . . ? C83 B2 C67 C72 -68.1(5) . . . . ? C75 B2 C67 C72 52.1(6) . . . . ? C91 B2 C67 C68 -18.3(7) . . . . ? C83 B2 C67 C68 103.1(5) . . . . ? C75 B2 C67 C68 -136.7(5) . . . . ? C72 C67 C68 C69 0.9(7) . . . . ? B2 C67 C68 C69 -170.6(5) . . . . ? C67 C68 C69 C70 0.3(8) . . . . ? C67 C68 C69 C73 -177.3(5) . . . . ? C68 C69 C70 C71 -0.3(8) . . . . ? C73 C69 C70 C71 177.2(5) . . . . ? C69 C70 C71 C72 -0.8(8) . . . . ? C69 C70 C71 C74 179.8(5) . . . . ? C68 C67 C72 C71 -2.0(7) . . . . ? B2 C67 C72 C71 170.0(5) . . . . ? C70 C71 C72 C67 2.1(8) . . . . ? C74 C71 C72 C67 -178.5(5) . . . . ? C68 C69 C73 F73C -161.6(6) . . . . ? C70 C69 C73 F73C 20.8(8) . . . . ? C68 C69 C73 F73B 77.2(7) . . . . ? C70 C69 C73 F73B -100.3(6) . . . . ? C68 C69 C73 F73A -40.8(7) . . . . ? C70 C69 C73 F73A 141.6(5) . . . . ? C70 C71 C74 F74A -133.7(6) . . . . ? C72 C71 C74 F74A 46.9(7) . . . . ? C70 C71 C74 F74C -12.3(7) . . . . ? C72 C71 C74 F74C 168.3(5) . . . . ? C70 C71 C74 F74B 107.3(6) . . . . ? C72 C71 C74 F74B -72.1(6) . . . . ? C91 B2 C75 C80 -101.9(5) . . . . ? C83 B2 C75 C80 134.2(5) . . . . ? C67 B2 C75 C80 20.0(7) . . . . ? C91 B2 C75 C76 72.4(5) . . . . ? C83 B2 C75 C76 -51.5(6) . . . . ? C67 B2 C75 C76 -165.7(4) . . . . ? C80 C75 C76 C77 -0.4(7) . . . . ? B2 C75 C76 C77 -175.1(5) . . . . ? C75 C76 C77 C78 -0.4(8) . . . . ? C75 C76 C77 C81 179.3(5) . . . . ? C76 C77 C78 C79 0.9(8) . . . . ? C81 C77 C78 C79 -178.8(6) . . . . ? C77 C78 C79 C80 -0.7(9) . . . . ? C77 C78 C79 C82 175.2(6) . . . . ? C76 C75 C80 C79 0.5(8) . . . . ? B2 C75 C80 C79 175.0(5) . . . . ? C78 C79 C80 C75 0.0(9) . . . . ? C82 C79 C80 C75 -176.0(6) . . . . ? C78 C77 C81 F81C 139.8(6) . . . . ? C76 C77 C81 F81C -39.9(8) . . . . ? C78 C77 C81 F81A -100.3(6) . . . . ? C76 C77 C81 F81A 80.0(7) . . . . ? C78 C77 C81 F81B 19.1(8) . . . . ? C76 C77 C81 F81B -160.6(5) . . . . ? C78 C79 C82 F82A 153.3(6) . . . . ? C80 C79 C82 F82A -30.6(9) . . . . ? C78 C79 C82 F82C 28.6(10) . . . . ? C80 C79 C82 F82C -155.4(7) . . . . ? C78 C79 C82 F82B -87.0(7) . . . . ? C80 C79 C82 F82B 89.0(8) . . . . ? C91 B2 C83 C84 44.0(6) . . . . ? C75 B2 C83 C84 162.8(4) . . . . ? C67 B2 C83 C84 -75.5(5) . . . . ? C91 B2 C83 C88 -145.5(5) . . . . ? C75 B2 C83 C88 -26.6(6) . . . . ? C67 B2 C83 C88 95.0(5) . . . . ? C88 C83 C84 C85 -1.3(7) . . . . ? B2 C83 C84 C85 169.7(5) . . . . ? C83 C84 C85 C86 0.1(8) . . . . ? C83 C84 C85 C89 177.9(5) . . . . ? C84 C85 C86 C87 0.5(8) . . . . ? C89 C85 C86 C87 -177.3(6) . . . . ? C84 C83 C88 C87 2.1(7) . . . . ? B2 C83 C88 C87 -169.0(4) . . . . ? C86 C85 C89 F89A -15.9(9) . . . . ? C84 C85 C89 F89A 166.3(6) . . . . ? C86 C85 C89 F89B 105.7(7) . . . . ? C84 C85 C89 F89B -72.1(8) . . . . ? C86 C85 C89 F89C -135.9(6) . . . . ? C84 C85 C89 F89C 46.3(8) . . . . ? C85 C86 C87 C88 0.4(8) . . . . ? C85 C86 C87 C90 -178.1(5) . . . . ? C83 C88 C87 C86 -1.7(8) . . . . ? C83 C88 C87 C90 176.8(5) . . . . ? C86 C87 C90 F90C -115.1(5) . . . . ? C88 C87 C90 F90C 66.4(5) . . . . ? C86 C87 C90 F90A 14.9(6) . . . . ? C88 C87 C90 F90A -163.7(3) . . . . ? C86 C87 C90 F90B 121.0(5) . . . . ? C88 C87 C90 F90B -57.5(5) . . . . ? C83 B2 C91 C92 22.6(7) . . . . ? C75 B2 C91 C92 -100.1(5) . . . . ? C67 B2 C91 C92 136.4(5) . . . . ? C83 B2 C91 C96 -162.6(4) . . . . ? C75 B2 C91 C96 74.8(5) . . . . ? C67 B2 C91 C96 -48.8(6) . . . . ? C96 C91 C92 C93 3.0(7) . . . . ? B2 C91 C92 C93 178.0(5) . . . . ? C91 C92 C93 C94 0.4(8) . . . . ? C91 C92 C93 C97 -176.1(5) . . . . ? C92 C93 C94 C95 -3.5(8) . . . . ? C97 C93 C94 C95 173.1(5) . . . . ? C92 C91 C96 C95 -3.4(7) . . . . ? B2 C91 C96 C95 -178.7(5) . . . . ? C94 C93 C97 F97A 145.9(5) . . . . ? C92 C93 C97 F97A -37.5(7) . . . . ? C94 C93 C97 F97C 23.0(7) . . . . ? C92 C93 C97 F97C -160.4(5) . . . . ? C94 C93 C97 F97B -94.5(6) . . . . ? C92 C93 C97 F97B 82.1(6) . . . . ? C91 C96 C95 C94 0.4(8) . . . . ? C91 C96 C95 C98 177.5(5) . . . . ? C93 C94 C95 C96 3.0(8) . . . . ? C93 C94 C95 C98 -174.1(5) . . . . ? C96 C95 C98 F98A -137.0(4) . . . . ? C94 C95 C98 F98A 40.1(6) . . . . ? C96 C95 C98 F98B 94.8(5) . . . . ? C94 C95 C98 F98B -88.1(5) . . . . ? C96 C95 C98 F98C -23.7(6) . . . . ? C94 C95 C98 F98C 153.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.907 _refine_diff_density_min -2.236 _refine_diff_density_rms 0.150 # Attachment 'rh00802.cif' data_rh00802 _database_code_depnum_ccdc_archive 'CCDC 697505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H37 Ir N2 P, C32 H12 B F24 ' _chemical_formula_sum 'C69 H49 B F24 Ir N2 P ' _chemical_formula_weight 1596.10 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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 P21/n _symmetry_space_group_name_Hall -P2yn 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 12.5044(3) _cell_length_b 35.3357(9) _cell_length_c 14.8836(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.9560(10) _cell_angle_gamma 90.00 _cell_volume 6456.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 194094 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 33.142 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 2.