Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alex Ionkin' _publ_contact_author_address ; DuPont Central Research & Development Experimental Station Wilmington DE 19880-0328 UNITED STATES OF AMERICA ; _publ_contact_author_email ALEX.S.IONKIN@USA.DUPONT.COM _publ_section_title ; Synthesis, Structural Characterization and the First Electroluminescent Properties of Tris- and Bis-cycloiridiated Complexes of Sterical Hindered Electron-Poor 2-(3,5-bis(trifluoromethyl)phenyl)-4-trifluoromethylpyridine. ; loop_ _publ_author_name 'Alex Ionkin' 'William J. Marshall' 'D. C. Roe' 'Ying Wang' # Attachment 'Ir-carbene-final.cif' data_03297 _database_code_depnum_ccdc_archive 'CCDC 257681' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H12 Ag3 F27 N2 O6' _chemical_formula_weight 1381.07 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' Ag Ag -0.8971 1.1015 '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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2935(15) _cell_length_b 12.797(2) _cell_length_c 19.913(3) _cell_angle_alpha 82.984(3) _cell_angle_beta 83.660(3) _cell_angle_gamma 83.647(3) _cell_volume 2074.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ireg.plate _exptl_crystal_colour colorlr _exptl_crystal_size_max .42 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .05 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13789 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9463 _reflns_number_gt 8320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+2.2107P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9463 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.007 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 Ag1 Ag 0.52647(2) 0.108548(16) 0.019942(10) 0.02969(6) Uani 1 1 d . . . Ag2 Ag 0.80247(2) -0.061181(15) 0.022808(10) 0.02971(6) Uani 1 1 d . . . Ag3 Ag 0.52466(2) 0.180525(15) 0.205703(10) 0.02901(6) Uani 1 1 d . . . F1 F 1.0965(2) 0.24551(18) 0.07213(11) 0.0592(6) Uani 1 1 d . . . F2 F 1.0112(3) 0.1752(2) 0.17090(11) 0.0753(7) Uani 1 1 d . . . F3 F 0.8816(3) 0.31240(18) 0.12628(15) 0.0741(7) Uani 1 1 d . . . F4 F 0.8757(8) 0.1163(9) -0.1922(2) 0.138(3) Uani 0.747(6) 1 d P . . F5 F 0.6390(6) 0.1462(5) -0.2183(3) 0.1045(19) Uani 0.747(6) 1 d P . . F6 F 0.7744(12) 0.0067(3) -0.2388(2) 0.108(2) Uani 0.747(6) 1 d P . . F4' F 0.663(3) 0.072(3) -0.2421(7) 0.138(3) Uani 0.253(6) 1 d P . . F5' F 0.878(2) 0.0148(16) -0.2150(9) 0.1045(19) Uani 0.253(6) 1 d P . . F6' F 0.793(3) 0.1639(11) -0.1957(7) 0.108(2) Uani 0.253(6) 1 d P . . F7 F 0.6532(3) -0.44855(14) 0.11392(10) 0.0573(6) Uani 1 1 d . . . F8 F 0.7530(3) -0.36576(15) 0.18335(10) 0.0564(6) Uani 1 1 d . . . F9 F 0.4943(3) -0.3559(2) 0.17984(13) 0.0762(8) Uani 1 1 d . . . F10 F 0.2197(3) 0.6470(2) 0.01697(14) 0.0840(9) Uani 1 1 d . . . F11 F -0.0066(3) 0.58709(19) 0.05445(12) 0.0648(6) Uani 1 1 d . . . F12 F 0.1015(4) 0.68247(17) 0.11350(14) 0.0796(8) Uani 1 1 d . . . F13 F 0.1497(6) 0.5777(3) 0.4279(2) 0.0746(12) Uani 0.762(4) 1 d P . . F14 F 0.2036(8) 0.4582(3) 0.50630(15) 0.0862(13) Uani 0.762(4) 1 d P . . F15 F 0.3915(4) 0.5169(4) 0.4397(3) 0.0933(16) Uani 0.762(4) 1 d P . . F13' F 0.306(2) 0.4704(10) 0.4877(8) 0.0746(12) Uani 0.238(4) 1 d P . . F14' F 0.308(2) 0.5821(9) 0.4044(5) 0.0862(13) Uani 0.238(4) 1 d P . . F15' F 0.0838(17) 0.5445(13) 0.4513(10) 0.0933(16) Uani 0.238(4) 1 d P . . F16 F 0.0253(7) 0.1258(3) 0.4537(3) 0.0852(12) Uani 0.594(3) 1 d P . . F17 F 0.2715(7) 0.0785(5) 0.4434(5) 0.110(3) Uani 0.594(3) 1 d P . . F18 F 0.1274(12) 0.0651(5) 0.3648(2) 0.108(3) Uani 0.594(3) 1 d P . . F16' F 0.2989(10) 0.0517(5) 0.3737(5) 0.0852(12) Uani 0.406(3) 1 d P . . F17' F 0.0553(11) 0.0862(8) 0.3899(7) 0.110(3) Uani 0.406(3) 1 d P . . F18' F 0.2043(19) 0.0932(8) 0.4665(4) 0.108(3) Uani 0.406(3) 1 d P . . F19 F 0.9521(6) -0.3171(2) 0.2979(2) 0.0727(13) Uani 0.714(3) 1 d P . . F20 F 1.0844(4) -0.2220(3) 0.3433(3) 0.0757(11) Uani 0.714(3) 1 d P . . F21 F 0.8700(6) -0.2747(4) 0.3962(2) 0.101(2) Uani 0.714(3) 1 d P . . F19' F 0.9584(16) -0.2346(7) 0.4038(6) 0.0727(13) Uani 0.286(3) 1 d P . . F20' F 0.8282(11) -0.3190(7) 0.3476(7) 0.0757(11) Uani 0.286(3) 1 d P . . F21' F 1.0483(18) -0.2720(11) 0.3082(6) 0.101(2) Uani 0.286(3) 1 d P . . F22 F 0.4877(3) 0.12166(17) 0.55105(10) 0.0654(7) Uani 1 1 d . . . F23 F 0.7001(3) 0.1862(3) 0.56809(11) 0.0811(8) Uani 1 1 d . . . F24 F 0.4852(4) 0.28739(17) 0.55161(11) 0.0770(8) Uani 1 1 d . . . F25 F 0.6846(14) 0.5066(4) 0.3504(3) 0.112(3) Uani 0.548(4) 1 d P . . F26 F 0.6388(8) 0.4459(4) 0.2626(3) 0.0835(14) Uani 0.548(4) 1 d P . . F27 F 0.8739(5) 0.4331(5) 0.2872(5) 0.090(2) Uani 0.548(4) 1 d P . . F25' F 0.8404(16) 0.4185(6) 0.2587(4) 0.112(3) Uani 0.452(4) 1 d P . . F26' F 0.8509(11) 0.4711(5) 0.3524(4) 0.0835(14) Uani 0.452(4) 1 d P . . F27' F 0.6289(6) 0.4906(6) 0.3095(6) 0.090(2) Uani 0.452(4) 1 d P . . O1 O 0.9417(2) 0.08073(15) 0.04914(10) 0.0339(4) Uani 1 1 d . . . O2 O 0.7116(2) 0.16635(15) 0.09322(9) 0.0291(4) Uani 1 1 d . . . O3 O 0.7161(2) 0.06349(16) -0.07446(10) 0.0358(4) Uani 1 1 d . . . O4 O 0.5906(2) -0.04916(17) -0.12425(10) 0.0359(4) Uani 1 1 d . . . O5 O 0.5593(3) -0.26533(16) 0.03985(11) 0.0420(5) Uani 1 1 d . . . O6 O 0.7192(3) -0.18945(15) 0.09990(10) 0.0344(4) Uani 1 1 d . . . N1 N 0.3848(3) 0.32680(16) 0.16801(11) 0.0265(4) Uani 1 1 d . . . N2 N 0.6719(3) 0.04489(17) 0.25373(11) 0.0268(4) Uani 1 1 d . . . C1 C 0.8613(3) 0.15016(19) 0.08078(12) 0.0240(5) Uani 1 1 d . . . C2 C 0.9631(3) 0.2228(2) 0.11186(15) 0.0356(6) Uani 1 1 d . . . C3 C 0.6777(3) 0.0237(2) -0.12362(13) 0.0295(5) Uani 1 1 d . . . C4 C 0.7464(4) 0.0730(3) -0.19382(16) 0.0425(7) Uani 1 1 d . . . C5 C 0.6401(3) -0.2605(2) 0.08779(13) 0.0288(5) Uani 1 1 d . . . C6 C 0.6358(4) -0.3584(2) 0.14199(15) 0.0368(6) Uani 1 1 d . . . C7 C 0.4105(3) 0.3545(2) 0.10050(13) 0.0303(5) Uani 1 1 d . . . H7A H 0.4841 0.3113 0.0748 0.036 Uiso 1 1 calc R . . C8 C 0.3322(3) 0.4443(2) 0.06765(14) 0.0321(6) Uani 1 1 d . . . H8A H 0.3518 0.4607 0.0209 0.039 Uiso 1 1 calc R . . C9 C 0.2245(3) 0.5088(2) 0.10587(14) 0.0309(6) Uani 1 1 d . . . C10 C 0.1972(3) 0.4819(2) 0.17561(14) 0.0314(6) Uani 1 1 d . . . H10A H 0.1256 0.5250 0.2021 0.038 Uiso 1 1 calc R . . C11 C 0.2786(3) 0.3896(2) 0.20531(13) 0.0265(5) Uani 1 1 d . . . C12 C 0.2530(3) 0.3604(2) 0.27996(13) 0.0273(5) Uani 1 1 d . . . C13 C 0.2562(3) 0.4368(2) 0.32405(14) 0.0312(6) Uani 1 1 d . . . H13A H 0.2751 0.5056 0.3066 0.037 Uiso 1 1 calc R . . C14 C 0.2312(3) 0.4103(2) 0.39389(14) 0.0329(6) Uani 1 1 d . . . C15 C 0.2023(4) 0.3081(2) 0.42081(15) 0.0368(6) Uani 1 1 d . . . H15A H 0.1855 0.2908 0.4676 0.044 Uiso 1 1 calc R . . C16 C 0.1987(4) 0.2328(2) 0.37728(14) 0.0337(6) Uani 1 1 d . . . C17 C 0.2249(3) 0.2573(2) 0.30715(14) 0.0299(5) Uani 1 1 d . . . H17A H 0.2236 0.2053 0.2785 0.036 Uiso 1 1 calc R . . C18 C 0.1354(4) 0.6072(3) 0.07249(18) 0.0451(8) Uani 1 1 d . . . C19 C 0.2397(4) 0.4932(3) 0.44026(17) 0.0462(8) Uani 1 1 d . . . C20 C 0.1691(4) 0.1217(3) 0.40678(17) 0.0465(8) Uani 1 1 d . . . C21 C 0.7019(3) -0.0403(2) 0.21934(14) 0.0303(5) Uani 1 1 d . . . H21A H 0.6656 -0.0357 0.1764 0.036 Uiso 1 1 calc R . . C22 C 0.7843(3) -0.1348(2) 0.24448(14) 0.0320(6) Uani 1 1 d . . . H22A H 0.8035 -0.1921 0.2191 0.038 Uiso 1 1 calc R . . C23 C 0.8366(3) -0.1412(2) 0.30837(14) 0.0283(5) Uani 1 1 d . . . C24 C 0.8084(3) -0.05397(19) 0.34462(13) 0.0256(5) Uani 1 1 d . . . H24A H 0.8444 -0.0571 0.3875 0.031 Uiso 1 1 calc R . . C25 C 0.7257(3) 0.03805(19) 0.31604(13) 0.0247(5) Uani 1 1 d . . . C26 C 0.6986(3) 0.1339(2) 0.35270(13) 0.0251(5) Uani 1 1 d . . . C27 C 0.6481(3) 0.12482(19) 0.42217(13) 0.0258(5) Uani 1 1 d . . . H27A H 0.6285 0.0591 0.4452 0.031 Uiso 1 1 calc R . . C28 C 0.6271(3) 0.2137(2) 0.45690(13) 0.0285(5) Uani 1 1 d . . . C29 C 0.6571(3) 0.3125(2) 0.42318(14) 0.0320(6) Uani 1 1 d . . . H29A H 0.6435 0.3720 0.4465 0.038 Uiso 1 1 calc R . . C30 C 0.7076(3) 0.3207(2) 0.35423(14) 0.0316(6) Uani 1 1 d . . . C31 C 0.7287(3) 0.2325(2) 0.31894(13) 0.0286(5) Uani 1 1 d . . . H31A H 0.7630 0.2393 0.2727 0.034 Uiso 1 1 calc R . . C32 C 0.9293(4) -0.2401(2) 0.33839(16) 0.0380(6) Uani 1 1 d . . . C33 C 0.5749(4) 0.2025(2) 0.53208(15) 0.0370(6) Uani 1 1 d . . . C34 C 0.7398(5) 0.4271(2) 0.31649(17) 0.0448(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 Ag1 0.03277(11) 0.03195(11) 0.02513(10) -0.00087(8) -0.00619(8) -0.00587(8) Ag2 0.03024(11) 0.02715(10) 0.03090(11) -0.00191(7) 0.00228(8) -0.00577(7) Ag3 0.03252(11) 0.02741(10) 0.02501(10) -0.00113(7) -0.00481(8) 0.00632(7) F1 0.0451(11) 0.0714(14) 0.0688(14) -0.0261(11) 0.0097(10) -0.0348(10) F2 0.0894(18) 0.0992(19) 0.0481(13) -0.0008(12) -0.0378(12) -0.0346(15) F3 0.0615(14) 0.0525(13) 0.120(2) -0.0560(14) -0.0137(14) -0.0004(10) F4 0.106(4) 0.277(8) 0.050(2) 0.009(4) 0.009(2) -0.144(5) F5 0.094(3) 0.110(4) 0.074(3) 0.063(3) 0.024(2) 0.034(3) F6 0.209(7) 0.067(2) 0.0331(19) -0.0100(15) 0.043(3) -0.001(3) F4' 0.106(4) 0.277(8) 0.050(2) 0.009(4) 0.009(2) -0.144(5) F5' 0.094(3) 0.110(4) 0.074(3) 0.063(3) 0.024(2) 0.034(3) F6' 0.209(7) 0.067(2) 0.0331(19) -0.0100(15) 0.043(3) -0.001(3) F7 0.0927(17) 0.0276(9) 0.0556(12) 0.0020(8) -0.0249(11) -0.0133(10) F8 0.0864(15) 0.0404(10) 0.0478(11) 0.0154(8) -0.0371(11) -0.0220(10) F9 0.0674(15) 0.0766(16) 0.0689(15) 0.0262(13) 0.0240(12) -0.0062(12) F10 0.0638(15) 0.0736(16) 0.0892(18) 0.0565(14) 0.0123(13) 0.0125(12) F11 0.0474(12) 0.0682(14) 0.0745(15) 0.0155(11) -0.0260(11) 0.0065(10) F12 0.112(2) 0.0353(11) 0.0889(18) -0.0001(11) -0.0353(15) 0.0227(12) F13 0.110(3) 0.0431(18) 0.074(2) -0.0249(15) -0.050(2) 0.0370(19) F14 0.175(4) 0.0550(19) 0.0302(15) -0.0122(12) -0.002(2) -0.019(2) F15 0.065(2) 0.094(3) 0.140(4) -0.081(3) -0.008(2) -0.017(2) F13' 0.110(3) 0.0431(18) 0.074(2) -0.0249(15) -0.050(2) 0.0370(19) F14' 0.175(4) 0.0550(19) 0.0302(15) -0.0122(12) -0.002(2) -0.019(2) F15' 0.065(2) 0.094(3) 0.140(4) -0.081(3) -0.008(2) -0.017(2) F16 0.084(3) 0.056(2) 0.101(3) 0.018(2) 0.030(2) -0.0156(19) F17 0.062(3) 0.072(3) 0.193(8) 0.083(4) -0.083(4) -0.036(2) F18 0.237(10) 0.065(3) 0.0369(19) 0.0065(17) -0.019(3) -0.083(4) F16' 0.084(3) 0.056(2) 0.101(3) 0.018(2) 0.030(2) -0.0156(19) F17' 0.062(3) 0.072(3) 0.193(8) 0.083(4) -0.083(4) -0.036(2) F18' 0.237(10) 0.065(3) 0.0369(19) 0.0065(17) -0.019(3) -0.083(4) F19 0.110(3) 0.0320(15) 0.082(3) -0.0207(15) -0.051(2) 0.0274(16) F20 0.0542(19) 0.0473(17) 0.127(3) 0.0151(19) -0.046(2) -0.0018(14) F21 0.115(4) 0.082(3) 0.063(2) 0.052(2) 0.050(2) 0.060(3) F19' 0.110(3) 0.0320(15) 0.082(3) -0.0207(15) -0.051(2) 0.0274(16) F20' 0.0542(19) 0.0473(17) 0.127(3) 0.0151(19) -0.046(2) -0.0018(14) F21' 0.115(4) 0.082(3) 0.063(2) 0.052(2) 0.050(2) 0.060(3) F22 0.1024(18) 0.0567(13) 0.0396(11) -0.0119(9) 0.0227(11) -0.0423(12) F23 0.0753(16) 0.138(2) 0.0339(11) -0.0019(13) -0.0181(11) -0.0240(16) F24 0.127(2) 0.0450(12) 0.0471(12) -0.0093(10) 0.0299(13) 0.0092(13) F25 0.226(9) 0.0303(18) 0.067(3) -0.0035(19) 0.050(4) -0.026(3) F26 0.108(4) 0.054(2) 0.094(3) 0.037(2) -0.046(3) -0.042(2) F27 0.0231(14) 0.055(3) 0.168(6) 0.061(3) 0.017(2) 0.0017(15) F25' 0.226(9) 0.0303(18) 0.067(3) -0.0035(19) 0.050(4) -0.026(3) F26' 0.108(4) 0.054(2) 0.094(3) 0.037(2) -0.046(3) -0.042(2) F27' 0.0231(14) 0.055(3) 0.168(6) 0.061(3) 0.017(2) 0.0017(15) O1 0.0272(9) 0.0351(10) 0.0408(11) -0.0143(8) 0.0038(8) -0.0051(8) O2 0.0233(9) 0.0372(10) 0.0271(9) -0.0066(7) -0.0007(7) -0.0026(7) O3 0.0390(11) 0.0412(11) 0.0284(10) -0.0048(8) -0.0014(8) -0.0101(9) O4 0.0372(11) 0.0437(11) 0.0277(10) -0.0021(8) -0.0028(8) -0.0110(9) O5 0.0567(14) 0.0338(11) 0.0383(12) 0.0004(9) -0.0209(10) -0.0060(9) O6 0.0467(12) 0.0292(10) 0.0284(10) 0.0009(8) -0.0066(8) -0.0106(8) N1 0.0286(11) 0.0246(10) 0.0267(11) -0.0041(8) -0.0055(8) -0.0010(8) N2 0.0295(11) 0.0270(11) 0.0231(10) -0.0010(8) -0.0049(8) 0.0006(8) C1 0.0254(12) 0.0247(12) 0.0218(11) -0.0012(9) -0.0022(9) -0.0041(9) C2 0.0317(14) 0.0405(16) 0.0374(15) -0.0118(12) -0.0044(12) -0.0074(12) C3 0.0250(12) 0.0340(14) 0.0272(13) -0.0002(10) -0.0010(10) 0.0014(10) C4 0.0445(17) 0.0499(19) 0.0321(15) 0.0017(13) 0.0012(13) -0.0119(14) C5 0.0347(14) 0.0258(12) 0.0248(12) -0.0007(10) -0.0024(10) -0.0016(10) C6 0.0462(17) 0.0320(14) 0.0334(15) 0.0037(11) -0.0084(12) -0.0120(12) C7 0.0363(14) 0.0300(13) 0.0249(13) -0.0039(10) -0.0041(10) -0.0023(11) C8 0.0359(14) 0.0322(14) 0.0281(13) 0.0030(10) -0.0060(11) -0.0073(11) C9 0.0278(13) 0.0272(13) 0.0364(14) 0.0073(11) -0.0079(11) -0.0041(10) C10 0.0282(13) 0.0278(13) 0.0361(15) -0.0008(11) -0.0012(11) 0.0018(10) C11 0.0240(12) 0.0265(12) 0.0280(13) -0.0006(10) -0.0043(10) 0.0006(9) C12 0.0238(12) 0.0278(12) 0.0291(13) -0.0019(10) -0.0024(10) 0.0011(9) C13 0.0291(13) 0.0289(13) 0.0351(14) -0.0039(11) -0.0040(11) 0.0004(10) C14 0.0317(14) 0.0358(14) 0.0319(14) -0.0087(11) -0.0061(11) 0.0013(11) C15 0.0379(15) 0.0449(16) 0.0278(14) -0.0016(12) -0.0063(11) -0.0052(12) C16 0.0357(15) 0.0339(14) 0.0318(14) 0.0025(11) -0.0083(11) -0.0062(11) C17 0.0295(13) 0.0291(13) 0.0318(14) -0.0033(10) -0.0081(10) -0.0017(10) C18 0.0425(17) 0.0385(17) 0.0486(19) 0.0141(14) -0.0070(14) 0.0026(13) C19 0.056(2) 0.0441(18) 0.0397(17) -0.0121(14) -0.0081(15) 0.0024(15) C20 0.059(2) 0.0450(18) 0.0376(17) 0.0096(14) -0.0154(15) -0.0189(15) C21 0.0358(14) 0.0301(13) 0.0255(13) -0.0048(10) -0.0089(10) 0.0023(11) C22 0.0370(15) 0.0260(13) 0.0344(14) -0.0083(11) -0.0076(11) 0.0004(11) C23 0.0285(13) 0.0234(12) 0.0321(13) 0.0008(10) -0.0043(10) -0.0025(10) C24 0.0291(12) 0.0240(12) 0.0236(12) 0.0009(9) -0.0059(10) -0.0027(9) C25 0.0253(12) 0.0241(12) 0.0246(12) 0.0003(9) -0.0031(9) -0.0041(9) C26 0.0249(12) 0.0255(12) 0.0251(12) -0.0011(9) -0.0054(9) -0.0025(9) C27 0.0286(12) 0.0222(11) 0.0268(12) 0.0004(9) -0.0045(10) -0.0049(9) C28 0.0316(13) 0.0283(13) 0.0263(13) -0.0027(10) -0.0049(10) -0.0046(10) C29 0.0379(15) 0.0248(13) 0.0349(14) -0.0070(10) -0.0040(11) -0.0060(10) C30 0.0371(14) 0.0243(13) 0.0327(14) 0.0017(10) -0.0039(11) -0.0049(10) C31 0.0319(13) 0.0273(13) 0.0259(13) 0.0008(10) -0.0047(10) -0.0024(10) C32 0.0466(17) 0.0271(14) 0.0396(16) -0.0022(11) -0.0099(13) 0.0028(12) C33 0.0516(18) 0.0320(14) 0.0287(14) -0.0055(11) -0.0026(12) -0.0084(12) C34 0.065(2) 0.0266(14) 0.0404(17) 0.0001(12) 0.0038(15) -0.0082(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 Ag1 O4 2.2731(19) 2_655 ? Ag1 O5 2.289(2) 2_655 ? Ag1 O3 2.398(2) . ? Ag1 O2 2.4581(18) . ? Ag1 Ag2 2.9764(5) . ? Ag1 Ag1 3.0705(6) 2_655 ? Ag1 Ag2 3.0885(5) 2_655 ? Ag2 O6 2.2201(19) . ? Ag2 O1 2.3949(19) . ? Ag2 O1 2.4325(19) 2_755 ? Ag2 O3 2.472(2) . ? Ag2 Ag1 3.0886(6) 2_655 ? Ag3 N1 2.187(2) . ? Ag3 N2 2.191(2) . ? Ag3 O2 2.5928(18) . ? F1 C2 1.325(3) . ? F2 C2 1.337(4) . ? F3 C2 1.311(4) . ? F4 F6' 0.870(18) . ? F4 C4 1.265(5) . ? F4 F5' 1.42(2) . ? F5 F4' 1.10(3) . ? F5 C4 1.308(5) . ? F5 F6' 1.45(3) . ? F6 F5' 1.04(2) . ? F6 F4' 1.18(3) . ? F6 C4 1.293(5) . ? F4' C4 1.247(14) . ? F5' C4 1.309(14) . ? F6' C4 1.259(18) . ? F7 C6 1.329(3) . ? F8 C6 1.330(3) . ? F9 C6 1.322(4) . ? F10 C18 1.319(4) . ? F11 C18 1.329(4) . ? F12 C18 1.325(4) . ? F13 F15' 0.802(15) . ? F13 C19 1.259(4) . ? F13 F14' 1.349(18) . ? F14 F13' 0.909(18) . ? F14 C19 1.349(5) . ? F14 F15' 1.764(19) . ? F15 F14' 1.227(15) . ? F15 F13' 1.256(19) . ? F15 C19 1.326(5) . ? F13' C19 1.136(11) . ? F14' C19 1.406(12) . ? F15' C19 1.391(15) . ? F16 F17' 1.411(14) . ? F16 C20 1.432(6) . ? F16 F18' 1.538(14) . ? F17 F18' 0.706(13) . ? F17 C20 1.222(5) . ? F17 F16' 1.458(10) . ? F18 F17' 0.782(14) . ? F18 C20 1.268(6) . ? F18 F16' 1.441(10) . ? F16' C20 1.473(8) . ? F17' C20 1.188(8) . ? F18' C20 1.257(9) . ? F19 F21' 1.09(2) . ? F19 C32 1.334(4) . ? F19 F20' 1.346(13) . ? F20 F21' 1.089(19) . ? F20 C32 1.348(4) . ? F20 F19' 1.510(14) . ? F21 F19' 0.976(10) . ? F21 C32 1.251(4) . ? F21 F20' 1.277(11) . ? F19' C32 1.363(10) . ? F20' C32 1.366(9) . ? F21' C32 1.159(9) . ? F22 C33 1.322(3) . ? F23 C33 1.310(4) . ? F24 C33 1.321(4) . ? F25 F27' 1.032(10) . ? F25 C34 1.303(6) . ? F25 F26' 1.407(10) . ? F26 F27' 1.142(11) . ? F26 C34 1.414(6) . ? F26 F25' 1.666(12) . ? F27 F25' 0.711(11) . ? F27 C34 1.204(6) . ? F27 F26' 1.428(10) . ? F25' C34 1.353(9) . ? F26' C34 1.427(7) . ? F27' C34 1.166(6) . ? O1 C1 1.243(3) . ? O1 Ag2 2.4324(19) 2_755 ? O2 C1 1.238(3) . ? O3 C3 1.243(3) . ? O4 C3 1.243(3) . ? O4 Ag1 2.2730(19) 2_655 ? O5 C5 1.236(3) . ? O5 Ag1 2.288(2) 2_655 ? O6 C5 1.239(3) . ? N1 C11 1.348(3) . ? N1 C7 1.347(3) . ? N2 C21 1.344(3) . ? N2 C25 1.354(3) . ? C1 C2 1.546(4) . ? C3 C4 1.538(4) . ? C5 C6 1.551(4) . ? C7 C8 1.384(4) . ? C8 C9 1.378(4) . ? C9 C10 1.389(4) . ? C9 C18 1.507(4) . ? C10 C11 1.394(4) . ? C11 C12 1.486(4) . ? C12 C13 1.396(4) . ? C12 C17 1.398(4) . ? C13 C14 1.389(4) . ? C14 C15 1.387(4) . ? C14 C19 1.501(4) . ? C15 C16 1.378(4) . ? C16 C17 1.392(4) . ? C16 C20 1.505(4) . ? C21 C22 1.387(4) . ? C22 C23 1.379(4) . ? C23 C24 1.387(4) . ? C23 C32 1.500(4) . ? C24 C25 1.387(3) . ? C25 C26 1.486(3) . ? C26 C31 1.391(4) . ? C26 C27 1.395(4) . ? C27 C28 1.387(4) . ? C28 C29 1.392(4) . ? C28 C33 1.506(4) . ? C29 C30 1.385(4) . ? C30 C31 1.386(4) . ? C30 C34 1.509(4) . ? 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 O4 Ag1 O5 123.60(8) 2_655 2_655 ? O4 Ag1 O3 145.15(7) 2_655 . ? O5 Ag1 O3 90.83(8) 2_655 . ? O4 Ag1 O2 79.50(7) 2_655 . ? O5 Ag1 O2 101.58(7) 2_655 . ? O3 Ag1 O2 100.39(6) . . ? O4 Ag1 Ag2 93.81(5) 2_655 . ? O5 Ag1 Ag2 141.78(6) 2_655 . ? O3 Ag1 Ag2 53.46(5) . . ? O2 Ag1 Ag2 75.72(4) . . ? O4 Ag1 Ag1 85.26(5) 2_655 2_655 ? O5 Ag1 Ag1 123.37(5) 2_655 2_655 ? O3 Ag1 Ag1 69.35(5) . 2_655 ? O2 Ag1 Ag1 133.21(5) . 2_655 ? Ag2 Ag1 Ag1 61.407(13) . 2_655 ? O4 Ag1 Ag2 81.60(5) 2_655 2_655 ? O5 Ag1 Ag2 77.86(6) 2_655 2_655 ? O3 Ag1 Ag2 102.90(5) . 2_655 ? O2 Ag1 Ag2 156.71(4) . 2_655 ? Ag2 Ag1 Ag2 119.204(13) . 2_655 ? Ag1 Ag1 Ag2 57.796(8) 2_655 2_655 ? O6 Ag2 O1 123.44(7) . . ? O6 Ag2 O1 122.62(7) . 2_755 ? O1 Ag2 O1 77.66(7) . 2_755 ? O6 Ag2 O3 142.88(7) . . ? O1 Ag2 O3 85.17(7) . . ? O1 Ag2 O3 83.42(7) 2_755 . ? O6 Ag2 Ag1 105.69(6) . . ? O1 Ag2 Ag1 81.32(5) . . ? O1 Ag2 Ag1 131.27(5) 2_755 . ? O3 Ag2 Ag1 51.21(5) . . ? O6 Ag2 Ag1 75.01(5) . 2_655 ? O1 Ag2 Ag1 141.84(5) . 2_655 ? O1 Ag2 Ag1 123.26(5) 2_755 2_655 ? O3 Ag2 Ag1 68.23(5) . 2_655 ? Ag1 Ag2 Ag1 60.797(13) . 2_655 ? N1 Ag3 N2 172.78(8) . . ? N1 Ag3 O2 94.54(7) . . ? N2 Ag3 O2 89.42(7) . . ? F6' F4 C4 69.5(15) . . ? F6' F4 F5' 122.0(16) . . ? C4 F4 F5' 57.9(6) . . ? F4' F5 C4 61.6(11) . . ? F4' F5 F6' 105.4(11) . . ? C4 F5 F6' 54.1(6) . . ? F5' F6 F4' 123.3(13) . . ? F5' F6 C4 67.1(10) . . ? F4' F6 C4 60.5(8) . . ? F5 F4' F6 129.5(13) . . ? F5 F4' C4 67.3(9) . . ? F6 F4' C4 64.4(12) . . ? F6 F5' C4 65.5(8) . . ? F6 F5' F4 113.0(11) . . ? C4 F5' F4 55.0(7) . . ? F4 F6' C4 70.2(11) . . ? F4 F6' F5 124.7(19) . . ? C4 F6' F5 57.3(11) . . ? F15' F13 C19 81.7(13) . . ? F15' F13 F14' 146.4(15) . . ? C19 F13 F14' 65.2(6) . . ? F13' F14 C19 56.5(8) . . ? F13' F14 F15' 101.2(9) . . ? C19 F14 F15' 51.0(5) . . ? F14' F15 F13' 111.5(9) . . ? F14' F15 C19 66.7(8) . . ? F13' F15 C19 52.1(6) . . ? F14 F13' C19 81.7(11) . . ? F14 F13' F15 146.6(12) . . ? C19 F13' F15 67.1(9) . . ? F15 F14' F13 108.9(8) . . ? F15 F14' C19 60.0(5) . . ? F13 F14' C19 54.3(6) . . ? F13 F15' C19 63.6(10) . . ? F13 F15' F14 103.2(14) . . ? C19 F15' F14 48.9(6) . . ? F17' F16 C20 49.4(3) . . ? F17' F16 F18' 89.7(5) . . ? C20 F16 F18' 49.9(3) . . ? F18' F17 C20 76.2(10) . . ? F18' F17 F16' 137.4(12) . . ? C20 F17 F16' 66.0(5) . . ? F17' F18 C20 66.0(8) . . ? F17' F18 F16' 128.0(11) . . ? C20 F18 F16' 65.5(5) . . ? F18 F16' F17 93.1(5) . . ? F18 F16' C20 51.6(3) . . ? F17 F16' C20 49.3(3) . . ? F18 F17' C20 77.1(8) . . ? F18 F17' F16 140.7(11) . . ? C20 F17' F16 66.2(7) . . ? F17 F18' C20 70.8(8) . . ? F17 F18' F16 129.5(13) . . ? C20 F18' F16 60.7(6) . . ? F21' F19 C32 56.1(5) . . ? F21' F19 F20' 112.8(7) . . ? C32 F19 F20' 61.3(5) . . ? F21' F20 C32 55.6(6) . . ? F21' F20 F19' 103.7(7) . . ? C32 F20 F19' 56.6(4) . . ? F19' F21 C32 74.3(7) . . ? F19' F21 F20' 137.1(10) . . ? C32 F21 F20' 65.4(5) . . ? F21 F19' C32 62.1(6) . . ? F21 F19' F20 113.4(9) . . ? C32 F19' F20 55.7(5) . . ? F21 F20' F19 107.5(6) . . ? F21 F20' C32 56.4(4) . . ? F19 F20' C32 58.9(5) . . ? F19 F21' F20 144.3(10) . . ? F19 F21' C32 72.8(9) . . ? F20 F21' C32 73.6(8) . . ? F27' F25 C34 58.5(4) . . ? F27' F25 F26' 117.3(7) . . ? C34 F25 F26' 63.4(5) . . ? F27' F26 C34 53.0(4) . . ? F27' F26 F25' 95.2(5) . . ? C34 F26 F25' 51.3(3) . . ? F25' F27 C34 85.9(10) . . ? F25' F27 F26' 149.7(12) . . ? C34 F27 F26' 65.1(4) . . ? F27 F25' C34 62.5(8) . . ? F27 F25' F26 112.6(11) . . ? C34 F25' F26 54.7(5) . . ? F25 F26' C34 54.7(3) . . ? F25 F26' F27 96.3(5) . . ? C34 F26' F27 49.9(3) . . ? F25 F27' F26 146.9(8) . . ? F25 F27' C34 72.4(6) . . ? F26 F27' C34 75.6(6) . . ? C1 O1 Ag2 117.90(16) . . ? C1 O1 Ag2 137.66(17) . 2_755 ? Ag2 O1 Ag2 102.34(7) . 2_755 ? C1 O2 Ag1 120.75(16) . . ? C1 O2 Ag3 132.49(16) . . ? Ag1 O2 Ag3 101.69(6) . . ? C3 O3 Ag1 123.56(17) . . ? C3 O3 Ag2 116.49(18) . . ? Ag1 O3 Ag2 75.34(6) . . ? C3 O4 Ag1 113.91(17) . 2_655 ? C5 O5 Ag1 116.98(18) . 2_655 ? C5 O6 Ag2 124.27(17) . . ? C11 N1 C7 118.6(2) . . ? C11 N1 Ag3 126.58(17) . . ? C7 N1 Ag3 114.86(17) . . ? C21 N2 C25 118.1(2) . . ? C21 N2 Ag3 116.17(17) . . ? C25 N2 Ag3 125.61(17) . . ? O2 C1 O1 129.0(2) . . ? O2 C1 C2 115.6(2) . . ? O1 C1 C2 115.3(2) . . ? F3 C2 F1 107.8(3) . . ? F3 C2 F2 105.4(3) . . ? F1 C2 F2 107.0(3) . . ? F3 C2 C1 113.6(2) . . ? F1 C2 C1 112.7(2) . . ? F2 C2 C1 110.0(2) . . ? O4 C3 O3 129.4(3) . . ? O4 C3 C4 115.5(2) . . ? O3 C3 C4 115.1(3) . . ? F4' C4 F6' 108.9(13) . . ? F4' C4 F4 129.6(6) . . ? F6' C4 F4 40.3(9) . . ? F4' C4 F6 55.1(15) . . ? F6' C4 F6 129.4(6) . . ? F4 C4 F6 108.1(5) . . ? F4' C4 F5' 99.8(14) . . ? F6' C4 F5' 104.1(11) . . ? F4 C4 F5' 67.2(10) . . ? F6 C4 F5' 47.3(10) . . ? F4' C4 F5 51.1(15) . . ? F6' C4 F5 68.6(11) . . ? F4 C4 F5 107.1(5) . . ? F6 C4 F5 104.9(4) . . ? F5' C4 F5 139.3(6) . . ? F4' C4 C3 116.9(6) . . ? F6' C4 C3 115.8(6) . . ? F4 C4 C3 113.3(3) . . ? F6 C4 C3 113.6(3) . . ? F5' C4 C3 109.4(5) . . ? F5 C4 C3 109.5(3) . . ? O5 C5 O6 130.4(3) . . ? O5 C5 C6 113.8(2) . . ? O6 C5 C6 115.8(2) . . ? F9 C6 F7 106.5(3) . . ? F9 C6 F8 107.9(3) . . ? F7 C6 F8 106.2(3) . . ? F9 C6 C5 110.7(3) . . ? F7 C6 C5 112.1(2) . . ? F8 C6 C5 113.2(2) . . ? N1 C7 C8 122.9(3) . . ? C9 C8 C7 118.5(3) . . ? C8 C9 C10 119.4(2) . . ? C8 C9 C18 120.5(3) . . ? C10 C9 C18 120.0(3) . . ? C9 C10 C11 119.1(2) . . ? N1 C11 C10 121.5(2) . . ? N1 C11 C12 118.6(2) . . ? C10 C11 C12 119.9(2) . . ? C13 C12 C17 119.1(2) . . ? C13 C12 C11 119.8(2) . . ? C17 C12 C11 121.1(2) . . ? C14 C13 C12 120.2(3) . . ? C15 C14 C13 120.7(3) . . ? C15 C14 C19 120.1(3) . . ? C13 C14 C19 119.1(3) . . ? C16 C15 C14 119.1(3) . . ? C15 C16 C17 121.2(3) . . ? C15 C16 C20 118.9(3) . . ? C17 C16 C20 119.9(3) . . ? C16 C17 C12 119.7(3) . . ? F10 C18 F12 107.7(3) . . ? F10 C18 F11 107.1(3) . . ? F12 C18 F11 106.2(3) . . ? F10 C18 C9 111.9(3) . . ? F12 C18 C9 112.4(3) . . ? F11 C18 C9 111.2(3) . . ? F13' C19 F13 125.4(6) . . ? F13' C19 F15 60.8(10) . . ? F13 C19 F15 108.4(4) . . ? F13' C19 F14 41.8(10) . . ? F13 C19 F14 107.0(4) . . ? F15 C19 F14 101.8(4) . . ? F13' C19 F15' 114.9(11) . . ? F13 C19 F15' 34.8(7) . . ? F15 C19 F15' 136.8(6) . . ? F14 C19 F15' 80.1(9) . . ? F13' C19 F14' 107.2(11) . . ? F13 C19 F14' 60.5(7) . . ? F15 C19 F14' 53.3(7) . . ? F14 C19 F14' 135.6(5) . . ? F15' C19 F14' 95.1(10) . . ? F13' C19 C14 118.6(6) . . ? F13 C19 C14 115.0(3) . . ? F15 C19 C14 110.9(3) . . ? F14 C19 C14 112.6(3) . . ? F15' C19 C14 107.7(6) . . ? F14' C19 C14 110.8(5) . . ? F17' C20 F17 128.6(4) . . ? F17' C20 F18' 116.7(7) . . ? F17 C20 F18' 33.1(7) . . ? F17' C20 F18 36.9(7) . . ? F17 C20 F18 115.4(6) . . ? F18' C20 F18 127.9(5) . . ? F17' C20 F16 64.4(7) . . ? F17 C20 F16 101.5(5) . . ? F18' C20 F16 69.4(6) . . ? F18 C20 F16 100.3(5) . . ? F17' C20 F16' 98.1(7) . . ? F17 C20 F16' 64.7(5) . . ? F18' C20 F16' 96.1(7) . . ? F18 C20 F16' 62.9(5) . . ? F16 C20 F16' 145.1(4) . . ? F17' C20 C16 117.1(4) . . ? F17 C20 C16 114.3(3) . . ? F18' C20 C16 117.1(5) . . ? F18 C20 C16 114.5(3) . . ? F16 C20 C16 108.7(3) . . ? F16' C20 C16 106.1(3) . . ? N2 C21 C22 123.4(2) . . ? C23 C22 C21 117.9(2) . . ? C22 C23 C24 119.8(2) . . ? C22 C23 C32 120.9(2) . . ? C24 C23 C32 119.3(2) . . ? C23 C24 C25 119.1(2) . . ? N2 C25 C24 121.7(2) . . ? N2 C25 C26 118.0(2) . . ? C24 C25 C26 120.3(2) . . ? C31 C26 C27 119.3(2) . . ? C31 C26 C25 120.6(2) . . ? C27 C26 C25 120.0(2) . . ? C28 C27 C26 120.1(2) . . ? C27 C28 C29 120.6(2) . . ? C27 C28 C33 119.6(2) . . ? C29 C28 C33 119.8(2) . . ? C30 C29 C28 118.9(2) . . ? C31 C30 C29 121.1(2) . . ? C31 C30 C34 119.1(3) . . ? C29 C30 C34 119.8(3) . . ? C30 C31 C26 120.0(2) . . ? F21' C32 F21 127.9(5) . . ? F21' C32 F19 51.0(10) . . ? F21 C32 F19 109.9(4) . . ? F21' C32 F20 50.8(10) . . ? F21 C32 F20 107.7(4) . . ? F19 C32 F20 101.1(3) . . ? F21' C32 F19' 109.3(10) . . ? F21 C32 F19' 43.6(5) . . ? F19 C32 F19' 133.8(4) . . ? F20 C32 F19' 67.7(6) . . ? F21' C32 F20' 106.7(10) . . ? F21 C32 F20' 58.2(6) . . ? F19 C32 F20' 59.8(6) . . ? F20 C32 F20' 141.9(4) . . ? F19' C32 F20' 100.6(7) . . ? F21' C32 C23 118.1(5) . . ? F21 C32 C23 113.8(3) . . ? F19 C32 C23 113.5(3) . . ? F20 C32 C23 109.9(3) . . ? F19' C32 C23 112.4(4) . . ? F20' C32 C23 108.0(4) . . ? F23 C33 F24 107.0(3) . . ? F23 C33 F22 106.1(3) . . ? F24 C33 F22 106.7(3) . . ? F23 C33 C28 111.9(3) . . ? F24 C33 C28 112.4(2) . . ? F22 C33 C28 112.2(2) . . ? F27' C34 F27 124.9(4) . . ? F27' C34 F25 49.1(5) . . ? F27 C34 F25 114.7(6) . . ? F27' C34 F25' 113.0(7) . . ? F27 C34 F25' 31.6(6) . . ? F25 C34 F25' 133.0(4) . . ? F27' C34 F26 51.5(6) . . ? F27 C34 F26 102.6(5) . . ? F25 C34 F26 100.1(5) . . ? F25' C34 F26 74.0(6) . . ? F27' C34 F26' 107.1(6) . . ? F27 C34 F26' 65.1(5) . . ? F25 C34 F26' 61.8(5) . . ? F25' C34 F26' 96.4(6) . . ? F26 C34 F26' 145.3(3) . . ? F27' C34 C30 118.0(4) . . ? F27 C34 C30 116.0(4) . . ? F25 C34 C30 113.8(3) . . ? F25' C34 C30 112.3(4) . . ? F26 C34 C30 107.2(3) . . ? F26' C34 C30 107.4(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 O4 Ag1 Ag2 O6 20.19(7) 2_655 . . . ? O5 Ag1 Ag2 O6 -170.99(10) 2_655 . . . ? O3 Ag1 Ag2 O6 -146.80(8) . . . . ? O2 Ag1 Ag2 O6 98.34(7) . . . . ? Ag1 Ag1 Ag2 O6 -62.30(5) 2_655 . . . ? Ag2 Ag1 Ag2 O6 -62.30(5) 2_655 . . . ? O4 Ag1 Ag2 O1 -102.23(7) 2_655 . . . ? O5 Ag1 Ag2 O1 66.58(10) 2_655 . . . ? O3 Ag1 Ag2 O1 90.78(8) . . . . ? O2 Ag1 Ag2 O1 -24.08(7) . . . . ? Ag1 Ag1 Ag2 O1 175.27(5) 2_655 . . . ? Ag2 Ag1 Ag2 O1 175.27(5) 2_655 . . . ? O4 Ag1 Ag2 O1 -167.29(8) 2_655 . . 