# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address _publ_author_footnote J.Fawcett ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; . D.Harding ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; . E.Hope ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; . K.Singh ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; . G.Solan ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; . _publ_contact_author_name 'Hope, Eric G' _publ_contact_author_email egh1@le.ac.uk _publ_section_title ; Stabilisation of iridium(III) fluorides complexes with NHCs ; _publ_contact_author_address ; Department of Chemistry University of Leicester Leicester LE1 7RH United Kingdom ; _publ_contact_author_fax '[+44] (0)116 252 3789' _publ_contact_author_phone '[+44] (0)116 252 2108' # Attachment '- Hope_5.cif' data_04171 _database_code_depnum_ccdc_archive 'CCDC 723140' _publ_section_title_footnote # remove if not required . #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H47 Ir N2 P)+ (B F4)-' _chemical_formula_sum 'C43 H47 B F4 Ir N2 P' _chemical_formula_weight 901.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.9712(16) _cell_length_b 15.996(2) _cell_length_c 19.958(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3821.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 2.743 _cell_measurement_theta_max 23.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 3.589 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5806 _exptl_absorpt_correction_T_max 0.7622 _exptl_absorpt_process_details ; absorption correction based on 16498 reflections(SADABS);Rint 0.057 before correction and 0.039 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32446 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8344 _reflns_number_gt 7445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(5) _refine_ls_number_reflns 8344 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 0.256039(15) 0.589349(10) 0.957188(8) 0.02090(5) Uani 1 1 d . . . P1 P 0.22156(10) 0.62845(7) 0.84519(6) 0.0233(3) Uani 1 1 d . . . N1 N 0.4174(3) 0.4417(2) 0.9333(2) 0.0282(10) Uani 1 1 d . . . N2 N 0.2525(4) 0.4029(2) 0.90497(16) 0.0287(8) Uani 1 1 d . . . C1 C 0.3087(4) 0.4696(3) 0.9324(2) 0.0233(11) Uani 1 1 d . . . C2 C 0.4250(5) 0.3623(3) 0.9047(3) 0.0393(15) Uani 1 1 d . . . H2 H 0.4902 0.3317 0.8981 0.047 Uiso 1 1 calc R . . C3 C 0.3235(4) 0.3386(3) 0.8889(3) 0.0388(14) Uani 1 1 d . . . H3 H 0.3033 0.2875 0.8702 0.047 Uiso 1 1 calc R . . C4 C 0.1673(4) 0.7053(3) 0.9831(3) 0.0281(13) Uani 1 1 d . . . C5 C 0.2828(4) 0.7184(3) 0.9880(2) 0.0260(13) Uani 1 1 d . . . C6 C 0.3445(4) 0.7242(3) 1.0560(2) 0.0362(13) Uani 1 1 d . . . H6A H 0.4042 0.7650 1.0526 0.043 