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.522 _exptl_absorpt_correction_T_max 0.574 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa 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 130673 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 33.00 _reflns_number_total 24270 _reflns_number_gt 20833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect, KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 for windows (Farugia)' _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+4.7721P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24270 _refine_ls_number_parameters 905 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _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 0.363779(4) 0.151862(2) 0.255371(4) 0.01440(2) Uani 1 1 d . . . P1 P 0.54030(3) 0.131995(11) 0.29845(3) 0.01593(7) Uani 1 1 d . . . N1 N 0.40294(11) 0.19505(4) 0.35465(9) 0.0178(2) Uani 1 1 d . . . N2 N 0.43248(11) 0.18462(4) 0.44464(9) 0.0178(2) Uani 1 1 d . . . C1 C 0.18902(13) 0.15961(5) 0.26229(11) 0.0209(3) Uani 1 1 d . . . H1 H 0.1903(17) 0.1741(6) 0.3159(15) 0.023 Uiso 1 1 d . . . C2 C 0.20708(13) 0.17715(5) 0.18274(11) 0.0198(3) Uani 1 1 d . . . H2 H 0.2214(17) 0.2032(6) 0.1861(14) 0.022 Uiso 1 1 d . . . C3 C 0.17249(14) 0.16070(5) 0.08746(11) 0.0240(3) Uani 1 1 d . . . H3A H 0.1495 0.1815 0.0435 0.029 Uiso 1 1 calc R . . H3B H 0.1090 0.1439 0.0866 0.029 Uiso 1 1 calc R . . C4 C 0.26496(15) 0.13807(5) 0.05669(11) 0.0241(3) Uani 1 1 d . . . H4A H 0.2325 0.1191 0.0106 0.029 Uiso 1 1 calc R . . H4B H 0.3094 0.1556 0.0270 0.029 Uiso 1 1 calc R . . C5 C 0.33819(13) 0.11810(5) 0.13469(11) 0.0203(3) Uani 1 1 d . . . H5 H 0.4073(18) 0.1104(6) 0.1216(14) 0.022 Uiso 1 1 d . . . C6 C 0.30134(13) 0.09781(4) 0.20481(11) 0.0203(3) Uani 1 1 d . . . H6 H 0.3494(17) 0.0794(6) 0.2323(15) 0.022 Uiso 1 1 d . . . C7 C 0.18159(14) 0.09121(5) 0.20895(13) 0.0251(3) Uani 1 1 d . . . H7A H 0.1738 0.0660 0.2362 0.030 Uiso 1 1 calc R . . H7B H 0.1382 0.0911 0.1459 0.030 Uiso 1 1 calc R . . C8 C 0.13576(14) 0.12164(5) 0.26560(13) 0.0259(3) Uani 1 1 d . . . H8A H 0.0565 0.1243 0.2423 0.031 Uiso 1 1 calc R . . H8B H 0.1461 0.1132 0.3301 0.031 Uiso 1 1 calc R . . C9 C 0.38794(13) 0.23292(4) 0.35442(11) 0.0194(3) Uani 1 1 d . . . C10 C 0.40501(14) 0.24632(4) 0.44477(12) 0.0215(3) Uani 1 1 d . . . H10 H 0.3982 0.2717 0.4638 0.026 Uiso 1 1 calc R . . C11 C 0.43363(13) 0.21525(4) 0.50078(11) 0.0190(3) Uani 1 1 d . . . C12 C 0.36296(14) 0.25523(4) 0.26951(11) 0.0219(3) Uani 1 1 d . . . C13 C 0.39688(16) 0.24326(5) 0.19000(13) 0.0288(4) Uani 1 1 d . . . H13 H 0.4375 0.2205 0.1907 0.035 Uiso 1 1 calc R . . C14 C 0.37179(18) 0.26426(6) 0.10981(14) 0.0344(4) Uani 1 1 d . . . H14 H 0.3936 0.2555 0.0557 0.041 Uiso 1 1 calc R . . C15 C 0.3151(2) 0.29793(6) 0.10897(16) 0.0418(5) Uani 1 1 d . . . H15 H 0.2983 0.3124 0.0544 0.050 Uiso 1 1 calc R . . C16 C 0.2828(2) 0.31039(6) 0.18778(17) 0.0484(6) Uani 1 1 d . . . H16 H 0.2442 0.3336 0.1871 0.058 Uiso 1 1 calc R . . C17 C 0.30627(19) 0.28926(5) 0.26804(14) 0.0351(4) Uani 1 1 d . . . H17 H 0.2837 0.2980 0.3218 0.042 Uiso 1 1 calc R . . C18 C 0.45932(13) 0.21319(5) 0.60132(11) 0.0207(3) Uani 1 1 d . . . C19 C 0.42014(15) 0.18415(5) 0.65006(12) 0.0260(3) Uani 1 1 d . . . H19 H 0.3770 0.1645 0.6180 0.031 Uiso 1 1 calc R . . C20 C 0.44394(17) 0.18382(6) 0.74515(13) 0.0319(4) Uani 1 1 d . . . H20 H 0.4184 0.1637 0.7777 0.038 Uiso 1 1 calc R . . C21 C 0.50487(17) 0.21283(6) 0.79282(13) 0.0339(4) Uani 1 1 d . . . H21 H 0.5207 0.2126 0.8578 0.041 Uiso 1 1 calc R . . C22 C 0.54243(17) 0.24208(6) 0.74506(13) 0.0326(4) Uani 1 1 d . . . H22 H 0.5834 0.2621 0.7775 0.039 Uiso 1 1 calc R . . C23 C 0.52058(15) 0.24229(5) 0.65005(12) 0.0263(3) Uani 1 1 d . . . H23 H 0.5474 0.2623 0.6179 0.032 Uiso 1 1 calc R . . C24 C 0.48224(14) 0.14750(4) 0.46793(11) 0.0209(3) Uani 1 1 d . . . H24A H 0.4278 0.1274 0.4476 0.025 Uiso 1 1 calc R . . H24B H 0.5054 0.1455 0.5352 0.025 Uiso 1 1 calc R . . C25 C 0.58118(14) 0.14160(5) 0.42215(11) 0.0225(3) Uani 1 1 d . . . H25A H 0.6249 0.1201 0.4519 0.027 Uiso 1 1 calc R . . H25B H 0.6275 0.1645 0.4311 0.027 Uiso 1 1 calc R . . C26 C 0.56803(12) 0.08205(4) 0.28533(11) 0.0183(3) Uani 1 1 d . . . C27 C 0.52993(14) 0.05610(5) 0.34322(13) 0.0242(3) Uani 1 1 d . . . H27 H 0.4965 0.0650 0.3915 0.029 Uiso 1 1 calc R . . C28 C 0.54093(15) 0.01756(5) 0.33025(15) 0.0299(4) Uani 1 1 d . . . H28 H 0.5149 0.0001 0.3695 0.036 Uiso 1 1 calc R . . C29 C 0.58996(17) 0.00454(5) 0.26003(14) 0.0322(4) Uani 1 1 d . . . H29 H 0.5968 -0.0219 0.2510 0.039 Uiso 1 1 calc R . . C30 C 0.62900(17) 0.02995(5) 0.20293(14) 0.0312(4) Uani 1 1 d . . . H30 H 0.6633 0.0209 0.1554 0.037 Uiso 1 1 calc R . . C31 C 0.61786(14) 0.06890(5) 0.21526(12) 0.0241(3) Uani 1 1 d . . . H31 H 0.6442 0.0863 0.1760 0.029 Uiso 1 1 calc R . . C32 C 0.64120(13) 0.15547(4) 0.24522(11) 0.0202(3) Uani 1 1 d . . . C33 C 0.75104(14) 0.15595(5) 0.28829(14) 0.0278(3) Uani 1 1 d . . . H33 H 0.7729 0.1445 0.3467 0.033 Uiso 1 1 calc R . . C34 C 0.82790(17) 0.17313(6) 0.24563(16) 0.0378(5) Uani 1 1 d . . . H34 H 0.9022 0.1738 0.2753 0.045 Uiso 1 1 calc R . . C35 C 0.79634(19) 0.18935(6) 0.15965(16) 0.0400(5) Uani 1 1 d . . . H35 H 0.8491 0.2012 0.1308 0.048 Uiso 1 1 calc R . . C36 C 0.68857(19) 0.18833(5) 0.11582(14) 0.0340(4) Uani 1 1 d . . . H36 H 0.6676 0.1991 0.0566 0.041 Uiso 1 1 calc R . . C37 C 0.61041(15) 0.17144(5) 0.15857(12) 0.0247(3) Uani 1 1 d . . . H37 H 0.5363 0.1709 0.1285 0.030 Uiso 1 1 calc R . . B1 B 0.89020(13) 0.91469(5) 0.24341(11) 0.0158(3) Uani 1 1 d . . . C38 C 1.01416(12) 0.91349(4) 