2_755 ? O5 Ag1 Ag2 O1 1.52(11) 2_655 . . 2_755 ? O3 Ag1 Ag2 O1 25.71(9) . . . 2_755 ? O2 Ag1 Ag2 O1 -89.15(8) . . . 2_755 ? Ag1 Ag1 Ag2 O1 110.21(6) 2_655 . . 2_755 ? Ag2 Ag1 Ag2 O1 110.21(6) 2_655 . . 2_755 ? O4 Ag1 Ag2 O3 166.99(8) 2_655 . . . ? O5 Ag1 Ag2 O3 -24.20(10) 2_655 . . . ? O2 Ag1 Ag2 O3 -114.86(7) . . . . ? Ag1 Ag1 Ag2 O3 84.50(6) 2_655 . . . ? Ag2 Ag1 Ag2 O3 84.50(6) 2_655 . . . ? O4 Ag1 Ag2 Ag1 82.50(5) 2_655 . . 2_655 ? O5 Ag1 Ag2 Ag1 -108.69(9) 2_655 . . 2_655 ? O3 Ag1 Ag2 Ag1 -84.50(6) . . . 2_655 ? O2 Ag1 Ag2 Ag1 160.65(5) . . . 2_655 ? Ag2 Ag1 Ag2 Ag1 0.0 2_655 . . 2_655 ? C4 F5 F4' F6 -17.9(12) . . . . ? F6' F5 F4' F6 15.0(18) . . . . ? F6' F5 F4' C4 32.9(8) . . . . ? F5' F6 F4' F5 -7(2) . . . . ? C4 F6 F4' F5 18.3(11) . . . . ? F5' F6 F4' C4 -25.0(11) . . . . ? F4' F6 F5' C4 23.5(10) . . . . ? F4' F6 F5' F4 -4.9(16) . . . . ? C4 F6 F5' F4 -28.5(7) . . . . ? F6' F4 F5' F6 3.9(19) . . . . ? C4 F4 F5' F6 32.0(8) . . . . ? F6' F4 F5' C4 -28.1(14) . . . . ? F5' F4 F6' C4 25.2(11) . . . . ? C4 F4 F6' F5 -18.7(12) . . . . ? F5' F4 F6' F5 6(2) . . . . ? F4' F5 F6' F4 -15(2) . . . . ? C4 F5 F6' F4 21.0(13) . . . . ? F4' F5 F6' C4 -36.1(10) . . . . ? F15' F14 F13' C19 -25.8(7) . . . . ? C19 F14 F13' F15 20.4(17) . . . . ? F15' F14 F13' F15 -5(2) . . . . ? F14' F15 F13' F14 10(2) . . . . ? C19 F15 F13' F14 -22.0(19) . . . . ? F14' F15 F13' C19 32.4(8) . . . . ? F13' F15 F14' F13 -2.9(10) . . . . ? C19 F15 F14' F13 24.5(5) . . . . ? F13' F15 F14' C19 -27.4(7) . . . . ? F15' F13 F14' F15 -16(2) . . . . ? C19 F13 F14' F15 -26.3(6) . . . . ? F15' F13 F14' C19 11(2) . . . . ? F14' F13 F15' C19 -10(2) . . . . ? C19 F13 F15' F14 29.4(6) . . . . ? F14' F13 F15' F14 20(3) . . . . ? F13' F14 F15' F13 -7.9(15) . . . . ? C19 F14 F15' F13 -35.7(10) . . . . ? F13' F14 F15' C19 27.8(9) . . . . ? F17' F18 F16' F17 6.1(13) . . . . ? C20 F18 F16' F17 28.7(4) . . . . ? F17' F18 F16' C20 -22.6(11) . . . . ? F18' F17 F16' F18 -0.2(18) . . . . ? C20 F17 F16' F18 -29.8(4) . . . . ? F18' F17 F16' C20 29.6(16) . . . . ? F16' F18 F17' C20 22.6(10) . . . . ? C20 F18 F17' F16 -20.9(13) . . . . ? F16' F18 F17' F16 2(2) . . . . ? C20 F16 F17' F18 22.4(14) . . . . ? F18' F16 F17' F18 -10.1(18) . . . . ? F18' F16 F17' C20 -32.5(5) . . . . ? F16' F17 F18' C20 -27.7(14) . . . . ? C20 F17 F18' F16 16.4(12) . . . . ? F16' F17 F18' F16 -11(3) . . . . ? F17' F16 F18' F17 14.4(17) . . . . ? C20 F16 F18' F17 -17.8(13) . . . . ? F17' F16 F18' C20 32.2(5) . . . . ? F20' F21 F19' C32 20.4(9) . . . . ? C32 F21 F19' F20 -22.3(5) . . . . ? F20' F21 F19' F20 -1.8(14) . . . . ? F21' F20 F19' F21 -7.1(10) . . . . ? C32 F20 F19' F21 23.9(6) . . . . ? F21' F20 F19' C32 -31.0(6) . . . . ? F19' F21 F20' F19 8.9(12) . . . . ? C32 F21 F20' F19 30.7(4) . . . . ? F19' F21 F20' C32 -21.7(10) . . . . ? F21' F19 F20' F21 -6.6(9) . . . . ? C32 F19 F20' F21 -29.7(4) . . . . ? F21' F19 F20' C32 23.2(6) . . . . ? C32 F19 F21' F20 20.4(12) . . . . ? F20' F19 F21' F20 -4.2(18) . . . . ? F20' F19 F21' C32 -24.5(6) . . . . ? C32 F20 F21' F19 -20.3(13) . . . . ? F19' F20 F21' F19 11.2(17) . . . . ? F19' F20 F21' C32 31.5(5) . . . . ? F26' F27 F25' C34 -15.9(18) . . . . ? C34 F27 F25' F26 22.8(8) . . . . ? F26' F27 F25' F26 7(3) . . . . ? F27' F26 F25' F27 7.1(12) . . . . ? C34 F26 F25' F27 -25.0(10) . . . . ? F27' F26 F25' C34 32.1(4) . . . . ? F27' F25 F26' C34 -23.8(5) . . . . ? F27' F25 F26' F27 5.4(7) . . . . ? C34 F25 F26' F27 29.2(3) . . . . ? F25' F27 F26' F25 -14(2) . . . . ? C34 F27 F26' F25 -31.4(4) . . . . ? F25' F27 F26' C34 18(2) . . . . ? C34 F25 F27' F26 -15.2(11) . . . . ? F26' F25 F27' F26 9.9(15) . . . . ? F26' F25 F27' C34 25.1(5) . . . . ? C34 F26 F27' F25 15.0(11) . . . . ? F25' F26 F27' F25 -16.3(14) . . . . ? F25' F26 F27' C34 -31.3(4) . . . . ? O6 Ag2 O1 C1 -72.5(2) . . . . ? O1 Ag2 O1 C1 166.4(2) 2_755 . . . ? O3 Ag2 O1 C1 82.11(19) . . . . ? Ag1 Ag2 O1 C1 30.66(18) . . . . ? Ag1 Ag2 O1 C1 37.3(2) 2_655 . . . ? O6 Ag2 O1 Ag2 121.12(8) . . . 2_755 ? O1 Ag2 O1 Ag2 0.0 2_755 . . 2_755 ? O3 Ag2 O1 Ag2 -84.30(8) . . . 2_755 ? Ag1 Ag2 O1 Ag2 -135.76(7) . . . 2_755 ? Ag1 Ag2 O1 Ag2 -129.07(5) 2_655 . . 2_755 ? O4 Ag1 O2 C1 133.1(2) 2_655 . . . ? O5 Ag1 O2 C1 -104.46(19) 2_655 . . . ? O3 Ag1 O2 C1 -11.4(2) . . . . ? Ag2 Ag1 O2 C1 36.38(18) . . . . ? Ag1 Ag1 O2 C1 59.9(2) 2_655 . . . ? Ag2 Ag1 O2 C1 169.36(14) 2_655 . . . ? O4 Ag1 O2 Ag3 -24.71(7) 2_655 . . . ? O5 Ag1 O2 Ag3 97.74(8) 2_655 . . . ? O3 Ag1 O2 Ag3 -169.25(7) . . . . ? Ag2 Ag1 O2 Ag3 -121.42(6) . . . . ? Ag1 Ag1 O2 Ag3 -97.89(6) 2_655 . . . ? Ag2 Ag1 O2 Ag3 11.56(16) 2_655 . . . ? N1 Ag3 O2 C1 131.6(2) . . . . ? N2 Ag3 O2 C1 -42.3(2) . . . . ? N1 Ag3 O2 Ag1 -74.49(8) . . . . ? N2 Ag3 O2 Ag1 111.56(8) . . . . ? O4 Ag1 O3 C3 89.2(2) 2_655 . . . ? O5 Ag1 O3 C3 -82.4(2) 2_655 . . . ? O2 Ag1 O3 C3 175.7(2) . . . . ? Ag2 Ag1 O3 C3 112.3(2) . . . . ? Ag1 Ag1 O3 C3 43.3(2) 2_655 . . . ? Ag2 Ag1 O3 C3 -4.6(2) 2_655 . . . ? O4 Ag1 O3 Ag2 -23.14(13) 2_655 . . . ? O5 Ag1 O3 Ag2 165.31(6) 2_655 . . . ? O2 Ag1 O3 Ag2 63.37(6) . . . . ? Ag1 Ag1 O3 Ag2 -69.07(4) 2_655 . . . ? Ag2 Ag1 O3 Ag2 -116.95(3) 2_655 . . . ? O6 Ag2 O3 C3 -59.7(2) . . . . ? O1 Ag2 O3 C3 156.74(19) . . . . ? O1 Ag2 O3 C3 78.63(19) 2_755 . . . ? Ag1 Ag2 O3 C3 -120.5(2) . . . . ? Ag1 Ag2 O3 C3 -51.20(18) 2_655 . . . ? O6 Ag2 O3 Ag1 60.86(12) . . . . ? O1 Ag2 O3 Ag1 -82.73(6) . . . . ? O1 Ag2 O3 Ag1 -160.84(6) 2_755 . . . ? Ag1 Ag2 O3 Ag1 69.33(4) 2_655 . . . ? O1 Ag2 O6 C5 176.3(2) . . . . ? O1 Ag2 O6 C5 -86.9(2) 2_755 . . . ? O3 Ag2 O6 C5 41.4(3) . . . . ? Ag1 Ag2 O6 C5 86.4(2) . . . . ? Ag1 Ag2 O6 C5 33.3(2) 2_655 . . . ? N2 Ag3 N1 C11 -45.7(7) . . . . ? O2 Ag3 N1 C11 -168.8(2) . . . . ? N2 Ag3 N1 C7 134.2(6) . . . . ? O2 Ag3 N1 C7 11.16(19) . . . . ? N1 Ag3 N2 C21 -172.5(6) . . . . ? O2 Ag3 N2 C21 -49.14(19) . . . . ? N1 Ag3 N2 C25 11.6(8) . . . . ? O2 Ag3 N2 C25 135.0(2) . . . . ? Ag1 O2 C1 O1 -25.0(4) . . . . ? Ag3 O2 C1 O1 124.8(3) . . . . ? Ag1 O2 C1 C2 158.29(17) . . . . ? Ag3 O2 C1 C2 -51.8(3) . . . . ? Ag2 O1 C1 O2 -11.4(4) . . . . ? Ag2 O1 C1 O2 148.6(2) 2_755 . . . ? Ag2 O1 C1 C2 165.23(17) . . . . ? Ag2 O1 C1 C2 -34.7(4) 2_755 . . . ? O2 C1 C2 F3 -22.5(4) . . . . ? O1 C1 C2 F3 160.4(3) . . . . ? O2 C1 C2 F1 -145.3(3) . . . . ? O1 C1 C2 F1 37.5(4) . . . . ? O2 C1 C2 F2 95.4(3) . . . . ? O1 C1 C2 F2 -81.7(3) . . . . ? Ag1 O4 C3 O3 4.4(4) 2_655 . . . ? Ag1 O4 C3 C4 -174.61(19) 2_655 . . . ? Ag1 O3 C3 O4 -44.2(4) . . . . ? Ag2 O3 C3 O4 45.3(4) . . . . ? Ag1 O3 C3 C4 134.8(2) . . . . ? Ag2 O3 C3 C4 -135.7(2) . . . . ? F5 F4' C4 F6' -39.4(10) . . . . ? F6 F4' C4 F6' 125.3(10) . . . . ? F5 F4' C4 F4 -79.7(14) . . . . ? F6 F4' C4 F4 85.1(17) . . . . ? F5 F4' C4 F6 -164.8(9) . . . . ? F5 F4' C4 F5' -148.1(9) . . . . ? F6 F4' C4 F5' 16.6(9) . . . . ? F6 F4' C4 F5 164.8(9) . . . . ? F5 F4' C4 C3 94.1(10) . . . . ? F6 F4' C4 C3 -101.1(7) . . . . ? F4 F6' C4 F4' -129.7(13) . . . . ? F5 F6' C4 F4' 32.1(11) . . . . ? F5 F6' C4 F4 161.7(11) . . . . ? F4 F6' C4 F6 -69.7(15) . . . . ? F5 F6' C4 F6 92.0(10) . . . . ? F4 F6' C4 F5' -23.9(12) . . . . ? F5 F6' C4 F5' 137.8(8) . . . . ? F4 F6' C4 F5 -161.7(11) . . . . ? F4 F6' C4 C3 96.2(9) . . . . ? F5 F6' C4 C3 -102.1(6) . . . . ? F6' F4 C4 F4' 71(2) . . . . ? F5' F4 C4 F4' -83.8(19) . . . . ? F5' F4 C4 F6' -154.8(12) . . . . ? F6' F4 C4 F6 130.3(10) . . . . ? F5' F4 C4 F6 -24.5(7) . . . . ? F6' F4 C4 F5' 154.8(12) . . . . ? F6' F4 C4 F5 17.8(11) . . . . ? F5' F4 C4 F5 -137.0(7) . . . . ? F6' F4 C4 C3 -103.0(10) . . . . ? F5' F4 C4 C3 102.2(7) . . . . ? F5' F6 C4 F4' 157.4(11) . . . . ? F5' F6 C4 F6' 70.9(15) . . . . ? F4' F6 C4 F6' -86.5(15) . . . . ? F5' F6 C4 F4 31.3(8) . . . . ? F4' F6 C4 F4 -126.2(9) . . . . ? F4' F6 C4 F5' -157.4(11) . . . . ? F5' F6 C4 F5 145.2(8) . . . . ? F4' F6 C4 F5 -12.2(9) . . . . ? F5' F6 C4 C3 -95.2(8) . . . . ? F4' F6 C4 C3 107.3(8) . . . . ? F6 F5' C4 F4' -18.6(11) . . . . ? F4 F5' C4 F4' 129.0(9) . . . . ? F6 F5' C4 F6' -131.1(10) . . . . ? F4 F5' C4 F6' 16.5(9) . . . . ? F6 F5' C4 F4 -147.6(8) . . . . ? F4 F5' C4 F6 147.6(8) . . . . ? F6 F5' C4 F5 -57.6(18) . . . . ? F4 F5' C4 F5 90.0(16) . . . . ? F6 F5' C4 C3 104.6(6) . . . . ? F4 F5' C4 C3 -107.8(4) . . . . ? F6' F5 C4 F4' -139.8(9) . . . . ? F4' F5 C4 F6' 139.8(9) . . . . ? F4' F5 C4 F4 127.5(7) . . . . ? F6' F5 C4 F4 -12.3(7) . . . . ? F4' F5 C4 F6 12.9(8) . . . . ? F6' F5 C4 F6 -126.9(7) . . . . ? F4' F5 C4 F5' 52.9(19) . . . . ? F6' F5 C4 F5' -86.9(18) . . . . ? F4' F5 C4 C3 -109.3(7) . . . . ? F6' F5 C4 C3 110.9(7) . . . . ? O4 C3 C4 F4' 30(2) . . . . ? O3 C3 C4 F4' -150(2) . . . . ? O4 C3 C4 F6' 159.9(14) . . . . ? O3 C3 C4 F6' -19.2(14) . . . . ? O4 C3 C4 F4 -155.6(7) . . . . ? O3 C3 C4 F4 25.2(7) . . . . ? O4 C3 C4 F6 -31.9(6) . . . . ? O3 C3 C4 F6 148.9(6) . . . . ? O4 C3 C4 F5' -82.8(14) . . . . ? O3 C3 C4 F5' 98.0(14) . . . . ? O4 C3 C4 F5 85.0(5) . . . . ? O3 C3 C4 F5 -94.2(5) . . . . ? Ag1 O5 C5 O6 -20.9(4) 2_655 . . . ? Ag1 O5 C5 C6 157.06(19) 2_655 . . . ? Ag2 O6 C5 O5 -18.7(4) . . . . ? Ag2 O6 C5 C6 163.45(18) . . . . ? O5 C5 C6 F9 -75.0(3) . . . . ? O6 C5 C6 F9 103.2(3) . . . . ? O5 C5 C6 F7 43.8(4) . . . . ? O6 C5 C6 F7 -138.0(3) . . . . ? O5 C5 C6 F8 163.8(3) . . . . ? O6 C5 C6 F8 -18.0(4) . . . . ? C11 N1 C7 C8 -0.3(4) . . . . ? Ag3 N1 C7 C8 179.7(2) . . . . ? N1 C7 C8 C9 0.7(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C7 C8 C9 C18 -179.6(3) . . . . ? C8 C9 C10 C11 -0.5(4) . . . . ? C18 C9 C10 C11 178.9(3) . . . . ? C7 N1 C11 C10 -0.5(4) . . . . ? Ag3 N1 C11 C10 179.41(19) . . . . ? C7 N1 C11 C12 -178.7(2) . . . . ? Ag3 N1 C11 C12 1.3(3) . . . . ? C9 C10 C11 N1 1.0(4) . . . . ? C9 C10 C11 C12 179.1(2) . . . . ? N1 C11 C12 C13 132.4(3) . . . . ? C10 C11 C12 C13 -45.8(4) . . . . ? N1 C11 C12 C17 -47.9(4) . . . . ? C10 C11 C12 C17 133.9(3) . . . . ? C17 C12 C13 C14 -0.2(4) . . . . ? C11 C12 C13 C14 179.6(2) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C12 C13 C14 C19 178.4(3) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C19 C14 C15 C16 -178.5(3) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C14 C15 C16 C20 179.3(3) . . . . ? C15 C16 C17 C12 -0.9(4) . . . . ? C20 C16 C17 C12 -179.7(3) . . . . ? C13 C12 C17 C16 0.8(4) . . . . ? C11 C12 C17 C16 -179.0(2) . . . . ? C8 C9 C18 F10 -28.8(4) . . . . ? C10 C9 C18 F10 151.8(3) . . . . ? C8 C9 C18 F12 -150.2(3) . . . . ? C10 C9 C18 F12 30.4(4) . . . . ? C8 C9 C18 F11 90.9(3) . . . . ? C10 C9 C18 F11 -88.4(4) . . . . ? F14 F13' C19 F13 75.3(12) . . . . ? F15 F13' C19 F13 -92.7(9) . . . . ? F14 F13' C19 F15 168.0(10) . . . . ? F15 F13' C19 F14 -168.0(10) . . . . ? F14 F13' C19 F15' 36.6(12) . . . . ? F15 F13' C19 F15' -131.3(8) . . . . ? F14 F13' C19 F14' 140.9(9) . . . . ? F15 F13' C19 F14' -27.1(8) . . . . ? F14 F13' C19 C14 -92.7(8) . . . . ? F15 F13' C19 C14 99.3(7) . . . . ? F15' F13 C19 F13' -83.3(17) . . . . ? F14' F13 C19 F13' 90.8(14) . . . . ? F15' F13 C19 F15 -150.0(12) . . . . ? F14' F13 C19 F15 24.1(5) . . . . ? F15' F13 C19 F14 -40.9(12) . . . . ? F14' F13 C19 F14 133.3(6) . . . . ? F14' F13 C19 F15' 174.1(13) . . . . ? F15' F13 C19 F14' -174.1(13) . . . . ? F15' F13 C19 C14 85.1(12) . . . . ? F14' F13 C19 C14 -100.8(6) . . . . ? F14' F15 C19 F13' -147.2(8) . . . . ? F14' F15 C19 F13 -26.3(6) . . . . ? F13' F15 C19 F13 120.8(7) . . . . ? F14' F15 C19 F14 -139.0(6) . . . . ? F13' F15 C19 F14 8.2(7) . . . . ? F14' F15 C19 F15' -50.9(14) . . . . ? F13' F15 C19 F15' 96.3(14) . . . . ? F13' F15 C19 F14' 147.2(8) . . . . ? F14' F15 C19 C14 100.9(6) . . . . ? F13' F15 C19 C14 -111.9(7) . . . . ? F15' F14 C19 F13' 146.7(10) . . . . ? F13' F14 C19 F13 -124.4(9) . . . . ? F15' F14 C19 F13 22.3(5) . . . . ? F13' F14 C19 F15 -10.7(9) . . . . ? F15' F14 C19 F15 136.0(6) . . . . ? F13' F14 C19 F15' -146.7(10) . . . . ? F13' F14 C19 F14' -59.4(15) . . . . ? F15' F14 C19 F14' 87.3(13) . . . . ? F13' F14 C19 C14 108.2(9) . . . . ? F15' F14 C19 C14 -105.1(6) . . . . ? F13 F15' C19 F13' 116.8(13) . . . . ? F14 F15' C19 F13' -23.8(10) . . . . ? F14 F15' C19 F13 -140.6(11) . . . . ? F13 F15' C19 F15 43.7(19) . . . . ? F14 F15' C19 F15 -96.8(10) . . . . ? F13 F15' C19 F14 140.6(11) . . . . ? F13 F15' C19 F14' 5.1(11) . . . . ? F14 F15' C19 F14' -135.4(5) . . . . ? F13 F15' C19 C14 -108.7(9) . . . . ? F14 F15' C19 C14 110.8(4) . . . . ? F15 F14' C19 F13' 29.7(9) . . . . ? F13 F14' C19 F13' -121.4(8) . . . . ? F15 F14' C19 F13 151.1(6) . . . . ? F13 F14' C19 F15 -151.1(6) . . . . ? F15 F14' C19 F14 66.6(11) . . . . ? F13 F14' C19 F14 -84.5(11) . . . . ? F15 F14' C19 F15' 147.7(8) . . . . ? F13 F14' C19 F15' -3.3(8) . . . . ? F15 F14' C19 C14 -101.1(5) . . . . ? F13 F14' C19 C14 107.8(4) . . . . ? C15 C14 C19 F13' 41.1(14) . . . . ? C13 C14 C19 F13' -137.5(13) . . . . ? C15 C14 C19 F13 -128.1(4) . . . . ? C13 C14 C19 F13 53.3(5) . . . . ? C15 C14 C19 F15 108.3(4) . . . . ? C13 C14 C19 F15 -70.3(5) . . . . ? C15 C14 C19 F14 -5.1(5) . . . . ? C13 C14 C19 F14 176.3(4) . . . . ? C15 C14 C19 F15' -91.5(10) . . . . ? C13 C14 C19 F15' 89.9(10) . . . . ? C15 C14 C19 F14' 165.7(9) . . . . ? C13 C14 C19 F14' -12.9(10) . . . . ? F18 F17' C20 F17 -81.4(12) . . . . ? F16 F17' C20 F17 84.3(9) . . . . ? F18 F17' C20 F18' -118.4(10) . . . . ? F16 F17' C20 F18' 47.3(8) . . . . ? F16 F17' C20 F18 165.7(9) . . . . ? F18 F17' C20 F16 -165.7(9) . . . . ? F18 F17' C20 F16' -17.4(8) . . . . ? F16 F17' C20 F16' 148.3(4) . . . . ? F18 F17' C20 C16 95.4(8) . . . . ? F16 F17' C20 C16 -98.9(5) . . . . ? F18' F17 C20 F17' -80.1(15) . . . . ? F16' F17 C20 F17' 79.7(10) . . . . ? F16' F17 C20 F18' 159.9(11) . . . . ? F18' F17 C20 F18 -121.2(10) . . . . ? F16' F17 C20 F18 38.6(5) . . . . ? F18' F17 C20 F16 -13.8(11) . . . . ? F16' F17 C20 F16 146.1(4) . . . . ? F18' F17 C20 F16' -159.9(11) . . . . ? F18' F17 C20 C16 103.0(10) . . . . ? F16' F17 C20 C16 -97.1(4) . . . . ? F17 F18' C20 F17' 120.4(11) . . . . ? F16 F18' C20 F17' -45.1(8) . . . . ? F16 F18' C20 F17 -165.5(11) . . . . ? F17 F18' C20 F18 78.4(13) . . . . ? F16 F18' C20 F18 -87.2(8) . . . . ? F17 F18' C20 F16 165.5(11) . . . . ? F17 F18' C20 F16' 18.2(10) . . . . ? F16 F18' C20 F16' -147.3(4) . . . . ? F17 F18' C20 C16 -93.4(10) . . . . ? F16 F18' C20 C16 101.1(5) . . . . ? F16' F18 C20 F17' -160.6(9) . . . . ? F17' F18 C20 F17 121.2(9) . . . . ? F16' F18 C20 F17 -39.4(5) . . . . ? F17' F18 C20 F18' 85.0(12) . . . . ? F16' F18 C20 F18' -75.6(9) . . . . ? F17' F18 C20 F16 13.1(9) . . . . ? F16' F18 C20 F16 -147.5(4) . . . . ? F17' F18 C20 F16' 160.6(9) . . . . ? F17' F18 C20 C16 -103.1(8) . . . . ? F16' F18 C20 C16 96.3(4) . . . . ? F18' F16 C20 F17' 135.5(7) . . . . ? F17' F16 C20 F17 -127.5(5) . . . . ? F18' F16 C20 F17 8.0(7) . . . . ? F17' F16 C20 F18' -135.5(7) . . . . ? F17' F16 C20 F18 -8.7(6) . . . . ? F18' F16 C20 F18 126.8(5) . . . . ? F17' F16 C20 F16' -65.4(9) . . . . ? F18' F16 C20 F16' 70.0(9) . . . . ? F17' F16 C20 C16 111.8(5) . . . . ? F18' F16 C20 C16 -112.8(5) . . . . ? F18 F16' C20 F17' 11.6(6) . . . . ? F17 F16' C20 F17' -129.0(5) . . . . ? F18 F16' C20 F17 140.7(5) . . . . ? F18 F16' C20 F18' 129.8(5) . . . . ? F17 F16' C20 F18' -10.9(6) . . . . ? F17 F16' C20 F18 -140.7(5) . . . . ? F18 F16' C20 F16 67.6(9) . . . . ? F17 F16' C20 F16 -73.1(9) . . . . ? F18 F16' C20 C16 -109.7(4) . . . . ? F17 F16' C20 C16 109.7(4) . . . . ? C15 C16 C20 F17' 122.1(10) . . . . ? C17 C16 C20 F17' -59.1(10) . . . . ? C15 C16 C20 F17 -60.7(7) . . . . ? C17 C16 C20 F17 118.2(6) . . . . ? C15 C16 C20 F18' -24.0(9) . . . . ? C17 C16 C20 F18' 154.9(9) . . . . ? C15 C16 C20 F18 163.2(6) . . . . ? C17 C16 C20 F18 -18.0(7) . . . . ? C15 C16 C20 F16 51.9(5) . . . . ? C17 C16 C20 F16 -129.2(4) . . . . ? C15 C16 C20 F16' -129.7(5) . . . . ? C17 C16 C20 F16' 49.1(6) . . . . ? C25 N2 C21 C22 0.4(4) . . . . ? Ag3 N2 C21 C22 -175.9(2) . . . . ? N2 C21 C22 C23 0.4(4) . . . . ? C21 C22 C23 C24 -1.0(4) . . . . ? C21 C22 C23 C32 -178.8(3) . . . . ? C22 C23 C24 C25 0.8(4) . . . . ? C32 C23 C24 C25 178.6(2) . . . . ? C21 N2 C25 C24 -0.6(4) . . . . ? Ag3 N2 C25 C24 175.21(18) . . . . ? C21 N2 C25 C26 177.4(2) . . . . ? Ag3 N2 C25 C26 -6.7(3) . . . . ? C23 C24 C25 N2 0.1(4) . . . . ? C23 C24 C25 C26 -178.0(2) . . . . ? N2 C25 C26 C31 -44.4(3) . . . . ? C24 C25 C26 C31 133.7(3) . . . . ? N2 C25 C26 C27 138.0(3) . . . . ? C24 C25 C26 C27 -44.0(3) . . . . ? C31 C26 C27 C28 0.5(4) . . . . ? C25 C26 C27 C28 178.2(2) . . . . ? C26 C27 C28 C29 -0.5(4) . . . . ? C26 C27 C28 C33 -179.1(2) . . . . ? C27 C28 C29 C30 0.3(4) . . . . ? C33 C28 C29 C30 178.9(3) . . . . ? C28 C29 C30 C31 -0.2(4) . . . . ? C28 C29 C30 C34 179.6(3) . . . . ? C29 C30 C31 C26 0.2(4) . . . . ? C34 C30 C31 C26 -179.6(3) . . . . ? C27 C26 C31 C30 -0.3(4) . . . . ? C25 C26 C31 C30 -178.0(2) . . . . ? F19 F21' C32 F21 85.7(11) . . . . ? F20 F21' C32 F21 -82.1(11) . . . . ? F20 F21' C32 F19 -167.8(7) . . . . ? F19 F21' C32 F20 167.8(7) . . . . ? F19 F21' C32 F19' 131.2(7) . . . . ? F20 F21' C32 F19' -36.5(7) . . . . ? F19 F21' C32 F20' 23.2(7) . . . . ? F20 F21' C32 F20' -144.6(6) . . . . ? F19 F21' C32 C23 -98.6(6) . . . . ? F20 F21' C32 C23 93.6(7) . . . . ? F19' F21 C32 F21' 77.8(15) . . . . ? F20' F21 C32 F21' -87.0(14) . . . . ? F19' F21 C32 F19 133.4(6) . . . . ? F20' F21 C32 F19 -31.4(5) . . . . ? F19' F21 C32 F20 24.1(7) . . . . ? F20' F21 C32 F20 -140.7(5) . . . . ? F20' F21 C32 F19' -164.8(8) . . . . ? F19' F21 C32 F20' 164.8(8) . . . . ? F19' F21 C32 C23 -98.0(6) . . . . ? F20' F21 C32 C23 97.1(5) . . . . ? F20' F19 C32 F21' 154.1(7) . . . . ? F21' F19 C32 F21 -123.2(7) . . . . ? F20' F19 C32 F21 30.9(5) . . . . ? F21' F19 C32 F20 -9.6(6) . . . . ? F20' F19 C32 F20 144.5(5) . . . . ? F21' F19 C32 F19' -79.3(10) . . . . ? F20' F19 C32 F19' 74.8(10) . . . . ? F21' F19 C32 F20' -154.1(7) . . . . ? F21' F19 C32 C23 108.0(6) . . . . ? F20' F19 C32 C23 -97.9(5) . . . . ? F19' F20 C32 F21' -142.6(7) . . . . ? F21' F20 C32 F21 124.9(6) . . . . ? F19' F20 C32 F21 -17.7(5) . . . . ? F21' F20 C32 F19 9.7(6) . . . . ? F19' F20 C32 F19 -133.0(5) . . . . ? F21' F20 C32 F19' 142.6(7) . . . . ? F21' F20 C32 F20' 64.1(12) . . . . ? F19' F20 C32 F20' -78.5(11) . . . . ? F21' F20 C32 C23 -110.6(6) . . . . ? F19' F20 C32 C23 106.8(4) . . . . ? F21 F19' C32 F21' -125.2(9) . . . . ? F20 F19' C32 F21' 29.9(8) . . . . ? F20 F19' C32 F21 155.1(6) . . . . ? F21 F19' C32 F19 -71.1(10) . . . . ? F20 F19' C32 F19 84.0(7) . . . . ? F21 F19' C32 F20 -155.1(6) . . . . ? F21 F19' C32 F20' -13.1(7) . . . . ? F20 F19' C32 F20' 142.0(5) . . . . ? F21 F19' C32 C23 101.6(5) . . . . ? F20 F19' C32 C23 -103.3(4) . . . . ? F21 F20' C32 F21' 124.6(8) . . . . ? F19 F20' C32 F21' -20.8(8) . . . . ? F19 F20' C32 F21 -145.4(5) . . . . ? F21 F20' C32 F19 145.4(5) . . . . ? F21 F20' C32 F20 77.9(11) . . . . ? F19 F20' C32 F20 -67.5(10) . . . . ? F21 F20' C32 F19' 10.6(6) . . . . ? F19 F20' C32 F19' -134.8(5) . . . . ? F21 F20' C32 C23 -107.4(4) . . . . ? F19 F20' C32 C23 107.2(3) . . . . ? C22 C23 C32 F21' 56.5(13) . . . . ? C24 C23 C32 F21' -121.3(13) . . . . ? C22 C23 C32 F21 -127.2(5) . . . . ? C24 C23 C32 F21 55.0(5) . . . . ? C22 C23 C32 F19 -0.5(5) . . . . ? C24 C23 C32 F19 -178.3(3) . . . . ? C22 C23 C32 F20 111.9(4) . . . . ? C24 C23 C32 F20 -65.9(4) . . . . ? C22 C23 C32 F19' -174.8(7) . . . . ? C24 C23 C32 F19' 7.4(7) . . . . ? C22 C23 C32 F20' -64.7(7) . . . . ? C24 C23 C32 F20' 117.5(7) . . . . ? C27 C28 C33 F23 91.0(3) . . . . ? C29 C28 C33 F23 -87.6(3) . . . . ? C27 C28 C33 F24 -148.5(3) . . . . ? C29 C28 C33 F24 32.9(4) . . . . ? C27 C28 C33 F22 -28.2(4) . . . . ? C29 C28 C33 F22 153.2(3) . . . . ? F25 F27' C34 F27 -94.0(8) . . . . ? F26 F27' C34 F27 77.5(7) . . . . ? F26 F27' C34 F25 171.5(7) . . . . ? F25 F27' C34 F25' -127.7(7) . . . . ? F26 F27' C34 F25' 43.8(6) . . . . ? F25 F27' C34 F26 -171.5(7) . . . . ? F25 F27' C34 F26' -22.8(6) . . . . ? F26 F27' C34 F26' 148.6(5) . . . . ? F25 F27' C34 C30 98.3(6) . . . . ? F26 F27' C34 C30 -90.2(5) . . . . ? F25' F27 C34 F27' -77.1(13) . . . . ? F26' F27 C34 F27' 94.1(8) . . . . ? F25' F27 C34 F25 -133.1(10) . . . . ? F26' F27 C34 F25 38.1(5) . . . . ? F26' F27 C34 F25' 171.2(11) . . . . ? F25' F27 C34 F26 -25.6(10) . . . . ? F26' F27 C34 F26 145.6(4) . . . . ? F25' F27 C34 F26' -171.2(11) . . . . ? F25' F27 C34 C30 90.8(10) . . . . ? F26' F27 C34 C30 -98.0(4) . . . . ? F26' F25 C34 F27' -155.1(6) . . . . ? F27' F25 C34 F27 115.7(6) . . . . ? F26' F25 C34 F27 -39.4(5) . . . . ? F27' F25 C34 F25' 84.2(11) . . . . ? F26' F25 C34 F25' -70.9(9) . . . . ? F27' F25 C34 F26 6.8(5) . . . . ? F26' F25 C34 F26 -148.4(4) . . . . ? F27' F25 C34 F26' 155.1(6) . . . . ? F27' F25 C34 C30 -107.2(5) . . . . ? F26' F25 C34 C30 97.7(4) . . . . ? F27 F25' C34 F27' 119.7(10) . . . . ? F26 F25' C34 F27' -34.2(6) . . . . ? F26 F25' C34 F27 -154.0(10) . . . . ? F27 F25' C34 F25 65.0(14) . . . . ? F26 F25' C34 F25 -89.0(9) . . . . ? F27 F25' C34 F26 154.0(10) . . . . ? F27 F25' C34 F26' 8.0(10) . . . . ? F26 F25' C34 F26' -145.9(4) . . . . ? F27 F25' C34 C30 -103.7(9) . . . . ? F26 F25' C34 C30 102.3(4) . . . . ? F25' F26 C34 F27' 138.5(5) . . . . ? F27' F26 C34 F27 -124.9(5) . . . . ? F25' F26 C34 F27 13.6(5) . . . . ? F27' F26 C34 F25 -6.5(5) . . . . ? F25' F26 C34 F25 132.0(5) . . . . ? F27' F26 C34 F25' -138.5(5) . . . . ? F27' F26 C34 F26' -60.8(10) . . . . ? F25' F26 C34 F26' 77.8(9) . . . . ? F27' F26 C34 C30 112.5(4) . . . . ? F25' F26 C34 C30 -109.0(4) . . . . ? F25 F26' C34 F27' 19.4(5) . . . . ? F27 F26' C34 F27' -121.1(5) . . . . ? F25 F26' C34 F27 140.6(5) . . . . ? F27 F26' C34 F25 -140.6(5) . . . . ? F25 F26' C34 F25' 135.9(5) . . . . ? F27 F26' C34 F25' -4.6(6) . . . . ? F25 F26' C34 F26 65.0(9) . . . . ? F27 F26' C34 F26 -75.6(9) . . . . ? F25 F26' C34 C30 -108.2(4) . . . . ? F27 F26' C34 C30 111.2(4) . . . . ? C31 C30 C34 F27' 111.7(9) . . . . ? C29 C30 C34 F27' -68.1(9) . . . . ? C31 C30 C34 F27 -57.0(7) . . . . ? C29 C30 C34 F27 123.2(6) . . . . ? C31 C30 C34 F25 166.5(6) . . . . ? C29 C30 C34 F25 -13.3(7) . . . . ? C31 C30 C34 F25' -22.5(8) . . . . ? C29 C30 C34 F25' 157.7(7) . . . . ? C31 C30 C34 F26 56.8(5) . . . . ? C29 C30 C34 F26 -123.0(5) . . . . ? C31 C30 C34 F26' -127.3(5) . . . . ? C29 C30 C34 F26' 53.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.621 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.079 #===END #===END data_03324 _database_code_depnum_ccdc_archive 'CCDC 257682' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H31 F36 Ir N4' _chemical_formula_weight 1696.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9220(13) _cell_length_b 15.9360(16) _cell_length_c 17.7587(18) _cell_angle_alpha 67.8845(17) _cell_angle_beta 72.2741(17) _cell_angle_gamma 69.862(2) _cell_volume 3115.