# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Highly active iridium(I) complexes for catalytic hydrogen isotope exchange ; _publ_contact_author_name 'W. J. Kerr' _publ_contact_author_email W.KERR@STRATH.AC.UK loop_ _publ_author_name W.J.Kerr S.Andersson J.A.Brown S.Irvine A.R.Kennedy ; G.N.Nilsson ; #===END data_5C _database_code_depnum_ccdc_archive 'CCDC 634672' #------------------------------------------------------ #---------------------COMPOUND 5C---------------------- #----------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.35 H48.30 Cl0.70 F6 Ir N2 O0.30 P2' _chemical_formula_weight 923.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ir Ir -1.4442 7.9887 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4652(2) _cell_length_b 13.3037(2) _cell_length_c 14.1374(3) _cell_angle_alpha 86.555(1) _cell_angle_beta 67.108(1) _cell_angle_gamma 71.527(1) _cell_volume 1879.25(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27569 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 923.4 _exptl_absorpt_coefficient_mu 3.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.57 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43703 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8614 _reflns_number_gt 7433 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+1.9869P] 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 SHELXL _refine_ls_extinction_coef 0.00042(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8614 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.917804(12) 0.816650(9) 0.731130(9) 0.01486(5) Uani 1 1 d . . . P1 P 1.00546(8) 0.66787(6) 0.61679(6) 0.01630(17) Uani 1 1 d . . . P2 P 1.50142(9) 0.68050(7) 0.30696(7) 0.0291(2) Uani 1 1 d . . . F1 F 1.4386(3) 0.75620(19) 0.40841(17) 0.0698(8) Uani 1 1 d . . . F2 F 1.4994(3) 0.58084(19) 0.37292(18) 0.0707(8) Uani 1 1 d . . . F3 F 1.3553(2) 0.6949(2) 0.3142(2) 0.0753(8) Uani 1 1 d . . . F4 F 1.5637(2) 0.60424(16) 0.20400(15) 0.0400(5) Uani 1 1 d . . . F5 F 1.5036(2) 0.78079(17) 0.23934(16) 0.0497(6) Uani 1 1 d . . . F6 F 1.6493(2) 0.6675(2) 0.2947(2) 0.0619(7) Uani 1 1 d . . . N1 N 0.7128(2) 0.7309(2) 0.89735(18) 0.0193(6) Uani 1 1 d . . . N2 N 0.8590(2) 0.7363(2) 0.95502(18) 0.0175(5) Uani 1 1 d . . . C1 C 0.8324(3) 0.7501(2) 0.8671(2) 0.0160(6) Uani 1 1 d . . . C2 C 0.6668(3) 0.7080(3) 1.0001(2) 0.0272(8) Uani 1 1 d . . . H2 H 0.5859 0.6932 1.0378 0.033 Uiso 1 1 calc R . . C3 C 0.7577(3) 0.7107(3) 1.0354(2) 0.0262(8) Uani 1 1 d . . . H3 H 0.7541 0.6975 1.1031 0.031 Uiso 1 1 calc R . . C4 C 0.6421(3) 0.7217(2) 0.8342(2) 0.0183(7) Uani 1 1 d . . . C5 C 0.5620(3) 0.8124(3) 0.8088(2) 0.0215(7) Uani 1 1 d . . . C6 C 0.4921(3) 0.7994(3) 0.7516(2) 0.0256(7) Uani 1 1 d . . . H6 H 0.4387 0.8607 0.7322 0.031 Uiso 1 1 calc R . . C7 C 0.4981(3) 0.7001(3) 0.7220(2) 0.0270(8) Uani 1 1 d . . . C8 C 0.5724(3) 0.6119(3) 0.7540(2) 0.0256(7) Uani 1 1 d . . . H8 H 0.5748 0.5434 0.7359 0.031 Uiso 1 1 calc R . . C9 C 0.6437(3) 0.6200(3) 0.8118(2) 0.0226(7) Uani 1 1 d . . . C10 C 0.5418(3) 0.9219(3) 0.8495(3) 0.0296(8) Uani 1 1 d . . . H10A H 0.4932 0.9294 0.9244 0.044 Uiso 1 1 calc R . . H10B H 0.4902 0.9758 0.8180 0.044 Uiso 1 1 calc R . . H10C H 0.6289 0.9314 0.8323 0.044 Uiso 1 1 calc R . . C11 C 0.4214(4) 0.6882(3) 0.6599(3) 0.0400(9) Uani 1 1 d . . . H11A H 0.4667 0.6198 0.6192 0.060 Uiso 1 1 calc R . . H11B H 0.4170 0.7460 0.6136 0.060 Uiso 1 1 calc R . . H11C H 0.3307 0.6912 0.7064 0.060 Uiso 1 1 calc R . . C12 C 0.7101(3) 0.5215(3) 0.8546(3) 0.0313(8) Uani 1 1 d . . . H12A H 0.6469 0.5123 0.9224 0.047 Uiso 1 1 calc R . . H12B H 0.7888 0.5293 0.8612 0.047 Uiso 1 1 calc R . . H12C H 0.7375 0.4593 0.8079 0.047 Uiso 1 1 calc R . . C13 C 0.9761(3) 0.7383(2) 0.9693(2) 0.0165(6) Uani 1 1 d . . . C14 C 0.9645(3) 0.8197(2) 1.0333(2) 0.0207(7) Uani 1 1 d . . . C15 C 1.0776(3) 0.8169(3) 1.0493(2) 0.0213(7) Uani 1 1 d . . . H15 H 1.0723 0.8720 1.0921 0.026 Uiso 1 1 calc R . . C16 C 1.1981(3) 0.7361(2) 1.0046(2) 0.0205(7) Uani 1 1 d . . . C17 C 1.2044(3) 0.6555(3) 0.9428(2) 0.0213(7) Uani 1 1 d . . . H17 H 1.2863 0.5996 0.9122 0.026 Uiso 1 1 calc R . . C18 C 1.0943(3) 0.6545(2) 0.9246(2) 0.0176(6) Uani 1 1 d . . . C19 C 0.8347(3) 0.9089(3) 1.0843(2) 0.0305(8) Uani 1 1 d . . . H19A H 0.7793 0.9174 1.0444 0.046 Uiso 1 1 calc R . . H19B H 0.8539 0.9752 1.0871 0.046 Uiso 1 1 calc R . . H19C H 0.7871 0.8920 1.1543 0.046 Uiso 1 1 calc R . . C20 C 1.3188(3) 0.7355(3) 1.0244(3) 0.0303(8) Uani 1 1 d . . . H20A H 1.3984 0.6815 0.9773 0.045 Uiso 1 1 calc R . . H20B H 1.3053 0.7189 1.0956 0.045 Uiso 1 1 calc R . . H20C H 1.3311 0.8055 1.0131 0.045 Uiso 1 1 calc R . . C21 C 1.1035(3) 0.5640(3) 0.8603(2) 0.0258(7) Uani 1 1 d . . . H21A H 1.0336 0.5327 0.8997 0.039 Uiso 1 1 calc R . . H21B H 1.1913 0.5098 0.8421 0.039 Uiso 1 1 calc R . . H21C H 1.0915 0.5904 0.7974 0.039 Uiso 1 1 calc R . . C22 C 0.8408(3) 0.9724(2) 0.8199(2) 0.0199(7) Uani 1 1 d . . . H22 H 0.7808 0.9675 0.8800 0.024 Uiso 1 1 d R . . C23 C 0.9743(3) 0.9233(2) 0.8024(2) 0.0197(7) Uani 1 1 d . . . H23 H 0.9962 0.8852 0.8566 0.024 Uiso 1 1 d R . . C24 C 1.0904(3) 0.9529(3) 0.7246(2) 0.0240(7) Uani 1 1 d . . . H24A H 1.1746 0.8971 0.7186 0.029 Uiso 1 1 calc R . . H24B H 1.0915 1.0202 0.7501 0.029 Uiso 1 1 calc R . . C25 C 1.0858(3) 0.9666(3) 0.6175(2) 0.0265(8) Uani 1 1 d . . . H25A H 1.0356 1.0413 0.6133 0.032 Uiso 1 1 calc R . . H25B H 1.1779 0.9509 0.5649 0.032 Uiso 1 1 calc R . . C26 C 1.0201(3) 0.8941(2) 0.5944(2) 0.0205(7) Uani 1 1 d . . . H26 H 1.0777 0.8398 0.5390 0.025 Uiso 1 1 d R . . C27 C 0.8834(3) 0.9240(2) 0.6163(2) 0.0212(7) Uani 1 1 d . . . H27 H 0.8551 0.8904 0.5761 0.025 Uiso 1 1 d R . . C28 C 0.7843(3) 1.0301(2) 0.6640(2) 0.0260(7) Uani 1 1 d . . . H28A H 0.6933 1.0273 0.6802 0.031 Uiso 1 1 calc R . . H28B H 0.7999 1.0839 0.6132 0.031 Uiso 1 1 calc R . . C29 C 0.7907(3) 1.0657(2) 0.7626(2) 0.0256(7) Uani 1 1 d . . . H29A H 0.8508 1.1096 0.7445 0.031 Uiso 1 1 calc R . . H29B H 0.7006 1.1106 0.8085 0.031 Uiso 1 1 calc R . . C30 C 1.1876(3) 0.6221(3) 0.5641(2) 0.0266(8) Uani 1 1 d . . . H30A H 1.2188 0.5952 0.6190 0.040 Uiso 1 1 calc R . . H30B H 1.2203 0.6813 0.5348 0.040 Uiso 1 1 calc R . . H30C H 1.2215 0.5651 0.5101 0.040 Uiso 1 1 calc R . . C31 C 0.9715(3) 0.5437(2) 0.6531(2) 0.0220(7) Uani 1 1 d . . . H31A H 0.8771 0.5539 0.6689 0.033 Uiso 1 1 calc R . . H31B H 0.9912 0.5209 0.7140 0.033 Uiso 1 1 calc R . . H31C H 1.0277 0.4892 0.5961 0.033 Uiso 1 1 calc R . . C32 C 0.9588(3) 0.6927(2) 0.5057(2) 0.0178(6) Uani 1 1 d . . . C33 C 1.0471(3) 0.7028(2) 0.4078(2) 0.0208(7) Uani 1 1 d . . . H33 H 1.1369 0.6956 0.3960 0.025 Uiso 1 1 calc R . . C34 C 1.0039(4) 0.7235(2) 0.3268(2) 0.0257(8) Uani 1 1 d . . . H34 H 1.0642 0.7308 0.2600 0.031 Uiso 1 1 calc R . . C35 C 0.8740(4) 0.7333(3) 0.3436(3) 0.0300(8) Uani 1 1 d . . . H35 H 0.8451 0.7468 0.2882 0.036 Uiso 1 1 calc R . . C36 C 0.7853(3) 0.7235(3) 0.4410(3) 0.0270(8) Uani 1 1 d . . . H36 H 0.6959 0.7298 0.4522 0.032 Uiso 1 1 calc R . . C37 C 0.8269(3) 0.7046(2) 0.5217(2) 0.0223(7) Uani 1 1 d . . . H37 H 0.7652 0.6996 0.5887 0.027 Uiso 1 1 calc R . . C1S C 0.5457(13) 1.0100(10) 0.5234(10) 0.044(3) Uiso 0.35 1 d P . 1 Cl1 Cl 0.3779(5) 1.0300(8) 0.6107(9) 0.0555(16) Uani 0.35 1 d P . 1 Cl2 Cl 0.4218(6) 1.0267(9) 0.6056(9) 0.067(2) Uani 0.35 1 d P . 1 O98 O 0.4816(10) 1.0363(7) 0.5865(8) 0.022(2) Uiso 0.30 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01971(7) 0.01528(7) 0.01105(6) 0.00086(4) -0.00560(5) -0.00802(5) P1 0.0176(4) 0.0173(4) 0.0137(4) -0.0009(3) -0.0047(3) -0.0065(3) P2 0.0254(5) 0.0338(5) 0.0216(4) 0.0040(4) -0.0035(4) -0.0086(4) F1 0.099(2) 0.0537(16) 0.0246(12) -0.0082(11) -0.0001(13) -0.0109(15) F2 0.100(2) 0.0449(15) 0.0372(14) 0.0190(11) -0.0063(14) -0.0134(14) F3 0.0249(13) 0.101(2) 0.088(2) 0.0145(17) -0.0070(13) -0.0248(14) F4 0.0440(13) 0.0463(13) 0.0294(11) -0.0020(10) -0.0072(10) -0.0220(11) F5 0.0511(14) 0.0387(13) 0.0355(12) 0.0100(10) 0.0008(11) -0.0068(11) F6 0.0431(14) 0.0822(19) 0.0707(18) -0.0096(14) -0.0351(13) -0.0145(13) N1 0.0148(13) 0.0292(15) 0.0152(13) 0.0058(11) -0.0065(11) -0.0087(12) N2 0.0150(13) 0.0259(14) 0.0113(12) 0.0030(10) -0.0049(10) -0.0067(11) C1 0.0148(15) 0.0174(16) 0.0153(15) 0.0002(12) -0.0061(12) -0.0037(13) C2 0.0195(17) 0.046(2) 0.0176(16) 0.0101(15) -0.0064(14) -0.0152(16) C3 0.0208(17) 0.043(2) 0.0152(16) 0.0100(14) -0.0060(14) -0.0137(16) C4 0.0138(15) 0.0303(18) 0.0131(14) 0.0047(13) -0.0050(12) -0.0109(14) C5 0.0162(16) 0.0294(18) 0.0197(16) 0.0038(13) -0.0067(13) -0.0092(14) C6 0.0210(17) 0.0309(19) 0.0271(18) 0.0059(15) -0.0131(15) -0.0072(15) C7 0.0222(18) 0.040(2) 0.0233(17) 0.0007(15) -0.0103(14) -0.0141(16) C8 0.0223(18) 0.0296(19) 0.0252(17) -0.0026(14) -0.0051(15) -0.0130(15) C9 0.0158(16) 0.0268(18) 0.0213(16) 0.0059(14) -0.0024(13) -0.0087(14) C10 0.0267(19) 0.0290(19) 0.036(2) 0.0002(15) -0.0164(16) -0.0063(16) C11 0.038(2) 0.050(2) 0.044(2) 0.0011(19) -0.0257(19) -0.0167(19) C12 0.0290(19) 0.0280(19) 0.035(2) 0.0095(16) -0.0112(16) -0.0099(16) C13 0.0144(15) 0.0256(17) 0.0111(14) 0.0058(12) -0.0064(12) -0.0074(13) C14 0.0198(16) 0.0245(17) 0.0131(15) 0.0018(13) -0.0048(13) -0.0031(14) C15 0.0256(18) 0.0271(18) 0.0167(15) 0.0002(13) -0.0110(14) -0.0117(15) C16 0.0188(16) 0.0288(18) 0.0146(15) 0.0043(13) -0.0067(13) -0.0089(14) C17 0.0190(17) 0.0256(18) 0.0164(15) 0.0007(13) -0.0052(13) -0.0055(14) C18 0.0192(16) 0.0226(17) 0.0122(14) 0.0028(12) -0.0062(12) -0.0081(14) C19 0.0258(19) 0.038(2) 0.0207(17) -0.0068(15) -0.0111(15) 0.0028(16) C20 0.0231(18) 0.047(2) 0.0237(18) -0.0040(16) -0.0077(15) -0.0154(17) C21 0.0264(18) 0.0260(18) 0.0274(18) -0.0014(14) -0.0155(15) -0.0044(15) C22 0.0272(18) 0.0182(16) 0.0135(15) -0.0032(12) -0.0055(13) -0.0082(14) C23 0.0322(19) 0.0193(16) 0.0155(15) -0.0002(12) -0.0121(14) -0.0146(14) C24 0.0281(18) 0.0258(18) 0.0221(17) -0.0014(13) -0.0083(14) -0.0151(15) C25 0.035(2) 0.0299(19) 0.0189(16) 0.0032(14) -0.0082(15) -0.0196(16) C26 0.0328(19) 0.0176(16) 0.0125(15) 0.0026(12) -0.0054(14) -0.0146(14) C27 0.038(2) 0.0184(16) 0.0131(15) 0.0058(12) -0.0136(14) -0.0124(15) C28 0.038(2) 0.0195(17) 0.0230(17) 0.0044(13) -0.0152(15) -0.0086(15) C29 0.0326(19) 0.0174(17) 0.0278(18) 0.0000(13) -0.0139(15) -0.0064(15) C30 0.0220(18) 0.0319(19) 0.0242(18) -0.0018(15) -0.0089(15) -0.0056(15) C31 0.0292(18) 0.0169(16) 0.0231(17) -0.0008(13) -0.0113(14) -0.0097(14) C32 0.0208(16) 0.0160(16) 0.0162(15) -0.0031(12) -0.0051(13) -0.0070(13) C33 0.0268(18) 0.0182(16) 0.0178(15) -0.0003(12) -0.0061(14) -0.0108(14) C34 0.041(2) 0.0191(17) 0.0186(16) 0.0047(13) -0.0109(15) -0.0130(16) C35 0.045(2) 0.0255(19) 0.0287(19) 0.0054(15) -0.0255(17) -0.0101(17) C36 0.0250(18) 0.0259(19) 0.036(2) 0.0012(15) -0.0186(16) -0.0072(15) C37 0.0219(17) 0.0212(17) 0.0203(16) -0.0013(13) -0.0056(14) -0.0050(14) Cl1 0.004(3) 0.048(3) 0.080(3) 0.034(2) 0.002(3) 0.008(3) Cl2 0.015(4) 0.069(3) 0.074(3) 0.045(2) 0.000(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.079(3) . ? Ir1 C27 2.167(3) . ? Ir1 C23 2.170(3) . ? Ir1 C26 2.221(3) . ? Ir1 C22 2.222(3) . ? Ir1 P1 2.3239(8) . ? P1 C31 1.815(3) . ? P1 C30 1.823(3) . ? P1 C32 1.827(3) . ? P2 F2 1.576(2) . ? P2 F1 1.581(2) . ? P2 F3 1.587(3) . ? P2 F6 1.589(2) . ? P2 F5 1.595(2) . ? P2 F4 1.602(2) . ? N1 C1 1.371(4) . ? N1 C2 1.390(4) . ? N1 C4 1.452(4) . ? N2 C1 1.379(4) . ? N2 C3 1.391(4) . ? N2 C13 1.442(4) . ? C2 C3 1.328(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 C9 1.401(4) . ? C5 C6 1.391(4) . ? C5 C10 1.513(4) . ? C6 C7 1.383(5) . ? C6 H6 0.9500 . ? C7 C8 1.382(5) . ? C7 C11 1.507(5) . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C12 1.514(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.393(4) . ? C13 C14 1.394(4) . ? C14 C15 1.389(4) . ? C14 C19 1.514(4) . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.391(4) . ? C16 C20 1.513(4) . ? C17 C18 1.386(4) . ? C17 H17 0.9500 . ? C18 C21 1.505(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.386(4) . ? C22 C29 1.522(4) . ? C22 H22 0.8755 . ? C23 C24 1.510(4) . ? C23 H23 0.9639 . ? C24 C25 1.533(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.514(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.398(4) . ? C26 H26 0.9674 . ? C27 C28 1.496(4) . ? C27 H27 0.9453 . ? C28 C29 1.535(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.390(4) . ? C32 C37 1.397(4) . ? C33 C34 1.396(4) . ? C33 H33 0.9500 . ? C34 C35 1.377(5) . ? C34 H34 0.9500 . ? C35 C36 1.386(5) . ? C35 H35 0.9500 . ? C36 C37 1.380(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C1S Cl2 1.401(14) . ? C1S C1S 1.53(2) 2_676 ? C1S Cl1 1.778(14) . ? C1S Cl2 1.779(18) 2_676 ? C1S Cl1 1.783(17) 2_676 ? Cl1 C1S 1.783(17) 2_676 ? Cl2 C1S 1.779(18) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C27 146.56(12) . . ? C1 Ir1 C23 94.63(11) . . ? C27 Ir1 C23 94.46(11) . . ? C1 Ir1 C26 173.80(11) . . ? C27 Ir1 C26 37.12(12) . . ? C23 Ir1 C26 79.45(11) . . ? C1 Ir1 C22 88.99(11) . . ? C27 Ir1 C22 79.44(11) . . ? C23 Ir1 C22 36.77(11) . . ? C26 Ir1 C22 87.34(11) . . ? C1 Ir1 P1 99.32(8) . . ? C27 Ir1 P1 92.62(8) . . ? C23 Ir1 P1 142.68(9) . . ? C26 Ir1 P1 84.52(8) . . ? C22 Ir1 P1 171.53(8) . . ? C31 P1 C30 100.84(15) . . ? C31 P1 C32 100.53(14) . . ? C30 P1 C32 105.75(14) . . ? C31 P1 Ir1 123.23(11) . . ? C30 P1 Ir1 111.44(11) . . ? C32 P1 Ir1 113.08(10) . . ? F2 P2 F1 90.41(13) . . ? F2 P2 F3 90.55(16) . . ? F1 P2 F3 89.38(16) . . ? F2 P2 F6 91.42(16) . . ? F1 P2 F6 92.12(15) . . ? F3 P2 F6 177.52(15) . . ? F2 P2 F5 179.49(15) . . ? F1 P2 F5 90.07(13) . . ? F3 P2 F5 89.29(14) . . ? F6 P2 F5 88.73(14) . . ? F2 P2 F4 89.78(13) . . ? F1 P2 F4 179.43(16) . . ? F3 P2 F4 90.08(14) . . ? F6 P2 F4 88.41(13) . . ? F5 P2 F4 89.74(12) . . ? C1 N1 C2 111.7(2) . . ? C1 N1 C4 128.2(2) . . ? C2 N1 C4 119.8(2) . . ? C1 N2 C3 111.1(2) . . ? C1 N2 C13 129.1(2) . . ? C3 N2 C13 119.7(2) . . ? N1 C1 N2 102.9(2) . . ? N1 C1 Ir1 124.5(2) . . ? N2 C1 Ir1 131.3(2) . . ? C3 C2 N1 107.0(3) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 107.4(3) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C5 C4 C9 121.5(3) . . ? C5 C4 N1 120.2(3) . . ? C9 C4 N1 117.8(3) . . ? C4 C5 C6 118.0(3) . . ? C4 C5 C10 121.2(3) . . ? C6 C5 C10 120.6(3) . . ? C7 C6 C5 122.1(3) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C11 120.8(3) . . ? C6 C7 C11 121.0(3) . . ? C7 C8 C9 122.3(3) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C8 C9 C4 117.6(3) . . ? C8 C9 C12 119.5(3) . . ? C4 C9 C12 122.8(3) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 122.4(3) . . ? C18 C13 N2 118.6(3) . . ? C14 C13 N2 118.8(3) . . ? C15 C14 C13 117.5(3) . . ? C15 C14 C19 120.3(3) . . ? C13 C14 C19 122.2(3) . . ? C16 C15 C14 122.0(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.5(3) . . ? C15 C16 C20 120.4(3) . . ? C17 C16 C20 121.1(3) . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C13 117.8(3) . . ? C17 C18 C21 120.3(3) . . ? C13 C18 C21 121.9(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C29 124.1(3) . . ? C23 C22 Ir1 69.57(17) . . ? C29 C22 Ir1 113.1(2) . . ? C23 C22 H22 118.1 . . ? C29 C22 H22 113.8 . . ? Ir1 C22 H22 107.3 . . ? C22 C23 C24 125.7(3) . . ? C22 C23 Ir1 73.66(17) . . ? C24 C23 Ir1 110.87(19) . . ? C22 C23 H23 118.5 . . ? C24 C23 H23 112.2 . . ? Ir1 C23 H23 105.3 . . ? C23 C24 C25 113.6(3) . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 111.9(2) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 123.3(3) . . ? C27 C26 Ir1 69.31(16) . . ? C25 C26 Ir1 113.49(19) . . ? C27 C26 H26 116.3 . . ? C25 C26 H26 115.5 . . ? Ir1 C26 H26 108.2 . . ? C26 C27 C28 125.1(3) . . ? C26 C27 Ir1 73.58(17) . . ? C28 C27 Ir1 112.0(2) . . ? C26 C27 H27 118.0 . . ? C28 C27 H27 112.1 . . ? Ir1 C27 H27 107.2 . . ? C27 C28 C29 113.8(3) . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C22 C29 C28 112.5(3) . . ? C22 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C22 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? P1 C30 H30A 109.5 . . ? P1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P1 C31 H31A 109.5 . . ? P1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 119.1(3) . . ? C33 C32 P1 123.1(2) . . ? C37 C32 P1 117.8(2) . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 119.9(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 120.6(3) . . ? C36 C37 H37 119.7 . . ? C32 C37 H37 119.7 . . ? Cl2 C1S C1S 74.6(11) . 2_676 ? Cl2 C1S Cl1 10.1(8) . . ? C1S C1S Cl1 64.7(9) 2_676 . ? Cl2 C1S Cl2 124.0(8) . 2_676 ? C1S C1S Cl2 49.4(8) 2_676 2_676 ? Cl1 C1S Cl2 114.1(8) . 2_676 ? Cl2 C1S Cl1 138.9(10) . 2_676 ? C1S C1S Cl1 64.4(9) 2_676 2_676 ? Cl1 C1S Cl1 129.1(7) . 2_676 ? Cl2 C1S Cl1 15.1(3) 2_676 2_676 ? C1S Cl1 C1S 50.9(7) . 2_676 ? C1S Cl2 C1S 56.0(8) . 2_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C31 8.08(15) . . . . ? C27 Ir1 P1 C31 -140.56(16) . . . . ? C23 Ir1 P1 C31 118.58(18) . . . . ? C26 Ir1 P1 C31 -176.83(16) . . . . ? C22 Ir1 P1 C31 -160.7(6) . . . . ? C1 Ir1 P1 C30 -111.84(14) . . . . ? C27 Ir1 P1 C30 99.52(14) . . . . ? C23 Ir1 P1 C30 -1.33(18) . . . . ? C26 Ir1 P1 C30 63.25(14) . . . . ? C22 Ir1 P1 C30 79.4(6) . . . . ? C1 Ir1 P1 C32 129.19(13) . . . . ? C27 Ir1 P1 C32 -19.45(13) . . . . ? C23 Ir1 P1 C32 -120.31(17) . . . . ? C26 Ir1 P1 C32 -55.72(13) . . . . ? C22 Ir1 P1 C32 -39.6(6) . . . . ? C2 N1 C1 N2 0.9(3) . . . . ? C4 N1 C1 N2 -172.3(3) . . . . ? C2 N1 C1 Ir1 -167.0(2) . . . . ? C4 N1 C1 Ir1 19.8(4) . . . . ? C3 N2 C1 N1 -0.5(3) . . . . ? C13 N2 C1 N1 175.0(3) . . . . ? C3 N2 C1 Ir1 166.2(2) . . . . ? C13 N2 C1 Ir1 -18.2(5) . . . . ? C27 Ir1 C1 N1 30.8(4) . . . . ? C23 Ir1 C1 N1 136.1(3) . . . . ? C26 Ir1 C1 N1 153.4(10) . . . . ? C22 Ir1 C1 N1 99.7(3) . . . . ? P1 Ir1 C1 N1 -78.6(2) . . . . ? C27 Ir1 C1 N2 -133.5(3) . . . . ? C23 Ir1 C1 N2 -28.2(3) . . . . ? C26 Ir1 C1 N2 -10.8(13) . . . . ? C22 Ir1 C1 N2 -64.5(3) . . . . ? P1 Ir1 C1 N2 117.1(3) . . . . ? C1 N1 C2 C3 -1.0(4) . . . . ? C4 N1 C2 C3 172.9(3) . . . . ? N1 C2 C3 N2 0.6(4) . . . . ? C1 N2 C3 C2 -0.1(4) . . . . ? C13 N2 C3 C2 -176.1(3) . . . . ? C1 N1 C4 C5 -82.5(4) . . . . ? C2 N1 C4 C5 104.7(3) . . . . ? C1 N1 C4 C9 105.6(3) . . . . ? C2 N1 C4 C9 -67.2(4) . . . . ? C9 C4 C5 C6 -6.0(4) . . . . ? N1 C4 C5 C6 -177.5(3) . . . . ? C9 C4 C5 C10 169.0(3) . . . . ? N1 C4 C5 C10 -2.5(4) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? C10 C5 C6 C7 -173.5(3) . . . . ? C5 C6 C7 C8 2.3(5) . . . . ? C5 C6 C7 C11 -180.0(3) . . . . ? C6 C7 C8 C9 -2.0(5) . . . . ? C11 C7 C8 C9 -179.7(3) . . . . ? C7 C8 C9 C4 -2.2(4) . . . . ? C7 C8 C9 C12 173.1(3) . . . . ? C5 C4 C9 C8 6.3(4) . . . . ? N1 C4 C9 C8 178.1(3) . . . . ? C5 C4 C9 C12 -168.8(3) . . . . ? N1 C4 C9 C12 2.9(4) . . . . ? C1 N2 C13 C18 -70.8(4) . . . . ? C3 N2 C13 C18 104.4(3) . . . . ? C1 N2 C13 C14 113.8(3) . . . . ? C3 N2 C13 C14 -71.0(4) . . . . ? C18 C13 C14 C15 1.9(4) . . . . ? N2 C13 C14 C15 177.2(3) . . . . ? C18 C13 C14 C19 -178.2(3) . . . . ? N2 C13 C14 C19 -2.9(4) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C19 C14 C15 C16 179.5(3) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C14 C15 C16 C20 -179.6(3) . . . . ? C15 C16 C17 C18 0.4(4) . . . . ? C20 C16 C17 C18 179.5(3) . . . . ? C16 C17 C18 C13 0.8(4) . . . . ? C16 C17 C18 C21 -177.8(3) . . . . ? C14 C13 C18 C17 -2.0(4) . . . . ? N2 C13 C18 C17 -177.3(2) . . . . ? C14 C13 C18 C21 176.6(3) . . . . ? N2 C13 C18 C21 1.3(4) . . . . ? C1 Ir1 C22 C23 99.12(18) . . . . ? C27 Ir1 C22 C23 -112.43(19) . . . . ? C26 Ir1 C22 C23 -75.88(18) . . . . ? P1 Ir1 C22 C23 -91.9(6) . . . . ? C1 Ir1 C22 C29 -141.5(2) . . . . ? C27 Ir1 C22 C29 7.0(2) . . . . ? C23 Ir1 C22 C29 119.4(3) . . . . ? C26 Ir1 C22 C29 43.5(2) . . . . ? P1 Ir1 C22 C29 27.5(7) . . . . ? C29 C22 C23 C24 -0.5(5) . . . . ? Ir1 C22 C23 C24 104.3(3) . . . . ? C29 C22 C23 Ir1 -104.7(3) . . . . ? C1 Ir1 C23 C22 -82.07(18) . . . . ? C27 Ir1 C23 C22 65.71(19) . . . . ? C26 Ir1 C23 C22 99.80(19) . . . . ? P1 Ir1 C23 C22 165.95(13) . . . . ? C1 Ir1 C23 C24 155.3(2) . . . . ? C27 Ir1 C23 C24 -56.9(2) . . . . ? C26 Ir1 C23 C24 -22.8(2) . . . . ? C22 Ir1 C23 C24 -122.6(3) . . . . ? P1 Ir1 C23 C24 43.3(3) . . . . ? C22 C23 C24 C25 -47.7(4) . . . . ? Ir1 C23 C24 C25 36.7(3) . . . . ? C23 C24 C25 C26 -31.5(4) . . . . ? C24 C25 C26 C27 91.2(4) . . . . ? C24 C25 C26 Ir1 11.3(4) . . . . ? C1 Ir1 C26 C27 -129.7(10) . . . . ? C23 Ir1 C26 C27 -112.15(19) . . . . ? C22 Ir1 C26 C27 -75.96(19) . . . . ? P1 Ir1 C26 C27 101.69(17) . . . . ? C1 Ir1 C26 C25 -11.3(12) . . . . ? C27 Ir1 C26 C25 118.4(3) . . . . ? C23 Ir1 C26 C25 6.3(2) . . . . ? C22 Ir1 C26 C25 42.5(2) . . . . ? P1 Ir1 C26 C25 -139.9(2) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? Ir1 C26 C27 C28 105.7(3) . . . . ? C25 C26 C27 Ir1 -105.2(3) . . . . ? C1 Ir1 C27 C26 171.33(19) . . . . ? C23 Ir1 C27 C26 65.96(19) . . . . ? C22 Ir1 C27 C26 99.67(19) . . . . ? P1 Ir1 C27 C26 -77.37(17) . . . . ? C1 Ir1 C27 C28 49.5(3) . . . . ? C23 Ir1 C27 C28 -55.8(2) . . . . ? C26 Ir1 C27 C28 -121.8(3) . . . . ? C22 Ir1 C27 C28 -22.1(2) . . . . ? P1 Ir1 C27 C28 160.8(2) . . . . ? C26 C27 C28 C29 -50.6(4) . . . . ? Ir1 C27 C28 C29 34.3(3) . . . . ? C23 C22 C29 C28 89.2(4) . . . . ? Ir1 C22 C29 C28 9.0(3) . . . . ? C27 C28 C29 C22 -28.2(4) . . . . ? C31 P1 C32 C33 -121.0(3) . . . . ? C30 P1 C32 C33 -16.4(3) . . . . ? Ir1 P1 C32 C33 105.8(2) . . . . ? C31 P1 C32 C37 60.8(3) . . . . ? C30 P1 C32 C37 165.3(2) . . . . ? Ir1 P1 C32 C37 -72.5(2) . . . . ? C37 C32 C33 C34 -0.7(4) . . . . ? P1 C32 C33 C34 -179.0(2) . . . . ? C32 C33 C34 C35 -0.4(5) . . . . ? C33 C34 C35 C36 0.5(5) . . . . ? C34 C35 C36 C37 0.4(5) . . . . ? C35 C36 C37 C32 -1.5(5) . . . . ? C33 C32 C37 C36 1.6(4) . . . . ? P1 C32 C37 C36 180.0(2) . . . . ? Cl2 C1S Cl1 C1S -169(5) . . . 2_676 ? Cl2 C1S Cl1 C1S 1.7(7) 2_676 . . 2_676 ? Cl1 C1S Cl1 C1S 0.000(2) 2_676 . . 2_676 ? Cl1 C1S Cl2 C1S 10(4) . . . 2_676 ? Cl2 C1S Cl2 C1S 0.000(1) 2_676 . . 2_676 ? Cl1 C1S Cl2 C1S -2.7(11) 2_676 . . 