# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.H.H.Ho ; School of Chemistry The University of New South Wales, Sydney, NSW 2052, Australia ; J.Wagler ; Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland ; A.Willis ; Research School of Chemistry Australian National University, Canberra, A. C. T. 0200, Australia ; B.Messerle ; School of Chemistry The University of New South Wales, Sydney, NSW 2052, Australia ; #TrackingRef '- NEW all-in-one CIFs.cif' # 1. SUBMISSION DETAILS _publ_contact_author ;Wagler, J\"org Institut f\"ur Anorganische Chemie Technische Universit\"at Bergakademie Freiberg Leipziger Str. 29 09596 Freiberg Bundesrepublik Deutschland and Messerle, Barbara A. School of Chemistry The University of New South Wales, Sydney, NSW 2052, Australia ; _publ_contact_author_fax 'JW: 03731 39-4058 ' _publ_contact_author_phone 'JW: 03731 39-3556 ' _publ_section_title ; Homo- and Heterobimetallic Rhodium(I) and/or Iridium(I) Complexes of Binucleating Bis(1-pyrazolyl)methane Ligands. Synthesis and Structures ; _publ_contact_author_name 'Wagler, Jorg' #===END data_compound1c _database_code_depnum_ccdc_archive 'CCDC 798119' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N8' _chemical_formula_sum 'C28 H22 N8' _chemical_formula_weight 470.54 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0732(3) _cell_length_b 23.3283(5) _cell_length_c 10.6167(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.0660(10) _cell_angle_gamma 90.00 _cell_volume 2312.08(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 32.63 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9245 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31238 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 32.00 _reflns_number_total 8008 _reflns_number_gt 5913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/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^)+(0.0718P)^2^+0.1640P] 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 8008 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 N1 N 0.46983(9) 0.13868(4) 0.78163(9) 0.01926(18) Uani 1 1 d . . . N2 N 0.59733(9) 0.11357(4) 0.85268(8) 0.01687(17) Uani 1 1 d . . . N3 N 0.92022(10) 0.06517(4) 0.93709(9) 0.01990(18) Uani 1 1 d . . . N4 N 0.83904(9) 0.10912(4) 0.86457(9) 0.01618(17) Uani 1 1 d . . . N5 N 0.78476(10) 0.22340(4) 0.52595(9) 0.01983(18) Uani 1 1 d . . . N6 N 0.80734(9) 0.18893(3) 0.43287(8) 0.01512(16) Uani 1 1 d . . . N7 N 1.18225(10) 0.18957(4) 0.53016(10) 0.02196(19) Uani 1 1 d . . . N8 N 1.04669(9) 0.18890(4) 0.43634(8) 0.01652(17) Uani 1 1 d . . . C1 C 0.40120(12) 0.13850(5) 0.86658(12) 0.0234(2) Uani 1 1 d . . . H1 H 0.3078 0.1537 0.8453 0.028 Uiso 1 1 calc R . . C2 C 0.48267(13) 0.11333(5) 0.99104(12) 0.0261(2) Uani 1 1 d . . . H2 H 0.4566 0.1083 1.0675 0.031 Uiso 1 1 calc R . . C3 C 0.60910(12) 0.09733(5) 0.97905(11) 0.0228(2) Uani 1 1 d . . . H3 H 0.6884 0.0787 1.0457 0.027 Uiso 1 1 calc R . . C4 C 1.04790(12) 0.08870(5) 1.00320(11) 0.0230(2) Uani 1 1 d . . . H4 H 1.1285 0.0683 1.0633 0.028 Uiso 1 1 calc R . . C5 C 1.04917(13) 0.14727(5) 0.97343(13) 0.0278(2) Uani 1 1 d . . . H5 H 1.1273 0.1732 1.0078 0.033 Uiso 1 1 calc R . . C6 C 0.91321(12) 0.15889(5) 0.88407(12) 0.0252(2) Uani 1 1 d . . . H6 H 0.8778 0.1949 0.8436 0.030 Uiso 1 1 calc R . . C7 C 0.68954(11) 0.10042(4) 0.77873(10) 0.01562(18) Uani 1 1 d . . . H7 H 0.6657 0.1284 0.7020 0.019 Uiso 1 1 calc R . . C8 C 0.65548(12) 0.24581(5) 0.45931(12) 0.0233(2) Uani 1 1 d . . . H8 H 0.6097 0.2721 0.4982 0.028 Uiso 1 1 calc R . . C9 C 0.59527(12) 0.22597(5) 0.32520(12) 0.0244(2) Uani 1 1 d . . . H9 H 0.5046 0.2357 0.2583 0.029 Uiso 1 1 calc R . . C10 C 0.69558(11) 0.18942(5) 0.31150(10) 0.0198(2) Uani 1 1 d . . . H10 H 0.6882 0.1685 0.2324 0.024 Uiso 1 1 calc R . . C11 C 1.25813(13) 0.21466(5) 0.46608(13) 0.0271(2) Uani 1 1 d . . . H11 H 1.3583 0.2215 0.5062 0.033 Uiso 1 1 calc R . . C12 C 1.17188(13) 0.22969(5) 0.33196(13) 0.0262(2) Uani 1 1 d . . . H12 H 1.2011 0.2479 0.2666 0.031 Uiso 1 1 calc R . . C13 C 1.03621(12) 0.21233(5) 0.31589(11) 0.0202(2) Uani 1 1 d . . . H13 H 0.9519 0.2160 0.2364 0.024 Uiso 1 1 calc R . . C14 C 0.93988(10) 0.15659(4) 0.46872(10) 0.01487(18) Uani 1 1 d . . . H14 H 0.9784 0.1513 0.5696 0.018 Uiso 1 1 calc R . . C15 C 0.66459(10) 0.04093(4) 0.71680(10) 0.01560(19) Uani 1 1 d . . . C16 C 0.59016(11) 0.00003(4) 0.75564(10) 0.0186(2) Uani 1 1 d . . . H16 H 0.5542 0.0088 0.8243 0.022 Uiso 1 1 calc R . . C17 C 0.56564(12) -0.05524(5) 0.69529(11) 0.0204(2) Uani 1 1 d . . . H17 H 0.5132 -0.0829 0.7234 0.024 Uiso 1 1 calc R . . C18 C 0.61674(11) -0.06881(4) 0.59754(11) 0.0194(2) Uani 1 1 d . . . H18 H 0.6020 -0.1062 0.5595 0.023 Uiso 1 1 calc R . . C19 C 0.69223(11) -0.02739(4) 0.55150(10) 0.01638(19) Uani 1 1 d . . . C20 C 0.73953(11) -0.04020(4) 0.44749(10) 0.01722(19) Uani 1 1 d . . . H20 H 0.7237 -0.0776 0.4091 0.021 Uiso 1 1 calc R . . C21 C 0.80960(11) 0.00029(4) 0.39785(10) 0.01604(19) Uani 1 1 d . . . C22 C 0.85932(11) -0.01376(4) 0.29251(10) 0.0189(2) Uani 1 1 d . . . H22 H 0.8414 -0.0509 0.2528 0.023 Uiso 1 1 calc R . . C23 C 0.93189(12) 0.02511(4) 0.24815(10) 0.0196(2) Uani 1 1 d . . . H23 H 0.9652 0.0150 0.1784 0.023 Uiso 1 1 calc R . . C24 C 0.95836(11) 0.08105(4) 0.30583(10) 0.01784(19) Uani 1 1 d . . . H24 H 1.0102 0.1078 0.2744 0.021 Uiso 1 1 calc R . . C25 C 0.91086(10) 0.09720(4) 0.40546(10) 0.01487(18) Uani 1 1 d . . . C26 C 0.83465(10) 0.05671(4) 0.45633(9) 0.01460(18) Uani 1 1 d . . . C27 C 0.78745(10) 0.06951(4) 0.56151(10) 0.01485(18) Uani 1 1 d . . . H27 H 0.8038 0.1068 0.6004 0.018 Uiso 1 1 calc R . . C28 C 0.71673(10) 0.02876(4) 0.61089(10) 0.01479(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0177(4) 0.0163(4) 0.0211(4) -0.0023(3) 0.0042(3) 0.0011(3) N2 0.0176(4) 0.0183(4) 0.0148(4) 0.0006(3) 0.0062(3) 0.0020(3) N3 0.0201(4) 0.0196(4) 0.0178(4) 0.0027(3) 0.0047(3) 0.0021(3) N4 0.0180(4) 0.0143(4) 0.0169(4) -0.0003(3) 0.0073(3) -0.0004(3) N5 0.0246(4) 0.0178(4) 0.0197(4) -0.0038(3) 0.0113(4) 0.0004(3) N6 0.0179(4) 0.0133(4) 0.0141(4) -0.0007(3) 0.0060(3) 0.0017(3) N7 0.0183(4) 0.0192(4) 0.0251(5) -0.0045(4) 0.0044(4) -0.0003(3) N8 0.0171(4) 0.0161(4) 0.0164(4) 0.0016(3) 0.0063(3) 0.0009(3) C1 0.0199(5) 0.0204(5) 0.0312(6) -0.0068(4) 0.0111(4) -0.0018(4) C2 0.0292(6) 0.0299(6) 0.0249(5) -0.0033(5) 0.0165(5) -0.0038(5) C3 0.0260(5) 0.0270(6) 0.0164(5) 0.0024(4) 0.0091(4) 0.0012(4) C4 0.0198(5) 0.0290(6) 0.0194(5) -0.0011(4) 0.0064(4) -0.0010(4) C5 0.0240(5) 0.0271(6) 0.0318(6) -0.0050(5) 0.0100(5) -0.0086(4) C6 0.0259(5) 0.0165(5) 0.0329(6) -0.0010(4) 0.0108(5) -0.0039(4) C7 0.0178(4) 0.0159(4) 0.0134(4) 0.0013(3) 0.0061(3) 0.0015(3) C8 0.0249(5) 0.0197(5) 0.0280(5) -0.0038(4) 0.0130(4) 0.0025(4) C9 0.0205(5) 0.0250(5) 0.0244(5) 0.0005(4) 0.0047(4) 0.0049(4) C10 0.0201(5) 0.0213(5) 0.0148(4) -0.0017(4) 0.0030(4) 0.0026(4) C11 0.0218(5) 0.0221(5) 0.0392(7) -0.0089(5) 0.0134(5) -0.0038(4) C12 0.0362(6) 0.0181(5) 0.0337(6) -0.0034(4) 0.0238(5) -0.0051(4) C13 0.0275(5) 0.0174(5) 0.0173(5) 0.0020(4) 0.0104(4) -0.0007(4) C14 0.0156(4) 0.0149(4) 0.0143(4) 0.0017(3) 0.0057(3) 0.0016(3) C15 0.0167(4) 0.0151(4) 0.0134(4) 0.0015(3) 0.0038(3) 0.0011(3) C16 0.0201(5) 0.0191(5) 0.0161(4) 0.0027(4) 0.0061(4) -0.0015(4) C17 0.0221(5) 0.0171(5) 0.0200(5) 0.0047(4) 0.0056(4) -0.0032(4) C18 0.0211(5) 0.0136(4) 0.0196(5) 0.0007(4) 0.0034(4) -0.0017(4) C19 0.0169(4) 0.0132(4) 0.0161(4) 0.0004(3) 0.0028(4) 0.0008(3) C20 0.0191(5) 0.0124(4) 0.0170(4) -0.0014(3) 0.0033(4) 0.0013(3) C21 0.0179(4) 0.0142(4) 0.0140(4) -0.0005(3) 0.0036(4) 0.0034(3) C22 0.0234(5) 0.0158(4) 0.0154(4) -0.0020(4) 0.0051(4) 0.0044(4) C23 0.0257(5) 0.0189(5) 0.0147(4) 0.0003(4) 0.0082(4) 0.0067(4) C24 0.0215(5) 0.0168(4) 0.0161(4) 0.0026(4) 0.0081(4) 0.0040(4) C25 0.0163(4) 0.0141(4) 0.0131(4) 0.0010(3) 0.0042(3) 0.0026(3) C26 0.0155(4) 0.0137(4) 0.0133(4) 0.0004(3) 0.0040(3) 0.0022(3) C27 0.0172(4) 0.0128(4) 0.0142(4) -0.0005(3) 0.0055(3) 0.0010(3) C28 0.0151(4) 0.0135(4) 0.0139(4) 0.0005(3) 0.0033(3) 0.0009(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 N1 C1 1.3265(14) . ? N1 N2 1.3541(12) . ? N2 C3 1.3558(13) . ? N2 C7 1.4564(13) . ? N3 C4 1.3303(14) . ? N3 N4 1.3563(12) . ? N4 C6 1.3538(14) . ? N4 C7 1.4520(13) . ? N5 C8 1.3333(14) . ? N5 N6 1.3580(12) . ? N6 C10 1.3557(13) . ? N6 C14 1.4541(12) . ? N7 C11 1.3343(15) . ? N7 N8 1.3547(12) . ? N8 C13 1.3579(13) . ? N8 C14 1.4566(13) . ? C1 C2 1.3963(17) . ? C1 H1 0.9500 . ? C2 C3 1.3781(16) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.4037(17) . ? C4 H4 0.9500 . ? C5 C6 1.3685(17) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C15 1.5159(14) . ? C7 H7 1.0000 . ? C8 C9 1.4002(16) . ? C8 H8 0.9500 . ? C9 C10 1.3709(15) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.4056(18) . ? C11 H11 0.9500 . ? C12 C13 1.3732(16) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C25 1.5195(14) . ? C14 H14 1.0000 . ? C15 C16 1.3691(14) . ? C15 C28 1.4368(14) . ? C16 C17 1.4195(15) . ? C16 H16 0.9500 . ? C17 C18 1.3578(16) . ? C17 H17 0.9500 . ? C18 C19 1.4249(14) . ? C18 H18 0.9500 . ? C19 C20 1.3895(15) . ? C19 C28 1.4344(14) . ? C20 C21 1.3954(14) . ? C20 H20 0.9500 . ? C21 C22 1.4247(14) . ? C21 C26 1.4367(13) . ? C22 C23 1.3555(16) . ? C22 H22 0.9500 . ? C23 C24 1.4236(15) . ? C23 H23 0.9500 . ? C24 C25 1.3675(14) . ? C24 H24 0.9500 . ? C25 C26 1.4438(14) . ? C26 C27 1.4004(14) . ? C27 C28 1.4024(14) . ? C27 H27 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 N2 104.33(9) . . ? N1 N2 C3 112.59(9) . . ? N1 N2 C7 117.03(8) . . ? C3 N2 C7 129.65(9) . . ? C4 N3 N4 104.18(9) . . ? C6 N4 N3 112.40(9) . . ? C6 N4 C7 126.77(9) . . ? N3 N4 C7 120.84(8) . . ? C8 N5 N6 104.08(8) . . ? C10 N6 N5 112.35(8) . . ? C10 N6 C14 127.31(8) . . ? N5 N6 C14 120.34(8) . . ? C11 N7 N8 104.03(9) . . ? N7 N8 C13 112.83(9) . . ? N7 N8 C14 117.54(8) . . ? C13 N8 C14 128.87(9) . . ? N1 C1 C2 111.93(10) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 105.16(10) . . ? C3 C2 H2 127.4 . . ? C1 C2 H2 127.4 . . ? N2 C3 C2 105.98(10) . . ? N2 C3 H3 127.0 . . ? C2 C3 H3 127.0 . . ? N3 C4 C5 111.81(10) . . ? N3 C4 H4 124.1 . . ? C5 C4 H4 124.1 . . ? C6 C5 C4 104.92(10) . . ? C6 C5 H5 127.5 . . ? C4 C5 H5 127.5 . . ? N4 C6 C5 106.70(10) . . ? N4 C6 H6 126.7 . . ? C5 C6 H6 126.7 . . ? N4 C7 N2 110.69(8) . . ? N4 C7 C15 111.35(8) . . ? N2 C7 C15 113.04(8) . . ? N4 C7 H7 107.1 . . ? N2 C7 H7 107.1 . . ? C15 C7 H7 107.1 . . ? N5 C8 C9 111.93(10) . . ? N5 C8 H8 124.0 . . ? C9 C8 H8 124.0 . . ? C10 C9 C8 104.99(10) . . ? C10 C9 H9 127.5 . . ? C8 C9 H9 127.5 . . ? N6 C10 C9 106.64(9) . . ? N6 C10 H10 126.7 . . ? C9 C10 H10 126.7 . . ? N7 C11 C12 111.81(10) . . ? N7 C11 H11 124.1 . . ? C12 C11 H11 124.1 . . ? C13 C12 C11 105.06(10) . . ? C13 C12 H12 127.5 . . ? C11 C12 H12 127.5 . . ? N8 C13 C12 106.26(10) . . ? N8 C13 H13 126.9 . . ? C12 C13 H13 126.9 . . ? N6 C14 N8 110.90(8) . . ? N6 C14 C25 110.61(8) . . ? N8 C14 C25 113.83(8) . . ? N6 C14 H14 107.0 . . ? N8 C14 H14 107.0 . . ? C25 C14 H14 107.0 . . ? C16 C15 C28 120.04(9) . . ? C16 C15 C7 121.85(9) . . ? C28 C15 C7 118.07(9) . . ? C15 C16 C17 121.27(10) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 120.35(10) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.56(10) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.88(9) . . ? C20 C19 C28 119.47(9) . . ? C18 C19 C28 119.63(9) . . ? C19 C20 C21 121.85(9) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 121.17(9) . . ? C20 C21 C26 119.24(9) . . ? C22 C21 C26 119.57(9) . . ? C23 C22 C21 120.89(9) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.14(10) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 121.45(10) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.93(9) . . ? C24 C25 C14 121.86(9) . . ? C26 C25 C14 118.18(8) . . ? C27 C26 C21 118.87(9) . . ? C27 C26 C25 123.11(9) . . ? C21 C26 C25 118.00(9) . . ? C26 C27 C28 121.73(9) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C27 C28 C19 118.84(9) . . ? C27 C28 C15 123.03(9) . . ? C19 C28 C15 118.12(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 C3 0.59(12) . . . . ? C1 N1 N2 C7 171.75(9) . . . . ? C4 N3 N4 C6 0.10(12) . . . . ? C4 N3 N4 C7 -179.40(9) . . . . ? C8 N5 N6 C10 -0.23(12) . . . . ? C8 N5 N6 C14 179.90(9) . . . . ? C11 N7 N8 C13 0.50(11) . . . . ? C11 N7 N8 C14 171.42(9) . . . . ? N2 N1 C1 C2 -0.33(12) . . . . ? N1 C1 C2 C3 -0.03(14) . . . . ? N1 N2 C3 C2 -0.62(13) . . . . ? C7 N2 C3 C2 -170.38(10) . . . . ? C1 C2 C3 N2 0.38(13) . . . . ? N4 N3 C4 C5 -0.10(12) . . . . ? N3 C4 C5 C6 0.07(14) . . . . ? N3 N4 C6 C5 -0.06(13) . . . . ? C7 N4 C6 C5 179.40(10) . . . . ? C4 C5 C6 N4 0.00(13) . . . . ? C6 N4 C7 N2 -86.37(12) . . . . ? N3 N4 C7 N2 93.05(10) . . . . ? C6 N4 C7 C15 146.99(10) . . . . ? N3 N4 C7 C15 -33.59(12) . . . . ? N1 N2 C7 N4 143.70(8) . . . . ? C3 N2 C7 N4 -46.91(14) . . . . ? N1 N2 C7 C15 -90.60(10) . . . . ? C3 N2 C7 C15 78.79(13) . . . . ? N6 N5 C8 C9 0.16(12) . . . . ? N5 C8 C9 C10 -0.04(14) . . . . ? N5 N6 C10 C9 0.21(12) . . . . ? C14 N6 C10 C9 -179.93(10) . . . . ? C8 C9 C10 N6 -0.10(13) . . . . ? N8 N7 C11 C12 -0.30(12) . . . . ? N7 C11 C12 C13 0.01(13) . . . . ? N7 N8 C13 C12 -0.50(12) . . . . ? C14 N8 C13 C12 -170.15(9) . . . . ? C11 C12 C13 N8 0.28(12) . . . . ? C10 N6 C14 N8 88.33(12) . . . . ? N5 N6 C14 N8 -91.82(10) . . . . ? C10 N6 C14 C25 -38.95(13) . . . . ? N5 N6 C14 C25 140.90(9) . . . . ? N7 N8 C14 N6 135.85(9) . . . . ? C13 N8 C14 N6 -54.91(13) . . . . ? N7 N8 C14 C25 -98.66(10) . . . . ? C13 N8 C14 C25 70.58(13) . . . . ? N4 C7 C15 C16 110.14(11) . . . . ? N2 C7 C15 C16 -15.20(13) . . . . ? N4 C7 C15 C28 -72.26(11) . . . . ? N2 C7 C15 C28 162.39(8) . . . . ? C28 C15 C16 C17 1.46(15) . . . . ? C7 C15 C16 C17 179.01(9) . . . . ? C15 C16 C17 C18 0.38(16) . . . . ? C16 C17 C18 C19 -1.71(16) . . . . ? C17 C18 C19 C20 -177.24(10) . . . . ? C17 C18 C19 C28 1.20(15) . . . . ? C18 C19 C20 C21 177.91(9) . . . . ? C28 C19 C20 C21 -0.54(15) . . . . ? C19 C20 C21 C22 179.07(9) . . . . ? C19 C20 C21 C26 0.46(15) . . . . ? C20 C21 C22 C23 -177.58(10) . . . . ? C26 C21 C22 C23 1.03(15) . . . . ? C21 C22 C23 C24 -0.59(15) . . . . ? C22 C23 C24 C25 -0.61(15) . . . . ? C23 C24 C25 C26 1.32(15) . . . . ? C23 C24 C25 C14 179.35(9) . . . . ? N6 C14 C25 C24 112.81(10) . . . . ? N8 C14 C25 C24 -12.84(13) . . . . ? N6 C14 C25 C26 -69.13(11) . . . . ? N8 C14 C25 C26 165.22(8) . . . . ? C20 C21 C26 C27 -0.19(14) . . . . ? C22 C21 C26 C27 -178.83(9) . . . . ? C20 C21 C26 C25 178.33(9) . . . . ? C22 C21 C26 C25 -0.31(13) . . . . ? C24 C25 C26 C27 177.61(9) . . . . ? C14 C25 C26 C27 -0.49(14) . . . . ? C24 C25 C26 C21 -0.85(14) . . . . ? C14 C25 C26 C21 -178.95(8) . . . . ? C21 C26 C27 C28 0.03(14) . . . . ? C25 C26 C27 C28 -178.41(9) . . . . ? C26 C27 C28 C19 -0.11(14) . . . . ? C26 C27 C28 C15 -178.75(9) . . . . ? C20 C19 C28 C27 0.36(14) . . . . ? C18 C19 C28 C27 -178.11(9) . . . . ? C20 C19 C28 C15 179.06(9) . . . . ? C18 C19 C28 C15 0.60(14) . . . . ? C16 C15 C28 C27 176.75(9) . . . . ? C7 C15 C28 C27 -0.89(14) . . . . ? C16 C15 C28 C19 -1.90(14) . . . . ? C7 C15 C28 C19 -179.54(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.438 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.055 #===END data_compound2a _database_code_depnum_ccdc_archive 'CCDC 798120' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 Ir N8, C32 H12 B F24 ' _chemical_formula_sum 'C68 H46 B F24 Ir N8' _chemical_formula_weight 1634.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 14.0601(4) _cell_length_b 14.2130(4) _cell_length_c 17.9485(5) _cell_angle_alpha 79.627(2) _cell_angle_beta 73.8860(10) _cell_angle_gamma 70.0460(10) _cell_volume 3224.48(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 32.57 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4435 _exptl_absorpt_correction_T_max 0.5444 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75016 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 32.00 _reflns_number_total 22118 _reflns_number_gt 18745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; One CF3 group (C68 F22 F23 F24) is disordered over two sites. The following restraints were used: sadi 0.001 c65 c68 c65 c68a sadi 0.001 c68 f22 c68 f23 c68 f24 c68a f22a c68a f23a c68a f24a and the C-atoms were refined with same anisotropic thermal displacement parameters (eadp c68 c68a). 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^)+(0.0322P)^2^+0.5568P] 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 22118 _refine_ls_number_parameters 961 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.909035(5) 0.929071(5) 0.739852(4) 0.01977(2) Uani 1 1 d . . . N1 N 0.85810(13) 0.93411(12) 0.86111(9) 0.0234(3) Uani 1 1 d . . . N2 N 0.81071(13) 0.86732(12) 0.90593(9) 0.0247(3) Uani 1 1 d . . . N3 N 0.77738(11) 0.88979(11) 0.74750(8) 0.0186(3) Uani 1 1 d . . . N4 N 0.73879(11) 0.83594(11) 0.81264(9) 0.0200(3) Uani 1 1 d . . . N5 N 0.53192(17) 0.59757(15) 0.68993(13) 0.0431(5) Uani 1 1 d . . . N6 N 0.56291(13) 0.54590(14) 0.75433(11) 0.0314(4) Uani 1 1 d . . . N7 N 0.57496(14) 0.63175(15) 0.90319(11) 0.0369(4) Uani 1 1 d . . . N8 N 0.63097(13) 0.55310(13) 0.85992(10) 0.0286(4) Uani 1 1 d . . . C1 C 0.98183(15) 0.86389(16) 0.63329(11) 0.0257(4) Uani 1 1 d . . . H1 H 0.9403(18) 0.8192(17) 0.6303(13) 0.031 Uiso 1 1 d . . . C2 C 0.93614(16) 0.96720(17) 0.61711(11) 0.0277(4) Uani 1 1 d . . . H2 H 0.8729(19) 0.9879(18) 0.6009(14) 0.033 Uiso 1 1 d . . . C3 C 0.99779(19) 1.04093(19) 0.58782(13) 0.0377(5) Uani 1 1 d . . . H3A H 0.9646 1.0936 0.5506 0.045 Uiso 1 1 calc R . . H3B H 1.0691 1.0053 0.5599 0.045 Uiso 1 1 calc R . . C4 C 1.0035(2) 1.0901(2) 0.65487(14) 0.0436(6) Uani 1 1 d . . . H4A H 1.0673 1.1106 0.6398 0.052 Uiso 1 1 calc R . . H4B H 0.9429 1.1514 0.6643 0.052 Uiso 1 1 calc R . . C5 C 1.00429(19) 1.02056(19) 0.72926(13) 0.0365(5) Uani 1 1 d . . . H5 H 0.981(2) 1.0624(19) 0.7753(15) 0.044 Uiso 1 1 d . . . C6 C 1.06520(18) 0.9193(2) 0.73503(14) 0.0375(5) Uani 1 1 d . . . H6 H 1.075(2) 0.890(2) 0.7848(16) 0.045 Uiso 1 1 d . . . C7 C 1.14404(18) 0.8655(2) 0.66711(15) 0.0476(6) Uani 1 1 d . . . H7A H 1.2029 0.8152 0.6863 0.057 Uiso 1 1 calc R . . H7B H 1.1718 0.9149 0.6289 0.057 Uiso 1 1 calc R . . C8 C 1.09668(17) 0.8126(2) 0.62647(14) 0.0408(5) Uani 1 1 d . . . H8A H 1.1330 0.8113 0.5707 0.049 Uiso 1 1 calc R . . H8B H 1.1078 0.7422 0.6498 0.049 Uiso 1 1 calc R . . C9 C 0.86506(18) 0.98921(16) 0.91119(12) 0.0321(4) Uani 1 1 d . . . H9 H 0.8936 1.0434 0.8967 0.039 Uiso 1 1 calc R . . C10 C 0.8247(2) 0.95635(18) 0.98721(12) 0.0403(5) Uani 1 1 d . . . H10 H 0.8213 0.9825 1.0334 0.048 Uiso 1 1 calc R . . C11 C 0.79096(18) 0.87868(17) 0.98213(11) 0.0348(5) Uani 1 1 d . . . H11 H 0.7595 0.8400 1.0244 0.042 Uiso 1 1 calc R . . C12 C 0.70250(14) 0.92397(14) 0.70797(11) 0.0229(4) Uani 1 1 d . . . H12 H 0.7076 0.9636 0.6592 0.027 Uiso 1 1 calc R . . C13 C 0.61613(15) 0.89363(15) 0.74792(13) 0.0297(4) Uani 1 1 d . . . H13 H 0.5529 0.9084 0.7324 0.036 Uiso 1 1 calc R . . C14 C 0.64147(14) 0.83813(14) 0.81425(12) 0.0275(4) Uani 1 1 d . . . H14 H 0.5985 0.8069 0.8541 0.033 Uiso 1 1 calc R . . C15 C 0.80051(14) 0.78812(13) 0.87013(11) 0.0226(4) Uani 1 1 d . . . H15 H 0.7603 0.7498 0.9116 0.027 Uiso 1 1 calc R . . C16 C 0.4690(2) 0.5522(2) 0.67854(18) 0.0524(7) Uani 1 1 d . . . H16 H 0.4343 0.5719 0.6371 0.063 Uiso 1 1 calc R . . C17 C 0.4605(2) 0.4727(3) 0.73441(18) 0.0625(9) Uani 1 1 d . . . H17 H 0.4198 0.4298 0.7387 0.075 Uiso 1 1 calc R . . C18 C 0.5230(2) 0.4689(2) 0.78234(16) 0.0527(7) Uani 1 1 d . . . H18 H 0.5356 0.4219 0.8261 0.063 Uiso 1 1 calc R . . C19 C 0.5784(2) 0.5922(2) 0.97522(14) 0.0469(6) Uani 1 1 d . . . H19 H 0.5453 0.6294 1.0194 0.056 Uiso 1 1 calc R . . C20 C 0.6352(2) 0.4910(2) 0.97980(15) 0.0473(6) Uani 1 1 d . . . H20 H 0.6482 0.4475 1.0252 0.057 Uiso 1 1 calc R . . C21 C 0.66842(18) 0.46809(18) 0.90413(14) 0.0370(5) Uani 1 1 d . . . H21 H 0.7099 0.4045 0.8862 0.044 Uiso 1 1 calc R . . C22 C 0.64415(15) 0.56875(15) 0.77617(12) 0.0264(4) Uani 1 1 d . . . H22 H 0.6358 0.6417 0.7603 0.032 Uiso 1 1 calc R . . C23 C 0.90661(14) 0.71453(13) 0.83791(11) 0.0228(4) Uani 1 1 d . . . C24 C 0.99429(16) 0.72163(15) 0.85248(13) 0.0302(4) Uani 1 1 d . . . H24 H 0.9875 0.7709 0.8847 0.036 Uiso 1 1 calc R . . C25 C 1.09469(17) 0.65795(16) 0.82106(15) 0.0370(5) Uani 1 1 d . . . H25 H 1.1541 0.6646 0.8324 0.044 Uiso 1 1 calc R . . C26 C 1.10618(16) 0.58721(16) 0.77473(14) 0.0328(4) Uani 1 1 d . . . H26 H 1.1740 0.5473 0.7513 0.039 Uiso 1 1 calc R . . C27 C 1.01758(15) 0.57233(14) 0.76101(12) 0.0262(4) Uani 1 1 d . . . C28 C 1.02814(15) 0.49583(14) 0.71781(12) 0.0277(4) Uani 1 1 d . . . H28 H 1.0960 0.4556 0.6947 0.033 Uiso 1 1 calc R . . C29 C 0.94303(15) 0.47632(14) 0.70733(11) 0.0258(4) Uani 1 1 d . . . C30 C 0.95509(17) 0.39966(16) 0.66047(13) 0.0330(5) Uani 1 1 d . . . H30 H 1.0229 0.3611 0.6357 0.040 Uiso 1 1 calc R . . C31 C 0.87107(18) 0.38144(16) 0.65106(13) 0.0343(5) Uani 1 1 d . . . H31 H 0.8802 0.3317 0.6186 0.041 Uiso 1 1 calc R . . C32 C 0.76879(16) 0.43643(15) 0.68961(12) 0.0301(4) Uani 1 1 d . . . H32 H 0.7106 0.4217 0.6833 0.036 Uiso 1 1 calc R . . C33 C 0.75312(15) 0.50969(14) 0.73528(11) 0.0253(4) Uani 1 1 d . . . C34 C 0.84044(14) 0.53407(13) 0.74416(11) 0.0225(4) Uani 1 1 d . . . C35 C 0.82939(14) 0.61248(13) 0.78668(11) 0.0222(3) Uani 1 1 d . . . H35 H 0.7615 0.6517 0.8106 0.027 Uiso 1 1 calc R . . C36 C 0.91494(14) 0.63457(13) 0.79482(10) 0.0215(3) Uani 1 1 d . . . F1 F 0.72618(11) 0.12890(11) 0.55081(9) 0.0483(4) Uani 1 1 d . . . F2 F 0.64222(11) 0.28505(12) 0.54151(10) 0.0578(4) Uani 1 1 d . . . F3 F 0.76379(12) 0.23030(14) 0.60378(11) 0.0667(5) Uani 1 1 d . . . F4 F 0.65713(18) 0.16996(17) 0.88267(13) 0.0937(7) Uani 1 1 d . . . F5 F 0.61075(16) 0.03921(13) 0.90335(10) 0.0720(6) Uani 1 1 d . . . F6 F 0.49822(16) 0.17806(17) 0.93475(10) 0.0899(8) Uani 1 1 d . . . F7 F 0.25619(9) 0.46572(8) 0.88820(7) 0.0282(2) Uani 1 1 d . . . F8 F 0.23509(17) 0.36361(13) 0.98872(9) 0.0651(5) Uani 1 1 d . . . F9 F 0.10622(12) 0.49015(13) 0.96525(10) 0.0645(5) Uani 1 1 d . . . F10 F -0.09149(12) 0.25086(15) 0.84085(10) 0.0639(5) Uani 1 1 d . . . F11 F -0.03625(12) 0.15227(13) 0.93291(12) 0.0635(5) Uani 1 1 d . . . F12 F -0.11981(11) 0.30496(14) 0.95053(11) 0.0717(6) Uani 1 1 d . . . F13 F 0.56417(13) -0.16031(18) 0.56311(12) 0.0905(7) Uani 1 1 d . . . F14 F 0.43705(15) -0.07909(11) 0.51279(8) 0.0583(5) Uani 1 1 d . . . F15 F 0.44430(16) -0.22401(11) 0.57170(8) 0.0620(5) Uani 1 1 d . . . F16 F 0.31856(16) -0.26351(11) 0.85096(9) 0.0659(5) Uani 1 1 d . . . F17 F 0.19524(11) -0.13221(12) 0.89199(8) 0.0504(4) Uani 1 1 d . . . F18 F 0.34427(13) -0.16326(12) 0.91339(8) 0.0544(4) Uani 1 1 d . . . F19 F 0.18695(15) 0.27994(13) 0.40090(8) 0.0592(5) Uani 1 1 d . . . F20 F 0.06234(11) 0.26830(14) 0.49937(10) 0.0622(5) Uani 1 1 d . . . F21 F 0.19744(13) 0.14412(10) 0.47449(9) 0.0486(4) Uani 1 1 d . . . C68 C 0.29732(17) 0.50054(16) 0.53503(16) 0.0343(6) Uani 0.70 1 d PD A 1 F22 F 0.2525(5) 0.5598(3) 0.4811(3) 0.0865(14) Uani 0.70 1 d PD A 1 F23 F 0.39726(19) 0.4905(2) 0.5138(2) 0.0664(8) Uani 0.70 1 d PD A 1 F24 F 0.2647(4) 0.5517(4) 0.5962(3) 0.0629(14) Uani 0.70 1 d PD A 1 C68A C 0.2789(5) 0.5083(2) 0.5373(4) 0.0343(6) Uani 0.30 1 d PD A 2 F22A F 0.2989(12) 0.5403(10) 0.5937(6) 0.088(5) Uani 0.30 1 d PD A 2 F23A F 0.1926(6) 0.5778(5) 0.5269(6) 0.079(3) Uani 0.30 1 d PD A 2 F24A F 0.3470(10) 0.5143(6) 0.4711(4) 0.090(3) Uani 0.30 1 d PD A 2 B1 B 0.31861(15) 0.17851(15) 0.71785(11) 0.0183(4) Uani 1 1 d . . . C37 C 0.43336(13) 0.17798(13) 0.72310(10) 0.0209(3) Uani 1 1 d . . . C38 C 0.50963(13) 0.19523(13) 0.65799(11) 0.0222(4) Uani 1 1 d . . . H38 H 0.4946 0.2084 0.6080 0.027 Uiso 1 1 calc R . . C39 C 0.60637(15) 0.19378(14) 0.66386(13) 0.0285(4) Uani 1 1 d . . . C40 C 0.63184(16) 0.17569(15) 0.73549(15) 0.0348(5) Uani 1 1 d . . . H40 H 0.6975 0.1764 0.7397 0.042 Uiso 1 1 calc R . . C41 C 0.55819(17) 0.15653(16) 0.80099(13) 0.0342(5) Uani 1 1 d . . . C42 C 0.46264(15) 0.15545(15) 0.79411(12) 0.0282(4) Uani 1 1 d . . . H42 H 0.4152 0.1387 0.8396 0.034 Uiso 1 1 calc R . . C43 C 0.68394(17) 0.21016(18) 0.59033(16) 0.0397(5) Uani 1 1 d . . . C44 C 0.5808(2) 0.1361(2) 0.87968(16) 0.0507(7) Uani 1 1 d . . . C45 C 0.22932(14) 0.23252(12) 0.79012(9) 0.0177(3) Uani 1 1 d . . . C46 C 0.24131(14) 0.30388(13) 0.82869(10) 0.0200(3) Uani 1 1 d . . . H46 H 0.3056 0.3183 0.8135 0.024 Uiso 1 1 calc R . . C47 C 0.16353(14) 0.35472(13) 0.88821(10) 0.0204(3) Uani 1 1 d . . . C48 C 0.06803(14) 0.33782(13) 0.91170(11) 0.0231(4) Uani 1 1 d . . . H48 H 0.0152 0.3717 0.9526 0.028 Uiso 1 1 calc R . . C49 C 0.05161(13) 0.26978(13) 0.87365(11) 0.0218(3) Uani 1 1 d . . . C50 C 0.12989(13) 0.21841(13) 0.81465(10) 0.0204(3) Uani 1 1 d . . . H50 H 0.1160 0.1723 0.7901 0.024 Uiso 1 1 calc R . . C51 C 0.18910(16) 0.41922(15) 0.93173(11) 0.0282(4) Uani 1 1 d . . . C52 C -0.04895(15) 0.24661(17) 0.89916(13) 0.0330(5) Uani 1 1 d . . . C53 C 0.33110(13) 0.05943(13) 0.71839(10) 0.0188(3) Uani 1 1 d . . . C54 C 0.38345(13) 0.00967(13) 0.65051(10) 0.0205(3) Uani 1 1 d . . . H54 H 0.4043 0.0480 0.6034 0.025 Uiso 1 1 calc R . . C55 C 0.40573(13) -0.09264(14) 0.64959(10) 0.0216(3) Uani 1 1 d . . . C56 C 0.37928(14) -0.15276(14) 0.71721(11) 0.0235(4) Uani 1 1 d . . . H56 H 0.3958 -0.2233 0.7169 0.028 Uiso 1 1 calc R . . C57 C 0.32815(15) -0.10613(14) 0.78475(11) 0.0235(4) Uani 1 1 d . . . C58 C 0.30422(14) -0.00255(14) 0.78507(10) 0.0233(4) Uani 1 1 d . . . H58 H 0.2682 0.0270 0.8325 0.028 Uiso 1 1 calc R . . C59 C 0.46294(18) -0.14002(17) 0.57521(13) 0.0360(5) Uani 1 1 d . . . C60 C 0.29737(19) -0.16703(16) 0.85948(13) 0.0355(5) Uani 1 1 d . . . C61 C 0.28668(12) 0.24593(13) 0.63892(10) 0.0176(3) Uani 1 1 d . . . C62 C 0.24092(13) 0.21786(13) 0.59003(10) 0.0192(3) Uani 1 1 d . . . H62 H 0.2281 0.1548 0.6019 0.023 Uiso 1 1 calc R . . C63 C 0.21363(14) 0.27903(14) 0.52475(10) 0.0220(3) Uani 1 1 d . . . C64 C 0.22930(15) 0.37244(15) 0.50554(11) 0.0260(4) Uani 1 1 d . . . H64 H 0.2111 0.4141 0.4607 0.031 Uiso 1 1 calc R . . C65 C 0.27250(15) 0.40296(14) 0.55405(11) 0.0243(4) Uani 1 1 d . . . C66 C 0.30037(14) 0.34127(13) 0.61897(10) 0.0211(3) Uani 1 1 d . . . H66 H 0.3297 0.3645 0.6510 0.025 Uiso 1 1 calc R . . C67 C 0.16559(16) 0.24419(16) 0.47467(12) 0.0298(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02269(4) 0.02427(4) 0.01664(3) -0.00093(2) -0.00575(2) -0.01220(3) N1 0.0314(8) 0.0223(8) 0.0202(7) -0.0026(6) -0.0079(6) -0.0110(6) N2 0.0324(8) 0.0227(8) 0.0179(7) -0.0007(6) -0.0039(6) -0.0094(6) N3 0.0209(7) 0.0180(7) 0.0175(7) -0.0025(5) -0.0028(5) -0.0077(5) N4 0.0192(7) 0.0180(7) 0.0220(7) -0.0009(6) -0.0021(5) -0.0076(5) N5 0.0454(11) 0.0343(10) 0.0568(13) -0.0078(9) -0.0264(10) -0.0080(9) N6 0.0265(8) 0.0327(9) 0.0389(10) -0.0093(8) -0.0078(7) -0.0109(7) N7 0.0341(9) 0.0381(10) 0.0411(11) -0.0175(8) 0.0062(8) -0.0194(8) N8 0.0267(8) 0.0293(9) 0.0317(9) -0.0097(7) -0.0015(7) -0.0117(7) C1 0.0255(9) 0.0357(11) 0.0165(8) -0.0029(7) -0.0013(7) -0.0126(8) C2 0.0275(9) 0.0425(12) 0.0169(8) 0.0006(8) -0.0050(7) -0.0173(8) C3 0.0411(12) 0.0488(14) 0.0267(10) 0.0098(9) -0.0074(9) -0.0252(11) C4 0.0554(15) 0.0471(14) 0.0398(13) 0.0082(11) -0.0107(11) -0.0368(12) C5 0.0465(13) 0.0499(14) 0.0294(11) 0.0003(10) -0.0103(9) -0.0360(11) C6 0.0333(11) 0.0608(16) 0.0320(11) 0.0085(10) -0.0173(9) -0.0303(11) C7 0.0215(10) 0.0712(18) 0.0474(14) 0.0046(13) -0.0094(10) -0.0148(11) C8 0.0256(10) 0.0521(14) 0.0354(12) -0.0037(10) 0.0011(9) -0.0071(10) C9 0.0467(12) 0.0289(10) 0.0270(10) -0.0085(8) -0.0129(9) -0.0132(9) C10 0.0620(15) 0.0393(12) 0.0207(10) -0.0092(9) -0.0096(10) -0.0139(11) C11 0.0471(12) 0.0347(11) 0.0166(9) -0.0010(8) -0.0039(8) -0.0085(9) C12 0.0241(8) 0.0215(9) 0.0258(9) -0.0040(7) -0.0097(7) -0.0065(7) C13 0.0214(9) 0.0272(10) 0.0432(12) -0.0073(9) -0.0100(8) -0.0070(7) C14 0.0198(8) 0.0229(9) 0.0395(11) -0.0056(8) -0.0009(7) -0.0095(7) C15 0.0263(9) 0.0191(8) 0.0210(8) 0.0013(7) -0.0029(7) -0.0092(7) C16 0.0445(14) 0.0610(17) 0.0634(18) -0.0198(14) -0.0239(13) -0.0150(13) C17 0.0577(18) 0.093(2) 0.0612(18) -0.0187(17) -0.0061(14) -0.0546(18) C18 0.0587(17) 0.0735(19) 0.0435(14) 0.0010(13) -0.0091(12) -0.0480(15) C19 0.0538(15) 0.0621(17) 0.0344(12) -0.0171(12) 0.0061(11) -0.0366(13) C20 0.0555(16) 0.0633(17) 0.0347(12) -0.0008(12) -0.0117(11) -0.0338(14) C21 0.0374(12) 0.0385(12) 0.0381(12) -0.0016(10) -0.0117(9) -0.0141(9) C22 0.0236(9) 0.0232(9) 0.0330(10) -0.0052(8) -0.0051(7) -0.0081(7) C23 0.0258(9) 0.0187(8) 0.0230(8) 0.0042(7) -0.0079(7) -0.0071(7) C24 0.0355(11) 0.0216(9) 0.0367(11) 0.0008(8) -0.0176(9) -0.0072(8) C25 0.0292(10) 0.0282(11) 0.0584(15) 0.0012(10) -0.0250(10) -0.0057(8) C26 0.0222(9) 0.0281(10) 0.0462(12) 0.0002(9) -0.0141(9) -0.0024(7) C27 0.0228(9) 0.0220(9) 0.0306(10) 0.0025(7) -0.0080(7) -0.0040(7) C28 0.0217(9) 0.0230(9) 0.0319(10) -0.0034(8) -0.0032(7) -0.0007(7) C29 0.0235(9) 0.0218(9) 0.0272(9) -0.0034(7) -0.0030(7) -0.0027(7) C30 0.0305(10) 0.0276(10) 0.0343(11) -0.0115(8) -0.0031(8) 0.0000(8) C31 0.0385(11) 0.0273(10) 0.0360(11) -0.0137(9) -0.0072(9) -0.0043(8) C32 0.0302(10) 0.0246(10) 0.0364(11) -0.0083(8) -0.0076(8) -0.0070(8) C33 0.0252(9) 0.0219(9) 0.0268(9) -0.0038(7) -0.0045(7) -0.0053(7) C34 0.0220(8) 0.0193(8) 0.0234(8) -0.0017(7) -0.0036(7) -0.0044(6) C35 0.0194(8) 0.0197(8) 0.0249(9) -0.0024(7) -0.0024(6) -0.0048(6) C36 0.0229(8) 0.0176(8) 0.0219(8) 0.0021(6) -0.0061(7) -0.0049(6) F1 0.0360(7) 0.0476(8) 0.0491(8) -0.0036(7) 0.0063(6) -0.0110(6) F2 0.0383(8) 0.0467(9) 0.0781(11) 0.0241(8) -0.0089(8) -0.0191(7) F3 0.0363(8) 0.0863(13) 0.0921(13) -0.0030(10) -0.0121(8) -0.0422(9) F4 0.1128(18) 0.1078(17) 0.1011(16) -0.0082(13) -0.0810(15) -0.0411(14) F5 0.0939(14) 0.0590(11) 0.0562(10) -0.0068(8) -0.0451(10) 0.0076(10) F6 0.0811(13) 0.1150(16) 0.0552(11) -0.0496(11) -0.0409(10) 0.0338(12) F7 0.0352(6) 0.0269(6) 0.0270(6) -0.0034(5) -0.0051(5) -0.0167(5) F8 0.1370(17) 0.0581(10) 0.0369(8) 0.0202(7) -0.0503(10) -0.0644(11) F9 0.0488(9) 0.0659(10) 0.0829(12) -0.0612(9) 0.0306(8) -0.0320(8) F10 0.0379(8) 0.1111(15) 0.0576(10) -0.0084(10) -0.0168(7) -0.0370(9) F11 0.0431(9) 0.0560(10) 0.0973(14) 0.0133(9) -0.0158(9) -0.0334(8) F12 0.0307(7) 0.0879(13) 0.0988(13) -0.0635(11) 0.0276(8) -0.0276(8) F13 0.0364(9) 0.1377(19) 0.0828(13) -0.0721(13) 0.0188(8) -0.0032(10) F14 0.1013(13) 0.0423(8) 0.0223(6) -0.0112(6) 0.0020(7) -0.0197(8) F15 0.1158(15) 0.0332(8) 0.0367(8) -0.0182(6) -0.0036(8) -0.0265(9) F16 0.1151(15) 0.0278(7) 0.0436(9) 0.0002(6) 0.0064(9) -0.0297(9) F17 0.0459(8) 0.0605(9) 0.0356(7) 0.0072(7) 0.0054(6) -0.0228(7) F18 0.0737(11) 0.0554(9) 0.0365(8) 0.0141(7) -0.0262(7) -0.0214(8) F19 0.1079(14) 0.0726(11) 0.0254(7) 0.0084(7) -0.0288(8) -0.0592(11) F20 0.0310(7) 0.0966(13) 0.0721(11) -0.0449(10) -0.0144(7) -0.0155(8) F21 0.0724(10) 0.0371(7) 0.0509(8) -0.0113(6) -0.0314(8) -0.0180(7) C68 0.0448(16) 0.0276(11) 0.0358(12) 0.0027(9) -0.0150(12) -0.0164(11) F22 0.164(4) 0.046(2) 0.100(3) 0.044(2) -0.105(3) -0.062(3) F23 0.0566(16) 0.0504(15) 0.093(2) -0.0059(16) 0.0054(15) -0.0362(13) F24 0.099(3) 0.0386(18) 0.056(2) -0.0227(19) 0.0043(19) -0.0361(18) C68A 0.0448(16) 0.0276(11) 0.0358(12) 0.0027(9) -0.0150(12) -0.0164(11) F22A 0.188(14) 0.057(6) 0.086(8) 0.040(5) -0.111(9) -0.082(8) F23A 0.090(6) 0.027(3) 0.122(8) 0.007(4) -0.051(5) -0.009(3) F24A 0.153(9) 0.055(5) 0.053(4) -0.013(4) 0.043(5) -0.073(6) B1 0.0184(8) 0.0192(9) 0.0165(8) -0.0055(7) -0.0016(7) -0.0051(7) C37 0.0203(8) 0.0185(8) 0.0236(8) -0.0079(7) -0.0056(6) -0.0025(6) C38 0.0192(8) 0.0181(8) 0.0302(9) -0.0061(7) -0.0058(7) -0.0048(6) C39 0.0207(8) 0.0199(9) 0.0461(12) -0.0066(8) -0.0078(8) -0.0060(7) C40 0.0252(9) 0.0256(10) 0.0602(14) -0.0152(10) -0.0202(10) -0.0024(8) C41 0.0369(11) 0.0264(10) 0.0418(12) -0.0142(9) -0.0230(9) 0.0036(8) C42 0.0290(9) 0.0257(9) 0.0268(9) -0.0091(8) -0.0089(7) 0.0006(7) C43 0.0235(10) 0.0359(12) 0.0604(15) 0.0041(11) -0.0089(10) -0.0149(9) C44 0.0506(15) 0.0498(15) 0.0515(15) -0.0231(12) -0.0308(12) 0.0089(12) C45 0.0295(9) 0.0131(7) 0.0136(7) -0.0006(6) -0.0078(6) -0.0084(6) C46 0.0207(8) 0.0189(8) 0.0202(8) -0.0036(6) -0.0013(6) -0.0079(6) C47 0.0255(8) 0.0169(8) 0.0179(8) -0.0041(6) -0.0014(6) -0.0071(6) C48 0.0250(9) 0.0178(8) 0.0223(8) -0.0067(7) 0.0005(7) -0.0038(7) C49 0.0183(8) 0.0209(8) 0.0242(9) -0.0053(7) -0.0016(6) -0.0045(6) C50 0.0207(8) 0.0186(8) 0.0216(8) -0.0058(6) -0.0040(6) -0.0045(6) C51 0.0373(10) 0.0278(10) 0.0211(9) -0.0080(7) 0.0029(7) -0.0168(8) C52 0.0222(9) 0.0366(11) 0.0398(12) -0.0143(9) -0.0003(8) -0.0088(8) C53 0.0155(7) 0.0212(8) 0.0184(8) -0.0053(6) -0.0020(6) -0.0041(6) C54 0.0194(8) 0.0218(8) 0.0183(8) -0.0041(6) -0.0003(6) -0.0058(6) C55 0.0182(8) 0.0246(9) 0.0218(8) -0.0104(7) -0.0008(6) -0.0053(6) C56 0.0230(8) 0.0199(8) 0.0286(9) -0.0066(7) -0.0056(7) -0.0059(7) C57 0.0272(9) 0.0213(9) 0.0213(8) -0.0016(7) -0.0036(7) -0.0086(7) C58 0.0258(9) 0.0226(9) 0.0186(8) -0.0053(7) -0.0010(7) -0.0057(7) C59 0.0426(12) 0.0311(11) 0.0295(11) -0.0152(9) 0.0020(9) -0.0078(9) C60 0.0469(13) 0.0282(11) 0.0295(10) 0.0003(8) -0.0053(9) -0.0134(9) C61 0.0135(7) 0.0203(8) 0.0173(7) -0.0065(6) 0.0000(6) -0.0036(6) C62 0.0177(7) 0.0210(8) 0.0186(8) -0.0050(6) -0.0007(6) -0.0069(6) C63 0.0210(8) 0.0273(9) 0.0195(8) -0.0057(7) -0.0035(6) -0.0088(7) C64 0.0307(10) 0.0269(9) 0.0206(8) 0.0001(7) -0.0071(7) -0.0093(8) C65 0.0289(9) 0.0218(9) 0.0242(9) -0.0023(7) -0.0064(7) -0.0101(7) C66 0.0222(8) 0.0214(8) 0.0222(8) -0.0056(7) -0.0064(6) -0.0069(6) C67 0.0333(10) 0.0369(11) 0.0246(9) -0.0055(8) -0.0083(8) -0.0151(9) _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 N3 2.0721(15) . ? Ir1 N1 2.1002(15) . ? Ir1 C1 2.1139(18) . ? Ir1 C5 2.116(2) . ? Ir1 C2 2.1301(19) . ? Ir1 C6 2.131(2) . ? N1 C9 1.336(2) . ? N1 N2 1.361(2) . ? N2 C11 1.346(2) . ? N2 C15 1.457(2) . ? N3 C12 1.338(2) . ? N3 N4 1.362(2) . ? N4 C14 1.350(2) . ? N4 C15 1.456(2) . ? N5 C16 1.333(3) . ? N5 N6 1.349(3) . ? N6 C18 1.353(3) . ? N6 C22 1.453(3) . ? N7 C19 1.320(3) . ? N7 N8 1.358(2) . ? N8 C21 1.349(3) . ? N8 C22 1.448(3) . ? C1 C2 1.400(3) . ? C1 C8 1.508(3) . ? C1 H1 1.01(2) . ? C2 C3 1.515(3) . ? C2 H2 0.95(2) . ? C3 C4 1.529(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.403(4) . ? C5 H5 1.02(3) . ? C6 C7 1.519(4) . ? C6 H6 0.94(3) . ? C7 C8 1.533(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.368(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C13 C14 1.368(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C23 1.526(2) . ? C15 H15 1.0000 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 C18 1.373(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.387(4) . ? C19 H19 0.9500 . ? C20 C21 1.368(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C33 1.520(3) . ? C22 H22 1.0000 . ? C23 C24 1.368(3) . ? C23 C36 1.442(3) . ? C24 C25 1.414(3) . ? C24 H24 0.9500 . ? C25 C26 1.358(3) . ? C25 H25 0.9500 . ? C26 C27 1.423(3) . ? C26 H26 0.9500 . ? C27 C28 1.391(3) . ? C27 C36 1.438(2) . ? C28 C29 1.384(3) . ? C28 H28 0.9500 . ? C29 C30 1.431(3) . ? C29 C34 1.432(2) . ? C30 C31 1.351(3) . ? C30 H30 0.9500 . ? C31 C32 1.426(3) . ? C31 H31 0.9500 . ? C32 C33 1.362(3) . ? C32 H32 0.9500 . ? C33 C34 1.439(3) . ? C34 C35 1.404(3) . ? C35 C36 1.392(3) . ? C35 H35 0.9500 . ? F1 C43 1.335(3) . ? F2 C43 1.330(3) . ? F3 C43 1.340(3) . ? F4 C44 1.335(3) . ? F5 C44 1.321(3) . ? F6 C44 1.335(3) . ? F7 C51 1.329(2) . ? F8 C51 1.348(3) . ? F9 C51 1.328(2) . ? F10 C52 1.326(3) . ? F11 C52 1.342(3) . ? F12 C52 1.316(2) . ? F13 C59 1.314(3) . ? F14 C59 1.342(3) . ? F15 C59 1.322(3) . ? F16 C60 1.328(3) . ? F17 C60 1.342(3) . ? F18 C60 1.331(3) . ? F19 C67 1.320(2) . ? F20 C67 1.334(3) . ? F21 C67 1.338(3) . ? C68 F22 1.3131(16) . ? C68 F24 1.3133(16) . ? C68 F23 1.3135(16) . ? C68 C65 1.502(3) . ? C68A F23A 1.3129(16) . ? C68A F24A 1.3131(16) . ? C68A F22A 1.3131(17) . ? C68A C65 1.502(3) . ? B1 C45 1.626(2) . ? B1 C53 1.639(3) . ? B1 C37 1.639(3) . ? B1 C61 1.642(3) . ? C37 C42 1.397(3) . ? C37 C38 1.399(3) . ? C38 C39 1.386(3) . ? C38 H38 0.9500 . ? C39 C40 1.386(3) . ? C39 C43 1.500(3) . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.388(3) . ? C41 C44 1.489(3) . ? C42 H42 0.9500 . ? C45 C46 1.404(2) . ? C45 C50 1.416(3) . ? C46 C47 1.396(2) . ? C46 H46 0.9500 . ? C47 C48 1.381(3) . ? C47 C51 1.489(3) . ? C48 C49 1.390(3) . ? C48 H48 0.9500 . ? C49 C50 1.396(2) . ? C49 C52 1.490(3) . ? C50 H50 0.9500 . ? C53 C58 1.396(3) . ? C53 C54 1.408(2) . ? C54 C55 1.381(3) . ? C54 H54 0.9500 . ? C55 C56 1.391(3) . ? C55 C59 1.497(2) . ? C56 C57 1.380(2) . ? C56 H56 0.9500 . ? C57 C58 1.394(3) . ? C57 C60 1.500(3) . ? C58 H58 0.9500 . ? C61 C62 1.399(2) . ? C61 C66 1.402(3) . ? C62 C63 1.390(3) . ? C62 H62 0.9500 . ? C63 C64 1.387(3) . ? C63 C67 1.495(3) . ? C64 C65 1.387(3) . ? C64 H64 0.9500 . ? C65 C66 1.390(3) . ? C66 H66 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ir1 N1 85.87(6) . . ? N3 Ir1 C1 90.77(7) . . ? N1 Ir1 C1 157.45(7) . . ? N3 Ir1 C5 159.51(8) . . ? N1 Ir1 C5 92.72(8) . . ? C1 Ir1 C5 97.97(9) . . ? N3 Ir1 C2 94.47(7) . . ? N1 Ir1 C2 163.98(7) . . ? C1 Ir1 C2 38.51(8) . . ? C5 Ir1 C2 81.36(8) . . ? N3 Ir1 C6 161.91(8) . . ? N1 Ir1 C6 95.06(8) . . ? C1 Ir1 C6 81.44(9) . . ? C5 Ir1 C6 38.58(10) . . ? C2 Ir1 C6 89.56(8) . . ? C9 N1 N2 105.30(16) . . ? C9 N1 Ir1 134.09(15) . . ? N2 N1 Ir1 120.53(11) . . ? C11 N2 N1 111.12(17) . . ? C11 N2 C15 128.58(18) . . ? N1 N2 C15 119.74(14) . . ? C12 N3 N4 105.27(15) . . ? C12 N3 Ir1 132.75(13) . . ? N4 N3 Ir1 120.23(11) . . ? C14 N4 N3 110.96(15) . . ? C14 N4 C15 128.89(16) . . ? N3 N4 C15 120.12(14) . . ? C16 N5 N6 104.1(2) . . ? N5 N6 C18 112.7(2) . . ? N5 N6 C22 117.45(19) . . ? C18 N6 C22 129.0(2) . . ? C19 N7 N8 103.5(2) . . ? C21 N8 N7 112.22(19) . . ? C21 N8 C22 128.67(18) . . ? N7 N8 C22 119.11(17) . . ? C2 C1 C8 124.8(2) . . ? C2 C1 Ir1 71.37(11) . . ? C8 C1 Ir1 111.66(14) . . ? C2 C1 H1 115.9(13) . . ? C8 C1 H1 115.6(13) . . ? Ir1 C1 H1 105.6(13) . . ? C1 C2 C3 123.47(19) . . ? C1 C2 Ir1 70.12(11) . . ? C3 C2 Ir1 113.76(14) . . ? C1 C2 H2 117.3(15) . . ? C3 C2 H2 113.2(15) . . ? Ir1 C2 H2 110.4(14) . . ? C2 C3 C4 111.34(18) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 112.4(2) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 125.4(2) . . ? C6 C5 Ir1 71.26(13) . . ? C4 C5 Ir1 110.64(15) . . ? C6 C5 H5 120.9(15) . . ? C4 C5 H5 109.0(15) . . ? Ir1 C5 H5 111.6(15) . . ? C5 C6 C7 124.3(2) . . ? C5 C6 Ir1 70.16(13) . . ? C7 C6 Ir1 113.54(15) . . ? C5 C6 H6 116.6(16) . . ? C7 C6 H6 115.5(16) . . ? Ir1 C6 H6 104.6(16) . . ? C6 C7 C8 112.27(18) . . ? 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 112.36(19) . . ? C1 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C1 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C10 110.6(2) . . ? N1 C9 H9 124.7 . . ? C10 C9 H9 124.7 . . ? C11 C10 C9 105.94(19) . . ? C11 C10 H10 127.0 . . ? C9 C10 H10 127.0 . . ? N2 C11 C10 107.06(19) . . ? N2 C11 H11 126.5 . . ? C10 C11 H11 126.5 . . ? N3 C12 C13 110.80(18) . . ? N3 C12 H12 124.6 . . ? C13 C12 H12 124.6 . . ? C14 C13 C12 105.56(17) . . ? C14 C13 H13 127.2 . . ? C12 C13 H13 127.2 . . ? N4 C14 C13 107.39(17) . . ? N4 C14 H14 126.3 . . ? C13 C14 H14 126.3 . . ? N4 C15 N2 107.81(14) . . ? N4 C15 C23 114.38(15) . . ? N2 C15 C23 111.33(16) . . ? N4 C15 H15 107.7 . . ? N2 C15 H15 107.7 . . ? C23 C15 H15 107.7 . . ? N5 C16 C17 111.7(2) . . ? N5 C16 H16 124.1 . . ? C17 C16 H16 124.1 . . ? C18 C17 C16 105.7(2) . . ? C18 C17 H17 127.2 . . ? C16 C17 H17 127.2 . . ? N6 C18 C17 105.8(3) . . ? N6 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? N7 C19 C20 113.2(2) . . ? N7 C19 H19 123.4 . . ? C20 C19 H19 123.4 . . ? C21 C20 C19 104.3(2) . . ? C21 C20 H20 127.9 . . ? C19 C20 H20 127.9 . . ? N8 C21 C20 106.9(2) . . ? N8 C21 H21 126.6 . . ? C20 C21 H21 126.6 . . ? N8 C22 N6 110.21(17) . . ? N8 C22 C33 110.88(16) . . ? N6 C22 C33 113.03(16) . . ? N8 C22 H22 107.5 . . ? N6 C22 H22 107.5 . . ? C33 C22 H22 107.5 . . ? C24 C23 C36 119.46(17) . . ? C24 C23 C15 120.02(17) . . ? C36 C23 C15 120.46(16) . . ? C23 C24 C25 122.03(19) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.62(19) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 121.12(18) . . ? C28 C27 C36 119.09(18) . . ? C26 C27 C36 119.74(18) . . ? C29 C28 C27 122.18(17) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 C30 121.54(17) . . ? C28 C29 C34 119.33(17) . . ? C30 C29 C34 119.13(18) . . ? C31 C30 C29 120.73(18) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.43(19) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 121.1(2) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 120.05(17) . . ? C32 C33 C22 121.24(18) . . ? C34 C33 C22 118.69(16) . . ? C35 C34 C29 118.62(17) . . ? C35 C34 C33 122.93(16) . . ? C29 C34 C33 118.45(16) . . ? C36 C35 C34 122.02(16) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C27 118.62(17) . . ? C35 C36 C23 123.57(16) . . ? C27 C36 C23 117.77(17) . . ? F22 C68 F24 106.1(4) . . ? F22 C68 F23 108.4(3) . . ? F24 C68 F23 103.3(3) . . ? F22 C68 C65 112.4(2) . . ? F24 C68 C65 111.5(3) . . ? F23 C68 C65 114.4(2) . . ? F23A C68A F24A 104.6(8) . . ? F23A C68A F22A 102.2(8) . . ? F24A C68A F22A 111.9(9) . . ? F23A C68A C65 114.9(5) . . ? F24A C68A C65 108.6(4) . . ? F22A C68A C65 114.2(8) . . ? C45 B1 C53 113.66(14) . . ? C45 B1 C37 110.28(14) . . ? C53 B1 C37 104.10(13) . . ? C45 B1 C61 105.35(13) . . ? C53 B1 C61 112.60(14) . . ? C37 B1 C61 110.98(15) . . ? C42 C37 C38 115.46(17) . . ? C42 C37 B1 121.12(17) . . ? C38 C37 B1 123.36(16) . . ? C39 C38 C37 122.30(18) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C40 C39 C38 121.1(2) . . ? C40 C39 C43 120.67(19) . . ? C38 C39 C43 118.2(2) . . ? C39 C40 C41 117.81(19) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? C42 C41 C40 120.55(19) . . ? C42 C41 C44 118.9(2) . . ? C40 C41 C44 120.5(2) . . ? C41 C42 C37 122.7(2) . . ? C41 C42 H42 118.7 . . ? C37 C42 H42 118.7 . . ? F2 C43 F1 106.1(2) . . ? F2 C43 F3 107.18(19) . . ? F1 C43 F3 105.82(18) . . ? F2 C43 C39 112.83(18) . . ? F1 C43 C39 111.84(18) . . ? F3 C43 C39 112.6(2) . . ? F5 C44 F4 105.3(2) . . ? F5 C44 F6 105.8(3) . . ? F4 C44 F6 106.6(2) . . ? F5 C44 C41 113.2(2) . . ? F4 C44 C41 112.7(3) . . ? F6 C44 C41 112.65(19) . . ? C46 C45 C50 114.43(15) . . ? C46 C45 B1 122.50(16) . . ? C50 C45 B1 122.84(15) . . ? C47 C46 C45 123.30(17) . . ? C47 C46 H46 118.3 . . ? C45 C46 H46 118.3 . . ? C48 C47 C46 120.76(16) . . ? C48 C47 C51 120.25(16) . . ? C46 C47 C51 118.67(17) . . ? C47 C48 C49 117.95(16) . . ? C47 C48 H48 121.0 . . ? C49 C48 H48 121.0 . . ? C48 C49 C50 121.11(17) . . ? C48 C49 C52 119.62(16) . . ? C50 C49 C52 119.17(17) . . ? C49 C50 C45 122.41(16) . . ? C49 C50 H50 118.8 . . ? C45 C50 H50 118.8 . . ? F9 C51 F7 106.50(16) . . ? F9 C51 F8 106.92(18) . . ? F7 C51 F8 104.87(18) . . ? F9 C51 C47 113.31(18) . . ? F7 C51 C47 113.88(15) . . ? F8 C51 C47 110.78(17) . . ? F12 C52 F10 107.30(19) . . ? F12 C52 F11 105.7(2) . . ? F10 C52 F11 104.23(19) . . ? F12 C52 C49 113.91(18) . . ? F10 C52 C49 113.46(18) . . ? F11 C52 C49 111.47(17) . . ? C58 C53 C54 114.98(16) . . ? C58 C53 B1 124.41(15) . . ? C54 C53 B1 120.14(15) . . ? C55 C54 C53 122.67(17) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C54 C55 C56 121.06(16) . . ? C54 C55 C59 119.37(18) . . ? C56 C55 C59 119.53(17) . . ? C57 C56 C55 117.58(16) . . ? C57 C56 H56 121.2 . . ? C55 C56 H56 121.2 . . ? C56 C57 C58 121.13(17) . . ? C56 C57 C60 120.00(17) . . ? C58 C57 C60 118.87(16) . . ? C57 C58 C53 122.57(16) . . ? C57 C58 H58 118.7 . . ? C53 C58 H58 118.7 . . ? F13 C59 F15 107.7(2) . . ? F13 C59 F14 105.3(2) . . ? F15 C59 F14 105.63(19) . . ? F13 C59 C55 112.18(19) . . ? F15 C59 C55 113.45(19) . . ? F14 C59 C55 112.04(17) . . ? F16 C60 F18 106.99(19) . . ? F16 C60 F17 107.0(2) . . ? F18 C60 F17 104.85(18) . . ? F16 C60 C57 113.33(18) . . ? F18 C60 C57 112.21(19) . . ? F17 C60 C57 111.89(18) . . ? C62 C61 C66 115.52(16) . . ? C62 C61 B1 124.85(16) . . ? C66 C61 B1 119.55(15) . . ? C63 C62 C61 122.30(17) . . ? C63 C62 H62 118.8 . . ? C61 C62 H62 118.8 . . ? C64 C63 C62 121.13(17) . . ? C64 C63 C67 119.29(17) . . ? C62 C63 C67 119.58(17) . . ? C63 C64 C65 117.68(17) . . ? C63 C64 H64 121.2 . . ? C65 C64 H64 121.2 . . ? C64 C65 C66 121.01(18) . . ? C64 C65 C68A 117.0(3) . . ? C66 C65 C68A 121.7(3) . . ? C64 C65 C68 120.99(18) . . ? C66 C65 C68 117.87(18) . . ? C65 C66 C61 122.33(17) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? F19 C67 F20 107.73(19) . . ? F19 C67 F21 105.71(17) . . ? F20 C67 F21 104.25(19) . . ? F19 C67 C63 113.19(18) . . ? F20 C67 C63 112.48(16) . . ? F21 C67 C63 112.85(17) . . ? 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 N3 Ir1 N1 C9 -147.7(2) . . . . ? C1 Ir1 N1 C9 130.3(2) . . . . ? C5 Ir1 N1 C9 11.9(2) . . . . ? C2 Ir1 N1 C9 -55.8(4) . . . . ? C6 Ir1 N1 C9 50.5(2) . . . . ? N3 Ir1 N1 N2 36.21(14) . . . . ? C1 Ir1 N1 N2 -45.8(3) . . . . ? C5 Ir1 N1 N2 -164.27(15) . . . . ? C2 Ir1 N1 N2 128.0(2) . . . . ? C6 Ir1 N1 N2 -125.66(15) . . . . ? C9 N1 N2 C11 -1.5(2) . . . . ? Ir1 N1 N2 C11 175.59(14) . . . . ? C9 N1 N2 C15 -173.61(17) . . . . ? Ir1 N1 N2 C15 3.5(2) . . . . ? N1 Ir1 N3 C12 131.04(16) . . . . ? C1 Ir1 N3 C12 -71.28(17) . . . . ? C5 Ir1 N3 C12 44.3(3) . . . . ? C2 Ir1 N3 C12 -32.90(17) . . . . ? C6 Ir1 N3 C12 -135.3(2) . . . . ? N1 Ir1 N3 N4 -31.46(12) . . . . ? C1 Ir1 N3 N4 126.22(13) . . . . ? C5 Ir1 N3 N4 -118.2(2) . . . . ? C2 Ir1 N3 N4 164.60(13) . . . . ? C6 Ir1 N3 N4 62.2(3) . . . . ? C12 N3 N4 C14 -1.09(19) . . . . ? Ir1 N3 N4 C14 165.68(12) . . . . ? C12 N3 N4 C15 -179.38(15) . . . . ? Ir1 N3 N4 C15 -12.60(19) . . . . ? C16 N5 N6 C18 1.2(3) . . . . ? C16 N5 N6 C22 171.8(2) . . . . ? C19 N7 N8 C21 -0.6(2) . . . . ? C19 N7 N8 C22 179.99(18) . . . . ? N3 Ir1 C1 C2 96.22(12) . . . . ? N1 Ir1 C1 C2 177.29(15) . . . . ? C5 Ir1 C1 C2 -65.19(13) . . . . ? C6 Ir1 C1 C2 -100.18(13) . . . . ? N3 Ir1 C1 C8 -142.79(16) . . . . ? N1 Ir1 C1 C8 -61.7(3) . . . . ? C5 Ir1 C1 C8 55.80(17) . . . . ? C2 Ir1 C1 C8 121.0(2) . . . . ? C6 Ir1 C1 C8 20.81(17) . . . . ? C8 C1 C2 C3 2.1(3) . . . . ? Ir1 C1 C2 C3 105.94(19) . . . . ? C8 C1 C2 Ir1 -103.9(2) . . . . ? N3 Ir1 C2 C1 -85.60(12) . . . . ? N1 Ir1 C2 C1 -176.2(2) . . . . ? C5 Ir1 C2 C1 114.60(14) . . . . ? C6 Ir1 C2 C1 76.74(13) . . . . ? N3 Ir1 C2 C3 155.61(16) . . . . ? N1 Ir1 C2 C3 65.0(3) . . . . ? C1 Ir1 C2 C3 -118.8(2) . . . . ? C5 Ir1 C2 C3 -4.19(17) . . . . ? C6 Ir1 C2 C3 -42.05(17) . . . . ? C1 C2 C3 C4 -94.9(3) . . . . ? Ir1 C2 C3 C4 -13.8(3) . . . . ? C2 C3 C4 C5 32.2(3) . . . . ? C3 C4 C5 C6 45.6(3) . . . . ? C3 C4 C5 Ir1 -35.6(3) . . . . ? N3 Ir1 C5 C6 -179.81(17) . . . . ? N1 Ir1 C5 C6 94.71(13) . . . . ? C1 Ir1 C5 C6 -65.38(14) . . . . ? C2 Ir1 C5 C6 -100.25(14) . . . . ? N3 Ir1 C5 C4 -58.1(3) . . . . ? N1 Ir1 C5 C4 -143.56(18) . . . . ? C1 Ir1 C5 C4 56.35(19) . . . . ? C2 Ir1 C5 C4 21.48(18) . . . . ? C6 Ir1 C5 C4 121.7(2) . . . . ? C4 C5 C6 C7 3.1(4) . . . . ? Ir1 C5 C6 C7 105.5(2) . . . . ? C4 C5 C6 Ir1 -102.4(2) . . . . ? N3 Ir1 C6 C5 179.78(19) . . . . ? N1 Ir1 C6 C5 -88.01(13) . . . . ? C1 Ir1 C6 C5 114.43(14) . . . . ? C2 Ir1 C6 C5 76.63(14) . . . . ? N3 Ir1 C6 C7 60.1(3) . . . . ? N1 Ir1 C6 C7 152.29(18) . . . . ? C1 Ir1 C6 C7 -5.27(18) . . . . ? C5 Ir1 C6 C7 -119.7(2) . . . . ? C2 Ir1 C6 C7 -43.07(19) . . . . ? C5 C6 C7 C8 -92.3(3) . . . . ? Ir1 C6 C7 C8 -11.0(3) . . . . ? C2 C1 C8 C7 49.0(3) . . . . ? Ir1 C1 C8 C7 -32.8(2) . . . . ? C6 C7 C8 C1 28.5(3) . . . . ? N2 N1 C9 C10 1.4(2) . . . . ? Ir1 N1 C9 C10 -175.17(16) . . . . ? N1 C9 C10 C11 -0.7(3) . . . . ? N1 N2 C11 C10 1.1(2) . . . . ? C15 N2 C11 C10 172.29(19) . . . . ? C9 C10 C11 N2 -0.2(3) . . . . ? N4 N3 C12 C13 0.9(2) . . . . ? Ir1 N3 C12 C13 -163.48(13) . . . . ? N3 C12 C13 C14 -0.4(2) . . . . ? N3 N4 C14 C13 0.9(2) . . . . ? C15 N4 C14 C13 178.97(17) . . . . ? C12 C13 C14 N4 -0.3(2) . . . . ? C14 N4 C15 N2 -111.0(2) . . . . ? N3 N4 C15 N2 66.94(19) . . . . ? C14 N4 C15 C23 124.60(19) . . . . ? N3 N4 C15 C23 -57.5(2) . . . . ? C11 N2 C15 N4 128.6(2) . . . . ? N1 N2 C15 N4 -60.8(2) . . . . ? C11 N2 C15 C23 -105.1(2) . . . . ? N1 N2 C15 C23 65.4(2) . . . . ? N6 N5 C16 C17 -0.3(3) . . . . ? N5 C16 C17 C18 -0.7(4) . . . . ? N5 N6 C18 C17 -1.6(3) . . . . ? C22 N6 C18 C17 -170.9(2) . . . . ? C16 C17 C18 N6 1.3(3) . . . . ? N8 N7 C19 C20 0.4(3) . . . . ? N7 C19 C20 C21 -0.1(3) . . . . ? N7 N8 C21 C20 0.5(3) . . . . ? C22 N8 C21 C20 179.9(2) . . . . ? C19 C20 C21 N8 -0.2(3) . . . . ? C21 N8 C22 N6 88.2(2) . . . . ? N7 N8 C22 N6 -92.5(2) . . . . ? C21 N8 C22 C33 -37.7(3) . . . . ? N7 N8 C22 C33 141.61(18) . . . . ? N5 N6 C22 N8 149.34(17) . . . . ? C18 N6 C22 N8 -41.8(3) . . . . ? N5 N6 C22 C33 -86.0(2) . . . . ? C18 N6 C22 C33 82.9(3) . . . . ? N4 C15 C23 C24 129.81(19) . . . . ? N2 C15 C23 C24 7.3(2) . . . . ? N4 C15 C23 C36 -52.8(2) . . . . ? N2 C15 C23 C36 -175.32(16) . . . . ? C36 C23 C24 C25 5.4(3) . . . . ? C15 C23 C24 C25 -177.21(19) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C24 C25 C26 C27 -3.7(3) . . . . ? C25 C26 C27 C28 -175.8(2) . . . . ? C25 C26 C27 C36 1.7(3) . . . . ? C26 C27 C28 C29 176.3(2) . . . . ? C36 C27 C28 C29 -1.2(3) . . . . ? C27 C28 C29 C30 177.8(2) . . . . ? C27 C28 C29 C34 -2.2(3) . . . . ? C28 C29 C30 C31 179.8(2) . . . . ? C34 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C32 -1.9(3) . . . . ? C30 C31 C32 C33 1.4(3) . . . . ? C31 C32 C33 C34 1.2(3) . . . . ? C31 C32 C33 C22 179.7(2) . . . . ? N8 C22 C33 C32 118.1(2) . . . . ? N6 C22 C33 C32 -6.2(3) . . . . ? N8 C22 C33 C34 -63.3(2) . . . . ? N6 C22 C33 C34 172.40(18) . . . . ? C28 C29 C34 C35 3.2(3) . . . . ? C30 C29 C34 C35 -176.76(18) . . . . ? C28 C29 C34 C33 -177.35(18) . . . . ? C30 C29 C34 C33 2.6(3) . . . . ? C32 C33 C34 C35 176.25(19) . . . . ? C22 C33 C34 C35 -2.4(3) . . . . ? C32 C33 C34 C29 -3.1(3) . . . . ? C22 C33 C34 C29 178.26(17) . . . . ? C29 C34 C35 C36 -0.9(3) . . . . ? C33 C34 C35 C36 179.74(18) . . . . ? C34 C35 C36 C27 -2.5(3) . . . . ? C34 C35 C36 C23 179.92(17) . . . . ? C28 C27 C36 C35 3.5(3) . . . . ? C26 C27 C36 C35 -174.04(19) . . . . ? C28 C27 C36 C23 -178.75(18) . . . . ? C26 C27 C36 C23 3.7(3) . . . . ? C24 C23 C36 C35 170.49(18) . . . . ? C15 C23 C36 C35 -6.9(3) . . . . ? C24 C23 C36 C27 -7.2(3) . . . . ? C15 C23 C36 C27 175.46(16) . . . . ? C45 B1 C37 C42 42.3(2) . . . . ? C53 B1 C37 C42 -79.93(19) . . . . ? C61 B1 C37 C42 158.69(16) . . . . ? C45 B1 C37 C38 -140.52(16) . . . . ? C53 B1 C37 C38 97.21(19) . . . . ? C61 B1 C37 C38 -24.2(2) . . . . ? C42 C37 C38 C39 -2.3(3) . . . . ? B1 C37 C38 C39 -179.60(16) . . . . ? C37 C38 C39 C40 -0.5(3) . . . . ? C37 C38 C39 C43 178.22(18) . . . . ? C38 C39 C40 C41 1.6(3) . . . . ? C43 C39 C40 C41 -177.08(19) . . . . ? C39 C40 C41 C42 0.2(3) . . . . ? C39 C40 C41 C44 179.73(19) . . . . ? C40 C41 C42 C37 -3.2(3) . . . . ? C44 C41 C42 C37 177.24(19) . . . . ? C38 C37 C42 C41 4.2(3) . . . . ? B1 C37 C42 C41 -178.49(17) . . . . ? C40 C39 C43 F2 -137.3(2) . . . . ? C38 C39 C43 F2 44.0(3) . . . . ? C40 C39 C43 F1 103.2(2) . . . . ? C38 C39 C43 F1 -75.5(2) . . . . ? C40 C39 C43 F3 -15.8(3) . . . . ? C38 C39 C43 F3 165.49(18) . . . . ? C42 C41 C44 F5 80.8(3) . . . . ? C40 C41 C44 F5 -98.8(3) . . . . ? C42 C41 C44 F4 -159.8(2) . . . . ? C40 C41 C44 F4 20.6(3) . . . . ? C42 C41 C44 F6 -39.2(3) . . . . ? C40 C41 C44 F6 141.3(2) . . . . ? C53 B1 C45 C46 141.72(16) . . . . ? C37 B1 C45 C46 25.3(2) . . . . ? C61 B1 C45 C46 -94.55(19) . . . . ? C53 B1 C45 C50 -44.2(2) . . . . ? C37 B1 C45 C50 -160.61(16) . . . . ? C61 B1 C45 C50 79.6(2) . . . . ? C50 C45 C46 C47 2.1(3) . . . . ? B1 C45 C46 C47 176.67(17) . . . . ? C45 C46 C47 C48 -1.0(3) . . . . ? C45 C46 C47 C51 172.47(17) . . . . ? C46 C47 C48 C49 -0.8(3) . . . . ? C51 C47 C48 C49 -174.18(18) . . . . ? C47 C48 C49 C50 1.4(3) . . . . ? C47 C48 C49 C52 177.78(18) . . . . ? C48 C49 C50 C45 -0.2(3) . . . . ? C52 C49 C50 C45 -176.64(18) . . . . ? C46 C45 C50 C49 -1.5(3) . . . . ? B1 C45 C50 C49 -176.02(17) . . . . ? C48 C47 C51 F9 -29.6(3) . . . . ? C46 C47 C51 F9 156.87(18) . . . . ? C48 C47 C51 F7 -151.52(18) . . . . ? C46 C47 C51 F7 34.9(3) . . . . ? C48 C47 C51 F8 90.6(2) . . . . ? C46 C47 C51 F8 -83.0(2) . . . . ? C48 C49 C52 F12 8.7(3) . . . . ? C50 C49 C52 F12 -174.9(2) . . . . ? C48 C49 C52 F10 131.8(2) . . . . ? C50 C49 C52 F10 -51.7(3) . . . . ? C48 C49 C52 F11 -110.9(2) . . . . ? C50 C49 C52 F11 65.6(3) . . . . ? C45 B1 C53 C58 -25.3(2) . . . . ? C37 B1 C53 C58 94.70(19) . . . . ? C61 B1 C53 C58 -145.00(17) . . . . ? C45 B1 C53 C54 162.90(16) . . . . ? C37 B1 C53 C54 -77.08(19) . . . . ? C61 B1 C53 C54 43.2(2) . . . . ? C58 C53 C54 C55 0.6(3) . . . . ? B1 C53 C54 C55 173.15(17) . . . . ? C53 C54 C55 C56 -1.6(3) . . . . ? C53 C54 C55 C59 -179.19(18) . . . . ? C54 C55 C56 C57 1.3(3) . . . . ? C59 C55 C56 C57 178.91(18) . . . . ? C55 C56 C57 C58 -0.2(3) . . . . ? C55 C56 C57 C60 179.84(18) . . . . ? C56 C57 C58 C53 -0.8(3) . . . . ? C60 C57 C58 C53 179.22(18) . . . . ? C54 C53 C58 C57 0.5(3) . . . . ? B1 C53 C58 C57 -171.63(17) . . . . ? C54 C55 C59 F13 83.3(3) . . . . ? C56 C55 C59 F13 -94.4(3) . . . . ? C54 C55 C59 F15 -154.4(2) . . . . ? C56 C55 C59 F15 27.9(3) . . . . ? C54 C55 C59 F14 -34.9(3) . . . . ? C56 C55 C59 F14 147.45(19) . . . . ? C56 C57 C60 F16 -3.9(3) . . . . ? C58 C57 C60 F16 176.1(2) . . . . ? C56 C57 C60 F18 117.4(2) . . . . ? C58 C57 C60 F18 -62.5(3) . . . . ? C56 C57 C60 F17 -125.0(2) . . . . ? C58 C57 C60 F17 55.0(3) . . . . ? C45 B1 C61 C62 -103.84(17) . . . . ? C53 B1 C61 C62 20.6(2) . . . . ? C37 B1 C61 C62 136.81(16) . . . . ? C45 B1 C61 C66 72.89(19) . . . . ? C53 B1 C61 C66 -162.71(14) . . . . ? C37 B1 C61 C66 -46.46(19) . . . . ? C66 C61 C62 C63 1.8(2) . . . . ? B1 C61 C62 C63 178.66(15) . . . . ? C61 C62 C63 C64 -1.0(3) . . . . ? C61 C62 C63 C67 179.61(16) . . . . ? C62 C63 C64 C65 -0.4(3) . . . . ? C67 C63 C64 C65 178.98(17) . . . . ? C63 C64 C65 C66 0.9(3) . . . . ? C63 C64 C65 C68A -173.9(3) . . . . ? C63 C64 C65 C68 176.67(18) . . . . ? F23A C68A C65 C64 48.4(7) . . . . ? F24A C68A C65 C64 -68.3(8) . . . . ? F22A C68A C65 C64 166.0(8) . . . . ? F23A C68A C65 C66 -126.4(6) . . . . ? F24A C68A C65 C66 116.9(8) . . . . ? F22A C68A C65 C66 -8.7(9) . . . . ? F22 C68 C65 C64 14.8(4) . . . . ? F24 C68 C65 C64 133.8(3) . . . . ? F23 C68 C65 C64 -109.4(3) . . . . ? F22 C68 C65 C66 -169.3(3) . . . . ? F24 C68 C65 C66 -50.3(3) . . . . ? F23 C68 C65 C66 66.5(3) . . . . ? C64 C65 C66 C61 0.0(3) . . . . ? C68A C65 C66 C61 174.6(3) . . . . ? C68 C65 C66 C61 -175.88(17) . . . . ? C62 C61 C66 C65 -1.3(2) . . . . ? B1 C61 C66 C65 -178.37(16) . . . . ? C64 C63 C67 F19 30.3(3) . . . . ? C62 C63 C67 F19 -150.22(19) . . . . ? C64 C63 C67 F20 -92.0(2) . . . . ? C62 C63 C67 F20 87.4(2) . . . . ? C64 C63 C67 F21 150.35(18) . . . . ? C62 C63 C67 F21 -30.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.782 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.092 #===END data_compound9 _database_code_depnum_ccdc_archive 'CCDC 798121' _publ_section_abstract ; The synthesis of a series of Rh(I) and Ir(I) homobimetallic complexes, 2-13, using a series of three different linking scaffolds is described. The cyclooctadiene (COD) complexes [M2(COD)2(Lscaffold)][BArF4]2 (2-7) where M = Rh(I) or Ir(I), and Lscaffold = bis(1-pyrazolyl)methane ligands, p-C6H4[CH(pz)2]2 (1a), m-C6H4[CH(pz)2]2 (1b) and the anthracene-bridged 1,8-C14H8[CH(pz)2]2 were synthesized. The COD co-ligands of 2-7 were replaced with the carbonyl co-ligands to form the analogous homobimetallic complexes, [M2(CO)4(Lscaffold)][BArF4]2 (8-13). The solid-state structures of the dicationic homobimetallic complexes 2, 3, 5, 6, 9, and 10, as well as the cationic monometallic complex 15 were characterized using X-ray crystallography. The solid-state XRD structures of the resulting dirhodium and diiridium complexes with the para- and meta-phenylene and anthracene scaffolds show that there are distinct differences between structures of complexes 2-10 due to the variation in the scaffold structures, in particular the relative positions of the two metal centres. Heterobimetallic RhIr complexes of the m-C6H4[CH(pz)2]2 ligand were also synthesized using a stepwise approach, and the observed exchange of the metal centres in the heterbimetallic complexes was found to be dependant on the nature of the coligand. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Ir2 N8 O4, 2(C32 H12 B F24), 6(C4 H8 O)' _chemical_formula_sum 'C112 H90 B2 F48 Ir2 N8 O10' _chemical_formula_weight 3025.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.6310(3) _cell_length_b 13.8922(3) _cell_length_c 18.4681(4) _cell_angle_alpha 95.3880(10) _cell_angle_beta 100.9730(10) _cell_angle_gamma 108.2100(10) _cell_volume 2980.90(12) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9809 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.16 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1494 _exptl_absorpt_coefficient_mu 2.