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description iregblok _exptl_crystal_colour dk.gold _exptl_crystal_size_max .28 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 2.295 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18319 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.30 _reflns_number_total 13836 _reflns_number_gt 11898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+1.8337P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13836 _refine_ls_number_parameters 921 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.003 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 0.319535(12) 0.281566(9) 0.307163(8) 0.02286(5) Uani 1 1 d . . . F1 F -0.0381(3) 0.6561(3) 0.4566(3) 0.0741(10) Uani 1 1 d . . . F2 F 0.0940(3) 0.6188(3) 0.5177(2) 0.0779(11) Uani 1 1 d . . . F3 F 0.1094(4) 0.7074(2) 0.3940(3) 0.1106(19) Uani 1 1 d . . . F4 F 0.6359(8) 0.2630(5) 0.5838(5) 0.183(4) Uani 1 1 d . . . F5 F 0.6077(5) 0.4022(3) 0.5106(5) 0.164(3) Uani 1 1 d . . . F6 F 0.7390(5) 0.2965(6) 0.4745(7) 0.196(4) Uani 1 1 d . . . F7 F 0.6579(3) 0.0573(2) 0.4238(2) 0.0670(10) Uani 1 1 d . . . F8 F 0.6170(2) 0.1279(2) 0.30317(17) 0.0559(8) Uani 1 1 d . . . F9 F 0.4971(3) 0.06799(18) 0.40617(18) 0.0521(7) Uani 1 1 d . . . F10 F -0.0198(4) 0.0714(3) 0.6771(2) 0.0921(13) Uani 1 1 d . . . F11 F -0.1123(3) 0.0898(3) 0.5917(3) 0.1017(16) Uani 1 1 d . . . F12 F 0.0329(4) -0.0278(2) 0.6122(3) 0.1034(16) Uani 1 1 d . . . F13 F -0.1992(8) 0.3829(9) 0.1983(10) 0.312(8) Uani 1 1 d . . . F14 F -0.1621(6) 0.2487(6) 0.2269(4) 0.170(4) Uani 1 1 d . . . F15 F -0.1094(6) 0.3279(6) 0.1086(3) 0.171(4) Uani 1 1 d . . . F16 F 0.1901(2) 0.4608(2) 0.03746(16) 0.0533(8) Uani 1 1 d . . . F17 F 0.3360(2) 0.3595(2) 0.08014(16) 0.0478(7) Uani 1 1 d . . . F18 F 0.2497(2) 0.47344(17) 0.13203(17) 0.0457(6) Uani 1 1 d . . . F19 F 0.4765(3) 0.5948(2) 0.2077(2) 0.0770(12) Uani 1 1 d . . . F20 F 0.6366(3) 0.5705(2) 0.1261(2) 0.0578(8) Uani 1 1 d . . . F21 F 0.4885(3) 0.63261(18) 0.0766(2) 0.0626(9) Uani 1 1 d . . . F22 F 0.8774(4) 0.0174(3) 0.2006(3) 0.123(2) Uani 1 1 d . . . F23 F 1.0158(3) 0.0132(3) 0.0957(3) 0.1134(17) Uani 1 1 d . . . F24 F 0.8759(4) -0.0308(3) 0.1059(3) 0.1064(16) Uani 1 1 d . . . F25 F 0.9500(3) 0.3580(3) -0.1504(3) 0.0868(12) Uani 1 1 d . . . F26 F 0.9492(4) 0.2401(3) -0.1817(2) 0.1017(16) Uani 1 1 d . . . F27 F 0.8054(3) 0.3585(2) -0.18621(18) 0.0640(9) Uani 1 1 d . . . F28 F 0.3139(3) 0.03871(18) 0.39905(16) 0.0511(7) Uani 1 1 d . . . F29 F 0.2172(3) 0.0659(2) 0.3090(2) 0.0575(8) Uani 1 1 d . . . F30 F 0.3573(3) -0.05600(18) 0.32958(18) 0.0593(9) Uani 1 1 d . . . F31 F 0.6586(5) -0.2278(3) 0.0711(4) 0.132(2) Uani 1 1 d . . . F32 F 0.7305(7) -0.2051(3) -0.0513(3) 0.163(3) Uani 1 1 d . . . F33 F 0.8201(5) -0.2155(3) 0.0316(5) 0.158(3) Uani 1 1 d . . . F34 F 0.5901(4) 0.1825(3) -0.2081(3) 0.1038(15) Uani 1 1 d . . . F35 F 0.7564(4) 0.1091(3) -0.2336(2) 0.1095(17) Uani 1 1 d . . . F36 F 0.7080(5) 0.2220(3) -0.1818(2) 0.0999(16) Uani 1 1 d . . . N1 N 0.2319(3) 0.3993(2) 0.35124(18) 0.0232(6) Uani 1 1 d . . . N15 N 0.2119(3) 0.2113(2) 0.40987(19) 0.0247(6) Uani 1 1 d . . . C1 C 0.1310(3) 0.4560(3) 0.3348(2) 0.0293(8) Uani 1 1 d . . . H1A H 0.0969 0.4432 0.3027 0.035 Uiso 1 1 calc R . . C2 C 0.0766(4) 0.5325(3) 0.3641(3) 0.0335(9) Uani 1 1 d . . . H2A H 0.0073 0.5706 0.3517 0.040 Uiso 1 1 calc R . . C3 C 0.1277(4) 0.5509(3) 0.4122(3) 0.0336(9) Uani 1 1 d . . . C4 C 0.2310(4) 0.4933(3) 0.4293(3) 0.0352(9) Uani 1 1 d . . . H4A H 0.2661 0.5053 0.4614 0.042 Uiso 1 1 calc R . . C5 C 0.2826(3) 0.4172(3) 0.3982(2) 0.0278(8) Uani 1 1 d . . . C6 C 0.3927(4) 0.3504(3) 0.4118(3) 0.0322(9) Uani 1 1 d . . . C7 C 0.4559(4) 0.3670(3) 0.4531(3) 0.0472(12) Uani 1 1 d . . . H7A H 0.4301 0.4204 0.4702 0.057 Uiso 1 1 calc R . . C8 C 0.5577(5) 0.3034(4) 0.4689(4) 0.0535(14) Uani 1 1 d . . . C9 C 0.5910(4) 0.2226(3) 0.4473(3) 0.0460(12) Uani 1 1 d . . . H9A H 0.6563 0.1776 0.4613 0.055 Uiso 1 1 calc R . . C10 C 0.5289(4) 0.2068(3) 0.4050(3) 0.0346(9) Uani 1 1 d . . . C11 C 0.4273(3) 0.2719(3) 0.3821(2) 0.0267(8) Uani 1 1 d . . . C12 C 0.0731(4) 0.6348(3) 0.4433(3) 0.0484(12) Uani 1 1 d . . . C13 C 0.6273(7) 0.3199(5) 0.5127(7) 0.097(3) Uani 1 1 d . . . C14 C 0.5734(4) 0.1152(3) 0.3851(3) 0.0426(11) Uani 1 1 d . . . C15 C 0.2336(4) 0.1696(3) 0.4875(2) 0.0299(8) Uani 1 1 d . . . H15A H 0.2985 0.1728 0.4974 0.036 Uiso 1 1 calc R . . C16 C 0.1628(4) 0.1225(3) 0.5523(2) 0.0339(9) Uani 1 1 d . . . H16A H 0.1797 0.0939 0.6050 0.041 Uiso 1 1 calc R . . C17 C 0.0660(4) 0.1192(3) 0.5366(3) 0.0364(10) Uani 1 1 d . . . C18 C 0.0414(4) 0.1639(3) 0.4590(3) 0.0363(9) Uani 1 1 d . . . H18A H -0.0246 0.1631 0.4487 0.044 Uiso 1 1 calc R . . C19 C 0.1154(3) 0.2104(3) 0.3958(3) 0.0294(8) Uani 1 1 d . . . C20 C 0.0994(4) 0.2591(3) 0.3101(3) 0.0313(9) Uani 1 1 d . . . C21 C 0.0031(4) 0.2619(4) 0.2880(3) 0.0492(12) Uani 1 1 d . . . H21A H -0.0499 0.2320 0.3272 0.059 Uiso 1 1 calc R . . C22 C -0.0133(5) 0.3088(4) 0.2083(3) 0.0543(14) Uani 1 1 d . . . C23 C 0.0644(4) 0.3543(3) 0.1508(3) 0.0428(11) Uani 1 1 d . . . H23A H 0.0527 0.3867 0.0970 0.051 Uiso 1 1 calc R . . C24 C 0.1602(4) 0.3524(3) 0.1724(2) 0.0304(8) Uani 1 1 d . . . C25 C 0.1849(3) 0.3021(3) 0.2521(2) 0.0257(8) Uani 1 1 d . . . C26 C -0.0099(5) 0.0633(4) 0.6041(3) 0.0541(14) Uani 1 1 d . . . C27 C -0.1120(8) 0.3070(8) 0.1829(6) 0.114(4) Uani 1 1 d . . . C28 C 0.2342(4) 0.4100(3) 0.1063(3) 0.0382(10) Uani 1 1 d . . . N29 N 0.5068(3) 0.2990(2) 0.16771(19) 0.0229(6) Uani 1 1 d . . . C30 C 0.4261(3) 0.3472(3) 0.2182(2) 0.0236(7) Uani 1 1 d . . . C31 C 0.4364(3) 0.4373(3) 0.2073(2) 0.0279(8) Uani 1 1 d . . . H31A H 0.3834 0.4733 0.2396 0.033 Uiso 1 1 calc R . . C32 C 0.5212(3) 0.4725(3) 0.1511(2) 0.0282(8) Uani 1 1 d . . . C33 C 0.6043(3) 0.4183(3) 0.1032(2) 0.0285(8) Uani 1 1 d . . . H33A H 0.6631 0.4419 0.0654 0.034 Uiso 1 1 calc R . . C34 C 0.5981(3) 0.3305(2) 0.1126(2) 0.0232(7) Uani 1 1 d . . . C35 C 0.6956(3) 0.2704(3) 0.0695(2) 0.0272(8) Uani 1 1 d . . . C36 C 0.7530(4) 0.1822(3) 0.1139(3) 0.0332(9) Uani 1 1 d . . . H36A H 0.7261 0.1569 0.1702 0.040 Uiso 1 1 calc R . . C37 C 0.8511(4) 0.1327(3) 0.0729(3) 0.0483(12) Uani 1 1 d . . . C38 C 0.8949(4) 0.1701(4) -0.0102(3) 0.0516(13) Uani 1 1 d . . . H38A H 0.9607 0.1365 -0.0368 0.062 Uiso 1 1 calc R . . C39 C 0.8390(4) 0.2583(3) -0.0530(3) 0.0416(11) Uani 1 1 d . . . C40 C 0.7397(3) 0.3084(3) -0.0138(3) 0.0320(9) Uani 1 1 d . . . H40A H 0.7027 0.3676 -0.0436 0.038 Uiso 1 1 calc R . . C41 C 0.5307(4) 0.5676(3) 0.1410(3) 0.0378(10) Uani 1 1 d . . . C42 C 0.9062(6) 0.0356(5) 0.1213(5) 0.078(2) Uani 1 1 d . . . C43 C 0.8854(5) 0.3034(4) -0.1432(4) 0.0612(16) Uani 1 1 d . . . C44 C 0.4855(3) 0.2119(2) 0.1764(2) 0.0229(7) Uani 1 1 d . . . C45 C 0.4059(3) 0.1795(2) 0.2492(2) 0.0241(7) Uani 1 1 d . . . C46 C 0.3998(4) 0.0904(3) 0.2553(2) 0.0291(8) Uani 1 1 d . . . C47 C 0.4602(4) 0.0473(3) 0.1936(2) 0.0321(9) Uani 1 1 d . . . H47A H 0.4555 -0.0121 0.2001 0.039 Uiso 1 1 calc R . . C48 C 0.5268(3) 0.0922(3) 0.1231(2) 0.0287(8) Uani 1 1 d . . . N49 N 0.5382(3) 0.1763(2) 0.11503(19) 0.0256(7) Uani 1 1 d . . . C50 C 0.5878(3) 0.0539(3) 0.0527(3) 0.0311(8) Uani 1 1 d . . . C51 C 0.6224(4) -0.0422(3) 0.0644(3) 0.0371(10) Uani 1 1 d . . . H51A H 0.6058 -0.0835 0.1170 0.045 Uiso 1 1 calc R . . C52 C 0.6823(4) -0.0771(3) -0.0028(3) 0.0420(11) Uani 1 1 d . . . C53 C 0.7063(4) -0.0169(3) -0.0811(3) 0.0433(11) Uani 1 1 d . . . H53A H 0.7466 -0.0401 -0.1254 0.052 Uiso 1 1 calc R . . C54 C 0.6694(4) 0.0796(3) -0.0931(3) 0.0416(11) Uani 1 1 d . . . C55 C 0.6118(4) 0.1143(3) -0.0261(3) 0.0341(9) Uani 1 1 d . . . H55A H 0.5895 0.1787 -0.0346 0.041 Uiso 1 1 calc R . . C56 C 0.3223(4) 0.0358(3) 0.3237(3) 0.0406(11) Uani 1 1 d . . . C57 C 0.7233(6) -0.1804(4) 0.0116(4) 0.0618(16) Uani 1 1 d . . . C58 C 0.6872(6) 0.1475(4) -0.1784(3) 0.0612(16) Uani 1 1 d . . . C63 C -0.264(2) 0.6886(18) 0.3040(11) 0.198(9) Uani 1 1 d . . . H63A H -0.2363 0.7106 0.2447 0.238 Uiso 1 1 calc R . . H63B H -0.1986 0.6707 0.3276 0.238 Uiso 1 1 calc R . . C65 C -0.3195(16) 0.8511(12) 0.3118(11) 0.221(9) Uani 1 1 d . . . H65A H -0.3858 0.8914 0.2908 0.331 Uiso 1 1 calc R . . H65B H -0.2546 0.8707 0.2750 0.331 Uiso 1 1 calc R . . H65C H -0.3255 0.8545 0.3658 0.331 Uiso 1 1 calc R . . C61 C -0.1986(18) 0.5435(16) 0.2826(13) 0.242(10) Uani 1 1 d . . . H61A H -0.2398 0.4990 0.2932 0.363 Uiso 1 1 calc R . . H61B H -0.1373 0.5140 0.3115 0.363 Uiso 1 1 calc R . . H61C H -0.1696 0.5656 0.2241 0.363 Uiso 1 1 calc R . . C64 C -0.310(2) 0.7694(13) 0.3166(18) 0.335(19) Uani 1 1 d . . . H64A H -0.3804 0.7815 0.3006 0.401 Uiso 1 1 calc R . . H64B H -0.3281 0.7459 0.3767 0.401 Uiso 1 1 calc R . . C62 C -0.265(3) 0.6139(19) 0.308(2) 0.38(3) Uani 1 1 d . . . H62A H -0.3324 0.6263 0.2885 0.451 Uiso 1 1 calc R . . H62B H -0.2839 0.5848 0.3678 0.451 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02738(9) 0.01767(8) 0.02381(8) -0.00763(5) -0.00379(5) -0.00590(5) F1 0.0483(19) 0.068(2) 0.117(3) -0.065(2) -0.0099(19) 0.0077(16) F2 0.085(3) 0.075(2) 0.088(3) -0.063(2) -0.017(2) 0.003(2) F3 0.156(4) 0.0384(19) 0.110(3) -0.044(2) 0.056(3) -0.040(2) F4 0.296(10) 0.137(5) 0.192(7) 0.024(5) -0.204(8) -0.094(6) F5 0.200(6) 0.075(3) 0.312(8) -0.088(4) -0.201(6) 0.013(3) F6 0.094(4) 0.207(8) 0.383(13) -0.169(9) -0.119(6) -0.004(5) F7 0.079(2) 0.0534(18) 0.0623(19) -0.0284(16) -0.0474(17) 0.0317(17) F8 0.0456(16) 0.075(2) 0.0360(14) -0.0239(14) -0.0090(12) 0.0063(15) F9 0.079(2) 0.0276(13) 0.0490(16) -0.0110(12) -0.0159(15) -0.0105(14) F10 0.100(3) 0.118(3) 0.0437(19) -0.004(2) 0.0151(19) -0.060(3) F11 0.061(2) 0.125(4) 0.083(3) 0.029(2) -0.006(2) -0.057(2) F12 0.117(3) 0.0397(19) 0.118(3) -0.007(2) 0.030(3) -0.044(2) F13 0.148(7) 0.343(15) 0.58(2) -0.253(16) -0.237(12) 0.041(9) F14 0.163(6) 0.261(8) 0.126(4) 0.051(5) -0.089(4) -0.171(6) F15 0.159(5) 0.324(10) 0.082(3) 0.014(5) -0.062(3) -0.175(7) F16 0.0522(17) 0.0627(19) 0.0340(14) 0.0094(13) -0.0205(12) -0.0181(15) F17 0.0399(15) 0.0612(18) 0.0352(13) -0.0140(13) -0.0069(11) -0.0062(13) F18 0.0570(17) 0.0276(13) 0.0522(16) 0.0001(11) -0.0176(13) -0.0182(12) F19 0.114(3) 0.0520(19) 0.074(2) -0.0448(17) 0.031(2) -0.048(2) F20 0.0517(18) 0.0422(16) 0.095(2) -0.0293(16) -0.0118(16) -0.0240(14) F21 0.076(2) 0.0214(13) 0.085(2) -0.0005(14) -0.0301(18) -0.0120(14) F22 0.139(4) 0.080(3) 0.079(3) -0.010(2) -0.040(3) 0.054(3) F23 0.060(2) 0.071(3) 0.169(5) -0.015(3) -0.040(3) 0.023(2) F24 0.100(3) 0.040(2) 0.137(4) -0.017(2) -0.009(3) 0.008(2) F25 0.069(2) 0.089(3) 0.088(3) -0.012(2) 0.017(2) -0.048(2) F26 0.124(3) 0.063(2) 0.062(2) -0.0262(19) 0.041(2) -0.002(2) F27 0.091(3) 0.0524(19) 0.0384(15) -0.0103(14) 0.0060(16) -0.0271(18) F28 0.079(2) 0.0318(14) 0.0326(13) -0.0102(11) 0.0113(13) -0.0217(14) F29 0.0511(18) 0.0542(18) 0.068(2) -0.0200(15) 0.0075(15) -0.0304(15) F30 0.087(2) 0.0240(13) 0.0547(17) -0.0185(12) 0.0237(15) -0.0249(14) F31 0.150(5) 0.035(2) 0.172(5) -0.044(3) 0.036(4) -0.024(3) F32 0.325(9) 0.052(2) 0.124(4) -0.059(3) -0.089(5) 0.009(4) F33 0.102(4) 0.056(3) 0.322(9) -0.063(4) -0.098(5) 0.029(3) F34 0.127(4) 0.105(3) 0.062(2) 0.002(2) -0.020(3) -0.040(3) F35 0.151(4) 0.088(3) 0.048(2) -0.031(2) 0.035(2) -0.020(3) F36 0.187(5) 0.085(3) 0.049(2) -0.0129(19) 0.001(2) -0.092(3) N1 0.0267(16) 0.0197(14) 0.0254(15) -0.0096(12) -0.0040(12) -0.0064(12) N15 0.0299(17) 0.0175(14) 0.0244(15) -0.0083(12) -0.0036(12) -0.0029(12) C1 0.028(2) 0.029(2) 0.032(2) -0.0123(16) -0.0071(16) -0.0050(16) C2 0.030(2) 0.026(2) 0.043(2) -0.0131(18) -0.0055(17) -0.0038(16) C3 0.032(2) 0.028(2) 0.043(2) -0.0184(18) -0.0001(17) -0.0079(17) C4 0.041(2) 0.029(2) 0.041(2) -0.0197(18) -0.0084(19) -0.0070(18) C5 0.030(2) 0.0250(19) 0.033(2) -0.0140(16) -0.0057(16) -0.0071(16) C6 0.035(2) 0.026(2) 0.037(2) -0.0107(17) -0.0106(17) -0.0056(17) C7 0.049(3) 0.036(2) 0.071(3) -0.022(2) -0.030(3) -0.008(2) C8 0.054(3) 0.041(3) 0.081(4) -0.018(3) -0.039(3) -0.009(2) C9 0.039(3) 0.036(2) 0.063(3) -0.008(2) -0.025(2) -0.005(2) C10 0.035(2) 0.029(2) 0.035(2) -0.0064(17) -0.0120(17) -0.0020(17) C11 0.029(2) 0.0236(18) 0.0261(18) -0.0053(15) -0.0046(15) -0.0081(15) C12 0.047(3) 0.037(3) 0.065(3) -0.032(2) -0.004(2) -0.004(2) C13 0.092(6) 0.055(4) 0.175(9) -0.021(5) -0.099(6) -0.009(4) C14 0.041(3) 0.040(3) 0.034(2) -0.0116(19) -0.0139(19) 0.011(2) C15 0.036(2) 0.0251(19) 0.0272(19) -0.0105(15) -0.0043(16) -0.0048(16) C16 0.040(2) 0.0243(19) 0.0265(19) -0.0052(16) -0.0021(17) -0.0025(17) C17 0.035(2) 0.0234(19) 0.039(2) -0.0079(17) 0.0069(18) -0.0085(17) C18 0.032(2) 0.033(2) 0.044(2) -0.0106(19) -0.0045(18) -0.0123(18) C19 0.029(2) 0.0229(18) 0.035(2) -0.0099(16) -0.0017(16) -0.0082(16) C20 0.035(2) 0.027(2) 0.036(2) -0.0076(16) -0.0083(17) -0.0136(17) C21 0.048(3) 0.050(3) 0.055(3) -0.001(2) -0.017(2) -0.030(2) C22 0.057(3) 0.058(3) 0.060(3) -0.005(3) -0.032(3) -0.027(3) C23 0.055(3) 0.042(3) 0.041(2) -0.007(2) -0.023(2) -0.017(2) C24 0.038(2) 0.0239(19) 0.033(2) -0.0098(16) -0.0115(17) -0.0069(17) C25 0.029(2) 0.0218(18) 0.0285(18) -0.0090(15) -0.0080(15) -0.0060(15) C26 0.049(3) 0.049(3) 0.049(3) 0.000(2) 0.004(2) -0.022(2) C27 0.097(6) 0.137(8) 0.107(7) 0.039(6) -0.071(5) -0.071(6) C28 0.044(3) 0.039(2) 0.030(2) -0.0041(18) -0.0124(18) -0.011(2) N29 0.0266(16) 0.0169(14) 0.0261(15) -0.0079(12) -0.0042(12) -0.0060(12) C30 0.0269(19) 0.0211(17) 0.0259(17) -0.0104(14) -0.0052(14) -0.0062(14) C31 0.033(2) 0.0222(18) 0.0306(19) -0.0118(15) -0.0050(16) -0.0064(15) C32 0.032(2) 0.0197(18) 0.035(2) -0.0087(15) -0.0094(16) -0.0069(15) C33 0.028(2) 0.0258(19) 0.033(2) -0.0081(16) -0.0035(16) -0.0109(16) C34 0.0251(19) 0.0199(17) 0.0261(17) -0.0075(14) -0.0080(14) -0.0046(14) C35 0.0255(19) 0.0210(18) 0.036(2) -0.0096(15) -0.0069(15) -0.0049(15) C36 0.035(2) 0.026(2) 0.035(2) -0.0098(17) -0.0068(17) -0.0025(17) C37 0.043(3) 0.033(2) 0.059(3) -0.018(2) -0.010(2) 0.006(2) C38 0.041(3) 0.045(3) 0.058(3) -0.027(2) 0.004(2) 0.003(2) C39 0.039(2) 0.036(2) 0.047(3) -0.022(2) 0.009(2) -0.012(2) C40 0.031(2) 0.026(2) 0.035(2) -0.0120(17) 0.0002(17) -0.0065(16) C41 0.040(2) 0.025(2) 0.048(2) -0.0137(19) -0.0024(19) -0.0110(18) C42 0.067(4) 0.057(4) 0.077(5) -0.024(3) -0.011(3) 0.025(3) C43 0.062(4) 0.049(3) 0.055(3) -0.022(3) 0.023(3) -0.019(3) C44 0.0252(19) 0.0191(17) 0.0253(17) -0.0093(14) -0.0057(14) -0.0036(14) C45 0.029(2) 0.0176(16) 0.0254(17) -0.0070(14) -0.0064(15) -0.0050(14) C46 0.039(2) 0.0202(18) 0.0292(19) -0.0088(15) -0.0027(16) -0.0108(16) C47 0.045(2) 0.0208(18) 0.034(2) -0.0136(16) -0.0044(18) -0.0102(17) C48 0.034(2) 0.0225(18) 0.0313(19) -0.0115(15) -0.0058(16) -0.0061(16) N49 0.0319(17) 0.0208(15) 0.0261(15) -0.0090(12) -0.0045(13) -0.0083(13) C50 0.035(2) 0.030(2) 0.034(2) -0.0178(17) -0.0038(17) -0.0093(17) C51 0.046(3) 0.027(2) 0.041(2) -0.0169(18) -0.0057(19) -0.0084(19) C52 0.048(3) 0.033(2) 0.050(3) -0.025(2) -0.009(2) -0.004(2) C53 0.044(3) 0.046(3) 0.046(3) -0.032(2) 0.002(2) -0.009(2) C54 0.050(3) 0.046(3) 0.036(2) -0.024(2) 0.002(2) -0.017(2) C55 0.042(2) 0.028(2) 0.036(2) -0.0165(17) -0.0004(18) -0.0120(18) C56 0.057(3) 0.0206(19) 0.042(2) -0.0142(18) 0.003(2) -0.0129(19) C57 0.077(4) 0.038(3) 0.068(4) -0.031(3) -0.007(3) -0.001(3) C58 0.092(5) 0.055(3) 0.040(3) -0.028(3) 0.011(3) -0.028(3) C63 0.26(2) 0.26(3) 0.142(13) -0.107(17) -0.012(13) -0.13(2) C65 0.31(2) 0.173(14) 0.250(19) -0.071(15) -0.196(18) -0.014(16) C61 0.25(2) 0.31(3) 0.26(2) -0.14(2) -0.075(18) -0.10(2) C64 0.41(4) 0.114(14) 0.36(3) -0.065(19) 0.04(3) -0.03(2) C62 0.47(6) 0.21(3) 0.34(4) -0.12(3) -0.04(3) 0.06(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 C30 1.977(4) . ? Ir1 C45 2.065(4) . ? Ir1 C25 2.119(4) . ? Ir1 N15 2.123(3) . ? Ir1 N1 2.125(3) . ? Ir1 C11 2.136(4) . ? F1 C12 1.324(6) . ? F2 C12 1.341(6) . ? F3 C12 1.298(6) . ? F4 C13 1.257(10) . ? F5 C13 1.236(8) . ? F6 C13 1.381(12) . ? F7 C14 1.342(5) . ? F8 C14 1.354(5) . ? F9 C14 1.323(6) . ? F10 C26 1.314(7) . ? F11 C26 1.303(7) . ? F12 C26 1.331(6) . ? F13 C27 1.390(14) . ? F14 C27 1.205(9) . ? F15 C27 1.227(10) . ? F16 C28 1.354(5) . ? F17 C28 1.332(5) . ? F18 C28 1.347(5) . ? F19 C41 1.324(5) . ? F20 C41 1.326(5) . ? F21 C41 1.334(5) . ? F22 C42 1.286(8) . ? F23 C42 1.312(8) . ? F24 C42 1.385(9) . ? F25 C43 1.349(7) . ? F26 C43 1.330(6) . ? F27 C43 1.332(7) . ? F28 C56 1.326(5) . ? F29 C56 1.348(6) . ? F30 C56 1.346(5) . ? F31 C57 1.297(8) . ? F32 C57 1.285(7) . ? F33 C57 1.283(8) . ? F34 C58 1.365(8) . ? F35 C58 1.294(6) . ? F36 C58 1.281(6) . ? N1 C1 1.351(5) . ? N1 C5 1.359(5) . ? N15 C19 1.350(5) . ? N15 C15 1.355(5) . ? C1 C2 1.383(5) . ? C2 C3 1.386(6) . ? C3 C4 1.382(6) . ? C3 C12 1.503(6) . ? C4 C5 1.393(5) . ? C5 C6 1.480(6) . ? C6 C7 1.391(6) . ? C6 C11 1.418(5) . ? C7 C8 1.388(7) . ? C8 C9 1.372(7) . ? C8 C13 1.491(8) . ? C9 C10 1.384(6) . ? C10 C11 1.426(6) . ? C10 C14 1.508(6) . ? C15 C16 1.380(6) . ? C16 C17 1.385(6) . ? C17 C18 1.370(6) . ? C17 C26 1.508(6) . ? C18 C19 1.390(6) . ? C19 C20 1.467(6) . ? C20 C21 1.398(6) . ? C20 C25 1.431(5) . ? C21 C22 1.372(7) . ? C22 C23 1.377(7) . ? C22 C27 1.488(8) . ? C23 C24 1.390(6) . ? C24 C25 1.412(5) . ? C24 C28 1.500(6) . ? N29 C30 1.370(5) . ? N29 C34 1.391(5) . ? N29 C44 1.450(4) . ? C30 C31 1.423(5) . ? C31 C32 1.359(6) . ? C32 C33 1.407(5) . ? C32 C41 1.502(5) . ? C33 C34 1.374(5) . ? C34 C35 1.492(5) . ? C35 C40 1.389(6) . ? C35 C36 1.397(6) . ? C36 C37 1.395(6) . ? C37 C38 1.384(7) . ? C37 C42 1.500(8) . ? C38 C39 1.380(7) . ? C39 C40 1.392(6) . ? C39 C43 1.513(7) . ? C44 N49 1.312(5) . ? C44 C45 1.431(5) . ? C45 C46 1.411(5) . ? C46 C47 1.399(5) . ? C46 C56 1.515(6) . ? C47 C48 1.383(6) . ? C48 N49 1.347(5) . ? C48 C50 1.484(5) . ? C50 C55 1.381(6) . ? C50 C51 1.390(6) . ? C51 C52 1.405(6) . ? C52 C53 1.375(7) . ? C52 C57 1.490(7) . ? C53 C54 1.396(7) . ? C54 C55 1.396(6) . ? C54 C58 1.497(7) . ? C63 C62 1.17(3) . ? C63 C64 1.29(2) . ? C65 C64 1.24(2) . ? C61 C62 1.30(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Ir1 C45 80.28(14) . . ? C30 Ir1 C25 105.67(15) . . ? C45 Ir1 C25 85.82(15) . . ? C30 Ir1 N15 175.26(13) . . ? C45 Ir1 N15 101.69(13) . . ? C25 Ir1 N15 78.85(13) . . ? C30 Ir1 N1 93.93(13) . . ? C45 Ir1 N1 172.59(12) . . ? C25 Ir1 N1 91.34(13) . . ? N15 Ir1 N1 84.44(11) . . ? C30 Ir1 C11 82.05(15) . . ? C45 Ir1 C11 105.06(15) . . ? C25 Ir1 C11 167.77(14) . . ? N15 Ir1 C11 93.26(13) . . ? N1 Ir1 C11 78.51(13) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Ir1 123.9(3) . . ? C5 N1 Ir1 116.8(2) . . ? C19 N15 C15 119.1(3) . . ? C19 N15 Ir1 116.8(2) . . ? C15 N15 Ir1 124.1(3) . . ? N1 C1 C2 122.4(4) . . ? C1 C2 C3 118.5(4) . . ? C4 C3 C2 119.5(4) . . ? C4 C3 C12 120.2(4) . . ? C2 C3 C12 120.3(4) . . ? C3 C4 C5 119.8(4) . . ? N1 C5 C4 120.4(4) . . ? N1 C5 C6 114.4(3) . . ? C4 C5 C6 125.2(4) . . ? C7 C6 C11 123.7(4) . . ? C7 C6 C5 118.9(4) . . ? C11 C6 C5 117.4(4) . . ? C8 C7 C6 119.7(4) . . ? C9 C8 C7 119.0(4) . . ? C9 C8 C13 120.2(5) . . ? C7 C8 C13 120.7(5) . . ? C8 C9 C10 121.1(4) . . ? C9 C10 C11 122.8(4) . . ? C9 C10 C14 116.3(4) . . ? C11 C10 C14 120.9(4) . . ? C6 C11 C10 113.4(4) . . ? C6 C11 Ir1 112.3(3) . . ? C10 C11 Ir1 134.2(3) . . ? F3 C12 F1 110.3(5) . . ? F3 C12 F2 106.1(5) . . ? F1 C12 F2 103.6(4) . . ? F3 C12 C3 112.1(4) . . ? F1 C12 C3 112.1(4) . . ? F2 C12 C3 112.1(4) . . ? F5 C13 F4 112.6(9) . . ? F5 C13 F6 104.9(8) . . ? F4 C13 F6 97.8(7) . . ? F5 C13 C8 115.1(6) . . ? F4 C13 C8 115.5(7) . . ? F6 C13 C8 108.9(8) . . ? F9 C14 F7 106.4(4) . . ? F9 C14 F8 107.0(4) . . ? F7 C14 F8 105.4(4) . . ? F9 C14 C10 114.0(4) . . ? F7 C14 C10 111.7(4) . . ? F8 C14 C10 111.8(4) . . ? N15 C15 C16 122.4(4) . . ? C15 C16 C17 118.0(4) . . ? C18 C17 C16 120.0(4) . . ? C18 C17 C26 120.2(4) . . ? C16 C17 C26 119.8(4) . . ? C17 C18 C19 119.8(4) . . ? N15 C19 C18 120.6(4) . . ? N15 C19 C20 114.5(3) . . ? C18 C19 C20 124.8(4) . . ? C21 C20 C25 122.6(4) . . ? C21 C20 C19 119.7(4) . . ? C25 C20 C19 117.8(4) . . ? C22 C21 C20 119.9(4) . . ? C21 C22 C23 119.8(4) . . ? C21 C22 C27 120.1(6) . . ? C23 C22 C27 120.0(5) . . ? C22 C23 C24 120.7(4) . . ? C23 C24 C25 122.6(4) . . ? C23 C24 C28 115.7(4) . . ? C25 C24 C28 121.7(4) . . ? C24 C25 C20 114.3(4) . . ? C24 C25 Ir1 133.5(3) . . ? C20 C25 Ir1 112.1(3) . . ? F11 C26 F10 105.4(5) . . ? F11 C26 F12 109.8(5) . . ? F10 C26 F12 105.6(5) . . ? F11 C26 C17 113.0(4) . . ? F10 C26 C17 112.2(5) . . ? F12 C26 C17 110.4(4) . . ? F14 C27 F15 114.8(9) . . ? F14 C27 F13 95.2(10) . . ? F15 C27 F13 97.4(9) . . ? F14 C27 C22 118.3(7) . . ? F15 C27 C22 118.1(8) . . ? F13 C27 C22 106.8(9) . . ? F17 C28 F18 106.9(4) . . ? F17 C28 F16 105.8(3) . . ? F18 C28 F16 105.2(4) . . ? F17 C28 C24 113.8(4) . . ? F18 C28 C24 111.9(3) . . ? F16 C28 C24 112.8(4) . . ? C30 N29 C34 124.2(3) . . ? C30 N29 C44 112.5(3) . . ? C34 N29 C44 123.3(3) . . ? N29 C30 C31 115.4(3) . . ? N29 C30 Ir1 118.4(2) . . ? C31 C30 Ir1 125.7(3) . . ? C32 C31 C30 122.0(4) . . ? C31 C32 C33 120.1(3) . . ? C31 C32 C41 121.1(4) . . ? C33 C32 C41 118.8(4) . . ? C34 C33 C32 119.6(4) . . ? C33 C34 N29 118.6(3) . . ? C33 C34 C35 117.8(3) . . ? N29 C34 C35 123.4(3) . . ? C40 C35 C36 119.4(4) . . ? C40 C35 C34 119.0(3) . . ? C36 C35 C34 121.0(4) . . ? C37 C36 C35 119.2(4) . . ? C38 C37 C36 121.5(4) . . ? C38 C37 C42 120.8(5) . . ? C36 C37 C42 117.6(5) . . ? C39 C38 C37 118.7(4) . . ? C38 C39 C40 120.9(4) . . ? C38 C39 C43 120.7(4) . . ? C40 C39 C43 118.4(4) . . ? C35 C40 C39 120.2(4) . . ? F19 C41 F20 107.6(4) . . ? F19 C41 F21 107.6(4) . . ? F20 C41 F21 105.5(4) . . ? F19 C41 C32 111.9(4) . . ? F20 C41 C32 112.5(4) . . ? F21 C41 C32 111.4(4) . . ? F22 C42 F23 112.3(7) . . ? F22 C42 F24 103.8(7) . . ? F23 C42 F24 101.6(5) . . ? F22 C42 C37 115.0(5) . . ? F23 C42 C37 112.4(6) . . ? F24 C42 C37 110.5(6) . . ? F26 C43 F27 107.1(5) . . ? F26 C43 F25 107.1(5) . . ? F27 C43 F25 106.3(5) . . ? F26 C43 C39 112.1(5) . . ? F27 C43 C39 113.0(4) . . ? F25 C43 C39 110.9(5) . . ? N49 C44 C45 129.4(3) . . ? N49 C44 N29 115.6(3) . . ? C45 C44 N29 115.0(3) . . ? C46 C45 C44 110.1(3) . . ? C46 C45 Ir1 137.6(3) . . ? C44 C45 Ir1 111.7(2) . . ? C47 C46 C45 121.8(4) . . ? C47 C46 C56 113.5(3) . . ? C45 C46 C56 124.6(3) . . ? C48 C47 C46 120.6(4) . . ? N49 C48 C47 120.1(3) . . ? N49 C48 C50 116.0(3) . . ? C47 C48 C50 123.9(3) . . ? C44 N49 C48 117.5(3) . . ? C55 C50 C51 119.0(4) . . ? C55 C50 C48 119.8(4) . . ? C51 C50 C48 121.2(4) . . ? C50 C51 C52 120.4(4) . . ? C53 C52 C51 120.5(4) . . ? C53 C52 C57 119.8(4) . . ? C51 C52 C57 119.7(5) . . ? C52 C53 C54 119.1(4) . . ? C53 C54 C55 120.4(4) . . ? C53 C54 C58 120.6(4) . . ? C55 C54 C58 119.0(4) . . ? C50 C55 C54 120.6(4) . . ? F28 C56 F30 105.3(4) . . ? F28 C56 F29 107.1(4) . . ? F30 C56 F29 106.0(4) . . ? F28 C56 C46 114.9(4) . . ? F30 C56 C46 111.5(3) . . ? F29 C56 C46 111.5(4) . . ? F33 C57 F32 107.0(6) . . ? F33 C57 F31 104.7(6) . . ? F32 C57 F31 103.8(6) . . ? F33 C57 C52 112.9(5) . . ? F32 C57 C52 113.7(5) . . ? F31 C57 C52 113.9(5) . . ? F36 C58 F35 112.7(5) . . ? F36 C58 F34 102.4(6) . . ? F35 C58 F34 101.9(5) . . ? F36 C58 C54 114.7(5) . . ? F35 C58 C54 113.8(5) . . ? F34 C58 C54 110.0(5) . . ? C62 C63 C64 154(3) . . ? C65 C64 C63 158(3) . . ? C63 C62 C61 139(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 Ir1 N1 C1 102.4(3) . . . . ? C45 Ir1 N1 C1 64.0(11) . . . . ? C25 Ir1 N1 C1 -3.4(3) . . . . ? N15 Ir1 N1 C1 -82.1(3) . . . . ? C11 Ir1 N1 C1 -176.5(3) . . . . ? C30 Ir1 N1 C5 -77.3(3) . . . . ? C45 Ir1 N1 C5 -115.7(10) . . . . ? C25 Ir1 N1 C5 176.9(3) . . . . ? N15 Ir1 N1 C5 98.3(3) . . . . ? C11 Ir1 N1 C5 3.8(3) . . . . ? C30 Ir1 N15 C19 163.0(15) . . . . ? C45 Ir1 N15 C19 -82.9(3) . . . . ? C25 Ir1 N15 C19 0.4(3) . . . . ? N1 Ir1 N15 C19 92.9(3) . . . . ? C11 Ir1 N15 C19 171.0(3) . . . . ? C30 Ir1 N15 C15 -15.9(17) . . . . ? C45 Ir1 N15 C15 98.3(3) . . . . ? C25 Ir1 N15 C15 -178.4(3) . . . . ? N1 Ir1 N15 C15 -85.9(3) . . . . ? C11 Ir1 N15 C15 -7.8(3) . . . . ? C5 N1 C1 C2 0.1(6) . . . . ? Ir1 N1 C1 C2 -179.6(3) . . . . ? N1 C1 C2 C3 -0.2(6) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C1 C2 C3 C12 178.3(4) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C12 C3 C4 C5 -178.2(4) . . . . ? C1 N1 C5 C4 0.0(6) . . . . ? Ir1 N1 C5 C4 179.7(3) . . . . ? C1 N1 C5 C6 -179.9(3) . . . . ? Ir1 N1 C5 C6 -0.2(4) . . . . ? C3 C4 C5 N1 0.0(6) . . . . ? C3 C4 C5 C6 180.0(4) . . . . ? N1 C5 C6 C7 174.6(4) . . . . ? C4 C5 C6 C7 -5.3(7) . . . . ? N1 C5 C6 C11 -5.9(5) . . . . ? C4 C5 C6 C11 174.2(4) . . . . ? C11 C6 C7 C8 -1.6(8) . . . . ? C5 C6 C7 C8 177.9(5) . . . . ? C6 C7 C8 C9 -3.6(9) . . . . ? C6 C7 C8 C13 179.7(6) . . . . ? C7 C8 C9 C10 4.7(9) . . . . ? C13 C8 C9 C10 -178.6(6) . . . . ? C8 C9 C10 C11 -0.6(8) . . . . ? C8 C9 C10 C14 -179.7(5) . . . . ? C7 C6 C11 C10 5.2(6) . . . . ? C5 C6 C11 C10 -174.2(4) . . . . ? C7 C6 C11 Ir1 -171.7(4) . . . . ? C5 C6 C11 Ir1 8.9(5) . . . . ? C9 C10 C11 C6 -4.1(6) . . . . ? C14 C10 C11 C6 174.9(4) . . . . ? C9 C10 C11 Ir1 171.9(4) . . . . ? C14 C10 C11 Ir1 -9.1(6) . . . . ? C30 Ir1 C11 C6 89.0(3) . . . . ? C45 Ir1 C11 C6 166.7(3) . . . . ? C25 Ir1 C11 C6 -41.0(8) . . . . ? N15 Ir1 C11 C6 -90.3(3) . . . . ? N1 Ir1 C11 C6 -6.6(3) . . . . ? C30 Ir1 C11 C10 -87.0(4) . . . . ? C45 Ir1 C11 C10 -9.4(4) . . . . ? C25 Ir1 C11 C10 143.0(6) . . . . ? N15 Ir1 C11 C10 93.7(4) . . . . ? N1 Ir1 C11 C10 177.3(4) . . . . ? C4 C3 C12 F3 84.3(6) . . . . ? C2 C3 C12 F3 -93.6(6) . . . . ? C4 C3 C12 F1 -150.9(5) . . . . ? C2 C3 C12 F1 31.1(7) . . . . ? C4 C3 C12 F2 -34.9(6) . . . . ? C2 C3 C12 F2 147.1(4) . . . . ? C9 C8 C13 F5 162.2(8) . . . . ? C7 C8 C13 F5 -21.1(13) . . . . ? C9 C8 C13 F4 -63.9(12) . . . . ? C7 C8 C13 F4 112.7(9) . . . . ? C9 C8 C13 F6 44.8(10) . . . . ? C7 C8 C13 F6 -138.5(7) . . . . ? C9 C10 C14 F9 130.4(4) . . . . ? C11 C10 C14 F9 -48.6(5) . . . . ? C9 C10 C14 F7 9.8(6) . . . . ? C11 C10 C14 F7 -169.3(4) . . . . ? C9 C10 C14 F8 -108.1(5) . . . . ? C11 C10 C14 F8 72.9(5) . . . . ? C19 N15 C15 C16 2.8(5) . . . . ? Ir1 N15 C15 C16 -178.4(3) . . . . ? N15 C15 C16 C17 -0.6(6) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C15 C16 C17 C26 176.0(4) . . . . ? C16 C17 C18 C19 1.6(6) . . . . ? C26 C17 C18 C19 -176.0(4) . . . . ? C15 N15 C19 C18 -2.8(5) . . . . ? Ir1 N15 C19 C18 178.3(3) . . . . ? C15 N15 C19 C20 178.8(3) . . . . ? Ir1 N15 C19 C20 -0.1(4) . . . . ? C17 C18 C19 N15 0.6(6) . . . . ? C17 C18 C19 C20 178.8(4) . . . . ? N15 C19 C20 C21 179.3(4) . . . . ? C18 C19 C20 C21 1.0(7) . . . . ? N15 C19 C20 C25 -0.5(5) . . . . ? C18 C19 C20 C25 -178.8(4) . . . . ? C25 C20 C21 C22 -1.3(8) . . . . ? C19 C20 C21 C22 178.9(5) . . . . ? C20 C21 C22 C23 -1.1(9) . . . . ? C20 C21 C22 C27 176.2(7) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C27 C22 C23 C24 -176.5(7) . . . . ? C22 C23 C24 C25 2.1(7) . . . . ? C22 C23 C24 C28 -175.9(5) . . . . ? C23 C24 C25 C20 -4.2(6) . . . . ? C28 C24 C25 C20 173.6(4) . . . . ? C23 C24 C25 Ir1 179.4(3) . . . . ? C28 C24 C25 Ir1 -2.8(6) . . . . ? C21 C20 C25 C24 3.8(6) . . . . ? C19 C20 C25 C24 -176.3(3) . . . . ? C21 C20 C25 Ir1 -179.0(4) . . . . ? C19 C20 C25 Ir1 0.8(4) . . . . ? C30 Ir1 C25 C24 -2.7(4) . . . . ? C45 Ir1 C25 C24 -81.4(4) . . . . ? N15 Ir1 C25 C24 175.8(4) . . . . ? N1 Ir1 C25 C24 91.8(4) . . . . ? C11 Ir1 C25 C24 125.3(6) . . . . ? C30 Ir1 C25 C20 -179.2(3) . . . . ? C45 Ir1 C25 C20 102.1(3) . . . . ? N15 Ir1 C25 C20 -0.6(3) . . . . ? N1 Ir1 C25 C20 -84.7(3) . . . . ? C11 Ir1 C25 C20 -51.1(8) . . . . ? C18 C17 C26 F11 -23.7(7) . . . . ? C16 C17 C26 F11 158.7(5) . . . . ? C18 C17 C26 F10 -142.8(5) . . . . ? C16 C17 C26 F10 39.6(6) . . . . ? C18 C17 C26 F12 99.7(6) . . . . ? C16 C17 C26 F12 -77.9(6) . . . . ? C21 C22 C27 F14 -15.7(16) . . . . ? C23 C22 C27 F14 161.6(10) . . . . ? C21 C22 C27 F15 -161.6(10) . . . . ? C23 C22 C27 F15 15.7(15) . . . . ? C21 C22 C27 F13 90.0(11) . . . . ? C23 C22 C27 F13 -92.7(11) . . . . ? C23 C24 C28 F17 -115.7(4) . . . . ? C25 C24 C28 F17 66.3(5) . . . . ? C23 C24 C28 F18 123.1(4) . . . . ? C25 C24 C28 F18 -54.9(5) . . . . ? C23 C24 C28 F16 4.7(6) . . . . ? C25 C24 C28 F16 -173.2(4) . . . . ? C34 N29 C30 C31 4.0(5) . . . . ? C44 N29 C30 C31 -174.5(3) . . . . ? C34 N29 C30 Ir1 -168.5(3) . . . . ? C44 N29 C30 Ir1 13.0(4) . . . . ? C45 Ir1 C30 N29 -4.9(3) . . . . ? C25 Ir1 C30 N29 -87.8(3) . . . . ? N15 Ir1 C30 N29 110.0(15) . . . . ? N1 Ir1 C30 N29 179.7(3) . . . . ? C11 Ir1 C30 N29 101.9(3) . . . . ? C45 Ir1 C30 C31 -176.6(4) . . . . ? C25 Ir1 C30 C31 100.6(3) . . . . ? N15 Ir1 C30 C31 -61.7(17) . . . . ? N1 Ir1 C30 C31 8.1(3) . . . . ? C11 Ir1 C30 C31 -69.7(3) . . . . ? N29 C30 C31 C32 -0.5(6) . . . . ? Ir1 C30 C31 C32 171.4(3) . . . . ? C30 C31 C32 C33 -1.9(6) . . . . ? C30 C31 C32 C41 -179.7(4) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? C41 C32 C33 C34 178.9(4) . . . . ? C32 C33 C34 N29 2.2(6) . . . . ? C32 C33 C34 C35 -171.8(3) . . . . ? C30 N29 C34 C33 -4.9(5) . . . . ? C44 N29 C34 C33 173.5(3) . . . . ? C30 N29 C34 C35 168.7(3) . . . . ? C44 N29 C34 C35 -13.0(5) . . . . ? C33 C34 C35 C40 -48.4(5) . . . . ? N29 C34 C35 C40 137.9(4) . . . . ? C33 C34 C35 C36 122.2(4) . . . . ? N29 C34 C35 C36 -51.4(5) . . . . ? C40 C35 C36 C37 -2.4(6) . . . . ? C34 C35 C36 C37 -172.9(4) . . . . ? C35 C36 C37 C38 2.1(8) . . . . ? C35 C36 C37 C42 -176.1(5) . . . . ? C36 C37 C38 C39 -0.5(8) . . . . ? C42 C37 C38 C39 177.6(6) . . . . ? C37 C38 C39 C40 -0.8(8) . . . . ? C37 C38 C39 C43 178.2(5) . . . . ? C36 C35 C40 C39 1.1(6) . . . . ? C34 C35 C40 C39 171.9(4) . . . . ? C38 C39 C40 C35 0.5(7) . . . . ? C43 C39 C40 C35 -178.5(5) . . . . ? C31 C32 C41 F19 21.7(6) . . . . ? C33 C32 C41 F19 -156.1(4) . . . . ? C31 C32 C41 F20 142.9(4) . . . . ? C33 C32 C41 F20 -34.9(6) . . . . ? C31 C32 C41 F21 -98.8(5) . . . . ? C33 C32 C41 F21 83.3(5) . . . . ? C38 C37 C42 F22 162.7(7) . . . . ? C36 C37 C42 F22 -19.1(10) . . . . ? C38 C37 C42 F23 32.5(10) . . . . ? C36 C37 C42 F23 -149.3(6) . . . . ? C38 C37 C42 F24 -80.2(8) . . . . ? C36 C37 C42 F24 98.0(6) . . . . ? C38 C39 C43 F26 26.4(8) . . . . ? C40 C39 C43 F26 -154.7(5) . . . . ? C38 C39 C43 F27 147.5(5) . . . . ? C40 C39 C43 F27 -33.5(7) . . . . ? C38 C39 C43 F25 -93.2(6) . . . . ? C40 C39 C43 F25 85.7(6) . . . . ? C30 N29 C44 N49 161.0(3) . . . . ? C34 N29 C44 N49 -17.6(5) . . . . ? C30 N29 C44 C45 -16.4(5) . . . . ? C34 N29 C44 C45 165.0(3) . . . . ? N49 C44 C45 C46 8.7(6) . . . . ? N29 C44 C45 C46 -174.4(3) . . . . ? N49 C44 C45 Ir1 -164.5(3) . . . . ? N29 C44 C45 Ir1 12.5(4) . . . . ? C30 Ir1 C45 C46 -174.8(5) . . . . ? C25 Ir1 C45 C46 -68.1(4) . . . . ? N15 Ir1 C45 C46 9.6(5) . . . . ? N1 Ir1 C45 C46 -135.8(9) . . . . ? C11 Ir1 C45 C46 106.2(4) . . . . ? C30 Ir1 C45 C44 -4.3(3) . . . . ? C25 Ir1 C45 C44 102.4(3) . . . . ? N15 Ir1 C45 C44 -179.9(3) . . . . ? N1 Ir1 C45 C44 34.6(11) . . . . ? C11 Ir1 C45 C44 -83.3(3) . . . . ? C44 C45 C46 C47 -3.7(6) . . . . ? Ir1 C45 C46 C47 166.8(3) . . . . ? C44 C45 C46 C56 -178.7(4) . . . . ? Ir1 C45 C46 C56 -8.1(7) . . . . ? C45 C46 C47 C48 -1.3(7) . . . . ? C56 C46 C47 C48 174.1(4) . . . . ? C46 C47 C48 N49 3.1(6) . . . . ? C46 C47 C48 C50 -176.1(4) . . . . ? C45 C44 N49 C48 -7.5(6) . . . . ? N29 C44 N49 C48 175.6(3) . . . . ? C47 C48 N49 C44 0.9(6) . . . . ? C50 C48 N49 C44 -179.8(4) . . . . ? N49 C48 C50 C55 -26.4(6) . . . . ? C47 C48 C50 C55 152.9(4) . . . . ? N49 C48 C50 C51 153.1(4) . . . . ? C47 C48 C50 C51 -27.7(6) . . . . ? C55 C50 C51 C52 0.9(7) . . . . ? C48 C50 C51 C52 -178.6(4) . . . . ? C50 C51 C52 C53 -0.8(7) . . . . ? C50 C51 C52 C57 177.2(5) . . . . ? C51 C52 C53 C54 -0.6(8) . . . . ? C57 C52 C53 C54 -178.6(5) . . . . ? C52 C53 C54 C55 1.9(8) . . . . ? C52 C53 C54 C58 -175.8(5) . . . . ? C51 C50 C55 C54 0.4(7) . . . . ? C48 C50 C55 C54 179.8(4) . . . . ? C53 C54 C55 C50 -1.8(7) . . . . ? C58 C54 C55 C50 176.0(5) . . . . ? C47 C46 C56 F28 143.7(4) . . . . ? C45 C46 C56 F28 -41.0(6) . . . . ? C47 C46 C56 F30 24.0(6) . . . . ? C45 C46 C56 F30 -160.7(4) . . . . ? C47 C46 C56 F29 -94.2(4) . . . . ? C45 C46 C56 F29 81.1(5) . . . . ? C53 C52 C57 F33 91.0(7) . . . . ? C51 C52 C57 F33 -87.0(7) . . . . ? C53 C52 C57 F32 -31.1(9) . . . . ? C51 C52 C57 F32 150.9(6) . . . . ? C53 C52 C57 F31 -149.8(6) . . . . ? C51 C52 C57 F31 32.2(8) . . . . ? C53 C54 C58 F36 -144.5(6) . . . . ? C55 C54 C58 F36 37.8(8) . . . . ? C53 C54 C58 F35 -12.8(9) . . . . ? C55 C54 C58 F35 169.5(5) . . . . ? C53 C54 C58 F34 100.8(6) . . . . ? C55 C54 C58 F34 -76.9(6) . . . . ? C62 C63 C64 C65 -172(7) . . . . ? C64 C63 C62 C61 175(5) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 2.819 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.114 #===END #===END data_03328 _database_code_depnum_ccdc_archive 'CCDC 257683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H10 F18 N2' _chemical_formula_weight 716.38 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4708(12) _cell_length_b 11.8225(14) _cell_length_c 12.6383(15) _cell_angle_alpha 104.597(2) _cell_angle_beta 105.654(2) _cell_angle_gamma 105.656(2) _cell_volume 1358.