# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kjc1238 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H40 Ir N4, F6 P' _chemical_formula_sum 'C30 H40 F6 Ir N4 P' _chemical_formula_weight 793.83 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.4200(3) _cell_length_b 11.6201(3) _cell_length_c 14.6854(3) _cell_angle_alpha 108.477(2) _cell_angle_beta 90.483(2) _cell_angle_gamma 116.2940(10) _cell_volume 1488.64(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9453 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 4.604 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4595 _exptl_absorpt_correction_T_max 0.7096 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10004 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10004 _reflns_number_gt 9453 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two complex units in the asymmetric unit are conformationally different. The structure can be refined in Cc, but the result is a disordered structure with partial occupancies. P1 gives an ordered structure and so refinement in Cc cannot be justified. The PF6 counter-ions were refined using a disordered model with two components on each site. Geometric and the displacement parameters were restrained to be similar for both components during refinement. ; _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^)+(0.0337P)^2^+5.5667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(7) _refine_ls_number_reflns 10004 _refine_ls_number_parameters 893 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2938(8) 0.4603(9) 0.6323(6) 0.0268(17) Uani 1 1 d . . . H1 H 1.3357 0.5571 0.6641 0.032 Uiso 1 1 calc R . . C2 C 1.3857(10) 0.4059(11) 0.6039(6) 0.037(2) Uani 1 1 d . . . H2 H 1.4879 0.4634 0.6174 0.045 Uiso 1 1 calc R . . C3 C 1.3273(12) 0.2655(13) 0.5552(7) 0.051(3) Uani 1 1 d . . . H3 H 1.3878 0.2247 0.5323 0.061 Uiso 1 1 calc R . . C4 C 1.1795(11) 0.1872(10) 0.5409(6) 0.038(2) Uani 1 1 d . . . H4 H 1.1360 0.0904 0.5082 0.046 Uiso 1 1 calc R . . C5 C 1.0941(9) 0.2491(8) 0.5739(5) 0.0259(16) Uani 1 1 d . . . C6 C 0.9358(9) 0.1586(8) 0.5636(6) 0.0302(17) Uani 1 1 d . . . H6 H 0.9174 0.1900 0.6315 0.036 Uiso 1 1 calc R . . C7 C 0.8784(12) 0.0118(8) 0.5402(6) 0.044(2) Uani 1 1 d . . . H7A H 0.7727 -0.0309 0.5368 0.066 Uiso 1 1 calc R . . H7B H 0.9226 -0.0044 0.5909 0.066 Uiso 1 1 calc R . . H7C H 0.9011 -0.0285 0.4771 0.066 Uiso 1 1 calc R . . C8 C 0.8712(8) 0.3317(8) 0.5368(5) 0.0207(14) Uani 1 1 d . . . C9 C 0.7595(8) 0.0995(7) 0.4131(5) 0.0255(16) Uani 1 1 d . . . H9 H 0.7736 0.0158 0.3939 0.031 Uiso 1 1 calc R . . C10 C 0.5979(9) 0.0615(9) 0.4169(6) 0.038(2) Uani 1 1 d . . . H10A H 0.5333 -0.0330 0.3711 0.045 Uiso 1 1 calc R . . H10B H 0.5774 0.0682 0.4835 0.045 Uiso 1 1 calc R . . C11 C 0.5771(9) 0.1684(9) 0.3862(6) 0.036(2) Uani 1 1 d . . . H11A H 0.5055 0.1228 0.3251 0.044 Uiso 1 1 calc R . . H11B H 0.5428 0.2210 0.4378 0.044 Uiso 1 1 calc R . . C12 C 0.7252(8) 0.2618(8) 0.3714(5) 0.0241(15) Uani 1 1 d . . . C13 C 0.7972(8) 0.1674(8) 0.3368(5) 0.0244(15) Uani 1 1 d . . . C14 C 0.7267(11) 0.3390(9) 0.3044(6) 0.037(2) Uani 1 1 d . . . H14A H 0.6841 0.2736 0.2375 0.056 Uiso 1 1 calc R . . H14B H 0.8272 0.4053 0.3065 0.056 Uiso 1 1 calc R . . H14C H 0.6699 0.3878 0.3262 0.056 Uiso 1 1 calc R . . C15 C 0.9579(9) 0.2410(9) 0.3347(6) 0.0345(19) Uani 1 1 d . . . H15A H 1.0077 0.3174 0.3968 0.052 Uiso 1 1 calc R . . H15B H 0.9723 0.2768 0.2814 0.052 Uiso 1 1 calc R . . H15C H 0.9978 0.1767 0.3245 0.052 Uiso 1 1 calc R . . C16 C 0.7207(10) 0.0568(10) 0.2345(6) 0.037(2) Uani 1 1 d . . . H16A H 0.7487 0.0992 0.1850 0.056 Uiso 1 1 calc R . . H16B H 0.6151 0.0166 0.2311 0.056 Uiso 1 1 calc R . . H16C H 0.7499 -0.0154 0.2227 0.056 Uiso 1 1 calc R . . C17 C 0.8340(8) 0.5049(8) 0.4999(6) 0.0297(17) Uani 1 1 d . . . H17A H 0.7971 0.5297 0.5611 0.036 Uiso 1 1 calc R . . H17B H 0.7771 0.5095 0.4481 0.036 Uiso 1 1 calc R . . C18 C 0.9884(13) 0.6060(12) 0.5130(8) 0.026(2) Uani 1 1 d . . . C19 C 1.0302(10) 0.6902(9) 0.4578(6) 0.0339(19) Uani 1 1 d . . . H19 H 0.9592 0.6855 0.4137 0.041 Uiso 1 1 calc R . . C20 C 1.1768(11) 0.7814(8) 0.4673(6) 0.037(2) Uani 1 1 d . . . H20 H 1.2068 0.8399 0.4303 0.045 Uiso 1 1 calc R . . C21 C 1.2770(10) 0.7850(8) 0.5312(6) 0.0346(19) Uani 1 1 d . . . H21 H 1.3777 0.8456 0.5386 0.041 Uiso 1 1 calc R . . C22 C 1.2291(8) 0.6988(8) 0.5850(5) 0.0261(16) Uani 1 1 d . . . H22 H 1.2994 0.7030 0.6294 0.031 Uiso 1 1 calc R . . C23 C 0.8406(7) 0.3792(8) 0.7449(5) 0.0242(16) Uani 1 1 d . . . H23 H 0.8119 0.3014 0.6867 0.029 Uiso 1 1 calc R . . C24 C 0.8256(8) 0.4854(8) 0.7368(6) 0.0254(16) Uani 1 1 d . . . H24 H 0.7880 0.4764 0.6743 0.031 Uiso 1 1 calc R . . C25 C 0.8642(9) 0.6153(8) 0.8194(6) 0.0314(18) Uani 1 1 d . . . H25A H 0.8500 0.5957 0.8805 0.038 Uiso 1 1 calc R . . H25B H 0.7979 0.6519 0.8091 0.038 Uiso 1 1 calc R . . C26 C 1.0215(10) 0.7244(8) 0.8306(6) 0.036(2) Uani 1 1 d . . . H26A H 1.0231 0.7837 0.7943 0.043 Uiso 1 1 calc R . . H26B H 1.0582 0.7832 0.9004 0.043 Uiso 1 1 calc R . . C27 C 1.1227(10) 0.6654(8) 0.7944(5) 0.0270(17) Uani 1 1 d . . . H27 H 1.1860 0.7030 0.7536 0.032 Uiso 1 1 calc R . . C28 C 1.1304(8) 0.5600(8) 0.8161(5) 0.0243(15) Uani 1 1 d . . . H28 H 1.1930 0.5256 0.7862 0.029 Uiso 1 1 calc R . . C29 C 1.0413(9) 0.4977(8) 0.8866(5) 0.0289(17) Uani 1 1 d . . . H29A H 1.0992 0.4729 0.9231 0.035 Uiso 1 1 calc R . . H29B H 1.0218 0.5676 0.9342 0.035 Uiso 1 1 calc R . . C30 C 0.8969(11) 0.3700(10) 0.8344(6) 0.023(2) Uani 1 1 d . . . H30A H 0.9108 0.2871 0.8166 0.027 Uiso 1 1 calc R . . H30B H 0.8250 0.3610 0.8789 0.027 Uiso 1 1 calc R . . C31 C 0.0480(9) 0.4834(8) 0.1445(6) 0.0229(15) Uani 1 1 d . . . H31 H 0.1057 0.5769 0.1851 0.028 Uiso 1 1 calc R . . C32 C -0.0969(9) 0.4377(10) 0.1095(6) 0.0324(18) Uani 1 1 d . . . H32 H -0.1356 0.5004 0.1228 0.039 Uiso 1 1 calc R . . C33 C -0.1827(8) 0.3027(10) 0.0564(5) 0.0322(19) Uani 1 1 d . . . H33 H -0.2822 0.2695 0.0323 0.039 Uiso 1 1 calc R . . C34 C -0.1229(8) 0.2140(9) 0.0378(5) 0.0266(16) Uani 1 1 d . . . H34 H -0.1822 0.1188 0.0020 0.032 Uiso 1 1 calc R . . C35 C 0.0231(8) 0.2639(7) 0.0715(5) 0.0192(14) Uani 1 1 d . . . C36 C 0.0915(7) 0.1715(7) 0.0572(5) 0.0188(13) Uani 1 1 d . . . H36 H 0.1448 0.1986 0.1237 0.023 Uiso 1 1 calc R . . C37 C -0.0078(9) 0.0223(8) 0.0294(6) 0.0309(18) Uani 1 1 d . . . H37A H -0.0765 -0.0097 -0.0300 0.046 Uiso 1 1 calc R . . H37B H -0.0615 0.0057 0.0823 0.046 Uiso 1 1 calc R . . H37C H 0.0490 -0.0277 0.0175 0.046 Uiso 1 1 calc R . . C38 C 0.3241(8) 0.3339(7) 0.0323(5) 0.0190(14) Uani 1 1 d . . . C39 C 0.1746(8) 0.1210(7) -0.1064(5) 0.0246(15) Uani 1 1 d . . . H39 H 0.1039 0.0232 -0.1174 0.029 Uiso 1 1 calc R . . C40 C 0.1157(8) 0.1805(9) -0.1657(6) 0.0299(17) Uani 1 1 d . . . H40A H 0.0564 0.2199 -0.1292 0.036 Uiso 1 1 calc R . . H40B H 0.0561 0.1093 -0.2289 0.036 Uiso 1 1 calc R . . C41 C 0.2562(9) 0.2941(8) -0.1808(6) 0.0285(17) Uani 1 1 d . . . H41A H 0.2569 0.2780 -0.2511 0.034 Uiso 1 1 calc R . . H41B H 0.2632 0.3859 -0.1481 0.034 Uiso 1 1 calc R . . C42 C 0.3835(8) 0.2844(7) -0.1350(5) 0.0237(15) Uani 1 1 d . . . C43 C 0.3164(9) 0.1333(8) -0.1414(5) 0.0258(16) Uani 1 1 d . . . C44 C 0.5144(10) 0.3288(10) -0.1846(6) 0.040(2) Uani 1 1 d . . . H44A H 0.5388 0.4185 -0.1888 0.059 Uiso 1 1 calc R . . H44B H 0.4921 0.2610 -0.2504 0.059 Uiso 1 1 calc R . . H44C H 0.5972 0.3358 -0.1468 0.059 Uiso 1 1 calc R . . C45 C 0.2802(10) 0.0340(9) -0.2482(6) 0.040(2) Uani 1 1 d . . . H45A H 0.2122 -0.0596 -0.2526 0.059 Uiso 1 1 calc R . . H45B H 0.3697 0.0361 -0.2698 0.059 Uiso 1 1 calc R . . H45C H 0.2357 0.0624 -0.2900 0.059 Uiso 1 1 calc R . . C46 C 0.4078(10) 0.1026(9) -0.0812(6) 0.038(2) Uani 1 1 d . . . H46A H 0.4333 0.1660 -0.0135 0.056 Uiso 1 1 calc R . . H46B H 0.4969 0.1141 -0.1078 0.056 Uiso 1 1 calc R . . H46C H 0.3524 0.0078 -0.0834 0.056 Uiso 1 1 calc R . . C47 C 0.5373(8) 0.5150(8) 0.0001(6) 0.0286(17) Uani 1 1 d . . . H47A H 0.6014 0.5384 0.0604 0.034 Uiso 1 1 calc R . . H47B H 0.5969 0.5221 -0.0520 0.034 Uiso 1 1 calc R . . C48 C 0.4826(12) 0.6152(10) 0.0166(7) 0.026(2) Uani 1 1 d . . . C49 C 0.5257(9) 0.7022(8) -0.0362(6) 0.0297(17) Uani 1 1 d . . . H49 H 0.5897 0.6967 -0.0811 0.036 Uiso 1 1 calc R . . C50 C 0.4744(10) 0.7983(9) -0.0228(6) 0.036(2) Uani 1 1 d . . . H50 H 0.5026 0.8592 -0.0579 0.044 Uiso 1 1 calc R . . C51 C 0.3809(9) 0.8009(8) 0.0435(6) 0.0305(17) Uani 1 1 d . . . H51 H 0.3422 0.8634 0.0539 0.037 Uiso 1 1 calc R . . C52 C 0.3444(9) 0.7121(8) 0.0944(5) 0.0274(16) Uani 1 1 d . . . H52 H 0.2813 0.7165 0.1402 0.033 Uiso 1 1 calc R . . C53 C 0.4173(10) 0.6597(8) 0.2958(5) 0.0291(17) Uani 1 1 d . . . H53 H 0.3872 0.6981 0.2570 0.035 Uiso 1 1 calc R . . C54 C 0.3102(9) 0.5546(8) 0.3186(5) 0.0269(16) Uani 1 1 d . . . H54 H 0.2120 0.5193 0.2901 0.032 Uiso 1 1 calc R . . C55 C 0.3421(9) 0.4940(8) 0.3862(5) 0.0269(16) Uani 1 1 d . . . H55A H 0.2636 0.4710 0.4253 0.032 Uiso 1 1 calc R . . H55B H 0.4343 0.5629 0.4317 0.032 Uiso 1 1 calc R . . C56 C 0.3544(12) 0.3637(12) 0.3308(7) 0.023(2) Uani 1 1 d . . . H56A H 0.4202 0.3532 0.3728 0.028 Uiso 1 1 calc R . . H56B H 0.2575 0.2822 0.3152 0.028 Uiso 1 1 calc R . . C57 C 0.4115(8) 0.3705(7) 0.2385(5) 0.0226(15) Uani 1 1 d . . . H57 H 0.3600 0.2931 0.1805 0.027 Uiso 1 1 calc R . . C58 C 0.5304(8) 0.4779(8) 0.2310(6) 0.0265(16) Uani 1 1 d . . . H58 H 0.5557 0.4689 0.1681 0.032 Uiso 1 1 calc R . . C59 C 0.6265(9) 0.6101(9) 0.3129(6) 0.035(2) Uani 1 1 d . . . H59A H 0.7269 0.6464 0.2993 0.042 Uiso 1 1 calc R . . H59B H 0.6279 0.5912 0.3740 0.042 Uiso 1 1 calc R . . C60 C 0.5777(10) 0.7178(8) 0.3276(6) 0.036(2) Uani 1 1 d . . . H60A H 0.6042 0.7763 0.3976 0.043 Uiso 1 1 calc R . . H60B H 0.6307 0.7772 0.2907 0.043 Uiso 1 1 calc R . . N1 N 1.1499(6) 0.3874(6) 0.6188(4) 0.0179(11) Uani 1 1 d . . . N2 N 0.8510(8) 0.2013(7) 0.5083(4) 0.0250(13) Uani 1 1 d . . . N3 N 0.8108(6) 0.3629(6) 0.4737(4) 0.0217(12) Uani 1 1 d . . . N4 N 1.0894(7) 0.6105(6) 0.5774(4) 0.0219(12) Uani 1 1 d . . . N5 N 0.1100(6) 0.4000(6) 0.1228(4) 0.0173(11) Uani 1 1 d . . . N6 N 0.2087(6) 0.2085(6) -0.0020(4) 0.0183(12) Uani 1 1 d . . . N7 N 0.4193(6) 0.3695(6) -0.0283(4) 0.0189(12) Uani 1 1 d . . . N8 N 0.3931(7) 0.6201(6) 0.0826(4) 0.0229(13) Uani 1 1 d . . . Ir1 Ir 0.999887(19) 0.472769(18) 0.666160(15) 0.01540(9) Uani 1 1 d . . . Ir2 Ir 0.344488(19) 0.471579(18) 0.165919(15) 0.01568(9) Uani 1 1 d . . . F1 F 0.1543(11) 1.0118(7) 0.2096(6) 0.096(3) Uani 