Uiso 1 1 calc R . . H6B H 0.2927 0.7433 1.0901 0.043 Uiso 1 1 calc R . . C7 C 0.3934(5) 0.6405(4) 1.0772(3) 0.0402(16) Uani 1 1 d . . . H7A H 0.4672 0.6350 1.0575 0.048 Uiso 1 1 calc R . . H7B H 0.4024 0.6405 1.1255 0.048 Uiso 1 1 calc R . . C8 C 0.3246(4) 0.5654(4) 1.0575(2) 0.0327(15) Uani 1 1 d . . . C9 C 0.2077(4) 0.5614(3) 1.0614(3) 0.0325(15) Uani 1 1 d . . . C10 C 0.1335(5) 0.6278(4) 1.0925(3) 0.0380(16) Uani 1 1 d . . . H10A H 0.1758 0.6584 1.1260 0.046 Uiso 1 1 calc R . . H10B H 0.0712 0.6009 1.1150 0.046 Uiso 1 1 calc R . . C11 C 0.0885(4) 0.6893(3) 1.0405(3) 0.0359(12) Uani 1 1 d . . . H11A H 0.0188 0.6676 1.0227 0.043 Uiso 1 1 calc R . . H11B H 0.0722 0.7419 1.0625 0.043 Uiso 1 1 calc R . . C12 C 0.0723(4) 0.6208(3) 0.8258(2) 0.0248(11) Uani 1 1 d . . . C13 C 0.0031(4) 0.5776(3) 0.8680(3) 0.0290(13) Uani 1 1 d . . . H13 H 0.0318 0.5549 0.9073 0.035 Uiso 1 1 calc R . . C14 C -0.1096(4) 0.5672(3) 0.8528(3) 0.0334(13) Uani 1 1 d . . . H14 H -0.1555 0.5368 0.8814 0.040 Uiso 1 1 calc R . . C15 C -0.1522(4) 0.6018(3) 0.7958(3) 0.0396(14) Uani 1 1 d . . . H15 H -0.2275 0.5951 0.7857 0.048 Uiso 1 1 calc R . . C16 C -0.0849(4) 0.6465(3) 0.7531(3) 0.0359(14) Uani 1 1 d . . . H16 H -0.1149 0.6704 0.7146 0.043 Uiso 1 1 calc R . . C17 C 0.0275(4) 0.6560(3) 0.7672(3) 0.0349(13) Uani 1 1 d . . . H17 H 0.0733 0.6857 0.7380 0.042 Uiso 1 1 calc R . . C18 C 0.2572(5) 0.7362(3) 0.82118(19) 0.0261(10) Uani 1 1 d . . . C19 C 0.1795(4) 0.8014(3) 0.8269(2) 0.0304(12) Uani 1 1 d . . . H19 H 0.1085 0.7908 0.8438 0.036 Uiso 1 1 calc R . . C20 C 0.2086(5) 0.8817(3) 0.8072(3) 0.0397(16) Uani 1 1 d . . . H20 H 0.1563 0.9245 0.8104 0.048 Uiso 1 1 calc R . . C21 C 0.3133(5) 0.8987(4) 0.7833(3) 0.0428(15) Uani 1 1 d . . . H21 H 0.3328 0.9529 0.7712 0.051 Uiso 1 1 calc R . . C22 C 0.3891(5) 0.8350(4) 0.7775(3) 0.0399(14) Uani 1 1 d . . . H22 H 0.4596 0.8458 0.7599 0.048 Uiso 1 1 calc R . . C23 C 0.3618(4) 0.7551(3) 0.7973(2) 0.0328(13) Uani 1 1 d . . . H23 H 0.4152 0.7130 0.7945 0.039 Uiso 1 1 calc R . . C24 C 0.2918(4) 0.5686(3) 0.7800(2) 0.0294(12) Uani 1 1 d . . . H24A H 0.3712 0.5796 0.7842 0.035 Uiso 1 1 calc R . . H24B H 0.2809 0.5099 0.7903 0.035 Uiso 1 1 calc R . . C25 C 0.2611(5) 0.5808(3) 0.70669(19) 0.0392(12) Uani 1 1 d . . . H25A H 0.1836 0.5678 0.7003 0.059 Uiso 1 1 calc R . . H25B H 0.3059 0.5445 0.6794 0.059 Uiso 1 1 calc R . . H25C H 0.2745 0.6379 0.6941 0.059 Uiso 1 1 calc R . . C26 C 0.1314(4) 0.3884(3) 0.9048(3) 0.0254(12) Uani 1 1 d . . . C27 C 0.0780(4) 0.3730(3) 0.9652(3) 0.0313(12) Uani 1 1 d . . . C28 C -0.0365(4) 0.3606(3) 0.9648(3) 0.0405(14) Uani 1 1 d . . . H28 H -0.0736 0.3545 1.0055 0.049 Uiso 1 1 calc R . . C29 C -0.0970(5) 0.3568(3) 