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description iregblok _exptl_crystal_colour colorless _exptl_crystal_size_max .50 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .35 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9024 _diffrn_reflns_av_R_equivalents 0.0125 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6203 _reflns_number_gt 4784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.8063P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6203 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.007 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 F1 F 0.3238(3) 0.72741(17) 0.7728(3) 0.1043(12) Uani 0.874(3) 1 d P . . F2 F 0.1573(4) 0.6348(2) 0.60734(17) 0.0859(9) Uani 0.874(3) 1 d P . . F3 F 0.1143(5) 0.6481(3) 0.7622(4) 0.0998(10) Uani 0.874(3) 1 d P . . F1' F 0.0847(19) 0.6187(13) 0.653(3) 0.1043(12) Uani 0.126(3) 1 d P . . F2' F 0.233(4) 0.6958(18) 0.7968(14) 0.0859(9) Uani 0.126(3) 1 d P . . F3' F 0.303(3) 0.6891(19) 0.669(3) 0.0998(10) Uani 0.126(3) 1 d P . . F4 F -0.35982(16) 0.00637(17) 0.29552(12) 0.0652(4) Uani 1 1 d . . . F5 F -0.41910(15) 0.11669(14) 0.42145(14) 0.0585(4) Uani 1 1 d . . . F6 F -0.48754(14) -0.08212(14) 0.37928(14) 0.0624(4) Uani 1 1 d . . . F7 F -0.1785(6) -0.1599(4) 0.7282(4) 0.1213(15) Uani 0.812(3) 1 d P . . F8 F -0.1263(4) -0.2488(2) 0.59222(18) 0.0708(7) Uani 0.812(3) 1 d P . . F9 F 0.0363(4) -0.1148(3) 0.7428(5) 0.1317(19) Uani 0.812(3) 1 d P . . F7' F -0.018(3) -0.1866(19) 0.648(2) 0.1213(15) Uani 0.188(3) 1 d P . . F8' F -0.0342(19) -0.0874(9) 0.7835(9) 0.0708(7) Uani 0.188(3) 1 d P . . F9' F -0.2117(17) -0.2104(14) 0.6653(19) 0.1317(19) Uani 0.188(3) 1 d P . . F10 F 0.14867(17) -0.02180(15) 1.02948(18) 0.0694(5) Uani 1 1 d . . . F11 F 0.3053(2) -0.06229(15) 0.96589(18) 0.0783(6) Uani 1 1 d . . . F12 F 0.3629(2) 0.04513(18) 1.14506(17) 0.0878(6) Uani 1 1 d . . . F13 F 0.8900(2) 0.19733(18) 0.84040(17) 0.0761(5) Uani 1 1 d . . . F14 F 0.94450(15) 0.32122(17) 1.01245(14) 0.0621(4) Uani 1 1 d . . . F15 F 1.00579(16) 0.3909(2) 0.88527(19) 0.0814(6) Uani 1 1 d . . . F16 F 0.67504(18) 0.43039(18) 0.57451(14) 0.0684(5) Uani 1 1 d . . . F17 F 0.60168(19) 0.56312(14) 0.66450(14) 0.0658(4) Uani 1 1 d . . . F18 F 0.45405(16) 0.38002(16) 0.54912(12) 0.0633(4) Uani 1 1 d . . . N1 N 0.25258(16) 0.27830(14) 0.69670(13) 0.0297(3) Uani 1 1 d . . . N16 N 0.36612(16) 0.36557(14) 0.96021(14) 0.0301(3) Uani 1 1 d . . . C2 C 0.36635(19) 0.38378(17) 0.74031(15) 0.0299(4) Uani 1 1 d . . . C3 C 0.3579(2) 0.50112(18) 0.74818(17) 0.0353(4) Uani 1 1 d . . . H3A H 0.4394 0.5732 0.7805 0.042 Uiso 1 1 calc R . . C4 C 0.2246(2) 0.50663(18) 0.70637(17) 0.0359(4) Uani 1 1 d . . . C5 C 0.1051(2) 0.39838(18) 0.66035(17) 0.0339(4) Uani 1 1 d . . . H5A H 0.0146 0.4010 0.6319 0.041 Uiso 1 1 calc R . . C6 C 0.1231(2) 0.28503(17) 0.65752(15) 0.0301(4) Uani 1 1 d . . . C7 C -0.00023(19) 0.16629(17) 0.61372(16) 0.0302(4) Uani 1 1 d . . . C8 C -0.1289(2) 0.14723(18) 0.53016(16) 0.0324(4) Uani 1 1 d . . . H8A H -0.1379 0.2093 0.4990 0.039 Uiso 1 1 calc R . . C9 C -0.2444(2) 0.03608(19) 0.49277(17) 0.0341(4) Uani 1 1 d . . . C10 C -0.2343(2) -0.05702(19) 0.53856(17) 0.0366(4) Uani 1 1 d . . . H10A H -0.3121 -0.1308 0.5142 0.044 Uiso 1 1 calc R . . C11 C -0.1051(2) -0.03807(18) 0.62200(17) 0.0352(4) Uani 1 1 d . . . C12 C 0.0112(2) 0.07106(18) 0.65860(16) 0.0318(4) Uani 1 1 d . . . H12A H 0.0972 0.0813 0.7131 0.038 Uiso 1 1 calc R . . C13 C 0.2066(3) 0.6295(2) 0.7108(2) 0.0455(5) Uani 1 1 d . . . C14 C -0.3778(2) 0.0188(2) 0.39779(19) 0.0422(5) Uani 1 1 d . . . C15 C -0.0935(3) -0.1382(2) 0.6733(2) 0.0447(5) Uani 1 1 d . . . C17 C 0.2746(2) 0.33553(18) 1.01365(17) 0.0330(4) Uani 1 1 d . . . H17A H 0.2300 0.3911 1.0346 0.040 Uiso 1 1 calc R . . C18 C 0.2420(2) 0.22640(19) 1.03978(18) 0.0357(4) Uani 1 1 d . . . H18A H 0.1764 0.2085 1.0760 0.043 Uiso 1 1 calc R . . C19 C 0.3106(2) 0.14510(18) 1.01002(17) 0.0331(4) Uani 1 1 d . . . C20 C 0.40697(19) 0.17444(18) 0.95561(16) 0.0307(4) Uani 1 1 d . . . H20A H 0.4542 0.1211 0.9351 0.037 Uiso 1 1 calc R . . C21 C 0.43147(18) 0.28590(17) 0.93225(15) 0.0276(4) Uani 1 1 d . . . C22 C 0.53550(19) 0.32022(16) 0.87450(16) 0.0284(4) Uani 1 1 d . . . C23 C 0.6643(2) 0.30361(17) 0.91302(17) 0.0318(4) Uani 1 1 d . . . H23A H 0.6838 0.2727 0.9739 0.038 Uiso 1 1 calc R . . C24 C 0.7641(2) 0.33270(19) 0.86150(18) 0.0357(4) Uani 1 1 d . . . C25 C 0.7364(2) 0.37743(19) 0.77033(18) 0.0377(4) Uani 1 1 d . . . H25A H 0.8031 0.3958 0.7353 0.045 Uiso 1 1 calc R . . C26 C 0.6083(2) 0.39491(19) 0.73108(17) 0.0354(4) Uani 1 1 d . . . C27 C 0.50674(19) 0.36834(16) 0.78285(16) 0.0296(4) Uani 1 1 d . . . C28 C 0.2813(2) 0.0265(2) 1.0377(2) 0.0443(5) Uani 1 1 d . . . C29 C 0.9011(2) 0.3113(2) 0.9009(2) 0.0462(5) Uani 1 1 d . . . C30 C 0.5841(3) 0.4416(2) 0.6296(2) 0.0470(5) 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 F1 0.0701(14) 0.0269(9) 0.156(3) 0.0141(12) -0.0262(16) 0.0123(9) F2 0.155(3) 0.0590(12) 0.0529(11) 0.0337(9) 0.0168(13) 0.0598(15) F3 0.148(3) 0.0731(15) 0.153(3) 0.0630(17) 0.105(2) 0.0798(18) F1' 0.0701(14) 0.0269(9) 0.156(3) 0.0141(12) -0.0262(16) 0.0123(9) F2' 0.155(3) 0.0590(12) 0.0529(11) 0.0337(9) 0.0168(13) 0.0598(15) F3' 0.148(3) 0.0731(15) 0.153(3) 0.0630(17) 0.105(2) 0.0798(18) F4 0.0530(8) 0.0973(12) 0.0351(7) 0.0195(7) 0.0057(6) 0.0256(8) F5 0.0432(7) 0.0558(8) 0.0654(9) 0.0144(7) 0.0027(6) 0.0246(7) F6 0.0363(7) 0.0544(9) 0.0696(10) 0.0179(7) -0.0016(6) 0.0005(6) F7 0.235(4) 0.108(2) 0.156(3) 0.106(2) 0.167(3) 0.113(3) F8 0.129(2) 0.0372(10) 0.0525(11) 0.0210(8) 0.0309(13) 0.0366(13) F9 0.093(2) 0.0667(17) 0.160(3) 0.075(2) -0.059(2) -0.0106(15) F7' 0.235(4) 0.108(2) 0.156(3) 0.106(2) 0.167(3) 0.113(3) F8' 0.129(2) 0.0372(10) 0.0525(11) 0.0210(8) 0.0309(13) 0.0366(13) F9' 0.093(2) 0.0667(17) 0.160(3) 0.075(2) -0.059(2) -0.0106(15) F10 0.0564(9) 0.0604(9) 0.1131(14) 0.0539(10) 0.0433(9) 0.0193(7) F11 0.1211(15) 0.0520(9) 0.1142(15) 0.0519(10) 0.0807(13) 0.0504(10) F12 0.0922(13) 0.0839(12) 0.0767(12) 0.0598(10) 0.0015(10) 0.0158(10) F13 0.0877(12) 0.0860(12) 0.0926(13) 0.0381(10) 0.0489(10) 0.0658(11) F14 0.0428(7) 0.1006(12) 0.0633(9) 0.0433(9) 0.0214(7) 0.0411(8) F15 0.0406(8) 0.1172(15) 0.1327(16) 0.0917(14) 0.0463(9) 0.0387(9) F16 0.0726(10) 0.0971(12) 0.0572(9) 0.0464(9) 0.0372(8) 0.0316(9) F17 0.0876(11) 0.0540(9) 0.0639(9) 0.0388(8) 0.0269(8) 0.0214(8) F18 0.0584(9) 0.0816(11) 0.0412(7) 0.0334(7) 0.0068(6) 0.0123(8) N1 0.0312(8) 0.0297(8) 0.0269(7) 0.0120(6) 0.0066(6) 0.0111(6) N16 0.0258(7) 0.0301(8) 0.0323(8) 0.0103(6) 0.0074(6) 0.0108(6) C2 0.0309(9) 0.0309(9) 0.0259(8) 0.0129(7) 0.0064(7) 0.0096(7) C3 0.0367(10) 0.0291(9) 0.0343(10) 0.0135(8) 0.0051(8) 0.0088(8) C4 0.0428(11) 0.0305(9) 0.0321(9) 0.0128(8) 0.0064(8) 0.0151(8) C5 0.0339(9) 0.0354(10) 0.0317(9) 0.0137(8) 0.0063(8) 0.0154(8) C6 0.0336(9) 0.0307(9) 0.0249(8) 0.0109(7) 0.0078(7) 0.0116(7) C7 0.0321(9) 0.0308(9) 0.0280(9) 0.0106(7) 0.0102(7) 0.0124(7) C8 0.0335(9) 0.0333(9) 0.0315(9) 0.0125(8) 0.0109(8) 0.0132(8) C9 0.0319(9) 0.0374(10) 0.0303(9) 0.0091(8) 0.0100(8) 0.0123(8) C10 0.0351(10) 0.0348(10) 0.0343(10) 0.0086(8) 0.0126(8) 0.0072(8) C11 0.0437(11) 0.0327(10) 0.0304(9) 0.0119(8) 0.0147(8) 0.0133(8) C12 0.0359(9) 0.0332(9) 0.0270(9) 0.0114(7) 0.0103(7) 0.0139(8) C13 0.0491(12) 0.0338(11) 0.0474(13) 0.0152(10) 0.0048(10) 0.0174(10) C14 0.0340(10) 0.0420(11) 0.0412(11) 0.0100(9) 0.0071(9) 0.0105(9) C15 0.0562(13) 0.0354(11) 0.0393(11) 0.0163(9) 0.0147(10) 0.0117(10) C17 0.0282(9) 0.0357(10) 0.0360(10) 0.0109(8) 0.0111(8) 0.0150(8) C18 0.0311(9) 0.0433(11) 0.0388(10) 0.0178(9) 0.0166(8) 0.0155(8) C19 0.0322(9) 0.0352(10) 0.0354(10) 0.0174(8) 0.0120(8) 0.0132(8) C20 0.0319(9) 0.0336(9) 0.0318(9) 0.0144(7) 0.0119(7) 0.0164(8) C21 0.0245(8) 0.0310(9) 0.0261(8) 0.0116(7) 0.0058(7) 0.0102(7) C22 0.0292(9) 0.0267(8) 0.0298(9) 0.0114(7) 0.0101(7) 0.0101(7) C23 0.0314(9) 0.0335(9) 0.0352(9) 0.0167(8) 0.0131(8) 0.0134(8) C24 0.0320(9) 0.0377(10) 0.0426(11) 0.0162(8) 0.0170(8) 0.0150(8) C25 0.0370(10) 0.0396(11) 0.0405(11) 0.0170(9) 0.0194(9) 0.0119(8) C26 0.0381(10) 0.0346(10) 0.0317(9) 0.0142(8) 0.0113(8) 0.0093(8) C27 0.0295(9) 0.0264(8) 0.0298(9) 0.0105(7) 0.0072(7) 0.0080(7) C28 0.0477(12) 0.0488(12) 0.0532(13) 0.0315(11) 0.0256(10) 0.0226(10) C29 0.0402(11) 0.0601(14) 0.0613(14) 0.0360(12) 0.0299(11) 0.0276(11) C30 0.0493(13) 0.0512(13) 0.0415(12) 0.0234(10) 0.0160(10) 0.0136(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 F2' 1.08(3) . ? F1 F3' 1.21(2) . ? F1 C13 1.310(3) . ? F2 F1' 1.07(4) . ? F2 C13 1.294(3) . ? F2 F3' 1.39(3) . ? F3 F2' 1.12(3) . ? F3 F1' 1.27(3) . ? F3 C13 1.335(3) . ? F1' C13 1.242(15) . ? F2' C13 1.079(16) . ? F3' C13 1.374(17) . ? F4 C14 1.333(3) . ? F5 C14 1.335(3) . ? F6 C14 1.332(3) . ? F7 F9' 0.78(2) . ? F7 C15 1.281(3) . ? F7 F8' 1.392(15) . ? F8 F7' 1.09(3) . ? F8 C15 1.331(3) . ? F8 F9' 1.52(3) . ? F9 F7' 1.16(2) . ? F9 F8' 1.079(12) . ? F9 C15 1.314(3) . ? F7' C15 1.160(13) . ? F8' C15 1.263(11) . ? F9' C15 1.261(17) . ? F10 C28 1.315(3) . ? F11 C28 1.332(3) . ? F12 C28 1.319(3) . ? F13 C29 1.327(3) . ? F14 C29 1.323(3) . ? F15 C29 1.335(3) . ? F16 C30 1.338(3) . ? F17 C30 1.336(3) . ? F18 C30 1.328(3) . ? N1 C2 1.332(2) . ? N1 C6 1.344(2) . ? N16 C17 1.337(2) . ? N16 C21 1.338(2) . ? C2 C3 1.394(3) . ? C2 C27 1.500(3) . ? C3 C4 1.378(3) . ? C4 C5 1.382(3) . ? C4 C13 1.504(3) . ? C5 C6 1.396(3) . ? C6 C7 1.480(3) . ? C7 C8 1.389(3) . ? C7 C12 1.400(3) . ? C8 C9 1.391(3) . ? C9 C10 1.381(3) . ? C9 C14 1.500(3) . ? C10 C11 1.393(3) . ? C11 C12 1.382(3) . ? C11 C15 1.503(3) . ? C17 C18 1.389(3) . ? C18 C19 1.385(3) . ? C19 C20 1.384(3) . ? C19 C28 1.502(3) . ? C20 C21 1.394(2) . ? C21 C22 1.491(2) . ? C22 C23 1.390(3) . ? C22 C27 1.412(2) . ? C23 C24 1.385(3) . ? C24 C25 1.379(3) . ? C24 C29 1.498(3) . ? C25 C26 1.390(3) . ? C26 C27 1.398(3) . ? C26 C30 1.506(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2' F1 F3' 115.9(15) . . ? F2' F1 C13 52.6(10) . . ? F3' F1 C13 66.0(11) . . ? F1' F2 C13 62.4(11) . . ? F1' F2 F3' 120.5(14) . . ? C13 F2 F3' 61.4(8) . . ? F2' F3 F1' 101.7(13) . . ? F2' F3 C13 51.2(9) . . ? F1' F3 C13 57.0(10) . . ? F2 F1' C13 67.5(13) . . ? F2 F1' F3 127.7(14) . . ? C13 F1' F3 64.4(12) . . ? C13 F2' F1 74.9(16) . . ? C13 F2' F3 74.8(16) . . ? F1 F2' F3 144.5(16) . . ? F1 F3' C13 60.6(8) . . ? F1 F3' F2 108.4(12) . . ? C13 F3' F2 55.8(9) . . ? F9' F7 C15 70.7(17) . . ? F9' F7 F8' 123.6(19) . . ? C15 F7 F8' 56.2(4) . . ? F7' F8 C15 56.3(6) . . ? F7' F8 F9' 102.5(8) . . ? C15 F8 F9' 52.0(5) . . ? F7' F9 F8' 115.8(12) . . ? F7' F9 C15 55.5(10) . . ? F8' F9 C15 62.8(7) . . ? F9 F7' C15 69.1(8) . . ? F9 F7' F8 135.1(13) . . ? C15 F7' F8 72.6(14) . . ? F9 F8' C15 67.7(6) . . ? F9 F8' F7 116.9(8) . . ? C15 F8' F7 57.4(6) . . ? F7 F9' C15 73.5(10) . . ? F7 F9' F8 124.5(19) . . ? C15 F9' F8 56.2(11) . . ? C2 N1 C6 118.45(16) . . ? C17 N16 C21 117.48(16) . . ? N1 C2 C3 123.31(17) . . ? N1 C2 C27 115.13(16) . . ? C3 C2 C27 121.56(16) . . ? C4 C3 C2 117.71(18) . . ? C3 C4 C5 120.00(18) . . ? C3 C4 C13 120.96(18) . . ? C5 C4 C13 119.04(18) . . ? C4 C5 C6 118.53(17) . . ? N1 C6 C5 121.98(17) . . ? N1 C6 C7 116.54(16) . . ? C5 C6 C7 121.46(17) . . ? C8 C7 C12 118.75(17) . . ? C8 C7 C6 121.62(17) . . ? C12 C7 C6 119.61(16) . . ? C7 C8 C9 120.50(18) . . ? C10 C9 C8 120.88(18) . . ? C10 C9 C14 121.34(18) . . ? C8 C9 C14 117.73(18) . . ? C9 C10 C11 118.61(18) . . ? C12 C11 C10 121.15(18) . . ? C12 C11 C15 119.86(19) . . ? C10 C11 C15 118.99(19) . . ? C11 C12 C7 120.10(18) . . ? F2' C13 F1' 105.7(18) . . ? F2' C13 F2 131.2(7) . . ? F1' C13 F2 50.0(17) . . ? F2' C13 F1 52.5(18) . . ? F1' C13 F1 132.4(7) . . ? F2 C13 F1 108.4(3) . . ? F2' C13 F3 54.0(18) . . ? F1' C13 F3 58.7(17) . . ? F2 C13 F3 106.1(2) . . ? F1 C13 F3 104.5(3) . . ? F2' C13 F3' 103.9(17) . . ? F1' C13 F3' 110.1(18) . . ? F2 C13 F3' 62.8(12) . . ? F1 C13 F3' 53.5(12) . . ? F3 C13 F3' 141.8(6) . . ? F2' C13 C4 116.5(7) . . ? F1' C13 C4 114.0(6) . . ? F2 C13 C4 112.3(2) . . ? F1 C13 C4 113.59(19) . . ? F3 C13 C4 111.5(2) . . ? F3' C13 C4 106.3(6) . . ? F6 C14 F4 106.68(18) . . ? F6 C14 F5 106.69(18) . . ? F4 C14 F5 106.05(19) . . ? F6 C14 C9 113.06(18) . . ? F4 C14 C9 111.62(18) . . ? F5 C14 C9 112.28(17) . . ? F7' C15 F9' 115.8(13) . . ? F7' C15 F8' 102.9(13) . . ? F9' C15 F8' 100.2(11) . . ? F7' C15 F7 132.9(6) . . ? F9' C15 F7 35.8(11) . . ? F8' C15 F7 66.3(7) . . ? F7' C15 F9 55.5(13) . . ? F9' C15 F9 130.5(6) . . ? F8' C15 F9 49.4(6) . . ? F7 C15 F9 108.9(3) . . ? F7' C15 F8 51.2(14) . . ? F9' C15 F8 71.8(12) . . ? F8' C15 F8 137.3(5) . . ? F7 C15 F8 104.5(3) . . ? F9 C15 F8 103.4(3) . . ? F7' C15 C11 113.8(5) . . ? F9' C15 C11 113.5(6) . . ? F8' C15 C11 108.7(4) . . ? F7 C15 C11 113.0(2) . . ? F9 C15 C11 113.4(2) . . ? F8 C15 C11 112.87(19) . . ? N16 C17 C18 124.02(17) . . ? C19 C18 C17 117.61(17) . . ? C20 C19 C18 119.58(17) . . ? C20 C19 C28 120.40(17) . . ? C18 C19 C28 120.02(18) . . ? C19 C20 C21 118.41(17) . . ? N16 C21 C20 122.89(16) . . ? N16 C21 C22 117.60(15) . . ? C20 C21 C22 119.51(16) . . ? C23 C22 C27 119.65(16) . . ? C23 C22 C21 118.26(16) . . ? C27 C22 C21 122.09(16) . . ? C24 C23 C22 120.61(17) . . ? C25 C24 C23 120.43(18) . . ? C25 C24 C29 119.08(18) . . ? C23 C24 C29 120.46(18) . . ? C24 C25 C26 119.65(18) . . ? C25 C26 C27 121.10(18) . . ? C25 C26 C30 116.72(18) . . ? C27 C26 C30 122.18(19) . . ? C26 C27 C22 118.55(17) . . ? C26 C27 C2 122.07(16) . . ? C22 C27 C2 119.32(16) . . ? F10 C28 F12 106.95(19) . . ? F10 C28 F11 106.6(2) . . ? F12 C28 F11 106.4(2) . . ? F10 C28 C19 112.42(18) . . ? F12 C28 C19 111.8(2) . . ? F11 C28 C19 112.26(17) . . ? F14 C29 F13 105.92(19) . . ? F14 C29 F15 107.9(2) . . ? F13 C29 F15 105.8(2) . . ? F14 C29 C24 113.14(18) . . ? F13 C29 C24 111.8(2) . . ? F15 C29 C24 111.86(18) . . ? F18 C30 F17 107.0(2) . . ? F18 C30 F16 106.65(19) . . ? F17 C30 F16 106.13(19) . . ? F18 C30 C26 112.51(18) . . ? F17 C30 C26 111.84(19) . . ? F16 C30 C26 112.29(19) . . ? 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 F3' F2 F1' C13 -21.1(11) . . . . ? C13 F2 F1' F3 24.3(11) . . . . ? F3' F2 F1' F3 3(2) . . . . ? F2' F3 F1' F2 1.2(18) . . . . ? C13 F3 F1' F2 -24.9(11) . . . . ? F2' F3 F1' C13 26.1(10) . . . . ? F3' F1 F2' C13 19.7(12) . . . . ? F3' F1 F2' F3 -12(3) . . . . ? C13 F1 F2' F3 -32(2) . . . . ? F1' F3 F2' C13 -28.3(10) . . . . ? F1' F3 F2' F1 4(3) . . . . ? C13 F3 F2' F1 32(2) . . . . ? F2' F1 F3' C13 -17.1(11) . . . . ? F2' F1 F3' F2 12.7(15) . . . . ? C13 F1 F3' F2 29.8(7) . . . . ? F1' F2 F3' F1 -10.2(15) . . . . ? C13 F2 F3' F1 -31.5(7) . . . . ? F1' F2 F3' C13 21.4(11) . . . . ? F8' F9 F7' C15 18.6(9) . . . . ? F8' F9 F7' F8 -14.4(19) . . . . ? C15 F9 F7' F8 -33.1(14) . . . . ? C15 F8 F7' F9 32.3(12) . . . . ? F9' F8 F7' F9 7.4(17) . . . . ? F9' F8 F7' C15 -24.8(7) . . . . ? F7' F9 F8' C15 -17.2(8) . . . . ? F7' F9 F8' F7 13.5(12) . . . . ? C15 F9 F8' F7 30.7(6) . . . . ? F9' F7 F8' F9 -11.3(15) . . . . ? C15 F7 F8' F9 -34.1(7) . . . . ? F9' F7 F8' C15 22.8(12) . . . . ? F8' F7 F9' C15 -20.0(10) . . . . ? C15 F7 F9' F8 25.0(10) . . . . ? F8' F7 F9' F8 5.1(18) . . . . ? F7' F8 F9' F7 -2.9(17) . . . . ? C15 F8 F9' F7 -29.2(11) . . . . ? F7' F8 F9' C15 26.3(8) . . . . ? C6 N1 C2 C3 0.5(3) . . . . ? C6 N1 C2 C27 179.62(16) . . . . ? N1 C2 C3 C4 -1.3(3) . . . . ? C27 C2 C3 C4 179.64(18) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C2 C3 C4 C13 -179.53(19) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C13 C4 C5 C6 -179.49(19) . . . . ? C2 N1 C6 C5 0.6(3) . . . . ? C2 N1 C6 C7 -177.93(16) . . . . ? C4 C5 C6 N1 -0.8(3) . . . . ? C4 C5 C6 C7 177.62(17) . . . . ? N1 C6 C7 C8 -153.06(17) . . . . ? C5 C6 C7 C8 28.4(3) . . . . ? N1 C6 C7 C12 28.1(2) . . . . ? C5 C6 C7 C12 -150.44(18) . . . . ? C12 C7 C8 C9 0.6(3) . . . . ? C6 C7 C8 C9 -178.24(17) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C7 C8 C9 C14 -176.85(18) . . . . ? C8 C9 C10 C11 -0.9(3) . . . . ? C14 C9 C10 C11 176.53(18) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C9 C10 C11 C15 179.33(18) . . . . ? C10 C11 C12 C7 1.4(3) . . . . ? C15 C11 C12 C7 -178.06(18) . . . . ? C8 C7 C12 C11 -1.6(3) . . . . ? C6 C7 C12 C11 177.25(17) . . . . ? F1 F2' C13 F1' -131.8(13) . . . . ? F3 F2' C13 F1' 29.4(15) . . . . ? F1 F2' C13 F2 -82(2) . . . . ? F3 F2' C13 F2 79.5(19) . . . . ? F3 F2' C13 F1 161.3(10) . . . . ? F1 F2' C13 F3 -161.3(10) . . . . ? F1 F2' C13 F3' -16.0(12) . . . . ? F3 F2' C13 F3' 145.3(10) . . . . ? F1 F2' C13 C4 100.5(8) . . . . ? F3 F2' C13 C4 -98.3(10) . . . . ? F2 F1' C13 F2' 131.1(13) . . . . ? F3 F1' C13 F2' -27.7(14) . . . . ? F3 F1' C13 F2 -158.8(9) . . . . ? F2 F1' C13 F1 78(2) . . . . ? F3 F1' C13 F1 -81(2) . . . . ? F2 F1' C13 F3 158.8(9) . . . . ? F2 F1' C13 F3' 19.6(12) . . . . ? F3 F1' C13 F3' -139.3(10) . . . . ? F2 F1' C13 C4 -99.7(8) . . . . ? F3 F1' C13 C4 101.4(7) . . . . ? F1' F2 C13 F2' -75(3) . . . . ? F3' F2 C13 F2' 85(2) . . . . ? F3' F2 C13 F1' 159.3(11) . . . . ? F1' F2 C13 F1 -130.4(9) . . . . ? F3' F2 C13 F1 28.8(7) . . . . ? F1' F2 C13 F3 -18.7(9) . . . . ? F3' F2 C13 F3 140.6(7) . . . . ? F1' F2 C13 F3' -159.3(11) . . . . ? F1' F2 C13 C4 103.3(9) . . . . ? F3' F2 C13 C4 -97.4(7) . . . . ? F3' F1 C13 F2' -160.6(13) . . . . ? F2' F1 C13 F1' 76(2) . . . . ? F3' F1 C13 F1' -84(2) . . . . ? F2' F1 C13 F2 128.3(10) . . . . ? F3' F1 C13 F2 -32.2(9) . . . . ? F2' F1 C13 F3 15.6(10) . . . . ? F3' F1 C13 F3 -145.0(9) . . . . ? F2' F1 C13 F3' 160.6(13) . . . . ? F2' F1 C13 C4 -106.1(10) . . . . ? F3' F1 C13 C4 93.3(9) . . . . ? F1' F3 C13 F2' 146.4(12) . . . . ? F2' F3 C13 F1' -146.4(12) . . . . ? F2' F3 C13 F2 -129.7(9) . . . . ? F1' F3 C13 F2 16.7(9) . . . . ? F2' F3 C13 F1 -15.3(9) . . . . ? F1' F3 C13 F1 131.1(9) . . . . ? F2' F3 C13 F3' -64(2) . . . . ? F1' F3 C13 F3' 83(2) . . . . ? F2' F3 C13 C4 107.8(9) . . . . ? F1' F3 C13 C4 -105.8(9) . . . . ? F1 F3' C13 F2' 15.8(12) . . . . ? F2 F3' C13 F2' -129.5(11) . . . . ? F1 F3' C13 F1' 128.5(12) . . . . ? F2 F3' C13 F1' -16.8(12) . . . . ? F1 F3' C13 F2 145.3(7) . . . . ? F2 F3' C13 F1 -145.3(7) . . . . ? F1 F3' C13 F3 64(2) . . . . ? F2 F3' C13 F3 -81.3(19) . . . . ? F1 F3' C13 C4 -107.6(4) . . . . ? F2 F3' C13 C4 107.1(4) . . . . ? C3 C4 C13 F2' -68(2) . . . . ? C5 C4 C13 F2' 111(2) . . . . ? C3 C4 C13 F1' 168(2) . . . . ? C5 C4 C13 F1' -12(2) . . . . ? C3 C4 C13 F2 113.5(3) . . . . ? C5 C4 C13 F2 -67.1(3) . . . . ? C3 C4 C13 F1 -9.9(4) . . . . ? C5 C4 C13 F1 169.5(3) . . . . ? C3 C4 C13 F3 -127.7(3) . . . . ? C5 C4 C13 F3 51.8(3) . . . . ? C3 C4 C13 F3' 46.8(14) . . . . ? C5 C4 C13 F3' -133.8(14) . . . . ? C10 C9 C14 F6 11.0(3) . . . . ? C8 C9 C14 F6 -171.49(18) . . . . ? C10 C9 C14 F4 -109.3(2) . . . . ? C8 C9 C14 F4 68.2(2) . . . . ? C10 C9 C14 F5 131.8(2) . . . . ? C8 C9 C14 F5 -50.7(3) . . . . ? F9 F7' C15 F9' -122.9(10) . . . . ? F8 F7' C15 F9' 33.3(12) . . . . ? F9 F7' C15 F8' -14.6(8) . . . . ? F8 F7' C15 F8' 141.6(7) . . . . ? F9 F7' C15 F7 -84.2(17) . . . . ? F8 F7' C15 F7 72.0(17) . . . . ? F8 F7' C15 F9 156.2(8) . . . . ? F9 F7' C15 F8 -156.2(8) . . . . ? F9 F7' C15 C11 102.9(6) . . . . ? F8 F7' C15 C11 -100.9(6) . . . . ? F7 F9' C15 F7' 128.4(14) . . . . ? F8 F9' C15 F7' -26.8(12) . . . . ? F7 F9' C15 F8' 18.5(11) . . . . ? F8 F9' C15 F8' -136.6(6) . . . . ? F8 F9' C15 F7 -155.2(11) . . . . ? F7 F9' C15 F9 62.9(18) . . . . ? F8 F9' C15 F9 -92.3(11) . . . . ? F7 F9' C15 F8 155.2(11) . . . . ? F7 F9' C15 C11 -97.2(8) . . . . ? F8 F9' C15 C11 107.6(5) . . . . ? F9 F8' C15 F7' 15.9(10) . . . . ? F7 F8' C15 F7' -131.4(8) . . . . ? F9 F8' C15 F9' 135.6(9) . . . . ? F7 F8' C15 F9' -11.7(9) . . . . ? F9 F8' C15 F7 147.3(6) . . . . ? F7 F8' C15 F9 -147.3(6) . . . . ? F9 F8' C15 F8 61.4(12) . . . . ? F7 F8' C15 F8 -85.9(10) . . . . ? F9 F8' C15 C11 -105.2(4) . . . . ? F7 F8' C15 C11 107.6(3) . . . . ? F9' F7 C15 F7' -74(2) . . . . ? F8' F7 C15 F7' 86(2) . . . . ? F8' F7 C15 F9' 160.0(12) . . . . ? F9' F7 C15 F8' -160.0(12) . . . . ? F9' F7 C15 F9 -134.3(11) . . . . ? F8' F7 C15 F9 25.7(5) . . . . ? F9' F7 C15 F8 -24.3(11) . . . . ? F8' F7 C15 F8 135.7(5) . . . . ? F9' F7 C15 C11 98.8(11) . . . . ? F8' F7 C15 C11 -101.2(5) . . . . ? F8' F9 C15 F7' -161.1(10) . . . . ? F7' F9 C15 F9' 96.2(16) . . . . ? F8' F9 C15 F9' -64.9(16) . . . . ? F7' F9 C15 F8' 161.1(10) . . . . ? F7' F9 C15 F7 129.6(8) . . . . ? F8' F9 C15 F7 -31.6(6) . . . . ? F7' F9 C15 F8 18.8(7) . . . . ? F8' F9 C15 F8 -142.3(6) . . . . ? F7' F9 C15 C11 -103.7(7) . . . . ? F8' F9 C15 C11 95.2(7) . . . . ? F9' F8 C15 F7' 148.6(9) . . . . ? F7' F8 C15 F9' -148.6(9) . . . . ? F7' F8 C15 F8' -63.3(13) . . . . ? F9' F8 C15 F8' 85.3(12) . . . . ? F7' F8 C15 F7 -133.9(8) . . . . ? F9' F8 C15 F7 14.7(6) . . . . ? F7' F8 C15 F9 -20.0(7) . . . . ? F9' F8 C15 F9 128.6(6) . . . . ? F7' F8 C15 C11 102.9(8) . . . . ? F9' F8 C15 C11 -108.5(6) . . . . ? C12 C11 C15 F7' -67.3(17) . . . . ? C10 C11 C15 F7' 113.2(17) . . . . ? C12 C11 C15 F9' 157.3(13) . . . . ? C10 C11 C15 F9' -22.2(14) . . . . ? C12 C11 C15 F8' 46.7(9) . . . . ? C10 C11 C15 F8' -132.8(9) . . . . ? C12 C11 C15 F7 118.3(4) . . . . ? C10 C11 C15 F7 -61.2(4) . . . . ? C12 C11 C15 F9 -6.3(5) . . . . ? C10 C11 C15 F9 174.2(4) . . . . ? C12 C11 C15 F8 -123.4(3) . . . . ? C10 C11 C15 F8 57.1(3) . . . . ? C21 N16 C17 C18 -1.1(3) . . . . ? N16 C17 C18 C19 1.0(3) . . . . ? C17 C18 C19 C20 -0.4(3) . . . . ? C17 C18 C19 C28 179.10(19) . . . . ? C18 C19 C20 C21 -0.1(3) . . . . ? C28 C19 C20 C21 -179.61(18) . . . . ? C17 N16 C21 C20 0.5(3) . . . . ? C17 N16 C21 C22 -178.97(16) . . . . ? C19 C20 C21 N16 0.1(3) . . . . ? C19 C20 C21 C22 179.56(17) . . . . ? N16 C21 C22 C23 135.97(18) . . . . ? C20 C21 C22 C23 -43.5(2) . . . . ? N16 C21 C22 C27 -44.1(2) . . . . ? C20 C21 C22 C27 136.37(18) . . . . ? C27 C22 C23 C24 -0.6(3) . . . . ? C21 C22 C23 C24 179.28(17) . . . . ? C22 C23 C24 C25 -0.7(3) . . . . ? C22 C23 C24 C29 -178.3(2) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C29 C24 C25 C26 178.5(2) . . . . ? C24 C25 C26 C27 0.3(3) . . . . ? C24 C25 C26 C30 -178.8(2) . . . . ? C25 C26 C27 C22 -1.5(3) . . . . ? C30 C26 C27 C22 177.53(19) . . . . ? C25 C26 C27 C2 -178.64(18) . . . . ? C30 C26 C27 C2 0.4(3) . . . . ? C23 C22 C27 C26 1.7(3) . . . . ? C21 C22 C27 C26 -178.22(17) . . . . ? C23 C22 C27 C2 178.89(17) . . . . ? C21 C22 C27 C2 -1.0(3) . . . . ? N1 C2 C27 C26 116.3(2) . . . . ? C3 C2 C27 C26 -64.6(3) . . . . ? N1 C2 C27 C22 -60.8(2) . . . . ? C3 C2 C27 C22 118.3(2) . . . . ? C20 C19 C28 F10 -146.4(2) . . . . ? C18 C19 C28 F10 34.1(3) . . . . ? C20 C19 C28 F12 93.2(3) . . . . ? C18 C19 C28 F12 -86.2(3) . . . . ? C20 C19 C28 F11 -26.2(3) . . . . ? C18 C19 C28 F11 154.3(2) . . . . ? C25 C24 C29 F14 152.8(2) . . . . ? C23 C24 C29 F14 -29.6(3) . . . . ? C25 C24 C29 F13 -87.7(2) . . . . ? C23 C24 C29 F13 89.9(2) . . . . ? C25 C24 C29 F15 30.7(3) . . . . ? C23 C24 C29 F15 -151.6(2) . . . . ? C25 C26 C30 F18 135.6(2) . . . . ? C27 C26 C30 F18 -43.5(3) . . . . ? C25 C26 C30 F17 -104.0(2) . . . . ? C27 C26 C30 F17 77.0(3) . . . . ? C25 C26 C30 F16 15.2(3) . . . . ? C27 C26 C30 F16 -163.86(19) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.418 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.053 #===END #===END data_03314 _database_code_depnum_ccdc_archive 'CCDC 257684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H30 F54 Ir2 N6' _chemical_formula_weight 2533.54 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' 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' 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 41.862(4) _cell_length_b 9.2252(9) _cell_length_c 22.004(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.2780(18) _cell_angle_gamma 90.00 _cell_volume 8386.