2_676 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.850 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.117 #===END # Attachment 'KerrAll.cif' data_5A _database_code_depnum_ccdc_archive 'CCDC 664296' #------------------------------------------------------ #---------------5A PPh3 complex------------------------ #------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H51 F6 Ir N2 O0.50 P2' _chemical_formula_weight 1020.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ir Ir -1.4442 7.9887 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0693(11) _cell_length_b 13.9078(14) _cell_length_c 15.0418(16) _cell_angle_alpha 88.499(3) _cell_angle_beta 75.174(3) _cell_angle_gamma 87.285(4) _cell_volume 2235.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 54624 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.99 _exptl_crystal_description 'fragment from decaying prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 3.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.550 _exptl_absorpt_correction_T_max 0.628 _exptl_absorpt_process_details Sortav/scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17769 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.03 _reflns_number_total 9632 _reflns_number_gt 7438 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect and Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.8458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9632 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Ir1 Ir 0.52694(2) 0.313362(15) 0.268779(17) 0.03254(9) Uani 1 1 d . . . P1 P 0.73863(13) 0.25753(10) 0.24048(11) 0.0329(3) Uani 1 1 d . . . P2 P 0.79995(16) 0.23868(13) 0.67552(12) 0.0480(4) Uani 1 1 d . . . F1 F 0.8663(9) 0.3184(6) 0.5955(6) 0.045(2) Uiso 0.50 1 d P . . F2 F 0.6715(9) 0.2736(9) 0.6501(7) 0.066(3) Uiso 0.50 1 d P . . F3 F 0.7213(8) 0.3013(6) 0.7558(5) 0.054(2) Uiso 0.50 1 d P . . F4 F 0.7476(9) 0.1699(6) 0.7617(7) 0.056(2) Uiso 0.50 1 d P . . F5 F 0.9376(8) 0.2339(8) 0.7003(6) 0.046(2) Uiso 0.50 1 d P . . F6 F 0.8713(9) 0.1535(6) 0.6093(6) 0.055(2) Uiso 0.50 1 d P . . N1 N 0.3939(4) 0.1383(3) 0.3649(3) 0.0336(10) Uani 1 1 d . . . N2 N 0.4320(4) 0.1161(3) 0.2184(3) 0.0314(10) Uani 1 1 d . . . C1 C 0.4454(5) 0.1819(4) 0.2811(4) 0.0309(12) Uani 1 1 d . . . C2 C 0.3531(5) 0.0478(4) 0.3525(4) 0.0384(13) Uani 1 1 d . . . H2 H 0.3158 0.0037 0.3997 0.046 Uiso 1 1 calc R . . C3 C 0.3761(5) 0.0343(4) 0.2619(4) 0.0394(14) Uani 1 1 d . . . H3 H 0.3576 -0.0209 0.2328 0.047 Uiso 1 1 calc R . . C4 C 0.3565(5) 0.1885(4) 0.4509(4) 0.0331(12) Uani 1 1 d . . . C5 C 0.2322(5) 0.2225(4) 0.4814(4) 0.0350(13) Uani 1 1 d . . . C6 C 0.1973(5) 0.2755(4) 0.5614(4) 0.0370(13) Uani 1 1 d . . . H6 H 0.1138 0.3011 0.5809 0.044 Uiso 1 1 calc R . . C7 C 0.2810(5) 0.2926(4) 0.6143(4) 0.0347(13) Uani 1 1 d . . . C8 C 0.4006(5) 0.2525(4) 0.5850(4) 0.0369(13) Uani 1 1 d . . . H8 H 0.4581 0.2615 0.6211 0.044 Uiso 1 1 calc R . . C9 C 0.4407(5) 0.1996(4) 0.5053(4) 0.0351(13) Uani 1 1 d . . . C10 C 0.1321(5) 0.2024(5) 0.4326(4) 0.0424(14) Uani 1 1 d . . . H10A H 0.0644 0.1686 0.4748 0.064 Uiso 1 1 calc R . . H10B H 0.1685 0.1624 0.3789 0.064 Uiso 1 1 calc R . . H10C H 0.0987 0.2634 0.4126 0.064 Uiso 1 1 calc R . . C11 C 0.2367(6) 0.3485(4) 0.7012(4) 0.0467(15) Uani 1 1 d . . . H11A H 0.1674 0.3159 0.7430 0.070 Uiso 1 1 calc R . . H11B H 0.2081 0.4134 0.6867 0.070 Uiso 1 1 calc R . . H11C H 0.3056 0.3528 0.7306 0.070 Uiso 1 1 calc R . . C12 C 0.5715(5) 0.1548(5) 0.4798(4) 0.0454(15) Uani 1 1 d . . . H12A H 0.6220 0.1891 0.4264 0.068 Uiso 1 1 calc R . . H12B H 0.5682 0.0870 0.4645 0.068 Uiso 1 1 calc R . . H12C H 0.6091 0.1590 0.5317 0.068 Uiso 1 1 calc R . . C13 C 0.4374(5) 0.1367(4) 0.1210(4) 0.0323(12) Uani 1 1 d . . . C14 C 0.3269(5) 0.1770(4) 0.1025(4) 0.0335(12) Uani 1 1 d . . . C15 C 0.3302(5) 0.2000(4) 0.0107(4) 0.0366(13) Uani 1 1 d . . . H15 H 0.2575 0.2289 -0.0030 0.044 Uiso 1 1 calc R . . C16 C 0.4343(5) 0.1826(4) -0.0600(4) 0.0359(13) Uani 1 1 d . . . C17 C 0.5398(5) 0.1380(4) -0.0383(4) 0.0376(13) Uani 1 1 d . . . H17 H 0.6123 0.1244 -0.0866 0.045 Uiso 1 1 calc R . . C18 C 0.5421(5) 0.1132(4) 0.0514(4) 0.0353(13) Uani 1 1 d . . . C19 C 0.2070(5) 0.1916(4) 0.1759(4) 0.0414(14) Uani 1 1 d . . . H19A H 0.1704 0.1292 0.1947 0.062 Uiso 1 1 calc R . . H19B H 0.1482 0.2329 0.1517 0.062 Uiso 1 1 calc R . . H19C H 0.2242 0.2222 0.2290 0.062 Uiso 1 1 calc R . . C20 C 0.4337(6) 0.2051(4) -0.1583(4) 0.0488(16) Uani 1 1 d . . . H20A H 0.3496 0.2282 -0.1610 0.073 Uiso 1 1 calc R . . H20B H 0.4576 0.1468 -0.1950 0.073 Uiso 1 1 calc R . . H20C H 0.4934 0.2550 -0.1830 0.073 Uiso 1 1 calc R . . C21 C 0.6544(5) 0.0569(4) 0.0681(4) 0.0413(14) Uani 1 1 d . . . H21A H 0.6997 0.0975 0.0998 0.062 Uiso 1 1 calc R . . H21B H 0.7097 0.0366 0.0092 0.062 Uiso 1 1 calc R . . H21C H 0.6266 -0.0001 0.1063 0.062 Uiso 1 1 calc R . . C22 C 0.3858(5) 0.3822(4) 0.2069(4) 0.0366(13) Uani 1 1 d . . . H22 H 0.3894 0.3236 0.1751 0.044 Uiso 1 1 calc R . . C23 C 0.3353(5) 0.3813(4) 0.3017(4) 0.0323(12) Uani 1 1 d . . . H23 H 0.3074 0.3216 0.3299 0.039 Uiso 1 1 calc R . . C24 C 0.3211(5) 0.4670(4) 0.3635(4) 0.0403(14) Uani 1 1 d . . . H24A H 0.2445 0.4612 0.4143 0.048 Uiso 1 1 calc R . . H24B H 0.3108 0.5264 0.3279 0.048 Uiso 1 1 calc R . . C25 C 0.4339(6) 0.4756(4) 0.4039(5) 0.0442(15) Uani 1 1 d . . . H25A H 0.4399 0.5437 0.4193 0.053 Uiso 1 1 calc R . . H25B H 0.4203 0.4372 0.4617 0.053 Uiso 1 1 calc R . . C26 C 0.5559(5) 0.4418(4) 0.3394(5) 0.0406(15) Uani 1 1 d . . . H26 H 0.6108 0.4026 0.3656 0.049 Uiso 1 1 calc R . . C27 C 0.5963(6) 0.4617(4) 0.2460(5) 0.0452(16) Uani 1 1 d . . . H27 H 0.6744 0.4338 0.2131 0.054 Uiso 1 1 calc R . . C28 C 0.5224(6) 0.5262(4) 0.1928(5) 0.0493(16) Uani 1 1 d . . . H28A H 0.4724 0.5754 0.2347 0.059 Uiso 1 1 calc R . . H28B H 0.5819 0.5602 0.1428 0.059 Uiso 1 1 calc R . . C29 C 0.4353(6) 0.4707(4) 0.1514(5) 0.0451(15) Uani 1 1 d . . . H29A H 0.3638 0.5140 0.1462 0.054 Uiso 1 1 calc R . . H29B H 0.4808 0.4509 0.0886 0.054 Uiso 1 1 calc R . . C30 C 0.8054(5) 0.2511(4) 0.1155(4) 0.0370(13) Uani 1 1 d . . . C31 C 0.7436(6) 0.2988(4) 0.0558(4) 0.0446(15) Uani 1 1 d . . . H31 H 0.6677 0.3349 0.0799 0.054 Uiso 1 1 calc R . . C32 C 0.7931(7) 0.2934(5) -0.0382(5) 0.0571(18) Uani 1 1 d . . . H32 H 0.7510 0.3263 -0.0785 0.069 Uiso 1 1 calc R . . C33 C 0.9032(7) 0.2407(6) -0.0744(5) 0.064(2) Uani 1 1 d . . . H33 H 0.9364 0.2370 -0.1391 0.077 Uiso 1 1 calc R . . C34 C 0.9645(6) 0.1933(6) -0.0150(5) 0.0589(19) Uani 1 1 d . . . H34 H 1.0403 0.1573 -0.0394 0.071 Uiso 1 1 calc R . . C35 C 0.9164(5) 0.1979(5) 0.0787(5) 0.0459(15) Uani 1 1 d . . . H35 H 0.9589 0.1649 0.1186 0.055 Uiso 1 1 calc R . . C36 C 0.7897(5) 0.1393(4) 0.2796(4) 0.0338(12) Uani 1 1 d . . . C37 C 0.7181(5) 0.0605(4) 0.2805(4) 0.0372(13) Uani 1 1 d . . . H37 H 0.6400 0.0690 0.2653 0.045 Uiso 1 1 calc R . . C38 C 0.7578(6) -0.0311(4) 0.3030(4) 0.0442(15) Uani 1 1 d . . . H38 H 0.7086 -0.0847 0.3008 0.053 Uiso 1 1 calc R . . C39 C 0.8699(6) -0.0444(4) 0.3287(5) 0.0477(16) Uani 1 1 d . . . H39 H 0.8966 -0.1066 0.3455 0.057 Uiso 1 1 calc R . . C40 C 0.9421(6) 0.0345(5) 0.3295(5) 0.0517(17) Uani 1 1 d . . . H40 H 1.0191 0.0261 0.3462 0.062 Uiso 1 1 calc R . . C41 C 0.9023(5) 0.1258(4) 0.3058(4) 0.0417(14) Uani 1 1 d . . . H41 H 0.9517 0.1794 0.3075 0.050 Uiso 1 1 calc R . . C42 C 0.8441(5) 0.3389(4) 0.2765(4) 0.0372(13) Uani 1 1 d . . . C43 C 0.9313(5) 0.3915(4) 0.2125(5) 0.0440(15) Uani 1 1 d . . . H43 H 0.9385 0.3849 0.1486 0.053 Uiso 1 1 calc R . . C44 C 1.0077(6) 0.4536(4) 0.2418(5) 0.0519(17) Uani 1 1 d . . . H44 H 1.0663 0.4894 0.1978 0.062 Uiso 1 1 calc R . . C45 C 0.9989(6) 0.4634(5) 0.3339(6) 0.0538(18) Uani 1 1 d . . . H45 H 1.0518 0.5056 0.3533 0.065 Uiso 1 1 calc R . . C46 C 0.9131(6) 0.4118(5) 0.3984(5) 0.0539(18) Uani 1 1 d . . . H46 H 0.9067 0.4188 0.4621 0.065 Uiso 1 1 calc R . . C47 C 0.8356(6) 0.3494(4) 0.3696(5) 0.0439(15) Uani 1 1 d . . . H47 H 0.7768 0.3140 0.4139 0.053 Uiso 1 1 calc R . . F7 F 0.6717(13) 0.1708(12) 0.6710(10) 0.052(4) Uiso 0.30 1 d P . . F8 F 0.7732(7) 0.3292(5) 0.7463(5) 0.0475(19) Uiso 0.50 1 d P . . F9 F 0.8012(12) 0.1487(8) 0.7581(8) 0.054(3) Uiso 0.35 1 d P . . F10 F 0.703(2) 0.3009(16) 0.6089(17) 0.035(5) Uiso 0.15 1 d P . . F11 F 0.8436(16) 0.1829(11) 0.5743(11) 0.063(4) Uiso 0.30 1 d P . . F12 F 0.8061(18) 0.3007(11) 0.5970(11) 0.069(4) Uiso 0.30 1 d P . . F13 F 0.9201(19) 0.2753(15) 0.6985(13) 0.046(5) Uiso 0.20 1 d P . . F14 F 0.913(2) 0.1967(16) 0.6923(14) 0.054(6) Uiso 0.20 1 d P . . F15 F 0.8126(18) 0.1520(13) 0.6097(13) 0.036(4) Uiso 0.20 1 d P . . F16 F 0.6762(16) 0.2182(18) 0.6597(12) 0.035(4) Uiso 0.20 1 d P . . F17 F 0.714(3) 0.165(2) 0.714(2) 0.066(8) Uiso 0.15 1 d P . . F18 F 0.877(3) 0.3340(19) 0.630(2) 0.050(7) Uiso 0.15 1 d P . . O1S O 0.9309(18) 0.5375(13) 0.0185(13) 0.058(5) Uiso 0.25 1 d P . . O2S O 0.836(2) 0.5556(15) 0.0037(15) 0.072(6) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02737(12) 0.02840(12) 0.04731(15) -0.00320(9) -0.01921(10) -0.00120(8) P1 0.0261(7) 0.0309(7) 0.0456(9) -0.0018(6) -0.0162(7) -0.0020(6) P2 0.0391(9) 0.0509(10) 0.0510(11) -0.0091(8) -0.0058(8) 0.0023(8) N1 0.027(2) 0.036(2) 0.041(3) -0.001(2) -0.014(2) -0.0032(19) N2 0.026(2) 0.033(2) 0.039(3) -0.004(2) -0.015(2) -0.0019(19) C1 0.023(3) 0.033(3) 0.040(3) -0.005(2) -0.014(2) 0.003(2) C2 0.043(3) 0.035(3) 0.041(4) 0.007(3) -0.016(3) -0.013(3) C3 0.033(3) 0.031(3) 0.057(4) -0.002(3) -0.016(3) -0.005(2) C4 0.034(3) 0.033(3) 0.035(3) 0.000(2) -0.013(3) -0.006(2) C5 0.029(3) 0.040(3) 0.041(3) 0.006(3) -0.017(3) -0.008(2) C6 0.029(3) 0.045(3) 0.037(3) 0.003(3) -0.010(3) 0.001(2) C7 0.038(3) 0.031(3) 0.038(3) 0.000(2) -0.015(3) -0.007(2) C8 0.034(3) 0.037(3) 0.044(4) 0.006(3) -0.018(3) -0.009(2) C9 0.032(3) 0.035(3) 0.039(3) 0.004(3) -0.011(3) -0.004(2) C10 0.028(3) 0.055(4) 0.047(4) -0.003(3) -0.015(3) -0.006(3) C11 0.044(4) 0.048(4) 0.052(4) -0.006(3) -0.020(3) 0.002(3) C12 0.031(3) 0.063(4) 0.045(4) -0.008(3) -0.016(3) 0.003(3) C13 0.029(3) 0.029(3) 0.041(3) 0.000(2) -0.015(3) -0.003(2) C14 0.032(3) 0.031(3) 0.043(3) -0.004(2) -0.017(3) -0.005(2) C15 0.032(3) 0.036(3) 0.044(4) -0.003(3) -0.014(3) 0.002(2) C16 0.043(3) 0.028(3) 0.040(3) -0.003(2) -0.017(3) -0.005(2) C17 0.035(3) 0.035(3) 0.041(4) -0.005(3) -0.004(3) -0.008(2) C18 0.032(3) 0.027(3) 0.049(4) -0.006(2) -0.012(3) -0.005(2) C19 0.029(3) 0.051(4) 0.047(4) -0.004(3) -0.014(3) -0.001(3) C20 0.056(4) 0.041(3) 0.050(4) -0.001(3) -0.014(3) -0.002(3) C21 0.033(3) 0.043(3) 0.052(4) -0.006(3) -0.018(3) 0.000(3) C22 0.030(3) 0.034(3) 0.051(4) 0.001(3) -0.020(3) 0.007(2) C23 0.028(3) 0.025(3) 0.045(4) 0.001(2) -0.012(3) 0.007(2) C24 0.038(3) 0.039(3) 0.048(4) -0.008(3) -0.017(3) -0.001(3) C25 0.043(3) 0.038(3) 0.057(4) -0.006(3) -0.021(3) 0.001(3) C26 0.040(3) 0.025(3) 0.067(5) -0.008(3) -0.033(3) -0.002(2) C27 0.037(3) 0.024(3) 0.080(5) -0.001(3) -0.026(3) -0.002(2) C28 0.044(4) 0.037(3) 0.071(5) 0.007(3) -0.023(3) -0.002(3) C29 0.041(3) 0.044(3) 0.054(4) 0.005(3) -0.020(3) 0.001(3) C30 0.033(3) 0.040(3) 0.044(3) -0.001(3) -0.019(3) -0.010(2) C31 0.043(3) 0.042(3) 0.054(4) -0.003(3) -0.021(3) -0.006(3) C32 0.061(5) 0.065(5) 0.050(4) 0.000(4) -0.021(4) -0.014(4) C33 0.060(5) 0.090(6) 