0.750(6) 1 d PDU A 1 F2 F 0.0718(8) 0.7905(7) 0.1263(4) 0.0517(19) Uani 0.750(6) 1 d PDU A 1 F3 F -0.0052(8) 0.7420(7) 0.2562(5) 0.060(2) Uani 0.750(6) 1 d PDU A 1 F4 F 0.0772(12) 0.9616(9) 0.3394(5) 0.106(3) Uani 0.750(6) 1 d PDU A 1 F5 F -0.0763(8) 0.8640(10) 0.1993(6) 0.087(3) Uani 0.750(6) 1 d PDU A 1 F6 F 0.2237(7) 0.8828(10) 0.2657(6) 0.074(3) Uani 0.750(6) 1 d PDU A 1 P1 P 0.0738(5) 0.8779(4) 0.2334(3) 0.0412(10) Uani 0.750(6) 1 d PDU A 1 F1A F 0.033(3) 0.993(2) 0.2338(16) 0.064(5) Uani 0.250(6) 1 d PDU A 2 F2A F -0.021(2) 0.777(2) 0.1564(14) 0.090(5) Uani 0.250(6) 1 d PDU A 2 F3A F 0.157(3) 0.800(2) 0.2572(18) 0.078(6) Uani 0.250(6) 1 d PDU A 2 F4A F 0.207(2) 1.0122(18) 0.3371(12) 0.060(5) Uani 0.250(6) 1 d PDU A 2 F5A F -0.014(2) 0.853(2) 0.3176(15) 0.077(5) Uani 0.250(6) 1 d PDU A 2 F6A F 0.209(2) 0.943(3) 0.1780(15) 0.080(5) Uani 0.250(6) 1 d PDU A 2 P1A P 0.0929(16) 0.8961(14) 0.2470(10) 0.059(4) Uani 0.250(6) 1 d PDU A 2 F7 F 0.583(4) 0.751(3) 0.6303(19) 0.056(7) Uani 0.160(11) 1 d PDU B 1 F8 F 0.670(4) 0.777(4) 0.777(2) 0.066(6) Uani 0.160(11) 1 d PDU B 1 F9 F 0.712(4) 0.992(3) 0.8345(18) 0.067(6) Uani 0.160(11) 1 d PDU B 1 F10 F 0.622(4) 0.966(3) 0.684(3) 0.074(8) Uani 0.160(11) 1 d PDU B 1 F11 F 0.491(3) 0.825(4) 0.759(3) 0.057(8) Uani 0.160(11) 1 d PDU B 1 F12 F 0.803(3) 0.921(4) 0.705(2) 0.069(6) Uani 0.160(11) 1 d PDU B 1 P2 P 0.647(2) 0.874(2) 0.7315(16) 0.058(4) Uani 0.160(11) 1 d PDU B 1 F7A F 0.5894(10) 0.7837(9) 0.6205(5) 0.057(2) Uani 0.840(11) 1 d PDU B 2 F8A F 0.6043(9) 0.7093(8) 0.7411(6) 0.071(2) Uani 0.840(11) 1 d PDU B 2 F9A F 0.7260(9) 0.9204(11) 0.8450(5) 0.082(3) Uani 0.840(11) 1 d PDU B 2 F10A F 0.7138(11) 0.9994(8) 0.7251(7) 0.086(3) Uani 0.840(11) 1 d PDU B 2 F11A F 0.5106(9) 0.8510(11) 0.7587(7) 0.072(3) Uani 0.840(11) 1 d PDU B 2 F12A F 0.8058(7) 0.8541(10) 0.7066(6) 0.070(2) Uani 0.840(11) 1 d PDU B 2 P2A P 0.6604(5) 0.8561(5) 0.7328(3) 0.0503(11) Uani 0.840(11) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(4) 0.044(5) 0.024(4) 0.019(4) 0.006(3) 0.020(4) C2 0.033(5) 0.069(7) 0.029(4) 0.027(4) 0.014(4) 0.033(5) C3 0.065(7) 0.090(9) 0.035(5) 0.029(5) 0.030(5) 0.063(7) C4 0.061(6) 0.044(5) 0.024(4) 0.007(4) 0.014(4) 0.040(5) C5 0.033(4) 0.035(4) 0.013(3) 0.009(3) 0.004(3) 0.019(4) C6 0.035(4) 0.026(4) 0.021(4) 0.011(3) -0.002(3) 0.007(3) C7 0.074(7) 0.019(4) 0.027(4) 0.004(3) -0.015(4) 0.016(4) C8 0.017(3) 0.031(4) 0.012(3) 0.007(3) 0.001(3) 0.010(3) C9 0.028(4) 0.017(3) 0.015(3) 0.002(3) -0.006(3) 0.000(3) C10 0.026(4) 0.037(5) 0.028(4) 0.009(4) 0.005(3) -0.002(4) C11 0.019(4) 0.037(5) 0.036(5) 0.007(4) 0.000(3) 0.003(4) C12 0.028(4) 0.026(4) 0.020(3) 0.006(3) -0.001(3) 0.016(3) C13 0.022(4) 0.026(4) 0.024(4) 0.010(3) 0.003(3) 0.011(3) C14 0.051(5) 0.041(5) 0.026(4) 0.013(4) -0.001(4) 0.027(4) C15 0.028(4) 0.034(5) 0.036(5) 0.012(4) 0.010(3) 0.010(4) C16 0.037(5) 0.042(5) 0.024(4) 0.006(4) -0.007(3) 0.015(4) C17 0.026(4) 0.036(5) 0.031(4) 0.013(3) 0.001(3) 0.017(4) C18 0.039(6) 0.021(5) 0.022(5) 0.007(4) 0.002(4) 0.017(4) C19 0.046(5) 0.035(5) 0.028(4) 0.020(4) 0.009(4) 0.019(4) C20 0.057(6) 0.025(4) 0.033(4) 0.019(4) 0.008(4) 0.015(4) C21 0.046(5) 0.022(4) 0.028(4) 0.010(3) 0.013(4) 0.009(4) C22 0.028(4) 0.026(4) 0.019(3) 0.007(3) 0.006(3) 0.009(3) C23 0.013(3) 0.032(4) 0.024(4) 0.017(3) 0.003(3) 0.002(3) C24 0.021(4) 0.032(4) 0.035(4) 0.019(3) 0.018(3) 0.017(3) C25 0.037(5) 0.029(4) 0.036(4) 0.012(3) 0.017(4) 0.021(4) C26 0.050(6) 0.019(4) 0.032(4) 0.004(3) 0.017(4) 0.014(4) C27 0.033(5) 0.011(4) 0.019(4) -0.001(3) 0.002(3) -0.001(3) C28 0.025(4) 0.027(4) 0.016(3) 0.003(3) 0.010(3) 0.012(3) C29 0.036(4) 0.033(4) 0.020(4) 0.009(3) 0.011(3) 0.018(4) C30 0.030(5) 0.025(5) 0.015(4) 0.011(4) 0.006(4) 0.013(4) C31 0.029(4) 0.022(4) 0.019(4) 0.003(3) 0.009(3) 0.016(3) C32 0.028(4) 0.052(5) 0.033(4) 0.023(4) 0.013(3) 0.027(4) C33 0.014(4) 0.054(6) 0.022(4) 0.016(4) 0.000(3) 0.009(4) C34 0.018(4) 0.034(4) 0.025(4) 0.011(3) 0.003(3) 0.010(3) C35 0.022(3) 0.024(4) 0.012(3) 0.008(3) 0.005(2) 0.010(3) C36 0.015(3) 0.019(3) 0.019(3) 0.006(3) 0.002(2) 0.005(3) C37 0.034(4) 0.020(4) 0.026(4) 0.006(3) 0.009(3) 0.004(3) C38 0.019(4) 0.015(3) 0.018(3) 0.004(3) -0.002(3) 0.006(3) C39 0.030(4) 0.013(3) 0.018(3) -0.003(3) 0.002(3) 0.005(3) C40 0.018(4) 0.046(5) 0.024(4) 0.010(3) -0.003(3) 0.015(4) C41 0.035(4) 0.032(4) 0.024(4) 0.013(3) 0.005(3) 0.018(4) C42 0.025(4) 0.020(4) 0.021(3) 0.005(3) 0.007(3) 0.008(3) C43 0.035(4) 0.020(4) 0.022(4) 0.002(3) 0.003(3) 0.017(3) C44 0.033(5) 0.042(5) 0.034(5) 0.010(4) 0.020(4) 0.012(4) C45 0.048(5) 0.035(5) 0.028(4) 0.002(4) 0.012(4) 0.020(4) C46 0.044(5) 0.039(5) 0.038(5) 0.007(4) 0.009(4) 0.031(4) C47 0.017(4) 0.024(4) 0.037(4) 0.008(3) 0.008(3) 0.005(3) C48 0.025(5) 0.014(4) 0.025(5) 0.001(3) -0.003(3) 0.003(4) C49 0.028(4) 0.024(4) 0.028(4) 0.010(3) 0.003(3) 0.004(3) C50 0.040(5) 0.028(4) 0.034(5) 0.015(4) 0.002(4) 0.008(4) C51 0.035(4) 0.019(4) 0.031(4) 0.007(3) -0.011(3) 0.009(3) C52 0.030(4) 0.022(4) 0.024(4) 0.004(3) -0.006(3) 0.010(3) C53 0.042(5) 0.017(4) 0.013(3) -0.003(3) -0.006(3) 0.007(4) C54 0.030(4) 0.030(4) 0.012(3) -0.004(3) -0.008(3) 0.014(3) C55 0.029(4) 0.023(4) 0.018(3) 0.000(3) -0.002(3) 0.008(3) C56 0.021(5) 0.029(5) 0.026(5) 0.015(4) 0.006(4) 0.014(4) C57 0.033(4) 0.021(4) 0.019(3) 0.006(3) 0.005(3) 0.017(3) C58 0.015(3) 0.035(4) 0.035(4) 0.021(3) -0.004(3) 0.010(3) C59 0.023(4) 0.033(5) 0.033(4) 0.014(4) -0.007(3) -0.001(3) C60 0.037(5) 0.017(4) 0.030(4) 0.004(3) -0.014(4) -0.003(4) N1 0.020(3) 0.025(3) 0.012(3) 0.005(2) 0.002(2) 0.014(3) N2 0.029(4) 0.020(3) 0.015(3) 0.002(2) -0.003(3) 0.006(3) N3 0.020(3) 0.025(3) 0.018(3) 0.008(2) -0.001(2) 0.008(3) N4 0.030(3) 0.021(3) 0.019(3) 0.010(2) 0.008(2) 0.014(3) N5 0.015(3) 0.019(3) 0.018(3) 0.007(2) 0.002(2) 0.008(2) N6 0.018(3) 0.013(3) 0.014(3) 0.000(2) 0.001(2) 0.003(2) N7 0.014(3) 0.020(3) 0.020(3) 0.006(2) 0.005(2) 0.007(2) N8 0.023(3) 0.015(3) 0.025(3) 0.007(2) -0.003(2) 0.004(2) Ir1 0.0172(2) 0.0157(2) 0.01370(18) 0.00576(15) 0.00286(14) 0.00770(17) Ir2 0.0153(2) 0.01208(19) 0.01522(19) 0.00175(14) -0.00171(14) 0.00489(16) F1 0.130(6) 0.059(5) 0.078(5) 0.036(4) -0.009(5) 0.020(5) F2 0.062(4) 0.061(4) 0.040(4) 0.017(3) 0.021(3) 0.036(4) F3 0.076(5) 0.061(4) 0.056(4) 0.038(3) 0.020(3) 0.031(4) F4 0.143(7) 0.088(6) 0.071(5) 0.001(4) 0.021(5) 0.058(5) F5 0.091(6) 0.117(6) 0.088(5) 0.045(5) 0.018(4) 0.071(5) F6 0.066(5) 0.076(5) 0.064(4) 0.030(4) 0.001(4) 0.017(4) P1 0.080(2) 0.0357(18) 0.0254(16) 0.0133(15) 0.0129(16) 0.0403(18) F1A 0.080(7) 0.067(7) 0.064(7) 0.025(6) 0.003(6) 0.051(6) F2A 0.099(7) 0.079(7) 0.076(7) 0.023(6) 0.011(7) 0.032(6) F3A 0.093(8) 0.068(8) 0.072(8) 0.018(6) 0.012(7) 0.040(6) F4A 0.068(8) 0.062(8) 0.056(8) 0.019(6) 0.003(6) 0.037(6) F5A 0.083(8) 0.075(8) 0.059(7) 0.033(6) 0.017(6) 0.020(6) F6A 0.083(7) 0.083(7) 0.064(7) 0.020(6) 0.023(6) 0.035(6) P1A 0.086(5) 0.051(5) 0.051(5) 0.015(4) 0.015(4) 0.042(4) F7 0.051(9) 0.056(9) 0.049(9) 0.017(7) 0.015(7) 0.016(7) F8 0.061(8) 0.064(8) 0.062(8) 0.022(7) -0.003(7) 0.021(6) F9 0.063(8) 0.064(8) 0.061(8) 0.019(7) 0.001(7) 0.021(6) F10 0.072(10) 0.071(10) 0.074(10) 0.021(8) 0.008(8) 0.032(7) F11 0.048(10) 0.067(10) 0.045(10) 0.025(8) 0.010(8) 0.015(7) F12 0.058(8) 0.066(8) 0.070(8) 0.024(7) 0.010(7) 0.019(6) P2 0.048(5) 0.059(5) 0.051(5) 0.017(4) 0.003(5) 0.015(4) F7A 0.056(4) 0.064(5) 0.038(3) 0.019(3) 0.002(3) 0.017(4) F8A 0.056(5) 0.060(5) 0.068(5) 0.030(4) -0.006(4) -0.002(4) F9A 0.065(4) 0.090(5) 0.050(4) 0.014(4) -0.016(3) 0.008(4) F10A 0.091(5) 0.056(4) 0.087(5) 0.028(4) 0.011(4) 0.013(4) F11A 0.052(4) 0.090(6) 0.054(4) 0.013(4) 0.003(3) 0.025(4) F12A 0.048(4) 0.079(5) 0.079(5) 0.038(4) 0.007(3) 0.020(4) P2A 0.0301(16) 0.053(2) 0.0390(16) 0.0154(15) -0.0088(13) -0.0035(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.330(10) . ? C1 C2 1.366(12) . ? C1 H1 0.9500 . ? C2 C3 1.385(15) . ? C2 H2 0.9500 . ? C3 C4 1.369(15) . ? C3 H3 0.9500 . ? C4 C5 1.377(11) . ? C4 H4 0.9500 . ? C5 N1 1.360(10) . ? C5 C6 1.486(11) . ? C6 C7 1.452(11) . ? C6 N2 1.522(10) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N3 1.339(9) . ? C8 N2 1.353(10) . ? C8 Ir1 2.032(7) . ? C9 N2 1.482(9) . ? C9 C13 1.524(10) . ? C9 C10 1.547(11) . ? C9 H9 1.0000 . ? C10 C11 1.544(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.510(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.522(10) . ? C12 N3 1.537(9) . ? C12 C13 1.552(11) . ? C13 C15 1.511(11) . ? C13 C16 1.547(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N3 1.473(10) . ? C17 C18 1.477(15) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N4 1.381(13) . ? C18 C19 1.392(13) . ? C19 C20 1.394(13) . ? C19 H19 0.9500 . ? C20 C21 1.376(13) . ? C20 H20 0.9500 . ? C21 C22 1.394(10) . ? C21 H21 0.9500 . ? C22 N4 1.336(10) . ? C22 H22 0.9500 . ? C23 C24 1.351(11) . ? C23 C30 1.489(11) . ? C23 Ir1 2.123(6) . ? C23 H23 0.9500 . ? C24 C25 1.486(11) . ? C24 Ir1 2.137(7) . ? C24 H24 0.9500 . ? C25 C26 1.531(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.512(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.393(11) . ? C27 Ir1 2.223(8) . ? C27 H27 0.9500 . ? C28 C29 1.535(10) . ? C28 Ir1 2.244(7) . ? C28 H28 0.9500 . ? C29 C30 1.528(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N5 1.350(9) . ? C31 C32 1.389(11) . ? C31 H31 0.9500 . ? C32 C33 1.356(13) . ? C32 H32 0.9500 . ? C33 C34 1.385(12) . ? C33 H33 0.9500 . ? C34 C35 1.386(10) . ? C34 H34 0.9500 . ? C35 N5 1.361(9) . ? C35 C36 1.498(10) . ? C36 C37 1.482(10) . ? C36 N6 1.491(8) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N6 1.340(9) . ? C38 N7 1.353(9) . ? C38 Ir2 2.039(7) . ? C39 N6 1.481(9) . ? C39 C43 1.529(11) . ? C39 C40 1.537(11) . ? C39 H39 1.0000 . ? C40 C41 1.554(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.546(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N7 1.502(9) . ? C42 C44 1.513(10) . ? C42 C43 1.545(10) . ? C43 C46 1.518(11) . ? C43 C45 1.547(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.467(14) . ? C47 N7 1.499(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 N8 1.357(13) . ? C48 C49 1.387(13) . ? C49 C50 1.401(12) . ? C49 H49 0.9500 . ? C50 C51 1.386(12) . ? C50 H50 0.9500 . ? C51 C52 1.384(10) . ? C51 H51 0.9500 . ? C52 N8 1.340(10) . ? C52 H52 0.9500 . ? C53 C54 1.381(12) . ? C53 C60 1.502(12) . ? C53 Ir2 2.203(7) . ? C53 H53 0.9500 . ? C54 C55 1.496(10) . ? C54 Ir2 2.243(7) . ? C54 H54 0.9500 . ? C55 C56 1.538(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.496(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.350(10) . ? C57 Ir2 2.124(7) . ? C57 H57 0.9500 . ? C58 C59 1.502(11) . ? C58 Ir2 2.115(7) . ? C58 H58 0.9500 . ? C59 C60 1.505(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? N1 Ir1 2.206(6) . ? N4 Ir1 2.270(5) . ? N5 Ir2 2.214(6) . ? N8 Ir2 2.303(6) . ? F1 P1 1.562(6) . ? F2 P1 1.573(6) . ? F3 P1 1.573(6) . ? F4 P1 1.542(6) . ? F5 P1 1.560(7) . ? F6 P1 1.601(7) . ? F1A P1A 1.562(10) . ? F2A P1A 1.565(10) . ? F3A P1A 1.574(10) . ? F4A P1A 1.550(10) . ? F5A P1A 1.558(11) . ? F6A P1A 1.600(11) . ? F7 P2 1.576(7) . ? F8 P2 1.576(7) . ? F9 P2 1.572(7) . ? F10 P2 1.555(7) . ? F11 P2 1.572(7) . ? F12 P2 1.563(7) . ? F7A P2A 1.588(6) . ? F8A P2A 1.586(7) . ? F9A P2A 1.579(7) . ? F10A P2A 1.548(8) . ? F11A P2A 1.590(7) . ? F12A P2A 1.574(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.7(9) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 118.9(9) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 117.9(9) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 119.8(9) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 122.7(8) . . ? N1 C5 C6 119.6(7) . . ? C4 C5 C6 117.7(8) . . ? C7 C6 C5 120.8(8) . . ? C7 C6 N2 115.9(7) . . ? C5 C6 N2 109.4(6) . . ? C7 C6 H6 102.6 . . ? C5 C6 H6 102.6 . . ? N2 C6 H6 102.