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_max .28 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .10 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4864 _exptl_absorpt_coefficient_mu 3.343 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22126 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.28 _reflns_number_total 11872 _reflns_number_gt 10884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _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 0.28(1) _refine_ls_number_reflns 11872 _refine_ls_number_parameters 1316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.003 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_1 Ir 0.383273(5) 0.84789(2) 0.168594(10) 0.01965(6) Uani 1 1 d . . . F1_1 F 0.38629(17) 1.3650(8) 0.4009(2) 0.090(2) Uani 1 1 d . . . F2_1 F 0.33747(19) 1.3108(6) 0.3907(3) 0.098(3) Uani 1 1 d . . . F3_1 F 0.35426(15) 1.4710(5) 0.3335(2) 0.0651(16) Uani 1 1 d . . . F4_1 F 0.27264(18) 0.6026(12) 0.3563(4) 0.167(5) Uani 1 1 d . . . F5_1 F 0.25210(19) 0.8015(8) 0.3317(4) 0.117(3) Uani 1 1 d . . . F6_1 F 0.23849(17) 0.6285(11) 0.2779(4) 0.129(4) Uani 1 1 d . . . F7_1 F 0.31732(13) 0.3861(5) 0.1794(2) 0.0564(15) Uani 1 1 d . . . F8_1 F 0.32153(11) 0.5268(6) 0.10348(18) 0.0494(13) Uani 1 1 d . . . F9_1 F 0.36308(11) 0.4767(5) 0.17144(19) 0.0418(10) Uani 1 1 d . . . F10_1 F 0.23740(13) 1.0677(9) 0.0153(3) 0.094(3) Uani 1 1 d . . . F11_1 F 0.25213(12) 0.9557(7) -0.0602(2) 0.0707(19) Uani 1 1 d . . . F12_1 F 0.26335(16) 1.1769(7) -0.0458(3) 0.087(2) Uani 1 1 d . . . F13_1 F 0.34896(17) 0.3128(6) -0.0542(2) 0.077(2) Uani 1 1 d . . . F14_1 F 0.34763(14) 0.4981(7) -0.11315(18) 0.0690(16) Uani 1 1 d . . . F15_1 F 0.39144(14) 0.3831(6) -0.0862(2) 0.0681(17) Uani 1 1 d . . . F16_1 F 0.44833(11) 0.4216(5) 0.1148(2) 0.0500(13) Uani 1 1 d . . . F17_1 F 0.45626(10) 0.6410(6) 0.1441(2) 0.0492(13) Uani 1 1 d . . . F18_1 F 0.42655(10) 0.5016(7) 0.18884(17) 0.0440(11) Uani 1 1 d . . . F19_1 F 0.46546(15) 0.6573(11) 0.4536(2) 0.105(3) Uani 1 1 d . . . F20_1 F 0.49734(18) 0.8153(7) 0.4262(2) 0.092(2) Uani 1 1 d . . . F21_1 F 0.50281(15) 0.5989(8) 0.4048(2) 0.080(2) Uani 1 1 d . . . F22_1 F 0.52860(16) 1.2202(8) 0.1392(5) 0.129(4) Uani 1 1 d . . . F23_1 F 0.54522(15) 1.0506(16) 0.1891(5) 0.205(7) Uani 1 1 d . . . F24_1 F 0.53760(18) 1.0285(12) 0.1014(5) 0.179(6) Uani 1 1 d . . . F25_1 F 0.42288(11) 1.1501(5) 0.00504(19) 0.0441(11) Uani 1 1 d . . . F26_1 F 0.39471(11) 0.9622(5) 0.01631(18) 0.0455(12) Uani 1 1 d . . . F27_1 F 0.38778(10) 1.1590(5) 0.0661(2) 0.0437(11) Uani 1 1 d . . . N1_1 N 0.37755(11) 1.0161(6) 0.2318(2) 0.0203(11) Uani 1 1 d . . . N15_1 N 0.34778(12) 0.9378(6) 0.1045(2) 0.0205(12) Uani 1 1 d . . . N29_1 N 0.41577(13) 0.7676(6) 0.2403(2) 0.0217(12) Uani 1 1 d . . . C1_1 C 0.39534(16) 1.1374(8) 0.2393(3) 0.0273(14) Uani 1 1 d . . . H1A_1 H 0.4119 1.1486 0.2162 0.033 Uiso 1 1 calc R . . C2_1 C 0.39035(17) 1.2462(8) 0.2795(3) 0.0299(16) Uani 1 1 d . . . H2A_1 H 0.4033 1.3287 0.2840 0.036 Uiso 1 1 calc R . . C3_1 C 0.36543(19) 1.2286(8) 0.3131(3) 0.0293(16) Uani 1 1 d . . . C4_1 C 0.34677(19) 1.1061(8) 0.3065(3) 0.0312(16) Uani 1 1 d . . . H4A_1 H 0.3305 1.0929 0.3301 0.037 Uiso 1 1 calc R . . C5_1 C 0.35247(14) 1.0010(9) 0.2638(3) 0.0239(13) Uani 1 1 d . . . C6_1 C 0.33404(14) 0.8647(8) 0.2516(3) 0.0244(13) Uani 1 1 d . . . C7_1 C 0.30848(16) 0.8405(9) 0.2842(3) 0.0336(15) Uani 1 1 d . . . H7A_1 H 0.3036 0.9089 0.3123 0.040 Uiso 1 1 calc R . . C8_1 C 0.29053(16) 0.7145(9) 0.2744(3) 0.0353(17) Uani 1 1 d . . . C9_1 C 0.29840(17) 0.6150(9) 0.2338(3) 0.0352(17) Uani 1 1 d . . . H9A_1 H 0.2863 0.5302 0.2271 0.042 Uiso 1 1 calc R . . C10_1 C 0.32399(18) 0.6369(8) 0.2021(3) 0.0285(15) Uani 1 1 d . . . C11_1 C 0.34295(16) 0.7662(8) 0.2082(3) 0.0245(14) Uani 1 1 d . . . C12_1 C 0.3596(2) 1.3431(10) 0.3592(3) 0.0415(18) Uani 1 1 d . . . C13_1 C 0.2647(2) 0.6851(10) 0.3121(4) 0.051(2) Uani 1 1 d . . . C14_1 C 0.33162(19) 0.5094(10) 0.1635(3) 0.0386(18) Uani 1 1 d . . . C15_1 C 0.33193(16) 1.0626(8) 0.1118(3) 0.0252(14) Uani 1 1 d . . . H15A_1 H 0.3400 1.1235 0.1444 0.030 Uiso 1 1 calc R . . C16_1 C 0.30440(16) 1.1028(8) 0.0731(3) 0.0312(16) Uani 1 1 d . . . H16A_1 H 0.2939 1.1890 0.0794 0.037 Uiso 1 1 calc R . . C17_1 C 0.29246(15) 1.0124(10) 0.0240(3) 0.0329(16) Uani 1 1 d . . . C18_1 C 0.30857(16) 0.8897(8) 0.0154(3) 0.0292(17) Uani 1 1 d . . . H18A_1 H 0.3007 0.8289 -0.0173 0.035 Uiso 1 1 calc R . . C19_1 C 0.33710(14) 0.8523(9) 0.0552(3) 0.0237(12) Uani 1 1 d . . . C20_1 C 0.35781(16) 0.7280(8) 0.0487(3) 0.0253(15) Uani 1 1 d . . . C21_1 C 0.35236(17) 0.6450(9) -0.0038(3) 0.0316(17) Uani 1 1 d . . . H21A_1 H 0.3353 0.6676 -0.0348 0.038 Uiso 1 1 calc R . . C22_1 C 0.37191(18) 0.5296(8) -0.0106(3) 0.0331(17) Uani 1 1 d . . . C23_1 C 0.39847(16) 0.5005(9) 0.0347(3) 0.0293(14) Uani 1 1 d . . . H23A_1 H 0.4123 0.4246 0.0292 0.035 Uiso 1 1 calc R . . C24_1 C 0.40439(16) 0.5838(7) 0.0878(3) 0.0248(14) Uani 1 1 d . . . C25_1 C 0.38385(15) 0.7007(7) 0.0983(3) 0.0232(13) Uani 1 1 d . . . C26_1 C 0.2617(2) 1.0511(11) -0.0169(4) 0.051(2) Uani 1 1 d . . . C27_1 C 0.3646(2) 0.4316(9) -0.0653(3) 0.043(2) Uani 1 1 d . . . C28_1 C 0.43343(18) 0.5376(8) 0.1336(3) 0.0337(17) Uani 1 1 d . . . C29_1 C 0.40743(17) 0.6804(8) 0.2846(3) 0.0302(16) Uani 1 1 d . . . H29A_1 H 0.3871 0.6368 0.2778 0.036 Uiso 1 1 calc R . . C30_1 C 0.42784(18) 0.6532(9) 0.3399(3) 0.0361(17) Uani 1 1 d . . . H30A_1 H 0.4213 0.5933 0.3696 0.043 Uiso 1 1 calc R . . C31_1 C 0.45798(18) 0.7176(9) 0.3493(3) 0.0333(17) Uani 1 1 d . . . C32_1 C 0.46773(18) 0.8007(8) 0.3027(3) 0.0359(18) Uani 1 1 d . . . H32A_1 H 0.4885 0.8393 0.3077 0.043 Uiso 1 1 calc R . . C33_1 C 0.44616(15) 0.8254(7) 0.2487(3) 0.0260(15) Uani 1 1 d . . . C34_1 C 0.45280(15) 0.9108(7) 0.1969(3) 0.0244(14) Uani 1 1 d . . . C35_1 C 0.48512(16) 0.9584(8) 0.1952(3) 0.0316(17) Uani 1 1 d . . . H35A_1 H 0.5016 0.9374 0.2276 0.038 Uiso 1 1 calc R . . C36_1 C 0.49163(16) 1.0361(8) 0.1449(3) 0.0331(16) Uani 1 1 d . . . C37_1 C 0.46679(16) 1.0700(8) 0.0977(3) 0.0307(15) Uani 1 1 d . . . H37A_1 H 0.4711 1.1241 0.0643 0.037 Uiso 1 1 calc R . . C38_1 C 0.43565(15) 1.0235(7) 0.1001(3) 0.0255(14) Uani 1 1 d . . . C39_1 C 0.42675(15) 0.9411(7) 0.1486(3) 0.0208(13) Uani 1 1 d . . . C40_1 C 0.4804(2) 0.6984(11) 0.4095(4) 0.047(2) Uani 1 1 d . . . C41_1 C 0.5251(2) 1.0844(11) 0.1423(4) 0.049(2) Uani 1 1 d . . . C42_1 C 0.41045(18) 1.0723(9) 0.0470(3) 0.0343(17) Uani 1 1 d . . . Ir2_2 Ir 0.124348(5) 0.99580(2) 0.320402(10) 0.02075(6) Uani 1 1 d . . . F28_2 F 0.16462(16) 0.3700(6) 0.1713(2) 0.0705(17) Uani 1 1 d . . . F29_2 F 0.19094(17) 0.5207(8) 0.1285(4) 0.115(3) Uani 1 1 d . . . F30_2 F 0.14266(19) 0.4802(9) 0.0938(2) 0.107(3) Uani 1 1 d . . . F31_2 F 0.24851(14) 1.2656(7) 0.1690(3) 0.0777(19) Uani 1 1 d . . . F32_2 F 0.26656(14) 1.0501(6) 0.1877(3) 0.0749(18) Uani 1 1 d . . . F33_2 F 0.27895(13) 1.2174(8) 0.2544(3) 0.0822(19) Uani 1 1 d . . . F34_2 F 0.19173(12) 1.4575(5) 0.3286(2) 0.0493(13) Uani 1 1 d . . . F35_2 F 0.18067(11) 1.3159(5) 0.39920(18) 0.0456(13) Uani 1 1 d . . . F36_2 F 0.14449(10) 1.3686(5) 0.32109(19) 0.0410(10) Uani 1 1 d . . . F37_2 F 0.25675(17) 0.7235(12) 0.5101(3) 0.144(4) Uani 1 1 d . . . F38_2 F 0.2436(2) 0.8793(10) 0.5693(3) 0.156(5) Uani 1 1 d . . . F39_2 F 0.2252(3) 0.6778(16) 0.5657(5) 0.195(6) Uani 1 1 d . . . F40_2 F 0.1395(2) 1.5056(8) 0.5566(2) 0.101(3) Uani 1 1 d . . . F41_2 F 0.13385(15) 1.3161(6) 0.60855(19) 0.0655(17) Uani 1 1 d . . . F42_2 F 0.09319(17) 1.4370(8) 0.5681(2) 0.086(2) Uani 1 1 d . . . F43_2 F 0.05546(11) 1.4253(5) 0.3584(2) 0.0464(12) Uani 1 1 d . . . F44_2 F 0.04877(10) 1.2077(5) 0.3257(2) 0.0439(11) Uani 1 1 d . . . F45_2 F 0.08307(10) 1.3454(6) 0.29236(17) 0.0435(10) Uani 1 1 d . . . F46_2 F 0.05194(12) 1.2494(7) 0.0334(2) 0.0668(17) Uani 1 1 d . . . F47_2 F 0.03348(15) 1.0374(6) 0.0387(2) 0.0766(19) Uani 1 1 d . . . F48_2 F 0.00957(12) 1.2177(8) 0.0720(2) 0.0663(17) Uani 1 1 d . . . F49_2 F -0.03707(12) 0.7719(8) 0.2604(3) 0.083(2) Uani 1 1 d . . . F50_2 F -0.02378(13) 0.6262(6) 0.3331(3) 0.0733(18) Uani 1 1 d . . . F51_2 F -0.03631(12) 0.8425(8) 0.3518(3) 0.092(2) Uani 1 1 d . . . F52_2 F 0.07583(11) 0.6794(5) 0.4686(2) 0.0460(12) Uani 1 1 d . . . F53_2 F 0.10546(11) 0.8662(6) 0.46629(18) 0.0473(12) Uani 1 1 d . . . F54_2 F 0.11465(11) 0.6748(5) 0.4158(2) 0.0492(12) Uani 1 1 d . . . N43_2 N 0.13375(12) 0.8300(7) 0.2582(2) 0.0234(12) Uani 1 1 d . . . N57_2 N 0.15636(13) 0.9073(6) 0.3904(2) 0.0211(12) Uani 1 1 d . . . N71_2 N 0.09523(13) 1.0795(6) 0.2439(2) 0.0231(12) Uani 1 1 d . . . C43_2 C 0.11586(17) 0.7108(8) 0.2437(3) 0.0292(15) Uani 1 1 d . . . H43A_2 H 0.0967 0.7013 0.2596 0.035 Uiso 1 1 calc R . . C44_2 C 0.12414(18) 0.6023(8) 0.2068(3) 0.0328(17) Uani 1 1 d . . . H44A_2 H 0.1106 0.5228 0.1970 0.039 Uiso 1 1 calc R . . C45_2 C 0.15258(18) 0.6135(8) 0.1849(3) 0.0292(16) Uani 1 1 d . . . C46_2 C 0.17184(18) 0.7351(7) 0.1998(3) 0.0301(15) Uani 1 1 d . . . H46A_2 H 0.1914 0.7438 0.1851 0.036 Uiso 1 1 calc R . . C47_2 C 0.16206(14) 0.8435(8) 0.2364(2) 0.0228(12) Uani 1 1 d . . . C48_2 C 0.18031(15) 0.9785(8) 0.2531(3) 0.0239(14) Uani 1 1 d . . . C49_2 C 0.20810(15) 1.0062(9) 0.2280(3) 0.0308(14) Uani 1 1 d . . . H49A_2 H 0.2151 0.9383 0.2018 0.037 Uiso 1 1 calc R . . C50_2 C 0.22544(17) 1.1326(8) 0.2412(3) 0.0355(17) Uani 1 1 d . . . C51_2 C 0.21400(17) 1.2338(8) 0.2791(3) 0.0325(16) Uani 1 1 d . . . H51A_2 H 0.2254 1.3193 0.2889 0.039 Uiso 1 1 calc R . . C52_2 C 0.18583(16) 1.2089(8) 0.3022(3) 0.0235(14) Uani 1 1 d . . . C53_2 C 0.16739(15) 1.0787(7) 0.2922(3) 0.0215(14) Uani 1 1 d . . . C54_2 C 0.16347(19) 0.4966(10) 0.1451(3) 0.0376(16) Uani 1 1 d . . . C55_2 C 0.2541(2) 1.1635(10) 0.2131(4) 0.049(2) Uani 1 1 d . . . C56_2 C 0.17571(18) 1.3346(10) 0.3374(3) 0.0342(17) Uani 1 1 d . . . C57_2 C 0.17334(17) 0.7846(8) 0.3859(3) 0.0273(15) Uani 1 1 d . . . H57A_2 H 0.1681 0.7283 0.3506 0.033 Uiso 1 1 calc R . . C58_2 C 0.19789(16) 0.7387(8) 0.4305(3) 0.0308(16) Uani 1 1 d . . . H58A_2 H 0.2088 0.6521 0.4266 0.037 Uiso 1 1 calc R . . C59_2 C 0.20586(17) 0.8269(9) 0.4818(3) 0.0340(18) Uani 1 1 d . . . C60_2 C 0.18861(17) 0.9496(9) 0.4881(3) 0.0339(18) Uani 1 1 d . . . H60A_2 H 0.1938 1.0075 0.5228 0.041 Uiso 1 1 calc R . . C61_2 C 0.16313(14) 0.9877(8) 0.4421(3) 0.0225(13) Uani 1 1 d . . . C62_2 C 0.14162(16) 1.1117(8) 0.4439(3) 0.0238(15) Uani 1 1 d . . . C63_2 C 0.14165(17) 1.1916(8) 0.4980(3) 0.0326(17) Uani 1 1 d . . . H63A_2 H 0.1566 1.1694 0.5327 0.039 Uiso 1 1 calc R . . C64_2 C 0.12041(19) 1.3002(8) 0.5007(3) 0.0335(16) Uani 1 1 d . . . C65_2 C 0.09836(17) 1.3308(8) 0.4504(3) 0.0299(15) Uani 1 1 d . . . H65A_2 H 0.0835 1.4047 0.4528 0.036 Uiso 1 1 calc R . . C66_2 C 0.09710(16) 1.2552(7) 0.3946(3) 0.0274(15) Uani 1 1 d . . . C67_2 C 0.11896(14) 1.1400(7) 0.3889(3) 0.0211(13) Uani 1 1 d . . . C68_2 C 0.2342(3) 0.7820(13) 0.5293(4) 0.065(3) Uani 1 1 d . . . C69_2 C 0.1223(2) 1.3885(10) 0.5576(3) 0.049(2) Uani 1 1 d . . . C70_2 C 0.07175(17) 1.3071(8) 0.3433(4) 0.0317(17) Uani 1 1 d . . . C71_2 C 0.10675(17) 1.1656(8) 0.2032(3) 0.0306(16) Uani 1 1 d . . . H71A_2 H 0.1275 1.2038 0.2131 0.037 Uiso 1 1 calc R . . C72_2 C 0.08829(18) 1.1990(9) 0.1462(3) 0.0325(16) Uani 1 1 d . . . H72A_2 H 0.0962 1.2616 0.1190 0.039 Uiso 1 1 calc R . . C73_2 C 0.05805(18) 1.1368(9) 0.1313(3) 0.0352(17) Uani 1 1 d . . . C74_2 C 0.04632(16) 1.0520(8) 0.1735(3) 0.0308(16) Uani 1 1 d . . . H74A_2 H 0.0256 1.0129 0.1642 0.037 Uiso 1 1 calc R . . C75_2 C 0.06521(15) 1.0233(7) 0.2308(3) 0.0266(15) Uani 1 1 d . . . C76_2 C 0.05504(16) 0.9327(7) 0.2794(3) 0.0252(14) Uani 1 1 d . . . C77_2 C 0.02331(16) 0.8884(8) 0.2751(3) 0.0335(17) Uani 1 1 d . . . H77A_2 H 0.0083 0.9142 0.2409 0.040 Uiso 1 1 calc R . . C78_2 C 0.01396(17) 0.8070(8) 0.3208(4) 0.0347(18) Uani 1 1 d . . . C79_2 C 0.03666(17) 0.7685(7) 0.3715(4) 0.0319(16) Uani 1 1 d . . . H79A_2 H 0.0304 0.7126 0.4026 0.038 Uiso 1 1 calc R . . C80_2 C 0.06881(17) 0.8132(7) 0.3760(3) 0.0296(16) Uani 1 1 d . . . C81_2 C 0.07930(15) 0.9016(7) 0.3306(3) 0.0252(14) Uani 1 1 d . . . C82_2 C 0.0382(2) 1.1629(10) 0.0689(3) 0.043(2) Uani 1 1 d . . . C83_2 C -0.02004(18) 0.7608(9) 0.3175(4) 0.044(2) Uani 1 1 d . . . C84_2 C 0.09102(19) 0.7590(8) 0.4308(3) 0.0342(17) 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_1 0.01984(11) 0.02020(11) 0.01837(10) -0.00009(10) 0.00143(9) -0.00241(10) F1_1 0.133(6) 0.084(5) 0.044(3) -0.037(3) -0.009(3) 0.009(5) F2_1 0.161(7) 0.047(4) 0.118(5) -0.043(4) 0.115(5) -0.039(4) F3_1 0.111(5) 0.030(3) 0.062(3) -0.004(2) 0.034(3) 0.013(3) F4_1 0.103(6) 0.257(12) 0.169(7) 0.178(8) 0.103(6) 0.092(7) F5_1 0.109(6) 0.086(5) 0.187(8) 0.013(5) 0.116(6) 0.001(5) F6_1 0.072(5) 0.183(10) 0.143(7) -0.006(7) 0.053(5) -0.067(6) F7_1 0.075(4) 0.035(3) 0.069(3) -0.006(2) 0.043(3) -0.026(2) F8_1 0.055(3) 0.062(4) 0.032(2) -0.014(2) 0.009(2) -0.023(3) F9_1 0.046(2) 0.027(2) 0.055(3) 0.000(2) 0.016(2) -0.003(2) F10_1 0.036(3) 0.174(8) 0.067(4) -0.019(4) -0.004(3) 0.042(4) F11_1 0.050(3) 0.081(5) 0.069(3) -0.026(3) -0.027(3) 0.023(3) F12_1 0.086(5) 0.067(4) 0.090(4) 0.022(4) -0.038(4) 0.021(4) F13_1 0.134(6) 0.048(4) 0.046(3) -0.022(3) 0.007(3) -0.035(4) F14_1 0.112(4) 0.053(3) 0.032(2) -0.015(3) -0.018(3) 0.029(4) F15_1 0.086(4) 0.072(4) 0.046(3) -0.023(3) 0.011(3) 0.024(3) F16_1 0.048(3) 0.040(3) 0.055(3) -0.014(2) -0.010(2) 0.023(2) F17_1 0.026(2) 0.042(3) 0.076(3) -0.011(3) -0.004(2) 0.000(2) F18_1 0.052(3) 0.048(3) 0.031(2) 0.013(3) 0.0017(19) 0.020(3) F19_1 0.070(4) 0.212(9) 0.029(3) 0.034(4) -0.008(3) -0.030(5) F20_1 0.126(5) 0.067(4) 0.059(3) 0.000(3) -0.055(3) -0.023(4) F21_1 0.069(4) 0.101(5) 0.058(3) 0.002(3) -0.025(3) 0.030(4) F22_1 0.055(4) 0.055(4) 0.289(12) -0.003(6) 0.062(6) -0.029(3) F23_1 0.032(3) 0.331(18) 0.238(11) 0.177(12) -0.017(5) -0.059(6) F24_1 0.083(5) 0.197(10) 0.291(12) -0.182(10) 0.133(8) -0.096(6) F25_1 0.045(3) 0.049(3) 0.041(2) 0.022(2) 0.016(2) -0.005(2) F26_1 0.053(3) 0.049(3) 0.030(2) 0.009(2) -0.005(2) -0.021(2) F27_1 0.034(2) 0.036(3) 0.063(3) 0.020(2) 0.016(2) 0.009(2) N1_1 0.019(2) 0.021(3) 0.020(2) 0.000(2) 0.004(2) -0.001(2) N15_1 0.017(3) 0.023(3) 0.020(3) -0.001(2) 0.001(2) 0.003(2) N29_1 0.027(3) 0.018(3) 0.019(3) 0.002(2) 0.000(2) -0.002(2) C1_1 0.022(3) 0.027(3) 0.035(4) -0.009(3) 0.009(3) -0.006(3) C2_1 0.029(4) 0.025(4) 0.037(4) -0.004(3) 0.008(3) -0.008(3) C3_1 0.044(4) 0.025(4) 0.019(3) 0.000(3) 0.005(3) -0.001(3) C4_1 0.045(4) 0.029(4) 0.022(3) 0.007(3) 0.011(3) -0.004(3) C5_1 0.027(3) 0.023(3) 0.022(3) 0.002(3) 0.004(2) -0.002(3) C6_1 0.026(3) 0.027(3) 0.020(3) 0.006(3) 0.004(2) -0.004(3) C7_1 0.035(4) 0.033(4) 0.037(3) 0.001(4) 0.017(3) -0.004(4) C8_1 0.023(3) 0.041(4) 0.046(4) 0.011(4) 0.016(3) -0.003(3) C9_1 0.028(4) 0.038(4) 0.041(4) 0.002(4) 0.011(3) -0.013(3) C10_1 0.034(4) 0.023(3) 0.029(3) 0.008(3) 0.006(3) -0.006(3) C11_1 0.023(3) 0.034(4) 0.016(3) 0.004(3) 0.001(3) 0.001(3) C12_1 0.066(5) 0.029(4) 0.034(4) -0.005(4) 0.024(4) -0.003(4) C13_1 0.056(6) 0.042(5) 0.064(6) 0.006(5) 0.036(5) -0.013(4) C14_1 0.043(4) 0.031(4) 0.042(4) -0.001(4) 0.009(3) -0.019(4) C15_1 0.025(3) 0.029(4) 0.020(3) -0.002(3) 0.001(3) 0.000(3) C16_1 0.028(4) 0.034(4) 0.032(4) 0.000(3) 0.006(3) 0.009(3) C17_1 0.022(3) 0.047(5) 0.029(3) -0.001(4) 0.002(3) 0.001(3) C18_1 0.026(3) 0.032(4) 0.026(3) -0.002(3) -0.008(3) -0.001(3) C19_1 0.022(3) 0.027(3) 0.022(3) -0.001(3) 0.002(2) -0.001(3) C20_1 0.025(3) 0.028(4) 0.024(3) 0.004(3) 0.006(3) 0.004(3) C21_1 0.035(4) 0.036(4) 0.021(3) -0.014(3) -0.004(3) 0.007(3) C22_1 0.050(4) 0.031(4) 0.018(3) -0.003(3) 0.004(3) -0.001(3) C23_1 0.040(4) 0.020(3) 0.029(3) -0.002(3) 0.009(3) 0.001(3) C24_1 0.027(3) 0.025(4) 0.020(3) 0.001(3) -0.001(3) -0.004(3) C25_1 0.025(3) 0.021(3) 0.025(3) -0.001(3) 0.007(3) -0.008(3) C26_1 0.037(5) 0.063(6) 0.050(5) -0.006(5) -0.001(4) 0.021(4) C27_1 0.075(6) 0.030(4) 0.023(4) -0.007(3) 0.006(4) 0.009(4) C28_1 0.036(4) 0.027(4) 0.035(4) -0.006(3) -0.002(3) 0.006(3) C29_1 0.030(4) 0.036(4) 0.025(3) 0.005(3) 0.003(3) -0.010(3) C30_1 0.043(4) 0.042(4) 0.023(3) 0.006(3) 0.003(3) -0.002(4) C31_1 0.033(4) 0.037(4) 0.026(3) 0.000(3) -0.005(3) -0.001(3) C32_1 0.028(4) 0.036(4) 0.040(4) -0.009(3) -0.006(3) -0.003(3) C33_1 0.022(3) 0.026(4) 0.028(3) -0.003(3) 0.001(3) -0.002(3) C34_1 0.018(3) 0.024(3) 0.031(3) -0.004(3) 0.004(3) -0.002(3) C35_1 0.021(3) 0.032(4) 0.040(4) -0.004(3) 0.002(3) -0.004(3) C36_1 0.024(3) 0.032(4) 0.045(4) -0.002(3) 0.012(3) -0.005(3) C37_1 0.029(4) 0.028(4) 0.037(4) 0.002(3) 0.012(3) 0.002(3) C38_1 0.023(3) 0.021(4) 0.034(3) -0.001(3) 0.009(3) -0.002(2) C39_1 0.020(3) 0.018(3) 0.025(3) -0.004(3) 0.003(3) 0.000(2) C40_1 0.047(5) 0.052(5) 0.036(4) 0.006(4) -0.010(4) -0.007(4) C41_1 0.025(4) 0.060(6) 0.064(6) 0.000(5) 0.016(4) -0.012(4) C42_1 0.037(4) 0.036(4) 0.031(4) 0.018(3) 0.008(3) -0.005(3) Ir2_2 0.02044(11) 0.01994(11) 0.02035(11) 0.00031(10) -0.00125(9) -0.00304(10) F28_2 0.121(5) 0.031(3) 0.072(3) 0.007(3) 0.052(3) 0.019(3) F29_2 0.113(5) 0.082(5) 0.179(7) -0.080(5) 0.113(6) -0.047(4) F30_2 0.163(7) 0.097(5) 0.047(3) -0.047(4) -0.027(4) 0.058(5) F31_2 0.066(4) 0.085(4) 0.091(4) 0.058(4) 0.039(3) 0.013(3) F32_2 0.070(4) 0.053(3) 0.119(5) 0.008(3) 0.069(4) -0.002(3) F33_2 0.034(3) 0.106(5) 0.108(5) 0.010(4) 0.016(3) -0.021(3) F34_2 0.060(3) 0.029(3) 0.065(3) -0.012(2) 0.029(3) -0.023(2) F35_2 0.046(3) 0.058(3) 0.032(2) -0.011(2) 0.0052(19) -0.019(2) F36_2 0.039(2) 0.031(3) 0.054(2) 0.000(2) 0.008(2) 0.000(2) F37_2 0.077(5) 0.254(11) 0.081(4) -0.082(6) -0.047(4) 0.116(6) F38_2 0.145(7) 0.151(8) 0.125(6) -0.096(6) -0.116(5) 0.108(7) F39_2 0.152(9) 0.248(15) 0.154(9) 0.113(11) -0.068(7) 0.024(10) F40_2 0.205(8) 0.060(4) 0.045(3) -0.029(3) 0.037(4) -0.046(5) F41_2 0.110(4) 0.058(4) 0.026(2) -0.002(2) 0.002(2) 0.023(3) F42_2 0.112(5) 0.095(5) 0.050(3) -0.014(3) 0.015(3) 0.058(4) F43_2 0.044(3) 0.031(2) 0.059(3) -0.010(2) -0.007(2) 0.016(2) F44_2 0.031(2) 0.033(2) 0.062(3) -0.010(2) -0.006(2) -0.0015(19) F45_2 0.048(2) 0.045(3) 0.033(2) 0.009(2) -0.0046(19) 0.009(3) F46_2 0.052(3) 0.110(5) 0.035(2) 0.025(3) -0.004(2) -0.005(3) F47_2 0.099(4) 0.066(4) 0.048(3) -0.015(3) -0.039(3) 0.008(3) F48_2 0.044(3) 0.115(5) 0.036(2) 0.015(3) -0.008(2) 0.022(3) F49_2 0.038(3) 0.116(5) 0.088(4) 0.023(4) -0.010(3) -0.035(3) F50_2 0.042(3) 0.049(3) 0.130(5) -0.003(3) 0.016(3) -0.024(3) F51_2 0.035(3) 0.091(5) 0.158(6) -0.070(5) 0.036(3) -0.016(3) F52_2 0.048(3) 0.044(3) 0.046(2) 0.021(2) 0.008(2) -0.013(2) F53_2 0.051(3) 0.053(3) 0.035(2) 0.012(2) 0.0000(19) -0.025(3) F54_2 0.040(3) 0.045(3) 0.063(3) 0.018(3) 0.010(2) 0.010(2) N43_2 0.022(3) 0.027(3) 0.019(2) -0.001(2) -0.001(2) 0.000(2) N57_2 0.025(3) 0.022(3) 0.017(2) 0.001(2) 0.004(2) -0.005(2) N71_2 0.025(3) 0.020(3) 0.022(3) -0.001(2) -0.003(2) -0.006(2) C43_2 0.025(3) 0.031(4) 0.029(3) -0.005(3) -0.001(3) 0.000(3) C44_2 0.035(4) 0.028(4) 0.033(4) -0.003(3) -0.003(3) -0.004(3) C45_2 0.040(4) 0.027(4) 0.022(3) 0.003(3) 0.010(3) 0.001(3) C46_2 0.042(4) 0.026(3) 0.023(3) 0.006(3) 0.008(3) -0.005(3) C47_2 0.027(3) 0.027(3) 0.015(2) 0.003(3) 0.006(2) -0.003(3) C48_2 0.025(3) 0.025(4) 0.020(3) 0.006(3) 0.001(2) -0.002(3) C49_2 0.025(3) 0.031(3) 0.037(3) 0.002(4) 0.009(3) 0.002(3) C50_2 0.030(4) 0.030(4) 0.048(4) 0.015(3) 0.008(3) -0.003(3) C51_2 0.030(4) 0.035(4) 0.031(4) 0.002(3) -0.001(3) -0.011(3) C52_2 0.020(3) 0.021(3) 0.028(3) 0.004(3) 0.000(3) -0.002(3) C53_2 0.023(3) 0.022(3) 0.017(3) 0.003(2) -0.004(2) -0.007(2) C54_2 0.054(5) 0.030(4) 0.030(3) -0.001(4) 0.012(3) -0.006(4) C55_2 0.033(4) 0.046(5) 0.074(6) 0.015(5) 0.025(4) 0.001(4) C56_2 0.038(4) 0.028(4) 0.037(4) 0.001(4) 0.007(3) -0.014(3) C57_2 0.038(4) 0.023(3) 0.021(3) 0.000(3) 0.007(3) 0.001(3) C58_2 0.031(4) 0.032(4) 0.028(3) 0.000(3) 0.002(3) 0.009(3) C59_2 0.030(3) 0.044(5) 0.026(3) 0.003(3) -0.002(3) 0.015(3) C60_2 0.032(4) 0.039(5) 0.029(4) -0.006(3) -0.003(3) 0.001(3) C61_2 0.022(3) 0.023(3) 0.023(3) 0.000(3) 0.005(2) -0.003(3) C62_2 0.021(3) 0.028(4) 0.022(3) 0.001(3) 0.005(3) 0.002(3) C63_2 0.040(4) 0.022(3) 0.031(3) -0.005(3) -0.009(3) 0.014(3) C64_2 0.046(4) 0.030(4) 0.026(3) -0.003(3) 0.008(3) 0.000(3) C65_2 0.033(4) 0.019(4) 0.037(4) 0.004(3) 0.006(3) 0.006(3) C66_2 0.029(4) 0.020(3) 0.031(3) 0.006(3) 0.001(3) 0.002(3) C67_2 0.015(3) 0.023(3) 0.025(3) -0.001(3) 0.000(2) -0.003(2) C68_2 0.067(6) 0.081(7) 0.038(5) -0.011(5) -0.023(5) 0.042(6) C69_2 0.074(6) 0.044(5) 0.029(4) 0.000(4) 0.006(4) 0.015(4) C70_2 0.024(4) 0.026(4) 0.042(4) -0.005(3) -0.003(3) 0.005(3) C71_2 0.030(4) 0.031(4) 0.030(3) 0.003(3) -0.001(3) -0.002(3) C72_2 0.036(4) 0.031(4) 0.028(3) 0.004(3) -0.001(3) 0.003(3) C73_2 0.038(4) 0.036(4) 0.028(3) -0.003(3) -0.007(3) 0.003(3) C74_2 0.021(3) 0.035(4) 0.033(4) 0.001(3) -0.005(3) 0.001(3) C75_2 0.023(3) 0.023(4) 0.031(3) -0.008(3) -0.004(3) -0.001(3) C76_2 0.024(3) 0.021(3) 0.030(3) -0.005(3) 0.001(3) -0.001(3) C77_2 0.025(3) 0.029(4) 0.045(4) -0.003(3) 0.001(3) 0.001(3) C78_2 0.021(3) 0.027(4) 0.054(5) -0.002(3) -0.003(3) -0.004(3) C79_2 0.026(4) 0.021(3) 0.050(4) 0.006(3) 0.012(3) -0.002(3) C80_2 0.027(3) 0.023(4) 0.036(4) -0.003(3) -0.002(3) -0.002(3) C81_2 0.023(3) 0.020(3) 0.032(3) 0.000(3) 0.003(3) 0.001(2) C82_2 0.048(5) 0.049(5) 0.028(4) 0.000(4) -0.004(4) 0.004(4) C83_2 0.022(4) 0.041(5) 0.067(5) -0.002(4) -0.001(4) -0.009(3) C84_2 0.038(4) 0.031(4) 0.036(4) 0.008(3) 0.013(3) -0.006(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_1 N29_1 2.048(5) . ? Ir1_1 N15_1 2.051(5) . ? Ir1_1 C25_1 2.061(6) . ? Ir1_1 C39_1 2.122(7) . ? Ir1_1 N1_1 2.123(5) . ? Ir1_1 C11_1 2.156(7) . ? F1_1 C12_1 1.342(10) . ? F2_1 C12_1 1.278(9) . ? F3_1 C12_1 1.312(10) . ? F4_1 C13_1 1.239(11) . ? F5_1 C13_1 1.300(11) . ? F6_1 C13_1 1.333(11) . ? F7_1 C14_1 1.357(9) . ? F8_1 C14_1 1.331(8) . ? F9_1 C14_1 1.335(9) . ? F10_1 C26_1 1.340(10) . ? F11_1 C26_1 1.311(10) . ? F12_1 C26_1 1.329(12) . ? F13_1 C27_1 1.319(10) . ? F14_1 C27_1 1.322(9) . ? F15_1 C27_1 1.358(10) . ? F16_1 C28_1 1.337(8) . ? F17_1 C28_1 1.343(9) . ? F18_1 C28_1 1.336(8) . ? F19_1 C40_1 1.293(10) . ? F20_1 C40_1 1.310(10) . ? F21_1 C40_1 1.328(11) . ? F22_1 C41_1 1.264(11) . ? F23_1 C41_1 1.261(11) . ? F24_1 C41_1 1.224(11) . ? F25_1 C42_1 1.339(8) . ? F26_1 C42_1 1.333(9) . ? F27_1 C42_1 1.358(9) . ? N1_1 C1_1 1.339(8) . ? N1_1 C5_1 1.362(8) . ? N15_1 C15_1 1.352(8) . ? N15_1 C19_1 1.358(8) . ? N29_1 C29_1 1.353(8) . ? N29_1 C33_1 1.364(8) . ? C1_1 C2_1 1.376(9) . ? C2_1 C3_1 1.382(10) . ? C3_1 C4_1 1.368(10) . ? C3_1 C12_1 1.511(10) . ? C4_1 C5_1 1.397(10) . ? C5_1 C6_1 1.477(10) . ? C6_1 C7_1 1.399(9) . ? C6_1 C11_1 1.412(9) . ? C7_1 C8_1 1.381(11) . ? C8_1 C9_1 1.359(11) . ? C8_1 C13_1 1.489(11) . ? C9_1 C10_1 1.384(10) . ? C10_1 C11_1 1.427(9) . ? C10_1 C14_1 1.515(12) . ? C15_1 C16_1 1.370(9) . ? C16_1 C17_1 1.391(10) . ? C17_1 C18_1 1.347(11) . ? C17_1 C26_1 1.491(10) . ? C18_1 C19_1 1.405(8) . ? C19_1 C20_1 1.458(10) . ? C20_1 C21_1 1.374(9) . ? C20_1 C25_1 1.435(9) . ? C21_1 C22_1 1.366(10) . ? C22_1 C23_1 1.394(9) . ? C22_1 C27_1 1.497(10) . ? C23_1 C24_1 1.388(9) . ? C24_1 C25_1 1.422(9) . ? C24_1 C28_1 1.509(9) . ? C29_1 C30_1 1.392(9) . ? C30_1 C31_1 1.380(10) . ? C31_1 C32_1 1.393(11) . ? C31_1 C40_1 1.506(10) . ? C32_1 C33_1 1.391(9) . ? C33_1 C34_1 1.448(9) . ? C34_1 C39_1 1.422(8) . ? C34_1 C35_1 1.429(9) . ? C35_1 C36_1 1.382(10) . ? C36_1 C37_1 1.381(10) . ? C36_1 C41_1 1.481(10) . ? C37_1 C38_1 1.381(9) . ? C38_1 C39_1 1.410(9) . ? C38_1 C42_1 1.511(9) . ? Ir2_2 N57_2 2.042(5) . ? Ir2_2 C67_2 2.050(6) . ? Ir2_2 N71_2 2.062(5) . ? Ir2_2 C81_2 2.121(7) . ? Ir2_2 N43_2 2.131(6) . ? Ir2_2 C53_2 2.140(6) . ? F28_2 C54_2 1.300(10) . ? F29_2 C54_2 1.281(9) . ? F30_2 C54_2 1.318(8) . ? F31_2 C55_2 1.345(10) . ? F32_2 C55_2 1.331(10) . ? F33_2 C55_2 1.360(10) . ? F34_2 C56_2 1.347(9) . ? F35_2 C56_2 1.353(8) . ? F36_2 C56_2 1.335(8) . ? F37_2 C68_2 1.219(11) . ? F38_2 C68_2 1.274(12) . ? F39_2 C68_2 1.343(16) . ? F40_2 C69_2 1.302(11) . ? F41_2 C69_2 1.326(9) . ? F42_2 C69_2 1.352(11) . ? F43_2 C70_2 1.356(8) . ? F44_2 C70_2 1.340(8) . ? F45_2 C70_2 1.332(9) . ? F46_2 C82_2 1.311(10) . ? F47_2 C82_2 1.333(10) . ? F48_2 C82_2 1.314(10) . ? F49_2 C83_2 1.344(10) . ? F50_2 C83_2 1.304(10) . ? F51_2 C83_2 1.329(10) . ? F52_2 C84_2 1.344(8) . ? F53_2 C84_2 1.342(9) . ? F54_2 C84_2 1.340(9) . ? N43_2 C43_2 1.340(9) . ? N43_2 C47_2 1.355(8) . ? N57_2 C61_2 1.349(8) . ? N57_2 C57_2 1.349(8) . ? N71_2 C71_2 1.344(9) . ? N71_2 C75_2 1.347(8) . ? C43_2 C44_2 1.368(10) . ? C44_2 C45_2 1.358(11) . ? C45_2 C46_2 1.389(10) . ? C45_2 C54_2 1.506(11) . ? C46_2 C47_2 1.387(10) . ? C47_2 C48_2 1.476(10) . ? C48_2 C49_2 1.390(9) . ? C48_2 C53_2 1.427(9) . ? C49_2 C50_2 1.379(10) . ? C50_2 C51_2 1.387(11) . ? C50_2 C55_2 1.463(11) . ? C51_2 C52_2 1.377(10) . ? C52_2 C53_2 1.425(9) . ? C52_2 C56_2 1.493(11) . ? C57_2 C58_2 1.369(9) . ? C58_2 C59_2 1.388(10) . ? C59_2 C60_2 1.361(10) . ? C59_2 C68_2 1.507(10) . ? C60_2 C61_2 1.391(9) . ? C61_2 C62_2 1.460(10) . ? C62_2 C63_2 1.399(9) . ? C62_2 C67_2 1.438(8) . ? C63_2 C64_2 1.347(10) . ? C64_2 C65_2 1.352(9) . ? C64_2 C69_2 1.485(10) . ? C65_2 C66_2 1.406(9) . ? C66_2 C67_2 1.421(9) . ? C66_2 C70_2 1.498(9) . ? C71_2 C72_2 1.397(9) . ? C72_2 C73_2 1.381(10) . ? C73_2 C74_2 1.365(11) . ? C73_2 C82_2 1.505(9) . ? C74_2 C75_2 1.402(9) . ? C75_2 C76_2 1.473(10) . ? C76_2 C77_2 1.378(9) . ? C76_2 C81_2 1.419(9) . ? C77_2 C78_2 1.363(10) . ? C78_2 C79_2 1.389(10) . ? C78_2 C83_2 1.476(10) . ? C79_2 C80_2 1.396(10) . ? C80_2 C81_2 1.412(10) . ? C80_2 C84_2 1.486(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N29_1 Ir1_1 N15_1 173.3(2) . . ? N29_1 Ir1_1 C25_1 104.6(2) . . ? N15_1 Ir1_1 C25_1 81.1(2) . . ? N29_1 Ir1_1 C39_1 79.7(2) . . ? N15_1 Ir1_1 C39_1 104.1(2) . . ? C25_1 Ir1_1 C39_1 89.8(2) . . ? N29_1 Ir1_1 N1_1 83.7(2) . . ? N15_1 Ir1_1 N1_1 90.5(2) . . ? C25_1 Ir1_1 N1_1 171.6(2) . . ? C39_1 Ir1_1 N1_1 91.8(2) . . ? N29_1 Ir1_1 C11_1 91.7(2) . . ? N15_1 Ir1_1 C11_1 83.8(2) . . ? C25_1 Ir1_1 C11_1 100.2(3) . . ? C39_1 Ir1_1 C11_1 168.1(2) . . ? N1_1 Ir1_1 C11_1 79.2(2) . . ? C1_1 N1_1 C5_1 118.8(6) . . ? C1_1 N1_1 Ir1_1 124.9(4) . . ? C5_1 N1_1 Ir1_1 116.2(4) . . ? C15_1 N15_1 C19_1 119.0(5) . . ? C15_1 N15_1 Ir1_1 125.3(4) . . ? C19_1 N15_1 Ir1_1 115.1(4) . . ? C29_1 