0.044(4) -0.018(4) -0.012(4) -0.023(4) C34 0.037(4) 0.080(5) 0.060(5) -0.016(4) -0.011(3) -0.005(3) C35 0.031(3) 0.059(4) 0.052(4) -0.013(3) -0.017(3) -0.005(3) C36 0.025(3) 0.038(3) 0.040(3) 0.000(3) -0.011(2) 0.001(2) C37 0.029(3) 0.035(3) 0.051(4) -0.003(3) -0.017(3) 0.001(2) C38 0.038(3) 0.038(3) 0.060(4) -0.002(3) -0.016(3) -0.005(3) C39 0.047(4) 0.035(3) 0.063(4) 0.011(3) -0.020(3) 0.001(3) C40 0.038(3) 0.047(4) 0.077(5) 0.009(3) -0.031(3) 0.001(3) C41 0.033(3) 0.041(3) 0.058(4) -0.005(3) -0.022(3) -0.003(3) C42 0.032(3) 0.037(3) 0.049(4) -0.005(3) -0.022(3) 0.003(2) C43 0.030(3) 0.042(3) 0.061(4) -0.010(3) -0.012(3) -0.006(3) C44 0.032(3) 0.043(4) 0.082(5) -0.008(3) -0.015(3) -0.007(3) C45 0.034(3) 0.048(4) 0.088(6) -0.018(4) -0.030(4) 0.001(3) C46 0.046(4) 0.050(4) 0.078(5) -0.021(4) -0.038(4) 0.011(3) C47 0.037(3) 0.041(3) 0.060(4) -0.004(3) -0.025(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.061(5) . ? Ir1 C26 2.179(5) . ? Ir1 C22 2.186(5) . ? Ir1 C23 2.222(5) . ? Ir1 C27 2.223(5) . ? Ir1 P1 2.3684(14) . ? P1 C30 1.838(6) . ? P1 C36 1.843(5) . ? P1 C42 1.849(6) . ? P2 F12 1.434(16) . ? P2 F14 1.44(2) . ? P2 F17 1.44(3) . ? P2 F16 1.491(17) . ? P2 F3 1.556(8) . ? P2 F15 1.559(17) . ? P2 F13 1.57(2) . ? P2 F4 1.592(9) . ? P2 F6 1.610(8) . ? P2 F2 1.614(10) . ? P2 F8 1.637(8) . ? P2 F18 1.65(3) . ? F1 F18 0.60(3) . ? F1 F12 0.716(16) . ? F2 F10 0.73(2) . ? F2 F16 0.78(2) . ? F2 F7 1.455(16) . ? F2 F12 1.56(2) . ? F3 F8 0.691(9) . ? F4 F9 0.641(12) . ? F4 F17 0.89(4) . ? F4 F7 1.774(16) . ? F5 F13 0.600(19) . ? F5 F14 0.62(2) . ? F6 F15 0.650(18) . ? F6 F11 0.774(15) . ? F6 F14 1.58(2) . ? N1 C1 1.381(7) . ? N1 C2 1.389(7) . ? N1 C4 1.441(7) . ? N2 C1 1.371(7) . ? N2 C3 1.387(7) . ? N2 C13 1.472(7) . ? C2 C3 1.338(8) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.398(8) . ? C4 C9 1.405(7) . ? C5 C6 1.386(8) . ? C5 C10 1.517(7) . ? C6 C7 1.398(8) . ? C6 H6 0.9500 . ? C7 C8 1.380(8) . ? C7 C11 1.497(8) . ? C8 C9 1.384(8) . ? C8 H8 0.9500 . ? C9 C12 1.508(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.382(8) . ? C13 C14 1.410(7) . ? C14 C15 1.400(8) . ? C14 C19 1.502(8) . ? C15 C16 1.370(8) . ? C15 H15 0.9500 . ? C16 C17 1.404(8) . ? C16 C20 1.505(8) . ? C17 C18 1.390(8) . ? C17 H17 0.9500 . ? C18 C21 1.509(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.392(8) . ? C22 C29 1.512(8) . ? C22 H22 0.9500 . ? C23 C24 1.508(8) . ? C23 H23 0.9500 . ? C24 C25 1.534(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.510(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.386(9) . ? C26 H26 0.9500 . ? C27 C28 1.530(8) . ? C27 H27 0.9500 . ? C28 C29 1.521(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C35 1.397(8) . ? C30 C31 1.397(8) . ? C31 C32 1.383(9) . ? C31 H31 0.9500 . ? C32 C33 1.384(10) . ? C32 H32 0.9500 . ? C33 C34 1.389(10) . ? C33 H33 0.9500 . ? C34 C35 1.376(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.381(7) . ? C36 C41 1.405(7) . ? C37 C38 1.390(8) . ? C37 H37 0.9500 . ? C38 C39 1.394(8) . ? C38 H38 0.9500 . ? C39 C40 1.390(9) . ? C39 H39 0.9500 . ? C40 C41 1.391(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.390(8) . ? C42 C43 1.396(8) . ? C43 C44 1.390(8) . ? C43 H43 0.9500 . ? C44 C45 1.374(10) . ? C44 H44 0.9500 . ? C45 C46 1.383(10) . ? C45 H45 0.9500 . ? C46 C47 1.399(8) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? F7 F16 0.68(2) . ? F7 F17 0.89(3) . ? F7 F15 1.61(2) . ? F8 F13 1.74(2) . ? F9 F17 1.32(4) . ? F9 F14 1.54(2) . ? F10 F12 1.11(2) . ? F10 F16 1.37(3) . ? F11 F15 0.70(2) . ? F11 F12 1.69(2) . ? F12 F18 1.15(3) . ? F13 F14 1.11(3) . ? F13 F18 1.46(3) . ? F15 F17 1.68(4) . ? F15 F16 1.74(3) . ? F16 F17 1.22(4) . ? O1S O2S 1.14(3) . ? O1S O1S 1.78(4) 2_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C26 146.3(3) . . ? C1 Ir1 C22 92.9(2) . . ? C26 Ir1 C22 95.0(2) . . ? C1 Ir1 C23 87.7(2) . . ? C26 Ir1 C23 79.5(2) . . ? C22 Ir1 C23 36.8(2) . . ? C1 Ir1 C27 172.5(2) . . ? C26 Ir1 C27 36.7(2) . . ? C22 Ir1 C27 79.6(2) . . ? C23 Ir1 C27 86.7(2) . . ? C1 Ir1 P1 98.45(14) . . ? C26 Ir1 P1 93.78(16) . . ? C22 Ir1 P1 144.67(17) . . ? C23 Ir1 P1 173.24(14) . . ? C27 Ir1 P1 87.42(16) . . ? C30 P1 C36 101.6(3) . . ? C30 P1 C42 102.5(3) . . ? C36 P1 C42 101.8(2) . . ? C30 P1 Ir1 108.69(18) . . ? C36 P1 Ir1 124.04(18) . . ? C42 P1 Ir1 115.46(18) . . ? F12 P2 F14 119.7(11) . . ? F12 P2 F17 130.2(18) . . ? F14 P2 F17 100.6(16) . . ? F12 P2 F16 82.0(11) . . ? F14 P2 F16 145.0(14) . . ? F17 P2 F16 49.3(16) . . ? F12 P2 F3 102.5(7) . . ? F14 P2 F3 113.8(9) . . ? F17 P2 F3 84.7(13) . . ? F16 P2 F3 84.4(8) . . ? F12 P2 F15 87.5(10) . . ? F14 P2 F15 83.5(12) . . ? F17 P2 F15 68.0(15) . . ? F16 P2 F15 69.4(11) . . ? F3 P2 F15 150.5(8) . . ? F12 P2 F13 95.8(11) . . ? F14 P2 F13 43.0(11) . . ? F17 P2 F13 134.0(17) . . ? F16 P2 F13 171.1(12) . . ? F3 P2 F13 87.8(8) . . ? F15 P2 F13 119.2(11) . . ? F12 P2 F4 161.6(9) . . ? F14 P2 F4 78.1(9) . . ? F17 P2 F4 33.8(14) . . ? F16 P2 F4 80.2(9) . . ? F3 P2 F4 71.5(4) . . ? F15 P2 F4 90.2(8) . . ? F13 P2 F4 101.2(8) . . ? F12 P2 F6 90.1(7) . . ? F14 P2 F6 62.2(9) . . ? F17 P2 F6 83.6(13) . . ? F16 P2 F6 93.0(9) . . ? F3 P2 F6 166.5(5) . . ? F15 P2 F6 23.6(7) . . ? F13 P2 F6 95.6(8) . . ? F4 P2 F6 95.0(5) . . ? F12 P2 F2 61.2(8) . . ? F14 P2 F2 172.8(10) . . ? F17 P2 F2 75.3(14) . . ? F16 P2 F2 28.8(8) . . ? F3 P2 F2 72.1(5) . . ? F15 P2 F2 89.4(8) . . ? F13 P2 F2 143.6(9) . . ? F4 P2 F2 100.6(6) . . ? F6 P2 F2 111.1(5) . . ? F12 P2 F8 92.6(7) . . ? F14 P2 F8 100.8(10) . . ? F17 P2 F8 108.3(13) . . ? F16 P2 F8 105.6(9) . . ? F3 P2 F8 24.8(3) . . ? F15 P2 F8 174.9(8) . . ? F13 P2 F8 65.9(8) . . ? F4 P2 F8 88.1(4) . . ? F6 P2 F8 161.4(5) . . ? F2 P2 F8 86.2(5) . . ? F12 P2 F18 43.0(12) . . ? F14 P2 F18 89.2(13) . . ? F17 P2 F18 170.0(16) . . ? F16 P2 F18 121.8(13) . . ? F3 P2 F18 90.0(11) . . ? F15 P2 F18 115.0(13) . . ? F13 P2 F18 54.0(12) . . ? F4 P2 F18 150.5(12) . . ? F6 P2 F18 102.5(11) . . ? F2 P2 F18 95.0(10) . . ? F8 P2 F18 68.0(11) . . ? F18 F1 F12 121(4) . . ? F18 F1 P2 78(3) . . ? F12 F1 P2 59.0(15) . . ? F10 F2 F16 129(3) . . ? F10 F2 F7 131(2) . . ? F16 F2 F7 3.7(17) . . ? F10 F2 F12 40.8(19) . . ? F16 F2 F12 105.3(18) . . ? F7 F2 F12 108.9(10) . . ? F10 F2 P2 94(2) . . ? F16 F2 P2 66.8(15) . . ? F7 F2 P2 69.7(7) . . ? F12 F2 P2 53.7(7) . . ? F8 F3 P2 84.2(11) . . ? F9 F4 F17 117(3) . . ? F9 F4 P2 92.5(16) . . ? F17 F4 P2 64(2) . . ? F9 F4 F7 122.0(19) . . ? F17 F4 F7 5(2) . . ? P2 F4 F7 62.7(6) . . ? F13 F5 F14 129(4) . . ? F13 F5 P2 71(2) . . ? F14 F5 P2 59(2) . . ? F15 F6 F11 58.4(18) . . ? F15 F6 F14 121(2) . . ? F11 F6 F14 125.5(17) . . ? F15 F6 P2 73.8(18) . . ? F11 F6 P2 81.1(13) . . ? F14 F6 P2 53.5(8) . . ? C1 N1 C2 110.6(5) . . ? C1 N1 C4 124.1(4) . . ? C2 N1 C4 123.3(5) . . ? C1 N2 C3 111.2(5) . . ? C1 N2 C13 125.6(4) . . ? C3 N2 C13 120.7(4) . . ? N2 C1 N1 103.6(4) . . ? N2 C1 Ir1 133.3(4) . . ? N1 C1 Ir1 123.0(4) . . ? C3 C2 N1 107.5(5) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 107.1(5) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C5 C4 C9 120.3(5) . . ? C5 C4 N1 118.4(5) . . ? C9 C4 N1 121.2(5) . . ? C6 C5 C4 118.7(5) . . ? C6 C5 C10 118.0(5) . . ? C4 C5 C10 123.3(5) . . ? C5 C6 C7 122.2(5) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 117.3(5) . . ? C8 C7 C11 123.1(5) . . ? C6 C7 C11 119.6(5) . . ? C7 C8 C9 122.9(5) . . ? C7 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C8 C9 C4 118.4(5) . . ? C8 C9 C12 119.8(5) . . ? C4 C9 C12 121.8(5) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.8(5) . . ? C18 C13 N2 122.0(5) . . ? C14 C13 N2 116.1(5) . . ? C15 C14 C13 117.4(5) . . ? C15 C14 C19 119.9(5) . . ? C13 C14 C19 122.7(5) . . ? C16 C15 C14 122.6(5) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 117.7(5) . . ? C15 C16 C20 121.4(5) . . ? C17 C16 C20 120.8(5) . . ? C18 C17 C16 122.4(5) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C13 C18 C17 117.9(5) . . ? C13 C18 C21 122.9(5) . . ? C17 C18 C21 119.2(5) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C29 124.1(5) . . ? C23 C22 Ir1 73.0(3) . . ? C29 C22 Ir1 111.0(4) . . ? C23 C22 H22 118.0 . . ? C29 C22 H22 118.0 . . ? Ir1 C22 H22 86.0 . . ? C22 C23 C24 125.5(5) . . ? C22 C23 Ir1 70.2(3) . . ? C24 C23 Ir1 113.0(4) . . ? C22 C23 H23 117.2 . . ? C24 C23 H23 117.2 . . ? Ir1 C23 H23 86.7 . . ? C23 C24 C25 112.2(5) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 113.1(5) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 126.9(5) . . ? C27 C26 Ir1 73.4(3) . . ? C25 C26 Ir1 109.6(4) . . ? C27 C26 H26 116.5 . . ? C25 C26 H26 116.5 . . ? Ir1 C26 H26 86.8 . . ? C26 C27 C28 123.8(6) . . ? C26 C27 Ir1 69.9(3) . . ? C28 C27 Ir1 112.7(4) . . ? C26 C27 H27 118.1 . . ? C28 C27 H27 118.1 . . ? Ir1 C27 H27 87.4 . . ? C29 C28 C27 113.1(5) . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C22 C29 C28 113.6(5) . . ? C22 C29 H29A 108.9 . . ? C28 C29 H29A 108.9 . . ? C22 C29 H29B 108.9 . . ? C28 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C35 C30 C31 119.1(6) . . ? C35 C30 P1 121.1(5) . . ? C31 C30 P1 119.8(5) . . ? C32 C31 C30 119.9(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.8(7) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C34 119.3(7) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 120.6(7) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C30 120.3(6) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C37 C36 C41 118.3(5) . . ? C37 C36 P1 119.7(4) . . ? C41 C36 P1 121.9(4) . . ? C36 C37 C38 121.4(5) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C37 C38 C39 120.0(5) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 119.2(5) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 120.4(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C36 120.6(5) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? C47 C42 C43 118.8(5) . . ? C47 C42 P1 119.5(5) . . ? C43 C42 P1 121.6(5) . . ? C44 C43 C42 120.3(6) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.5(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 120.0(6) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C47 119.9(7) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 120.4(6) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? F16 F7 F17 102(3) . . ? F16 F7 F2 4.2(19) . . ? F17 F7 F2 103(2) . . ? F16 F7 F15 89(2) . . ? F17 F7 F15 79(2) . . ? F2 F7 F15 93.4(11) . . ? F16 F7 P2 56(2) . . ? F17 F7 P2 54(2) . . ? F2 F7 P2 59.4(7) . . ? F15 F7 P2 54.9(8) . . ? F16 F7 F4 98(2) . . ? F17 F7 F4 5(2) . . ? F2 F7 F4 99.1(9) . . ? F15 F7 F4 82.4(10) . . ? P2 F7 F4 53.6(5) . . ? F3 F8 P2 71.0(10) . . ? F3 F8 F13 119.1(13) . . ? P2 F8 F13 55.1(7) . . ? F4 F9 F17 37.2(18) . . ? F4 F9 F14 116.1(19) . . ? F17 F9 F14 101.1(17) . . ? F4 F9 P2 65.9(14) . . ? F17 F9 P2 53.9(13) . . ? F14 F9 P2 51.4(8) . . ? F2 F10 F12 114(3) . . ? F2 F10 F16 26.6(16) . . ? F12 F10 F16 101.0(19) . . ? F2 F10 P2 61.9(18) . . ? F12 F10 P2 51.8(12) . . ? F16 F10 P2 53.4(10) . . ? F15 F11 F6 52.0(18) . . ? F15 F11 P2 68.3(19) . . ? F6 F11 P2 71.7(13) . . ? F15 F11 F12 113(2) . . ? F6 F11 F12 117.0(17) . . ? P2 