0.22322(10) 0.0159(2) Uani 1 1 d . . . C39 C 1.03240(12) 0.89952(4) 0.13896(10) 0.0172(3) Uani 1 1 d . . . H39 H 0.9714 0.8936 0.0926 0.021 Uiso 1 1 calc R . . C40 C 1.13663(12) 0.89409(4) 0.12104(11) 0.0177(3) Uani 1 1 d . . . C41 C 1.22786(12) 0.90216(4) 0.18712(11) 0.0194(3) Uani 1 1 d . . . H41 H 1.2992 0.8985 0.1753 0.023 Uiso 1 1 calc R . . C42 C 1.21173(12) 0.91578(4) 0.27153(11) 0.0178(3) Uani 1 1 d . . . C43 C 1.10735(12) 0.92141(4) 0.28899(10) 0.0175(3) Uani 1 1 d . . . H43 H 1.0992 0.9309 0.3470 0.021 Uiso 1 1 calc R . . C44 C 1.14840(13) 0.87829(5) 0.03011(12) 0.0223(3) Uani 1 1 d . . . F44A F 1.08378(10) 0.89531(4) -0.04043(7) 0.0342(2) Uani 1 1 d . . . F44B F 1.11903(12) 0.84145(3) 0.02242(9) 0.0392(3) Uani 1 1 d . . . F44C F 1.24898(9) 0.88098(4) 0.01373(9) 0.0435(3) Uani 1 1 d . . . C45 C 1.31040(13) 0.92464(5) 0.34221(12) 0.0234(3) Uani 1 1 d . . . F45A F 1.36070(12) 0.95593(4) 0.32338(10) 0.0506(4) Uani 1 1 d . . . F45B F 1.28898(10) 0.92937(4) 0.42653(8) 0.0392(3) Uani 1 1 d . . . F45C F 1.38546(10) 0.89682(4) 0.35042(9) 0.0440(3) Uani 1 1 d . . . C46 C 0.80312(11) 0.92877(4) 0.15315(10) 0.0148(2) Uani 1 1 d . . . C47 C 0.69288(12) 0.91883(4) 0.14150(10) 0.0167(3) Uani 1 1 d . . . H47 H 0.6705 0.9018 0.1837 0.020 Uiso 1 1 calc R . . C48 C 0.61507(12) 0.93310(4) 0.07000(11) 0.0179(3) Uani 1 1 d . . . C49 C 0.64344(13) 0.95795(5) 0.00600(11) 0.0195(3) Uani 1 1 d . . . H49 H 0.5904 0.9675 -0.0431 0.023 Uiso 1 1 calc R . . C50 C 0.75252(13) 0.96840(4) 0.01657(11) 0.0188(3) Uani 1 1 d . . . C51 C 0.83013(12) 0.95439(4) 0.08871(10) 0.0171(3) Uani 1 1 d . . . H51 H 0.9036 0.9624 0.0945 0.021 Uiso 1 1 calc R . . C52 C 0.49938(13) 0.92007(5) 0.06156(12) 0.0244(3) Uani 1 1 d . . . F52A F 0.47029(10) 0.91705(5) 0.14255(9) 0.0522(4) Uani 1 1 d . . . F52B F 0.48350(11) 0.88595(4) 0.02290(13) 0.0583(5) Uani 1 1 d . . . F52C F 0.42809(10) 0.94281(5) 0.01128(11) 0.0547(4) Uani 1 1 d . . . C53 C 0.78728(15) 0.99646(5) -0.04828(12) 0.0254(3) Uani 1 1 d . . . F53A F 0.80254(13) 1.03085(3) -0.01064(10) 0.0436(3) Uani 1 1 d . . . F53B F 0.88172(11) 0.98682(4) -0.07201(9) 0.0411(3) Uani 1 1 d . . . F53C F 0.71500(12) 1.00033(4) -0.12578(9) 0.0489(4) Uani 1 1 d . . . C54 C 0.87161(12) 0.94500(4) 0.32234(10) 0.0158(2) Uani 1 1 d . . . C55 C 0.79711(12) 0.93803(4) 0.37994(10) 0.0178(3) Uani 1 1 d . . . H55 H 0.7622 0.9141 0.3772 0.021 Uiso 1 1 calc R . . C56 C 0.77252(13) 0.96507(4) 0.44108(11) 0.0190(3) Uani 1 1 d . . . C57 C 0.81911(13) 1.00082(5) 0.44612(11) 0.0207(3) Uani 1 1 d . . . H57 H 0.8023 1.0193 0.4878 0.025 Uiso 1 1 calc R . . C58 C 0.89132(13) 1.00874(4) 0.38806(11) 0.0189(3) Uani 1 1 d . . . C59 C 0.91737(12) 0.98146(4) 0.32796(10) 0.0178(3) Uani 1 1 d . . . H59 H 0.9675 0.9877 0.2897 0.021 Uiso 1 1 calc R . . C60 C 0.69360(15) 0.95449(5) 0.50109(12) 0.0267(3) Uani 1 1 d . . . F60A F 0.60020(9) 0.93999(4) 0.45331(8) 0.0351(3) Uani 1 1 d . . . F60B F 0.73161(11) 0.92718(5) 0.56082(9) 0.0501(4) Uani 1 1 d . . . F60C F 0.66404(16) 0.98339(4) 0.54740(13) 0.0733(6) Uani 1 1 d . . . C61 C 0.93772(15) 1.04791(5) 0.38727(12) 0.0253(3) Uani 1 1 d . . . F61A F 1.03909(10) 1.04798(4) 0.37030(11) 0.0452(3) Uani 1 1 d . . . F61B F 0.88048(13) 1.06976(4) 0.32458(13) 0.0686(6) Uani 1 1 d . . . F61C F 0.94741(16) 1.06530(4) 0.46809(11) 0.0611(5) Uani 1 1 d . . . C62 C 0.86909(12) 0.87059(4) 0.27132(10) 0.0164(3) Uani 1 1 d . C . C63 C 0.89401(13) 0.85752(5) 0.36202(11) 0.0195(3) Uani 1 1 d . . . H63 H 0.9190 0.8751 0.4097 0.023 Uiso 1 1 calc R . . C64 C 0.88318(14) 0.81947(5) 0.38419(11) 0.0216(3) Uani 1 1 d . C . C65 C 0.85060(15) 0.79252(5) 0.31707(11) 0.0241(3) Uani 1 1 d . . . H65 H 0.8433 0.7667 0.3324 0.029 Uiso 1 1 calc R A 1 C67 C 0.83660(13) 0.84275(4) 0.20465(11) 0.0190(3) Uani 1 1 d . . . H67 H 0.8192 0.8502 0.1422 0.023 Uiso 1 1 calc R B 1 C68 C 0.90122(18) 0.80880(6) 0.48337(12) 0.0304(4) Uani 1 1 d . . . F68A F 0.90689(16) 0.77141(4) 0.49771(9) 0.0551(4) Uani 1 1 d . C . F68B F 0.82008(13) 0.82128(5) 0.52320(9) 0.0525(4) Uani 1 1 d . C . F68C F 0.99251(13) 0.82300(5) 0.53204(9) 0.0509(4) Uani 1 1 d . C . C66A C 0.82882(15) 0.80460(5) 0.22640(11) 0.0225(3) Uani 0.25 1 d PD C 1 C69A C 0.8118(4) 0.77521(7) 0.15241(17) 0.0289(5) Uani 0.25 1 d PGD C 1 F69A F 0.8740(4) 0.77669(7) 0.08893(17) 0.0569(4) Uani 0.25 1 d PRD C 1 F69B F 0.7061(4) 0.77499(7) 0.11464(17) 0.0372(4) Uani 0.25 1 d PRD C 1 F69C F 0.8417(4) 0.74060(7) 0.18284(17) 0.0467(17) Uani 0.25 1 d PRD C 1 C66B C 0.82882(15) 0.80460(5) 0.22640(11) 0.0225(3) Uani 0.75 1 d PD C 2 C69B C 0.79208(11) 0.77732(3) 0.14956(6) 0.0289(5) Uani 0.75 1 d PGD C 2 F69D F 0.86754(11) 0.77436(3) 0.09750(6) 0.0569(4) Uani 0.75 1 d PRD C 2 F69E F 0.70467(11) 0.78867(3) 0.08964(6) 0.0372(4) Uani 0.75 1 d PRD C 2 F69F F 0.76860(11) 0.74300(3) 0.17749(6) 0.0729(10) Uani 0.75 1 d PRD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01586(3) 0.01287(2) 0.01406(2) -0.00021(2) 0.00179(2) 0.00182(2) P1 0.01636(16) 0.01333(16) 0.01774(16) -0.00113(13) 0.00231(13) 0.00149(12) N1 0.0214(6) 0.0139(5) 0.0175(6) -0.0001(4) 0.0021(5) 0.0019(4) N2 0.0225(6) 0.0146(5) 0.0161(5) -0.0010(4) 0.0032(5) 0.0022(5) C1 0.0183(7) 0.0247(8) 0.0195(7) -0.0001(6) 0.0034(5) 0.0035(5) C2 0.0192(7) 0.0188(7) 0.0203(7) 0.0005(5) 0.0005(5) 0.0057(5) C3 0.0259(8) 0.0271(8) 0.0170(7) 0.0020(6) -0.0010(6) 