N29_1 C33_1 118.6(5) . . ? C29_1 N29_1 Ir1_1 123.6(4) . . ? C33_1 N29_1 Ir1_1 116.9(4) . . ? N1_1 C1_1 C2_1 123.4(6) . . ? C1_1 C2_1 C3_1 117.6(6) . . ? C4_1 C3_1 C2_1 120.5(7) . . ? C4_1 C3_1 C12_1 119.9(7) . . ? C2_1 C3_1 C12_1 119.6(7) . . ? C3_1 C4_1 C5_1 119.3(7) . . ? N1_1 C5_1 C4_1 120.4(7) . . ? N1_1 C5_1 C6_1 114.6(6) . . ? C4_1 C5_1 C6_1 124.9(6) . . ? C7_1 C6_1 C11_1 123.5(7) . . ? C7_1 C6_1 C5_1 117.6(6) . . ? C11_1 C6_1 C5_1 118.9(6) . . ? C8_1 C7_1 C6_1 119.8(7) . . ? C9_1 C8_1 C7_1 119.1(6) . . ? C9_1 C8_1 C13_1 121.2(7) . . ? C7_1 C8_1 C13_1 119.5(7) . . ? C8_1 C9_1 C10_1 121.5(7) . . ? C9_1 C10_1 C11_1 122.6(7) . . ? C9_1 C10_1 C14_1 114.8(6) . . ? C11_1 C10_1 C14_1 122.5(6) . . ? C6_1 C11_1 C10_1 113.4(6) . . ? C6_1 C11_1 Ir1_1 111.0(5) . . ? C10_1 C11_1 Ir1_1 135.6(5) . . ? F2_1 C12_1 F3_1 110.8(8) . . ? F2_1 C12_1 F1_1 105.1(7) . . ? F3_1 C12_1 F1_1 102.9(8) . . ? F2_1 C12_1 C3_1 114.2(7) . . ? F3_1 C12_1 C3_1 112.0(6) . . ? F1_1 C12_1 C3_1 110.9(7) . . ? F4_1 C13_1 F5_1 108.6(9) . . ? F4_1 C13_1 F6_1 107.1(9) . . ? F5_1 C13_1 F6_1 99.7(9) . . ? F4_1 C13_1 C8_1 115.0(9) . . ? F5_1 C13_1 C8_1 113.8(7) . . ? F6_1 C13_1 C8_1 111.3(8) . . ? F8_1 C14_1 F9_1 107.8(6) . . ? F8_1 C14_1 F7_1 105.9(6) . . ? F9_1 C14_1 F7_1 104.1(7) . . ? F8_1 C14_1 C10_1 113.6(7) . . ? F9_1 C14_1 C10_1 113.3(6) . . ? F7_1 C14_1 C10_1 111.4(6) . . ? N15_1 C15_1 C16_1 122.5(6) . . ? C15_1 C16_1 C17_1 118.8(7) . . ? C18_1 C17_1 C16_1 119.2(6) . . ? C18_1 C17_1 C26_1 121.3(7) . . ? C16_1 C17_1 C26_1 119.5(7) . . ? C17_1 C18_1 C19_1 120.9(7) . . ? N15_1 C19_1 C18_1 119.5(7) . . ? N15_1 C19_1 C20_1 114.2(5) . . ? C18_1 C19_1 C20_1 126.3(6) . . ? C21_1 C20_1 C25_1 123.0(6) . . ? C21_1 C20_1 C19_1 119.9(6) . . ? C25_1 C20_1 C19_1 117.1(6) . . ? C22_1 C21_1 C20_1 120.4(6) . . ? C21_1 C22_1 C23_1 119.7(6) . . ? C21_1 C22_1 C27_1 120.7(6) . . ? C23_1 C22_1 C27_1 119.6(7) . . ? C24_1 C23_1 C22_1 120.6(7) . . ? C23_1 C24_1 C25_1 121.8(6) . . ? C23_1 C24_1 C28_1 114.9(6) . . ? C25_1 C24_1 C28_1 123.3(6) . . ? C24_1 C25_1 C20_1 114.5(6) . . ? C24_1 C25_1 Ir1_1 134.6(5) . . ? C20_1 C25_1 Ir1_1 110.8(5) . . ? F11_1 C26_1 F12_1 105.8(7) . . ? F11_1 C26_1 F10_1 106.9(8) . . ? F12_1 C26_1 F10_1 104.8(8) . . ? F11_1 C26_1 C17_1 114.3(7) . . ? F12_1 C26_1 C17_1 113.1(8) . . ? F10_1 C26_1 C17_1 111.3(7) . . ? F13_1 C27_1 F14_1 108.3(8) . . ? F13_1 C27_1 F15_1 104.5(7) . . ? F14_1 C27_1 F15_1 104.5(6) . . ? F13_1 C27_1 C22_1 113.3(6) . . ? F14_1 C27_1 C22_1 112.0(6) . . ? F15_1 C27_1 C22_1 113.5(7) . . ? F16_1 C28_1 F18_1 105.2(6) . . ? F16_1 C28_1 F17_1 105.5(6) . . ? F18_1 C28_1 F17_1 105.8(6) . . ? F16_1 C28_1 C24_1 112.7(6) . . ? F18_1 C28_1 C24_1 114.1(6) . . ? F17_1 C28_1 C24_1 112.9(6) . . ? N29_1 C29_1 C30_1 122.9(6) . . ? C31_1 C30_1 C29_1 118.1(7) . . ? C30_1 C31_1 C32_1 119.7(6) . . ? C30_1 C31_1 C40_1 120.5(7) . . ? C32_1 C31_1 C40_1 119.8(7) . . ? C33_1 C32_1 C31_1 119.5(7) . . ? N29_1 C33_1 C32_1 121.0(6) . . ? N29_1 C33_1 C34_1 113.5(5) . . ? C32_1 C33_1 C34_1 125.5(6) . . ? C39_1 C34_1 C35_1 122.4(6) . . ? C39_1 C34_1 C33_1 118.2(6) . . ? C35_1 C34_1 C33_1 119.4(6) . . ? C36_1 C35_1 C34_1 119.4(6) . . ? C37_1 C36_1 C35_1 119.8(6) . . ? C37_1 C36_1 C41_1 120.3(7) . . ? C35_1 C36_1 C41_1 119.8(7) . . ? C38_1 C37_1 C36_1 120.1(7) . . ? C37_1 C38_1 C39_1 124.2(6) . . ? C37_1 C38_1 C42_1 115.1(6) . . ? C39_1 C38_1 C42_1 120.7(6) . . ? C38_1 C39_1 C34_1 114.1(6) . . ? C38_1 C39_1 Ir1_1 135.7(5) . . ? C34_1 C39_1 Ir1_1 110.2(5) . . ? F19_1 C40_1 F20_1 109.7(8) . . ? F19_1 C40_1 F21_1 106.8(8) . . ? F20_1 C40_1 F21_1 103.5(7) . . ? F19_1 C40_1 C31_1 112.7(7) . . ? F20_1 C40_1 C31_1 112.5(7) . . ? F21_1 C40_1 C31_1 111.2(7) . . ? F24_1 C41_1 F23_1 100.9(11) . . ? F24_1 C41_1 F22_1 108.2(10) . . ? F23_1 C41_1 F22_1 102.8(10) . . ? F24_1 C41_1 C36_1 114.9(8) . . ? F23_1 C41_1 C36_1 113.9(8) . . ? F22_1 C41_1 C36_1 114.7(8) . . ? F26_1 C42_1 F25_1 105.9(6) . . ? F26_1 C42_1 F27_1 107.0(6) . . ? F25_1 C42_1 F27_1 105.4(6) . . ? F26_1 C42_1 C38_1 113.0(6) . . ? F25_1 C42_1 C38_1 113.1(6) . . ? F27_1 C42_1 C38_1 111.9(6) . . ? N57_2 Ir2_2 C67_2 80.9(2) . . ? N57_2 Ir2_2 N71_2 174.3(2) . . ? C67_2 Ir2_2 N71_2 103.7(2) . . ? N57_2 Ir2_2 C81_2 104.0(2) . . ? C67_2 Ir2_2 C81_2 89.0(2) . . ? N71_2 Ir2_2 C81_2 79.7(2) . . ? N57_2 Ir2_2 N43_2 91.8(2) . . ? C67_2 Ir2_2 N43_2 172.6(2) . . ? N71_2 Ir2_2 N43_2 83.7(2) . . ? C81_2 Ir2_2 N43_2 91.9(2) . . ? N57_2 Ir2_2 C53_2 83.2(2) . . ? C67_2 Ir2_2 C53_2 100.3(2) . . ? N71_2 Ir2_2 C53_2 92.5(2) . . ? C81_2 Ir2_2 C53_2 169.1(2) . . ? N43_2 Ir2_2 C53_2 79.6(2) . . ? C43_2 N43_2 C47_2 118.6(6) . . ? C43_2 N43_2 Ir2_2 126.1(5) . . ? C47_2 N43_2 Ir2_2 115.1(5) . . ? C61_2 N57_2 C57_2 118.9(6) . . ? C61_2 N57_2 Ir2_2 116.1(4) . . ? C57_2 N57_2 Ir2_2 124.7(4) . . ? C71_2 N71_2 C75_2 120.5(5) . . ? C71_2 N71_2 Ir2_2 122.5(4) . . ? C75_2 N71_2 Ir2_2 116.0(4) . . ? N43_2 C43_2 C44_2 123.8(7) . . ? C45_2 C44_2 C43_2 118.4(7) . . ? C44_2 C45_2 C46_2 119.2(7) . . ? C44_2 C45_2 C54_2 121.1(7) . . ? C46_2 C45_2 C54_2 119.7(7) . . ? C47_2 C46_2 C45_2 120.3(7) . . ? N43_2 C47_2 C46_2 119.8(6) . . ? N43_2 C47_2 C48_2 115.9(6) . . ? C46_2 C47_2 C48_2 124.3(6) . . ? C49_2 C48_2 C53_2 122.9(6) . . ? C49_2 C48_2 C47_2 119.2(6) . . ? C53_2 C48_2 C47_2 117.8(5) . . ? C50_2 C49_2 C48_2 121.1(7) . . ? C49_2 C50_2 C51_2 118.4(7) . . ? C49_2 C50_2 C55_2 121.0(8) . . ? C51_2 C50_2 C55_2 120.6(7) . . ? C52_2 C51_2 C50_2 120.6(7) . . ? C51_2 C52_2 C53_2 123.9(7) . . ? C51_2 C52_2 C56_2 113.2(6) . . ? C53_2 C52_2 C56_2 122.8(6) . . ? C48_2 C53_2 C52_2 113.0(6) . . ? C48_2 C53_2 Ir2_2 111.2(4) . . ? C52_2 C53_2 Ir2_2 135.8(5) . . ? F29_2 C54_2 F28_2 108.2(8) . . ? F29_2 C54_2 F30_2 106.0(7) . . ? F28_2 C54_2 F30_2 104.3(8) . . ? F29_2 C54_2 C45_2 114.3(7) . . ? F28_2 C54_2 C45_2 112.3(6) . . ? F30_2 C54_2 C45_2 111.1(7) . . ? F32_2 C55_2 F31_2 106.4(8) . . ? F32_2 C55_2 F33_2 104.9(7) . . ? F31_2 C55_2 F33_2 104.5(7) . . ? F32_2 C55_2 C50_2 115.3(7) . . ? F31_2 C55_2 C50_2 112.5(7) . . ? F33_2 C55_2 C50_2 112.4(8) . . ? F36_2 C56_2 F34_2 104.6(7) . . ? F36_2 C56_2 F35_2 106.5(6) . . ? F34_2 C56_2 F35_2 104.5(6) . . ? F36_2 C56_2 C52_2 113.0(6) . . ? F34_2 C56_2 C52_2 113.0(6) . . ? F35_2 C56_2 C52_2 114.3(7) . . ? N57_2 C57_2 C58_2 123.3(6) . . ? C57_2 C58_2 C59_2 117.1(6) . . ? C60_2 C59_2 C58_2 120.5(6) . . ? C60_2 C59_2 C68_2 122.0(7) . . ? C58_2 C59_2 C68_2 117.5(7) . . ? C59_2 C60_2 C61_2 119.6(7) . . ? N57_2 C61_2 C60_2 120.4(7) . . ? N57_2 C61_2 C62_2 114.0(5) . . ? C60_2 C61_2 C62_2 125.6(6) . . ? C63_2 C62_2 C67_2 122.1(6) . . ? C63_2 C62_2 C61_2 121.4(6) . . ? C67_2 C62_2 C61_2 116.4(6) . . ? C64_2 C63_2 C62_2 121.3(6) . . ? C63_2 C64_2 C65_2 119.2(7) . . ? C63_2 C64_2 C69_2 120.0(7) . . ? C65_2 C64_2 C69_2 120.8(7) . . ? C64_2 C65_2 C66_2 122.4(7) . . ? C65_2 C66_2 C67_2 121.0(6) . . ? C65_2 C66_2 C70_2 115.0(6) . . ? C67_2 C66_2 C70_2 124.0(6) . . ? C66_2 C67_2 C62_2 114.1(6) . . ? C66_2 C67_2 Ir2_2 134.4(5) . . ? C62_2 C67_2 Ir2_2 111.5(5) . . ? F37_2 C68_2 F38_2 112.4(10) . . ? F37_2 C68_2 F39_2 101.3(11) . . ? F38_2 C68_2 F39_2 100.2(10) . . ? F37_2 C68_2 C59_2 116.7(8) . . ? F38_2 C68_2 C59_2 114.0(8) . . ? F39_2 C68_2 C59_2 110.2(10) . . ? F40_2 C69_2 F41_2 107.8(8) . . ? F40_2 C69_2 F42_2 104.2(8) . . ? F41_2 C69_2 F42_2 103.8(7) . . ? F40_2 C69_2 C64_2 113.3(7) . . ? F41_2 C69_2 C64_2 113.5(7) . . ? F42_2 C69_2 C64_2 113.5(7) . . ? F45_2 C70_2 F44_2 106.0(6) . . ? F45_2 C70_2 F43_2 104.8(6) . . ? F44_2 C70_2 F43_2 104.8(5) . . ? F45_2 C70_2 C66_2 114.4(6) . . ? F44_2 C70_2 C66_2 112.7(6) . . ? F43_2 C70_2 C66_2 113.2(6) . . ? N71_2 C71_2 C72_2 121.5(7) . . ? C73_2 C72_2 C71_2 118.4(7) . . ? C74_2 C73_2 C72_2 119.5(6) . . ? C74_2 C73_2 C82_2 120.5(7) . . ? C72_2 C73_2 C82_2 120.0(7) . . ? C73_2 C74_2 C75_2 120.6(7) . . ? N71_2 C75_2 C74_2 119.4(6) . . ? N71_2 C75_2 C76_2 115.6(5) . . ? C74_2 C75_2 C76_2 125.0(6) . . ? C77_2 C76_2 C81_2 123.6(7) . . ? C77_2 C76_2 C75_2 120.4(6) . . ? C81_2 C76_2 C75_2 115.9(6) . . ? C78_2 C77_2 C76_2 120.0(6) . . ? C77_2 C78_2 C79_2 119.5(7) . . ? C77_2 C78_2 C83_2 120.8(7) . . ? C79_2 C78_2 C83_2 119.7(7) . . ? C78_2 C79_2 C80_2 120.6(7) . . ? C79_2 C80_2 C81_2 121.8(6) . . ? C79_2 C80_2 C84_2 115.4(7) . . ? C81_2 C80_2 C84_2 122.9(6) . . ? C80_2 C81_2 C76_2 114.4(6) . . ? C80_2 C81_2 Ir2_2 134.0(5) . . ? C76_2 C81_2 Ir2_2 111.6(5) . . ? F48_2 C82_2 F46_2 106.8(7) . . ? F48_2 C82_2 F47_2 107.2(7) . . ? F46_2 C82_2 F47_2 106.1(7) . . ? F48_2 C82_2 C73_2 112.8(7) . . ? F46_2 C82_2 C73_2 114.2(7) . . ? F47_2 C82_2 C73_2 109.3(7) . . ? F50_2 C83_2 F51_2 107.3(8) . . ? F50_2 C83_2 F49_2 104.5(7) . . ? F51_2 C83_2 F49_2 104.1(7) . . ? F50_2 C83_2 C78_2 114.7(7) . . ? F51_2 C83_2 C78_2 112.7(7) . . ? F49_2 C83_2 C78_2 112.7(7) . . ? F54_2 C84_2 F53_2 106.8(6) . . ? F54_2 C84_2 F52_2 106.1(6) . . ? F53_2 C84_2 F52_2 104.8(6) . . ? F54_2 C84_2 C80_2 112.7(6) . . ? F53_2 C84_2 C80_2 112.9(6) . . ? F52_2 C84_2 C80_2 113.0(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 N29_1 Ir1_1 N1_1 C1_1 88.8(5) . . . . ? N15_1 Ir1_1 N1_1 C1_1 -94.8(5) . . . . ? C25_1 Ir1_1 N1_1 C1_1 -91.6(16) . . . . ? C39_1 Ir1_1 N1_1 C1_1 9.4(5) . . . . ? C11_1 Ir1_1 N1_1 C1_1 -178.3(5) . . . . ? N29_1 Ir1_1 N1_1 C5_1 -95.5(4) . . . . ? N15_1 Ir1_1 N1_1 C5_1 80.9(4) . . . . ? C25_1 Ir1_1 N1_1 C5_1 84.2(17) . . . . ? C39_1 Ir1_1 N1_1 C5_1 -174.9(4) . . . . ? C11_1 Ir1_1 N1_1 C5_1 -2.6(4) . . . . ? N29_1 Ir1_1 N15_1 C15_1 34(2) . . . . ? C25_1 Ir1_1 N15_1 C15_1 -177.0(6) . . . . ? C39_1 Ir1_1 N15_1 C15_1 -89.4(5) . . . . ? N1_1 Ir1_1 N15_1 C15_1 2.5(5) . . . . ? C11_1 Ir1_1 N15_1 C15_1 81.6(5) . . . . ? N29_1 Ir1_1 N15_1 C19_1 -136.5(17) . . . . ? C25_1 Ir1_1 N15_1 C19_1 12.2(5) . . . . ? C39_1 Ir1_1 N15_1 C19_1 99.8(5) . . . . ? N1_1 Ir1_1 N15_1 C19_1 -168.3(5) . . . . ? C11_1 Ir1_1 N15_1 C19_1 -89.2(5) . . . . ? N15_1 Ir1_1 N29_1 C29_1 55(2) . . . . ? C25_1 Ir1_1 N29_1 C29_1 -93.2(6) . . . . ? C39_1 Ir1_1 N29_1 C29_1 179.7(6) . . . . ? N1_1 Ir1_1 N29_1 C29_1 86.7(5) . . . . ? C11_1 Ir1_1 N29_1 C29_1 7.8(6) . . . . ? N15_1 Ir1_1 N29_1 C33_1 -113.9(19) . . . . ? C25_1 Ir1_1 N29_1 C33_1 98.1(5) . . . . ? C39_1 Ir1_1 N29_1 C33_1 11.0(5) . . . . ? N1_1 Ir1_1 N29_1 C33_1 -81.9(5) . . . . ? C11_1 Ir1_1 N29_1 C33_1 -160.9(5) . . . . ? C5_1 N1_1 C1_1 C2_1 2.4(10) . . . . ? Ir1_1 N1_1 C1_1 C2_1 178.0(5) . . . . ? N1_1 C1_1 C2_1 C3_1 -0.6(11) . . . . ? C1_1 C2_1 C3_1 C4_1 0.5(10) . . . . ? C1_1 C2_1 C3_1 C12_1 178.3(7) . . . . ? C2_1 C3_1 C4_1 C5_1 -2.2(11) . . . . ? C12_1 C3_1 C4_1 C5_1 -179.9(6) . . . . ? C1_1 N1_1 C5_1 C4_1 -4.0(9) . . . . ? Ir1_1 N1_1 C5_1 C4_1 180.0(5) . . . . ? C1_1 N1_1 C5_1 C6_1 179.1(5) . . . . ? Ir1_1 N1_1 C5_1 C6_1 3.1(7) . . . . ? C3_1 C4_1 C5_1 N1_1 4.0(10) . . . . ? C3_1 C4_1 C5_1 C6_1 -179.5(6) . . . . ? N1_1 C5_1 C6_1 C7_1 178.3(6) . . . . ? C4_1 C5_1 C6_1 C7_1 1.6(10) . . . . ? N1_1 C5_1 C6_1 C11_1 -1.7(8) . . . . ? C4_1 C5_1 C6_1 C11_1 -178.4(6) . . . . ? C11_1 C6_1 C7_1 C8_1 0.0(10) . . . . ? C5_1 C6_1 C7_1 C8_1 -180.0(6) . . . . ? C6_1 C7_1 C8_1 C9_1 1.0(11) . . . . ? C6_1 C7_1 C8_1 C13_1 176.2(7) . . . . ? C7_1 C8_1 C9_1 C10_1 0.1(11) . . . . ? C13_1 C8_1 C9_1 C10_1 -175.0(7) . . . . ? C8_1 C9_1 C10_1 C11_1 -2.3(11) . . . . ? C8_1 C9_1 C10_1 C14_1 174.2(7) . . . . ? C7_1 C6_1 C11_1 C10_1 -1.9(9) . . . . ? C5_1 C6_1 C11_1 C10_1 178.1(6) . . . . ? C7_1 C6_1 C11_1 Ir1_1 179.5(5) . . . . ? C5_1 C6_1 C11_1 Ir1_1 -0.5(7) . . . . ? C9_1 C10_1 C11_1 C6_1 3.0(9) . . . . ? C14_1 C10_1 C11_1 C6_1 -173.1(6) . . . . ? C9_1 C10_1 C11_1 Ir1_1 -178.9(5) . . . . ? C14_1 C10_1 C11_1 Ir1_1 4.9(11) . . . . ? N29_1 Ir1_1 C11_1 C6_1 84.9(4) . . . . ? N15_1 Ir1_1 C11_1 C6_1 -90.2(4) . . . . ? C25_1 Ir1_1 C11_1 C6_1 -169.9(4) . . . . ? C39_1 Ir1_1 C11_1 C6_1 42.3(15) . . . . ? N1_1 Ir1_1 C11_1 C6_1 1.6(4) . . . . ? N29_1 Ir1_1 C11_1 C10_1 -93.2(7) . . . . ? N15_1 Ir1_1 C11_1 C10_1 91.7(7) . . . . ? C25_1 Ir1_1 C11_1 C10_1 12.0(7) . . . . ? C39_1 Ir1_1 C11_1 C10_1 -135.8(11) . . . . ? N1_1 Ir1_1 C11_1 C10_1 -176.5(7) . . . . ? C4_1 C3_1 C12_1 F2_1 2.5(11) . . . . ? C2_1 C3_1 C12_1 F2_1 -175.2(8) . . . . ? C4_1 C3_1 C12_1 F3_1 -124.5(8) . . . . ? C2_1 C3_1 C12_1 F3_1 57.7(10) . . . . ? C4_1 C3_1 C12_1 F1_1 121.1(8) . . . . ? C2_1 C3_1 C12_1 F1_1 -56.7(9) . . . . ? C9_1 C8_1 C13_1 F4_1 76.6(12) . . . . ? C7_1 C8_1 C13_1 F4_1 -98.5(11) . . . . ? C9_1 C8_1 C13_1 F5_1 -157.2(9) . . . . ? C7_1 C8_1 C13_1 F5_1 27.7(13) . . . . ? C9_1 C8_1 C13_1 F6_1 -45.5(12) . . . . ? C7_1 C8_1 C13_1 F6_1 139.4(9) . . . . ? C9_1 C10_1 C14_1 F8_1 104.1(7) . . . . ? C11_1 C10_1 C14_1 F8_1 -79.5(8) . . . . ? C9_1 C10_1 C14_1 F9_1 -132.5(7) . . . . ? C11_1 C10_1 C14_1 F9_1 43.9(10) . . . . ? C9_1 C10_1 C14_1 F7_1 -15.5(9) . . . . ? C11_1 C10_1 C14_1 F7_1 160.9(6) . . . . ? C19_1 N15_1 C15_1 C16_1 3.6(10) . . . . ? Ir1_1 N15_1 C15_1 C16_1 -166.9(5) . . . . ? N15_1 C15_1 C16_1 C17_1 -0.6(11) . . . . ? C15_1 C16_1 C17_1 C18_1 -1.2(11) . . . . ? C15_1 C16_1 C17_1 C26_1 177.3(7) . . . . ? C16_1 C17_1 C18_1 C19_1 0.1(11) . . . . ? C26_1 C17_1 C18_1 C19_1 -178.4(7) . . . . ? C15_1 N15_1 C19_1 C18_1 -4.7(10) . . . . ? Ir1_1 N15_1 C19_1 C18_1 166.8(5) . . . . ? C15_1 N15_1 C19_1 C20_1 174.4(6) . . . . ? Ir1_1 N15_1 C19_1 C20_1 -14.2(7) . . . . ? C17_1 C18_1 C19_1 N15_1 2.9(11) . . . . ? C17_1 C18_1 C19_1 C20_1 -176.0(7) . . . . ? N15_1 C19_1 C20_1 C21_1 -170.6(7) . . . . ? C18_1 C19_1 C20_1 C21_1 8.3(11) . . . . ? N15_1 C19_1 C20_1 C25_1 7.9(9) . . . . ? C18_1 C19_1 C20_1 C25_1 -173.2(7) . . . . ? C25_1 C20_1 C21_1 C22_1 0.6(12) . . . . ? C19_1 C20_1 C21_1 C22_1 179.1(7) . . . . ? C20_1 C21_1 C22_1 C23_1 -3.2(12) . . . . ? C20_1 C21_1 C22_1 C27_1 175.1(7) . . . . ? C21_1 C22_1 C23_1 C24_1 2.9(11) . . . . ? C27_1 C22_1 C23_1 C24_1 -175.5(7) . . . . ? C22_1 C23_1 C24_1 C25_1 0.1(11) . . . . ? C22_1 C23_1 C24_1 C28_1 178.4(7) . . . . ? C23_1 C24_1 C25_1 C20_1 -2.5(10) . . . . ? C28_1 C24_1 C25_1 C20_1 179.3(7) . . . . ? C23_1 C24_1 C25_1 Ir1_1 179.6(5) . . . . ? C28_1 C24_1 C25_1 Ir1_1 1.4(11) . . . . ? C21_1 C20_1 C25_1 C24_1 2.2(10) . . . . ? C19_1 C20_1 C25_1 C24_1 -176.3(6) . . . . ? C21_1 C20_1 C25_1 Ir1_1 -179.4(6) . . . . ? C19_1 C20_1 C25_1 Ir1_1 2.1(8) . . . . ? N29_1 Ir1_1 C25_1 C24_1 -12.9(7) . . . . ? N15_1 Ir1_1 C25_1 C24_1 170.7(7) . . . . ? C39_1 Ir1_1 C25_1 C24_1 66.3(7) . . . . ? N1_1 Ir1_1 C25_1 C24_1 167.4(13) . . . . ? C11_1 Ir1_1 C25_1 C24_1 -107.4(7) . . . . ? N29_1 Ir1_1 C25_1 C20_1 169.1(5) . . . . ? N15_1 Ir1_1 C25_1 C20_1 -7.3(5) . . . . ? C39_1 Ir1_1 C25_1 C20_1 -111.6(5) . . . . ? N1_1 Ir1_1 C25_1 C20_1 -10.6(19) . . . . ? C11_1 Ir1_1 C25_1 C20_1 74.7(5) . . . . ? C18_1 C17_1 C26_1 F11_1 0.8(13) . . . . ? C16_1 C17_1 C26_1 F11_1 -177.7(8) . . . . ? C18_1 C17_1 C26_1 F12_1 -120.4(9) . . . . ? C16_1 C17_1 C26_1 F12_1 61.2(10) . . . . ? C18_1 C17_1 C26_1 F10_1 122.1(9) . . . . ? C16_1 C17_1 C26_1 F10_1 -56.4(12) . . . . ? C21_1 C22_1 C27_1 F13_1 -97.4(9) . . . . ? C23_1 C22_1 C27_1 F13_1 80.9(10) . . . . ? C21_1 C22_1 C27_1 F14_1 25.5(11) . . . . ? C23_1 C22_1 C27_1 F14_1 -156.1(7) . . . . ? C21_1 C22_1 C27_1 F15_1 143.6(7) . . . . ? C23_1 C22_1 C27_1 F15_1 -38.1(10) . . . . ? C23_1 C24_1 C28_1 F16_1 -0.8(9) . . . . ? C25_1 C24_1 C28_1 F16_1 177.5(6) . . . . ? C23_1 C24_1 C28_1 F18_1 -120.6(7) . . . . ? C25_1 C24_1 C28_1 F18_1 57.6(9) . . . . ? C23_1 C24_1 C28_1 F17_1 118.6(7) . . . . ? C25_1 C24_1 C28_1 F17_1 -63.2(9) . . . . ? C33_1 N29_1 C29_1 C30_1 3.5(11) . . . . ? Ir1_1 N29_1 C29_1 C30_1 -165.0(6) . . . . ? N29_1 C29_1 C30_1 C31_1 -0.5(12) . . . . ? C29_1 C30_1 C31_1 C32_1 -3.3(12) . . . . ? C29_1 C30_1 C31_1 C40_1 176.8(8) . . . . ? C30_1 C31_1 C32_1 C33_1 4.1(12) . . . . ? C40_1 C31_1 C32_1 C33_1 -176.0(7) . . . . ? C29_1 N29_1 C33_1 C32_1 -2.7(10) . . . . ? Ir1_1 N29_1 C33_1 C32_1 166.6(5) . . . . ? C29_1 N29_1 C33_1 C34_1 177.1(6) . . . . ? Ir1_1 N29_1 C33_1 C34_1 -13.7(7) . . . . ? C31_1 C32_1 C33_1 N29_1 -1.0(11) . . . . ? C31_1 C32_1 C33_1 C34_1 179.2(7) . . . . ? N29_1 C33_1 C34_1 C39_1 8.4(9) . . . . ? C32_1 C33_1 C34_1 C39_1 -171.9(7) . . . . ? N29_1 C33_1 C34_1 C35_1 -170.1(6) . . . . ? C32_1 C33_1 C34_1 C35_1 9.6(11) . . . . ? C39_1 C34_1 C35_1 C36_1 -0.4(10) . . . . ? C33_1 C34_1 C35_1 C36_1 178.0(6) . . . . ? C34_1 C35_1 C36_1 C37_1 1.6(11) . . . . ? C34_1 C35_1 C36_1 C41_1 -179.2(7) . . . . ? C35_1 C36_1 C37_1 C38_1 -1.5(11) . . . . ? C41_1 C36_1 C37_1 C38_1 179.4(7) . . . . ? C36_1 C37_1 C38_1 C39_1 0.0(11) . . . . ? C36_1 C37_1 C38_1 C42_1 177.7(7) . . . . ? C37_1 C38_1 C39_1 C34_1 1.1(10) . . . . ? C42_1 C38_1 C39_1 C34_1 -176.4(6) . . . . ? C37_1 C38_1 C39_1 Ir1_1 -178.7(5) . . . . ? C42_1 C38_1 C39_1 Ir1_1 3.7(10) . . . . ? C35_1 C34_1 C39_1 C38_1 -0.9(9) . . . . ? C33_1 C34_1 C39_1 C38_1 -179.4(6) . . . . ? C35_1 C34_1 C39_1 Ir1_1 179.0(5) . . . . ? C33_1 C34_1 C39_1 Ir1_1 0.5(7) . . . . ? N29_1 Ir1_1 C39_1 C38_1 174.1(7) . . . . ? N15_1 Ir1_1 C39_1 C38_1 -11.6(7) . . . . ? C25_1 Ir1_1 C39_1 C38_1 69.2(7) . . . . ? N1_1 Ir1_1 C39_1 C38_1 -102.6(7) . . . . ? C11_1 Ir1_1 C39_1 C38_1 -142.5(11) . . . . ? N29_1 Ir1_1 C39_1 C34_1 -5.8(4) . . . . ? N15_1 Ir1_1 C39_1 C34_1 168.5(4) . . . . ? C25_1 Ir1_1 C39_1 C34_1 -110.7(5) . . . . ? N1_1 Ir1_1 C39_1 C34_1 77.5(5) . . . . ? C11_1 Ir1_1 C39_1 C34_1 37.6(15) . . . . ? C30_1 C31_1 C40_1 F19_1 -19.2(13) . . . . ? C32_1 C31_1 C40_1 F19_1 160.9(9) . . . . ? C30_1 C31_1 C40_1 F20_1 -143.8(9) . . . . ? C32_1 C31_1 C40_1 F20_1 36.3(12) . . . . ? C30_1 C31_1 C40_1 F21_1 100.6(10) . . . . ? C32_1 C31_1 C40_1 F21_1 -79.3(10) . . . . ? C37_1 C36_1 C41_1 F24_1 -66.6(14) . . . . ? C35_1 C36_1 C41_1 F24_1 114.2(11) . . . . ? C37_1 C36_1 C41_1 F23_1 177.7(11) . . . . ? C35_1 C36_1 C41_1 F23_1 -1.5(15) . . . . ? C37_1 C36_1 C41_1 F22_1 59.7(13) . . . . ? C35_1 C36_1 C41_1 F22_1 -119.5(10) . . . . ? C37_1 C38_1 C42_1 F26_1 122.2(7) . . . . ? C39_1 C38_1 C42_1 F26_1 -60.0(9) . . . . ? C37_1 C38_1 C42_1 F25_1 1.8(10) . . . . ? C39_1 C38_1 C42_1 F25_1 179.6(6) . . . . ? C37_1 C38_1 C42_1 F27_1 -117.0(7) . . . . ? C39_1 C38_1 C42_1 F27_1 60.8(9) . . . . ? N57_2 Ir2_2 N43_2 C43_2 97.7(5) . . . . ? C67_2 Ir2_2 N43_2 C43_2 90.6(19) . . . . ? N71_2 Ir2_2 N43_2 C43_2 -85.9(5) . . . . ? C81_2 Ir2_2 N43_2 C43_2 -6.5(5) . . . . ? C53_2 Ir2_2 N43_2 C43_2 -179.6(5) . . . . ? N57_2 Ir2_2 N43_2 C47_2 -76.3(4) . . . . ? C67_2 Ir2_2 N43_2 C47_2 -83.4(19) . . . . ? N71_2 Ir2_2 N43_2 C47_2 100.1(4) . . . . ? C81_2 Ir2_2 N43_2 C47_2 179.5(4) . . . . ? C53_2 Ir2_2 N43_2 C47_2 6.4(4) . . . . ? C67_2 Ir2_2 N57_2 C61_2 -9.8(5) . . . . ? N71_2 Ir2_2 N57_2 C61_2 133(2) . . . . ? C81_2 Ir2_2 N57_2 C61_2 -96.5(5) . . . . ? N43_2 Ir2_2 N57_2 C61_2 171.1(5) . . . . ? C53_2 Ir2_2 N57_2 C61_2 91.8(5) . . . . ? C67_2 Ir2_2 N57_2 C57_2 177.7(5) . . . . ? N71_2 Ir2_2 N57_2 C57_2 -40(2) . . . . ? C81_2 Ir2_2 N57_2 C57_2 91.0(5) . . . . ? N43_2 Ir2_2 N57_2 C57_2 -1.4(5) . . . . ? C53_2 Ir2_2 N57_2 C57_2 -80.7(5) . . . . ? N57_2 Ir2_2 N71_2 C71_2 -47(2) . . . . ? C67_2 Ir2_2 N71_2 C71_2 95.2(6) . . . . ? C81_2 Ir2_2 N71_2 C71_2 -178.4(6) . . . . ? N43_2 Ir2_2 N71_2 C71_2 -85.3(6) . . . . ? C53_2 Ir2_2 N71_2 C71_2 -6.1(6) . . . . ? N57_2 Ir2_2 N71_2 C75_2 122(2) . . . . ? C67_2 Ir2_2 N71_2 C75_2 -96.2(5) . . . . ? C81_2 Ir2_2 N71_2 C75_2 -9.7(5) . . . . ? N43_2 Ir2_2 N71_2 C75_2 83.4(5) . . . . ? C53_2 Ir2_2 N71_2 C75_2 162.6(5) . . . . ? C47_2 N43_2 C43_2 C44_2 -1.4(10) . . . . ? Ir2_2 N43_2 C43_2 C44_2 -175.2(5) . . . . ? N43_2 C43_2 C44_2 C45_2 1.9(11) . . . . ? C43_2 C44_2 C45_2 C46_2 -1.1(10) . . . . ? C43_2 C44_2 C45_2 C54_2 178.8(6) . . . . ? C44_2 C45_2 C46_2 C47_2 -0.1(10) . . . . ? C54_2 C45_2 C46_2 C47_2 180.0(6) . . . . ? C43_2 N43_2 C47_2 C46_2 0.1(9) . . . . ? Ir2_2 N43_2 C47_2 C46_2 174.6(5) . . . . ? C43_2 N43_2 C47_2 C48_2 178.9(5) . . . . ? Ir2_2 N43_2 C47_2 C48_2 -6.6(6) . . . . ? C45_2 C46_2 C47_2 N43_2 0.6(9) . . . . ? C45_2 C46_2 C47_2 C48_2 -178.1(6) . . . . ? N43_2 C47_2 C48_2 C49_2 -174.3(5) . . . . ? C46_2 C47_2 C48_2 C49_2 4.5(9) . . . . ? N43_2 C47_2 C48_2 C53_2 2.3(8) . . . . ? C46_2 C47_2 C48_2 C53_2 -178.9(6) . . . . ? C53_2 C48_2 C49_2 C50_2 1.9(10) . . . . ? C47_2 C48_2 C49_2 C50_2 178.4(6) . . . . ? C48_2 C49_2 C50_2 C51_2 -1.7(10) . . . . ? C48_2 C49_2 C50_2 C55_2 -178.0(7) . . . . ? C49_2 C50_2 C51_2 C52_2 -0.7(11) . . . . ? C55_2 C50_2 C51_2 C52_2 175.7(7) . . . . ? C50_2 C51_2 C52_2 C53_2 3.0(11) . . . . ? C50_2 C51_2 C52_2 C56_2 -175.0(6) . . . . ? C49_2 C48_2 C53_2 C52_2 0.2(9) . . . . ? C47_2 C48_2 C53_2 C52_2 -176.3(5) . . . . ? C49_2 C48_2 C53_2 Ir2_2 179.5(5) . . . . ? C47_2 C48_2 C53_2 Ir2_2 3.0(7) . . . . ? C51_2 C52_2 C53_2 C48_2 -2.7(9) . . . . ? C56_2 C52_2 C53_2 C48_2 175.1(6) . . . . ? C51_2 C52_2 C53_2 Ir2_2 178.2(5) . . . . ? C56_2 C52_2 C53_2 Ir2_2 -3.9(10) . . . . ? N57_2 Ir2_2 C53_2 C48_2 88.3(4) . . . . ? C67_2 Ir2_2 C53_2 C48_2 167.7(4) . . . . ? N71_2 Ir2_2 C53_2 C48_2 -88.0(4) . . . . ? C81_2 Ir2_2 C53_2 C48_2 -43.9(15) . . . . ? N43_2 Ir2_2 C53_2 C48_2 -4.8(4) . . . . ? N57_2 Ir2_2 C53_2 C52_2 -92.7(6) . . . . ? C67_2 Ir2_2 C53_2 C52_2 -13.3(7) . . . . ? N71_2 Ir2_2 C53_2 C52_2 91.1(6) . . . . ? C81_2 Ir2_2 C53_2 C52_2 135.2(12) . . . . ? N43_2 Ir2_2 C53_2 C52_2 174.3(6) . . . . ? C44_2 C45_2 C54_2 F29_2 -179.1(8) . . . . ? C46_2 C45_2 C54_2 F29_2 0.8(11) . . . . ? C44_2 C45_2 C54_2 F28_2 -55.4(9) . . . . ? C46_2 C45_2 C54_2 F28_2 124.5(8) . . . . ? C44_2 C45_2 C54_2 F30_2 61.0(10) . . . . ? C46_2 C45_2 C54_2 F30_2 -119.1(8) . . . . ? C49_2 C50_2 C55_2 F32_2 -16.2(12) . . . . ? C51_2 C50_2 C55_2 F32_2 167.6(8) . . . . ? C49_2 C50_2 C55_2 F31_2 106.1(9) . . . . ? C51_2 C50_2 C55_2 F31_2 -70.2(10) . . . . ? C49_2 C50_2 C55_2 F33_2 -136.4(8) . . . . ? C51_2 C50_2 C55_2 F33_2 47.4(10) . . . . ? C51_2 C52_2 C56_2 F36_2 132.1(6) . . . . ? C53_2 C52_2 C56_2 F36_2 -46.0(9) . . . . ? C51_2 C52_2 C56_2 F34_2 13.6(9) . . . . ? C53_2 C52_2 C56_2 F34_2 -164.5(6) . . . . ? C51_2 C52_2 C56_2 F35_2 -105.8(7) . . . . ? C53_2 C52_2 C56_2 F35_2 76.1(8) . . . . ? C61_2 N57_2 C57_2 C58_2 -1.9(10) . . . . ? Ir2_2 N57_2 C57_2 C58_2 170.4(6) . . . . ? N57_2 C57_2 C58_2 C59_2 -1.9(11) . . . . ? C57_2 C58_2 C59_2 C60_2 3.2(11) . . . . ? C57_2 C58_2 C59_2 C68_2 -176.2(8) . . . . ? C58_2 C59_2 C60_2 C61_2 -1.0(12) . . . . ? C68_2 C59_2 C60_2 C61_2 178.4(9) . . . . ? C57_2 N57_2 C61_2 C60_2 4.2(9) . . . . ? Ir2_2 N57_2 C61_2 C60_2 -168.7(5) . . . . ? C57_2 N57_2 C61_2 C62_2 -175.5(6) . . . . ? Ir2_2 N57_2 C61_2 C62_2 11.6(7) . . . . ? C59_2 C60_2 C61_2 N57_2 -2.8(11) . . . . ? C59_2 C60_2 C61_2 C62_2 176.8(7) . . . . ? N57_2 C61_2 C62_2 C63_2 169.0(7) . . . . ? C60_2 C61_2 C62_2 C63_2 -10.6(11) . . . . ? N57_2 C61_2 C62_2 C67_2 -6.5(9) . . . . ? C60_2 C61_2 C62_2 C67_2 173.8(7) . . . . ? C67_2 C62_2 C63_2 C64_2 -0.4(12) . . . . ? C61_2 C62_2 C63_2 C64_2 -175.7(7) . . . . ? C62_2 C63_2 C64_2 C65_2 0.9(12) . . . . ? C62_2 C63_2 C64_2 C69_2 -176.5(8) . . . . ? C63_2 C64_2 C65_2 C66_2 -1.2(12) . . . . ? C69_2 C64_2 C65_2 C66_2 176.2(7) . . . . ? C64_2 C65_2 C66_2 C67_2 1.0(11) . . . . ? C64_2 C65_2 C66_2 C70_2 -178.2(7) . . . . ? C65_2 C66_2 C67_2 C62_2 -0.4(10) . . . . ? C70_2 C66_2 C67_2 C62_2 178.7(6) . . . . ? C65_2 C66_2 C67_2 Ir2_2 175.9(5) . . . . ? C70_2 C66_2 C67_2 Ir2_2 -5.0(11) . . . . ? C63_2 C62_2 C67_2 C66_2 0.2(10) . . . . ? C61_2 C62_2 C67_2 C66_2 175.7(6) . . . . ? C63_2 C62_2 C67_2 Ir2_2 -177.0(6) . . . . ? C61_2 C62_2 C67_2 Ir2_2 -1.5(8) . . . . ? N57_2 Ir2_2 C67_2 C66_2 -170.7(7) . . . . ? N71_2 Ir2_2 C67_2 C66_2 12.9(7) . . . . ? C81_2 Ir2_2 C67_2 C66_2 -66.3(7) . . . . ? N43_2 Ir2_2 C67_2 C66_2 -163.6(15) . . . . ? C53_2 Ir2_2 C67_2 C66_2 108.0(7) . . . . ? N57_2 Ir2_2 C67_2 C62_2 5.7(5) . . . . ? N71_2 Ir2_2 C67_2 C62_2 -170.8(5) . . . . ? C81_2 Ir2_2 C67_2 C62_2 110.1(5) . . . . ? N43_2 Ir2_2 C67_2 C62_2 13(2) . . . . ? C53_2 Ir2_2 C67_2 C62_2 -75.6(5) . . . . ? C60_2 C59_2 C68_2 F37_2 -144.6(11) . . . . ? C58_2 C59_2 C68_2 F37_2 34.9(16) . . . . ? C60_2 C59_2 C68_2 F38_2 -11.0(16) . . . . ? C58_2 C59_2 C68_2 F38_2 168.5(10) . . . . ? C60_2 C59_2 C68_2 F39_2 100.7(12) . . . . ? C58_2 C59_2 C68_2 F39_2 -79.9(12) . . . . ? C63_2 C64_2 C69_2 F40_2 93.4(10) . . . . ? C65_2 C64_2 C69_2 F40_2 -83.9(11) . . . . ? C63_2 C64_2 C69_2 F41_2 -29.9(12) . . . . ? C65_2 C64_2 C69_2 F41_2 152.8(8) . . . . ? C63_2 C64_2 C69_2 F42_2 -148.1(8) . . . . ? C65_2 C64_2 C69_2 F42_2 34.6(11) . . . . ? C65_2 C66_2 C70_2 F45_2 123.8(7) . . . . ? C67_2 C66_2 C70_2 F45_2 -55.3(9) . . . . ? C65_2 C66_2 C70_2 F44_2 -114.9(7) . . . . ? C67_2 C66_2 C70_2 F44_2 66.0(9) . . . . ? C65_2 C66_2 C70_2 F43_2 3.9(9) . . . . ? C67_2 C66_2 C70_2 F43_2 -175.2(6) . . . . ? C75_2 N71_2 C71_2 C72_2 -0.4(11) . . . . ? Ir2_2 N71_2 C71_2 C72_2 167.8(6) . . . . ? N71_2 C71_2 C72_2 C73_2 -2.5(12) . . . . ? C71_2 C72_2 C73_2 C74_2 3.8(12) . . . . ? C71_2 C72_2 C73_2 C82_2 -176.4(7) . . . . ? C72_2 C73_2 C74_2 C75_2 -2.4(12) . . . . ? C82_2 C73_2 C74_2 C75_2 177.7(7) . . . . ? C71_2 N71_2 C75_2 C74_2 1.8(10) . . . . ? Ir2_2 N71_2 C75_2 C74_2 -167.1(5) . . . . ? C71_2 N71_2 C75_2 C76_2 -179.0(6) . . . . ? Ir2_2 N71_2 C75_2 C76_2 12.1(8) . . . . ? C73_2 C74_2 C75_2 N71_2 -0.4(11) . . . . ? C73_2 C74_2 C75_2 C76_2 -179.5(7) . . . . ? N71_2 C75_2 C76_2 C77_2 169.9(6) . . . . ? C74_2 C75_2 C76_2 C77_2 -11.0(11) . . . . ? N71_2 C75_2 C76_2 C81_2 -7.3(9) . . . . ? C74_2 C75_2 C76_2 C81_2 171.9(7) . . . . ? C81_2 C76_2 C77_2 C78_2 -1.8(11) . . . . ? C75_2 C76_2 C77_2 C78_2 -178.7(6) . . . . ? C76_2 C77_2 C78_2 C79_2 -0.3(11) . . . . ? C76_2 C77_2 C78_2 C83_2 178.9(7) . . . . ? C77_2 C78_2 C79_2 C80_2 0.3(11) . . . . ? C83_2 C78_2 C79_2 C80_2 -178.9(7) . . . . ? C78_2 C79_2 C80_2 C81_2 1.8(11) . . . . ? C78_2 C79_2 C80_2 C84_2 -177.1(7) . . . . ? C79_2 C80_2 C81_2 C76_2 -3.6(10) . . . . ? C84_2 C80_2 C81_2 C76_2 175.3(6) . . . . ? C79_2 C80_2 C81_2 Ir2_2 178.4(6) . . . . ? C84_2 C80_2 C81_2 Ir2_2 -2.7(11) . . . . ? C77_2 C76_2 C81_2 C80_2 3.7(10) . . . . ? C75_2 C76_2 C81_2 C80_2 -179.3(6) . . . . ? C77_2 C76_2 C81_2 Ir2_2 -177.9(5) . . . . ? C75_2 C76_2 C81_2 Ir2_2 -0.9(7) . . . . ? N57_2 Ir2_2 C81_2 C80_2 7.8(7) . . . . ? C67_2 Ir2_2 C81_2 C80_2 -72.6(7) . . . . ? N71_2 Ir2_2 C81_2 C80_2 -176.6(7) . . . . ? N43_2 Ir2_2 C81_2 C80_2 100.1(7) . . . . ? C53_2 Ir2_2 C81_2 C80_2 138.4(12) . . . . ? N57_2 Ir2_2 C81_2 C76_2 -170.2(5) . . . . ? C67_2 Ir2_2 C81_2 C76_2 109.4(5) . . . . ? N71_2 Ir2_2 C81_2 C76_2 5.4(5) . . . . ? N43_2 Ir2_2 C81_2 C76_2 -77.9(5) . . . . ? C53_2 Ir2_2 C81_2 C76_2 -39.6(16) . . . . ? C74_2 C73_2 C82_2 F48_2 56.1(11) . . . . ? C72_2 C73_2 C82_2 F48_2 -123.8(9) . . . . ? C74_2 C73_2 C82_2 F46_2 178.2(7) . . . . ? C72_2 C73_2 C82_2 F46_2 -1.6(11) . . . . ? C74_2 C73_2 C82_2 F47_2 -63.1(10) . . . . ? C72_2 C73_2 C82_2 F47_2 117.1(9) . . . . ? C77_2 C78_2 C83_2 F50_2 136.5(8) . . . . ? C79_2 C78_2 C83_2 F50_2 -44.3(11) . . . . ? C77_2 C78_2 C83_2 F51_2 -100.4(10) . . . . ? C79_2 C78_2 C83_2 F51_2 78.8(10) . . . . ? C77_2 C78_2 C83_2 F49_2 17.1(11) . . . . ? C79_2 C78_2 C83_2 F49_2 -163.7(7) . . . . ? C79_2 C80_2 C84_2 F54_2 117.8(7) . . . . ? C81_2 C80_2 C84_2 F54_2 -61.2(9) . . . . ? C79_2 C80_2 C84_2 F53_2 -121.2(7) . . . . ? C81_2 C80_2 C84_2 F53_2 59.9(9) . . . . ? C79_2 C80_2 C84_2 F52_2 -2.5(10) . . . . ? C81_2 C80_2 C84_2 F52_2 178.