F11 F12 50.4(7) . . ? F1 F12 F10 158(3) . . ? F1 F12 F18 26.9(18) . . ? F10 F12 F18 138(2) . . ? F1 F12 P2 95.7(18) . . ? F10 F12 P2 90.7(17) . . ? F18 F12 P2 78.6(16) . . ? F1 F12 F2 152(2) . . ? F10 F12 F2 25.6(13) . . ? F18 F12 F2 125(2) . . ? P2 F12 F2 65.1(8) . . ? F1 F12 F11 100.9(19) . . ? F10 F12 F11 100.4(17) . . ? F18 F12 F11 110.9(18) . . ? P2 F12 F11 64.1(8) . . ? F2 F12 F11 89.6(11) . . ? F5 F13 F14 26(2) . . ? F5 F13 F18 134(3) . . ? F14 F13 F18 115(2) . . ? F5 F13 P2 88(2) . . ? F14 F13 P2 62.1(15) . . ? F18 F13 P2 65.9(14) . . ? F5 F13 F8 129(3) . . ? F14 F13 F8 110.6(18) . . ? F18 F13 F8 69.4(14) . . ? P2 F13 F8 59.0(7) . . ? F5 F14 F13 24.8(19) . . ? F5 F14 P2 100(3) . . ? F13 F14 P2 74.9(15) . . ? F5 F14 F9 126(3) . . ? F13 F14 F9 117.3(18) . . ? P2 F14 F9 71.6(11) . . ? F5 F14 F6 137(3) . . ? F13 F14 F6 121.3(19) . . ? P2 F14 F6 64.3(10) . . ? F9 F14 F6 88.3(14) . . ? F6 F15 F11 70(2) . . ? F6 F15 P2 82.6(19) . . ? F11 F15 P2 87(2) . . ? F6 F15 F7 144(3) . . ? F11 F15 F7 125(3) . . ? P2 F15 F7 67.4(9) . . ? F6 F15 F17 114(3) . . ? F11 F15 F17 136(3) . . ? P2 F15 F17 52.5(12) . . ? F7 F15 F17 31.2(12) . . ? F6 F15 F16 136(2) . . ? F11 F15 F16 103(3) . . ? P2 F15 F16 53.5(8) . . ? F7 F15 F16 22.9(7) . . ? F17 F15 F16 41.9(13) . . ? F7 F16 F2 172(4) . . ? F7 F16 F17 45(2) . . ? F2 F16 F17 137(3) . . ? F7 F16 F10 161(3) . . ? F2 F16 F10 24.9(15) . . ? F17 F16 F10 142(3) . . ? F7 F16 P2 102(2) . . ? F2 F16 P2 84.4(18) . . ? F17 F16 P2 63.0(17) . . ? F10 F16 P2 79.3(14) . . ? F7 F16 F15 68(2) . . ? F2 F16 F15 120(2) . . ? F17 F16 F15 66.5(18) . . ? F10 F16 F15 97.9(15) . . ? P2 F16 F15 57.1(9) . . ? F7 F17 F4 169(4) . . ? F7 F17 F16 32.9(17) . . ? F4 F17 F16 139(4) . . ? F7 F17 F9 164(4) . . ? F4 F17 F9 25.7(14) . . ? F16 F17 F9 146(3) . . ? F7 F17 P2 95(3) . . ? F4 F17 P2 83(3) . . ? F16 F17 P2 67.7(17) . . ? F9 F17 P2 78.4(19) . . ? F7 F17 F15 70(2) . . ? F4 F17 F15 117(3) . . ? F16 F17 F15 72(2) . . ? F9 F17 F15 94.0(19) . . ? P2 F17 F15 59.4(13) . . ? F1 F18 F12 32(2) . . ? F1 F18 F13 125(4) . . ? F12 F18 F13 117(2) . . ? F1 F18 P2 81(3) . . ? F12 F18 P2 58.4(14) . . ? F13 F18 P2 60.1(13) . . ? O2S O1S O1S 142(2) . 2_765 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C30 92.8(2) . . . . ? C26 Ir1 P1 C30 -118.7(3) . . . . ? C22 Ir1 P1 C30 -14.6(3) . . . . ? C23 Ir1 P1 C30 -112.7(13) . . . . ? C27 Ir1 P1 C30 -82.5(3) . . . . ? C1 Ir1 P1 C36 -26.2(3) . . . . ? C26 Ir1 P1 C36 122.3(3) . . . . ? C22 Ir1 P1 C36 -133.6(3) . . . . ? C23 Ir1 P1 C36 128.3(13) . . . . ? C27 Ir1 P1 C36 158.4(3) . . . . ? C1 Ir1 P1 C42 -152.6(3) . . . . ? C26 Ir1 P1 C42 -4.2(3) . . . . ? C22 Ir1 P1 C42 100.0(3) . . . . ? C23 Ir1 P1 C42 1.9(13) . . . . ? C27 Ir1 P1 C42 32.0(3) . . . . ? C3 N2 C1 N1 -0.9(5) . . . . ? C13 N2 C1 N1 161.1(4) . . . . ? C3 N2 C1 Ir1 176.1(4) . . . . ? C13 N2 C1 Ir1 -21.9(8) . . . . ? C2 N1 C1 N2 1.2(5) . . . . ? C4 N1 C1 N2 -163.0(4) . . . . ? C2 N1 C1 Ir1 -176.1(4) . . . . ? C4 N1 C1 Ir1 19.6(6) . . . . ? C26 Ir1 C1 N2 171.7(4) . . . . ? C22 Ir1 C1 N2 68.2(5) . . . . ? C23 Ir1 C1 N2 104.6(5) . . . . ? C27 Ir1 C1 N2 63(2) . . . . ? P1 Ir1 C1 N2 -78.3(5) . . . . ? C26 Ir1 C1 N1 -11.8(6) . . . . ? C22 Ir1 C1 N1 -115.3(4) . . . . ? C23 Ir1 C1 N1 -78.9(4) . . . . ? C27 Ir1 C1 N1 -120.2(18) . . . . ? P1 Ir1 C1 N1 98.2(4) . . . . ? C1 N1 C2 C3 -1.1(6) . . . . ? C4 N1 C2 C3 163.3(5) . . . . ? N1 C2 C3 N2 0.5(6) . . . . ? C1 N2 C3 C2 0.3(6) . . . . ? C13 N2 C3 C2 -162.8(5) . . . . ? C1 N1 C4 C5 93.5(6) . . . . ? C2 N1 C4 C5 -68.9(7) . . . . ? C1 N1 C4 C9 -89.3(6) . . . . ? C2 N1 C4 C9 108.3(6) . . . . ? C9 C4 C5 C6 6.3(8) . . . . ? N1 C4 C5 C6 -176.5(5) . . . . ? C9 C4 C5 C10 -172.2(5) . . . . ? N1 C4 C5 C10 5.0(8) . . . . ? C4 C5 C6 C7 -2.7(8) . . . . ? C10 C5 C6 C7 175.9(5) . . . . ? C5 C6 C7 C8 -1.5(8) . . . . ? C5 C6 C7 C11 -178.6(5) . . . . ? C6 C7 C8 C9 2.0(8) . . . . ? C11 C7 C8 C9 179.1(5) . . . . ? C7 C8 C9 C4 1.6(8) . . . . ? C7 C8 C9 C12 -177.6(5) . . . . ? C5 C4 C9 C8 -5.8(8) . . . . ? N1 C4 C9 C8 177.0(5) . . . . ? C5 C4 C9 C12 173.4(5) . . . . ? N1 C4 C9 C12 -3.8(8) . . . . ? C1 N2 C13 C18 102.2(6) . . . . ? C3 N2 C13 C18 -97.3(6) . . . . ? C1 N2 C13 C14 -81.3(6) . . . . ? C3 N2 C13 C14 79.2(6) . . . . ? C18 C13 C14 C15 -5.3(8) . . . . ? N2 C13 C14 C15 178.2(5) . . . . ? C18 C13 C14 C19 172.1(5) . . . . ? N2 C13 C14 C19 -4.5(7) . . . . ? C13 C14 C15 C16 1.8(8) . . . . ? C19 C14 C15 C16 -175.7(5) . . . . ? C14 C15 C16 C17 1.3(8) . . . . ? C14 C15 C16 C20 177.9(5) . . . . ? C15 C16 C17 C18 -1.1(8) . . . . ? C20 C16 C17 C18 -177.7(5) . . . . ? C14 C13 C18 C17 5.5(8) . . . . ? N2 C13 C18 C17 -178.2(5) . . . . ? C14 C13 C18 C21 -170.7(5) . . . . ? N2 C13 C18 C21 5.6(8) . . . . ? C16 C17 C18 C13 -2.3(8) . . . . ? C16 C17 C18 C21 174.1(5) . . . . ? C1 Ir1 C22 C23 82.2(3) . . . . ? C26 Ir1 C22 C23 -65.0(4) . . . . ? C27 Ir1 C22 C23 -98.5(4) . . . . ? P1 Ir1 C22 C23 -168.8(2) . . . . ? C1 Ir1 C22 C29 -157.2(4) . . . . ? C26 Ir1 C22 C29 55.6(5) . . . . ? C23 Ir1 C22 C29 120.7(6) . . . . ? C27 Ir1 C22 C29 22.2(4) . . . . ? P1 Ir1 C22 C29 -48.1(6) . . . . ? C29 C22 C23 C24 0.5(8) . . . . ? Ir1 C22 C23 C24 104.7(5) . . . . ? C29 C22 C23 Ir1 -104.2(5) . . . . ? C1 Ir1 C23 C22 -98.0(3) . . . . ? C26 Ir1 C23 C22 113.3(4) . . . . ? C27 Ir1 C23 C22 77.0(4) . . . . ? P1 Ir1 C23 C22 107.2(13) . . . . ? C1 Ir1 C23 C24 140.7(4) . . . . ? C26 Ir1 C23 C24 -7.9(4) . . . . ? C22 Ir1 C23 C24 -121.2(5) . . . . ? C27 Ir1 C23 C24 -44.2(4) . . . . ? P1 Ir1 C23 C24 -14.0(16) . . . . ? C22 C23 C24 C25 -92.4(7) . . . . ? Ir1 C23 C24 C25 -11.0(6) . . . . ? C23 C24 C25 C26 33.5(7) . . . . ? C24 C25 C26 C27 44.0(8) . . . . ? C24 C25 C26 Ir1 -39.6(6) . . . . ? C1 Ir1 C26 C27 -168.1(3) . . . . ? C22 Ir1 C26 C27 -65.2(4) . . . . ? C23 Ir1 C26 C27 -98.7(4) . . . . ? P1 Ir1 C26 C27 80.5(3) . . . . ? C1 Ir1 C26 C25 -44.1(6) . . . . ? C22 Ir1 C26 C25 58.8(4) . . . . ? C23 Ir1 C26 C25 25.3(4) . . . . ? C27 Ir1 C26 C25 124.0(6) . . . . ? P1 Ir1 C26 C25 -155.4(4) . . . . ? C25 C26 C27 C28 2.1(9) . . . . ? Ir1 C26 C27 C28 104.4(5) . . . . ? C25 C26 C27 Ir1 -102.3(5) . . . . ? C1 Ir1 C27 C26 118.1(19) . . . . ? C22 Ir1 C27 C26 113.2(4) . . . . ? C23 Ir1 C27 C26 76.8(4) . . . . ? P1 Ir1 C27 C26 -99.9(3) . . . . ? C1 Ir1 C27 C28 -1(2) . . . . ? C26 Ir1 C27 C28 -119.3(6) . . . . ? C22 Ir1 C27 C28 -6.2(5) . . . . ? C23 Ir1 C27 C28 -42.6(5) . . . . ? P1 Ir1 C27 C28 140.8(5) . . . . ? C26 C27 C28 C29 -91.4(7) . . . . ? Ir1 C27 C28 C29 -11.0(7) . . . . ? C23 C22 C29 C28 47.7(7) . . . . ? Ir1 C22 C29 C28 -35.5(6) . . . . ? C27 C28 C29 C22 30.7(8) . . . . ? C36 P1 C30 C35 -30.9(5) . . . . ? C42 P1 C30 C35 74.1(5) . . . . ? Ir1 P1 C30 C35 -163.2(4) . . . . ? C36 P1 C30 C31 148.1(5) . . . . ? C42 P1 C30 C31 -106.9(5) . . . . ? Ir1 P1 C30 C31 15.8(5) . . . . ? C35 C30 C31 C32 -0.4(9) . . . . ? P1 C30 C31 C32 -179.5(5) . . . . ? C30 C31 C32 C33 0.4(10) . . . . ? C31 C32 C33 C34 -0.4(11) . . . . ? C32 C33 C34 C35 0.4(11) . . . . ? C33 C34 C35 C30 -0.4(10) . . . . ? C31 C30 C35 C34 0.4(9) . . . . ? P1 C30 C35 C34 179.4(5) . . . . ? C30 P1 C36 C37 -86.2(5) . . . . ? C42 P1 C36 C37 168.2(5) . . . . ? Ir1 P1 C36 C37 36.1(6) . . . . ? C30 P1 C36 C41 91.6(5) . . . . ? C42 P1 C36 C41 -14.1(6) . . . . ? Ir1 P1 C36 C41 -146.2(4) . . . . ? C41 C36 C37 C38 -2.6(9) . . . . ? P1 C36 C37 C38 175.2(5) . . . . ? C36 C37 C38 C39 2.4(10) . . . . ? C37 C38 C39 C40 -1.4(10) . . . . ? C38 C39 C40 C41 0.7(10) . . . . ? C39 C40 C41 C36 -1.0(10) . . . . ? C37 C36 C41 C40 1.9(9) . . . . ? P1 C36 C41 C40 -175.9(5) . . . . ? C30 P1 C42 C47 -169.7(4) . . . . ? C36 P1 C42 C47 -64.8(5) . . . . ? Ir1 P1 C42 C47 72.3(5) . . . . ? C30 P1 C42 C43 11.2(5) . . . . ? C36 P1 C42 C43 116.1(5) . . . . ? Ir1 P1 C42 C43 -106.8(5) . . . . ? C47 C42 C43 C44 -0.3(9) . . . . ? P1 C42 C43 C44 178.7(5) . . . . ? C42 C43 C44 C45 0.5(9) . . . . ? C43 C44 C45 C46 -0.5(10) . . . . ? C44 C45 C46 C47 0.3(9) . . . . ? C43 C42 C47 C46 0.1(8) . . . . ? P1 C42 C47 C46 -178.9(4) . . . . ? C45 C46 C47 C42 -0.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.259 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.132 #===END data_5B _database_code_depnum_ccdc_archive 'CCDC 664297' #------------------------------------------------------ #---------------5B PBn3 complex------------------------ #------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H59 Cl2 F6 Ir N2 P2' _chemical_formula_weight 1139.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ir Ir -1.4442 7.9887 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8482(3) _cell_length_b 13.8711(3) _cell_length_c 17.1765(5) _cell_angle_alpha 80.229(2) _cell_angle_beta 76.144(2) _cell_angle_gamma 76.183(2) _cell_volume 2419.42(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10788 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'CUT NEEDLE' _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 2.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data is from scalepack ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49352 _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11028 _reflns_number_gt 8127 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+2.5106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11028 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.033536(17) 0.219182(13) 0.711998(10) 0.02454(6) Uani 1 1 d . . . P1 P 0.13627(11) 0.25377(8) 0.80649(6) 0.0251(3) Uani 1 1 d . B . P2 P 0.53171(12) 0.63704(9) 0.74555(7) 0.0339(3) Uani 1 1 d . . . F1 F 0.6762(3) 0.5862(4) 0.7419(3) 0.0740(18) Uani 0.848(8) 1 d P C . F2 F 0.5167(3) 0.6667(2) 0.83310(15) 0.0522(7) Uani 1 1 d . C . F3 F 0.5734(5) 0.7422(3) 0.70856(19) 0.0744(19) Uani 0.848(8) 1 d P C . F4 F 0.3827(4) 0.6953(3) 0.7474(3) 0.0704(16) Uani 0.848(8) 1 d P C . F5 F 0.5422(3) 0.6109(2) 0.65686(15) 0.0664(9) Uani 1 1 d . C . F6 F 0.4825(5) 0.5385(3) 0.7809(2) 0.0550(13) Uani 0.848(8) 1 d P C . N1 N 0.2460(3) 0.1948(2) 0.54915(19) 0.0259(8) Uani 1 1 d . . . N2 N 0.2003(3) 0.3448(2) 0.57997(19) 0.0254(8) Uani 1 1 d . . . C1 C 0.1743(4) 0.2518(3) 0.6100(2) 0.0221(9) Uani 1 1 d . . . C2 C 0.3101(4) 0.2525(3) 0.4854(2) 0.0312(10) Uani 1 1 d . . . H2 H 0.3651 0.2296 0.4373 0.037 Uiso 1 1 calc R . . C3 C 0.2806(4) 0.3457(3) 0.5041(2) 0.0296(10) Uani 1 1 d . . . H3 H 0.3092 0.4020 0.4717 0.035 Uiso 1 1 calc R . . C4 C 0.2632(4) 0.0885(3) 0.5450(2) 0.0260(10) Uani 1 1 d . . . C5 C 0.2023(4) 0.0599(3) 0.4922(2) 0.0275(10) Uani 1 1 d . . . C6 C 0.2181(4) -0.0419(3) 0.4892(2) 0.0319(11) Uani 1 1 d . . . H6 H 0.1758 -0.0632 0.4548 0.038 Uiso 1 1 calc R . . C7 C 0.2939(4) -0.1137(3) 0.5350(2) 0.0299(10) Uani 1 1 d . . . C8 C 0.3569(4) -0.0812(3) 0.5838(2) 0.0297(10) Uani 1 1 d . . . H8 H 0.4091 -0.1293 0.6153 0.036 Uiso 1 1 calc R . . C9 C 0.3459(4) 0.0198(3) 0.5880(2) 0.0256(10) Uani 1 1 d . . . C10 C 0.1213(4) 0.1345(3) 0.4401(2) 0.0351(11) Uani 1 1 d . . . H10A H 0.0787 0.1934 0.4681 0.053 Uiso 1 1 calc R . . H10B H 0.0555 0.1039 0.4292 0.053 Uiso 1 1 calc R . . H10C H 0.1773 0.1546 0.3889 0.053 Uiso 1 1 calc R . . C11 C 