0.9065(3) 0.0391(15) Uani 1 1 d . . . C30 C -0.0398(5) 0.3653(3) 0.8479(3) 0.0408(15) Uani 1 1 d . . . H30 H -0.0796 0.3607 0.8080 0.049 Uiso 1 1 calc R . . C31 C 0.0744(4) 0.3805(3) 0.8439(3) 0.0319(12) Uani 1 1 d . . . C32 C 0.1276(5) 0.3869(4) 0.7765(3) 0.0550(18) Uani 1 1 d . . . H32A H 0.1182 0.4425 0.7594 0.082 Uiso 1 1 calc R . . H32B H 0.0931 0.3477 0.7465 0.082 Uiso 1 1 calc R . . H32C H 0.2059 0.3745 0.7801 0.082 Uiso 1 1 calc R . . C33 C -0.2223(5) 0.3434(4) 0.9067(3) 0.073(2) Uani 1 1 d . . . H33A H -0.2461 0.3276 0.9508 0.109 Uiso 1 1 calc R . . H33B H -0.2411 0.3000 0.8755 0.109 Uiso 1 1 calc R . . H33C H -0.2590 0.3943 0.8938 0.109 Uiso 1 1 calc R . . C34 C 0.1419(5) 0.3577(3) 1.0292(3) 0.0583(19) Uani 1 1 d . . . H34A H 0.1568 0.2991 1.0338 0.087 Uiso 1 1 calc R . . H34B H 0.0983 0.3765 1.0667 0.087 Uiso 1 1 calc R . . H34C H 0.2112 0.3879 1.0279 0.087 Uiso 1 1 calc R . . C35 C 0.5134(4) 0.4770(3) 0.9674(3) 0.0271(11) Uani 1 1 d . . . C36 C 0.5733(4) 0.5432(3) 0.9405(2) 0.0253(11) Uani 1 1 d . . . C37 C 0.6719(4) 0.5664(3) 0.9713(2) 0.0306(12) Uani 1 1 d . . . H37 H 0.7102 0.6127 0.9550 0.037 Uiso 1 1 calc R . . C38 C 0.7164(4) 0.5233(3) 1.0257(2) 0.0286(12) Uani 1 1 d . . . C39 C 0.6527(4) 0.4598(3) 1.0521(3) 0.0317(12) Uani 1 1 d . . . H39 H 0.6789 0.4322 1.0900 0.038 Uiso 1 1 calc R . . C40 C 0.5515(4) 0.4348(3) 1.0252(2) 0.0287(12) Uani 1 1 d . . . C41 C 0.5335(4) 0.5863(4) 0.8786(2) 0.0332(13) Uani 1 1 d . . . H41A H 0.5224 0.5459 0.8436 0.050 Uiso 1 1 calc R . . H41B H 0.5883 0.6265 0.8645 0.050 Uiso 1 1 calc R . . H41C H 0.4643 0.6144 0.8877 0.050 Uiso 1 1 calc R . . C42 C 0.8301(4) 0.5434(3) 1.0513(3) 0.0369(13) Uani 1 1 d . . . H42A H 0.8515 0.5028 1.0843 0.055 Uiso 1 1 calc R . . H42B H 0.8296 0.5980 1.0712 0.055 Uiso 1 1 calc R . . H42C H 0.8824 0.5424 1.0148 0.055 Uiso 1 1 calc R . . C43 C 0.4893(4) 0.3636(3) 1.0575(3) 0.0442(15) Uani 1 1 d . . . H43A H 0.5327 0.3133 1.0539 0.066 Uiso 1 1 calc R . . H43B H 0.4189 0.3559 1.0353 0.066 Uiso 1 1 calc R . . H43C H 0.4766 0.3761 1.1039 0.066 Uiso 1 1 calc R . . B1 B 0.5873(5) 0.6568(4) 0.6926(4) 0.0360(16) Uani 1 1 d . . . F1 F 0.6190(3) 0.7071(2) 0.74540(16) 0.0571(10) Uani 1 1 d . . . F2 F 0.5046(3) 0.69729(19) 0.65689(16) 0.0517(9) Uani 1 1 d . . . F3 F 0.5497(3) 0.5817(2) 0.71521(18) 0.0640(10) Uani 1 1 d . . . F4 F 0.6801(3) 0.6459(2) 0.65123(18) 0.0643(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02343(8) 0.02104(8) 0.01822(8) 0.00011(7) 0.00034(11) 0.00014(11) P1 0.0254(8) 0.0248(6) 0.0198(6) 0.0006(5) -0.0004(5) 0.0000(5) N1 0.028(2) 0.026(2) 0.031(2) 0.0005(19) 0.0011(19) 0.0031(18) N2 0.0268(19) 0.0241(18) 0.035(2) -0.0011(16) -0.002(2) -0.004(3) C1 