0.0051(6) C4 0.0281(8) 0.0282(8) 0.0151(6) -0.0010(6) 0.0019(6) 0.0030(6) C5 0.0222(7) 0.0194(7) 0.0188(7) -0.0050(5) 0.0028(5) 0.0022(5) C6 0.0209(7) 0.0157(6) 0.0222(7) -0.0012(5) -0.0012(6) 0.0013(5) C7 0.0221(7) 0.0212(7) 0.0304(8) 0.0024(6) 0.0009(6) -0.0037(6) C8 0.0208(7) 0.0296(9) 0.0279(8) 0.0047(7) 0.0060(6) -0.0016(6) C9 0.0195(7) 0.0142(6) 0.0241(7) -0.0003(5) 0.0032(5) 0.0010(5) C10 0.0244(7) 0.0149(6) 0.0251(7) -0.0038(6) 0.0043(6) 0.0007(5) C11 0.0191(7) 0.0172(6) 0.0212(7) -0.0044(5) 0.0055(5) -0.0015(5) C12 0.0247(7) 0.0140(6) 0.0250(8) 0.0010(5) -0.0005(6) -0.0021(5) C13 0.0335(9) 0.0242(8) 0.0297(9) 0.0057(7) 0.0084(7) 0.0007(7) C14 0.0403(11) 0.0331(10) 0.0290(9) 0.0070(8) 0.0048(8) -0.0067(8) C15 0.0514(13) 0.0310(10) 0.0362(11) 0.0130(8) -0.0091(9) -0.0053(9) C16 0.0693(17) 0.0226(9) 0.0456(13) 0.0068(9) -0.0083(12) 0.0134(10) C17 0.0502(12) 0.0183(8) 0.0324(10) -0.0022(7) -0.0034(8) 0.0091(8) C18 0.0203(7) 0.0213(7) 0.0211(7) -0.0044(6) 0.0058(6) -0.0012(6) C19 0.0279(8) 0.0274(8) 0.0240(8) -0.0040(6) 0.0082(6) -0.0067(6) C20 0.0367(10) 0.0383(10) 0.0234(8) -0.0005(7) 0.0121(7) -0.0089(8) C21 0.0383(10) 0.0434(11) 0.0207(8) -0.0054(7) 0.0076(7) -0.0062(8) C22 0.0370(10) 0.0348(10) 0.0254(8) -0.0096(7) 0.0043(7) -0.0096(8) C23 0.0302(8) 0.0247(8) 0.0243(8) -0.0051(6) 0.0060(6) -0.0062(7) C24 0.0292(8) 0.0155(7) 0.0178(6) 0.0007(5) 0.0037(6) 0.0047(6) C25 0.0225(7) 0.0229(7) 0.0199(7) -0.0029(6) -0.0011(6) 0.0063(6) C26 0.0162(6) 0.0152(6) 0.0225(7) -0.0011(5) 0.0007(5) 0.0019(5) C27 0.0221(7) 0.0181(7) 0.0327(9) 0.0038(6) 0.0058(6) 0.0025(6) C28 0.0266(8) 0.0171(7) 0.0435(10) 0.0063(7) 0.0005(7) 0.0017(6) C29 0.0340(9) 0.0159(7) 0.0413(10) -0.0044(7) -0.0064(8) 0.0051(7) C30 0.0357(10) 0.0236(8) 0.0321(9) -0.0078(7) 0.0012(7) 0.0086(7) C31 0.0271(8) 0.0200(7) 0.0248(7) -0.0038(6) 0.0038(6) 0.0034(6) C32 0.0213(7) 0.0143(6) 0.0264(7) -0.0043(6) 0.0075(6) -0.0005(5) C33 0.0215(7) 0.0253(8) 0.0373(9) -0.0064(7) 0.0077(7) -0.0018(6) C34 0.0267(9) 0.0387(11) 0.0510(13) -0.0173(9) 0.0151(8) -0.0101(8) C35 0.0445(12) 0.0366(10) 0.0474(12) -0.0166(9) 0.0301(10) -0.0179(9) C36 0.0502(12) 0.0251(8) 0.0321(9) -0.0047(7) 0.0219(9) -0.0067(8) C37 0.0313(8) 0.0192(7) 0.0257(8) -0.0034(6) 0.0111(7) -0.0011(6) B1 0.0147(7) 0.0179(7) 0.0149(7) -0.0004(5) 0.0031(5) -0.0003(5) C38 0.0155(6) 0.0160(6) 0.0163(6) 0.0004(5) 0.0031(5) 0.0000(5) C39 0.0148(6) 0.0189(6) 0.0179(6) -0.0017(5) 0.0033(5) -0.0012(5) C40 0.0168(6) 0.0180(6) 0.0193(6) -0.0024(5) 0.0058(5) -0.0012(5) C41 0.0160(6) 0.0195(7) 0.0232(7) -0.0014(6) 0.0054(5) -0.0006(5) C42 0.0149(6) 0.0172(6) 0.0202(7) -0.0004(5) 0.0006(5) -0.0008(5) C43 0.0166(6) 0.0187(6) 0.0169(6) -0.0005(5) 0.0022(5) 0.0005(5) C44 0.0187(7) 0.0253(8) 0.0246(7) -0.0066(6) 0.0084(6) -0.0039(6) F44A 0.0425(7) 0.0402(6) 0.0200(5) -0.0012(4) 0.0067(5) 0.0039(5) F44B 0.0677(9) 0.0202(5) 0.0336(6) -0.0085(4) 0.0195(6) -0.0071(5) F44C 0.0218(5) 0.0740(10) 0.0386(7) -0.0255(6) 0.0155(5) -0.0078(6) C45 0.0181(7) 0.0252(8) 0.0253(8) -0.0039(6) 0.0001(6) 0.0000(6) F45A 0.0446(7) 0.0482(8) 0.0505(8) 0.0077(6) -0.0126(6) -0.0281(6) F45B 0.0280(6) 0.0616(8) 0.0246(5) -0.0100(5) -0.0036(4) 0.0041(5) F45C 0.0276(6) 0.0485(8) 0.0480(7) -0.0158(6) -0.0133(5) 0.0175(5) C46 0.0144(6) 0.0142(6) 0.0159(6) -0.0014(5) 0.0036(5) -0.0001(5) C47 0.0160(6) 0.0176(6) 0.0175(6) -0.0017(5) 0.0054(5) -0.0001(5) C48 0.0140(6) 0.0205(7) 0.0192(6) -0.0029(5) 0.0034(5) 0.0008(5) C49 0.0182(6) 0.0203(7) 0.0189(6) -0.0010(5) 0.0011(5) 0.0037(5) C50 0.0215(7) 0.0166(6) 0.0184(6) 0.0008(5) 0.0042(5) 0.0009(5) C51 0.0165(6) 0.0157(6) 0.0193(6) -0.0001(5) 0.0038(5) -0.0015(5) C52 0.0155(7) 0.0339(9) 0.0239(7) -0.0028(7) 0.0039(6) 0.0000(6) F52A 0.0225(6) 0.1067(13) 0.0301(6) -0.0032(7) 0.0114(5) -0.0168(7) F52B 0.0283(6) 0.0536(9) 0.0970(13) -0.0378(9) 0.0220(7) -0.0196(6) F52C 0.0168(5) 0.0737(10) 0.0695(10) 0.0278(8) -0.0025(6) 0.0052(6) C53 0.0301(8) 0.0211(7) 0.0250(8) 0.0051(6) 0.0048(6) -0.0008(6) F53A 0.0686(9) 0.0181(5) 0.0477(7) 0.0041(5) 0.0200(7) -0.0077(5) F53B 0.0431(7) 0.0412(7) 0.0461(7) 0.0178(6) 0.0265(6) 0.0058(5) F53C 0.0489(8) 0.0598(9) 0.0320(6) 0.0261(6) -0.0070(6) -0.0129(7) C54 0.0139(6) 0.0177(6) 0.0154(6) 0.0004(5) 0.0019(5) 0.0000(5) C55 0.0179(6) 0.0171(6) 0.0189(6) -0.0004(5) 0.0046(5) -0.0006(5) C56 0.0200(7) 0.0202(7) 0.0182(6) -0.0007(5) 0.0073(5) -0.0008(5) C57 0.0233(7) 0.0192(7) 0.0203(7) -0.0038(5) 0.0060(6) 0.0006(6) C58 0.0185(7) 0.0176(7) 0.0202(7) -0.0013(5) 0.0028(5) -0.0020(5) C59 0.0173(6) 0.0182(6) 0.0181(6) 0.0004(5) 0.0039(5) -0.0015(5) C60 0.0313(9) 0.0261(8) 0.0266(8) -0.0025(7) 0.0150(7) -0.0013(7) F60A 0.0214(5) 0.0455(7) 0.0399(6) 0.0119(5) 0.0100(5) -0.0028(5) F60B 0.0332(6) 0.0805(11) 0.0371(7) 0.0343(7) 0.0084(5) -0.0008(7) F60C 0.1039(14) 0.0450(8) 0.0976(13) -0.0360(8) 0.0864(12) -0.0296(9) C61 0.0269(8) 0.0201(7) 0.0287(8) -0.0022(6) 0.0045(6) -0.0041(6) F61A 0.0325(6) 0.0305(6) 0.0755(10) 0.0009(6) 0.0178(6) -0.0116(5) F61B 0.0586(9) 0.0253(6) 0.1010(13) 0.0263(7) -0.0378(9) -0.0106(6) F61C 0.0972(13) 0.0414(8) 0.0540(9) -0.0270(7) 0.0377(9) -0.0372(8) C62 0.0151(6) 0.0178(6) 0.0170(6) 0.0005(5) 0.0054(5) 0.0008(5) C63 0.0204(7) 0.0204(7) 0.0176(6) 0.0002(5) 0.0037(5) 0.0032(5) C64 0.0257(8) 0.0227(7) 0.0171(7) 0.0039(6) 0.0061(6) 0.0054(6) C65 0.0363(9) 0.0170(7) 