0.3095(5) -0.2242(3) 0.5301(3) 0.0439(12) Uani 1 1 d . . . H11A H 0.3464 -0.2634 0.5753 0.066 Uiso 1 1 calc R . . H11B H 0.3675 -0.2418 0.4790 0.066 Uiso 1 1 calc R . . H11C H 0.2245 -0.2390 0.5329 0.066 Uiso 1 1 calc R . . C12 C 0.4296(4) 0.0507(3) 0.6343(2) 0.0334(11) Uani 1 1 d . . . H12A H 0.4131 0.1238 0.6299 0.050 Uiso 1 1 calc R . . H12B H 0.5213 0.0248 0.6117 0.050 Uiso 1 1 calc R . . H12C H 0.4087 0.0234 0.6912 0.050 Uiso 1 1 calc R . . C13 C 0.1640(4) 0.4352(3) 0.6196(2) 0.0253(10) Uani 1 1 d . . . C14 C 0.2628(4) 0.4712(3) 0.6372(2) 0.0296(10) Uani 1 1 d . . . C15 C 0.2290(4) 0.5602(3) 0.6721(3) 0.0360(11) Uani 1 1 d . . . H15 H 0.2946 0.5839 0.6867 0.043 Uiso 1 1 calc R . . C16 C 0.1033(5) 0.6147(3) 0.6862(3) 0.0363(11) Uani 1 1 d . . . C17 C 0.0084(4) 0.5790(3) 0.6650(2) 0.0333(11) Uani 1 1 d . . . H17 H -0.0783 0.6164 0.6742 0.040 Uiso 1 1 calc R . . C18 C 0.0357(4) 0.4898(3) 0.6305(2) 0.0289(10) Uani 1 1 d . . . C19 C 0.4060(4) 0.4218(3) 0.6168(3) 0.0376(12) Uani 1 1 d . . . H19A H 0.4147 0.3500 0.6155 0.056 Uiso 1 1 calc R . . H19B H 0.4495 0.4315 0.6578 0.056 Uiso 1 1 calc R . . H19C H 0.4460 0.4519 0.5638 0.056 Uiso 1 1 calc R . . C20 C 0.0700(5) 0.7114(3) 0.7237(3) 0.0534(14) Uani 1 1 d . . . H20A H -0.0231 0.7397 0.7291 0.080 Uiso 0.50 1 calc PR . . H20B H 0.1195 0.7589 0.6891 0.080 Uiso 0.50 1 calc PR . . H20C H 0.0920 0.6980 0.7771 0.080 Uiso 0.50 1 calc PR . . H20D H 0.1487 0.7247 0.7345 0.080 Uiso 0.50 1 calc PR . . H20E H 0.0061 0.7055 0.7744 0.080 Uiso 0.50 1 calc PR . . H20F H 0.0336 0.7664 0.6864 0.080 Uiso 0.50 1 calc PR . . C21 C -0.0698(4) 0.4564(3) 0.6062(3) 0.0338(11) Uani 1 1 d . . . H21A H -0.0399 0.4389 0.5509 0.051 Uiso 1 1 calc R . . H21B H -0.1468 0.5107 0.6088 0.051 Uiso 1 1 calc R . . H21C H -0.0916 0.3979 0.6430 0.051 Uiso 1 1 calc R . . C22 C -0.0318(4) 0.1193(3) 0.6511(2) 0.0306(10) Uani 1 1 d . . . H22 H 0.0561 0.1042 0.6232 0.037 Uiso 1 1 calc R . . C23 C -0.1010(4) 0.2145(3) 0.6339(2) 0.0332(11) Uani 1 1 d . . . H23 H -0.0568 0.2591 0.5952 0.040 Uiso 1 1 calc R . . C24 C -0.2424(4) 0.2542(4) 0.6716(3) 0.0402(12) Uani 1 1 d . . . H24A H -0.2903 0.1994 0.6811 0.048 Uiso 1 1 calc R . . H24B H -0.2806 0.3074 0.6328 0.048 Uiso 1 1 calc R . . C25 C -0.2618(4) 0.2968(4) 0.7520(3) 0.0421(12) Uani 1 1 d . . . H25A H -0.2696 0.3702 0.7409 0.051 Uiso 1 1 calc R . . H25B H -0.3442 0.2838 0.7873 0.051 Uiso 1 1 calc R . . C26 C -0.1536(4) 0.2533(3) 0.7963(2) 0.0331(11) Uani 1 1 d . . . H26 H -0.1158 0.2982 0.8145 0.040 Uiso 1 1 calc R . . C27 C -0.1059(4) 0.1522(3) 0.8122(2) 0.0325(11) Uani 1 1 d . . . H27 H -0.0351 0.1314 0.8390 0.039 Uiso 1 1 calc R . . C28 C -0.1597(5) 0.0730(3) 0.7896(2) 0.0378(12) Uani 1 1 d . . . H28A H -0.2512 0.1003 0.7854 0.045 Uiso 1 1 calc R . . H28B H -0.1580 0.0156 0.8326 0.045 Uiso 1 1 calc R . . C29 C -0.0819(4) 0.0373(3) 0.7095(2) 0.0359(11) Uani 1 1 d . . . H29A H -0.0077 -0.0170 0.7199 0.043 Uiso 1 1 calc R . . H29B H -0.1376 0.0094 0.6851 0.043 Uiso 1 1 calc R . . C30 C 0.3140(4) 0.2402(3) 0.7766(2) 0.0308(10) Uani 1 1 d . . . H30A H 0.3502 0.1766 0.7528 0.037 Uiso 1 1 calc R . . H30B H 0.3327 0.2949 0.7333 0.037 Uiso 1 1 calc R . . C31 C 0.3859(4) 0.2411(3) 0.8406(2) 0.0275(10) Uani 1 1 d . . . C32 C 0.4037(4) 0.3297(3) 0.8594(3) 0.0380(11) Uani 1 1 d . . . H32 H 0.3701 0.3912 0.8305 0.046 Uiso 1 1 calc R . . C33 C 0.4689(5) 0.3306(5) 0.9191(3) 0.0576(16) Uani 1 1 d . . . H33 H 0.4792 0.3924 0.9309 0.069 Uiso 1 1 calc R . . C34 C 0.5183(5) 0.2436(5) 0.9608(3) 0.0612(17) Uani 1 1 d . . . H34 H 0.5621 0.2444 1.0023 0.073 Uiso 1 1 calc R . . C35 C 0.5049(5) 0.1540(4) 0.9430(3) 0.0549(15) Uani 1 1 d . . . H35 H 0.5413 0.0930 0.9715 0.066 Uiso 1 1 calc R . . C36 C 0.4383(4) 0.1524(4) 0.8834(3) 0.0416(12) Uani 1 1 d . . . H36 H 0.4285 0.0903 0.8718 0.050 Uiso 1 1 calc R . . C37 C 0.0879(4) 0.3805(3) 0.8402(2) 0.0303(10) Uani 1 1 d . . . H37A H 0.1590 0.3909 0.8627 0.036 Uiso 1 1 calc R A 1 H37B H 0.0809 0.4302 0.7919 0.036 Uiso 1 1 calc R A 1 C38 C -0.0392(11) 0.4036(8) 0.9032(5) 0.026(4) Uiso 0.63(2) 1 d P B 1 C39 C -0.1497(9) 0.4606(9) 0.8777(7) 0.035(4) Uiso 0.63(2) 1 d P B 1 H39 H -0.1460 0.4846 0.8222 0.042 Uiso 0.63(2) 1 calc PR B 1 C40 C -0.2656(8) 0.4823(7) 0.9337(6) 0.038(2) Uiso 0.63(2) 1 d P B 1 H40 H -0.3407 0.5220 0.9163 0.045 Uiso 0.63(2) 1 calc PR B 1 C41 C -0.2721(9) 0.4471(6) 1.0132(5) 0.036(2) Uiso 0.63(2) 1 d P B 1 H41 H -0.3539 0.4569 1.0496 0.043 Uiso 0.63(2) 1 calc PR B 1 C42 C -0.1639(11) 0.3981(5) 1.0418(5) 0.035(2) Uiso 0.63(2) 1 d P B 1 H42 H -0.1679 0.3793 1.0980 0.042 Uiso 0.63(2) 1 calc PR B 1 C43 C -0.0463(11) 0.3764(6) 0.9853(4) 0.031(2) Uiso 0.63(2) 1 d P B 1 H43 H 0.0301 0.3422 1.0040 0.038 Uiso 0.63(2) 1 calc PR B 1 C44 C 0.1194(4) 0.1705(3) 0.9016(2) 0.0260(10) Uani 1 1 d . . . H44A H 0.1700 0.1884 0.9359 0.031 Uiso 1 1 calc R B . H44B H 0.0271 0.1846 0.9296 0.031 Uiso 1 1 calc R . . C45 C 0.1613(4) 0.0585(3) 0.8973(2) 0.0249(9) Uani 1 1 d . B . C46 C 0.1936(4) 0.0151(3) 0.8253(2) 0.0319(11) Uani 1 1 d . . . H46 H 0.1893 0.0568 0.7756 0.038 Uiso 1 1 calc R B . C47 C 0.2315(4) -0.0864(3) 0.8253(3) 0.0358(11) Uani 1 1 d . B . H47 H 0.2534 -0.1141 0.7756 0.043 Uiso 1 1 calc R . . C48 C 0.2382(4) -0.1487(3) 0.8961(3) 0.0359(11) Uani 1 1 d . . . H48 H 0.2647 -0.2191 0.8957 0.043 Uiso 1 1 calc R B . C49 C 0.2056(4) -0.1074(3) 0.9680(3) 0.0349(11) Uani 1 1 d . B . H49 H 0.2093 -0.1498 1.0174 0.042 Uiso 1 1 calc R . . C50 C 0.1678(4) -0.0047(3) 0.9689(2) 0.0278(10) Uani 1 1 d . . . H50 H 0.1462 0.0227 1.0187 0.033 Uiso 1 1 calc R B . C51 C 0.6972(6) 0.7973(4) 0.8438(3) 0.0604(16) Uani 1 1 d . D . H51A H 0.6260 0.7725 0.8838 0.072 Uiso 1 1 calc R . . H51B H 0.7367 0.7469 0.8056 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.6310(8) 0.9122(2) 0.7894(9) 0.083(3) Uani 0.72(2) 1 d P . . Cl2 Cl 0.81382(16) 0.80910(10) 0.89370(8) 0.0679(4) Uani 1 1 d . . . F1A F 0.631(2) 0.5363(17) 0.7878(15) 0.069(8) Uiso 0.152(8) 1 d P C 1 F4A F 0.452(3) 0.7076(17) 0.7027(16) 0.065(8) Uiso 0.152(8) 1 d P C 1 Cl1A Cl 0.6011(9) 0.9086(7) 0.8275(7) 0.054(2) Uiso 0.28(2) 1 d P D 1 F3A F 0.6618(18) 0.6798(16) 0.7074(10) 0.033(6) Uiso 0.152(8) 1 d P C 1 F6A F 0.421(2) 0.5760(17) 0.7841(13) 0.038(6) Uiso 0.152(8) 1 d P C 1 C39A C -0.2502(10) 0.4651(10) 0.9559(9) 0.055(6) Uiso 0.37(2) 1 d PG B 2 H39A H -0.3351 0.4936 0.9469 0.066 Uiso 0.37(2) 1 calc PR B 2 C40A C -0.2295(13) 0.4401(8) 1.0343(7) 0.040(5) Uiso 0.37(2) 1 d PG B 2 H40A H -0.3002 0.4515 1.0788 0.048 Uiso 0.37(2) 1 calc PR B 2 C41A C -0.1052(16) 0.3984(7) 1.0474(5) 0.033(4) Uiso 0.37(2) 1 d PG B 2 H41A H -0.0910 0.3813 1.1010 0.040 Uiso 0.37(2) 1 calc PR B 2 C43A C -0.0016(12) 0.3817(8) 0.9822(6) 0.032(4) Uiso 0.37(2) 1 d PG B 2 H43A H 0.0833 0.3532 0.9912 0.039 Uiso 0.37(2) 1 calc PR B 2 C42A C -0.0223(11) 0.4067(10) 0.9038(5) 0.026(8) Uiso 0.37(2) 1 d PG B 2 C38A C -0.1466(12) 0.4484(11) 0.8907(6) 0.037(7) Uiso 0.37(2) 1 d PG B 2 H38A H -0.1607 0.4654 0.8371 0.044 Uiso 0.37(2) 1 calc PR 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 Ir1 0.02486(10) 0.02880(10) 0.01900(8) 0.00027(6) -0.00299(6) -0.00745(7) P1 0.0269(7) 0.0264(6) 0.0214(6) -0.0012(5) -0.0039(5) -0.0063(5) P2 0.0379(8) 0.0389(7) 0.0252(6) -0.0022(5) -0.0027(5) -0.0136(6) F1 0.027(2) 0.114(4) 0.079(3) -0.035(3) -0.008(2) 0.004(2) F2 0.0589(19) 0.0681(19) 0.0340(15) -0.0140(14) -0.0012(13) -0.0247(16) F3 0.144(5) 0.061(3) 0.039(2) 0.0086(18) -0.027(2) -0.062(3) F4 0.052(3) 0.080(3) 0.079(3) -0.044(2) -0.028(3) 0.026(2) F5 0.077(2) 0.103(2) 0.0333(16) -0.0236(16) 0.0074(15) -0.053(2) F6 0.084(4) 0.038(2) 0.045(2) 0.0034(18) -0.006(2) -0.029(3) N1 0.026(2) 0.0253(19) 0.0210(18) 0.0017(15) -0.0016(15) -0.0025(16) N2 0.025(2) 0.025(2) 0.0218(18) 0.0014(15) -0.0015(15) -0.0026(16) C1 0.016(2) 0.030(2) 0.019(2) 0.0014(18) -0.0058(17) -0.0038(19) C2 0.026(3) 0.038(3) 0.024(2) 0.003(2) -0.0011(19) -0.004(2) C3 0.027(3) 0.029(3) 0.024(2) 0.0034(19) 0.0025(19) -0.003(2) C4 0.027(2) 0.027(2) 0.018(2) -0.0002(18) 0.0023(18) -0.003(2) C5 0.024(2) 0.036(3) 0.021(2) -0.0031(19) -0.0003(18) -0.008(2) C6 0.030(3) 0.042(3) 0.025(2) -0.008(2) -0.001(2) -0.011(2) C7 0.033(3) 0.031(3) 0.024(2) -0.0038(19) -0.004(2) -0.005(2) C8 0.026(3) 0.030(3) 0.026(2) 0.0028(19) -0.0032(19) 0.000(2) C9 0.024(2) 0.030(2) 0.017(2) 0.0015(18) 0.0007(18) 0.000(2) C10 0.039(3) 0.039(3) 0.025(2) 0.000(2) -0.012(2) -0.001(2) C11 0.056(3) 0.032(3) 0.044(3) -0.002(2) -0.014(3) -0.008(2) C12 0.031(3) 0.037(3) 0.028(2) -0.004(2) -0.005(2) -0.002(2) C13 0.029(3) 0.022(2) 0.022(2) 0.0064(17) -0.0075(19) -0.006(2) C14 0.030(3) 0.029(2) 0.026(2) 0.0091(19) -0.004(2) -0.010(2) C15 0.037(3) 0.032(3) 0.039(3) 0.005(2) -0.011(2) -0.011(2) C16 0.042(3) 0.029(3) 0.035(3) 0.002(2) -0.009(2) -0.005(2) C17 0.033(3) 0.030(3) 0.029(2) 0.008(2) -0.005(2) 0.000(2) C18 0.030(3) 0.029(2) 0.022(2) 0.0065(19) -0.0028(19) -0.006(2) C19 0.030(3) 0.037(3) 0.042(3) 0.008(2) -0.003(2) -0.014(2) C20 0.064(4) 0.041(3) 0.053(3) -0.017(3) -0.016(3) 0.004(3) C21 0.028(3) 0.032(3) 0.038(3) 0.003(2) -0.011(2) 0.001(2) C22 0.025(3) 0.047(3) 0.025(2) -0.007(2) -0.0032(19) -0.019(2) C23 0.030(3) 0.049(3) 0.026(2) 0.002(2) -0.007(2) -0.022(2) C24 0.029(3) 0.049(3) 0.045(3) 0.001(2) -0.014(2) -0.010(2) C25 0.029(3) 0.052(3) 0.042(3) -0.009(2) 0.002(2) -0.009(2) C26 0.025(3) 0.046(3) 0.030(3) -0.008(2) 0.006(2) -0.018(2) C27 0.028(3) 0.045(3) 0.026(2) -0.002(2) -0.001(2) -0.017(2) C28 0.047(3) 0.040(3) 0.029(2) 0.004(2) -0.001(2) -0.024(2) C29 0.041(3) 0.043(3) 0.027(2) -0.004(2) -0.001(2) -0.021(2) C30 0.028(3) 0.034(3) 0.029(2) -0.005(2) -0.001(2) -0.008(2) C31 0.026(2) 0.032(3) 0.023(2) -0.0029(19) -0.0009(19) -0.007(2) C32 0.024(3) 0.037(3) 0.051(3) -0.012(2) -0.007(2) 0.000(2) C33 0.029(3) 0.077(4) 0.074(4) -0.045(4) -0.012(3) 0.002(3) C34 0.037(3) 0.115(6) 0.037(3) -0.029(4) -0.008(3) -0.012(4) C35 0.033(3) 0.073(4) 0.048(3) 0.020(3) -0.016(3) -0.003(3) C36 0.035(3) 0.041(3) 0.049(3) 0.005(2) -0.012(2) -0.012(2) C37 0.031(3) 0.026(2) 0.034(3) -0.0036(19) -0.005(2) -0.007(2) C44 0.029(2) 0.027(2) 0.022(2) -0.0048(18) -0.0037(19) -0.005(2) C45 0.024(2) 0.023(2) 0.024(2) 0.0015(18) -0.0037(18) -0.0027(19) C46 0.042(3) 0.032(3) 0.021(2) 0.0004(19) -0.008(2) -0.006(2) C47 0.046(3) 0.028(3) 0.031(3) -0.007(2) -0.005(2) -0.002(2) C48 0.038(3) 0.024(2) 0.040(3) 0.000(2) -0.004(2) -0.002(2) C49 0.035(3) 0.035(3) 0.025(2) 0.008(2) -0.002(2) -0.002(2) C50 0.030(3) 0.031(3) 0.018(2) -0.0006(18) -0.0032(18) -0.001(2) C51 0.079(4) 0.052(3) 0.057(4) -0.009(3) -0.013(3) -0.027(3) Cl1 0.071(3) 0.0564(15) 0.141(7) -0.010(2) -0.059(4) -0.0161(14) Cl2 0.1001(13) 0.0595(9) 0.0540(9) -0.0060(7) -0.0353(8) -0.0169(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.094(4) . ? Ir1 C26 2.193(4) . ? Ir1 C22 2.198(4) . ? Ir1 C23 2.224(4) . ? Ir1 C27 2.235(4) . ? Ir1 P1 2.3436(11) . ? P1 C44 1.831(4) . ? P1 C30 1.845(4) . ? P1 C37 1.860(4) . ? P2 F4A 1.38(2) . ? P2 F1 1.549(4) . ? P2 F6 1.560(3) . ? P2 F6A 1.58(2) . ? P2 F2 1.587(3) . ? P2 F5 1.597(3) . ? P2 F3A 1.612(17) . ? P2 F3 1.612(3) . ? P2 