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 2.596 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.122 #===END #===END data_03137 _database_code_depnum_ccdc_archive 'CCDC 257685' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H29 F18 Ir N2 O2' _chemical_formula_weight 1091.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 20.852(4) _cell_length_b 16.227(3) _cell_length_c 24.092(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8152(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rect _exptl_crystal_colour gold _exptl_crystal_size_max .24 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .05 _exptl_crystal_density_meas multirun _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 3.395 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50219 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9831 _reflns_number_gt 6483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+21.2656P] 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 9831 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.009 _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 Ir1 Ir 0.215009(9) 0.120841(11) 0.282046(8) 0.01587(7) Uani 1 1 d . . . F1 F 0.2775(2) 0.4328(3) 0.09325(18) 0.0681(14) Uani 1 1 d . . . F2 F 0.2784(5) 0.3267(3) 0.0447(2) 0.156(4) Uani 1 1 d . . . F3 F 0.1924(3) 0.3879(4) 0.0597(3) 0.126(3) Uani 1 1 d . . . F4 F 0.0748(2) -0.0718(3) 0.05710(19) 0.0795(16) Uani 1 1 d . . . F5 F 0.0304(2) 0.0459(2) 0.04653(15) 0.0551(11) Uani 1 1 d . . . F6 F -0.01430(19) -0.0458(3) 0.09706(16) 0.0563(12) Uani 1 1 d . . . F7 F 0.05555(18) -0.1064(2) 0.27584(14) 0.0407(9) Uani 1 1 d . . . F8 F 0.09358(15) -0.00974(19) 0.32656(12) 0.0285(7) Uani 1 1 d . . . F9 F 0.15717(17) -0.09770(19) 0.28840(13) 0.0350(8) Uani 1 1 d . . . F10 F 0.2967(2) -0.1919(2) 0.46704(18) 0.0703(14) Uani 1 1 d . . . F11 F 0.3365(4) -0.0854(4) 0.4999(3) 0.134(3) Uani 1 1 d . . . F12 F 0.2420(3) -0.1177(4) 0.5184(2) 0.118(3) Uani 1 1 d . . . F13 F 0.0713(3) 0.2393(6) 0.5273(2) 0.168(4) Uani 1 1 d . . . F14 F 0.0118(4) 0.1533(4) 0.5093(3) 0.169(4) Uani 1 1 d . . . F15 F -0.0042(4) 0.2667(6) 0.4821(2) 0.188(5) Uani 1 1 d . . . F16 F 0.03357(18) 0.3183(2) 0.29683(15) 0.0454(10) Uani 1 1 d . . . F17 F 0.07661(16) 0.2278(2) 0.24409(13) 0.0336(8) Uani 1 1 d . . . F18 F 0.13434(18) 0.3264(2) 0.27767(14) 0.0371(8) Uani 1 1 d . . . O1 O 0.28842(17) 0.0756(2) 0.23022(14) 0.0225(8) Uani 1 1 d . . . O2 O 0.28457(16) 0.1788(2) 0.33242(14) 0.0221(8) Uani 1 1 d . . . N1 N 0.21618(19) 0.2108(2) 0.22339(17) 0.0184(9) Uani 1 1 d . . . N15 N 0.2291(2) 0.0315(2) 0.33982(17) 0.0193(9) Uani 1 1 d . . . C1 C 0.2517(3) 0.2806(3) 0.2279(2) 0.0261(13) Uani 1 1 d . . . H1A H 0.2694 0.2941 0.2621 0.031 Uiso 1 1 calc R . . C2 C 0.2623(3) 0.3317(4) 0.1836(3) 0.0333(14) Uani 1 1 d . . . H2A H 0.2872 0.3788 0.1874 0.040 Uiso 1 1 calc R . . C3 C 0.2350(3) 0.3113(3) 0.1333(2) 0.0286(13) Uani 1 1 d . . . C4 C 0.1982(3) 0.2411(3) 0.1279(2) 0.0247(12) Uani 1 1 d . . . H4A H 0.1800 0.2274 0.0939 0.030 Uiso 1 1 calc R . . C5 C 0.1887(2) 0.1910(3) 0.1740(2) 0.0203(11) Uani 1 1 d . . . C6 C 0.1513(2) 0.1148(3) 0.1755(2) 0.0174(10) Uani 1 1 d . . . C7 C 0.1162(3) 0.0890(3) 0.1296(2) 0.0226(11) Uani 1 1 d . . . H7A H 0.1179 0.1188 0.0966 0.027 Uiso 1 1 calc R . . C8 C 0.0789(3) 0.0188(3) 0.1331(2) 0.0241(12) Uani 1 1 d . . . C9 C 0.0757(3) -0.0245(3) 0.1827(2) 0.0253(12) Uani 1 1 d . . . H9A H 0.0501 -0.0713 0.1852 0.030 Uiso 1 1 calc R . . C10 C 0.1104(2) 0.0013(3) 0.2289(2) 0.0189(11) Uani 1 1 d . . . C11 C 0.1514(2) 0.0704(3) 0.2274(2) 0.0196(11) Uani 1 1 d . . . C12 C 0.2475(4) 0.3642(4) 0.0826(3) 0.0489(19) Uani 1 1 d . . . C13 C 0.0427(3) -0.0131(4) 0.0832(3) 0.0346(14) Uani 1 1 d . . . C14 C 0.1038(3) -0.0518(3) 0.2797(2) 0.0254(12) Uani 1 1 d . . . C15 C 0.2720(3) -0.0304(3) 0.3338(2) 0.0250(12) Uani 1 1 d . . . H15A H 0.2902 -0.0398 0.2991 0.030 Uiso 1 1 calc R . . C16 C 0.2897(3) -0.0803(4) 0.3780(2) 0.0305(13) Uani 1 1 d . . . H16A H 0.3189 -0.1229 0.3730 0.037 Uiso 1 1 calc R . . C17 C 0.2631(3) -0.0653(3) 0.4293(2) 0.0272(12) Uani 1 1 d . . . C18 C 0.2189(3) -0.0020(3) 0.4362(2) 0.0255(12) Uani 1 1 d . . . H18A H 0.2006 0.0081 0.4707 0.031 Uiso 1 1 calc R . . C19 C 0.2027(2) 0.0459(3) 0.3904(2) 0.0197(11) Uani 1 1 d . . . C20 C 0.1565(2) 0.1151(3) 0.3902(2) 0.0208(11) Uani 1 1 d . . . C21 C 0.1207(3) 0.1319(3) 0.4377(2) 0.0234(11) Uani 1 1 d . . . H21A H 0.1266 0.1012 0.4699 0.028 Uiso 1 1 calc R . . C22 C 0.0762(3) 0.1952(3) 0.4362(2) 0.0269(12) Uani 1 1 d . . . C23 C 0.0670(3) 0.2395(3) 0.3882(2) 0.0261(12) Uani 1 1 d . . . H23A H 0.0370 0.2818 0.3876 0.031 Uiso 1 1 calc R . . C24 C 0.1024(2) 0.2213(3) 0.3403(2) 0.0207(11) Uani 1 1 d . . . C25 C 0.1500(2) 0.1586(3) 0.3394(2) 0.0192(10) Uani 1 1 d . . . C26 C 0.2845(4) -0.1149(4) 0.4788(3) 0.0443(18) Uani 1 1 d . . . C27 C 0.0377(3) 0.2145(4) 0.4868(3) 0.0403(16) Uani 1 1 d . . . C28 C 0.0870(3) 0.2721(3) 0.2897(2) 0.0279(13) Uani 1 1 d . . . C29 C 0.3878(3) 0.0720(4) 0.1830(2) 0.0299(13) Uani 1 1 d . . . C30 C 0.3475(3) 0.0986(3) 0.2335(2) 0.0250(12) Uani 1 1 d . . . C31 C 0.3729(3) 0.1375(3) 0.2787(2) 0.0291(13) Uani 1 1 d . . . H31A H 0.4173 0.1420 0.2775 0.035 Uiso 1 1 calc R . . C32 C 0.3457(3) 0.1716(3) 0.3260(2) 0.0253(12) Uani 1 1 d . . . C33 C 0.3853(3) 0.1973(4) 0.3769(2) 0.0280(13) Uani 1 1 d . . . C34 C 0.3923(4) -0.0213(4) 0.1829(3) 0.062(2) Uani 1 1 d . . . H34A H 0.3500 -0.0445 0.1816 0.093 Uiso 1 1 calc R . . H34B H 0.4136 -0.0395 0.2161 0.093 Uiso 1 1 calc R . . H34C H 0.4163 -0.0391 0.1511 0.093 Uiso 1 1 calc R . . C35 C 0.4562(3) 0.1080(5) 0.1833(3) 0.061(2) Uani 1 1 d . . . H35A H 0.4777 0.0920 0.2169 0.092 Uiso 1 1 calc R . . H35B H 0.4540 0.1670 0.1813 0.092 Uiso 1 1 calc R . . H35C H 0.4796 0.0873 0.1519 0.092 Uiso 1 1 calc R . . C36 C 0.3542(4) 0.1019(6) 0.1307(3) 0.066(3) Uani 1 1 d . . . H36A H 0.3121 0.0780 0.1287 0.099 Uiso 1 1 calc R . . H36B H 0.3786 0.0857 0.0987 0.099 Uiso 1 1 calc R . . H36C H 0.3506 0.1609 0.1317 0.099 Uiso 1 1 calc R . . C37 C 0.3587(3) 0.2763(4) 0.4020(3) 0.0426(16) Uani 1 1 d . . . H37A H 0.3136 0.2699 0.4088 0.064 Uiso 1 1 calc R . . H37B H 0.3654 0.3212 0.3767 0.064 Uiso 1 1 calc R . . H37C H 0.3803 0.2878 0.4363 0.064 Uiso 1 1 calc R . . C38 C 0.3770(3) 0.1258(4) 0.4188(3) 0.0425(16) Uani 1 1 d . . . H38A H 0.3327 0.1212 0.4291 0.064 Uiso 1 1 calc R . . H38B H 0.4024 0.1366 0.4513 0.064 Uiso 1 1 calc R . . H38C H 0.3909 0.0752 0.4021 0.064 Uiso 1 1 calc R . . C39 C 0.4572(3) 0.2091(5) 0.3640(3) 0.0445(17) Uani 1 1 d . . . H39A H 0.4621 0.2502 0.3356 0.067 Uiso 1 1 calc R . . H39B H 0.4750 0.1579 0.3513 0.067 Uiso 1 1 calc R . . H39C H 0.4792 0.2266 0.3969 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01353(10) 0.02060(10) 0.01347(11) -0.00080(8) -0.00112(8) 0.00053(8) F1 0.096(4) 0.053(2) 0.055(3) 0.021(2) -0.010(3) -0.040(3) F2 0.345(12) 0.058(3) 0.064(4) 0.007(3) 0.116(6) -0.021(5) F3 0.107(5) 0.166(6) 0.106(5) 0.105(5) -0.067(4) -0.075(4) F4 0.075(3) 0.094(4) 0.069(3) -0.060(3) -0.026(3) 0.021(3) F5 0.070(3) 0.064(3) 0.031(2) 0.0066(19) -0.024(2) -0.028(2) F6 0.048(2) 0.076(3) 0.045(2) 0.004(2) -0.018(2) -0.034(2) F7 0.045(2) 0.0391(19) 0.038(2) 0.0083(16) -0.0079(17) -0.0274(17) F8 0.0287(18) 0.0351(17) 0.0217(17) 0.0004(14) 0.0042(14) -0.0024(14) F9 0.039(2) 0.0300(17) 0.036(2) 0.0044(14) 0.0019(16) 0.0118(15) F10 0.115(4) 0.045(2) 0.051(3) 0.016(2) -0.005(3) 0.033(2) F11 0.171(7) 0.117(5) 0.114(5) 0.063(4) -0.119(5) -0.055(5) F12 0.178(6) 0.136(5) 0.041(3) 0.050(3) 0.049(4) 0.112(5) F13 0.080(5) 0.351(12) 0.073(4) -0.116(6) 0.032(4) -0.017(6) F14 0.256(10) 0.088(4) 0.162(7) -0.030(4) 0.183(7) -0.035(5) F15 0.223(8) 0.281(9) 0.060(4) 0.057(5) 0.079(5) 0.216(8) F16 0.045(2) 0.053(2) 0.039(2) 0.0017(18) -0.0009(18) 0.0332(19) F17 0.0327(19) 0.045(2) 0.0234(18) -0.0045(15) -0.0075(15) 0.0080(16) F18 0.046(2) 0.0303(17) 0.035(2) 0.0081(15) -0.0007(17) -0.0031(16) O1 0.0170(18) 0.032(2) 0.0184(19) -0.0044(15) 0.0007(16) -0.0015(16) O2 0.0173(18) 0.0286(18) 0.021(2) -0.0019(15) -0.0029(16) 0.0008(16) N1 0.016(2) 0.023(2) 0.017(2) -0.0006(17) -0.0018(19) -0.0029(17) N15 0.019(2) 0.024(2) 0.016(2) 0.0001(18) -0.0007(18) 0.0013(17) C1 0.026(3) 0.024(3) 0.028(3) 0.002(2) -0.006(2) -0.007(2) C2 0.035(3) 0.028(3) 0.037(4) 0.006(3) -0.007(3) -0.012(3) C3 0.030(3) 0.030(3) 0.025(3) 0.004(2) -0.001(3) -0.006(2) C4 0.026(3) 0.028(3) 0.020(3) 0.000(2) -0.004(2) -0.002(2) C5 0.018(3) 0.024(3) 0.018(3) -0.002(2) -0.001(2) -0.001(2) C6 0.023(3) 0.017(2) 0.012(2) 0.0003(19) -0.001(2) 0.002(2) C7 0.022(3) 0.029(3) 0.017(3) -0.002(2) -0.004(2) 0.003(2) C8 0.019(3) 0.032(3) 0.021(3) -0.007(2) -0.004(2) -0.002(2) C9 0.025(3) 0.025(3) 0.026(3) -0.008(2) -0.003(2) -0.002(2) C10 0.020(3) 0.019(2) 0.018(3) -0.001(2) -0.001(2) 0.000(2) C11 0.017(2) 0.023(2) 0.019(3) -0.005(2) -0.001(2) 0.003(2) C12 0.064(5) 0.057(5) 0.026(4) 0.007(3) -0.009(4) -0.027(4) C13 0.038(4) 0.039(3) 0.026(3) -0.008(3) -0.010(3) -0.009(3) C14 0.026(3) 0.023(3) 0.027(3) 0.001(2) -0.003(3) -0.006(2) C15 0.027(3) 0.029(3) 0.019(3) -0.001(2) 0.001(2) 0.010(2) C16 0.032(3) 0.031(3) 0.028(3) -0.001(2) -0.004(3) 0.010(3) C17 0.032(3) 0.024(3) 0.026(3) 0.001(2) -0.006(3) 0.002(2) C18 0.033(3) 0.027(3) 0.017(3) 0.003(2) 0.002(2) 0.002(2) C19 0.022(3) 0.021(2) 0.016(3) 0.000(2) -0.004(2) 0.001(2) C20 0.016(2) 0.030(3) 0.017(3) -0.002(2) -0.002(2) -0.004(2) C21 0.026(3) 0.030(3) 0.014(3) -0.002(2) 0.002(2) 0.001(2) C22 0.021(3) 0.035(3) 0.025(3) -0.006(2) 0.003(2) 0.003(2) C23 0.021(3) 0.031(3) 0.026(3) -0.007(2) 0.001(2) 0.005(2) C24 0.016(2) 0.022(2) 0.024(3) -0.002(2) 0.001(2) -0.002(2) C25 0.018(2) 0.026(3) 0.015(3) -0.002(2) -0.003(2) -0.005(2) C26 0.069(5) 0.039(4) 0.025(3) 0.004(3) -0.006(4) 0.021(4) C27 0.042(4) 0.054(4) 0.025(4) -0.006(3) 0.011(3) 0.013(3) C28 0.023(3) 0.030(3) 0.030(3) -0.003(2) -0.003(3) 0.007(2) C29 0.019(3) 0.042(3) 0.029(3) -0.001(3) 0.005(3) 0.003(3) C30 0.019(3) 0.031(3) 0.025(3) 0.001(2) 0.002(2) 0.005(2) C31 0.032(3) 0.039(3) 0.016(3) -0.005(2) -0.009(2) 0.020(3) C32 0.022(3) 0.029(3) 0.024(3) 0.008(2) -0.007(2) -0.004(2) C33 0.022(3) 0.039(3) 0.023(3) 0.000(2) -0.010(2) -0.007(2) C34 0.064(5) 0.052(4) 0.069(6) -0.012(4) 0.033(5) 0.005(4) C35 0.033(4) 0.090(6) 0.060(5) -0.024(4) 0.022(4) -0.008(4) C36 0.054(5) 0.122(7) 0.023(4) 0.009(4) 0.015(4) 0.026(5) C37 0.048(4) 0.047(4) 0.033(4) -0.012(3) -0.015(3) -0.002(3) C38 0.042(4) 0.050(4) 0.035(4) 0.013(3) -0.019(3) -0.006(3) C39 0.026(3) 0.071(5) 0.036(4) -0.008(3) -0.013(3) -0.010(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 C25 2.030(5) . ? Ir1 N15 2.031(4) . ? Ir1 N1 2.032(4) . ? Ir1 C11 2.039(5) . ? Ir1 O1 2.108(3) . ? Ir1 O2 2.112(3) . ? F1 C12 1.302(7) . ? F2 C12 1.273(9) . ? F3 C12 1.330(10) . ? F4 C13 1.323(7) . ? F5 C13 1.328(7) . ? F6 C13 1.343(7) . ? F7 C14 1.344(6) . ? F8 C14 1.337(6) . ? F9 C14 1.356(6) . ? F10 C26 1.306(7) . ? F11 C26 1.291(9) . ? F12 C26 1.302(9) . ? F13 C27 1.268(8) . ? F14 C27 1.254(8) . ? F15 C27 1.221(8) . ? F16 C28 1.353(6) . ? F17 C28 1.331(6) . ? F18 C28 1.354(7) . ? O1 C30 1.290(6) . ? O2 C32 1.289(6) . ? N1 C1 1.356(6) . ? N1 C5 1.360(6) . ? N15 C15 1.353(6) . ? N15 C19 1.356(6) . ? C1 C2 1.369(8) . ? C2 C3 1.381(8) . ? C3 C4 1.379(8) . ? C3 C12 1.514(8) . ? C4 C5 1.389(7) . ? C5 C6 1.463(7) . ? C6 C7 1.392(7) . ? C6 C11 1.443(7) . ? C7 C8 1.382(7) . ? C8 C9 1.388(7) . ? C8 C13 1.512(7) . ? C9 C10 1.391(7) . ? C10 C11 1.410(7) . ? C10 C14 1.503(7) . ? C15 C16 1.386(7) . ? C16 C17 1.377(8) . ? C17 C18 1.390(8) . ? C17 C26 1.505(8) . ? C18 C19 1.393(7) . ? C19 C20 1.480(7) . ? C20 C21 1.393(7) . ? C20 C25 1.419(7) . ? C21 C22 1.384(7) . ? C22 C23 1.374(8) . ? C22 C27 1.494(8) . ? C23 C24 1.401(7) . ? C24 C25 1.423(7) . ? C24 C28 1.507(7) . ? C29 C34 1.518(9) . ? C29 C36 1.522(9) . ? C29 C30 1.539(8) . ? C29 C35 1.541(9) . ? C30 C31 1.366(7) . ? C31 C32 1.390(7) . ? C32 C33 1.536(7) . ? C33 C37 1.523(8) . ? C33 C39 1.543(8) . ? C33 C38 1.548(8) . ? 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 C25 Ir1 N15 81.11(18) . . ? C25 Ir1 N1 105.34(18) . . ? N15 Ir1 N1 170.99(17) . . ? C25 Ir1 C11 97.3(2) . . ? N15 Ir1 C11 104.45(18) . . ? N1 Ir1 C11 81.24(18) . . ? C25 Ir1 O1 173.37(17) . . ? N15 Ir1 O1 92.99(15) . . ? N1 Ir1 O1 80.19(15) . . ? C11 Ir1 O1 87.12(17) . . ? C25 Ir1 O2 86.17(17) . . ? N15 Ir1 O2 79.92(15) . . ? N1 Ir1 O2 94.08(15) . . ? C11 Ir1 O2 174.78(17) . . ? O1 Ir1 O2 89.82(14) . . ? C30 O1 Ir1 123.9(3) . . ? C32 O2 Ir1 124.7(3) . . ? C1 N1 C5 119.8(4) . . ? C1 N1 Ir1 123.4(4) . . ? C5 N1 Ir1 115.7(3) . . ? C15 N15 C19 119.5(4) . . ? C15 N15 Ir1 123.5(4) . . ? C19 N15 Ir1 115.7(3) . . ? N1 C1 C2 122.1(5) . . ? C1 C2 C3 118.2(5) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 C12 119.3(5) . . ? C2 C3 C12 120.1(5) . . ? C3 C4 C5 119.2(5) . . ? N1 C5 C4 120.0(5) . . ? N1 C5 C6 113.7(4) . . ? C4 C5 C6 126.3(5) . . ? C7 C6 C11 122.7(5) . . ? C7 C6 C5 120.9(4) . . ? C11 C6 C5 116.4(4) . . ? C8 C7 C6 119.7(5) . . ? C7 C8 C9 119.8(5) . . ? C7 C8 C13 121.0(5) . . ? C9 C8 C13 119.2(5) . . ? C8 C9 C10 120.7(5) . . ? C9 C10 C11 122.4(5) . . ? C9 C10 C14 115.4(5) . . ? C11 C10 C14 122.1(4) . . ? C10 C11 C6 114.7(4) . . ? C10 C11 Ir1 134.2(4) . . ? C6 C11 Ir1 111.1(3) . . ? F2 C12 F1 107.9(7) . . ? F2 C12 F3 106.1(7) . . ? F1 C12 F3 104.4(7) . . ? F2 C12 C3 113.2(6) . . ? F1 C12 C3 114.1(6) . . ? F3 C12 C3 110.5(6) . . ? F4 C13 F5 107.5(5) . . ? F4 C13 F6 106.4(5) . . ? F5 C13 F6 106.3(5) . . ? F4 C13 C8 111.8(5) . . ? F5 C13 C8 112.2(5) . . ? F6 C13 C8 112.3(5) . . ? F8 C14 F7 106.0(4) . . ? F8 C14 F9 106.2(4) . . ? F7 C14 F9 105.2(4) . . ? F8 C14 C10 114.2(4) . . ? F7 C14 C10 113.0(4) . . ? F9 C14 C10 111.5(5) . . ? N15 C15 C16 121.8(5) . . ? C17 C16 C15 118.7(5) . . ? C16 C17 C18 120.3(5) . . ? C16 C17 C26 119.9(5) . . ? C18 C17 C26 119.8(5) . . ? C17 C18 C19 118.6(5) . . ? N15 C19 C18 121.1(5) . . ? N15 C19 C20 113.1(4) . . ? C18 C19 C20 125.7(5) . . ? C21 C20 C25 124.1(5) . . ? C21 C20 C19 119.7(5) . . ? C25 C20 C19 116.2(4) . . ? C22 C21 C20 118.9(5) . . ? C23 C22 C21 120.3(5) . . ? C23 C22 C27 120.1(5) . . ? C21 C22 C27 119.7(5) . . ? C22 C23 C24 120.6(5) . . ? C23 C24 C25 122.1(5) . . ? C23 C24 C28 116.1(5) . . ? C25 C24 C28 121.8(5) . . ? C20 C25 C24 114.1(5) . . ? C20 C25 Ir1 111.9(4) . . ? C24 C25 Ir1 133.9(4) . . ? F11 C26 F12 107.2(7) . . ? F11 C26 F10 106.0(6) . . ? F12 C26 F10 105.0(6) . . ? F11 C26 C17 111.2(6) . . ? F12 C26 C17 113.4(6) . . ? F10 C26 C17 113.5(5) . . ? F15 C27 F14 106.4(8) . . ? F15 C27 F13 104.3(8) . . ? F14 C27 F13 99.0(7) . . ? F15 C27 C22 117.0(6) . . ? F14 C27 C22 114.7(6) . . ? F13 C27 C22 113.5(6) . . ? F17 C28 F16 105.7(4) . . ? F17 C28 F18 107.1(5) . . ? F16 C28 F18 105.5(4) . . ? F17 C28 C24 114.0(4) . . ? F16 C28 C24 112.0(5) . . ? F18 C28 C24 111.9(4) . . ? C34 C29 C36 110.2(6) . . ? C34 C29 C30 108.3(5) . . ? C36 C29 C30 108.2(5) . . ? C34 C29 C35 108.7(6) . . ? C36 C29 C35 108.0(6) . . ? C30 C29 C35 113.3(5) . . ? O1 C30 C31 123.5(5) . . ? O1 C30 C29 113.1(5) . . ? C31 C30 C29 123.2(5) . . ? C30 C31 C32 132.9(6) . . ? O2 C32 C31 122.6(5) . . ? O2 C32 C33 114.4(5) . . ? C31 C32 C33 122.9(5) . . ? C37 C33 C32 110.4(5) . . ? C37 C33 C39 109.3(5) . . ? C32 C33 C39 113.3(5) . . ? C37 C33 C38 109.4(5) . . ? C32 C33 C38 104.9(4) . . ? C39 C33 C38 109.5(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 C25 Ir1 O1 C30 -62.7(16) . . . . ? N15 Ir1 O1 C30 -89.9(4) . . . . ? N1 Ir1 O1 C30 84.2(4) . . . . ? C11 Ir1 O1 C30 165.8(4) . . . . ? O2 Ir1 O1 C30 -10.0(4) . . . . ? C25 Ir1 O2 C32 169.8(4) . . . . ? N15 Ir1 O2 C32 88.2(4) . . . . ? N1 Ir1 O2 C32 -85.1(4) . . . . ? C11 Ir1 O2 C32 -59.1(19) . . . . ? O1 Ir1 O2 C32 -4.9(4) . . . . ? C25 Ir1 N1 C1 83.8(4) . . . . ? N15 Ir1 N1 C1 -51.2(12) . . . . ? C11 Ir1 N1 C1 179.0(4) . . . . ? O1 Ir1 N1 C1 -92.5(4) . . . . ? O2 Ir1 N1 C1 -3.4(4) . . . . ? C25 Ir1 N1 C5 -108.2(4) . . . . ? N15 Ir1 N1 C5 116.8(10) . . . . ? C11 Ir1 N1 C5 -13.0(4) . . . . ? O1 Ir1 N1 C5 75.5(4) . . . . ? O2 Ir1 N1 C5 164.7(4) . . . . ? C25 Ir1 N15 C15 179.9(4) . . . . ? N1 Ir1 N15 C15 -43.7(12) . . . . ? C11 Ir1 N15 C15 84.7(4) . . . . ? O1 Ir1 N15 C15 -3.1(4) . . . . ? O2 Ir1 N15 C15 -92.4(4) . . . . ? C25 Ir1 N15 C19 -13.2(4) . . . . ? N1 Ir1 N15 C19 123.1(10) . . . . ? C11 Ir1 N15 C19 -108.5(4) . . . . ? O1 Ir1 N15 C19 163.7(4) . . . . ? O2 Ir1 N15 C19 74.4(4) . . . . ? C5 N1 C1 C2 -1.5(8) . . . . ? Ir1 N1 C1 C2 166.1(4) . . . . ? N1 C1 C2 C3 0.9(9) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C1 C2 C3 C12 -177.7(6) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C12 C3 C4 C5 177.7(6) . . . . ? C1 N1 C5 C4 1.4(7) . . . . ? Ir1 N1 C5 C4 -167.0(4) . . . . ? C1 N1 C5 C6 -179.3(5) . . . . ? Ir1 N1 C5 C6 12.2(6) . . . . ? C3 C4 C5 N1 -0.8(8) . . . . ? C3 C4 C5 C6 -180.0(5) . . . . ? N1 C5 C6 C7 175.2(5) . . . . ? C4 C5 C6 C7 -5.7(8) . . . . ? N1 C5 C6 C11 -2.8(6) . . . . ? C4 C5 C6 C11 176.4(5) . . . . ? C11 C6 C7 C8 1.0(8) . . . . ? C5 C6 C7 C8 -176.9(5) . . . . ? C6 C7 C8 C9 1.2(8) . . . . ? C6 C7 C8 C13 -177.1(5) . . . . ? C7 C8 C9 C10 -0.8(8) . . . . ? C13 C8 C9 C10 177.5(5) . . . . ? C8 C9 C10 C11 -1.8(8) . . . . ? C8 C9 C10 C14 -178.9(5) . . . . ? C9 C10 C11 C6 3.7(7) . . . . ? C14 C10 C11 C6 -179.4(5) . . . . ? C9 C10 C11 Ir1 -173.5(4) . . . . ? C14 C10 C11 Ir1 3.4(8) . . . . ? C7 C6 C11 C10 -3.3(7) . . . . ? C5 C6 C11 C10 174.6(4) . . . . ? C7 C6 C11 Ir1 174.5(4) . . . . ? C5 C6 C11 Ir1 -7.6(5) . . . . ? C25 Ir1 C11 C10 -67.6(5) . . . . ? N15 Ir1 C11 C10 15.0(5) . . . . ? N1 Ir1 C11 C10 -172.1(5) . . . . ? O1 Ir1 C11 C10 107.4(5) . . . . ? O2 Ir1 C11 C10 161.6(15) . . . . ? C25 Ir1 C11 C6 115.1(4) . . . . ? N15 Ir1 C11 C6 -162.3(3) . . . . ? N1 Ir1 C11 C6 10.6(3) . . . . ? O1 Ir1 C11 C6 -69.9(3) . . . . ? O2 Ir1 C11 C6 -16(2) . . . . ? C4 C3 C12 F2 -62.2(9) . . . . ? C2 C3 C12 F2 115.2(8) . . . . ? C4 C3 C12 F1 173.9(6) . . . . ? C2 C3 C12 F1 -8.7(10) . . . . ? C4 C3 C12 F3 56.6(9) . . . . ? C2 C3 C12 F3 -126.0(7) . . . . ? C7 C8 C13 F4 96.2(7) . . . . ? C9 C8 C13 F4 -82.0(7) . . . . ? C7 C8 C13 F5 -24.6(8) . . . . ? C9 C8 C13 F5 157.1(5) . . . . ? C7 C8 C13 F6 -144.3(5) . . . . ? C9 C8 C13 F6 37.5(8) . . . . ? C9 C10 C14 F8 -133.8(5) . . . . ? C11 C10 C14 F8 49.1(7) . . . . ? C9 C10 C14 F7 -12.5(7) . . . . ? C11 C10 C14 F7 170.4(5) . . . . ? C9 C10 C14 F9 105.8(5) . . . . ? C11 C10 C14 F9 -71.4(6) . . . . ? C19 N15 C15 C16 0.4(8) . . . . ? Ir1 N15 C15 C16 166.8(4) . . . . ? N15 C15 C16 C17 -0.7(9) . . . . ? C15 C16 C17 C18 0.8(9) . . . . ? C15 C16 C17 C26 -176.2(6) . . . . ? C16 C17 C18 C19 -0.5(9) . . . . ? C26 C17 C18 C19 176.4(6) . . . . ? C15 N15 C19 C18 -0.1(7) . . . . ? Ir1 N15 C19 C18 -167.5(4) . . . . ? C15 N15 C19 C20 -179.6(4) . . . . ? Ir1 N15 C19 C20 13.0(5) . . . . ? C17 C18 C19 N15 0.2(8) . . . . ? C17 C18 C19 C20 179.6(5) . . . . ? N15 C19 C20 C21 173.6(5) . . . . ? C18 C19 C20 C21 -5.9(8) . . . . ? N15 C19 C20 C25 -4.1(6) . . . . ? C18 C19 C20 C25 176.5(5) . . . . ? C25 C20 C21 C22 -0.5(8) . . . . ? C19 C20 C21 C22 -178.0(5) . . . . ? C20 C21 C22 C23 1.1(8) . . . . ? C20 C21 C22 C27 -179.6(5) . . . . ? C21 C22 C23 C24 0.0(8) . . . . ? C27 C22 C23 C24 -179.3(5) . . . . ? C22 C23 C24 C25 -1.6(8) . . . . ? C22 C23 C24 C28 178.3(5) . . . . ? C21 C20 C25 C24 -1.0(7) . . . . ? C19 C20 C25 C24 176.5(4) . . . . ? C21 C20 C25 Ir1 175.9(4) . . . . ? C19 C20 C25 Ir1 -6.5(5) . . . . ? C23 C24 C25 C20 2.1(7) . . . . ? C28 C24 C25 C20 -177.9(5) . . . . ? C23 C24 C25 Ir1 -174.0(4) . . . . ? C28 C24 C25 Ir1 6.0(8) . . . . ? N15 Ir1 C25 C20 10.2(3) . . . . ? N1 Ir1 C25 C20 -163.4(3) . . . . ? C11 Ir1 C25 C20 113.8(4) . . . . ? O1 Ir1 C25 C20 -17.2(16) . . . . ? O2 Ir1 C25 C20 -70.2(3) . . . . ? N15 Ir1 C25 C24 -173.6(5) . . . . ? N1 Ir1 C25 C24 12.8(5) . . . . ? C11 Ir1 C25 C24 -70.1(5) . . . . ? O1 Ir1 C25 C24 158.9(12) . . . . ? O2 Ir1 C25 C24 106.0(5) . . . . ? C16 C17 C26 F11 82.9(8) . . . . ? C18 C17 C26 F11 -94.0(8) . . . . ? C16 C17 C26 F12 -156.2(7) . . . . ? C18 C17 C26 F12 26.9(9) . . . . ? C16 C17 C26 F10 -36.4(9) . . . . ? C18 C17 C26 F10 146.6(6) . . . . ? C23 C22 C27 F15 4.6(11) . . . . ? C21 C22 C27 F15 -174.6(8) . . . . ? C23 C22 C27 F14 130.2(8) . . . . ? C21 C22 C27 F14 -49.0(10) . . . . ? C23 C22 C27 F13 -117.0(8) . . . . ? C21 C22 C27 F13 63.7(9) . . . . ? C23 C24 C28 F17 -130.2(5) . . . . ? C25 C24 C28 F17 49.8(7) . . . . ? C23 C24 C28 F16 -10.2(7) . . . . ? C25 C24 C28 F16 169.8(5) . . . . ? C23 C24 C28 F18 108.1(5) . . . . ? C25 C24 C28 F18 -71.9(6) . . . . ? Ir1 O1 C30 C31 17.6(7) . . . . ? Ir1 O1 C30 C29 -166.7(3) . . . . ? C34 C29 C30 O1 -66.1(7) . . . . ? C36 C29 C30 O1 53.4(7) . . . . ? C35 C29 C30 O1 173.2(5) . . . . ? C34 C29 C30 C31 109.6(7) . . . . ? C36 C29 C30 C31 -130.9(6) . . . . ? C35 C29 C30 C31 -11.1(8) . . . . ? O1 C30 C31 C32 -10.1(10) . . . . ? C29 C30 C31 C32 174.6(6) . . . . ? Ir1 O2 C32 C31 12.8(7) . . . . ? Ir1 O2 C32 C33 -162.4(3) . . . . ? C30 C31 C32 O2 -7.2(10) . . . . ? C30 C31 C32 C33 167.6(6) . . . . ? O2 C32 C33 C37 -42.7(6) . . . . ? C31 C32 C33 C37 142.2(6) . . . . ? O2 C32 C33 C39 -165.5(5) . . . . ? C31 C32 C33 C39 19.3(8) . . . . ? O2 C32 C33 C38 75.1(6) . . . . ? C31 C32 C33 C38 -100.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.967 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.161 #===END data_03125 _database_code_depnum_ccdc_archive 'CCDC 257686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 F18 Ir N2 O12 P3' _chemical_formula_weight 1285.71 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' 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' 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' P P 0.1023 0.0942 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.923(6) _cell_length_b 14.898(8) _cell_length_c 15.863(8) _cell_angle_alpha 64.147(8) _cell_angle_beta 85.432(9) _cell_angle_gamma 85.384(9) _cell_volume 2313(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .14 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .01 _exptl_crystal_density_meas multirun _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.122 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28327 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1259 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.39 _reflns_number_total 10851 _reflns_number_gt 7065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10851 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.242 _refine_ls_shift/su_mean 0.009 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_1 Ir 0.89188(3) 0.10779(2) 0.09475(2) 0.02575(11) Uani 1 1 d . . . P1_1 P 0.83607(18) 0.02289(15) -0.06683(15) 0.0278(4) Uani 1 1 d . . . F1_1 F 0.8510(7) 0.4765(4) -0.3448(4) 0.0722(19) Uani 1 1 d . . . F2_1 F 0.9881(6) 0.5434(4) -0.3068(4) 0.0716(19) Uani 1 1 d . . . F3_1 F 0.7996(6) 0.5691(4) -0.2751(4) 0.0641(18) Uani 1 1 d . . . F4_1 F 0.3001(6) 0.3153(6) 0.0855(10) 0.150(5) Uani 1 1 d . . . F5_1 F 0.3935(6) 0.4423(5) 0.0381(7) 0.117(4) Uani 1 1 d . . . F6_1 F 0.3625(11) 0.3572(10) 0.1779(8) 0.188(6) Uani 1 1 d . . . F7_1 F 0.5575(6) 0.0542(6) 0.3422(4) 0.095(3) Uani 1 1 d . . . F8_1 F 0.7527(6) 0.0414(5) 0.3206(4) 0.076(2) Uani 1 1 d . . . F9_1 F 0.6330(6) -0.0286(4) 0.2668(5) 0.078(2) Uani 1 1 d . . . F10_1 F 0.9448(8) -0.3879(5) 0.4066(5) 0.103(3) Uani 1 1 d . . . F11_1 F 0.7853(7) -0.3430(5) 0.4639(5) 0.091(2) Uani 1 1 d . . . F12_1 F 0.9582(8) -0.3225(5) 0.5006(5) 0.108(3) Uani 1 1 d . . . F13_1 F 1.3167(15) 0.101(4) 0.391(2) 0.131(19) Uani 0.57(5) 1 d P . . F14_1 F 1.168(3) 0.048(2) 0.4945(10) 0.092(11) Uani 0.57(5) 1 d P . . F15_1 F 1.192(4) 0.2000(16) 0.4205(19) 0.101(10) Uani 0.57(5) 1 d P . . F13'_1 F 1.156(3) 0.120(5) 0.474(2) 0.111(19) Uani 0.43(5) 1 d P . . F14'_1 F 1.284(5) 0.186(2) 0.380(2) 0.111(19) Uani 0.43(5) 1 d P . . F15'_1 F 1.281(4) 0.034(2) 0.441(3) 0.096(17) Uani 0.43(5) 1 d P . . F16_1 F 1.0303(6) 0.3910(4) 0.1442(4) 0.0582(16) Uani 1 1 d . . . F17_1 F 0.8765(5) 0.3415(3) 0.1041(4) 0.0450(13) Uani 1 1 d . . . F18_1 F 1.0533(5) 0.3416(4) 0.0359(3) 0.0487(13) Uani 1 1 d . . . O1_1 O 0.8030(5) 0.0619(4) 0.0042(3) 0.0289(12) Uani 1 1 d . . . O2_1 O 0.9346(5) -0.0567(4) -0.0471(4) 0.0295(12) Uani 1 1 d . . . O3_1 O 0.8695(6) 0.1094(4) -0.1658(4) 0.0409(15) Uani 1 1 d . . . O4_1 O 0.7106(5) -0.0154(5) -0.0772(5) 0.0437(15) Uani 1 1 d . . . N1_1 N 0.9016(6) 0.2401(5) -0.0221(4) 0.0264(14) Uani 1 1 d . . . N17_1 N 0.8855(6) -0.0307(5) 0.2024(4) 0.0275(14) Uani 1 1 d . . . C1_1 C 0.7835(10) 0.1907(8) -0.2111(7) 0.057(3) Uani 1 1 d . . . H1A_1 H 0.8214 0.2388 -0.2679 0.086 Uiso 1 1 calc R . . H1B_1 H 0.7581 0.2216 -0.1702 0.086 Uiso 1 1 calc R . . H1C_1 H 0.7131 0.1664 -0.2257 0.086 Uiso 1 1 calc R . . C2_1 C 0.7040(10) -0.0572(10) -0.1439(9) 0.076(4) Uani 1 1 d . . . H2B_1 H 0.6198 -0.0678 -0.1487 0.114 Uiso 1 1 calc R . . H2C_1 H 0.7510 -0.1197 -0.1229 0.114 Uiso 1 1 calc R . . H2D_1 H 0.7368 -0.0117 -0.2042 0.114 Uiso 1 1 calc R . . C3_1 C 0.9975(8) 0.2645(6) -0.0838(6) 0.0331(19) Uani 1 1 d . . . H3A_1 H 1.0682 0.2225 -0.0702 0.040 Uiso 1 1 calc R . . C4_1 C 0.9957(8) 0.3492(6) -0.1665(6) 0.037(2) Uani 1 1 d . . . H4A_1 H 1.0643 0.3662 -0.2079 0.044 Uiso 1 1 calc R . . C5_1 C 0.8871(8) 0.4094(6) -0.1867(6) 0.0328(19) Uani 1 1 d . . . C6_1 C 0.7891(8) 0.3845(6) -0.1234(6) 0.0337(19) Uani 1 1 d . . . H6A_1 H 0.7173 0.4252 -0.1358 0.040 Uiso 1 1 calc R . . C7_1 C 0.7973(7) 0.2978(5) -0.0400(5) 0.0272(17) Uani 1 1 d . . . C8_1 C 0.7026(7) 0.2642(6) 0.0340(6) 0.0271(17) Uani 1 1 d . . . C9_1 C 0.5944(7) 0.3217(6) 0.0286(6) 0.0309(18) Uani 1 1 d . . . H9A_1 H 0.5789 0.3797 -0.0256 0.037 Uiso 1 1 calc R . . C10_1 C 0.5103(8) 0.2925(6) 0.1039(7) 0.040(2) Uani 1 1 d . . . C11_1 C 0.5357(8) 0.2057(7) 0.1827(7) 0.044(2) Uani 