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N2 116.9(6) . . ? N3 C8 Ir1 123.1(6) . . ? N2 C8 Ir1 119.9(5) . . ? N2 C9 C13 108.7(6) . . ? N2 C9 C10 110.0(6) . . ? C13 C9 C10 104.6(6) . . ? N2 C9 H9 111.1 . . ? C13 C9 H9 111.1 . . ? C10 C9 H9 111.1 . . ? C11 C10 C9 104.2(6) . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C12 C11 C10 105.2(7) . . ? C12 C11 H11A 110.7 . . ? C10 C11 H11A 110.7 . . ? C12 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C11 C12 C14 115.9(7) . . ? C11 C12 N3 106.0(6) . . ? C14 C12 N3 110.7(6) . . ? C11 C12 C13 104.2(6) . . ? C14 C12 C13 113.9(6) . . ? N3 C12 C13 105.4(6) . . ? C15 C13 C9 114.7(6) . . ? C15 C13 C16 107.9(7) . . ? C9 C13 C16 109.2(6) . . ? C15 C13 C12 115.1(7) . . ? C9 C13 C12 98.0(6) . . ? C16 C13 C12 111.8(6) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 113.0(7) . . ? N3 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N3 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N4 C18 C19 121.3(10) . . ? N4 C18 C17 118.8(9) . . ? C19 C18 C17 119.9(9) . . ? C18 C19 C20 119.7(9) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 118.7(7) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 119.2(8) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N4 C22 C21 123.3(8) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C24 C23 C30 127.5(8) . . ? C24 C23 Ir1 72.1(4) . . ? C30 C23 Ir1 115.7(5) . . ? C24 C23 H23 116.2 . . ? C30 C23 H23 116.2 . . ? Ir1 C23 H23 81.8 . . ? C23 C24 C25 124.1(8) . . ? C23 C24 Ir1 70.9(4) . . ? C25 C24 Ir1 116.2(5) . . ? C23 C24 H24 118.0 . . ? C25 C24 H24 118.0 . . ? Ir1 C24 H24 83.0 . . ? C24 C25 C26 112.4(6) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 113.8(7) . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 125.1(7) . . ? C28 C27 Ir1 72.7(4) . . ? C26 C27 Ir1 108.5(6) . . ? C28 C27 H27 117.4 . . ? C26 C27 H27 117.4 . . ? Ir1 C27 H27 88.7 . . ? C27 C28 C29 122.2(7) . . ? C27 C28 Ir1 71.0(4) . . ? C29 C28 Ir1 112.4(5) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? Ir1 C28 H28 86.7 . . ? C30 C29 C28 112.7(6) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C23 C30 C29 110.7(7) . . ? C23 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C23 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? N5 C31 C32 122.4(7) . . ? N5 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C33 C32 C31 119.4(8) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 119.0(7) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C33 C34 C35 120.1(7) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? N5 C35 C34 120.9(7) . . ? N5 C35 C36 116.9(6) . . ? C34 C35 C36 122.2(7) . . ? C37 C36 N6 115.3(6) . . ? C37 C36 C35 117.1(6) . . ? N6 C36 C35 110.3(5) . . ? C37 C36 H36 104.1 . . ? N6 C36 H36 104.1 . . ? C35 C36 H36 104.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 N7 117.5(6) . . ? N6 C38 Ir2 120.9(5) . . ? N7 C38 Ir2 121.4(5) . . ? N6 C39 C43 108.7(6) . . ? N6 C39 C40 108.6(6) . . ? C43 C39 C40 105.2(6) . . ? N6 C39 H39 111.4 . . ? C43 C39 H39 111.4 . . ? C40 C39 H39 111.4 . . ? C39 C40 C41 103.1(6) . . ? C39 C40 H40A 111.2 . . ? C41 C40 H40A 111.2 . . ? C39 C40 H40B 111.2 . . ? C41 C40 H40B 111.2 . . ? H40A C40 H40B 109.1 . . ? C42 C41 C40 105.6(6) . . ? C42 C41 H41A 110.6 . . ? C40 C41 H41A 110.6 . . ? C42 C41 H41B 110.6 . . ? C40 C41 H41B 110.6 . . ? H41A C41 H41B 108.8 . . ? N7 C42 C44 111.9(6) . . ? N7 C42 C43 105.9(5) . . ? C44 C42 C43 114.4(7) . . ? N7 C42 C41 107.6(6) . . ? C44 C42 C41 112.4(7) . . ? C43 C42 C41 104.1(6) . . ? C46 C43 C39 114.7(6) . . ? C46 C43 C42 115.1(7) . . ? C39 C43 C42 97.9(6) . . ? C46 C43 C45 108.5(7) . . ? C39 C43 C45 108.8(7) . . ? C42 C43 C45 111.3(6) . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N7 113.5(7) . . ? C48 C47 H47A 108.9 . . ? N7 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? N7 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? N8 C48 C49 122.6(10) . . ? N8 C48 C47 119.2(8) . . ? C49 C48 C47 118.2(9) . . ? C48 C49 C50 119.7(8) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 C49 117.4(7) . . ? C51 C50 H50 121.3 . . ? C49 C50 H50 121.3 . . ? C52 C51 C50 119.6(8) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? N8 C52 C51 123.6(8) . . ? N8 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? C54 C53 C60 124.9(8) . . ? C54 C53 Ir2 73.5(4) . . ? C60 C53 Ir2 108.1(6) . . ? C54 C53 H53 117.5 . . ? C60 C53 H53 117.5 . . ? Ir2 C53 H53 88.3 . . ? C53 C54 C55 122.9(7) . . ? C53 C54 Ir2 70.3(4) . . ? C55 C54 Ir2 114.1(5) . . ? C53 C54 H54 118.6 . . ? C55 C54 H54 118.6 . . ? Ir2 C54 H54 85.7 . . ? C54 C55 C56 111.9(6) . . ? C54 C55 H55A 109.2 . . ? C56 C55 H55A 109.2 . . ? C54 C55 H55B 109.2 . . ? C56 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C57 C56 C55 111.2(8) . . ? C57 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C57 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C56 125.2(8) . . ? C58 C57 Ir2 71.1(4) . . ? C56 C57 Ir2 115.4(6) . . ? C58 C57 H57 117.4 . . ? C56 C57 H57 117.4 . . ? Ir2 C57 H57 83.4 . . ? C57 C58 C59 126.1(8) . . ? C57 C58 Ir2 71.8(4) . . ? C59 C58 Ir2 114.7(6) . . ? C57 C58 H58 116.9 . . ? C59 C58 H58 116.9 . . ? Ir2 C58 H58 83.3 . . ? C58 C59 C60 113.1(6) . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59B 109.0 . . ? C60 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C53 C60 C59 113.8(7) . . ? C53 C60 H60A 108.8 . . ? C59 C60 H60A 108.8 . . ? C53 C60 H60B 108.8 . . ? C59 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? C1 N1 C5 116.0(7) . . ? C1 N1 Ir1 125.2(5) . . ? C5 N1 Ir1 118.8(5) . . ? C8 N2 C9 119.7(6) . . ? C8 N2 C6 122.3(6) . . ? C9 N2 C6 117.4(6) . . ? C8 N3 C17 118.9(6) . . ? C8 N3 C12 124.2(6) . . ? C17 N3 C12 116.8(5) . . ? C22 N4 C18 117.7(7) . . ? C22 N4 Ir1 125.9(5) . . ? C18 N4 Ir1 116.3(6) . . ? C31 N5 C35 118.0(6) . . ? C31 N5 Ir2 123.8(5) . . ? C35 N5 Ir2 118.2(5) . . ? C38 N6 C39 121.1(6) . . ? C38 N6 C36 119.2(6) . . ? C39 N6 C36 117.6(5) . . ? C38 N7 C47 119.8(6) . . ? C38 N7 C42 121.3(6) . . ? C47 N7 C42 115.7(5) . . ? C52 N8 C48 117.2(7) . . ? C52 N8 Ir2 126.5(5) . . ? C48 N8 Ir2 116.3(6) . . ? C8 Ir1 C23 91.4(3) . . ? C8 Ir1 C24 95.3(3) . . ? C23 Ir1 C24 37.0(3) . . ? C8 Ir1 N1 84.1(3) . . ? C23 Ir1 N1 118.0(3) . . ? C24 Ir1 N1 155.0(3) . . ? C8 Ir1 C27 163.7(3) . . ? C23 Ir1 C27 93.4(3) . . ? C24 Ir1 C27 79.5(3) . . ? N1 Ir1 C27 107.2(3) . . ? C8 Ir1 C28 159.7(3) . . ? C23 Ir1 C28 78.0(3) . . ? C24 Ir1 C28 86.7(3) . . ? N1 Ir1 C28 85.6(2) . . ? C27 Ir1 C28 36.3(3) . . ? C8 Ir1 N4 83.6(3) . . ? C23 Ir1 N4 151.5(3) . . ? C24 Ir1 N4 115.4(3) . . ? N1 Ir1 N4 89.5(2) . . ? C27 Ir1 N4 84.8(3) . . ? C28 Ir1 N4 113.9(2) . . ? C38 Ir2 C58 96.1(3) . . ? C38 Ir2 C57 92.0(3) . . ? C58 Ir2 C57 37.1(3) . . ? C38 Ir2 C53 163.8(3) . . ? C58 Ir2 C53 80.0(3) . . ? C57 Ir2 C53 94.1(3) . . ? C38 Ir2 N5 84.9(3) . . ? C58 Ir2 N5 157.0(2) . . ? C57 Ir2 N5 119.9(3) . . ? C53 Ir2 N5 104.9(3) . . ? C38 Ir2 C54 159.9(3) . . ? C58 Ir2 C54 86.0(3) . . ? C57 Ir2 C54 77.6(3) . . ? C53 Ir2 C54 36.2(3) . . ? N5 Ir2 C54 85.5(2) . . ? C38 Ir2 N8 83.7(2) . . ? C58 Ir2 N8 114.7(3) . . ? C57 Ir2 N8 151.1(3) . . ? C53 Ir2 N8 83.7(3) . . ? N5 Ir2 N8 88.2(2) . . ? C54 Ir2 N8 113.6(3) . . ? F4 P1 F5 91.5(4) . . ? F4 P1 F1 91.4(4) . . ? F5 P1 F1 90.5(5) . . ? F4 P1 F3 89.4(4) . . ? F5 P1 F3 90.3(4) . . ? F1 P1 F3 178.8(6) . . ? F4 P1 F2 178.5(5) . . ? F5 P1 F2 89.6(4) . . ? F1 P1 F2 89.6(4) . . ? F3 P1 F2 89.6(4) . . ? F4 P1 F6 90.4(4) . . ? F5 P1 F6 176.7(5) . . ? F1 P1 F6 92.1(6) . . ? F3 P1 F6 87.1(4) . . ? F2 P1 F6 88.4(4) . . ? F4A P1A F5A 88.3(9) . . ? F4A P1A F1A 91.8(9) . . ? F5A P1A F1A 91.1(10) . . ? F4A P1A F2A 178.8(11) . . ? F5A P1A F2A 91.6(10) . . ? F1A P1A F2A 89.3(9) . . ? F4A P1A F3A 88.3(9) . . ? F5A P1A F3A 91.2(10) . . ? F1A P1A F3A 177.7(12) . . ? F2A P1A F3A 90.5(9) . . ? F4A P1A F6A 89.6(10) . . ? F5A P1A F6A 177.5(11) . . ? F1A P1A F6A 90.2(10) . . ? F2A P1A F6A 90.5(10) . . ? F3A P1A F6A 87.5(9) . . ? F10 P2 F12 90.7(5) . . ? F10 P2 F9 92.8(8) . . ? F12 P2 F9 90.0(5) . . ? F10 P2 F11 90.4(5) . . ? F12 P2 F11 178.9(7) . . ? F9 P2 F11 90.0(5) . . ? F10 P2 F7 89.7(6) . . ? F12 P2 F7 90.1(5) . . ? F9 P2 F7 177.5(8) . . ? F11 P2 F7 89.8(5) . . ? F10 P2 F8 178.6(8) . . ? F12 P2 F8 89.8(5) . . ? F9 P2 F8 88.6(6) . . ? F11 P2 F8 89.2(5) . . ? F7 P2 F8 89.0(5) . . ? F10A P2A F12A 91.4(5) . . ? F10A P2A F9A 92.3(5) . . ? F12A P2A F9A 90.6(5) . . ? F10A P2A F8A 179.4(6) . . ? F12A P2A F8A 89.2(5) . . ? F9A P2A F8A 87.5(5) . . ? F10A P2A F7A 90.6(5) . . ? F12A P2A F7A 90.2(4) . . ? F9A P2A F7A 176.9(5) . . ? F8A P2A F7A 89.5(5) . . ? F10A P2A F11A 91.2(6) . . ? F12A P2A F11A 177.4(6) . . ? F9A P2A F11A 89.7(5) . . ? F8A P2A F11A 88.3(5) . . ? F7A P2A F11A 89.4(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.391 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 965593' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kjc1239 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H40 Ir N4, F6 P' _chemical_formula_sum 'C30 H40 F6 Ir N4 P' _chemical_formula_weight 793.83 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.3682(2) _cell_length_b 