0.0210(7) 0.0032(6) 0.0101(6) 0.0027(6) C67 0.0244(7) 0.0174(7) 0.0161(6) 0.0008(5) 0.0060(5) 0.0001(5) C68 0.0441(11) 0.0285(9) 0.0190(7) 0.0044(6) 0.0069(7) 0.0055(8) F68A 0.1100(13) 0.0283(6) 0.0257(6) 0.0122(5) 0.0096(7) 0.0066(7) F68B 0.0630(9) 0.0762(11) 0.0238(6) 0.0090(6) 0.0222(6) 0.0191(8) F68C 0.0588(9) 0.0627(9) 0.0242(6) 0.0126(6) -0.0099(6) -0.0098(7) C66A 0.0336(8) 0.0170(7) 0.0186(7) 0.0009(5) 0.0093(6) 0.0006(6) C69A 0.0481(14) 0.0175(8) 0.0220(8) 0.0004(6) 0.0094(8) 0.0000(8) F69A 0.0626(10) 0.0730(11) 0.0404(8) -0.0281(8) 0.0232(7) 0.0045(8) F69B 0.0465(8) 0.0297(9) 0.0326(8) -0.0074(6) 0.0007(7) -0.0071(8) F69C 0.089(5) 0.012(2) 0.033(3) -0.0016(18) -0.005(3) -0.003(3) C66B 0.0336(8) 0.0170(7) 0.0186(7) 0.0009(5) 0.0093(6) 0.0006(6) C69B 0.0481(14) 0.0175(8) 0.0220(8) 0.0004(6) 0.0094(8) 0.0000(8) F69D 0.0626(10) 0.0730(11) 0.0404(8) -0.0281(8) 0.0232(7) 0.0045(8) F69E 0.0465(8) 0.0297(9) 0.0326(8) -0.0074(6) 0.0007(7) -0.0071(8) F69F 0.167(3) 0.0200(9) 0.0273(9) 0.0003(7) 0.0077(13) -0.0314(13) _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 N1 2.1160(13) . ? Ir1 C5 2.1291(15) . ? Ir1 C6 2.1449(16) . ? Ir1 C1 2.2241(16) . ? Ir1 C2 2.2364(15) . ? Ir1 P1 2.2886(4) . ? P1 C32 1.8131(16) . ? P1 C26 1.8163(15) . ? P1 C25 1.8461(17) . ? N1 C9 1.3510(19) . ? N1 N2 1.3706(18) . ? N2 C11 1.3657(19) . ? N2 C24 1.465(2) . ? C1 C2 1.392(2) . ? C1 C8 1.503(2) . ? C1 H1 0.95(2) . ? C2 C3 1.518(2) . ? C2 H2 0.94(2) . ? C3 C4 1.545(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.510(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.414(2) . ? C5 H5 0.96(2) . ? C6 C7 1.528(2) . ? C6 H6 0.93(2) . ? C7 C8 1.542(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.403(2) . ? C9 C12 1.472(2) . ? C10 C11 1.384(2) . ? C10 H10 0.9500 . ? C11 C18 1.471(2) . ? C12 C17 1.394(2) . ? C12 C13 1.396(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.384(3) . ? C14 H14 0.9500 . ? C15 C16 1.383(4) . ? C15 H15 0.9500 . ? C16 C17 1.392(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.398(2) . ? C18 C23 1.400(2) . ? C19 C20 1.390(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 C22 1.386(3) . ? C21 H21 0.9500 . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.536(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.392(2) . ? C26 C27 1.402(2) . ? C27 C28 1.386(2) . ? C27 H27 0.9500 . ? C28 C29 1.387(3) . ? C28 H28 0.9500 . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 C31 1.399(2) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.393(2) . ? C32 C33 1.401(2) . ? C33 C34 1.388(3) . ? C33 H33 0.9500 . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 C37 1.397(2) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? B1 C38 1.635(2) . ? B1 C46 1.638(2) . ? B1 C54 1.639(2) . ? B1 C62 1.647(2) . ? C38 C43 1.400(2) . ? C38 C39 1.406(2) . ? C39 C40 1.392(2) . ? C39 H39 0.9500 . ? C40 C41 1.387(2) . ? C40 C44 1.497(2) . ? C41 C42 1.395(2) . ? C41 H41 0.9500 . ? C42 C43 1.393(2) . ? C42 C45 1.494(2) . ? C43 H43 0.9500 . ? C44 F44C 1.3292(19) . ? C44 F44A 1.340(2) . ? C44 F44B 1.352(2) . ? C45 F45A 1.328(2) . ? C45 F45B 1.343(2) . ? C45 F45C 1.349(2) . ? C46 C47 1.401(2) . ? C46 C51 1.406(2) . ? C47 C48 1.393(2) . ? C47 H47 0.9500 . ? C48 C49 1.390(2) . ? C48 C52 1.500(2) . ? C49 C50 1.393(2) . ? C49 H49 0.9500 . ? C50 C51 1.394(2) . ? C50 C53 1.504(2) . ? C51 H51 0.9500 . ? C52 F52C 1.322(2) . ? C52 F52A 1.328(2) . ? C52 F52B 1.335(2) . ? C53 F53C 1.330(2) . ? C53 F53A 1.337(2) . ? C53 F53B 1.339(2) . ? C54 C55 1.402(2) . ? C54 C59 1.406(2) . ? C55 C56 1.393(2) . ? C55 H55 0.9500 . ? C56 C57 1.387(2) . ? C56 C60 1.499(2) . ? C57 C58 1.392(2) . ? C57 H57 0.9500 . ? C58 C59 1.395(2) . ? C58 C61 1.502(2) . ? C59 H59 0.9500 . ? C60 F60C 1.324(2) . ? C60 F60B 1.337(2) . ? C60 F60A 1.348(2) . ? C61 F61B 1.313(2) . ? C61 F61C 1.336(2) . ? C61 F61A 1.339(2) . ? C62 C67 1.402(2) . ? C62 C63 1.405(2) . ? C63 C64 1.397(2) . ? C63 H63 0.9500 . ? C64 C65 1.384(2) . ? C64 C68 1.498(2) . ? C65 C66A 1.392(2) . ? C65 H65 0.9500 . ? C67 C66A 1.394(2) . ? C67 H67 0.9500 . ? C68 F68C 1.329(3) . ? C68 F68A 1.338(2) . ? C68 F68B 1.343(2) . ? C66A C69A 1.499(2) . ? C69A F69C 1.3330 . ? C69A F69B 1.3334 . ? C69A F69A 1.3344 . ? C69B F69F 1.3327 . ? C69B F69D 1.3340 . ? C69B F69E 1.3342 . ? 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 Ir1 C5 166.15(6) . . ? N1 Ir1 C6 155.20(6) . . ? C5 Ir1 C6 38.63(6) . . ? N1 Ir1 C1 88.73(6) . . ? C5 Ir1 C1 96.70(6) . . ? C6 Ir1 C1 80.24(6) . . ? N1 Ir1 C2 96.58(5) . . ? C5 Ir1 C2 80.72(6) . . ? C6 Ir1 C2 87.66(6) . . ? C1 Ir1 C2 36.38(6) . . ? N1 Ir1 P1 86.72(4) . . ? C5 Ir1 P1 92.68(4) . . ? C6 Ir1 P1 95.31(4) . . ? C1 Ir1 P1 158.21(4) . . ? C2 Ir1 P1 165.41(4) . . ? C32 P1 C26 103.57(7) . . ? C32 P1 C25 105.53(8) . . ? C26 P1 C25 105.28(8) . . ? C32 P1 Ir1 116.83(6) . . ? C26 P1 Ir1 117.49(5) . . ? C25 P1 Ir1 107.01(5) . . ? C9 N1 N2 106.29(12) . . ? C9 N1 Ir1 134.35(11) . . ? N2 N1 Ir1 118.16(9) . . ? C11 N2 N1 110.74(12) . . ? C11 N2 C24 127.60(13) . . ? N1 N2 C24 119.72(12) . . ? C2 C1 C8 124.74(15) . . ? C2 C1 Ir1 72.29(9) . . ? C8 C1 Ir1 109.70(11) . . ? C2 C1 H1 119.8(13) . . ? C8 C1 H1 113.1(13) . . ? Ir1 C1 H1 104.3(13) . . ? C1 C2 C3 124.10(15) . . ? C1 C2 Ir1 71.33(9) . . ? C3 C2 Ir1 111.50(10) . . ? C1 C2 H2 116.9(13) . . ? C3 C2 H2 116.4(13) . . ? Ir1 C2 H2 