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3346 _exptl_absorpt_correction_T_max 0.4374 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48457 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14341 _reflns_number_gt 11743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; This structure bears numerous disordered parts. Firstly, two of the three THF solvent molecules were refined over two sites each (O4, C49-C52; O5, C53-C56). In the refinement of these molecules the following restraints were used: sadi 0.001 o4 c49 o4 c52 o4a c49a o4a c52a sadi 0.001 c49 c50 c50 c51 c51 c52 c49a c50a c50a c51a c51a c52a sadi 0.001 o5 c53 o5 c56 o5a c53a o5a c56a sadi 0.001 c53 c54 c55 c56 c53a c54a c55a c56a sadi 0.001 c54 c55 c54a c55a same o5 c53 c54 c55 c56 Furthermore, three thermal displacement variables were used for each molecule: eadp o4 c49 c50 c51 c52 eadp o4a c49a c50a c51a c52a eadp o5 c53 c54 c55 c56 eadp o5a c53a c54a c55a c56a Secondly, three CF3 groups of the anion are disordered over two sites (C19 F1 F2 F3; C27 F7 F8 F9; C28 F10/F110 F11/F111 F12/F112). The following restraints were used in the refinement: sadi 0.001 c19 f1 c19 f2 c19 f3 c19 f1a c19 f2a c19 f3a sadi 0.001 c27 f7 c27 f8 c27 f9 c27 f7a c27 f8a c27 f9a sadi 0.001 c28 f10 c28 f11 c28 f12 c28 f110 c28 f111 c28 f112 and same anisotropic displacement parameters were used for corresponding fluorine atoms, which are located opposite to each other, i.e., eadp f1 f1a eadp f2 f2a eadp f3 f3a eadp f7 f7a eadp f8 f8a eadp f9 f9a eadp f10 f110 eadp f11 f111 eadp f12 f112 Finally, the iridium complex itself is disordered over two sites in close proximity to one another, and therefore corresponding bonds were restrained to same bond lenghts, and corresponding atoms were refined with same thermal anisotropic displacement parameters: sadi 0.001 ir1 c1 ir2 c1a sadi 0.001 ir1 c2 ir2 c2a sadi 0.001 c1 o1 c1a o1a c2 o2 c2a o2a sadi 0.001 n1 n2 n1a n2a sadi 0.001 n1 ir1 n1a ir2 sadi 0.001 n1 c3 n1a c3a sadi 0.001 c3 c4 c3a c4a sadi 0.001 c4 c5 c4a c5a sadi 0.001 c5 n2 c5a n2a sadi 0.001 n2 c9 n2a c9a sadi 0.001 n3 ir1 n3a ir2 sadi 0.001 n3 n4 n3a n4a sadi 0.001 n4 c9 n4a c9a sadi 0.001 n3 c6 n3a c6a sadi 0.001 c6 c7 c6a c7a sadi 0.001 c7 c8 c7a c8a sadi 0.001 c8 n2 c8a n2a eadp ir1 ir2 eadp c1 c1a eadp c2 c2a eadp o1 o1a eadp o2 o2a eadp c9 c9a eadp n1 n1a eadp n2 n2a eadp c3 c3a eadp c4 c4a eadp c5 c5a eadp n3 n3a eadp n4 n4a eadp c6 c6a eadp c7 c7a eadp c8 c8a same c9 n2 n1 c3 c4 c5 same n4 n3 c6 c7 c8 The position of C9 (exyz c9 c9a) was used as anchor of the disordered moiety at the non-disordered phenylene group. 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^)+(0.0432P)^2^+2.0239P] 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 14341 _refine_ls_number_parameters 886 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.058 _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 O3 O 0.1383(3) 0.6851(2) 0.68465(15) 0.0629(7) Uani 1 1 d . A 1 C45 C 0.1694(5) 0.7657(3) 0.6435(2) 0.0697(12) Uani 1 1 d . A 1 H45A H 0.2361 0.8231 0.6743 0.084 Uiso 1 1 calc R A 1 H45B H 0.1050 0.7917 0.6295 0.084 Uiso 1 1 calc R A 1 C46 C 0.1989(3) 0.7265(3) 0.5750(2) 0.0581(10) Uani 1 1 d . A 1 H46A H 0.2815 0.7585 0.5769 0.070 Uiso 1 1 calc R A 1 H46B H 0.1536 0.7397 0.5295 0.070 Uiso 1 1 calc R A 1 C47 C 0.1683(4) 0.6129(3) 0.5767(2) 0.0696(12) Uani 1 1 d . A 1 H47A H 0.0903 0.5745 0.5459 0.084 Uiso 1 1 calc R A 1 H47B H 0.2237 0.5856 0.5584 0.084 Uiso 1 1 calc R A 1 C48 C 0.1742(3) 0.6064(3) 0.6567(2) 0.0520(8) Uani 1 1 d . A 1 H48A H 0.1233 0.5386 0.6627 0.062 Uiso 1 1 calc R A 1 H48B H 0.2535 0.6162 0.6834 0.062 Uiso 1 1 calc R A 1 O4 O 0.8382(7) 0.1604(5) 0.8743(4) 0.0826(13) Uani 0.61 1 d PD B 1 C49 C 0.8213(7) 0.2534(6) 0.8602(5) 0.0826(13) Uani 0.61 1 d PD B 1 H49A H 0.8142 0.2579 0.8064 0.099 Uiso 0.61 1 calc PR B 1 H49B H 0.8877 0.3125 0.8892 0.099 Uiso 0.61 1 calc PR B 1 C50 C 0.7167(7) 0.2560(7) 0.8820(5) 0.0826(13) Uani 0.61 1 d PD B 1 H50A H 0.7227 0.3268 0.9015 0.099 Uiso 0.61 1 calc PR B 1 H50B H 0.6486 0.2260 0.8398 0.099 Uiso 0.61 1 calc PR B 1 C51 C 0.7134(7) 0.1922(6) 0.9407(5) 0.0826(13) Uani 0.61 1 d PD B 1 H51A H 0.7375 0.2363 0.9904 0.099 Uiso 0.61 1 calc PR B 1 H51B H 0.6342 0.1449 0.9350 0.099 Uiso 0.61 1 calc PR B 1 C52 C 0.7901(8) 0.1331(7) 0.9357(5) 0.0826(13) Uani 0.61 1 d PD B 1 H52A H 0.8509 0.1506 0.9822 0.099 Uiso 0.61 1 calc PR B 1 H52B H 0.7469 0.0585 0.9273 0.099 Uiso 0.61 1 calc PR B 1 O4A O 0.8185(13) 0.1471(11) 0.8577(5) 0.101(2) Uani 0.39 1 d PD C 2 C49A C 0.7443(14) 0.1833(12) 0.8090(7) 0.101(2) Uani 0.39 1 d PD C 2 H49C H 0.6824 0.1255 0.7747 0.121 Uiso 0.39 1 calc PR C 2 H49D H 0.7868 0.2302 0.7791 0.121 Uiso 0.39 1 calc PR C 2 C50A C 0.6981(15) 0.2376(15) 0.8597(6) 0.101(2) Uani 0.39 1 d PD C 2 H50C H 0.6165 0.1980 0.8557 0.121 Uiso 0.39 1 calc PR C 2 H50D H 0.7028 0.3056 0.8456 0.121 Uiso 0.39 1 calc PR C 2 C51A C 0.7633(15) 0.2509(13) 0.9365(7) 0.101(2) Uani 0.39 1 d PD C 2 H51C H 0.7121 0.2394 0.9717 0.121 Uiso 0.39 1 calc PR C 2 H51D H 0.8213 0.3205 0.9520 0.121 Uiso 0.39 1 calc PR C 2 C52A C 0.8179(16) 0.1724(13) 0.9335(7) 0.101(2) Uani 0.39 1 d PD C 2 H52C H 0.8971 0.1993 0.9647 0.121 Uiso 0.39 1 calc PR C 2 H52D H 0.7741 0.1110 0.9519 0.121 Uiso 0.39 1 calc PR C 2 O5 O 0.2080(7) 0.9759(6) 0.3111(3) 0.1023(14) Uani 0.61 1 d PD D 1 C53 C 0.1598(10) 0.9905(8) 0.3747(4) 0.1023(14) Uani 0.61 1 d PD D 1 H53A H 0.0752 0.9657 0.3589 0.123 Uiso 0.61 1 calc PR D 1 H53B H 0.1864 1.0644 0.3959 0.123 Uiso 0.61 1 calc PR D 1 C54 C 0.1964(11) 0.9330(8) 0.4315(5) 0.1023(14) Uani 0.61 1 d PD D 1 H54A H 0.1410 0.8625 0.4250 0.123 Uiso 0.61 1 calc PR D 1 H54B H 0.2076 0.9687 0.4828 0.123 Uiso 0.61 1 calc PR D 1 C55 C 0.3115(10) 0.9321(8) 0.4143(4) 0.1023(14) Uani 0.61 1 d PD D 1 H55A H 0.3755 0.9935 0.4428 0.123 Uiso 0.61 1 calc PR D 1 H55B H 0.3277 0.8699 0.4276 0.123 Uiso 0.61 1 calc PR D 1 C56 C 0.2971(9) 0.9326(8) 0.3336(4) 0.1023(14) Uani 0.61 1 d PD D 1 H56A H 0.3696 0.9747 0.3226 0.123 Uiso 0.61 1 calc PR D 1 H56B H 0.2748 0.8618 0.3063 0.123 Uiso 0.61 1 calc PR D 1 O5A O 0.1902(11) 1.0110(8) 0.3277(6) 0.123(3) Uani 0.39 1 d PD E 2 C53A C 0.1164(16) 1.0334(11) 0.3730(8) 0.123(3) Uani 0.39 1 d PD E 2 H53C H 0.0460 1.0370 0.3407 0.148 Uiso 0.39 1 calc PR E 2 H53D H 0.1565 1.1004 0.4064 0.148 Uiso 0.39 1 calc PR E 2 C54A C 0.0869(15) 0.9510(10) 0.4176(8) 0.123(3) Uani 0.39 1 d PD E 2 H54C H 0.0092 0.9008 0.3956 0.148 Uiso 0.39 1 calc PR E 2 H54D H 0.0915 0.9786 0.4699 0.148 Uiso 0.39 1 calc PR E 2 C55A C 0.1809(18) 0.9026(12) 0.4125(9) 0.123(3) Uani 0.39 1 d PD E 2 H55C H 0.2261 0.9064 0.4633 0.148 Uiso 0.39 1 calc PR E 2 H55D H 0.1445 0.8293 0.3895 0.148 Uiso 0.39 1 calc PR E 2 C56A C 0.2572(14) 0.9567(12) 0.3675(8) 0.123(3) Uani 0.39 1 d PD E 2 H56C H 0.3302 1.0049 0.3995 0.148 Uiso 0.39 1 calc PR E 2 H56D H 0.2739 0.9079 0.3325 0.148 Uiso 0.39 1 calc PR E 2 Ir1 Ir 0.182890(13) 0.927078(11) 0.841914(9) 0.03355(5) Uani 0.88 1 d PD F 1 O1 O 0.4320(2) 1.0357(3) 0.9084(3) 0.1023(17) Uani 0.88 1 d PD F 1 O2 O 0.2321(3) 0.7337(3) 0.8651(3) 0.0718(10) Uani 0.88 1 d PD F 1 C1 C 0.3368(3) 0.9958(3) 0.8831(3) 0.0563(12) Uani 0.88 1 d PD F 1 C2 C 0.2109(3) 0.8061(3) 0.8563(3) 0.0447(9) Uani 0.88 1 d PD F 1 Ir2 Ir 0.17198(12) 0.95190(10) 0.82468(8) 0.03355(5) Uani 0.12 1 d PD G 2 O1A O 0.4188(7) 1.0827(18) 0.869(2) 0.1023(17) Uani 0.12 1 d PD G 2 O2A O 0.246(3) 0.7732(19) 0.858(3) 0.0718(10) Uani 0.12 1 d PD G 2 C1A C 0.3247(8) 1.033(2) 0.853(2) 0.0563(12) Uani 0.12 1 d PD G 2 C2A C 0.220(3) 0.842(2) 0.846(2) 0.0447(9) Uani 0.12 1 d PD G 2 C9 C -0.0460(3) 0.9974(2) 0.83911(17) 0.0355(6) Uani 0.88 1 d PD F 1 H9 H -0.1156 1.0181 0.8268 0.043 Uiso 0.88 1 calc PR F 1 N2 N 0.0468(2) 1.0713(2) 0.81615(18) 0.0334(7) Uani 0.88 1 d PD F 1 N1 N 0.1509(2) 1.0595(2) 0.82092(17) 0.0330(7) Uani 0.88 1 d PD F 1 C3 C 0.2143(4) 1.1417(3) 0.7966(2) 0.0434(9) Uani 0.88 1 d PD F 1 H3 H 0.2916 1.1547 0.7935 0.052 Uiso 0.88 1 calc PR F 1 C4 C 0.1515(4) 1.2044(3) 0.7768(2) 0.0507(11) Uani 0.88 1 d PD F 1 H4 H 0.1764 1.2668 0.7578 0.061 Uiso 0.88 1 calc PR F 1 C5 C 0.0458(4) 1.1578(3) 0.7901(2) 0.0438(10) Uani 0.88 1 d PD F 1 H5 H -0.0169 1.1825 0.7823 0.053 Uiso 0.88 1 calc PR F 1 C9A C -0.0460(3) 0.9974(2) 0.83911(17) 0.0355(6) Uani 0.12 1 d PD G 2 H9A H -0.1207 1.0100 0.8327 0.043 Uiso 0.12 1 calc PR G 2 N2A N 0.0152(15) 1.0745(16) 0.7994(15) 0.0334(7) Uani 0.12 1 d PD G 2 N1A N 0.1247(16) 1.0770(10) 0.8023(16) 0.0330(7) Uani 0.12 1 d PD G 2 C3A C 0.175(2) 1.1583(18) 0.7717(18) 0.0434(9) Uani 0.12 1 d PD G 2 H3A H 0.2498 1.1765 0.7628 0.052 Uiso 0.12 1 calc PR G 2 C4A C 0.099(2) 1.2109(19) 0.7553(19) 0.0507(11) Uani 0.12 1 d PD G 2 H4A H 0.1125 1.2713 0.7331 0.061 Uiso 0.12 1 calc PR G 2 C5A C 0.002(2) 1.1596(19) 0.777(2) 0.0438(10) Uani 0.12 1 d PD G 2 H5A H -0.0629 1.1806 0.7761 0.053 Uiso 0.12 1 calc PR G 2 N4 N -0.0709(6) 0.8974(4) 0.7945(6) 0.0317(11) Uani 0.88 1 d PD F 1 N3 N 0.0110(3) 0.8531(7) 0.7928(10) 0.0309(8) Uani 0.88 1 d PD F 1 C6 C -0.0429(8) 0.7604(7) 0.7505(7) 0.0394(19) Uani 0.88 1 d PD F 1 H6 H -0.0070 0.7123 0.7386 0.047 Uiso 0.88 1 calc PR F 1 C7 C -0.1589(8) 0.7448(6) 0.7264(4) 0.0451(18) Uani 0.88 1 d PD F 1 H7 H -0.2164 0.6850 0.6968 0.054 Uiso 0.88 1 calc PR F 1 C8 C -0.1729(5) 0.8336(4) 0.7542(7) 0.0416(11) Uani 0.88 1 d PD F 1 H8 H -0.2428 0.8477 0.7463 0.050 Uiso 0.88 1 calc PR F 1 N4A N -0.084(5) 0.893(3) 0.799(5) 0.0317(11) Uani 0.12 1 d PD G 2 N3A N 0.0033(17) 0.855(5) 0.796(7) 0.0309(8) Uani 0.12 1 d PD G 2 C6A C -0.042(6) 0.770(6) 0.744(6) 0.0394(19) Uani 0.12 1 d PD G 2 H6A H -0.0014 0.7278 0.7289 0.047 Uiso 0.12 1 calc PR G 2 C7A C -0.157(6) 0.753(5) 0.715(4) 0.0451(18) Uani 0.12 1 d PD G 2 H7A H -0.2079 0.7030 0.6746 0.054 Uiso 0.12 1 calc PR G 2 C8A C -0.183(3) 0.824(2) 0.759(5) 0.0416(11) Uani 0.12 1 d PD G 2 H8A H -0.2577 0.8252 0.7599 0.050 Uiso 0.12 1 calc PR G 2 C10 C -0.0172(2) 0.9977(2) 0.92288(16) 0.0317(6) Uani 1 1 d . . . C11 C 0.0593(3) 1.0829(2) 0.97155(18) 0.0415(7) Uani 1 1 d . . . H11 H 0.1003 1.1406 0.9523 0.050 Uiso 1 1 calc R . . C12 C -0.0772(3) 0.9144(2) 0.95219(18) 0.0399(7) Uani 1 1 d . . . H12 H -0.1309 0.8553 0.9195 0.048 Uiso 1 1 calc R . . B1 B 0.5101(2) 0.5349(2) 0.25689(15) 0.0230(5) Uani 1 1 d . . . F1 F 0.4492(2) 0.6850(4) 0.0052(2) 0.1011(17) Uani 0.76 1 d PD H 1 F2 F 0.6204(4) 0.78333(17) 0.0286(2) 0.0906(13) Uani 0.76 1 d PD H 1 F3 F 0.5636(3) 0.6557(3) -0.05251(12) 0.0649(10) Uani 0.76 1 d PD H 1 F1A F 0.6132(11) 0.6956(14) -0.0374(6) 0.1011(17) Uani 0.24 1 d PD H 2 F2A F 0.4478(4) 0.6429(7) -0.0212(8) 0.0906(13) Uani 0.24 1 d PD H 2 F3A F 0.5542(12) 0.7753(5) 0.0449(5) 0.0649(10) Uani 0.24 1 d PD H 2 F4 F 0.91609(17) 0.60451(18) 0.12039(14) 0.0649(6) Uani 1 1 d . . . F5 F 0.81447(19) 0.45392(17) 0.06458(12) 0.0599(6) Uani 1 1 d . . . F6 F 0.86058(19) 0.4823(2) 0.18354(13) 0.0720(7) Uani 1 1 d . . . F7 F 0.5234(3) 0.1779(2) 0.14814(17) 0.0706(9) Uani 0.82 1 d PD I 1 F8 F 0.3679(2) 0.1034(3) 0.1703(3) 0.1071(15) Uani 0.82 1 d PD I 1 F9 F 0.5192(5) 0.0894(3) 0.23224(19) 0.1058(15) Uani 0.82 1 d PD I 1 F7A F 0.4088(16) 0.0696(5) 0.2190(9) 0.0706(9) Uani 0.18 1 d PD I 2 F8A F 0.5736(7) 0.1402(14) 0.2132(12) 0.1071(15) Uani 0.18 1 d PD I 2 F9A F 0.436(3) 0.1576(16) 0.1334(3) 0.1058(15) Uani 0.18 1 d PD I 2 F10 F 0.5062(5) 0.2295(3) 0.48399(17) 0.0920(13) Uani 0.81 1 d PD J 1 F11 F 0.3747(3) 0.2895(6) 0.4659(2) 0.142(2) Uani 0.81 1 d PD J 1 F12 F 0.5439(5) 0.3869(2) 0.50870(14) 0.0957(14) Uani 0.81 1 d PD J 1 F110 F 0.4283(16) 0.3632(12) 0.4879(8) 0.0920(13) Uani 0.19 1 d PD J 2 F111 F 0.5790(6) 0.333(3) 0.5067(6) 0.142(2) Uani 0.19 1 d PD J 2 F112 F 0.424(2) 0.2126(6) 0.4673(8) 0.0957(14) Uani 0.19 1 d PD J 2 F13 F 0.9380(3) 0.8039(2) 0.5076(2) 0.1281(15) Uani 1 1 d . . . F14 F 0.9361(2) 0.6798(3) 0.43114(19) 0.1137(12) Uani 1 1 d . . . F15 F 0.8446(3) 0.6523(3) 0.51303(18) 0.1132(12) Uani 1 1 d . . . F16 F 0.7332(3) 0.99838(19) 0.3749(2) 0.1291(14) Uani 1 1 d . . . F17 F 0.5737(4) 0.9358(2) 0.4000(2) 0.1340(16) Uani 1 1 d . . . F18 F 0.5895(3) 0.92624(19) 0.28836(15) 0.0888(9) Uani 1 1 d . . . F19 F 0.0678(2) 0.45483(19) 0.04646(11) 0.0700(7) Uani 1 1 d . . . F20 F 0.00347(17) 0.3324(2) 0.10305(11) 0.0698(7) Uani 1 1 d . . . F21 F 0.14329(16) 0.33877(16) 0.05265(11) 0.0510(5) Uani 1 1 d . . . F22 F 0.1274(3) 0.5259(3) 0.38442(17) 0.1132(12) Uani 1 1 d . . . F23 F 0.0818(2) 0.6254(3) 0.31721(14) 0.0936(10) Uani 1 1 d . . . F24 F 0.2446(2) 0.6731(2) 0.39034(16) 0.0991(11) Uani 1 1 d . . . C13 C 0.5654(2) 0.55099(19) 0.18379(13) 0.0226(5) Uani 1 1 d . . . C14 C 0.5311(2) 0.60291(19) 0.12745(13) 0.0244(5) Uani 1 1 d . . . H14 H 0.4656 0.6227 0.1274 0.029 Uiso 1 1 calc R . . C15 C 0.5900(2) 0.6265(2) 0.07135(14) 0.0273(5) Uani 1 1 d . . . C16 C 0.6853(2) 0.5990(2) 0.06904(15) 0.0322(6) Uani 1 1 d . . . H16 H 0.7244 0.6139 0.0301 0.039 Uiso 1 1 calc R . . C17 C 0.7226(2) 0.5491(2) 0.12503(15) 0.0304(6) Uani 1 1 d . . . C18 C 0.6640(2) 0.5256(2) 0.18080(14) 0.0264(5) Uani 1 1 d . . . H18 H 0.6914 0.4911 0.2183 0.032 Uiso 1 1 calc R . . C19 C 0.55492(17) 0.68699(16) 0.01426(12) 0.0339(6) Uani 1 1 d . . . C20 C 0.8279(3) 0.5222(3) 0.12379(18) 0.0407(7) Uani 1 1 d . . . C21 C 0.5069(2) 0.42563(19) 0.28483(14) 0.0232(5) Uani 1 1 d . . . C22 C 0.4981(2) 0.3388(2) 0.23623(14) 0.0254(5) Uani 1 1 d . . . H22 H 0.5006 0.3446 0.1857 0.031 Uiso 1 1 calc R . . C23 C 0.4859(2) 0.2444(2) 0.25905(15) 0.0291(5) Uani 1 1 d . . . C24 C 0.4812(2) 0.2327(2) 0.33219(16) 0.0344(6) Uani 1 1 d . . . H24 H 0.4732 0.1682 0.3482 0.041 Uiso 1 1 calc R . . C25 C 0.4887(2) 0.3172(2) 0.38115(15) 0.0341(6) Uani 1 1 d . . . C26 C 0.5010(2) 0.4114(2) 0.35798(14) 0.0283(5) Uani 1 1 d . . . H26 H 0.5055 0.4681 0.3930 0.034 Uiso 1 1 calc R . . C27 C 0.47475(19) 0.1542(2) 0.20340(15) 0.0409(7) Uani 1 1 d . . . C28 C 0.4796(2) 0.30601(17) 0.45986(18) 0.0533(9) Uani 1 1 d . . . C29 C 0.5942(2) 0.6353(2) 0.31819(14) 0.0248(5) Uani 1 1 d . . . C30 C 0.6922(2) 0.6346(2) 0.36824(15) 0.0294(5) Uani 1 1 d . . . H30 H 0.7058 0.5715 0.3713 0.035 Uiso 1 1 calc R . . C31 C 0.7702(2) 0.7240(2) 0.41370(16) 0.0370(6) Uani 1 1 d . . . C32 C 0.7537(3) 0.8166(2) 0.41061(17) 0.0400(7) Uani 1 1 d . . . H32 H 0.8070 0.8775 0.4416 0.048 Uiso 1 1 calc R . . C33 C 0.6576(3) 0.8194(2) 0.36122(16) 0.0359(6) Uani 1 1 d . . . C34 C 0.5805(2) 0.7309(2) 0.31635(15) 0.0297(6) Uani 1 1 d . . . H34 H 0.5156 0.7352 0.2829 0.036 Uiso 1 1 calc R . . C35 C 0.8720(3) 0.7162(3) 0.4658(2) 0.0593(10) Uani 1 1 d . . . C36 C 0.6366(4) 0.9186(3) 0.3564(2) 0.0577(10) Uani 1 1 d . . . C37 C 0.3760(2) 0.52859(19) 0.24044(13) 0.0228(5) Uani 1 1 d . . . C38 C 0.2978(2) 0.47177(19) 0.17462(13) 0.0231(5) Uani 1 1 d . . . H38 H 0.3251 0.4428 0.1365 0.028 Uiso 1 1 calc R . . C39 C 0.1812(2) 0.4562(2) 0.16310(14) 0.0251(5) Uani 1 1 d . . . C40 C 0.1383(2) 0.4974(2) 0.21753(15) 0.0297(6) Uani 1 1 d . . . H40 H 0.0588 0.4874 0.2098 0.036 Uiso 1 1 calc R . . C41 C 0.2141(2) 0.5533(2) 0.28318(15) 0.0295(5) Uani 1 1 d . . . C42 C 0.3303(2) 0.5681(2) 0.29487(14) 0.0266(5) Uani 1 1 d . . . H42 H 0.3801 0.6061 0.3410 0.032 Uiso 1 1 calc R . . C43 C 0.1002(2) 0.3963(2) 0.09216(15) 0.0317(6) Uani 1 1 d . . . C44 C 0.1679(3) 0.5950(3) 0.34335(19) 0.0477(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.092(2) 0.0581(15) 0.0628(16) 0.0199(13) 0.0465(15) 0.0393(15) C45 0.101(4) 0.055(2) 0.066(3) 0.020(2) 0.032(2) 0.035(2) C46 0.054(2) 0.081(3) 0.052(2) 0.028(2) 0.0194(18) 0.032(2) C47 0.093(3) 0.067(3) 0.056(2) 0.007(2) 0.028(2) 0.032(2) C48 0.056(2) 0.052(2) 0.057(2) 0.0150(17) 0.0203(18) 0.0256(18) O4 0.094(3) 0.080(2) 0.119(3) 0.043(2) 0.070(3) 0.058(2) C49 0.094(3) 0.080(2) 0.119(3) 0.043(2) 0.070(3) 0.058(2) C50 0.094(3) 0.080(2) 0.119(3) 0.043(2) 0.070(3) 0.058(2) C51 0.094(3) 0.080(2) 0.119(3) 0.043(2) 0.070(3) 0.058(2) C52 0.094(3) 0.080(2) 0.119(3) 0.043(2) 0.070(3) 0.058(2) O4A 0.136(6) 0.106(5) 0.082(4) -0.006(3) 0.010(4) 0.086(5) C49A 0.136(6) 0.106(5) 0.082(4) -0.006(3) 0.010(4) 0.086(5) C50A 0.136(6) 0.106(5) 0.082(4) -0.006(3) 0.010(4) 0.086(5) C51A 0.136(6) 0.106(5) 0.082(4) -0.006(3) 0.010(4) 0.086(5) C52A 0.136(6) 0.106(5) 0.082(4) -0.006(3) 0.010(4) 0.086(5) O5 0.157(4) 0.095(3) 0.067(2) 0.025(2) 0.021(2) 0.060(3) C53 0.157(4) 0.095(3) 0.067(2) 0.025(2) 0.021(2) 0.060(3) C54 0.157(4) 0.095(3) 0.067(2) 0.025(2) 0.021(2) 0.060(3) C55 0.157(4) 0.095(3) 0.067(2) 0.025(2) 0.021(2) 0.060(3) C56 0.157(4) 0.095(3) 0.067(2) 0.025(2) 0.021(2) 0.060(3) O5A 0.223(10) 0.081(4) 0.064(4) 0.019(3) 0.036(4) 0.044(5) C53A 0.223(10) 0.081(4) 0.064(4) 0.019(3) 0.036(4) 0.044(5) C54A 0.223(10) 0.081(4) 0.064(4) 0.019(3) 0.036(4) 0.044(5) C55A 0.223(10) 0.081(4) 0.064(4) 0.019(3) 0.036(4) 0.044(5) C56A 0.223(10) 0.081(4) 0.064(4) 0.019(3) 0.036(4) 0.044(5) Ir1 0.02779(7) 0.03133(9) 0.04293(10) 0.00021(5) 0.01581(6) 0.00913(5) O1 0.0321(17) 0.072(3) 0.174(5) -0.055(3) -0.005(2) 0.0159(17) O2 0.056(2) 0.055(2) 0.122(3) 0.036(2) 0.0348(19) 0.029(2) C1 0.037(2) 0.044(2) 0.084(3) -0.018(2) 0.014(2) 0.0182(18) C2 0.0300(18) 0.045(3) 0.062(3) 0.010(2) 0.0201(17) 0.011(2) Ir2 0.02779(7) 0.03133(9) 0.04293(10) 0.00021(5) 0.01581(6) 0.00913(5) O1A 0.0321(17) 0.072(3) 0.174(5) -0.055(3) -0.005(2) 0.0159(17) O2A 0.056(2) 0.055(2) 0.122(3) 0.036(2) 0.0348(19) 0.029(2) C1A 0.037(2) 0.044(2) 0.084(3) -0.018(2) 0.014(2) 0.0182(18) C2A 0.0300(18) 0.045(3) 0.062(3) 0.010(2) 0.0201(17) 0.011(2) C9 0.0397(16) 0.0317(14) 0.0431(16) 0.0059(12) 0.0234(13) 0.0150(13) N2 0.0410(18) 0.0308(12) 0.0320(19) 0.0050(12) 0.0168(16) 0.0122(13) N1 0.0357(16) 0.0269(13) 0.038(2) 0.0009(11) 0.0216(14) 0.0064(11) C3 0.055(2) 0.0317(17) 0.041(2) -0.0012(15) 0.028(2) 0.0026(16) C4 0.077(3) 0.0318(18) 0.044(3) 0.0075(17) 0.030(2) 0.010(2) C5 0.068(3) 0.0337(16) 0.037(2) 0.0080(14) 0.021(2) 0.022(2) C9A 0.0397(16) 0.0317(14) 0.0431(16) 0.0059(12) 0.0234(13) 0.0150(13) N2A 0.0410(18) 0.0308(12) 0.0320(19) 0.0050(12) 0.0168(16) 0.0122(13) N1A 0.0357(16) 0.0269(13) 0.038(2) 0.0009(11) 0.0216(14) 0.0064(11) C3A 0.055(2) 0.0317(17) 0.041(2) -0.0012(15) 0.028(2) 0.0026(16) C4A 0.077(3) 0.0318(18) 0.044(3) 0.0075(17) 0.030(2) 0.010(2) C5A 0.068(3) 0.0337(16) 0.037(2) 0.0080(14) 0.021(2) 0.022(2) N4 0.030(2) 0.0335(13) 0.035(2) 0.0025(13) 0.0173(17) 0.0106(12) N3 0.0285(13) 0.0281(12) 0.038(2) 0.0002(10) 0.0178(17) 0.0083(12) C6 0.0410(17) 0.030(3) 0.046(3) 0.000(3) 0.0187(17) 0.0075(17) C7 0.0382(18) 0.040(2) 0.047(3) -0.001(2) 0.011(2) 0.0003(17) C8 0.029(2) 0.048(2) 0.047(3) 0.008(2) 0.0134(18) 0.0090(15) N4A 0.030(2) 0.0335(13) 0.035(2) 0.0025(13) 0.0173(17) 0.0106(12) N3A 0.0285(13) 0.0281(12) 0.038(2) 0.0002(10) 0.0178(17) 0.0083(12) C6A 0.0410(17) 0.030(3) 0.046(3) 0.000(3) 0.0187(17) 0.0075(17) C7A 0.0382(18) 0.040(2) 0.047(3) -0.001(2) 0.011(2) 0.0003(17) C8A 0.029(2) 0.048(2) 0.047(3) 0.008(2) 0.0134(18) 0.0090(15) C10 0.0367(15) 0.0286(13) 0.0387(15) 0.0046(11) 0.0225(12) 0.0156(12) C11 0.0502(19) 0.0300(14) 0.0453(17) 0.0075(13) 0.0271(15) 0.0051(13) C12 0.0448(18) 0.0287(14) 0.0449(17) 0.0009(12) 0.0223(14) 0.0052(13) B1 0.0202(13) 0.0293(14) 0.0220(13) 0.0050(11) 0.0072(11) 0.0106(11) F1 0.065(2) 0.198(5) 0.106(3) 0.117(3) 0.052(2) 0.091(3) F2 0.143(4) 0.0270(13) 0.067(2) 0.0053(13) -0.037(2) 0.0179(17) F3 0.119(3) 0.082(2) 0.0208(11) 0.0137(12) 0.0208(15) 0.067(2) F1A 0.065(2) 0.198(5) 0.106(3) 0.117(3) 0.052(2) 0.091(3) F2A 0.143(4) 0.0270(13) 0.067(2) 0.0053(13) -0.037(2) 0.0179(17) F3A 0.119(3) 0.082(2) 0.0208(11) 0.0137(12) 0.0208(15) 0.067(2) F4 0.0303(10) 0.0698(14) 0.0970(17) 0.0058(12) 0.0273(11) 0.0150(10) F5 0.0595(13) 0.0699(14) 0.0709(14) 0.0063(11) 0.0348(11) 0.0406(12) F6 0.0514(13) 0.138(2) 0.0673(14) 0.0499(15) 0.0333(11) 0.0679(15) F7 0.113(3) 0.0444(14) 0.0685(17) 0.0013(13) 0.0583(18) 0.0271(17) F8 0.0497(18) 0.100(3) 0.133(3) -0.080(3) 0.0201(19) 0.0000(18) F9 0.203(5) 0.078(2) 0.072(2) 0.0106(18) 0.016(3) 0.107(3) F7A 0.113(3) 0.0444(14) 0.0685(17) 0.0013(13) 0.0583(18) 0.0271(17) F8A 0.0497(18) 0.100(3) 0.133(3) -0.080(3) 0.0201(19) 0.0000(18) F9A 0.203(5) 0.078(2) 0.072(2) 0.0106(18) 0.016(3) 0.107(3) F10 0.192(4) 0.0677(19) 0.0394(17) 0.0331(15) 0.034(2) 0.064(2) F11 0.088(3) 0.304(7) 0.071(3) 0.085(4) 0.061(2) 0.079(4) F12 0.184(4) 0.0613(19) 0.0228(13) 0.0090(12) 0.0150(19) 0.019(2) F110 0.192(4) 0.0677(19) 0.0394(17) 0.0331(15) 0.034(2) 0.064(2) F111 0.088(3) 0.304(7) 0.071(3) 0.085(4) 0.061(2) 0.079(4) F112 0.184(4) 0.0613(19) 0.0228(13) 0.0090(12) 0.0150(19) 0.019(2) F13 0.091(2) 0.084(2) 0.147(3) -0.043(2) -0.079(2) 0.0243(17) F14 0.0596(17) 0.166(3) 0.110(2) -0.028(2) -0.0173(16) 0.067(2) F15 0.081(2) 0.143(3) 0.097(2) 0.053(2) -0.0258(17) 0.032(2) F16 0.131(3) 0.0303(13) 0.181(4) 0.0222(17) -0.021(3) -0.0023(15) F17 0.248(5) 0.096(2) 0.152(3) 0.057(2) 0.135(3) 0.126(3) F18 0.142(3) 0.0609(15) 0.0795(17) 0.0219(13) 0.0119(17) 0.0610(17) F19 0.0930(18) 0.0752(15) 0.0382(11) 0.0105(10) -0.0143(11) 0.0406(14) F20 0.0312(10) 0.1055(18) 0.0391(11) -0.0066(11) 0.0102(9) -0.0191(11) F21 0.0345(10) 0.0592(12) 0.0500(11) -0.0186(9) 0.0039(8) 0.0144(9) F22 0.163(3) 0.127(3) 0.094(2) 0.0317(19) 0.105(2) 0.062(2) F23 0.0715(17) 0.159(3) 0.0713(16) -0.0246(16) 0.0136(13) 0.0825(19) F24 0.0470(14) 0.133(2) 0.0945(19) -0.0680(18) 0.0196(13) 0.0217(15) C13 0.0196(11) 0.0268(12) 0.0218(12) 0.0018(9) 0.0056(9) 0.0084(10) C14 0.0231(12) 0.0281(12) 0.0228(12) 0.0004(10) 0.0057(10) 0.0105(10) C15 0.0293(13) 0.0316(13) 0.0212(12) 0.0020(10) 0.0060(10) 0.0111(11) C16 0.0351(15) 0.0430(16) 0.0252(13) 0.0080(11) 0.0151(12) 0.0168(13) C17 0.0250(13) 0.0431(15) 0.0285(14) 0.0060(12) 0.0113(11) 0.0160(12) C18 0.0244(13) 0.0322(13) 0.0256(13) 0.0056(10) 0.0072(10) 0.0128(11) C19 0.0431(17) 0.0364(15) 0.0237(13) 0.0040(11) 0.0068(12) 0.0165(13) C20 0.0332(16) 0.0593(19) 0.0421(17) 0.0151(15) 0.0203(14) 0.0244(15) C21 0.0165(11) 0.0306(13) 0.0240(12) 0.0048(10) 0.0056(9) 0.0092(10) C22 0.0217(12) 0.0321(13) 0.0245(12) 0.0049(10) 0.0061(10) 0.0113(10) C23 0.0232(13) 0.0310(13) 0.0337(14) 0.0046(11) 0.0063(11) 0.0103(11) C24 0.0339(15) 0.0335(14) 0.0379(15) 0.0128(12) 0.0083(12) 0.0122(12) C25 0.0328(15) 0.0412(16) 0.0289(14) 0.0112(12) 0.0082(12) 0.0111(13) C26 0.0270(13) 0.0334(14) 0.0255(13) 0.0041(11) 0.0081(11) 0.0106(11) C27 0.0451(18) 0.0331(15) 0.0479(18) 0.0051(13) 0.0146(15) 0.0162(14) C28 0.070(3) 0.054(2) 0.0442(19) 0.0220(17) 0.0248(18) 0.0211(19) C29 0.0241(13) 0.0303(13) 0.0226(12) 0.0055(10) 0.0118(10) 0.0089(10) C30 0.0247(13) 0.0356(14) 0.0278(13) 0.0027(11) 0.0074(11) 0.0102(11) C31 0.0278(14) 0.0432(16) 0.0342(15) 0.0012(13) 0.0069(12) 0.0057(12) C32 0.0380(17) 0.0351(15) 0.0371(16) -0.0011(12) 0.0111(13) -0.0006(13) C33 0.0445(17) 0.0285(14) 0.0336(15) 0.0046(11) 0.0158(13) 0.0072(12) C34 0.0307(14) 0.0328(14) 0.0281(13) 0.0084(11) 0.0105(11) 0.0111(11) C35 0.0383(19) 0.061(2) 0.059(2) -0.0104(19) -0.0129(17) 0.0103(18) C36 0.082(3) 0.0336(17) 0.058(2) 0.0074(16) 0.021(2) 0.0192(18) C37 0.0210(12) 0.0271(12) 0.0241(12) 0.0062(10) 0.0088(10) 0.0108(10) C38 0.0216(12) 0.0281(12) 0.0233(12) 0.0050(10) 0.0087(10) 0.0110(10) C39 0.0218(12) 0.0303(13) 0.0268(13) 0.0081(10) 0.0096(10) 0.0105(10) C40 0.0208(12) 0.0382(14) 0.0357(14) 0.0082(12) 0.0111(11) 0.0143(11) C41 0.0259(13) 0.0367(14) 0.0302(14) 0.0025(11) 0.0116(11) 0.0142(11) C42 0.0249(13) 0.0335(13) 0.0233(12) 0.0028(10) 0.0080(10) 0.0117(11) C43 0.0236(13) 0.0447(16) 0.0282(14) 0.0063(12) 0.0088(11) 0.0118(12) C44 0.0346(17) 0.068(2) 0.0415(18) -0.0096(16) 0.0153(14) 0.0204(16) _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 O3 C48 1.401(4) . ? O3 C45 1.409(5) . ? C45 C46 1.488(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.507(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.478(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O4 C49 1.413(4) . ? O4 C52 1.413(4) . ? C49 C50 1.463(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.463(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.463(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? O4A C52A 1.413(4) . ? O4A C49A 1.413(4) . ? C49A C50A 1.462(4) . ? C49A H49C 0.9900 . ? C49A H49D 0.9900 . ? C50A C51A 1.462(4) . ? C50A H50C 0.9900 . ? C50A H50D 0.9900 . ? C51A C52A 1.463(4) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C52A H52C 0.9900 . ? C52A H52D 0.9900 . ? O5 C56 1.447(6) . ? O5 C53 1.447(6) . ? C53 C54 1.468(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.549(16) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.468(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O5A C56A 1.447(6) . ? O5A C53A 1.448(6) . ? C53A C54A 1.468(7) . ? C53A H53C 0.9900 . ? C53A H53D 0.9900 . ? C54A C55A 1.549(16) . ? C54A H54C 0.9900 . ? C54A H54D 0.9900 . ? C55A C56A 1.468(7) . ? C55A H55C 0.9900 . ? C55A H55D 0.9900 . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? Ir1 C1 1.847(4) . ? Ir1 C2 1.855(4) . ? Ir1 N1 2.058(3) . ? Ir1 N3 2.067(5) . ? O1 C1 1.137(4) . ? O2 C2 1.136(4) . ? Ir2 C1A 1.847(4) . ? Ir2 C2A 1.855(4) . ? Ir2 N1A 2.058(3) . ? Ir2 N3A 2.067(4) . ? O1A C1A 1.137(4) . ? O2A C2A 1.137(4) . ? C9 N4 1.456(4) . ? C9 N2 1.458(4) . ? C9 C10 1.520(4) . ? C9 H9 1.0000 . ? N2 C5 1.338(4) . ? N2 N1 1.363(4) . ? N1 C3 1.344(4) . ? C3 C4 1.380(7) . ? C3 H3 0.9500 . ? C4 C5 1.369(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? N2A C5A 1.338(4) . ? N2A N1A 1.363(4) . ? N1A C3A 1.344(4) . ? C3A C4A 1.380(7) . ? C3A H3A 0.9500 . ? C4A C5A 1.369(6) . ? C4A H4A 0.9500 . ? C5A H5A 0.9500 . ? N4 C8 1.341(5) . ? N4 N3 1.362(4) . ? N3 C6 1.339(5) . ? C6 C7 1.387(5) . ? C6 H6 0.9500 . ? C7 C8 1.367(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? N4A C8A 1.343(17) . ? N4A N3A 1.362(4) . ? N3A C6A 1.339(5) . ? C6A C7A 1.387(5) . ? C6A H6A 0.9500 . ? C7A C8A 1.367(6) . ? C7A H7A 0.9500 . ? C8A H8A 0.9500 . ? C10 C11 1.377(4) . ? C10 C12 1.391(4) . ? C11 C12 1.378(4) 2_577 ? C11 H11 0.9500 . ? C12 C11 1.378(4) 2_577 ? C12 H12 0.9500 . ? B1 C29 1.636(4) . ? B1 C37 1.636(4) . ? B1 C13 1.637(3) . ? B1 C21 1.639(4) . ? F1 C19 1.3043(18) . ? F2 C19 1.3052(18) . ? F3 C19 1.3050(18) . ? F1A C19 1.3047(19) . ? F2A C19 1.3049(19) . ? F3A C19 1.3046(19) . ? F4 C20 1.340(4) . ? F5 C20 1.326(4) . ? F6 C20 1.334(4) . ? F7 C27 1.305(2) . ? F8 C27 1.305(2) . ? F9 C27 1.304(2) . ? F7A C27 1.305(2) . ? F8A C27 1.304(2) . ? F9A C27 1.304(2) . ? F10 C28 1.302(2) . ? F11 C28 1.302(2) . ? F12 C28 1.302(2) . ? F110 C28 1.302(2) . ? F111 C28 1.302(2) . ? F112 C28 1.302(2) . ? F13 C35 1.310(5) . ? F14 C35 1.309(5) . ? F15 C35 1.318(5) . ? F16 C36 1.326(5) . ? F17 C36 1.289(5) . ? F18 C36 1.314(5) . ? F19 C43 1.322(3) . ? F20 C43 1.330(3) . ? F21 C43 1.334(3) . ? F22 C44 1.317(5) . ? F23 C44 1.312(4) . ? F24 C44 1.309(4) . ? C13 C14 1.399(3) . ? C13 C18 1.405(3) . ? C14 C15 1.393(3) . ? C14 H14 0.9500 . ? C15 C16 1.378(4) . ? C15 C19 1.495(4) . ? C16 C17 1.388(4) . ? C16 H16 0.9500 . ? C17 C18 1.384(3) . ? C17 C20 1.493(4) . ? C18 H18 0.9500 . ? C21 C22 1.395(4) . ? C21 C26 1.396(3) . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 C27 1.497(4) . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.388(4) . ? C25 C28 1.498(4) . ? C26 H26 0.9500 . ? C29 C34 1.395(4) . ? C29 C30 1.400(4) . ? C30 C31 1.394(4) . ? C30 H30 0.9500 . ? C31 C32 1.371(4) . ? C31 C35 1.491(5) . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 C34 1.378(4) . ? C33 C36 1.489(4) . ? C34 H34 0.9500 . ? C37 C38 1.397(4) . ? C37 C42 1.400(3) . ? C38 C39 1.390(3) . ? C38 H38 0.9500 . ? C39 C40 1.387(4) . ? C39 C43 1.486(4) . ? C40 C41 1.381(4) . ? C40 H40 0.9500 . ? C41 C42 1.387(4) . ? C41 C44 1.499(4) . ? C42 H42 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C48 O3 C45 107.6(3) . . ? O3 C45 C46 108.8(3) . . ? O3 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? O3 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C45 C46 C47 103.3(3) . . ? C45 C46 H46A 111.1 . . ? C47 C46 H46A 111.1 . . ? C45 C46 H46B 111.1 . . ? C47 C46 H46B 111.1 . . ? H46A C46 H46B 109.1 . . ? C48 C47 C46 103.3(3) . . ? C48 C47 H47A 111.1 . . ? C46 C47 H47A 111.1 . . ? C48 C47 H47B 111.1 . . ? C46 C47 H47B 111.1 . . ? H47A C47 H47B 109.1 . . ? O3 C48 C47 105.8(3) . . ? O3 C48 H48A 110.6 . . ? C47 C48 H48A 110.6 . . ? O3 C48 H48B 110.6 . . ? C47 C48 H48B 110.6 . . ? H48A C48 H48B 108.7 . . ? C49 O4 C52 106.5(5) . . ? O4 C49 C50 108.7(5) . . ? O4 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O4 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? C51 C50 C49 100.8(5) . . ? C51 C50 H50A 111.6 . . ? C49 C50 H50A 111.6 . . ? C51 C50 H50B 111.6 . . ? C49 C50 H50B 111.6 . . ? H50A C50 H50B 109.4 . . ? C52 C51 C50 109.6(6) . . ? C52 C51 H51A 109.7 . . ? C50 C51 H51A 109.7 . . ? C52 C51 H51B 109.7 . . ? C50 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? O4 C52 C51 105.7(5) . . ? O4 C52 H52A 110.6 . . ? C51 C52 H52A 110.6 . . ? O4 C52 H52B 110.6 . . ? C51 C52 H52B 110.6 . . ? H52A C52 H52B 108.7 . . ? C52A O4A C49A 112.4(10) . . ? O4A C49A C50A 103.5(10) . . ? O4A C49A H49C 111.1 . . ? C50A C49A H49C 111.1 . . ? O4A C49A H49D 111.1 . . ? C50A C49A H49D 111.1 . . ? H49C C49A H49D 109.0 . . ? C49A C50A C51A 109.6(10) . . ? C49A C50A H50C 109.7 . . ? C51A C50A H50C 109.7 . . ? C49A C50A H50D 109.7 . . ? C51A C50A H50D 109.7 . . ? H50C C50A H50D 108.2 . . ? C50A C51A C52A 103.5(11) . . ? C50A C51A H51C 111.1 . . ? C52A C51A H51C 111.1 . . ? C50A C51A H51D 111.1 . . ? C52A C51A H51D 111.1 . . ? H51C C51A H51D 109.0 . . ? O4A C52A C51A 106.4(10) . . ? O4A C52A H52C 110.4 . . ? C51A C52A H52C 110.4 . . ? O4A C52A H52D 110.4 . . ? C51A C52A H52D 110.4 . . ? H52C C52A H52D 108.6 . . ? C56 O5 C53 108.1(6) . . ? O5 C53 C54 109.1(8) . . ? O5 C53 H53A 109.9 . . ? C54 C53 H53A 109.9 . . ? O5 C53 H53B 109.9 . . ? C54 C53 H53B 109.9 . . ? H53A C53 H53B 108.3 . . ? C53 C54 C55 100.9(8) . . ? C53 C54 H54A 111.6 . . ? C55 C54 H54A 111.6 . . ? C53 C54 H54B 111.6 . . ? C55 C54 H54B 111.6 . . ? H54A C54 H54B 109.4 . . ? C56 C55 C54 105.4(8) . . ? C56 C55 H55A 110.7 . . ? C54 C55 H55A 110.7 . . ? C56 C55 H55B 110.7 . . ? C54 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? O5 C56 C55 106.8(7) . . ? O5 C56 H56A 110.4 . . ? C55 C56 H56A 110.4 . . ? O5 C56 H56B 110.4 . . ? C55 C56 H56B 110.4 . . ? H56A C56 H56B 108.6 . . ? C56A O5A C53A 108.9(11) . . ? O5A C53A C54A 107.9(10) . . ? O5A C53A H53C 110.1 . . ? C54A C53A H53C 110.1 . . ? O5A C53A H53D 110.1 . . ? C54A C53A H53D 110.1 . . ? H53C C53A H53D 108.4 . . ? C53A C54A C55A 101.3(11) . . ? C53A C54A H54C 111.5 . . ? C55A C54A H54C 111.5 . . ? C53A C54A H54D 111.5 . . ? C55A C54A H54D 111.5 . . ? H54C C54A H54D 109.3 . . ? C56A C55A C54A 110.7(12) . . ? C56A C55A H55C 109.5 . . ? C54A C55A H55C 109.5 . . ? C56A C55A H55D 109.5 . . ? C54A C55A H55D 109.5 . . ? H55C C55A H55D 108.1 . . ? O5A C56A C55A 102.0(12) . . ? O5A C56A H56C 111.4 . . ? C55A C56A H56C 111.4 . . ? O5A C56A H56D 111.4 . . ? C55A C56A H56D 111.4 . . ? H56C C56A H56D 109.2 . . ? C1 Ir1 C2 87.5(2) . . ? C1 Ir1 N1 93.25(17) . . ? C2 Ir1 N1 177.46(17) . . ? C1 Ir1 N3 178.0(6) . . ? C2 Ir1 N3 93.8(4) . . ? N1 Ir1 N3 85.3(4) . . ? O1 C1 Ir1 178.2(4) . . ? O2 C2 Ir1 177.5(3) . . ? C1A Ir2 C2A 86.9(16) . . ? C1A Ir2 N1A 91.3(12) . . ? C2A Ir2 N1A 178.1(13) . . ? C1A Ir2 N3A 177(4) . . ? C2A Ir2 N3A 90(3) . . ? N1A Ir2 N3A 92(3) . . ? O1A C1A Ir2 178(4) . . ? O2A C2A Ir2 178(3) . . ? N4 C9 N2 107.9(4) . . ? N4 C9 C10 113.6(5) . . ? N2 C9 C10 111.4(3) . . ? N4 C9 H9 107.9 . . ? N2 C9 H9 107.9 . . ? C10 C9 H9 107.9 . . ? C5 N2 N1 110.7(3) . . ? C5 N2 C9 127.5(3) . . ? N1 N2 C9 121.7(3) . . ? C3 N1 N2 105.2(3) . . ? C3 N1 Ir1 130.0(3) . . ? N2 N1 Ir1 123.8(2) . . ? N1 C3 C4 110.6(3) . . ? N1 C3 H3 124.7 . . ? C4 C3 H3 124.7 . . ? C5 C4 C3 105.7(3) . . ? C5 C4 H4 127.2 . . ? C3 C4 H4 127.2 . . ? N2 C5 C4 107.8(4) . . ? N2 C5 H5 126.1 . . ? C4 C5 H5 126.1 . . ? C5A N2A N1A 109.7(11) . . ? C3A N1A N2A 106.8(11) . . ? C3A N1A Ir2 130.8(15) . . ? N2A N1A Ir2 120.5(11) . . ? N1A C3A C4A 108.5(13) . . ? N1A C3A H3A 125.7 . . ? C4A C3A H3A 125.7 . . ? C5A C4A C3A 107.1(15) . . ? C5A C4A H4A 126.5 . . ? C3A C4A H4A 126.5 . . ? N2A C5A C4A 107.2(13) . . ? N2A C5A H5A 126.4 . . ? C4A C5A H5A 126.4 . . ? C8 N4 N3 110.2(3) . . ? C8 N4 C9 127.6(5) . . ? N3 N4 C9 122.1(6) . . ? C6 N3 N4 105.8(3) . . ? C6 N3 Ir1 130.4(5) . . ? N4 N3 Ir1 123.6(5) . . ? N3 C6 C7 110.3(4) . . ? N3 C6 H6 124.9 . . ? C7 C6 H6 124.9 . . ? C8 C7 C6 105.5(4) . . ? C8 C7 H7 127.3 . . ? C6 C7 H7 127.3 . . ? N4 C8 C7 108.1(4) . . ? N4 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? C8A N4A N3A 109.8(16) . . ? C6A N3A N4A 105.8(18) . . ? C6A N3A Ir2 127(6) . . ? N4A N3A Ir2 121(4) . . ? N3A C6A C7A 110.0(17) . . ? N3A C6A H6A 125.0 . . ? C7A C6A H6A 125.0 . . ? C8A C7A C6A 105.3(18) . . ? C8A C7A H7A 127.3 . . ? C6A C7A H7A 127.3 . . ? N4A C8A C7A 107(2) . . ? N4A C8A H8A 126.3 . . ? C7A C8A H8A 126.3 . . ? C11 C10 C12 118.6(3) . . ? C11 C10 C9 121.5(2) . . ? C12 C10 C9 119.5(3) . . ? C10 C11 C12 121.0(3) . 2_577 ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 2_577 . ? C11 C12 C10 120.4(3) 2_577 . ? C11 C12 H12 119.8 2_577 . ? C10 C12 H12 119.8 . . ? C29 B1 C37 112.4(2) . . ? C29 B1 C13 102.45(19) . . ? C37 B1 C13 113.2(2) . . ? C29 B1 C21 113.2(2) . . ? C37 B1 C21 103.72(19) . . ? C13 B1 C21 112.2(2) . . ? C14 C13 C18 115.8(2) . . ? C14 C13 B1 123.9(2) . . ? C18 C13 B1 119.7(2) . . ? C15 C14 C13 122.0(2) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C16 C15 C14 121.0(2) . . ? C16 C15 C19 118.2(2) . . ? C14 C15 C19 120.7(2) . . ? C15 C16 C17 118.3(2) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 120.8(2) . . ? C18 C17 C20 121.0(2) . . ? C16 C17 C20 118.2(2) . . ? C17 C18 C13 122.2(2) . . ? C17 C18 H18 118.9 . . ? C13 C18 H18 118.9 . . ? F3A C19 F1A 112.7(9) . . ? F3A C19 F2A 101.6(8) . . ? F1A C19 F2A 105.5(9) . . ? F1 C19 F3 104.6(3) . . ? F1 C19 F2 107.3(3) . . ? F3 C19 F2 103.5(3) . . ? F1 C19 C15 114.8(2) . . ? F3A C19 C15 112.1(4) . . ? F1A C19 C15 112.9(6) . . ? F2A C19 C15 111.3(6) . . ? F3 C19 C15 113.2(2) . . ? F2 C19 C15 112.5(2) . . ? F5 C20 F6 106.2(3) . . ? F5 C20 F4 105.4(2) . . ? F6 C20 F4 107.9(3) . . ? F5 C20 C17 112.7(3) . . ? F6 C20 C17 112.7(2) . . ? F4 C20 C17 111.5(3) . . ? C22 C21 C26 115.8(2) . . ? C22 C21 B1 122.8(2) . . ? C26 C21 B1 121.1(2) . . ? C23 C22 C21 122.4(2) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C24 C23 C22 120.6(3) . . ? C24 C23 C27 120.0(2) . . ? C22 C23 C27 119.4(2) . . ? C25 C24 C23 118.1(2) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C26 121.0(2) . . ? C24 C25 C28 119.4(2) . . ? C26 C25 C28 119.6(2) . . ? C25 C26 C21 122.0(3) . . ? C25 C26 H26 119.0 . . ? C21 C26 H26 119.0 . . ? F9A C27 F8A 110.8(15) . . ? F9A C27 F7A 107.5(14) . . ? F8A C27 F7A 102.4(12) . . ? F9 C27 F8 107.8(4) . . ? F9 C27 F7 104.8(3) . . ? F8 C27 F7 103.7(3) . . ? F9 C27 C23 113.6(2) . . ? F9A C27 C23 116.5(6) . . ? F8A C27 C23 108.4(7) . . ? F7A C27 C23 110.4(6) . . ? F8 C27 C23 111.7(2) . . ? F7 C27 C23 114.5(2) . . ? F110 C28 F112 105.7(13) . . ? F110 C28 F111 103.6(14) . . ? F112 C28 F111 106.3(16) . . ? F11 C28 F12 106.8(4) . . ? F11 C28 F10 105.1(4) . . ? F12 C28 F10 105.4(3) . . ? F11 C28 C25 110.4(3) . . ? F110 C28 C25 113.9(6) . . ? F112 C28 C25 113.5(7) . . ? F111 C28 C25 113.0(7) . . ? F12 C28 C25 113.5(2) . . ? F10 C28 C25 114.9(2) . . ? C34 C29 C30 115.8(2) . . ? C34 C29 B1 121.0(2) . . ? C30 C29 B1 122.7(2) . . ? C31 C30 C29 121.8(3) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 120.8(3) . . ? C32 C31 C35 120.9(3) . . ? C30 C31 C35 118.4(3) . . ? C31 C32 C33 118.5(3) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 C36 119.4(3) . . ? C32 C33 C36 120.0(3) . . ? C33 C34 C29 122.5(3) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? F14 C35 F13 107.6(4) . . ? F14 C35 F15 103.7(4) . . ? F13 C35 F15 105.3(4) . . ? F14 C35 C31 112.8(3) . . ? F13 C35 C31 113.5(3) . . ? F15 C35 C31 113.2(3) . . ? F17 C36 F18 107.9(4) . . ? F17 C36 F16 106.1(4) . . ? F18 C36 F16 103.7(3) . . ? F17 C36 C33 113.2(3) . . ? F18 C36 C33 113.2(3) . . ? F16 C36 C33 112.1(4) . . ? C38 C37 C42 116.3(2) . . ? C38 C37 B1 121.2(2) . . ? C42 C37 B1 122.0(2) . . ? C39 C38 C37 122.1(2) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C40 C39 C38 120.5(2) . . ? C40 C39 C43 118.6(2) . . ? C38 C39 C43 120.9(2) . . ? C41 C40 C39 118.3(2) . . ? C41 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? C40 C41 C42 121.2(2) . . ? C40 C41 C44 118.7(2) . . ? C42 C41 C44 120.2(3) . . ? C41 C42 C37 121.7(2) . . ? C41 C42 H42 119.2 . . ? C37 C42 H42 119.2 . . ? F19 C43 F20 105.2(2) . . ? F19 C43 F21 105.6(2) . . ? F20 C43 F21 106.1(3) . . ? F19 C43 C39 113.0(2) . . ? F20 C43 C39 112.8(2) . . ? F21 C43 C39 113.4(2) . . ? F24 C44 F23 106.5(3) . . ? F24 C44 F22 105.8(3) . . ? F23 C44 F22 104.6(3) . . ? F24 C44 C41 113.5(3) . . ? F23 C44 C41 113.2(3) . . ? F22 C44 C41 112.5(3) . . ? 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 C48 O3 C45 C46 14.9(5) . . . . ? O3 C45 C46 C47 6.4(5) . . . . ? C45 C46 C47 C48 -23.8(5) . . . . ? C45 O3 C48 C47 -30.6(5) . . . . ? C46 C47 C48 O3 33.8(4) . . . . ? C52 O4 C49 C50 -30.0(12) . . . . ? O4 C49 C50 C51 28.1(11) . . . . ? C49 C50 C51 C52 -16.4(11) . . . . ? C49 O4 C52 C51 18.2(11) . . . . ? C50 C51 C52 O4 -0.5(12) . . . . ? C52A O4A C49A C50A 2(2) . . . . ? O4A C49A C50A C51A 12(2) . . . . ? C49A C50A C51A C52A -20(2) . . . . ? C49A O4A C52A C51A -15(2) . . . . ? C50A C51A C52A O4A 21(2) . . . . ? C56 O5 C53 C54 -14.4(12) . . . . ? O5 C53 C54 C55 27.5(11) . . . . ? C53 C54 C55 C56 -30.8(11) . . . . ? C53 O5 C56 C55 -6.4(12) . . . . ? C54 C55 C56 O5 23.5(11) . . . . ? C56A O5A C53A C54A -31.1(17) . . . . ? O5A C53A C54A C55A 17.9(17) . . . . ? C53A C54A C55A C56A 0.1(19) . . . . ? C53A O5A C56A C55A 29.3(15) . . . . ? C54A C55A C56A O5A -17.6(18) . . . . ? N4 C9 N2 C5 122.6(6) . . . . ? C10 C9 N2 C5 -112.1(4) . . . . ? N4 C9 N2 N1 -59.0(6) . . . . ? C10 C9 N2 N1 66.3(4) . . . . ? C5 N2 N1 C3 -0.2(4) . . . . ? C9 N2 N1 C3 -178.9(3) . . . . ? C5 N2 N1 Ir1 -169.8(3) . . . . ? C9 N2 N1 Ir1 11.5(5) . . . . ? C1 Ir1 N1 C3 39.2(4) . . . . ? N3 Ir1 N1 C3 -139.4(6) . . . . ? C1 Ir1 N1 N2 -154.0(3) . . . . ? N3 Ir1 N1 N2 27.5(5) . . . . ? N2 N1 C3 C4 0.0(4) . . . . ? Ir1 N1 C3 C4 168.7(3) . . . . ? N1 C3 C4 C5 0.2(5) . . . . ? N1 N2 C5 C4 0.4(5) . . . . ? C9 N2 C5 C4 179.0(4) . . . . ? C3 C4 C5 N2 -0.4(5) . . . . ? C5A N2A N1A C3A -8(4) . . . . ? C5A N2A N1A Ir2 -174(2) . . . . ? C1A Ir2 N1A C3A 38(3) . . . . ? N3A Ir2 N1A C3A -143(5) . . . . ? C1A Ir2 N1A N2A -160(3) . . . . ? N3A Ir2 N1A N2A 19(4) . . . . ? N2A N1A C3A C4A 5(4) . . . . ? Ir2 N1A C3A C4A 169(2) . . . . ? N1A C3A C4A C5A 0(4) . . . . ? N1A N2A C5A C4A 8(4) . . . . ? C3A C4A C5A N2A -5(4) . . . . ? N2 C9 N4 C8 -127.7(9) . . . . ? C10 C9 N4 C8 108.3(9) . . . . ? N2 C9 N4 N3 56.7(12) . . . . ? C10 C9 N4 N3 -67.3(11) . . . . ? C8 N4 N3 C6 0.0(15) . . . . ? C9 N4 N3 C6 176.3(11) . . . . ? C8 N4 N3 Ir1 176.1(10) . . . . ? C9 N4 N3 Ir1 -7.5(17) . . . . ? C2 Ir1 N3 C6 -31.9(16) . . . . ? N1 Ir1 N3 C6 145.7(16) . . . . ? C2 Ir1 N3 N4 153.0(13) . . . . ? N1 Ir1 N3 N4 -29.5(12) . . . . ? N4 N3 C6 C7 -1.1(16) . . . . ? Ir1 N3 C6 C7 -176.9(12) . . . . ? N3 C6 C7 C8 1.7(14) . . . . ? N3 N4 C8 C7 1.1(12) . . . . ? C9 N4 C8 C7 -175.0(10) . . . . ? C6 C7 C8 N4 -1.7(10) . . . . ? C8A N4A N3A C6A 9(12) . . . . ? C8A N4A N3A Ir2 163(8) . . . . ? C2A Ir2 N3A C6A -56(11) . . . . ? N1A Ir2 N3A C6A 124(10) . . . . ? C2A Ir2 N3A N4A 156(9) . . . . ? N1A Ir2 N3A N4A -24(9) . . . . ? N4A N3A C6A C7A -1(13) . . . . ? Ir2 N3A C6A C7A -152(9) . . . . ? N3A C6A C7A C8A -7(12) . . . . ? N3A N4A C8A C7A -14(10) . . . . ? C6A C7A C8A N4A 13(10) . . . . ? N4 C9 C10 C11 147.3(4) . . . . ? N2 C9 C10 C11 25.2(4) . . . . ? N4 C9 C10 C12 -39.2(4) . . . . ? N2 C9 C10 C12 -161.2(3) . . . . ? C12 C10 C11 C12 0.6(5) . . . 2_577 ? C9 C10 C11 C12 174.2(3) . . . 2_577 ? C11 C10 C12 C11 -0.6(5) . . . 2_577 ? C9 C10 C12 C11 -174.3(3) . . . 2_577 ? C29 B1 C13 C14 -91.4(3) . . . . ? C37 B1 C13 C14 30.0(3) . . . . ? C21 B1 C13 C14 146.9(2) . . . . ? C29 B1 C13 C18 78.9(3) . . . . ? C37 B1 C13 C18 -159.7(2) . . . . ? C21 B1 C13 C18 -42.8(3) . . . . ? C18 C13 C14 C15 0.9(4) . . . . ? B1 C13 C14 C15 171.5(2) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C13 C14 C15 C19 -176.7(2) . . . . ? C14 C15 C16 C17 -1.3(4) . . . . ? C19 C15 C16 C17 175.7(2) . . . . ? C15 C16 C17 C18 1.3(4) . . . . ? C15 C16 C17 C20 -178.2(3) . . . . ? C16 C17 C18 C13 -0.2(4) . . . . ? C20 C17 C18 C13 179.3(3) . . . . ? C14 C13 C18 C17 -0.9(4) . . . . ? B1 C13 C18 C17 -172.0(2) . . . . ? C16 C15 C19 F1 161.0(3) . . . . ? C14 C15 C19 F1 -22.0(4) . . . . ? C16 C15 C19 F3A -120.7(7) . . . . ? C14 C15 C19 F3A 56.3(7) . . . . ? C16 C15 C19 F1A 7.9(9) . . . . ? C14 C15 C19 F1A -175.1(9) . . . . ? C16 C15 C19 F2A 126.3(7) . . . . ? C14 C15 C19 F2A -56.7(7) . . . . ? C16 C15 C19 F3 40.9(4) . . . . ? C14 C15 C19 F3 -142.1(3) . . . . ? C16 C15 C19 F2 -76.0(4) . . . . ? C14 C15 C19 F2 101.0(3) . . . . ? C18 C17 C20 F5 115.5(3) . . . . ? C16 C17 C20 F5 -65.0(4) . . . . ? C18 C17 C20 F6 -4.7(4) . . . . ? C16 C17 C20 F6 174.8(3) . . . . ? C18 C17 C20 F4 -126.2(3) . . . . ? C16 C17 C20 F4 53.3(4) . . . . ? C29 B1 C21 C22 -144.2(2) . . . . ? C37 B1 C21 C22 93.7(3) . . . . ? C13 B1 C21 C22 -28.8(3) . . . . ? C29 B1 C21 C26 42.6(3) . . . . ? C37 B1 C21 C26 -79.6(3) . . . . ? C13 B1 C21 C26 157.9(2) . . . . ? C26 C21 C22 C23 -0.9(4) . . . . ? B1 C21 C22 C23 -174.5(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C21 C22 C23 C27 178.9(2) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C27 C23 C24 C25 -178.2(2) . . . . ? C23 C24 C25 C26 -0.3(4) . . . . ? C23 C24 C25 C28 177.8(2) . . . . ? C24 C25 C26 C21 -0.3(4) . . . . ? C28 C25 C26 C21 -178.4(2) . . . . ? C22 C21 C26 C25 0.8(4) . . . . ? B1 C21 C26 C25 174.6(2) . . . . ? C24 C23 C27 F9 -33.8(4) . . . . ? C22 C23 C27 F9 147.7(4) . . . . ? C24 C23 C27 F9A 154.2(16) . . . . ? C22 C23 C27 F9A -24.3(17) . . . . ? C24 C23 C27 F8A -80.1(12) . . . . ? C22 C23 C27 F8A 101.4(12) . . . . ? C24 C23 C27 F7A 31.4(11) . . . . ? C22 C23 C27 F7A -147.2(11) . . . . ? C24 C23 C27 F8 88.4(4) . . . . ? C22 C23 C27 F8 -90.2(4) . . . . ? C24 C23 C27 F7 -154.2(3) . . . . ? C22 C23 C27 F7 27.3(4) . . . . ? C24 C25 C28 F11 -95.0(5) . . . . ? C26 C25 C28 F11 83.2(5) . . . . ? C24 C25 C28 F110 -145.3(10) . . . . ? C26 C25 C28 F110 32.8(11) . . . . ? C24 C25 C28 F112 -24.3(14) . . . . ? C26 C25 C28 F112 153.8(14) . . . . ? C24 C25 C28 F111 96.8(18) . . . . ? C26 C25 C28 F111 -85.1(18) . . . . ? C24 C25 C28 F12 145.1(4) . . . . ? C26 C25 C28 F12 -36.8(4) . . . . ? C24 C25 C28 F10 23.6(4) . . . . ? C26 C25 C28 F10 -158.3(4) . . . . ? C37 B1 C29 C34 -41.7(3) . . . . ? C13 B1 C29 C34 80.1(3) . . . . ? C21 B1 C29 C34 -158.9(2) . . . . ? C37 B1 C29 C30 147.3(2) . . . . ? C13 B1 C29 C30 -90.9(3) . . . . ? C21 B1 C29 C30 30.1(3) . . . . ? C34 C29 C30 C31 0.6(4) . . . . ? B1 C29 C30 C31 172.0(2) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C29 C30 C31 C35 179.6(3) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? C35 C31 C32 C33 -179.9(3) . . . . ? C31 C32 C33 C34 0.0(4) . . . . ? C31 C32 C33 C36 179.8(3) . . . . ? C32 C33 C34 C29 0.3(4) . . . . ? C36 C33 C34 C29 -179.5(3) . . . . ? C30 C29 C34 C33 -0.6(4) . . . . ? B1 C29 C34 C33 -172.2(2) . . . . ? C32 C31 C35 F14 -120.8(4) . . . . ? C30 C31 C35 F14 59.3(5) . . . . ? C32 C31 C35 F13 1.9(5) . . . . ? C30 C31 C35 F13 -178.0(4) . . . . ? C32 C31 C35 F15 121.9(4) . . . . ? C30 C31 C35 F15 -58.1(5) . . . . ? C34 C33 C36 F17 87.6(4) . . . . ? C32 C33 C36 F17 -92.2(5) . . . . ? C34 C33 C36 F18 -35.6(5) . . . . ? C32 C33 C36 F18 144.6(3) . . . . ? C34 C33 C36 F16 -152.4(3) . . . . ? C32 C33 C36 F16 27.8(5) . . . . ? C29 B1 C37 C38 158.4(2) . . . . ? C13 B1 C37 C38 42.9(3) . . . . ? C21 B1 C37 C38 -78.9(3) . . . . ? C29 B1 C37 C42 -29.9(3) . . . . ? C13 B1 C37 C42 -145.5(2) . . . . ? C21 B1 C37 C42 92.7(3) . . . . ? C42 C37 C38 C39 0.8(3) . . . . ? B1 C37 C38 C39 172.9(2) . . . . ? C37 C38 C39 C40 0.1(4) . . . . ? C37 C38 C39 C43 179.4(2) . . . . ? C38 C39 C40 C41 -0.4(4) . . . . ? C43 C39 C40 C41 -179.8(2) . . . . ? C39 C40 C41 C42 -0.1(4) . . . . ? C39 C40 C41 C44 -177.9(3) . . . . ? C40 C41 C42 C37 1.0(4) . . . . ? C44 C41 C42 C37 178.8(3) . . . . ? C38 C37 C42 C41 -1.3(4) . . . . ? B1 C37 C42 C41 -173.3(2) . . . . ? C40 C39 C43 F19 76.2(3) . . . . ? C38 C39 C43 F19 -103.1(3) . . . . ? C40 C39 C43 F20 -42.9(4) . . . . ? C38 C39 C43 F20 137.7(3) . . . . ? C40 C39 C43 F21 -163.6(2) . . . . ? C38 C39 C43 F21 17.0(4) . . . . ? C40 C41 C44 F24 -157.9(3) . . . . ? C42 C41 C44 F24 24.3(5) . . . . ? C40 C41 C44 F23 -36.3(4) . . . . ? C42 C41 C44 F23 145.9(3) . . . . ? C40 C41 C44 F22 82.1(4) . . . . ? C42 C41 C44 F22 -95.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.808 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.079 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 798122' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 Ir2 N8, 2(C32 H12 B F24), 0.2(C H2 Cl2)' _chemical_formula_sum 'C100.20 H66.40 B2 Cl0.40 F48 Ir2 N8' _chemical_formula_weight 2714.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.1567(3) _cell_length_b 26.1697(5) _cell_length_c 15.2518(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.4040(10) _cell_angle_gamma 90.00 _cell_volume 5108.25(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9800 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 32.40 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2652.8 _exptl_absorpt_coefficient_mu 2.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3710 _exptl_absorpt_correction_T_max 0.5151 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61231 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 32.00 _reflns_number_total 17747 _reflns_number_gt 14160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; Three CF3 groups are disordered over two sites each (C33 F7 F8 F9; C49 F19 F20 F21; C50 F22 F23 F24). C50 was refined on two sites, only one site was refined for C33 and C49, respectively. The following restraints were used: sadi 0.001 c33 f7a c33 f8a c33 f9a sadi 0.001 c49 f19a c49 f20a c49 f21a sadi 0.001 c47 c50 c47 c50a sadi 0.001 c50 f22 c50 f23 c50 f24 c50a f22a c50a f23a c50a f24a same c50 f22 f23 f24 isor 0.01 f22a f23a f24a as well as same anisotropic displacement parameters for some of the atoms: eadp f19 f19a eadp f20 f20a eadp f21 f21a eadp f7 f7a eadp f8 f8a eadp f9 f9a eadp c50 c50a Furthermore, a dichloromethane molecule with very low site occupancy (10 percent) was refined using the following restraint sadi 0.001 cl1 c51 cl2 c51 and only three variables of thermal vibration for the whole molecule, i.e., eadp cl1 cl2 c51 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^)+(0.0322P)^2^+4.9464P] 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 17747 _refine_ls_number_parameters 784 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.204045(7) -0.004499(3) 0.373418(6) 0.01976(3) Uani 1 1 d . . . N1 N 0.18910(16) 0.00594(7) 0.50539(15) 0.0232(4) Uani 1 1 d . . . N2 N 0.25083(16) 0.04002(7) 0.56078(14) 0.0222(4) Uani 1 1 d . . . N3 N 0.23999(16) 0.07300(7) 0.37339(13) 0.0207(4) Uani 1 1 d . . . N4 N 0.28748(15) 0.09716(7) 0.45101(14) 0.0207(4) Uani 1 1 d . . . C1 C 0.1066(2) -0.07014(10) 0.3515(2) 0.0352(6) Uani 1 1 d . . . H1 H 0.0587 -0.0730 0.3935 0.042 Uiso 1 1 calc R . . C2 C 0.2099(2) -0.08542(9) 0.3896(2) 0.0333(6) Uani 1 1 d . . . H2 H 0.2220 -0.0971 0.4537 0.040 Uiso 1 1 calc R . . C3 C 0.2794(2) -0.11156(10) 0.3355(2) 0.0384(7) Uani 1 1 d . . . H3A H 0.3271 -0.1356 0.3753 0.046 Uiso 1 1 calc R . . H3B H 0.2351 -0.1316 0.2861 0.046 Uiso 1 1 calc R . . C4 C 0.3435(2) -0.07371(11) 0.2959(2) 0.0367(6) Uani 1 1 d . . . H4A H 0.4128 -0.0698 0.3379 0.044 Uiso 1 1 calc R . . H4B H 0.3550 -0.0876 0.2386 0.044 Uiso 1 1 calc R . . C5 C 0.2927(2) -0.02166(10) 0.27811(18) 0.0287(5) Uani 1 1 d . . . H5 H 0.3423 0.0061 0.2709 0.034 Uiso 1 1 calc R . . C6 C 0.1896(2) -0.01243(10) 0.23176(18) 0.0322(6) Uani 1 1 d . . . H6 H 0.1790 0.0205 0.1975 0.039 Uiso 1 1 calc R . . C7 C 0.1167(3) -0.05513(12) 0.1894(2) 0.0457(8) Uani 1 1 d . . . H7A H 0.0694 -0.0425 0.1333 0.055 Uiso 1 1 calc R . . H7B H 0.1583 -0.0836 0.1730 0.055 Uiso 1 1 calc R . . C8 C 0.0519(2) -0.07483(14) 0.2525(2) 0.0495(9) Uani 1 1 d . . . H8A H 0.0348 -0.1112 0.2385 0.059 Uiso 1 1 calc R . . H8B H -0.0146 -0.0556 0.2415 0.059 Uiso 1 1 calc R . . C9 C 0.1297(2) -0.01561(10) 0.5557(2) 0.0299(5) Uani 1 1 d . . . H9 H 0.0782 -0.0410 0.5350 0.036 Uiso 1 1 calc R . . C10 C 0.1540(3) 0.00450(11) 0.6425(2) 0.0375(7) Uani 1 1 d . . . H10 H 0.1233 -0.0044 0.6910 0.045 Uiso 1 1 calc R . . C11 C 0.2309(2) 0.03956(10) 0.64373(17) 0.0293(5) Uani 1 1 d . . . H11 H 0.2643 0.0599 0.6937 0.035 Uiso 1 1 calc R . . C12 C 0.2120(2) 0.11008(9) 0.31280(18) 0.0279(5) Uani 1 1 d . . . H12 H 0.1764 0.1048 0.2518 0.033 Uiso 1 1 calc R . . C13 C 0.2421(2) 0.15758(10) 0.3510(2) 0.0362(6) Uani 1 1 d . . . H13 H 0.2315 0.1899 0.3220 0.043 Uiso 1 1 calc R . . C14 C 0.2900(2) 0.14814(9) 0.43872(19) 0.0288(5) Uani 1 1 d . . . H14 H 0.3196 0.1728 0.4829 0.035 Uiso 1 1 calc R . . C15 C 0.33339(18) 0.06687(8) 0.53028(16) 0.0205(4) Uani 1 1 d . . . H15 H 0.3673 0.0910 0.5792 0.025 Uiso 1 1 calc R . . C16 C 0.41807(17) 0.03096(8) 0.51266(15) 0.0179(4) Uani 1 1 d . . . C17 C 0.48416(18) 0.04764(9) 0.45959(16) 0.0216(4) Uani 1 1 d . . . H17 H 0.4737 0.0804 0.4320 0.026 Uiso 1 1 calc R . . C18 C 0.56558(18) 0.01681(9) 0.44655(16) 0.0210(4) Uani 1 1 d . . . H18 H 0.6101 0.0284 0.4097 0.025 Uiso 1 1 calc R . . F1 F 0.48725(17) 0.14273(10) 1.30713(16) 0.0701(7) Uani 1 1 d . . . F2 F 0.6175(2) 0.17139(8) 1.40373(13) 0.0598(6) Uani 1 1 d . . . F3 F 0.63735(18) 0.10760(7) 1.32289(13) 0.0523(5) Uani 1 1 d . . . F4 F 0.64317(19) 0.35202(7) 1.2167(2) 0.0920(10) Uani 1 1 d . . . F5 F 0.7760(3) 0.32245(10) 1.30696(17) 0.0967(10) Uani 1 1 d . . . F6 F 0.77875(16) 0.33344(7) 1.17145(15) 0.0515(5) Uani 1 1 d . . . F7 F 0.15348(18) 0.08886(17) 0.9336(2) 0.0777(9) Uani 0.84 1 d P A 1 F8 F 0.2308(3) 0.0732(2) 1.0669(3) 0.124(2) Uani 0.84 1 d P A 1 F9 F 0.2142(2) 0.14833(13) 1.0205(3) 0.0937(15) Uani 0.84 1 d P A 1 F7A F 0.2564(11) 0.1073(9) 1.0827(9) 0.0777(9) Uani 0.16 1 d PD A 2 F8A F 0.1867(17) 0.1395(9) 0.9677(18) 0.124(2) Uani 0.16 1 d PD A 2 F9A F 0.1817(14) 0.0613(6) 0.992(2) 0.0937(15) Uani 0.16 1 d PD a 2 F10 F 0.45591(16) 0.01423(7) 0.75851(12) 0.0443(4) Uani 1 1 d . . . F11 F 0.4035(2) -0.03616(8) 0.84874(17) 0.0725(8) Uani 1 1 d . . . F12 F 0.56524(17) -0.01559(7) 0.87134(13) 0.0511(5) Uani 1 1 d . . . F13 F 0.49144(15) 0.17415(7) 0.64022(12) 0.0452(5) Uani 1 1 d . . . F14 F 0.57505(19) 0.24222(11) 0.62558(14) 0.0708(7) Uani 1 1 d . . . F15 F 0.40734(16) 0.24264(7) 0.59423(12) 0.0466(5) Uani 1 1 d . . . F16 F 0.3627(2) 0.35001(9) 0.93276(17) 0.0751(8) Uani 1 1 d . . . F17 F 0.5003(2) 0.38250(9) 0.9104(3) 0.1054(12) Uani 1 1 d . . . F18 F 0.3643(3) 0.37581(9) 0.80371(17) 0.0905(10) Uani 1 1 d . . . F19 F 0.9629(3) 0.03450(12) 1.05503(19) 0.0915(12) Uani 0.89 1 d P B 1 F20 F 0.9937(2) 0.08392(10) 1.1668(2) 0.0696(8) Uani 0.89 1 d P B 1 F21 F 0.85530(16) 0.04105(9) 1.13924(18) 0.0508(6) Uani 0.89 1 d P B 1 F19A F 0.901(3) 0.0640(10) 1.1740(13) 0.0915(12) Uani 0.11 1 d PD B 2 F20A F 0.8810(18) 0.0261(6) 1.0648(16) 0.0696(8) Uani 0.11 1 d PD B 2 F21A F 1.0134(10) 0.0640(9) 1.1093(18) 0.0508(6) Uani 0.11 1 d PD B 2 C50 C 0.9301(2) 0.20960(12) 0.8823(2) 0.0293(7) Uani 0.72 1 d PD C 1 F22 F 1.0251(3) 0.19269(13) 0.8828(3) 0.0702(13) Uani 0.72 1 d PD C 1 F23 F 0.9408(7) 0.25737(15) 0.9117(5) 0.0558(18) Uani 0.72 1 d PD C 1 F24 F 0.8808(3) 0.21333(17) 0.7963(2) 0.0664(11) Uani 0.72 1 d PD C 1 C50A C 0.9445(5) 0.2113(3) 0.8981(4) 0.0293(7) Uani 0.28 1 d PD C 2 F22A F 0.9188(17) 0.2603(4) 0.8924(14) 0.048(4) Uani 0.28 1 d PDU C 2 F23A F 0.9361(8) 0.1951(3) 0.8145(6) 0.053(2) Uani 0.28 1 d PDU C 2 F24A F 1.0446(5) 0.2102(3) 0.9401(6) 0.053(2) Uani 0.28 1 d PDU C 2 B1 B 0.5912(2) 0.17773(9) 0.98711(18) 0.0179(4) Uani 1 1 d . . . C19 C 0.60738(17) 0.19963(8) 1.09000(16) 0.0189(4) Uani 1 1 d . . . C20 C 0.65362(18) 0.24754(8) 1.11457(16) 0.0212(4) Uani 1 1 d . . . H20 H 0.6707 0.2686 1.0693 0.025 Uiso 1 1 calc R . . C21 C 0.67524(19) 0.26509(9) 1.20315(17) 0.0242(5) Uani 1 1 d . . . C22 C 0.6552(2) 0.23512(10) 1.27215(18) 0.0282(5) Uani 1 1 d . . . H22 H 0.6706 0.2470 1.3327 0.034 Uiso 1 1 calc R . . C23 C 0.6122(2) 0.18734(9) 1.24969(17) 0.0256(5) Uani 1 1 d . . . C24 C 0.58815(19) 0.17023(9) 1.16069(17) 0.0235(5) Uani 1 1 d . . . H24 H 0.5576 0.1374 1.1477 0.028 Uiso 1 1 calc R . . C25 C 0.7166(2) 0.31803(11) 1.2237(2) 0.0371(6) Uani 1 1 d . . . C26 C 0.5889(3) 0.15247(11) 1.3205(2) 0.0366(6) Uani 1 1 d . . . C27 C 0.50903(17) 0.12982(8) 0.96827(16) 0.0189(4) Uani 1 1 d . . . C28 C 0.41173(18) 0.13371(9) 0.99093(18) 0.0246(5) Uani 1 1 d . . . H28 H 0.3970 0.1635 1.0215 0.029 Uiso 1 1 calc R . . C29 C 0.33677(19) 0.09596(10) 0.97048(19) 0.0287(5) Uani 1 1 d . . . C30 C 0.3537(2) 0.05242(10) 0.92428(17) 0.0273(5) Uani 1 1 d . . . H30 H 0.3018 0.0266 0.9094 0.033 Uiso 1 1 calc R . . C31 C 0.4487(2) 0.04768(9) 0.90045(16) 0.0237(5) Uani 1 1 d . . . C32 C 0.52495(18) 0.08547(8) 0.92269(16) 0.0206(4) Uani 1 1 d . . . H32 H 0.5897 0.0809 0.9063 0.025 Uiso 1 1 calc R . . C33 C 0.2360(2) 0.10066(14) 0.9997(3) 0.0458(8) Uani 1 1 d D . . C34 C 0.4685(2) 0.00259(10) 0.84646(19) 0.0328(6) Uani 1 1 d . . . C35 C 0.54239(17) 0.21970(8) 0.90879(16) 0.0191(4) Uani 1 1 d . . . C36 C 0.53710(19) 0.20737(9) 0.81830(16) 0.0225(5) Uani 1 1 d . . . H36 H 0.5640 0.1754 0.8049 0.027 Uiso 1 1 calc R . . C37 C 0.49437(19) 0.23990(9) 0.74772(17) 0.0247(5) Uani 1 1 d . . . C38 C 0.4553(2) 0.28743(10) 0.76403(19) 0.0299(5) Uani 1 1 d . . . H38 H 0.4270 0.3102 0.7161 0.036 Uiso 1 1 calc R . . C39 C 0.4592(2) 0.30028(9) 0.85209(19) 0.0297(5) Uani 1 1 d . . . C40 C 0.50086(19) 0.26716(9) 0.92331(18) 0.0239(5) Uani 1 1 d . . . H40 H 0.5009 0.2772 0.9832 0.029 Uiso 1 1 calc R . . C41 C 0.4931(2) 0.22501(12) 0.6532(2) 0.0355(6) Uani 1 1 d . . . C42 C 0.4223(3) 0.35191(11) 0.8745(2) 0.0448(8) Uani 1 1 d . . . C43 C 0.70978(18) 0.16144(8) 0.98123(15) 0.0188(4) Uani 1 1 d . . . C44 C 0.76112(17) 0.12121(8) 1.03464(16) 0.0201(4) Uani 1 1 d . . . H44 H 0.7231 0.1011 1.0679 0.024 Uiso 1 1 calc R . . C45 C 0.86574(18) 0.10981(8) 1.04045(16) 0.0216(4) Uani 1 1 d . . . C46 C 0.92422(19) 0.13842(9) 0.99323(18) 0.0247(5) Uani 1 1 d . . . H46 H 0.9960 0.1312 0.9979 0.030 Uiso 1 1 calc R . . C47 C 0.87507(19) 0.17774(9) 0.93922(17) 0.0233(5) Uani 1 1 d . . . C48 C 0.77017(18) 0.18894(8) 0.93353(17) 0.0209(4) Uani 1 1 d . . . H48 H 0.7387 0.2163 0.8958 0.025 Uiso 1 1 calc R . . C49 C 0.9178(2) 0.06689(10) 1.0982(2) 0.0313(6) Uani 1 1 d . . . Cl1 Cl 0.3098(9) 0.2070(5) 0.1729(8) 0.069(2) Uani 0.10 1 d PD D 1 C51 C 0.358(4) 0.2613(15) 0.131(2) 0.069(2) Uani 0.10 1 d PD D 1 H51A H 0.3558 0.2908 0.1715 0.083 Uiso 0.10 1 calc PR D 1 H51B H 0.4307 0.2558 0.1268 0.083 Uiso 0.10 1 calc PR D 1 Cl2 Cl 0.2779(9) 0.2726(5) 0.0255(7) 0.069(2) Uani 0.10 1 d PD D 1 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 0.02037(4) 0.01663(4) 0.02204(5) -0.00139(3) 0.00440(3) -0.00057(3) N1 0.0235(9) 0.0213(9) 0.0264(10) 0.0015(8) 0.0091(8) 0.0012(7) N2 0.0238(10) 0.0244(9) 0.0193(10) -0.0013(7) 0.0069(8) 0.0023(7) N3 0.0207(9) 0.0192(9) 0.0207(10) -0.0003(7) 0.0015(8) -0.0003(7) N4 0.0216(9) 0.0168(8) 0.0225(10) -0.0006(7) 0.0029(8) 0.0007(7) C1 0.0327(14) 0.0237(12) 0.0530(19) -0.0113(12) 0.0176(13) -0.0092(10) C2 0.0400(15) 0.0182(10) 0.0466(18) 0.0016(10) 0.0201(14) -0.0014(10) C3 0.0427(17) 0.0238(12) 0.0519(19) -0.0003(12) 0.0177(14) 0.0103(11) C4 0.0401(16) 0.0352(14) 0.0391(17) -0.0010(12) 0.0177(13) 0.0105(12) C5 0.0361(14) 0.0291(12) 0.0236(13) -0.0009(10) 0.0124(11) 0.0032(10) C6 0.0480(17) 0.0254(12) 0.0203(12) -0.0028(9) 0.0019(11) 0.0014(11) C7 0.054(2) 0.0392(16) 0.0348(17) -0.0112(13) -0.0082(15) 0.0044(14) C8 0.0301(15) 0.0540(19) 0.061(2) -0.0307(17) 0.0026(15) -0.0081(13) C9 0.0283(13) 0.0272(12) 0.0384(15) 0.0072(10) 0.0163(11) 0.0021(9) C10 0.0446(16) 0.0384(15) 0.0373(16) 0.0085(12) 0.0253(13) 0.0077(12) C11 0.0383(15) 0.0318(13) 0.0200(12) 0.0018(9) 0.0112(11) 0.0116(10) C12 0.0281(13) 0.0233(11) 0.0277(13) 0.0060(9) -0.0029(10) 0.0003(9) C13 0.0390(15) 0.0201(11) 0.0432(17) 0.0081(11) -0.0031(13) -0.0008(10) C14 0.0308(13) 0.0170(10) 0.0365(15) -0.0007(9) 0.0031(11) -0.0004(9) C15 0.0214(11) 0.0219(10) 0.0171(11) -0.0016(8) 0.0023(9) -0.0004(8) C16 0.0179(10) 0.0203(9) 0.0144(10) 0.0003(8) 0.0017(8) 0.0003(7) C17 0.0219(11) 0.0223(10) 0.0201(12) 0.0059(8) 0.0041(9) 0.0021(8) C18 0.0225(11) 0.0232(10) 0.0179(11) 0.0034(8) 0.0061(9) -0.0013(8) F1 0.0474(12) 0.1056(19) 0.0623(14) 0.0426(13) 0.0228(11) -0.0091(12) F2 0.1024(18) 0.0547(12) 0.0274(10) 0.0083(8) 0.0255(11) 0.0060(12) F3 0.0858(15) 0.0307(9) 0.0497(12) 0.0165(8) 0.0348(11) 0.0113(9) F4 0.0624(15) 0.0256(9) 0.205(3) -0.0220(14) 0.0651(19) -0.0002(9) F5 0.151(3) 0.0735(17) 0.0521(15) -0.0207(12) -0.0039(16) -0.0565(18) F6 0.0583(12) 0.0329(9) 0.0730(14) -0.0132(9) 0.0347(11) -0.0191(8) F7 0.0160(11) 0.116(3) 0.098(2) -0.016(2) 0.0068(13) -0.0059(14) F8 0.058(2) 0.209(5) 0.130(3) 0.117(3) 0.070(2) 0.052(3) F9 0.0397(17) 0.078(2) 0.179(4) -0.051(2) 0.059(2) -0.0080(14) F7A 0.0160(11) 0.116(3) 0.098(2) -0.016(2) 0.0068(13) -0.0059(14) F8A 0.058(2) 0.209(5) 0.130(3) 0.117(3) 0.070(2) 0.052(3) F9A 0.0397(17) 0.078(2) 0.179(4) -0.051(2) 0.059(2) -0.0080(14) F10 0.0543(12) 0.0527(10) 0.0226(8) -0.0055(7) 0.0019(8) 0.0010(9) F11 0.109(2) 0.0378(10) 0.0885(17) -0.0280(11) 0.0595(16) -0.0419(12) F12 0.0657(13) 0.0405(10) 0.0405(11) -0.0098(8) -0.0014(9) 0.0240(9) F13 0.0559(12) 0.0476(10) 0.0279(9) -0.0061(7) 0.0012(8) 0.0197(9) F14 0.0621(14) 0.119(2) 0.0400(12) -0.0088(12) 0.0289(11) -0.0295(14) F15 0.0568(12) 0.0493(10) 0.0262(9) 0.0072(8) -0.0057(8) 0.0143(9) F16 0.103(2) 0.0565(13) 0.0833(17) 0.0093(12) 0.0567(16) 0.0436(13) F17 0.0692(17) 0.0377(12) 0.209(4) -0.0522(17) 0.032(2) 0.0043(11) F18 0.143(3) 0.0583(14) 0.0720(17) 0.0223(12) 0.0281(17) 0.0712(16) F19 0.157(3) 0.0760(19) 0.0558(16) 0.0275(15) 0.054(2) 0.090(2) F20 0.0515(15) 0.0654(16) 0.0687(18) 0.0170(14) -0.0335(13) -0.0045(12) F21 0.0339(11) 0.0506(13) 0.0652(16) 0.0343(11) 0.0062(10) 0.0070(9) F19A 0.157(3) 0.0760(19) 0.0558(16) 0.0275(15) 0.054(2) 0.090(2) F20A 0.0515(15) 0.0654(16) 0.0687(18) 0.0170(14) -0.0335(13) -0.0045(12) F21A 0.0339(11) 0.0506(13) 0.0652(16) 0.0343(11) 0.0062(10) 0.0070(9) C50 0.0239(15) 0.0249(12) 0.043(2) -0.0013(13) 0.0157(14) -0.0030(10) F22 0.045(2) 0.056(2) 0.131(4) 0.041(2) 0.062(3) 0.0186(16) F23 0.096(5) 0.0255(19) 0.059(3) -0.0011(18) 0.044(3) -0.019(2) F24 0.064(2) 0.103(3) 0.0348(17) 0.0121(18) 0.0171(17) -0.036(2) C50A 0.0239(15) 0.0249(12) 0.043(2) -0.0013(13) 0.0157(14) -0.0030(10) F22A 0.059(6) 0.023(4) 0.073(9) 0.019(4) 0.039(6) 0.020(4) F23A 0.079(6) 0.049(4) 0.046(5) -0.017(3) 0.042(4) -0.022(4) F24A 0.024(3) 0.062(5) 0.077(6) 0.026(4) 0.018(4) -0.010(3) B1 0.0177(11) 0.0163(10) 0.0202(12) 0.0011(9) 0.0054(9) 0.0018(8) C19 0.0163(10) 0.0182(9) 0.0234(11) 0.0016(8) 0.0068(9) 0.0014(7) C20 0.0208(11) 0.0204(10) 0.0237(12) 0.0008(8) 0.0074(9) -0.0012(8) C21 0.0234(12) 0.0228(11) 0.0265(13) -0.0037(9) 0.0062(10) -0.0012(8) C22 0.0303(13) 0.0321(13) 0.0233(13) -0.0048(10) 0.0083(10) 0.0038(10) C23 0.0320(13) 0.0253(11) 0.0222(12) 0.0057(9) 0.0116(10) 0.0067(9) C24 0.0258(12) 0.0189(10) 0.0270(13) 0.0034(9) 0.0083(10) 0.0012(8) C25 0.0438(17) 0.0307(13) 0.0392(17) -0.0120(12) 0.0145(14) -0.0065(12) C26 0.0457(17) 0.0391(15) 0.0281(15) 0.0095(11) 0.0150(13) 0.0047(12) C27 0.0163(10) 0.0188(9) 0.0213(11) 0.0035(8) 0.0038(8) 0.0018(7) C28 0.0183(11) 0.0243(11) 0.0314(13) 0.0028(9) 0.0062(10) 0.0031(8) C29 0.0171(11) 0.0353(13) 0.0326(14) 0.0070(11) 0.0038(10) -0.0008(9) C30 0.0242(12) 0.0280(12) 0.0271(13) 0.0040(10) 0.0009(10) -0.0070(9) C31 0.0285(12) 0.0206(10) 0.0191(11) 0.0029(8) -0.0003(9) -0.0033(9) C32 0.0209(11) 0.0211(10) 0.0200(11) 0.0026(8) 0.0048(9) -0.0005(8) C33 0.0220(14) 0.056(2) 0.061(2) 0.0044(16) 0.0112(14) -0.0024(13) C34 0.0449(16) 0.0252(12) 0.0270(13) -0.0021(10) 0.0054(11) -0.0090(11) C35 0.0157(10) 0.0183(9) 0.0234(12) 0.0028(8) 0.0042(8) 0.0013(7) C36 0.0222(11) 0.0208(10) 0.0238(12) 0.0024(8) 0.0036(9) 0.0029(8) C37 0.0227(12) 0.0286(11) 0.0222(12) 0.0042(9) 0.0041(9) 0.0028(9) C38 0.0278(13) 0.0273(12) 0.0337(15) 0.0113(10) 0.0051(11) 0.0079(9) C39 0.0332(14) 0.0217(11) 0.0354(15) 0.0046(10) 0.0105(11) 0.0107(9) C40 0.0227(11) 0.0224(10) 0.0281(13) 0.0006(9) 0.0090(10) 0.0042(8) C41 0.0333(15) 0.0444(16) 0.0281(15) 0.0075(12) 0.0055(12) 0.0052(12) C42 0.057(2) 0.0301(14) 0.050(2) 0.0064(13) 0.0174(16) 0.0210(13) C43 0.0207(10) 0.0163(9) 0.0190(11) -0.0014(8) 0.0039(8) -0.0008(7) C44 0.0177(10) 0.0209(10) 0.0215(11) 0.0009(8) 0.0044(9) -0.0018(8) C45 0.0196(11) 0.0202(10) 0.0239(12) -0.0021(8) 0.0031(9) 0.0030(8) C46 0.0183(11) 0.0219(10) 0.0345(14) -0.0051(9) 0.0077(10) -0.0001(8) C47 0.0216(11) 0.0195(10) 0.0312(13) -0.0030(9) 0.0112(10) -0.0032(8) C48 0.0205(11) 0.0159(9) 0.0271(12) -0.0001(8) 0.0073(9) 0.0001(8) C49 0.0253(13) 0.0315(13) 0.0356(15) 0.0046(11) 0.0038(11) 0.0080(10) Cl1 0.071(5) 0.083(5) 0.063(5) 0.021(4) 0.032(4) 0.023(4) C51 0.071(5) 0.083(5) 0.063(5) 0.021(4) 0.032(4) 0.023(4) Cl2 0.071(5) 0.083(5) 0.063(5) 0.021(4) 0.032(4) 0.023(4) _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 N3 2.0825(19) . ? Ir1 N1 2.085(2) . ? Ir1 C5 2.112(3) . ? Ir1 C1 2.123(2) . ? Ir1 C2 2.131(2) . ? Ir1 C6 2.135(3) . ? N1 C9 1.340(3) . ? N1 N2 1.360(3) . ? N2 C11 1.350(3) . ? N2 C15 1.458(3) . ? N3 C12 1.332(3) . ? N3 N4 1.360(3) . ? N4 C14 1.349(3) . ? N4 C15 1.455(3) . ? C1 C2 1.406(4) . ? C1 C8 1.520(5) . ? C1 H1 1.0000 . ? C2 C3 1.529(4) . ? C2 H2 1.0000 . ? C3 C4 1.514(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.514(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.398(4) . ? C5 H5 1.0000 . ? C6 C7 1.516(4) . ? C6 H6 1.0000 . ? C7 C8 1.516(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C10 C11 1.363(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C13 C14 1.362(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.528(3) . ? C15 H15 1.0000 . ? C16 C17 1.389(3) . ? C16 C18 1.391(3) 3_656 ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 C16 1.391(3) 3_656 ? C18 H18 0.9500 . ? F1 C26 1.330(4) . ? F2 C26 1.334(4) . ? F3 C26 1.333(3) . ? F4 C25 1.300(4) . ? F5 C25 1.332(4) . ? F6 C25 1.330(3) . ? F7 C33 1.335(4) . ? F8 C33 1.268(4) . ? F9 C33 1.335(5) . ? F7A C33 1.244(12) . ? F8A C33 1.243(12) . ? F9A C33 1.244(12) . ? F10 C34 1.348(3) . ? F11 C34 1.332(3) . ? F12 C34 1.329(4) . ? F13 C41 1.345(4) . ? F14 C41 1.324(4) . ? F15 C41 1.350(3) . ? F16 C42 1.316(4) . ? F17 C42 1.317(4) . ? F18 C42 1.326(4) . ? F19 C49 1.298(3) . ? F20 C49 1.344(4) . ? F21 C49 1.329(4) . ? F19A C49 1.232(12) . ? F20A C49 1.232(12) . ? F21A C49 1.232(12) . ? C50 F22 1.3244(19) . ? C50 F23 1.325(2) . ? C50 F24 1.3248(19) . ? C50 C47 1.505(3) . ? C50A F24A 1.324(2) . ? C50A F23A 1.324(2) . ? C50A F22A 1.324(2) . ? C50A C47 1.505(4) . ? B1 C27 1.637(3) . ? B1 C19 1.638(4) . ? B1 C43 1.640(3) . ? B1 C35 1.640(3) . ? C19 C24 1.395(3) . ? C19 C20 1.406(3) . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 C22 1.386(4) . ? C21 C25 1.495(4) . ? C22 C23 1.383(4) . ? C22 H22 0.9500 . ? C23 C24 1.394(4) . ? C23 C26 1.498(4) . ? C24 H24 0.9500 . ? C27 C32 1.394(3) . ? C27 C28 1.405(3) . ? C28 C29 1.379(3) . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C29 C33 1.498(4) . ? C30 C31 1.386(4) . ? C30 H30 0.9500 . ? C31 C32 1.393(3) . ? C31 C34 1.496(4) . ? C32 H32 0.9500 . ? C35 C40 1.395(3) . ? C35 C36 1.403(3) . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.390(3) . ? C37 C41 1.490(4) . ? C38 C39 1.374(4) . ? C38 H38 0.9500 . ? C39 C40 1.398(3) . ? C39 C42 1.501(4) . ? C40 H40 0.9500 . ? C43 C48 1.395(3) . ? C43 C44 1.405(3) . ? C44 C45 1.391(3) . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 C49 1.492(3) . ? C46 C47 1.382(3) . ? C46 H46 0.9500 . ? C47 C48 1.394(3) . ? C48 H48 0.9500 . ? Cl1 C51 1.73(3) . ? C51 Cl2 1.73(3) . ? C51 H51A 0.9900 . ? C51 H51B 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 N3 Ir1 N1 86.84(8) . . ? N3 Ir1 C5 92.59(9) . . ? N1 Ir1 C5 151.99(10) . . ? N3 Ir1 C1 156.47(10) . . ? N1 Ir1 C1 93.97(10) . . ? C5 Ir1 C1 97.43(11) . . ? N3 Ir1 C2 164.92(10) . . ? N1 Ir1 C2 91.54(10) . . ? C5 Ir1 C2 81.83(10) . . ? C1 Ir1 C2 38.60(11) . . ? N3 Ir1 C6 93.52(9) . . ? N1 Ir1 C6 169.58(10) . . ? C5 Ir1 C6 38.43(11) . . ? C1 Ir1 C6 81.56(12) . . ? C2 Ir1 C6 90.76(11) . . ? C9 N1 N2 105.3(2) . . ? C9 N1 Ir1 134.08(19) . . ? N2 N1 Ir1 120.59(15) . . ? C11 N2 N1 111.0(2) . . ? C11 N2 C15 128.6(2) . . ? N1 N2 C15 119.99(19) . . ? C12 N3 N4 105.22(19) . . ? C12 N3 Ir1 133.13(17) . . ? N4 N3 Ir1 120.74(14) . . ? C14 N4 N3 111.1(2) . . ? C14 N4 C15 129.5(2) . . ? N3 N4 C15 119.26(18) . . ? C2 C1 C8 125.3(3) . . ? C2 C1 Ir1 71.02(15) . . ? C8 C1 Ir1 110.6(2) . . ? C2 C1 H1 114.0 . . ? C8 C1 H1 114.0 . . ? Ir1 C1 H1 114.0 . . ? C1 C2 C3 123.1(3) . . ? C1 C2 Ir1 70.38(15) . . ? C3 C2 Ir1 113.07(18) . . ? C1 C2 H2 114.2 . . ? C3 C2 H2 114.2 . . ? Ir1 C2 H2 114.2 . . ? C4 C3 C2 112.4(2) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 113.3(2) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.6(3) . . ? C6 C5 Ir1 71.66(16) . . ? C4 C5 Ir1 111.05(18) . . ? C6 C5 H5 113.6 . . ? C4 C5 H5 113.6 . . ? Ir1 C5 H5 113.6 . . ? C5 C6 C7 122.1(3) . . ? C5 C6 Ir1 69.92(15) . . ? C7 C6 Ir1 113.7(2) . . ? C5 C6 H6 114.5 . . ? C7 C6 H6 114.5 . . ? Ir1 C6 H6 114.5 . . ? C8 C7 C6 111.9(3) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C1 113.4(2) . . ? C7 C8 H8A 108.9 . . ? C1 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C1 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N1 C9 C10 110.5(2) . . ? N1 C9 H9 124.8 . . ? C10 C9 H9 124.8 . . ? C11 C10 C9 105.9(2) . . ? C11 C10 H10 127.1 . . ? C9 C10 H10 127.1 . . ? N2 C11 C10 107.3(2) . . ? N2 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? N3 C12 C13 110.8(2) . . ? N3 C12 H12 124.6 . . ? C13 C12 H12 124.6 . . ? C14 C13 C12 105.7(2) . . ? C14 C13 H13 127.1 . . ? C12 C13 H13 127.1 . . ? N4 C14 C13 107.2(2) . . ? N4 C14 H14 126.4 . . ? C13 C14 H14 126.4 . . ? N4 C15 N2 109.35(19) . . ? N4 C15 C16 111.60(19) . . ? N2 C15 C16 112.78(18) . . ? N4 C15 H15 107.6 . . ? N2 C15 H15 107.6 . . ? C16 C15 H15 107.6 . . ? C17 C16 C18 119.4(2) . 3_656 ? C17 C16 C15 119.32(19) . . ? C18 C16 C15 121.2(2) 3_656 . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C16 C18 C17 120.1(2) 3_656 . ? C16 C18 H18 119.9 3_656 . ? C17 C18 H18 119.9 . . ? F22 C50 F23 106.7(5) . . ? F22 C50 F24 106.0(3) . . ? F23 C50 F24 104.7(4) . . ? F22 C50 C47 113.0(2) . . ? F23 C50 C47 110.8(5) . . ? F24 C50 C47 114.9(3) . . ? F24A C50A F23A 108.1(8) . . ? F24A C50A F22A 105.2(10) . . ? F23A C50A F22A 106.5(10) . . ? F24A C50A C47 114.7(5) . . ? F23A C50A C47 107.0(5) . . ? F22A C50A C47 115.0(12) . . ? C27 B1 C19 111.73(18) . . ? C27 B1 C43 112.91(17) . . ? C19 B1 C43 103.26(18) . . ? C27 B1 C35 104.71(18) . . ? C19 B1 C35 113.93(18) . . ? C43 B1 C35 110.56(18) . . ? C24 C19 C20 115.5(2) . . ? C24 C19 B1 122.8(2) . . ? C20 C19 B1 121.3(2) . . ? C21 C20 C19 122.1(2) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C20 121.2(2) . . ? C22 C21 C25 119.3(2) . . ? C20 C21 C25 119.5(2) . . ? C23 C22 C21 117.6(2) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 C23 C24 121.3(2) . . ? C22 C23 C26 120.8(2) . . ? C24 C23 C26 117.9(2) . . ? C23 C24 C19 122.3(2) . . ? C23 C24 H24 118.8 . . ? C19 C24 H24 118.8 . . ? F4 C25 F6 107.0(3) . . ? F4 C25 F5 106.2(3) . . ? F6 C25 F5 103.8(3) . . ? F4 C25 C21 112.9(3) . . ? F6 C25 C21 113.6(2) . . ? F5 C25 C21 112.7(3) . . ? F1 C26 F3 107.0(3) . . ? F1 C26 F2 105.6(3) . . ? F3 C26 F2 105.8(2) . . ? F1 C26 C23 111.9(2) . . ? F3 C26 C23 112.4(2) . . ? F2 C26 C23 113.6(3) . . ? C32 C27 C28 115.7(2) . . ? C32 C27 B1 123.8(2) . . ? C28 C27 B1 120.2(2) . . ? C29 C28 C27 122.5(2) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 120.9(2) . . ? C28 C29 C33 120.6(3) . . ? C30 C29 C33 118.5(3) . . ? C29 C30 C31 117.9(2) . . ? C29 C30 H30 121.0 . . ? C31 C30 H30 121.0 . . ? C30 C31 C32 121.0(2) . . ? C30 C31 C34 119.9(2) . . ? C32 C31 C34 119.1(2) . . ? C31 C32 C27 122.0(2) . . ? C31 C32 H32 119.0 . . ? C27 C32 H32 119.0 . . ? F8A C33 F9A 113.8(17) . . ? F8A C33 F7A 104.8(16) . . ? F9A C33 F7A 101.3(16) . . ? F8 C33 F9 106.5(4) . . ? F8 C33 F7 107.0(4) . . ? F9 C33 F7 102.4(3) . . ? F8A C33 C29 111.6(8) . . ? F9A C33 C29 115.6(7) . . ? F7A C33 C29 108.5(7) . . ? F8 C33 C29 114.3(3) . . ? F9 C33 C29 113.6(3) . . ? F7 C33 C29 112.2(3) . . ? F12 C34 F11 107.3(2) . . ? F12 C34 F10 104.7(2) . . ? F11 C34 F10 105.4(2) . . ? F12 C34 C31 113.7(2) . . ? F11 C34 C31 113.0(3) . . ? F10 C34 C31 111.9(2) . . ? C40 C35 C36 115.4(2) . . ? C40 C35 B1 125.6(2) . . ? C36 C35 B1 118.95(19) . . ? C37 C36 C35 122.8(2) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 120.7(2) . . ? C36 C37 C41 120.2(2) . . ? C38 C37 C41 119.0(2) . . ? C39 C38 C37 117.5(2) . . ? C39 C38 H38 121.2 . . ? C37 C38 H38 121.2 . . ? C38 C39 C40 121.8(2) . . ? C38 C39 C42 120.1(2) . . ? C40 C39 C42 118.0(3) . . ? C35 C40 C39 121.7(2) . . ? C35 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? F14 C41 F13 106.0(3) . . ? F14 C41 F15 106.8(2) . . ? F13 C41 F15 105.0(2) . . ? F14 C41 C37 113.0(3) . . ? F13 C41 C37 113.4(2) . . ? F15 C41 C37 112.0(2) . . ? F16 C42 F17 105.8(3) . . ? F16 C42 F18 104.3(3) . . ? F17 C42 F18 107.3(3) . . ? F16 C42 C39 113.2(3) . . ? F17 C42 C39 112.4(3) . . ? F18 C42 C39 113.2(3) . . ? C48 C43 C44 115.7(2) . . ? C48 C43 B1 123.95(19) . . ? C44 C43 B1 119.9(2) . . ? C45 C44 C43 122.2(2) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C46 C45 C44 120.7(2) . . ? C46 C45 C49 118.5(2) . . ? C44 C45 C49 120.8(2) . . ? C47 C46 C45 118.2(2) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C48 120.9(2) . . ? C46 C47 C50A 116.0(4) . . ? C48 C47 C50A 122.6(4) . . ? C46 C47 C50 122.4(2) . . ? C48 C47 C50 116.7(2) . . ? C47 C48 C43 122.3(2) . . ? C47 C48 H48 118.8 . . ? C43 C48 H48 118.8 . . ? F19A C49 F21A 105.7(19) . . ? F19A C49 F20A 101(2) . . ? F21A C49 F20A 107.2(16) . . ? F19 C49 F21 108.2(3) . . ? F19 C49 F20 105.5(3) . . ? F21 C49 F20 103.3(3) . . ? F19A C49 C45 116.2(9) . . ? F21A C49 C45 116.3(8) . . ? F20A C49 C45 109.0(9) . . ? F19 C49 C45 113.2(2) . . ? F21 C49 C45 114.3(2) . . ? F20 C49 C45 111.5(2) . . ? Cl2 C51 Cl1 107(3) . . ? Cl2 C51 H51A 110.4 . . ? Cl1 C51 H51A 110.4 . . ? Cl2 C51 H51B 110.4 . . ? Cl1 C51 H51B 110.4 . . ? H51A C51 H51B 108.6 . . ? 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 N3 Ir1 N1 C9 148.4(2) . . . . ? C5 Ir1 N1 C9 -122.0(3) . . . . ? C1 Ir1 N1 C9 -8.0(2) . . . . ? C2 Ir1 N1 C9 -46.6(2) . . . . ? C6 Ir1 N1 C9 56.1(6) . . . . ? N3 Ir1 N1 N2 -33.92(17) . . . . ? C5 Ir1 N1 N2 55.7(3) . . . . ? C1 Ir1 N1 N2 169.65(18) . . . . ? C2 Ir1 N1 N2 131.08(18) . . . . ? C6 Ir1 N1 N2 -126.2(5) . . . . ? C9 N1 N2 C11 0.3(3) . . . . ? Ir1 N1 N2 C11 -177.93(16) . . . . ? C9 N1 N2 C15 173.8(2) . . . . ? Ir1 N1 N2 C15 -4.5(3) . . . . ? N1 Ir1 N3 C12 -137.7(2) . . . . ? C5 Ir1 N3 C12 70.3(3) . . . . ? C1 Ir1 N3 C12 -45.0(4) . . . . ? C2 Ir1 N3 C12 138.1(4) . . . . ? C6 Ir1 N3 C12 31.8(3) . . . . ? N1 Ir1 N3 N4 29.61(17) . . . . ? C5 Ir1 N3 N4 -122.34(18) . . . . ? C1 Ir1 N3 N4 122.3(3) . . . . ? C2 Ir1 N3 N4 -54.6(4) . . . . ? C6 Ir1 N3 N4 -160.82(18) . . . . ? C12 N3 N4 C14 -0.6(3) . . . . ? Ir1 N3 N4 C14 -171.09(17) . . . . ? C12 N3 N4 C15 -176.4(2) . . . . ? Ir1 N3 N4 C15 13.2(3) . . . . ? N3 Ir1 C1 C2 -178.7(2) . . . . ? N1 Ir1 C1 C2 -87.50(18) . . . . ? C5 Ir1 C1 C2 66.86(19) . . . . ? C6 Ir1 C1 C2 101.97(19) . . . . ? N3 Ir1 C1 C8 59.8(3) . . . . ? N1 Ir1 C1 C8 151.0(2) . . . . ? C5 Ir1 C1 C8 -54.7(2) . . . . ? C2 Ir1 C1 C8 -121.5(3) . . . . ? C6 Ir1 C1 C8 -19.6(2) . . . . ? C8 C1 C2 C3 -3.1(4) . . . . ? Ir1 C1 C2 C3 -105.3(2) . . . . ? C8 C1 C2 Ir1 102.2(3) . . . . ? N3 Ir1 C2 C1 178.0(3) . . . . ? N1 Ir1 C2 C1 94.43(18) . . . . ? C5 Ir1 C2 C1 -112.90(19) . . . . ? C6 Ir1 C2 C1 -75.41(19) . . . . ? N3 Ir1 C2 C3 -63.4(5) . . . . ? N1 Ir1 C2 C3 -147.0(2) . . . . ? C5 Ir1 C2 C3 5.7(2) . . . . ? C1 Ir1 C2 C3 118.6(3) . . . . ? C6 Ir1 C2 C3 43.2(2) . . . . ? C1 C2 C3 C4 91.1(3) . . . . ? Ir1 C2 C3 C4 10.2(3) . . . . ? C2 C3 C4 C5 -27.7(4) . . . . ? C3 C4 C5 C6 -49.9(4) . . . . ? C3 C4 C5 Ir1 32.2(3) . . . . ? N3 Ir1 C5 C6 -92.39(16) . . . . ? N1 Ir1 C5 C6 179.46(16) . . . . ? C1 Ir1 C5 C6 66.27(17) . . . . ? C2 Ir1 C5 C6 101.68(17) . . . . ? N3 Ir1 C5 C4 145.6(2) . . . . ? N1 Ir1 C5 C4 57.4(3) . . . . ? C1 Ir1 C5 C4 -55.8(2) . . . . ? C2 Ir1 C5 C4 -20.3(2) . . . . ? C6 Ir1 C5 C4 -122.0(3) . . . . ? C4 C5 C6 C7 -2.9(4) . . . . ? Ir1 C5 C6 C7 -106.0(3) . . . . ? C4 C5 C6 Ir1 103.2(3) . . . . ? N3 Ir1 C6 C5 89.74(16) . . . . ? N1 Ir1 C6 C5 -178.6(4) . . . . ? C1 Ir1 C6 C5 -113.41(17) . . . . ? C2 Ir1 C6 C5 -75.80(17) . . . . ? N3 Ir1 C6 C7 -153.0(2) . . . . ? N1 Ir1 C6 C7 -61.3(6) . . . . ? C5 Ir1 C6 C7 117.3(3) . . . . ? C1 Ir1 C6 C7 3.9(2) . . . . ? C2 Ir1 C6 C7 41.5(2) . . . . ? C5 C6 C7 C8 93.2(4) . . . . ? Ir1 C6 C7 C8 12.8(3) . . . . ? C6 C7 C8 C1 -29.9(4) . . . . ? C2 C1 C8 C7 -48.0(4) . . . . ? Ir1 C1 C8 C7 32.8(3) . . . . ? N2 N1 C9 C10 -0.3(3) . . . . ? Ir1 N1 C9 C10 177.62(19) . . . . ? N1 C9 C10 C11 0.2(3) . . . . ? N1 N2 C11 C10 -0.2(3) . . . . ? C15 N2 C11 C10 -173.0(2) . . . . ? C9 C10 C11 N2 0.0(3) . . . . ? N4 N3 C12 C13 0.5(3) . . . . ? Ir1 N3 C12 C13 169.2(2) . . . . ? N3 C12 C13 C14 -0.2(3) . . . . ? N3 N4 C14 C13 0.5(3) . . . . ? C15 N4 C14 C13 175.7(2) . . . . ? C12 C13 C14 N4 -0.2(3) . . . . ? C14 N4 C15 N2 119.1(3) . . . . ? N3 N4 C15 N2 -66.0(3) . . . . ? C14 N4 C15 C16 -115.4(3) . . . . ? N3 N4 C15 C16 59.4(3) . . . . ? C11 N2 C15 N4 -127.0(2) . . . . ? N1 N2 C15 N4 60.9(3) . . . . ? C11 N2 C15 C16 108.2(3) . . . . ? N1 N2 C15 C16 -63.9(3) . . . . ? N4 C15 C16 C17 37.8(3) . . . . ? N2 C15 C16 C17 161.4(2) . . . . ? N4 C15 C16 C18 -146.4(2) . . . 3_656 ? N2 C15 C16 C18 -22.8(3) . . . 3_656 ? C18 C16 C17 C18 0.5(4) 3_656 . . . ? C15 C16 C17 C18 176.4(2) . . . . ? C16 C17 C18 C16 -0.5(4) . . . 3_656 ? C27 B1 C19 C24 23.2(3) . . . . ? C43 B1 C19 C24 -98.4(2) . . . . ? C35 B1 C19 C24 141.6(2) . . . . ? C27 B1 C19 C20 -164.5(2) . . . . ? C43 B1 C19 C20 73.9(2) . . . . ? C35 B1 C19 C20 -46.1(3) . . . . ? C24 C19 C20 C21 -2.2(3) . . . . ? B1 C19 C20 C21 -175.0(2) . . . . ? C19 C20 C21 C22 2.3(4) . . . . ? C19 C20 C21 C25 -175.2(2) . . . . ? C20 C21 C22 C23 -0.6(4) . . . . ? C25 C21 C22 C23 176.9(2) . . . . ? C21 C22 C23 C24 -1.0(4) . . . . ? C21 C22 C23 C26 179.6(2) . . . . ? C22 C23 C24 C19 1.0(4) . . . . ? C26 C23 C24 C19 -179.6(2) . . . . ? C20 C19 C24 C23 0.6(3) . . . . ? B1 C19 C24 C23 173.3(2) . . . . ? C22 C21 C25 F4 -89.4(4) . . . . ? C20 C21 C25 F4 88.1(3) . . . . ? C22 C21 C25 F6 148.7(3) . . . . ? C20 C21 C25 F6 -33.8(4) . . . . ? C22 C21 C25 F5 31.0(4) . . . . ? C20 C21 C25 F5 -151.5(3) . . . . ? C22 C23 C26 F1 116.9(3) . . . . ? C24 C23 C26 F1 -62.6(3) . . . . ? C22 C23 C26 F3 -122.7(3) . . . . ? C24 C23 C26 F3 57.9(4) . . . . ? C22 C23 C26 F2 -2.6(4) . . . . ? C24 C23 C26 F2 178.0(2) . . . . ? C19 B1 C27 C32 -136.8(2) . . . . ? C43 B1 C27 C32 -20.9(3) . . . . ? C35 B1 C27 C32 99.4(2) . . . . ? C19 B1 C27 C28 49.2(3) . . . . ? C43 B1 C27 C28 165.1(2) . . . . ? C35 B1 C27 C28 -74.6(3) . . . . ? C32 C27 C28 C29 0.7(4) . . . . ? B1 C27 C28 C29 175.1(2) . . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C27 C28 C29 C33 177.2(3) . . . . ? C28 C29 C30 C31 0.9(4) . . . . ? C33 C29 C30 C31 -177.7(3) . . . . ? C29 C30 C31 C32 0.3(4) . . . . ? C29 C30 C31 C34 -176.9(2) . . . . ? C30 C31 C32 C27 -1.0(4) . . . . ? C34 C31 C32 C27 176.2(2) . . . . ? C28 C27 C32 C31 0.5(3) . . . . ? B1 C27 C32 C31 -173.7(2) . . . . ? C28 C29 C33 F8A 59.7(18) . . . . ? C30 C29 C33 F8A -121.6(18) . . . . ? C28 C29 C33 F9A -168.1(18) . . . . ? C30 C29 C33 F9A 10.5(18) . . . . ? C28 C29 C33 F7A -55.2(12) . . . . ? C30 C29 C33 F7A 123.4(12) . . . . ? C28 C29 C33 F8 -103.6(5) . . . . ? C30 C29 C33 F8 75.1(5) . . . . ? C28 C29 C33 F9 18.9(5) . . . . ? C30 C29 C33 F9 -162.5(3) . . . . ? C28 C29 C33 F7 134.4(3) . . . . ? C30 C29 C33 F7 -46.9(4) . . . . ? C30 C31 C34 F12 -141.2(3) . . . . ? C32 C31 C34 F12 41.5(3) . . . . ? C30 C31 C34 F11 -18.5(4) . . . . ? C32 C31 C34 F11 164.2(3) . . . . ? C30 C31 C34 F10 100.4(3) . . . . ? C32 C31 C34 F10 -76.9(3) . . . . ? C27 B1 C35 C40 112.0(2) . . . . ? C19 B1 C35 C40 -10.3(3) . . . . ? C43 B1 C35 C40 -126.1(2) . . . . ? C27 B1 C35 C36 -65.4(3) . . . . ? C19 B1 C35 C36 172.2(2) . . . . ? C43 B1 C35 C36 56.5(3) . . . . ? C40 C35 C36 C37 0.4(3) . . . . ? B1 C35 C36 C37 178.1(2) . . . . ? C35 C36 C37 C38 0.9(4) . . . . ? C35 C36 C37 C41 178.7(2) . . . . ? C36 C37 C38 C39 -1.1(4) . . . . ? C41 C37 C38 C39 -179.0(3) . . . . ? C37 C38 C39 C40 0.1(4) . . . . ? C37 C38 C39 C42 177.5(3) . . . . ? C36 C35 C40 C39 -1.4(4) . . . . ? B1 C35 C40 C39 -178.9(2) . . . . ? C38 C39 C40 C35 1.2(4) . . . . ? C42 C39 C40 C35 -176.2(3) . . . . ? C36 C37 C41 F14 -93.3(3) . . . . ? C38 C37 C41 F14 84.6(3) . . . . ? C36 C37 C41 F13 27.4(4) . . . . ? C38 C37 C41 F13 -154.6(2) . . . . ? C36 C37 C41 F15 146.0(2) . . . . ? C38 C37 C41 F15 -36.0(4) . . . . ? C38 C39 C42 F16 134.8(3) . . . . ? C40 C39 C42 F16 -47.7(4) . . . . ? C38 C39 C42 F17 -105.5(4) . . . . ? C40 C39 C42 F17 72.0(4) . . . . ? C38 C39 C42 F18 16.3(5) . . . . ? C40 C39 C42 F18 -166.2(3) . . . . ? C27 B1 C43 C48 132.8(2) . . . . ? C19 B1 C43 C48 -106.4(2) . . . . ? C35 B1 C43 C48 15.8(3) . . . . ? C27 B1 C43 C44 -55.1(3) . . . . ? C19 B1 C43 C44 65.8(2) . . . . ? C35 B1 C43 C44 -172.0(2) . . . . ? C48 C43 C44 C45 0.7(3) . . . . ? B1 C43 C44 C45 -172.1(2) . . . . ? C43 C44 C45 C46 0.3(4) . . . . ? C43 C44 C45 C49 179.8(2) . . . . ? C44 C45 C46 C47 -1.2(4) . . . . ? C49 C45 C46 C47 179.3(2) . . . . ? C45 C46 C47 C48 1.1(4) . . . . ? C45 C46 C47 C50A 173.2(4) . . . . ? C45 C46 C47 C50 -177.4(2) . . . . ? F24A C50A C47 C46 -21.0(9) . . . . ? F23A C50A C47 C46 98.8(7) . . . . ? F22A C50A C47 C46 -143.2(10) . . . . ? F24A C50A C47 C48 150.9(6) . . . . ? F23A C50A C47 C48 -89.3(8) . . . . ? F22A C50A C47 C48 28.7(11) . . . . ? F24A C50A C47 C50 -151(3) . . . . ? F23A C50A C47 C50 -31(2) . . . . ? F22A C50A C47 C50 87(3) . . . . ? F22 C50 C47 C46 6.3(5) . . . . ? F23 C50 C47 C46 -113.3(5) . . . . ? F24 C50 C47 C46 128.2(3) . . . . ? F22 C50 C47 C48 -172.2(3) . . . . ? F23 C50 C47 C48 68.1(4) . . . . ? F24 C50 C47 C48 -50.3(4) . . . . ? F22 C50 C47 C50A 61(2) . . . . ? F23 C50 C47 C50A -59(2) . . . . ? F24 C50 C47 C50A -177(3) . . . . ? C46 C47 C48 C43 -0.1(4) . . . . ? C50A C47 C48 C43 -171.6(4) . . . . ? C50 C47 C48 C43 178.5(2) . . . . ? C44 C43 C48 C47 -0.8(3) . . . . ? B1 C43 C48 C47 171.7(2) . . . . ? C46 C45 C49 F19A 135(2) . . . . ? C44 C45 C49 F19A -45(2) . . . . ? C46 C45 C49 F21A 9.3(17) . . . . ? C44 C45 C49 F21A -170.1(16) . . . . ? C46 C45 C49 F20A -111.9(16) . . . . ? C44 C45 C49 F20A 68.7(16) . . . . ? C46 C45 C49 F19 -54.2(4) . . . . ? C44 C45 C49 F19 126.3(3) . . . . ? C46 C45 C49 F21 -178.7(3) . . . . ? C44 C45 C49 F21 1.9(4) . . . . ? C46 C45 C49 F20 64.6(3) . . . . ? C44 C45 C49 F20 -114.9(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.165 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.101 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 798123' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 N8 Rh2, 2(C32 H12 B F24), 0.3(C H2 Cl2)' _chemical_formula_sum 'C100.30 H66.60 B2 Cl0.60 F48 N8 Rh2 ' _chemical_formula_weight 2544.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.1485(3) _cell_length_b 26.1740(6) _cell_length_c 15.2911(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.5880(10) _cell_angle_gamma 90.00 _cell_volume 5115.12(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9777 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 30.00 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2533.2 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8658 _exptl_absorpt_correction_T_max 0.9105 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD aea 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 54454 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 14416 _reflns_number_gt 11927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; Three CF3 groups are disordered over two sites each (C33 F7 F8 F9; C49 F19 F20 F21; C50 F22 F23 F24). C50 was refined on two sites, only one site was refined for C33 and C49, respectively. The following restraints were used: sadi 0.001 c33 f7a c33 f8a c33 f9a sadi 0.001 c49 f19a c49 f20a c49 f21a sadi 0.001 c47 c50 c47 c50a sadi 0.001 c50 f22 c50 f23 c50 f24 c50a f22a c50a f23a c50a f24a same c50 f22 f23 f24 isor 0.01 f22a f23a f24a as well as same anisotropic displacement parameters for some of the atoms: eadp f19 f19a eadp f20 f20a eadp f21 f21a eadp f7 f7a eadp f8 f8a eadp f9 f9a eadp c50 c50a Furthermore, a dichloromethane molecule with very low site occupancy (15 percent) was refined using the following restraint sadi 0.001 cl1 c51 cl2 c51 and only three variables of thermal vibration for the whole molecule, i.e., eadp cl1 cl2 c51 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^)+(0.0492P)^2^+4.3632P] 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 14416 _refine_ls_number_parameters 788 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.063 _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 0.205541(12) -0.004830(5) 0.371941(10) 0.01963(5) Uani 1 1 d . . . N1 N 0.18839(13) 0.00549(6) 0.50406(12) 0.0228(3) Uani 1 1 d . . . N2 N 0.25033(13) 0.03964(6) 0.55930(11) 0.0222(3) Uani 1 1 d . . . N3 N 0.24068(13) 0.07326(6) 0.37242(11) 0.0208(3) Uani 1 1 d . . . N4 N 0.28709(13) 0.09711(6) 0.45078(11) 0.0209(3) Uani 1 1 d . . . C1 C 0.10662(18) -0.07004(8) 0.34795(17) 0.0337(5) Uani 1 1 d . . . H1 H 0.0581 -0.0727 0.3892 0.040 Uiso 1 1 calc R . . C2 C 0.20780(18) -0.08614(8) 0.38621(16) 0.0313(5) Uani 1 1 d . . . H2 H 0.2186 -0.0982 0.4498 0.038 Uiso 1 1 calc R . . C3 C 0.27824(19) -0.11196(8) 0.33351(18) 0.0357(5) Uani 1 1 d . . . H3A H 0.2344 -0.1306 0.2819 0.043 Uiso 1 1 calc R . . H3B H 0.3234 -0.1372 0.3727 0.043 Uiso 1 1 calc R . . C4 C 0.34690(18) -0.07360(9) 0.29881(16) 0.0330(5) Uani 1 1 d . . . H4A H 0.4136 -0.0696 0.3445 0.040 Uiso 1 1 calc R . . H4B H 0.3635 -0.0874 0.2435 0.040 Uiso 1 1 calc R . . C5 C 0.29661(17) -0.02176(8) 0.27815(14) 0.0272(4) Uani 1 1 d . . . H5 H 0.3468 0.0059 0.2717 0.033 Uiso 1 1 calc R . . C6 C 0.19431(19) -0.01285(8) 0.23040(14) 0.0302(4) Uani 1 1 d . . . H6 H 0.1843 0.0201 0.1963 0.036 Uiso 1 1 calc R . . C7 C 0.1208(2) -0.05508(10) 0.18738(17) 0.0412(6) Uani 1 1 d . . . H7A H 0.1621 -0.0844 0.1737 0.049 Uiso 1 1 calc R . . H7B H 0.0760 -0.0427 0.1300 0.049 Uiso 1 1 calc R . . C8 C 0.0519(2) -0.07268(11) 0.24903(19) 0.0453(7) Uani 1 1 d . . . H8A H -0.0117 -0.0511 0.2382 0.054 Uiso 1 1 calc R . . H8B H 0.0295 -0.1083 0.2336 0.054 Uiso 1 1 calc R . . C9 C 0.12939(17) -0.01589(8) 0.55393(16) 0.0299(4) Uani 1 1 d . . . H9 H 0.0777 -0.0412 0.5329 0.036 Uiso 1 1 calc R . . C10 C 0.1536(2) 0.00387(9) 0.64103(17) 0.0361(5) Uani 1 1 d . . . H10 H 0.1230 -0.0052 0.6893 0.043 Uiso 1 1 calc R . . C11 C 0.23082(18) 0.03913(8) 0.64241(14) 0.0294(4) Uani 1 1 d . . . H11 H 0.2644 0.0595 0.6923 0.035 Uiso 1 1 calc R . . C12 C 0.21146(17) 0.11085(8) 0.31311(15) 0.0284(4) Uani 1 1 d . . . H12 H 0.1764 0.1059 0.2519 0.034 Uiso 1 1 calc R . . C13 C 0.23913(19) 0.15841(8) 0.35283(17) 0.0372(5) Uani 1 1 d . . . H13 H 0.2269 0.1910 0.3248 0.045 Uiso 1 1 calc R . . C14 C 0.28742(17) 0.14837(8) 0.44020(16) 0.0295(4) Uani 1 1 d . . . H14 H 0.3160 0.1728 0.4852 0.035 Uiso 1 1 calc R . . C15 C 0.33287(15) 0.06652(7) 0.52969(13) 0.0212(4) Uani 1 1 d . . . H15 H 0.3667 0.0905 0.5789 0.025 Uiso 1 1 calc R . . C16 C 0.41760(14) 0.03074(7) 0.51212(12) 0.0185(3) Uani 1 1 d . . . C17 C 0.48472(15) 0.04781(7) 0.46028(13) 0.0221(4) Uani 1 1 d . . . H17 H 0.4746 0.0807 0.4332 0.027 Uiso 1 1 calc R . . C18 C 0.56639(15) 0.01721(7) 0.44788(13) 0.0213(4) Uani 1 1 d . . . H18 H 0.6115 0.0291 0.4119 0.026 Uiso 1 1 calc R . . F1 F 0.48495(15) 0.14211(9) 1.30638(14) 0.0749(6) Uani 1 1 d . . . F2 F 0.61410(17) 0.17115(7) 1.40317(11) 0.0624(5) Uani 1 1 d . . . F3 F 0.63568(15) 0.10761(6) 1.32328(11) 0.0541(4) Uani 1 1 d . . . F4 F 0.64004(16) 0.35186(6) 1.2161(2) 0.0884(8) Uani 1 1 d . . . F5 F 0.7734(2) 0.32234(9) 1.30774(14) 0.0946(9) Uani 1 1 d . . . F6 F 0.77671(13) 0.33343(6) 1.17244(12) 0.0519(4) Uani 1 1 d . . . F7 F 0.15263(15) 0.08913(14) 0.93162(19) 0.0765(7) Uani 0.85 1 d P A 1 F8 F 0.2293(3) 0.07115(19) 1.0641(3) 0.1210(16) Uani 0.85 1 d P A 1 F9 F 0.2145(2) 0.14725(12) 1.0208(3) 0.0969(12) Uani 0.85 1 d P A 1 F7A F 0.2512(10) 0.1089(9) 1.0789(8) 0.0765(7) Uani 0.15 1 d PD A 2 F8A F 0.1857(15) 0.1380(9) 0.9646(17) 0.1210(16) Uani 0.15 1 d PD A 2 F9A F 0.1787(13) 0.0615(6) 0.985(2) 0.0969(12) Uani 0.15 1 d PD A 2 F10 F 0.45647(13) 0.01420(6) 0.75831(9) 0.0431(3) Uani 1 1 d . . . F11 F 0.40430(18) -0.03659(6) 0.84830(14) 0.0714(6) Uani 1 1 d . . . F12 F 0.56596(14) -0.01556(6) 0.87102(11) 0.0501(4) Uani 1 1 d . . . F13 F 0.49015(13) 0.17322(6) 0.64176(9) 0.0449(4) Uani 1 1 d . . . F14 F 0.57526(15) 0.24085(9) 0.62740(12) 0.0692(6) Uani 1 1 d . . . F15 F 0.40693(13) 0.24210(6) 0.59528(9) 0.0471(4) Uani 1 1 d . . . F16 F 0.36085(19) 0.34931(8) 0.93205(15) 0.0790(7) Uani 1 1 d . . . F17 F 0.49811(18) 0.38187(8) 0.9103(2) 0.1124(11) Uani 1 1 d . . . F18 F 0.3625(2) 0.37496(8) 0.80332(15) 0.0902(8) Uani 1 1 d . . . F19 F 0.9603(3) 0.03314(10) 1.05621(16) 0.0953(11) Uani 0.89 1 d P B 1 F20 F 0.99492(19) 0.08260(9) 1.16835(18) 0.0734(7) Uani 0.89 1 d P B 1 F21 F 0.85523(13) 0.04085(8) 1.14177(15) 0.0506(5) Uani 0.89 1 d P B 1 F19A F 0.905(3) 0.0664(9) 1.1766(10) 0.0953(11) Uani 0.11 1 d PD B 2 F20A F 0.8787(16) 0.0259(5) 1.0695(14) 0.0734(7) Uani 0.11 1 d PD B 2 F21A F 1.0120(8) 0.0637(7) 1.1099(15) 0.0506(5) Uani 0.11 1 d PD B 2 C50 C 0.93034(19) 0.20879(12) 0.8845(2) 0.0295(6) Uani 0.63 1 d PD C 1 F22 F 1.0251(3) 0.19216(14) 0.8851(3) 0.0711(12) Uani 0.63 1 d PD C 1 F23 F 0.9404(7) 0.25671(14) 0.9117(6) 0.0575(18) Uani 0.63 1 d PD C 1 F24 F 0.8814(3) 0.21263(18) 0.7990(2) 0.0719(12) Uani 0.63 1 d PD C 1 C50A C 0.9440(3) 0.2109(2) 0.8997(3) 0.0295(6) Uani 0.37 1 d PD C 2 F22A F 0.9171(11) 0.2595(3) 0.8953(11) 0.053(3) Uani 0.37 1 d PDU C 2 F23A F 0.9371(6) 0.1938(2) 0.8174(4) 0.0608(17) Uani 0.37 1 d PDU C 2 F24A F 1.0439(3) 0.2099(2) 0.9411(4) 0.0570(15) Uani 0.37 1 d PDU C 2 B1 B 0.59121(16) 0.17737(8) 0.98790(14) 0.0182(4) Uani 1 1 d . . . C19 C 0.60692(14) 0.19935(7) 1.09057(13) 0.0196(3) Uani 1 1 d . . . C20 C 0.65267(15) 0.24724(7) 1.11566(13) 0.0217(4) Uani 1 1 d . . . H20 H 0.6699 0.2683 1.0707 0.026 Uiso 1 1 calc R . . C21 C 0.67363(16) 0.26493(8) 1.20362(14) 0.0256(4) Uani 1 1 d . . . C22 C 0.65283(17) 0.23491(8) 1.27223(14) 0.0289(4) Uani 1 1 d . . . H22 H 0.6677 0.2468 1.3326 0.035 Uiso 1 1 calc R . . C23 C 0.60982(17) 0.18719(8) 1.24958(14) 0.0266(4) Uani 1 1 d . . . C24 C 0.58670(16) 0.16981(7) 1.16104(13) 0.0233(4) Uani 1 1 d . . . H24 H 0.5563 0.1369 1.1480 0.028 Uiso 1 1 calc R . . C25 C 0.7147(2) 0.31787(9) 1.22439(17) 0.0375(5) Uani 1 1 d . . . C26 C 0.5862(2) 0.15224(10) 1.32013(16) 0.0374(5) Uani 1 1 d . . . C27 C 0.50911(14) 0.12929(7) 0.96865(13) 0.0191(3) Uani 1 1 d . . . C28 C 0.41154(15) 0.13306(8) 0.99073(14) 0.0248(4) Uani 1 1 d . . . H28 H 0.3967 0.1627 1.0212 0.030 Uiso 1 1 calc R . . C29 C 0.33631(15) 0.09522(9) 0.96981(15) 0.0283(4) Uani 1 1 d . . . C30 C 0.35383(16) 0.05180(8) 0.92330(15) 0.0285(4) Uani 1 1 d . . . H30 H 0.3019 0.0260 0.9080 0.034 Uiso 1 1 calc R . . C31 C 0.44886(16) 0.04700(7) 0.89970(13) 0.0240(4) Uani 1 1 d . . . C32 C 0.52544(15) 0.08499(7) 0.92273(13) 0.0205(3) Uani 1 1 d . . . H32 H 0.5904 0.0805 0.9067 0.025 Uiso 1 1 calc R . . C33 C 0.23482(19) 0.09983(11) 0.9977(2) 0.0457(6) Uani 1 1 d . . . C34 C 0.4685(2) 0.00222(8) 0.84586(15) 0.0318(5) Uani 1 1 d . . . C35 C 0.54227(14) 0.21929(7) 0.90964(13) 0.0196(3) Uani 1 1 d . . . C36 C 0.53675(15) 0.20672(7) 0.81927(13) 0.0224(4) Uani 1 1 d . . . H36 H 0.5636 0.1747 0.8060 0.027 Uiso 1 1 calc R . . C37 C 0.49364(16) 0.23924(8) 0.74875(13) 0.0248(4) Uani 1 1 d . . . C38 C 0.45444(17) 0.28678(8) 0.76484(15) 0.0305(4) Uani 1 1 d . . . H38 H 0.4260 0.3094 0.7168 0.037 Uiso 1 1 calc R . . C39 C 0.45834(18) 0.29987(8) 0.85283(16) 0.0300(4) Uani 1 1 d . . . C40 C 0.50016(16) 0.26660(8) 0.92379(14) 0.0248(4) Uani 1 1 d . . . H40 H 0.4999 0.2766 0.9835 0.030 Uiso 1 1 calc R . . C41 C 0.49183(19) 0.22420(10) 0.65422(15) 0.0347(5) Uani 1 1 d . . . C42 C 0.4209(2) 0.35120(10) 0.8746(2) 0.0458(6) Uani 1 1 d . . . C43 C 0.70990(14) 0.16104(7) 0.98282(12) 0.0182(3) Uani 1 1 d . . . C44 C 0.76104(15) 0.12074(7) 1.03642(13) 0.0203(4) Uani 1 1 d . . . H44 H 0.7229 0.1006 1.0694 0.024 Uiso 1 1 calc R . . C45 C 0.86550(15) 0.10946(7) 1.04256(13) 0.0218(4) Uani 1 1 d . . . C46 C 0.92488(15) 0.13803(7) 0.99630(14) 0.0246(4) Uani 1 1 d . . . H46 H 0.9968 0.1307 1.0015 0.030 Uiso 1 1 calc R . . C47 C 0.87597(15) 0.17755(7) 0.94248(14) 0.0238(4) Uani 1 1 d . . . C48 C 0.77078(15) 0.18867(7) 0.93582(13) 0.0210(4) Uani 1 1 d . . . H48 H 0.7394 0.2160 0.8980 0.025 Uiso 1 1 calc R . . C49 C 0.91755(17) 0.06626(9) 1.10031(16) 0.0313(5) Uani 1 1 d . . . Cl1 Cl 0.3094(5) 0.2070(3) 0.1748(4) 0.0735(12) Uani 0.15 1 d PD D 1 C51 C 0.356(2) 0.2614(9) 0.1323(13) 0.0735(12) Uani 0.15 1 d PD D 1 H51A H 0.3539 0.2910 0.1721 0.088 Uiso 0.15 1 calc PR D 1 H51B H 0.4296 0.2562 0.1283 0.088 Uiso 0.15 1 calc PR D 1 Cl2 Cl 0.2769(5) 0.2727(3) 0.0259(4) 0.0735(12) Uani 0.15 1 d PD D 1 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 0.02037(8) 0.01667(7) 0.02178(8) -0.00155(5) 0.00482(5) -0.00081(5) N1 0.0223(8) 0.0217(8) 0.0263(8) 0.0012(6) 0.0090(6) 0.0000(6) N2 0.0238(8) 0.0234(8) 0.0206(8) -0.0008(6) 0.0077(6) 0.0021(6) N3 0.0217(8) 0.0187(7) 0.0206(8) -0.0001(6) 0.0019(6) -0.0004(6) N4 0.0210(8) 0.0171(7) 0.0232(8) -0.0019(6) 0.0026(6) 0.0011(6) C1 0.0300(11) 0.0249(10) 0.0492(14) -0.0099(9) 0.0152(10) -0.0087(8) C2 0.0374(12) 0.0156(9) 0.0440(13) 0.0010(8) 0.0161(10) -0.0027(8) C3 0.0377(12) 0.0228(10) 0.0476(14) -0.0016(9) 0.0125(10) 0.0079(9) C4 0.0312(11) 0.0352(12) 0.0342(12) -0.0023(9) 0.0111(9) 0.0082(9) C5 0.0339(11) 0.0279(10) 0.0224(9) -0.0022(8) 0.0115(8) 0.0006(8) C6 0.0422(12) 0.0246(10) 0.0217(9) -0.0026(7) 0.0035(9) 0.0039(9) C7 0.0445(14) 0.0371(13) 0.0342(12) -0.0132(10) -0.0065(10) 0.0059(10) C8 0.0280(12) 0.0470(15) 0.0564(16) -0.0256(12) 0.0012(11) -0.0035(10) C9 0.0273(10) 0.0274(10) 0.0392(12) 0.0072(9) 0.0160(9) 0.0020(8) C10 0.0432(13) 0.0371(12) 0.0356(12) 0.0090(9) 0.0244(10) 0.0085(10) C11 0.0355(11) 0.0328(11) 0.0221(9) 0.0012(8) 0.0114(8) 0.0113(9) C12 0.0278(10) 0.0242(10) 0.0291(10) 0.0049(8) -0.0016(8) -0.0007(8) C13 0.0393(12) 0.0199(10) 0.0452(13) 0.0069(9) -0.0043(10) -0.0010(9) C14 0.0304(11) 0.0162(9) 0.0384(11) -0.0017(8) 0.0011(9) -0.0008(7) C15 0.0214(9) 0.0212(9) 0.0198(9) -0.0014(7) 0.0023(7) -0.0005(7) C16 0.0170(8) 0.0206(8) 0.0166(8) 0.0000(6) 0.0015(6) -0.0002(6) C17 0.0202(9) 0.0231(9) 0.0227(9) 0.0062(7) 0.0047(7) 0.0003(7) C18 0.0191(9) 0.0242(9) 0.0210(9) 0.0034(7) 0.0057(7) -0.0019(7) F1 0.0476(10) 0.1155(17) 0.0655(12) 0.0489(12) 0.0212(9) -0.0100(11) F2 0.1090(16) 0.0553(10) 0.0297(8) 0.0076(7) 0.0298(9) 0.0071(10) F3 0.0866(13) 0.0324(8) 0.0533(10) 0.0176(7) 0.0365(9) 0.0118(8) F4 0.0633(12) 0.0263(8) 0.191(3) -0.0219(11) 0.0604(15) 0.0005(8) F5 0.149(2) 0.0712(14) 0.0489(11) -0.0180(10) -0.0053(13) -0.0531(15) F6 0.0574(10) 0.0338(8) 0.0734(11) -0.0136(7) 0.0330(9) -0.0181(7) F7 0.0165(9) 0.115(2) 0.0936(19) -0.0084(16) 0.0050(10) -0.0062(11) F8 0.0573(17) 0.197(4) 0.132(3) 0.114(3) 0.0690(19) 0.053(2) F9 0.0427(14) 0.0791(18) 0.185(4) -0.048(2) 0.0595(19) -0.0040(12) F7A 0.0165(9) 0.115(2) 0.0936(19) -0.0084(16) 0.0050(10) -0.0062(11) F8A 0.0573(17) 0.197(4) 0.132(3) 0.114(3) 0.0690(19) 0.053(2) F9A 0.0427(14) 0.0791(18) 0.185(4) -0.048(2) 0.0595(19) -0.0040(12) F10 0.0522(9) 0.0504(9) 0.0232(6) -0.0054(6) 0.0018(6) 0.0007(7) F11 0.1046(16) 0.0364(9) 0.0907(14) -0.0274(9) 0.0580(13) -0.0400(10) F12 0.0622(10) 0.0395(8) 0.0418(8) -0.0102(6) -0.0016(7) 0.0226(7) F13 0.0564(9) 0.0456(8) 0.0289(7) -0.0059(6) 0.0025(6) 0.0193(7) F14 0.0614(12) 0.1117(17) 0.0430(10) -0.0076(10) 0.0292(9) -0.0271(11) F15 0.0573(10) 0.0485(9) 0.0271(7) 0.0065(6) -0.0070(6) 0.0145(7) F16 0.1058(17) 0.0589(12) 0.0894(15) 0.0089(10) 0.0575(14) 0.0456(11) F17 0.0675(14) 0.0411(11) 0.225(3) -0.0594(16) 0.0271(17) 0.0061(10) F18 0.137(2) 0.0575(12) 0.0773(14) 0.0218(10) 0.0277(14) 0.0668(13) F19 0.167(3) 0.0762(16) 0.0584(14) 0.0290(12) 0.0583(17) 0.0940(19) F20 0.0516(12) 0.0687(14) 0.0748(15) 0.0226(12) -0.0356(11) -0.0083(10) F21 0.0348(9) 0.0494(11) 0.0653(12) 0.0346(9) 0.0072(8) 0.0081(8) F19A 0.167(3) 0.0762(16) 0.0584(14) 0.0290(12) 0.0583(17) 0.0940(19) F20A 0.0516(12) 0.0687(14) 0.0748(15) 0.0226(12) -0.0356(11) -0.0083(10) F21A 0.0348(9) 0.0494(11) 0.0653(12) 0.0346(9) 0.0072(8) 0.0081(8) C50 0.0253(13) 0.0261(11) 0.0407(16) -0.0021(11) 0.0152(12) -0.0049(9) F22 0.047(2) 0.058(2) 0.129(4) 0.044(2) 0.063(2) 0.0209(16) F23 0.100(5) 0.0221(19) 0.066(3) -0.0046(19) 0.051(3) -0.019(2) F24 0.071(3) 0.110(4) 0.0358(16) 0.0135(18) 0.0170(17) -0.042(2) C50A 0.0253(13) 0.0261(11) 0.0407(16) -0.0021(11) 0.0152(12) -0.0049(9) F22A 0.052(4) 0.031(3) 0.091(7) 0.027(3) 0.045(4) 0.020(3) F23A 0.098(5) 0.050(3) 0.052(3) -0.016(3) 0.054(3) -0.027(3) F24A 0.023(2) 0.066(4) 0.083(4) 0.030(3) 0.015(2) -0.009(2) B1 0.0168(9) 0.0158(9) 0.0225(9) 0.0012(7) 0.0057(7) 0.0009(7) C19 0.0171(8) 0.0188(8) 0.0237(9) 0.0009(7) 0.0066(7) 0.0023(6) C20 0.0211(9) 0.0208(9) 0.0243(9) 0.0007(7) 0.0075(7) -0.0010(7) C21 0.0255(10) 0.0237(9) 0.0279(10) -0.0037(7) 0.0073(8) -0.0008(7) C22 0.0320(11) 0.0329(11) 0.0230(10) -0.0033(8) 0.0090(8) 0.0062(9) C23 0.0308(10) 0.0266(10) 0.0258(10) 0.0058(8) 0.0133(8) 0.0059(8) C24 0.0249(9) 0.0194(9) 0.0272(10) 0.0033(7) 0.0091(8) 0.0024(7) C25 0.0428(13) 0.0315(12) 0.0408(13) -0.0112(10) 0.0149(11) -0.0073(10) C26 0.0473(14) 0.0393(13) 0.0296(11) 0.0100(9) 0.0171(10) 0.0048(11) C27 0.0169(8) 0.0178(8) 0.0220(8) 0.0036(6) 0.0033(7) 0.0011(6) C28 0.0194(9) 0.0246(9) 0.0304(10) 0.0034(8) 0.0060(8) 0.0030(7) C29 0.0158(9) 0.0338(11) 0.0348(11) 0.0072(9) 0.0047(8) -0.0002(8) C30 0.0232(10) 0.0281(10) 0.0315(10) 0.0046(8) 0.0011(8) -0.0074(8) C31 0.0270(10) 0.0209(9) 0.0222(9) 0.0022(7) 0.0021(7) -0.0038(7) C32 0.0191(8) 0.0205(9) 0.0220(9) 0.0028(7) 0.0052(7) 0.0000(7) C33 0.0220(11) 0.0536(16) 0.0629(18) 0.0052(13) 0.0129(11) -0.0016(10) C34 0.0420(13) 0.0239(10) 0.0286(10) -0.0013(8) 0.0063(9) -0.0071(9) C35 0.0169(8) 0.0184(8) 0.0239(9) 0.0021(7) 0.0054(7) -0.0001(6) C36 0.0215(9) 0.0209(9) 0.0244(9) 0.0013(7) 0.0046(7) 0.0029(7) C37 0.0234(9) 0.0263(10) 0.0242(9) 0.0036(7) 0.0044(7) 0.0018(7) C38 0.0297(11) 0.0273(10) 0.0338(11) 0.0114(8) 0.0063(9) 0.0079(8) C39 0.0306(11) 0.0229(10) 0.0377(12) 0.0042(8) 0.0101(9) 0.0100(8) C40 0.0243(10) 0.0228(9) 0.0283(10) 0.0009(7) 0.0079(8) 0.0046(7) C41 0.0334(12) 0.0416(13) 0.0278(11) 0.0058(9) 0.0043(9) 0.0039(10) C42 0.0547(16) 0.0305(12) 0.0531(16) 0.0043(11) 0.0145(13) 0.0205(11) C43 0.0182(8) 0.0166(8) 0.0196(8) -0.0012(6) 0.0040(6) -0.0009(6) C44 0.0193(9) 0.0201(8) 0.0213(9) 0.0001(7) 0.0042(7) -0.0003(7) C45 0.0199(9) 0.0202(9) 0.0238(9) -0.0031(7) 0.0025(7) 0.0019(7) C46 0.0176(9) 0.0217(9) 0.0351(11) -0.0053(8) 0.0072(8) 0.0006(7) C47 0.0217(9) 0.0179(8) 0.0351(11) -0.0029(7) 0.0130(8) -0.0031(7) C48 0.0213(9) 0.0170(8) 0.0260(9) -0.0003(7) 0.0081(7) -0.0005(7) C49 0.0264(10) 0.0323(11) 0.0343(11) 0.0032(9) 0.0055(9) 0.0080(8) Cl1 0.071(3) 0.089(3) 0.067(2) 0.022(2) 0.030(2) 0.017(2) C51 0.071(3) 0.089(3) 0.067(2) 0.022(2) 0.030(2) 0.017(2) Cl2 0.071(3) 0.089(3) 0.067(2) 0.022(2) 0.030(2) 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 Rh1 N3 2.0951(16) . ? Rh1 N1 2.1022(17) . ? Rh1 C5 2.120(2) . ? Rh1 C1 2.125(2) . ? Rh1 C2 2.139(2) . ? Rh1 C6 2.145(2) . ? N1 C9 1.332(3) . ? N1 N2 1.361(2) . ? N2 C11 1.354(3) . ? N2 C15 1.452(3) . ? N3 C12 1.332(3) . ? N3 N4 1.362(2) . ? N4 C14 1.352(2) . ? N4 C15 1.455(2) . ? C1 C2 1.387(3) . ? C1 C8 1.516(4) . ? C1 H1 1.0000 . ? C2 C3 1.521(3) . ? C2 H2 1.0000 . ? C3 C4 1.526(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.510(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.391(3) . ? C5 H5 1.0000 . ? C6 C7 1.513(3) . ? C6 H6 1.0000 . ? C7 C8 1.524(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.394(3) . ? C9 H9 0.9500 . ? C10 C11 1.368(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C12 H12 0.9500 . ? C13 C14 1.363(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.527(3) . ? C15 H15 1.0000 . ? C16 C18 1.390(3) 3_656 ? C16 C17 1.391(3) . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 C16 1.390(3) 3_656 ? C18 H18 0.9500 . ? F1 C26 1.325(3) . ? F2 C26 1.332(3) . ? F3 C26 1.332(3) . ? F4 C25 1.309(3) . ? F5 C25 1.331(3) . ? F6 C25 1.329(3) . ? F7 C33 1.324(4) . ? F8 C33 1.278(4) . ? F9 C33 1.334(4) . ? F7A C33 1.232(11) . ? F8A C33 1.232(11) . ? F9A C33 1.232(11) . ? F10 C34 1.348(3) . ? F11 C34 1.327(3) . ? F12 C34 1.332(3) . ? F13 C41 1.347(3) . ? F14 C41 1.331(3) . ? F15 C41 1.344(3) . ? F16 C42 1.314(4) . ? F17 C42 1.309(4) . ? F18 C42 1.331(3) . ? F19 C49 1.304(3) . ? F20 C49 1.343(3) . ? F21 C49 1.326(3) . ? F19A C49 1.218(10) . ? F20A C49 1.218(10) . ? F21A C49 1.218(10) . ? C50 F22 1.3182(17) . ? C50 F23 1.3184(17) . ? C50 F24 1.3186(17) . ? C50 C47 1.505(3) . ? C50A F24A 1.3180(17) . ? C50A F23A 1.3181(17) . ? C50A F22A 1.3181(17) . ? C50A C47 1.504(3) . ? B1 C43 1.637(3) . ? B1 C19 1.639(3) . ? B1 C27 1.639(3) . ? B1 C35 1.640(3) . ? C19 C24 1.401(3) . ? C19 C20 1.404(3) . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 C25 1.494(3) . ? C22 C23 1.381(3) . ? C22 H22 0.9500 . ? C23 C24 1.393(3) . ? C23 C26 1.501(3) . ? C24 H24 0.9500 . ? C27 C32 1.398(3) . ? C27 C28 1.405(3) . ? C28 C29 1.383(3) . ? C28 H28 0.9500 . ? C29 C30 1.388(3) . ? C29 C33 1.498(3) . ? C30 C31 1.385(3) . ? C30 H30 0.9500 . ? C31 C32 1.400(3) . ? C31 C34 1.489(3) . ? C32 H32 0.9500 . ? C35 C40 1.394(3) . ? C35 C36 1.406(3) . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 C41 1.493(3) . ? C38 C39 1.378(3) . ? C38 H38 0.9500 . ? C39 C40 1.399(3) . ? C39 C42 1.495(3) . ? C40 H40 0.9500 . ? C43 C48 1.397(3) . ? C43 C44 1.406(2) . ? C44 C45 1.386(3) . ? C44 H44 0.9500 . ? C45 C46 1.389(3) . ? C45 C49 1.498(3) . ? C46 C47 1.383(3) . ? C46 H46 0.9500 . ? C47 C48 1.394(3) . ? C48 H48 0.9500 . ? Cl1 C51 1.738(18) . ? C51 Cl2 1.738(18) . ? C51 H51A 0.9900 . ? C51 H51B 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 N3 Rh1 N1 86.83(6) . . ? N3 Rh1 C5 92.70(7) . . ? N1 Rh1 C5 151.91(8) . . ? N3 Rh1 C1 155.47(8) . . ? N1 Rh1 C1 93.99(8) . . ? C5 Rh1 C1 97.78(9) . . ? N3 Rh1 C2 166.55(8) . . ? N1 Rh1 C2 91.82(8) . . ? C5 Rh1 C2 82.21(8) . . ? C1 Rh1 C2 37.97(9) . . ? N3 Rh1 C6 93.54(7) . . ? N1 Rh1 C6 170.01(8) . . ? C5 Rh1 C6 38.07(9) . . ? C1 Rh1 C6 81.54(9) . . ? C2 Rh1 C6 90.09(9) . . ? C9 N1 N2 105.35(17) . . ? C9 N1 Rh1 134.79(15) . . ? N2 N1 Rh1 119.81(12) . . ? C11 N2 N1 110.99(17) . . ? C11 N2 C15 128.14(18) . . ? N1 N2 C15 120.44(15) . . ? C12 N3 N4 104.98(16) . . ? C12 N3 Rh1 133.64(14) . . ? N4 N3 Rh1 120.21(12) . . ? C14 N4 N3 111.29(16) . . ? C14 N4 C15 129.28(17) . . ? N3 N4 C15 119.33(15) . . ? C2 C1 C8 126.2(2) . . ? C2 C1 Rh1 71.56(12) . . ? C8 C1 Rh1 109.66(17) . . ? C2 C1 H1 113.8 . . ? C8 C1 H1 113.8 . . ? Rh1 C1 H1 113.8 . . ? C1 C2 C3 123.7(2) . . ? C1 C2 Rh1 70.47(12) . . ? C3 C2 Rh1 112.55(15) . . ? C1 C2 H2 114.2 . . ? C3 C2 H2 114.2 . . ? Rh1 C2 H2 114.2 . . ? C2 C3 C4 112.04(18) . . ? 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 113.47(18) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.6(2) . . ? C6 C5 Rh1 71.93(13) . . ? C4 C5 Rh1 109.60(14) . . ? C6 C5 H5 113.9 . . ? C4 C5 H5 113.9 . . ? Rh1 C5 H5 113.9 . . ? C5 C6 C7 123.1(2) . . ? C5 C6 Rh1 70.00(12) . . ? C7 C6 Rh1 113.30(17) . . ? C5 C6 H6 114.3 . . ? C7 C6 H6 114.3 . . ? Rh1 C6 H6 114.3 . . ? C6 C7 C8 111.33(19) . . ? 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 113.1(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 111.0(2) . . ? N1 C9 H9 124.5 . . ? C10 C9 H9 124.5 . . ? C11 C10 C9 105.50(19) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 107.2(2) . . ? N2 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? N3 C12 C13 111.02(19) . . ? N3 C12 H12 124.5 . . ? C13 C12 H12 124.5 . . ? C14 C13 C12 105.57(19) . . ? C14 C13 H13 127.2 . . ? C12 C13 H13 127.2 . . ? N4 C14 C13 107.15(19) . . ? N4 C14 H14 126.4 . . ? C13 C14 H14 126.4 . . ? N2 C15 N4 109.34(15) . . ? N2 C15 C16 112.80(15) . . ? N4 C15 C16 111.61(15) . . ? N2 C15 H15 107.6 . . ? N4 C15 H15 107.6 . . ? C16 C15 H15 107.6 . . ? C18 C16 C17 119.33(17) 3_656 . ? C18 C16 C15 121.16(16) 3_656 . ? C17 C16 C15 119.35(16) . . ? C18 C17 C16 120.48(17) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C16 120.19(17) . 3_656 ? C17 C18 H18 119.9 . . ? C16 C18 H18 119.9 3_656 . ? F22 C50 F23 106.7(4) . . ? F22 C50 F24 105.8(3) . . ? F23 C50 F24 103.3(5) . . ? F22 C50 C47 113.3(2) . . ? F23 C50 C47 110.9(5) . . ? F24 C50 C47 115.9(2) . . ? F24A C50A F23A 106.8(6) . . ? F24A C50A F22A 105.5(7) . . ? F23A C50A F22A 108.7(8) . . ? F24A C50A C47 114.1(4) . . ? F23A C50A C47 107.7(4) . . ? F22A C50A C47 113.7(8) . . ? C43 B1 C19 103.30(14) . . ? C43 B1 C27 112.70(15) . . ? C19 B1 C27 111.78(15) . . ? C43 B1 C35 110.80(15) . . ? C19 B1 C35 113.81(15) . . ? C27 B1 C35 104.70(15) . . ? C24 C19 C20 115.40(18) . . ? C24 C19 B1 122.60(17) . . ? C20 C19 B1 121.64(16) . . ? C21 C20 C19 122.51(18) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C20 C21 C22 120.94(19) . . ? C20 C21 C25 119.68(19) . . ? C22 C21 C25 119.33(19) . . ? C23 C22 C21 117.66(19) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 C23 C24 121.47(19) . . ? C22 C23 C26 120.8(2) . . ? C24 C23 C26 117.7(2) . . ? C23 C24 C19 121.99(19) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? F4 C25 F6 106.6(2) . . ? F4 C25 F5 106.6(2) . . ? F6 C25 F5 104.2(2) . . ? F4 C25 C21 112.6(2) . . ? F6 C25 C21 113.52(19) . . ? F5 C25 C21 112.6(2) . . ? F1 C26 F2 105.5(2) . . ? F1 C26 F3 107.1(2) . . ? F2 C26 F3 105.6(2) . . ? F1 C26 C23 112.2(2) . . ? F2 C26 C23 113.7(2) . . ? F3 C26 C23 112.25(19) . . ? C32 C27 C28 115.83(17) . . ? C32 C27 B1 123.68(16) . . ? C28 C27 B1 120.20(17) . . ? C29 C28 C27 122.56(19) . . ? C29 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 C29 C30 120.59(19) . . ? C28 C29 C33 120.9(2) . . ? C30 C29 C33 118.5(2) . . ? C31 C30 C29 118.43(19) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? C30 C31 C32 120.63(19) . . ? C30 C31 C34 119.98(19) . . ? C32 C31 C34 119.33(19) . . ? C27 C32 C31 121.95(18) . . ? C27 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? F8A C33 F9A 111.0(16) . . ? F8A C33 F7A 102.0(15) . . ? F9A C33 F7A 105.8(15) . . ? F8 C33 F7 107.0(3) . . ? F8 C33 F9 106.5(4) . . ? F7 C33 F9 102.7(3) . . ? F8A C33 C29 111.3(7) . . ? F9A C33 C29 115.5(7) . . ? F7A C33 C29 110.2(6) . . ? F8 C33 C29 113.6(2) . . ? F7 C33 C29 112.8(3) . . ? F9 C33 C29 113.4(2) . . ? F11 C34 F12 107.4(2) . . ? F11 C34 F10 106.19(19) . . ? F12 C34 F10 104.4(2) . . ? F11 C34 C31 113.1(2) . . ? F12 C34 C31 113.29(18) . . ? F10 C34 C31 111.77(18) . . ? C40 C35 C36 115.46(17) . . ? C40 C35 B1 125.68(17) . . ? C36 C35 B1 118.79(16) . . ? C37 C36 C35 122.56(18) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C36 C37 C38 120.83(19) . . ? C36 C37 C41 120.12(19) . . ? C38 C37 C41 119.02(19) . . ? C39 C38 C37 117.72(19) . . ? C39 C38 H38 121.1 . . ? C37 C38 H38 121.1 . . ? C38 C39 C40 121.34(19) . . ? C38 C39 C42 120.1(2) . . ? C40 C39 C42 118.5(2) . . ? C35 C40 C39 122.05(19) . . ? C35 C40 H40 119.0 . . ? C39 C40 H40 119.0 . . ? F14 C41 F15 107.1(2) . . ? F14 C41 F13 105.5(2) . . ? F15 C41 F13 105.49(19) . . ? F14 C41 C37 112.6(2) . . ? F15 C41 C37 112.3(2) . . ? F13 C41 C37 113.21(19) . . ? F17 C42 F16 105.8(3) . . ? F17 C42 F18 107.3(3) . . ? F16 C42 F18 104.1(2) . . ? F17 C42 C39 112.4(2) . . ? F16 C42 C39 113.3(2) . . ? F18 C42 C39 113.3(2) . . ? C48 C43 C44 115.78(17) . . ? C48 C43 B1 123.86(16) . . ? C44 C43 B1 119.92(16) . . ? C45 C44 C43 121.99(18) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C44 C45 C46 121.17(18) . . ? C44 C45 C49 120.59(18) . . ? C46 C45 C49 118.24(18) . . ? C47 C46 C45 117.87(18) . . ? C47 C46 H46 121.1 . . ? C45 C46 H46 121.1 . . ? C46 C47 C48 120.96(18) . . ? C46 C47 C50A 116.8(3) . . ? C48 C47 C50A 121.9(3) . . ? C46 C47 C50 122.58(19) . . ? C48 C47 C50 116.38(19) . . ? C47 C48 C43 122.23(18) . . ? C47 C48 H48 118.9 . . ? C43 C48 H48 118.9 . . ? F19A C49 F21A 104.7(17) . . ? F19A C49 F20A 103.5(19) . . ? F21A C49 F20A 108.7(14) . . ? F19A C49 F19 132.2(8) . . ? F21A C49 F19 58.3(11) . . ? F20A C49 F19 54.3(12) . . ? F19A C49 F21 45.7(17) . . ? F21A C49 F21 129.9(7) . . ? F20A C49 F21 60.1(13) . . ? F19 C49 F21 107.7(2) . . ? F19A C49 F20 60.6(17) . . ? F21A C49 F20 50.1(11) . . ? F20A C49 F20 138.4(7) . . ? F19 C49 F20 105.8(2) . . ? F21 C49 F20 103.3(2) . . ? F19A C49 C45 114.5(8) . . ? F21A C49 C45 115.2(7) . . ? F20A C49 C45 109.5(7) . . ? F19 C49 C45 112.9(2) . . ? F21 C49 C45 114.36(18) . . ? F20 C49 C45 112.0(2) . . ? Cl2 C51 Cl1 107.5(16) . . ? Cl2 C51 H51A 110.2 . . ? Cl1 C51 H51A 110.2 . . ? Cl2 C51 H51B 110.2 . . ? Cl1 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Rh1 N1 C9 148.5(2) . . . . ? C5 Rh1 N1 C9 -121.7(2) . . . . ? C1 Rh1 N1 C9 -6.9(2) . . . . ? C2 Rh1 N1 C9 -44.8(2) . . . . ? N3 Rh1 N1 N2 -34.42(14) . . . . ? C5 Rh1 N1 N2 55.4(2) . . . . ? C1 Rh1 N1 N2 170.14(15) . . . . ? C2 Rh1 N1 N2 132.18(15) . . . . ? C9 N1 N2 C11 0.6(2) . . . . ? Rh1 N1 N2 C11 -177.24(13) . . . . ? C9 N1 N2 C15 173.69(17) . . . . ? Rh1 N1 N2 C15 -4.1(2) . . . . ? N1 Rh1 N3 C12 -135.9(2) . . . . ? C5 Rh1 N3 C12 72.3(2) . . . . ? C1 Rh1 N3 C12 -43.2(3) . . . . ? C2 Rh1 N3 C12 139.6(3) . . . . ? C6 Rh1 N3 C12 34.1(2) . . . . ? N1 Rh1 N3 N4 29.69(14) . . . . ? C5 Rh1 N3 N4 -122.19(15) . . . . ? C1 Rh1 N3 N4 122.3(2) . . . . ? C2 Rh1 N3 N4 -54.9(4) . . . . ? C6 Rh1 N3 N4 -160.31(15) . . . . ? C12 N3 N4 C14 -0.5(2) . . . . ? Rh1 N3 N4 C14 -169.71(14) . . . . ? C12 N3 N4 C15 -177.21(17) . . . . ? Rh1 N3 N4 C15 13.6(2) . . . . ? N3 Rh1 C1 C2 -178.95(16) . . . . ? N1 Rh1 C1 C2 -87.85(14) . . . . ? C5 Rh1 C1 C2 66.59(15) . . . . ? C6 Rh1 C1 C2 101.14(15) . . . . ? N3 Rh1 C1 C8 58.3(3) . . . . ? N1 Rh1 C1 C8 149.36(16) . . . . ? C5 Rh1 C1 C8 -56.20(17) . . . . ? C2 Rh1 C1 C8 -122.8(2) . . . . ? C6 Rh1 C1 C8 -21.65(16) . . . . ? C8 C1 C2 C3 -3.4(4) . . . . ? Rh1 C1 C2 C3 -104.6(2) . . . . ? C8 C1 C2 Rh1 101.3(2) . . . . ? N3 Rh1 C2 C1 178.1(3) . . . . ? N1 Rh1 C2 C1 94.15(15) . . . . ? C5 Rh1 C2 C1 -113.41(15) . . . . ? C6 Rh1 C2 C1 -76.05(15) . . . . ? N3 Rh1 C2 C3 -62.6(4) . . . . ? N1 Rh1 C2 C3 -146.53(17) . . . . ? C5 Rh1 C2 C3 5.90(17) . . . . ? C1 Rh1 C2 C3 119.3(2) . . . . ? C6 Rh1 C2 C3 43.27(18) . . . . ? C1 C2 C3 C4 92.4(3) . . . . ? Rh1 C2 C3 C4 11.5(3) . . . . ? C2 C3 C4 C5 -31.0(3) . . . . ? C3 C4 C5 C6 -46.1(3) . . . . ? C3 C4 C5 Rh1 35.3(2) . . . . ? N3 Rh1 C5 C6 -92.30(13) . . . . ? N1 Rh1 C5 C6 179.38(14) . . . . ? C1 Rh1 C5 C6 65.47(14) . . . . ? C2 Rh1 C5 C6 100.21(14) . . . . ? N3 Rh1 C5 C4 145.42(15) . . . . ? N1 Rh1 C5 C4 57.1(2) . . . . ? C1 Rh1 C5 C4 -56.81(17) . . . . ? C2 Rh1 C5 C4 -22.07(16) . . . . ? C6 Rh1 C5 C4 -122.3(2) . . . . ? C4 C5 C6 C7 -3.8(4) . . . . ? Rh1 C5 C6 C7 -105.4(2) . . . . ? C4 C5 C6 Rh1 101.6(2) . . . . ? N3 Rh1 C6 C5 89.86(13) . . . . ? C1 Rh1 C6 C5 -114.31(14) . . . . ? C2 Rh1 C6 C5 -77.19(14) . . . . ? N3 Rh1 C6 C7 -151.74(16) . . . . ? C5 Rh1 C6 C7 118.4(2) . . . . ? C1 Rh1 C6 C7 4.08(17) . . . . ? C2 Rh1 C6 C7 41.21(17) . . . . ? C5 C6 C7 C8 95.0(3) . . . . ? Rh1 C6 C7 C8 14.4(3) . . . . ? C2 C1 C8 C7 -44.6(3) . . . . ? Rh1 C1 C8 C7 36.5(2) . . . . ? C6 C7 C8 C1 -33.5(3) . . . . ? N2 N1 C9 C10 -0.6(2) . . . . ? Rh1 N1 C9 C10 176.74(15) . . . . ? N1 C9 C10 C11 0.4(3) . . . . ? N1 N2 C11 C10 -0.3(2) . . . . ? C15 N2 C11 C10 -172.79(19) . . . . ? C9 C10 C11 N2 0.0(2) . . . . ? N4 N3 C12 C13 0.2(2) . . . . ? Rh1 N3 C12 C13 167.32(17) . . . . ? N3 C12 C13 C14 0.1(3) . . . . ? N3 N4 C14 C13 0.6(3) . . . . ? C15 N4 C14 C13 176.9(2) . . . . ? C12 C13 C14 N4 -0.4(3) . . . . ? C11 N2 C15 N4 -127.0(2) . . . . ? N1 N2 C15 N4 61.2(2) . . . . ? C11 N2 C15 C16 108.2(2) . . . . ? N1 N2 C15 C16 -63.6(2) . . . . ? C14 N4 C15 N2 117.1(2) . . . . ? N3 N4 C15 N2 -66.9(2) . . . . ? C14 N4 C15 C16 -117.4(2) . . . . ? N3 N4 C15 C16 58.6(2) . . . . ? N2 C15 C16 C18 -22.6(2) . . . 3_656 ? N4 C15 C16 C18 -146.21(17) . . . 3_656 ? N2 C15 C16 C17 161.94(17) . . . . ? N4 C15 C16 C17 38.4(2) . . . . ? C18 C16 C17 C18 0.5(3) 3_656 . . . ? C15 C16 C17 C18 176.05(17) . . . . ? C16 C17 C18 C16 -0.5(3) . . . 3_656 ? C43 B1 C19 C24 -98.7(2) . . . . ? C27 B1 C19 C24 22.8(2) . . . . ? C35 B1 C19 C24 141.13(18) . . . . ? C43 B1 C19 C20 74.1(2) . . . . ? C27 B1 C19 C20 -164.44(16) . . . . ? C35 B1 C19 C20 -46.1(2) . . . . ? C24 C19 C20 C21 -1.9(3) . . . . ? B1 C19 C20 C21 -175.17(18) . . . . ? C19 C20 C21 C22 2.0(3) . . . . ? C19 C20 C21 C25 -175.3(2) . . . . ? C20 C21 C22 C23 -0.6(3) . . . . ? C25 C21 C22 C23 176.7(2) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C21 C22 C23 C26 179.3(2) . . . . ? C22 C23 C24 C19 0.8(3) . . . . ? C26 C23 C24 C19 -179.27(19) . . . . ? C20 C19 C24 C23 0.5(3) . . . . ? B1 C19 C24 C23 173.72(18) . . . . ? C20 C21 C25 F4 87.8(3) . . . . ? C22 C21 C25 F4 -89.5(3) . . . . ? C20 C21 C25 F6 -33.4(3) . . . . ? C22 C21 C25 F6 149.3(2) . . . . ? C20 C21 C25 F5 -151.6(2) . . . . ? C22 C21 C25 F5 31.1(3) . . . . ? C22 C23 C26 F1 117.3(3) . . . . ? C24 C23 C26 F1 -62.6(3) . . . . ? C22 C23 C26 F2 -2.3(3) . . . . ? C24 C23 C26 F2 177.8(2) . . . . ? C22 C23 C26 F3 -122.1(2) . . . . ? C24 C23 C26 F3 58.0(3) . . . . ? C43 B1 C27 C32 -21.4(2) . . . . ? C19 B1 C27 C32 -137.19(18) . . . . ? C35 B1 C27 C32 99.2(2) . . . . ? C43 B1 C27 C28 164.98(17) . . . . ? C19 B1 C27 C28 49.2(2) . . . . ? C35 B1 C27 C28 -74.5(2) . . . . ? C32 C27 C28 C29 0.9(3) . . . . ? B1 C27 C28 C29 175.02(18) . . . . ? C27 C28 C29 C30 -1.6(3) . . . . ? C27 C28 C29 C33 177.6(2) . . . . ? C28 C29 C30 C31 1.0(3) . . . . ? C33 C29 C30 C31 -178.3(2) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? C29 C30 C31 C34 -176.98(19) . . . . ? C28 C27 C32 C31 0.5(3) . . . . ? B1 C27 C32 C31 -173.45(17) . . . . ? C30 C31 C32 C27 -1.1(3) . . . . ? C34 C31 C32 C27 176.26(18) . . . . ? C28 C29 C33 F8A 60.4(17) . . . . ? C30 C29 C33 F8A -120.4(16) . . . . ? C28 C29 C33 F9A -171.9(17) . . . . ? C30 C29 C33 F9A 7.4(17) . . . . ? C28 C29 C33 F7A -52.1(12) . . . . ? C30 C29 C33 F7A 127.2(12) . . . . ? C28 C29 C33 F8 -104.9(4) . . . . ? C30 C29 C33 F8 74.3(4) . . . . ? C28 C29 C33 F7 133.0(3) . . . . ? C30 C29 C33 F7 -47.7(3) . . . . ? C28 C29 C33 F9 16.8(4) . . . . ? C30 C29 C33 F9 -163.9(3) . . . . ? C30 C31 C34 F11 -19.1(3) . . . . ? C32 C31 C34 F11 163.6(2) . . . . ? C30 C31 C34 F12 -141.7(2) . . . . ? C32 C31 C34 F12 41.0(3) . . . . ? C30 C31 C34 F10 100.7(2) . . . . ? C32 C31 C34 F10 -76.6(3) . . . . ? C43 B1 C35 C40 -126.33(19) . . . . ? C19 B1 C35 C40 -10.4(3) . . . . ? C27 B1 C35 C40 111.9(2) . . . . ? C43 B1 C35 C36 56.8(2) . . . . ? C19 B1 C35 C36 172.65(16) . . . . ? C27 B1 C35 C36 -65.0(2) . . . . ? C40 C35 C36 C37 0.8(3) . . . . ? B1 C35 C36 C37 177.99(18) . . . . ? C35 C36 C37 C38 0.8(3) . . . . ? C35 C36 C37 C41 178.82(19) . . . . ? C36 C37 C38 C39 -1.1(3) . . . . ? C41 C37 C38 C39 -179.2(2) . . . . ? C37 C38 C39 C40 0.0(3) . . . . ? C37 C38 C39 C42 177.8(2) . . . . ? C36 C35 C40 C39 -1.9(3) . . . . ? B1 C35 C40 C39 -178.95(19) . . . . ? C38 C39 C40 C35 1.7(3) . . . . ? C42 C39 C40 C35 -176.2(2) . . . . ? C36 C37 C41 F14 -92.3(3) . . . . ? C38 C37 C41 F14 85.8(3) . . . . ? C36 C37 C41 F15 146.7(2) . . . . ? C38 C37 C41 F15 -35.2(3) . . . . ? C36 C37 C41 F13 27.4(3) . . . . ? C38 C37 C41 F13 -154.5(2) . . . . ? C38 C39 C42 F17 -105.7(3) . . . . ? C40 C39 C42 F17 72.1(3) . . . . ? C38 C39 C42 F16 134.4(3) . . . . ? C40 C39 C42 F16 -47.8(3) . . . . ? C38 C39 C42 F18 16.1(4) . . . . ? C40 C39 C42 F18 -166.0(2) . . . . ? C19 B1 C43 C48 -106.13(19) . . . . ? C27 B1 C43 C48 133.06(18) . . . . ? C35 B1 C43 C48 16.1(2) . . . . ? C19 B1 C43 C44 65.9(2) . . . . ? C27 B1 C43 C44 -55.0(2) . . . . ? C35 B1 C43 C44 -171.90(16) . . . . ? C48 C43 C44 C45 0.4(3) . . . . ? B1 C43 C44 C45 -172.18(17) . . . . ? C43 C44 C45 C46 0.6(3) . . . . ? C43 C44 C45 C49 179.99(18) . . . . ? C44 C45 C46 C47 -1.2(3) . . . . ? C49 C45 C46 C47 179.41(19) . . . . ? C45 C46 C47 C48 0.7(3) . . . . ? C45 C46 C47 C50A 174.7(3) . . . . ? C45 C46 C47 C50 -175.8(2) . . . . ? F24A C50A C47 C46 -22.0(6) . . . . ? F23A C50A C47 C46 96.4(5) . . . . ? F22A C50A C47 C46 -143.0(7) . . . . ? F24A C50A C47 C48 151.9(4) . . . . ? F23A C50A C47 C48 -89.7(6) . . . . ? F22A C50A C47 C48 30.8(8) . . . . ? F24A C50A C47 C50 -149(2) . . . . ? F23A C50A C47 C50 -30.6(16) . . . . ? F22A C50A C47 C50 90(2) . . . . ? F22 C50 C47 C46 4.9(4) . . . . ? F23 C50 C47 C46 -115.0(4) . . . . ? F24 C50 C47 C46 127.6(3) . . . . ? F22 C50 C47 C48 -171.7(3) . . . . ? F23 C50 C47 C48 68.3(4) . . . . ? F24 C50 C47 C48 -49.1(4) . . . . ? F22 C50 C47 C50A 62.7(17) . . . . ? F23 C50 C47 C50A -57.3(19) . . . . ? F24 C50 C47 C50A -175(2) . . . . ? C46 C47 C48 C43 0.3(3) . . . . ? C50A C47 C48 C43 -173.3(3) . . . . ? C50 C47 C48 C43 177.1(2) . . . . ? C44 C43 C48 C47 -0.9(3) . . . . ? B1 C43 C48 C47 171.41(18) . . . . ? C44 C45 C49 F19A -50(2) . . . . ? C46 C45 C49 F19A 130(2) . . . . ? C44 C45 C49 F21A -171.1(14) . . . . ? C46 C45 C49 F21A 8.3(14) . . . . ? C44 C45 C49 F20A 66.0(15) . . . . ? C46 C45 C49 F20A -114.6(15) . . . . ? C44 C45 C49 F19 124.5(3) . . . . ? C46 C45 C49 F19 -56.1(3) . . . . ? C44 C45 C49 F21 0.9(3) . . . . ? C46 C45 C49 F21 -179.7(2) . . . . ? C44 C45 C49 F20 -116.2(3) . . . . ? C46 C45 C49 F20 63.