10.7035(2) _cell_length_c 14.4653(2) _cell_angle_alpha 106.2400(10) _cell_angle_beta 96.2640(10) _cell_angle_gamma 90.7710(10) _cell_volume 1530.42(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10033 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 4.478 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4006 _exptl_absorpt_correction_T_max 0.4391 _exptl_absorpt_process_details Denzo/Scalpack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10368 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10368 _reflns_number_gt 10033 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains one enantiomer. It can be refined in P-1, but the result is a disordered structure with partial occupancies. P1 gives an ordered structure and so refinement in P-1 cannot be justified. The PF6 counter-ions were refined using a disordered model with two components on each site. Some geometric and the displacement parameters were restrained during to be similar for both components during refinement. There is a small void is small empty void with no residual electron density in the structure. ; _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^)+(0.0205P)^2^+4.6112P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(7) _refine_ls_number_reflns 10368 _refine_ls_number_parameters 893 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2514(12) 0.1671(11) 0.5049(7) 0.022(2) Uani 1 1 d . . . C2 C 0.3028(11) -0.0627(10) 0.4284(8) 0.034(2) Uani 1 1 d D . . C3 C 0.4292(14) -0.0637(14) 0.5030(10) 0.055(4) Uani 1 1 d D . . H3A H 0.4049 -0.0475 0.5695 0.066 Uiso 1 1 calc R . . H3B H 0.4688 -0.1495 0.4848 0.066 Uiso 1 1 calc R . . C4 C 0.5242(15) 0.0417(16) 0.4990(11) 0.061(4) Uani 1 1 d . . . H4A H 0.5472 0.1046 0.5636 0.073 Uiso 1 1 calc R . . H4B H 0.6044 0.0049 0.4732 0.073 Uiso 1 1 calc R . . C5 C 0.4482(10) 0.1035(11) 0.4308(8) 0.032(2) Uani 1 1 d . . . H5 H 0.5089 0.1442 0.3972 0.038 Uiso 1 1 calc R . . C6 C 0.3632(9) -0.0063(9) 0.3558(7) 0.025(2) Uani 1 1 d . . . C7 C 0.2273(11) -0.1910(9) 0.3830(8) 0.067(3) Uani 1 1 d . . . H7A H 0.2000 -0.2257 0.4341 0.100 Uiso 1 1 calc R . . H7B H 0.2824 -0.2531 0.3437 0.100 Uiso 1 1 calc R . . H7C H 0.1504 -0.1775 0.3417 0.100 Uiso 1 1 calc R . . C8 C 0.2642(8) 0.0439(9) 0.2887(6) 0.0309(19) Uani 1 1 d . . . H8A H 0.3106 0.0873 0.2498 0.046 Uiso 1 1 calc R . . H8B H 0.2091 0.1059 0.3279 0.046 Uiso 1 1 calc R . . H8C H 0.2101 -0.0297 0.2455 0.046 Uiso 1 1 calc R . . C9 C 0.4484(10) -0.1000(11) 0.2937(9) 0.036(2) Uani 1 1 d . . . H9A H 0.5030 -0.1428 0.3343 0.054 Uiso 1 1 calc R . . H9B H 0.5036 -0.0521 0.2631 0.054 Uiso 1 1 calc R . . H9C H 0.3936 -0.1659 0.2434 0.054 Uiso 1 1 calc R . . C10 C 0.0879(9) 0.0025(7) 0.4931(5) 0.0193(14) Uani 1 1 d D . . H10A H 0.0731 0.0370 0.5619 0.023 Uiso 1 1 calc R . . H10B H 0.0816 -0.0938 0.4768 0.023 Uiso 1 1 calc R . . C11 C -0.0156(8) 0.0441(8) 0.4337(6) 0.0298(18) Uani 1 1 d . . . C12 C -0.0994(8) -0.0475(8) 0.3652(6) 0.0440(19) Uani 1 1 d . . . H12 H -0.0916 -0.1377 0.3591 0.053 Uiso 1 1 calc R . . C13 C -0.1937(8) -0.0070(8) 0.3062(6) 0.047(2) Uani 1 1 d . . . H13 H -0.2500 -0.0687 0.2583 0.057 Uiso 1 1 calc R . . C14 C -0.2044(7) 0.1241(9) 0.3180(6) 0.0429(19) Uani 1 1 d . . . H14 H -0.2683 0.1549 0.2786 0.052 Uiso 1 1 calc R . . C15 C -0.1191(7) 0.2112(9) 0.3896(6) 0.0315(17) Uani 1 1 d . . . H15 H -0.1283 0.3018 0.3983 0.038 Uiso 1 1 calc R . . C16 C 0.3998(10) 0.3417(12) 0.4882(6) 0.041(3) Uani 1 1 d D . . H16 H 0.3780 0.3876 0.5545 0.049 Uiso 1 1 calc R . . C17 C 0.3062(10) 0.3946(10) 0.4296(7) 0.027(2) Uani 1 1 d . . . C18 C 0.3466(8) 0.4387(7) 0.3561(6) 0.0317(18) Uani 1 1 d . . . H18 H 0.4354 0.4353 0.3452 0.038 Uiso 1 1 calc R . . C19 C 0.2578(9) 0.4879(7) 0.2982(6) 0.0366(19) Uani 1 1 d . . . H19 H 0.2839 0.5172 0.2466 0.044 Uiso 1 1 calc R . . C20 C 0.1320(9) 0.4929(7) 0.3172(5) 0.0286(18) Uani 1 1 d . . . H20 H 0.0691 0.5270 0.2792 0.034 Uiso 1 1 calc R . . C21 C 0.0958(10) 0.4482(10) 0.3926(7) 0.029(2) Uani 1 1 d . . . H21 H 0.0084 0.4560 0.4067 0.035 Uiso 1 1 calc R . . C22 C 0.5401(7) 0.3745(8) 0.4999(7) 0.048(2) Uani 1 1 d . . . H22A H 0.5838 0.3402 0.5505 0.073 Uiso 1 1 calc R . . H22B H 0.5546 0.4694 0.5184 0.073 Uiso 1 1 calc R . . H22C H 0.5752 0.3358 0.4386 0.073 Uiso 1 1 calc R . . C23 C -0.0472(12) 0.4119(11) 0.6173(8) 0.034(3) Uani 1 1 d . . . H23 H -0.0931 0.3820 0.5541 0.040 Uiso 1 1 calc R . . C24 C 0.0540(11) 0.5043(12) 0.6306(9) 0.034(2) Uani 1 1 d . . . H24 H 0.0773 0.5275 0.5756 0.041 Uiso 1 1 calc R . . C25 C 0.1282(11) 0.5691(11) 0.7281(8) 0.039(3) Uani 1 1 d . . . H25A H 0.0719 0.5696 0.7792 0.047 Uiso 1 1 calc R . . H25B H 0.1504 0.6608 0.7318 0.047 Uiso 1 1 calc R . . C26 C 0.2515(11) 0.5025(12) 0.7475(8) 0.040(3) Uani 1 1 d . . . H26A H 0.3251 0.5452 0.7280 0.048 Uiso 1 1 calc R . . H26B H 0.2692 0.5123 0.8179 0.048 Uiso 1 1 calc R . . C27 C 0.2419(8) 0.3632(8) 0.6942(6) 0.0181(15) Uani 1 1 d D . . H27 H 0.3087 0.3306 0.6551 0.022 Uiso 1 1 calc R . . C28 C 0.1438(9) 0.2757(8) 0.6963(6) 0.0224(17) Uani 1 1 d D . . H28 H 0.1509 0.1869 0.6617 0.027 Uiso 1 1 calc R . . C29 C 0.0242(13) 0.3117(12) 0.7506(8) 0.044(3) Uani 1 1 d . . . H29A H -0.0052 0.2353 0.7699 0.053 Uiso 1 1 calc R . . H29B H 0.0504 0.3827 0.8107 0.053 Uiso 1 1 calc R . . C30 C -0.0905(12) 0.3553(11) 0.6927(9) 0.046(3) Uani 1 1 d . . . H30A H -0.1514 0.2796 0.6611 0.055 Uiso 1 1 calc R . . H30B H -0.1376 0.4212 0.7376 0.055 Uiso 1 1 calc R . . C31 C 0.5829(10) 1.0423(11) 0.8874(7) 0.020(2) Uani 1 1 d . . . C32 C 0.3654(10) 1.0989(11) 0.9477(9) 0.032(2) Uani 1 1 d . . . C33 C 0.3270(14) 1.1875(15) 0.8778(10) 0.050(3) Uani 1 1 d . . . H33A H 0.3255 1.1358 0.8092 0.060 Uiso 1 1 calc R . . H33B H 0.2396 1.2213 0.8876 0.060 Uiso 1 1 calc R . . C34 C 0.4303(14) 1.3030(14) 0.9023(10) 0.049(3) Uani 1 1 d . . . H34A H 0.4708 1.3079 0.8444 0.059 Uiso 1 1 calc R . . H34B H 0.3930 1.3875 0.9319 0.059 Uiso 1 1 calc R . . C35 C 0.5220(10) 1.2636(10) 0.9719(8) 0.029(2) Uani 1 1 d . . . H35 H 0.5719 1.3420 1.0164 0.034 Uiso 1 1 calc R . . C36 C 0.4462(8) 1.1966(9) 1.0302(6) 0.0203(17) Uani 1 1 d . . . C37 C 0.2540(7) 1.0291(9) 0.9729(8) 0.061(3) Uani 1 1 d . . . H37A H 0.2872 0.9765 1.0152 0.091 Uiso 1 1 calc R . . H37B H 0.2065 0.9723 0.9134 0.091 Uiso 1 1 calc R . . H37C H 0.1956 1.0929 1.0066 0.091 Uiso 1 1 calc R . . C38 C 0.5315(8) 1.1405(10) 1.1010(6) 0.035(2) Uani 1 1 d . . . H38A H 0.4774 1.0856 1.1269 0.052 Uiso 1 1 calc R . . H38B H 0.5739 1.2119 1.1543 0.052 Uiso 1 1 calc R . . H38C H 0.5977 1.0880 1.0668 0.052 Uiso 1 1 calc R . . C39 C 0.3583(10) 1.2971(11) 1.0928(8) 0.036(2) Uani 1 1 d . . . H39A H 0.2849 1.3153 1.0506 0.054 Uiso 1 1 calc R . . H39B H 0.4095 1.3780 1.1256 0.054 Uiso 1 1 calc R . . H39C H 0.3257 1.2605 1.1413 0.054 Uiso 1 1 calc R . . C40 C 0.4337(7) 0.8644(8) 0.8752(5) 0.0156(14) Uani 1 1 d D . . H40A H 0.4465 0.8230 0.8067 0.019 Uiso 1 1 calc R . . H40B H 0.3414 0.8487 0.8823 0.019 Uiso 1 1 calc R . . C41 C 0.5156(9) 0.8019(9) 0.9373(7) 0.027(2) Uani 1 1 d . . . C42 C 0.4597(9) 0.7395(8) 0.9974(7) 0.041(2) Uani 1 1 d . . . H42 H 0.3682 0.7358 0.9980 0.049 Uiso 1 1 calc R . . C43 C 0.5397(9) 0.6837(9) 1.0556(7) 0.045(2) Uani 1 1 d . . . H43 H 0.5042 0.6454 1.0996 0.054 Uiso 1 1 calc R . . C44 C 0.6721(10) 0.6837(8) 1.0498(6) 0.038(2) Uani 1 1 d . . . H44 H 0.7285 0.6426 1.0873 0.046 Uiso 1 1 calc R . . C45 C 0.7195(9) 0.7460(10) 0.9872(8) 0.029(2) Uani 1 1 d . . . H45 H 0.8103 0.7466 0.9829 0.034 Uiso 1 1 calc R . . C46 C 0.7516(13) 1.2228(11) 0.9285(8) 0.058(3) Uani 1 1 d D . . H46 H 0.7747 1.1782 0.8672 0.069 Uiso 1 1 calc R . . C47 C 0.8369(8) 1.1689(8) 0.9911(6) 0.0304(18) Uani 1 1 d . . . C48 C 0.9034(8) 1.2509(8) 1.0765(6) 0.043(2) Uani 1 1 d . . . H48 H 0.8967 1.3426 1.0915 0.052 Uiso 1 1 calc R . . C49 C 0.9789(8) 1.1962(11) 1.1385(6) 0.059(3) Uani 1 1 d . . . H49 H 1.0222 1.2500 1.1979 0.070 Uiso 1 1 calc R . . C50 C 0.9906(7) 1.0674(10) 1.1145(6) 0.050(2) Uani 1 1 d . . . H50 H 1.0439 1.0289 1.1556 0.060 Uiso 1 1 calc R . . C51 C 0.9242(7) 0.9908(9) 1.0290(6) 0.0339(18) Uani 1 1 d . . . H51 H 0.9346 0.8995 1.0123 0.041 Uiso 1 1 calc R . . C52 C 0.7652(9) 1.3608(8) 0.9272(7) 0.051(2) Uani 1 1 d . . . H52A H 0.6980 1.3774 0.8795 0.076 Uiso 1 1 calc R . . H52B H 0.8512 1.3773 0.9096 0.076 Uiso 1 1 calc R . . H52C H 0.7555 1.4186 0.9916 0.076 Uiso 1 1 calc R . . C53 C 0.6266(9) 0.8795(10) 0.6940(7) 0.032(2) Uani 1 1 d D . . H53 H 0.5517 0.9100 0.7242 0.039 Uiso 1 1 calc R . . C54 C 0.7237(9) 0.9702(9) 0.7060(6) 0.0276(19) Uani 1 1 d D . . H54 H 0.7155 1.0540 0.7475 0.033 Uiso 1 1 calc R . . C55 C 0.8411(13) 0.9434(12) 0.6572(9) 0.047(3) Uani 1 1 d . . . H55A H 0.8708 1.0226 0.6416 0.057 Uiso 1 1 calc R . . H55B H 0.8207 0.8736 0.5955 0.057 Uiso 1 1 calc R . . C56 C 0.9492(11) 0.9015(12) 0.7206(9) 0.045(3) Uani 1 1 d . . . H56A H 1.0030 0.9796 0.7592 0.054 Uiso 1 1 calc R . . H56B H 1.0055 0.8432 0.6782 0.054 Uiso 1 1 calc R . . C57 C 0.8997(11) 0.8306(11) 0.7901(8) 0.026(2) Uani 1 1 d . . . H57 H 0.9360 0.8582 0.8561 0.031 Uiso 1 1 calc R . . C58 C 0.8071(10) 0.7307(11) 0.7632(8) 0.024(2) Uani 1 1 d . . . H58 H 0.7796 0.6963 0.8120 0.029 Uiso 1 1 calc R . . C59 C 0.7461(10) 0.6721(11) 0.6593(8) 0.038(2) Uani 1 1 d . . . H59A H 0.8077 0.6847 0.6146 0.046 Uiso 1 1 calc R . . H59B H 0.7299 0.5773 0.6474 0.046 Uiso 1 1 calc R . . C60 C 0.6203(11) 0.7330(11) 0.6381(8) 0.044(3) Uani 1 1 d . . . H60A H 0.5481 0.6880 0.6573 0.053 Uiso 1 1 calc R . . H60B H 0.6030 0.7226 0.5676 0.053 Uiso 1 1 calc R . . N1 N -0.0265(7) 0.1748(8) 0.4458(6) 0.0255(16) Uani 1 1 d . . . N2 N 0.2164(9) 0.0412(9) 0.4836(6) 0.0254(18) Uani 1 1 d . . . N3 N 0.3646(9) 0.2030(9) 0.4833(7) 0.028(2) Uani 1 1 d . . . N4 N 0.1795(8) 0.3944(8) 0.4460(6) 0.0216(17) Uani 1 1 d . . . N5 N 0.6446(7) 0.8052(8) 0.9327(6) 0.0188(16) Uani 1 1 d . . . N6 N 0.4611(8) 1.0051(9) 0.8976(6) 0.0209(17) Uani 1 1 d . . . N7 N 0.6108(9) 1.1734(9) 0.9204(6) 0.0249(18) Uani 1 1 d . . . N8 N 0.8447(7) 1.0392(7) 0.9677(5) 0.0227(15) Uani 1 1 d . . . Ir1 Ir 0.123808(16) 0.307100(16) 0.559131(13) 0.02017(8) Uani 1 1 d . . . Ir2 Ir 0.716513(15) 0.915026(15) 0.836667(13) 0.01790(8) Uani 1 1 d . . . P1 P 0.7191(4) 0.5729(5) 0.3113(3) 0.0365(11) Uani 0.744(8) 1 d PDU A 1 F1 F 0.7135(7) 0.7013(6) 0.2796(6) 0.057(2) Uani 0.744(8) 1 d PDU A 1 F2 F 0.8091(8) 0.5174(8) 0.2291(6) 0.080(3) Uani 0.744(8) 1 d PDU A 1 F3 F 0.7186(12) 0.4380(9) 0.3332(8) 0.082(3) Uani 0.744(8) 1 