0.026(3) 0.024(3) 0.020(3) 0.001(2) 0.000(2) -0.003(2) C2 0.029(3) 0.024(3) 0.065(5) -0.011(3) 0.001(3) 0.008(2) C3 0.040(3) 0.027(3) 0.049(4) -0.009(3) 0.000(3) 0.008(3) C4 0.031(3) 0.018(3) 0.036(3) -0.008(2) 0.010(2) -0.001(2) C5 0.042(3) 0.014(2) 0.021(3) -0.0052(19) -0.007(2) 0.005(2) C6 0.040(3) 0.039(3) 0.029(3) -0.006(3) 0.000(2) -0.012(3) C7 0.035(3) 0.062(4) 0.023(3) -0.012(3) -0.006(3) 0.006(3) C8 0.039(3) 0.052(4) 0.008(3) 0.002(2) -0.001(2) 0.007(3) C9 0.050(3) 0.028(3) 0.019(3) 0.007(2) 0.010(2) 0.002(2) C10 0.033(3) 0.049(4) 0.032(4) 0.002(3) 0.005(3) -0.006(3) C11 0.039(3) 0.036(3) 0.033(3) -0.005(3) 0.001(3) 0.003(2) C12 0.025(3) 0.026(3) 0.023(3) -0.005(2) -0.004(2) 0.003(2) C13 0.033(3) 0.029(3) 0.025(3) -0.003(3) 0.000(2) 0.003(3) C14 0.031(3) 0.024(3) 0.045(4) -0.003(2) 0.007(3) -0.002(2) C15 0.027(3) 0.043(4) 0.049(4) -0.014(3) -0.004(3) 0.001(3) C16 0.038(3) 0.038(3) 0.032(3) -0.001(3) -0.016(3) 0.000(3) C17 0.038(3) 0.038(3) 0.029(3) 0.003(3) -0.004(2) -0.004(3) C18 0.029(3) 0.030(2) 0.019(2) 0.0053(18) -0.003(3) 0.005(3) C19 0.039(3) 0.032(3) 0.020(3) -0.001(2) -0.001(2) 0.000(2) C20 0.060(4) 0.025(3) 0.034(3) 0.002(2) -0.012(3) 0.007(3) C21 0.063(4) 0.030(3) 0.036(4) 0.010(3) -0.003(3) -0.014(3) C22 0.045(4) 0.048(4) 0.027(3) 0.006(3) 0.001(3) -0.018(3) C23 0.039(3) 0.036(3) 0.024(3) 0.001(2) -0.006(2) -0.006(3) C24 0.037(3) 0.031(3) 0.021(3) 0.000(2) 0.000(2) 0.000(2) C25 0.047(3) 0.051(3) 0.020(2) -0.006(2) -0.003(3) -0.001(4) C26 0.028(3) 0.016(3) 0.032(3) -0.006(2) -0.003(2) 0.000(2) C27 0.040(3) 0.026(3) 0.028(3) -0.003(2) 0.000(3) -0.004(2) C28 0.042(3) 0.031(3) 0.048(4) -0.010(3) 0.016(3) -0.011(2) C29 0.033(3) 0.027(3) 0.057(4) -0.002(3) 0.002(3) -0.003(3) C30 0.042(3) 0.031(3) 0.050(4) -0.001(3) -0.025(3) -0.006(3) C31 0.043(3) 0.021(3) 0.031(3) -0.002(2) -0.004(3) -0.003(2) C32 0.076(4) 0.057(4) 0.033(4) -0.008(3) -0.004(3) -0.030(4) C33 0.035(4) 0.061(4) 0.122(6) -0.016(4) 0.004(4) -0.009(3) C34 0.082(5) 0.046(4) 0.047(4) 0.016(3) -0.024(4) -0.034(3) C35 0.025(3) 0.023(3) 0.032(3) 0.000(2) 0.000(2) 0.006(2) C36 0.030(3) 0.024(3) 0.022(3) -0.004(2) 0.003(2) 0.005(2) C37 0.032(3) 0.029(3) 0.032(3) -0.001(2) 0.006(2) -0.001(2) C38 0.029(3) 0.032(3) 0.025(3) -0.003(2) 0.002(2) 0.004(2) C39 0.034(3) 0.034(3) 0.027(3) 0.005(2) -0.005(2) 0.007(2) C40 0.033(3) 0.026(3) 0.028(3) 0.005(2) 0.002(2) 0.003(2) C41 0.028(3) 0.038(3) 0.034(3) 0.006(3) -0.001(2) -0.002(3) C42 0.035(3) 0.042(3) 0.034(3) 0.000(3) -0.003(3) 0.002(2) C43 0.036(3) 0.043(3) 0.053(4) 0.014(3) -0.006(3) 0.001(3) B1 0.031(4) 0.035(4) 0.042(4) 0.012(3) 0.014(3) 0.009(3) F1 0.058(2) 0.066(3) 0.046(2) -0.006(2) -0.0050(18) 0.008(2) F2 0.057(2) 