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.506 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.072 #===END data_compound10 _database_code_depnum_ccdc_archive 'CCDC 798124' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C32 H12 B F24), C24 H18 N8 O4 Rh2, 0.125(C H2 Cl2) ' _chemical_formula_sum 'C88.125 H42.25 B2 Cl0.25 F48 N8 O4 Rh2' _chemical_formula_weight 2425.35 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.1319(3) _cell_length_b 19.1238(4) _cell_length_c 31.7567(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.6480(10) _cell_angle_gamma 90.00 _cell_volume 9520.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9717 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 24.67 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4781.1 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.9062 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85461 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 33929 _reflns_number_gt 28061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; Three CF3 groups are disordered over two sites each (C87 F25 F26 F27; C175/C178 F91 F92 F93; C176/C177 F94 F95 F96). The following restraints were used: sadi 0.005 c171 c175 c171 c178 sadi 0.001 c175 f91 c178 f91a sadi 0.001 c175 f92 c178 f92a sadi 0.001 c175 f93 c178 f93a sadi 0.005 c176 c173 c177 c173 sadi 0.001 c176 f94 c177 f94a sadi 0.001 c176 f95 c177 f95a sadi 0.001 c176 f96 c177 f96a same c175 f91 f92 f93 same c176 f94 f95 f96 sadi 0.001 c87 f25a c87 f26a c87 f27a as well as same anisotropic displacement parameters for some of the atoms: eadp c175 c178 eadp f91 f91a eadp f92 f92a eadp f93 f93a eadp f94 f94a eadp f95 f95a eadp f96 f96a eadp c176 c177 eadp f25 f25a eadp f26 f26a eadp f27 f27a Furthermore, a dichloromethane molecule with very low site occupancy (25 percent, equally disordered over two sites) was refined using the following restraints: sadi 0.001 cl1a c1a cl2a c1a cl1b c1b cl2b c1b, same cl1a c1a cl2a, and only three variables of thermal vibration for the whole molecule, i.e., eadp cl1a cl1b cl2a cl2b c1a c1b. One hydrogen atom of one of these dichloromethane molecules was refined (using riding model) in very close proximity to an aromatic hydrogen atom with full site occupancy. An unusually short contact (1.88 Angstroms) is thus simulated. This problem could arise from the C-atom of this CH2 group being located very close to a Cl-site of the alternative CH2Cl2 position, which might have driven the refinement of the C-atom coordinates into a false position. 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+2.7246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(11) _refine_ls_number_reflns 33929 _refine_ls_number_parameters 2795 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.94410(2) 0.54171(2) 0.519849(13) 0.04378(10) Uani 1 1 d . . . Rh2 Rh 1.10235(2) 0.33435(2) 0.647140(12) 0.03484(8) Uani 1 1 d . . . O1 O 0.9142(3) 0.4921(3) 0.42838(18) 0.0999(17) Uani 1 1 d . . . O2 O 1.1275(3) 0.5006(3) 0.53120(18) 0.0937(16) Uani 1 1 d . . . O3 O 1.2208(3) 0.4149(2) 0.60678(17) 0.0854(14) Uani 1 1 d . . . O4 O 1.1164(2) 0.2075(2) 0.59352(13) 0.0623(10) Uani 1 1 d . . . N1 N 0.8158(2) 0.56478(19) 0.51062(13) 0.0398(9) Uani 1 1 d . . . N2 N 0.7762(2) 0.57114(19) 0.54361(13) 0.0380(9) Uani 1 1 d . . . N3 N 0.9631(2) 0.5869(2) 0.58109(12) 0.0427(9) Uani 1 1 d . . . N4 N 0.8975(2) 0.5990(2) 0.60019(12) 0.0400(9) Uani 1 1 d . . . N5 N 1.0325(2) 0.27705(19) 0.68206(12) 0.0340(8) Uani 1 1 d . . . N6 N 0.9810(2) 0.30723(18) 0.70503(11) 0.0301(8) Uani 1 1 d . . . N7 N 1.0916(2) 0.4202(2) 0.68574(12) 0.0372(9) Uani 1 1 d . . . N8 N 1.0298(2) 0.42541(19) 0.70833(11) 0.0332(8) Uani 1 1 d . . . C1 C 0.9268(4) 0.5091(4) 0.4635(2) 0.0668(16) Uani 1 1 d . . . C2 C 1.0598(4) 0.5170(3) 0.5275(2) 0.0598(15) Uani 1 1 d . . . C3 C 0.7554(3) 0.5768(3) 0.47410(18) 0.0527(13) Uani 1 1 d . . . H3 H 0.7645 0.5764 0.4456 0.063 Uiso 1 1 calc R . . C4 C 0.6781(3) 0.5898(3) 0.48427(19) 0.0549(14) Uani 1 1 d . . . H4 H 0.6255 0.6003 0.4645 0.066 Uiso 1 1 calc R . . C5 C 0.6921(3) 0.5848(2) 0.52784(18) 0.0462(12) Uani 1 1 d . . . H5 H 0.6506 0.5899 0.5444 0.055 Uiso 1 1 calc R . . C6 C 1.0291(3) 0.6220(3) 0.60587(18) 0.0565(15) Uani 1 1 d . . . H6 H 1.0840 0.6252 0.5999 0.068 Uiso 1 1 calc R . . C7 C 1.0078(4) 0.6520(3) 0.6404(2) 0.0630(16) Uani 1 1 d . . . H7 H 1.0443 0.6781 0.6628 0.076 Uiso 1 1 calc R . . C8 C 0.9227(4) 0.6375(3) 0.63662(18) 0.0530(13) Uani 1 1 d . . . H8 H 0.8886 0.6516 0.6558 0.064 Uiso 1 1 calc R . . C9 C 0.8194(3) 0.5576(2) 0.58831(14) 0.0353(10) Uani 1 1 d . . . H9 H 0.7809 0.5749 0.6066 0.042 Uiso 1 1 calc R . . C10 C 0.8362(2) 0.4806(2) 0.59925(14) 0.0289(9) Uani 1 1 d . . . C11 C 0.7893(2) 0.4283(2) 0.57400(13) 0.0291(9) Uani 1 1 d . . . H11 H 0.7508 0.4397 0.5473 0.035 Uiso 1 1 calc R . . C12 C 0.7988(2) 0.3600(2) 0.58758(14) 0.0325(9) Uani 1 1 d . . . H12 H 0.7671 0.3242 0.5702 0.039 Uiso 1 1 calc R . . C13 C 0.8549(2) 0.3431(2) 0.62704(13) 0.0282(9) Uani 1 1 d . . . H13 H 0.8611 0.2958 0.6364 0.034 Uiso 1 1 calc R . . C14 C 0.9012(2) 0.3945(2) 0.65235(13) 0.0261(9) Uani 1 1 d . . . C15 C 0.8920(2) 0.4631(2) 0.63786(13) 0.0253(9) Uani 1 1 d . . . H15 H 0.9249 0.4988 0.6549 0.030 Uiso 1 1 calc R . . C16 C 1.1738(4) 0.3845(3) 0.61999(18) 0.0545(14) Uani 1 1 d . . . C17 C 1.1116(3) 0.2557(3) 0.61309(17) 0.0457(12) Uani 1 1 d . . . C18 C 1.0395(3) 0.2111(2) 0.69497(16) 0.0408(11) Uani 1 1 d . . . H18 H 1.0722 0.1769 0.6844 0.049 Uiso 1 1 calc R . . C19 C 0.9933(3) 0.1979(3) 0.72562(15) 0.0396(11) Uani 1 1 d . . . H19 H 0.9882 0.1549 0.7398 0.048 Uiso 1 1 calc R . . C20 C 0.9567(3) 0.2610(2) 0.73088(15) 0.0365(10) Uani 1 1 d . . . H20 H 0.9202 0.2700 0.7498 0.044 Uiso 1 1 calc R . . C21 C 1.1428(3) 0.4754(3) 0.69880(17) 0.0459(12) Uani 1 1 d . . . H21 H 1.1928 0.4854 0.6890 0.055 Uiso 1 1 calc R . . C22 C 1.1135(3) 0.5154(3) 0.7280(2) 0.0564(15) Uani 1 1 d . . . H22 H 1.1382 0.5571 0.7417 0.068 Uiso 1 1 calc R . . C23 C 1.0416(3) 0.4827(3) 0.73347(16) 0.0430(11) Uani 1 1 d . . . H23 H 1.0062 0.4978 0.7517 0.052 Uiso 1 1 calc R . . C24 C 0.9551(2) 0.3806(2) 0.69783(13) 0.0271(9) Uani 1 1 d . . . H24 H 0.9192 0.3921 0.7186 0.032 Uiso 1 1 calc R . . B1 B 0.4372(3) 0.7261(2) 0.45848(14) 0.0215(9) Uani 1 1 d . . . F1 F 0.4620(3) 0.99523(16) 0.44341(11) 0.0786(11) Uani 1 1 d . . . F2 F 0.3699(3) 1.02066(17) 0.38679(14) 0.0956(14) Uani 1 1 d . . . F3 F 0.4939(4) 1.0016(2) 0.3829(2) 0.155(3) Uani 1 1 d . . . F4 F 0.3212(3) 0.72410(19) 0.29214(10) 0.0830(12) Uani 1 1 d . . . F5 F 0.23450(18) 0.8129(3) 0.28575(10) 0.0869(13) Uani 1 1 d . . . F6 F 0.3529(2) 0.8196(2) 0.26933(9) 0.0647(9) Uani 1 1 d . . . F7 F 0.5935(3) 0.5908(3) 0.35607(16) 0.125(2) Uani 1 1 d . . . F8 F 0.4751(3) 0.5809(2) 0.31505(11) 0.1065(17) Uani 1 1 d . . . F9 F 0.5364(3) 0.49086(17) 0.34268(11) 0.0827(12) Uani 1 1 d . . . F10 F 0.3146(2) 0.43100(18) 0.43383(12) 0.0770(11) Uani 1 1 d . . . F11 F 0.4384(2) 0.40631(16) 0.47102(11) 0.0705(10) Uani 1 1 d . . . F12 F 0.3589(3) 0.47216(17) 0.49807(12) 0.0849(12) Uani 1 1 d . . . F13 F 0.5954(2) 0.69031(19) 0.62172(9) 0.0614(9) Uani 1 1 d . . . F14 F 0.6649(3) 0.78579(18) 0.63085(9) 0.0728(10) Uani 1 1 d . . . F15 F 0.7276(2) 0.6905(2) 0.62265(10) 0.0791(11) Uani 1 1 d . . . F16 F 0.73751(19) 0.7801(2) 0.43591(9) 0.0810(12) Uani 1 1 d . . . F17 F 0.7858(2) 0.8505(2) 0.48907(13) 0.0903(13) Uani 1 1 d . . . F18 F 0.82384(18) 0.7459(2) 0.49318(11) 0.0833(12) Uani 1 1 d . . . F19 F 0.3741(2) 0.86585(17) 0.59683(10) 0.0653(9) Uani 1 1 d . . . F20 F 0.2448(2) 0.8963(2) 0.57345(13) 0.0876(13) Uani 1 1 d . . . F21 F 0.3401(3) 0.93346(17) 0.54306(12) 0.0825(12) Uani 1 1 d . . . F22 F 0.1374(2) 0.6222(2) 0.46908(13) 0.0808(11) Uani 1 1 d . . . F23 F 0.0823(2) 0.7158(3) 0.44255(17) 0.128(2) Uani 1 1 d . . . F24 F 0.0879(2) 0.6902(2) 0.50927(14) 0.0964(14) Uani 1 1 d . . . C49 C 0.4174(2) 0.7836(2) 0.41884(13) 0.0241(8) Uani 1 1 d . . . C50 C 0.4380(2) 0.8541(2) 0.42630(13) 0.0257(9) Uani 1 1 d . . . H50 H 0.4663 0.8688 0.4546 0.031 Uiso 1 1 calc R . . C51 C 0.4181(3) 0.9034(2) 0.39303(14) 0.0301(9) Uani 1 1 d . . . C52 C 0.3773(3) 0.8839(2) 0.35133(14) 0.0315(10) Uani 1 1 d . . . H52 H 0.3648 0.9175 0.3287 0.038 Uiso 1 1 calc R . . C53 C 0.3552(2) 0.8150(2) 0.34327(13) 0.0287(9) Uani 1 1 d . . . C54 C 0.3736(2) 0.7662(2) 0.37675(12) 0.0240(8) Uani 1 1 d . . . H54 H 0.3556 0.7193 0.3707 0.029 Uiso 1 1 calc R . . C55 C 0.4387(4) 0.9783(3) 0.40217(17) 0.0487(13) Uani 1 1 d . . . C56 C 0.3152(3) 0.7933(3) 0.29847(15) 0.0428(12) Uani 1 1 d . . . C57 C 0.4408(2) 0.6456(2) 0.44036(12) 0.0220(8) Uani 1 1 d . . . C58 C 0.4774(2) 0.6324(2) 0.40529(12) 0.0256(9) Uani 1 1 d . . . H58 H 0.4989 0.6706 0.3920 0.031 Uiso 1 1 calc R . . C59 C 0.4836(3) 0.5660(2) 0.38921(13) 0.0302(9) Uani 1 1 d . . . C60 C 0.4524(3) 0.5086(2) 0.40731(14) 0.0329(10) Uani 1 1 d . . . H60 H 0.4550 0.4629 0.3959 0.039 Uiso 1 1 calc R . . C61 C 0.4170(3) 0.5201(2) 0.44276(14) 0.0312(9) Uani 1 1 d . . . C62 C 0.4125(2) 0.5866(2) 0.45869(12) 0.0243(8) Uani 1 1 d . . . H62 H 0.3890 0.5925 0.4832 0.029 Uiso 1 1 calc R . . C63 C 0.5225(3) 0.5564(3) 0.35126(17) 0.0474(13) Uani 1 1 d . . . C64 C 0.3822(3) 0.4585(2) 0.46161(16) 0.0424(11) Uani 1 1 d . . . C65 C 0.5331(2) 0.7402(2) 0.49047(12) 0.0222(8) Uani 1 1 d . . . C66 C 0.5526(2) 0.7283(2) 0.53493(12) 0.0229(8) Uani 1 1 d . . . H66 H 0.5088 0.7126 0.5481 0.027 Uiso 1 1 calc R . . C67 C 0.6345(2) 0.7386(2) 0.56088(13) 0.0269(9) Uani 1 1 d . . . C68 C 0.7011(3) 0.7598(2) 0.54254(14) 0.0346(10) Uani 1 1 d . . . H68 H 0.7569 0.7672 0.5600 0.042 Uiso 1 1 calc R . . C69 C 0.6831(2) 0.7697(3) 0.49821(13) 0.0349(10) Uani 1 1 d . . . C70 C 0.6001(2) 0.7608(2) 0.47313(13) 0.0261(9) Uani 1 1 d . . . H70 H 0.5893 0.7693 0.4428 0.031 Uiso 1 1 calc R . . C71 C 0.6538(3) 0.7274(3) 0.60855(14) 0.0373(11) Uani 1 1 d . . . C72 C 0.7549(3) 0.7891(4) 0.47829(16) 0.0533(15) Uani 1 1 d . . . C73 C 0.3611(2) 0.7395(2) 0.48411(12) 0.0224(8) Uani 1 1 d . . . C74 C 0.3686(2) 0.7949(2) 0.51322(12) 0.0262(9) Uani 1 1 d . . . H74 H 0.4213 0.8193 0.5212 0.031 Uiso 1 1 calc R . . C75 C 0.3008(3) 0.8161(2) 0.53129(13) 0.0313(10) Uani 1 1 d . . . C76 C 0.2242(3) 0.7815(2) 0.52055(14) 0.0353(11) Uani 1 1 d . . . H76 H 0.1782 0.7954 0.5327 0.042 Uiso 1 1 calc R . . C77 C 0.2150(3) 0.7265(2) 0.49193(14) 0.0351(10) Uani 1 1 d . . . C78 C 0.2813(2) 0.7057(2) 0.47360(13) 0.0286(9) Uani 1 1 d . . . H78 H 0.2725 0.6680 0.4536 0.034 Uiso 1 1 calc R . . C79 C 0.3137(3) 0.8769(3) 0.56076(16) 0.0421(12) Uani 1 1 d . . . C80 C 0.1304(3) 0.6900(3) 0.4779(2) 0.0555(15) Uani 1 1 d . . . B2 B 0.9382(3) 0.2169(2) 0.95255(15) 0.0234(10) Uani 1 1 d . . . F25 F 0.8076(8) 0.0191(3) 1.0357(2) 0.123(4) Uani 0.71 1 d P A 1 F26 F 0.8610(4) 0.0846(4) 1.0873(2) 0.0937(17) Uani 0.71 1 d P A 1 F27 F 0.7286(4) 0.0731(4) 1.0705(2) 0.105(3) Uani 0.71 1 d P A 1 F25A F 0.781(2) 0.0865(8) 1.0908(5) 0.123(4) Uani 0.29 1 d PD A 2 F26A F 0.7252(10) 0.0362(8) 1.0352(5) 0.0937(17) Uani 0.29 1 d PD A 2 F27A F 0.8466(11) 0.0270(9) 1.0536(7) 0.105(3) Uani 0.29 1 d PD A 2 F28 F 0.5944(2) 0.2665(3) 0.92988(15) 0.1054(15) Uani 1 1 d . . . F29 F 0.6553(3) 0.3460(2) 0.9722(2) 0.130(2) Uani 1 1 d . . . F30 F 0.5803(2) 0.2688(2) 0.99470(13) 0.0941(13) Uani 1 1 d . . . F31 F 1.20401(17) 0.17054(16) 1.13009(8) 0.0494(7) Uani 1 1 d . . . F32 F 1.06757(17) 0.15619(18) 1.11728(8) 0.0545(8) Uani 1 1 d . . . F33 F 1.12078(19) 0.25928(16) 1.12125(8) 0.0528(8) Uani 1 1 d . . . F34 F 1.25038(19) 0.1911(3) 0.94092(10) 0.1092(18) Uani 1 1 d . . . F35 F 1.2776(3) 0.0999(3) 0.9786(2) 0.147(2) Uani 1 1 d . . . F36 F 1.32940(16) 0.1954(2) 1.00342(9) 0.0694(10) Uani 1 1 d . . . F37 F 0.9225(3) -0.07294(17) 0.85826(13) 0.0873(13) Uani 1 1 d . . . F38 F 1.04135(18) -0.03229(15) 0.89137(11) 0.0617(8) Uani 1 1 d . . . F39 F 0.9482(3) -0.05699(16) 0.92590(12) 0.0798(12) Uani 1 1 d . . . F40 F 0.83054(19) 0.1562(2) 0.76588(9) 0.0747(11) Uani 1 1 d . . . F41 F 0.72476(16) 0.10738(18) 0.78021(9) 0.0586(8) Uani 1 1 d . . . F42 F 0.7468(3) 0.2121(2) 0.79791(11) 0.0910(13) Uani 1 1 d . . . F43 F 1.0707(3) 0.3371(2) 0.83600(14) 0.0999(15) Uani 1 1 d . . . F44 F 0.9559(2) 0.3850(2) 0.80785(10) 0.0862(12) Uani 1 1 d . . . F45 F 1.0570(3) 0.4472(2) 0.84170(12) 0.1007(15) Uani 1 1 d . . . F46 F 0.8487(4) 0.5217(2) 0.93868(16) 0.132(2) Uani 1 1 d . . . F47 F 0.9713(3) 0.5296(2) 0.97741(16) 0.1187(18) Uani 1 1 d . . . F48 F 0.8807(3) 0.46998(18) 0.99863(14) 0.1003(15) Uani 1 1 d . . . C81 C 0.8583(2) 0.2071(2) 0.97582(12) 0.0243(8) Uani 1 1 d . . . C82 C 0.8569(2) 0.1506(2) 1.00420(12) 0.0266(9) Uani 1 1 d . . . H82 H 0.9053 0.1208 1.0117 0.032 Uiso 1 1 calc R . . C83 C 0.7874(3) 0.1370(2) 1.02159(13) 0.0340(10) Uani 1 1 d . . . C84 C 0.7151(3) 0.1793(3) 1.01180(15) 0.0395(11) Uani 1 1 d . . . H84 H 0.6679 0.1707 1.0242 0.047 Uiso 1 1 calc R . . C85 C 0.7145(3) 0.2336(3) 0.98379(16) 0.0412(12) Uani 1 1 d . . . C86 C 0.7836(2) 0.2476(2) 0.96602(14) 0.0312(9) Uani 1 1 d . . . H86 H 0.7802 0.2858 0.9466 0.037 Uiso 1 1 calc R . . C87 C 0.7902(4) 0.0772(3) 1.05123(18) 0.0547(14) Uani 1 1 d . . . C88 C 0.6377(3) 0.2783(4) 0.9710(2) 0.0676(18) Uani 1 1 d . . . C89 C 1.0302(2) 0.20129(19) 0.98636(12) 0.0203(8) Uani 1 1 d . . . C90 C 1.0439(2) 0.2061(2) 1.03144(12) 0.0228(8) Uani 1 1 d . . . H90 H 0.9974 0.2183 1.0436 0.027 Uiso 1 1 calc R . . C91 C 1.1236(2) 0.1937(2) 1.05925(13) 0.0264(9) Uani 1 1 d . . . C92 C 1.1941(2) 0.1789(2) 1.04315(13) 0.0273(9) Uani 1 1 d . . . H92 H 1.2483 0.1704 1.0620 0.033 Uiso 1 1 calc R . . C93 C 1.1830(2) 0.1768(2) 0.99846(13) 0.0303(9) Uani 1 1 d . . . C94 C 1.1024(2) 0.1863(2) 0.97060(13) 0.0265(9) Uani 1 1 d . . . H94 H 1.0966 0.1825 0.9402 0.032 Uiso 1 1 calc R . . C95 C 1.1296(3) 0.1958(3) 1.10631(14) 0.0372(11) Uani 1 1 d . . . C96 C 1.2589(3) 0.1644(4) 0.98073(16) 0.0539(15) Uani 1 1 d . . . C97 C 0.9184(2) 0.1612(2) 0.91270(12) 0.0215(8) Uani 1 1 d . . . C98 C 0.9484(2) 0.0917(2) 0.91647(12) 0.0234(8) Uani 1 1 d . . . H98 H 0.9853 0.0770 0.9429 0.028 Uiso 1 1 calc R . . C99 C 0.9254(2) 0.0442(2) 0.88273(13) 0.0289(9) Uani 1 1 d . . . C100 C 0.8728(3) 0.0627(2) 0.84359(13) 0.0301(10) Uani 1 1 d . . . H100 H 0.8582 0.0298 0.8206 0.036 Uiso 1 1 calc R . . C101 C 0.8419(2) 0.1301(2) 0.83868(13) 0.0272(9) Uani 1 1 d . . . C102 C 0.8627(2) 0.1784(2) 0.87264(13) 0.0261(9) Uani 1 1 d . . . H102 H 0.8388 0.2240 0.8686 0.031 Uiso 1 1 calc R . . C103 C 0.9602(3) -0.0283(2) 0.88961(15) 0.0364(10) Uani 1 1 d . . . C104 C 0.7884(3) 0.1523(3) 0.79629(14) 0.0362(10) Uani 1 1 d . . . C105 C 0.9464(2) 0.2967(2) 0.93478(12) 0.0228(8) Uani 1 1 d . . . C106 C 0.9777(2) 0.3099(2) 0.89825(13) 0.0276(9) Uani 1 1 d . . . H106 H 0.9925 0.2713 0.8826 0.033 Uiso 1 1 calc R . . C107 C 0.9881(3) 0.3774(2) 0.88367(14) 0.0316(10) Uani 1 1 d . . . C108 C 0.9673(3) 0.4341(2) 0.90517(14) 0.0377(11) Uani 1 1 d . . . H108 H 0.9732 0.4801 0.8950 0.045 Uiso 1 1 calc R . . C109 C 0.9372(3) 0.4232(2) 0.94261(14) 0.0377(11) Uani 1 1 d . . . C110 C 0.9281(2) 0.3562(2) 0.95691(13) 0.0304(9) Uani 1 1 d . . . H110 H 0.9088 0.3500 0.9827 0.036 Uiso 1 1 calc R . . C111 C 1.0193(3) 0.3878(3) 0.84350(17) 0.0451(12) Uani 1 1 d . . . C112 C 0.9123(5) 0.4854(3) 0.9650(2) 0.0655(17) Uani 1 1 d . . . Rh3 Rh 0.41612(2) 1.08736(3) 0.865998(14) 0.05058(11) Uani 1 1 d . . . Rh4 Rh 0.56450(3) 0.86138(3) 0.940024(17) 0.05946(13) Uani 1 1 d . . . O5 O 0.3816(3) 0.8362(3) 0.8972(2) 0.126(2) Uani 1 1 d . . . O6 O 0.5168(5) 0.9253(5) 1.0165(3) 0.163(4) Uani 1 1 d . . . O7 O 0.4162(4) 1.2066(3) 0.9267(2) 0.136(3) Uani 1 1 d . . . O8 O 0.3427(4) 0.9938(3) 0.9235(2) 0.120(2) Uani 1 1 d . . . N9 N 0.4669(2) 1.1525(2) 0.82615(12) 0.0373(9) Uani 1 1 d . . . N10 N 0.5126(2) 1.12675(19) 0.79846(11) 0.0325(8) Uani 1 1 d . . . N11 N 0.4164(2) 1.0081(2) 0.82136(13) 0.0404(9) Uani 1 1 d . . . N12 N 0.4714(2) 1.00675(19) 0.79473(12) 0.0331(8) Uani 1 1 d . . . N13 N 0.5985(3) 0.8198(2) 0.88620(14) 0.0531(11) Uani 1 1 d . . . N14 N 0.6748(2) 0.8313(2) 0.87746(12) 0.0413(9) Uani 1 1 d . . . N15 N 0.6933(2) 0.8683(2) 0.97008(13) 0.0451(10) Uani 1 1 d . . . N16 N 0.7536(2) 0.8683(2) 0.94687(12) 0.0357(8) Uani 1 1 d . . . C25 C 0.4163(4) 1.1602(4) 0.9042(2) 0.085(2) Uani 1 1 d . . . C26 C 0.3711(4) 1.0288(4) 0.9022(3) 0.081(2) Uani 1 1 d . . . C27 C 0.3641(3) 0.9545(3) 0.80891(19) 0.0533(14) Uani 1 1 d . . . H27 H 0.3181 0.9423 0.8214 0.064 Uiso 1 1 calc R . . C28 C 0.3860(3) 0.9189(3) 0.77521(19) 0.0558(14) Uani 1 1 d . . . H28 H 0.3595 0.8782 0.7610 0.067 Uiso 1 1 calc R . . C29 C 0.4542(3) 0.9546(3) 0.76639(16) 0.0427(12) Uani 1 1 d . . . H29 H 0.4832 0.9439 0.7444 0.051 Uiso 1 1 calc R . . C30 C 0.4598(3) 1.2206(3) 0.81768(18) 0.0495(14) Uani 1 1 d . . . H30 H 0.4294 1.2520 0.8317 0.059 Uiso 1 1 calc R . . C31 C 0.5009(3) 1.2405(3) 0.78658(17) 0.0494(13) Uani 1 1 d . . . H31 H 0.5058 1.2861 0.7756 0.059 Uiso 1 1 calc R . . C32 C 0.5337(3) 1.1788(3) 0.77479(16) 0.0420(11) Uani 1 1 d . . . H32 H 0.5658 1.1741 0.7534 0.050 Uiso 1 1 calc R . . C33 C 0.5426(2) 1.0567(2) 0.80198(13) 0.0301(9) Uani 1 1 d . . . H33 H 0.5728 1.0493 0.7782 0.036 Uiso 1 1 calc R . . C34 C 0.6074(2) 1.0419(2) 0.84481(12) 0.0232(8) Uani 1 1 d . . . C35 C 0.6451(2) 1.0950(2) 0.87195(13) 0.0290(9) Uani 1 1 d . . . H35 H 0.6287 1.1421 0.8649 0.035 Uiso 1 1 calc R . . C36 C 0.7072(2) 1.0803(2) 0.90977(13) 0.0304(9) Uani 1 1 d . . . H36 H 0.7319 1.1171 0.9287 0.036 Uiso 1 1 calc R . . C37 C 0.7322(3) 1.0123(2) 0.91925(13) 0.0308(9) Uani 1 1 d . . . H37 H 0.7747 1.0022 0.9448 0.037 Uiso 1 1 calc R . . C38 C 0.6960(2) 0.9580(2) 0.89173(13) 0.0285(9) Uani 1 1 d . . . C39 C 0.6329(2) 0.9727(2) 0.85517(13) 0.0267(9) Uani 1 1 d . . . H39 H 0.6066 0.9356 0.8369 0.032 Uiso 1 1 calc R . . C40 C 0.4502(4) 0.8473(4) 0.9135(3) 0.088(2) Uani 1 1 d . . . C41 C 0.5360(5) 0.8997(5) 0.9857(3) 0.105(3) Uani 1 1 d . . . C42 C 0.5583(4) 0.7753(3) 0.8544(2) 0.0745(19) Uani 1 1 d . . . H42 H 0.5027 0.7567 0.8518 0.089 Uiso 1 1 calc R . . C43 C 0.6103(5) 0.7611(4) 0.8267(2) 0.081(2) Uani 1 1 d . . . H43 H 0.5973 0.7315 0.8020 0.097 Uiso 1 1 calc R . . C44 C 0.6828(4) 0.7973(3) 0.84117(19) 0.0625(16) Uani 1 1 d . . . H44 H 0.7304 0.7989 0.8284 0.075 Uiso 1 1 calc R . . C45 C 0.7362(4) 0.8602(3) 1.01101(18) 0.0574(14) Uani 1 1 d . . . H45 H 0.7104 0.8574 1.0349 0.069 Uiso 1 1 calc R . . C46 C 0.8222(4) 0.8565(3) 1.01432(18) 0.0556(14) Uani 1 1 d . . . H46 H 0.8658 0.8518 1.0401 0.067 Uiso 1 1 calc R . . C47 C 0.8324(3) 0.8609(2) 0.97295(17) 0.0434(12) Uani 1 1 d . . . H47 H 0.8848 0.8590 0.9642 0.052 Uiso 1 1 calc R . . C48 C 0.7319(3) 0.8840(2) 0.90066(14) 0.0332(10) Uani 1 1 d . . . H48 H 0.7857 0.8817 0.8903 0.040 Uiso 1 1 calc R . . B3 B 0.4633(3) 0.5209(2) 0.75428(14) 0.0219(9) Uani 1 1 d . . . F49 F 0.7791(2) 0.3515(2) 0.85432(16) 0.1039(15) Uani 1 1 d . . . F50 F 0.7060(4) 0.4085(2) 0.88857(13) 0.1192(19) Uani 1 1 d . . . F51 F 0.6497(2) 0.3257(2) 0.84856(14) 0.0998(15) Uani 1 1 d . . . F52 F 0.85360(18) 0.5293(2) 0.75984(16) 0.0938(13) Uani 1 1 d . . . F53 F 0.7791(3) 0.4855(3) 0.70303(19) 0.165(3) Uani 1 1 d . . . F54 F 0.7600(2) 0.5890(3) 0.71965(13) 0.0924(13) Uani 1 1 d . . . F55 F 0.2821(2) 0.3083(2) 0.81886(12) 0.0853(13) Uani 1 1 d . . . F56 F 0.2008(3) 0.39337(19) 0.79444(16) 0.1040(17) Uani 1 1 d . . . F57 F 0.1850(2) 0.2967(2) 0.76259(13) 0.0942(14) Uani 1 1 d . . . F58 F 0.4105(2) 0.33100(16) 0.63300(8) 0.0530(7) Uani 1 1 d . . . F59 F 0.46548(19) 0.25621(17) 0.68135(10) 0.0594(8) Uani 1 1 d . . . F60 F 0.33286(19) 0.25069(15) 0.65072(9) 0.0516(7) Uani 1 1 d . . . F61 F 0.5007(2) 0.80505(15) 0.66319(10) 0.0626(9) Uani 1 1 d . . . F62 F 0.4831(2) 0.79624(15) 0.72811(11) 0.0614(8) Uani 1 1 d . . . F63 F 0.59634(16) 0.75540(15) 0.71307(9) 0.0472(7) Uani 1 1 d . . . F64 F 0.3164(2) 0.53331(18) 0.58586(10) 0.0745(10) Uani 1 1 d . . . F65 F 0.3528(3) 0.6244(2) 0.56323(10) 0.0997(15) Uani 1 1 d . . . F66 F 0.2491(3) 0.6256(4) 0.59127(16) 0.168(3) Uani 1 1 d . . . F67 F 0.5947(3) 0.6229(4) 0.91328(14) 0.143(2) Uani 1 1 d . . . F68 F 0.5160(6) 0.5576(4) 0.93467(16) 0.218(5) Uani 1 1 d . . . F69 F 0.4972(3) 0.6627(3) 0.93614(14) 0.129(2) Uani 1 1 d . . . F70 F 0.20472(18) 0.66955(17) 0.76628(11) 0.0615(9) Uani 1 1 d . . . F71 F 0.1967(2) 0.6530(2) 0.83133(14) 0.0978(14) Uani 1 1 d . . . F72 F 0.2577(2) 0.74425(19) 0.81473(13) 0.0793(11) Uani 1 1 d . . . C113 C 0.5640(2) 0.4978(2) 0.76709(13) 0.0265(9) Uani 1 1 d . . . C114 C 0.5922(3) 0.4496(2) 0.80005(14) 0.0325(10) Uani 1 1 d . . . H114 H 0.5516 0.4302 0.8141 0.039 Uiso 1 1 calc R . . C115 C 0.6770(3) 0.4281(3) 0.81362(17) 0.0438(12) Uani 1 1 d . . . C116 C 0.7374(3) 0.4543(3) 0.79378(18) 0.0448(13) Uani 1 1 d . . . H116 H 0.7955 0.4404 0.8031 0.054 Uiso 1 1 calc R . . C117 C 0.7120(3) 0.5013(2) 0.75987(17) 0.0401(12) Uani 1 1 d . . . C118 C 0.6262(2) 0.5226(2) 0.74642(14) 0.0294(9) Uani 1 1 d . . . H118 H 0.6101 0.5543 0.7229 0.035 Uiso 1 1 calc R . . C119 C 0.7025(3) 0.3780(3) 0.85056(19) 0.0557(15) Uani 1 1 d . . . C120 C 0.7742(3) 0.5260(3) 0.7355(2) 0.0590(16) Uani 1 1 d . . . C121 C 0.4079(2) 0.4497(2) 0.74348(12) 0.0237(8) Uani 1 1 d . . . C122 C 0.3476(2) 0.4268(2) 0.76629(13) 0.0286(9) Uani 1 1 d . . . H122 H 0.3366 0.4551 0.7889 0.034 Uiso 1 1 calc R . . C123 C 0.3043(2) 0.3644(2) 0.75662(13) 0.0281(9) Uani 1 1 d . . . C124 C 0.3173(2) 0.3211(2) 0.72389(14) 0.0305(10) Uani 1 1 d . . . H124 H 0.2870 0.2783 0.7174 0.037 Uiso 1 1 calc R . . C125 C 0.3765(2) 0.3422(2) 0.70066(12) 0.0266(9) Uani 1 1 d . . . C126 C 0.4205(2) 0.4042(2) 0.71105(12) 0.0254(9) Uani 1 1 d . . . H126 H 0.4616 0.4167 0.6953 0.030 Uiso 1 1 calc R . . C127 C 0.2438(3) 0.3411(3) 0.78354(17) 0.0431(12) Uani 1 1 d . . . C128 C 0.3956(3) 0.2949(2) 0.66662(14) 0.0353(10) Uani 1 1 d . . . C129 C 0.4441(2) 0.5758(2) 0.71296(12) 0.0217(8) Uani 1 1 d . . . C130 C 0.4816(2) 0.6425(2) 0.71913(13) 0.0284(9) Uani 1 1 d . . . H130 H 0.5170 0.6536 0.7467 0.034 Uiso 1 1 calc R . . C131 C 0.4694(2) 0.6930(2) 0.68685(14) 0.0289(9) Uani 1 1 d . . . C132 C 0.4177(2) 0.6791(2) 0.64605(13) 0.0282(9) Uani 1 1 d . . . H132 H 0.4087 0.7130 0.6236 0.034 Uiso 1 1 calc R . . C133 C 0.3800(2) 0.6138(2) 0.63945(13) 0.0274(9) Uani 1 1 d . . . C134 C 0.3922(2) 0.5638(2) 0.67204(12) 0.0222(8) Uani 1 1 d . . . H134 H 0.3642 0.5199 0.6662 0.027 Uiso 1 1 calc R . . C135 C 0.5116(3) 0.7624(2) 0.69711(16) 0.0395(11) Uani 1 1 d . . . C136 C 0.3216(3) 0.5991(3) 0.59626(16) 0.0463(12) Uani 1 1 d . . . C137 C 0.4374(2) 0.5642(2) 0.79410(12) 0.0248(9) Uani 1 1 d . . . C138 C 0.4871(3) 0.5699(2) 0.83635(14) 0.0335(10) Uani 1 1 d . . . H138 H 0.5413 0.5477 0.8436 0.040 Uiso 1 1 calc R . . C139 C 0.4595(3) 0.6073(3) 0.86831(14) 0.0390(11) Uani 1 1 d . . . C140 C 0.3829(3) 0.6415(2) 0.85929(15) 0.0392(11) Uani 1 1 d . . . H140 H 0.3646 0.6669 0.8812 0.047 Uiso 1 1 calc R . . C141 C 0.3328(3) 0.6381(2) 0.81764(14) 0.0345(10) Uani 1 1 d . . . C142 C 0.3592(3) 0.6006(2) 0.78586(14) 0.0313(10) Uani 1 1 d . . . H142 H 0.3234 0.5993 0.7575 0.038 Uiso 1 1 calc R . . C143 C 0.5167(4) 0.6097(4) 0.91293(17) 0.0644(18) Uani 1 1 d . . . C144 C 0.2496(3) 0.6760(3) 0.80724(18) 0.0499(13) Uani 1 1 d . . . B4 B 0.0360(3) 0.9246(2) 0.73858(14) 0.0234(9) Uani 1 1 d . . . F73 F 0.2898(2) 0.7764(2) 0.71786(14) 0.0874(13) Uani 1 1 d . . . F74 F 0.2276(2) 0.70125(19) 0.67475(12) 0.0753(10) Uani 1 1 d . . . F75 F 0.2851(3) 0.7849(3) 0.6503(2) 0.163(3) Uani 1 1 d . . . F76 F 0.0047(3) 0.8330(3) 0.54605(11) 0.1210(19) Uani 1 1 d . . . F77 F -0.0768(3) 0.8984(3) 0.56777(12) 0.1122(17) Uani 1 1 d . . . F78 F -0.0869(3) 0.7912(3) 0.57703(15) 0.145(2) Uani 1 1 d . . . F79 F 0.19683(17) 0.88224(15) 0.90143(8) 0.0480(7) Uani 1 1 d . . . F80 F 0.2085(2) 0.77133(16) 0.90575(9) 0.0595(8) Uani 1 1 d . . . F81 F 0.10426(19) 0.82233(18) 0.92343(8) 0.0572(8) Uani 1 1 d . . . F82 F -0.0046(2) 0.62494(15) 0.80501(11) 0.0609(8) Uani 1 1 d . . . F83 F -0.11819(19) 0.68340(17) 0.78423(11) 0.0634(9) Uani 1 1 d . . . F84 F -0.0384(3) 0.66300(17) 0.74045(10) 0.0796(12) Uani 1 1 d . . . F85 F 0.3028(3) 1.04297(19) 0.69865(16) 0.1048(16) Uani 1 1 d . . . F86 F 0.3328(2) 1.1336(3) 0.73550(11) 0.0936(14) Uani 1 1 d . . . F87 F 0.23089(19) 1.1336(2) 0.68181(11) 0.0787(12) Uani 1 1 d . . . F88 F 0.1461(3) 1.09416(18) 0.87481(9) 0.0947(15) Uani 1 1 d . . . F89 F 0.1863(2) 1.18657(16) 0.84851(10) 0.0652(9) Uani 1 1 d . . . F90 F 0.0543(3) 1.1589(2) 0.83344(13) 0.0892(13) Uani 1 1 d . . . C175 C -0.1856(8) 1.0874(7) 0.6425(3) 0.064(2) Uani 0.39 1 d PD B 1 F91 F -0.1189(12) 1.1294(10) 0.6416(8) 0.087(3) Uani 0.39 1 d PD B 1 F92 F -0.1917(8) 1.0532(7) 0.6036(4) 0.110(3) Uani 0.39 1 d PD B 1 F93 F -0.2634(8) 1.1098(6) 0.6387(4) 0.0910(18) Uani 0.39 1 d PD B 1 C178 C -0.1749(6) 1.0963(5) 0.6479(3) 0.064(2) Uani 0.61 1 d PD B 2 F91A F -0.1092(7) 1.1088(6) 0.6294(5) 0.087(3) Uani 0.61 1 d PD B 2 F92A F -0.2413(6) 1.0816(5) 0.6127(3) 0.110(3) Uani 0.61 1 d PD B 2 F93A F -0.1957(5) 1.1559(3) 0.6625(2) 0.0910(18) Uani 0.61 1 d PD B 2 C176 C -0.2852(5) 0.9218(8) 0.7393(4) 0.062(2) Uani 0.39 1 d PD B 1 F94 F -0.2974(7) 0.9566(7) 0.7741(4) 0.081(2) Uani 0.39 1 d PD B 1 F95 F -0.275(3) 0.8552(7) 0.7525(13) 0.112(5) Uani 0.39 1 d PD B 1 F96 F -0.3590(5) 0.9202(7) 0.7107(4) 0.101(2) Uani 0.39 1 d PD B 1 C177 C -0.2794(4) 0.9310(6) 0.7477(3) 0.062(2) Uani 0.61 1 d PD B 2 F94A F -0.2567(4) 0.9304(4) 0.7913(2) 0.081(2) Uani 0.61 1 d PD B 2 F95A F -0.2888(19) 0.8625(5) 0.7393(8) 0.112(5) Uani 0.61 1 d PD B 2 F96A F -0.3528(3) 0.9641(4) 0.7362(3) 0.101(2) Uani 0.61 1 d PD B 2 C145 C 0.0581(2) 0.8842(2) 0.69651(12) 0.0233(8) Uani 1 1 d . . . C146 C 0.1356(2) 0.8470(2) 0.70302(14) 0.0317(10) Uani 1 1 d . . . H146 H 0.1729 0.8465 0.7311 0.038 Uiso 1 1 calc R . . C147 C 0.1588(3) 0.8111(2) 0.66969(15) 0.0366(11) Uani 1 1 d . . . C148 C 0.1054(3) 0.8098(3) 0.62866(16) 0.0436(13) Uani 1 1 d . . . H148 H 0.1210 0.7849 0.6058 0.052 Uiso 1 1 calc R . . C149 C 0.0296(3) 0.8454(3) 0.62178(14) 0.0409(12) Uani 1 1 d . . . C150 C 0.0058(3) 0.8806(2) 0.65558(14) 0.0323(10) Uani 1 1 d . . . H150 H -0.0483 0.9030 0.6501 0.039 Uiso 1 1 calc R . . C151 C 0.2398(3) 0.7700(3) 0.67736(19) 0.0532(14) Uani 1 1 d . . . C152 C -0.0314(4) 0.8412(5) 0.57856(18) 0.0699(19) Uani 1 1 d . . . C153 C 0.0458(2) 0.8648(2) 0.77633(12) 0.0233(8) Uani 1 1 d . . . C154 C 0.0957(2) 0.8703(2) 0.81911(12) 0.0240(8) Uani 1 1 d . . . H154 H 0.1271 0.9119 0.8279 0.029 Uiso 1 1 calc R . . C155 C 0.1001(2) 0.8159(2) 0.84894(12) 0.0257(9) Uani 1 1 d . . . C156 C 0.0582(2) 0.7541(2) 0.83767(13) 0.0272(9) Uani 1 1 d . . . H156 H 0.0619 0.7173 0.8581 0.033 Uiso 1 1 calc R . . C157 C 0.0097(3) 0.7467(2) 0.79526(13) 0.0291(9) Uani 1 1 d . . . C158 C 0.0045(3) 0.8002(2) 0.76575(13) 0.0270(9) Uani 1 1 d . . . H158 H -0.0284 0.7932 0.7370 0.032 Uiso 1 1 calc R . . C159 C 0.1525(3) 0.8239(2) 0.89448(13) 0.0322(9) Uani 1 1 d . . . C160 C -0.0371(3) 0.6798(3) 0.78139(16) 0.0449(12) Uani 1 1 d . . . C161 C 0.0997(2) 0.9912(2) 0.75310(12) 0.0229(8) Uani 1 1 d . . . C162 C 0.1593(2) 1.0135(2) 0.72991(13) 0.0248(8) Uani 1 1 d . . . H162 H 0.1653 0.9874 0.7053 0.030 Uiso 1 1 calc R . . C163 C 0.2099(2) 1.0726(2) 0.74197(13) 0.0293(9) Uani 1 1 d . . . C164 C 0.2032(3) 1.1118(2) 0.77757(14) 0.0349(10) Uani 1 1 d . . . H164 H 0.2379 1.1520 0.7858 0.042 Uiso 1 1 calc R . . C165 C 0.1454(3) 1.0915(2) 0.80078(13) 0.0329(9) Uani 1 1 d . . . C166 C 0.0929(2) 1.0331(2) 0.78812(12) 0.0263(9) Uani 1 1 d . . . H166 H 0.0515 1.0216 0.8039 0.032 Uiso 1 1 calc R . . C167 C 0.2685(3) 1.0949(3) 0.71461(15) 0.0367(11) Uani 1 1 d . . . C168 C 0.1337(4) 1.1324(3) 0.83893(15) 0.0480(13) Uani 1 1 d . . . C169 C -0.0618(2) 0.9553(2) 0.72488(12) 0.0257(9) Uani 1 1 d . . . C170 C -0.0805(3) 1.0096(2) 0.69420(14) 0.0310(9) Uani 1 1 d . . . H170 H -0.0354 1.0290 0.6834 0.037 Uiso 1 1 calc R . . C171 C -0.1627(3) 1.0360(3) 0.67905(15) 0.0428(11) Uani 1 1 d . . . C172 C -0.2293(3) 1.0095(3) 0.69507(18) 0.0491(13) Uani 1 1 d . . . H172 H -0.2857 1.0270 0.6850 0.059 Uiso 1 1 calc R . . C173 C -0.2125(3) 0.9579(3) 0.72557(17) 0.0432(12) Uani 1 1 d . . . C174 C -0.1296(2) 0.9303(2) 0.74110(15) 0.0328(10) Uani 1 1 d . . . H174 H -0.1199 0.8947 0.7626 0.039 Uiso 1 1 calc R . . Cl1A Cl 0.7280(9) 0.9100(8) 0.1109(4) 0.0800(19) Uani 0.125 1 d PD C 1 C1A C 0.6395(13) 0.942(2) 0.1212(17) 0.0800(19) Uani 0.125 1 d PD C 1 H1A H 0.6549 0.9607 0.1512 0.096 Uiso 0.125 1 calc PR C 1 H1B H 0.6231 0.9833 0.1019 0.096 Uiso 0.125 1 calc PR C 1 Cl2A Cl 0.5525(10) 0.8942(8) 0.1169(4) 0.0800(19) Uani 0.125 1 d PD C 1 Cl1B Cl 0.6627(10) 0.9625(8) 0.1150(4) 0.0800(19) Uani 0.125 1 d PD D 2 C1B C 0.582(3) 0.9061(14) 0.1077(17) 0.0800(19) Uani 0.125 1 d PD D 2 H1C H 0.5683 0.8983 0.1361 0.096 Uiso 0.125 1 calc PR D 2 H1D H 0.5321 0.9279 0.0883 0.096 Uiso 0.125 1 calc PR D 2 Cl2B Cl 0.5983(10) 0.8288(8) 0.0873(4) 0.0800(19) Uani 0.125 1 d PD D 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 0.03868(19) 0.0396(2) 0.0491(2) 0.00510(19) 0.00248(17) -0.00396(17) Rh2 0.02742(15) 0.0350(2) 0.0440(2) 0.00411(17) 0.01219(14) 0.00078(15) O1 0.099(4) 0.126(5) 0.076(3) -0.028(3) 0.024(3) 0.003(3) O2 0.041(2) 0.114(4) 0.122(4) -0.001(3) 0.012(2) 0.006(2) O3 0.089(3) 0.068(3) 0.116(4) 0.018(3) 0.058(3) -0.012(2) O4 0.065(2) 0.059(3) 0.073(3) -0.015(2) 0.035(2) 0.004(2) N1 0.041(2) 0.029(2) 0.042(2) 0.0043(17) -0.0041(18) 0.0007(16) N2 0.0372(19) 0.023(2) 0.047(2) 0.0064(17) -0.0040(18) 0.0040(16) N3 0.0329(19) 0.045(2) 0.045(2) 0.012(2) -0.0012(17) -0.0105(18) N4 0.042(2) 0.026(2) 0.045(2) 0.0000(18) -0.0035(18) -0.0069(17) N5 0.0262(17) 0.028(2) 0.050(2) 0.0031(18) 0.0130(16) 0.0029(15) N6 0.0243(16) 0.034(2) 0.0316(19) 0.0010(16) 0.0052(15) 0.0020(14) N7 0.0263(17) 0.033(2) 0.050(2) 0.0062(18) 0.0041(17) 0.0014(16) N8 0.0313(18) 0.030(2) 0.036(2) -0.0006(17) 0.0027(16) 0.0029(15) C1 0.059(3) 0.068(4) 0.078(5) -0.002(4) 0.025(3) 0.001(3) C2 0.051(3) 0.055(4) 0.074(4) 0.000(3) 0.016(3) -0.007(3) C3 0.059(3) 0.036(3) 0.049(3) 0.002(2) -0.015(3) 0.009(2) C4 0.048(3) 0.038(3) 0.065(4) -0.004(3) -0.016(3) 0.016(2) C5 0.041(2) 0.024(3) 0.068(4) 0.004(2) 0.001(2) 0.009(2) C6 0.048(3) 0.059(4) 0.053(3) 0.011(3) -0.007(3) -0.024(3) C7 0.069(4) 0.054(4) 0.056(4) -0.007(3) -0.004(3) -0.028(3) C8 0.067(3) 0.033(3) 0.052(3) -0.004(3) 0.000(3) -0.014(3) C9 0.033(2) 0.031(3) 0.037(2) -0.003(2) -0.0029(19) 0.0008(18) C10 0.0234(19) 0.028(2) 0.037(2) 0.0006(19) 0.0102(18) -0.0004(17) C11 0.0254(19) 0.029(2) 0.030(2) -0.0041(19) 0.0019(17) -0.0025(17) C12 0.0288(19) 0.028(2) 0.040(2) -0.005(2) 0.0069(19) -0.0057(18) C13 0.0284(18) 0.025(2) 0.032(2) 0.0014(18) 0.0092(17) 0.0024(17) C14 0.0181(17) 0.030(2) 0.032(2) -0.0023(19) 0.0099(16) 0.0004(16) C15 0.0187(17) 0.025(2) 0.032(2) -0.0043(18) 0.0041(16) -0.0015(16) C16 0.064(3) 0.046(3) 0.063(3) 0.010(3) 0.034(3) -0.001(3) C17 0.033(2) 0.053(4) 0.054(3) 0.007(3) 0.016(2) 0.000(2) C18 0.034(2) 0.030(3) 0.057(3) 0.003(2) 0.008(2) 0.005(2) C19 0.038(2) 0.031(3) 0.047(3) 0.009(2) 0.005(2) -0.005(2) C20 0.026(2) 0.041(3) 0.041(3) 0.006(2) 0.0042(19) -0.0035(19) C21 0.033(2) 0.036(3) 0.063(3) 0.002(3) -0.002(2) -0.012(2) C22 0.048(3) 0.030(3) 0.076(4) -0.008(3) -0.015(3) -0.009(2) C23 0.045(3) 0.032(3) 0.045(3) -0.008(2) -0.004(2) 0.000(2) C24 0.0202(17) 0.031(2) 0.028(2) -0.0032(18) 0.0020(16) 0.0044(16) B1 0.0204(19) 0.023(2) 0.021(2) -0.0002(19) 0.0042(17) -0.0005(18) F1 0.130(3) 0.0266(17) 0.063(2) -0.0079(15) -0.009(2) -0.0075(18) F2 0.132(3) 0.0305(19) 0.101(3) 0.0009(19) -0.019(3) 0.018(2) F3 0.234(6) 0.073(3) 0.216(6) -0.054(3) 0.171(5) -0.102(4) F4 0.127(3) 0.059(2) 0.0443(19) -0.0015(17) -0.017(2) -0.007(2) F5 0.0344(15) 0.170(4) 0.0448(18) -0.015(2) -0.0127(14) 0.009(2) F6 0.0654(19) 0.094(3) 0.0308(15) 0.0035(16) 0.0040(14) 0.0000(19) F7 0.116(3) 0.143(4) 0.153(4) -0.090(4) 0.108(3) -0.060(3) F8 0.172(4) 0.113(3) 0.050(2) 0.036(2) 0.057(3) 0.069(3) F9 0.154(4) 0.041(2) 0.071(2) -0.0060(17) 0.062(2) 0.027(2) F10 0.074(2) 0.058(2) 0.085(2) 0.0233(19) -0.0104(19) -0.0344(18) F11 0.095(3) 0.0336(18) 0.082(2) 0.0283(17) 0.019(2) 0.0091(17) F12 0.151(4) 0.0386(19) 0.089(3) 0.0028(18) 0.075(3) -0.019(2) F13 0.070(2) 0.081(2) 0.0303(15) 0.0107(15) 0.0056(14) -0.0197(18) F14 0.126(3) 0.059(2) 0.0313(16) -0.0164(15) 0.0142(18) -0.015(2) F15 0.064(2) 0.128(3) 0.0398(17) 0.0154(19) 0.0011(15) 0.047(2) F16 0.0435(16) 0.167(4) 0.0357(17) -0.012(2) 0.0157(14) -0.028(2) F17 0.081(2) 0.107(3) 0.097(3) -0.014(2) 0.047(2) -0.055(2) F18 0.0328(15) 0.151(4) 0.068(2) -0.002(2) 0.0159(15) 0.0035(19) F19 0.081(2) 0.056(2) 0.0510(18) -0.0069(16) 0.0004(17) 0.0084(18) F20 0.0581(19) 0.104(3) 0.112(3) -0.052(2) 0.041(2) 0.0137(19) F21 0.153(4) 0.0330(19) 0.075(2) -0.0040(17) 0.054(2) 0.000(2) F22 0.0560(19) 0.066(3) 0.127(3) -0.025(2) 0.036(2) -0.0298(18) F23 0.046(2) 0.156(5) 0.151(4) 0.064(4) -0.035(2) -0.042(3) F24 0.063(2) 0.108(3) 0.141(3) -0.033(3) 0.071(2) -0.041(2) C49 0.0162(16) 0.024(2) 0.032(2) 0.0004(18) 0.0049(16) 0.0043(15) C50 0.0297(19) 0.022(2) 0.024(2) 0.0016(17) 0.0041(17) -0.0037(16) C51 0.032(2) 0.022(2) 0.036(2) 0.0000(19) 0.0075(19) -0.0002(17) C52 0.030(2) 0.031(3) 0.033(2) 0.012(2) 0.0081(19) 0.0039(18) C53 0.0251(19) 0.032(3) 0.026(2) 0.0036(18) -0.0001(17) 0.0007(17) C54 0.0242(18) 0.017(2) 0.030(2) 0.0059(17) 0.0050(17) -0.0035(16) C55 0.070(3) 0.029(3) 0.048(3) 0.008(2) 0.015(3) -0.013(3) C56 0.056(3) 0.026(3) 0.038(3) 0.009(2) -0.005(2) -0.001(2) C57 0.0157(16) 0.024(2) 0.024(2) -0.0034(17) 0.0002(15) 0.0026(15) C58 0.0201(17) 0.026(2) 0.028(2) 0.0040(18) -0.0006(16) -0.0005(16) C59 0.028(2) 0.028(2) 0.030(2) -0.0028(18) -0.0025(17) 0.0064(17) C60 0.041(2) 0.021(2) 0.033(2) -0.0059(19) 0.003(2) 0.0028(19) C61 0.034(2) 0.023(2) 0.033(2) 0.0045(19) 0.0017(19) 0.0024(17) C62 0.0243(17) 0.023(2) 0.023(2) 0.0040(18) -0.0001(16) 0.0018(17) C63 0.060(3) 0.037(3) 0.048(3) -0.007(2) 0.020(3) -0.003(2) C64 0.060(3) 0.022(3) 0.043(3) 0.002(2) 0.007(2) 0.000(2) C65 0.0226(17) 0.017(2) 0.026(2) -0.0027(16) 0.0027(16) 0.0012(15) C66 0.0257(19) 0.020(2) 0.023(2) 0.0019(17) 0.0056(16) 0.0017(16) C67 0.0263(19) 0.025(2) 0.027(2) -0.0029(18) 0.0022(17) 0.0045(17) C68 0.0229(19) 0.047(3) 0.031(2) -0.006(2) 0.0010(18) 0.0011(19) C69 0.0236(19) 0.051(3) 0.029(2) -0.012(2) 0.0049(18) -0.0069(19) C70 0.0253(19) 0.028(2) 0.023(2) -0.0044(17) 0.0010(16) -0.0059(17) C71 0.035(2) 0.043(3) 0.032(2) -0.006(2) 0.005(2) 0.002(2) C72 0.029(2) 0.095(5) 0.034(3) -0.009(3) 0.004(2) -0.016(3) C73 0.0216(17) 0.023(2) 0.022(2) 0.0071(17) 0.0036(16) 0.0033(16) C74 0.0282(19) 0.024(2) 0.026(2) 0.0059(18) 0.0058(17) 0.0049(17) C75 0.040(2) 0.031(3) 0.023(2) 0.0080(18) 0.0089(18) 0.0110(19) C76 0.032(2) 0.038(3) 0.042(3) 0.016(2) 0.021(2) 0.011(2) C77 0.028(2) 0.039(3) 0.039(3) 0.015(2) 0.0089(19) 0.0005(19) C78 0.0249(19) 0.027(2) 0.033(2) 0.0112(19) 0.0050(17) 0.0009(17) C79 0.044(2) 0.044(3) 0.043(3) 0.004(2) 0.019(2) 0.012(2) C80 0.030(2) 0.059(4) 0.081(4) 0.012(3) 0.020(3) -0.008(2) B2 0.022(2) 0.018(2) 0.030(2) -0.003(2) 0.0058(19) -0.0018(17) F25 0.288(13) 0.033(3) 0.069(4) 0.008(3) 0.083(6) 0.017(5) F26 0.100(4) 0.097(4) 0.078(4) 0.045(3) 0.009(3) -0.019(3) F27 0.088(4) 0.161(7) 0.088(4) 0.057(5) 0.064(4) 0.013(4) F25A 0.288(13) 0.033(3) 0.069(4) 0.008(3) 0.083(6) 0.017(5) F26A 0.100(4) 0.097(4) 0.078(4) 0.045(3) 0.009(3) -0.019(3) F27A 0.088(4) 0.161(7) 0.088(4) 0.057(5) 0.064(4) 0.013(4) F28 0.0424(18) 0.168(5) 0.103(3) 0.026(3) 0.012(2) 0.041(2) F29 0.068(2) 0.057(3) 0.275(7) 0.009(3) 0.060(3) 0.033(2) F30 0.0495(19) 0.132(4) 0.113(3) 0.003(3) 0.044(2) 0.030(2) F31 0.0439(15) 0.071(2) 0.0271(13) 0.0012(13) -0.0040(12) 0.0132(14) F32 0.0459(15) 0.088(2) 0.0304(14) 0.0106(15) 0.0105(12) -0.0114(15) F33 0.0652(18) 0.058(2) 0.0314(14) -0.0151(14) 0.0036(13) 0.0132(15) F34 0.0324(15) 0.263(6) 0.0356(18) -0.001(3) 0.0142(14) 0.005(2) F35 0.091(3) 0.101(4) 0.280(7) -0.067(4) 0.106(4) 0.017(3) F36 0.0233(13) 0.135(3) 0.0480(17) -0.0009(19) 0.0053(13) -0.0074(16) F37 0.109(3) 0.0341(19) 0.094(3) -0.0266(19) -0.025(2) 0.0214(19) F38 0.0490(16) 0.0361(17) 0.105(3) 0.0080(17) 0.0287(17) 0.0137(13) F39 0.135(3) 0.0326(18) 0.094(3) 0.0282(18) 0.072(2) 0.0281(19) F40 0.0517(17) 0.134(3) 0.0353(16) 0.0273(19) 0.0046(14) -0.012(2) F41 0.0349(14) 0.085(2) 0.0450(16) 0.0028(16) -0.0115(13) -0.0148(15) F42 0.131(3) 0.065(2) 0.048(2) -0.0104(18) -0.035(2) 0.043(2) F43 0.121(3) 0.087(3) 0.125(3) 0.053(3) 0.096(3) 0.040(3) F44 0.085(2) 0.135(4) 0.0384(18) 0.001(2) 0.0148(18) -0.004(2) F45 0.167(4) 0.072(3) 0.079(3) -0.009(2) 0.061(3) -0.069(3) F46 0.202(6) 0.071(3) 0.105(3) -0.025(3) 0.000(4) 0.073(3) F47 0.157(4) 0.075(3) 0.141(4) -0.075(3) 0.068(3) -0.057(3) F48 0.175(4) 0.039(2) 0.116(3) -0.019(2) 0.093(3) 0.007(2) C81 0.0256(18) 0.020(2) 0.026(2) -0.0074(17) 0.0026(17) -0.0031(16) C82 0.0267(19) 0.026(2) 0.026(2) -0.0085(18) 0.0038(17) 0.0002(17) C83 0.042(2) 0.037(3) 0.024(2) -0.008(2) 0.0101(19) -0.011(2) C84 0.029(2) 0.048(3) 0.045(3) -0.015(2) 0.015(2) -0.006(2) C85 0.027(2) 0.042(3) 0.053(3) -0.019(2) 0.008(2) 0.001(2) C86 0.028(2) 0.029(2) 0.035(2) -0.006(2) 0.0046(18) 0.0023(18) C87 0.061(3) 0.052(4) 0.061(4) -0.004(3) 0.032(3) -0.011(3) C88 0.033(3) 0.070(5) 0.104(5) -0.019(4) 0.024(3) 0.007(3) C89 0.0202(17) 0.0127(19) 0.026(2) -0.0021(16) 0.0018(16) -0.0030(14) C90 0.0205(17) 0.020(2) 0.028(2) -0.0015(17) 0.0063(16) -0.0016(15) C91 0.029(2) 0.022(2) 0.028(2) 0.0030(18) 0.0066(17) -0.0013(17) C92 0.0227(18) 0.028(2) 0.028(2) -0.0017(18) 0.0011(17) 0.0028(17) C93 0.0222(18) 0.038(3) 0.030(2) -0.0024(19) 0.0047(17) 0.0039(18) C94 0.0279(19) 0.030(2) 0.021(2) 0.0024(18) 0.0043(16) 0.0016(17) C95 0.035(2) 0.044(3) 0.030(2) -0.002(2) 0.0012(19) 0.002(2) C96 0.032(2) 0.091(5) 0.037(3) -0.007(3) 0.006(2) 0.012(3) C97 0.0157(16) 0.022(2) 0.026(2) 0.0001(17) 0.0040(15) 0.0013(15) C98 0.0240(17) 0.023(2) 0.0227(19) 0.0013(17) 0.0039(15) -0.0007(16) C99 0.0263(19) 0.025(2) 0.037(2) -0.001(2) 0.0107(18) 0.0031(18) C100 0.034(2) 0.032(3) 0.025(2) -0.0117(18) 0.0097(18) -0.0065(18) C101 0.0250(19) 0.029(2) 0.026(2) -0.0039(18) 0.0009(17) -0.0032(17) C102 0.0244(18) 0.022(2) 0.033(2) -0.0015(18) 0.0083(17) 0.0014(16) C103 0.043(2) 0.026(2) 0.041(3) -0.006(2) 0.013(2) 0.005(2) C104 0.040(2) 0.037(3) 0.029(2) -0.008(2) 0.000(2) -0.003(2) C105 0.0205(17) 0.019(2) 0.023(2) 0.0001(17) -0.0066(15) -0.0005(15) C106 0.0218(18) 0.024(2) 0.032(2) -0.0008(18) -0.0034(17) 0.0013(16) C107 0.030(2) 0.028(3) 0.032(2) 0.0038(19) -0.0040(18) -0.0064(18) C108 0.052(3) 0.022(2) 0.032(3) 0.011(2) -0.005(2) -0.004(2) C109 0.049(3) 0.024(2) 0.033(2) -0.006(2) -0.003(2) -0.004(2) C110 0.032(2) 0.029(2) 0.025(2) -0.0010(18) -0.0044(17) -0.0031(18) C111 0.050(3) 0.040(3) 0.047(3) 0.010(2) 0.015(3) 0.003(2) C112 0.116(5) 0.025(3) 0.054(4) -0.008(3) 0.016(4) -0.002(3) Rh3 0.03690(19) 0.0585(3) 0.0629(3) -0.0243(2) 0.02496(18) -0.01236(19) Rh4 0.0386(2) 0.0523(3) 0.0891(3) 0.0071(3) 0.0185(2) -0.00865(19) O5 0.045(3) 0.111(4) 0.215(7) 0.000(5) 0.017(3) -0.014(3) O6 0.142(6) 0.190(8) 0.194(8) -0.095(7) 0.111(6) -0.050(5) O7 0.135(5) 0.139(5) 0.176(6) -0.114(5) 0.121(5) -0.092(4) O8 0.147(5) 0.107(4) 0.142(5) -0.024(4) 0.108(5) -0.039(4) N9 0.0274(18) 0.039(2) 0.042(2) -0.0135(18) 0.0016(16) 0.0088(16) N10 0.0295(17) 0.032(2) 0.034(2) -0.0039(17) 0.0031(16) 0.0031(15) N11 0.0276(18) 0.037(2) 0.054(2) -0.0129(19) 0.0051(18) 0.0000(17) N12 0.0271(17) 0.033(2) 0.036(2) -0.0043(17) 0.0000(16) 0.0019(15) N13 0.050(2) 0.037(3) 0.062(3) 0.008(2) -0.007(2) -0.013(2) N14 0.046(2) 0.026(2) 0.044(2) -0.0020(19) -0.0048(18) -0.0024(18) N15 0.042(2) 0.041(2) 0.049(3) 0.009(2) 0.0052(19) -0.0010(19) N16 0.0353(18) 0.030(2) 0.038(2) 0.0046(17) 0.0008(16) 0.0020(16) C25 0.074(4) 0.107(6) 0.095(5) -0.060(5) 0.066(4) -0.046(4) C26 0.068(4) 0.085(5) 0.108(5) -0.037(4) 0.054(4) -0.029(4) C27 0.033(2) 0.052(3) 0.071(4) -0.012(3) 0.005(2) -0.009(2) C28 0.044(3) 0.049(3) 0.068(4) -0.020(3) 0.000(3) -0.010(2) C29 0.034(2) 0.045(3) 0.043(3) -0.016(2) -0.004(2) 0.005(2) C30 0.036(2) 0.036(3) 0.065(4) -0.018(3) -0.011(2) 0.014(2) C31 0.047(3) 0.038(3) 0.053(3) 0.004(3) -0.007(3) 0.006(2) C32 0.036(2) 0.039(3) 0.042(3) -0.001(2) -0.010(2) 0.004(2) C33 0.0267(19) 0.029(2) 0.032(2) -0.0107(19) 0.0026(17) 0.0034(17) C34 0.0182(16) 0.026(2) 0.025(2) -0.0028(18) 0.0053(15) 0.0004(16) C35 0.0269(19) 0.026(2) 0.035(2) -0.0011(19) 0.0094(18) 0.0010(17) C36 0.0263(19) 0.030(2) 0.034(2) -0.008(2) 0.0044(18) -0.0093(18) C37 0.029(2) 0.034(3) 0.027(2) -0.0015(19) 0.0027(18) -0.0004(18) C38 0.0245(19) 0.026(2) 0.035(2) -0.0017(19) 0.0069(18) -0.0034(17) C39 0.0262(19) 0.020(2) 0.033(2) -0.0074(18) 0.0055(17) -0.0054(16) C40 0.032(3) 0.076(5) 0.155(7) 0.011(5) 0.020(4) -0.004(3) C41 0.076(5) 0.086(6) 0.146(8) 0.008(6) 0.009(5) -0.036(4) C42 0.071(4) 0.050(4) 0.087(5) 0.000(4) -0.012(4) -0.026(3) C43 0.110(6) 0.053(4) 0.061(4) -0.010(3) -0.018(4) -0.002(4) C44 0.079(4) 0.042(3) 0.057(4) -0.006(3) -0.004(3) 0.010(3) C45 0.078(4) 0.051(3) 0.045(3) 0.006(3) 0.018(3) 0.004(3) C46 0.065(3) 0.041(3) 0.049(3) 0.006(3) -0.011(3) 0.010(3) C47 0.039(2) 0.023(2) 0.060(3) 0.001(2) -0.006(2) 0.003(2) C48 0.037(2) 0.022(2) 0.037(2) 0.0026(19) 0.0033(19) 0.0022(18) B3 0.0163(18) 0.026(3) 0.023(2) -0.0014(19) 0.0043(17) -0.0012(17) F49 0.060(2) 0.073(3) 0.154(4) 0.033(3) -0.023(2) 0.0242(19) F50 0.194(5) 0.085(3) 0.054(2) 0.006(2) -0.019(3) 0.042(3) F51 0.082(2) 0.077(3) 0.108(3) 0.047(2) -0.042(2) -0.019(2) F52 0.0234(14) 0.083(3) 0.170(4) 0.014(3) 0.0107(19) -0.0113(16) F53 0.140(4) 0.212(6) 0.193(5) -0.160(5) 0.139(4) -0.129(4) F54 0.0420(17) 0.126(4) 0.119(3) 0.049(3) 0.0403(19) 0.010(2) F55 0.0532(18) 0.126(3) 0.087(2) 0.066(2) 0.0370(18) 0.020(2) F56 0.105(3) 0.055(2) 0.197(5) 0.038(3) 0.125(3) 0.026(2) F57 0.068(2) 0.129(4) 0.096(3) -0.004(2) 0.039(2) -0.061(2) F58 0.081(2) 0.0449(17) 0.0375(14) -0.0095(14) 0.0221(14) -0.0221(16) F59 0.0557(17) 0.066(2) 0.0519(18) -0.0221(16) 0.0046(14) 0.0226(16) F60 0.0623(17) 0.0444(17) 0.0468(16) -0.0143(14) 0.0103(14) -0.0260(14) F61 0.074(2) 0.0356(17) 0.068(2) 0.0211(15) -0.0026(17) -0.0152(15) F62 0.069(2) 0.0367(17) 0.084(2) -0.0245(16) 0.0299(18) -0.0100(15) F63 0.0359(13) 0.0451(17) 0.0567(17) 0.0014(14) 0.0028(13) -0.0143(12) F64 0.110(3) 0.053(2) 0.0428(18) -0.0062(16) -0.0175(18) -0.018(2) F65 0.156(4) 0.100(3) 0.0346(18) 0.0113(19) 0.004(2) -0.043(3) F66 0.063(2) 0.286(8) 0.114(4) -0.126(5) -0.061(2) 0.081(4) F67 0.067(3) 0.272(8) 0.074(3) -0.055(4) -0.017(2) -0.021(4) F68 0.334(10) 0.176(6) 0.067(3) 0.060(4) -0.110(5) -0.120(7) F69 0.121(4) 0.171(5) 0.072(3) -0.080(3) -0.022(3) 0.029(3) F70 0.0411(15) 0.063(2) 0.079(2) -0.0107(18) 0.0113(16) 0.0176(14) F71 0.071(2) 0.115(3) 0.131(3) 0.047(3) 0.071(2) 0.043(2) F72 0.083(2) 0.055(2) 0.095(3) -0.027(2) 0.011(2) 0.0202(18) C113 0.0226(18) 0.026(2) 0.028(2) -0.0087(18) -0.0002(17) 0.0009(17) C114 0.027(2) 0.028(2) 0.037(2) -0.002(2) -0.0024(18) 0.0015(18) C115 0.035(2) 0.032(3) 0.054(3) -0.007(2) -0.009(2) 0.007(2) C116 0.020(2) 0.034(3) 0.071(4) -0.017(3) -0.009(2) 0.0029(19) C117 0.026(2) 0.031(3) 0.063(3) -0.025(2) 0.009(2) -0.0058(19) C118 0.0201(18) 0.030(2) 0.038(2) -0.0111(19) 0.0074(17) -0.0043(16) C119 0.051(3) 0.043(3) 0.055(4) -0.001(3) -0.025(3) 0.008(3) C120 0.031(2) 0.062(4) 0.092(4) -0.028(4) 0.030(3) -0.012(2) C121 0.0152(16) 0.027(2) 0.028(2) 0.0068(17) 0.0034(15) 0.0054(15) C122 0.0224(18) 0.030(2) 0.034(2) 0.0049(19) 0.0078(17) 0.0007(17) C123 0.0211(17) 0.028(2) 0.035(2) 0.0094(19) 0.0073(17) 0.0051(17) C124 0.0237(18) 0.021(2) 0.042(2) 0.0068(19) -0.0026(18) 0.0007(16) C125 0.0220(17) 0.029(2) 0.027(2) 0.0001(18) 0.0009(16) 0.0003(17) C126 0.0222(18) 0.031(2) 0.022(2) 0.0041(17) 0.0033(16) -0.0009(16) C127 0.031(2) 0.041(3) 0.062(3) 0.010(3) 0.019(2) 0.000(2) C128 0.041(2) 0.026(2) 0.035(2) -0.003(2) 0.001(2) -0.006(2) C129 0.0194(16) 0.023(2) 0.024(2) -0.0012(17) 0.0069(15) 0.0024(15) C130 0.0240(18) 0.034(2) 0.025(2) -0.0007(19) 0.0027(17) 0.0025(17) C131 0.0255(19) 0.025(2) 0.038(2) -0.0023(19) 0.0117(18) -0.0033(17) C132 0.0262(19) 0.026(2) 0.032(2) 0.0072(18) 0.0062(18) 0.0008(17) C133 0.0284(19) 0.025(2) 0.029(2) -0.0001(18) 0.0067(17) 0.0035(17) C134 0.0196(17) 0.019(2) 0.027(2) -0.0047(16) 0.0022(16) 0.0002(14) C135 0.041(2) 0.030(3) 0.051(3) 0.000(2) 0.017(2) -0.002(2) C136 0.049(3) 0.040(3) 0.044(3) 0.005(2) -0.002(2) -0.006(2) C137 0.0253(18) 0.027(2) 0.023(2) 0.0000(17) 0.0063(16) -0.0033(16) C138 0.031(2) 0.036(3) 0.031(2) -0.0018(19) 0.0026(18) -0.0072(18) C139 0.045(3) 0.044(3) 0.026(2) -0.011(2) 0.004(2) -0.013(2) C140 0.049(3) 0.036(3) 0.040(3) -0.013(2) 0.025(2) -0.012(2) C141 0.036(2) 0.032(3) 0.040(3) -0.009(2) 0.019(2) -0.0093(19) C142 0.030(2) 0.034(3) 0.033(2) -0.0019(19) 0.0132(18) 0.0005(18) C143 0.077(4) 0.086(5) 0.025(3) -0.023(3) 0.002(3) -0.027(4) C144 0.053(3) 0.047(3) 0.058(3) -0.006(3) 0.029(3) 0.008(3) B4 0.021(2) 0.028(3) 0.021(2) -0.005(2) 0.0063(18) -0.0046(18) F73 0.0398(17) 0.083(3) 0.130(3) -0.038(3) 0.001(2) 0.0189(17) F74 0.080(2) 0.053(2) 0.093(3) -0.0098(19) 0.020(2) 0.0137(18) F75 0.140(4) 0.168(5) 0.238(6) 0.142(5) 0.159(4) 0.115(4) F76 0.109(3) 0.219(6) 0.0355(18) -0.041(3) 0.017(2) -0.012(4) F77 0.112(3) 0.163(5) 0.038(2) -0.019(3) -0.031(2) 0.035(3) F78 0.128(4) 0.189(6) 0.084(3) 0.015(3) -0.042(3) -0.109(4) F79 0.0528(16) 0.0463(18) 0.0339(14) 0.0056(13) -0.0116(12) -0.0104(14) F80 0.0678(19) 0.0485(19) 0.0484(17) 0.0083(15) -0.0141(15) 0.0257(16) F81 0.0634(17) 0.082(2) 0.0315(14) -0.0088(15) 0.0211(13) -0.0142(17) F82 0.079(2) 0.0268(16) 0.075(2) 0.0018(15) 0.0132(17) -0.0130(15) F83 0.0529(17) 0.052(2) 0.082(2) -0.0124(17) 0.0090(16) -0.0260(15) F84 0.151(4) 0.052(2) 0.0440(18) -0.0236(15) 0.039(2) -0.050(2) F85 0.129(3) 0.047(2) 0.187(4) 0.002(2) 0.136(3) -0.004(2) F86 0.0547(19) 0.166(4) 0.061(2) 0.003(2) 0.0140(17) -0.068(2) F87 0.0462(17) 0.124(3) 0.069(2) 0.057(2) 0.0194(16) 0.0021(19) F88 0.208(5) 0.048(2) 0.0342(17) -0.0102(16) 0.039(2) -0.041(3) F89 0.103(3) 0.0413(18) 0.0531(18) -0.0169(15) 0.0228(18) -0.0374(18) F90 0.093(3) 0.094(3) 0.092(3) -0.056(2) 0.045(2) -0.007(2) C175 0.039(4) 0.076(5) 0.065(4) 0.017(4) -0.014(3) 0.020(4) F91 0.101(4) 0.067(7) 0.084(9) 0.034(5) 0.006(4) 0.019(5) F92 0.099(6) 0.100(7) 0.090(5) 0.044(5) -0.057(5) -0.012(5) F93 0.114(5) 0.053(4) 0.095(4) 0.022(3) 0.002(4) 0.027(3) C178 0.039(4) 0.076(5) 0.065(4) 0.017(4) -0.014(3) 0.020(4) F91A 0.101(4) 0.067(7) 0.084(9) 0.034(5) 0.006(4) 0.019(5) F92A 0.099(6) 0.100(7) 0.090(5) 0.044(5) -0.057(5) -0.012(5) F93A 0.114(5) 0.053(4) 0.095(4) 0.022(3) 0.002(4) 0.027(3) C176 0.027(3) 0.053(5) 0.111(6) -0.047(5) 0.027(3) -0.016(3) F94 0.058(5) 0.097(6) 0.104(6) -0.032(5) 0.051(4) -0.023(4) F95 0.093(9) 0.087(4) 0.186(15) -0.055(5) 0.093(10) -0.051(4) F96 0.029(2) 0.132(7) 0.150(7) 0.000(4) 0.038(4) 0.009(3) C177 0.027(3) 0.053(5) 0.111(6) -0.047(5) 0.027(3) -0.016(3) F94A 0.058(5) 0.097(6) 0.104(6) -0.032(5) 0.051(4) -0.023(4) F95A 0.093(9) 0.087(4) 0.186(15) -0.055(5) 0.093(10) -0.051(4) F96A 0.029(2) 0.132(7) 0.150(7) 0.000(4) 0.038(4) 0.009(3) C145 0.0243(18) 0.019(2) 0.026(2) -0.0021(17) 0.0066(17) -0.0048(15) C146 0.0260(19) 0.036(3) 0.033(2) -0.0036(19) 0.0081(17) -0.0017(18) C147 0.036(2) 0.030(3) 0.050(3) -0.009(2) 0.022(2) -0.0071(19) C148 0.044(3) 0.050(3) 0.047(3) -0.028(2) 0.030(2) -0.024(2) C149 0.044(2) 0.051(3) 0.028(2) -0.013(2) 0.009(2) -0.018(2) C150 0.0256(19) 0.037(3) 0.034(2) -0.007(2) 0.0080(18) -0.0026(18) C151 0.043(3) 0.055(4) 0.070(4) -0.020(3) 0.030(3) 0.000(3) C152 0.049(3) 0.120(6) 0.037(3) -0.010(4) 0.004(3) -0.018(4) C153 0.0228(17) 0.022(2) 0.026(2) -0.0023(17) 0.0068(16) 0.0026(16) C154 0.0178(16) 0.023(2) 0.030(2) -0.0031(18) 0.0049(16) 0.0001(16) C155 0.0245(18) 0.027(2) 0.028(2) -0.0012(17) 0.0113(17) 0.0061(16) C156 0.032(2) 0.023(2) 0.031(2) 0.0031(18) 0.0169(18) 0.0000(17) C157 0.036(2) 0.023(2) 0.032(2) -0.0047(18) 0.0160(19) -0.0060(18) C158 0.031(2) 0.025(2) 0.028(2) -0.0036(18) 0.0119(18) 0.0010(17) C159 0.036(2) 0.026(2) 0.032(2) 0.000(2) 0.0042(18) 0.0022(19) C160 0.068(3) 0.030(3) 0.040(3) -0.007(2) 0.019(2) -0.016(2) C161 0.0209(17) 0.023(2) 0.023(2) 0.0075(17) 0.0013(15) 0.0043(16) C162 0.0220(18) 0.026(2) 0.025(2) 0.0006(17) 0.0034(16) 0.0051(16) C163 0.0219(18) 0.030(2) 0.036(2) 0.0090(19) 0.0059(17) -0.0021(17) C164 0.035(2) 0.030(3) 0.036(2) 0.005(2) 0.0022(19) -0.0111(19) C165 0.040(2) 0.024(2) 0.033(2) 0.001(2) 0.0046(19) -0.0025(19) C166 0.032(2) 0.021(2) 0.027(2) 0.0060(18) 0.0100(17) 0.0023(17) C167 0.031(2) 0.036(3) 0.043(3) 0.009(2) 0.009(2) -0.009(2) C168 0.073(4) 0.039(3) 0.036(3) -0.007(2) 0.020(3) -0.019(3) C169 0.0255(19) 0.027(2) 0.023(2) -0.0058(18) 0.0016(16) 0.0006(17) C170 0.0258(19) 0.030(2) 0.035(2) 0.001(2) 0.0035(18) 0.0022(18) C171 0.039(2) 0.039(3) 0.044(3) -0.005(2) -0.004(2) 0.009(2) C172 0.025(2) 0.052(3) 0.065(3) -0.013(3) 0.000(2) 0.011(2) C173 0.027(2) 0.048(3) 0.056(3) -0.020(3) 0.014(2) -0.001(2) C174 0.0219(19) 0.033(3) 0.044(3) -0.012(2) 0.0103(18) -0.0027(18) Cl1A 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) C1A 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) Cl2A 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) Cl1B 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) C1B 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) Cl2B 0.109(5) 0.076(5) 0.062(4) 0.019(3) 0.033(4) 0.002(4) _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 C1 1.852(7) . ? Rh1 C2 1.884(6) . ? Rh1 N1 2.068(4) . ? Rh1 N3 2.084(4) . ? Rh2 C16 1.860(5) . ? Rh2 C17 1.878(6) . ? Rh2 N5 2.071(3) . ? Rh2 N7 2.081(4) . ? O1 C1 1.134(7) . ? O2 C2 1.117(7) . ? O3 C16 1.114(6) . ? O4 C17 1.125(6) . ? N1 C3 1.347(6) . ? N1 N2 1.355(5) . ? N2 C5 1.355(6) . ? N2 C9 1.450(6) . ? N3 C6 1.345(6) . ? N3 N4 1.359(5) . ? N4 C8 1.351(6) . ? N4 C9 1.459(6) . ? N5 C18 1.323(6) . ? N5 N6 1.358(5) . ? N6 C20 1.327(6) . ? N6 C24 1.465(5) . ? N7 C21 1.344(6) . ? N7 N8 1.362(5) . ? N8 C23 1.343(6) . ? N8 C24 1.452(5) . ? C3 C4 1.383(8) . ? C3 H3 0.9500 . ? C4 C5 1.352(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.352(8) . ? C6 H6 0.9500 . ? C7 C8 1.379(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.522(6) . ? C9 H9 1.0000 . ? C10 C15 1.381(6) . ? C10 C11 1.390(6) . ? C11 C12 1.372(6) . ? C11 H11 0.9500 . ? C12 C13 1.400(6) . ? C12 H12 0.9500 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 C24 1.524(6) . ? C15 H15 0.9500 . ? C18 C19 1.381(6) . ? C18 H18 0.9500 . ? C19 C20 1.372(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.370(8) . ? C21 H21 0.9500 . ? C22 C23 1.363(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24 1.0000 . ? B1 C73 1.645(5) . ? B1 C49 1.646(6) . ? B1 C57 1.648(6) . ? B1 C65 1.661(5) . ? F1 C55 1.315(6) . ? F2 C55 1.367(7) . ? F3 C55 1.276(6) . ? F4 C56 1.346(6) . ? F5 C56 1.323(6) . ? F6 C56 1.320(6) . ? F7 C63 1.298(6) . ? F8 C63 1.308(6) . ? F9 C63 1.314(6) . ? F10 C64 1.338(6) . ? F11 C64 1.335(6) . ? F12 C64 1.325(6) . ? F13 C71 1.324(5) . ? F14 C71 1.311(6) . ? F15 C71 1.366(5) . ? F16 C72 1.320(5) . ? F17 C72 1.290(7) . ? F18 C72 1.376(7) . ? F19 C79 1.334(6) . ? F20 C79 1.321(5) . ? F21 C79 1.334(6) . ? F22 C80 1.337(7) . ? F23 C80 1.301(7) . ? F24 C80 1.337(6) . ? C49 C50 1.395(6) . ? C49 C54 1.396(6) . ? C50 C51 1.396(6) . ? C50 H50 0.9500 . ? C51 C52 1.384(6) . ? C51 C55 1.484(7) . ? C52 C53 1.372(6) . ? C52 H52 0.9500 . ? C53 C54 1.393(6) . ? C53 C56 1.476(6) . ? C54 H54 0.9500 . ? C57 C62 1.396(5) . ? C57 C58 1.402(5) . ? C58 C59 1.380(6) . ? C58 H58 0.9500 . ? C59 C60 1.387(6) . ? C59 C63 1.496(6) . ? C60 C61 1.394(6) . ? C60 H60 0.9500 . ? C61 C62 1.376(6) . ? C61 C64 1.490(6) . ? C62 H62 0.9500 . ? C65 C70 1.380(5) . ? C65 C66 1.391(5) . ? C66 C67 1.395(5) . ? C66 H66 0.9500 . ? C67 C68 1.399(6) . ? C67 C71 1.487(6) . ? C68 C69 1.382(6) . ? C68 H68 0.9500 . ? C69 C70 1.398(5) . ? C69 C72 1.491(6) . ? C70 H70 0.9500 . ? C73 C74 1.393(6) . ? C73 C78 1.409(5) . ? C74 C75 1.410(5) . ? C74 H74 0.9500 . ? C75 C76 1.372(6) . ? C75 C79 1.476(7) . ? C76 C77 1.375(7) . ? C76 H76 0.9500 . ? C77 C78 1.390(6) . ? C77 C80 1.505(6) . ? C78 H78 0.9500 . ? B2 C97 1.628(6) . ? B2 C89 1.640(6) . ? B2 C81 1.641(5) . ? B2 C105 1.644(6) . ? F25 C87 1.272(8) . ? F26 C87 1.421(8) . ? F27 C87 1.287(7) . ? F25A C87 1.311(10) . ? F26A C87 1.312(10) . ? F27A C87 1.312(10) . ? F28 C88 1.348(8) . ? F29 C88 1.323(8) . ? F30 C88 1.335(7) . ? F31 C95 1.348(5) . ? F32 C95 1.365(5) . ? F33 C95 1.323(6) . ? F34 C96 1.341(6) . ? F35 C96 1.275(8) . ? F36 C96 1.333(6) . ? F37 C103 1.343(6) . ? F38 C103 1.299(5) . ? F39 C103 1.331(5) . ? F40 C104 1.307(5) . ? F41 C104 1.344(5) . ? F42 C104 1.334(6) . ? F43 C111 1.333(6) . ? F44 C111 1.336(6) . ? F45 C111 1.296(6) . ? F46 C112 1.352(8) . ? F47 C112 1.265(7) . ? F48 C112 1.319(7) . ? C81 C86 1.404(6) . ? C81 C82 1.411(6) . ? C82 C83 1.387(6) . ? C82 H82 0.9500 . ? C83 C84 1.393(7) . ? C83 C87 1.475(7) . ? C84 C85 1.366(7) . ? C84 H84 0.9500 . ? C85 C86 1.388(6) . ? C85 C88 1.481(7) . ? C86 H86 0.9500 . ? C89 C90 1.399(5) . ? C89 C94 1.403(5) . ? C90 C91 1.398(5) . ? C90 H90 0.9500 . ? C91 C92 1.382(5) . ? C91 C95 1.475(6) . ? C92 C93 1.389(6) . ? C92 H92 0.9500 . ? C93 C94 1.401(6) . ? C93 C96 1.483(6) . ? C94 H94 0.9500 . ? C97 C98 1.409(5) . ? C97 C102 1.412(6) . ? C98 C99 1.387(6) . ? C98 H98 0.9500 . ? C99 C100 1.376(6) . ? C99 C103 1.492(6) . ? C100 C101 1.379(6) . ? C100 H100 0.9500 . ? C101 C102 1.399(6) . ? C101 C104 1.479(6) . ? C102 H102 0.9500 . ? C105 C106 1.393(6) . ? C105 C110 1.404(6) . ? C106 C107 1.395(6) . ? C106 H106 0.9500 . ? C107 C108 1.365(6) . ? C107 C111 1.491(6) . ? C108 C109 1.403(6) . ? C108 H108 0.9500 . ? C109 C110 1.378(6) . ? C109 C112 1.490(7) . ? C110 H110 0.9500 . ? Rh3 C25 1.848(6) . ? Rh3 C26 1.870(8) . ? Rh3 N11 2.076(4) . ? Rh3 N9 2.077(4) . ? Rh4 C41 1.780(12) . ? Rh4 C40 1.857(6) . ? Rh4 N13 2.072(5) . ? Rh4 N15 2.076(4) . ? O5 C40 1.127(7) . ? O6 C41 1.197(11) . ? O7 C25 1.139(7) . ? O8 C26 1.125(8) . ? N9 C30 1.329(6) . ? N9 N10 1.366(5) . ? N10 C32 1.339(6) . ? N10 C33 1.420(5) . ? N11 C27 1.327(6) . ? N11 N12 1.363(5) . ? N12 C29 1.329(6) . ? N12 C33 1.469(5) . ? N13 N14 1.343(6) . ? N13 C42 1.362(8) . ? N14 C44 1.355(7) . ? N14 C48 1.445(6) . ? N15 C45 1.329(7) . ? N15 N16 1.353(5) . ? N16 C47 1.351(6) . ? N16 C48 1.457(6) . ? C27 C28 1.383(8) . ? C27 H27 0.9500 . ? C28 C29 1.377(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.368(8) . ? C30 H30 0.9500 . ? C31 C32 1.379(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.533(6) . ? C33 H33 1.0000 . ? C34 C35 1.378(6) . ? C34 C39 1.401(6) . ? C35 C36 1.399(6) . ? C35 H35 0.9500 . ? C36 C37 1.375(6) . ? C36 H36 0.9500 . ? C37 C38 1.393(6) . ? C37 H37 0.9500 . ? C38 C39 1.380(6) . ? C38 C48 1.530(6) . ? C39 H39 0.9500 . ? C42 C43 1.381(10) . ? C42 H42 0.9500 . ? C43 C44 1.343(9) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.368(8) . ? C45 H45 0.9500 . ? C46 C47 1.365(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48 1.0000 . ? B3 C121 1.622(6) . ? B3 C113 1.639(5) . ? B3 C137 1.646(6) . ? B3 C129 1.652(6) . ? F49 C119 1.315(6) . ? F50 C119 1.329(7) . ? F51 C119 1.305(7) . ? F52 C120 1.332(6) . ? F53 C120 1.307(6) . ? F54 C120 1.304(7) . ? F55 C127 1.306(6) . ? F56 C127 1.308(6) . ? F57 C127 1.329(6) . ? F58 C128 1.340(5) . ? F59 C128 1.338(5) . ? F60 C128 1.324(5) . ? F61 C135 1.329(6) . ? F62 C135 1.347(5) . ? F63 C135 1.347(5) . ? F64 C136 1.299(6) . ? F65 C136 1.356(6) . ? F66 C136 1.250(6) . ? F67 C143 1.281(7) . ? F68 C143 1.215(8) . ? F69 C143 1.333(7) . ? F70 C144 1.337(6) . ? F71 C144 1.348(6) . ? F72 C144 1.327(6) . ? C113 C114 1.389(6) . ? C113 C118 1.404(6) . ? C114 C115 1.395(6) . ? C114 H114 0.9500 . ? C115 C116 1.375(7) . ? C115 C119 1.495(7) . ? C116 C117 1.388(7) . ? C116 H116 0.9500 . ? C117 C118 1.409(6) . ? C117 C120 1.482(7) . ? C118 H118 0.9500 . ? C121 C126 1.398(6) . ? C121 C122 1.412(5) . ? C122 C123 1.379(6) . ? C122 H122 0.9500 . ? C123 C124 1.384(6) . ? C123 C127 1.509(6) . ? C124 C125 1.397(6) . ? C124 H124 0.9500 . ? C125 C126 1.382(6) . ? C125 C128 1.496(6) . ? C126 H126 0.9500 . ? C129 C134 1.389(5) . ? C129 C130 1.405(6) . ? C130 C131 1.389(6) . ? C130 H130 0.9500 . ? C131 C132 1.391(6) . ? C131 C135 1.492(6) . ? C132 C133 1.382(6) . ? C132 H132 0.9500 . ? C133 C134 1.389(6) . ? C133 C136 1.496(6) . ? C134 H134 0.9500 . ? C137 C138 1.396(6) . ? C137 C142 1.409(6) . ? C138 C139 1.397(6) . ? C138 H138 0.9500 . ? C139 C140 1.367(7) . ? C139 C143 1.498(7) . ? C140 C141 1.379(6) . ? C140 H140 0.9500 . ? C141 C142 1.385(6) . ? C141 C144 1.493(7) . ? C142 H142 0.9500 . ? B4 C161 1.634(6) . ? B4 C153 1.637(6) . ? B4 C169 1.644(6) . ? B4 C145 1.653(5) . ? F73 C151 1.353(7) . ? F74 C151 1.329(7) . ? F75 C151 1.284(6) . ? F76 C152 1.309(6) . ? F77 C152 1.316(9) . ? F78 C152 1.303(8) . ? F79 C159 1.315(5) . ? F80 C159 1.342(5) . ? F81 C159 1.338(5) . ? F82 C160 1.324(6) . ? F83 C160 1.335(6) . ? F84 C160 1.334(5) . ? F85 C167 1.297(6) . ? F86 C167 1.318(5) . ? F87 C167 1.305(5) . ? F88 C168 1.329(6) . ? F89 C168 1.327(6) . ? F90 C168 1.349(7) . ? C175 F93 1.305(9) . ? C175 F91 1.348(9) . ? C175 F92 1.381(9) . ? C175 C171 1.498(9) . ? C178 F93A 1.305(9) . ? C178 F91A 1.348(8) . ? C178 F92A 1.381(9) . ? C178 C171 1.502(8) . ? C176 F96 1.316(9) . ? C176 F95 1.339(11) . ? C176 F94 1.344(9) . ? C176 C173 1.511(8) . ? C177 F96A 1.316(9) . ? C177 F95A 1.339(11) . ? C177 F94A 1.344(9) . ? C177 C173 1.511(7) . ? C145 C150 1.374(6) . ? C145 C146 1.411(5) . ? C146 C147 1.384(6) . ? C146 H146 0.9500 . ? C147 C148 1.382(7) . ? C147 C151 1.496(7) . ? C148 C149 1.372(7) . ? C148 H148 0.9500 . ? C149 C150 1.396(6) . ? C149 C152 1.490(7) . ? C150 H150 0.9500 . ? C153 C158 1.406(6) . ? C153 C154 1.410(5) . ? C154 C155 1.397(6) . ? C154 H154 0.9500 . ? C155 C156 1.366(6) . ? C155 C159 1.501(6) . ? C156 C157 1.396(6) . ? C156 H156 0.9500 . ? C157 C158 1.376(6) . ? C157 C160 1.498(6) . ? C158 H158 0.9500 . ? C161 C166 1.395(6) . ? C161 C162 1.409(5) . ? C162 C163 1.394(6) . ? C162 H162 0.9500 . ? C163 C164 1.381(6) . ? C163 C167 1.490(5) . ? C164 C165 1.374(6) . ? C164 H164 0.9500 . ? C165 C166 1.402(6) . ? C165 C168 1.491(6) . ? C166 H166 0.9500 . ? C169 C174 1.399(6) . ? C169 C170 1.407(6) . ? C170 C171 1.394(6) . ? C170 H170 0.9500 . ? C171 C172 1.389(7) . ? C172 C173 1.365(8) . ? C172 H172 0.9500 . ? C173 C174 1.414(6) . ? C174 H174 0.9500 . ? Cl1A C1A 1.66(2) . ? C1A Cl2A 1.66(2) . ? C1A H1A 0.9900 . ? C1A H1B 0.9900 . ? Cl1B C1B 1.66(2) . ? C1B Cl2B 1.66(2) . ? C1B H1C 0.9900 . ? C1B H1D 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 C1 Rh1 C2 87.7(3) . . ? C1 Rh1 N1 91.0(2) . . ? C2 Rh1 N1 177.7(2) . . ? C1 Rh1 N3 175.2(2) . . ? C2 Rh1 N3 93.5(2) . . ? N1 Rh1 N3 88.04(15) . . ? C16 Rh2 C17 90.2(2) . . ? C16 Rh2 N5 174.7(2) . . ? C17 Rh2 N5 90.67(17) . . ? C16 Rh2 N7 90.8(2) . . ? C17 Rh2 N7 178.93(19) . . ? N5 Rh2 N7 88.32(14) . . ? C3 N1 N2 105.8(4) . . ? C3 N1 Rh1 130.9(4) . . ? N2 N1 Rh1 123.2(3) . . ? C5 N2 N1 110.2(4) . . ? C5 N2 C9 127.2(4) . . ? N1 N2 C9 122.4(3) . . ? C6 N3 N4 104.3(4) . . ? C6 N3 Rh1 132.4(4) . . ? N4 N3 Rh1 121.9(3) . . ? C8 N4 N3 111.5(4) . . ? C8 N4 C9 125.7(4) . . ? N3 N4 C9 120.6(4) . . ? C18 N5 N6 104.9(3) . . ? C18 N5 Rh2 130.8(3) . . ? N6 N5 Rh2 122.8(3) . . ? C20 N6 N5 110.9(4) . . ? C20 N6 C24 128.3(3) . . ? N5 N6 C24 120.7(3) . . ? C21 N7 N8 104.7(4) . . ? C21 N7 Rh2 132.1(3) . . ? N8 N7 Rh2 122.7(3) . . ? C23 N8 N7 110.7(4) . . ? C23 N8 C24 127.8(4) . . ? N7 N8 C24 120.4(3) . . ? O1 C1 Rh1 176.7(7) . . ? O2 C2 Rh1 177.7(6) . . ? N1 C3 C4 109.8(5) . . ? N1 C3 H3 125.1 . . ? C4 C3 H3 125.1 . . ? C5 C4 C3 106.5(4) . . ? C5 C4 H4 126.8 . . ? C3 C4 H4 126.8 . . ? C4 C5 N2 107.7(5) . . ? C4 C5 H5 126.2 . . ? N2 C5 H5 126.2 . . ? N3 C6 C7 111.6(5) . . ? N3 C6 H6 124.2 . . ? C7 C6 H6 124.2 . . ? C6 C7 C8 106.4(5) . . ? C6 C7 H7 126.8 . . ? C8 C7 H7 126.8 . . ? N4 C8 C7 106.1(5) . . ? N4 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N2 C9 N4 110.1(4) . . ? N2 C9 C10 114.5(4) . . ? N4 C9 C10 111.6(3) . . ? N2 C9 H9 106.7 . . ? N4 C9 H9 106.7 . . ? C10 C9 H9 106.7 . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C9 118.8(4) . . ? C11 C10 C9 121.5(4) . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 118.9(4) . . ? C13 C14 C24 122.6(4) . . ? C15 C14 C24 118.2(4) . . ? C10 C15 C14 121.4(4) . . ? C10 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? O3 C16 Rh2 174.6(6) . . ? O4 C17 Rh2 178.1(4) . . ? N5 C18 C19 111.9(4) . . ? N5 C18 H18 124.1 . . ? C19 C18 H18 124.1 . . ? C20 C19 C18 104.2(4) . . ? C20 C19 H19 127.9 . . ? C18 C19 H19 127.9 . . ? N6 C20 C19 108.2(4) . . ? N6 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? N7 C21 C22 111.2(4) . . ? N7 C21 H21 124.4 . . ? C22 C21 H21 124.4 . . ? C23 C22 C21 105.6(4) . . ? C23 C22 H22 127.2 . . ? C21 C22 H22 127.2 . . ? N8 C23 C22 107.7(5) . . ? N8 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? N8 C24 N6 109.9(3) . . ? N8 C24 C14 111.8(3) . . ? N6 C24 C14 113.2(3) . . ? N8 C24 H24 107.2 . . ? N6 C24 H24 107.2 . . ? C14 C24 H24 107.2 . . ? C73 B1 C49 104.0(3) . . ? C73 B1 C57 114.2(3) . . ? C49 B1 C57 111.9(3) . . ? C73 B1 C65 111.6(3) . . ? C49 B1 C65 110.0(3) . . ? C57 B1 C65 105.1(3) . . ? C50 C49 C54 116.0(4) . . ? C50 C49 B1 121.4(3) . . ? C54 C49 B1 122.4(3) . . ? C49 C50 C51 121.4(4) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C52 C51 C50 121.0(4) . . ? C52 C51 C55 118.8(4) . . ? C50 C51 C55 120.2(4) . . ? C53 C52 C51 118.8(4) . . ? C53 C52 H52 120.6 . . ? C51 C52 H52 120.6 . . ? C52 C53 C54 120.1(4) . . ? C52 C53 C56 119.0(4) . . ? C54 C53 C56 120.9(4) . . ? C53 C54 C49 122.7(4) . . ? C53 C54 H54 118.7 . . ? C49 C54 H54 118.7 . . ? F3 C55 F1 108.9(5) . . ? F3 C55 F2 102.8(5) . . ? F1 C55 F2 103.2(5) . . ? F3 C55 C51 113.1(5) . . ? F1 C55 C51 115.5(4) . . ? F2 C55 C51 112.1(4) . . ? F6 C56 F5 105.1(4) . . ? F6 C56 F4 102.1(4) . . ? F5 C56 F4 109.4(4) . . ? F6 C56 C53 113.6(4) . . ? F5 C56 C53 112.9(4) . . ? F4 C56 C53 113.0(4) . . ? C62 C57 C58 115.2(4) . . ? C62 C57 B1 124.6(3) . . ? C58 C57 B1 120.2(3) . . ? C59 C58 C57 122.7(4) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C58 C59 C60 120.6(4) . . ? C58 C59 C63 119.4(4) . . ? C60 C59 C63 120.0(4) . . ? C59 C60 C61 117.8(4) . . ? C59 C60 H60 121.1 . . ? C61 C60 H60 121.1 . . ? C62 C61 C60 120.7(4) . . ? C62 C61 C64 121.6(4) . . ? C60 C61 C64 117.7(4) . . ? C61 C62 C57 122.9(3) . . ? C61 C62 H62 118.6 . . ? C57 C62 H62 118.6 . . ? F7 C63 F8 103.8(5) . . ? F7 C63 F9 108.6(5) . . ? F8 C63 F9 104.6(4) . . ? F7 C63 C59 111.7(4) . . ? F8 C63 C59 113.3(4) . . ? F9 C63 C59 114.1(4) . . ? F12 C64 F11 105.6(4) . . ? F12 C64 F10 107.4(5) . . ? F11 C64 F10 105.0(4) . . ? F12 C64 C61 114.0(4) . . ? F11 C64 C61 112.4(4) . . ? F10 C64 C61 111.8(4) . . ? C70 C65 C66 116.2(3) . . ? C70 C65 B1 120.4(3) . . ? C66 C65 B1 123.3(3) . . ? C65 C66 C67 122.1(3) . . ? C65 C66 H66 118.9 . . ? C67 C66 H66 118.9 . . ? C66 C67 C68 120.6(4) . . ? C66 C67 C71 121.5(4) . . ? C68 C67 C71 117.9(4) . . ? C69 C68 C67 117.8(4) . . ? C69 C68 H68 121.1 . . ? C67 C68 H68 121.1 . . ? C68 C69 C70 120.4(4) . . ? C68 C69 C72 118.0(4) . . ? C70 C69 C72 121.6(4) . . ? C65 C70 C69 122.8(4) . . ? C65 C70 H70 118.6 . . ? C69 C70 H70 118.6 . . ? F14 C71 F13 107.6(4) . . ? F14 C71 F15 105.4(4) . . ? F13 C71 F15 104.5(4) . . ? F14 C71 C67 113.4(4) . . ? F13 C71 C67 113.8(4) . . ? F15 C71 C67 111.4(3) . . ? F17 C72 F16 111.4(5) . . ? F17 C72 F18 103.1(4) . . ? F16 C72 F18 103.4(4) . . ? F17 C72 C69 113.8(5) . . ? F16 C72 C69 113.6(4) . . ? F18 C72 C69 110.5(5) . . ? C74 C73 C78 116.0(3) . . ? C74 C73 B1 119.3(3) . . ? C78 C73 B1 124.0(4) . . ? C73 C74 C75 122.3(4) . . ? C73 C74 H74 118.8 . . ? C75 C74 H74 118.8 . . ? C76 C75 C74 120.0(4) . . ? C76 C75 C79 121.4(4) . . ? C74 C75 C79 118.5(4) . . ? C75 C76 C77 118.9(4) . . ? C75 C76 H76 120.6 . . ? C77 C76 H76 120.6 . . ? C76 C77 C78 121.5(4) . . ? C76 C77 C80 120.0(4) . . ? C78 C77 C80 118.4(4) . . ? C77 C78 C73 121.3(4) . . ? C77 C78 H78 119.3 . . ? C73 C78 H78 119.3 . . ? F20 C79 F19 106.2(4) . . ? F20 C79 F21 106.0(4) . . ? F19 C79 F21 104.5(4) . . ? F20 C79 C75 114.3(4) . . ? F19 C79 C75 112.6(4) . . ? F21 C79 C75 112.5(4) . . ? F23 C80 F22 104.5(6) . . ? F23 C80 F24 109.6(5) . . ? F22 C80 F24 104.0(4) . . ? F23 C80 C77 113.3(4) . . ? F22 C80 C77 113.4(4) . . ? F24 C80 C77 111.5(5) . . ? C97 B2 C89 111.8(3) . . ? C97 B2 C81 104.1(3) . . ? C89 B2 C81 111.7(3) . . ? C97 B2 C105 111.0(3) . . ? C89 B2 C105 105.1(3) . . ? C81 B2 C105 113.3(3) . . ? C86 C81 C82 114.9(4) . . ? C86 C81 B2 124.2(4) . . ? C82 C81 B2 120.5(3) . . ? C83 C82 C81 122.3(4) . . ? C83 C82 H82 118.8 . . ? C81 C82 H82 118.8 . . ? C82 C83 C84 121.0(4) . . ? C82 C83 C87 119.6(4) . . ? C84 C83 C87 119.4(4) . . ? C85 C84 C83 117.6(4) . . ? C85 C84 H84 121.2 . . ? C83 C84 H84 121.2 . . ? C84 C85 C86 121.9(4) . . ? C84 C85 C88 119.6(5) . . ? C86 C85 C88 118.5(5) . . ? C85 C86 C81 122.2(4) . . ? C85 C86 H86 118.9 . . ? C81 C86 H86 118.9 . . ? F25 C87 F27 113.3(7) . . ? F25A C87 F27A 106.0(13) . . ? F25A C87 F26A 101.2(14) . . ? F27A C87 F26A 93.7(13) . . ? F25 C87 F26 101.0(7) . . ? F27 C87 F26 100.8(5) . . ? F25 C87 C83 114.0(5) . . ? F27 C87 C83 116.0(6) . . ? F25A C87 C83 120.9(8) . . ? F27A C87 C83 121.4(7) . . ? F26A C87 C83 108.3(7) . . ? F26 C87 C83 109.6(5) . . ? F29 C88 F30 106.9(5) . . ? F29 C88 F28 104.5(7) . . ? F30 C88 F28 104.7(5) . . ? F29 C88 C85 113.4(5) . . ? F30 C88 C85 114.4(6) . . ? F28 C88 C85 112.1(5) . . ? C90 C89 C94 115.7(3) . . ? C90 C89 B2 124.0(3) . . ? C94 C89 B2 120.2(3) . . ? C91 C90 C89 122.4(3) . . ? C91 C90 H90 118.8 . . ? C89 C90 H90 118.8 . . ? C92 C91 C90 121.1(4) . . ? C92 C91 C95 121.2(4) . . ? C90 C91 C95 117.8(3) . . ? C91 C92 C93 117.7(4) . . ? C91 C92 H92 121.1 . . ? C93 C92 H92 121.1 . . ? C92 C93 C94 121.2(4) . . ? C92 C93 C96 118.3(4) . . ? C94 C93 C96 120.5(4) . . ? C93 C94 C89 121.8(4) . . ? C93 C94 H94 119.1 . . ? C89 C94 H94 119.1 . . ? F33 C95 F31 106.6(4) . . ? F33 C95 F32 105.7(4) . . ? F31 C95 F32 105.5(4) . . ? F33 C95 C91 113.7(4) . . ? F31 C95 C91 113.2(4) . . ? F32 C95 C91 111.5(4) . . ? F35 C96 F36 106.1(5) . . ? F35 C96 F34 107.0(5) . . ? F36 C96 F34 103.0(5) . . ? F35 C96 C93 113.7(5) . . ? F36 C96 C93 113.5(4) . . ? F34 C96 C93 112.7(4) . . ? C98 C97 C102 115.4(4) . . ? C98 C97 B2 123.4(3) . . ? C102 C97 B2 120.9(3) . . ? C99 C98 C97 121.9(4) . . ? C99 C98 H98 119.0 . . ? C97 C98 H98 119.0 . . ? C100 C99 C98 121.7(4) . . ? C100 C99 C103 120.1(4) . . ? C98 C99 C103 118.2(4) . . ? C99 C100 C101 118.2(4) . . ? C99 C100 H100 120.9 . . ? C101 C100 H100 120.9 . . ? C100 C101 C102 121.0(4) . . ? C100 C101 C104 119.3(4) . . ? C102 C101 C104 119.7(4) . . ? C101 C102 C97 121.8(4) . . ? C101 C102 H102 119.1 . . ? C97 C102 H102 119.1 . . ? F38 C103 F39 106.8(4) . . ? F38 C103 F37 105.7(4) . . ? F39 C103 F37 104.3(4) . . ? F38 C103 C99 113.6(4) . . ? F39 C103 C99 112.5(3) . . ? F37 C103 C99 113.1(4) . . ? F40 C104 F42 109.5(4) . . ? F40 C104 F41 103.9(4) . . ? F42 C104 F41 102.5(4) . . ? F40 C104 C101 113.3(4) . . ? F42 C104 C101 113.7(4) . . ? F41 C104 C101 113.1(4) . . ? C106 C105 C110 115.5(4) . . ? C106 C105 B2 121.8(3) . . ? C110 C105 B2 122.5(3) . . ? C105 C106 C107 122.6(4) . . ? C105 C106 H106 118.7 . . ? C107 C106 H106 118.7 . . ? C108 C107 C106 120.4(4) . . ? C108 C107 C111 119.6(4) . . ? C106 C107 C111 119.9(4) . . ? C107 C108 C109 118.8(4) . . ? C107 C108 H108 120.6 . . ? C109 C108 H108 120.6 . . ? C110 C109 C108 120.1(4) . . ? C110 C109 C112 121.6(4) . . ? C108 C109 C112 118.3(4) . . ? C109 C110 C105 122.5(4) . . ? C109 C110 H110 118.8 . . ? C105 C110 H110 118.8 . . ? F45 C111 F43 108.1(4) . . ? F45 C111 F44 105.7(4) . . ? F43 C111 F44 101.8(5) . . ? F45 C111 C107 114.3(4) . . ? F43 C111 C107 113.9(4) . . ? F44 C111 C107 112.0(4) . . ? F47 C112 F48 107.7(5) . . ? F47 C112 F46 104.7(5) . . ? F48 C112 F46 103.6(6) . . ? F47 C112 C109 114.5(6) . . ? F48 C112 C109 114.0(5) . . ? F46 C112 C109 111.4(5) . . ? C25 Rh3 C26 89.3(3) . . ? C25 Rh3 N11 177.9(3) . . ? C26 Rh3 N11 92.6(2) . . ? C25 Rh3 N9 90.5(2) . . ? C26 Rh3 N9 179.6(3) . . ? N11 Rh3 N9 87.52(15) . . ? C41 Rh4 C40 90.5(4) . . ? C41 Rh4 N13 178.2(3) . . ? C40 Rh4 N13 89.9(3) . . ? C41 Rh4 N15 91.3(3) . . ? C40 Rh4 N15 175.3(3) . . ? N13 Rh4 N15 88.45(16) . . ? C30 N9 N10 104.9(4) . . ? C30 N9 Rh3 133.1(3) . . ? N10 N9 Rh3 121.8(3) . . ? C32 N10 N9 109.9(4) . . ? C32 N10 C33 128.3(4) . . ? N9 N10 C33 121.0(4) . . ? C27 N11 N12 105.2(4) . . ? C27 N11 Rh3 131.6(3) . . ? N12 N11 Rh3 123.0(3) . . ? C29 N12 N11 111.8(4) . . ? C29 N12 C33 128.7(4) . . ? N11 N12 C33 119.3(3) . . ? N14 N13 C42 104.4(5) . . ? N14 N13 Rh4 122.8(3) . . ? C42 N13 Rh4 132.7(4) . . ? N13 N14 C44 111.9(4) . . ? N13 N14 C48 120.9(4) . . ? C44 N14 C48 126.3(5) . . ? C45 N15 N16 104.9(4) . . ? C45 N15 Rh4 132.5(4) . . ? N16 N15 Rh4 121.4(3) . . ? C47 N16 N15 111.1(4) . . ? C47 N16 C48 127.4(4) . . ? N15 N16 C48 121.0(3) . . ? O7 C25 Rh3 177.8(8) . . ? O8 C26 Rh3 178.9(8) . . ? N11 C27 C28 110.5(5) . . ? N11 C27 H27 124.8 . . ? C28 C27 H27 124.8 . . ? C29 C28 C27 106.0(5) . . ? C29 C28 H28 127.0 . . ? C27 C28 H28 127.0 . . ? N12 C29 C28 106.5(4) . . ? N12 C29 H29 126.8 . . ? C28 C29 H29 126.8 . . ? N9 C30 C31 112.7(4) . . ? N9 C30 H30 123.7 . . ? C31 C30 H30 123.7 . . ? C30 C31 C32 103.9(5) . . ? C30 C31 H31 128.1 . . ? C32 C31 H31 128.1 . . ? N10 C32 C31 108.6(5) . . ? N10 C32 H32 125.7 . . ? C31 C32 H32 125.7 . . ? N10 C33 N12 111.2(3) . . ? N10 C33 C34 113.1(3) . . ? N12 C33 C34 111.2(3) . . ? N10 C33 H33 107.0 . . ? N12 C33 H33 107.0 . . ? C34 C33 H33 107.0 . . ? C35 C34 C39 119.2(4) . . ? C35 C34 C33 121.7(4) . . ? C39 C34 C33 118.9(3) . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 119.5(4) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 120.6(4) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 119.6(4) . . ? C39 C38 C48 121.0(4) . . ? C37 C38 C48 119.2(4) . . ? C38 C39 C34 120.5(4) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? O5 C40 Rh4 177.4(7) . . ? O6 C41 Rh4 179.7(9) . . ? N13 C42 C43 109.9(6) . . ? N13 C42 H42 125.0 . . ? C43 C42 H42 125.0 . . ? C44 C43 C42 106.9(6) . . ? C44 C43 H43 126.5 . . ? C42 C43 H43 126.5 . . ? C43 C44 N14 106.8(6) . . ? C43 C44 H44 126.6 . . ? N14 C44 H44 126.6 . . ? N15 C45 C46 111.4(5) . . ? N15 C45 H45 124.3 . . ? C46 C45 H45 124.3 . . ? C47 C46 C45 105.9(5) . . ? C47 C46 H46 127.1 . . ? C45 C46 H46 127.1 . . ? N16 C47 C46 106.7(4) . . ? N16 C47 H47 126.7 . . ? C46 C47 H47 126.7 . . ? N14 C48 N16 110.1(4) . . ? N14 C48 C38 112.6(3) . . ? N16 C48 C38 111.6(4) . . ? N14 C48 H48 107.5 . . ? N16 C48 H48 107.5 . . ? C38 C48 H48 107.5 . . ? C121 B3 C113 106.9(3) . . ? C121 B3 C137 110.9(3) . . ? C113 B3 C137 111.2(3) . . ? C121 B3 C129 112.1(3) . . ? C113 B3 C129 110.9(3) . . ? C137 B3 C129 104.9(3) . . ? C114 C113 C118 115.7(4) . . ? C114 C113 B3 119.7(3) . . ? C118 C113 B3 124.6(4) . . ? C113 C114 C115 123.4(4) . . ? C113 C114 H114 118.3 . . ? C115 C114 H114 118.3 . . ? C116 C115 C114 120.1(5) . . ? C116 C115 C119 119.9(4) . . ? C114 C115 C119 120.0(5) . . ? C115 C116 C117 118.7(4) . . ? C115 C116 H116 120.7 . . ? C117 C116 H116 120.7 . . ? C116 C117 C118 120.7(4) . . ? C116 C117 C120 120.0(4) . . ? C118 C117 C120 119.2(5) . . ? C113 C118 C117 121.3(4) . . ? C113 C118 H118 119.3 . . ? C117 C118 H118 119.3 . . ? F51 C119 F49 107.3(5) . . ? F51 C119 F50 105.5(6) . . ? F49 C119 F50 104.4(5) . . ? F51 C119 C115 113.4(4) . . ? F49 C119 C115 113.4(5) . . ? F50 C119 C115 112.1(5) . . ? F54 C120 F53 106.3(6) . . ? F54 C120 F52 103.8(4) . . ? F53 C120 F52 104.9(5) . . ? F54 C120 C117 114.7(4) . . ? F53 C120 C117 113.3(4) . . ? F52 C120 C117 112.8(6) . . ? C126 C121 C122 115.0(4) . . ? C126 C121 B3 120.6(3) . . ? C122 C121 B3 124.3(4) . . ? C123 C122 C121 121.8(4) . . ? C123 C122 H122 119.1 . . ? C121 C122 H122 119.1 . . ? C122 C123 C124 121.8(4) . . ? C122 C123 C127 119.4(4) . . ? C124 C123 C127 118.8(4) . . ? C123 C124 C125 117.8(4) . . ? C123 C124 H124 121.1 . . ? C125 C124 H124 121.1 . . ? C126 C125 C124 119.9(4) . . ? C126 C125 C128 120.7(3) . . ? C124 C125 C128 119.3(4) . . ? C125 C126 C121 123.6(3) . . ? C125 C126 H126 118.2 . . ? C121 C126 H126 118.2 . . ? F55 C127 F56 108.2(5) . . ? F55 C127 F57 105.1(4) . . ? F56 C127 F57 105.1(4) . . ? F55 C127 C123 112.9(4) . . ? F56 C127 C123 112.3(4) . . ? F57 C127 C123 112.7(4) . . ? F60 C128 F59 106.6(4) . . ? F60 C128 F58 106.8(3) . . ? F59 C128 F58 105.6(4) . . ? F60 C128 C125 113.1(4) . . ? F59 C128 C125 112.5(4) . . ? F58 C128 C125 111.8(4) . . ? C134 C129 C130 115.2(3) . . ? C134 C129 B3 126.6(3) . . ? C130 C129 B3 118.2(3) . . ? C131 C130 C129 123.2(4) . . ? C131 C130 H130 118.4 . . ? C129 C130 H130 118.4 . . ? C130 C131 C132 120.2(4) . . ? C130 C131 C135 118.6(4) . . ? C132 C131 C135 121.1(4) . . ? C133 C132 C131 117.4(4) . . ? C133 C132 H132 121.3 . . ? C131 C132 H132 121.3 . . ? C132 C133 C134 122.0(4) . . ? C132 C133 C136 117.9(4) . . ? C134 C133 C136 120.1(4) . . ? C129 C134 C133 122.0(4) . . ? C129 C134 H134 119.0 . . ? C133 C134 H134 119.0 . . ? F61 C135 F62 107.1(4) . . ? F61 C135 F63 107.1(4) . . ? F62 C135 F63 105.3(4) . . ? F61 C135 C131 113.7(4) . . ? F62 C135 C131 111.7(4) . . ? F63 C135 C131 111.4(4) . . ? F66 C136 F64 110.9(5) . . ? F66 C136 F65 105.4(5) . . ? F64 C136 F65 99.4(4) . . ? F66 C136 C133 114.1(4) . . ? F64 C136 C133 113.8(4) . . ? F65 C136 C133 111.9(4) . . ? C138 C137 C142 115.2(4) . . ? C138 C137 B3 125.9(4) . . ? C142 C137 B3 118.9(3) . . ? C137 C138 C139 122.0(4) . . ? C137 C138 H138 119.0 . . ? C139 C138 H138 119.0 . . ? C140 C139 C138 121.3(4) . . ? C140 C139 C143 120.5(4) . . ? C138 C139 C143 118.2(5) . . ? C139 C140 C141 118.3(4) . . ? C139 C140 H140 120.8 . . ? C141 C140 H140 120.8 . . ? C140 C141 C142 120.8(4) . . ? C140 C141 C144 118.8(4) . . ? C142 C141 C144 120.4(4) . . ? C141 C142 C137 122.4(4) . . ? C141 C142 H142 118.8 . . ? C137 C142 H142 118.8 . . ? F68 C143 F67 107.3(8) . . ? F68 C143 F69 106.0(6) . . ? F67 C143 F69 101.8(5) . . ? F68 C143 C139 115.3(5) . . ? F67 C143 C139 113.5(5) . . ? F69 C143 C139 111.9(6) . . ? F72 C144 F70 105.9(5) . . ? F72 C144 F71 105.6(4) . . ? F70 C144 F71 104.6(5) . . ? F72 C144 C141 113.1(5) . . ? F70 C144 C141 115.0(4) . . ? F71 C144 C141 111.9(4) . . ? C161 B4 C153 113.1(3) . . ? C161 B4 C169 107.2(3) . . ? C153 B4 C169 111.3(3) . . ? C161 B4 C145 110.6(3) . . ? C153 B4 C145 105.3(3) . . ? C169 B4 C145 109.2(3) . . ? F93 C175 F91 123.8(14) . . ? F93 C175 F92 102.1(11) . . ? F91 C175 F92 98.7(12) . . ? F93 C175 C171 110.1(9) . . ? F91 C175 C171 110.8(15) . . ? F92 C175 C171 109.6(10) . . ? F93A C178 F91A 107.1(8) . . ? F93A C178 F92A 104.4(7) . . ? F91A C178 F92A 102.9(9) . . ? F93A C178 C171 116.2(7) . . ? F91A C178 C171 115.4(8) . . ? F92A C178 C171 109.4(8) . . ? F96 C176 F95 102.5(18) . . ? F96 C176 F94 107.1(11) . . ? F95 C176 F94 104.1(19) . . ? F96 C176 C173 116.7(9) . . ? F95 C176 C173 119(3) . . ? F94 C176 C173 106.6(9) . . ? F96A C177 F95A 111.3(13) . . ? F96A C177 F94A 107.4(7) . . ? F95A C177 F94A 100.9(11) . . ? F96A C177 C173 113.6(8) . . ? F95A C177 C173 107.4(16) . . ? F94A C177 C173 115.5(6) . . ? C150 C145 C146 116.0(4) . . ? C150 C145 B4 125.9(3) . . ? C146 C145 B4 118.0(3) . . ? C147 C146 C145 121.8(4) . . ? C147 C146 H146 119.1 . . ? C145 C146 H146 119.1 . . ? C148 C147 C146 120.6(4) . . ? C148 C147 C151 118.0(4) . . ? C146 C147 C151 121.3(4) . . ? C149 C148 C147 118.3(4) . . ? C149 C148 H148 120.8 . . ? C147 C148 H148 120.8 . . ? C148 C149 C150 120.9(4) . . ? C148 C149 C152 119.3(5) . . ? C150 C149 C152 119.6(5) . . ? C145 C150 C149 122.2(4) . . ? C145 C150 H150 118.9 . . ? C149 C150 H150 118.9 . . ? F75 C151 F74 106.1(5) . . ? F75 C151 F73 108.1(5) . . ? F74 C151 F73 101.2(5) . . ? F75 C151 C147 112.8(5) . . ? F74 C151 C147 113.5(4) . . ? F73 C151 C147 114.2(4) . . ? F78 C152 F76 108.2(6) . . ? F78 C152 F77 105.3(6) . . ? F76 C152 F77 102.6(6) . . ? F78 C152 C149 111.8(5) . . ? F76 C152 C149 114.4(5) . . ? F77 C152 C149 113.6(6) . . ? C158 C153 C154 115.2(4) . . ? C158 C153 B4 118.7(3) . . ? C154 C153 B4 126.0(4) . . ? C155 C154 C153 121.6(4) . . ? C155 C154 H154 119.2 . . ? C153 C154 H154 119.2 . . ? C156 C155 C154 121.6(4) . . ? C156 C155 C159 118.2(4) . . ? C154 C155 C159 120.3(4) . . ? C155 C156 C157 118.1(4) . . ? C155 C156 H156 121.0 . . ? C157 C156 H156 121.0 . . ? C158 C157 C156 120.8(4) . . ? C158 C157 C160 119.3(4) . . ? C156 C157 C160 119.9(4) . . ? C157 C158 C153 122.7(4) . . ? C157 C158 H158 118.6 . . ? C153 C158 H158 118.6 . . ? F79 C159 F81 106.6(4) . . ? F79 C159 F80 106.6(3) . . ? F81 C159 F80 105.3(4) . . ? F79 C159 C155 114.1(4) . . ? F81 C159 C155 111.9(3) . . ? F80 C159 C155 111.8(3) . . ? F82 C160 F84 105.9(4) . . ? F82 C160 F83 105.4(4) . . ? F84 C160 F83 106.7(4) . . ? F82 C160 C157 113.9(4) . . ? F84 C160 C157 112.6(4) . . ? F83 C160 C157 111.7(4) . . ? C166 C161 C162 115.7(4) . . ? C166 C161 B4 120.7(3) . . ? C162 C161 B4 123.3(3) . . ? C163 C162 C161 121.9(4) . . ? C163 C162 H162 119.0 . . ? C161 C162 H162 119.0 . . ? C164 C163 C162 120.8(4) . . ? C164 C163 C167 120.3(4) . . ? C162 C163 C167 118.8(4) . . ? C165 C164 C163 118.6(4) . . ? C165 C164 H164 120.7 . . ? C163 C164 H164 120.7 . . ? C164 C165 C166 120.8(4) . . ? C164 C165 C168 121.3(4) . . ? C166 C165 C168 117.9(4) . . ? C161 C166 C165 122.1(4) . . ? C161 C166 H166 119.0 . . ? C165 C166 H166 119.0 . . ? F85 C167 F87 106.5(4) . . ? F85 C167 F86 105.6(4) . . ? F87 C167 F86 104.3(4) . . ? F85 C167 C163 113.4(4) . . ? F87 C167 C163 112.8(4) . . ? F86 C167 C163 113.5(4) . . ? F89 C168 F88 105.9(4) . . ? F89 C168 F90 105.9(5) . . ? F88 C168 F90 105.3(4) . . ? F89 C168 C165 113.5(4) . . ? F88 C168 C165 112.6(4) . . ? F90 C168 C165 113.0(4) . . ? C174 C169 C170 116.7(4) . . ? C174 C169 B4 124.4(4) . . ? C170 C169 B4 118.9(3) . . ? C171 C170 C169 122.5(4) . . ? C171 C170 H170 118.7 . . ? C169 C170 H170 118.7 . . ? C172 C171 C170 119.8(5) . . ? C172 C171 C175 116.9(6) . . ? C170 C171 C175 123.1(6) . . ? C172 C171 C178 122.0(5) . . ? C170 C171 C178 118.1(5) . . ? C173 C172 C171 118.8(4) . . ? C173 C172 H172 120.6 . . ? C171 C172 H172 120.6 . . ? C172 C173 C174 122.1(4) . . ? C172 C173 C176 119.8(6) . . ? C174 C173 C176 117.6(7) . . ? C172 C173 C177 122.2(5) . . ? C174 C173 C177 115.5(6) . . ? C169 C174 C173 120.1(4) . . ? C169 C174 H174 120.0 . . ? C173 C174 H174 120.0 . . ? Cl2A C1A Cl1A 122(3) . . ? Cl2A C1A H1A 106.8 . . ? Cl1A C1A H1A 106.8 . . ? Cl2A C1A H1B 106.8 . . ? Cl1A C1A H1B 106.8 . . ? H1A C1A H1B 106.7 . . ? Cl2B C1B Cl1B 117(3) . . ? Cl2B C1B H1C 108.1 . . ? Cl1B C1B H1C 108.1 . . ? Cl2B C1B H1D 108.1 . . ? Cl1B C1B H1D 108.1 . . ? H1C C1B H1D 107.3 . . ? 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 C1 Rh1 N1 C3 -22.3(5) . . . . ? N3 Rh1 N1 C3 152.9(4) . . . . ? C1 Rh1 N1 N2 158.2(4) . . . . ? N3 Rh1 N1 N2 -26.6(3) . . . . ? C3 N1 N2 C5 1.8(5) . . . . ? Rh1 N1 N2 C5 -178.6(3) . . . . ? C3 N1 N2 C9 176.1(4) . . . . ? Rh1 N1 N2 C9 -4.2(5) . . . . ? C2 Rh1 N3 C6 33.4(5) . . . . ? N1 Rh1 N3 C6 -148.3(5) . . . . ? C2 Rh1 N3 N4 -161.9(4) . . . . ? N1 Rh1 N3 N4 16.3(3) . . . . ? C6 N3 N4 C8 -2.7(5) . . . . ? Rh1 N3 N4 C8 -171.1(3) . . . . ? C6 N3 N4 C9 -166.7(4) . . . . ? Rh1 N3 N4 C9 24.9(5) . . . . ? C17 Rh2 N5 C18 36.9(4) . . . . ? N7 Rh2 N5 C18 -142.7(4) . . . . ? C17 Rh2 N5 N6 -159.1(3) . . . . ? N7 Rh2 N5 N6 21.2(3) . . . . ? C18 N5 N6 C20 -0.5(5) . . . . ? Rh2 N5 N6 C20 -168.0(3) . . . . ? C18 N5 N6 C24 -177.1(4) . . . . ? Rh2 N5 N6 C24 15.4(5) . . . . ? C16 Rh2 N7 C21 -24.8(5) . . . . ? N5 Rh2 N7 C21 150.0(4) . . . . ? C16 Rh2 N7 N8 164.3(4) . . . . ? N5 Rh2 N7 N8 -20.9(3) . . . . ? C21 N7 N8 C23 1.5(5) . . . . ? Rh2 N7 N8 C23 174.6(3) . . . . ? C21 N7 N8 C24 170.5(4) . . . . ? Rh2 N7 N8 C24 -16.5(5) . . . . ? N2 N1 C3 C4 -0.7(6) . . . . ? Rh1 N1 C3 C4 179.8(3) . . . . ? N1 C3 C4 C5 -0.7(6) . . . . ? C3 C4 C5 N2 1.8(6) . . . . ? N1 N2 C5 C4 -2.3(5) . . . . ? C9 N2 C5 C4 -176.3(4) . . . . ? N4 N3 C6 C7 3.0(6) . . . . ? Rh1 N3 C6 C7 169.6(4) . . . . ? N3 C6 C7 C8 -2.2(7) . . . . ? N3 N4 C8 C7 1.5(6) . . . . ? C9 N4 C8 C7 164.5(5) . . . . ? C6 C7 C8 N4 0.4(6) . . . . ? C5 N2 C9 N4 -133.1(5) . . . . ? N1 N2 C9 N4 53.6(5) . . . . ? C5 N2 C9 C10 100.2(5) . . . . ? N1 N2 C9 C10 -73.1(5) . . . . ? C8 N4 C9 N2 132.9(5) . . . . ? N3 N4 C9 N2 -65.4(5) . . . . ? C8 N4 C9 C10 -98.8(5) . . . . ? N3 N4 C9 C10 62.8(5) . . . . ? N2 C9 C10 C15 166.6(3) . . . . ? N4 C9 C10 C15 40.7(5) . . . . ? N2 C9 C10 C11 -21.2(6) . . . . ? N4 C9 C10 C11 -147.1(4) . . . . ? C15 C10 C11 C12 0.1(6) . . . . ? C9 C10 C11 C12 -172.1(4) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C14 -0.2(6) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C12 C13 C14 C24 172.6(3) . . . . ? C11 C10 C15 C14 -1.2(6) . . . . ? C9 C10 C15 C14 171.2(4) . . . . ? C13 C14 C15 C10 1.5(5) . . . . ? C24 C14 C15 C10 -172.2(3) . . . . ? N6 N5 C18 C19 0.2(5) . . . . ? Rh2 N5 C18 C19 166.3(3) . . . . ? N5 C18 C19 C20 0.1(5) . . . . ? N5 N6 C20 C19 0.6(5) . . . . ? C24 N6 C20 C19 176.8(4) . . . . ? C18 C19 C20 N6 -0.4(5) . . . . ? N8 N7 C21 C22 -1.3(5) . . . . ? Rh2 N7 C21 C22 -173.4(3) . . . . ? N7 C21 C22 C23 0.6(6) . . . . ? N7 N8 C23 C22 -1.2(5) . . . . ? C24 N8 C23 C22 -169.1(4) . . . . ? C21 C22 C23 N8 0.3(6) . . . . ? C23 N8 C24 N6 -130.7(4) . . . . ? N7 N8 C24 N6 62.4(5) . . . . ? C23 N8 C24 C14 102.8(5) . . . . ? N7 N8 C24 C14 -64.1(5) . . . . ? C20 N6 C24 N8 122.0(4) . . . . ? N5 N6 C24 N8 -62.0(4) . . . . ? C20 N6 C24 C14 -112.3(4) . . . . ? N5 N6 C24 C14 63.7(4) . . . . ? C13 C14 C24 N8 148.1(3) . . . . ? C15 C14 C24 N8 -38.5(5) . . . . ? C13 C14 C24 N6 23.4(5) . . . . ? C15 C14 C24 N6 -163.2(3) . . . . ? C73 B1 C49 C50 77.1(4) . . . . ? C57 B1 C49 C50 -159.1(3) . . . . ? C65 B1 C49 C50 -42.6(4) . . . . ? C73 B1 C49 C54 -97.9(4) . . . . ? C57 B1 C49 C54 25.9(5) . . . . ? C65 B1 C49 C54 142.4(3) . . . . ? C54 C49 C50 C51 -2.0(5) . . . . ? B1 C49 C50 C51 -177.3(3) . . . . ? C49 C50 C51 C52 -0.3(6) . . . . ? C49 C50 C51 C55 178.3(4) . . . . ? C50 C51 C52 C53 1.2(6) . . . . ? C55 C51 C52 C53 -177.4(4) . . . . ? C51 C52 C53 C54 0.2(6) . . . . ? C51 C52 C53 C56 -177.2(4) . . . . ? C52 C53 C54 C49 -2.6(6) . . . . ? C56 C53 C54 C49 174.7(4) . . . . ? C50 C49 C54 C53 3.4(5) . . . . ? B1 C49 C54 C53 178.7(3) . . . . ? C52 C51 C55 F3 -66.1(7) . . . . ? C50 C51 C55 F3 115.3(6) . . . . ? C52 C51 C55 F1 167.4(4) . . . . ? C50 C51 C55 F1 -11.2(7) . . . . ? C52 C51 C55 F2 49.6(6) . . . . ? C50 C51 C55 F2 -129.0(5) . . . . ? C52 C53 C56 F6 44.6(6) . . . . ? C54 C53 C56 F6 -132.8(4) . . . . ? C52 C53 C56 F5 -75.0(5) . . . . ? C54 C53 C56 F5 107.7(5) . . . . ? C52 C53 C56 F4 160.3(4) . . . . ? C54 C53 C56 F4 -17.1(6) . . . . ? C73 B1 C57 C62 -27.1(5) . . . . ? C49 B1 C57 C62 -144.9(3) . . . . ? C65 B1 C57 C62 95.6(4) . . . . ? C73 B1 C57 C58 155.8(3) . . . . ? C49 B1 C57 C58 37.9(5) . . . . ? C65 B1 C57 C58 -81.5(4) . . . . ? C62 C57 C58 C59 1.4(5) . . . . ? B1 C57 C58 C59 178.8(4) . . . . ? C57 C58 C59 C60 0.5(6) . . . . ? C57 C58 C59 C63 179.1(4) . . . . ? C58 C59 C60 C61 -1.7(6) . . . . ? C63 C59 C60 C61 179.7(4) . . . . ? C59 C60 C61 C62 0.8(6) . . . . ? C59 C60 C61 C64 178.9(4) . . . . ? C60 C61 C62 C57 1.2(6) . . . . ? C64 C61 C62 C57 -176.8(4) . . . . ? C58 C57 C62 C61 -2.3(5) . . . . ? B1 C57 C62 C61 -179.6(4) . . . . ? C58 C59 C63 F7 47.0(7) . . . . ? C60 C59 C63 F7 -134.4(5) . . . . ? C58 C59 C63 F8 -69.8(6) . . . . ? C60 C59 C63 F8 108.8(5) . . . . ? C58 C59 C63 F9 170.6(4) . . . . ? C60 C59 C63 F9 -10.8(7) . . . . ? C62 C61 C64 F12 -9.4(7) . . . . ? C60 C61 C64 F12 172.5(4) . . . . ? C62 C61 C64 F11 -129.6(4) . . . . ? C60 C61 C64 F11 52.4(6) . . . . ? C62 C61 C64 F10 112.7(5) . . . . ? C60 C61 C64 F10 -65.4(6) . . . . ? C73 B1 C65 C70 -152.6(4) . . . . ? C49 B1 C65 C70 -37.6(5) . . . . ? C57 B1 C65 C70 83.1(4) . . . . ? C73 B1 C65 C66 31.5(5) . . . . ? C49 B1 C65 C66 146.5(4) . . . . ? C57 B1 C65 C66 -92.8(4) . . . . ? C70 C65 C66 C67 1.9(6) . . . . ? B1 C65 C66 C67 178.0(4) . . . . ? C65 C66 C67 C68 -1.7(6) . . . . ? C65 C66 C67 C71 178.3(4) . . . . ? C66 C67 C68 C69 -0.4(6) . . . . ? C71 C67 C68 C69 179.6(4) . . . . ? C67 C68 C69 C70 2.1(7) . . . . ? C67 C68 C69 C72 -177.2(5) . . . . ? C66 C65 C70 C69 -0.2(6) . . . . ? B1 C65 C70 C69 -176.3(4) . . . . ? C68 C69 C70 C65 -1.9(7) . . . . ? C72 C69 C70 C65 177.4(5) . . . . ? C66 C67 C71 F14 -106.4(5) . . . . ? C68 C67 C71 F14 73.6(5) . . . . ? C66 C67 C71 F13 17.0(6) . . . . ? C68 C67 C71 F13 -163.0(4) . . . . ? C66 C67 C71 F15 134.9(4) . . . . ? C68 C67 C71 F15 -45.1(6) . . . . ? C68 C69 C72 F17 -67.5(7) . . . . ? C70 C69 C72 F17 113.3(5) . . . . ? C68 C69 C72 F16 163.7(5) . . . . ? C70 C69 C72 F16 -15.6(8) . . . . ? C68 C69 C72 F18 47.9(6) . . . . ? C70 C69 C72 F18 -131.3(5) . . . . ? C49 B1 C73 C74 -79.9(4) . . . . ? C57 B1 C73 C74 157.8(3) . . . . ? C65 B1 C73 C74 38.7(5) . . . . ? C49 B1 C73 C78 89.2(4) . . . . ? C57 B1 C73 C78 -33.1(5) . . . . ? C65 B1 C73 C78 -152.2(4) . . . . ? C78 C73 C74 C75 0.2(6) . . . . ? B1 C73 C74 C75 170.1(4) . . . . ? C73 C74 C75 C76 0.4(6) . . . . ? C73 C74 C75 C79 -178.0(4) . . . . ? C74 C75 C76 C77 -0.3(6) . . . . ? C79 C75 C76 C77 178.1(4) . . . . ? C75 C76 C77 C78 -0.4(6) . . . . ? C75 C76 C77 C80 -177.0(4) . . . . ? C76 C77 C78 C73 1.0(6) . . . . ? C80 C77 C78 C73 177.6(4) . . . . ? C74 C73 C78 C77 -0.8(6) . . . . ? B1 C73 C78 C77 -170.3(4) . . . . ? C76 C75 C79 F20 -3.4(6) . . . . ? C74 C75 C79 F20 175.0(4) . . . . ? C76 C75 C79 F19 117.9(5) . . . . ? C74 C75 C79 F19 -63.7(5) . . . . ? C76 C75 C79 F21 -124.4(5) . . . . ? C74 C75 C79 F21 54.0(6) . . . . ? C76 C77 C80 F23 92.3(6) . . . . ? C78 C77 C80 F23 -84.4(6) . . . . ? C76 C77 C80 F22 -148.9(5) . . . . ? C78 C77 C80 F22 34.5(7) . . . . ? C76 C77 C80 F24 -31.9(7) . . . . ? C78 C77 C80 F24 151.5(5) . . . . ? C97 B2 C81 C86 -93.6(4) . . . . ? C89 B2 C81 C86 145.6(4) . . . . ? C105 B2 C81 C86 27.1(5) . . . . ? C97 B2 C81 C82 79.0(4) . . . . ? C89 B2 C81 C82 -41.8(5) . . . . ? C105 B2 C81 C82 -160.2(3) . . . . ? C86 C81 C82 C83 -1.0(6) . . . . ? B2 C81 C82 C83 -174.3(4) . . . . ? C81 C82 C83 C84 -0.3(6) . . . . ? C81 C82 C83 C87 -179.7(4) . . . . ? C82 C83 C84 C85 1.4(6) . . . . ? C87 C83 C84 C85 -179.2(4) . . . . ? C83 C84 C85 C86 -1.1(7) . . . . ? C83 C84 C85 C88 177.6(5) . . . . ? C84 C85 C86 C81 -0.3(7) . . . . ? C88 C85 C86 C81 -179.0(5) . . . . ? C82 C81 C86 C85 1.3(6) . . . . ? B2 C81 C86 C85 174.3(4) . . . . ? C82 C83 C87 F25 -54.4(9) . . . . ? C84 C83 C87 F25 126.2(8) . . . . ? C82 C83 C87 F27 171.2(6) . . . . ? C84 C83 C87 F27 -8.2(8) . . . . ? C82 C83 C87 F25A 121.1(17) . . . . ? C84 C83 C87 F25A -58.3(18) . . . . ? C82 C83 C87 F27A -16.7(15) . . . . ? C84 C83 C87 F27A 163.9(14) . . . . ? C82 C83 C87 F26A -123.0(11) . . . . ? C84 C83 C87 F26A 57.5(11) . . . . ? C82 C83 C87 F26 58.0(6) . . . . ? C84 C83 C87 F26 -121.4(6) . . . . ? C84 C85 C88 F29 134.6(6) . . . . ? C86 C85 C88 F29 -46.6(8) . . . . ? C84 C85 C88 F30 11.7(8) . . . . ? C86 C85 C88 F30 -169.6(5) . . . . ? C84 C85 C88 F28 -107.3(6) . . . . ? C86 C85 C88 F28 71.4(7) . . . . ? C97 B2 C89 C90 -139.6(4) . . . . ? C81 B2 C89 C90 -23.3(5) . . . . ? C105 B2 C89 C90 99.9(4) . . . . ? C97 B2 C89 C94 44.7(5) . . . . ? C81 B2 C89 C94 160.9(3) . . . . ? C105 B2 C89 C94 -75.8(4) . . . . ? C94 C89 C90 C91 -2.9(6) . . . . ? B2 C89 C90 C91 -178.8(4) . . . . ? C89 C90 C91 C92 3.0(6) . . . . ? C89 C90 C91 C95 -176.2(4) . . . . ? C90 C91 C92 C93 0.0(6) . . . . ? C95 C91 C92 C93 179.1(4) . . . . ? C91 C92 C93 C94 -2.9(6) . . . . ? C91 C92 C93 C96 177.2(4) . . . . ? C92 C93 C94 C89 2.9(7) . . . . ? C96 C93 C94 C89 -177.1(5) . . . . ? C90 C89 C94 C93 0.0(6) . . . . ? B2 C89 C94 C93 176.1(4) . . . . ? C92 C91 C95 F33 111.0(5) . . . . ? C90 C91 C95 F33 -69.9(5) . . . . ? C92 C91 C95 F31 -10.8(6) . . . . ? C90 C91 C95 F31 168.3(4) . . . . ? C92 C91 C95 F32 -129.7(4) . . . . ? C90 C91 C95 F32 49.4(5) . . . . ? C92 C93 C96 F35 84.0(6) . . . . ? C94 C93 C96 F35 -96.0(6) . . . . ? C92 C93 C96 F36 -37.5(7) . . . . ? C94 C93 C96 F36 142.6(5) . . . . ? C92 C93 C96 F34 -154.0(5) . . . . ? C94 C93 C96 F34 26.0(7) . . . . ? C89 B2 C97 C98 30.1(5) . . . . ? C81 B2 C97 C98 -90.7(4) . . . . ? C105 B2 C97 C98 147.0(3) . . . . ? C89 B2 C97 C102 -155.7(3) . . . . ? C81 B2 C97 C102 83.5(4) . . . . ? C105 B2 C97 C102 -38.7(4) . . . . ? C102 C97 C98 C99 1.0(5) . . . . ? B2 C97 C98 C99 175.5(3) . . . . ? C97 C98 C99 C100 0.7(6) . . . . ? C97 C98 C99 C103 180.0(3) . . . . ? C98 C99 C100 C101 -0.9(6) . . . . ? C103 C99 C100 C101 179.8(4) . . . . ? C99 C100 C101 C102 -0.5(6) . . . . ? C99 C100 C101 C104 177.2(4) . . . . ? C100 C101 C102 C97 2.3(6) . . . . ? C104 C101 C102 C97 -175.5(4) . . . . ? C98 C97 C102 C101 -2.4(5) . . . . ? B2 C97 C102 C101 -177.0(3) . . . . ? C100 C99 C103 F38 108.6(5) . . . . ? C98 C99 C103 F38 -70.7(5) . . . . ? C100 C99 C103 F39 -129.8(4) . . . . ? C98 C99 C103 F39 50.9(5) . . . . ? C100 C99 C103 F37 -11.9(6) . . . . ? C98 C99 C103 F37 168.8(4) . . . . ? C100 C101 C104 F40 -68.5(5) . . . . ? C102 C101 C104 F40 109.3(5) . . . . ? C100 C101 C104 F42 165.7(4) . . . . ? C102 C101 C104 F42 -16.5(6) . . . . ? C100 C101 C104 F41 49.4(5) . . . . ? C102 C101 C104 F41 -132.9(4) . . . . ? C97 B2 C105 C106 -31.6(5) . . . . ? C89 B2 C105 C106 89.4(4) . . . . ? C81 B2 C105 C106 -148.4(3) . . . . ? C97 B2 C105 C110 152.9(3) . . . . ? C89 B2 C105 C110 -86.1(4) . . . . ? C81 B2 C105 C110 36.1(5) . . . . ? C110 C105 C106 C107 -1.7(6) . . . . ? B2 C105 C106 C107 -177.5(4) . . . . ? C105 C106 C107 C108 -0.1(6) . . . . ? C105 C106 C107 C111 -178.1(4) . . . . ? C106 C107 C108 C109 1.3(6) . . . . ? C111 C107 C108 C109 179.3(4) . . . . ? C107 C108 C109 C110 -0.6(7) . . . . ? C107 C108 C109 C112 -178.2(5) . . . . ? C108 C109 C110 C105 -1.4(7) . . . . ? C112 C109 C110 C105 176.1(5) . . . . ? C106 C105 C110 C109 2.5(6) . . . . ? B2 C105 C110 C109 178.3(4) . . . . ? C108 C107 C111 F45 27.2(7) . . . . ? C106 C107 C111 F45 -154.8(5) . . . . ? C108 C107 C111 F43 152.2(5) . . . . ? C106 C107 C111 F43 -29.8(7) . . . . ? C108 C107 C111 F44 -93.0(5) . . . . ? C106 C107 C111 F44 85.0(5) . . . . ? C110 C109 C112 F47 123.9(6) . . . . ? C108 C109 C112 F47 -58.5(7) . . . . ? C110 C109 C112 F48 -0.8(9) . . . . ? C108 C109 C112 F48 176.8(5) . . . . ? C110 C109 C112 F46 -117.6(6) . . . . ? C108 C109 C112 F46 60.0(7) . . . . ? C25 Rh3 N9 C30 -31.2(5) . . . . ? N11 Rh3 N9 C30 148.2(4) . . . . ? C25 Rh3 N9 N10 155.4(4) . . . . ? N11 Rh3 N9 N10 -25.2(3) . . . . ? C30 N9 N10 C32 1.3(5) . . . . ? Rh3 N9 N10 C32 176.4(3) . . . . ? C30 N9 N10 C33 171.7(4) . . . . ? Rh3 N9 N10 C33 -13.3(5) . . . . ? C26 Rh3 N11 C27 33.7(5) . . . . ? N9 Rh3 N11 C27 -146.7(5) . . . . ? C26 Rh3 N11 N12 -153.3(4) . . . . ? N9 Rh3 N11 N12 26.3(3) . . . . ? C27 N11 N12 C29 0.4(5) . . . . ? Rh3 N11 N12 C29 -174.2(3) . . . . ? C27 N11 N12 C33 -175.5(4) . . . . ? Rh3 N11 N12 C33 9.9(5) . . . . ? C40 Rh4 N13 N14 160.5(4) . . . . ? N15 Rh4 N13 N14 -23.9(4) . . . . ? C40 Rh4 N13 C42 -23.6(6) . . . . ? N15 Rh4 N13 C42 152.0(5) . . . . ? C42 N13 N14 C44 1.7(6) . . . . ? Rh4 N13 N14 C44 178.5(3) . . . . ? C42 N13 N14 C48 171.2(4) . . . . ? Rh4 N13 N14 C48 -11.9(6) . . . . ? C41 Rh4 N15 C45 37.0(6) . . . . ? N13 Rh4 N15 C45 -144.8(5) . . . . ? C41 Rh4 N15 N16 -157.7(4) . . . . ? N13 Rh4 N15 N16 20.5(4) . . . . ? C45 N15 N16 C47 -0.4(5) . . . . ? Rh4 N15 N16 C47 -169.2(3) . . . . ? C45 N15 N16 C48 -173.0(4) . . . . ? Rh4 N15 N16 C48 18.1(6) . . . . ? N12 N11 C27 C28 0.7(6) . . . . ? Rh3 N11 C27 C28 174.7(4) . . . . ? N11 C27 C28 C29 -1.5(7) . . . . ? N11 N12 C29 C28 -1.3(5) . . . . ? C33 N12 C29 C28 174.1(4) . . . . ? C27 C28 C29 N12 1.7(6) . . . . ? N10 N9 C30 C31 -1.7(5) . . . . ? Rh3 N9 C30 C31 -176.0(3) . . . . ? N9 C30 C31 C32 1.5(6) . . . . ? N9 N10 C32 C31 -0.5(5) . . . . ? C33 N10 C32 C31 -170.0(4) . . . . ? C30 C31 C32 N10 -0.6(5) . . . . ? C32 N10 C33 N12 -129.3(4) . . . . ? N9 N10 C33 N12 62.3(5) . . . . ? C32 N10 C33 C34 104.6(5) . . . . ? N9 N10 C33 C34 -63.8(5) . . . . ? C29 N12 C33 N10 124.9(5) . . . . ? N11 N12 C33 N10 -60.0(5) . . . . ? C29 N12 C33 C34 -108.0(5) . . . . ? N11 N12 C33 C34 67.0(4) . . . . ? N10 C33 C34 C35 -13.2(5) . . . . ? N12 C33 C34 C35 -139.2(3) . . . . ? N10 C33 C34 C39 171.0(3) . . . . ? N12 C33 C34 C39 45.0(4) . . . . ? C39 C34 C35 C36 -0.9(5) . . . . ? C33 C34 C35 C36 -176.7(3) . . . . ? C34 C35 C36 C37 1.6(6) . . . . ? C35 C36 C37 C38 -0.4(6) . . . . ? C36 C37 C38 C39 -1.6(6) . . . . ? C36 C37 C38 C48 173.6(4) . . . . ? C37 C38 C39 C34 2.3(6) . . . . ? C48 C38 C39 C34 -172.8(3) . . . . ? C35 C34 C39 C38 -1.0(5) . . . . ? C33 C34 C39 C38 174.8(3) . . . . ? N14 N13 C42 C43 -0.8(7) . . . . ? Rh4 N13 C42 C43 -177.2(4) . . . . ? N13 C42 C43 C44 -0.3(8) . . . . ? C42 C43 C44 N14 1.3(7) . . . . ? N13 N14 C44 C43 -1.9(6) . . . . ? C48 N14 C44 C43 -170.8(5) . . . . ? N16 N15 C45 C46 1.2(6) . . . . ? Rh4 N15 C45 C46 168.2(4) . . . . ? N15 C45 C46 C47 -1.5(7) . . . . ? N15 N16 C47 C46 -0.5(6) . . . . ? C48 N16 C47 C46 171.6(4) . . . . ? C45 C46 C47 N16 1.2(6) . . . . ? N13 N14 C48 N16 60.0(5) . . . . ? C44 N14 C48 N16 -132.0(5) . . . . ? N13 N14 C48 C38 -65.1(5) . . . . ? C44 N14 C48 C38 102.9(5) . . . . ? C47 N16 C48 N14 124.7(5) . . . . ? N15 N16 C48 N14 -64.0(5) . . . . ? C47 N16 C48 C38 -109.6(5) . . . . ? N15 N16 C48 C38 61.7(5) . . . . ? C39 C38 C48 N14 -20.8(5) . . . . ? C37 C38 C48 N14 164.1(4) . . . . ? C39 C38 C48 N16 -145.2(4) . . . . ? C37 C38 C48 N16 39.8(5) . . . . ? C121 B3 C113 C114 -55.0(5) . . . . ? C137 B3 C113 C114 66.2(5) . . . . ? C129 B3 C113 C114 -177.5(4) . . . . ? C121 B3 C113 C118 123.8(4) . . . . ? C137 B3 C113 C118 -114.9(4) . . . . ? C129 B3 C113 C118 1.4(5) . . . . ? C118 C113 C114 C115 2.4(6) . . . . ? B3 C113 C114 C115 -178.6(4) . . . . ? C113 C114 C115 C116 -0.8(7) . . . . ? C113 C114 C115 C119 177.6(4) . . . . ? C114 C115 C116 C117 -0.9(7) . . . . ? C119 C115 C116 C117 -179.3(4) . . . . ? C115 C116 C117 C118 0.9(7) . . . . ? C115 C116 C117 C120 -175.1(4) . . . . ? C114 C113 C118 C117 -2.4(6) . . . . ? B3 C113 C118 C117 178.7(4) . . . . ? C116 C117 C118 C113 0.8(6) . . . . ? C120 C117 C118 C113 176.8(4) . . . . ? C116 C115 C119 F51 -137.2(5) . . . . ? C114 C115 C119 F51 44.4(7) . . . . ? C116 C115 C119 F49 -14.5(7) . . . . ? C114 C115 C119 F49 167.1(5) . . . . ? C116 C115 C119 F50 103.4(6) . . . . ? C114 C115 C119 F50 -75.0(6) . . . . ? C116 C117 C120 F54 -149.9(5) . . . . ? C118 C117 C120 F54 34.0(7) . . . . ? C116 C117 C120 F53 87.7(7) . . . . ? C118 C117 C120 F53 -88.4(7) . . . . ? C116 C117 C120 F52 -31.4(7) . . . . ? C118 C117 C120 F52 152.6(5) . . . . ? C113 B3 C121 C126 -57.7(4) . . . . ? C137 B3 C121 C126 -179.1(3) . . . . ? C129 B3 C121 C126 64.1(4) . . . . ? C113 B3 C121 C122 119.3(4) . . . . ? C137 B3 C121 C122 -2.1(5) . . . . ? C129 B3 C121 C122 -118.9(4) . . . . ? C126 C121 C122 C123 -0.6(6) . . . . ? B3 C121 C122 C123 -177.8(4) . . . . ? C121 C122 C123 C124 -0.3(6) . . . . ? C121 C122 C123 C127 177.1(4) . . . . ? C122 C123 C124 C125 0.2(6) . . . . ? C127 C123 C124 C125 -177.2(4) . . . . ? C123 C124 C125 C126 0.8(6) . . . . ? C123 C124 C125 C128 176.8(4) . . . . ? C124 C125 C126 C121 -1.8(6) . . . . ? C128 C125 C126 C121 -177.8(4) . . . . ? C122 C121 C126 C125 1.7(6) . . . . ? B3 C121 C126 C125 178.9(4) . . . . ? C122 C123 C127 F55 -84.3(5) . . . . ? C124 C123 C127 F55 93.2(5) . . . . ? C122 C123 C127 F56 38.4(6) . . . . ? C124 C123 C127 F56 -144.2(5) . . . . ? C122 C123 C127 F57 156.8(4) . . . . ? C124 C123 C127 F57 -25.7(6) . . . . ? C126 C125 C128 F60 -159.8(4) . . . . ? C124 C125 C128 F60 24.2(6) . . . . ? C126 C125 C128 F59 79.4(5) . . . . ? C124 C125 C128 F59 -96.7(5) . . . . ? C126 C125 C128 F58 -39.1(5) . . . . ? C124 C125 C128 F58 144.8(4) . . . . ? C121 B3 C129 C134 -4.3(5) . . . . ? C113 B3 C129 C134 115.1(4) . . . . ? C137 B3 C129 C134 -124.8(4) . . . . ? C121 B3 C129 C130 174.0(3) . . . . ? C113 B3 C129 C130 -66.6(4) . . . . ? C137 B3 C129 C130 53.6(4) . . . . ? C134 C129 C130 C131 -1.0(5) . . . . ? B3 C129 C130 C131 -179.5(3) . . . . ? C129 C130 C131 C132 0.3(6) . . . . ? C129 C130 C131 C135 179.4(3) . . . . ? C130 C131 C132 C133 0.0(5) . . . . ? C135 C131 C132 C133 -179.1(4) . . . . ? C131 C132 C133 C134 0.4(6) . . . . ? C131 C132 C133 C136 177.6(4) . . . . ? C130 C129 C134 C133 1.3(5) . . . . ? B3 C129 C134 C133 179.7(3) . . . . ? C132 C133 C134 C129 -1.1(6) . . . . ? C136 C133 C134 C129 -178.3(4) . . . . ? C130 C131 C135 F61 175.5(4) . . . . ? C132 C131 C135 F61 -5.4(6) . . . . ? C130 C131 C135 F62 -63.1(5) . . . . ? C132 C131 C135 F62 116.0(4) . . . . ? C130 C131 C135 F63 54.4(5) . . . . ? C132 C131 C135 F63 -126.5(4) . . . . ? C132 C133 C136 F66 -77.7(7) . . . . ? C134 C133 C136 F66 99.6(6) . . . . ? C132 C133 C136 F64 153.6(4) . . . . ? C134 C133 C136 F64 -29.1(6) . . . . ? C132 C133 C136 F65 41.9(6) . . . . ? C134 C133 C136 F65 -140.8(4) . . . . ? C121 B3 C137 C138 107.1(4) . . . . ? C113 B3 C137 C138 -11.7(5) . . . . ? C129 B3 C137 C138 -131.7(4) . . . . ? C121 B3 C137 C142 -74.2(4) . . . . ? C113 B3 C137 C142 166.9(4) . . . . ? C129 B3 C137 C142 46.9(4) . . . . ? C142 C137 C138 C139 2.0(6) . . . . ? B3 C137 C138 C139 -179.4(4) . . . . ? C137 C138 C139 C140 -1.4(7) . . . . ? C137 C138 C139 C143 179.1(5) . . . . ? C138 C139 C140 C141 0.1(7) . . . . ? C143 C139 C140 C141 179.6(5) . . . . ? C139 C140 C141 C142 0.5(7) . . . . ? C139 C140 C141 C144 -179.1(4) . . . . ? C140 C141 C142 C137 0.2(7) . . . . ? C144 C141 C142 C137 179.7(4) . . . . ? C138 C137 C142 C141 -1.4(6) . . . . ? B3 C137 C142 C141 179.9(4) . . . . ? C140 C139 C143 F68 102.2(8) . . . . ? C138 C139 C143 F68 -78.3(8) . . . . ? C140 C139 C143 F67 -133.5(6) . . . . ? C138 C139 C143 F67 46.0(8) . . . . ? C140 C139 C143 F69 -19.0(8) . . . . ? C138 C139 C143 F69 160.5(5) . . . . ? C140 C141 C144 F72 58.7(6) . . . . ? C142 C141 C144 F72 -120.8(5) . . . . ? C140 C141 C144 F70 -179.5(4) . . . . ? C142 C141 C144 F70 1.0(7) . . . . ? C140 C141 C144 F71 -60.3(6) . . . . ? C142 C141 C144 F71 120.1(5) . . . . ? C161 B4 C145 C150 -113.6(4) . . . . ? C153 B4 C145 C150 123.8(4) . . . . ? C169 B4 C145 C150 4.1(5) . . . . ? C161 B4 C145 C146 69.6(4) . . . . ? C153 B4 C145 C146 -53.0(4) . . . . ? C169 B4 C145 C146 -172.7(3) . . . . ? C150 C145 C146 C147 2.2(6) . . . . ? B4 C145 C146 C147 179.4(4) . . . . ? C145 C146 C147 C148 -1.0(6) . . . . ? C145 C146 C147 C151 -178.0(4) . . . . ? C146 C147 C148 C149 0.6(7) . . . . ? C151 C147 C148 C149 177.7(5) . . . . ? C147 C148 C149 C150 -1.5(7) . . . . ? C147 C148 C149 C152 -176.3(5) . . . . ? C146 C145 C150 C149 -3.2(6) . . . . ? B4 C145 C150 C149 180.0(4) . . . . ? C148 C149 C150 C145 2.9(7) . . . . ? C152 C149 C150 C145 177.7(5) . . . . ? C148 C147 C151 F75 53.6(7) . . . . ? C146 C147 C151 F75 -129.3(6) . . . . ? C148 C147 C151 F74 -67.1(6) . . . . ? C146 C147 C151 F74 109.9(5) . . . . ? C148 C147 C151 F73 177.5(4) . . . . ? C146 C147 C151 F73 -5.4(7) . . . . ? C148 C149 C152 F78 92.8(7) . . . . ? C150 C149 C152 F78 -82.1(8) . . . . ? C148 C149 C152 F76 -30.7(9) . . . . ? C150 C149 C152 F76 154.4(6) . . . . ? C148 C149 C152 F77 -148.1(5) . . . . ? C150 C149 C152 F77 37.0(7) . . . . ? C161 B4 C153 C158 -170.4(3) . . . . ? C169 B4 C153 C158 68.8(4) . . . . ? C145 B4 C153 C158 -49.5(4) . . . . ? C161 B4 C153 C154 6.6(5) . . . . ? C169 B4 C153 C154 -114.2(4) . . . . ? C145 B4 C153 C154 127.5(4) . . . . ? C158 C153 C154 C155 -2.6(5) . . . . ? B4 C153 C154 C155 -179.7(3) . . . . ? C153 C154 C155 C156 2.0(5) . . . . ? C153 C154 C155 C159 -178.9(3) . . . . ? C154 C155 C156 C157 -0.6(5) . . . . ? C159 C155 C156 C157 -179.8(3) . . . . ? C155 C156 C157 C158 0.1(6) . . . . ? C155 C156 C157 C160 179.8(4) . . . . ? C156 C157 C158 C153 -0.9(6) . . . . ? C160 C157 C158 C153 179.4(4) . . . . ? C154 C153 C158 C157 2.1(5) . . . . ? B4 C153 C158 C157 179.4(3) . . . . ? C156 C155 C159 F79 174.0(3) . . . . ? C154 C155 C159 F79 -5.1(5) . . . . ? C156 C155 C159 F81 -64.9(5) . . . . ? C154 C155 C159 F81 115.9(4) . . . . ? C156 C155 C159 F80 52.9(5) . . . . ? C154 C155 C159 F80 -126.2(4) . . . . ? C158 C157 C160 F82 156.1(4) . . . . ? C156 C157 C160 F82 -23.6(6) . . . . ? C158 C157 C160 F84 35.4(6) . . . . ? C156 C157 C160 F84 -144.3(4) . . . . ? C158 C157 C160 F83 -84.6(5) . . . . ? C156 C157 C160 F83 95.7(5) . . . . ? C153 B4 C161 C166 -61.9(5) . . . . ? C169 B4 C161 C166 61.2(4) . . . . ? C145 B4 C161 C166 -179.8(3) . . . . ? C153 B4 C161 C162 123.0(4) . . . . ? C169 B4 C161 C162 -113.9(4) . . . . ? C145 B4 C161 C162 5.1(5) . . . . ? C166 C161 C162 C163 1.6(5) . . . . ? B4 C161 C162 C163 176.9(4) . . . . ? C161 C162 C163 C164 0.1(6) . . . . ? C161 C162 C163 C167 -177.1(4) . . . . ? C162 C163 C164 C165 -0.3(6) . . . . ? C167 C163 C164 C165 176.9(4) . . . . ? C163 C164 C165 C166 -1.3(6) . . . . ? C163 C164 C165 C168 -178.6(4) . . . . ? C162 C161 C166 C165 -3.2(6) . . . . ? B4 C161 C166 C165 -178.6(4) . . . . ? C164 C165 C166 C161 3.2(6) . . . . ? C168 C165 C166 C161 -179.4(4) . . . . ? C164 C163 C167 F85 146.1(5) . . . . ? C162 C163 C167 F85 -36.7(6) . . . . ? C164 C163 C167 F87 -92.8(5) . . . . ? C162 C163 C167 F87 84.5(5) . . . . ? C164 C163 C167 F86 25.6(6) . . . . ? C162 C163 C167 F86 -157.2(4) . . . . ? C164 C165 C168 F89 -2.8(7) . . . . ? C166 C165 C168 F89 179.8(4) . . . . ? C164 C165 C168 F88 -123.2(5) . . . . ? C166 C165 C168 F88 59.5(6) . . . . ? C164 C165 C168 F90 117.7(5) . . . . ? C166 C165 C168 F90 -59.6(6) . . . . ? C161 B4 C169 C174 -128.4(4) . . . . ? C153 B4 C169 C174 -4.2(5) . . . . ? C145 B4 C169 C174 111.7(4) . . . . ? C161 B4 C169 C170 52.8(5) . . . . ? C153 B4 C169 C170 177.0(3) . . . . ? C145 B4 C169 C170 -67.1(5) . . . . ? C174 C169 C170 C171 -2.4(6) . . . . ? B4 C169 C170 C171 176.4(4) . . . . ? C169 C170 C171 C172 1.4(7) . . . . ? C169 C170 C171 C175 -172.2(8) . . . . ? C169 C170 C171 C178 177.2(6) . . . . ? F93 C175 C171 C172 14.2(14) . . . . ? F91 C175 C171 C172 154.9(10) . . . . ? F92 C175 C171 C172 -97.3(10) . . . . ? F93 C175 C171 C170 -172.0(9) . . . . ? F91 C175 C171 C170 -31.4(15) . . . . ? F92 C175 C171 C170 76.5(13) . . . . ? F93 C175 C171 C178 -107(4) . . . . ? F91 C175 C171 C178 33(3) . . . . ? F92 C175 C171 C178 141(4) . . . . ? F93A C178 C171 C172 64.2(11) . . . . ? F91A C178 C171 C172 -169.2(7) . . . . ? F92A C178 C171 C172 -53.7(10) . . . . ? F93A C178 C171 C170 -111.4(8) . . . . ? F91A C178 C171 C170 15.1(11) . . . . ? F92A C178 C171 C170 130.6(8) . . . . ? F93A C178 C171 C175 128(4) . . . . ? F91A C178 C171 C175 -106(4) . . . . ? F92A C178 C171 C175 10(3) . . . . ? C170 C171 C172 C173 0.1(7) . . . . ? C175 C171 C172 C173 174.1(7) . . . . ? C178 C171 C172 C173 -175.5(6) . . . . ? C171 C172 C173 C174 -0.5(7) . . . . ? C171 C172 C173 C176 -172.2(8) . . . . ? C171 C172 C173 C177 174.1(6) . . . . ? F96 C176 C173 C172 26.8(17) . . . . ? F95 C176 C173 C172 150.3(19) . . . . ? F94 C176 C173 C172 -92.8(10) . . . . ? F96 C176 C173 C174 -145.3(12) . . . . ? F95 C176 C173 C174 -22(2) . . . . ? F94 C176 C173 C174 95.1(11) . . . . ? F96 C176 C173 C177 132(5) . . . . ? F95 C176 C173 C177 -105(4) . . . . ? F94 C176 C173 C177 12(3) . . . . ? F96A C177 C173 C172 -2.9(11) . . . . ? F95A C177 C173 C172 120.6(12) . . . . ? F94A C177 C173 C172 -127.7(8) . . . . ? F96A C177 C173 C174 172.0(7) . . . . ? F95A C177 C173 C174 -64.5(12) . . . . ? F94A C177 C173 C174 47.2(10) . . . . ? F96A C177 C173 C176 -85(4) . . . . ? F95A C177 C173 C176 38(4) . . . . ? F94A C177 C173 C176 150(4) . . . . ? C170 C169 C174 C173 2.0(6) . . . . ? B4 C169 C174 C173 -176.7(4) . . . . ? C172 C173 C174 C169 -0.7(7) . . . . ? C176 C173 C174 C169 171.2(7) . . . . ? C177 C173 C174 C169 -175.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.962 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.068 #===END data_compound15 _database_code_depnum_ccdc_archive 'CCDC 798125' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C28 H30 Ir N8' _chemical_formula_sum 'C60 H42 B F24 Ir N8' _chemical_formula_weight 1534.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2724(4) _cell_length_b 25.0291(7) _cell_length_c 19.2865(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.4760(10) _cell_angle_gamma 90.00 _cell_volume 6076.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9798 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.41 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5494 _exptl_absorpt_correction_T_max 0.7375 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53760 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12893 _reflns_number_gt 10498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; This structure bears four disordered CF3 groups (over two sites each), i.e., C35 F4 F5 F6; C43 F7 F8 F9; C52 F16 F17 F18; C59 F19 F20 F21. The following restrains were used in the refinement: isor 0.01 f6 sadi 0.001 c35 f6 c35 f6a sadi 0.001 c35 f5 c35 f5a sadi 0.001 c35 f4 c35 f4a sadi 0.001 c43 f9 c43 f9a sadi 0.001 c43 f8 c43 f8a sadi 0.001 c43 f7 c43 f7a sadi 0.001 c52 f18 c52 f18a sadi 0.001 c52 f17 c52 f17a sadi 0.001 c52 f16 c52 f16a sadi 0.001 c59 f21 c59a f21a sadi 0.001 c59 f20 c59a f20a sadi 0.001 c59 f19 c59a f19a 'same c59 f19 f20 f21' for the second site Furthermore, same anisotropic displacement parameters were refined for corresponding atoms (corresponding F-atoms are opposite to each other): eadp f21 f21a eadp f20 f20a eadp f19 f19a eadp f16 f16a eadp f17 f17a eadp f18 f18a eadp f6 f6a eadp f5 f5a eadp f4 f4a eadp f7 f7a eadp f8 f8a eadp f9 f9a eadp c59 c59a exyz c59 c59a 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^)+(0.0486P)^2^+35.3959P] 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 12893 _refine_ls_number_parameters 883 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.397759(16) 0.567997(8) 0.734723(12) 0.02392(8) Uani 1 1 d . . . N1 N 0.3584(3) 0.62954(18) 0.6568(3) 0.0243(10) Uani 1 1 d . . . N2 N 0.4034(4) 0.63101(17) 0.6023(3) 0.0244(10) Uani 1 1 d . . . N3 N 0.5458(4) 0.56862(18) 0.7207(3) 0.0254(9) Uani 1 1 d . . . N4 N 0.5571(4) 0.57839(17) 0.6551(3) 0.0227(9) Uani 1 1 d . . . N5 N 0.3887(4) 0.3462(2) 0.4814(3) 0.0353(12) Uani 1 1 d . . . N6 N 0.3786(4) 0.34292(18) 0.5490(2) 0.0252(10) Uani 1 1 d . . . N7 N 0.5958(4) 0.3959(2) 0.5901(3) 0.0345(12) Uani 1 1 d . . . N8 N 0.5336(4) 0.38420(18) 0.6317(2) 0.0258(10) Uani 1 1 d . . . C1 C 0.2623(4) 0.5786(2) 0.7693(4) 0.0316(13) Uani 1 1 d . . . H1 H 0.2295 0.6149 0.7590 0.038 Uiso 1 1 calc R . . C2 C 0.2384(5) 0.5451(3) 0.7084(3) 0.0310(13) Uani 1 1 d . . . H2 H 0.1908 0.5617 0.6625 0.037 Uiso 1 1 calc R . . C3 C 0.2282(5) 0.4850(3) 0.7114(4) 0.0392(15) Uani 1 1 d . . . H3A H 0.1613 0.4762 0.7213 0.047 Uiso 1 1 calc R . . H3B H 0.2235 0.4699 0.6630 0.047 Uiso 1 1 calc R . . C4 C 0.3195(5) 0.4589(2) 0.7688(4) 0.0378(15) Uani 1 1 d . . . H4A H 0.3294 0.4221 0.7530 0.045 Uiso 1 1 calc R . . H4B H 0.3026 0.4564 0.8151 0.045 Uiso 1 1 calc R . . C5 C 0.4222(5) 0.4904(2) 0.7817(3) 0.0295(12) Uani 1 1 d . . . H5 H 0.4811 0.4699 0.7721 0.035 Uiso 1 1 calc R . . C6 C 0.4565(5) 0.5295(2) 0.8375(3) 0.0294(12) Uani 1 1 d . . . H6 H 0.5354 0.5317 0.8600 0.035 Uiso 1 1 calc R . . C7 C 0.3958(5) 0.5468(3) 0.8878(3) 0.0362(14) Uani 1 1 d . . . H7A H 0.4299 0.5790 0.9149 0.043 Uiso 1 1 calc R . . H7B H 0.3998 0.5181 0.9239 0.043 Uiso 1 1 calc R . . C8 C 0.2798(5) 0.5590(2) 0.8475(3) 0.0321(13) Uani 1 1 d . . . H8A H 0.2545 0.5866 0.8747 0.039 Uiso 1 1 calc R . . H8B H 0.2370 0.5263 0.8458 0.039 Uiso 1 1 calc R . . C9 C 0.3035(5) 0.6745(2) 0.6506(3) 0.0318(13) Uani 1 1 d . . . H9 H 0.2643 0.6849 0.6819 0.038 Uiso 1 1 calc R . . C10 C 0.3116(5) 0.7048(2) 0.5912(4) 0.0408(15) Uani 1 1 d . . . H10 H 0.2793 0.7383 0.5747 0.049 Uiso 1 1 calc R . . C11 C 0.3756(5) 0.6758(2) 0.5622(3) 0.0330(13) Uani 1 1 d . . . H11 H 0.3967 0.6855 0.5212 0.040 Uiso 1 1 calc R . . C12 C 0.6463(5) 0.5632(3) 0.7667(4) 0.0406(15) Uani 1 1 d . . . H12 H 0.6646 0.5563 0.8176 0.049 Uiso 1 1 calc R . . C13 C 0.7180(5) 0.5691(4) 0.7291(4) 0.056(2) Uani 1 1 d . . . H13 H 0.7932 0.5672 0.7487 0.067 Uiso 1 1 calc R . . C14 C 0.6594(5) 0.5781(3) 0.6584(4) 0.0368(14) Uani 1 1 d . . . H14 H 0.6861 0.5834 0.6186 0.044 Uiso 1 1 calc R . . C15 C 0.4649(4) 0.5851(2) 0.5901(3) 0.0263(12) Uani 1 1 d . . . H15 H 0.4904 0.5935 0.5478 0.032 Uiso 1 1 calc R . . C16 C 0.3956(4) 0.5356(2) 0.5716(3) 0.0250(11) Uani 1 1 d . . . C17 C 0.4392(4) 0.4846(2) 0.5928(3) 0.0231(11) Uani 1 1 d . . . H17 H 0.5116 0.4812 0.6217 0.028 Uiso 1 1 calc R . . C18 C 0.3765(4) 0.4395(2) 0.5714(3) 0.0253(11) Uani 1 1 d . . . C19 C 0.2704(5) 0.4447(2) 0.5287(3) 0.0323(13) Uani 1 1 d . . . H19 H 0.2272 0.4138 0.5141 0.039 Uiso 1 1 calc R . . C20 C 0.2285(5) 0.4944(3) 0.5076(4) 0.0377(15) Uani 1 1 d . . . H20 H 0.1562 0.4977 0.4783 0.045 Uiso 1 1 calc R . . C21 C 0.2897(5) 0.5399(2) 0.5282(4) 0.0344(14) Uani 1 1 d . . . H21 H 0.2597 0.5741 0.5129 0.041 Uiso 1 1 calc R . . C22 C 0.3434(6) 0.3011(3) 0.4495(4) 0.0457(17) Uani 1 1 d . . . H22 H 0.3404 0.2909 0.4014 0.055 Uiso 1 1 calc R . . C23 C 0.3025(7) 0.2716(3) 0.4924(5) 0.057(2) Uani 1 1 d . . . H23 H 0.2642 0.2391 0.4801 0.068 Uiso 1 1 calc R . . C24 C 0.3272(6) 0.2981(3) 0.5566(4) 0.0451(17) Uani 1 1 d . . . H24 H 0.3113 0.2872 0.5992 0.054 Uiso 1 1 calc R . . C25 C 0.6934(6) 0.3962(3) 0.6380(4) 0.0479(17) Uani 1 1 d . . . H25 H 0.7557 0.4030 0.6252 0.058 Uiso 1 1 calc R . . C26 C 0.6939(6) 0.3856(3) 0.7083(4) 0.054(2) Uani 1 1 d . . . H26 H 0.7537 0.3840 0.7514 0.065 Uiso 1 1 calc R . . C27 C 0.5901(6) 0.3778(3) 0.7026(3) 0.0400(15) Uani 1 1 d . . . H27 H 0.5628 0.3694 0.7413 0.048 Uiso 1 1 calc R . . C28 C 0.4191(5) 0.3848(2) 0.6020(3) 0.0247(11) Uani 1 1 d . . . H28 H 0.3915 0.3775 0.6437 0.030 Uiso 1 1 calc R . . B1 B 0.0184(5) 0.6749(2) 0.9087(3) 0.0177(11) Uani 1 1 d . . . F1 F -0.1209(3) 0.6286(2) 0.6141(2) 0.0565(12) Uani 1 1 d . . . F2 F 0.0463(3) 0.64221(17) 0.6437(2) 0.0460(10) Uani 1 1 d . . . F3 F -0.0168(3) 0.56371(16) 0.6103(2) 0.0471(10) Uani 1 1 d . . . F4 F 0.0179(8) 0.4666(2) 0.9155(4) 0.071(3) Uani 0.71 1 d PD A 1 F5 F 0.0619(9) 0.4454(3) 0.8220(6) 0.093(3) Uani 0.71 1 d PD A 1 F6 F -0.0981(8) 0.4518(4) 0.8204(7) 0.107(3) Uani 0.71 1 d PDU A 1 F4A F -0.018(3) 0.4363(5) 0.8043(9) 0.071(3) Uani 0.29 1 d PD A 2 F5A F -0.0993(18) 0.4658(7) 0.8679(16) 0.093(3) Uani 0.29 1 d PD A 2 F6A F 0.065(2) 0.4700(11) 0.9093(12) 0.107(3) Uani 0.29 1 d PD A 2 F7 F 0.4367(13) 0.5748(6) 1.0633(5) 0.136(5) Uani 0.74 1 d PD B 1 F8 F 0.3302(5) 0.5903(4) 1.1195(4) 0.075(2) Uani 0.74 1 d PD B 1 F9 F 0.4560(9) 0.6387(5) 1.1304(5) 0.103(3) Uani 0.74 1 d PD B 1 F7A F 0.370(4) 0.6372(15) 1.1397(9) 0.136(5) Uani 0.26 1 d PD B 2 F8A F 0.4814(10) 0.6150(15) 1.0934(17) 0.075(2) Uani 0.26 1 d PD B 2 F9A F 0.349(2) 0.5639(8) 1.0730(15) 0.103(3) Uani 0.26 1 d PD B 2 F10 F 0.4447(4) 0.6980(2) 0.8577(3) 0.0796(17) Uani 1 1 d . . . F11 F 0.4208(4) 0.77252(18) 0.9032(3) 0.0654(14) Uani 1 1 d . . . F12 F 0.3083(3) 0.7437(2) 0.8058(2) 0.0603(12) Uani 1 1 d . . . F13 F -0.3434(3) 0.73350(16) 0.7294(2) 0.0504(10) Uani 1 1 d . . . F14 F -0.3657(3) 0.81416(19) 0.7596(2) 0.0548(12) Uani 1 1 d . . . F15 F -0.2956(3) 0.7990(2) 0.6770(2) 0.0564(12) Uani 1 1 d . . . F16 F 0.0317(6) 0.9101(2) 0.8597(3) 0.0735(17) Uani 0.92 1 d PD C 1 F17 F -0.0558(4) 0.9107(2) 0.9331(4) 0.0579(13) Uani 0.92 1 d PD C 1 F18 F 0.0951(4) 0.87440(18) 0.9643(4) 0.083(2) Uani 0.92 1 d PD C 1 F16A F -0.003(7) 0.890(2) 0.974(2) 0.0735(17) Uani 0.08 1 d PD C 2 F17A F 0.102(3) 0.886(2) 0.900(4) 0.0579(13) Uani 0.08 1 d PD C 2 F18A F -0.044(5) 0.9234(13) 0.878(5) 0.083(2) Uani 0.08 1 d PD C 2 C59 C -0.2803(5) 0.6028(3) 1.0002(4) 0.0457(17) Uani 0.84 1 d PD D 1 F19 F -0.3124(6) 0.5958(4) 1.0565(3) 0.093(3) Uani 0.84 1 d PD D 1 F20 F -0.2768(5) 0.5545(2) 0.9705(4) 0.0682(17) Uani 0.84 1 d PD D 1 F21 F -0.3571(5) 0.6269(3) 0.9493(4) 0.080(3) Uani 0.84 1 d PD D 1 C59A C -0.2803(5) 0.6028(3) 1.0002(4) 0.0457(17) Uani 0.16 1 d PD D 2 F19A F -0.348(2) 0.6097(18) 0.9355(11) 0.093(3) Uani 0.16 1 d PD D 2 F20A F -0.331(3) 0.6254(11) 1.0432(18) 0.0682(17) Uani 0.16 1 d PD D 2 F21A F -0.267(2) 0.5520(7) 1.019(2) 0.080(3) Uani 0.16 1 d PD D 2 F22 F 0.0313(6) 0.6748(2) 1.2255(2) 0.087(2) Uani 1 1 d . . . F23 F -0.0510(4) 0.7450(2) 1.1846(3) 0.0723(15) Uani 1 1 d . . . F24 F 0.1019(4) 0.7344(2) 1.1767(2) 0.0716(15) Uani 1 1 d . . . C29 C -0.0038(4) 0.6263(2) 0.8495(3) 0.0197(10) Uani 1 1 d . . . C30 C -0.0030(4) 0.5725(2) 0.8704(3) 0.0233(11) Uani 1 1 d . . . H30 H 0.0012 0.5640 0.9192 0.028 Uiso 1 1 calc R . . C31 C -0.0083(4) 0.5313(2) 0.8209(3) 0.0296(13) Uani 1 1 d . . . C32 C -0.0154(4) 0.5413(2) 0.7487(3) 0.0290(12) Uani 1 1 d . . . H32 H -0.0194 0.5129 0.7153 0.035 Uiso 1 1 calc R . . C33 C -0.0162(4) 0.5936(2) 0.7272(3) 0.0259(12) Uani 1 1 d . . . C34 C -0.0101(4) 0.6350(2) 0.7758(3) 0.0214(10) Uani 1 1 d . . . H34 H -0.0102 0.6707 0.7590 0.026 Uiso 1 1 calc R . . C35 C -0.0083(6) 0.4743(3) 0.8481(3) 0.0492(19) Uani 1 1 d . . . C36 C -0.0260(5) 0.6072(3) 0.6494(3) 0.0373(15) Uani 1 1 d . . . C37 C 0.1484(4) 0.67779(19) 0.9377(3) 0.0184(10) Uani 1 1 d . . . C38 C 0.2108(4) 0.6476(2) 0.9986(3) 0.0223(11) Uani 1 1 d . . . H38 H 0.1764 0.6281 1.0269 0.027 Uiso 1 1 calc R . . C39 C 0.3201(5) 0.6458(2) 1.0178(3) 0.0272(12) Uani 1 1 d . . . C40 C 0.3738(4) 0.6726(2) 0.9775(3) 0.0263(12) Uani 1 1 d . . . H40 H 0.4491 0.6714 0.9910 0.032 Uiso 1 1 calc R . . C41 C 0.3147(4) 0.7012(2) 0.9170(3) 