103.0(13) . . ? C2 C3 C4 112.26(14) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 113.12(13) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 124.71(15) . . ? C6 C5 Ir1 71.29(9) . . ? C4 C5 Ir1 111.02(11) . . ? C6 C5 H5 115.9(13) . . ? C4 C5 H5 114.5(13) . . ? Ir1 C5 H5 109.4(13) . . ? C5 C6 C7 124.51(15) . . ? C5 C6 Ir1 70.08(9) . . ? C7 C6 Ir1 114.57(11) . . ? C5 C6 H6 114.0(13) . . ? C7 C6 H6 115.7(13) . . ? Ir1 C6 H6 107.9(14) . . ? C6 C7 C8 112.61(14) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 113.04(14) . . ? C1 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C1 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C10 109.64(14) . . ? N1 C9 C12 122.64(14) . . ? C10 C9 C12 127.65(14) . . ? C11 C10 C9 106.51(14) . . ? C11 C10 H10 126.7 . . ? C9 C10 H10 126.7 . . ? N2 C11 C10 106.79(14) . . ? N2 C11 C18 123.91(14) . . ? C10 C11 C18 129.30(14) . . ? C17 C12 C13 118.91(17) . . ? C17 C12 C9 119.99(16) . . ? C13 C12 C9 121.09(15) . . ? C14 C13 C12 120.71(18) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 119.85(19) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 120.0(2) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C19 C18 C23 118.80(16) . . ? C19 C18 C11 122.26(15) . . ? C23 C18 C11 118.87(15) . . ? C20 C19 C18 120.42(17) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.29(18) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 119.66(18) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.40(18) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 120.41(17) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? N2 C24 C25 111.00(13) . . ? N2 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? N2 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 P1 111.94(11) . . ? C24 C25 H25A 109.2 . . ? P1 C25 H25A 109.2 . . ? C24 C25 H25B 109.2 . . ? P1 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C31 C26 C27 119.64(15) . . ? C31 C26 P1 121.78(12) . . ? C27 C26 P1 118.38(12) . . ? C28 C27 C26 120.18(17) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.06(18) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.28(16) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C31 120.07(18) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C26 C31 C30 119.76(17) . . ? C26 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C37 C32 C33 119.53(16) . . ? C37 C32 P1 119.80(13) . . ? C33 C32 P1 120.58(14) . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.34(18) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.0(2) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C32 C37 C36 120.03(18) . . ? C32 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C38 B1 C46 111.27(12) . . ? C38 B1 C54 114.67(12) . . ? C46 B1 C54 103.10(12) . . ? C38 B1 C62 103.01(12) . . ? C46 B1 C62 112.40(12) . . ? C54 B1 C62 112.72(12) . . ? C43 C38 C39 116.05(13) . . ? C43 C38 B1 123.96(13) . . ? C39 C38 B1 119.55(13) . . ? C40 C39 C38 122.38(14) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C41 C40 C39 120.64(14) . . ? C41 C40 C44 120.59(14) . . ? C39 C40 C44 118.75(14) . . ? C40 C41 C42 117.99(14) . . ? C40 C41 H41 121.0 . . ? C42 C41 H41 121.0 . . ? C43 C42 C41 121.21(14) . . ? C43 C42 C45 121.09(14) . . ? C41 C42 C45 117.69(14) . . ? C42 C43 C38 121.74(14) . . ? C42 C43 H43 119.1 . . ? C38 C43 H43 119.1 . . ? F44C C44 F44A 105.97(14) . . ? F44C C44 F44B 107.72(14) . . ? F44A C44 F44B 104.62(14) . . ? F44C C44 C40 113.47(14) . . ? F44A C44 C40 113.14(14) . . ? F44B C44 C40 111.34(14) . . ? F45A C45 F45B 106.27(15) . . ? F45A C45 F45C 106.06(15) . . ? F45B C45 F45C 105.37(15) . . ? F45A C45 C42 112.75(15) . . ? F45B C45 C42 113.54(14) . . ? F45C C45 C42 112.24(14) . . ? C47 C46 C51 115.81(13) . . ? C47 C46 B1 120.69(13) . . ? C51 C46 B1 123.15(13) . . ? C48 C47 C46 122.12(14) . . ? C48 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C49 C48 C47 121.34(14) . . ? C49 C48 C52 120.26(14) . . ? C47 C48 C52 118.37(14) . . ? C48 C49 C50 117.51(14) . . ? C48 C49 H49 121.2 . . ? C50 C49 H49 121.2 . . ? C49 C50 C51 121.09(14) . . ? C49 C50 C53 119.89(15) . . ? C51 C50 C53 118.97(14) . . ? C50 C51 C46 122.12(14) . . ? C50 C51 H51 118.9 . . ? C46 C51 H51 118.9 . . ? F52C C52 F52A 106.94(15) . . ? F52C C52 F52B 106.03(16) . . ? F52A C52 F52B 105.95(17) . . ? F52C C52 C48 113.37(15) . . ? F52A C52 C48 112.01(14) . . ? F52B C52 C48 112.04(14) . . ? F53C C53 F53A 106.81(15) . . ? F53C C53 F53B 106.58(16) . . ? F53A C53 F53B 106.20(15) . . ? F53C C53 C50 113.12(15) . . ? F53A C53 C50 111.47(15) . . ? F53B C53 C50 112.22(14) . . ? C55 C54 C59 115.76(13) . . ? C55 C54 B1 121.65(13) . . ? C59 C54 B1 122.02(13) . . ? C56 C55 C54 122.25(14) . . ? C56 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C57 C56 C55 121.14(14) . . ? C57 C56 C60 120.81(14) . . ? C55 C56 C60 118.05(14) . . ? C56 C57 C58 117.70(14) . . ? C56 C57 H57 121.1 . . ? C58 C57 H57 121.2 . . ? C57 C58 C59 121.16(14) . . ? C57 C58 C61 119.17(14) . . ? C59 C58 C61 119.61(14) . . ? C58 C59 C54 121.96(14) . . ? C58 C59 H59 119.0 . . ? C54 C59 H59 119.0 . . ? F60C C60 F60B 108.05(17) . . ? F60C C60 F60A 105.57(16) . . ? F60B C60 F60A 103.86(15) . . ? F60C C60 C56 113.49(15) . . ? F60B C60 C56 112.66(15) . . ? F60A C60 C56 112.52(14) . . ? F61B C61 F61C 108.26(18) . . ? F61B C61 F61A 105.82(17) . . ? F61C C61 F61A 104.01(16) . . ? F61B C61 