0.046(2) 0.052(2) 0.0135(17) -0.0168(18) -0.0024(17) F3 0.064(2) 0.045(2) 0.083(3) 0.030(2) 0.026(2) 0.011(2) F4 0.073(2) 0.046(2) 0.074(3) -0.0006(19) 0.042(2) 0.0090(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.077(5) . ? Ir1 C5 2.177(5) . ? Ir1 C8 2.197(5) . ? Ir1 C4 2.200(5) . ? Ir1 C9 2.204(5) . ? Ir1 P1 2.3575(12) . ? P1 C24 1.821(4) . ? P1 C12 1.832(5) . ? P1 C18 1.839(4) . ? N1 C1 1.375(5) . ? N1 C2 1.396(6) . ? N1 C35 1.450(6) . ? N2 C3 1.373(6) . ? N2 C1 1.374(5) . ? N2 C26 1.468(7) . ? C2 C3 1.312(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.402(7) . ? C4 C11 1.505(7) . ? C5 C6 1.549(6) . ? C6 C7 1.520(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.510(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.402(7) . ? C9 C10 1.518(7) . ? C10 C11 1.528(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.367(6) . ? C12 C17 1.405(6) . ? C13 C14 1.393(6) . ? C13 H13 0.9300 . ? C14 C15 1.365(7) . ? C14 H14 0.9300 . ? C15 C16 1.373(7) . ? C15 H15 0.9300 . ? C16 C17 1.383(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.373(7) . ? C18 C19 1.403(6) . ? C19 C20 1.388(7) . ? C19 H19 0.9300 . ? C20 C21 1.368(7) . ? C20 H20 0.9300 . ? C21 C22 1.369(8) . ? C21 H21 0.9300 . ? C22 C23 1.379(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.521(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.386(7) . ? C26 C31 1.399(7) . ? C27 C28 1.385(6) . ? C27 C34 1.510(7) . ? C28 C29 1.371(8) . ? C28 H28 0.9300 . ? C29 C30 1.364(7) . ? C29 C33 1.515(7) . ? C30 C31 1.391(7) . ? C30 H30 0.9300 . ? C31 C32 1.492(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.387(6) . ? C35 C40 1.411(6) . ? C36 C37 1.382(6) . ? C36 C41 1.493(6) . ? C37 C38 1.392(6) . ? C37 H37 0.9300 . ? C38 C39 1.375(6) . ? C38 C42 1.488(6) . ? C39 C40 1.384(6) . ? C39 H39 0.9300 . ? C40 C43 1.506(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? B1 F3 1.360(7) . ? B1 F1 1.379(7) . ? B1 F2 1.382(7) . ? B1 F4 1.395(6) . ? 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 C5 153.78(18) . . ? C1 Ir1 C8 86.73(19) . . ? C5 Ir1 C8 81.6(2) . . ? C1 Ir1 C4 168.74(17) . . ? C5 Ir1 C4 37.36(18) . . ? C8 Ir1 C4 96.5(2) . . ? C1 Ir1 C9 96.77(19) . . ? C5 Ir1 C9 87.97(19) . . ? C8 Ir1 C9 37.16(17) . . ? C4 Ir1 C9 79.75(19) . . ? C1 Ir1 P1 94.12(13) . . ? C5 Ir1 P1 92.39(13) . . ? C8 Ir1 P1 167.30(15) . . ? C4 Ir1 P1 85.11(14) . . ? C9 Ir1 P1 154.45(15) . . ? C24 P1 C12 105.4(2) . . ? C24 P1 C18 101.5(2) . . ? C12 P1 C18 103.5(2) . . ? C24 P1 Ir1 117.18(15) . . ? C12 P1 Ir1 110.66(16) . . ? C18 P1 Ir1 117.06(13) . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C35 129.1(4) . . ? C2 N1 C35 119.6(4) . . ? C3 N2 C1 111.8(4) . . ? C3 N2 C26 119.5(4) . . ? C1 N2 C26 127.4(4) . . ? N2 C1 N1 102.6(4) . . ? N2 C1 Ir1 131.4(3) . . ? N1 C1 Ir1 125.6(3) . . ? C3 C2 N1 107.5(5) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 107.5(5) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C5 C4 C11 126.2(5) . . ? C5 C4 Ir1 70.5(3) . . ? C11 C4 Ir1 109.7(3) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 Ir1 72.2(3) . . ? C6 C5 Ir1 112.0(3) . . ? C7 C6 C5 112.0(4) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 114.7(4) . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 124.5(6) . . ? C9 C8 Ir1 71.7(3) . . ? C7 C8 Ir1 107.6(4) . . ? C8 C9 C10 125.1(6) . . ? C8 C9 Ir1 71.2(3) . . ? C10 C9 Ir1 113.5(4) . . ? C9 C10 C11 112.2(5) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C4 C11 C10 113.9(4) . . ? C4 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C4 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C17 118.9(5) . . ? C13 C12 P1 119.6(4) . . ? C17 C12 P1 121.4(4) . . ? C12 C13 C14 120.9(5) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.6(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 120.1(5) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 119.8(5) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C23 C18 C19 118.0(4) . . ? C23 C18 P1 120.5(4) . . ? C19 C18 P1 121.4(4) . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.3(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 121.3(5) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 P1 120.5(3) . . ? C25 C24 H24A 107.2 . . ? P1 C24 H24A 107.2 . . ? C25 C24 H24B 107.2 . . ? P1 C24 H24B 107.2 . . ? H24A C24 H24B 106.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 120.9(5) . . ? C27 C26 N2 118.8(4) . . ? C31 C26 N2 119.9(5) . . ? C28 C27 C26 118.5(5) . . ? C28 C27 C34 118.8(5) . . ? C26 C27 C34 122.1(5) . . ? C29 C28 C27 122.2(6) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C30 C29 C28 117.3(5) . . ? C30 C29 C33 120.8(6) . . ? C28 C29 C33 121.9(6) . . ? C29 C30 C31 124.1(5) . . ? C29 C30 H30 118.0 . . ? C31 C30 H30 118.0 . . ? C30 C31 C26 116.5(5) . . ? C30 C31 C32 118.9(5) . . ? C26 C31 C32 124.7(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 121.0(4) . . ? C36 C35 N1 121.6(4) . . ? C40 C35 N1 117.0(4) . . ? C37 C36 C35 118.3(4) . . ? C37 C36 C41 121.1(4) . . ? C35 C36 C41 120.6(4) . . ? C36 C37 C38 122.8(5) . . ? C36 C37 H37 118.6 . . ? C38 C37 H37 118.6 . . ? C39 C38 C37 116.9(4) . . ? C39 C38 C42 122.4(5) . . ? C37 C38 C42 120.6(5) . . ? C38 C39 C40 123.3(5) . . ? C38 C39 H39 118.3 . . ? C40 C39 H39 118.3 . . ? C39 C40 C35 117.5(4) . . ? C39 C40 C43 119.0(4) . . ? C35 C40 C43 123.5(4) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? F3 B1 F1 110.7(5) . . ? F3 B1 F2 110.4(5) . . ? F1 B1 F2 108.5(5) . . ? F3 B1 F4 110.5(5) . . ? F1 B1 F4 107.8(5) . . ? F2 B1 F4 108.