0.0251(11) Uani 1 1 d . . . C42 C 0.2046(4) 0.7036(2) 0.8982(3) 0.0212(10) Uani 1 1 d . . . H42 H 0.1664 0.7239 0.8565 0.025 Uiso 1 1 calc R . . C43 C 0.3818(5) 0.6128(3) 1.0822(4) 0.0457(17) Uani 1 1 d . . . C44 C 0.3717(5) 0.7290(2) 0.8711(3) 0.0315(13) Uani 1 1 d . . . C45 C -0.0370(4) 0.7312(2) 0.8733(3) 0.0196(10) Uani 1 1 d . . . C46 C -0.1376(4) 0.7329(2) 0.8218(3) 0.0191(10) Uani 1 1 d . . . H46 H -0.1716 0.7003 0.8023 0.023 Uiso 1 1 calc R . . C47 C -0.1903(4) 0.7810(2) 0.7979(3) 0.0224(11) Uani 1 1 d . . . C48 C -0.1433(4) 0.8291(2) 0.8256(3) 0.0257(12) Uani 1 1 d . . . H48 H -0.1788 0.8619 0.8091 0.031 Uiso 1 1 calc R . . C49 C -0.0446(4) 0.8286(2) 0.8772(3) 0.0261(12) Uani 1 1 d . . . C50 C 0.0083(4) 0.7800(2) 0.9011(3) 0.0206(10) Uani 1 1 d . . . H50 H 0.0765 0.7805 0.9370 0.025 Uiso 1 1 calc R . . C51 C -0.2968(5) 0.7812(2) 0.7411(3) 0.0297(13) Uani 1 1 d . . . C52 C 0.0076(5) 0.8802(2) 0.9088(4) 0.0376(15) Uani 1 1 d . . . C53 C -0.0329(4) 0.6637(2) 0.9743(3) 0.0191(10) Uani 1 1 d . . . C54 C -0.1286(4) 0.6370(2) 0.9630(3) 0.0227(11) Uani 1 1 d . . . H54 H -0.1623 0.6211 0.9166 0.027 Uiso 1 1 calc R . . C55 C -0.1765(4) 0.6327(2) 1.0171(3) 0.0256(11) Uani 1 1 d . . . C56 C -0.1304(5) 0.6550(2) 1.0854(3) 0.0281(12) Uani 1 1 d . . . H56 H -0.1624 0.6514 1.1228 0.034 Uiso 1 1 calc R . . C57 C -0.0364(5) 0.6829(2) 1.0976(3) 0.0247(11) Uani 1 1 d . . . C58 C 0.0116(4) 0.6874(2) 1.0437(3) 0.0222(11) Uani 1 1 d . . . H58 H 0.0761 0.7069 1.0537 0.027 Uiso 1 1 calc R . . C60 C 0.0140(6) 0.7087(3) 1.1706(3) 0.0389(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02086(11) 0.02322(11) 0.02802(12) 0.00184(9) 0.00823(8) 0.00011(9) N1 0.020(2) 0.022(2) 0.030(2) 0.0019(19) 0.0074(19) 0.0024(18) N2 0.026(2) 0.018(2) 0.031(2) 0.0017(18) 0.012(2) 0.0018(18) N3 0.023(2) 0.026(2) 0.027(2) 0.001(2) 0.0082(19) -0.0027(19) N4 0.021(2) 0.019(2) 0.029(2) 0.0026(18) 0.0100(19) -0.0003(17) N5 0.042(3) 0.039(3) 0.027(3) -0.006(2) 0.013(2) -0.009(2) N6 0.033(3) 0.021(2) 0.024(2) -0.0001(18) 0.012(2) -0.0044(19) N7 0.030(3) 0.038(3) 0.037(3) -0.004(2) 0.012(2) -0.001(2) N8 0.031(3) 0.023(2) 0.022(2) -0.0024(18) 0.007(2) 0.0036(19) C1 0.021(3) 0.031(3) 0.047(4) 0.000(3) 0.015(3) 0.005(2) C2 0.021(3) 0.041(3) 0.034(3) 0.002(3) 0.012(2) -0.003(2) C3 0.037(3) 0.040(4) 0.046(4) -0.019(3) 0.021(3) -0.018(3) C4 0.047(4) 0.018(3) 0.049(4) -0.003(3) 0.017(3) -0.010(3) C5 0.034(3) 0.024(3) 0.035(3) 0.007(2) 0.017(3) 0.004(2) C6 0.028(3) 0.028(3) 0.032(3) 0.005(2) 0.009(2) 0.001(2) C7 0.044(4) 0.038(3) 0.031(3) -0.008(3) 0.017(3) -0.006(3) C8 0.038(3) 0.032(3) 0.033(3) -0.008(2) 0.020(3) 0.000(3) C9 0.034(3) 0.029(3) 0.034(3) -0.002(2) 0.012(3) 0.006(2) C10 0.044(4) 0.023(3) 0.054(4) 0.014(3) 0.013(3) 0.009(3) C11 0.038(3) 0.027(3) 0.034(3) 0.004(2) 0.012(3) 0.001(3) C12 0.027(3) 0.060(4) 0.030(3) 0.010(3) 0.004(3) -0.002(3) C13 0.023(3) 0.096(6) 0.048(4) 0.022(4) 0.009(3) 0.003(4) C14 0.023(3) 0.047(4) 0.044(4) 0.006(3) 0.016(3) 0.001(3) C15 0.025(3) 0.020(3) 0.030(3) 0.003(2) 0.004(2) 0.001(2) C16 0.023(3) 0.023(3) 0.029(3) -0.002(2) 0.008(2) 0.000(2) C17 0.024(3) 0.025(3) 0.021(3) -0.001(2) 0.008(2) 0.002(2) C18 0.025(3) 0.026(3) 0.024(3) -0.003(2) 0.008(2) -0.001(2) C19 0.027(3) 0.031(3) 0.036(3) -0.005(2) 0.005(3) -0.004(2) C20 0.022(3) 0.035(3) 0.045(4) -0.004(3) -0.005(3) 0.001(2) C21 0.029(3) 0.026(3) 0.042(4) 0.002(3) 0.003(3) 0.006(2) C22 0.053(4) 0.047(4) 0.031(3) -0.017(3) 0.005(3) -0.004(3) C23 0.071(5) 0.034(4) 0.060(5) -0.012(3) 0.012(4) -0.026(4) C24 0.063(5) 0.034(3) 0.044(4) 0.003(3) 0.024(3) -0.018(3) C25 0.032(4) 0.051(4) 0.057(5) -0.006(4) 0.009(3) 0.000(3) C26 0.048(4) 0.057(5) 0.040(4) -0.003(4) -0.010(3) -0.001(4) C27 0.053(4) 0.034(3) 0.026(3) 0.002(3) 0.002(3) 0.005(3) C28 0.033(3) 0.020(3) 0.022(3) -0.001(2) 0.011(2) -0.001(2) B1 0.021(3) 0.015(3) 0.016(3) 0.002(2) 0.005(2) 0.001(2) F1 0.041(2) 0.094(3) 0.028(2) 0.000(2) 0.0015(17) 0.022(2) F2 0.055(2) 0.056(2) 0.0303(19) -0.0029(17) 0.0183(18) -0.009(2) F3 0.051(2) 0.054(2) 0.037(2) -0.0258(18) 0.0153(18) -0.0044(19) F4 0.149(8) 0.010(2) 0.062(4) 0.005(2) 0.045(5) 0.002(4) F5 0.154(8) 0.025(3) 0.138(8) 0.023(4) 0.100(7) 0.033(4) F6 0.098(6) 0.046(4) 0.143(7) 0.029(4) -0.012(5) -0.035(4) F4A 0.149(8) 0.010(2) 0.062(4) 0.005(2) 0.045(5) 0.002(4) F5A 0.154(8) 0.025(3) 0.138(8) 0.023(4) 0.100(7) 0.033(4) F6A 0.098(6) 0.046(4) 0.143(7) 0.029(4) -0.012(5) -0.035(4) F7 0.198(11) 0.160(10) 0.058(5) 0.060(6) 0.052(7) 0.148(9) F8 0.042(3) 0.121(6) 0.055(4) 0.065(4) 0.004(3) 0.012(4) F9 0.082(6) 0.138(8) 0.050(4) 0.036(5) -0.036(4) -0.043(6) F7A 0.198(11) 0.160(10) 0.058(5) 0.060(6) 0.052(7) 0.148(9) F8A 0.042(3) 0.121(6) 0.055(4) 0.065(4) 0.004(3) 0.012(4) F9A 0.082(6) 0.138(8) 0.050(4) 0.036(5) -0.036(4) -0.043(6) F10 0.087(4) 0.063(3) 0.126(5) 0.028(3) 0.087(4) 0.024(3) F11 0.084(3) 0.055(3) 0.063(3) -0.012(2) 0.030(3) -0.046(3) F12 0.050(3) 0.090(3) 0.044(2) 0.017(2) 0.020(2) -0.018(2) F13 0.033(2) 0.043(2) 0.057(3) 0.0002(19) -0.0103(18) -0.0008(17) F14 0.032(2) 0.072(3) 0.050(2) -0.022(2) -0.0005(18) 0.026(2) F15 0.047(2) 0.091(3) 0.0259(19) 0.018(2) 0.0046(17) 0.004(2) F16 0.102(5) 0.033(3) 0.099(4) -0.005(3) 0.052(4) -0.028(3) F17 0.053(3) 0.036(2) 0.089(4) -0.033(3) 0.029(3) -0.005(2) F18 0.052(3) 0.024(2) 0.126(5) -0.011(3) -0.036(3) -0.005(2) F16A 0.102(5) 0.033(3) 0.099(4) -0.005(3) 0.052(4) -0.028(3) F17A 0.053(3) 0.036(2) 0.089(4) -0.033(3) 0.029(3) -0.005(2) F18A 0.052(3) 0.024(2) 0.126(5) -0.011(3) -0.036(3) -0.005(2) C59 0.031(3) 0.064(5) 0.046(4) 0.004(4) 0.017(3) -0.008(3) F19 0.093(5) 0.145(7) 0.062(4) -0.026(4) 0.055(4) -0.083(5) F20 0.054(3) 0.049(3) 0.103(5) -0.021(3) 0.027(4) -0.032(3) F21 0.028(3) 0.076(5) 0.114(6) 0.021(4) -0.007(3) -0.011(3) C59A 0.031(3) 0.064(5) 0.046(4) 0.004(4) 0.017(3) -0.008(3) F19A 0.093(5) 0.145(7) 0.062(4) -0.026(4) 0.055(4) -0.083(5) F20A 0.054(3) 0.049(3) 0.103(5) -0.021(3) 0.027(4) -0.032(3) F21A 0.028(3) 0.076(5) 0.114(6) 0.021(4) -0.007(3) -0.011(3) F22 0.171(6) 0.059(3) 0.018(2) -0.001(2) 0.012(3) -0.017(3) F23 0.090(4) 0.061(3) 0.074(3) -0.041(3) 0.038(3) -0.005(3) F24 0.065(3) 0.111(4) 0.043(2) -0.039(3) 0.023(2) -0.042(3) C29 0.017(2) 0.016(2) 0.024(3) -0.001(2) 0.004(2) 0.0014(19) C30 0.021(3) 0.017(2) 0.027(3) 0.005(2) 0.001(2) 0.001(2) C31 0.022(3) 0.017(3) 0.046(4) -0.005(2) 0.005(2) 0.004(2) C32 0.025(3) 0.026(3) 0.031(3) -0.011(2) 0.003(2) 0.003(2) C33 0.018(3) 0.033(3) 0.026(3) -0.008(2) 0.007(2) 0.002(2) C34 0.018(2) 0.022(3) 0.022(3) -0.002(2) 0.005(2) 0.000(2) C35 0.060(5) 0.021(3) 0.056(5) 0.002(3) 0.002(4) 0.004(3) C36 0.027(3) 0.059(4) 0.024(3) -0.020(3) 0.007(2) 0.000(3) C37 0.021(2) 0.012(2) 0.021(3) -0.0034(19) 0.006(2) -0.0002(18) C38 0.028(3) 0.021(3) 0.017(2) -0.001(2) 0.006(2) 0.002(2) C39 0.028(3) 0.031(3) 0.019(3) -0.001(2) 0.003(2) 0.005(2) C40 0.018(3) 0.030(3) 0.027(3) -0.008(2) 0.002(2) -0.003(2) C41 0.028(3) 0.018(2) 0.031(3) -0.005(2) 0.011(2) -0.004(2) C42 0.025(3) 0.014(2) 0.023(3) -0.002(2) 0.006(2) 0.000(2) C43 0.030(3) 0.071(5) 0.034(4) 0.010(3) 0.006(3) 0.013(3) C44 0.027(3) 0.030(3) 0.040(3) 0.000(3) 0.014(3) -0.004(2) C45 0.024(3) 0.019(2) 0.018(2) 0.0006(19) 0.010(2) 0.002(2) C46 0.024(3) 0.016(2) 0.019(2) -0.0002(19) 0.010(2) 0.0030(19) C47 0.022(3) 0.026(3) 0.024(3) 0.004(2) 0.013(2) 0.004(2) C48 0.028(3) 0.019(3) 0.033(3) 0.002(2) 0.015(2) 0.007(2) C49 0.027(3) 0.019(3) 0.035(3) 0.002(2) 0.013(2) 0.001(2) C50 0.021(3) 0.019(2) 0.024(3) 0.000(2) 0.009(2) 0.002(2) C51 0.026(3) 0.031(3) 0.033(3) -0.002(2) 0.011(2) 0.009(2) C52 0.026(3) 0.019(3) 0.067(5) 0.000(3) 0.014(3) 0.000(2) C53 0.022(3) 0.018(2) 0.018(2) 0.0028(19) 0.007(2) 0.0033(19) C54 0.025(3) 0.020(2) 0.020(3) 0.001(2) 0.002(2) -0.001(2) C55 0.023(3) 0.022(3) 0.033(3) 0.005(2) 0.010(2) -0.001(2) C56 0.032(3) 0.028(3) 0.029(3) 0.006(2) 0.017(2) 0.010(2) C57 0.033(3) 0.020(3) 0.022(3) -0.002(2) 0.010(2) 0.003(2) C58 0.027(3) 0.017(2) 0.023(3) -0.002(2) 0.008(2) -0.003(2) C60 0.055(4) 0.039(4) 0.029(3) -0.010(3) 0.022(3) -0.005(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 N3 2.066(5) . ? Ir1 C2 2.092(6) . ? Ir1 N1 2.100(4) . ? Ir1 C6 2.118(6) . ? Ir1 C1 2.123(6) . ? Ir1 C5 2.124(6) . ? N1 C9 1.326(7) . ? N1 N2 1.363(6) . ? N2 C11 1.346(7) . ? N2 C15 1.471(7) . ? N3 N4 1.344(6) . ? N3 C12 1.354(8) . ? N4 C14 1.339(7) . ? N4 C15 1.458(7) . ? N5 C22 1.334(8) . ? N5 N6 1.354(7) . ? N6 C24 1.345(8) . ? N6 C28 1.445(7) . ? N7 C25 1.331(9) . ? N7 N8 1.352(7) . ? N8 C27 1.346(8) . ? N8 C28 1.443(7) . ? C1 C2 1.395(9) . ? C1 C8 1.531(9) . ? C1 H1 1.0000 . ? C2 C3 1.514(9) . ? C2 H2 1.0000 . ? C3 C4 1.506(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.526(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.420(8) . ? C5 H5 1.0000 . ? C6 C7 1.506(8) . ? C6 H6 1.0000 . ? C7 C8 1.520(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.406(9) . ? C9 H9 0.9500 . ? C10 C11 1.365(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.374(10) . ? C12 H12 0.9500 . ? C13 C14 1.359(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.518(8) . ? C15 H15 1.0000 . ? C16 C21 1.394(8) . ? C16 C17 1.405(7) . ? C17 C18 1.386(8) . ? C17 H17 0.9500 . ? C18 C19 1.394(8) . ? C18 C28 1.527(7) . ? C19 C20 1.372(9) . ? C19 H19 0.9500 . ? C20 C21 1.382(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.346(11) . ? C22 H22 0.9500 . ? C23 C24 1.350(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.381(11) . ? C25 H25 0.9500 . ? C26 C27 1.361(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28 1.0000 . ? B1 C29 1.631(7) . ? B1 C45 1.635(7) . ? B1 C37 1.638(8) . ? B1 C53 1.639(7) . ? F1 C36 1.341(7) . ? F2 C36 1.330(8) . ? F3 C36 1.350(7) . ? F4 C35 1.249(8) . ? F5 C35 1.393(9) . ? F6 C35 1.272(11) . ? F4A C35 1.249(8) . ? F5A C35 1.393(9) . ? F6A C35 1.273(11) . ? F7 C43 1.319(10) . ? F8 C43 1.272(8) . ? F9 C43 1.293(10) . ? F7A C43 1.319(10) . ? F8A C43 1.272(8) . ? F9A C43 1.293(10) . ? F10 C44 1.330(7) . ? F11 C44 1.319(7) . ? F12 C44 1.326(7) . ? F13 C51 1.331(7) . ? F14 C51 1.361(6) . ? F15 C51 1.319(7) . ? F16 C52 1.323(8) . ? F17 C52 1.326(8) . ? F18 C52 1.315(8) . ? F16A C52 1.323(9) . ? F17A C52 1.326(8) . ? F18A C52 1.315(8) . ? C59 F19 1.299(9) . ? C59 F21 1.317(9) . ? C59 F20 1.344(9) . ? C59 C55 1.510(8) . ? F22 C60 1.318(8) . ? F23 C60 1.337(8) . ? F24 C60 1.306(8) . ? C29 C30 1.405(7) . ? C29 C34 1.414(7) . ? C30 C31 1.391(8) . ? C30 H30 0.9500 . ? C31 C32 1.388(9) . ? C31 C35 1.521(9) . ? C32 C33 1.372(8) . ? C32 H32 0.9500 . ? C33 C34 1.382(7) . ? C33 C36 1.504(8) . ? C34 H34 0.9500 . ? C37 C42 1.386(7) . ? C37 C38 1.421(7) . ? C38 C39 1.379(8) . ? C38 H38 0.9500 . ? C39 C40 1.382(8) . ? C39 C43 1.500(8) . ? C40 C41 1.382(8) . ? C40 H40 0.9500 . ? C41 C42 1.390(7) . ? C41 C44 1.504(8) . ? C42 H42 0.9500 . ? C45 C46 1.389(7) . ? C45 C50 1.393(7) . ? C46 C47 1.394(7) . ? C46 H46 0.9500 . ? C47 C48 1.384(8) . ? C47 C51 1.489(8) . ? C48 C49 1.371(8) . ? C48 H48 0.9500 . ? C49 C50 1.408(7) . ? C49 C52 1.500(8) . ? C50 H50 0.9500 . ? C53 C54 1.389(7) . ? C53 C58 1.412(7) . ? C54 C55 1.389(8) . ? C54 H54 0.9500 . ? C55 C56 1.382(8) . ? C56 C57 1.384(8) . ? C56 H56 0.9500 . ? C57 C58 1.384(7) . ? C57 C60 1.500(8) . ? C58 H58 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ir1 C2 154.2(2) . . ? N3 Ir1 N1 86.10(18) . . ? C2 Ir1 N1 91.4(2) . . ? N3 Ir1 C6 92.4(2) . . ? C2 Ir1 C6 98.4(2) . . ? N1 Ir1 C6 159.7(2) . . ? N3 Ir1 C1 167.1(2) . . ? C2 Ir1 C1 38.7(2) . . ? N1 Ir1 C1 95.2(2) . . ? C6 Ir1 C1 81.9(2) . . ? N3 Ir1 C5 92.3(2) . . ? C2 Ir1 C5 81.9(2) . . ? N1 Ir1 C5 161.1(2) . . ? C6 Ir1 C5 39.1(2) . . ? C1 Ir1 C5 90.6(2) . . ? C9 N1 N2 105.7(5) . . ? C9 N1 Ir1 133.8(4) . . ? N2 N1 Ir1 120.1(3) . . ? C11 N2 N1 111.0(5) . . ? C11 N2 C15 128.5(5) . . ? N1 N2 C15 120.2(4) . . ? N4 N3 C12 104.7(5) . . ? N4 N3 Ir1 121.3(3) . . ? C12 N3 Ir1 134.0(4) . . ? C14 N4 N3 111.6(5) . . ? C14 N4 C15 127.2(5) . . ? N3 N4 C15 121.1(4) . . ? C22 N5 N6 103.0(5) . . ? C24 N6 N5 111.4(5) . . ? C24 N6 C28 127.9(5) . . ? N5 N6 C28 120.6(4) . . ? C25 N7 N8 103.5(5) . . ? C27 N8 N7 112.3(5) . . ? C27 N8 C28 125.5(5) . . ? N7 N8 C28 121.8(5) . . ? C2 C1 C8 124.0(5) . . ? C2 C1 Ir1 69.5(3) . . ? C8 C1 Ir1 113.0(4) . . ? C2 C1 H1 114.1 . . ? C8 C1 H1 114.1 . . ? Ir1 C1 H1 114.1 . . ? C1 C2 C3 124.4(6) . . ? C1 C2 Ir1 71.9(3) . . ? C3 C2 Ir1 111.0(4) . . ? C1 C2 H2 114.0 . . ? C3 C2 H2 114.0 . . ? Ir1 C2 H2 114.0 . . ? C4 C3 C2 113.5(5) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 111.4(5) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 Ir1 70.2(3) . . ? C4 C5 Ir1 113.3(4) . . ? C6 C5 H5 114.5 . . ? C4 C5 H5 114.5 . . ? Ir1 C5 H5 114.5 . . ? C5 C6 C7 125.2(5) . . ? C5 C6 Ir1 70.7(3) . . ? C7 C6 Ir1 111.0(4) . . ? C5 C6 H6 114.0 . . ? C7 C6 H6 114.0 . . ? Ir1 C6 H6 114.0 . . ? C6 C7 C8 113.0(5) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C1 112.4(5) . . ? C7 C8 H8A 109.1 . . ? C1 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C1 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C10 110.4(5) . . ? N1 C9 H9 124.8 . . ? C10 C9 H9 124.8 . . ? C11 C10 C9 105.4(5) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 107.4(5) . . ? N2 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? N3 C12 C13 110.4(6) . . ? N3 C12 H12 124.8 . . ? C13 C12 H12 124.8 . . ? C14 C13 C12 106.0(6) . . ? C14 C13 H13 127.0 . . ? C12 C13 H13 127.0 . . ? N4 C14 C13 107.3(6) . . ? N4 C14 H14 126.3 . . ? C13 C14 H14 126.3 . . ? N4 C15 N2 108.0(4) . . ? N4 C15 C16 112.9(4) . . ? N2 C15 C16 110.5(4) . . ? N4 C15 H15 108.4 . . ? N2 C15 H15 108.4 . . ? C16 C15 H15 108.4 . . ? C21 C16 C17 119.3(5) . . ? C21 C16 C15 119.8(5) . . ? C17 C16 C15 120.7(5) . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 C28 120.1(5) . . ? C19 C18 C28 119.5(5) . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 119.8(5) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? N5 C22 C23 113.0(6) . . ? N5 C22 H22 123.5 . . ? C23 C22 H22 123.5 . . ? C22 C23 C24 105.5(6) . . ? C22 C23 H23 127.3 . . ? C24 C23 H23 127.3 . . ? N6 C24 C23 107.1(6) . . ? N6 C24 H24 126.5 . . ? C23 C24 H24 126.5 . . ? N7 C25 C26 112.3(7) . . ? N7 C25 H25 123.8 . . ? C26 C25 H25 123.8 . . ? C27 C26 C25 105.0(6) . . ? C27 C26 H26 127.5 . . ? C25 C26 H26 127.5 . . ? N8 C27 C26 106.7(6) . . ? N8 C27 H27 126.6 . . ? C26 C27 H27 126.6 . . ? N8 C28 N6 112.4(4) . . ? N8 C28 C18 112.1(4) . . ? N6 C28 C18 111.5(4) . . ? N8 C28 H28 106.8 . . ? N6 C28 H28 106.8 . . ? C18 C28 H28 106.8 . . ? C29 B1 C45 113.1(4) . . ? C29 B1 C37 102.0(4) . . ? C45 B1 C37 113.0(4) . . ? C29 B1 C53 112.7(4) . . ? C45 B1 C53 103.2(4) . . ? C37 B1 C53 113.2(4) . . ? F19 C59 F21 107.6(7) . . ? F19 C59 F20 107.5(7) . . ? F21 C59 F20 102.6(7) . . ? F19 C59 C55 113.9(6) . . ? F21 C59 C55 111.8(6) . . ? F20 C59 C55 112.7(6) . . ? C30 C29 C34 115.4(5) . . ? C30 C29 B1 122.1(5) . . ? C34 C29 B1 121.9(4) . . ? C31 C30 C29 121.3(5) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 121.8(5) . . ? C32 C31 C35 120.6(5) . . ? C30 C31 C35 117.7(5) . . ? C33 C32 C31 117.9(5) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 121.1(5) . . ? C32 C33 C36 120.4(5) . . ? C34 C33 C36 118.4(5) . . ? C33 C34 C29 122.5(5) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? F4 C35 F6 106.5(9) . . ? F4A C35 F6A 116.7(19) . . ? F4 C35 F5 107.4(7) . . ? F6 C35 F5 105.4(9) . . ? F4A C35 F5A 98.9(16) . . ? F6A C35 F5A 102(2) . . ? F4A C35 C31 119.4(9) . . ? F4 C35 C31 118.2(6) . . ? F6 C35 C31 111.9(6) . . ? F6A C35 C31 108.4(12) . . ? F5 C35 C31 106.8(6) . . ? F5A C35 C31 109.4(9) . . ? F2 C36 F1 106.3(6) . . ? F2 C36 F3 106.9(5) . . ? F1 C36 F3 106.1(5) . . ? F2 C36 C33 113.2(5) . . ? F1 C36 C33 111.5(5) . . ? F3 C36 C33 112.4(6) . . ? C42 C37 C38 115.3(5) . . ? C42 C37 B1 121.7(4) . . ? C38 C37 B1 122.3(4) . . ? C39 C38 C37 121.8(5) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 121.3(5) . . ? C38 C39 C43 119.4(5) . . ? C40 C39 C43 119.3(5) . . ? C41 C40 C39 118.1(5) . . ? C41 C40 H40 121.0 . . ? C39 C40 H40 121.0 . . ? C40 C41 C42 120.8(5) . . ? C40 C41 C44 118.7(5) . . ? C42 C41 C44 120.6(5) . . ? C37 C42 C41 122.7(5) . . ? C37 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? F8A C43 F8 129.7(11) . . ? F8A C43 F9A 111(2) . . ? F8 C43 F9A 55.9(17) . . ? F8A C43 F9 48.9(16) . . ? F8 C43 F9 103.8(7) . . ? F9A C43 F9 136.0(11) . . ? F8A C43 F7A 104(2) . . ? F8 C43 F7A 60(2) . . ? F9A C43 F7A 115(3) . . ? F9 C43 F7A 55(2) . . ? F8A C43 F7 56.0(16) . . ? F8 C43 F7 106.2(9) . . ? F9A C43 F7 58.0(16) . . ? F9 C43 F7 101.4(9) . . ? F7A C43 F7 142.3(11) . . ? F8A C43 C39 112.5(10) . . ? F8 C43 C39 117.6(5) . . ? F9A C43 C39 109.6(10) . . ? F9 C43 C39 114.3(7) . . ? F7A C43 C39 105.2(10) . . ? F7 C43 C39 112.0(6) . . ? F11 C44 F12 106.7(5) . . ? F11 C44 F10 106.9(5) . . ? F12 C44 F10 105.0(6) . . ? F11 C44 C41 111.8(5) . . ? F12 C44 C41 113.7(5) . . ? F10 C44 C41 112.2(5) . . ? C46 C45 C50 116.6(5) . . ? C46 C45 B1 121.9(4) . . ? C50 C45 B1 120.9(4) . . ? C45 C46 C47 122.1(5) . . ? C45 C46 H46 119.0 . . ? C47 C46 H46 119.0 . . ? C48 C47 C46 120.4(5) . . ? C48 C47 C51 119.1(5) . . ? C46 C47 C51 120.4(5) . . ? C49 C48 C47 118.8(5) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 120.5(5) . . ? C48 C49 C52 119.9(5) . . ? C50 C49 C52 119.5(5) . . ? C45 C50 C49 121.5(5) . . ? C45 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? F15 C51 F13 106.7(5) . . ? F15 C51 F14 104.5(5) . . ? F13 C51 F14 105.8(5) . . ? F15 C51 C47 113.6(5) . . ? F13 C51 C47 113.8(5) . . ? F14 C51 C47 111.7(5) . . ? F18 C52 F18A 131(3) . . ? F18 C52 F16A 65(4) . . ? F18A C52 F16A 94(6) . . ? F18 C52 F16 107.0(6) . . ? F18A C52 F16 55(5) . . ? F16A C52 F16 134(2) . . ? F18 C52 F17A 59(3) . . ? F18A C52 F17A 104(6) . . ? F16A C52 F17A 119(5) . . ? F16 C52 F17A 53(4) . . ? F18 C52 F17 105.8(7) . . ? F18A C52 F17 52(5) . . ? F16A C52 F17 45(4) . . ? F16 C52 F17 104.6(5) . . ? F17A C52 F17 136(2) . . ? F18 C52 C49 114.3(5) . . ? F18A C52 C49 115(2) . . ? F16A C52 C49 112(2) . . ? F16 C52 C49 112.4(6) . . ? F17A C52 C49 112(2) . . ? F17 C52 C49 112.1(5) . . ? C54 C53 C58 116.0(5) . . ? C54 C53 B1 122.9(5) . . ? C58 C53 B1 120.5(5) . . ? C55 C54 C53 122.2(5) . . ? C55 C54 H54 118.9 . . ? C53 C54 H54 118.9 . . ? C56 C55 C54 121.1(5) . . ? C56 C55 C59 120.3(5) . . ? C54 C55 C59 118.7(5) . . ? C55 C56 C57 117.9(5) . . ? C55 C56 H56 121.0 . . ? C57 C56 H56 121.0 . . ? C56 C57 C58 121.2(5) . . ? C56 C57 C60 119.1(5) . . ? C58 C57 C60 119.7(5) . . ? C57 C58 C53 121.6(5) . . ? C57 C58 H58 119.2 . . ? C53 C58 H58 119.2 . . ? F24 C60 F22 108.8(7) . . ? F24 C60 F23 105.2(6) . . ? F22 C60 F23 103.6(6) . . ? F24 C60 C57 114.6(5) . . ? F22 C60 C57 112.9(5) . . ? F23 C60 C57 111.0(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 N3 Ir1 N1 C9 -139.5(6) . . . . ? C2 Ir1 N1 C9 66.3(6) . . . . ? C6 Ir1 N1 C9 -53.0(9) . . . . ? C1 Ir1 N1 C9 27.7(6) . . . . ? C5 Ir1 N1 C9 135.0(7) . . . . ? N3 Ir1 N1 N2 31.8(4) . . . . ? C2 Ir1 N1 N2 -122.5(4) . . . . ? C6 Ir1 N1 N2 118.3(6) . . . . ? C1 Ir1 N1 N2 -161.0(4) . . . . ? C5 Ir1 N1 N2 -53.7(8) . . . . ? C9 N1 N2 C11 -1.0(6) . . . . ? Ir1 N1 N2 C11 -174.4(4) . . . . ? C9 N1 N2 C15 -176.0(5) . . . . ? Ir1 N1 N2 C15 10.6(6) . . . . ? C2 Ir1 N3 N4 49.8(7) . . . . ? N1 Ir1 N3 N4 -35.3(4) . . . . ? C6 Ir1 N3 N4 165.0(4) . . . . ? C1 Ir1 N3 N4 -131.4(9) . . . . ? C5 Ir1 N3 N4 125.8(4) . . . . ? C2 Ir1 N3 C12 -133.8(7) . . . . ? N1 Ir1 N3 C12 141.1(6) . . . . ? C6 Ir1 N3 C12 -18.6(6) . . . . ? C1 Ir1 N3 C12 44.9(12) . . . . ? C5 Ir1 N3 C12 -57.8(6) . . . . ? C12 N3 N4 C14 1.2(6) . . . . ? Ir1 N3 N4 C14 178.6(4) . . . . ? C12 N3 N4 C15 178.2(5) . . . . ? Ir1 N3 N4 C15 -4.5(6) . . . . ? C22 N5 N6 C24 -1.3(7) . . . . ? C22 N5 N6 C28 179.6(5) . . . . ? C25 N7 N8 C27 0.3(7) . . . . ? C25 N7 N8 C28 174.1(5) . . . . ? N3 Ir1 C1 C2 -179.2(8) . . . . ? N1 Ir1 C1 C2 85.7(4) . . . . ? C6 Ir1 C1 C2 -114.5(4) . . . . ? C5 Ir1 C1 C2 -76.2(4) . . . . ? N3 Ir1 C1 C8 -59.8(11) . . . . ? C2 Ir1 C1 C8 119.3(6) . . . . ? N1 Ir1 C1 C8 -154.9(4) . . . . ? C6 Ir1 C1 C8 4.8(4) . . . . ? C5 Ir1 C1 C8 43.1(4) . . . . ? C8 C1 C2 C3 -1.0(9) . . . . ? Ir1 C1 C2 C3 103.5(6) . . . . ? C8 C1 C2 Ir1 -104.5(5) . . . . ? N3 Ir1 C2 C1 179.5(4) . . . . ? N1 Ir1 C2 C1 -96.5(4) . . . . ? C6 Ir1 C2 C1 65.7(4) . . . . ? C5 Ir1 C2 C1 101.2(4) . . . . ? N3 Ir1 C2 C3 58.8(7) . . . . ? N1 Ir1 C2 C3 142.7(4) . . . . ? C6 Ir1 C2 C3 -55.1(5) . . . . ? C1 Ir1 C2 C3 -120.7(6) . . . . ? C5 Ir1 C2 C3 -19.5(4) . . . . ? C1 C2 C3 C4 -48.8(8) . . . . ? Ir1 C2 C3 C4 33.1(7) . . . . ? C2 C3 C4 C5 -30.2(8) . . . . ? C3 C4 C5 C6 93.9(7) . . . . ? C3 C4 C5 Ir1 13.3(7) . . . . ? N3 Ir1 C5 C6 91.1(3) . . . . ? C2 Ir1 C5 C6 -114.2(4) . . . . ? N1 Ir1 C5 C6 175.6(5) . . . . ? C1 Ir1 C5 C6 -76.4(4) . . . . ? N3 Ir1 C5 C4 -151.2(4) . . . . ? C2 Ir1 C5 C4 3.5(4) . . . . ? N1 Ir1 C5 C4 -66.7(8) . . . . ? C6 Ir1 C5 C4 117.7(6) . . . . ? C1 Ir1 C5 C4 41.3(5) . . . . ? C4 C5 C6 C7 -3.1(9) . . . . ? Ir1 C5 C6 C7 102.6(6) . . . . ? C4 C5 C6 Ir1 -105.6(5) . . . . ? N3 Ir1 C6 C5 -90.6(3) . . . . ? C2 Ir1 C6 C5 65.9(4) . . . . ? N1 Ir1 C6 C5 -175.9(5) . . . . ? C1 Ir1 C6 C5 101.0(4) . . . . ? N3 Ir1 C6 C7 148.1(4) . . . . ? C2 Ir1 C6 C7 -55.4(5) . . . . ? N1 Ir1 C6 C7 62.8(8) . . . . ? C1 Ir1 C6 C7 -20.3(4) . . . . ? C5 Ir1 C6 C7 -121.4(6) . . . . ? C5 C6 C7 C8 -47.9(8) . . . . ? Ir1 C6 C7 C8 32.7(6) . . . . ? C6 C7 C8 C1 -28.9(7) . . . . ? C2 C1 C8 C7 91.5(7) . . . . ? Ir1 C1 C8 C7 11.5(6) . . . . ? N2 N1 C9 C10 1.0(7) . . . . ? Ir1 N1 C9 C10 173.2(4) . . . . ? N1 C9 C10 C11 -0.7(8) . . . . ? N1 N2 C11 C10 0.5(7) . . . . ? C15 N2 C11 C10 175.0(6) . . . . ? C9 C10 C11 N2 0.1(7) . . . . ? N4 N3 C12 C13 -0.6(8) . . . . ? Ir1 N3 C12 C13 -177.4(5) . . . . ? N3 C12 C13 C14 -0.2(9) . . . . ? N3 N4 C14 C13 -1.4(8) . . . . ? C15 N4 C14 C13 -178.1(6) . . . . ? C12 C13 C14 N4 0.9(9) . . . . ? C14 N4 C15 N2 -123.2(6) . . . . ? N3 N4 C15 N2 60.4(6) . . . . ? C14 N4 C15 C16 114.3(6) . . . . ? N3 N4 C15 C16 -62.1(6) . . . . ? C11 N2 C15 N4 122.6(6) . . . . ? N1 N2 C15 N4 -63.4(6) . . . . ? C11 N2 C15 C16 -113.5(6) . . . . ? N1 N2 C15 C16 60.5(6) . . . . ? N4 C15 C16 C21 158.6(5) . . . . ? N2 C15 C16 C21 37.5(7) . . . . ? N4 C15 C16 C17 -26.7(7) . . . . ? N2 C15 C16 C17 -147.7(5) . . . . ? C21 C16 C17 C18 -1.0(8) . . . . ? C15 C16 C17 C18 -175.8(5) . . . . ? C16 C17 C18 C19 0.3(8) . . . . ? C16 C17 C18 C28 -172.2(5) . . . . ? C17 C18 C19 C20 0.3(9) . . . . ? C28 C18 C19 C20 172.9(6) . . . . ? C18 C19 C20 C21 -0.2(10) . . . . ? C19 C20 C21 C16 -0.5(10) . . . . ? C17 C16 C21 C20 1.1(9) . . . . ? C15 C16 C21 C20 175.9(6) . . . . ? N6 N5 C22 C23 2.6(8) . . . . ? N5 C22 C23 C24 -2.9(10) . . . . ? N5 N6 C24 C23 -0.4(9) . . . . ? C28 N6 C24 C23 178.6(6) . . . . ? C22 C23 C24 N6 1.9(9) . . . . ? N8 N7 C25 C26 -0.6(8) . . . . ? N7 C25 C26 C27 0.7(9) . . . . ? N7 N8 C27 C26 0.1(7) . . . . ? C28 N8 C27 C26 -173.4(6) . . . . ? C25 C26 C27 N8 -0.4(8) . . . . ? C27 N8 C28 N6 -119.9(6) . . . . ? N7 N8 C28 N6 67.2(6) . . . . ? C27 N8 C28 C18 113.5(6) . . . . ? N7 N8 C28 C18 -59.4(6) . . . . ? C24 N6 C28 N8 107.6(7) . . . . ? N5 N6 C28 N8 -73.5(6) . . . . ? C24 N6 C28 C18 -125.5(7) . . . . ? N5 N6 C28 C18 53.4(7) . . . . ? C17 C18 C28 N8 -19.5(7) . . . . ? C19 C18 C28 N8 168.0(5) . . . . ? C17 C18 C28 N6 -146.6(5) . . . . ? C19 C18 C28 N6 40.9(7) . . . . ? C45 B1 C29 C30 -153.7(5) . . . . ? C37 B1 C29 C30 84.6(6) . . . . ? C53 B1 C29 C30 -37.1(7) . . . . ? C45 B1 C29 C34 35.3(7) . . . . ? C37 B1 C29 C34 -86.3(5) . . . . ? C53 B1 C29 C34 151.9(5) . . . . ? C34 C29 C30 C31 -0.1(8) . . . . ? B1 C29 C30 C31 -171.6(5) . . . . ? C29 C30 C31 C32 -0.4(8) . . . . ? C29 C30 C31 C35 -179.3(5) . . . . ? C30 C31 C32 C33 0.4(8) . . . . ? C35 C31 C32 C33 179.3(5) . . . . ? C31 C32 C33 C34 0.1(8) . . . . ? C31 C32 C33 C36 -178.7(5) . . . . ? C32 C33 C34 C29 -0.6(8) . . . . ? C36 C33 C34 C29 178.2(5) . . . . ? C30 C29 C34 C33 0.6(8) . . . . ? B1 C29 C34 C33 172.1(5) . . . . ? C32 C31 C35 F4A -2.3(19) . . . . ? C30 C31 C35 F4A 176.6(18) . . . . ? C32 C31 C35 F4 166.8(7) . . . . ? C30 C31 C35 F4 -14.3(10) . . . . ? C32 C31 C35 F6 -69.0(11) . . . . ? C30 C31 C35 F6 109.9(10) . . . . ? C32 C31 C35 F6A 134.6(19) . . . . ? C30 C31 C35 F6A -46(2) . . . . ? C32 C31 C35 F5 45.8(9) . . . . ? C30 C31 C35 F5 -135.3(7) . . . . ? C32 C31 C35 F5A -115.2(15) . . . . ? C30 C31 C35 F5A 63.7(15) . . . . ? C32 C33 C36 F2 -130.8(6) . . . . ? C34 C33 C36 F2 50.4(7) . . . . ? C32 C33 C36 F1 109.4(6) . . . . ? C34 C33 C36 F1 -69.4(7) . . . . ? C32 C33 C36 F3 -9.5(8) . . . . ? C34 C33 C36 F3 171.6(5) . . . . ? C29 B1 C37 C42 80.5(5) . . . . ? C45 B1 C37 C42 -41.3(6) . . . . ? C53 B1 C37 C42 -158.2(4) . . . . ? C29 B1 C37 C38 -89.9(5) . . . . ? C45 B1 C37 C38 148.3(5) . . . . ? C53 B1 C37 C38 31.4(6) . . . . ? C42 C37 C38 C39 1.9(7) . . . . ? B1 C37 C38 C39 172.9(5) . . . . ? C37 C38 C39 C40 -1.3(8) . . . . ? C37 C38 C39 C43 -179.4(5) . . . . ? C38 C39 C40 C41 -0.3(8) . . . . ? C43 C39 C40 C41 177.8(5) . . . . ? C39 C40 C41 C42 1.1(8) . . . . ? C39 C40 C41 C44 -177.9(5) . . . . ? C38 C37 C42 C41 -1.0(7) . . . . ? B1 C37 C42 C41 -172.1(5) . . . . ? C40 C41 C42 C37 -0.5(8) . . . . ? C44 C41 C42 C37 178.5(5) . . . . ? C38 C39 C43 F8A -180(2) . . . . ? C40 C39 C43 F8A 2(2) . . . . ? C38 C39 C43 F8 -4.3(10) . . . . ? C40 C39 C43 F8 177.6(8) . . . . ? C38 C39 C43 F9A 57(2) . . . . ? C40 C39 C43 F9A -122(2) . . . . ? C38 C39 C43 F9 -126.4(10) . . . . ? C40 C39 C43 F9 55.5(11) . . . . ? C38 C39 C43 F7A -68(3) . . . . ? C40 C39 C43 F7A 114(3) . . . . ? C38 C39 C43 F7 119.0(12) . . . . ? C40 C39 C43 F7 -59.1(13) . . . . ? C40 C41 C44 F11 -75.0(7) . . . . ? C42 C41 C44 F11 106.0(6) . . . . ? C40 C41 C44 F12 164.1(5) . . . . ? C42 C41 C44 F12 -15.0(8) . . . . ? C40 C41 C44 F10 45.1(8) . . . . ? C42 C41 C44 F10 -133.9(6) . . . . ? C29 B1 C45 C46 39.4(7) . . . . ? C37 B1 C45 C46 154.7(5) . . . . ? C53 B1 C45 C46 -82.7(5) . . . . ? C29 B1 C45 C50 -150.0(5) . . . . ? C37 B1 C45 C50 -34.7(6) . . . . ? C53 B1 C45 C50 88.0(5) . . . . ? C50 C45 C46 C47 1.2(7) . . . . ? B1 C45 C46 C47 172.3(5) . . . . ? C45 C46 C47 C48 -0.4(8) . . . . ? C45 C46 C47 C51 178.2(5) . . . . ? C46 C47 C48 C49 -0.5(8) . . . . ? C51 C47 C48 C49 -179.2(5) . . . . ? C47 C48 C49 C50 0.5(8) . . . . ? C47 C48 C49 C52 -179.2(5) . . . . ? C46 C45 C50 C49 -1.1(7) . . . . ? B1 C45 C50 C49 -172.3(5) . . . . ? C48 C49 C50 C45 0.3(8) . . . . ? C52 C49 C50 C45 -180.0(5) . . . . ? C48 C47 C51 F15 70.6(7) . . . . ? C46 C47 C51 F15 -108.1(6) . . . . ? C48 C47 C51 F13 -167.1(5) . . . . ? C46 C47 C51 F13 14.2(7) . . . . ? C48 C47 C51 F14 -47.2(7) . . . . ? C46 C47 C51 F14 134.0(5) . . . . ? C48 C49 C52 F18 171.5(6) . . . . ? C50 C49 C52 F18 -8.3(9) . . . . ? C48 C49 C52 F18A -6(6) . . . . ? C50 C49 C52 F18A 174(6) . . . . ? C48 C49 C52 F16A 100(4) . . . . ? C50 C49 C52 F16A -80(4) . . . . ? C48 C49 C52 F16 -66.3(8) . . . . ? C50 C49 C52 F16 113.9(7) . . . . ? C48 C49 C52 F17A -124(4) . . . . ? C50 C49 C52 F17A 57(4) . . . . ? C48 C49 C52 F17 51.2(9) . . . . ? C50 C49 C52 F17 -128.6(6) . . . . ? C29 B1 C53 C54 -35.4(7) . . . . ? C45 B1 C53 C54 87.0(6) . . . . ? C37 B1 C53 C54 -150.5(5) . . . . ? C29 B1 C53 C58 153.4(5) . . . . ? C45 B1 C53 C58 -84.3(5) . . . . ? C37 B1 C53 C58 38.2(6) . . . . ? C58 C53 C54 C55 -1.4(8) . . . . ? B1 C53 C54 C55 -173.1(5) . . . . ? C53 C54 C55 C56 -0.1(8) . . . . ? C53 C54 C55 C59 -179.8(5) . . . . ? F19 C59 C55 C56 -7.1(10) . . . . ? F21 C59 C55 C56 115.2(7) . . . . ? F20 C59 C55 C56 -129.9(6) . . . . ? F19 C59 C55 C54 172.6(7) . . . . ? F21 C59 C55 C54 -65.1(8) . . . . ? F20 C59 C55 C54 49.8(8) . . . . ? C54 C55 C56 C57 1.5(8) . . . . ? C59 C55 C56 C57 -178.8(5) . . . . ? C55 C56 C57 C58 -1.4(8) . . . . ? C55 C56 C57 C60 178.5(5) . . . . ? C56 C57 C58 C53 -0.2(8) . . . . ? C60 C57 C58 C53 179.9(5) . . . . ? C54 C53 C58 C57 1.6(7) . . . . ? B1 C53 C58 C57 173.4(5) . . . . ? C56 C57 C60 F24 -179.4(6) . . . . ? C58 C57 C60 F24 0.5(9) . . . . ? C56 C57 C60 F22 55.2(8) . . . . ? C58 C57 C60 F22 -124.9(7) . . . . ? C56 C57 C60 F23 -60.5(7) . . . . ? C58 C57 C60 F23 119.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.000 _refine_diff_density_min -1.749 _refine_diff_density_rms 0.143 #===END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 798126' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H46 N8 Rh2), 4(C32 H12 B F24), 5(C H2 Cl2)' _chemical_formula_sum 'C221 H150 B4 Cl10 F96 N16 Rh4' _chemical_formula_weight 5662.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall C-2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 38.2718(4) _cell_length_b 14.0298(1) _cell_length_c 25.8175(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.802(2) _cell_angle_gamma 90.00 _cell_volume 11781.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 104834 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5644 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Kappa CCD' _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 126307 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 26439 _reflns_number_gt 24447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski, Minor, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski, Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; One of the three dichloromethane solvent molecules (C111/112 Cl5 Cl6) is disordered over two sites and was refined with thre restraints sadi 0.001 c111 cl5 c111 cl6 c112 cl5a c112 cl6a and three thermal displacement variables for each of the molecular sites (eadp cl5 cl6 c111; eadp cl5a cl6a c112). Furthermore, seven CF3 groups are disordered over two sites each and were refined with the following sets of restraints: Group 1 eadp c59 c59a exyz c59 c59a eadp f7 f7a eadp f8 f8a eadp f9 f9a 'same c59 f7 f8 f9' for the second site Group 2 eadp c67 c67a exyz c67 c67a eadp f13 f13a eadp f14 f14a eadp f15 f15a 'same C67 f13 f14 f15' for the second site Group 3 eadp c76 c76a sadi 0.001 c71 c76 c71 c76a eadp f22 f22a eadp f23 f23a eadp f24 f24a 'same c76 f22 f23 f24' for the second site Group 4 eadp c83a c83 exyz c83 c83a eadp f28 f28a eadp f29 f29a eadp f30 f30a 'same c83 f28 f29 f30' for the second site Group 5 eadp f31 f31a eadp f32 f32a eadp f33 f33a sadi 0.001 c91 f31 c91 f32 c91 f33 c91 f31a c91 f32a c91 f33a Group 6 eadp c99 c99a exyz c99 c99a eadp f37 f37a eadp f38 f38a eadp f39 f39a 'same c99 f37 f38 f39' for the second site Group 7 eadp c100 c200 sadi 0.001 c100 c97 c200 c97 isor 0.01 f40 f42 sadi 0.001 f40 c100 f41 c100 f42 c100 f40a c200 f41a c200 f42a c200 eadp f40 f40a eadp f41 f41a eadp f42 f42a 'same c100 f40 f41 f42' for the second site 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+8.7825P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(13) _refine_ls_number_reflns 26439 _refine_ls_number_parameters 1690 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.050 _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 0.119183(12) 0.235903(17) 0.435823(18) 0.03113(5) Uani 1 1 d . . . Rh2 Rh 0.363936(12) 0.207503(16) 0.726021(18) 0.03254(5) Uani 1 1 d . . . N1 N 0.10932(8) 0.1622(2) 0.49856(12) 0.0382(6) Uani 1 1 d . . . N2 N 0.13556(9) 0.0931(2) 0.53533(12) 0.0411(6) Uani 1 1 d . . . N3 N 0.18265(8) 0.22660(19) 0.50130(13) 0.0350(5) Uani 1 1 d . . . N4 N 0.19580(8) 0.16088(18) 0.54662(11) 0.0349(5) Uani 1 1 d . . . N5 N 0.32599(8) 0.09067(19) 0.71269(11) 0.0352(5) Uani 1 1 d . . . N6 N 0.31578(8) 0.02473(18) 0.66861(12) 0.0333(5) Uani 1 1 d . . . N7 N 0.34079(8) 0.20327(19) 0.63310(12) 0.0348(5) Uani 1 1 d . . . N8 N 0.32468(8) 0.12300(18) 0.59918(12) 0.0363(5) Uani 1 1 d . . . C1 C 0.05708(10) 0.2126(3) 0.36549(15) 0.0417(7) Uani 1 1 d . . . H1 H 0.0472(13) 0.156(3) 0.3803(19) 0.050 Uiso 1 1 d . . . C2 C 0.06074(10) 0.3018(3) 0.39183(16) 0.0426(7) Uani 1 1 d . . . H2 H 0.0537(14) 0.301(3) 0.420(2) 0.051 Uiso 1 1 d . . . C3 C 0.06228(14) 0.3977(3) 0.3648(2) 0.0610(10) Uani 1 1 d . . . H3A H 0.0342 0.4149 0.3313 0.073 Uiso 1 1 calc R . . H3B H 0.0717 0.4476 0.3966 0.073 Uiso 1 1 calc R . . C4 C 0.09098(14) 0.3956(3) 0.3403(2) 0.0638(11) Uani 1 1 d . . . H4A H 0.0755 0.3737 0.2974 0.077 Uiso 1 1 calc R . . H4B H 0.1012 0.4608 0.3412 0.077 Uiso 1 1 calc R . . C5 C 0.12715(12) 0.3299(3) 0.37778(17) 0.0497(8) Uani 1 1 d . . . H5 H 0.1514(14) 0.370(3) 0.407(2) 0.060 Uiso 1 1 d . . . C6 C 0.12778(12) 0.2361(3) 0.36155(17) 0.0493(9) Uani 1 1 d . . . H6 H 0.1548(15) 0.203(3) 0.384(2) 0.059 Uiso 1 1 d . . . C7 C 0.09261(13) 0.1843(3) 0.30781(17) 0.0539(9) Uani 1 1 d . . . H7A H 0.0988 0.1152 0.3118 0.065 Uiso 1 1 calc R . . H7B H 0.0904 0.2068 0.2698 0.065 Uiso 1 1 calc R . . C8 C 0.05166(12) 0.1995(3) 0.30295(16) 0.0503(8) Uani 1 1 d . . . H8A H 0.0336 0.1439 0.2824 0.060 Uiso 1 1 calc R . . H8B H 0.0380 0.2566 0.2777 0.060 Uiso 1 1 calc R . . C9 C 0.37848(13) 0.2361(3) 0.81773(17) 0.0487(8) Uani 1 1 d . . . H9 H 0.3578(15) 0.218(3) 0.823(2) 0.058 Uiso 1 1 d . . . C10 C 0.40528(11) 0.1672(3) 0.81895(15) 0.0465(8) Uani 1 1 d . . . H10 H 0.4010(13) 0.092(3) 0.816(2) 0.056 Uiso 1 1 d . . . C11 C 0.44866(12) 0.1862(4) 0.8352(2) 0.0712(13) Uani 1 1 d . . . H11A H 0.4589 0.1295 0.8244 0.085 Uiso 1 1 calc R . . H11B H 0.4663 0.1950 0.8799 0.085 Uiso 1 1 calc R . . C12 C 0.45317(15) 0.2725(5) 0.8042(2) 0.0816(16) Uani 1 1 d . . . H12A H 0.4765 0.2620 0.7984 0.098 Uiso 1 1 calc R . . H12B H 0.4598 0.3286 0.8310 0.098 Uiso 1 1 calc R . . C13 C 0.41436(14) 0.2939(4) 0.7420(2) 0.0647(13) Uani 1 1 d . . . H13 H 0.4186(18) 0.267(4) 0.714(3) 0.078 Uiso 1 1 d . . . C14 C 0.38366(16) 0.3517(3) 0.73519(19) 0.0649(12) Uani 1 1 d . . . H14 H 0.3647(17) 0.375(4) 0.686(3) 0.078 Uiso 1 1 d . . . C15 C 0.3806(2) 0.4014(4) 0.7853(2) 0.0817(15) Uani 1 1 d . . . H15A H 0.3993 0.4571 0.8000 0.098 Uiso 1 1 calc R . . H15B H 0.3522 0.4254 0.7678 0.098 Uiso 1 1 calc R . . C16 C 0.39112(16) 0.3391(3) 0.8370(2) 0.0689(12) Uani 1 1 d . . . H16A H 0.3773 0.3628 0.8579 0.083 Uiso 1 1 calc R . . H16B H 0.4212 0.3418 0.8665 0.083 Uiso 1 1 calc R . . C17 C 0.07762(11) 0.1578(3) 0.50711(17) 0.0521(9) Uani 1 1 d . . . H17 H 0.0543 0.1985 0.4877 0.062 Uiso 1 1 calc R . . C18 C 0.08341(15) 0.0866(4) 0.5477(2) 0.0723(13) Uani 1 1 d . . . H18 H 0.0656 0.0697 0.5614 0.087 Uiso 1 1 calc R . . C19 C 0.12027(13) 0.0453(3) 0.56420(18) 0.0593(10) Uani 1 1 d . . . H19 H 0.1327 -0.0073 0.5910 0.071 Uiso 1 1 calc R . . C20 C 0.21103(10) 0.2952(3) 0.52429(18) 0.0444(8) Uani 1 1 d . . . H20 H 0.2101 0.3512 0.5029 0.053 Uiso 1 1 calc R . . C21 C 0.24218(14) 0.2738(3) 0.5839(2) 0.0546(9) Uani 1 1 d . . . H21 H 0.2660 0.3106 0.6099 0.066 Uiso 1 1 calc R . . C22 C 0.23138(10) 0.1899(3) 0.59709(17) 0.0491(9) Uani 1 1 d . . . H22 H 0.2460 0.1570 0.6349 0.059 Uiso 1 1 calc R . . C23 C 0.17354(10) 0.0724(2) 0.53654(14) 0.0387(7) Uani 1 1 d . . . H23 H 0.1908 0.0318 0.5733 0.046 Uiso 1 1 calc R . . C24 C 0.30918(10) 0.0606(3) 0.74374(14) 0.0414(7) Uani 1 1 d . . . H24 H 0.3104 0.0941 0.7767 0.050 Uiso 1 1 calc R . . C25 C 0.28952(10) -0.0266(3) 0.72131(15) 0.0443(7) Uani 1 1 d . . . H25 H 0.2756 -0.0635 0.7358 0.053 Uiso 1 1 calc R . . C26 C 0.29465(10) -0.0476(2) 0.67417(15) 0.0395(7) Uani 1 1 d . . . H26 H 0.2851 -0.1033 0.6496 0.047 Uiso 1 1 calc R . . C27 C 0.33670(12) 0.2709(2) 0.59341(16) 0.0446(8) Uani 1 1 d . . . H27 H 0.3448 0.3355 0.6039 0.053 Uiso 1 1 calc R . . C28 C 0.31898(15) 0.2335(3) 0.53503(17) 0.0559(10) Uani 1 1 d . . . H28 H 0.3128 0.2662 0.4989 0.067 Uiso 1 1 calc R . . C29 C 0.31246(13) 0.1394(3) 0.54080(16) 0.0512(9) Uani 1 1 d . . . H29 H 0.3012 0.0935 0.5090 0.061 Uiso 1 1 calc R . . C30 C 0.33336(10) 0.0295(2) 0.62942(14) 0.0359(6) Uani 1 1 d . . . H30 H 0.3639 0.0228 0.6563 0.043 Uiso 1 1 calc R . . C31 C 0.16693(10) 0.0158(2) 0.48203(14) 0.0377(7) Uani 1 1 d . . . C32 C 0.12797(12) -0.0024(2) 0.43393(17) 0.0493(8) Uani 1 1 d . . . H32 H 0.1051 0.0236 0.4340 0.059 Uiso 1 1 calc R . . C33 C 0.12107(14) -0.0597(3) 0.38372(17) 0.0589(10) Uani 1 1 d . . . H33 H 0.0939 -0.0677 0.3496 0.071 Uiso 1 1 calc R . . C34 C 0.15257(14) -0.1022(3) 0.38438(17) 0.0563(10) Uani 1 1 d . . . H34 H 0.1475 -0.1411 0.3510 0.068 Uiso 1 1 calc R . . C35 C 0.19370(12) -0.0901(2) 0.43460(15) 0.0460(8) Uani 1 1 d . . . C36 C 0.22656(14) -0.1402(2) 0.43892(17) 0.0520(9) Uani 1 1 d . . . H36 H 0.2213 -0.1827 0.4070 0.062 Uiso 1 1 calc R . . C37 C 0.26648(12) -0.1306(2) 0.48771(18) 0.0466(8) Uani 1 1 d . . . C38 C 0.29929(15) -0.1880(3) 0.4935(2) 0.0634(11) Uani 1 1 d . . . H38 H 0.2934 -0.2341 0.4630 0.076 Uiso 1 1 calc R . . C39 C 0.33773(15) -0.1789(3) 0.5401(3) 0.0674(12) Uani 1 1 d . . . H39 H 0.3586 -0.2193 0.5428 0.081 Uiso 1 1 calc R . . C40 C 0.34794(13) -0.1086(3) 0.5861(2) 0.0530(9) Uani 1 1 d . . . H40 H 0.3756 -0.1020 0.6191 0.064 Uiso 1 1 calc R . . C41 C 0.31790(11) -0.0505(2) 0.58297(16) 0.0407(7) Uani 1 1 d . . . C42 C 0.27536(11) -0.0627(2) 0.53494(15) 0.0387(7) Uani 1 1 d . . . C43 C 0.24241(10) -0.0124(2) 0.53079(13) 0.0349(6) Uani 1 1 d . . . H43 H 0.2479 0.0331 0.5614 0.042 Uiso 1 1 calc R . . C44 C 0.20179(10) -0.0264(2) 0.48361(13) 0.0355(6) Uani 1 1 d . . . F25 F 0.34943(10) 0.5668(4) 0.64796(15) 0.1170(16) Uani 1 1 d . . . F26 F 0.29513(16) 0.4873(3) 0.6027(2) 0.1116(13) Uani 1 1 d . . . F27 F 0.29976(11) 0.6129(3) 0.56190(13) 0.0850(9) Uani 1 1 d . . . C83 C 0.19946(11) 0.7787(2) 0.60511(16) 0.0450(8) Uani 0.68 1 d PD A 1 F28 F 0.18805(17) 0.7918(4) 0.5457(2) 0.0837(13) Uani 0.68 1 d PD A 1 F29 F 0.16831(14) 0.7387(4) 0.5996(3) 0.098(2) Uani 0.68 1 d PD A 1 F30 F 0.20135(14) 0.8681(3) 0.6233(3) 0.0924(17) Uani 0.68 1 d PD A 1 C83A C 0.19946(11) 0.7787(2) 0.60511(16) 0.0450(8) Uani 0.32 1 d PD A 2 F28A F 0.1875(3) 0.8221(10) 0.6412(4) 0.0837(13) Uani 0.32 1 d PD A 2 F29A F 0.1995(3) 0.8376(9) 0.5717(7) 0.098(2) Uani 0.32 1 d PD A 2 F30A F 0.1704(4) 0.7131(8) 0.5766(6) 0.0924(17) Uani 0.32 1 d PD A 2 F31 F 0.2739(3) 0.3160(6) 0.7556(5) 0.147(3) Uani 0.69 1 d PD B 1 F32 F 0.22697(12) 0.3616(5) 0.7662(4) 0.127(3) Uani 0.69 1 d PD B 1 F33 F 0.2730(4) 0.2627(4) 0.8247(4) 0.187(6) Uani 0.69 1 d PD B 1 F31A F 0.2423(6) 0.3169(13) 0.8155(9) 0.147(3) Uani 0.31 1 d PD B 2 F32A F 0.2831(4) 0.2600(6) 0.8065(12) 0.127(3) Uani 0.31 1 d PD B 2 F33A F 0.2470(10) 0.3594(11) 0.7382(3) 0.187(6) Uani 0.31 1 d PD B 2 F34 F 0.36010(14) 0.3951(2) 1.02249(16) 0.0950(11) Uani 1 1 d . . . F35 F 0.34870(17) 0.5417(3) 1.02740(17) 0.1149(15) Uani 1 1 d . . . F36 F 0.40187(12) 0.4983(3) 1.02646(15) 0.1035(12) Uani 1 1 d . . . C99 C 0.48096(12) 0.5839(3) 0.93018(19) 0.0580(10) Uani 0.68 1 d PD C 1 F37 F 0.4764(3) 0.4982(4) 0.9087(4) 0.120(3) Uani 0.68 1 d PD C 1 F38 F 0.4831(3) 0.5733(9) 0.9822(3) 0.128(3) Uani 0.68 1 d PD C 1 F39 F 0.51742(13) 0.6090(6) 0.9436(5) 0.115(3) Uani 0.68 1 d PD C 1 C99A C 0.48096(12) 0.5839(3) 0.93018(19) 0.0580(10) Uani 0.32 1 d PD C 2 F37A F 0.5078(6) 0.6266(9) 0.9804(8) 0.120(3) Uani 0.32 1 d PD C 2 F38A F 0.4996(7) 0.5438(19) 0.9074(7) 0.128(3) Uani 0.32 1 d PD C 2 F39A F 0.4693(3) 0.5116(14) 0.9490(12) 0.115(3) Uani 0.32 1 d PD C 2 F43 F 0.38064(12) 1.0195(3) 0.9072(2) 0.1032(13) Uani 1 1 d . . . F44 F 0.36619(10) 1.0209(2) 0.97667(12) 0.0814(9) Uani 1 1 d . . . F45 F 0.32890(11) 1.09574(18) 0.89343(15) 0.0858(9) Uani 1 1 d . . . F46 F 0.22381(9) 0.8901(3) 0.90609(18) 0.1070(14) Uani 1 1 d . . . F47 F 0.19240(7) 0.8494(2) 0.81396(13) 0.0754(8) Uani 1 1 d . . . F48 F 0.22077(11) 0.7456(3) 0.8831(2) 0.0967(12) Uani 1 1 d . . . C77 C 0.29803(9) 0.6817(2) 0.74163(14) 0.0337(6) Uani 1 1 d . . . C78 C 0.26031(10) 0.7275(2) 0.70552(15) 0.0348(6) Uani 1 1 d . . . H78 H 0.2486 0.7608 0.7249 0.042 Uiso 1 1 calc R . . C79 C 0.23915(10) 0.7261(2) 0.64203(16) 0.0399(7) Uani 1 1 d . . . C80 C 0.25488(11) 0.6790(3) 0.61117(16) 0.0473(8) Uani 1 1 d . . . H80 H 0.2409 0.6802 0.5680 0.057 Uiso 1 1 calc R . . C81 C 0.29177(11) 0.6301(3) 0.64593(16) 0.0465(8) Uani 1 1 d . . . C82 C 0.31280(10) 0.6319(2) 0.70923(15) 0.0406(7) Uani 1 1 d . . . H82 H 0.3381 0.5984 0.7317 0.049 Uiso 1 1 calc R . . C84 C 0.30941(14) 0.5770(4) 0.61540(18) 0.0654(12) Uani 1 1 d . . . C85 C 0.32004(10) 0.5829(2) 0.84397(16) 0.0376(6) Uani 1 1 d . . . C86 C 0.29575(10) 0.5059(2) 0.80869(17) 0.0435(7) Uani 1 1 d . . . H86 H 0.2811 0.5106 0.7655 0.052 Uiso 1 1 calc R . . C87 C 0.29269(13) 0.4238(3) 0.8351(2) 0.0571(10) Uani 1 1 d . . . C88 C 0.31396(14) 0.4120(3) 0.8978(2) 0.0584(10) Uani 1 1 d . . . H88 H 0.3122 0.3543 0.9155 0.070 Uiso 1 1 calc R . . C89 C 0.33785(14) 0.4871(3) 0.9338(2) 0.0519(9) Uani 1 1 d . . . C90 C 0.33997(11) 0.5705(2) 0.90692(16) 0.0403(7) Uani 1 1 d . . . H90 H 0.3558 0.6219 0.9326 0.048 Uiso 1 1 calc R . . C91 C 0.26614(13) 0.3437(3) 0.7965(3) 0.0891(18) Uani 1 1 d . . . C92 C 0.3618(2) 0.4797(3) 1.0021(2) 0.0721(14) Uani 1 1 d . . . C93 C 0.37441(9) 0.6936(2) 0.83483(14) 0.0326(6) Uani 1 1 d . . . C94 C 0.40705(9) 0.6353(2) 0.87450(14) 0.0349(6) Uani 1 1 d . . . H94 H 0.4021 0.5836 0.8936 0.042 Uiso 1 1 calc R . . C95 C 0.44696(10) 0.6504(3) 0.88709(15) 0.0421(7) Uani 1 1 d . . . C96 C 0.45559(11) 0.7245(3) 0.86039(19) 0.0481(8) Uani 1 1 d . . . H96 H 0.4827 0.7352 0.8693 0.058 Uiso 1 1 calc R . . C97 C 0.42351(11) 0.7825(3) 0.82029(18) 0.0450(8) Uani 1 1 d . . . C98 C 0.38406(10) 0.7669(2) 0.80776(16) 0.0384(7) Uani 1 1 d . . . H98 H 0.3626 0.8078 0.7795 0.046 Uiso 1 1 calc R . . C101 C 0.31320(9) 0.7708(2) 0.84436(13) 0.0316(6) Uani 1 1 d . . . C102 C 0.33686(9) 0.8538(2) 0.86891(13) 0.0337(6) Uani 1 1 d . . . H102 H 0.3622 0.8590 0.8708 0.040 Uiso 1 1 calc R . . C103 C 0.32428(10) 0.9283(2) 0.89048(13) 0.0364(6) Uani 1 1 d . . . C104 C 0.28752(10) 0.9239(2) 0.88950(14) 0.0377(7) Uani 1 1 d . . . H104 H 0.2787 0.9755 0.9037 0.045 Uiso 1 1 calc R . . C105 C 0.26434(9) 0.8414(3) 0.86709(14) 0.0379(7) Uani 1 1 d . . . C106 C 0.27731(10) 0.7662(2) 0.84544(15) 0.0355(6) Uani 1 1 d . . . H106 H 0.2610 0.7101 0.8310 0.043 Uiso 1 1 calc R . . C107 C 0.35025(13) 1.0148(3) 0.91699(18) 0.0498(8) Uani 1 1 d . . . C108 C 0.22529(11) 0.8315(3) 0.86648(17) 0.0479(8) Uani 1 1 d . . . B2 B 0.32624(10) 0.6816(2) 0.81636(16) 0.0324(6) Uani 1 1 d . . . C100 C 0.43331(18) 0.8657(4) 0.7942(3) 0.0616(13) Uani 0.53 1 d PD C 1 F40 F 0.4593(3) 0.8430(7) 0.7783(6) 0.110(3) Uani 0.53 1 d PDU C 1 F41 F 0.40139(17) 0.9078(8) 0.7495(5) 0.118(4) Uani 0.53 1 d PD C 1 F42 F 0.4501(5) 0.9359(6) 0.8325(4) 0.140(3) Uani 0.53 1 d PDU C 1 C200 C 0.4299(2) 0.8581(5) 0.7856(3) 0.0616(13) Uani 0.47 1 d PD C 2 F40A F 0.4111(4) 0.9367(6) 0.7827(7) 0.110(3) Uani 0.47 1 d PD C 2 F41A F 0.46767(18) 0.8875(10) 0.8105(6) 0.118(4) Uani 0.47 1 d PD C 2 F42A F 0.4183(5) 0.8322(8) 0.7304(4) 0.140(3) Uani 0.47 1 d PD C 2 F1 F 0.22371(8) 0.0836(3) 0.79629(14) 0.0880(10) Uani 1 1 d . . . F2 F 0.20689(9) 0.1245(3) 0.70745(19) 0.0962(12) Uani 1 1 d . . . F3 F 0.19985(9) -0.0209(2) 0.72581(19) 0.0864(10) Uani 1 1 d . . . F4 F 0.06277(9) -0.11395(18) 0.66633(15) 0.0752(8) Uani 1 1 d . . . F5 F 0.01937(9) -0.0047(2) 0.61251(12) 0.0817(9) Uani 1 1 d . . . F6 F 0.03515(9) -0.0311(2) 0.70299(14) 0.0734(7) Uani 1 1 d . . . C59 C -0.04774(14) 0.2763(3) 0.51485(19) 0.0645(12) Uani 0.60 1 d PD D 1 F7 F -0.0320(3) 0.2035(7) 0.5077(4) 0.147(5) Uani 0.60 1 d PD D 1 F8 F -0.0557(4) 0.3333(5) 0.4679(2) 0.112(2) Uani 0.60 1 d PD D 1 F9 F -0.0853(3) 0.2593(10) 0.5014(4) 0.148(5) Uani 0.60 1 d PD D 1 C59A C -0.04774(14) 0.2763(3) 0.51485(19) 0.0645(12) Uani 0.40 1 d PD D 2 F7A F -0.0839(5) 0.2973(11) 0.4798(6) 0.147(5) Uani 0.40 1 d PD D 2 F8A F -0.0485(5) 0.1835(9) 0.5264(4) 0.112(2) Uani 0.40 1 d PD D 2 F9A F -0.0277(5) 0.2682(19) 0.4860(6) 0.148(5) Uani 0.40 1 d PD D 2 F10 F -0.07276(9) 0.5488(3) 0.62049(17) 0.0993(12) Uani 1 1 d . . . F11 F -0.03979(19) 0.4985(3) 0.7096(2) 0.142(2) Uani 1 1 d . . . F12 F -0.01401(10) 0.5985(2) 0.6807(2) 0.0976(11) Uani 1 1 d . . . C67 C 0.07793(14) 0.2973(4) 0.90215(19) 0.0638(12) Uani 0.74 1 d PD E 1 F13 F 0.04960(15) 0.2269(4) 0.8677(2) 0.0850(12) Uani 0.74 1 d PD E 1 F14 F 0.0559(2) 0.3626(4) 0.9030(4) 0.114(2) Uani 0.74 1 d PD E 1 F15 F 0.09899(17) 0.2577(7) 0.9551(2) 0.137(3) Uani 0.74 1 d PD E 1 C67A C 0.07793(14) 0.2973(4) 0.90215(19) 0.0638(12) Uani 0.26 1 d PD E 2 F13A F 0.0923(5) 0.3548(11) 0.9558(6) 0.0850(12) Uani 0.26 1 d PD E 2 F14A F 0.0850(7) 0.2222(11) 0.9259(12) 0.114(2) Uani 0.26 1 d PD E 2 F15A F 0.0421(5) 0.334(2) 0.8735(7) 0.137(3) Uani 0.26 1 d PD E 2 F16 F 0.21326(10) 0.4637(3) 0.98123(14) 0.0947(11) Uani 1 1 d . . . F17 F 0.21045(10) 0.5138(3) 0.90315(17) 0.1017(12) Uani 1 1 d . . . F18 F 0.23552(8) 0.3779(3) 0.9363(2) 0.1139(15) Uani 1 1 d . . . F19 F 0.1386(2) 0.6769(3) 0.7563(3) 0.164(3) Uani 1 1 d . . . F20 F 0.1190(3) 0.7246(4) 0.6701(6) 0.245(5) Uani 1 1 d . . . F21 F 0.1791(2) 0.6976(4) 0.7263(3) 0.157(3) Uani 1 1 d . . . C76 C 0.1600(5) 0.4239(13) 0.5891(9) 0.064(3) Uani 0.55 1 d PD F 1 F22 F 0.1968(3) 0.4533(7) 0.6131(4) 0.120(3) Uani 0.55 1 d PD F 1 F23 F 0.1384(4) 0.4648(8) 0.5358(4) 0.126(3) Uani 0.55 1 d PD F 1 F24 F 0.1590(3) 0.3305(5) 0.5791(4) 0.097(3) Uani 0.55 1 d PD F 1 C76A C 0.1472(6) 0.4133(17) 0.5797(10) 0.064(3) Uani 0.45 1 d PD F 2 F22A F 0.1160(4) 0.4077(9) 0.5245(4) 0.120(3) Uani 0.45 1 d PD F 2 F23A F 0.1652(5) 0.3261(11) 0.5964(6) 0.126(3) Uani 0.45 1 d PD F 2 F24A F 0.1766(4) 0.4680(6) 0.5777(5) 0.097(3) Uani 0.45 1 d PD F 2 C45 C 0.10283(10) 0.2138(2) 0.70918(14) 0.0359(6) Uani 1 1 d . . . C46 C 0.14233(10) 0.1866(2) 0.72436(15) 0.0386(7) Uani 1 1 d . . . H46 H 0.1628 0.2343 0.7364 0.046 Uiso 1 1 calc R . . C47 C 0.15265(10) 0.0920(3) 0.72242(15) 0.0408(7) Uani 1 1 d . . . C48 C 0.12387(11) 0.0198(2) 0.70531(15) 0.0400(7) Uani 1 1 d . . . H48 H 0.1307 -0.0448 0.7037 0.048 Uiso 1 1 calc R . . C49 C 0.08460(10) 0.0458(2) 0.69053(14) 0.0385(7) Uani 1 1 d . . . C50 C 0.07469(10) 0.1397(2) 0.69333(14) 0.0374(6) Uani 1 1 d . . . H50 H 0.0478 0.1542 0.6841 0.045 Uiso 1 1 calc R . . C51 C 0.19500(13) 0.0701(3) 0.7372(2) 0.0538(9) Uani 1 1 d . . . C52 C 0.05086(12) -0.0267(3) 0.66774(18) 0.0505(9) Uani 1 1 d . . . C53 C 0.04236(10) 0.3480(2) 0.67054(14) 0.0367(6) Uani 1 1 d . . . C54 C 0.01822(11) 0.3054(2) 0.61335(15) 0.0412(7) Uani 1 1 d . . . H54 H 0.0305 0.2595 0.6007 0.049 Uiso 1 1 calc R . . C55 C -0.02335(12) 0.3279(3) 0.57404(15) 0.0486(8) Uani 1 1 d . . . C56 C -0.04166(11) 0.3976(3) 0.58943(16) 0.0465(8) Uani 1 1 d . . . H56 H -0.0697 0.4142 0.5624 0.056 Uiso 1 1 calc R . . C57 C -0.01845(11) 0.4428(2) 0.64484(16) 0.0418(7) Uani 1 1 d . . . C58 C 0.02290(10) 0.4168(2) 0.68518(14) 0.0368(6) Uani 1 1 d . . . H58 H 0.0380 0.4474 0.7237 0.044 Uiso 1 1 calc R . . C60 C -0.03631(12) 0.5208(3) 0.66366(19) 0.0500(8) Uani 1 1 d . . . C61 C 0.10914(9) 0.3423(2) 0.78607(14) 0.0340(6) Uani 1 1 d . . . C62 C 0.08703(10) 0.3149(3) 0.81322(15) 0.0398(7) Uani 1 1 d . . . H62 H 0.0604 0.2882 0.7884 0.048 Uiso 1 1 calc R . . C63 C 0.10298(11) 0.3257(3) 0.87485(16) 0.0455(8) Uani 1 1 d . . . C64 C 0.14155(11) 0.3642(3) 0.91316(16) 0.0497(8) Uani 1 1 d . . . H64 H 0.1521 0.3721 0.9554 0.060 Uiso 1 1 calc R . . C65 C 0.16417(11) 0.3906(3) 0.88835(15) 0.0470(8) Uani 1 1 d . . . C66 C 0.14855(10) 0.3795(3) 0.82631(14) 0.0389(7) Uani 1 1 d . . . H66 H 0.1651 0.3977 0.8106 0.047 Uiso 1 1 calc R . . C68 C 0.20586(12) 0.4340(3) 0.92746(18) 0.0556(10) Uani 1 1 d . . . C69 C 0.11265(10) 0.4010(2) 0.68927(14) 0.0360(6) Uani 1 1 d . . . C70 C 0.11777(15) 0.4963(3) 0.7076(2) 0.0553(10) Uani 1 1 d . . . H70 H 0.1095 0.5155 0.7348 0.066 Uiso 1 1 calc R . . C71 C 0.13454(19) 0.5641(3) 0.6877(3) 0.0717(15) Uani 1 1 d . . . C72 C 0.14609(18) 0.5391(3) 0.6474(2) 0.0691(14) Uani 1 1 d . . . H72 H 0.1579 0.5847 0.6340 0.083 Uiso 1 1 calc R . . C73 C 0.14017(14) 0.4469(3) 0.62705(19) 0.0522(9) Uani 1 1 d . . . C74 C 0.12433(11) 0.3797(2) 0.64810(15) 0.0415(7) Uani 1 1 d . . . H74 H 0.1213 0.3161 0.6338 0.050 Uiso 1 1 calc R . . C75 C 0.1447(3) 0.6619(5) 0.7153(4) 0.103(2) Uani 1 1 d . . . B1 B 0.09145(11) 0.3256(3) 0.71336(16) 0.0347(7) Uani 1 1 d . . . Cl1 Cl 0.45002(7) 0.32268(15) 0.63272(9) 0.1088(5) Uani 1 1 d . . . C109 C 0.4564(3) 0.2913(7) 0.5732(4) 0.116(3) Uani 1 1 d D . . H10A H 0.4615 0.3499 0.5568 0.139 Uiso 1 1 calc R . . H10B H 0.4811 0.2505 0.5894 0.139 Uiso 1 1 calc R . . Cl2 Cl 0.41546(8) 0.23215(17) 0.51469(10) 0.1296(8) Uani 1 1 d . . . Cl3 Cl 0.46631(11) 0.6844(2) 0.68166(19) 0.1662(12) Uani 1 1 d . . . Cl4 Cl 0.47011(14) 0.5353(2) 0.76009(18) 0.1809(14) Uani 1 1 d . . . C110 C 0.4489(2) 0.5773(6) 0.6878(4) 0.116(2) Uani 1 1 d . . . H11C H 0.4540 0.5303 0.6639 0.139 Uiso 1 1 calc R . . H11D H 0.4187 0.5817 0.6692 0.139 Uiso 1 1 calc R . . Cl5 Cl 0.0329(4) 0.4449(10) 0.4917(6) 0.158(3) Uani 0.30 1 d PD G 1 C111 C -0.0008(9) 0.5332(19) 0.4626(10) 0.158(3) Uani 0.30 1 d PD G 1 H11E H 0.0068 0.5737 0.4387 0.190 Uiso 0.30 1 calc PR G 1 H11F H -0.0279 0.5047 0.4334 0.190 Uiso 0.30 1 calc PR G 1 Cl6 Cl -0.0073(4) 0.6047(8) 0.5079(5) 0.158(3) Uani 0.30 1 d PD G 1 Cl5A Cl 0.0236(6) 0.4728(11) 0.4792(10) 0.144(4) Uani 0.20 1 d PD H 2 C112 C 0.0263(17) 0.5333(11) 0.5363(16) 0.144(4) Uani 0.20 1 d PD H 2 H11G H 0.0025 0.5151 0.5394 0.172 Uiso 0.20 1 calc PR H 2 H11H H 0.0514 0.5130 0.5745 0.172 Uiso 0.20 1 calc PR H 2 Cl6A Cl 0.0270(5) 0.6509(9) 0.5319(8) 0.144(4) Uani 0.20 1 d PD H 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 0.02540(10) 0.03885(11) 0.02953(10) 0.00316(9) 0.01474(8) 0.00060(9) Rh2 0.02679(10) 0.03630(11) 0.03098(10) 0.00146(9) 0.01279(8) -0.00288(9) N1 0.0319(13) 0.0505(16) 0.0333(12) 0.0048(11) 0.0180(11) 0.0029(11) N2 0.0431(15) 0.0450(15) 0.0353(13) 0.0063(11) 0.0209(12) 0.0007(12) N3 0.0274(12) 0.0387(14) 0.0384(13) -0.0034(11) 0.0170(11) -0.0033(10) N4 0.0310(12) 0.0352(13) 0.0294(11) -0.0023(10) 0.0096(10) 0.0053(10) N5 0.0339(12) 0.0394(13) 0.0328(12) 0.0024(10) 0.0180(10) -0.0039(10) N6 0.0311(12) 0.0330(12) 0.0396(13) 0.0041(10) 0.0212(10) -0.0014(10) N7 0.0352(13) 0.0351(13) 0.0322(12) -0.0012(10) 0.0165(11) -0.0044(10) N8 0.0389(13) 0.0309(12) 0.0372(13) -0.0004(10) 0.0187(11) -0.0051(10) C1 0.0251(14) 0.057(2) 0.0361(16) 0.0016(14) 0.0114(12) -0.0005(14) C2 0.0315(16) 0.054(2) 0.0392(17) 0.0047(14) 0.0164(14) 0.0102(14) C3 0.066(3) 0.051(2) 0.051(2) 0.0110(17) 0.0210(19) 0.0157(19) C4 0.064(2) 0.054(2) 0.053(2) 0.0167(18) 0.0176(19) -0.006(2) C5 0.0484(19) 0.056(2) 0.0447(18) 0.0125(16) 0.0244(16) -0.0106(17) C6 0.045(2) 0.075(3) 0.0411(18) 0.0073(17) 0.0313(16) -0.0025(18) C7 0.062(2) 0.070(2) 0.0369(17) -0.0016(17) 0.0304(17) -0.0022(19) C8 0.0424(18) 0.064(2) 0.0375(17) -0.0031(16) 0.0164(15) -0.0033(16) C9 0.046(2) 0.067(2) 0.0370(17) -0.0104(16) 0.0240(16) -0.0125(18) C10 0.0431(18) 0.054(2) 0.0303(15) 0.0055(14) 0.0112(13) 0.0001(16) C11 0.0349(19) 0.082(3) 0.064(3) 0.008(2) 0.0036(18) 0.0008(19) C12 0.040(2) 0.125(5) 0.067(3) 0.004(3) 0.019(2) -0.015(2) C13 0.049(2) 0.089(3) 0.045(2) 0.000(2) 0.0170(18) -0.033(2) C14 0.079(3) 0.051(2) 0.049(2) -0.0028(18) 0.024(2) -0.022(2) C15 0.111(4) 0.055(3) 0.066(3) -0.015(2) 0.038(3) -0.006(3) C16 0.075(3) 0.062(3) 0.074(3) -0.021(2) 0.042(3) -0.011(2) C17 0.0395(17) 0.076(3) 0.0480(18) 0.0100(18) 0.0282(15) 0.0034(17) C18 0.063(3) 0.103(4) 0.064(2) 0.023(3) 0.043(2) -0.004(2) C19 0.064(2) 0.073(3) 0.0453(19) 0.0212(18) 0.0319(18) 0.000(2) C20 0.0325(16) 0.0445(18) 0.0545(19) -0.0106(15) 0.0217(15) -0.0050(13) C21 0.0304(14) 0.054(2) 0.059(2) -0.0182(16) 0.0098(14) -0.0021(13) C22 0.0353(17) 0.050(2) 0.0442(18) -0.0141(15) 0.0085(14) 0.0071(14) C23 0.0395(16) 0.0383(16) 0.0326(14) 0.0023(12) 0.0151(13) 0.0061(13) C24 0.0396(16) 0.0515(19) 0.0354(15) 0.0017(13) 0.0214(13) -0.0059(14) C25 0.0404(17) 0.0521(19) 0.0423(16) 0.0072(14) 0.0232(14) -0.0071(14) C26 0.0434(17) 0.0304(15) 0.0445(16) 0.0073(12) 0.0230(14) -0.0056(12) C27 0.052(2) 0.0379(17) 0.0403(17) 0.0034(13) 0.0216(15) -0.0127(14) C28 0.078(3) 0.050(2) 0.0371(17) 0.0066(15) 0.0282(18) -0.0186(19) C29 0.074(2) 0.0454(19) 0.0396(17) -0.0075(14) 0.0336(17) -0.0182(18) C30 0.0427(16) 0.0302(14) 0.0422(15) 0.0035(12) 0.0274(14) 0.0011(12) C31 0.0479(17) 0.0256(14) 0.0315(14) -0.0015(11) 0.0154(13) -0.0023(12) C32 0.050(2) 0.0369(16) 0.0455(17) -0.0012(14) 0.0147(16) -0.0027(14) C33 0.063(2) 0.0407(19) 0.0432(18) -0.0103(15) 0.0078(17) -0.0102(17) C34 0.077(3) 0.0396(18) 0.0418(18) -0.0140(15) 0.0245(18) -0.0149(18) C35 0.067(2) 0.0319(15) 0.0402(16) -0.0072(13) 0.0285(16) -0.0137(15) C36 0.083(3) 0.0323(16) 0.054(2) -0.0160(15) 0.046(2) -0.0170(17) C37 0.068(2) 0.0318(16) 0.060(2) -0.0107(14) 0.0470(19) -0.0096(15) C38 0.080(3) 0.041(2) 0.095(3) -0.026(2) 0.064(3) -0.0091(19) C39 0.075(3) 0.0397(19) 0.117(4) -0.024(2) 0.071(3) -0.0068(19) C40 0.058(2) 0.0357(17) 0.084(3) -0.0029(17) 0.051(2) -0.0003(15) C41 0.0540(19) 0.0306(15) 0.0539(18) 0.0021(13) 0.0396(16) 0.0005(13) C42 0.0550(19) 0.0275(14) 0.0486(17) -0.0007(12) 0.0376(16) 0.0006(13) C43 0.0482(17) 0.0258(13) 0.0347(14) -0.0018(11) 0.0246(13) -0.0039(12) C44 0.0511(17) 0.0232(13) 0.0330(14) 0.0000(11) 0.0227(13) -0.0042(12) F25 0.0643(18) 0.210(5) 0.0664(17) -0.037(2) 0.0273(15) 0.042(2) F26 0.173(4) 0.067(2) 0.147(3) -0.024(2) 0.121(3) 0.003(2) F27 0.096(2) 0.112(3) 0.0635(16) 0.0107(16) 0.0533(17) 0.0255(19) C83 0.0353(17) 0.0418(18) 0.0459(18) 0.0034(14) 0.0131(14) -0.0024(13) F28 0.080(3) 0.109(4) 0.054(2) 0.032(2) 0.029(2) 0.041(3) F29 0.045(2) 0.082(3) 0.160(6) 0.079(4) 0.049(3) 0.015(2) F30 0.064(2) 0.057(2) 0.092(3) -0.015(2) -0.003(2) 0.0235(18) C83A 0.0353(17) 0.0418(18) 0.0459(18) 0.0034(14) 0.0131(14) -0.0024(13) F28A 0.080(3) 0.109(4) 0.054(2) 0.032(2) 0.029(2) 0.041(3) F29A 0.045(2) 0.082(3) 0.160(6) 0.079(4) 0.049(3) 0.015(2) F30A 0.064(2) 0.057(2) 0.092(3) -0.015(2) -0.003(2) 0.0235(18) F31 0.134(6) 0.106(5) 0.225(9) -0.105(6) 0.110(6) -0.066(4) F32 0.041(2) 0.123(5) 0.167(6) -0.047(4) 0.021(3) -0.025(2) F33 0.257(13) 0.047(3) 0.132(6) 0.001(3) 0.018(6) -0.075(5) F31A 0.134(6) 0.106(5) 0.225(9) -0.105(6) 0.110(6) -0.066(4) F32A 0.041(2) 0.123(5) 0.167(6) -0.047(4) 0.021(3) -0.025(2) F33A 0.257(13) 0.047(3) 0.132(6) 0.001(3) 0.018(6) -0.075(5) F34 0.166(3) 0.0548(16) 0.092(2) 0.0228(15) 0.087(2) -0.0051(18) F35 0.216(5) 0.075(2) 0.087(2) 0.0097(17) 0.103(3) 0.034(3) F36 0.104(3) 0.127(3) 0.0591(16) 0.0245(18) 0.0290(17) -0.022(2) C99 0.0412(19) 0.068(3) 0.055(2) 0.0151(19) 0.0191(17) 0.0064(18) F37 0.094(4) 0.060(3) 0.124(5) -0.003(3) 0.001(4) 0.032(3) F38 0.110(5) 0.195(8) 0.075(3) 0.075(4) 0.047(3) 0.081(5) F39 0.033(2) 0.115(4) 0.163(6) 0.073(5) 0.029(3) 0.016(2) C99A 0.0412(19) 0.068(3) 0.055(2) 0.0151(19) 0.0191(17) 0.0064(18) F37A 0.094(4) 0.060(3) 0.124(5) -0.003(3) 0.001(4) 0.032(3) F38A 0.110(5) 0.195(8) 0.075(3) 0.075(4) 0.047(3) 0.081(5) F39A 0.033(2) 0.115(4) 0.163(6) 0.073(5) 0.029(3) 0.016(2) F43 0.112(3) 0.082(2) 0.168(3) -0.064(2) 0.109(3) -0.060(2) F44 0.096(2) 0.080(2) 0.0446(12) -0.0215(13) 0.0208(13) -0.0418(17) F45 0.113(2) 0.0344(12) 0.092(2) -0.0043(12) 0.0421(18) -0.0088(14) F46 0.0596(16) 0.156(3) 0.128(3) -0.089(3) 0.0648(19) -0.0314(19) F47 0.0363(12) 0.107(2) 0.0702(16) 0.0073(16) 0.0193(11) -0.0010(13) F48 0.080(2) 0.096(2) 0.160(4) 0.045(2) 0.095(2) 0.0201(17) C77 0.0356(15) 0.0299(14) 0.0350(14) -0.0009(11) 0.0182(12) -0.0021(12) C78 0.0326(15) 0.0296(14) 0.0438(16) -0.0008(12) 0.0213(13) -0.0025(11) C79 0.0356(16) 0.0343(16) 0.0407(16) -0.0013(12) 0.0139(13) -0.0034(12) C80 0.0413(17) 0.052(2) 0.0381(17) -0.0043(15) 0.0140(14) -0.0014(15) C81 0.0436(18) 0.050(2) 0.0419(17) -0.0101(15) 0.0201(15) 0.0012(15) C82 0.0349(15) 0.0441(18) 0.0396(16) -0.0060(13) 0.0173(13) 0.0045(13) C84 0.058(2) 0.091(3) 0.0387(19) -0.005(2) 0.0201(18) 0.015(2) C85 0.0371(16) 0.0313(15) 0.0510(18) -0.0002(13) 0.0276(14) -0.0008(12) C86 0.0372(16) 0.0383(17) 0.0523(19) -0.0020(14) 0.0217(15) -0.0047(13) C87 0.048(2) 0.0389(19) 0.085(3) -0.0048(19) 0.036(2) -0.0100(16) C88 0.065(2) 0.0354(18) 0.086(3) 0.0096(18) 0.048(2) -0.0104(17) C89 0.067(2) 0.0419(19) 0.067(2) 0.0080(17) 0.049(2) -0.0005(17) C90 0.0518(19) 0.0315(15) 0.0482(17) -0.0011(13) 0.0336(16) -0.0039(13) C91 0.077(4) 0.048(3) 0.131(5) -0.010(3) 0.047(4) -0.023(3) C92 0.123(5) 0.043(2) 0.074(3) 0.014(2) 0.068(3) -0.002(2) C93 0.0328(14) 0.0350(15) 0.0332(14) -0.0014(11) 0.0195(12) -0.0011(11) C94 0.0336(15) 0.0365(15) 0.0342(14) 0.0031(12) 0.0177(12) -0.0002(12) C95 0.0356(16) 0.0491(18) 0.0393(16) 0.0058(14) 0.0182(13) 0.0043(14) C96 0.0333(17) 0.057(2) 0.056(2) 0.0080(16) 0.0250(16) 0.0014(15) C97 0.0399(18) 0.051(2) 0.0513(19) 0.0098(15) 0.0293(16) 0.0021(14) C98 0.0375(16) 0.0416(17) 0.0415(16) 0.0089(13) 0.0245(14) 0.0057(13) C101 0.0316(14) 0.0333(14) 0.0296(13) 0.0001(11) 0.0159(12) -0.0017(11) C102 0.0340(14) 0.0363(15) 0.0322(14) 0.0015(11) 0.0183(12) -0.0039(12) C103 0.0452(17) 0.0310(15) 0.0310(14) -0.0023(11) 0.0188(13) -0.0035(12) C104 0.0417(16) 0.0376(16) 0.0336(14) -0.0025(12) 0.0197(13) 0.0064(13) C105 0.0314(15) 0.0462(18) 0.0344(14) -0.0005(13) 0.0161(12) 0.0031(13) C106 0.0330(15) 0.0375(16) 0.0374(15) -0.0023(12) 0.0196(13) -0.0044(12) C107 0.062(2) 0.0442(19) 0.0480(19) -0.0088(15) 0.0318(18) -0.0123(17) C108 0.0361(17) 0.060(2) 0.0482(18) -0.0089(17) 