F4 1.621(4) . ? P2 F1A 1.72(2) . ? F1 F1A 1.06(2) . ? F1 F3A 1.323(19) . ? F3 F3A 1.127(19) . ? F3 F4A 1.53(2) . ? F4 F4A 0.96(2) . ? F4 F6A 1.66(2) . ? F5 F4A 1.65(3) . ? F6 F6A 0.74(2) . ? F6 F1A 1.64(2) . ? N1 C1 1.385(5) . ? N1 C2 1.388(5) . ? N1 C4 1.453(5) . ? N2 C1 1.374(5) . ? N2 C3 1.383(5) . ? N2 C13 1.454(5) . ? C2 C3 1.331(5) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.389(5) . ? C4 C5 1.396(5) . ? C5 C6 1.389(6) . ? C5 C10 1.507(6) . ? C6 C7 1.392(6) . ? C6 H6 0.9500 . ? C7 C8 1.387(6) . ? C7 C11 1.516(6) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C9 C12 1.512(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.397(6) . ? C13 C18 1.402(6) . ? C14 C15 1.396(6) . ? C14 C19 1.523(6) . ? C15 C16 1.379(6) . ? C15 H15 0.9500 . ? C16 C17 1.386(6) . ? C16 C20 1.514(6) . ? C17 C18 1.399(6) . ? C17 H17 0.9500 . ? C18 C21 1.499(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.376(6) . ? C22 C29 1.498(5) . ? C22 H22 0.9500 . ? C23 C24 1.523(6) . ? C23 H23 0.9500 . ? C24 C25 1.543(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.501(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.379(6) . ? C26 H26 0.9500 . ? C27 C28 1.502(6) . ? C27 H27 0.9500 . ? C28 C29 1.526(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.496(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.389(6) . ? C31 C36 1.391(6) . ? C32 C33 1.381(7) . ? C32 H32 0.9500 . ? C33 C34 1.356(7) . ? C33 H33 0.9500 . ? C34 C35 1.377(7) . ? C34 H34 0.9500 . ? C35 C36 1.394(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42A 1.434(9) . ? C37 C38 1.538(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C43 1.386(9) . ? C38 C39 1.390(12) . ? C39 C40 1.390(10) . ? C39 H39 0.9500 . ? C40 C41 1.361(12) . ? C40 H40 0.9500 . ? C41 C42 1.365(11) . ? C41 H41 0.9500 . ? C42 C43 1.408(10) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.520(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.390(5) . ? C45 C46 1.399(5) . ? C46 C47 1.370(5) . ? C46 H46 0.9500 . ? C47 C48 1.374(6) . ? C47 H47 0.9500 . ? C48 C49 1.384(6) . ? C48 H48 0.9500 . ? C49 C50 1.387(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 Cl2 1.740(5) . ? C51 Cl1 1.788(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? Cl1 Cl1A 0.656(8) . ? C39A C40A 1.3900 . ? C39A C38A 1.3900 . ? C39A H39A 0.9500 . ? C40A C41A 1.3900 . ? C40A H40A 0.9500 . ? C41A C43A 1.3900 . ? C41A H41A 0.9500 . ? C43A C42A 1.3900 . ? C43A H43A 0.9500 . ? C42A C38A 1.3900 . ? C38A H38A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C26 153.73(16) . . ? C1 Ir1 C22 92.63(15) . . ? C26 Ir1 C22 93.60(16) . . ? C1 Ir1 C23 90.62(15) . . ? C26 Ir1 C23 79.64(16) . . ? C22 Ir1 C23 36.26(15) . . ? C1 Ir1 C27 167.84(15) . . ? C26 Ir1 C27 36.27(15) . . ? C22 Ir1 C27 77.51(15) . . ? C23 Ir1 C27 85.60(15) . . ? C1 Ir1 P1 96.10(11) . . ? C26 Ir1 P1 89.39(12) . . ? C22 Ir1 P1 153.84(12) . . ? C23 Ir1 P1 166.68(12) . . ? C27 Ir1 P1 90.02(11) . . ? C44 P1 C30 101.49(19) . . ? C44 P1 C37 103.18(18) . . ? C30 P1 C37 100.85(19) . . ? C44 P1 Ir1 113.99(13) . . ? C30 P1 Ir1 116.29(13) . . ? C37 P1 Ir1 118.64(15) . . ? F4A P2 F1 141.5(12) . . ? F4A P2 F6 115.5(10) . . ? F1 P2 F6 93.7(3) . . ? F4A P2 F6A 92.6(12) . . ? F1 P2 F6A 120.4(8) . . ? F6 P2 F6A 27.1(7) . . ? F4A P2 F2 110.6(11) . . ? F1 P2 F2 91.73(19) . . ? F6 P2 F2 91.97(17) . . ? F6A P2 F2 87.0(8) . . ? F4A P2 F5 67.1(11) . . ? F1 P2 F5 90.32(19) . . ? F6 P2 F5 88.92(17) . . ? F6A P2 F5 92.8(8) . . ? F2 P2 F5 177.71(19) . . ? F4A P2 F3A 96.3(12) . . ? F1 P2 F3A 49.4(7) . . ? F6 P2 F3A 142.6(8) . . ? F6A P2 F3A 169.6(11) . . ? F2 P2 F3A 94.8(6) . . ? F5 P2 F3A 85.7(6) . . ? F4A P2 F3 61.1(10) . . ? F1 P2 F3 89.9(2) . . ? F6 P2 F3 176.4(3) . . ? F6A P2 F3 149.5(8) . . ? F2 P2 F3 88.32(16) . . ? F5 P2 F3 90.66(16) . . ? F3A P2 F3 40.9(7) . . ? F4A P2 F4 36.3(11) . . ? F1 P2 F4 177.2(3) . . ? F6 P2 F4 89.1(2) . . ? F6A P2 F4 62.4(8) . . ? F2 P2 F4 88.26(18) . . ? F5 P2 F4 89.64(19) . . ? F3A P2 F4 127.8(8) . . ? F3 P2 F4 87.3(3) . . ? F4A P2 F1A 170.6(12) . . ? F1 P2 F1A 37.6(8) . . ? F6 P2 F1A 59.6(8) . . ? F6A P2 F1A 84.6(11) . . ? F2 P2 F1A 78.3(8) . . ? F5 P2 F1A 104.0(8) . . ? F3A P2 F1A 85.8(11) . . ? F3 P2 F1A 123.9(9) . . ? F4 P2 F1A 145.0(9) . . ? F1A F1 F3A 143.5(15) . . ? F1A F1 P2 79.8(13) . . ? F3A F1 P2 67.7(8) . . ? F3A F3 F4A 113.2(13) . . ? F3A F3 P2 69.5(9) . . ? F4A F3 P2 51.9(9) . . ? F4A F4 P2 58.0(15) . . ? F4A F4 F6A 106.8(16) . . ? P2 F4 F6A 57.7(7) . . ? P2 F5 F4A 50.1(8) . . ? F6A F6 P2 78.2(18) . . ? F6A F6 F1A 136(2) . . ? P2 F6 F1A 65.0(8) . . ? C1 N1 C2 111.2(3) . . ? C1 N1 C4 129.8(3) . . ? C2 N1 C4 119.0(3) . . ? C1 N2 C3 112.3(3) . . ? C1 N2 C13 128.8(3) . . ? C3 N2 C13 118.7(3) . . ? N2 C1 N1 102.2(3) . . ? N2 C1 Ir1 125.9(3) . . ? N1 C1 Ir1 131.0(3) . . ? C3 C2 N1 107.4(4) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 106.8(3) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C9 C4 C5 122.2(4) . . ? C9 C4 N1 119.9(4) . . ? C5 C4 N1 117.7(4) . . ? C6 C5 C4 117.4(4) . . ? C6 C5 C10 120.0(4) . . ? C4 C5 C10 122.6(4) . . ? C5 C6 C7 122.2(4) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C11 121.0(4) . . ? C6 C7 C11 120.9(4) . . ? C7 C8 C9 122.0(4) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C4 C9 C8 117.8(4) . . ? C4 C9 C12 122.8(4) . . ? C8 C9 C12 119.3(4) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.6(4) . . ? C14 C13 N2 117.9(4) . . ? C18 C13 N2 120.1(4) . . ? C15 C14 C13 118.1(4) . . ? C15 C14 C19 118.0(4) . . ? C13 C14 C19 123.8(4) . . ? C16 C15 C14 122.0(4) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.4(4) . . ? C15 C16 C20 120.7(4) . . ? C17 C16 C20 120.9(4) . . ? C16 C17 C18 122.4(4) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 117.4(4) . . ? C17 C18 C21 120.1(4) . . ? C13 C18 C21 122.5(4) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C20 H20D 109.5 . . ? H20A C20 H20D 141.1 . . ? H20B C20 H20D 56.3 . . ? H20C C20 H20D 56.3 . . ? C16 C20 H20E 109.5 . . ? H20A C20 H20E 56.3 . . ? H20B C20 H20E 141.1 . . ? H20C C20 H20E 56.3 . . ? H20D C20 H20E 109.5 . . ? C16 C20 H20F 109.5 . . ? H20A C20 H20F 56.3 . . ? H20B C20 H20F 56.3 . . ? H20C C20 H20F 141.1 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C29 126.2(4) . . ? C23 C22 Ir1 72.9(2) . . ? C29 C22 Ir1 111.7(3) . . ? C23 C22 H22 116.9 . . ? C29 C22 H22 116.9 . . ? Ir1 C22 H22 85.2 . . ? C22 C23 C24 125.4(4) . . ? C22 C23 Ir1 70.8(2) . . ? C24 C23 Ir1 112.5(3) . . ? C22 C23 H23 117.3 . . ? C24 C23 H23 117.3 . . ? Ir1 C23 H23 86.5 . . ? C23 C24 C25 113.9(4) . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 113.6(4) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 124.0(4) . . ? C27 C26 Ir1 73.5(2) . . ? C25 C26 Ir1 111.2(3) . . ? C27 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? Ir1 C26 H26 85.2 . . ? C26 C27 C28 123.6(4) . . ? C26 C27 Ir1 70.2(2) . . ? C28 C27 Ir1 114.7(3) . . ? C26 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? Ir1 C27 H27 85.2 . . ? C27 C28 C29 111.4(3) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C22 C29 C28 112.6(3) . . ? C22 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C22 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 P1 117.7(3) . . ? C31 C30 H30A 107.9 . . ? P1 C30 H30A 107.9 . . ? C31 C30 H30B 107.9 . . ? P1 C30 H30B 107.9 . . ? H30A C30 H30B 107.2 . . ? C32 C31 C36 117.5(4) . . ? C32 C31 C30 121.7(4) . . ? C36 C31 C30 120.9(4) . . ? C33 C32 C31 121.8(5) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C34 C33 C32 120.1(5) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.1(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.4(4) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C42A C37 C38 6.6(8) . . ? C42A C37 P1 121.9(6) . . ? C38 C37 P1 117.5(5) . . ? C42A C37 H37A 101.4 . . ? C38 C37 H37A 107.9 . . ? P1 C37 H37A 107.9 . . ? C42A C37 H37B 109.5 . . ? C38 C37 H37B 107.9 . . ? P1 C37 H37B 107.9 . . ? H37A C37 H37B 107.2 . . ? C43 C38 C39 118.1(9) . . ? C43 C38 C37 122.7(8) . . ? C39 C38 C37 119.0(7) . . ? C40 C39 C38 119.9(11) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.4(10) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 121.6(7) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C41 C42 C43 117.8(7) . . ? C41 C42 H42 121.1 . . ? C43 C42 H42 121.1 . . ? C38 C43 C42 121.7(8) . . ? C38 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C45 C44 P1 117.8(3) . . ? C45 C44 H44A 107.9 . . ? P1 C44 H44A 107.9 . . ? C45 C44 H44B 107.9 . . ? P1 C44 H44B 107.9 . . ? H44A C44 H44B 107.2 . . ? C50 C45 C46 118.0(4) . . ? C50 C45 C44 118.2(3) . . ? C46 C45 C44 123.8(4) . . ? C47 C46 C45 121.1(4) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C48 120.9(4) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C49 118.9(4) . . ? C47 C48 H48 120.5 . . ? C49 C48 H48 120.5 . . ? C48 C49 C50 120.7(4) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 C45 120.4(4) . . ? C49 C50 H50 119.8 . . ? C45 C50 H50 119.8 . . ? Cl2 C51 Cl1 113.0(3) . . ? Cl2 C51 H51A 109.0 . . ? Cl1 C51 H51A 109.0 . . ? Cl2 C51 H51B 109.0 . . ? Cl1 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? Cl1A Cl1 C51 68.7(10) . . ? F1 F1A F6 112.6(18) . . ? F1 F1A P2 62.6(12) . . ? F6 F1A P2 55.4(7) . . ? F4 F4A P2 85.7(17) . . ? F4 F4A F3 125(2) . . ? P2 F4A F3 67.0(11) . . ? F4 F4A F5 117.7(19) . . ? P2 F4A F5 62.8(10) . . ? F3 F4A F5 91.4(14) . . ? F3 F3A F1 131.4(15) . . ? F3 F3A P2 69.6(9) . . ? F1 F3A P2 62.8(7) . . ? F6 F6A P2 74.7(18) . . ? F6 F6A F4 134(2) . . ? P2 F6A F4 59.9(8) . . ? C40A C39A C38A 120.0 . . ? C40A C39A H39A 120.0 . . ? C38A C39A H39A 120.0 . . ? C41A C40A C39A 120.0 . . ? C41A C40A H40A 120.0 . . ? C39A C40A H40A 120.0 . . ? C40A C41A C43A 120.0 . . ? C40A C41A H41A 120.0 . . ? C43A C41A H41A 120.0 . . ? C41A C43A C42A 120.0 . . ? C41A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C38A C42A C43A 120.0 . . ? C38A C42A C37 123.5(7) . . ? C43A C42A C37 116.4(7) . . ? C42A C38A C39A 120.0 . . ? C42A C38A H38A 120.0 . . ? C39A C38A H38A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C44 -143.37(18) . . . . ? C26 Ir1 P1 C44 62.38(19) . . . . ? C22 Ir1 P1 C44 -34.6(3) . . . . ? C23 Ir1 P1 C44 96.7(5) . . . . ? C27 Ir1 P1 C44 26.11(19) . . . . ? C1 Ir1 P1 C30 -25.78(19) . . . . ? C26 Ir1 P1 C30 180.0(2) . . . . ? C22 Ir1 P1 C30 83.0(3) . . . . ? C23 Ir1 P1 C30 -145.7(5) . . . . ? C27 Ir1 P1 C30 143.70(19) . . . . ? C1 Ir1 P1 C37 94.81(18) . . . . ? C26 Ir1 P1 C37 -59.44(19) . . . . ? C22 Ir1 P1 C37 -156.4(3) . . . . ? C23 Ir1 P1 C37 -25.1(5) . . . . ? C27 Ir1 P1 C37 -95.71(19) . . . . ? F4A P2 F1 F1A -164.7(19) . . . . ? F6 P2 F1 F1A -24.0(13) . . . . ? F6A P2 F1 F1A -19.5(15) . . . . ? F2 P2 F1 F1A 68.1(12) . . . . ? F5 P2 F1 F1A -112.9(12) . . . . ? F3A P2 F1 F1A 163.0(15) . . . . ? F3 P2 F1 F1A 156.4(12) . . . . ? F4 P2 F1 F1A 158(4) . . . . ? F4A P2 F1 F3A 32.3(18) . . . . ? F6 P2 F1 F3A 173.0(8) . . . . ? F6A P2 F1 F3A 177.5(12) . . . . ? F2 P2 F1 F3A -94.9(8) . . . . ? F5 P2 F1 F3A 84.1(8) . . . . ? F3 P2 F1 F3A -6.6(8) . . . . ? F4 P2 F1 F3A -5(4) . . . . ? F1A P2 F1 