C58 112.85(15) . . ? F61C C61 C58 112.70(15) . . ? F61A C61 C58 112.60(14) . . ? C67 C62 C63 115.53(14) . . ? C67 C62 B1 121.63(13) . . ? C63 C62 B1 122.45(13) . . ? C64 C63 C62 121.98(15) . . ? C64 C63 H63 119.0 . . ? C62 C63 H63 119.0 . . ? C65 C64 C63 121.34(15) . . ? C65 C64 C68 120.43(15) . . ? C63 C64 C68 118.13(15) . . ? C64 C65 C66A 117.71(15) . . ? C64 C65 H65 121.1 . . ? C66A C65 H65 121.1 . . ? C66A C67 C62 122.55(14) . . ? C66A C67 H67 118.7 . . ? C62 C67 H67 118.7 . . ? F68C C68 F68A 105.78(17) . . ? F68C C68 F68B 106.16(17) . . ? F68A C68 F68B 105.98(17) . . ? F68C C68 C64 113.26(16) . . ? F68A C68 C64 113.51(16) . . ? F68B C68 C64 111.55(16) . . ? C65 C66A C67 120.82(15) . . ? C65 C66A C69A 118.28(19) . . ? C67 C66A C69A 120.38(18) . . ? F69C C69A F69B 109.3 . . ? F69C C69A F69A 96.4 . . ? F69B C69A F69A 111.5 . . ? F69C C69A C66A 113.23(15) . . ? F69B C69A C66A 107.76(18) . . ? F69A C69A C66A 118.18(17) . . ? F69F C69B F69D 109.4 . . ? F69F C69B F69E 106.3 . . ? F69D C69B F69E 102.4 . . ? 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 Ir1 P1 C32 -84.40(7) . . . . ? C5 Ir1 P1 C32 81.75(7) . . . . ? C6 Ir1 P1 C32 120.38(7) . . . . ? C1 Ir1 P1 C32 -162.68(13) . . . . ? C2 Ir1 P1 C32 19.18(18) . . . . ? N1 Ir1 P1 C26 151.57(7) . . . . ? C5 Ir1 P1 C26 -42.28(8) . . . . ? C6 Ir1 P1 C26 -3.65(8) . . . . ? C1 Ir1 P1 C26 73.29(14) . . . . ? C2 Ir1 P1 C26 -104.85(18) . . . . ? N1 Ir1 P1 C25 33.55(7) . . . . ? C5 Ir1 P1 C25 -160.31(8) . . . . ? C6 Ir1 P1 C25 -121.67(8) . . . . ? C1 Ir1 P1 C25 -44.73(14) . . . . ? C2 Ir1 P1 C25 137.13(18) . . . . ? C5 Ir1 N1 C9 43.4(3) . . . . ? C6 Ir1 N1 C9 -133.21(16) . . . . ? C1 Ir1 N1 C9 -70.08(15) . . . . ? C2 Ir1 N1 C9 -34.49(16) . . . . ? P1 Ir1 N1 C9 131.24(15) . . . . ? C5 Ir1 N1 N2 -151.2(2) . . . . ? C6 Ir1 N1 N2 32.3(2) . . . . ? C1 Ir1 N1 N2 95.40(11) . . . . ? C2 Ir1 N1 N2 130.99(11) . . . . ? P1 Ir1 N1 N2 -63.28(10) . . . . ? C9 N1 N2 C11 1.45(17) . . . . ? Ir1 N1 N2 C11 -167.78(10) . . . . ? C9 N1 N2 C24 -163.89(14) . . . . ? Ir1 N1 N2 C24 26.88(18) . . . . ? N1 Ir1 C1 C2 102.89(10) . . . . ? C5 Ir1 C1 C2 -64.33(10) . . . . ? C6 Ir1 C1 C2 -99.42(10) . . . . ? P1 Ir1 C1 C2 -179.20(9) . . . . ? N1 Ir1 C1 C8 -135.71(12) . . . . ? C5 Ir1 C1 C8 57.07(12) . . . . ? C6 Ir1 C1 C8 21.98(12) . . . . ? C2 Ir1 C1 C8 121.40(16) . . . . ? P1 Ir1 C1 C8 -57.81(19) . . . . ? C8 C1 C2 C3 1.7(3) . . . . ? Ir1 C1 C2 C3 103.79(15) . . . . ? C8 C1 C2 Ir1 -102.07(16) . . . . ? N1 Ir1 C2 C1 -78.81(10) . . . . ? C5 Ir1 C2 C1 114.90(11) . . . . ? C6 Ir1 C2 C1 76.67(10) . . . . ? P1 Ir1 C2 C1 178.82(14) . . . . ? N1 Ir1 C2 C3 161.00(12) . . . . ? C5 Ir1 C2 C3 -5.29(12) . . . . ? C6 Ir1 C2 C3 -43.52(12) . . . . ? C1 Ir1 C2 C3 -120.19(16) . . . . ? P1 Ir1 C2 C3 58.6(2) . . . . ? C1 C2 C3 C4 -94.55(19) . . . . ? Ir1 C2 C3 C4 -13.11(18) . . . . ? C2 C3 C4 C5 33.3(2) . . . . ? C3 C4 C5 C6 43.6(2) . . . . ? C3 C4 C5 Ir1 -37.63(18) . . . . ? N1 Ir1 C5 C6 -177.7(2) . . . . ? C1 Ir1 C5 C6 -65.15(10) . . . . ? C2 Ir1 C5 C6 -97.95(10) . . . . ? P1 Ir1 C5 C6 95.15(9) . . . . ? N1 Ir1 C5 C4 -56.8(3) . . . . ? C6 Ir1 C5 C4 120.93(16) . . . . ? C1 Ir1 C5 C4 55.78(12) . . . . ? C2 Ir1 C5 C4 22.98(12) . . . . ? P1 Ir1 C5 C4 -143.92(11) . . . . ? C4 C5 C6 C7 3.7(3) . . . . ? Ir1 C5 C6 C7 106.71(15) . . . . ? C4 C5 C6 Ir1 -103.06(15) . . . . ? N1 Ir1 C6 C5 178.69(12) . . . . ? C1 Ir1 C6 C5 113.87(10) . . . . ? C2 Ir1 C6 C5 78.03(10) . . . . ? P1 Ir1 C6 C5 -87.65(9) . . . . ? N1 Ir1 C6 C7 58.89(19) . . . . ? C5 Ir1 C6 C7 -119.79(16) . . . . ? C1 Ir1 C6 C7 -5.92(12) . . . . ? C2 Ir1 C6 C7 -41.76(12) . . . . ? P1 Ir1 C6 C7 152.56(11) . . . . ? C5 C6 C7 C8 -93.0(2) . . . . ? Ir1 C6 C7 C8 -11.03(18) . . . . ? C2 C1 C8 C7 47.1(2) . . . . ? Ir1 C1 C8 C7 -34.56(17) . . . . ? C6 C7 C8 C1 30.5(2) . . . . ? N2 N1 C9 C10 -1.69(17) . . . . ? Ir1 N1 C9 C10 164.99(12) . . . . ? N2 N1 C9 C12 175.53(14) . . . . ? Ir1 N1 C9 C12 -17.8(2) . . . . ? N1 C9 C10 C11 1.33(19) . . . . ? C12 C9 C10 C11 -175.72(16) . . . . ? N1 N2 C11 C10 -0.64(17) . . . . ? C24 N2 C11 C10 163.26(15) . . . . ? N1 N2 C11 C18 178.35(14) . . . . ? C24 N2 C11 C18 -17.8(2) . . . . ? C9 C10 C11 N2 -0.41(18) . . . . ? C9 C10 C11 C18 -179.33(16) . . . . ? N1 C9 C12 C17 153.86(17) . . . . ? C10 C9 C12 C17 -29.4(3) . . . . ? N1 C9 C12 C13 -27.3(2) . . . . ? C10 C9 C12 C13 149.39(18) . . . . ? C17 C12 C13 C14 -2.0(3) . . . . ? C9 C12 C13 C14 179.21(17) . . . . ? C12 C13 C14 C15 1.7(3) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C12 0.1(4) . . . . ? C13 C12 C17 C16 1.1(3) . . . . ? C9 C12 C17 C16 179.9(2) . . . . ? N2 C11 C18 C19 -41.5(2) . . . . ? C10 C11 C18 C19 137.29(19) . . . . ? N2 C11 C18 C23 141.78(17) . . . . ? C10 C11 C18 C23 -39.5(3) . . . . ? C23 C18 C19 C20 -1.5(3) . . . . ? C11 C18 C19 C20 -178.27(17) . . . . ? C18 C19 C20 C21 1.5(3) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? C20 C21 C22 C23 -0.8(3) . . . . ? C21 C22 C23 C18 0.7(3) . . . . ? C19 C18 C23 C22 0.4(3) . . . . ? C11 C18 C23 C22 177.28(17) . . . . ? C11 N2 C24 C25 -109.32(17) . . . . ? N1 N2 C24 C25 53.30(19) . . . . ? N2 C24 C25 P1 -74.59(15) . . . . ? C32 P1 C25 C24 143.43(11) . . . . ? C26 P1 C25 C24 -107.40(12) . . . . ? Ir1 P1 C25 C24 18.33(13) . . . . ? C32 P1 C26 C31 -25.53(15) . . . . ? C25 P1 C26 C31 -136.11(14) . . . . ? Ir1 P1 C26 C31 104.94(13) . . . . ? C32 