0.0225(15) 0.0021(16) B2 0.0310(15) 0.0303(16) 0.0378(16) -0.0014(13) 0.0195(13) -0.0013(12) C100 0.053(3) 0.071(3) 0.073(3) 0.020(3) 0.042(3) -0.001(2) F40 0.124(6) 0.095(4) 0.168(7) 0.045(4) 0.116(6) 0.022(4) F41 0.045(2) 0.148(7) 0.127(5) 0.105(5) 0.021(3) -0.012(3) F42 0.197(7) 0.108(4) 0.115(5) 0.021(4) 0.082(5) -0.047(5) C200 0.053(3) 0.071(3) 0.073(3) 0.020(3) 0.042(3) -0.001(2) F40A 0.124(6) 0.095(4) 0.168(7) 0.045(4) 0.116(6) 0.022(4) F41A 0.045(2) 0.148(7) 0.127(5) 0.105(5) 0.021(3) -0.012(3) F42A 0.197(7) 0.108(4) 0.115(5) 0.021(4) 0.082(5) -0.047(5) F1 0.0453(14) 0.104(2) 0.0768(18) -0.0044(17) 0.0062(13) 0.0175(14) F2 0.0658(17) 0.105(2) 0.150(3) 0.053(2) 0.079(2) 0.0289(16) F3 0.0687(17) 0.0561(15) 0.150(3) -0.0198(17) 0.068(2) 0.0047(13) F4 0.0774(17) 0.0413(13) 0.103(2) -0.0086(13) 0.0449(16) -0.0118(12) F5 0.0687(16) 0.0649(16) 0.0620(15) 0.0109(12) 0.0005(13) -0.0273(13) F6 0.0746(17) 0.0670(16) 0.0959(19) 0.0100(14) 0.0568(16) -0.0141(13) C59 0.066(3) 0.061(3) 0.042(2) -0.0037(18) 0.011(2) 0.002(2) F7 0.129(6) 0.127(6) 0.064(4) -0.050(4) -0.032(4) 0.080(5) F8 0.156(6) 0.108(4) 0.039(2) -0.008(2) 0.028(3) -0.014(4) F9 0.105(5) 0.257(12) 0.070(4) -0.075(6) 0.039(4) -0.095(7) C59A 0.066(3) 0.061(3) 0.042(2) -0.0037(18) 0.011(2) 0.002(2) F7A 0.129(6) 0.127(6) 0.064(4) -0.050(4) -0.032(4) 0.080(5) F8A 0.156(6) 0.108(4) 0.039(2) -0.008(2) 0.028(3) -0.014(4) F9A 0.105(5) 0.257(12) 0.070(4) -0.075(6) 0.039(4) -0.095(7) F10 0.0592(16) 0.093(2) 0.103(2) -0.0131(19) 0.0136(16) 0.0361(16) F11 0.252(6) 0.101(3) 0.175(4) 0.064(3) 0.182(5) 0.091(3) F12 0.0769(19) 0.0565(16) 0.160(3) -0.0367(19) 0.062(2) -0.0084(14) C67 0.059(3) 0.092(3) 0.049(2) 0.020(2) 0.035(2) 0.013(2) F13 0.086(3) 0.107(3) 0.095(3) -0.004(2) 0.070(3) -0.027(2) F14 0.137(5) 0.094(3) 0.195(7) -0.003(4) 0.145(6) 0.007(3) F15 0.076(3) 0.249(10) 0.068(3) 0.075(4) 0.027(2) -0.023(4) C67A 0.059(3) 0.092(3) 0.049(2) 0.020(2) 0.035(2) 0.013(2) F13A 0.086(3) 0.107(3) 0.095(3) -0.004(2) 0.070(3) -0.027(2) F14A 0.137(5) 0.094(3) 0.195(7) -0.003(4) 0.145(6) 0.007(3) F15A 0.076(3) 0.249(10) 0.068(3) 0.075(4) 0.027(2) -0.023(4) F16 0.0706(18) 0.121(3) 0.0653(17) -0.0428(18) 0.0173(14) -0.0146(18) F17 0.0666(18) 0.094(2) 0.099(2) 0.0042(19) 0.0128(17) -0.0283(17) F18 0.0368(13) 0.088(2) 0.154(3) -0.056(2) 0.0080(16) 0.0081(13) F19 0.295(7) 0.092(3) 0.239(6) -0.099(4) 0.233(6) -0.095(4) F20 0.268(10) 0.068(3) 0.429(15) -0.026(5) 0.204(10) 0.046(4) F21 0.220(6) 0.120(3) 0.223(6) -0.093(4) 0.179(6) -0.107(4) C76 0.076(10) 0.061(5) 0.078(7) -0.023(3) 0.057(8) -0.032(6) F22 0.149(6) 0.152(6) 0.103(4) -0.053(4) 0.096(4) -0.041(5) F23 0.165(7) 0.174(7) 0.094(4) 0.025(4) 0.106(5) 0.049(5) F24 0.168(6) 0.072(3) 0.140(6) -0.058(3) 0.142(6) -0.057(3) C76A 0.076(10) 0.061(5) 0.078(7) -0.023(3) 0.057(8) -0.032(6) F22A 0.149(6) 0.152(6) 0.103(4) -0.053(4) 0.096(4) -0.041(5) F23A 0.165(7) 0.174(7) 0.094(4) 0.025(4) 0.106(5) 0.049(5) F24A 0.168(6) 0.072(3) 0.140(6) -0.058(3) 0.142(6) -0.057(3) C45 0.0352(15) 0.0392(16) 0.0296(14) 0.0020(11) 0.0146(12) 0.0010(12) C46 0.0342(15) 0.0366(16) 0.0402(16) -0.0023(13) 0.0164(13) -0.0042(12) C47 0.0399(17) 0.0430(17) 0.0379(15) 0.0035(13) 0.0194(14) 0.0011(13) C48 0.0509(18) 0.0307(15) 0.0375(16) 0.0072(12) 0.0225(14) 0.0075(13) C49 0.0422(17) 0.0381(16) 0.0349(15) 0.0040(12) 0.0200(13) -0.0050(13) C50 0.0368(15) 0.0386(16) 0.0382(15) 0.0039(12) 0.0208(13) 0.0003(13) C51 0.050(2) 0.046(2) 0.063(2) 0.0028(17) 0.0279(18) 0.0041(16) C52 0.053(2) 0.0393(18) 0.055(2) 0.0088(15) 0.0257(17) -0.0059(15) C53 0.0381(16) 0.0343(15) 0.0358(14) 0.0041(12) 0.0181(13) -0.0005(12) C54 0.0455(18) 0.0419(17) 0.0324(15) 0.0024(13) 0.0179(14) 0.0044(14) C55 0.0476(19) 0.0458(19) 0.0344(16) 0.0044(14) 0.0093(14) -0.0019(15) C56 0.0359(16) 0.0443(19) 0.0438(17) 0.0084(14) 0.0105(14) 0.0026(14) C57 0.0395(16) 0.0389(17) 0.0414(16) 0.0096(13) 0.0174(14) 0.0042(13) C58 0.0363(15) 0.0353(15) 0.0333(14) 0.0014(12) 0.0146(12) -0.0005(12) C60 0.0482(19) 0.0420(19) 0.059(2) 0.0104(16) 0.0277(17) 0.0113(15) C61 0.0328(14) 0.0345(15) 0.0338(14) -0.0007(12) 0.0168(12) 0.0002(12) C62 0.0355(16) 0.0457(18) 0.0381(16) 0.0074(13) 0.0194(13) 0.0049(13) C63 0.0453(18) 0.057(2) 0.0398(16) 0.0085(15) 0.0259(15) 0.0111(16) C64 0.0449(18) 0.067(2) 0.0327(15) 0.0059(15) 0.0170(14) 0.0115(17) C65 0.0390(17) 0.053(2) 0.0362(16) -0.0019(14) 0.0107(14) 0.0084(15) C66 0.0314(15) 0.0472(18) 0.0341(15) -0.0023(13) 0.0146(12) 0.0010(13) C68 0.0416(19) 0.064(2) 0.0463(19) -0.0092(18) 0.0128(16) 0.0022(17) C69 0.0374(15) 0.0374(16) 0.0344(14) -0.0029(12) 0.0198(13) -0.0019(12) C70 0.089(3) 0.0387(19) 0.067(2) -0.0111(17) 0.061(2) -0.0103(19) C71 0.118(4) 0.046(2) 0.099(4) -0.022(2) 0.090(4) -0.024(2) C72 0.118(4) 0.046(2) 0.086(3) -0.021(2) 0.083(3) -0.025(2) C73 0.073(3) 0.049(2) 0.054(2) -0.0102(16) 0.047(2) -0.0084(18) C74 0.0540(19) 0.0358(16) 0.0404(16) -0.0078(13) 0.0288(15) -0.0036(14) C75 0.165(7) 0.071(4) 0.140(6) -0.026(4) 0.125(6) -0.033(4) B1 0.0355(16) 0.0361(17) 0.0332(16) -0.0015(13) 0.0186(14) -0.0006(14) Cl1 0.1352(15) 0.0988(12) 0.0953(11) 0.0028(9) 0.0627(11) -0.0089(11) C109 0.122(6) 0.137(7) 0.101(5) -0.010(5) 0.066(5) -0.037(5) Cl2 0.1368(18) 0.1119(14) 0.0879(12) -0.0066(10) 0.0234(12) -0.0107(12) Cl3 0.196(3) 0.1238(18) 0.248(4) 0.037(2) 0.164(3) -0.0045(18) Cl4 0.298(4) 0.130(2) 0.205(3) 0.025(2) 0.194(3) 0.009(2) C110 0.095(5) 0.112(6) 0.141(7) -0.003(5) 0.062(5) -0.013(4) Cl5 0.159(6) 0.162(6) 0.148(5) -0.009(5) 0.078(5) 0.048(5) C111 0.159(6) 0.162(6) 0.148(5) -0.009(5) 0.078(5) 0.048(5) Cl6 0.159(6) 0.162(6) 0.148(5) -0.009(5) 0.078(5) 0.048(5) Cl5A 0.139(8) 0.112(6) 0.202(11) -0.002(6) 0.106(8) -0.012(5) C112 0.139(8) 0.112(6) 0.202(11) -0.002(6) 0.106(8) -0.012(5) Cl6A 0.139(8) 0.112(6) 0.202(11) -0.002(6) 0.106(8) -0.012(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 Rh1 N3 2.109(3) . ? Rh1 C6 2.110(3) . ? Rh1 C2 2.114(3) . ? Rh1 N1 2.117(3) . ? Rh1 C1 2.122(3) . ? Rh1 C5 2.135(3) . ? Rh2 N7 2.075(3) . ? Rh2 N5 2.095(3) . ? Rh2 C13 2.127(4) . ? Rh2 C14 2.128(4) . ? Rh2 C10 2.140(3) . ? Rh2 C9 2.165(4) . ? N1 C17 1.344(4) . ? N1 N2 1.358(4) . ? N2 C19 1.344(5) . ? N2 C23 1.467(4) . ? N3 C20 1.334(4) . ? N3 N4 1.361(4) . ? N4 C22 1.359(4) . ? N4 C23 1.449(4) . ? N5 C24 1.333(4) . ? N5 N6 1.355(4) . ? N6 C26 1.351(4) . ? N6 C30 1.483(4) . ? N7 C27 1.344(4) . ? N7 N8 1.359(4) . ? N8 C29 1.342(4) . ? N8 C30 1.473(4) . ? C1 C2 1.396(5) . ? C1 C8 1.527(5) . ? C1 H1 1.04(4) . ? C2 C3 1.531(6) . ? C2 H2 0.91(4) . ? C3 C4 1.530(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.513(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.385(6) . ? C5 H5 1.01(5) . ? C6 C7 1.516(6) . ? C6 H6 1.00(5) . ? C7 C8 1.520(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.398(6) . ? C9 C16 1.522(6) . ? C9 H9 0.91(5) . ? C10 C11 1.506(6) . ? C10 H10 1.06(5) . ? C11 C12 1.512(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.536(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.360(8) . ? C13 H13 0.91(6) . ? C14 C15 1.527(7) . ? C14 H14 1.12(6) . ? C15 C16 1.464(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.369(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.396(6) . ? C20 H20 0.9500 . ? C21 C22 1.349(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C31 1.516(4) . ? C23 H23 1.0000 . ? C24 C25 1.393(5) . ? C24 H24 0.9500 . ? C25 C26 1.364(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.389(5) . ? C27 H27 0.9500 . ? C28 C29 1.366(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C41 1.516(5) . ? C30 H30 1.0000 . ? C31 C32 1.371(5) . ? C31 C44 1.440(5) . ? C32 C33 1.427(5) . ? C32 H32 0.9500 . ? C33 C34 1.337(6) . ? C33 H33 0.9500 . ? C34 C35 1.427(6) . ? C34 H34 0.9500 . ? C35 C36 1.393(6) . ? C35 C44 1.443(4) . ? C36 C37 1.382(6) . ? C36 H36 0.9500 . ? C37 C38 1.431(6) . ? C37 C42 1.440(4) . ? C38 C39 1.327(7) . ? C38 H38 0.9500 . ? C39 C40 1.432(6) . ? C39 H39 0.9500 . ? C40 C41 1.376(5) . ? C40 H40 0.9500 . ? C41 C42 1.446(5) . ? C42 C43 1.399(5) . ? C43 C44 1.394(5) . ? C43 H43 0.9500 . ? F25 C84 1.310(5) . ? F26 C84 1.342(7) . ? F27 C84 1.327(5) . ? C83 F29 1.256(5) . ? C83 F30 1.329(5) . ? C83 F28 1.368(6) . ? C83 C79 1.494(5) . ? F31 C91 1.299(4) . ? F32 C91 1.299(4) . ? F33 C91 1.299(4) . ? F31A C91 1.299(4) . ? F32A C91 1.299(4) . ? F33A C91 1.299(4) . ? F34 C92 1.313(5) . ? F35 C92 1.334(6) . ? F36 C92 1.341(7) . ? C99 F39 1.297(6) . ? C99 F37 1.297(7) . ? C99 F38 1.309(7) . ? C99 C95 1.508(5) . ? F43 C107 1.316(5) . ? F44 C107 1.328(5) . ? F45 C107 1.342(5) . ? F46 C108 1.336(5) . ? F47 C108 1.299(5) . ? F48 C108 1.321(5) . ? C77 C78 1.396(4) . ? C77 C82 1.416(4) . ? C77 B2 1.641(5) . ? C78 C79 1.394(5) . ? C78 H78 0.9500 . ? C79 C80 1.393(5) . ? C80 C81 1.391(5) . ? C80 H80 0.9500 . ? C81 C82 1.390(5) . ? C81 C84 1.481(6) . ? C82 H82 0.9500 . ? C85 C90 1.395(5) . ? C85 C86 1.403(5) . ? C85 B2 1.631(5) . ? C86 C87 1.376(6) . ? C86 H86 0.9500 . ? C87 C88 1.385(7) . ? C87 C91 1.490(7) . ? C88 C89 1.383(6) . ? C88 H88 0.9500 . ? C89 C90 1.385(5) . ? C89 C92 1.503(7) . ? C90 H90 0.9500 . ? C93 C94 1.390(4) . ? C93 C98 1.398(5) . ? C93 B2 1.652(4) . ? C94 C95 1.400(5) . ? C94 H94 0.9500 . ? C95 C96 1.380(5) . ? C96 C97 1.379(5) . ? C96 H96 0.9500 . ? C97 C98 1.385(5) . ? C97 C100 1.490(5) . ? C97 C200 1.490(5) . ? C98 H98 0.9500 . ? C101 C106 1.390(4) . ? C101 C102 1.405(4) . ? C101 B2 1.648(5) . ? C102 C103 1.384(5) . ? C102 H102 0.9500 . ? C103 C104 1.395(5) . ? C103 C107 1.488(5) . ? C104 C105 1.385(5) . ? C104 H104 0.9500 . ? C105 C106 1.402(5) . ? C105 C108 1.493(5) . ? C106 H106 0.9500 . ? C100 F41 1.300(4) . ? C100 F42 1.300(4) . ? C100 F40 1.300(4) . ? C200 F40A 1.300(4) . ? C200 F42A 1.300(4) . ? C200 F41A 1.300(4) . ? F1 C51 1.343(5) . ? F2 C51 1.321(5) . ? F3 C51 1.345(5) . ? F4 C52 1.313(5) . ? F5 C52 1.330(5) . ? F6 C52 1.330(5) . ? C59 F7 1.247(7) . ? C59 F9 1.309(10) . ? C59 F8 1.345(8) . ? C59 C55 1.492(6) . ? F10 C60 1.305(5) . ? F11 C60 1.299(5) . ? F12 C60 1.310(5) . ? C67 F14 1.253(7) . ? C67 F15 1.290(6) . ? C67 F13 1.388(7) . ? C67 C63 1.512(6) . ? F16 C68 1.329(5) . ? F17 C68 1.341(6) . ? F18 C68 1.298(5) . ? F19 C75 1.216(7) . ? F20 C75 1.376(13) . ? F21 C75 1.293(8) . ? C76 F22 1.274(15) . ? C76 F23 1.31(3) . ? C76 F24 1.332(17) . ? C76 C73 1.556(8) . ? C76A F22A 1.29(2) . ? C76A F23A 1.36(3) . ? C76A F24A 1.387(18) . ? C76A C73 1.462(10) . ? C45 C50 1.394(5) . ? C45 C46 1.400(5) . ? C45 B1 1.646(5) . ? C46 C47 1.394(5) . ? C46 H46 0.9500 . ? C47 C48 1.386(5) . ? C47 C51 1.489(5) . ? C48 C49 1.391(5) . ? C48 H48 0.9500 . ? C49 C50 1.383(5) . ? C49 C52 1.500(5) . ? C50 H50 0.9500 . ? C53 C58 1.388(5) . ? C53 C54 1.398(5) . ? C53 B1 1.631(5) . ? C54 C55 1.400(5) . ? C54 H54 0.9500 . ? C55 C56 1.378(6) . ? C56 C57 1.378(5) . ? C56 H56 0.9500 . ? C57 C58 1.409(5) . ? C57 C60 1.500(5) . ? C58 H58 0.9500 . ? C61 C66 1.405(4) . ? C61 C62 1.407(5) . ? C61 B1 1.643(4) . ? C62 C63 1.380(5) . ? C62 H62 0.9500 . ? C63 C64 1.382(6) . ? C64 C65 1.372(6) . ? C64 H64 0.9500 . ? C65 C66 1.392(5) . ? C65 C68 1.496(5) . ? C66 H66 0.9500 . ? C69 C74 1.386(5) . ? C69 C70 1.398(5) . ? C69 B1 1.642(5) . ? C70 C71 1.390(6) . ? C70 H70 0.9500 . ? C71 C72 1.372(6) . ? C71 C75 1.500(7) . ? C72 C73 1.369(6) . ? C72 H72 0.9500 . ? C73 C74 1.378(5) . ? C74 H74 0.9500 . ? Cl1 C109 1.735(8) . ? C109 Cl2 1.711(8) . ? C109 H10A 0.9900 . ? C109 H10B 0.9900 . ? Cl3 C110 1.685(9) . ? Cl4 C110 1.700(10) . ? C110 H11C 0.9900 . ? C110 H11D 0.9900 . ? Cl5 C111 1.656(10) . ? C111 Cl6 1.656(10) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? Cl5A C112 1.656(10) . ? C112 Cl6A 1.656(10) . ? C112 H11G 0.9900 . ? C112 H11H 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 N3 Rh1 C6 93.63(14) . . ? N3 Rh1 C2 154.59(13) . . ? C6 Rh1 C2 97.97(15) . . ? N3 Rh1 N1 87.18(10) . . ? C6 Rh1 N1 150.74(15) . . ? C2 Rh1 N1 93.44(12) . . ? N3 Rh1 C1 166.86(12) . . ? C6 Rh1 C1 82.15(15) . . ? C2 Rh1 C1 38.46(15) . . ? N1 Rh1 C1 90.49(12) . . ? N3 Rh1 C5 94.06(13) . . ? C6 Rh1 C5 38.08(17) . . ? C2 Rh1 C5 81.65(15) . . ? N1 Rh1 C5 171.06(14) . . ? C1 Rh1 C5 90.25(14) . . ? N7 Rh2 N5 87.19(10) . . ? N7 Rh2 C13 91.83(14) . . ? N5 Rh2 C13 163.22(18) . . ? N7 Rh2 C14 93.79(14) . . ? N5 Rh2 C14 159.49(17) . . ? C13 Rh2 C14 37.3(2) . . ? N7 Rh2 C10 154.41(13) . . ? N5 Rh2 C10 90.94(13) . . ? C13 Rh2 C10 82.73(16) . . ? C14 Rh2 C10 96.73(16) . . ? N7 Rh2 C9 167.66(14) . . ? N5 Rh2 C9 94.66(13) . . ? C13 Rh2 C9 89.87(17) . . ? C14 Rh2 C9 80.24(17) . . ? C10 Rh2 C9 37.89(16) . . ? C17 N1 N2 104.6(3) . . ? C17 N1 Rh1 133.5(2) . . ? N2 N1 Rh1 121.3(2) . . ? C19 N2 N1 111.5(3) . . ? C19 N2 C23 127.3(3) . . ? N1 N2 C23 121.0(3) . . ? C20 N3 N4 105.1(3) . . ? C20 N3 Rh1 129.5(2) . . ? N4 N3 Rh1 118.64(19) . . ? C22 N4 N3 110.5(3) . . ? C22 N4 C23 128.7(3) . . ? N3 N4 C23 120.6(2) . . ? C24 N5 N6 105.8(3) . . ? C24 N5 Rh2 131.4(2) . . ? N6 N5 Rh2 122.72(18) . . ? C26 N6 N5 110.3(2) . . ? C26 N6 C30 128.2(3) . . ? N5 N6 C30 120.6(2) . . ? C27 N7 N8 105.3(3) . . ? C27 N7 Rh2 132.0(2) . . ? N8 N7 Rh2 122.76(19) . . ? C29 N8 N7 110.7(3) . . ? C29 N8 C30 126.6(3) . . ? N7 N8 C30 119.9(2) . . ? C2 C1 C8 123.1(3) . . ? C2 C1 Rh1 70.45(19) . . ? C8 C1 Rh1 113.0(2) . . ? C2 C1 H1 118(2) . . ? C8 C1 H1 115(2) . . ? Rh1 C1 H1 105(2) . . ? C1 C2 C3 125.8(3) . . ? C1 C2 Rh1 71.08(19) . . ? C3 C2 Rh1 110.2(3) . . ? C1 C2 H2 113(3) . . ? C3 C2 H2 119(3) . . ? Rh1 C2 H2 104(3) . . ? C4 C3 C2 112.3(3) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 111.2(3) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 122.8(4) . . ? C6 C5 Rh1 70.0(2) . . ? C4 C5 Rh1 113.8(3) . . ? C6 C5 H5 127(3) . . ? C4 C5 H5 108(3) . . ? Rh1 C5 H5 103(3) . . ? C5 C6 C7 125.7(4) . . ? C5 C6 Rh1 72.0(2) . . ? C7 C6 Rh1 110.0(2) . . ? C5 C6 H6 117(3) . . ? C7 C6 H6 117(3) . . ? Rh1 C6 H6 95(3) . . ? C6 C7 C8 112.8(3) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C1 111.7(3) . . ? C7 C8 H8A 109.3 . . ? C1 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C1 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C16 123.1(4) . . ? C10 C9 Rh2 70.1(2) . . ? C16 C9 Rh2 112.8(3) . . ? C10 C9 H9 120(3) . . ? C16 C9 H9 111(3) . . ? Rh2 C9 H9 112(3) . . ? C9 C10 C11 124.9(4) . . ? C9 C10 Rh2 72.0(2) . . ? C11 C10 Rh2 108.7(3) . . ? C9 C10 H10 127(2) . . ? C11 C10 H10 108(2) . . ? Rh2 C10 H10 101(2) . . ? C10 C11 C12 114.2(4) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 C13 113.1(4) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 123.1(5) . . ? C14 C13 Rh2 71.4(3) . . ? C12 C13 Rh2 111.8(3) . . ? C14 C13 H13 131(4) . . ? C12 C13 H13 106(4) . . ? Rh2 C13 H13 97(4) . . ? C13 C14 C15 127.5(4) . . ? C13 C14 Rh2 71.3(3) . . ? C15 C14 Rh2 110.4(3) . . ? C13 C14 H14 109(3) . . ? C15 C14 H14 122(3) . . ? Rh2 C14 H14 100(3) . . ? C16 C15 C14 113.1(4) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C9 112.4(4) . . ? C15 C16 H16A 109.1 . . ? C9 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C9 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N1 C17 C18 111.1(4) . . ? N1 C17 H17 124.4 . . ? C18 C17 H17 124.4 . . ? C19 C18 C17 105.6(4) . . ? C19 C18 H18 127.2 . . ? C17 C18 H18 127.2 . . ? N2 C19 C18 107.2(4) . . ? N2 C19 H19 126.4 . . ? C18 C19 H19 126.4 . . ? N3 C20 C21 110.9(4) . . ? N3 C20 H20 124.5 . . ? C21 C20 H20 124.5 . . ? C22 C21 C20 105.6(4) . . ? C22 C21 H21 127.2 . . ? C20 C21 H21 127.2 . . ? C21 C22 N4 107.8(3) . . ? C21 C22 H22 126.1 . . ? N4 C22 H22 126.1 . . ? N4 C23 N2 108.5(3) . . ? N4 C23 C31 114.2(3) . . ? N2 C23 C31 113.9(3) . . ? N4 C23 H23 106.6 . . ? N2 C23 H23 106.6 . . ? C31 C23 H23 106.6 . . ? N5 C24 C25 110.7(3) . . ? N5 C24 H24 124.6 . . ? C25 C24 H24 124.6 . . ? C26 C25 C24 105.1(3) . . ? C26 C25 H25 127.4 . . ? C24 C25 H25 127.4 . . ? N6 C26 C25 107.9(3) . . ? N6 C26 H26 126.0 . . ? C25 C26 H26 126.0 . . ? N7 C27 C28 110.7(3) . . ? N7 C27 H27 124.6 . . ? C28 C27 H27 124.6 . . ? C29 C28 C27 105.1(3) . . ? C29 C28 H28 127.5 . . ? C27 C28 H28 127.5 . . ? N8 C29 C28 108.2(3) . . ? N8 C29 H29 125.9 . . ? C28 C29 H29 125.9 . . ? N8 C30 N6 110.2(2) . . ? N8 C30 C41 110.8(2) . . ? N6 C30 C41 112.2(2) . . ? N8 C30 H30 107.8 . . ? N6 C30 H30 107.8 . . ? C41 C30 H30 107.8 . . ? C32 C31 C44 119.9(3) . . ? C32 C31 C23 120.5(3) . . ? C44 C31 C23 119.3(3) . . ? C31 C32 C33 121.3(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 122.0(3) . . ? C36 C35 C44 118.4(3) . . ? C34 C35 C44 119.7(4) . . ? C37 C36 C35 122.8(3) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 121.9(3) . . ? C36 C37 C42 119.4(3) . . ? C38 C37 C42 118.7(4) . . ? C39 C38 C37 122.3(4) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C40 120.3(4) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 120.3(4) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 120.6(3) . . ? C40 C41 C30 115.2(3) . . ? C42 C41 C30 124.1(3) . . ? C43 C42 C37 117.9(3) . . ? C43 C42 C41 124.6(3) . . ? C37 C42 C41 117.5(3) . . ? C44 C43 C42 122.8(3) . . ? C44 C43 H43 118.6 . . ? C42 C43 H43 118.6 . . ? C43 C44 C31 123.8(3) . . ? C43 C44 C35 118.6(3) . . ? C31 C44 C35 117.5(3) . . ? F29 C83 F30 109.4(5) . . ? F29 C83 F28 102.1(5) . . ? F30 C83 F28 101.2(4) . . ? F29 C83 C79 115.9(3) . . ? F30 C83 C79 113.1(3) . . ? F28 C83 C79 113.5(4) . . ? F39 C99 F37 104.4(6) . . ? F39 C99 F38 106.2(6) . . ? F37 C99 F38 104.8(6) . . ? F39 C99 C95 114.7(4) . . ? F37 C99 C95 112.9(4) . . ? F38 C99 C95 113.0(4) . . ? C78 C77 C82 115.3(3) . . ? C78 C77 B2 126.4(3) . . ? C82 C77 B2 118.3(3) . . ? C79 C78 C77 122.3(3) . . ? C79 C78 H78 118.8 . . ? C77 C78 H78 118.8 . . ? C80 C79 C78 121.4(3) . . ? C80 C79 C83 118.0(3) . . ? C78 C79 C83 120.6(3) . . ? C81 C80 C79 117.6(3) . . ? C81 C80 H80 121.2 . . ? C79 C80 H80 121.2 . . ? C82 C81 C80 120.8(3) . . ? C82 C81 C84 119.4(3) . . ? C80 C81 C84 119.8(3) . . ? C81 C82 C77 122.6(3) . . ? C81 C82 H82 118.7 . . ? C77 C82 H82 118.7 . . ? F25 C84 F27 107.4(4) . . ? F25 C84 F26 104.1(5) . . ? F27 C84 F26 104.3(4) . . ? F25 C84 C81 114.8(4) . . ? F27 C84 C81 114.1(4) . . ? F26 C84 C81 111.2(4) . . ? C90 C85 C86 115.4(3) . . ? C90 C85 B2 119.9(3) . . ? C86 C85 B2 124.7(3) . . ? C87 C86 C85 121.6(4) . . ? C87 C86 H86 119.2 . . ? C85 C86 H86 119.2 . . ? C86 C87 C88 121.9(4) . . ? C86 C87 C91 120.4(4) . . ? C88 C87 C91 117.8(4) . . ? C89 C88 C87 117.9(3) . . ? C89 C88 H88 121.0 . . ? C87 C88 H88 121.0 . . ? C88 C89 C90 120.0(4) . . ? C88 C89 C92 121.0(4) . . ? C90 C89 C92 119.1(4) . . ? C89 C90 C85 123.2(3) . . ? C89 C90 H90 118.4 . . ? C85 C90 H90 118.4 . . ? F32A C91 F33A 107.6(16) . . ? F32 C91 F31 104.8(7) . . ? F32 C91 F33 109.5(8) . . ? F31 C91 F33 97.4(8) . . ? F32A C91 F31A 92.3(13) . . ? F33A C91 F31A 114.0(17) . . ? F32 C91 C87 114.9(4) . . ? F32A C91 C87 117.1(9) . . ? F33A C91 C87 114.6(7) . . ? F31 C91 C87 113.7(4) . . ? F33 C91 C87 114.8(5) . . ? F31A C91 C87 109.4(7) . . ? F34 C92 F35 106.4(4) . . ? F34 C92 F36 105.9(5) . . ? F35 C92 F36 106.0(5) . . ? F34 C92 C89 113.8(4) . . ? F35 C92 C89 112.0(5) . . ? F36 C92 C89 112.1(4) . . ? C94 C93 C98 115.5(3) . . ? C94 C93 B2 125.8(3) . . ? C98 C93 B2 118.7(3) . . ? C93 C94 C95 121.9(3) . . ? C93 C94 H94 119.0 . . ? C95 C94 H94 119.0 . . ? C96 C95 C94 121.1(3) . . ? C96 C95 C99 119.6(3) . . ? C94 C95 C99 119.3(3) . . ? C97 C96 C95 117.8(3) . . ? C97 C96 H96 121.1 . . ? C95 C96 H96 121.1 . . ? C96 C97 C98 120.8(3) . . ? C96 C97 C100 117.7(4) . . ? C98 C97 C100 121.4(4) . . ? C96 C97 C200 120.5(4) . . ? C98 C97 C200 118.5(4) . . ? C97 C98 C93 122.8(3) . . ? C97 C98 H98 118.6 . . ? C93 C98 H98 118.6 . . ? C106 C101 C102 116.0(3) . . ? C106 C101 B2 120.3(3) . . ? C102 C101 B2 123.7(3) . . ? C103 C102 C101 122.0(3) . . ? C103 C102 H102 119.0 . . ? C101 C102 H102 119.0 . . ? C102 C103 C104 121.3(3) . . ? C102 C103 C107 120.7(3) . . ? C104 C103 C107 117.9(3) . . ? C105 C104 C103 117.6(3) . . ? C105 C104 H104 121.2 . . ? C103 C104 H104 121.2 . . ? C104 C105 C106 120.8(3) . . ? C104 C105 C108 120.0(3) . . ? C106 C105 C108 119.3(3) . . ? C101 C106 C105 122.3(3) . . ? C101 C106 H106 118.8 . . ? C105 C106 H106 118.8 . . ? F43 C107 F44 107.9(4) . . ? F43 C107 F45 105.1(4) . . ? F44 C107 F45 105.6(3) . . ? F43 C107 C103 113.3(3) . . ? F44 C107 C103 111.9(3) . . ? F45 C107 C103 112.4(3) . . ? F47 C108 F48 107.1(4) . . ? F47 C108 F46 105.8(4) . . ? F48 C108 F46 104.3(4) . . ? F47 C108 C105 114.0(3) . . ? F48 C108 C105 112.5(3) . . ? F46 C108 C105 112.4(3) . . ? C85 B2 C77 110.9(3) . . ? C85 B2 C101 107.8(2) . . ? C77 B2 C101 110.6(2) . . ? C85 B2 C93 111.0(3) . . ? C77 B2 C93 106.4(2) . . ? C101 B2 C93 110.2(2) . . ? F41 C100 F42 100.8(8) . . ? F41 C100 F40 110.3(7) . . ? F42 C100 F40 105.8(8) . . ? F41 C100 C97 114.5(5) . . ? F42 C100 C97 113.1(5) . . ? F40 C100 C97 111.6(5) . . ? F40A C200 F42A 108.4(9) . . ? F40A C200 F41A 101.4(8) . . ? F42A C200 F41A 106.3(9) . . ? F40A C200 C97 112.0(6) . . ? F42A C200 C97 113.0(6) . . ? F41A C200 C97 114.8(5) . . ? F7 C59 F9 111.0(8) . . ? F7 C59 F8 104.6(7) . . ? F9 C59 F8 100.0(7) . . ? F7 C59 C55 117.2(4) . . ? F9 C59 C55 111.5(5) . . ? F8 C59 C55 110.9(5) . . ? F14 C67 F15 110.3(6) . . ? F14 C67 F13 103.0(5) . . ? F15 C67 F13 102.3(6) . . ? F14 C67 C63 114.5(5) . . ? F15 C67 C63 114.3(4) . . ? F13 C67 C63 111.2(4) . . ? F22 C76 F23 107.1(14) . . ? F22 C76 F24 108.8(14) . . ? F23 C76 F24 106.9(10) . . ? F22 C76 C73 114.1(8) . . ? F23 C76 C73 108.9(13) . . ? F24 C76 C73 110.7(12) . . ? F22A C76A F23A 108.4(12) . . ? F22A C76A F24A 107(2) . . ? F23A C76A F24A 102.9(13) . . ? F22A C76A C73 118.3(12) . . ? F23A C76A C73 108(2) . . ? F24A C76A C73 111.3(8) . . ? C50 C45 C46 115.6(3) . . ? C50 C45 B1 122.7(3) . . ? C46 C45 B1 121.7(3) . . ? C47 C46 C45 122.3(3) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C48 C47 C46 121.0(3) . . ? C48 C47 C51 120.4(3) . . ? C46 C47 C51 118.6(3) . . ? C47 C48 C49 117.3(3) . . ? C47 C48 H48 121.4 . . ? C49 C48 H48 121.4 . . ? C50 C49 C48 121.5(3) . . ? C50 C49 C52 117.6(3) . . ? C48 C49 C52 120.8(3) . . ? C49 C50 C45 122.3(3) . . ? C49 C50 H50 118.8 . . ? C45 C50 H50 118.8 . . ? F2 C51 F1 104.6(4) . . ? F2 C51 F3 107.0(4) . . ? F1 C51 F3 104.9(4) . . ? F2 C51 C47 113.2(3) . . ? F1 C51 C47 113.0(4) . . ? F3 C51 C47 113.4(3) . . ? F4 C52 F5 108.6(4) . . ? F4 C52 F6 105.3(3) . . ? F5 C52 F6 105.3(3) . . ? F4 C52 C49 113.8(3) . . ? F5 C52 C49 111.7(3) . . ? F6 C52 C49 111.6(3) . . ? C58 C53 C54 115.7(3) . . ? C58 C53 B1 122.8(3) . . ? C54 C53 B1 121.2(3) . . ? C53 C54 C55 122.4(3) . . ? C53 C54 H54 118.8 . . ? C55 C54 H54 118.8 . . ? C56 C55 C54 120.5(3) . . ? C56 C55 C59 120.0(3) . . ? C54 C55 C59 119.5(4) . . ? C57 C56 C55 118.6(3) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C56 C57 C58 120.4(3) . . ? C56 C57 C60 121.2(3) . . ? C58 C57 C60 118.4(3) . . ? C53 C58 C57 122.3(3) . . ? C53 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? F11 C60 F10 105.9(4) . . ? F11 C60 F12 104.8(4) . . ? F10 C60 F12 104.5(4) . . ? F11 C60 C57 113.8(3) . . ? F10 C60 C57 114.1(3) . . ? F12 C60 C57 112.9(3) . . ? C66 C61 C62 115.2(3) . . ? C66 C61 B1 122.2(3) . . ? C62 C61 B1 122.4(3) . . ? C63 C62 C61 121.8(3) . . ? C63 C62 H62 119.1 . . ? C61 C62 H62 119.1 . . ? C62 C63 C64 121.7(3) . . ? C62 C63 C67 120.3(4) . . ? C64 C63 C67 118.0(3) . . ? C65 C64 C63 118.0(3) . . ? C65 C64 H64 121.0 . . ? C63 C64 H64 121.0 . . ? C64 C65 C66 120.9(3) . . ? C64 C65 C68 120.4(3) . . ? C66 C65 C68 118.7(4) . . ? C65 C66 C61 122.4(3) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? F18 C68 F16 108.7(4) . . ? F18 C68 F17 105.7(4) . . ? F16 C68 F17 102.6(4) . . ? F18 C68 C65 113.3(4) . . ? F16 C68 C65 113.4(4) . . ? F17 C68 C65 112.4(3) . . ? C74 C69 C70 115.0(3) . . ? C74 C69 B1 125.1(3) . . ? C70 C69 B1 119.8(3) . . ? C71 C70 C69 122.6(3) . . ? C71 C70 H70 118.7 . . ? C69 C70 H70 118.7 . . ? C72 C71 C70 120.1(4) . . ? C72 C71 C75 119.3(4) . . ? C70 C71 C75 120.2(4) . . ? C73 C72 C71 118.6(4) . . ? C73 C72 H72 120.7 . . ? C71 C72 H72 120.7 . . ? C72 C73 C74 120.9(3) . . ? C72 C73 C76A 124.0(11) . . ? C74 C73 C76A 114.9(10) . . ? C72 C73 C76 113.6(7) . . ? C74 C73 C76 124.6(7) . . ? C73 C74 C69 122.8(3) . . ? C73 C74 H74 118.6 . . ? C69 C74 H74 118.6 . . ? F19 C75 F21 112.4(7) . . ? F19 C75 F20 104.3(8) . . ? F21 C75 F20 97.4(6) . . ? F19 C75 C71 116.9(5) . . ? F21 C75 C71 115.9(6) . . ? F20 C75 C71 107.0(7) . . ? C53 B1 C69 104.0(3) . . ? C53 B1 C61 112.4(3) . . ? C69 B1 C61 110.6(3) . . ? C53 B1 C45 112.9(3) . . ? C69 B1 C45 112.9(3) . . ? C61 B1 C45 104.3(2) . . ? Cl2 C109 Cl1 114.5(5) . . ? Cl2 C109 H10A 108.6 . . ? Cl1 C109 H10A 108.6 . . ? Cl2 C109 H10B 108.6 . . ? Cl1 C109 H10B 108.6 . . ? H10A C109 H10B 107.6 . . ? Cl3 C110 Cl4 115.4(5) . . ? Cl3 C110 H11C 108.4 . . ? Cl4 C110 H11C 108.4 . . ? Cl3 C110 H11D 108.4 . . ? Cl4 C110 H11D 108.4 . . ? H11C C110 H11D 107.5 . . ? Cl6 C111 Cl5 120.3(14) . . ? Cl6 C111 H11E 107.3 . . ? Cl5 C111 H11E 107.3 . . ? Cl6 C111 H11F 107.3 . . ? Cl5 C111 H11F 107.3 . . ? H11E C111 H11F 106.9 . . ? Cl6A C112 Cl5A 116.5(16) . . ? Cl6A C112 H11G 108.2 . . ? Cl5A C112 H11G 108.2 . . ? Cl6A C112 H11H 108.2 . . ? Cl5A C112 H11H 108.2 . . ? H11G C112 H11H 107.3 . . ? 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 N3 Rh1 N1 C17 155.1(4) . . . . ? C6 Rh1 N1 C17 -112.5(4) . . . . ? C2 Rh1 N1 C17 0.6(4) . . . . ? C1 Rh1 N1 C17 -37.8(4) . . . . ? N3 Rh1 N1 N2 -35.6(2) . . . . ? C6 Rh1 N1 N2 56.8(4) . . . . ? C2 Rh1 N1 N2 169.8(3) . . . . ? C1 Rh1 N1 N2 131.5(3) . . . . ? C17 N1 N2 C19 2.0(4) . . . . ? Rh1 N1 N2 C19 -170.0(3) . . . . ? C17 N1 N2 C23 177.1(3) . . . . ? Rh1 N1 N2 C23 5.1(4) . . . . ? C6 Rh1 N3 C20 81.2(3) . . . . ? C2 Rh1 N3 C20 -36.0(5) . . . . ? N1 Rh1 N3 C20 -128.1(3) . . . . ? C1 Rh1 N3 C20 151.9(5) . . . . ? C5 Rh1 N3 C20 43.1(3) . . . . ? C6 Rh1 N3 N4 -132.2(2) . . . . ? C2 Rh1 N3 N4 110.6(3) . . . . ? N1 Rh1 N3 N4 18.5(2) . . . . ? C1 Rh1 N3 N4 -61.5(7) . . . . ? C5 Rh1 N3 N4 -170.3(2) . . . . ? C20 N3 N4 C22 1.2(3) . . . . ? Rh1 N3 N4 C22 -152.7(2) . . . . ? C20 N3 N4 C23 -176.3(3) . . . . ? Rh1 N3 N4 C23 29.8(3) . . . . ? N7 Rh2 N5 C24 -153.6(3) . . . . ? C13 Rh2 N5 C24 119.4(5) . . . . ? C14 Rh2 N5 C24 -60.3(5) . . . . ? C10 Rh2 N5 C24 51.9(3) . . . . ? C9 Rh2 N5 C24 14.2(3) . . . . ? N7 Rh2 N5 N6 30.7(2) . . . . ? C13 Rh2 N5 N6 -56.4(6) . . . . ? C14 Rh2 N5 N6 124.0(4) . . . . ? C10 Rh2 N5 N6 -123.8(2) . . . . ? C9 Rh2 N5 N6 -161.6(2) . . . . ? C24 N5 N6 C26 -3.0(3) . . . . ? Rh2 N5 N6 C26 173.7(2) . . . . ? C24 N5 N6 C30 -173.0(3) . . . . ? Rh2 N5 N6 C30 3.7(4) . . . . ? N5 Rh2 N7 C27 154.1(3) . . . . ? C13 Rh2 N7 C27 -42.7(4) . . . . ? C14 Rh2 N7 C27 -5.4(4) . . . . ? C10 Rh2 N7 C27 -119.6(4) . . . . ? C9 Rh2 N7 C27 55.1(8) . . . . ? N5 Rh2 N7 N8 -23.9(2) . . . . ? C13 Rh2 N7 N8 139.3(3) . . . . ? C14 Rh2 N7 N8 176.6(3) . . . . ? C10 Rh2 N7 N8 62.4(4) . . . . ? C9 Rh2 N7 N8 -122.9(6) . . . . ? C27 N7 N8 C29 2.3(4) . . . . ? Rh2 N7 N8 C29 -179.2(3) . . . . ? C27 N7 N8 C30 164.3(3) . . . . ? Rh2 N7 N8 C30 -17.2(4) . . . . ? N3 Rh1 C1 C2 174.6(5) . . . . ? C6 Rh1 C1 C2 -113.5(2) . . . . ? N1 Rh1 C1 C2 94.9(2) . . . . ? C5 Rh1 C1 C2 -76.2(2) . . . . ? N3 Rh1 C1 C8 -66.9(7) . . . . ? C6 Rh1 C1 C8 5.1(3) . . . . ? C2 Rh1 C1 C8 118.6(4) . . . . ? N1 Rh1 C1 C8 -146.5(3) . . . . ? C5 Rh1 C1 C8 42.4(3) . . . . ? C8 C1 C2 C3 -3.5(5) . . . . ? Rh1 C1 C2 C3 101.7(4) . . . . ? C8 C1 C2 Rh1 -105.2(3) . . . . ? N3 Rh1 C2 C1 -177.1(3) . . . . ? C6 Rh1 C2 C1 66.5(2) . . . . ? N1 Rh1 C2 C1 -86.4(2) . . . . ? C5 Rh1 C2 C1 101.1(2) . . . . ? N3 Rh1 C2 C3 60.7(4) . . . . ? C6 Rh1 C2 C3 -55.6(3) . . . . ? N1 Rh1 C2 C3 151.4(3) . . . . ? C1 Rh1 C2 C3 -122.1(4) . . . . ? C5 Rh1 C2 C3 -21.1(3) . . . . ? C1 C2 C3 C4 -45.0(5) . . . . ? Rh1 C2 C3 C4 35.8(4) . . . . ? C2 C3 C4 C5 -33.1(5) . . . . ? C3 C4 C5 C6 95.8(5) . . . . ? C3 C4 C5 Rh1 15.0(5) . . . . ? N3 Rh1 C5 C6 90.7(2) . . . . ? C2 Rh1 C5 C6 -114.5(2) . . . . ? C1 Rh1 C5 C6 -76.9(2) . . . . ? N3 Rh1 C5 C4 -151.4(3) . . . . ? C6 Rh1 C5 C4 117.9(4) . . . . ? C2 Rh1 C5 C4 3.4(3) . . . . ? C1 Rh1 C5 C4 41.1(3) . . . . ? C4 C5 C6 C7 -4.0(6) . . . . ? Rh1 C5 C6 C7 102.1(3) . . . . ? C4 C5 C6 Rh1 -106.1(4) . . . . ? N3 Rh1 C6 C5 -92.0(2) . . . . ? C2 Rh1 C6 C5 65.4(2) . . . . ? N1 Rh1 C6 C5 177.3(2) . . . . ? C1 Rh1 C6 C5 100.6(2) . . . . ? N3 Rh1 C6 C7 145.7(3) . . . . ? C2 Rh1 C6 C7 -57.0(3) . . . . ? N1 Rh1 C6 C7 55.0(4) . . . . ? C1 Rh1 C6 C7 -21.8(3) . . . . ? C5 Rh1 C6 C7 -122.3(4) . . . . ? C5 C6 C7 C8 -46.3(5) . . . . ? Rh1 C6 C7 C8 35.4(4) . . . . ? C6 C7 C8 C1 -31.6(5) . . . . ? C2 C1 C8 C7 93.6(4) . . . . ? Rh1 C1 C8 C7 12.7(4) . . . . ? N7 Rh2 C9 C10 -176.3(5) . . . . ? N5 Rh2 C9 C10 85.5(2) . . . . ? C13 Rh2 C9 C10 -78.3(3) . . . . ? C14 Rh2 C9 C10 -114.5(3) . . . . ? N7 Rh2 C9 C16 -57.7(8) . . . . ? N5 Rh2 C9 C16 -155.9(3) . . . . ? C13 Rh2 C9 C16 40.3(4) . . . . ? C14 Rh2 C9 C16 4.1(3) . . . . ? C10 Rh2 C9 C16 118.6(4) . . . . ? C16 C9 C10 C11 -4.1(6) . . . . ? Rh2 C9 C10 C11 100.7(4) . . . . ? C16 C9 C10 Rh2 -104.8(4) . . . . ? N7 Rh2 C10 C9 178.2(3) . . . . ? N5 Rh2 C10 C9 -96.4(2) . . . . ? C13 Rh2 C10 C9 99.2(3) . . . . ? C14 Rh2 C10 C9 64.6(3) . . . . ? N7 Rh2 C10 C11 56.5(5) . . . . ? N5 Rh2 C10 C11 142.0(3) . . . . ? C13 Rh2 C10 C11 -22.4(3) . . . . ? C14 Rh2 C10 C11 -57.1(3) . . . . ? C9 Rh2 C10 C11 -121.7(4) . . . . ? C9 C10 C11 C12 -46.7(6) . . . . ? Rh2 C10 C11 C12 34.1(5) . . . . ? C10 C11 C12 C13 -28.7(7) . . . . ? C11 C12 C13 C14 90.0(7) . . . . ? C11 C12 C13 Rh2 8.6(7) . . . . ? N7 Rh2 C13 C14 93.9(3) . . . . ? N5 Rh2 C13 C14 -179.9(4) . . . . ? C10 Rh2 C13 C14 -111.2(3) . . . . ? C9 Rh2 C13 C14 -73.9(3) . . . . ? N7 Rh2 C13 C12 -147.1(4) . . . . ? N5 Rh2 C13 C12 -60.7(7) . . . . ? C14 Rh2 C13 C12 119.1(5) . . . . ? C10 Rh2 C13 C12 7.8(4) . . . . ? C9 Rh2 C13 C12 45.2(4) . . . . ? C12 C13 C14 C15 -2.6(7) . . . . ? Rh2 C13 C14 C15 101.7(5) . . . . ? C12 C13 C14 Rh2 -104.3(4) . . . . ? N7 Rh2 C14 C13 -88.0(3) . . . . ? N5 Rh2 C14 C13 179.8(3) . . . . ? C10 Rh2 C14 C13 68.6(3) . . . . ? C9 Rh2 C14 C13 102.8(3) . . . . ? N7 Rh2 C14 C15 147.9(4) . . . . ? N5 Rh2 C14 C15 55.8(6) . . . . ? C13 Rh2 C14 C15 -124.0(5) . . . . ? C10 Rh2 C14 C15 -55.4(4) . . . . ? C9 Rh2 C14 C15 -21.2(4) . . . . ? C13 C14 C15 C16 -44.9(7) . . . . ? Rh2 C14 C15 C16 36.6(6) . . . . ? C14 C15 C16 C9 -33.6(7) . . . . ? C10 C9 C16 C15 95.2(5) . . . . ? Rh2 C9 C16 C15 14.8(5) . . . . ? N2 N1 C17 C18 -0.9(5) . . . . ? Rh1 N1 C17 C18 169.7(3) . . . . ? N1 C17 C18 C19 -0.5(6) . . . . ? N1 N2 C19 C18 -2.3(5) . . . . ? C23 N2 C19 C18 -177.0(4) . . . . ? C17 C18 C19 N2 1.7(5) . . . . ? N4 N3 C20 C21 0.0(4) . . . . ? Rh1 N3 C20 C21 150.0(3) . . . . ? N3 C20 C21 C22 -1.1(5) . . . . ? C20 C21 C22 N4 1.8(5) . . . . ? N3 N4 C22 C21 -1.9(4) . . . . ? C23 N4 C22 C21 175.3(3) . . . . ? C22 N4 C23 N2 109.3(3) . . . . ? N3 N4 C23 N2 -73.8(3) . . . . ? C22 N4 C23 C31 -122.6(3) . . . . ? N3 N4 C23 C31 54.4(4) . . . . ? C19 N2 C23 N4 -133.8(4) . . . . ? N1 N2 C23 N4 52.0(4) . . . . ? C19 N2 C23 C31 97.9(4) . . . . ? N1 N2 C23 C31 -76.4(4) . . . . ? N6 N5 C24 C25 2.4(4) . . . . ? Rh2 N5 C24 C25 -173.9(2) . . . . ? N5 C24 C25 C26 -0.9(4) . . . . ? N5 N6 C26 C25 2.5(4) . . . . ? C30 N6 C26 C25 171.6(3) . . . . ? C24 C25 C26 N6 -0.9(4) . . . . ? N8 N7 C27 C28 -1.3(4) . . . . ? Rh2 N7 C27 C28 -179.6(3) . . . . ? N7 C27 C28 C29 -0.1(5) . . . . ? N7 N8 C29 C28 -2.5(5) . . . . ? C30 N8 C29 C28 -163.0(3) . . . . ? C27 C28 C29 N8 1.6(5) . . . . ? C29 N8 C30 N6 -137.3(3) . . . . ? N7 N8 C30 N6 63.8(4) . . . . ? C29 N8 C30 C41 -12.5(5) . . . . ? N7 N8 C30 C41 -171.4(3) . . . . ? C26 N6 C30 N8 136.1(3) . . . . ? N5 N6 C30 N8 -55.8(3) . . . . ? C26 N6 C30 C41 12.1(4) . . . . ? N5 N6 C30 C41 -179.8(3) . . . . ? N4 C23 C31 C32 -118.1(3) . . . . ? N2 C23 C31 C32 7.2(4) . . . . ? N4 C23 C31 C44 67.7(4) . . . . ? N2 C23 C31 C44 -166.9(3) . . . . ? C44 C31 C32 C33 -2.5(5) . . . . ? C23 C31 C32 C33 -176.7(3) . . . . ? C31 C32 C33 C34 4.4(6) . . . . ? C32 C33 C34 C35 -1.1(6) . . . . ? C33 C34 C35 C36 174.2(4) . . . . ? C33 C34 C35 C44 -3.9(6) . . . . ? C34 C35 C36 C37 -178.8(3) . . . . ? C44 C35 C36 C37 -0.7(5) . . . . ? C35 C36 C37 C38 175.2(4) . . . . ? C35 C36 C37 C42 -3.3(5) . . . . ? C36 C37 C38 C39 179.7(4) . . . . ? C42 C37 C38 C39 -1.8(6) . . . . ? C37 C38 C39 C40 -1.4(7) . . . . ? C38 C39 C40 C41 0.7(7) . . . . ? C39 C40 C41 C42 3.2(5) . . . . ? C39 C40 C41 C30 -172.1(3) . . . . ? N8 C30 C41 C40 114.9(3) . . . . ? N6 C30 C41 C40 -121.5(3) . . . . ? N8 C30 C41 C42 -60.2(4) . . . . ? N6 C30 C41 C42 63.4(4) . . . . ? C36 C37 C42 C43 3.2(5) . . . . ? C38 C37 C42 C43 -175.3(3) . . . . ? C36 C37 C42 C41 -175.9(3) . . . . ? C38 C37 C42 C41 5.5(5) . . . . ? C40 C41 C42 C43 174.6(3) . . . . ? C30 C41 C42 C43 -10.5(5) . . . . ? C40 C41 C42 C37 -6.3(5) . . . . ? C30 C41 C42 C37 168.6(3) . . . . ? C37 C42 C43 C44 0.8(4) . . . . ? C41 C42 C43 C44 179.9(3) . . . . ? C42 C43 C44 C31 172.3(3) . . . . ? C42 C43 C44 C35 -4.8(4) . . . . ? C32 C31 C44 C43 -179.5(3) . . . . ? C23 C31 C44 C43 -5.3(4) . . . . ? C32 C31 C44 C35 -2.4(4) . . . . ? C23 C31 C44 C35 171.8(3) . . . . ? C36 C35 C44 C43 4.7(4) . . . . ? C34 C35 C44 C43 -177.2(3) . . . . ? C36 C35 C44 C31 -172.6(3) . . . . ? C34 C35 C44 C31 5.5(5) . . . . ? C82 C77 C78 C79 -1.4(5) . . . . ? B2 C77 C78 C79 177.8(3) . . . . ? C77 C78 C79 C80 -0.4(5) . . . . ? C77 C78 C79 C83 -178.1(3) . . . . ? F29 C83 C79 C80 103.8(6) . . . . ? F30 C83 C79 C80 -128.6(5) . . . . ? F28 C83 C79 C80 -14.0(5) . . . . ? F29 C83 C79 C78 -78.5(6) . . . . ? F30 C83 C79 C78 49.1(6) . . . . ? F28 C83 C79 C78 163.7(4) . . . . ? C78 C79 C80 C81 2.5(5) . . . . ? C83 C79 C80 C81 -179.8(3) . . . . ? C79 C80 C81 C82 -2.6(6) . . . . ? C79 C80 C81 C84 178.6(4) . . . . ? C80 C81 C82 C77 0.7(6) . . . . ? C84 C81 C82 C77 179.5(4) . . . . ? C78 C77 C82 C81 1.3(5) . . . . ? B2 C77 C82 C81 -178.0(3) . . . . ? C82 C81 C84 F25 -25.2(7) . . . . ? C80 C81 C84 F25 153.6(5) . . . . ? C82 C81 C84 F27 -149.8(4) . . . . ? C80 C81 C84 F27 29.0(6) . . . . ? C82 C81 C84 F26 92.6(5) . . . . ? C80 C81 C84 F26 -88.6(5) . . . . ? C90 C85 C86 C87 -1.0(5) . . . . ? B2 C85 C86 C87 178.5(3) . . . . ? C85 C86 C87 C88 -1.3(6) . . . . ? C85 C86 C87 C91 179.1(4) . . . . ? C86 C87 C88 C89 1.8(7) . . . . ? C91 C87 C88 C89 -178.5(4) . . . . ? C87 C88 C89 C90 -0.1(6) . . . . ? C87 C88 C89 C92 180.0(4) . . . . ? C88 C89 C90 C85 -2.3(6) . . . . ? C92 C89 C90 C85 177.6(4) . . . . ? C86 C85 C90 C89 2.8(5) . . . . ? B2 C85 C90 C89 -176.7(3) . . . . ? C86 C87 C91 F32 -67.5(8) . . . . ? C88 C87 C91 F32 112.8(7) . . . . ? C86 C87 C91 F32A 126.9(15) . . . . ? C88 C87 C91 F32A -52.8(15) . . . . ? C86 C87 C91 F33A -1(2) . . . . ? C88 C87 C91 F33A 180(2) . . . . ? C86 C87 C91 F31 53.2(8) . . . . ? C88 C87 C91 F31 -126.5(7) . . . . ? C86 C87 C91 F33 164.2(8) . . . . ? C88 C87 C91 F33 -15.5(10) . . . . ? C86 C87 C91 F31A -130.0(12) . . . . ? C88 C87 C91 F31A 50.3(12) . . . . ? C88 C89 C92 F34 5.0(7) . . . . ? C90 C89 C92 F34 -175.0(4) . . . . ? C88 C89 C92 F35 -115.8(5) . . . . ? C90 C89 C92 F35 64.3(6) . . . . ? C88 C89 C92 F36 125.2(5) . . . . ? C90 C89 C92 F36 -54.8(6) . . . . ? C98 C93 C94 C95 1.1(5) . . . . ? B2 C93 C94 C95 179.4(3) . . . . ? C93 C94 C95 C96 0.0(5) . . . . ? C93 C94 C95 C99 -179.5(3) . . . . ? F39 C99 C95 C96 7.0(9) . . . . ? F37 C99 C95 C96 -112.5(8) . . . . ? F38 C99 C95 C96 128.9(8) . . . . ? F39 C99 C95 C94 -173.5(7) . . . . ? F37 C99 C95 C94 67.0(8) . . . . ? F38 C99 C95 C94 -51.6(9) . . . . ? C94 C95 C96 C97 -0.8(6) . . . . ? C99 C95 C96 C97 178.7(4) . . . . ? C95 C96 C97 C98 0.4(6) . . . . ? C95 C96 C97 C100 176.6(4) . . . . ? C95 C96 C97 C200 -174.3(5) . . . . ? C96 C97 C98 C93 0.8(6) . . . . ? C100 C97 C98 C93 -175.3(4) . . . . ? C200 C97 C98 C93 175.6(4) . . . . ? C94 C93 C98 C97 -1.5(5) . . . . ? B2 C93 C98 C97 -179.9(3) . . . . ? C106 C101 C102 C103 -2.7(4) . . . . ? B2 C101 C102 C103 178.2(3) . . . . ? C101 C102 C103 C104 0.8(5) . . . . ? C101 C102 C103 C107 179.2(3) . . . . ? C102 C103 C104 C105 1.1(5) . . . . ? C107 C103 C104 C105 -177.4(3) . . . . ? C103 C104 C105 C106 -1.0(5) . . . . ? C103 C104 C105 C108 178.3(3) . . . . ? C102 C101 C106 C105 2.8(5) . . . . ? B2 C101 C106 C105 -178.0(3) . . . . ? C104 C105 C106 C101 -1.1(5) . . . . ? C108 C105 C106 C101 179.6(3) . . . . ? C102 C103 C107 F43 11.8(5) . . . . ? C104 C103 C107 F43 -169.7(4) . . . . ? C102 C103 C107 F44 -110.6(4) . . . . ? C104 C103 C107 F44 67.9(5) . . . . ? C102 C103 C107 F45 130.8(4) . . . . ? C104 C103 C107 F45 -50.8(4) . . . . ? C104 C105 C108 F47 99.2(4) . . . . ? C106 C105 C108 F47 -81.5(4) . . . . ? C104 C105 C108 F48 -138.5(4) . . . . ? C106 C105 C108 F48 40.8(5) . . . . ? C104 C105 C108 F46 -21.2(5) . . . . ? C106 C105 C108 F46 158.2(4) . . . . ? C90 C85 B2 C77 -177.1(3) . . . . ? C86 C85 B2 C77 3.5(4) . . . . ? C90 C85 B2 C101 -55.9(4) . . . . ? C86 C85 B2 C101 124.7(3) . . . . ? C90 C85 B2 C93 64.9(4) . . . . ? C86 C85 B2 C93 -114.6(3) . . . . ? C78 C77 B2 C85 100.2(4) . . . . ? C82 C77 B2 C85 -80.6(3) . . . . ? C78 C77 B2 C101 -19.3(4) . . . . ? C82 C77 B2 C101 159.9(3) . . . . ? C78 C77 B2 C93 -139.0(3) . . . . ? C82 C77 B2 C93 40.2(4) . . . . ? C106 C101 B2 C85 -45.6(4) . . . . ? C102 C101 B2 C85 133.5(3) . . . . ? C106 C101 B2 C77 75.8(3) . . . . ? C102 C101 B2 C77 -105.1(3) . . . . ? C106 C101 B2 C93 -166.9(3) . . . . ? C102 C101 B2 C93 12.2(4) . . . . ? C94 C93 B2 C85 -7.4(4) . . . . ? C98 C93 B2 C85 170.8(3) . . . . ? C94 C93 B2 C77 -128.2(3) . . . . ? C98 C93 B2 C77 50.1(4) . . . . ? C94 C93 B2 C101 111.9(3) . . . . ? C98 C93 B2 C101 -69.8(4) . . . . ? C96 C97 C100 F41 169.0(9) . . . . ? C98 C97 C100 F41 -14.8(11) . . . . ? C200 C97 C100 F41 57(3) . . . . ? C96 C97 C100 F42 -76.3(9) . . . . ? C98 C97 C100 F42 99.9(9) . . . . ? C200 C97 C100 F42 172(3) . . . . ? C96 C97 C100 F40 42.8(9) . . . . ? C98 C97 C100 F40 -141.0(8) . . . . ? C200 C97 C100 F40 -69(3) . . . . ? C96 C97 C200 F40A -138.9(9) . . . . ? C98 C97 C200 F40A 46.3(10) . . . . ? C100 C97 C200 F40A -66(3) . . . . ? C96 C97 C200 F42A 98.3(10) . . . . ? C98 C97 C200 F42A -76.5(10) . . . . ? C100 C97 C200 F42A 171(4) . . . . ? C96 C97 C200 F41A -23.9(12) . . . . ? C98 C97 C200 F41A 161.2(11) . . . . ? C100 C97 C200 F41A 49(3) . . . . ? C50 C45 C46 C47 1.4(5) . . . . ? B1 C45 C46 C47 178.4(3) . . . . ? C45 C46 C47 C48 -0.2(5) . . . . ? C45 C46 C47 C51 177.8(3) . . . . ? C46 C47 C48 C49 -0.3(5) . . . . ? C51 C47 C48 C49 -178.2(3) . . . . ? C47 C48 C49 C50 -0.6(5) . . . . ? C47 C48 C49 C52 176.1(3) . . . . ? C48 C49 C50 C45 2.0(5) . . . . ? C52 C49 C50 C45 -174.8(3) . . . . ? C46 C45 C50 C49 -2.3(5) . . . . ? B1 C45 C50 C49 -179.3(3) . . . . ? C48 C47 C51 F2 128.8(4) . . . . ? C46 C47 C51 F2 -49.3(5) . . . . ? C48 C47 C51 F1 -112.5(4) . . . . ? C46 C47 C51 F1 69.5(5) . . . . ? C48 C47 C51 F3 6.6(5) . . . . ? C46 C47 C51 F3 -171.4(4) . . . . ? C50 C49 C52 F4 179.8(3) . . . . ? C48 C49 C52 F4 3.0(5) . . . . ? C50 C49 C52 F5 56.5(5) . . . . ? C48 C49 C52 F5 -120.4(4) . . . . ? C50 C49 C52 F6 -61.1(4) . . . . ? C48 C49 C52 F6 122.1(4) . . . . ? C58 C53 C54 C55 -2.2(5) . . . . ? B1 C53 C54 C55 -175.8(3) . . . . ? C53 C54 C55 C56 3.4(6) . . . . ? C53 C54 C55 C59 -177.2(4) . . . . ? F7 C59 C55 C56 -167.9(10) . . . . ? F9 C59 C55 C56 -38.5(9) . . . . ? F8 C59 C55 C56 72.1(8) . . . . ? F7 C59 C55 C54 12.7(11) . . . . ? F9 C59 C55 C54 142.1(8) . . . . ? F8 C59 C55 C54 -107.3(7) . . . . ? C54 C55 C56 C57 -1.6(6) . . . . ? C59 C55 C56 C57 179.0(4) . . . . ? C55 C56 C57 C58 -1.1(5) . . . . ? C55 C56 C57 C60 178.6(3) . . . . ? C54 C53 C58 C57 -0.6(5) . . . . ? B1 C53 C58 C57 173.0(3) . . . . ? C56 C57 C58 C53 2.2(5) . . . . ? C60 C57 C58 C53 -177.5(3) . . . . ? C56 C57 C60 F11 113.2(5) . . . . ? C58 C57 C60 F11 -67.1(5) . . . . ? C56 C57 C60 F10 -8.5(5) . . . . ? C58 C57 C60 F10 171.2(4) . . . . ? C56 C57 C60 F12 -127.5(4) . . . . ? C58 C57 C60 F12 52.2(5) . . . . ? C66 C61 C62 C63 1.1(5) . . . . ? B1 C61 C62 C63 177.2(3) . . . . ? C61 C62 C63 C64 0.0(6) . . . . ? C61 C62 C63 C67 178.7(4) . . . . ? F14 C67 C63 C62 -89.9(7) . . . . ? F15 C67 C63 C62 141.5(7) . . . . ? F13 C67 C63 C62 26.3(6) . . . . ? F14 C67 C63 C64 88.8(6) . . . . ? F15 C67 C63 C64 -39.8(8) . . . . ? F13 C67 C63 C64 -154.9(4) . . . . ? C62 C63 C64 C65 -0.8(6) . . . . ? C67 C63 C64 C65 -179.5(4) . . . . ? C63 C64 C65 C66 0.4(6) . . . . ? C63 C64 C65 C68 179.1(4) . . . . ? C64 C65 C66 C61 0.8(6) . . . . ? C68 C65 C66 C61 -177.9(3) . . . . ? C62 C61 C66 C65 -1.5(5) . . . . ? B1 C61 C66 C65 -177.7(3) . . . . ? C64 C65 C68 F18 109.3(5) . . . . ? C66 C65 C68 F18 -72.0(5) . . . . ? C64 C65 C68 F16 -15.1(6) . . . . ? C66 C65 C68 F16 163.5(4) . . . . ? C64 C65 C68 F17 -130.9(4) . . . . ? C66 C65 C68 F17 47.7(5) . . . . ? C74 C69 C70 C71 -2.0(7) . . . . ? B1 C69 C70 C71 -178.3(5) . . . . ? C69 C70 C71 C72 1.3(9) . . . . ? C69 C70 C71 C75 -171.6(6) . . . . ? C70 C71 C72 C73 0.9(9) . . . . ? C75 C71 C72 C73 173.8(6) . . . . ? C71 C72 C73 C74 -2.3(8) . . . . ? C71 C72 C73 C76A 173.5(12) . . . . ? C71 C72 C73 C76 -171.9(11) . . . . ? F22A C76A C73 C72 -96.8(17) . . . . ? F23A C76A C73 C72 139.7(13) . . . . ? F24A C76A C73 C72 27(2) . . . . ? F22A C76A C73 C74 79(2) . . . . ? F23A C76A C73 C74 -44.2(15) . . . . ? F24A C76A C73 C74 -156.6(15) . . . . ? F22A C76A C73 C76 -151(9) . . . . ? F23A C76A C73 C76 85(7) . . . . ? F24A C76A C73 C76 -27(6) . . . . ? F22 C76 C73 C72 47(2) . . . . ? F23 C76 C73 C72 -72.8(10) . . . . ? F24 C76 C73 C72 169.9(11) . . . . ? F22 C76 C73 C74 -122.4(14) . . . . ? F23 C76 C73 C74 118.0(11) . . . . ? F24 C76 C73 C74 0.8(19) . . . . ? F22 C76 C73 C76A 179(9) . . . . ? F23 C76 C73 C76A 60(7) . . . . ? F24 C76 C73 C76A -58(6) . . . . ? C72 C73 C74 C69 1.6(7) . . . . ? C76A C73 C74 C69 -174.6(11) . . . . ? C76 C73 C74 C69 170.0(10) . . . . ? C70 C69 C74 C73 0.6(6) . . . . ? B1 C69 C74 C73 176.7(4) . . . . ? C72 C71 C75 F19 -170.9(8) . . . . ? C70 C71 C75 F19 2.0(12) . . . . ? C72 C71 C75 F21 -34.7(11) . . . . ? C70 C71 C75 F21 138.2(7) . . . . ? C72 C71 C75 F20 72.6(9) . . . . ? C70 C71 C75 F20 -114.5(7) . . . . ? C58 C53 B1 C69 -87.7(3) . . . . ? C54 C53 B1 C69 85.5(4) . . . . ? C58 C53 B1 C61 31.9(4) . . . . ? C54 C53 B1 C61 -154.9(3) . . . . ? C58 C53 B1 C45 149.6(3) . . . . ? C54 C53 B1 C45 -37.2(4) . . . . ? C74 C69 B1 C53 -97.6(4) . . . . ? C70 C69 B1 C53 78.4(4) . . . . ? C74 C69 B1 C61 141.6(3) . . . . ? C70 C69 B1 C61 -42.5(4) . . . . ? C74 C69 B1 C45 25.1(4) . . . . ? C70 C69 B1 C45 -158.9(3) . . . . ? C66 C61 B1 C53 -143.7(3) . . . . ? C62 C61 B1 C53 40.5(4) . . . . ? C66 C61 B1 C69 -28.0(4) . . . . ? C62 C61 B1 C69 156.2(3) . . . . ? C66 C61 B1 C45 93.7(3) . . . . ? C62 C61 B1 C45 -82.2(4) . . . . ? C50 C45 B1 C53 -25.4(4) . . . . ? C46 C45 B1 C53 157.8(3) . . . . ? C50 C45 B1 C69 -143.0(3) . . . . ? C46 C45 B1 C69 40.2(4) . . . . ? C50 C45 B1 C61 96.9(3) . . . . ? C46 C45 B1 C61 -79.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.848 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.066 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 798127' #TrackingRef '- NEW all-in-one CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 Ir2 N8, 2(C32 H12 B F24), C H2 Cl2' _chemical_formula_sum 'C101 H68 B2 Cl2 F48 Ir2 N8' _chemical_formula_weight 2782.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.5673(1) _cell_length_b 17.6438(2) _cell_length_c 24.3971(2) _cell_angle_alpha 86.700(1) _cell_angle_beta 89.240(1) _cell_angle_gamma 77.418(1) _cell_volume 5271.02(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 96434 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 2.709 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Kappa CCD' _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 116633 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 24176 _reflns_number_gt 19570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski, Minor, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski, Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farugia)' _computing_publication_material 'Shelx-97/ciftab(Sheldrick, 1997)' _refine_special_details ; This structure bears numerous disorders. Firstly, the dichloromethane solvent molecule was refined in three sites with the following restraints: isor 0.003 cl1a eadp cl1c c1c cl2c eadp cl2a cl1a c1a eadp cl2b c1b cl1b sadi 0.001 c1a cl1a c1a cl2a c1b cl1b c1b cl2b c1c cl1c c1c cl2c same cl1a c1a cl2a same cl1a c1a cl2a Secondly, the cyclooctadiene (-CH2CH2-, C18 C19 C22 C23) groups at Ir2 are twofold disordered in a cross-wise manner and were refined with the following restraints: exyz c16 c16a exyz c17 c17a exyz c20 c20a exyz c21 c21a eadp c16 c16a eadp c17 c17a eadp c18 c18a eadp c19 c19a eadp c20 c20a eadp c21 c21a eadp c22 c22a eadp c23 c23a sadi 0.001 c18 c19 c18a c19a c22 c23 c22a c23a sadi 0.001 c17 c18 c17a c18a c19 c20 c19a c20a c21 c22 c21a c22a c23 c16 = C23A C16A Finally, five CF3 groups of the anions are twofold disordered each. The following sets of restraints were used in the refinement: Group 1 sadi 0.001 c47 c51 c47 c51a sadi 0.001 c51 f7 c51 f8 c51 f9 c51a f7a c51a f8a c51a f9a eadp c51 c51a eadp f7 f7a eadp f8 f8a eadp f9 f9a same c51 f7 f8 f9 Group 2 sadi 0.001 c52 c49 c52a c49 sadi 0.001 c52 f10 c52 f11 c52 f12 c52a f10a c52a f11a c52a f12a eadp c52 c52a eadp f10 f10a eadp f11 f11a eadp f12 f12a same c52 f10 f11 f12 Group 3 sadi 0.001 c92 f40 c92 f41 c92 f42 c92 f40a c92 f41a c92 f42a eadp f40 f40a eadp f41 f41a eadp f42 f42a Group 4 sadi 0.001 c71 c75 c71 c75a sadi 0.001 c75 f25 c75 f26 c75 f27 c75a f25a c75a f26a c75a f27a eadp c75 c75a eadp f25 f25a eadp f26 f26a eadp f27 f27a Group 5 sadi 0.001 c67 f19 c67 f20 c67 f21 c67 f19a c67 f20a c67 f21a eadp f19 f19a eadp f20 f20a eadp f21 f21a 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+4.1681P] 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 24176 _refine_ls_number_parameters 1552 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.050 _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 0.917089(11) 0.458111(8) 0.747977(6) 0.03445(5) Uani 1 1 d . . . Ir2 Ir 1.012153(11) 0.867290(8) 0.723660(6) 0.03733(5) Uani 1 1 d . . . C16 C 1.1795(3) 0.8433(3) 0.70082(18) 0.0574(12) Uani 0.45 1 d PD A 1 H16 H 1.2266 0.8265 0.7339 0.069 Uiso 0.45 1 calc PR A 1 C17 C 1.1386(4) 0.9249(3) 0.69865(18) 0.0630(13) Uani 0.45 1 d PD A 1 H17 H 1.1664 0.9534 0.7276 0.076 Uiso 0.45 1 calc PR A 1 C18 C 1.1340(12) 0.9627(13) 0.6405(4) 0.081(4) Uani 0.45 1 d PD A 1 H18A H 1.1829 0.9290 0.6153 0.097 Uiso 0.45 1 calc PR A 1 H18B H 1.1542 1.0140 0.6401 0.097 Uiso 0.45 1 calc PR A 1 C19 C 1.0137(14) 0.9713(8) 0.6249(6) 0.068(3) Uani 0.45 1 d PD A 1 H19A H 0.9717 1.0192 0.6409 0.081 Uiso 0.45 1 calc PR A 1 H19B H 1.0079 0.9798 0.5845 0.081 Uiso 0.45 1 calc PR A 1 C20 C 0.9578(4) 0.9049(3) 0.64215(19) 0.0614(12) Uani 0.45 1 d PD A 1 H20 H 0.8766 0.9200 0.6390 0.074 Uiso 0.45 1 calc PR A 1 C21 C 0.9976(3) 0.8245(3) 0.64543(16) 0.0522(11) Uani 0.45 1 d PD A 1 H21 H 0.9418 0.7923 0.6424 0.063 Uiso 0.45 1 calc PR A 1 C22 C 1.1069(6) 0.7939(11) 0.6174(6) 0.054(3) Uani 0.45 1 d PD A 1 H22A H 1.1193 0.8321 0.5880 0.064 Uiso 0.45 1 calc PR A 1 H22B H 1.1053 0.7446 0.6004 0.064 Uiso 0.45 1 calc PR A 1 C23 C 1.2006(11) 0.7801(5) 0.6592(4) 0.0521(19) Uani 0.45 1 d PD A 1 H23A H 1.2070 0.7284 0.6786 0.063 Uiso 0.45 1 calc PR A 1 H23B H 1.2701 0.7806 0.6398 0.063 Uiso 0.45 1 calc PR A 1 C16A C 1.1795(3) 0.8433(3) 0.70082(18) 0.0574(12) Uani 0.55 1 d PD A 2 H16A H 1.2337 0.8209 0.7303 0.069 Uiso 0.55 1 calc PR A 2 C17A C 1.1386(4) 0.9249(3) 0.69865(18) 0.0630(13) Uani 0.55 1 d PD A 2 H17A H 1.1660 0.9503 0.7295 0.076 Uiso 0.55 1 calc PR A 2 C18A C 1.0933(10) 0.9827(8) 0.6511(4) 0.081(4) Uani 0.55 1 d PD A 2 H18C H 1.1557 0.9978 0.6314 0.097 Uiso 0.55 1 calc PR A 2 H18D H 1.0495 1.0301 0.6667 0.097 Uiso 0.55 1 calc PR A 2 C19A C 1.0226(13) 0.9554(7) 0.6086(4) 0.068(3) Uani 0.55 1 d PD A 2 H19C H 0.9731 1.0003 0.5897 0.081 Uiso 0.55 1 calc PR A 2 H19D H 1.0687 0.9248 0.5809 0.081 Uiso 0.55 1 calc PR A 2 C20A C 0.9578(4) 0.9049(3) 0.64215(19) 0.0614(12) Uani 0.55 1 d PD A 2 H20A H 0.8769 0.9216 0.6381 0.074 Uiso 0.55 1 calc PR A 2 C21A C 0.9976(3) 0.8245(3) 0.64543(16) 0.0522(11) Uani 0.55 1 d PD A 2 H21A H 0.9374 0.7957 0.6445 0.063 Uiso 0.55 1 calc PR A 2 C22A C 1.1067(5) 0.7744(7) 0.6282(5) 0.054(3) Uani 0.55 1 d PD A 2 H22C H 1.1070 0.7691 0.5880 0.064 Uiso 0.55 1 calc PR A 2 H22D H 1.1163 0.7217 0.6464 0.064 Uiso 0.55 1 calc PR A 2 C23A C 1.2014(9) 0.8111(5) 0.6439(2) 0.0521(19) Uani 0.55 1 d PD A 2 H23C H 1.2707 0.7715 0.6442 0.063 Uiso 0.55 1 calc PR A 2 H23D H 1.2081 0.8535 0.6166 0.063 Uiso 0.55 1 calc PR A 2 N1 N 0.8073(2) 0.54912(17) 0.70759(12) 0.0355(6) Uani 1 1 d . . . N2 N 0.8418(2) 0.59662(17) 0.66898(12) 0.0352(6) Uani 1 1 d . . . N3 N 1.0084(2) 0.45113(18) 0.67557(13) 0.0405(7) Uani 1 1 d . . . N4 N 1.0078(3) 0.51466(19) 0.64206(13) 0.0400(7) Uani 1 1 d . . . N5 N 0.8595(2) 0.84857(19) 0.74883(14) 0.0417(7) Uani 1 1 d . . . N6 N 0.8500(2) 0.80287(19) 0.79470(13) 0.0386(7) Uani 1 1 d . . . N7 N 1.0522(2) 0.85780(18) 0.80684(12) 0.0371(7) Uani 1 1 d . . . N8 N 1.0108(2) 0.80894(17) 0.84200(12) 0.0336(6) Uani 1 1 d . . . C1 C 0.9972(4) 0.3458(2) 0.7780(2) 0.0571(11) Uani 1 1 d . . . H1 H 1.0377 0.3132 0.7490 0.069 Uiso 1 1 calc R . . C2 C 1.0531(4) 0.4000(3) 0.7971(2) 0.0609(12) Uani 1 1 d . . . H2 H 1.1257 0.3986 0.7795 0.073 Uiso 1 1 calc R . . C3 C 1.0447(5) 0.4245(4) 0.8555(2) 0.089(2) Uani 1 1 d . . . H3A H 1.0353 0.3797 0.8800 0.107 Uiso 1 1 calc R . . H3B H 1.1142 0.4379 0.8655 0.107 Uiso 1 1 calc R . . C4 C 0.9544(5) 0.4913(4) 0.8654(2) 0.0757(16) Uani 1 1 d . . . H4A H 0.9829 0.5395 0.8629 0.091 Uiso 1 1 calc R . . H4B H 0.9268 0.4851 0.9032 0.091 Uiso 1 1 calc R . . C5 C 0.8600(4) 0.5006(3) 0.82539(16) 0.0521(10) Uani 1 1 d . . . H5 H 0.8123 0.5541 0.8229 0.063 Uiso 1 1 calc R . . C6 C 0.8065(4) 0.4419(3) 0.81224(17) 0.0492(10) Uani 1 1 d . . . H6 H 0.7281 0.4617 0.8021 0.059 Uiso 1 1 calc R . . C7 C 0.8309(5) 0.3605(3) 0.8393(2) 0.0746(15) Uani 1 1 d . . . H7A H 0.8510 0.3632 0.8781 0.090 Uiso 1 1 calc R . . H7B H 0.7641 0.3394 0.8389 0.090 Uiso 1 1 calc R . . C8 C 0.9211(6) 0.3060(3) 0.8117(3) 0.0836(18) Uani 1 1 d . . . H8A H 0.8887 0.2740 0.7874 0.100 Uiso 1 1 calc R . . H8B H 0.9643 0.2704 0.8401 0.100 Uiso 1 1 calc R . . C9 C 0.6986(3) 0.5732(2) 0.70878(17) 0.0437(9) Uani 1 1 d . . . H9 H 0.6514 0.5504 0.7319 0.052 Uiso 1 1 calc R . . C10 C 0.6643(3) 0.6362(2) 0.67157(19) 0.0497(10) Uani 1 1 d . . . H10 H 0.5915 0.6638 0.6647 0.060 Uiso 1 1 calc R . . C11 C 0.7557(3) 0.6500(2) 0.64719(17) 0.0469(9) Uani 1 1 d . . . H11 H 0.7594 0.6898 0.6198 0.056 Uiso 1 1 calc R . . C12 C 1.0677(3) 0.3921(3) 0.6489(2) 0.0531(11) Uani 1 1 d . . . H12 H 1.0820 0.3391 0.6621 0.064 Uiso 1 1 calc R . . C13 C 1.1052(4) 0.4188(3) 0.5994(2) 0.0691(15) Uani 1 1 d . . . H13 H 1.1494 0.3885 0.5733 0.083 Uiso 1 1 calc R . . C14 C 1.0659(4) 0.4977(3) 0.59583(19) 0.0546(11) Uani 1 1 d . . . H14 H 1.0773 0.5331 0.5667 0.066 Uiso 1 1 calc R . . C15 C 0.9573(3) 0.5912(2) 0.65998(15) 0.0387(8) Uani 1 1 d . . . H15 H 0.9645 0.6296 0.6291 0.046 Uiso 1 1 calc R . . C24 C 0.7582(3) 0.8773(3) 0.7316(2) 0.0600(12) Uani 1 1 d . . . H24 H 0.7391 0.9123 0.7004 0.072 Uiso 1 1 calc R . . C25 C 0.6847(4) 0.8494(4) 0.7653(2) 0.0755(16) Uani 1 1 d . . . H25 H 0.6077 0.8609 0.7615 0.091 Uiso 1 1 calc R . . C26 C 0.7446(3) 0.8020(3) 0.8052(2) 0.0596(13) Uani 1 1 d . . . H26 H 0.7174 0.7739 0.8345 0.072 Uiso 1 1 calc R . . C27 C 1.1053(3) 0.8966(2) 0.83843(17) 0.0419(9) Uani 1 1 d . . . H27 H 1.1419 0.9357 0.8250 0.050 Uiso 1 1 calc R . . C28 C 1.1002(3) 0.8725(2) 0.89327(17) 0.0436(9) Uani 1 1 d . . . H28 H 1.1317 0.8910 0.9236 0.052 Uiso 1 1 calc R . . C29 C 1.0400(3) 0.8163(2) 0.89445(15) 0.0377(8) Uani 1 1 d . . . H29 H 1.0221 0.7878 0.9261 0.045 Uiso 1 1 calc R . . C30 C 0.9471(3) 0.7569(2) 0.82183(16) 0.0370(8) Uani 1 1 d . . . H30 H 0.9229 0.7278 0.8544 0.044 Uiso 1 1 calc R . . C31 C 1.0147(3) 0.6128(2) 0.70957(15) 0.0351(7) Uani 1 1 d . . . C32 C 0.9585(3) 0.67010(19) 0.74281(14) 0.0337(7) Uani 1 1 d . . . H32 H 0.8829 0.6907 0.7369 0.040 Uiso 1 1 calc R . . C33 C 1.0118(3) 0.69708(19) 0.78420(15) 0.0335(7) Uani 1 1 d . . . C34 C 1.1216(3) 0.6656(2) 0.79385(16) 0.0402(8) Uani 1 1 d . . . H34 H 1.1584 0.6836 0.8226 0.048 Uiso 1 1 calc R . . C35 C 1.1774(3) 0.6077(2) 0.76130(17) 0.0450(9) Uani 1 1 d . . . H35 H 1.2525 0.5860 0.7680 0.054 Uiso 1 1 calc R . . C36 C 1.1245(3) 0.5814(2) 0.71920(16) 0.0398(8) Uani 1 1 d . . . H36 H 1.1633 0.5421 0.6970 0.048 Uiso 1 1 calc R . . B1 B 0.6078(3) 0.2283(2) -0.00011(15) 0.0295(7) Uani 1 1 d . . . F1 F 0.6137(4) -0.02723(17) 0.11929(14) 0.1035(13) Uani 1 1 d . . . F2 F 0.5556(3) 0.00500(19) 0.19562(17) 0.1057(13) Uani 1 1 d . . . F3 F 0.7225(3) -0.01217(17) 0.1799(2) 0.1162(16) Uani 1 1 d . . . F4 F 0.4444(2) 0.32334(18) 0.20515(13) 0.0765(8) Uani 1 1 d . . . F5 F 0.5905(3) 0.35961(17) 0.18871(12) 0.0692(8) Uani 1 1 d . . . F6 F 0.5842(3) 0.27263(18) 0.25290(11) 0.0975(12) Uani 1 1 d . . . C51 C 0.9977(4) 0.1122(3) -0.07201(19) 0.0517(14) Uani 0.58 1 d PD B 1 F7 F 1.0143(6) 0.1796(4) -0.0591(5) 0.111(4) Uani 0.58 1 d PD B 1 F8 F 1.0642(5) 0.0561(5) -0.0444(5) 0.120(4) Uani 0.58 1 d PD B 1 F9 F 1.0275(5) 0.1058(5) -0.1234(2) 0.0932(15) Uani 0.58 1 d PD B 1 C51A C 0.9996(4) 0.1118(5) -0.0581(3) 0.0517(14) Uani 0.42 1 d PD B 2 F7A F 1.0703(8) 0.0540(6) -0.0778(8) 0.111(4) Uani 0.42 1 d PD B 2 F8A F 1.0172(8) 0.1733(7) -0.0861(7) 0.120(4) Uani 0.42 1 d PD B 2 F9A F 1.0401(7) 0.1213(8) -0.0105(3) 0.0932(15) Uani 0.42 1 d PD B 2 C52 C 0.7134(3) -0.0424(3) -0.0782(2) 0.0716(16) Uani 0.81 1 d PD B 1 F10 F 0.6702(10) -0.0735(4) -0.0360(3) 0.172(4) Uani 0.81 1 d PD B 1 F11 F 0.6407(6) -0.0317(3) -0.1173(4) 0.137(3) Uani 0.81 1 d PD B 1 F12 F 0.7913(3) -0.0978(3) -0.0953(4) 0.111(2) Uani 0.81 1 d PD B 1 C52A C 0.7215(14) -0.0452(6) -0.0779(9) 0.0716(16) Uani 0.19 1 d PD B 2 F10A F 0.748(4) -0.0571(18) -0.1292(11) 0.172(4) Uani 0.19 1 d PD B 2 F11A F 0.776(2) -0.1035(11) -0.0470(16) 0.137(3) Uani 0.19 1 d PD B 2 F12A F 0.6197(13) -0.0480(14) -0.0688(17) 0.111(2) Uani 0.19 1 d PD B 2 F13 F 0.9089(2) 0.36229(15) 0.07081(12) 0.0657(7) Uani 1 1 d . . . F14 F 0.7984(3) 0.4645(3) 0.08859(18) 0.1195(17) Uani 1 1 d . . . F15 F 0.9034(3) 0.4642(2) 0.02078(16) 0.1050(14) Uani 1 1 d . . . F16 F 0.6035(3) 0.56161(16) -0.10755(14) 0.0810(10) Uani 1 1 d . . . F17 F 0.5474(2) 0.47288(16) -0.14542(10) 0.0667(7) Uani 1 1 d . . . F18 F 0.4568(2) 0.53097(17) -0.08040(12) 0.0767(9) Uani 1 1 d . . . F19 F 0.2072(9) 0.3597(8) 0.0571(6) 0.113(3) Uani 0.46 1 d PD C 1 F20 F 0.1042(5) 0.3362(14) -0.0016(3) 0.136(3) Uani 0.46 1 d PD C 1 F21 F 0.1685(12) 0.2544(4) 0.0591(5) 0.095(2) Uani 0.46 1 d PD C 1 F19A F 0.1111(6) 0.2742(6) 0.0208(6) 0.113(3) Uani 0.54 1 d PD C 2 F20A F 0.2150(6) 0.2955(12) 0.07694(17) 0.136(3) Uani 0.54 1 d PD C 2 F21A F 0.1534(9) 0.3806(3) 0.0177(5) 0.095(2) Uani 0.54 1 d PD C 2 F22 F 0.3121(3) 0.29586(18) -0.18686(12) 0.0834(9) Uani 1 1 d . . . F23 F 0.2496(3) 0.1971(2) -0.16456(13) 0.0921(11) Uani 1 1 d . . . F24 F 0.4166(3) 0.1838(2) -0.18227(12) 0.0929(11) Uani 1 1 d . . . C37 C 0.6078(3) 0.20134(19) 0.06597(14) 0.0302(7) Uani 1 1 d . . . C38 C 0.6193(3) 0.1238(2) 0.08516(15) 0.0344(7) Uani 1 1 d . . . H38 H 0.6315 0.0846 0.0593 0.041 Uiso 1 1 calc R . . C39 C 0.6138(3) 0.1016(2) 0.14042(15) 0.0375(8) Uani 1 1 d . . . C40 C 0.5946(3) 0.1568(2) 0.17984(15) 0.0379(8) Uani 1 1 d . . . H40 H 0.5912 0.1419 0.2178 0.045 Uiso 1 1 calc R . . C41 C 0.5807(3) 0.2341(2) 0.16204(14) 0.0351(7) Uani 1 1 d . . . C42 C 0.5870(3) 0.2565(2) 0.10623(14) 0.0334(7) Uani 1 1 d . . . H42 H 0.5771 0.3102 0.0954 0.040 Uiso 1 1 calc R . . C43 C 0.6287(4) 0.0170(2) 0.15862(18) 0.0495(10) Uani 1 1 d . . . C44 C 0.5522(3) 0.2960(3) 0.20242(16) 0.0472(9) Uani 1 1 d . . . C45 C 0.6966(3) 0.16063(19) -0.03084(13) 0.0313(7) Uani 1 1 d . . . C46 C 0.8045(3) 0.1660(2) -0.04041(15) 0.0358(7) Uani 1 1 d . . . H46 H 0.8254 0.2131 -0.0333 0.043 Uiso 1 1 calc R . . C47 C 0.8826(3) 0.1050(2) -0.06000(17) 0.0426(9) Uani 1 1 d . . . C48 C 0.8549(3) 0.0364(2) -0.07257(18) 0.0497(10) Uani 1 1 d . . . H48 H 0.9079 -0.0054 -0.0860 0.060 Uiso 1 1 calc R . . C49 C 0.7479(3) 0.0303(2) -0.06508(17) 0.0453(9) Uani 1 1 d . . . C50 C 0.6707(3) 0.0909(2) -0.04471(15) 0.0387(8) Uani 1 1 d . . . H50 H 0.5978 0.0848 -0.0400 0.046 Uiso 1 1 calc R . . C53 C 0.6419(3) 0.31260(18) -0.00998(13) 0.0296(7) Uani 1 1 d . . . C54 C 0.7257(3) 0.33206(19) 0.01999(14) 0.0327(7) Uani 1 1 d . . . H54 H 0.7633 0.2951 0.0468 0.039 Uiso 1 1 calc R . . C55 C 0.7560(3) 0.40348(19) 0.01200(15) 0.0344(7) Uani 1 1 d . . . C56 C 0.7021(3) 0.4593(2) -0.02686(15) 0.0374(8) Uani 1 1 d . . . H56 H 0.7223 0.5080 -0.0328 0.045 Uiso 1 1 calc R . . C57 C 0.6189(3) 0.4418(2) -0.05646(14) 0.0344(7) Uani 1 1 d . . . C58 C 0.5898(3) 0.37015(19) -0.04821(14) 0.0328(7) Uani 1 1 d . . . H58 H 0.5321 0.3601 -0.0695 0.039 Uiso 1 1 calc R . . C59 C 0.8414(3) 0.4233(2) 0.04684(19) 0.0471(9) Uani 