1 1 d . . . H11A_1 H 0.4792 0.1870 0.2337 0.053 Uiso 1 1 calc R . . C12_1 C 0.6380(8) 0.1465(6) 0.1899(6) 0.038(2) Uani 1 1 d . . . C13_1 C 0.7298(7) 0.1730(6) 0.1152(6) 0.0294(18) Uani 1 1 d . . . C14_1 C 0.8798(9) 0.4994(7) -0.2781(6) 0.044(2) Uani 1 1 d . . . C15_1 C 0.3944(10) 0.3518(8) 0.1008(9) 0.062(3) Uani 1 1 d . . . C16_1 C 0.6461(10) 0.0541(9) 0.2800(8) 0.063(3) Uani 1 1 d . . . C18_1 C 0.8281(8) -0.1064(6) 0.1995(6) 0.0348(19) Uani 1 1 d . . . H18A_1 H 0.7842 -0.0939 0.1473 0.042 Uiso 1 1 calc R . . C19_1 C 0.8326(8) -0.1999(6) 0.2702(6) 0.037(2) Uani 1 1 d . . . H19A_1 H 0.7932 -0.2513 0.2670 0.044 Uiso 1 1 calc R . . C20_1 C 0.8975(8) -0.2161(6) 0.3469(6) 0.039(2) Uani 1 1 d . . . C21_1 C 0.9611(8) -0.1413(6) 0.3496(6) 0.037(2) Uani 1 1 d . . . H21A_1 H 1.0079 -0.1529 0.4002 0.044 Uiso 1 1 calc R . . C22_1 C 0.9527(7) -0.0485(6) 0.2746(6) 0.0315(18) Uani 1 1 d . . . C23_1 C 1.0088(8) 0.0409(6) 0.2676(6) 0.0319(19) Uani 1 1 d . . . C24_1 C 1.0821(8) 0.0343(7) 0.3385(6) 0.039(2) Uani 1 1 d . . . H24A_1 H 1.0998 -0.0273 0.3881 0.047 Uiso 1 1 calc R . . C25_1 C 1.1282(8) 0.1201(7) 0.3343(6) 0.040(2) Uani 1 1 d . . . C26_1 C 1.0966(8) 0.2103(7) 0.2620(6) 0.038(2) Uani 1 1 d . . . H26A_1 H 1.1250 0.2682 0.2605 0.045 Uiso 1 1 calc R . . C27_1 C 1.0238(8) 0.2179(6) 0.1912(6) 0.0348(19) Uani 1 1 d . . . C28_1 C 0.9803(7) 0.1318(6) 0.1891(5) 0.0275(17) Uani 1 1 d . . . C29_1 C 0.9002(11) -0.3183(8) 0.4287(7) 0.055(3) Uani 1 1 d . . . C30_1 C 1.2067(11) 0.1142(9) 0.4090(7) 0.053(3) Uani 1 1 d . . . C31_1 C 0.9948(9) 0.3209(7) 0.1198(7) 0.043(2) Uani 1 1 d . . . P32_2 P 0.5871(3) 0.6329(3) 0.2015(3) 0.0825(11) Uani 1 1 d . . . O33_2 O 0.497(2) 0.5706(14) 0.3126(15) 0.288(12) Uani 1 1 d . . . H33_2 H 0.4514 0.6119 0.3219 0.431 Uiso 1 1 calc R . . O34_2 O 0.7016(11) 0.6542(10) 0.2184(14) 0.194(8) Uani 1 1 d . . . O35_2 O 0.5910(9) 0.5646(7) 0.1527(8) 0.110(4) Uani 1 1 d . . . O37_2 O 0.4956(7) 0.7212(7) 0.1442(7) 0.086(3) Uani 1 1 d . . . C36_2 C 0.6832(18) 0.4849(12) 0.1749(14) 0.144(8) Uani 1 1 d . . . H36A_2 H 0.6809 0.4550 0.1324 0.216 Uiso 1 1 calc R . . H36B_2 H 0.6679 0.4355 0.2380 0.216 Uiso 1 1 calc R . . H36C_2 H 0.7627 0.5107 0.1693 0.216 Uiso 1 1 calc R . . C38_2 C 0.5307(17) 0.8160(11) 0.0833(13) 0.133(7) Uani 1 1 d . . . H38A_2 H 0.4691 0.8645 0.0859 0.199 Uiso 1 1 calc R . . H38B_2 H 0.5398 0.8214 0.0206 0.199 Uiso 1 1 calc R . . H38C_2 H 0.6076 0.8278 0.1011 0.199 Uiso 1 1 calc R . . P39_2 P 0.6956(3) 0.2529(3) 0.5037(3) 0.0745(10) Uani 1 1 d . . . O40_2 O 0.7740(14) 0.1894(13) 0.5649(10) 0.193(8) Uani 1 1 d . . . O41_2 O 0.534(2) 0.2313(15) 0.5200(12) 0.255(11) Uani 1 1 d . . . H41_2 H 0.5123 0.2195 0.4776 0.382 Uiso 1 1 calc R . . O42_2 O 0.693(2) 0.3578(13) 0.4905(19) 0.303(15) Uani 1 1 d . . . O44_2 O 0.7124(13) 0.2643(11) 0.4021(8) 0.153(5) Uani 1 1 d . . . C43_2 C 0.7517(16) 0.4365(10) 0.4604(12) 0.111(6) Uani 1 1 d . . . H43A_2 H 0.7040 0.4860 0.4740 0.167 Uiso 1 1 calc R . . H43B_2 H 0.7671 0.4613 0.3938 0.167 Uiso 1 1 calc R . . H43C_2 H 0.8285 0.4219 0.4904 0.167 Uiso 1 1 calc R . . C45_2 C 0.8221(19) 0.2249(15) 0.3698(15) 0.169(10) Uani 1 1 d . . . H45A_2 H 0.8007 0.2015 0.3256 0.254 Uiso 1 1 calc R . . H45B_2 H 0.8587 0.1705 0.4223 0.254 Uiso 1 1 calc R . . H45C_2 H 0.8795 0.2765 0.3402 0.254 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1_1 0.02756(17) 0.02548(17) 0.02429(18) -0.01094(12) -0.00006(11) -0.00198(11) P1_1 0.0258(11) 0.0306(11) 0.0292(11) -0.0147(9) -0.0050(9) 0.0002(8) F1_1 0.127(6) 0.052(4) 0.036(3) -0.018(3) -0.014(4) 0.007(4) F2_1 0.079(4) 0.050(4) 0.050(4) 0.010(3) 0.009(3) -0.006(3) F3_1 0.089(5) 0.035(3) 0.046(3) -0.003(3) 0.009(3) 0.021(3) F4_1 0.036(4) 0.077(6) 0.324(16) -0.076(8) -0.014(6) 0.003(4) F5_1 0.058(4) 0.049(4) 0.190(9) -0.016(5) 0.046(5) 0.019(3) F6_1 0.169(10) 0.259(14) 0.141(9) -0.115(10) -0.027(8) 0.153(10) F7_1 0.074(5) 0.105(6) 0.053(4) 0.003(4) 0.039(4) 0.023(4) F8_1 0.073(5) 0.101(5) 0.034(3) -0.018(3) 0.008(3) 0.030(4) F9_1 0.068(4) 0.040(3) 0.096(5) -0.006(3) 0.033(4) -0.009(3) F10_1 0.172(8) 0.034(4) 0.070(5) -0.002(3) 0.026(5) 0.023(4) F11_1 0.081(5) 0.057(4) 0.084(5) 0.014(4) 0.020(4) -0.010(4) F12_1 0.161(8) 0.066(5) 0.058(5) 0.022(4) -0.044(5) -0.037(5) F13_1 0.029(8) 0.30(6) 0.10(2) -0.12(3) -0.013(10) 0.006(19) F14_1 0.12(2) 0.102(17) 0.033(7) 0.003(9) -0.037(9) -0.037(15) F15_1 0.16(2) 0.091(14) 0.085(17) -0.063(12) -0.073(17) 0.034(14) F13'_1 0.107(19) 0.18(5) 0.037(17) -0.05(2) -0.020(15) 0.06(3) F14'_1 0.14(4) 0.084(19) 0.11(2) -0.027(16) -0.08(3) -0.039(19) F15'_1 0.11(3) 0.10(2) 0.10(3) -0.064(17) -0.09(3) 0.055(17) F16_1 0.081(4) 0.035(3) 0.070(4) -0.029(3) -0.030(3) -0.007(3) F17_1 0.049(3) 0.031(3) 0.057(3) -0.020(2) -0.013(3) 0.003(2) F18_1 0.062(4) 0.045(3) 0.033(3) -0.009(2) -0.002(3) -0.014(3) O1_1 0.030(3) 0.036(3) 0.022(3) -0.013(2) -0.007(2) 0.000(2) O2_1 0.025(3) 0.031(3) 0.029(3) -0.010(2) -0.004(2) 0.001(2) O3_1 0.050(4) 0.036(3) 0.031(3) -0.011(3) -0.001(3) 0.011(3) O4_1 0.028(3) 0.061(4) 0.060(4) -0.042(4) -0.009(3) 0.001(3) N1_1 0.028(3) 0.024(3) 0.026(4) -0.011(3) -0.003(3) 0.005(3) N17_1 0.030(4) 0.033(4) 0.020(3) -0.012(3) 0.001(3) -0.002(3) C1_1 0.076(8) 0.052(6) 0.042(6) -0.020(5) -0.018(5) 0.022(6) C2_1 0.049(7) 0.122(11) 0.106(10) -0.090(9) -0.011(6) -0.016(7) C3_1 0.036(5) 0.026(4) 0.030(5) -0.006(4) -0.006(4) 0.004(3) C4_1 0.041(5) 0.032(5) 0.031(5) -0.008(4) 0.003(4) -0.004(4) C5_1 0.048(5) 0.029(4) 0.026(4) -0.016(4) -0.001(4) 0.000(4) C6_1 0.039(5) 0.022(4) 0.036(5) -0.010(4) -0.002(4) 0.008(3) C7_1 0.029(4) 0.023(4) 0.032(5) -0.015(3) -0.001(3) 0.002(3) C8_1 0.027(4) 0.025(4) 0.033(5) -0.017(4) -0.002(3) 0.000(3) C9_1 0.024(4) 0.030(4) 0.045(5) -0.021(4) -0.003(4) 0.000(3) C10_1 0.027(4) 0.036(5) 0.066(7) -0.031(5) 0.007(4) -0.002(4) C11_1 0.036(5) 0.046(6) 0.059(6) -0.032(5) 0.016(4) -0.012(4) C12_1 0.035(5) 0.036(5) 0.039(5) -0.014(4) 0.011(4) -0.008(4) C13_1 0.026(4) 0.036(5) 0.032(5) -0.021(4) 0.002(3) -0.005(3) C14_1 0.059(6) 0.034(5) 0.034(5) -0.012(4) 0.011(5) -0.001(4) C15_1 0.045(6) 0.045(6) 0.087(9) -0.026(6) 0.027(6) 0.008(5) C16_1 0.048(7) 0.066(8) 0.045(6) -0.004(5) 0.021(5) 0.011(5) C18_1 0.035(5) 0.043(5) 0.033(5) -0.022(4) 0.003(4) -0.011(4) C19_1 0.045(5) 0.032(5) 0.034(5) -0.014(4) 0.004(4) -0.009(4) C20_1 0.049(5) 0.028(5) 0.028(5) -0.001(4) 0.004(4) -0.004(4) C21_1 0.054(6) 0.032(5) 0.018(4) -0.004(4) 0.002(4) -0.010(4) C22_1 0.035(5) 0.035(5) 0.025(4) -0.014(4) 0.003(4) -0.006(4) C23_1 0.038(5) 0.033(4) 0.032(5) -0.021(4) 0.005(4) -0.004(4) C24_1 0.052(6) 0.045(5) 0.020(4) -0.013(4) -0.004(4) -0.004(4) C25_1 0.049(6) 0.040(5) 0.034(5) -0.019(4) -0.009(4) 0.000(4) C26_1 0.043(5) 0.043(5) 0.036(5) -0.023(4) 0.003(4) -0.013(4) C27_1 0.044(5) 0.038(5) 0.028(5) -0.019(4) 0.002(4) -0.006(4) C28_1 0.029(4) 0.029(4) 0.019(4) -0.006(3) 0.002(3) 0.004(3) C29_1 0.066(7) 0.038(6) 0.044(6) -0.002(5) -0.004(5) -0.004(5) C30_1 0.062(7) 0.066(8) 0.036(6) -0.024(6) -0.013(5) -0.013(6) C31_1 0.047(6) 0.034(5) 0.055(6) -0.026(5) -0.012(5) -0.002(4) P32_2 0.054(2) 0.104(3) 0.115(3) -0.073(3) -0.025(2) 0.0211(19) O33_2 0.29(2) 0.191(18) 0.26(2) 0.009(17) -0.10(2) 0.123(17) O34_2 0.102(9) 0.177(13) 0.41(2) -0.219(16) -0.134(12) 0.054(8) O35_2 0.108(8) 0.087(7) 0.163(10) -0.075(7) -0.074(7) 0.026(6) O37_2 0.056(5) 0.092(7) 0.121(8) -0.057(6) -0.015(5) 0.006(5) C36_2 0.191(19) 0.092(12) 0.182(19) -0.088(13) -0.103(16) 0.077(13) C38_2 0.147(16) 0.076(11) 0.143(16) -0.007(11) -0.023(13) -0.053(11) P39_2 0.0541(19) 0.079(2) 0.108(3) -0.058(2) 0.0059(19) -0.0129(17) O40_2 0.176(14) 0.265(19) 0.162(13) -0.113(14) -0.122(12) 0.099(13) O41_2 0.30(3) 0.28(2) 0.171(15) -0.110(16) 0.044(15) 0.099(19) O42_2 0.37(3) 0.141(14) 0.45(4) -0.19(2) 0.15(3) -0.123(17) O44_2 0.149(11) 0.202(14) 0.086(8) -0.047(9) -0.009(8) 0.036(10) C43_2 0.137(15) 0.057(9) 0.150(15) -0.050(10) -0.018(12) -0.013(9) C45_2 0.161(19) 0.164(19) 0.18(2) -0.089(17) 0.053(16) 0.054(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1_1 C28_1 2.013(8) . ? Ir1_1 C13_1 2.022(8) . ? Ir1_1 N17_1 2.026(6) . ? Ir1_1 N1_1 2.037(6) . ? Ir1_1 O1_1 2.158(5) . ? Ir1_1 O2_1 2.187(5) 2_755 ? P1_1 O2_1 1.479(5) . ? P1_1 O1_1 1.487(5) . ? P1_1 O4_1 1.574(6) . ? P1_1 O3_1 1.575(6) . ? F1_1 C14_1 1.311(11) . ? F2_1 C14_1 1.346(11) . ? F3_1 C14_1 1.319(10) . ? F4_1 C15_1 1.288(14) . ? F5_1 C15_1 1.280(12) . ? F6_1 C15_1 1.279(14) . ? F7_1 C16_1 1.327(11) . ? F8_1 C16_1 1.337(13) . ? F9_1 C16_1 1.356(14) . ? F10_1 C29_1 1.283(12) . ? F11_1 C29_1 1.344(12) . ? F12_1 C29_1 1.323(13) . ? F13_1 F15'_1 1.05(3) . ? F13_1 F14'_1 1.22(3) . ? F13_1 C30_1 1.23(2) . ? F14_1 F13'_1 0.98(4) . ? F14_1 C30_1 1.342(18) . ? F14_1 F15'_1 1.50(4) . ? F15_1 F13'_1 1.19(5) . ? F15_1 F14'_1 1.20(4) . ? F15_1 C30_1 1.36(2) . ? F13'_1 C30_1 1.17(2) . ? F14'_1 C30_1 1.31(3) . ? F15'_1 C30_1 1.32(2) . ? F16_1 C31_1 1.354(9) . ? F17_1 C31_1 1.321(10) . ? F18_1 C31_1 1.345(11) . ? O2_1 Ir1_1 2.187(5) 2_755 ? O3_1 C1_1 1.424(11) . ? O4_1 C2_1 1.451(11) . ? N1_1 C3_1 1.333(10) . ? N1_1 C7_1 1.341(9) . ? N17_1 C22_1 1.326(10) . ? N17_1 C18_1 1.353(10) . ? C3_1 C4_1 1.367(11) . ? C4_1 C5_1 1.397(12) . ? C5_1 C6_1 1.364(11) . ? C5_1 C14_1 1.487(12) . ? C6_1 C7_1 1.391(11) . ? C7_1 C8_1 1.441(11) . ? C8_1 C9_1 1.389(10) . ? C8_1 C13_1 1.436(11) . ? C9_1 C10_1 1.377(12) . ? C10_1 C11_1 1.379(13) . ? C10_1 C15_1 1.475(12) . ? C11_1 C12_1 1.346(12) . ? C12_1 C13_1 1.426(11) . ? C12_1 C16_1 1.493(13) . ? C18_1 C19_1 1.355(11) . ? C19_1 C20_1 1.376(12) . ? C20_1 C21_1 1.378(12) . ? C20_1 C29_1 1.509(12) . ? C21_1 C22_1 1.377(11) . ? C22_1 C23_1 1.468(11) . ? C23_1 C24_1 1.396(11) . ? C23_1 C28_1 1.415(11) . ? C24_1 C25_1 1.384(12) . ? C25_1 C26_1 1.373(12) . ? C25_1 C30_1 1.485(12) . ? C26_1 C27_1 1.387(12) . ? C27_1 C28_1 1.419(11) . ? C27_1 C31_1 1.483(12) . ? P32_2 O34_2 1.389(11) . ? P32_2 O35_2 1.520(10) . ? P32_2 O37_2 1.564(9) . ? P32_2 O33_2 1.84(2) . ? O35_2 C36_2 1.431(15) . ? O37_2 C38_2 1.383(15) . ? P39_2 O40_2 1.332(12) . ? P39_2 O42_2 1.482(15) . ? P39_2 O44_2 1.541(12) . ? P39_2 O41_2 1.80(2) . ? O42_2 C43_2 1.263(18) . ? O44_2 C45_2 1.447(18) . ? 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 C28_1 Ir1_1 C13_1 95.0(3) . . ? C28_1 Ir1_1 N17_1 81.1(3) . . ? C13_1 Ir1_1 N17_1 102.0(3) . . ? C28_1 Ir1_1 N1_1 103.3(3) . . ? C13_1 Ir1_1 N1_1 81.5(3) . . ? N17_1 Ir1_1 N1_1 174.2(2) . . ? C28_1 Ir1_1 O1_1 172.6(2) . . ? C13_1 Ir1_1 O1_1 88.9(3) . . ? N17_1 Ir1_1 O1_1 92.0(2) . . ? N1_1 Ir1_1 O1_1 83.4(2) . . ? C28_1 Ir1_1 O2_1 90.3(3) . 2_755 ? C13_1 Ir1_1 O2_1 169.9(3) . 2_755 ? N17_1 Ir1_1 O2_1 87.3(2) . 2_755 ? N1_1 Ir1_1 O2_1 89.0(2) . 2_755 ? O1_1 Ir1_1 O2_1 86.8(2) . 2_755 ? O2_1 P1_1 O1_1 118.7(3) . . ? O2_1 P1_1 O4_1 110.4(3) . . ? O1_1 P1_1 O4_1 102.6(3) . . ? O2_1 P1_1 O3_1 107.2(3) . . ? O1_1 P1_1 O3_1 111.5(3) . . ? O4_1 P1_1 O3_1 105.7(4) . . ? F15'_1 F13_1 F14'_1 127(3) . . ? F15'_1 F13_1 C30_1 69.9(19) . . ? F14'_1 F13_1 C30_1 64.5(18) . . ? F13'_1 F14_1 C30_1 57.7(16) . . ? F13'_1 F14_1 F15'_1 105(2) . . ? C30_1 F14_1 F15'_1 55.0(12) . . ? F13'_1 F15_1 F14'_1 108(2) . . ? F13'_1 F15_1 C30_1 53.7(14) . . ? F14'_1 F15_1 C30_1 61.1(15) . . ? F14_1 F13'_1 C30_1 77(3) . . ? F14_1 F13'_1 F15_1 145(3) . . ? C30_1 F13'_1 F15_1 71(2) . . ? F13_1 F14'_1 F15_1 120(3) . . ? F13_1 F14'_1 C30_1 58.2(14) . . ? F15_1 F14'_1 C30_1 66(2) . . ? F13_1 F15'_1 C30_1 61.4(18) . . ? F13_1 F15'_1 F14_1 114(3) . . ? C30_1 F15'_1 F14_1 56.5(14) . . ? P1_1 O1_1 Ir1_1 139.4(3) . . ? P1_1 O2_1 Ir1_1 147.5(3) . 2_755 ? C1_1 O3_1 P1_1 120.8(6) . . ? C2_1 O4_1 P1_1 119.5(6) . . ? C3_1 N1_1 C7_1 120.6(7) . . ? C3_1 N1_1 Ir1_1 123.9(5) . . ? C7_1 N1_1 Ir1_1 115.0(5) . . ? C22_1 N17_1 C18_1 119.5(7) . . ? C22_1 N17_1 Ir1_1 116.5(5) . . ? C18_1 N17_1 Ir1_1 123.7(6) . . ? N1_1 C3_1 C4_1 122.3(8) . . ? C3_1 C4_1 C5_1 117.8(8) . . ? C6_1 C5_1 C4_1 119.9(8) . . ? C6_1 C5_1 C14_1 120.9(8) . . ? C4_1 C5_1 C14_1 119.2(8) . . ? C5_1 C6_1 C7_1 119.5(7) . . ? N1_1 C7_1 C6_1 119.9(7) . . ? N1_1 C7_1 C8_1 114.7(7) . . ? C6_1 C7_1 C8_1 125.4(7) . . ? C9_1 C8_1 C13_1 122.3(7) . . ? C9_1 C8_1 C7_1 120.7(7) . . ? C13_1 C8_1 C7_1 116.8(7) . . ? C10_1 C9_1 C8_1 119.6(8) . . ? C9_1 C10_1 C11_1 118.6(8) . . ? C9_1 C10_1 C15_1 121.2(9) . . ? C11_1 C10_1 C15_1 120.2(8) . . ? C12_1 C11_1 C10_1 123.6(8) . . ? C11_1 C12_1 C13_1 120.7(8) . . ? C11_1 C12_1 C16_1 115.2(8) . . ? C13_1 C12_1 C16_1 124.1(8) . . ? C12_1 C13_1 C8_1 115.0(7) . . ? C12_1 C13_1 Ir1_1 134.1(6) . . ? C8_1 C13_1 Ir1_1 110.8(5) . . ? F1_1 C14_1 F3_1 108.4(8) . . ? F1_1 C14_1 F2_1 106.0(7) . . ? F3_1 C14_1 F2_1 105.8(7) . . ? F1_1 C14_1 C5_1 111.3(7) . . ? F3_1 C14_1 C5_1 112.9(7) . . ? F2_1 C14_1 C5_1 112.1(8) . . ? F6_1 C15_1 F5_1 105.3(11) . . ? F6_1 C15_1 F4_1 102.8(11) . . ? F5_1 C15_1 F4_1 104.7(11) . . ? F6_1 C15_1 C10_1 113.9(11) . . ? F5_1 C15_1 C10_1 115.2(8) . . ? F4_1 C15_1 C10_1 113.7(9) . . ? F7_1 C16_1 F8_1 106.9(10) . . ? F7_1 C16_1 F9_1 106.1(9) . . ? F8_1 C16_1 F9_1 107.2(9) . . ? F7_1 C16_1 C12_1 111.8(8) . . ? F8_1 C16_1 C12_1 113.2(9) . . ? F9_1 C16_1 C12_1 111.2(10) . . ? N17_1 C18_1 C19_1 122.1(8) . . ? C18_1 C19_1 C20_1 117.7(8) . . ? C19_1 C20_1 C21_1 121.1(8) . . ? C19_1 C20_1 C29_1 119.2(8) . . ? C21_1 C20_1 C29_1 119.7(9) . . ? C22_1 C21_1 C20_1 117.6(8) . . ? N17_1 C22_1 C21_1 121.8(8) . . ? N17_1 C22_1 C23_1 113.0(7) . . ? C21_1 C22_1 C23_1 125.1(8) . . ? C24_1 C23_1 C28_1 123.3(7) . . ? C24_1 C23_1 C22_1 119.8(8) . . ? C28_1 C23_1 C22_1 116.8(7) . . ? C25_1 C24_1 C23_1 119.5(8) . . ? C26_1 C25_1 C24_1 118.9(8) . . ? C26_1 C25_1 C30_1 121.0(8) . . ? C24_1 C25_1 C30_1 120.2(8) . . ? C25_1 C26_1 C27_1 122.2(8) . . ? C26_1 C27_1 C28_1 121.2(8) . . ? C26_1 C27_1 C31_1 115.7(7) . . ? C28_1 C27_1 C31_1 123.1(7) . . ? C23_1 C28_1 C27_1 114.8(7) . . ? C23_1 C28_1 Ir1_1 111.1(6) . . ? C27_1 C28_1 Ir1_1 134.0(6) . . ? F10_1 C29_1 F12_1 109.3(10) . . ? F10_1 C29_1 F11_1 105.9(9) . . ? F12_1 C29_1 F11_1 104.1(9) . . ? F10_1 C29_1 C20_1 113.5(9) . . ? F12_1 C29_1 C20_1 113.4(9) . . ? F11_1 C29_1 C20_1 110.0(8) . . ? F13'_1 C30_1 F13_1 131.3(18) . . ? F13'_1 C30_1 F15'_1 107(2) . . ? F13_1 C30_1 F15'_1 48.7(16) . . ? F13'_1 C30_1 F14'_1 102(2) . . ? F13_1 C30_1 F14'_1 57.3(18) . . ? F15'_1 C30_1 F14'_1 102(2) . . ? F13'_1 C30_1 F14_1 45(2) . . ? F13_1 C30_1 F14_1 113.1(18) . . ? F15'_1 C30_1 F14_1 68.5(17) . . ? F14'_1 C30_1 F14_1 132.9(17) . . ? F13'_1 C30_1 F15_1 56(2) . . ? F13_1 C30_1 F15_1 107.7(19) . . ? F15'_1 C30_1 F15_1 134.9(15) . . ? F14'_1 C30_1 F15_1 53.1(18) . . ? F14_1 C30_1 F15_1 100.1(17) . . ? F13'_1 C30_1 C25_1 116.3(17) . . ? F13_1 C30_1 C25_1 112.4(12) . . ? F15'_1 C30_1 C25_1 114.2(13) . . ? F14'_1 C30_1 C25_1 113.6(14) . . ? F14_1 C30_1 C25_1 112.2(11) . . ? F15_1 C30_1 C25_1 110.6(12) . . ? F17_1 C31_1 F18_1 106.5(7) . . ? F17_1 C31_1 F16_1 105.7(7) . . ? F18_1 C31_1 F16_1 104.5(7) . . ? F17_1 C31_1 C27_1 114.1(8) . . ? F18_1 C31_1 C27_1 113.1(7) . . ? F16_1 C31_1 C27_1 112.2(7) . . ? O34_2 P32_2 O35_2 114.7(7) . . ? O34_2 P32_2 O37_2 119.0(7) . . ? O35_2 P32_2 O37_2 104.0(5) . . ? O34_2 P32_2 O33_2 110.1(11) . . ? O35_2 P32_2 O33_2 106.4(9) . . ? O37_2 P32_2 O33_2 101.3(6) . . ? C36_2 O35_2 P32_2 119.6(9) . . ? C38_2 O37_2 P32_2 124.2(10) . . ? O40_2 P39_2 O42_2 115.9(14) . . ? O40_2 P39_2 O44_2 116.9(9) . . ? O42_2 P39_2 O44_2 102.5(12) . . ? O40_2 P39_2 O41_2 120.2(11) . . ? O42_2 P39_2 O41_2 100.7(12) . . ? O44_2 P39_2 O41_2 97.2(8) . . ? C43_2 O42_2 P39_2 145.9(19) . . ? C45_2 O44_2 P39_2 121.6(12) . . ? 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 F15'_1 F14_1 F13'_1 C30_1 28(2) . . . . ? C30_1 F14_1 F13'_1 F15_1 -23(4) . . . . ? F15'_1 F14_1 F13'_1 F15_1 5(6) . . . . ? F14'_1 F15_1 F13'_1 F14_1 -6(6) . . . . ? C30_1 F15_1 F13'_1 F14_1 24(5) . . . . ? F14'_1 F15_1 F13'_1 C30_1 -30(2) . . . . ? F15'_1 F13_1 F14'_1 F15_1 -11(4) . . . . ? C30_1 F13_1 F14'_1 F15_1 22(2) . . . . ? F15'_1 F13_1 F14'_1 C30_1 -33(3) . . . . ? F13'_1 F15_1 F14'_1 F13_1 7(3) . . . . ? C30_1 F15_1 F14'_1 F13_1 -21(2) . . . . ? F13'_1 F15_1 F14'_1 C30_1 27.6(19) . . . . ? F14'_1 F13_1 F15'_1 C30_1 32(2) . . . . ? F14'_1 F13_1 F15'_1 F14_1 9(4) . . . . ? C30_1 F13_1 F15'_1 F14_1 -22.5(19) . . . . ? F13'_1 F14_1 F15'_1 F13_1 -6(3) . . . . ? C30_1 F14_1 F15'_1 F13_1 24(2) . . . . ? F13'_1 F14_1 F15'_1 C30_1 -29(2) . . . . ? O2_1 P1_1 O1_1 Ir1_1 44.0(6) . . . . ? O4_1 P1_1 O1_1 Ir1_1 165.9(5) . . . . ? O3_1 P1_1 O1_1 Ir1_1 -81.4(5) . . . . ? C28_1 Ir1_1 O1_1 P1_1 -73(2) . . . . ? C13_1 Ir1_1 O1_1 P1_1 165.3(5) . . . . ? N17_1 Ir1_1 O1_1 P1_1 -92.7(5) . . . . ? N1_1 Ir1_1 O1_1 P1_1 83.8(5) . . . . ? O2_1 Ir1_1 O1_1 P1_1 -5.6(5) 2_755 . . . ? O1_1 P1_1 O2_1 Ir1_1 -127.1(6) . . . 2_755 ? O4_1 P1_1 O2_1 Ir1_1 115.0(6) . . . 2_755 ? O3_1 P1_1 O2_1 Ir1_1 0.3(7) . . . 2_755 ? O2_1 P1_1 O3_1 C1_1 170.6(7) . . . . ? O1_1 P1_1 O3_1 C1_1 -57.9(8) . . . . ? O4_1 P1_1 O3_1 C1_1 52.9(7) . . . . ? O2_1 P1_1 O4_1 C2_1 -54.4(8) . . . . ? O1_1 P1_1 O4_1 C2_1 178.2(8) . . . . ? O3_1 P1_1 O4_1 C2_1 61.2(8) . . . . ? C28_1 Ir1_1 N1_1 C3_1 84.3(7) . . . . ? C13_1 Ir1_1 N1_1 C3_1 177.4(7) . . . . ? N17_1 Ir1_1 N1_1 C3_1 -55(3) . . . . ? O1_1 Ir1_1 N1_1 C3_1 -92.7(7) . . . . ? O2_1 Ir1_1 N1_1 C3_1 -5.8(7) 2_755 . . . ? C28_1 Ir1_1 N1_1 C7_1 -103.6(6) . . . . ? C13_1 Ir1_1 N1_1 C7_1 -10.5(6) . . . . ? N17_1 Ir1_1 N1_1 C7_1 117(2) . . . . ? O1_1 Ir1_1 N1_1 C7_1 79.4(6) . . . . ? O2_1 Ir1_1 N1_1 C7_1 166.3(5) 2_755 . . . ? C28_1 Ir1_1 N17_1 C22_1 -10.0(6) . . . . ? C13_1 Ir1_1 N17_1 C22_1 -103.2(6) . . . . ? N1_1 Ir1_1 N17_1 C22_1 130(2) . . . . ? O1_1 Ir1_1 N17_1 C22_1 167.5(6) . . . . ? O2_1 Ir1_1 N17_1 C22_1 80.8(6) 2_755 . . . ? C28_1 Ir1_1 N17_1 C18_1 177.1(7) . . . . ? C13_1 Ir1_1 N17_1 C18_1 83.9(7) . . . . ? N1_1 Ir1_1 N17_1 C18_1 -42(3) . . . . ? O1_1 Ir1_1 N17_1 C18_1 -5.4(6) . . . . ? O2_1 Ir1_1 N17_1 C18_1 -92.1(6) 2_755 . . . ? C7_1 N1_1 C3_1 C4_1 1.2(12) . . . . ? Ir1_1 N1_1 C3_1 C4_1 172.8(6) . . . . ? N1_1 C3_1 C4_1 C5_1 -2.0(13) . . . . ? C3_1 C4_1 C5_1 C6_1 2.2(12) . . . . ? C3_1 C4_1 C5_1 C14_1 -177.0(8) . . . . ? C4_1 C5_1 C6_1 C7_1 -1.6(13) . . . . ? C14_1 C5_1 C6_1 C7_1 177.6(8) . . . . ? C3_1 N1_1 C7_1 C6_1 -0.5(12) . . . . ? Ir1_1 N1_1 C7_1 C6_1 -172.8(6) . . . . ? C3_1 N1_1 C7_1 C8_1 -178.1(7) . . . . ? Ir1_1 N1_1 C7_1 C8_1 9.5(9) . . . . ? C5_1 C6_1 C7_1 N1_1 0.7(12) . . . . ? C5_1 C6_1 C7_1 C8_1 178.1(8) . . . . ? N1_1 C7_1 C8_1 C9_1 173.9(7) . . . . ? C6_1 C7_1 C8_1 C9_1 -3.6(12) . . . . ? N1_1 C7_1 C8_1 C13_1 -1.7(10) . . . . ? C6_1 C7_1 C8_1 C13_1 -179.2(7) . . . . ? C13_1 C8_1 C9_1 C10_1 1.3(12) . . . . ? C7_1 C8_1 C9_1 C10_1 -174.0(8) . . . . ? C8_1 C9_1 C10_1 C11_1 -0.6(12) . . . . ? C8_1 C9_1 C10_1 C15_1 179.9(9) . . . . ? C9_1 C10_1 C11_1 C12_1 -1.1(14) . . . . ? C15_1 C10_1 C11_1 C12_1 178.4(10) . . . . ? C10_1 C11_1 C12_1 C13_1 2.0(14) . . . . ? C10_1 C11_1 C12_1 C16_1 -178.0(10) . . . . ? C11_1 C12_1 C13_1 C8_1 -1.2(12) . . . . ? C16_1 C12_1 C13_1 C8_1 178.8(9) . . . . ? C11_1 C12_1 C13_1 Ir1_1 -178.8(7) . . . . ? C16_1 C12_1 C13_1 Ir1_1 1.3(15) . . . . ? C9_1 C8_1 C13_1 C12_1 -0.4(11) . . . . ? C7_1 C8_1 C13_1 C12_1 175.1(7) . . . . ? C9_1 C8_1 C13_1 Ir1_1 177.7(6) . . . . ? C7_1 C8_1 C13_1 Ir1_1 -6.8(9) . . . . ? C28_1 Ir1_1 C13_1 C12_1 -70.7(9) . . . . ? N17_1 Ir1_1 C13_1 C12_1 11.2(9) . . . . ? N1_1 Ir1_1 C13_1 C12_1 -173.5(9) . . . . ? O1_1 Ir1_1 C13_1 C12_1 103.0(8) . . . . ? O2_1 Ir1_1 C13_1 C12_1 167.7(11) 2_755 . . . ? C28_1 Ir1_1 C13_1 C8_1 111.6(5) . . . . ? N17_1 Ir1_1 C13_1 C8_1 -166.4(5) . . . . ? N1_1 Ir1_1 C13_1 C8_1 8.9(5) . . . . ? O1_1 Ir1_1 C13_1 C8_1 -74.7(5) . . . . ? O2_1 Ir1_1 C13_1 C8_1 -10.0(18) 2_755 . . . ? C6_1 C5_1 C14_1 F1_1 -95.6(10) . . . . ? C4_1 C5_1 C14_1 F1_1 83.6(11) . . . . ? C6_1 C5_1 C14_1 F3_1 26.6(13) . . . . ? C4_1 C5_1 C14_1 F3_1 -154.2(8) . . . . ? C6_1 C5_1 C14_1 F2_1 145.9(8) . . . . ? C4_1 C5_1 C14_1 F2_1 -34.9(11) . . . . ? C9_1 C10_1 C15_1 F6_1 -140.9(12) . . . . ? C11_1 C10_1 C15_1 F6_1 39.6(16) . . . . ? C9_1 C10_1 C15_1 F5_1 -19.1(16) . . . . ? C11_1 C10_1 C15_1 F5_1 161.5(11) . . . . ? C9_1 C10_1 C15_1 F4_1 101.8(12) . . . . ? C11_1 C10_1 C15_1 F4_1 -77.7(15) . . . . ? C11_1 C12_1 C16_1 F7_1 -8.7(15) . . . . ? C13_1 C12_1 C16_1 F7_1 171.3(9) . . . . ? C11_1 C12_1 C16_1 F8_1 -129.4(9) . . . . ? C13_1 C12_1 C16_1 F8_1 50.5(14) . . . . ? C11_1 C12_1 C16_1 F9_1 109.8(10) . . . . ? C13_1 C12_1 C16_1 F9_1 -70.3(12) . . . . ? C22_1 N17_1 C18_1 C19_1 2.8(12) . . . . ? Ir1_1 N17_1 C18_1 C19_1 175.5(6) . . . . ? N17_1 C18_1 C19_1 C20_1 0.5(12) . . . . ? C18_1 C19_1 C20_1 C21_1 -3.3(13) . . . . ? C18_1 C19_1 C20_1 C29_1 177.5(8) . . . . ? C19_1 C20_1 C21_1 C22_1 2.8(13) . . . . ? C29_1 C20_1 C21_1 C22_1 -178.0(8) . . . . ? C18_1 N17_1 C22_1 C21_1 -3.3(12) . . . . ? Ir1_1 N17_1 C22_1 C21_1 -176.5(6) . . . . ? C18_1 N17_1 C22_1 C23_1 -179.9(7) . . . . ? Ir1_1 N17_1 C22_1 C23_1 6.9(9) . . . . ? C20_1 C21_1 C22_1 N17_1 0.5(12) . . . . ? C20_1 C21_1 C22_1 C23_1 176.7(8) . . . . ? N17_1 C22_1 C23_1 C24_1 179.8(7) . . . . ? C21_1 C22_1 C23_1 C24_1 3.3(13) . . . . ? N17_1 C22_1 C23_1 C28_1 2.5(10) . . . . ? C21_1 C22_1 C23_1 C28_1 -174.0(8) . . . . ? C28_1 C23_1 C24_1 C25_1 1.3(13) . . . . ? C22_1 C23_1 C24_1 C25_1 -175.9(8) . . . . ? C23_1 C24_1 C25_1 C26_1 2.4(13) . . . . ? C23_1 C24_1 C25_1 C30_1 -179.7(9) . . . . ? C24_1 C25_1 C26_1 C27_1 -2.4(13) . . . . ? C30_1 C25_1 C26_1 C27_1 179.8(9) . . . . ? C25_1 C26_1 C27_1 C28_1 -1.3(13) . . . . ? C25_1 C26_1 C27_1 C31_1 178.2(8) . . . . ? C24_1 C23_1 C28_1 C27_1 -4.7(11) . . . . ? C22_1 C23_1 C28_1 C27_1 172.5(7) . . . . ? C24_1 C23_1 C28_1 Ir1_1 172.5(6) . . . . ? C22_1 C23_1 C28_1 Ir1_1 -10.3(9) . . . . ? C26_1 C27_1 C28_1 C23_1 4.7(11) . . . . ? C31_1 C27_1 C28_1 C23_1 -174.8(8) . . . . ? C26_1 C27_1 C28_1 Ir1_1 -171.7(6) . . . . ? C31_1 C27_1 C28_1 Ir1_1 8.8(13) . . . . ? C13_1 Ir1_1 C28_1 C23_1 111.8(6) . . . . ? N17_1 Ir1_1 C28_1 C23_1 10.5(5) . . . . ? N1_1 Ir1_1 C28_1 C23_1 -165.8(5) . . . . ? O1_1 Ir1_1 C28_1 C23_1 -10(2) . . . . ? O2_1 Ir1_1 C28_1 C23_1 -76.7(5) 2_755 . . . ? C13_1 Ir1_1 C28_1 C27_1 -71.7(8) . . . . ? N17_1 Ir1_1 C28_1 C27_1 -173.1(8) . . . . ? N1_1 Ir1_1 C28_1 C27_1 10.7(8) . . . . ? O1_1 Ir1_1 C28_1 C27_1 166.8(15) . . . . ? O2_1 Ir1_1 C28_1 C27_1 99.8(8) 2_755 . . . ? C19_1 C20_1 C29_1 F10_1 59.0(13) . . . . ? C21_1 C20_1 C29_1 F10_1 -120.2(11) . . . . ? C19_1 C20_1 C29_1 F12_1 -175.5(9) . . . . ? C21_1 C20_1 C29_1 F12_1 5.3(14) . . . . ? C19_1 C20_1 C29_1 F11_1 -59.5(12) . . . . ? C21_1 C20_1 C29_1 F11_1 121.4(10) . . . . ? F14_1 F13'_1 C30_1 F13_1 -82(4) . . . . ? F15_1 F13'_1 C30_1 F13_1 84(3) . . . . ? F14_1 F13'_1 C30_1 F15'_1 -33(3) . . . . ? F15_1 F13'_1 C30_1 F15'_1 133.2(19) . . . . ? F14_1 F13'_1 C30_1 F14'_1 -140(2) . . . . ? F15_1 F13'_1 C30_1 F14'_1 26.6(19) . . . . ? F15_1 F13'_1 C30_1 F14_1 166(3) . . . . ? F14_1 F13'_1 C30_1 F15_1 -166(3) . . . . ? F14_1 F13'_1 C30_1 C25_1 96.0(19) . . . . ? F15_1 F13'_1 C30_1 C25_1 -98(2) . . . . ? F15'_1 F13_1 C30_1 F13'_1 75(4) . . . . ? F14'_1 F13_1 C30_1 F13'_1 -77(4) . . . . ? F14'_1 F13_1 C30_1 F15'_1 -152(3) . . . . ? F15'_1 F13_1 C30_1 F14'_1 152(3) . . . . ? F15'_1 F13_1 C30_1 F14_1 25(3) . . . . ? F14'_1 F13_1 C30_1 F14_1 -127(2) . . . . ? F15'_1 F13_1 C30_1 F15_1 135(2) . . . . ? F14'_1 F13_1 C30_1 F15_1 -18(2) . . . . ? F15'_1 F13_1 C30_1 C25_1 -103(2) . . . . ? F14'_1 F13_1 C30_1 C25_1 104.5(18) . . . . ? F13_1 F15'_1 C30_1 F13'_1 -131(3) . . . . ? F14_1 F15'_1 C30_1 F13'_1 25(3) . . . . ? F14_1 F15'_1 C30_1 F13_1 155(2) . . . . ? F13_1 F15'_1 C30_1 F14'_1 -23(3) . . . . ? F14_1 F15'_1 C30_1 F14'_1 132(2) . . . . ? F13_1 F15'_1 C30_1 F14_1 -155(2) . . . . ? F13_1 F15'_1 C30_1 F15_1 -72(4) . . . . ? F14_1 F15'_1 C30_1 F15_1 83(3) . . . . ? F13_1 F15'_1 C30_1 C25_1 99(2) . . . . ? F14_1 F15'_1 C30_1 C25_1 -105.6(14) . . . . ? F13_1 F14'_1 C30_1 F13'_1 131.4(19) . . . . ? F15_1 F14'_1 C30_1 F13'_1 -28(2) . . . . ? F15_1 F14'_1 C30_1 F13_1 -159(3) . . . . ? F13_1 F14'_1 C30_1 F15'_1 21(2) . . . . ? F15_1 F14'_1 C30_1 F15'_1 -138(2) . . . . ? F13_1 F14'_1 C30_1 F14_1 92(3) . . . . ? F15_1 F14'_1 C30_1 F14_1 -67(3) . . . . ? F13_1 F14'_1 C30_1 F15_1 159(3) . . . . ? F13_1 F14'_1 C30_1 C25_1 -102.4(16) . . . . ? F15_1 F14'_1 C30_1 C25_1 99(2) . . . . ? F15'_1 F14_1 C30_1 F13'_1 -146(3) . . . . ? F13'_1 F14_1 C30_1 F13_1 126(3) . . . . ? F15'_1 F14_1 C30_1 F13_1 -20(2) . . . . ? F13'_1 F14_1 C30_1 F15'_1 146(3) . . . . ? F13'_1 F14_1 C30_1 F14'_1 60(4) . . . . ? F15'_1 F14_1 C30_1 F14'_1 -86(3) . . . . ? F13'_1 F14_1 C30_1 F15_1 12(3) . . . . ? F15'_1 F14_1 C30_1 F15_1 -134.4(17) . . . . ? F13'_1 F14_1 C30_1 C25_1 -106(3) . . . . ? F15'_1 F14_1 C30_1 C25_1 108.3(15) . . . . ? F14'_1 F15_1 C30_1 F13'_1 147(2) . . . . ? F13'_1 F15_1 C30_1 F13_1 -128(2) . . . . ? F14'_1 F15_1 C30_1 F13_1 19(2) . . . . ? F13'_1 F15_1 C30_1 F15'_1 -80(3) . . . . ? F14'_1 F15_1 C30_1 F15'_1 67(4) . . . . ? F13'_1 F15_1 C30_1 F14'_1 -147(2) . . . . ? F13'_1 F15_1 C30_1 F14_1 -10(2) . . . . ? F14'_1 F15_1 C30_1 F14_1 136.9(19) . . . . ? F13'_1 F15_1 C30_1 C25_1 108.5(18) . . . . ? F14'_1 F15_1 C30_1 C25_1 -104.7(18) . . . . ? C26_1 C25_1 C30_1 F13'_1 89(4) . . . . ? C24_1 C25_1 C30_1 F13'_1 -89(4) . . . . ? C26_1 C25_1 C30_1 F13_1 -92(3) . . . . ? C24_1 C25_1 C30_1 F13_1 90(3) . . . . ? C26_1 C25_1 C30_1 F15'_1 -145(3) . . . . ? C24_1 C25_1 C30_1 F15'_1 37(3) . . . . ? C26_1 C25_1 C30_1 F14'_1 -29(4) . . . . ? C24_1 C25_1 C30_1 F14'_1 153(3) . . . . ? C26_1 C25_1 C30_1 F14_1 139(2) . . . . ? C24_1 C25_1 C30_1 F14_1 -39(2) . . . . ? C26_1 C25_1 C30_1 F15_1 28(2) . . . . ? C24_1 C25_1 C30_1 F15_1 -150(2) . . . . ? C26_1 C27_1 C31_1 F17_1 -129.3(8) . . . . ? C28_1 C27_1 C31_1 F17_1 50.2(11) . . . . ? C26_1 C27_1 C31_1 F18_1 108.9(8) . . . . ? C28_1 C27_1 C31_1 F18_1 -71.6(11) . . . . ? C26_1 C27_1 C31_1 F16_1 -9.1(11) . . . . ? C28_1 C27_1 C31_1 F16_1 170.5(8) . . . . ? O34_2 P32_2 O35_2 C36_2 36.6(18) . . . . ? O37_2 P32_2 O35_2 C36_2 168.2(14) . . . . ? O33_2 P32_2 O35_2 C36_2 -85.3(15) . . . . ? O34_2 P32_2 O37_2 C38_2 22.2(16) . . . . ? O35_2 P32_2 O37_2 C38_2 -106.9(13) . . . . ? O33_2 P32_2 O37_2 C38_2 142.9(14) . . . . ? O40_2 P39_2 O42_2 C43_2 67(5) . . . . ? O44_2 P39_2 O42_2 C43_2 -61(5) . . . . ? O41_2 P39_2 O42_2 C43_2 -161(4) . . . . ? O40_2 P39_2 O44_2 C45_2 -13(2) . . . . ? O42_2 P39_2 O44_2 C45_2 115.3(18) . . . . ? O41_2 P39_2 O44_2 C45_2 -141.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 2.995 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.197 #===END