d PDU A 1 F4 F 0.6242(9) 0.6270(9) 0.3885(6) 0.065(3) Uani 0.744(8) 1 d PDU A 1 F5 F 0.8450(9) 0.6307(10) 0.3845(6) 0.078(3) Uani 0.744(8) 1 d PDU A 1 F6 F 0.5967(8) 0.5166(9) 0.2336(7) 0.071(3) Uani 0.744(8) 1 d PDU A 1 P1A P 0.7212(13) 0.5381(13) 0.3038(9) 0.052(3) Uani 0.256(8) 1 d PDU A 2 F1A F 0.5982(17) 0.611(2) 0.3368(17) 0.070(5) Uani 0.256(8) 1 d PDU A 2 F2A F 0.658(2) 0.5091(19) 0.1943(11) 0.063(4) Uani 0.256(8) 1 d PDU A 2 F3A F 0.8362(18) 0.451(2) 0.2662(16) 0.059(5) Uani 0.256(8) 1 d PDU A 2 F4A F 0.783(2) 0.552(2) 0.4102(11) 0.073(5) Uani 0.256(8) 1 d PDU A 2 F5A F 0.789(2) 0.6677(19) 0.2956(19) 0.072(5) Uani 0.256(8) 1 d PDU A 2 F6A F 0.6480(17) 0.4059(15) 0.3035(14) 0.049(5) Uani 0.256(8) 1 d PDU A 2 P2 P 0.0981(15) 0.6398(14) 0.0535(9) 0.033(3) Uani 0.28(3) 1 d PDU B 1 F7 F 0.018(2) 0.756(2) 0.1089(17) 0.049(6) Uani 0.28(3) 1 d PDU B 1 F8 F 0.129(2) 0.718(2) -0.0185(17) 0.048(5) Uani 0.28(3) 1 d PDU B 1 F9 F 0.176(2) 0.523(2) -0.0041(19) 0.050(6) Uani 0.28(3) 1 d PDU B 1 F10 F 0.066(2) 0.561(3) 0.1250(18) 0.045(5) Uani 0.28(3) 1 d PDU B 1 F11 F 0.2248(17) 0.704(2) 0.1229(15) 0.044(5) Uani 0.28(3) 1 d PDU B 1 F12 F -0.0289(17) 0.579(2) -0.0150(14) 0.032(5) Uani 0.28(3) 1 d PDU B 1 P2A P 0.1046(6) 0.6375(6) 0.0542(4) 0.0245(12) Uani 0.72(3) 1 d PDU B 2 F7A F 0.0640(10) 0.5167(12) 0.0897(11) 0.055(3) Uani 0.72(3) 1 d PDU B 2 F8A F -0.0101(10) 0.6065(11) -0.0308(7) 0.043(2) Uani 0.72(3) 1 d PDU B 2 F9A F 0.1442(9) 0.7585(11) 0.0165(11) 0.049(3) Uani 0.72(3) 1 d PDU B 2 F10A F 0.2241(10) 0.6685(13) 0.1362(8) 0.058(3) Uani 0.72(3) 1 d PDU B 2 F11A F 0.0114(11) 0.7288(12) 0.1230(8) 0.049(2) Uani 0.72(3) 1 d PDU B 2 F12A F 0.1933(10) 0.5476(11) -0.0166(7) 0.040(2) Uani 0.72(3) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(6) 0.019(5) 0.011(4) 0.002(4) 0.004(4) 0.013(4) C2 0.049(5) 0.019(4) 0.037(5) 0.010(4) 0.010(4) 0.014(4) C3 0.065(8) 0.056(8) 0.048(6) 0.024(6) -0.005(6) 0.038(6) C4 0.059(8) 0.062(8) 0.055(8) 0.010(6) -0.010(6) 0.034(6) C5 0.021(4) 0.034(5) 0.039(5) 0.007(4) 0.000(4) 0.015(4) C6 0.024(4) 0.019(4) 0.024(4) -0.005(3) -0.003(3) 0.004(3) C7 0.077(7) 0.046(6) 0.081(7) 0.017(5) 0.029(6) 0.001(5) C8 0.035(5) 0.035(5) 0.021(4) 0.007(3) 0.000(3) 0.011(3) C9 0.027(4) 0.030(5) 0.043(5) -0.005(4) 0.006(4) 0.010(4) C10 0.034(4) 0.006(3) 0.019(3) 0.002(2) 0.010(3) 0.005(2) C11 0.033(4) 0.024(4) 0.034(5) 0.008(3) 0.007(3) -0.002(3) C12 0.048(5) 0.029(4) 0.050(5) 0.006(4) 0.004(4) -0.014(3) C13 0.036(4) 0.044(5) 0.051(5) -0.001(4) -0.004(4) -0.013(3) C14 0.025(3) 0.059(5) 0.043(5) 0.014(4) -0.003(3) -0.004(3) C15 0.025(4) 0.039(4) 0.031(4) 0.011(3) 0.005(3) 0.000(3) C16 0.038(5) 0.038(5) 0.041(6) 0.001(5) 0.000(4) 0.001(4) C17 0.028(4) 0.025(4) 0.027(4) 0.005(4) 0.004(3) -0.002(3) C18 0.037(4) 0.019(4) 0.037(4) 0.000(3) 0.019(3) -0.002(3) C19 0.064(6) 0.017(4) 0.033(4) 0.007(3) 0.021(4) 0.004(3) C20 0.061(5) 0.009(4) 0.017(3) 0.001(3) 0.013(3) 0.006(3) C21 0.040(5) 0.025(4) 0.024(4) 0.011(4) 0.005(4) 0.000(3) C22 0.024(4) 0.040(4) 0.066(6) -0.007(4) -0.002(4) -0.008(3) C23 0.045(6) 0.038(6) 0.021(4) 0.008(4) 0.013(4) 0.030(5) C24 0.043(6) 0.028(5) 0.029(5) 0.000(4) 0.017(4) 0.012(4) C25 0.055(6) 0.025(4) 0.032(5) -0.003(4) 0.012(4) 0.012(4) C26 0.046(5) 0.045(6) 0.018(4) -0.006(4) -0.001(4) 0.007(4) C27 0.020(3) 0.022(4) 0.013(3) 0.005(3) 0.004(3) 0.004(3) C28 0.026(4) 0.024(4) 0.018(4) 0.006(3) 0.004(3) 0.004(3) C29 0.066(7) 0.049(6) 0.025(4) 0.019(4) 0.015(4) 0.013(5) C30 0.057(6) 0.045(6) 0.046(6) 0.022(5) 0.029(5) 0.026(5) C31 0.020(5) 0.022(5) 0.016(5) 0.004(4) -0.003(4) 0.004(4) C32 0.020(4) 0.029(5) 0.040(5) -0.004(4) 0.003(4) 0.010(3) C33 0.046(6) 0.058(8) 0.041(6) 0.012(5) -0.009(5) 0.031(6) C34 0.055(6) 0.052(7) 0.045(6) 0.020(5) 0.005(5) 0.027(5) C35 0.039(5) 0.018(4) 0.030(4) 0.005(3) 0.014(4) 0.016(3) C36 0.022(4) 0.021(4) 0.018(4) 0.004(3) 0.005(3) 0.008(3) C37 0.025(4) 0.045(5) 0.098(8) -0.008(5) 0.023(4) 0.003(3) C38 0.035(5) 0.053(6) 0.017(3) 0.010(4) 0.002(3) 0.009(4) C39 0.032(5) 0.041(6) 0.035(5) 0.004(4) 0.018(4) 0.009(4) C40 0.012(3) 0.016(3) 0.015(3) -0.002(3) 0.002(2) 0.005(2) C41 0.021(4) 0.020(4) 0.037(5) 0.003(4) 0.007(3) 0.004(3) C42 0.035(4) 0.030(5) 0.060(6) 0.010(4) 0.021(4) -0.004(3) C43 0.061(6) 0.032(5) 0.054(6) 0.019(4) 0.036(5) 0.008(4) C44 0.068(6) 0.013(4) 0.036(5) 0.007(4) 0.016(4) 0.009(4) C45 0.024(4) 0.027(5) 0.037(5) 0.010(4) 0.007(3) 0.010(3) C46 0.060(7) 0.050(6) 0.071(8) 0.023(6) 0.023(6) 0.001(5) C47 0.029(4) 0.027(4) 0.029(4) -0.005(3) 0.012(3) -0.006(3) C48 0.043(4) 0.033(4) 0.041(4) -0.014(4) 0.020(4) -0.011(3) C49 0.036(4) 0.080(7) 0.037(5) -0.020(5) 0.002(4) -0.017(4) C50 0.024(4) 0.082(7) 0.031(4) -0.001(4) -0.004(3) -0.004(4) C51 0.018(3) 0.049(5) 0.030(4) 0.006(4) -0.001(3) 0.003(3) C52 0.061(5) 0.032(4) 0.065(6) 0.016(4) 0.028(5) 0.001(4) C53 0.034(5) 0.031(5) 0.029(4) 0.005(4) -0.003(4) 0.006(4) C54 0.031(4) 0.026(4) 0.025(4) 0.006(3) -0.001(3) 0.005(3) C55 0.067(7) 0.043(6) 0.042(6) 0.019(5) 0.031(5) 0.017(5) C56 0.042(5) 0.048(6) 0.052(6) 0.018(5) 0.033(5) 0.017(4) C57 0.025(4) 0.028(4) 0.022(4) 0.000(3) 0.011(3) 0.008(3) C58 0.024(4) 0.023(4) 0.023(4) 0.005(4) 0.001(3) 0.008(3) C59 0.044(5) 0.035(5) 0.025(4) -0.005(4) -0.001(4) 0.021(4) C60 0.049(6) 0.039(5) 0.029(5) -0.010(4) -0.010(4) 0.020(4) N1 0.019(3) 0.034(4) 0.028(4) 0.013(3) 0.008(3) 0.003(3) N2 0.037(4) 0.016(4) 0.025(4) 0.006(3) 0.009(3) 0.014(3) N3 0.027(4) 0.024(4) 0.028(4) 0.000(3) 0.000(3) 0.007(3) N4 0.028(4) 0.015(3) 0.022(3) 0.006(3) 0.004(3) 0.001(3) N5 0.016(3) 0.016(3) 0.021(3) 0.000(3) 0.002(2) -0.001(2) N6 0.013(3) 0.022(4) 0.021(4) -0.003(3) -0.002(3) 0.010(3) N7 0.033(4) 0.025(4) 0.019(3) 0.006(3) 0.014(3) 0.007(3) N8 0.019(3) 0.025(3) 0.021(3) -0.002(3) 0.011(2) 0.003(2) Ir1 0.02653(19) 0.01985(19) 0.01477(16) 0.00490(14) 0.00423(14) 0.00900(15) Ir2 0.02135(17) 0.01704(18) 0.01365(16) 0.00146(13) 0.00181(13) 0.00656(14) P1 0.0357(19) 0.034(2) 0.050(2) 0.0225(18) 0.0200(16) 0.0121(15) F1 0.062(5) 0.049(4) 0.064(4) 0.031(3) -0.007(4) -0.007(3) F2 0.079(5) 0.080(5) 0.079(5) 0.009(4) 0.040(4) 0.020(4) F3 0.110(6) 0.055(5) 0.094(6) 0.044(4) 0.015(5) 0.015(4) F4 0.066(5) 0.075(6) 0.049(5) 0.001(4) 0.030(4) 0.011(4) F5 0.064(5) 0.088(6) 0.077(6) 0.025(5) -0.013(4) 0.012(4) F6 0.059(5) 0.068(5) 0.076(5) 0.013(4) -0.005(4) -0.024(4) P1A 0.049(5) 0.051(5) 0.059(5) 0.021(4) 0.008(4) 0.006(4) F1A 0.063(7) 0.069(8) 0.078(8) 0.016(7) 0.016(7) 0.014(6) F2A 0.070(8) 0.066(7) 0.056(7) 0.028(6) 0.002(6) -0.004(7) F3A 0.055(8) 0.061(8) 0.059(8) 0.013(7) 0.006(7) 0.021(7) F4A 0.071(8) 0.080(8) 0.066(7) 0.017(7) -0.002(7) 0.015(7) F5A 0.073(8) 0.067(8) 0.076(8) 0.019(6) 0.012(7) -0.007(7) F6A 0.050(8) 0.049(8) 0.055(8) 0.022(6) 0.014(7) -0.004(6) P2 0.034(5) 0.033(5) 0.037(5) 0.016(4) 0.007(4) 0.000(4) F7 0.058(8) 0.042(8) 0.046(8) 0.012(6) 0.004(7) 0.012(7) F8 0.064(8) 0.044(8) 0.038(7) 0.019(6) 0.003(6) -0.014(6) F9 0.053(8) 0.044(8) 0.053(8) 0.011(6) 0.006(7) 0.025(7) F10 0.058(8) 0.046(8) 0.041(7) 0.027(6) 0.007(6) -0.011(6) F11 0.032(7) 0.047(8) 0.043(8) 0.003(6) -0.010(6) -0.007(6) F12 0.019(6) 0.044(8) 0.034(7) 0.010(6) 0.005(6) -0.013(6) P2A 0.0168(17) 0.025(2) 0.034(2) 0.0113(18) 0.0055(16) 0.0021(16) F7A 0.061(5) 0.044(5) 0.066(5) 0.029(4) 0.000(4) -0.015(4) F8A 0.030(4) 0.059(5) 0.042(4) 0.019(4) -0.002(3) 0.002(3) F9A 0.054(4) 0.035(4) 0.070(6) 0.031(4) 0.020(4) 0.004(3) F10A 0.054(5) 0.057(5) 0.057(5) 0.017(4) -0.025(4) -0.016(4) F11A 0.055(4) 0.050(5) 0.046(4) 0.009(4) 0.030(4) 0.016(4) F12A 0.043(4) 0.045(5) 0.035(4) 0.011(3) 0.015(3) 0.021(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.326(15) . ? C1 N2 1.331(14) . ? C1 Ir1 2.058(11) . ? C2 C7 1.512(14) . ? C2 C6 1.533(14) . ? C2 N2 1.538(15) . ? C2 C3 1.605(14) . ? C3 C4 1.51(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.496(17) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.475(15) . ? C5 C6 1.545(13) . ? C5 H5 1.0000 . ? C6 C9 1.512(15) . ? C6 C8 1.540(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.422(12) . ? C10 C11 1.454(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N1 1.368(12) . ? C11 C12 1.394(11) . ? C12 C13 1.382(12) . ? C12 H12 0.9500 . ? C13 C14 1.373(12) . ? C13 H13 0.9500 . ? C14 C15 1.401(11) . ? C14 H14 0.9500 . ? C15 N1 1.324(11) . ? C15 H15 0.9500 . ? C16 C17 1.444(16) . ? C16 C22 1.472(12) . ? C16 N3 1.505(15) . ? C16 H16 1.0000 . ? C17 N4 1.360(13) . ? C17 C18 1.378(12) . ? C18 C19 1.385(12) . ? C18 H18 0.9500 . ? C19 C20 1.361(13) . ? C19 H19 0.9500 . ? C20 C21 1.391(12) . ? C20 H20 0.9500 . ? C21 N4 1.341(13) . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.392(16) . ? C23 C30 1.492(16) . ? C23 Ir1 2.228(11) . ? C23 H23 0.9500 . ? C24 C25 1.504(17) . ? C24 Ir1 2.244(12) . ? C24 H24 0.9500 . ? C25 C26 1.510(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.471(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.381(10) . ? C27 Ir1 2.116(8) . ? C27 H27 0.9500 . ? C28 C29 1.536(16) . ? C28 Ir1 2.093(8) . ? C28 H28 0.9500 . ? C29 C30 1.533(17) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N6 1.354(14) . ? C31 N7 1.366(14) . ? C31 Ir2 2.007(11) . ? C32 C37 1.498(13) . ? C32 C36 1.511(13) . ? C32 N6 1.515(14) . ? C32 C33 1.595(17) . ? C33 C34 1.56(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.461(16) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N7 1.451(14) . ? C35 C36 1.520(13) . ? C35 H35 1.0000 . ? C36 C38 1.533(12) . ? C36 C39 1.571(14) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N6 1.466(12) . ? C40 C41 1.470(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N5 1.347(12) . ? C41 C42 1.401(13) . ? C42 C43 1.376(13) . ? C42 H42 0.9500 . ? C43 C44 1.384(14) . ? C43 H43 0.9500 . ? C44 C45 1.390(13) . ? C44 H44 0.9500 . ? C45 N5 1.335(13) . ? C45 H45 0.9500 . ? C46 C47 1.437(16) . ? C46 C52 1.488(13) . ? C46 N7 1.527(15) . ? C46 H46 0.9400 . ? C47 N8 1.340(12) . ? C47 C48 1.400(11) . ? C48 C49 1.383(14) . ? C48 H48 0.9500 . ? C49 C50 1.335(14) . ? C49 H49 0.9500 . ? C50 C51 1.381(11) . ? C50 H50 0.9500 . ? C51 N8 1.357(11) . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.352(12) . ? C53 C60 1.547(15) . ? C53 Ir2 2.098(9) . ? C53 H53 0.9500 . ? C54 C55 1.465(16) . ? C54 Ir2 2.140(10) . ? C54 H54 0.9400 . ? C55 C56 1.522(18) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.542(16) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.370(14) . ? C57 Ir2 2.205(11) . ? C57 H57 0.9500 . ? C58 C59 1.519(15) . ? C58 Ir2 2.236(11) . ? C58 H58 0.9500 . ? C59 C60 1.506(15) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? N1 Ir1 2.282(8) . ? N4 Ir1 2.221(8) . ? N5 Ir2 2.232(8) . ? N8 Ir2 2.263(7) . ? P1 F3 1.563(8) . ? P1 F4 1.563(7) . ? P1 F1 1.565(7) . ? P1 F2 1.581(7) . ? P1 F5 1.587(8) . ? P1 F6 1.590(8) . ? P1A F1A 1.556(11) . ? P1A F4A 1.567(11) . ? P1A F3A 1.572(12) . ? P1A F5A 1.584(12) . ? P1A F2A 1.589(11) . ? P1A F6A 1.596(11) . ? P2 F8 1.562(8) . ? P2 F10 1.564(8) . ? P2 F12 1.571(9) . ? P2 F7 1.576(9) . ? P2 F9 1.582(9) . ? P2 F11 1.584(9) . ? P2A F8A 1.575(7) . ? P2A F12A 1.581(8) . ? P2A F10A 1.581(8) . ? P2A F7A 1.587(8) . ? P2A F11A 1.603(8) . ? P2A F9A 1.604(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 N3 C1 N2 120.0(10) . . ? N3 C1 Ir1 119.4(8) . . ? N2 C1 Ir1 120.4(8) . . ? C7 C2 C6 114.2(9) . . ? C7 C2 N2 111.2(9) . . ? C6 C2 N2 107.2(8) . . ? C7 C2 C3 116.9(9) . . ? C6 C2 C3 100.3(9) . . ? N2 C2 C3 106.1(9) . . ? C4 C3 C2 108.0(10) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C3 101.6(11) . . ? C5 C4 H4A 111.4 . . ? C3 C4 H4A 111.4 . . ? C5 C4 H4B 111.4 . . ? C3 C4 H4B 111.4 . . ? H4A C4 H4B 109.3 . . ? N3 C5 C4 110.8(10) . . ? N3 C5 C6 109.7(8) . . ? C4 C5 C6 106.9(10) . . ? N3 C5 H5 109.8 . . ? C4 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C9 C6 C2 113.2(9) . . ? C9 C6 C8 108.5(8) . . ? C2 C6 C8 114.4(8) . . ? C9 C6 C5 109.9(8) . . ? C2 C6 C5 97.1(8) . . ? C8 C6 C5 113.5(8) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 115.9(7) . . ? N2 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? N2 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? N1 C11 C12 121.3(8) . . ? N1 C11 C10 118.2(7) . . ? C12 C11 C10 120.5(7) . . ? C13 C12 C11 120.0(8) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 118.8(7) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 118.5(8) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? N1 C15 C14 123.9(8) . . ? N1 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C17 C16 C22 122.9(9) . . ? C17 C16 N3 112.3(8) . . ? C22 C16 N3 115.0(9) . . ? C17 C16 H16 100.5 . . ? C22 C16 H16 100.5 . . ? N3 C16 H16 100.5 . . ? N4 C17 C18 121.9(9) . . ? N4 C17 C16 118.9(9) . . ? C18 C17 C16 119.2(9) . . ? C17 C18 C19 120.0(8) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 118.1(7) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 119.9(9) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? N4 C21 C20 122.5(10) . . ? N4 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C30 126.3(11) . . ? C24 C23 Ir1 72.5(7) . . ? C30 C23 Ir1 109.0(8) . . ? C24 C23 H23 116.8 . . ? C30 C23 H23 116.8 . . ? Ir1 C23 H23 88.5 . . ? C23 C24 C25 123.0(11) . . ? C23 C24 Ir1 71.2(7) . . ? C25 C24 Ir1 113.4(8) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? Ir1 C24 H24 85.4 . . ? C24 C25 C26 113.0(9) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 111.6(9) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 125.4(8) . . ? C28 C27 Ir1 69.9(5) . . ? C26 C27 Ir1 117.3(7) . . ? C28 C27 H27 117.3 . . ? C26 C27 H27 117.3 . . ? Ir1 C27 H27 82.8 . . ? C27 C28 C29 124.7(8) . . ? C27 C28 Ir1 71.8(5) . . ? C29 C28 Ir1 113.4(7) . . ? C27 C28 H28 117.7 . . ? C29 C28 H28 117.7 . . ? Ir1 C28 H28 84.8 . . ? C30 C29 C28 114.8(9) . . ? C30 C29 H29A 108.6 . . ? C28 C29 H29A 108.6 . . ? C30 C29 H29B 108.6 . . ? C28 C29 H29B 108.6 . . ? H29A C29 H29B 107.5 . . ? C23 C30 C29 111.9(10) . . ? C23 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? C23 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? N6 C31 N7 114.6(10) . . ? N6 C31 Ir2 123.0(8) . . ? N7 C31 Ir2 122.2(8) . . ? C37 C32 C36 117.1(9) . . ? C37 C32 N6 111.9(9) . . ? C36 C32 N6 105.3(8) . . ? C37 C32 C33 115.4(9) . . ? C36 C32 C33 100.3(9) . . ? N6 C32 C33 105.5(10) . . ? C34 C33 C32 108.0(10) . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33B 110.1 . . ? C32 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C35 C34 C33 99.7(10) . . ? C35 C34 H34A 111.8 . . ? C33 C34 H34A 111.8 . . ? C35 C34 H34B 111.8 . . ? C33 C34 H34B 111.8 . . ? H34A C34 H34B 109.6 . . ? N7 C35 C34 109.6(10) . . ? N7 C35 C36 109.4(8) . . ? C34 C35 C36 108.7(10) . . ? N7 C35 H35 109.7 . . ? C34 C35 H35 109.7 . . ? C36 C35 H35 109.7 . . ? C32 C36 C35 99.1(8) . . ? C32 C36 C38 116.1(8) . . ? C35 C36 C38 114.2(8) . . ? C32 C36 C39 111.1(8) . . ? C35 C36 C39 109.6(8) . . ? C38 C36 C39 106.6(8) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 C41 113.7(7) . . ? N6 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? N6 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? N5 C41 C42 121.9(9) . . ? N5 C41 C40 117.6(8) . . ? C42 C41 C40 120.5(8) . . ? C43 C42 C41 118.8(8) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 119.8(7) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 117.7(9) . . ? C43 C44 H44 121.1 . . ? C45 C44 H44 121.1 . . ? N5 C45 C44 123.7(9) . . ? N5 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? C47 C46 C52 122.5(9) . . ? C47 C46 N7 112.1(8) . . ? C52 C46 N7 113.6(10) . . ? C47 C46 H46 101.5 . . ? C52 C46 H46 101.5 . . ? N7 C46 H46 101.5 . . ? N8 C47 C48 121.9(9) . . ? N8 C47 C46 118.0(8) . . ? C48 C47 C46 120.0(9) . . ? C49 C48 C47 119.0(8) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C50 C49 C48 119.6(8) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 119.2(9) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? N8 C51 C50 123.4(9) . . ? N8 C51 H51 118.3 . . ? C50 C51 H51 118.3 . . ? C46 C52 H52A 109.5 . . ? C46 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C46 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C60 129.2(9) . . ? C54 C53 Ir2 73.1(6) . . ? C60 C53 Ir2 112.1(7) . . ? C54 C53 H53 115.4 . . ? C60 C53 H53 115.4 . . ? Ir2 C53 H53 84.3 . . ? C53 C54 C55 122.8(9) . . ? C53 C54 Ir2 69.7(6) . . ? C55 C54 Ir2 117.9(8) . . ? C53 C54 H54 118.6 . . ? C55 C54 H54 118.6 . . ? Ir2 C54 H54 82.7 . . ? C54 C55 C56 111.2(9) . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C55 C56 C57 113.7(9) . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56B 108.8 . . ? C57 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C58 C57 C56 124.5(10) . . ? C58 C57 Ir2 73.3(7) . . ? C56 C57 Ir2 108.7(8) . . ? C58 C57 H57 117.7 . . ? C56 C57 H57 117.7 . . ? Ir2 C57 H57 88.0 . . ? C57 C58 C59 123.3(10) . . ? C57 C58 Ir2 70.8(7) . . ? C59 C58 Ir2 112.5(7) . . ? C57 C58 H58 118.3 . . ? C59 C58 H58 118.3 . . ? Ir2 C58 H58 86.8 . . ? C60 C59 C58 112.0(9) . . ? C60 C59 H59A 109.2 . . ? C58 C59 H59A 109.2 . . ? C60 C59 H59B 109.2 . . ? C58 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 C53 110.6(8) . . ? C59 C60 H60A 109.5 . . ? C53 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C53 C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? C15 N1 C11 117.6(8) . . ? C15 N1 Ir1 126.9(6) . . ? C11 N1 Ir1 115.5(6) . . ? C1 N2 C10 120.2(9) . . ? C1 N2 C2 120.2(9) . . ? C10 N2 C2 118.3(8) . . ? C1 N3 C5 119.8(9) . . ? C1 N3 C16 122.6(10) . . ? C5 N3 C16 116.0(9) . . ? C21 N4 C17 117.4(9) . . ? C21 N4 Ir1 124.0(7) . . ? C17 N4 Ir1 118.6(7) . . ? C45 N5 C41 118.1(9) . . ? C45 N5 Ir2 125.2(6) . . ? C41 N5 Ir2 116.7(7) . . ? C31 N6 C40 116.0(8) . . ? C31 N6 C32 123.4(9) . . ? C40 N6 C32 119.6(8) . . ? C31 N7 C35 122.4(9) . . ? C31 N7 C46 118.5(9) . . ? C35 N7 C46 117.1(9) . . ? C47 N8 C51 116.8(8) . . ? C47 N8 Ir2 118.8(6) . . ? C51 N8 Ir2 124.2(6) . . ? C1 Ir1 C28 93.7(4) . . ? C1 Ir1 C27 90.3(4) . . ? C28 Ir1 C27 38.3(3) . . ? C1 Ir1 N4 84.4(4) . . ? C28 Ir1 N4 154.7(3) . . ? C27 Ir1 N4 116.4(3) . . ? C1 Ir1 C23 164.5(4) . . ? C28 Ir1 C23 80.9(4) . . ? C27 Ir1 C23 94.2(4) . . ? N4 Ir1 C23 106.6(4) . . ? C1 Ir1 C24 158.6(4) . . ? C28 Ir1 C24 87.0(4) . . ? C27 Ir1 C24 77.1(4) . . ? N4 Ir1 C24 85.9(4) . . ? C23 Ir1 C24 36.3(4) . . ? C1 Ir1 N1 84.5(4) . . ? C28 Ir1 N1 116.1(3) . . ? C27 Ir1 N1 153.6(3) . . ? N4 Ir1 N1 88.9(3) . . ? C23 Ir1 N1 84.9(4) . . ? C24 Ir1 N1 114.3(4) . . ? C31 Ir2 C53 91.4(4) . . ? C31 Ir2 C54 94.9(4) . . ? C53 Ir2 C54 37.2(3) . . ? C31 Ir2 C57 162.5(4) . . ? C53 Ir2 C57 93.4(4) . . ? C54 Ir2 C57 79.0(4) . . ? C31 Ir2 N5 84.6(4) . . ? C53 Ir2 N5 119.4(3) . . ? C54 Ir2 N5 156.6(3) . . ? C57 Ir2 N5 107.5(4) . . ? C31 Ir2 C58 161.2(4) . . ? C53 Ir2 C58 78.9(4) . . ? C54 Ir2 C58 87.1(4) . . ? C57 Ir2 C58 35.9(4) . . ? N5 Ir2 C58 86.2(4) . . ? C31 Ir2 N8 83.1(4) . . ? C53 Ir2 N8 151.5(3) . . ? C54 Ir2 N8 115.2(3) . . ? C57 Ir2 N8 84.7(3) . . ? N5 Ir2 N8 88.0(3) . . ? C58 Ir2 N8 112.9(3) . . ? F3 P1 F4 91.4(6) . . ? F3 P1 F1 174.7(6) . . ? F4 P1 F1 90.9(5) . . ? F3 P1 F2 89.2(5) . . ? F4 P1 F2 177.1(6) . . ? F1 P1 F2 88.2(4) . . ? F3 P1 F5 94.9(6) . . ? F4 P1 F5 93.6(6) . . ? F1 P1 F5 89.8(5) . . ? F2 P1 F5 89.2(5) . . ? F3 P1 F6 86.8(6) . . ? F4 P1 F6 88.8(6) . . ? F1 P1 F6 88.5(5) . . ? F2 P1 F6 88.4(5) . . ? F5 P1 F6 177.1(6) . . ? F1A P1A F4A 93.4(10) . . ? F1A P1A F3A 174.1(11) . . ? F4A P1A F3A 88.7(10) . . ? F1A P1A F5A 91.2(10) . . ? F4A P1A F5A 95.7(10) . . ? F3A P1A F5A 94.0(11) . . ? F1A P1A F2A 89.1(10) . . ? F4A P1A F2A 174.4(11) . . ? F3A P1A F2A 88.3(9) . . ? F5A P1A F2A 89.3(10) . . ? F1A P1A F6A 88.4(10) . . ? F4A P1A F6A 88.8(10) . . ? F3A P1A F6A 86.2(10) . . ? F5A P1A F6A 175.5(11) . . ? F2A P1A F6A 86.2(9) . . ? F8 P2 F10 179.5(8) . . ? F8 P2 F12 89.8(6) . . ? F10 P2 F12 89.8(6) . . ? F8 P2 F7 90.3(6) . . ? F10 P2 F7 89.8(6) . . ? F12 P2 F7 89.4(7) . . ? F8 P2 F9 89.4(6) . . ? F10 P2 F9 90.5(6) . . ? F12 P2 F9 89.3(9) . . ? F7 P2 F9 178.7(10) . . ? F8 P2 F11 89.6(6) . . ? F10 P2 F11 90.9(6) . . ? F12 P2 F11 178.6(9) . . ? F7 P2 F11 89.4(6) . . ? F9 P2 F11 91.9(10) . . ? F8A P2A F12A 89.1(5) . . ? F8A P2A F10A 177.5(6) . . ? F12A P2A F10A 88.9(6) . . ? F8A P2A F7A 92.5(5) . . ? F12A P2A F7A 89.8(6) . . ? F10A P2A F7A 88.9(5) . . ? F8A P2A F11A 89.1(5) . . ? F12A P2A F11A 178.1(6) . . ? F10A P2A F11A 92.9(5) . . ? F7A P2A F11A 90.9(6) . . ? F8A P2A F9A 86.5(5) . . ? F12A P2A F9A 89.9(5) . . ? F10A P2A F9A 92.1(5) . . ? F7A P2A F9A 179.0(6) . . ? F11A P2A F9A 89.5(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.132 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 965594' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kjc1234 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 N3 O, F6 P' _chemical_formula_sum 'C24 H32 F6 N3 O P' _chemical_formula_weight 523.50 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6919(2) _cell_length_b 17.3620(6) _cell_length_c 16.9847(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.288(2) _cell_angle_gamma 90.00 _cell_volume 2558.92(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9321 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 30.