F3A -163.0(15) . . . . ? F4A P2 F3 F3A -145.9(16) . . . . ? F1 P2 F3 F3A 7.6(9) . . . . ? F6 P2 F3 F3A -166(3) . . . . ? F6A P2 F3 F3A -179.4(18) . . . . ? F2 P2 F3 F3A 99.4(9) . . . . ? F5 P2 F3 F3A -82.7(9) . . . . ? F4 P2 F3 F3A -172.3(9) . . . . ? F1A P2 F3 F3A 24.7(13) . . . . ? F1 P2 F3 F4A 153.5(13) . . . . ? F6 P2 F3 F4A -20(3) . . . . ? F6A P2 F3 F4A -33(2) . . . . ? F2 P2 F3 F4A -114.8(13) . . . . ? F5 P2 F3 F4A 63.2(13) . . . . ? F3A P2 F3 F4A 145.9(16) . . . . ? F4 P2 F3 F4A -26.4(13) . . . . ? F1A P2 F3 F4A 170.6(15) . . . . ? F1 P2 F4 F4A 40(5) . . . . ? F6 P2 F4 F4A -138.5(17) . . . . ? F6A P2 F4 F4A -142.9(19) . . . . ? F2 P2 F4 F4A 129.5(17) . . . . ? F5 P2 F4 F4A -49.6(17) . . . . ? F3A P2 F4 F4A 34.7(18) . . . . ? F3 P2 F4 F4A 41.1(17) . . . . ? F1A P2 F4 F4A -164(2) . . . . ? F4A P2 F4 F6A 142.9(19) . . . . ? F1 P2 F4 F6A -177(100) . . . . ? F6 P2 F4 F6A 4.4(9) . . . . ? F2 P2 F4 F6A -87.6(9) . . . . ? F5 P2 F4 F6A 93.4(9) . . . . ? F3A P2 F4 F6A 177.7(11) . . . . ? F3 P2 F4 F6A -176.0(9) . . . . ? F1A P2 F4 F6A -21.0(16) . . . . ? F1 P2 F5 F4A -147.9(11) . . . . ? F6 P2 F5 F4A 118.4(11) . . . . ? F6A P2 F5 F4A 91.6(13) . . . . ? F2 P2 F5 F4A 6(4) . . . . ? F3A P2 F5 F4A -98.6(13) . . . . ? F3 P2 F5 F4A -58.0(11) . . . . ? F4 P2 F5 F4A 29.3(11) . . . . ? F1A P2 F5 F4A 176.7(13) . . . . ? F4A P2 F6 F6A -34(2) . . . . ? F1 P2 F6 F6A 171.4(19) . . . . ? F2 P2 F6 F6A 79.6(19) . . . . ? F5 P2 F6 F6A -98.3(19) . . . . ? F3A P2 F6 F6A -180(2) . . . . ? F3 P2 F6 F6A -15(4) . . . . ? F4 P2 F6 F6A -8.7(19) . . . . ? F1A P2 F6 F6A 155(2) . . . . ? F4A P2 F6 F1A 170.8(14) . . . . ? F1 P2 F6 F1A 16.7(9) . . . . ? F6A P2 F6 F1A -155(2) . . . . ? F2 P2 F6 F1A -75.2(9) . . . . ? F5 P2 F6 F1A 106.9(9) . . . . ? F3A P2 F6 F1A 25.4(13) . . . . ? F3 P2 F6 F1A -170(3) . . . . ? F4 P2 F6 F1A -163.4(9) . . . . ? C3 N2 C1 N1 1.5(4) . . . . ? C13 N2 C1 N1 -173.0(4) . . . . ? C3 N2 C1 Ir1 -168.6(3) . . . . ? C13 N2 C1 Ir1 17.0(6) . . . . ? C2 N1 C1 N2 -0.8(4) . . . . ? C4 N1 C1 N2 177.8(4) . . . . ? C2 N1 C1 Ir1 168.6(3) . . . . ? C4 N1 C1 Ir1 -12.8(6) . . . . ? C26 Ir1 C1 N2 32.8(6) . . . . ? C22 Ir1 C1 N2 136.4(3) . . . . ? C23 Ir1 C1 N2 100.2(3) . . . . ? C27 Ir1 C1 N2 171.8(6) . . . . ? P1 Ir1 C1 N2 -68.3(3) . . . . ? C26 Ir1 C1 N1 -134.3(4) . . . . ? C22 Ir1 C1 N1 -30.7(4) . . . . ? C23 Ir1 C1 N1 -66.9(4) . . . . ? C27 Ir1 C1 N1 4.7(10) . . . . ? P1 Ir1 C1 N1 124.6(3) . . . . ? C1 N1 C2 C3 -0.2(5) . . . . ? C4 N1 C2 C3 -179.0(4) . . . . ? N1 C2 C3 N2 1.1(5) . . . . ? C1 N2 C3 C2 -1.7(5) . . . . ? C13 N2 C3 C2 173.4(4) . . . . ? C1 N1 C4 C9 -76.5(5) . . . . ? C2 N1 C4 C9 102.0(4) . . . . ? C1 N1 C4 C5 108.2(5) . . . . ? C2 N1 C4 C5 -73.3(5) . . . . ? C9 C4 C5 C6 5.5(6) . . . . ? N1 C4 C5 C6 -179.3(3) . . . . ? C9 C4 C5 C10 -174.8(4) . . . . ? N1 C4 C5 C10 0.4(5) . . . . ? C4 C5 C6 C7 -1.6(6) . . . . ? C10 C5 C6 C7 178.8(4) . . . . ? C5 C6 C7 C8 -1.2(6) . . . . ? C5 C6 C7 C11 -179.8(4) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? C11 C7 C8 C9 178.8(4) . . . . ? C5 C4 C9 C8 -6.5(6) . . . . ? N1 C4 C9 C8 178.4(3) . . . . ? C5 C4 C9 C12 169.5(4) . . . . ? N1 C4 C9 C12 -5.5(6) . . . . ? C7 C8 C9 C4 3.6(6) . . . . ? C7 C8 C9 C12 -172.6(4) . . . . ? C1 N2 C13 C14 112.2(4) . . . . ? C3 N2 C13 C14 -61.9(5) . . . . ? C1 N2 C13 C18 -75.1(5) . . . . ? C3 N2 C13 C18 110.8(4) . . . . ? C18 C13 C14 C15 4.8(6) . . . . ? N2 C13 C14 C15 177.4(3) . . . . ? C18 C13 C14 C19 -172.0(4) . . . . ? N2 C13 C14 C19 0.6(6) . . . . ? C13 C14 C15 C16 -2.8(6) . . . . ? C19 C14 C15 C16 174.2(4) . . . . ? C14 C15 C16 C17 0.3(6) . . . . ? C14 C15 C16 C20 -179.6(4) . . . . ? C15 C16 C17 C18 0.4(6) . . . . ? C20 C16 C17 C18 -179.7(4) . . . . ? C16 C17 C18 C13 1.5(6) . . . . ? C16 C17 C18 C21 -177.9(4) . . . . ? C14 C13 C18 C17 -4.2(6) . . . . ? N2 C13 C18 C17 -176.6(3) . . . . ? C14 C13 C18 C21 175.3(4) . . . . ? N2 C13 C18 C21 2.8(6) . . . . ? C1 Ir1 C22 C23 -87.4(3) . . . . ? C26 Ir1 C22 C23 67.0(3) . . . . ? C27 Ir1 C22 C23 99.7(3) . . . . ? P1 Ir1 C22 C23 163.0(2) . . . . ? C1 Ir1 C22 C29 149.6(3) . . . . ? C26 Ir1 C22 C29 -55.9(3) . . . . ? C23 Ir1 C22 C29 -122.9(4) . . . . ? C27 Ir1 C22 C29 -23.2(3) . . . . ? P1 Ir1 C22 C29 40.1(5) . . . . ? C29 C22 C23 C24 0.1(7) . . . . ? Ir1 C22 C23 C24 -104.5(4) . . . . ? C29 C22 C23 Ir1 104.7(4) . . . . ? C1 Ir1 C23 C22 93.6(3) . . . . ? C26 Ir1 C23 C22 -110.9(3) . . . . ? C27 Ir1 C23 C22 -74.8(3) . . . . ? P1 Ir1 C23 C22 -145.9(4) . . . . ? C1 Ir1 C23 C24 -145.0(3) . . . . ? C26 Ir1 C23 C24 10.4(3) . . . . ? C22 Ir1 C23 C24 121.3(4) . . . . ? C27 Ir1 C23 C24 46.5(3) . . . . ? P1 Ir1 C23 C24 -24.6(7) . . . . ? C22 C23 C24 C25 86.5(5) . . . . ? Ir1 C23 C24 C25 4.6(5) . . . . ? C23 C24 C25 C26 -25.4(6) . . . . ? C24 C25 C26 C27 -50.1(6) . . . . ? C24 C25 C26 Ir1 33.9(5) . . . . ? C1 Ir1 C26 C27 166.5(3) . . . . ? C22 Ir1 C26 C27 63.1(3) . . . . ? C23 Ir1 C26 C27 96.7(3) . . . . ? P1 Ir1 C26 C27 -90.9(2) . . . . ? C1 Ir1 C26 C25 45.8(5) . . . . ? C22 Ir1 C26 C25 -57.5(3) . . . . ? C23 Ir1 C26 C25 -23.9(3) . . . . ? C27 Ir1 C26 C25 -120.7(4) . . . . ? P1 Ir1 C26 C25 148.5(3) . . . . ? C25 C26 C27 C28 -2.3(6) . . . . ? Ir1 C26 C27 C28 -107.1(4) . . . . ? C25 C26 C27 Ir1 104.8(4) . . . . ? C1 Ir1 C27 C26 -150.6(7) . . . . ? C22 Ir1 C27 C26 -114.2(3) . . . . ? C23 Ir1 C27 C26 -78.5(3) . . . . ? P1 Ir1 C27 C26 88.9(2) . . . . ? C1 Ir1 C27 C28 -31.8(10) . . . . ? C26 Ir1 C27 C28 118.8(5) . . . . ? C22 Ir1 C27 C28 4.6(3) . . . . ? C23 Ir1 C27 C28 40.4(3) . . . . ? P1 Ir1 C27 C28 -152.2(3) . . . . ? C26 C27 C28 C29 96.2(5) . . . . ? Ir1 C27 C28 C29 14.4(5) . . . . ? C23 C22 C29 C28 -45.3(6) . . . . ? Ir1 C22 C29 C28 38.9(5) . . . . ? C27 C28 C29 C22 -34.7(6) . . . . ? C44 P1 C30 C31 -43.5(3) . . . . ? C37 P1 C30 C31 62.5(3) . . . . ? Ir1 P1 C30 C31 -167.8(3) . . . . ? P1 C30 C31 C32 -87.5(4) . . . . ? P1 C30 C31 C36 92.9(4) . . . . ? C36 C31 C32 C33 -1.0(6) . . . . ? C30 C31 C32 C33 179.3(4) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C33 C34 C35 C36 -1.4(8) . . . . ? C32 C31 C36 C35 0.4(6) . . . . ? C30 C31 C36 C35 -179.9(4) . . . . ? C34 C35 C36 C31 0.7(7) . . . . ? C44 P1 C37 C42A -43.1(7) . . . . ? C30 P1 C37 C42A -147.8(6) . . . . ? Ir1 P1 C37 C42A 84.0(6) . . . . ? C44 P1 C37 C38 -48.8(5) . . . . ? C30 P1 C37 C38 -153.5(5) . . . . ? Ir1 P1 C37 C38 78.3(5) . . . . ? C42A C37 C38 C43 -50(7) . . . . ? P1 C37 C38 C43 82.9(10) . . . . ? C42A C37 C38 C39 125(7) . . . . ? P1 C37 C38 C39 -102.0(8) . . . . ? C43 C38 C39 C40 -4.7(12) . . . . ? C37 C38 C39 C40 180.0(8) . . . . ? C38 C39 C40 C41 -0.8(11) . . . . ? C39 C40 C41 C42 6.4(11) . . . . ? C40 C41 C42 C43 -5.9(11) . . . . ? C39 C38 C43 C42 5.1(12) . . . . ? C37 C38 C43 C42 -179.8(8) . . . . ? C41 C42 C43 C38 0.1(11) . . . . ? C30 P1 C44 C45 -71.4(3) . . . . ? C37 P1 C44 C45 -175.5(3) . . . . ? Ir1 P1 C44 C45 54.5(3) . . . . ? P1 C44 C45 C50 170.3(3) . . . . ? P1 C44 C45 C46 -9.7(5) . . . . ? C50 C45 C46 C47 -0.4(6) . . . . ? C44 C45 C46 C47 179.6(4) . . . . ? C45 C46 C47 C48 0.3(7) . . . . ? C46 C47 C48 C49 0.2(7) . . . . ? C47 C48 C49 C50 -0.5(7) . . . . ? C48 C49 C50 C45 0.4(6) . . . . ? C46 C45 C50 C49 0.1(6) . . . . ? C44 C45 C50 C49 -179.9(4) . . . . ? Cl2 C51 Cl1 Cl1A -84.4(10) . . . . ? F3A F1 F1A F6 52(3) . . . . ? P2 F1 F1A F6 24.7(12) . . . . ? F3A F1 F1A P2 27(2) . . . . ? F6A F6 F1A F1 -64(3) . . . . ? P2 F6 F1A F1 -26.8(13) . . . . ? F6A F6 F1A P2 -37(3) . . . . ? F4A P2 F1A F1 90(8) . . . . ? F6 P2 F1A F1 152.0(14) . . . . ? F6A P2 F1A F1 163.2(13) . . . . ? F2 P2 F1A F1 -108.7(11) . . . . ? F5 P2 F1A F1 71.7(11) . . . . ? F3A P2 F1A F1 -12.9(11) . . . . ? F3 P2 F1A F1 -28.8(15) . . . . ? F4 P2 F1A F1 -178.2(3) . . . . ? F4A P2 F1A F6 -62(8) . . . . ? F1 P2 F1A F6 -152.0(14) . . . . ? F6A P2 F1A F6 11.2(9) . . . . ? F2 P2 F1A F6 99.3(6) . . . . ? F5 P2 F1A F6 -80.3(6) . . . . ? F3A P2 F1A F6 -164.9(8) . . . . ? F3 P2 F1A F6 179.2(3) . . . . ? F4 P2 F1A F6 29.8(15) . . . . ? F6A F4 F4A P2 -32.1(15) . . . . ? P2 F4 F4A F3 -57.8(19) . . . . ? F6A F4 F4A F3 -90(2) . . . . ? P2 F4 F4A F5 56.1(15) . . . . ? F6A F4 F4A F5 24(2) . . . . ? F1 P2 F4A F4 -177.2(4) . . . . ? F6 P2 F4A F4 47.2(18) . . . . ? F6A P2 F4A F4 32.3(16) . . . . ? F2 P2 F4A F4 -55.5(16) . . . . ? F5 P2 F4A F4 124.3(16) . . . . ? F3A P2 F4A F4 -153.1(14) . . . . ? F3 P2 F4A F4 -131.4(19) . . . . ? F1A P2 F4A F4 105(8) . . . . ? F1 P2 F4A F3 -45.8(18) . . . . ? F6 P2 F4A F3 178.6(3) . . . . ? F6A P2 F4A F3 163.7(11) . . . . ? F2 P2 F4A F3 75.9(9) . . . . ? F5 P2 F4A F3 -104.3(9) . . . . ? F3A P2 F4A F3 -21.7(10) . . . . ? F4 P2 F4A F3 131.4(19) . . . . ? F1A P2 F4A F3 -124(8) . . . . ? F1 P2 F4A F5 58.6(15) . . . . ? F6 P2 F4A F5 -77.0(8) . . . . ? F6A P2 F4A F5 -92.0(9) . . . . ? F2 P2 F4A F5 -179.76(18) . . . . ? F3A P2 F4A F5 82.7(7) . . . . ? F3 P2 F4A F5 104.3(9) . . . . ? F4 P2 F4A F5 -124.3(16) . . . . ? F1A P2 F4A F5 -20(8) . . . . ? F3A F3 F4A F4 101(3) . . . . ? P2 F3 F4A F4 66(2) . . . . ? F3A F3 F4A P2 34.9(15) . . . . ? F3A F3 F4A F5 -24.7(16) . . . . ? P2 F3 F4A F5 -59.5(8) . . . . ? P2 F5 F4A F4 -69(2) . . . . ? P2 F5 F4A F3 63.2(9) . . . . ? F4A F3 F3A F1 -41(2) . . . . ? P2 F3 F3A F1 -12.0(14) . . . . ? F4A F3 F3A P2 -28.7(13) . . . . ? F1A F1 F3A F3 -16(3) . . . . ? P2 F1 F3A F3 12.6(15) . . . . ? F1A F1 F3A P2 -29(2) . . . . ? F4A P2 F3A F3 29.6(13) . . . . ? F1 P2 F3A F3 -169.9(12) . . . . ? F6 P2 F3A F3 178.6(3) . . . . ? F6A P2 F3A F3 178(5) . . . . ? F2 P2 F3A F3 -81.8(7) . . . . ? F5 P2 F3A F3 96.0(7) . . . . ? F4 P2 F3A F3 9.7(11) . . . . ? F1A P2 F3A F3 -159.7(11) . . . . ? F4A P2 F3A F1 -160.5(12) . . . . ? F6 P2 F3A F1 -11.5(13) . . . . ? F6A P2 F3A F1 -12(6) . . . . ? F2 P2 F3A F1 88.1(5) . . . . ? F5 P2 F3A F1 -94.1(5) . . . . ? F3 P2 F3A F1 169.9(12) . . . . ? F4 P2 F3A F1 179.7(3) . . . . ? F1A P2 F3A F1 10.3(9) . . . . ? F1A F6 F6A P2 34(3) . . . . ? P2 F6 F6A F4 12(2) . . . . ? F1A F6 F6A F4 45(5) . . . . ? F4A P2 F6A F6 149(2) . . . . ? F1 P2 F6A F6 -10(2) . . . . ? F2 P2 F6A F6 -100.2(17) . . . . ? F5 P2 F6A F6 82.1(17) . . . . ? F3A P2 F6A F6 1(7) . . . . ? F3 P2 F6A F6 178.2(5) . . . . ? F4 P2 F6A F6 170(2) . . . . ? F1A P2 F6A F6 -21.7(18) . . . . ? F4A P2 F6A F4 -20.9(11) . . . . ? F1 P2 F6A F4 179.9(2) . . . . ? F6 P2 F6A F4 -170(2) . . . . ? F2 P2 F6A F4 89.6(5) . . . . ? F5 P2 F6A F4 -88.1(5) . . . . ? F3A P2 F6A F4 -170(5) . . . . ? F3 P2 F6A F4 8.0(18) . . . . ? F1A P2 F6A F4 168.1(9) . . . . ? F4A F4 F6A F6 19(4) . . . . ? P2 F4 F6A F6 -13(3) . . . . ? F4A F4 F6A P2 32.3(17) . . . . ? C38A C39A C40A C41A 0.0 . . . . ? C39A C40A C41A C43A 0.0 . . . . ? C40A C41A C43A C42A 0.0 . . . . ? C41A C43A C42A C38A 0.0 . . . . ? C41A C43A C42A C37 -175.7(11) . . . . ? C38 C37 C42A C38A -41(7) . . . . ? P1 C37 C42A C38A -91.0(8) . . . . ? C38 C37 C42A C43A 134(7) . . . . ? P1 C37 C42A C43A 84.5(8) . . . . ? C43A C42A C38A C39A 0.0 . . . . ? C37 C42A C38A C39A 175.4(11) . . . . ? C40A C39A C38A C42A 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.092 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.132