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C24 -21.0(2) . . . . ? C5 Ir1 P1 C24 133.6(2) . . . . ? C8 Ir1 P1 C24 72.5(7) . . . . ? C4 Ir1 P1 C24 170.3(2) . . . . ? C9 Ir1 P1 C24 -136.1(4) . . . . ? C1 Ir1 P1 C12 99.8(2) . . . . ? C5 Ir1 P1 C12 -105.6(2) . . . . ? C8 Ir1 P1 C12 -166.8(7) . . . . ? C4 Ir1 P1 C12 -68.9(2) . . . . ? C9 Ir1 P1 C12 -15.3(4) . . . . ? C1 Ir1 P1 C18 -141.9(2) . . . . ? C5 Ir1 P1 C18 12.7(2) . . . . ? C8 Ir1 P1 C18 -48.5(7) . . . . ? C4 Ir1 P1 C18 49.3(2) . . . . ? C9 Ir1 P1 C18 102.9(4) . . . . ? C3 N2 C1 N1 -1.1(5) . . . . ? C26 N2 C1 N1 165.6(4) . . . . ? C3 N2 C1 Ir1 172.1(4) . . . . ? C26 N2 C1 Ir1 -21.2(6) . . . . ? C2 N1 C1 N2 2.3(5) . . . . ? C35 N1 C1 N2 -167.4(4) . . . . ? C2 N1 C1 Ir1 -171.4(4) . . . . ? C35 N1 C1 Ir1 18.8(7) . . . . ? C5 Ir1 C1 N2 -169.9(4) . . . . ? C8 Ir1 C1 N2 126.8(4) . . . . ? C4 Ir1 C1 N2 19.7(11) . . . . ? C9 Ir1 C1 N2 90.9(4) . . . . ? P1 Ir1 C1 N2 -65.9(4) . . . . ? C5 Ir1 C1 N1 2.0(7) . . . . ? C8 Ir1 C1 N1 -61.4(4) . . . . ? C4 Ir1 C1 N1 -168.5(8) . . . . ? C9 Ir1 C1 N1 -97.2(4) . . . . ? P1 Ir1 C1 N1 105.9(4) . . . . ? C1 N1 C2 C3 -2.8(6) . . . . ? C35 N1 C2 C3 168.0(5) . . . . ? N1 C2 C3 N2 2.0(6) . . . . ? C1 N2 C3 C2 -0.6(6) . . . . ? C26 N2 C3 C2 -168.4(4) . . . . ? C1 Ir1 C4 C5 173.1(8) . . . . ? C8 Ir1 C4 C5 66.9(4) . . . . ? C9 Ir1 C4 C5 100.2(3) . . . . ? P1 Ir1 C4 C5 -100.4(3) . . . . ? C1 Ir1 C4 C11 50.4(11) . . . . ? C5 Ir1 C4 C11 -122.6(5) . . . . ? C8 Ir1 C4 C11 -55.7(4) . . . . ? C9 Ir1 C4 C11 -22.4(4) . . . . ? P1 Ir1 C4 C11 137.0(3) . . . . ? C11 C4 C5 C6 -4.5(9) . . . . ? Ir1 C4 C5 C6 -105.1(5) . . . . ? C11 C4 C5 Ir1 100.6(5) . . . . ? C1 Ir1 C5 C4 -176.9(3) . . . . ? C8 Ir1 C5 C4 -112.5(4) . . . . ? C9 Ir1 C5 C4 -75.7(3) . . . . ? P1 Ir1 C5 C4 78.7(3) . . . . ? C1 Ir1 C5 C6 -58.1(6) . . . . ? C8 Ir1 C5 C6 6.3(3) . . . . ? C4 Ir1 C5 C6 118.8(5) . . . . ? C9 Ir1 C5 C6 43.1(3) . . . . ? P1 Ir1 C5 C6 -162.5(3) . . . . ? C4 C5 C6 C7 94.8(6) . . . . ? Ir1 C5 C6 C7 12.5(5) . . . . ? C5 C6 C7 C8 -34.6(6) . . . . ? C6 C7 C8 C9 -40.9(8) . . . . ? C6 C7 C8 Ir1 38.6(5) . . . . ? C1 Ir1 C8 C9 -105.7(4) . . . . ? C5 Ir1 C8 C9 97.8(4) . . . . ? C4 Ir1 C8 C9 63.5(4) . . . . ? P1 Ir1 C8 C9 160.1(4) . . . . ? C1 Ir1 C8 C7 132.9(4) . . . . ? C5 Ir1 C8 C7 -23.6(3) . . . . ? C4 Ir1 C8 C7 -57.9(4) . . . . ? C9 Ir1 C8 C7 -121.4(6) . . . . ? P1 Ir1 C8 C7 38.7(9) . . . . ? C7 C8 C9 C10 -6.8(10) . . . . ? Ir1 C8 C9 C10 -106.0(5) . . . . ? C7 C8 C9 Ir1 99.1(6) . . . . ? C1 Ir1 C9 C8 75.4(4) . . . . ? C5 Ir1 C9 C8 -78.7(4) . . . . ? C4 Ir1 C9 C8 -115.4(4) . . . . ? P1 Ir1 