P1 C26 C27 159.68(13) . . . . ? C25 P1 C26 C27 49.10(15) . . . . ? Ir1 P1 C26 C27 -69.85(14) . . . . ? C31 C26 C27 C28 -0.6(3) . . . . ? P1 C26 C27 C28 174.33(14) . . . . ? C26 C27 C28 C29 0.2(3) . . . . ? C27 C28 C29 C30 0.5(3) . . . . ? C28 C29 C30 C31 -0.8(3) . . . . ? C27 C26 C31 C30 0.3(3) . . . . ? P1 C26 C31 C30 -174.42(14) . . . . ? C29 C30 C31 C26 0.4(3) . . . . ? C26 P1 C32 C37 103.88(13) . . . . ? C25 P1 C32 C37 -145.73(13) . . . . ? Ir1 P1 C32 C37 -26.99(14) . . . . ? C26 P1 C32 C33 -72.69(14) . . . . ? C25 P1 C32 C33 37.70(15) . . . . ? Ir1 P1 C32 C33 156.45(11) . . . . ? C37 C32 C33 C34 1.7(3) . . . . ? P1 C32 C33 C34 178.25(14) . . . . ? C32 C33 C34 C35 -1.0(3) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C34 C35 C36 C37 1.0(3) . . . . ? C33 C32 C37 C36 -1.0(2) . . . . ? P1 C32 C37 C36 -177.63(13) . . . . ? C35 C36 C37 C32 -0.3(3) . . . . ? C46 B1 C38 C43 146.59(14) . . . . ? C54 B1 C38 C43 30.1(2) . . . . ? C62 B1 C38 C43 -92.77(16) . . . . ? C46 B1 C38 C39 -41.34(18) . . . . ? C54 B1 C38 C39 -157.86(13) . . . . ? C62 B1 C38 C39 79.29(16) . . . . ? C43 C38 C39 C40 -0.5(2) . . . . ? B1 C38 C39 C40 -173.21(14) . . . . ? C38 C39 C40 C41 0.5(2) . . . . ? C38 C39 C40 C44 178.70(15) . . . . ? C39 C40 C41 C42 0.0(2) . . . . ? C44 C40 C41 C42 -178.14(15) . . . . ? C40 C41 C42 C43 -0.5(2) . . . . ? C40 C41 C42 C45 -179.65(15) . . . . ? C41 C42 C43 C38 0.4(2) . . . . ? C45 C42 C43 C38 179.55(15) . . . . ? C39 C38 C43 C42 0.1(2) . . . . ? B1 C38 C43 C42 172.43(14) . . . . ? C41 C40 C44 F44C -13.8(2) . . . . ? C39 C40 C44 F44C 167.96(15) . . . . ? C41 C40 C44 F44A -134.59(16) . . . . ? C39 C40 C44 F44A 47.2(2) . . . . ? C41 C40 C44 F44B 107.92(17) . . . . ? C39 C40 C44 F44B -70.3(2) . . . . ? C43 C42 C45 F45A -106.11(19) . . . . ? C41 C42 C45 F45A 73.1(2) . . . . ? C43 C42 C45 F45B 14.8(2) . . . . ? C41 C42 C45 F45B -165.99(15) . . . . ? C43 C42 C45 F45C 134.19(16) . . . . ? C41 C42 C45 F45C -46.6(2) . . . . ? C38 B1 C46 C47 155.76(13) . . . . ? C54 B1 C46 C47 -80.84(16) . . . . ? C62 B1 C46 C47 40.82(18) . . . . ? C38 B1 C46 C51 -31.33(19) . . . . ? C54 B1 C46 C51 92.06(16) . . . . ? C62 B1 C46 C51 -146.28(14) . . . . ? C51 C46 C47 C48 0.7(2) . . . . ? B1 C46 C47 C48 174.07(14) . . . . ? C46 C47 C48 C49 0.3(2) . . . . ? C46 C47 C48 C52 178.45(14) . . . . ? C47 C48 C49 C50 -0.7(2) . . . . ? C52 C48 C49 C50 -178.76(14) . . . . ? C48 C49 C50 C51 0.0(2) . . . . ? C48 C49 C50 C53 -177.47(15) . . . . ? C49 C50 C51 C46 1.0(2) . . . . ? C53 C50 C51 C46 178.54(14) . . . . ? C47 C46 C51 C50 -1.3(2) . . . . ? B1 C46 C51 C50 -174.56(14) . . . . ? C49 C48 C52 F52C -21.2(2) . . . . ? C47 C48 C52 F52C 160.71(16) . . . . ? C49 C48 C52 F52A -142.29(17) . . . . ? C47 C48 C52 F52A 39.6(2) . . . . ? C49 C48 C52 F52B 98.8(2) . . . . ? C47 C48 C52 F52B -79.3(2) . . . . ? C49 C50 C53 F53C -18.6(2) . . . . ? C51 C50 C53 F53C 163.86(16) . . . . ? C49 C50 C53 F53A 101.78(18) . . . . ? C51 C50 C53 F53A -75.8(2) . . . . ? C49 C50 C53 F53B -139.24(16) . . . . ? C51 C50 C53 F53B 43.2(2) . . . . ? C38 B1 C54 C55 -147.46(14) . . . . ? C46 B1 C54 C55 91.41(16) . . . . ? C62 B1 C54 C55 -30.02(19) . . . . ? C38 B1 C54 C59 41.61(19) . . . . ? C46 B1 C54 C59 -79.51(16) . . . . ? C62 B1 C54 C59 159.05(13) . . . . ? C59 C54 C55 C56 -2.0(2) . . . . ? B1 C54 C55 C56 -173.48(14) . . . . ? C54 C55 C56 C57 1.7(2) . . . . ? C54 C55 C56 C60 -178.67(15) . . . . ? C55 C56 C57 C58 -0.1(2) . . . . ? C60 C56 C57 C58 -179.72(16) . . . . ? C56 C57 C58 C59 -1.1(2) . . . . ? C56 C57 C58 C61 176.07(15) . . . . ? C57 C58 C59 C54 0.6(2) . . . . ? C61 C58 C59 C54 -176.49(15) . . . . ? C55 C54 C59 C58 0.9(2) . . . . ? B1 C54 C59 C58 172.32(14) . . . . ? C57 C56 C60 F60C 8.5(3) . . . . ? C55 C56 C60 F60C -171.20(18) . . . . ? C57 C56 C60 F60B -114.73(19) . . . . ? C55 C56 C60 F60B 65.6(2) . . . . ? C57 C56 C60 F60A 128.27(17) . . . . ? C55 C56 C60 F60A -51.4(2) . . . . ? C57 C58 C61 F61B -92.8(2) . . . . ? C59 C58 C61 F61B 84.3(2) . . . . ? C57 C58 C61 F61C 30.2(2) . . . . ? C59 C58 C61 F61C -152.65(17) . . . . ? C57 C58 C61 F61A 147.46(16) . . . . ? C59 C58 C61 F61A -35.4(2) . . . . ? C38 B1 C62 C67 -82.45(16) . . . . ? C46 B1 C62 C67 37.41(19) . . . . ? C54 B1 C62 C67 153.41(14) . . . . ? C38 B1 C62 C63 90.18(16) . . . . ? C46 B1 C62 C63 -149.96(14) . . . . ? C54 B1 C62 C63 -33.96(19) . . . . ? C67 C62 C63 C64 -2.2(2) . . . . ? B1 C62 C63 C64 -175.28(14) . . . . ? C62 C63 C64 C65 2.2(3) . . . . ? C62 C63 C64 C68 -174.15(15) . . . . ? C63 C64 C65 C66A 0.0(3) . . . . ? C68 C64 C65 C66A 176.20(17) . . . . ? C63 C62 C67 C66A 0.3(2) . . . . ? B1 C62 C67 C66A 173.42(15) . . . . ? C65 C64 C68 F68C 134.76(19) . . . . ? C63 C64 C68 F68C -48.9(2) . . . . ? C65 C64 C68 F68A 14.1(3) . . . . ? C63 C64 C68 F68A -169.54(17) . . . . ? C65 C64 C68 F68B -105.5(2) . . . . ? C63 C64 C68 F68B 70.8(2) . . . . ? C64 C65 C66A C67 -1.9(3) . . . . ? C64 C65 C66A C69A 169.9(2) . . . . ? C62 C67 C66A C65 1.8(3) . . . . ? C62 C67 C66A C69A -169.9(2) . . . . ? C65 C66A C69A F69C -13.1(2) . . . . ? C67 C66A C69A F69C 158.79(13) . . . . ? C65 C66A C69A F69B 107.92(17) . . . . ? C67 C66A C69A F69B -80.23(19) . . . . ? C65 C66A C69A F69A -124.67(15) . . . . ? C67 C66A C69A F69A 47.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.195 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.079