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9185 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11234 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 30.50 _reflns_number_total 11234 _reflns_number_gt 9321 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0411P)^2^+2.0554P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(10) _refine_ls_number_reflns 11234 _refine_ls_number_parameters 641 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3500(4) 0.80484(16) 0.63355(16) 0.0320(6) Uani 1 1 d . . . H1 H 1.2621 0.8038 0.5977 0.038 Uiso 1 1 calc R . . C2 C 1.4661(3) 0.80063(18) 0.76829(16) 0.0301(6) Uani 1 1 d . . . C3 C 1.5218(4) 0.88464(19) 0.7756(2) 0.0400(7) Uani 1 1 d . . . H3A H 1.5862 0.8923 0.8250 0.048 Uiso 1 1 calc R . . H3B H 1.4334 0.9206 0.7751 0.048 Uiso 1 1 calc R . . C4 C 1.6182(4) 0.8973(2) 0.7021(2) 0.0454(8) Uani 1 1 d . . . H4A H 1.5694 0.9366 0.6666 0.054 Uiso 1 1 calc R . . H4B H 1.7241 0.9142 0.7182 0.054 Uiso 1 1 calc R . . C5 C 1.6204(4) 0.81833(19) 0.66123(19) 0.0399(7) Uani 1 1 d . . . H5 H 1.7191 0.8098 0.6350 0.048 Uiso 1 1 calc R . . C6 C 1.5997(3) 0.75944(18) 0.72741(17) 0.0334(6) Uani 1 1 d . . . C7 C 1.4254(4) 0.7625(2) 0.84501(18) 0.0424(8) Uani 1 1 d . . . H7A H 1.3465 0.7930 0.8697 0.064 Uiso 1 1 calc R . . H7B H 1.5177 0.7593 0.8808 0.064 Uiso 1 1 calc R . . H7C H 1.3857 0.7105 0.8340 0.064 Uiso 1 1 calc R . . C8 C 1.7486(4) 0.7569(3) 0.7811(2) 0.0526(9) Uani 1 1 d . . . H8A H 1.7334 0.7230 0.8261 0.079 Uiso 1 1 calc R . . H8B H 1.7737 0.8089 0.8002 0.079 Uiso 1 1 calc R . . H8C H 1.8332 0.7372 0.7512 0.079 Uiso 1 1 calc R . . C9 C 1.5619(4) 0.67801(19) 0.6987(2) 0.0426(8) Uani 1 1 d . . . H9A H 1.4598 0.6776 0.6710 0.064 Uiso 1 1 calc R . . H9B H 1.5623 0.6430 0.7439 0.064 Uiso 1 1 calc R . . H9C H 1.6393 0.6612 0.6626 0.064 Uiso 1 1 calc R . . C10 C 1.1689(3) 0.80008(18) 0.73609(18) 0.0325(6) Uani 1 1 d . . . H10A H 1.1590 0.7604 0.7774 0.039 Uiso 1 1 calc R . . H10B H 1.0972 0.7864 0.6909 0.039 Uiso 1 1 calc R . . C11 C 1.1232(3) 0.87723(18) 0.76821(18) 0.0335(6) Uani 1 1 d . . . C12 C 1.1060(4) 0.94031(19) 0.71698(19) 0.0356(7) Uani 1 1 d . . . C13 C 1.0686(4) 1.0130(2) 0.7446(2) 0.0491(9) Uani 1 1 d . . . H13 H 1.0603 1.0557 0.7096 0.059 Uiso 1 1 calc R . . C14 C 1.0436(5) 1.0221(2) 0.8242(3) 0.0575(10) Uani 1 1 d . . . H14 H 1.0193 1.0715 0.8440 0.069 Uiso 1 1 calc R . . C15 C 1.0537(5) 0.9604(3) 0.8742(2) 0.0588(11) Uani 1 1 d . . . H15 H 1.0332 0.9669 0.9281 0.071 Uiso 1 1 calc R . . C16 C 1.0937(4) 0.8884(2) 0.8467(2) 0.0442(8) Uani 1 1 d . . . H16 H 1.1010 0.8461 0.8822 0.053 Uiso 1 1 calc R . . C17 C 1.1017(5) 0.9839(3) 0.5831(2) 0.0614(11) Uani 1 1 d . . . H17A H 0.9951 1.0018 0.5851 0.092 Uiso 1 1 calc R . . H17B H 1.1183 0.9640 0.5302 0.092 Uiso 1 1 calc R . . H17C H 1.1723 1.0269 0.5950 0.092 Uiso 1 1 calc R . . C18 C 1.5196(5) 0.8122(2) 0.52016(19) 0.0453(8) Uani 1 1 d . . . H18 H 1.6130 0.7796 0.5140 0.054 Uiso 1 1 calc R . . C19 C 1.5581(4) 0.8933(2) 0.49449(17) 0.0384(7) Uani 1 1 d . . . C20 C 1.7013(4) 0.9090(2) 0.4691(2) 0.0519(9) Uani 1 1 d . . . H20 H 1.7770 0.8697 0.4674 0.062 Uiso 1 1 calc R . . C21 C 1.7332(5) 0.9835(3) 0.4459(2) 0.0601(11) Uani 1 1 d . . . H21 H 1.8323 0.9965 0.4290 0.072 Uiso 1 1 calc R . . C22 C 1.6222(5) 1.0374(2) 0.4477(2) 0.0526(10) Uani 1 1 d . . . H22 H 1.6416 1.0886 0.4312 0.063 Uiso 1 1 calc R . . C23 C 1.4793(4) 1.0176(2) 0.4737(2) 0.0459(8) Uani 1 1 d . . . H23 H 1.4021 1.0562 0.4751 0.055 Uiso 1 1 calc R . . C24 C 1.3917(5) 0.7790(3) 0.4681(2) 0.0623(12) Uani 1 1 d . . . H24A H 1.3642 0.7281 0.4878 0.093 Uiso 1 1 calc R . . H24B H 1.4252 0.7742 0.4142 0.093 Uiso 1 1 calc R . . H24C H 1.3017 0.8130 0.4683 0.093 Uiso 1 1 calc R . . C25 C 0.6887(5) 0.8200(2) 0.11067(18) 0.0438(8) Uani 1 1 d . . . H25 H 0.7697 0.7852 0.1006 0.053 Uiso 1 1 calc R . . C26 C 0.5958(4) 0.94857(19) 0.13782(18) 0.0348(7) Uani 1 1 d . . . C27 C 0.5599(4) 0.9357(2) 0.22466(19) 0.0452(8) Uani 1 1 d . . . H27A H 0.6556 0.9250 0.2572 0.054 Uiso 1 1 calc R . . H27B H 0.5095 0.9817 0.2460 0.054 Uiso 1 1 calc R . . C28 C 0.4520(5) 0.8666(3) 0.2244(2) 0.0622(11) Uani 1 1 d . . . H28A H 0.3533 0.8805 0.2470 0.075 Uiso 1 1 calc R . . H28B H 0.4996 0.8235 0.2552 0.075 Uiso 1 1 calc R . . C29 C 0.4265(5) 0.8448(3) 0.1377(2) 0.0564(10) Uani 1 1 d . . . H29 H 0.3219 0.8221 0.1263 0.068 Uiso 1 1 calc R . . C30 C 0.4473(4) 0.9188(3) 0.0918(2) 0.0507(9) Uani 1 1 d . . . C31 C 0.6349(5) 1.0306(2) 0.1183(3) 0.0542(9) Uani 1 1 d . . . H31A H 0.7276 1.0464 0.1498 0.081 Uiso 1 1 calc R . . H31B H 0.5488 1.0642 0.1302 0.081 Uiso 1 1 calc R . . H31C H 0.6539 1.0345 0.0621 0.081 Uiso 1 1 calc R . . C32 C 0.4613(5) 0.9090(3) 0.0036(2) 0.0599(11) Uani 1 1 d . . . H32A H 0.5451 0.8729 -0.0057 0.090 Uiso 1 1 calc R . . H32B H 0.4836 0.9589 -0.0201 0.090 Uiso 1 1 calc R . . H32C H 0.3643 0.8887 -0.0204 0.090 Uiso 1 1 calc R . . C33 C 0.3094(5) 0.9721(4) 0.1037(3) 0.0819(16) Uani 1 1 d . . . H33A H 0.2137 0.9457 0.0865 0.123 Uiso 1 1 calc R . . H33B H 0.3199 1.0192 0.0727 0.123 Uiso 1 1 calc R . . H33C H 0.3065 0.9854 0.1597 0.123 Uiso 1 1 calc R . . C34 C 0.8839(4) 0.9202(2) 0.11689(19) 0.0428(8) Uani 1 1 d . . . H34A H 0.8871 0.9667 0.0833 0.051 Uiso 1 1 calc R . . H34B H 0.9444 0.8795 0.0920 0.051 Uiso 1 1 calc R . . C35 C 0.9601(4) 0.9386(3) 0.1965(2) 0.0466(9) Uani 1 1 d . . . C36 C 0.9901(4) 0.8792(3) 0.2496(2) 0.0522(10) Uani 1 1 d . . . C37 C 1.0657(4) 0.8945(3) 0.3236(2) 0.0640(12) Uani 1 1 d . . . H37 H 1.0856 0.8541 0.3606 0.077 Uiso 1 1 calc R . . C38 C 1.1097(5) 0.9683(4) 0.3413(2) 0.0684(14) Uani 1 1 d . . . H38 H 1.1626 0.9784 0.3907 0.082 Uiso 1 1 calc R . . C39 C 1.0796(5) 1.0296(4) 0.2894(3) 0.0748(15) Uani 1 1 d . . . H39 H 1.1100 1.0806 0.3034 0.090 Uiso 1 1 calc R . . C40 C 1.0030(4) 1.0140(3) 0.2155(2) 0.0498(9) Uani 1 1 d . . . H40 H 0.9808 1.0546 0.1791 0.060 Uiso 1 1 calc R . . C41 C 0.9743(7) 0.7434(3) 0.2756(3) 0.0835(16) Uani 1 1 d . . . H41A H 1.0844 0.7405 0.2914 0.125 Uiso 1 1 calc R . . H41B H 0.9428 0.6963 0.2472 0.125 Uiso 1 1 calc R . . H41C H 0.9149 0.7487 0.3226 0.125 Uiso 1 1 calc R . . C42 C 0.4979(5) 0.7114(2) 0.1066(2) 0.0594(10) Uani 1 1 d . . . H42 H 0.3924 0.7118 0.0798 0.071 Uiso 1 1 calc R . . C43 C 0.4854(5) 0.6740(2) 0.1875(2) 0.0554(10) Uani 1 1 d . . . C44 C 0.3521(6) 0.6386(3) 0.1997(3) 0.0778(15) Uani 1 1 d . . . H44 H 0.2731 0.6358 0.1588 0.093 Uiso 1 1 calc R . . C45 C 0.3316(6) 0.6070(3) 0.2710(3) 0.0798(15) Uani 1 1 d . . . H45 H 0.2373 0.5819 0.2806 0.096 Uiso 1 1 calc R . . C46 C 0.4428(6) 0.6109(3) 0.3272(2) 0.0635(11) Uani 1 1 d . . . H46 H 0.4275 0.5904 0.3780 0.076 Uiso 1 1 calc R . . C47 C 0.5814(6) 0.6451(3) 0.3118(3) 0.0702(13) Uani 1 1 d . . . H47 H 0.6623 0.6459 0.3519 0.084 Uiso 1 1 calc R . . C48 C 0.5976(7) 0.6654(3) 0.0574(3) 0.0829(17) Uani 1 1 d . . . H48A H 0.6122 0.6927 0.0079 0.124 Uiso 1 1 calc R . . H48B H 0.5492 0.6153 0.0459 0.124 Uiso 1 1 calc R . . H48C H 0.6978 0.6575 0.0857 0.124 Uiso 1 1 calc R . . N1 N 1.3287(3) 0.79937(14) 0.71009(13) 0.0265(5) Uani 1 1 d . . . N2 N 1.4864(3) 0.81159(15) 0.60503(14) 0.0353(6) Uani 1 1 d . . . N3 N 1.4457(3) 0.94635(17) 0.49677(16) 0.0399(6) Uani 1 1 d . . . N4 N 0.7217(3) 0.89402(15) 0.11863(14) 0.0317(5) Uani 1 1 d . . . N5 N 0.5481(4) 0.79204(18) 0.11610(17) 0.0543(9) Uani 1 1 d . . . N6 N 0.6047(4) 0.6776(2) 0.2407(2) 0.0619(9) Uani 1 1 d . . . O1 O 1.1301(3) 0.92387(15) 0.64002(14) 0.0515(7) Uani 1 1 d . . . O2 O 0.9466(4) 0.80853(17) 0.22532(15) 0.0607(8) Uani 1 1 d . . . F1 F 1.1286(2) 0.67691(12) 0.57495(12) 0.0499(5) Uani 1 1 d . . . F2 F 0.8885(3) 0.71580(16) 0.59342(14) 0.0711(8) Uani 1 1 d . . . F3 F 0.8246(3) 0.7008(2) 0.46378(15) 0.0811(9) Uani 1 1 d . . . F4 F 1.0646(3) 0.66015(14) 0.44504(13) 0.0608(6) Uani 1 1 d . . . F5 F 1.0250(3) 0.77468(14) 0.50350(16) 0.0691(7) Uani 1 1 d . . . F6 F 0.9290(3) 0.60098(15) 0.53655(14) 0.0685(7) Uani 1 1 d . . . F7 F 1.0021(2) 0.69558(14) 0.08063(10) 0.0515(5) Uani 1 1 d . . . F8 F 0.9067(2) 0.75330(13) -0.03029(12) 0.0516(5) Uani 1 1 d . . . F9 F 1.0753(2) 0.68805(16) -0.10128(10) 0.0556(5) Uani 1 1 d . . . F10 F 1.1706(3) 0.62944(14) 0.01105(14) 0.0612(6) Uani 1 1 d . . . F11 F 1.1606(3) 0.75903(14) 0.00256(13) 0.0571(6) Uani 1 1 d . . . F12 F 0.9170(3) 0.62319(14) -0.02427(14) 0.0604(6) Uani 1 1 d . . . P1 P 0.97676(9) 0.68778(6) 0.51912(5) 0.03894(18) Uani 1 1 d . . . P2 P 1.03765(9) 0.69083(6) -0.01049(4) 0.03407(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0438(16) 0.0212(14) 0.0306(13) 0.0009(11) -0.0029(12) -0.0001(12) C2 0.0281(13) 0.0330(16) 0.0290(13) -0.0001(11) -0.0018(10) -0.0013(12) C3 0.0411(17) 0.0332(17) 0.0456(17) -0.0145(14) 0.0019(14) -0.0053(14) C4 0.0454(19) 0.0337(18) 0.057(2) -0.0034(15) 0.0055(16) -0.0157(15) C5 0.0379(16) 0.0361(18) 0.0466(17) 0.0009(14) 0.0112(13) -0.0054(14) C6 0.0294(14) 0.0322(16) 0.0386(15) -0.0003(12) 0.0026(12) 0.0017(13) C7 0.0455(18) 0.051(2) 0.0299(14) 0.0070(14) -0.0012(13) 0.0055(16) C8 0.0319(17) 0.064(3) 0.061(2) -0.0029(19) -0.0015(15) 0.0047(17) C9 0.0485(18) 0.0293(18) 0.0503(18) 0.0037(14) 0.0061(14) 0.0066(15) C10 0.0275(14) 0.0290(15) 0.0408(15) 0.0038(12) 0.0002(11) -0.0028(12) C11 0.0273(14) 0.0346(17) 0.0385(15) 0.0020(13) 0.0005(12) 0.0006(12) C12 0.0322(16) 0.0327(16) 0.0419(17) 0.0026(13) 0.0042(12) 0.0044(13) C13 0.050(2) 0.037(2) 0.061(2) 0.0053(16) 0.0065(17) 0.0113(17) C14 0.060(2) 0.044(2) 0.069(3) -0.0090(19) 0.002(2) 0.0150(19) C15 0.060(3) 0.068(3) 0.049(2) -0.0129(19) 0.0060(18) 0.021(2) C16 0.0400(18) 0.051(2) 0.0427(17) 0.0031(15) 0.0068(14) 0.0094(16) C17 0.073(3) 0.059(3) 0.052(2) 0.0260(19) 0.0046(19) 0.021(2) C18 0.062(2) 0.042(2) 0.0335(16) 0.0017(14) 0.0115(15) -0.0024(17) C19 0.0504(19) 0.0367(18) 0.0284(14) 0.0040(12) 0.0050(13) -0.0009(15) C20 0.046(2) 0.062(3) 0.049(2) 0.0099(17) 0.0089(16) 0.0134(18) C21 0.043(2) 0.080(3) 0.058(2) 0.022(2) 0.0080(17) -0.010(2) C22 0.056(2) 0.048(2) 0.052(2) 0.0186(17) -0.0096(17) -0.0210(19) C23 0.0457(19) 0.039(2) 0.053(2) 0.0042(15) -0.0008(15) 0.0001(16) C24 0.088(3) 0.063(3) 0.0369(18) -0.0058(17) 0.0119(18) -0.029(2) C25 0.071(2) 0.0318(18) 0.0292(15) 0.0002(12) 0.0116(15) 0.0066(16) C26 0.0298(15) 0.0367(17) 0.0377(16) -0.0018(13) -0.0001(12) -0.0007(13) C27 