1 1 d . . . C60 C 0.5566(3) 0.5011(2) -0.09703(16) 0.0426(9) Uani 1 1 d . . . C61 C 0.4842(3) 0.23686(18) -0.02386(14) 0.0313(7) Uani 1 1 d . . . C62 C 0.3931(3) 0.2631(2) 0.00910(15) 0.0354(7) Uani 1 1 d . . . H62 H 0.4038 0.2716 0.0465 0.043 Uiso 1 1 calc R . . C63 C 0.2870(3) 0.2769(2) -0.01132(16) 0.0387(8) Uani 1 1 d . . . C64 C 0.2678(3) 0.2643(2) -0.06527(16) 0.0410(8) Uani 1 1 d . . . H64 H 0.1955 0.2726 -0.0789 0.049 Uiso 1 1 calc R . . C65 C 0.3565(3) 0.2393(2) -0.09901(15) 0.0370(8) Uani 1 1 d . . . C66 C 0.4620(3) 0.2253(2) -0.07850(14) 0.0338(7) Uani 1 1 d . . . H66 H 0.5213 0.2071 -0.1024 0.041 Uiso 1 1 calc R . . C67 C 0.1927(3) 0.30689(18) 0.02525(15) 0.0487(10) Uani 1 1 d . . . C68 C 0.3349(3) 0.2285(3) -0.15808(17) 0.0472(9) Uani 1 1 d . . . B2 B 0.5140(3) 0.7354(2) 0.46255(16) 0.0307(8) Uani 1 1 d . . . C75 C 0.4855(4) 0.8881(2) 0.63685(18) 0.0528(11) Uani 0.69 1 d PD D 1 F25 F 0.5150(7) 0.9516(4) 0.6488(2) 0.0908(16) Uani 0.69 1 d PD D 1 F26 F 0.4082(6) 0.8828(8) 0.67210(18) 0.135(3) Uani 0.69 1 d PD D 1 F27 F 0.5704(9) 0.8341(4) 0.6514(3) 0.142(4) Uani 0.69 1 d PD D 1 C75A C 0.4784(9) 0.8837(6) 0.6383(2) 0.0528(11) Uani 0.31 1 d PD D 2 F25A F 0.4690(18) 0.8216(8) 0.6680(5) 0.0908(16) Uani 0.31 1 d PD D 2 F26A F 0.5822(12) 0.8802(19) 0.6445(5) 0.135(3) Uani 0.31 1 d PD D 2 F27A F 0.427(2) 0.9422(12) 0.6655(8) 0.142(4) Uani 0.31 1 d PD D 2 F28 F 0.3250(3) 1.08298(16) 0.47762(17) 0.0963(11) Uani 1 1 d . . . F29 F 0.1902(3) 1.0324(2) 0.48903(19) 0.1157(15) Uani 1 1 d . . . F30 F 0.2856(3) 1.01438(19) 0.41717(14) 0.1074(14) Uani 1 1 d . . . F31 F 0.0975(2) 0.7130(2) 0.4057(2) 0.1151(15) Uani 1 1 d . . . F32 F 0.1098(2) 0.82534(18) 0.38450(18) 0.0973(12) Uani 1 1 d . . . F33 F 0.0947(3) 0.7478(4) 0.32423(19) 0.153(2) Uani 1 1 d . . . F34 F 0.4471(3) 0.6581(2) 0.22690(11) 0.0943(11) Uani 1 1 d . . . F35 F 0.4592(3) 0.55136(18) 0.27368(14) 0.0871(10) Uani 1 1 d . . . F36 F 0.5883(2) 0.61087(18) 0.27485(11) 0.0711(8) Uani 1 1 d . . . F37 F 0.8613(2) 0.7739(2) 0.55791(10) 0.0769(9) Uani 1 1 d . . . F38 F 0.9583(3) 0.68660(17) 0.51247(16) 0.0915(11) Uani 1 1 d . . . F39 F 0.9717(2) 0.80427(17) 0.49866(11) 0.0671(7) Uani 1 1 d . . . F40 F 0.8586(3) 0.8424(3) 0.30506(15) 0.0830(12) Uani 0.84 1 d PD E 1 F41 F 0.7054(5) 0.9148(2) 0.3119(2) 0.1044(16) Uani 0.84 1 d PD E 1 F42 F 0.7221(7) 0.8023(5) 0.28264(14) 0.148(3) Uani 0.84 1 d PD E 1 F40A F 0.6673(8) 0.871(2) 0.2922(8) 0.0830(12) Uani 0.16 1 d PD E 2 F41A F 0.805(2) 0.7908(10) 0.2850(6) 0.1044(16) Uani 0.16 1 d PD E 2 F42A F 0.810(4) 0.899(2) 0.3131(8) 0.148(3) Uani 0.16 1 d PD E 2 F43 F 0.3507(2) 0.49601(15) 0.61640(15) 0.0794(9) Uani 1 1 d . . . F44 F 0.3798(3) 0.5888(2) 0.66168(12) 0.0836(10) Uani 1 1 d . . . F45 F 0.2678(2) 0.61200(16) 0.59567(12) 0.0682(8) Uani 1 1 d . . . F46 F 0.7744(2) 0.45514(19) 0.59928(11) 0.0773(9) Uani 1 1 d . . . F47 F 0.7516(3) 0.4151(2) 0.52214(19) 0.1242(18) Uani 1 1 d . . . F48 F 0.8281(2) 0.5082(2) 0.52946(18) 0.1108(15) Uani 1 1 d . . . C69 C 0.4583(3) 0.81241(19) 0.49625(14) 0.0304(7) Uani 1 1 d . . . C70 C 0.4830(3) 0.8168(2) 0.55163(14) 0.0335(7) Uani 1 1 d . . . H70 H 0.5237 0.7718 0.5710 0.040 Uiso 1 1 calc R . . C71 C 0.4499(3) 0.8851(2) 0.57915(15) 0.0384(8) Uani 1 1 d . . . C72 C 0.3872(3) 0.9509(2) 0.55329(16) 0.0433(9) Uani 1 1 d . . . H72 H 0.3630 0.9971 0.5723 0.052 Uiso 1 1 calc R . . C73 C 0.3606(3) 0.9478(2) 0.49882(16) 0.0379(8) Uani 1 1 d . . . C74 C 0.3966(3) 0.8804(2) 0.47088(15) 0.0339(7) Uani 1 1 d . . . H74 H 0.3785 0.8807 0.4332 0.041 Uiso 1 1 calc R . . C76 C 0.2901(4) 1.0179(3) 0.47075(19) 0.0542(11) Uani 1 1 d . . . C77 C 0.4399(3) 0.72111(19) 0.41096(14) 0.0312(7) Uani 1 1 d . . . C78 C 0.3269(3) 0.7439(2) 0.41021(15) 0.0363(7) Uani 1 1 d . . . H78 H 0.2907 0.7708 0.4401 0.044 Uiso 1 1 calc R . . C79 C 0.2648(3) 0.7285(2) 0.36676(17) 0.0425(9) Uani 1 1 d . . . C80 C 0.3136(3) 0.6895(2) 0.32251(16) 0.0442(9) Uani 1 1 d . . . H80 H 0.2714 0.6795 0.2928 0.053 Uiso 1 1 calc R . . C81 C 0.4268(3) 0.6652(2) 0.32273(15) 0.0396(8) Uani 1 1 d . . . C82 C 0.4872(3) 0.6804(2) 0.36561(14) 0.0339(7) Uani 1 1 d . . . H82 H 0.5642 0.6627 0.3646 0.041 Uiso 1 1 calc R . . C83 C 0.1439(3) 0.7549(3) 0.3691(2) 0.0603(12) Uani 1 1 d . . . C84 C 0.4806(4) 0.6225(3) 0.27481(17) 0.0503(10) Uani 1 1 d . . . C85 C 0.6305(3) 0.75526(18) 0.44245(13) 0.0294(7) Uani 1 1 d . . . C86 C 0.7169(3) 0.74825(19) 0.47925(13) 0.0309(7) Uani 1 1 d . . . H86 H 0.7092 0.7272 0.5154 0.037 Uiso 1 1 calc R . . C87 C 0.8136(3) 0.77066(19) 0.46527(14) 0.0324(7) Uani 1 1 d . . . C88 C 0.8292(3) 0.8018(2) 0.41325(14) 0.0350(7) Uani 1 1 d . . . H88 H 0.8953 0.8169 0.4035 0.042 Uiso 1 1 calc R . . C89 C 0.7446(3) 0.8102(2) 0.37574(14) 0.0335(7) Uani 1 1 d . . . C90 C 0.6479(3) 0.78797(19) 0.39039(14) 0.0321(7) Uani 1 1 d . . . H90 H 0.5912 0.7954 0.3639 0.039 Uiso 1 1 calc R . . C91 C 0.9015(3) 0.7593(3) 0.50721(17) 0.0460(9) Uani 1 1 d . . . C92 C 0.7578(2) 0.84222(19) 0.31921(16) 0.0496(10) Uani 1 1 d . . . C93 C 0.5300(3) 0.65699(19) 0.50366(14) 0.0310(7) Uani 1 1 d . . . C94 C 0.4458(3) 0.6437(2) 0.53807(15) 0.0348(7) Uani 1 1 d . . . H94 H 0.3789 0.6812 0.5374 0.042 Uiso 1 1 calc R . . C95 C 0.4555(3) 0.5782(2) 0.57312(15) 0.0356(7) Uani 1 1 d . . . C96 C 0.5527(3) 0.5222(2) 0.57655(14) 0.0351(7) Uani 1 1 d . . . H96 H 0.5601 0.4775 0.6010 0.042 Uiso 1 1 calc R . . C97 C 0.6378(3) 0.5342(2) 0.54316(14) 0.0327(7) Uani 1 1 d . . . C98 C 0.6263(3) 0.59893(19) 0.50675(14) 0.0322(7) Uani 1 1 d . . . H98 H 0.6854 0.6041 0.4832 0.039 Uiso 1 1 calc R . . C99 C 0.3645(3) 0.5682(2) 0.61125(18) 0.0467(9) Uani 1 1 d . . . C100 C 0.7459(3) 0.4779(2) 0.54788(16) 0.0409(8) Uani 1 1 d . . . Cl1A Cl 0.8107(7) 0.0742(5) 0.7710(4) 0.207(2) Uani 0.52 1 d PDU F 1 C1A C 0.6719(10) 0.104(2) 0.7678(8) 0.207(2) Uani 0.52 1 d PD F 1 H1A H 0.6400 0.0740 0.7967 0.248 Uiso 0.52 1 calc PR F 1 H1B H 0.6519 0.1593 0.7763 0.248 Uiso 0.52 1 calc PR F 1 Cl2A Cl 0.6136(9) 0.0938(7) 0.7064(5) 0.207(2) Uani 0.52 1 d PD F 1 Cl1B Cl 0.7356(9) 0.1461(5) 0.7940(3) 0.176(3) Uani 0.36 1 d PD G 2 C1B C 0.639(2) 0.109(2) 0.7620(7) 0.176(3) Uani 0.36 1 d PD G 2 H1C H 0.5685 0.1466 0.7659 0.211 Uiso 0.36 1 calc PR G 2 H1D H 0.6332 0.0607 0.7829 0.211 Uiso 0.36 1 calc PR G 2 Cl2B Cl 0.6537(13) 0.0893(7) 0.6943(4) 0.176(3) Uani 0.36 1 d PD G 2 Cl1C Cl 0.754(2) 0.0757(15) 0.7152(12) 0.187(8) Uani 0.12 1 d PD H 3 C1C C 0.820(4) 0.125(4) 0.757(4) 0.187(8) Uani 0.12 1 d PD H 3 H1E H 0.7774 0.1323 0.7918 0.224 Uiso 0.12 1 calc PR H 3 H1F H 0.8173 0.1770 0.7396 0.224 Uiso 0.12 1 calc PR H 3 Cl2C Cl 0.952(3) 0.0850(15) 0.7746(11) 0.187(8) Uani 0.12 1 d PD H 3 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 0.03251(8) 0.03575(8) 0.03538(8) -0.00888(6) 0.00088(6) -0.00637(6) Ir2 0.03289(8) 0.04205(8) 0.03842(8) -0.00453(6) -0.00767(6) -0.01010(6) C16 0.033(2) 0.088(3) 0.058(3) -0.021(2) -0.0004(18) -0.022(2) C17 0.067(3) 0.087(4) 0.051(3) -0.002(2) -0.005(2) -0.051(3) C18 0.088(10) 0.109(9) 0.059(5) 0.017(6) 0.011(5) -0.057(8) C19 0.098(5) 0.069(6) 0.036(7) 0.004(5) -0.012(5) -0.017(5) C20 0.054(3) 0.080(3) 0.047(3) 0.015(2) -0.021(2) -0.010(2) C21 0.054(2) 0.073(3) 0.036(2) -0.0057(19) -0.0168(18) -0.024(2) C22 0.065(3) 0.064(7) 0.034(5) -0.009(5) -0.001(2) -0.015(3) C23 0.048(3) 0.066(6) 0.046(4) -0.004(4) 0.011(4) -0.021(5) C16A 0.033(2) 0.088(3) 0.058(3) -0.021(2) -0.0004(18) -0.022(2) C17A 0.067(3) 0.087(4) 0.051(3) -0.002(2) -0.005(2) -0.051(3) C18A 0.088(10) 0.109(9) 0.059(5) 0.017(6) 0.011(5) -0.057(8) C19A 0.098(5) 0.069(6) 0.036(7) 0.004(5) -0.012(5) -0.017(5) C20A 0.054(3) 0.080(3) 0.047(3) 0.015(2) -0.021(2) -0.010(2) C21A 0.054(2) 0.073(3) 0.036(2) -0.0057(19) -0.0168(18) -0.024(2) C22A 0.065(3) 0.064(7) 0.034(5) -0.009(5) -0.001(2) -0.015(3) C23A 0.048(3) 0.066(6) 0.046(4) -0.004(4) 0.011(4) -0.021(5) N1 0.0319(15) 0.0416(16) 0.0352(16) -0.0111(13) 0.0025(12) -0.0103(12) N2 0.0372(16) 0.0401(16) 0.0298(15) -0.0079(12) 0.0004(12) -0.0101(13) N3 0.0352(16) 0.0422(17) 0.0462(18) -0.0155(14) 0.0094(13) -0.0100(13) N4 0.0382(16) 0.0467(18) 0.0393(17) -0.0190(14) 0.0096(13) -0.0152(14) N5 0.0310(15) 0.0473(18) 0.0482(19) -0.0162(15) -0.0050(13) -0.0074(13) N6 0.0266(14) 0.0512(18) 0.0410(17) -0.0189(14) 0.0009(12) -0.0109(13) N7 0.0312(15) 0.0473(17) 0.0353(16) -0.0115(13) -0.0020(12) -0.0115(13) N8 0.0288(14) 0.0392(15) 0.0350(16) -0.0124(12) 0.0002(12) -0.0092(12) C1 0.065(3) 0.042(2) 0.058(3) -0.005(2) -0.002(2) 0.004(2) C2 0.050(3) 0.056(3) 0.070(3) -0.010(2) -0.022(2) 0.008(2) C3 0.088(4) 0.093(4) 0.075(4) -0.025(3) -0.045(3) 0.013(3) C4 0.093(4) 0.092(4) 0.042(3) -0.022(3) -0.019(3) -0.014(3) C5 0.058(3) 0.062(3) 0.034(2) -0.0171(19) 0.0083(18) -0.003(2) C6 0.050(2) 0.061(3) 0.037(2) 0.0008(18) 0.0083(17) -0.013(2) C7 0.081(4) 0.076(4) 0.070(4) 0.012(3) 0.001(3) -0.028(3) C8 0.125(5) 0.056(3) 0.068(4) 0.008(3) 0.002(3) -0.019(3) C9 0.0321(18) 0.050(2) 0.048(2) -0.0133(18) 0.0028(16) -0.0051(16) C10 0.038(2) 0.051(2) 0.056(3) -0.0111(19) -0.0032(18) 0.0015(17) C11 0.054(2) 0.045(2) 0.040(2) -0.0040(17) -0.0097(18) -0.0053(18) C12 0.045(2) 0.047(2) 0.071(3) -0.031(2) 0.026(2) -0.0132(18) C13 0.063(3) 0.067(3) 0.086(4) -0.046(3) 0.043(3) -0.026(2) C14 0.053(2) 0.073(3) 0.048(2) -0.029(2) 0.023(2) -0.031(2) C15 0.042(2) 0.044(2) 0.0327(19) -0.0090(15) 0.0082(15) -0.0137(16) C24 0.033(2) 0.081(3) 0.062(3) -0.016(2) -0.014(2) -0.001(2) C25 0.026(2) 0.128(5) 0.073(3) -0.032(3) -0.004(2) -0.009(2) C26 0.031(2) 0.100(4) 0.054(3) -0.033(3) 0.0083(19) -0.023(2) C27 0.0342(19) 0.046(2) 0.048(2) -0.0097(17) -0.0077(16) -0.0134(16) C28 0.0380(19) 0.050(2) 0.045(2) -0.0182(17) -0.0086(16) -0.0098(17) C29 0.0354(18) 0.044(2) 0.0323(18) -0.0130(15) -0.0029(14) -0.0024(15) C30 0.0346(18) 0.0425(19) 0.038(2) -0.0133(15) 0.0019(15) -0.0147(15) C31 0.0376(18) 0.0375(18) 0.0349(18) -0.0093(14) 0.0058(14) -0.0170(15) C32 0.0315(17) 0.0365(18) 0.0353(19) -0.0085(14) 0.0035(14) -0.0109(14) C33 0.0337(17) 0.0325(17) 0.0362(18) -0.0072(14) 0.0036(14) -0.0103(14) C34 0.0370(19) 0.045(2) 0.041(2) -0.0127(16) -0.0039(16) -0.0126(16) C35 0.0358(19) 0.045(2) 0.055(2) -0.0122(18) -0.0021(17) -0.0080(16) C36 0.0353(18) 0.0398(19) 0.047(2) -0.0129(16) 0.0081(16) -0.0108(15) B1 0.0315(18) 0.0282(17) 0.0279(18) -0.0056(14) -0.0003(14) -0.0033(14) F1 0.194(4) 0.0435(15) 0.079(2) 0.0070(15) -0.031(2) -0.038(2) F2 0.124(3) 0.068(2) 0.124(3) 0.026(2) 0.048(2) -0.029(2) F3 0.071(2) 0.0568(18) 0.219(5) 0.055(2) -0.065(3) -0.0241(15) F4 0.0578(17) 0.084(2) 0.082(2) -0.0312(16) 0.0170(14) 0.0033(14) F5 0.090(2) 0.0661(17) 0.0594(17) -0.0275(14) 0.0055(15) -0.0281(15) F6 0.159(3) 0.081(2) 0.0297(14) -0.0120(13) -0.0271(17) 0.028(2) C51 0.044(2) 0.057(3) 0.050(4) -0.007(3) 0.010(2) 0.000(2) F7 0.049(3) 0.087(5) 0.206(11) -0.062(6) 0.055(5) -0.027(3) F8 0.031(3) 0.135(8) 0.175(9) 0.096(7) -0.006(4) -0.005(3) F9 0.064(3) 0.134(5) 0.082(4) -0.014(4) 0.028(3) -0.021(3) C51A 0.044(2) 0.057(3) 0.050(4) -0.007(3) 0.010(2) 0.000(2) F7A 0.049(3) 0.087(5) 0.206(11) -0.062(6) 0.055(5) -0.027(3) F8A 0.031(3) 0.135(8) 0.175(9) 0.096(7) -0.006(4) -0.005(3) F9A 0.064(3) 0.134(5) 0.082(4) -0.014(4) 0.028(3) -0.021(3) C52 0.054(3) 0.053(3) 0.107(5) -0.039(3) -0.008(3) 0.001(2) F10 0.273(10) 0.089(4) 0.194(7) -0.057(4) 0.096(7) -0.118(6) F11 0.106(4) 0.089(3) 0.221(7) -0.063(4) -0.084(5) -0.013(3) F12 0.071(3) 0.061(3) 0.200(6) -0.081(3) -0.016(3) 0.005(2) C52A 0.054(3) 0.053(3) 0.107(5) -0.039(3) -0.008(3) 0.001(2) F10A 0.273(10) 0.089(4) 0.194(7) -0.057(4) 0.096(7) -0.118(6) F11A 0.106(4) 0.089(3) 0.221(7) -0.063(4) -0.084(5) -0.013(3) F12A 0.071(3) 0.061(3) 0.200(6) -0.081(3) -0.016(3) 0.005(2) F13 0.0597(16) 0.0610(16) 0.0792(19) 0.0052(14) -0.0300(14) -0.0200(13) F14 0.065(2) 0.149(3) 0.144(3) -0.106(3) -0.029(2) 0.005(2) F15 0.096(2) 0.124(3) 0.114(3) 0.059(2) -0.051(2) -0.081(2) F16 0.093(2) 0.0560(16) 0.095(2) 0.0355(16) -0.0307(18) -0.0278(15) F17 0.088(2) 0.0649(16) 0.0363(13) -0.0019(12) -0.0129(13) 0.0069(14) F18 0.0602(17) 0.0816(19) 0.0643(18) 0.0202(15) 0.0167(13) 0.0300(14) F19 0.083(5) 0.092(4) 0.185(8) -0.075(5) 0.089(5) -0.054(4) F20 0.048(3) 0.273(11) 0.056(3) 0.003(6) 0.016(2) 0.027(5) F21 0.103(5) 0.049(3) 0.118(5) 0.011(3) 0.066(4) 0.006(3) F19A 0.083(5) 0.092(4) 0.185(8) -0.075(5) 0.089(5) -0.054(4) F20A 0.048(3) 0.273(11) 0.056(3) 0.003(6) 0.016(2) 0.027(5) F21A 0.103(5) 0.049(3) 0.118(5) 0.011(3) 0.066(4) 0.006(3) F22 0.122(3) 0.077(2) 0.0467(16) 0.0143(14) -0.0184(17) -0.0176(19) F23 0.095(2) 0.145(3) 0.0562(18) -0.0160(19) -0.0194(16) -0.065(2) F24 0.077(2) 0.134(3) 0.0514(17) -0.0417(18) -0.0199(15) 0.022(2) C37 0.0244(15) 0.0335(16) 0.0323(17) -0.0029(13) -0.0025(13) -0.0053(13) C38 0.0326(17) 0.0343(17) 0.0363(19) -0.0026(14) -0.0021(14) -0.0071(14) C39 0.0321(17) 0.0389(19) 0.042(2) 0.0049(15) -0.0044(15) -0.0097(14) C40 0.0295(17) 0.050(2) 0.0336(19) 0.0045(15) -0.0023(14) -0.0083(15) C41 0.0293(17) 0.0445(19) 0.0301(17) -0.0050(14) 0.0010(13) -0.0042(14) C42 0.0303(16) 0.0362(17) 0.0318(17) -0.0026(14) -0.0008(13) -0.0030(14) C43 0.056(2) 0.046(2) 0.050(2) 0.0094(19) -0.0064(19) -0.0209(19) C44 0.049(2) 0.054(2) 0.034(2) -0.0022(17) 0.0020(17) -0.0006(19) C45 0.0327(17) 0.0317(16) 0.0275(16) -0.0014(13) -0.0009(13) -0.0024(13) C46 0.0350(18) 0.0358(18) 0.0355(19) -0.0042(14) -0.0012(14) -0.0047(14) C47 0.0348(19) 0.044(2) 0.045(2) -0.0040(17) 0.0032(16) 0.0008(16) C48 0.046(2) 0.043(2) 0.055(3) -0.0157(18) 0.0007(19) 0.0046(18) C49 0.045(2) 0.038(2) 0.051(2) -0.0141(17) -0.0084(18) -0.0008(16) C50 0.0372(19) 0.0371(18) 0.041(2) -0.0103(15) -0.0038(15) -0.0045(15) C53 0.0297(16) 0.0285(16) 0.0290(16) -0.0039(13) 0.0026(13) -0.0023(13) C54 0.0306(17) 0.0308(16) 0.0349(18) -0.0026(13) 0.0006(14) -0.0026(13) C55 0.0328(17) 0.0319(17) 0.0385(19) -0.0052(14) 0.0029(14) -0.0064(14) C56 0.0389(19) 0.0330(17) 0.040(2) -0.0019(15) 0.0069(15) -0.0065(15) C57 0.0363(18) 0.0331(17) 0.0307(17) -0.0020(13) 0.0040(14) -0.0010(14) C58 0.0315(17) 0.0357(17) 0.0292(17) -0.0043(13) 0.0008(13) -0.0025(14) C59 0.041(2) 0.042(2) 0.060(3) -0.0057(19) -0.0060(18) -0.0125(17) C60 0.048(2) 0.0390(19) 0.037(2) 0.0052(15) 0.0037(16) -0.0032(16) C61 0.0336(17) 0.0281(16) 0.0324(17) -0.0015(13) 0.0000(13) -0.0076(13) C62 0.0321(17) 0.0399(18) 0.0343(18) -0.0042(14) -0.0015(14) -0.0073(14) C63 0.0302(17) 0.0406(19) 0.043(2) 0.0012(16) 0.0039(15) -0.0041(15) C64 0.0297(17) 0.043(2) 0.049(2) 0.0038(17) -0.0061(16) -0.0072(15) C65 0.0385(19) 0.0364(18) 0.0360(19) -0.0010(14) -0.0057(15) -0.0081(15) C66 0.0318(17) 0.0358(18) 0.0322(18) -0.0028(14) 0.0010(14) -0.0041(14) C67 0.036(2) 0.053(2) 0.054(3) -0.0004(19) 0.0075(18) -0.0038(18) C68 0.043(2) 0.057(2) 0.039(2) -0.0012(18) -0.0114(17) -0.0074(19) B2 0.0289(18) 0.0317(18) 0.0311(19) -0.0069(15) -0.0003(15) -0.0047(15) C75 0.061(3) 0.057(3) 0.043(2) -0.015(2) -0.002(2) -0.018(2) F25 0.136(5) 0.099(4) 0.057(3) -0.020(2) -0.024(3) -0.063(4) F26 0.118(5) 0.294(10) 0.032(2) -0.021(4) 0.015(3) -0.128(7) F27 0.182(8) 0.117(4) 0.094(5) -0.064(4) -0.095(5) 0.062(5) C75A 0.061(3) 0.057(3) 0.043(2) -0.015(2) -0.002(2) -0.018(2) F25A 0.136(5) 0.099(4) 0.057(3) -0.020(2) -0.024(3) -0.063(4) F26A 0.118(5) 0.294(10) 0.032(2) -0.021(4) 0.015(3) -0.128(7) F27A 0.182(8) 0.117(4) 0.094(5) -0.064(4) -0.095(5) 0.062(5) F28 0.111(3) 0.0361(14) 0.138(3) 0.0074(17) -0.022(2) -0.0111(15) F29 0.0489(18) 0.103(3) 0.170(4) 0.049(3) 0.015(2) 0.0232(17) F30 0.150(3) 0.072(2) 0.070(2) 0.0009(16) -0.033(2) 0.045(2) F31 0.0429(17) 0.101(3) 0.194(5) 0.023(3) 0.023(2) -0.0070(17) F32 0.0450(16) 0.0672(19) 0.178(4) -0.026(2) -0.0183(19) -0.0015(14) F33 0.0451(18) 0.290(6) 0.117(3) -0.090(4) -0.030(2) -0.002(3) F34 0.122(3) 0.116(3) 0.0332(15) -0.0126(16) -0.0045(16) 0.004(2) F35 0.109(2) 0.0775(19) 0.093(2) -0.0511(18) 0.0368(19) -0.0496(18) F36 0.0627(17) 0.099(2) 0.0571(17) -0.0334(15) 0.0189(13) -0.0225(15) F37 0.0685(18) 0.139(3) 0.0352(14) -0.0085(15) -0.0108(12) -0.0465(18) F38 0.080(2) 0.0672(18) 0.119(3) -0.0038(18) -0.062(2) 0.0054(16) F39 0.0529(15) 0.098(2) 0.0618(16) 0.0028(15) -0.0178(12) -0.0427(15) F40 0.059(2) 0.140(3) 0.050(2) 0.024(2) 0.0136(16) -0.030(2) F41 0.103(3) 0.099(3) 0.087(3) 0.057(3) 0.017(3) 0.012(3) F42 0.245(7) 0.237(7) 0.0236(18) -0.009(3) -0.001(3) -0.191(6) F40A 0.059(2) 0.140(3) 0.050(2) 0.024(2) 0.0136(16) -0.030(2) F41A 0.103(3) 0.099(3) 0.087(3) 0.057(3) 0.017(3) 0.012(3) F42A 0.245(7) 0.237(7) 0.0236(18) -0.009(3) -0.001(3) -0.191(6) F43 0.0710(18) 0.0509(15) 0.118(3) 0.0027(15) 0.0469(18) -0.0216(13) F44 0.077(2) 0.136(3) 0.0458(16) -0.0205(17) 0.0244(14) -0.0372(19) F45 0.0392(13) 0.0751(18) 0.084(2) 0.0098(15) 0.0223(13) -0.0029(12) F46 0.0647(17) 0.096(2) 0.0522(16) 0.0061(15) -0.0059(13) 0.0228(15) F47 0.089(2) 0.097(2) 0.168(4) -0.091(3) -0.059(2) 0.047(2) F48 0.0355(15) 0.108(3) 0.169(4) 0.068(3) 0.0183(18) 0.0090(15) C69 0.0260(15) 0.0343(16) 0.0315(17) -0.0053(13) -0.0007(12) -0.0068(13) C70 0.0315(17) 0.0391(18) 0.0301(17) -0.0031(14) -0.0011(13) -0.0074(14) C71 0.0404(19) 0.043(2) 0.0325(19) -0.0078(15) 0.0029(15) -0.0093(16) C72 0.046(2) 0.042(2) 0.044(2) -0.0184(17) 0.0042(17) -0.0098(17) C73 0.0362(18) 0.0343(18) 0.043(2) -0.0078(15) -0.0019(15) -0.0048(14) C74 0.0321(17) 0.0358(17) 0.0331(18) -0.0041(14) -0.0038(14) -0.0048(14) C76 0.055(3) 0.046(2) 0.055(3) -0.0066(19) -0.008(2) 0.0061(19) C77 0.0313(16) 0.0335(17) 0.0301(17) -0.0038(13) -0.0027(13) -0.0089(13) C78 0.0311(17) 0.0398(18) 0.040(2) -0.0085(15) -0.0013(14) -0.0095(14) C79 0.0324(18) 0.052(2) 0.047(2) -0.0055(17) -0.0061(16) -0.0149(16) C80 0.047(2) 0.051(2) 0.039(2) -0.0041(17) -0.0101(17) -0.0183(18) C81 0.050(2) 0.0412(19) 0.0323(18) -0.0076(15) -0.0007(16) -0.0179(17) C82 0.0325(17) 0.0360(17) 0.0354(18) -0.0045(14) -0.0014(14) -0.0116(14) C83 0.037(2) 0.068(3) 0.079(3) -0.018(3) -0.012(2) -0.014(2) C84 0.061(3) 0.055(2) 0.040(2) -0.0164(19) 0.0051(19) -0.021(2) C85 0.0276(16) 0.0310(16) 0.0299(17) -0.0080(13) -0.0002(13) -0.0055(13) C86 0.0339(17) 0.0345(17) 0.0253(16) -0.0050(13) -0.0028(13) -0.0083(13) C87 0.0312(16) 0.0357(17) 0.0312(17) -0.0075(13) -0.0061(13) -0.0076(14) C88 0.0331(17) 0.0388(18) 0.0363(19) -0.0078(14) 0.0029(14) -0.0135(14) C89 0.0367(18) 0.0367(18) 0.0288(17) -0.0062(14) 0.0005(14) -0.0111(14) C90 0.0358(17) 0.0337(17) 0.0278(16) -0.0041(13) -0.0052(13) -0.0088(14) C91 0.041(2) 0.059(2) 0.042(2) -0.0011(18) -0.0085(17) -0.0190(19) C92 0.051(2) 0.067(3) 0.035(2) -0.0018(19) 0.0002(18) -0.024(2) C93 0.0306(16) 0.0336(17) 0.0296(17) -0.0088(13) 0.0013(13) -0.0069(13) C94 0.0323(17) 0.0351(17) 0.0367(19) -0.0070(14) 0.0024(14) -0.0053(14) C95 0.0330(17) 0.0386(18) 0.0373(19) -0.0082(15) 0.0072(14) -0.0114(14) C96 0.0388(18) 0.0345(17) 0.0322(18) -0.0025(14) 0.0018(14) -0.0086(14) C97 0.0329(17) 0.0348(17) 0.0303(17) -0.0066(13) 0.0001(13) -0.0059(14) C98 0.0317(17) 0.0333(17) 0.0324(17) -0.0076(13) 0.0046(13) -0.0072(13) C99 0.043(2) 0.046(2) 0.051(2) -0.0019(18) 0.0136(18) -0.0107(17) C100 0.0383(19) 0.0378(19) 0.044(2) -0.0007(16) 0.0034(16) -0.0027(15) Cl1A 0.208(3) 0.205(3) 0.208(4) -0.004(2) -0.008(3) -0.051(3) C1A 0.208(3) 0.205(3) 0.208(4) -0.004(2) -0.008(3) -0.051(3) Cl2A 0.208(3) 0.205(3) 0.208(4) -0.004(2) -0.008(3) -0.051(3) Cl1B 0.279(9) 0.142(4) 0.116(4) 0.044(3) -0.074(5) -0.076(5) C1B 0.279(9) 0.142(4) 0.116(4) 0.044(3) -0.074(5) -0.076(5) Cl2B 0.279(9) 0.142(4) 0.116(4) 0.044(3) -0.074(5) -0.076(5) Cl1C 0.26(2) 0.135(13) 0.158(17) 0.011(11) 0.049(17) -0.039(14) C1C 0.26(2) 0.135(13) 0.158(17) 0.011(11) 0.049(17) -0.039(14) Cl2C 0.26(2) 0.135(13) 0.158(17) 0.011(11) 0.049(17) -0.039(14) _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 2.083(3) . ? Ir1 N3 2.089(3) . ? Ir1 C1 2.111(4) . ? Ir1 C6 2.130(4) . ? Ir1 C5 2.130(4) . ? Ir1 C2 2.134(4) . ? Ir2 N7 2.086(3) . ? Ir2 N5 2.095(3) . ? Ir2 C21 2.117(4) . ? Ir2 C16 2.126(4) . ? Ir2 C17 2.130(4) . ? Ir2 C20 2.132(4) . ? C16 C17 1.417(7) . ? C16 C23 1.530(4) . ? C16 H16 1.0000 . ? C17 C18 1.530(4) . ? C17 H17 1.0000 . ? C18 C19 1.537(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.530(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.395(7) . ? C20 H20 1.0000 . ? C21 C22 1.530(4) . ? C21 H21 1.0000 . ? C22 C23 1.537(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C18A C19A 1.537(7) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C22A C23A 1.537(7) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? N1 C9 1.341(5) . ? N1 N2 1.354(4) . ? N2 C11 1.362(5) . ? N2 C15 1.447(5) . ? N3 C12 1.338(5) . ? N3 N4 1.347(4) . ? N4 C14 1.348(5) . ? N4 C15 1.450(5) . ? N5 C24 1.327(5) . ? N5 N6 1.361(5) . ? N6 C26 1.349(5) . ? N6 C30 1.453(5) . ? N7 C27 1.334(4) . ? N7 N8 1.360(4) . ? N8 C29 1.357(4) . ? N8 C30 1.452(4) . ? C1 C2 1.405(7) . ? C1 C8 1.513(8) . ? C1 H1 1.0000 . ? C2 C3 1.508(7) . ? C2 H2 1.0000 . ? C3 C4 1.477(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.521(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.405(6) . ? C5 H5 1.0000 . ? C6 C7 1.516(7) . ? C6 H6 1.0000 . ? C7 C8 1.497(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.389(6) . ? C9 H9 0.9500 . ? C10 C11 1.350(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.370(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C31 1.525(5) . ? C15 H15 1.0000 . ? C24 C25 1.380(7) . ? C24 H24 0.9500 . ? C25 C26 1.365(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.385(6) . ? C27 H27 0.9500 . ? C28 C29 1.371(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C33 1.529(5) . ? C30 H30 1.0000 . ? C31 C36 1.388(5) . ? C31 C32 1.396(5) . ? C32 C33 1.381(5) . ? C32 H32 0.9500 . ? C33 C34 1.387(5) . ? C34 C35 1.391(5) . ? C34 H34 0.9500 . ? C35 C36 1.385(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? B1 C61 1.638(5) . ? B1 C53 1.640(5) . ? B1 C45 1.653(5) . ? B1 C37 1.654(5) . ? F1 C43 1.312(5) . ? F2 C43 1.321(5) . ? F3 C43 1.283(5) . ? F4 C44 1.338(5) . ? F5 C44 1.338(5) . ? F6 C44 1.316(5) . ? C51 F8 1.308(3) . ? C51 F7 1.308(3) . ? C51 F9 1.308(3) . ? C51 C47 1.502(6) . ? C51A F9A 1.308(3) . ? C51A F7A 1.308(3) . ? C51A F8A 1.308(3) . ? C51A C47 1.502(6) . ? C52 F10 1.307(3) . ? C52 F11 1.307(3) . ? C52 F12 1.307(3) . ? C52 C49 1.492(6) . ? C52A F12A 1.307(3) . ? C52A F11A 1.307(3) . ? C52A F10A 1.307(3) . ? C52A C49 1.492(6) . ? F13 C59 1.327(5) . ? F14 C59 1.326(5) . ? F15 C59 1.309(5) . ? F16 C60 1.339(5) . ? F17 C60 1.323(5) . ? F18 C60 1.319(5) . ? F19 C67 1.290(3) . ? F20 C67 1.290(3) . ? F21 C67 1.290(3) . ? F19A C67 1.290(3) . ? F20A C67 1.290(3) . ? F21A C67 1.290(3) . ? F22 C68 1.322(5) . ? F23 C68 1.325(5) . ? F24 C68 1.308(5) . ? C37 C38 1.397(5) . ? C37 C42 1.405(5) . ? C38 C39 1.387(5) . ? C38 H38 0.9500 . ? C39 C40 1.390(5) . ? C39 C43 1.505(5) . ? C40 C41 1.381(5) . ? C40 H40 0.9500 . ? C41 C42 1.402(5) . ? C41 C44 1.496(5) . ? C42 H42 0.9500 . ? C45 C46 1.396(5) . ? C45 C50 1.400(5) . ? C46 C47 1.392(5) . ? C46 H46 0.9500 . ? C47 C48 1.381(6) . ? C48 C49 1.381(6) . ? C48 H48 0.9500 . ? C49 C50 1.389(5) . ? C50 H50 0.9500 . ? C53 C58 1.396(5) . ? C53 C54 1.402(5) . ? C54 C55 1.397(5) . ? C54 H54 0.9500 . ? C55 C56 1.395(5) . ? C55 C59 1.489(5) . ? C56 C57 1.377(5) . ? C56 H56 0.9500 . ? C57 C58 1.394(5) . ? C57 C60 1.493(5) . ? C58 H58 0.9500 . ? C61 C62 1.400(5) . ? C61 C66 1.401(5) . ? C62 C63 1.395(5) . ? C62 H62 0.9500 . ? C63 C64 1.380(5) . ? C63 C67 1.495(5) . ? C64 C65 1.385(5) . ? C64 H64 0.9500 . ? C65 C66 1.389(5) . ? C65 C68 1.500(5) . ? C66 H66 0.9500 . ? B2 C77 1.638(5) . ? B2 C93 1.638(5) . ? B2 C85 1.642(5) . ? B2 C69 1.647(5) . ? C75 F26 1.304(3) . ? C75 F25 1.304(3) . ? C75 F27 1.304(3) . ? C75 C71 1.490(6) . ? C75A F27A 1.304(3) . ? C75A F25A 1.304(3) . ? C75A F26A 1.304(3) . ? C75A C71 1.490(6) . ? F28 C76 1.335(5) . ? F29 C76 1.304(6) . ? F30 C76 1.315(6) . ? F31 C83 1.335(6) . ? F32 C83 1.299(5) . ? F33 C83 1.290(6) . ? F34 C84 1.324(5) . ? F35 C84 1.341(5) . ? F36 C84 1.325(5) . ? F37 C91 1.347(5) . ? F38 C91 1.325(5) . ? F39 C91 1.317(5) . ? F40 C92 1.309(3) . ? F41 C92 1.309(3) . ? F42 C92 1.309(3) . ? F40A C92 1.309(3) . ? F41A C92 1.309(3) . ? F42A C92 1.309(3) . ? F43 C99 1.322(5) . ? F44 C99 1.330(5) . ? F45 C99 1.337(5) . ? F46 C100 1.324(5) . ? F47 C100 1.292(5) . ? F48 C100 1.325(5) . ? C69 C74 1.395(5) . ? C69 C70 1.401(5) . ? C70 C71 1.393(5) . ? C70 H70 0.9500 . ? C71 C72 1.378(5) . ? C72 C73 1.382(5) . ? C72 H72 0.9500 . ? C73 C74 1.391(5) . ? C73 C76 1.491(5) . ? C74 H74 0.9500 . ? C77 C78 1.390(5) . ? C77 C82 1.407(5) . ? C78 C79 1.398(5) . ? C78 H78 0.9500 . ? C79 C80 1.378(6) . ? C79 C83 1.490(6) . ? C80 C81 1.394(5) . ? C80 H80 0.9500 . ? C81 C82 1.373(5) . ? C81 C84 1.500(5) . ? C82 H82 0.9500 . ? C85 C86 1.398(4) . ? C85 C90 1.399(5) . ? C86 C87 1.390(5) . ? C86 H86 0.9500 . ? C87 C88 1.382(5) . ? C87 C91 1.489(5) . ? C88 C89 1.390(5) . ? C88 H88 0.9500 . ? C89 C90 1.393(5) . ? C89 C92 1.481(5) . ? C90 H90 0.9500 . ? C93 C94 1.393(5) . ? C93 C98 1.405(5) . ? C94 C95 1.381(5) . ? C94 H94 0.9500 . ? C95 C96 1.393(5) . ? C95 C99 1.499(5) . ? C96 C97 1.381(5) . ? C96 H96 0.9500 . ? C97 C98 1.389(5) . ? C97 C100 1.499(5) . ? C98 H98 0.9500 . ? Cl1A C1A 1.709(10) . ? C1A Cl2A 1.709(10) . ? C1A H1A 0.9900 . ? C1A H1B 0.9900 . ? Cl1B C1B 1.709(10) . ? C1B Cl2B 1.709(10) . ? C1B H1C 0.9900 . ? C1B H1D 0.9900 . ? Cl1C C1C 1.709(10) . ? C1C Cl2C 1.709(10) . ? C1C H1E 0.9900 . ? C1C H1F 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 N1 Ir1 N3 86.59(12) . . ? N1 Ir1 C1 162.28(16) . . ? N3 Ir1 C1 93.03(16) . . ? N1 Ir1 C6 94.35(14) . . ? N3 Ir1 C6 164.65(15) . . ? C1 Ir1 C6 81.44(19) . . ? N1 Ir1 C5 90.47(15) . . ? N3 Ir1 C5 156.81(16) . . ? C1 Ir1 C5 96.59(18) . . ? C6 Ir1 C5 38.52(17) . . ? N1 Ir1 C2 159.08(16) . . ? N3 Ir1 C2 93.29(17) . . ? C1 Ir1 C2 38.64(18) . . ? C6 Ir1 C2 91.25(19) . . ? C5 Ir1 C2 81.44(18) . . ? N7 Ir2 N5 86.37(12) . . ? N7 Ir2 C21 155.01(15) . . ? N5 Ir2 C21 92.41(14) . . ? N7 Ir2 C16 91.49(14) . . ? N5 Ir2 C16 159.96(17) . . ? C21 Ir2 C16 81.19(16) . . ? N7 Ir2 C17 95.05(14) . . ? N5 Ir2 C17 161.14(18) . . ? C21 Ir2 C17 94.05(18) . . ? C16 Ir2 C17 38.9(2) . . ? N7 Ir2 C20 166.65(17) . . ? N5 Ir2 C20 93.24(15) . . ? C21 Ir2 C20 38.33(18) . . ? C16 Ir2 C20 93.34(18) . . ? C17 Ir2 C20 81.07(17) . . ? C17 C16 C23 135.8(6) . . ? C17 C16 Ir2 70.7(3) . . ? C23 C16 Ir2 109.6(6) . . ? C17 C16 H16 110.4 . . ? C23 C16 H16 110.4 . . ? Ir2 C16 H16 110.4 . . ? C16 C17 C18 113.5(10) . . ? C16 C17 Ir2 70.4(2) . . ? C18 C17 Ir2 118.1(7) . . ? C16 C17 H17 115.7 . . ? C18 C17 H17 115.7 . . ? Ir2 C17 H17 115.7 . . ? C17 C18 C19 102.4(10) . . ? C17 C18 H18A 111.3 . . ? C19 C18 H18A 111.3 . . ? C17 C18 H18B 111.3 . . ? C19 C18 H18B 111.3 . . ? H18A C18 H18B 109.2 . . ? C20 C19 C18 118.2(15) . . ? C20 C19 H19A 107.8 . . ? C18 C19 H19A 107.8 . . ? C20 C19 H19B 107.8 . . ? C18 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? C21 C20 C19 130.9(8) . . ? C21 C20 Ir2 70.2(2) . . ? C19 C20 Ir2 105.9(7) . . ? C21 C20 H20 113.0 . . ? C19 C20 H20 113.0 . . ? Ir2 C20 H20 113.0 . . ? C20 C21 C22 116.8(8) . . ? C20 C21 Ir2 71.4(2) . . ? C22 C21 Ir2 113.9(6) . . ? C20 C21 H21 115.8 . . ? C22 C21 H21 115.8 . . ? Ir2 C21 H21 115.8 . . ? C21 C22 C23 110.6(9) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C16 C23 C22 110.2(10) . . ? C16 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C16 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C19A C18A H18C 108.0 . . ? C19A C18A H18D 108.0 . . ? H18C C18A H18D 107.3 . . ? C18A C19A H19C 110.8 . . ? C18A C19A H19D 110.8 . . ? H19C C19A H19D 108.9 . . ? C23A C22A H22C 109.5 . . ? C23A C22A H22D 109.5 . . ? H22C C22A H22D 108.1 . . ? C22A C23A H23C 109.9 . . ? C22A C23A H23D 109.9 . . ? H23C C23A H23D 108.3 . . ? C9 N1 N2 105.2(3) . . ? C9 N1 Ir1 133.7(3) . . ? N2 N1 Ir1 121.0(2) . . ? N1 N2 C11 110.5(3) . . ? N1 N2 C15 120.2(3) . . ? C11 N2 C15 129.0(3) . . ? C12 N3 N4 104.8(3) . . ? C12 N3 Ir1 133.8(3) . . ? N4 N3 Ir1 121.2(2) . . ? N3 N4 C14 112.4(3) . . ? N3 N4 C15 119.9(3) . . ? C14 N4 C15 127.4(4) . . ? C24 N5 N6 105.6(3) . . ? C24 N5 Ir2 133.7(3) . . ? N6 N5 Ir2 120.5(2) . . ? C26 N6 N5 110.9(3) . . ? C26 N6 C30 128.6(4) . . ? N5 N6 C30 120.1(3) . . ? C27 N7 N8 105.4(3) . . ? C27 N7 Ir2 134.0(3) . . ? N8 N7 Ir2 120.3(2) . . ? C29 N8 N7 110.6(3) . . ? C29 N8 C30 128.5(3) . . ? N7 N8 C30 120.9(3) . . ? C2 C1 C8 125.6(5) . . ? C2 C1 Ir1 71.6(2) . . ? C8 C1 Ir1 111.5(3) . . ? C2 C1 H1 113.6 . . ? C8 C1 H1 113.6 . . ? Ir1 C1 H1 113.6 . . ? C1 C2 C3 122.8(5) . . ? C1 C2 Ir1 69.8(2) . . ? C3 C2 Ir1 112.7(3) . . ? C1 C2 H2 114.5 . . ? C3 C2 H2 114.5 . . ? Ir1 C2 H2 114.5 . . ? C4 C3 C2 114.4(4) . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 113.8(4) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.9(4) . . ? C6 C5 Ir1 70.7(2) . . ? C4 C5 Ir1 110.5(3) . . ? C6 C5 H5 113.8 . . ? C4 C5 H5 113.8 . . ? Ir1 C5 H5 113.8 . . ? C5 C6 C7 124.0(4) . . ? C5 C6 Ir1 70.8(2) . . ? C7 C6 Ir1 113.5(3) . . ? C5 C6 H6 113.8 . . ? C7 C6 H6 113.8 . . ? Ir1 C6 H6 113.8 . . ? C8 C7 C6 113.2(4) . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C1 114.3(4) . . ? C7 C8 H8A 108.7 . . ? C1 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C10 110.8(4) . . ? N1 C9 H9 124.6 . . ? C10 C9 H9 124.6 . . ? C11 C10 C9 105.8(4) . . ? C11 C10 H10 127.1 . . ? C9 C10 H10 127.1 . . ? C10 C11 N2 107.7(4) . . ? C10 C11 H11 126.2 . . ? N2 C11 H11 126.2 . . ? N3 C12 C13 110.6(4) . . ? N3 C12 H12 124.7 . . ? C13 C12 H12 124.7 . . ? C14 C13 C12 106.2(4) . . ? C14 C13 H13 126.9 . . ? C12 C13 H13 126.9 . . ? N4 C14 C13 105.9(4) . . ? N4 C14 H14 127.0 . . ? C13 C14 H14 127.0 . . ? N2 C15 N4 109.9(3) . . ? N2 C15 C31 112.9(3) . . ? N4 C15 C31 112.4(3) . . ? N2 C15 H15 107.1 . . ? N4 C15 H15 107.1 . . ? C31 C15 H15 107.1 . . ? N5 C24 C25 110.5(5) . . ? N5 C24 H24 124.8 . . ? C25 C24 H24 124.8 . . ? C26 C25 C24 106.5(4) . . ? C26 C25 H25 126.8 . . ? C24 C25 H25 126.8 . . ? N6 C26 C25 106.6(4) . . ? N6 C26 H26 126.7 . . ? C25 C26 H26 126.7 . . ? N7 C27 C28 111.3(4) . . ? N7 C27 H27 124.3 . . ? C28 C27 H27 124.3 . . ? C29 C28 C27 105.3(3) . . ? C29 C28 H28 127.3 . . ? C27 C28 H28 127.3 . . ? N8 C29 C28 107.4(3) . . ? N8 C29 H29 126.3 . . ? C28 C29 H29 126.3 . . ? N8 C30 N6 109.0(3) . . ? N8 C30 C33 113.2(3) . . ? N6 C30 C33 111.4(3) . . ? N8 C30 H30 107.7 . . ? N6 C30 H30 107.7 . . ? C33 C30 H30 107.7 . . ? C36 C31 C32 119.5(3) . . ? C36 C31 C15 121.0(3) . . ? C32 C31 C15 119.3(3) . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 C30 119.4(3) . . ? C34 C33 C30 120.5(3) . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.5(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 119.8(3) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C61 B1 C53 108.2(3) . . ? C61 B1 C45 111.6(3) . . ? C53 B1 C45 109.9(3) . . ? C61 B1 C37 108.2(3) . . ? C53 B1 C37 111.3(3) . . ? C45 B1 C37 107.5(3) . . ? F8 C51 F7 109.9(7) . . ? F8 C51 F9 105.8(6) . . ? F7 C51 F9 105.2(6) . . ? F8 C51 C47 108.7(4) . . ? F7 C51 C47 111.8(5) . . ? F9 C51 C47 115.3(4) . . ? F9A C51A F7A 104.2(9) . . ? F9A C51A F8A 100.2(9) . . ? F7A C51A F8A 104.2(9) . . ? F9A C51A C47 117.9(6) . . ? F7A C51A C47 115.4(7) . . ? F8A C51A C47 112.9(7) . . ? F10 C52 F11 105.9(6) . . ? F10 C52 F12 105.5(6) . . ? F11 C52 F12 103.7(5) . . ? F10 C52 C49 112.5(4) . . ? F11 C52 C49 113.4(4) . . ? F12 C52 C49 115.1(4) . . ? F12A C52A F11A 103.6(16) . . ? F12A C52A F10A 111.0(18) . . ? F11A C52A F10A 108.8(18) . . ? F12A C52A C49 113.7(14) . . ? F11A C52A C49 112.2(14) . . ? F10A C52A C49 107.5(15) . . ? C38 C37 C42 115.7(3) . . ? C38 C37 B1 122.8(3) . . ? C42 C37 B1 121.3(3) . . ? C39 C38 C37 122.8(3) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C38 C39 C40 120.8(3) . . ? C38 C39 C43 120.3(4) . . ? C40 C39 C43 118.9(3) . . ? C41 C40 C39 117.8(3) . . ? C41 C40 H40 121.1 . . ? C39 C40 H40 121.1 . . ? C40 C41 C42 121.5(3) . . ? C40 C41 C44 119.8(3) . . ? C42 C41 C44 118.6(3) . . ? C41 C42 C37 121.4(3) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? F3 C43 F1 107.6(4) . . ? F3 C43 F2 106.5(4) . . ? F1 C43 F2 102.8(4) . . ? F3 C43 C39 113.4(3) . . ? F1 C43 C39 113.7(3) . . ? F2 C43 C39 112.1(4) . . ? F6 C44 F5 107.6(4) . . ? F6 C44 F4 106.0(4) . . ? F5 C44 F4 103.4(3) . . ? F6 C44 C41 114.0(3) . . ? F5 C44 C41 113.6(3) . . ? F4 C44 C41 111.4(3) . . ? C46 C45 C50 115.4(3) . . ? C46 C45 B1 122.5(3) . . ? C50 C45 B1 121.8(3) . . ? C47 C46 C45 122.5(3) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C48 C47 C46 120.6(4) . . ? C48 C47 C51A 121.4(4) . . ? C46 C47 C51A 117.3(4) . . ? C48 C47 C51 117.1(4) . . ? C46 C47 C51 122.1(4) . . ? C49 C48 C47 118.1(4) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? C48 C49 C50 121.0(4) . . ? C48 C49 C52A 116.6(7) . . ? C50 C49 C52A 122.4(8) . . ? C48 C49 C52 120.4(3) . . ? C50 C49 C52 118.6(4) . . ? C49 C50 C45 122.3(4) . . ? C49 C50 H50 118.9 . . ? C45 C50 H50 118.9 . . ? C58 C53 C54 115.2(3) . . ? C58 C53 B1 122.8(3) . . ? C54 C53 B1 122.0(3) . . ? C55 C54 C53 122.7(3) . . ? C55 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? C56 C55 C54 120.2(3) . . ? C56 C55 C59 118.9(3) . . ? C54 C55 C59 120.8(3) . . ? C57 C56 C55 118.2(3) . . ? C57 C56 H56 120.9 . . ? C55 C56 H56 120.9 . . ? C56 C57 C58 121.0(3) . . ? C56 C57 C60 119.8(3) . . ? C58 C57 C60 119.2(3) . . ? C57 C58 C53 122.7(3) . . ? C57 C58 H58 118.7 . . ? C53 C58 H58 118.7 . . ? F15 C59 F14 105.9(4) . . ? F15 C59 F13 105.9(3) . . ? F14 C59 F13 103.7(4) . . ? F15 C59 C55 114.2(4) . . ? F14 C59 C55 111.8(3) . . ? F13 C59 C55 114.6(3) . . ? F18 C60 F17 106.7(3) . . ? F18 C60 F16 105.8(3) . . ? F17 C60 F16 105.1(3) . . ? F18 C60 C57 112.8(3) . . ? F17 C60 C57 112.9(3) . . ? F16 C60 C57 113.0(3) . . ? C62 C61 C66 115.8(3) . . ? C62 C61 B1 120.8(3) . . ? C66 C61 B1 123.3(3) . . ? C63 C62 C61 122.0(3) . . ? C63 C62 H62 119.0 . . ? C61 C62 H62 119.0 . . ? C64 C63 C62 120.9(3) . . ? C64 C63 C67 119.3(3) . . ? C62 C63 C67 119.8(3) . . ? C63 C64 C65 118.4(3) . . ? C63 C64 H64 120.8 . . ? C65 C64 H64 120.8 . . ? C64 C65 C66 120.6(3) . . ? C64 C65 C68 118.0(3) . . ? C66 C65 C68 121.4(3) . . ? C65 C66 C61 122.4(3) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? F21 C67 F21A 132.6(5) . . ? F21 C67 F19 103.0(7) . . ? F21A C67 F19 54.3(6) . . ? F21 C67 F19A 54.3(6) . . ? F21A C67 F19A 105.7(6) . . ? F19 C67 F19A 130.5(5) . . ? F21 C67 F20 105.4(8) . . ? F21A C67 F20 56.2(8) . . ? F19 C67 F20 106.1(9) . . ? F19A C67 F20 54.5(7) . . ? F21 C67 F20A 52.1(6) . . ? F21A C67 F20A 105.5(7) . . ? F19 C67 F20A 54.9(7) . . ? F19A C67 F20A 102.3(7) . . ? F20 C67 F20A 133.1(5) . . ? F21 C67 C63 113.7(5) . . ? F21A C67 C63 113.7(4) . . ? F19 C67 C63 114.9(4) . . ? F19A C67 C63 114.6(4) . . ? F20 C67 C63 112.9(5) . . ? F20A C67 C63 113.9(4) . . ? F24 C68 F22 107.5(4) . . ? F24 C68 F23 106.0(4) . . ? F22 C68 F23 105.2(3) . . ? F24 C68 C65 113.4(3) . . ? F22 C68 C65 111.4(4) . . ? F23 C68 C65 112.8(4) . . ? C77 B2 C93 106.5(3) . . ? C77 B2 C85 112.4(3) . . ? C93 B2 C85 112.5(3) . . ? C77 B2 C69 113.4(3) . . ? C93 B2 C69 109.9(3) . . ? C85 B2 C69 102.2(3) . . ? F26 C75 F25 103.7(5) . . ? F26 C75 F27 107.3(7) . . ? F25 C75 F27 102.6(5) . . ? F26 C75 C71 112.2(4) . . ? F25 C75 C71 116.0(4) . . ? F27 C75 C71 114.0(4) . . ? F27A C75A F25A 105.5(13) . . ? F27A C75A F26A 106.7(14) . . ? F25A C75A F26A 99.7(11) . . ? F27A C75A C71 116.2(9) . . ? F25A C75A C71 116.1(8) . . ? F26A C75A C71 111.0(9) . . ? C74 C69 C70 115.5(3) . . ? C74 C69 B2 123.2(3) . . ? C70 C69 B2 120.7(3) . . ? C71 C70 C69 122.1(3) . . ? C71 C70 H70 118.9 . . ? C69 C70 H70 118.9 . . ? C72 C71 C70 121.0(3) . . ? C72 C71 C75A 120.7(5) . . ? C70 C71 C75A 118.2(5) . . ? C72 C71 C75 119.2(3) . . ? C70 C71 C75 119.8(3) . . ? C71 C72 C73 117.9(3) . . ? C71 C72 H72 121.0 . . ? C73 C72 H72 121.0 . . ? C72 C73 C74 121.0(3) . . ? C72 C73 C76 118.6(3) . . ? C74 C73 C76 120.4(3) . . ? C73 C74 C69 122.3(3) . . ? C73 C74 H74 118.8 . . ? C69 C74 H74 118.8 . . ? F29 C76 F30 107.4(4) . . ? F29 C76 F28 104.6(4) . . ? F30 C76 F28 104.2(4) . . ? F29 C76 C73 113.2(4) . . ? F30 C76 C73 113.8(3) . . ? F28 C76 C73 112.9(4) . . ? C78 C77 C82 115.6(3) . . ? C78 C77 B2 122.9(3) . . ? C82 C77 B2 121.5(3) . . ? C77 C78 C79 122.0(3) . . ? C77 C78 H78 119.0 . . ? C79 C78 H78 119.0 . . ? C80 C79 C78 121.1(3) . . ? C80 C79 C83 120.2(4) . . ? C78 C79 C83 118.7(4) . . ? C79 C80 C81 117.8(3) . . ? C79 C80 H80 121.1 . . ? C81 C80 H80 121.1 . . ? C82 C81 C80 120.7(3) . . ? C82 C81 C84 121.1(4) . . ? C80 C81 C84 118.2(3) . . ? C81 C82 C77 122.7(3) . . ? C81 C82 H82 118.6 . . ? C77 C82 H82 118.6 . . ? F33 C83 F32 108.6(5) . . ? F33 C83 F31 102.3(5) . . ? F32 C83 F31 102.7(4) . . ? F33 C83 C79 114.3(4) . . ? F32 C83 C79 114.5(4) . . ? F31 C83 C79 113.1(4) . . ? F34 C84 F36 106.6(4) . . ? F34 C84 F35 105.6(4) . . ? F36 C84 F35 105.2(4) . . ? F34 C84 C81 112.9(4) . . ? F36 C84 C81 114.0(3) . . ? F35 C84 C81 111.8(3) . . ? C86 C85 C90 114.8(3) . . ? C86 C85 B2 121.0(3) . . ? C90 C85 B2 123.8(3) . . ? C87 C86 C85 123.0(3) . . ? C87 C86 H86 118.5 . . ? C85 C86 H86 118.5 . . ? C88 C87 C86 121.0(3) . . ? C88 C87 C91 120.3(3) . . ? C86 C87 C91 118.7(3) . . ? C87 C88 C89 117.6(3) . . ? C87 C88 H88 121.2 . . ? C89 C88 H88 121.2 . . ? C88 C89 C90 120.8(3) . . ? C88 C89 C92 119.7(3) . . ? C90 C89 C92 119.4(3) . . ? C89 C90 C85 122.8(3) . . ? C89 C90 H90 118.6 . . ? C85 C90 H90 118.6 . . ? F39 C91 F38 107.2(4) . . ? F39 C91 F37 105.3(3) . . ? F38 C91 F37 103.9(4) . . ? F39 C91 C87 114.5(3) . . ? F38 C91 C87 113.0(3) . . ? F37 C91 C87 112.0(3) . . ? F42 C92 F42A 130.5(10) . . ? F42 C92 F40A 59.0(15) . . ? F42A C92 F40A 102(2) . . ? F42 C92 F41A 45.9(13) . . ? F42A C92 F41A 105(2) . . ? F40A C92 F41A 99.5(17) . . ? F42 C92 F41 107.7(5) . . ? F42A C92 F41 59(2) . . ? F40A C92 F41 50.8(16) . . ? F41A C92 F41 132.4(10) . . ? F42 C92 F40 105.5(4) . . ? F42A C92 F40 49(2) . . ? F40A C92 F40 129.4(9) . . ? F41A C92 F40 62.5(14) . . ? F41 C92 F40 104.9(4) . . ? F42 C92 C89 111.5(3) . . ? F42A C92 C89 117.6(10) . . ? F40A C92 C89 115.8(9) . . ? F41A C92 C89 114.7(9) . . ? F41 C92 C89 112.1(3) . . ? F40 C92 C89 114.6(3) . . ? C94 C93 C98 115.5(3) . . ? C94 C93 B2 120.8(3) . . ? C98 C93 B2 123.7(3) . . ? C95 C94 C93 122.7(3) . . ? C95 C94 H94 118.6 . . ? C93 C94 H94 118.6 . . ? C94 C95 C96 120.9(3) . . ? C94 C95 C99 120.8(3) . . ? C96 C95 C99 118.1(3) . . ? C97 C96 C95 117.6(3) . . ? C97 C96 H96 121.2 . . ? C95 C96 H96 121.2 . . ? C96 C97 C98 121.2(3) . . ? C96 C97 C100 119.3(3) . . ? C98 C97 C100 119.4(3) . . ? C97 C98 C93 122.1(3) . . ? C97 C98 H98 119.0 . . ? C93 C98 H98 119.0 . . ? F43 C99 F44 106.5(4) . . ? F43 C99 F45 105.8(3) . . ? F44 C99 F45 105.0(3) . . ? F43 C99 C95 113.6(3) . . ? F44 C99 C95 112.2(3) . . ? F45 C99 C95 113.2(3) . . ? F47 C100 F46 106.2(4) . . ? F47 C100 F48 106.1(4) . . ? F46 C100 F48 102.9(4) . . ? F47 C100 C97 114.4(3) . . ? F46 C100 C97 113.2(3) . . ? F48 C100 C97 113.0(3) . . ? Cl2A C1A Cl1A 116.0(13) . . ? Cl2A C1A H1A 108.3 . . ? Cl1A C1A H1A 108.3 . . ? Cl2A C1A H1B 108.3 . . ? Cl1A C1A H1B 108.3 . . ? H1A C1A H1B 107.4 . . ? Cl1B C1B Cl2B 120.2(14) . . ? Cl1B C1B H1C 107.3 . . ? Cl2B C1B H1C 107.3 . . ? Cl1B C1B H1D 107.3 . . ? Cl2B C1B H1D 107.3 . . ? H1C C1B H1D 106.9 . . ? Cl1C C1C Cl2C 119(2) . . ? Cl1C C1C H1E 107.7 . . ? Cl2C C1C H1E 107.7 . . ? Cl1C C1C H1F 107.7 . . ? Cl2C C1C H1F 107.7 . . ? H1E C1C H1F 107.1 . . ? 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 N7 Ir2 C16 C17 -96.2(2) . . . . ? N5 Ir2 C16 C17 -179.7(4) . . . . ? C21 Ir2 C16 C17 107.8(3) . . . . ? C20 Ir2 C16 C17 71.3(3) . . . . ? N7 Ir2 C16 C23 130.8(5) . . . . ? N5 Ir2 C16 C23 47.3(8) . . . . ? C21 Ir2 C16 C23 -25.2(5) . . . . ? C17 Ir2 C16 C23 -133.0(6) . . . . ? C20 Ir2 C16 C23 -61.6(6) . . . . ? C23 C16 C17 C18 -14.4(12) . . . . ? Ir2 C16 C17 C18 -113.0(7) . . . . ? C23 C16 C17 Ir2 98.6(8) . . . . ? N7 Ir2 C17 C16 86.1(2) . . . . ? N5 Ir2 C17 C16 179.7(4) . . . . ? C21 Ir2 C17 C16 -70.6(3) . . . . ? C20 Ir2 C17 C16 -106.8(3) . . . . ? N7 Ir2 C17 C18 -167.1(10) . . . . ? N5 Ir2 C17 C18 -73.5(11) . . . . ? C21 Ir2 C17 C18 36.2(10) . . . . ? C16 Ir2 C17 C18 106.8(10) . . . . ? C20 Ir2 C17 C18 0.0(10) . . . . ? C16 C17 C18 C19 99.1(13) . . . . ? Ir2 C17 C18 C19 19.6(18) . . . . ? C17 C18 C19 C20 -40.1(19) . . . . ? C18 C19 C20 C21 -36.0(17) . . . . ? C18 C19 C20 Ir2 41.4(15) . . . . ? N7 Ir2 C20 C21 -177.7(5) . . . . ? N5 Ir2 C20 C21 -89.8(2) . . . . ? C16 Ir2 C20 C21 71.3(3) . . . . ? C17 Ir2 C20 C21 108.3(3) . . . . ? N7 Ir2 C20 C19 53.9(11) . . . . ? N5 Ir2 C20 C19 141.8(8) . . . . ? C21 Ir2 C20 C19 -128.4(8) . . . . ? C16 Ir2 C20 C19 -57.1(8) . . . . ? C17 Ir2 C20 C19 -20.1(8) . . . . ? C19 C20 C21 C22 -13.7(12) . . . . ? Ir2 C20 C21 C22 -108.0(7) . . . . ? C19 C20 C21 Ir2 94.3(9) . . . . ? N7 Ir2 C21 C20 178.8(3) . . . . ? N5 Ir2 C21 C20 92.2(3) . . . . ? C16 Ir2 C21 C20 -106.9(3) . . . . ? C17 Ir2 C21 C20 -70.1(3) . . . . ? N7 Ir2 C21 C22 -69.4(9) . . . . ? N5 Ir2 C21 C22 -156.0(9) . . . . ? C16 Ir2 C21 C22 4.9(9) . . . . ? C17 Ir2 C21 C22 41.7(9) . . . . ? C20 Ir2 C21 C22 111.8(9) . . . . ? C20 C21 C22 C23 96.7(12) . . . . ? Ir2 C21 C22 C23 16.3(15) . . . . ? C17 C16 C23 C22 -40.9(13) . . . . ? Ir2 C16 C23 C22 41.2(10) . . . . ? C21 C22 C23 C16 -37.3(15) . . . . ? N3 Ir1 N1 C9 145.0(3) . . . . ? C1 Ir1 N1 C9 55.8(7) . . . . ? C6 Ir1 N1 C9 -19.6(4) . . . . ? C5 Ir1 N1 C9 -58.0(4) . . . . ? C2 Ir1 N1 C9 -124.7(5) . . . . ? N3 Ir1 N1 N2 -31.4(2) . . . . ? C1 Ir1 N1 N2 -120.7(5) . . . . ? C6 Ir1 N1 N2 164.0(3) . . . . ? C5 Ir1 N1 N2 125.6(3) . . . . ? C2 Ir1 N1 N2 58.9(6) . . . . ? C9 N1 N2 C11 0.9(4) . . . . ? Ir1 N1 N2 C11 178.2(2) . . . . ? C9 N1 N2 C15 174.9(3) . . . . ? Ir1 N1 N2 C15 -7.8(4) . . . . ? N1 Ir1 N3 C12 -142.8(4) . . . . ? C1 Ir1 N3 C12 19.5(4) . . . . ? C6 Ir1 N3 C12 -48.8(8) . . . . ? C5 Ir1 N3 C12 134.0(5) . . . . ? C2 Ir1 N3 C12 58.2(4) . . . . ? N1 Ir1 N3 N4 30.5(3) . . . . ? C1 Ir1 N3 N4 -167.3(3) . . . . ? C6 Ir1 N3 N4 124.5(5) . . . . ? C5 Ir1 N3 N4 -52.7(5) . . . . ? C2 Ir1 N3 N4 -128.6(3) . . . . ? C12 N3 N4 C14 -1.0(4) . . . . ? Ir1 N3 N4 C14 -176.0(3) . . . . ? C12 N3 N4 C15 -175.2(3) . . . . ? Ir1 N3 N4 C15 9.8(4) . . . . ? N7 Ir2 N5 C24 141.9(4) . . . . ? C21 Ir2 N5 C24 -63.1(4) . . . . ? C16 Ir2 N5 C24 -133.7(5) . . . . ? C17 Ir2 N5 C24 46.9(7) . . . . ? C20 Ir2 N5 C24 -24.7(4) . . . . ? N7 Ir2 N5 N6 -31.9(3) . . . . ? C21 Ir2 N5 N6 123.1(3) . . . . ? C16 Ir2 N5 N6 52.4(5) . . . . ? C17 Ir2 N5 N6 -126.9(4) . . . . ? C20 Ir2 N5 N6 161.4(3) . . . . ? C24 N5 N6 C26 1.3(4) . . . . ? Ir2 N5 N6 C26 176.6(3) . . . . ? C24 N5 N6 C30 175.0(3) . . . . ? Ir2 N5 N6 C30 -9.7(4) . . . . ? N5 Ir2 N7 C27 -138.1(4) . . . . ? C21 Ir2 N7 C27 134.0(4) . . . . ? C16 Ir2 N7 C27 61.9(4) . . . . ? C17 Ir2 N7 C27 23.1(4) . . . . ? C20 Ir2 N7 C27 -49.3(8) . . . . ? N5 Ir2 N7 N8 33.6(2) . . . . ? C21 Ir2 N7 N8 -54.3(4) . . . . ? C16 Ir2 N7 N8 -126.5(3) . . . . ? C17 Ir2 N7 N8 -165.3(3) . . . . ? C20 Ir2 N7 N8 122.3(6) . . . . ? C27 N7 N8 C29 -1.4(4) . . . . ? Ir2 N7 N8 C29 -175.1(2) . . . . ? C27 N7 N8 C30 180.0(3) . . . . ? Ir2 N7 N8 C30 6.2(4) . . . . ? N1 Ir1 C1 C2 179.7(4) . . . . ? N3 Ir1 C1 C2 91.5(3) . . . . ? C6 Ir1 C1 C2 -102.9(3) . . . . ? C5 Ir1 C1 C2 -67.4(3) . . . . ? N1 Ir1 C1 C8 -58.3(7) . . . . ? N3 Ir1 C1 C8 -146.6(4) . . . . ? C6 Ir1 C1 C8 19.0(4) . . . . ? C5 Ir1 C1 C8 54.5(4) . . . . ? C2 Ir1 C1 C8 121.9(5) . . . . ? C8 C1 C2 C3 1.0(7) . . . . ? Ir1 C1 C2 C3 104.6(4) . . . . ? C8 C1 C2 Ir1 -103.6(5) . . . . ? N1 Ir1 C2 C1 -179.8(4) . . . . ? N3 Ir1 C2 C1 -90.7(3) . . . . ? C6 Ir1 C2 C1 74.6(3) . . . . ? C5 Ir1 C2 C1 112.0(3) . . . . ? N1 Ir1 C2 C3 62.1(7) . . . . ? N3 Ir1 C2 C3 151.1(4) . . . . ? C1 Ir1 C2 C3 -118.2(6) . . . . ? C6 Ir1 C2 C3 -43.6(4) . . . . ? C5 Ir1 C2 C3 -6.2(4) . . . . ? C1 C2 C3 C4 -88.6(7) . . . . ? Ir1 C2 C3 C4 -8.7(7) . . . . ? C2 C3 C4 C5 25.6(8) . . . . ? C3 C4 C5 C6 50.6(7) . . . . ? C3 C4 C5 Ir1 -29.9(6) . . . . ? N1 Ir1 C5 C6 96.4(3) . . . . ? N3 Ir1 C5 C6 178.8(3) . . . . ? C1 Ir1 C5 C6 -67.3(3) . . . . ? C2 Ir1 C5 C6 -103.0(3) . . . . ? N1 Ir1 C5 C4 -141.4(4) . . . . ? N3 Ir1 C5 C4 -59.0(6) . . . . ? C1 Ir1 C5 C4 54.9(4) . . . . ? C6 Ir1 C5 C4 122.2(5) . . . . ? C2 Ir1 C5 C4 19.2(4) . . . . ? C4 C5 C6 C7 4.1(7) . . . . ? Ir1 C5 C6 C7 105.9(4) . . . . ? C4 C5 C6 Ir1 -101.8(4) . . . . ? N1 Ir1 C6 C5 -85.3(3) . . . . ? N3 Ir1 C6 C5 -178.2(5) . . . . ? C1 Ir1 C6 C5 112.1(3) . . . . ? C2 Ir1 C6 C5 74.5(3) . . . . ? N1 Ir1 C6 C7 155.1(4) . . . . ? N3 Ir1 C6 C7 62.2(7) . . . . ? C1 Ir1 C6 C7 -7.6(4) . . . . ? C5 Ir1 C6 C7 -119.6(5) . . . . ? C2 Ir1 C6 C7 -45.1(4) . . . . ? C5 C6 C7 C8 -87.5(6) . . . . ? Ir1 C6 C7 C8 -5.6(6) . . . . ? C6 C7 C8 C1 22.0(8) . . . . ? C2 C1 C8 C7 54.2(7) . . . . ? Ir1 C1 C8 C7 -28.0(6) . . . . ? N2 N1 C9 C10 -0.6(4) . . . . ? Ir1 N1 C9 C10 -177.4(3) . . . . ? N1 C9 C10 C11 0.2(5) . . . . ? C9 C10 C11 N2 0.4(5) . . . . ? N1 N2 C11 C10 -0.8(4) . . . . ? C15 N2 C11 C10 -174.1(3) . . . . ? N4 N3 C12 C13 1.0(5) . . . . ? Ir1 N3 C12 C13 175.0(3) . . . . ? N3 C12 C13 C14 -0.6(6) . . . . ? N3 N4 C14 C13 0.7(5) . . . . ? C15 N4 C14 C13 174.4(4) . . . . ? C12 C13 C14 N4 -0.1(5) . . . . ? N1 N2 C15 N4 61.9(4) . . . . ? C11 N2 C15 N4 -125.3(4) . . . . ? N1 N2 C15 C31 -64.5(4) . . . . ? C11 N2 C15 C31 108.3(4) . . . . ? N3 N4 C15 N2 -63.0(4) . . . . ? C14 N4 C15 N2 123.7(4) . . . . ? N3 N4 C15 C31 63.7(4) . . . . ? C14 N4 C15 C31 -109.6(4) . . . . ? N6 N5 C24 C25 -1.1(5) . . . . ? Ir2 N5 C24 C25 -175.6(3) . . . . ? N5 C24 C25 C26 0.6(6) . . . . ? N5 N6 C26 C25 -0.9(5) . . . . ? C30 N6 C26 C25 -173.9(4) . . . . ? C24 C25 C26 N6 0.2(6) . . . . ? N8 N7 C27 C28 1.0(4) . . . . ? Ir2 N7 C27 C28 173.5(3) . . . . ? N7 C27 C28 C29 -0.3(4) . . . . ? N7 N8 C29 C28 1.2(4) . . . . ? C30 N8 C29 C28 179.7(3) . . . . ? C27 C28 C29 N8 -0.5(4) . . . . ? C29 N8 C30 N6 120.0(4) . . . . ? N7 N8 C30 N6 -61.6(4) . . . . ? C29 N8 C30 C33 -115.5(4) . . . . ? N7 N8 C30 C33 62.9(4) . . . . ? C26 N6 C30 N8 -124.1(4) . . . . ? N5 N6 C30 N8 63.4(4) . . . . ? C26 N6 C30 C33 110.3(4) . . . . ? N5 N6 C30 C33 -62.2(4) . . . . ? N2 C15 C31 C36 152.2(3) . . . . ? N4 C15 C31 C36 27.1(5) . . . . ? N2 C15 C31 C32 -33.7(5) . . . . ? N4 C15 C31 C32 -158.7(3) . . . . ? C36 C31 C32 C33 1.6(5) . . . . ? C15 C31 C32 C33 -172.7(3) . . . . ? C31 C32 C33 C34 -1.7(5) . . . . ? C31 C32 C33 C30 -176.9(3) . . . . ? N8 C30 C33 C32 -149.3(3) . . . . ? N6 C30 C33 C32 -26.1(5) . . . . ? N8 C30 C33 C34 35.4(5) . . . . ? N6 C30 C33 C34 158.7(3) . . . . ? C32 C33 C34 C35 0.7(6) . . . . ? C30 C33 C34 C35 176.0(4) . . . . ? C33 C34 C35 C36 0.3(6) . . . . ? C34 C35 C36 C31 -0.4(6) . . . . ? C32 C31 C36 C35 -0.5(6) . . . . ? C15 C31 C36 C35 173.6(4) . . . . ? C61 B1 C37 C38 84.0(4) . . . . ? C53 B1 C37 C38 -157.2(3) . . . . ? C45 B1 C37 C38 -36.7(4) . . . . ? C61 B1 C37 C42 -90.7(3) . . . . ? C53 B1 C37 C42 28.1(4) . . . . ? C45 B1 C37 C42 148.5(3) . . . . ? C42 C37 C38 C39 -1.7(5) . . . . ? B1 C37 C38 C39 -176.7(3) . . . . ? C37 C38 C39 C40 0.9(5) . . . . ? C37 C38 C39 C43 -179.0(3) . . . . ? C38 C39 C40 C41 0.4(5) . . . . ? C43 C39 C40 C41 -179.7(3) . . . . ? C39 C40 C41 C42 -0.9(5) . . . . ? C39 C40 C41 C44 175.8(3) . . . . ? C40 C41 C42 C37 0.1(5) . . . . ? C44 C41 C42 C37 -176.6(3) . . . . ? C38 C37 C42 C41 1.2(5) . . . . ? B1 C37 C42 C41 176.3(3) . . . . ? C38 C39 C43 F3 104.0(5) . . . . ? C40 C39 C43 F3 -76.0(5) . . . . ? C38 C39 C43 F1 -19.3(6) . . . . ? C40 C39 C43 F1 160.7(4) . . . . ? C38 C39 C43 F2 -135.4(4) . . . . ? C40 C39 C43 F2 44.7(5) . . . . ? C40 C41 C44 F6 25.7(6) . . . . ? C42 C41 C44 F6 -157.6(4) . . . . ? C40 C41 C44 F5 149.5(3) . . . . ? C42 C41 C44 F5 -33.8(5) . . . . ? C40 C41 C44 F4 -94.2(4) . . . . ? C42 C41 C44 F4 82.5(4) . . . . ? C61 B1 C45 C46 146.9(3) . . . . ? C53 B1 C45 C46 26.8(4) . . . . ? C37 B1 C45 C46 -94.5(4) . . . . ? C61 B1 C45 C50 -38.7(4) . . . . ? C53 B1 C45 C50 -158.8(3) . . . . ? C37 B1 C45 C50 79.9(4) . . . . ? C50 C45 C46 C47 -2.9(5) . . . . ? B1 C45 C46 C47 171.8(3) . . . . ? C45 C46 C47 C48 2.1(6) . . . . ? C45 C46 C47 C51A -168.2(5) . . . . ? C45 C46 C47 C51 177.9(4) . . . . ? F9A C51A C47 C48 -113.1(9) . . . . ? F7A C51A C47 C48 10.9(13) . . . . ? F8A C51A C47 C48 130.7(11) . . . . ? F9A C51A C47 C46 57.2(10) . . . . ? F7A C51A C47 C46 -178.8(10) . . . . ? F8A C51A C47 C46 -59.1(12) . . . . ? F9A C51A C47 C51 173(3) . . . . ? F7A C51A C47 C51 -63(2) . . . . ? F8A C51A C47 C51 56(2) . . . . ? F8 C51 C47 C48 -59.2(8) . . . . ? F7 C51 C47 C48 179.3(7) . . . . ? F9 C51 C47 C48 59.3(7) . . . . ? F8 C51 C47 C46 124.9(7) . . . . ? F7 C51 C47 C46 3.4(8) . . . . ? F9 C51 C47 C46 -116.7(6) . . . . ? F8 C51 C47 C51A 53(2) . . . . ? F7 C51 C47 C51A -68(2) . . . . ? F9 C51 C47 C51A 172(3) . . . . ? C46 C47 C48 C49 -0.1(6) . . . . ? C51A C47 C48 C49 169.9(5) . . . . ? C51 C47 C48 C49 -176.1(4) . . . . ? C47 C48 C49 C50 -1.0(6) . . . . ? C47 C48 C49 C52A -178.7(10) . . . . ? C47 C48 C49 C52 179.8(4) . . . . ? F12A C52A C49 C48 179(2) . . . . ? F11A C52A C49 C48 61(2) . . . . ? F10A C52A C49 C48 -58(2) . . . . ? F12A C52A C49 C50 1(3) . . . . ? F11A C52A C49 C50 -116(2) . . . . ? F10A C52A C49 C50 124(3) . . . . ? F12A C52A C49 C52 -20(12) . . . . ? F11A C52A C49 C52 -137(14) . . . . ? F10A C52A C49 C52 103(13) . . . . ? F10 C52 C49 C48 122.4(7) . . . . ? F11 C52 C49 C48 -117.5(7) . . . . ? F12 C52 C49 C48 1.6(8) . . . . ? F10 C52 C49 C50 -56.9(7) . . . . ? F11 C52 C49 C50 63.2(7) . . . . ? F12 C52 C49 C50 -177.7(6) . . . . ? F10 C52 C49 C52A 103(13) . . . . ? F11 C52 C49 C52A -137(14) . . . . ? F12 C52 C49 C52A -18(13) . . . . ? C48 C49 C50 C45 0.0(6) . . . . ? C52A C49 C50 C45 177.7(10) . . . . ? C52 C49 C50 C45 179.3(4) . . . . ? C46 C45 C50 C49 1.8(5) . . . . ? B1 C45 C50 C49 -172.9(3) . . . . ? C61 B1 C53 C58 -19.8(4) . . . . ? C45 B1 C53 C58 102.3(4) . . . . ? C37 B1 C53 C58 -138.7(3) . . . . ? C61 B1 C53 C54 159.7(3) . . . . ? C45 B1 C53 C54 -78.2(4) . . . . ? C37 B1 C53 C54 40.9(4) . . . . ? C58 C53 C54 C55 -0.7(5) . . . . ? B1 C53 C54 C55 179.8(3) . . . . ? C53 C54 C55 C56 0.4(5) . . . . ? C53 C54 C55 C59 176.7(3) . . . . ? C54 C55 C56 C57 0.3(5) . . . . ? C59 C55 C56 C57 -176.1(3) . . . . ? C55 C56 C57 C58 -0.5(5) . . . . ? C55 C56 C57 C60 177.8(3) . . . . ? C56 C57 C58 C53 0.2(5) . . . . ? C60 C57 C58 C53 -178.2(3) . . . . ? C54 C53 C58 C57 0.4(5) . . . . ? B1 C53 C58 C57 179.9(3) . . . . ? C56 C55 C59 F15 -39.3(5) . . . . ? C54 C55 C59 F15 144.3(4) . . . . ? C56 C55 C59 F14 80.8(5) . . . . ? C54 C55 C59 F14 -95.6(5) . . . . ? C56 C55 C59 F13 -161.7(4) . . . . ? C54 C55 C59 F13 22.0(5) . . . . ? C56 C57 C60 F18 -108.0(4) . . . . ? C58 C57 C60 F18 70.4(5) . . . . ? C56 C57 C60 F17 130.9(4) . . . . ? C58 C57 C60 F17 -50.6(5) . . . . ? C56 C57 C60 F16 11.9(5) . . . . ? C58 C57 C60 F16 -169.7(3) . . . . ? C53 B1 C61 C62 -86.5(4) . . . . ? C45 B1 C61 C62 152.4(3) . . . . ? C37 B1 C61 C62 34.2(4) . . . . ? C53 B1 C61 C66 88.0(4) . . . . ? C45 B1 C61 C66 -33.1(4) . . . . ? C37 B1 C61 C66 -151.2(3) . . . . ? C66 C61 C62 C63 -0.2(5) . . . . ? B1 C61 C62 C63 174.7(3) . . . . ? C61 C62 C63 C64 0.8(6) . . . . ? C61 C62 C63 C67 -178.4(3) . . . . ? C62 C63 C64 C65 -1.5(5) . . . . ? C67 C63 C64 C65 177.6(3) . . . . ? C63 C64 C65 C66 1.7(5) . . . . ? C63 C64 C65 C68 -177.8(3) . . . . ? C64 C65 C66 C61 -1.2(5) . . . . ? C68 C65 C66 C61 178.3(3) . . . . ? C62 C61 C66 C65 0.4(5) . . . . ? B1 C61 C66 C65 -174.4(3) . . . . ? C64 C63 C67 F21 103.5(10) . . . . ? C62 C63 C67 F21 -77.3(10) . . . . ? C64 C63 C67 F21A -78.2(9) . . . . ? C62 C63 C67 F21A 101.0(9) . . . . ? C64 C63 C67 F19 -138.2(10) . . . . ? C62 C63 C67 F19 40.9(11) . . . . ? C64 C63 C67 F19A 43.6(10) . . . . ? C62 C63 C67 F19A -137.3(9) . . . . ? C64 C63 C67 F20 -16.4(13) . . . . ? C62 C63 C67 F20 162.7(13) . . . . ? C64 C63 C67 F20A 160.9(11) . . . . ? C62 C63 C67 F20A -19.9(11) . . . . ? C64 C65 C68 F24 -160.4(4) . . . . ? C66 C65 C68 F24 20.1(6) . . . . ? C64 C65 C68 F22 78.1(5) . . . . ? C66 C65 C68 F22 -101.4(4) . . . . ? C64 C65 C68 F23 -40.0(5) . . . . ? C66 C65 C68 F23 140.5(4) . . . . ? C77 B2 C69 C74 -35.0(4) . . . . ? C93 B2 C69 C74 -154.1(3) . . . . ? C85 B2 C69 C74 86.2(4) . . . . ? C77 B2 C69 C70 153.8(3) . . . . ? C93 B2 C69 C70 34.7(4) . . . . ? C85 B2 C69 C70 -85.0(4) . . . . ? C74 C69 C70 C71 -1.2(5) . . . . ? B2 C69 C70 C71 170.7(3) . . . . ? C69 C70 C71 C72 2.5(6) . . . . ? C69 C70 C71 C75A 178.9(6) . . . . ? C69 C70 C71 C75 -175.5(3) . . . . ? F27A C75A C71 C72 10.8(19) . . . . ? F25A C75A C71 C72 135.7(14) . . . . ? F26A C75A C71 C72 -111.3(16) . . . . ? F27A C75A C71 C70 -165.6(18) . . . . ? F25A C75A C71 C70 -40.7(16) . . . . ? F26A C75A C71 C70 72.3(18) . . . . ? F27A C75A C71 C75 85(6) . . . . ? F25A C75A C71 C75 -150(6) . . . . ? F26A C75A C71 C75 -37(6) . . . . ? F26 C75 C71 C72 79.0(8) . . . . ? F25 C75 C71 C72 -39.8(8) . . . . ? F27 C75 C71 C72 -158.7(7) . . . . ? F26 C75 C71 C70 -102.9(8) . . . . ? F25 C75 C71 C70 138.2(6) . . . . ? F27 C75 C71 C70 19.3(8) . . . . ? F26 C75 C71 C75A -29(6) . . . . ? F25 C75 C71 C75A -148(6) . . . . ? F27 C75 C71 C75A 93(6) . . . . ? C70 C71 C72 C73 -1.7(6) . . . . ? C75A C71 C72 C73 -178.0(6) . . . . ? C75 C71 C72 C73 176.3(4) . . . . ? C71 C72 C73 C74 -0.4(6) . . . . ? C71 C72 C73 C76 178.2(4) . . . . ? C72 C73 C74 C69 1.7(6) . . . . ? C76 C73 C74 C69 -176.9(4) . . . . ? C70 C69 C74 C73 -0.9(5) . . . . ? B2 C69 C74 C73 -172.5(3) . . . . ? C72 C73 C76 F29 -68.6(6) . . . . ? C74 C73 C76 F29 110.0(5) . . . . ? C72 C73 C76 F30 168.4(4) . . . . ? C74 C73 C76 F30 -13.0(6) . . . . ? C72 C73 C76 F28 49.9(6) . . . . ? C74 C73 C76 F28 -131.4(4) . . . . ? C93 B2 C77 C78 91.8(4) . . . . ? C85 B2 C77 C78 -144.5(3) . . . . ? C69 B2 C77 C78 -29.2(5) . . . . ? C93 B2 C77 C82 -84.3(4) . . . . ? C85 B2 C77 C82 39.3(4) . . . . ? C69 B2 C77 C82 154.6(3) . . . . ? C82 C77 C78 C79 -1.0(5) . . . . ? B2 C77 C78 C79 -177.4(3) . . . . ? C77 C78 C79 C80 0.1(6) . . . . ? C77 C78 C79 C83 180.0(4) . . . . ? C78 C79 C80 C81 0.6(6) . . . . ? C83 C79 C80 C81 -179.2(4) . . . . ? C79 C80 C81 C82 -0.5(6) . . . . ? C79 C80 C81 C84 179.8(4) . . . . ? C80 C81 C82 C77 -0.5(6) . . . . ? C84 C81 C82 C77 179.3(3) . . . . ? C78 C77 C82 C81 1.2(5) . . . . ? B2 C77 C82 C81 177.7(3) . . . . ? C80 C79 C83 F33 -9.2(7) . . . . ? C78 C79 C83 F33 171.0(5) . . . . ? C80 C79 C83 F32 -135.4(5) . . . . ? C78 C79 C83 F32 44.7(6) . . . . ? C80 C79 C83 F31 107.3(5) . . . . ? C78 C79 C83 F31 -72.5(5) . . . . ? C82 C81 C84 F34 -130.3(4) . . . . ? C80 C81 C84 F34 49.5(5) . . . . ? C82 C81 C84 F36 -8.3(6) . . . . ? C80 C81 C84 F36 171.4(4) . . . . ? C82 C81 C84 F35 110.8(4) . . . . ? C80 C81 C84 F35 -69.5(5) . . . . ? C77 B2 C85 C86 -162.2(3) . . . . ? C93 B2 C85 C86 -42.0(4) . . . . ? C69 B2 C85 C86 75.9(4) . . . . ? C77 B2 C85 C90 25.1(4) . . . . ? C93 B2 C85 C90 145.3(3) . . . . ? C69 B2 C85 C90 -96.8(4) . . . . ? C90 C85 C86 C87 -1.1(5) . . . . ? B2 C85 C86 C87 -174.4(3) . . . . ? C85 C86 C87 C88 0.2(5) . . . . ? C85 C86 C87 C91 -178.8(3) . . . . ? C86 C87 C88 C89 0.4(5) . . . . ? C91 C87 C88 C89 179.3(3) . . . . ? C87 C88 C89 C90 0.1(5) . . . . ? C87 C88 C89 C92 -179.2(3) . . . . ? C88 C89 C90 C85 -1.1(5) . . . . ? C92 C89 C90 C85 178.2(3) . . . . ? C86 C85 C90 C89 1.5(5) . . . . ? B2 C85 C90 C89 174.7(3) . . . . ? C88 C87 C91 F39 23.4(5) . . . . ? C86 C87 C91 F39 -157.7(3) . . . . ? C88 C87 C91 F38 -99.9(4) . . . . ? C86 C87 C91 F38 79.1(5) . . . . ? C88 C87 C91 F37 143.1(4) . . . . ? C86 C87 C91 F37 -37.9(5) . . . . ? C88 C89 C92 F42 135.9(6) . . . . ? C90 C89 C92 F42 -43.4(6) . . . . ? C88 C89 C92 F42A -38(3) . . . . ? C90 C89 C92 F42A 142(3) . . . . ? C88 C89 C92 F40A -159.2(19) . . . . ? C90 C89 C92 F40A 21.5(19) . . . . ? C88 C89 C92 F41A 85.8(17) . . . . ? C90 C89 C92 F41A -93.5(17) . . . . ? C88 C89 C92 F41 -103.3(5) . . . . ? C90 C89 C92 F41 77.4(5) . . . . ? C88 C89 C92 F40 16.1(5) . . . . ? C90 C89 C92 F40 -163.1(4) . . . . ? C77 B2 C93 C94 -76.6(4) . . . . ? C85 B2 C93 C94 159.9(3) . . . . ? C69 B2 C93 C94 46.7(4) . . . . ? C77 B2 C93 C98 102.8(3) . . . . ? C85 B2 C93 C98 -20.7(4) . . . . ? C69 B2 C93 C98 -133.9(3) . . . . ? C98 C93 C94 C95 0.2(5) . . . . ? B2 C93 C94 C95 179.6(3) . . . . ? C93 C94 C95 C96 1.4(5) . . . . ? C93 C94 C95 C99 177.2(3) . . . . ? C94 C95 C96 C97 -0.9(5) . . . . ? C99 C95 C96 C97 -176.8(3) . . . . ? C95 C96 C97 C98 -1.2(5) . . . . ? C95 C96 C97 C100 176.4(3) . . . . ? C96 C97 C98 C93 2.9(5) . . . . ? C100 C97 C98 C93 -174.7(3) . . . . ? C94 C93 C98 C97 -2.3(5) . . . . ? B2 C93 C98 C97 178.3(3) . . . . ? C94 C95 C99 F43 141.2(4) . . . . ? C96 C95 C99 F43 -42.9(5) . . . . ? C94 C95 C99 F44 -98.0(4) . . . . ? C96 C95 C99 F44 77.9(4) . . . . ? C94 C95 C99 F45 20.6(5) . . . . ? C96 C95 C99 F45 -163.5(3) . . . . ? C96 C97 C100 F47 80.8(5) . . . . ? C98 C97 C100 F47 -101.5(5) . . . . ? C96 C97 C100 F46 -41.0(5) . . . . ? C98 C97 C100 F46 136.6(4) . . . . ? C96 C97 C100 F48 -157.6(4) . . . . ? C98 C97 C100 F48 20.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.405 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.110