0.0446(19) 0.055(2) 0.0373(17) -0.0104(15) 0.0078(14) 0.0051(17) C28 0.066(3) 0.077(3) 0.046(2) 0.0019(19) 0.0276(19) -0.011(2) C29 0.053(2) 0.061(3) 0.056(2) -0.0110(19) 0.0162(18) -0.025(2) C30 0.0375(18) 0.066(3) 0.048(2) -0.0029(18) 0.0008(15) -0.0158(18) C31 0.056(2) 0.035(2) 0.071(3) -0.0009(17) -0.0038(19) 0.0043(17) C32 0.059(3) 0.074(3) 0.045(2) 0.0016(19) -0.0091(18) -0.017(2) C33 0.039(2) 0.122(5) 0.085(3) 0.000(3) -0.004(2) 0.013(3) C34 0.0309(16) 0.063(2) 0.0349(16) 0.0052(15) 0.0064(12) 0.0003(16) C35 0.0283(16) 0.074(3) 0.0385(17) 0.0026(16) 0.0075(13) -0.0043(16) C36 0.0369(19) 0.078(3) 0.0423(18) 0.0014(18) 0.0065(15) 0.0103(19) C37 0.039(2) 0.102(4) 0.051(2) -0.002(2) 0.0048(17) 0.011(2) C38 0.043(2) 0.118(5) 0.044(2) 0.007(2) 0.0002(17) -0.005(3) C39 0.054(3) 0.110(4) 0.060(3) -0.008(3) 0.003(2) -0.040(3) C40 0.0388(18) 0.066(3) 0.0444(19) 0.0009(17) 0.0042(15) -0.0206(18) C41 0.091(4) 0.080(4) 0.078(3) 0.023(3) -0.004(3) 0.035(3) C42 0.077(3) 0.044(2) 0.057(2) -0.0045(17) -0.0008(19) -0.014(2) C43 0.081(3) 0.045(2) 0.0407(17) -0.0003(15) 0.0001(17) -0.026(2) C44 0.096(4) 0.056(3) 0.078(3) 0.026(2) -0.033(3) -0.034(3) C45 0.066(3) 0.062(3) 0.110(4) 0.030(3) -0.001(3) -0.020(2) C46 0.097(3) 0.046(2) 0.048(2) 0.0179(18) 0.010(2) 0.000(2) C47 0.083(3) 0.054(3) 0.069(3) -0.004(2) -0.035(2) 0.013(2) C48 0.136(5) 0.040(2) 0.079(3) -0.009(2) 0.056(3) -0.008(3) N1 0.0283(11) 0.0244(12) 0.0267(11) 0.0005(9) 0.0006(9) -0.0008(10) N2 0.0473(15) 0.0306(14) 0.0286(12) 0.0009(10) 0.0083(10) -0.0036(12) N3 0.0395(15) 0.0379(16) 0.0424(15) 0.0009(12) 0.0035(12) -0.0044(12) N4 0.0318(12) 0.0333(14) 0.0305(11) 0.0007(10) 0.0050(10) 0.0006(11) N5 0.087(2) 0.0373(17) 0.0399(15) -0.0040(12) 0.0124(15) -0.0267(17) N6 0.063(2) 0.064(2) 0.0586(19) -0.0073(17) 0.0072(16) -0.0093(19) O1 0.0701(18) 0.0444(15) 0.0402(13) 0.0134(10) 0.0050(11) 0.0227(13) O2 0.086(2) 0.0492(17) 0.0462(14) 0.0050(12) 0.0007(13) 0.0260(16) F1 0.0431(10) 0.0454(13) 0.0600(12) -0.0071(10) -0.0084(9) 0.0056(9) F2 0.0550(13) 0.093(2) 0.0665(14) -0.0344(13) 0.0133(11) 0.0112(13) F3 0.0498(12) 0.116(2) 0.0746(15) -0.0234(17) -0.0253(11) 0.0119(15) F4 0.0750(15) 0.0620(15) 0.0473(12) -0.0059(10) 0.0197(11) 0.0071(12) F5 0.0757(17) 0.0390(13) 0.0910(18) 0.0061(12) -0.0105(13) 0.0054(12) F6 0.0857(17) 0.0568(15) 0.0641(14) -0.0145(12) 0.0147(12) -0.0347(14) F7 0.0718(13) 0.0528(13) 0.0307(8) 0.0043(9) 0.0101(8) 0.0094(12) F8 0.0475(12) 0.0604(15) 0.0468(11) 0.0078(10) 0.0011(9) 0.0137(11) F9 0.0642(12) 0.0727(15) 0.0311(9) -0.0056(11) 0.0132(8) -0.0069(14) F10 0.0615(14) 0.0584(16) 0.0637(14) -0.0004(11) 0.0024(11) 0.0217(12) F11 0.0539(13) 0.0603(15) 0.0560(13) 0.0003(11) -0.0055(10) -0.0207(11) F12 0.0602(14) 0.0531(15) 0.0685(15) -0.0061(11) 0.0081(11) -0.0239(12) P1 0.0328(4) 0.0400(4) 0.0437(4) -0.0123(4) 0.0001(3) 0.0004(4) P2 0.0359(4) 0.0369(4) 0.0296(3) -0.0007(3) 0.0034(3) -0.0026(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.312(4) . ? C1 N1 1.327(4) . ? C1 H1 0.9500 . ? C2 N1 1.506(3) . ? C2 C7 1.522(4) . ? C2 C3 1.540(4) . ? C2 C6 1.560(4) . ? C3 C4 1.559(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.537(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.467(4) . ? C5 C6 1.538(4) . ? C5 H5 1.0000 . ? C6 C9 1.525(5) . ? C6 C8 1.541(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.481(4) . ? C10 C11 1.508(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.386(4) . ? C11 C12 1.401(4) . ? C12 O1 1.366(4) . ? C12 C13 1.391(5) . ? C13 C14 1.391(6) . ? C13 H13 0.9500 . ? C14 C15 1.366(6) . ? C14 H14 0.9500 . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O1 1.434(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N2 1.486(4) . ? C18 C24 1.495(5) . ? C18 C19 1.518(5) . ? C18 H18 1.0000 . ? C19 N3 1.345(5) . ? C19 C20 1.367(5) . ? C20 C21 1.385(6) . ? C20 H20 0.9500 . ? C21 C22 1.345(6) . ? C21 H21 0.9500 . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 N3 1.335(5) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N4 1.323(4) . ? C25 N5 1.323(5) . ? C25 H25 0.9500 . ? C26 N4 1.497(4) . ? C26 C31 1.505(5) . ? C26 C27 1.541(5) . ? C26 C30 1.558(5) . ? C27 C28 1.521(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.523(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N5 1.461(5) . ? C29 C30 1.520(6) . ? C29 H29 1.0000 . ? C30 C32 1.520(5) . ? C30 C33 1.537(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 N4 1.483(4) . ? C34 C35 1.506(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.386(6) . ? C35 C40 1.393(6) . ? C36 O2 1.341(5) . ? C36 C37 1.409(5) . ? C37 C38 1.366(7) . ? C37 H37 0.9500 . ? C38 C39 1.397(7) . ? C38 H38 0.9500 . ? C39 C40 1.412(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 O2 1.429(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C48 1.473(6) . ? C42 N5 1.473(5) . ? C42 C43 1.529(5) . ? C42 H42 1.0000 . ? C43 C44 1.338(6) . ? C43 N6 1.337(5) . ? C44 C45 1.351(7) . ? C44 H44 0.9500 . ? C45 C46 1.321(7) . ? C45 H45 0.9500 . ? C46 C47 1.381(7) . ? C46 H46 0.9500 . ? C47 N6 1.360(6) . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? F1 P1 1.592(2) . ? F2 P1 1.590(2) . ? F3 P1 1.594(2) . ? F4 P1 1.583(2) . ? F5 P1 1.592(3) . ? F6 P1 1.595(3) . ? F7 P2 1.5977(18) . ? F8 P2 1.594(2) . ? F9 P2 1.5953(18) . ? F10 P2 1.599(2) . ? F11 P2 1.602(2) . ? F12 P2 1.583(2) . ? 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 N2 C1 N1 123.2(3) . . ? N2 C1 H1 118.4 . . ? N1 C1 H1 118.4 . . ? N1 C2 C7 109.9(2) . . ? N1 C2 C3 107.5(2) . . ? C7 C2 C3 115.5(3) . . ? N1 C2 C6 106.5(2) . . ? C7 C2 C6 113.4(3) . . ? C3 C2 C6 103.4(2) . . ? C2 C3 C4 104.4(2) . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3B 110.9 . . ? C4 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C5 C4 C3 104.9(3) . . ? C5 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? N2 C5 C4 109.6(3) . . ? N2 C5 C6 107.5(2) . . ? C4 C5 C6 104.9(3) . . ? N2 C5 H5 111.5 . . ? C4 C5 H5 111.5 . . ? C6 C5 H5 111.5 . . ? C9 C6 C5 114.5(3) . . ? C9 C6 C8 108.7(3) . . ? C5 C6 C8 108.8(3) . . ? C9 C6 C2 114.5(3) . . ? C5 C6 C2 98.2(2) . . ? C8 C6 C2 111.8(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 112.7(2) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C16 C11 C12 117.9(3) . . ? C16 C11 C10 122.7(3) . . ? C12 C11 C10 119.4(3) . . ? O1 C12 C13 124.3(3) . . ? O1 C12 C11 114.5(3) . . ? C13 C12 C11 121.2(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.4(4) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 121.0(4) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C24 113.1(3) . . ? N2 C18 C19 110.1(3) . . ? C24 C18 C19 110.9(3) . . ? N2 C18 H18 107.5 . . ? C24 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? N3 C19 C20 123.2(3) . . ? N3 C19 C18 117.0(3) . . ? C20 C19 C18 119.7(3) . . ? C19 C20 C21 118.5(4) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 119.2(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.5(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N3 C23 C22 122.6(4) . . ? N3 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 N5 123.0(3) . . ? N4 C25 H25 118.5 . . ? N5 C25 H25 118.5 . . ? N4 C26 C31 111.9(3) . . ? N4 C26 C27 107.9(3) . . ? C31 C26 C27 114.2(3) . . ? N4 C26 C30 106.0(3) . . ? C31 C26 C30 113.2(3) . . ? C27 C26 C30 102.9(3) . . ? C28 C27 C26 105.7(3) . . ? C28 C27 H27A 110.6 . . ? C26 C27 H27A 110.6 . . ? C28 C27 H27B 110.6 . . ? C26 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? C27 C28 C29 104.8(3) . . ? C27 C28 H28A 110.8 . . ? C29 C28 H28A 110.8 . . ? C27 C28 H28B 110.8 . . ? C29 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? N5 C29 C30 107.0(3) . . ? N5 C29 C28 109.4(4) . . ? C30 C29 C28 105.6(3) . . ? N5 C29 H29 111.5 . . ? C30 C29 H29 111.5 . . ? C28 C29 H29 111.5 . . ? C29 C30 C32 115.4(4) . . ? C29 C30 C33 109.0(4) . . ? C32 C30 C33 107.8(4) . . ? C29 C30 C26 98.2(3) . . ? C32 C30 C26 114.9(3) . . ? C33 C30 C26 111.4(3) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C35 114.6(3) . . ? N4 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? N4 C34 H34B 108.6 . . ? C35 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C40 120.7(3) . . ? C36 C35 C34 118.9(4) . . ? C40 C35 C34 120.4(4) . . ? O2 C36 C35 116.2(3) . . ? O2 C36 C37 123.8(4) . . ? C35 C36 C37 120.0(5) . . ? C38 C37 C36 118.9(5) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.6 . . ? C37 C38 C39 122.4(4) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C38 C39 C40 118.4(5) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? C35 C40 C39 119.5(4) . . ? C35 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C48 C42 N5 113.4(4) . . ? C48 C42 C43 110.7(4) . . ? N5 C42 C43 109.9(3) . . ? C48 C42 H42 107.5 . . ? N5 C42 H42 107.5 . . ? C43 C42 H42 107.5 . . ? C44 C43 N6 124.2(4) . . ? C44 C43 C42 116.2(4) . . ? N6 C43 C42 119.6(4) . . ? C43 C44 C45 119.1(4) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 119.8(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 119.8(4) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? N6 C47 C46 121.4(4) . . ? N6 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C1 N1 C10 118.5(2) . . ? C1 N1 C2 119.5(2) . . ? C10 N1 C2 121.7(2) . . ? C1 N2 C5 117.9(2) . . ? C1 N2 C18 126.0(3) . . ? C5 N2 C18 116.1(3) . . ? C23 N3 C19 117.0(3) . . ? C25 N4 C34 119.7(3) . . ? C25 N4 C26 118.7(3) . . ? C34 N4 C26 121.2(3) . . ? C25 N5 C29 118.2(3) . . ? C25 N5 C42 127.6(4) . . ? C29 N5 C42 114.2(3) . . ? C43 N6 C47 115.6(4) . . ? C12 O1 C17 117.6(3) . . ? C36 O2 C41 120.3(4) . . ? F4 P1 F2 179.82(17) . . ? F4 P1 F1 90.92(13) . . ? F2 P1 F1 89.14(12) . . ? F4 P1 F5 90.63(15) . . ? F2 P1 F5 89.19(16) . . ? F1 P1 F5 89.67(13) . . ? F4 P1 F3 89.79(14) . . ? F2 P1 F3 90.15(14) . . ? F1 P1 F3 178.60(17) . . ? F5 P1 F3 89.12(17) . . ? F4 P1 F6 90.21(14) . . ? F2 P1 F6 89.96(15) . . ? F1 P1 F6 89.60(14) . . ? F5 P1 F6 178.89(15) . . ? F3 P1 F6 91.60(17) . . ? F12 P2 F8 90.85(12) . . ? F12 P2 F9 90.32(13) . . ? F8 P2 F9 90.01(12) . . ? F12 P2 F7 91.05(13) . . ? F8 P2 F7 89.65(11) . . ? F9 P2 F7 178.59(15) . . ? F12 P2 F10 90.20(15) . . ? F8 P2 F10 178.62(14) . . ? F9 P2 F10 90.88(13) . . ? F7 P2 F10 89.43(12) . . ? F12 P2 F11 179.36(14) . . ? F8 P2 F11 89.35(14) . . ? F9 P2 F11 89.08(12) . . ? F7 P2 F11 89.55(12) . . ? F10 P2 F11 89.62(13) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.137 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.050 _database_code_depnum_ccdc_archive 'CCDC 965595'