C9 C8 -170.0(2) . . . . ? C1 Ir1 C9 C10 -163.6(4) . . . . ? C5 Ir1 C9 C10 42.2(4) . . . . ? C8 Ir1 C9 C10 120.9(6) . . . . ? C4 Ir1 C9 C10 5.5(4) . . . . ? P1 Ir1 C9 C10 -49.1(6) . . . . ? C8 C9 C10 C11 95.2(7) . . . . ? Ir1 C9 C10 C11 12.3(6) . . . . ? C5 C4 C11 C10 -43.0(8) . . . . ? Ir1 C4 C11 C10 36.7(5) . . . . ? C9 C10 C11 C4 -32.7(7) . . . . ? C24 P1 C12 C13 112.6(4) . . . . ? C18 P1 C12 C13 -141.2(4) . . . . ? Ir1 P1 C12 C13 -15.0(4) . . . . ? C24 P1 C12 C17 -65.2(4) . . . . ? C18 P1 C12 C17 41.0(4) . . . . ? Ir1 P1 C12 C17 167.3(4) . . . . ? C17 C12 C13 C14 1.1(8) . . . . ? P1 C12 C13 C14 -176.7(4) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C13 C14 C15 C16 0.3(8) . . . . ? C14 C15 C16 C17 0.8(8) . . . . ? C15 C16 C17 C12 -0.9(8) . . . . ? C13 C12 C17 C16 -0.1(8) . . . . ? P1 C12 C17 C16 177.7(4) . . . . ? C24 P1 C18 C23 -39.1(4) . . . . ? C12 P1 C18 C23 -148.2(4) . . . . ? Ir1 P1 C18 C23 89.8(4) . . . . ? C24 P1 C18 C19 141.2(4) . . . . ? C12 P1 C18 C19 32.1(4) . . . . ? Ir1 P1 C18 C19 -90.0(4) . . . . ? C23 C18 C19 C20 1.4(7) . . . . ? P1 C18 C19 C20 -178.9(4) . . . . ? C18 C19 C20 C21 -1.1(8) . . . . ? C19 C20 C21 C22 1.4(9) . . . . ? C20 C21 C22 C23 -2.0(9) . . . . ? C19 C18 C23 C22 -2.0(7) . . . . ? P1 C18 C23 C22 178.3(4) . . . . ? C21 C22 C23 C18 2.3(8) . . . . ? C12 P1 C24 C25 47.3(4) . . . . ? C18 P1 C24 C25 -60.4(4) . . . . ? Ir1 P1 C24 C25 170.8(3) . . . . ? C3 N2 C26 C27 98.9(5) . . . . ? C1 N2 C26 C27 -66.8(6) . . . . ? C3 N2 C26 C31 -73.5(6) . . . . ? C1 N2 C26 C31 120.7(5) . . . . ? C31 C26 C27 C28 -8.5(7) . . . . ? N2 C26 C27 C28 179.1(4) . . . . ? C31 C26 C27 C34 162.9(5) . . . . ? N2 C26 C27 C34 -9.5(7) . . . . ? C26 C27 C28 C29 4.9(8) . . . . ? C34 C27 C28 C29 -166.8(5) . . . . ? C27 C28 C29 C30 0.5(8) . . . . ? C27 C28 C29 C33 -179.8(5) . . . . ? C28 C29 C30 C31 -2.5(8) . . . . ? C33 C29 C30 C31 177.8(5) . . . . ? C29 C30 C31 C26 -0.9(8) . . . . ? C29 C30 C31 C32 178.8(5) . . . . ? C27 C26 C31 C30 6.5(7) . . . . ? N2 C26 C31 C30 178.8(4) . . . . ? C27 C26 C31 C32 -173.2(5) . . . . ? N2 C26 C31 C32 -0.9(7) . . . . ? C1 N1 C35 C36 -81.8(6) . . . . ? C2 N1 C35 C36 109.2(5) . . . . ? C1 N1 C35 C40 105.6(5) . . . . ? C2 N1 C35 C40 -63.4(6) . . . . ? C40 C35 C36 C37 0.6(7) . . . . ? N1 C35 C36 C37 -171.7(4) . . . . ? C40 C35 C36 C41 178.8(4) . . . . ? N1 C35 C36 C41 6.4(7) . . . . ? C35 C36 C37 C38 3.6(7) . . . . ? C41 C36 C37 C38 -174.6(5) . . . . ? C36 C37 C38 C39 -5.6(7) . . . . ? C36 C37 C38 C42 171.6(4) . . . . ? C37 C38 C39 C40 3.5(7) . . . . ? C42 C38 C39 C40 -173.6(4) . . . . ? C38 C39 C40 C35 0.4(7) . . . . ? C38 C39 C40 C43 179.1(5) . . . . ? C36 C35 C40 C39 -2.5(7) . . . . ? N1 C35 C40 C39 170.2(4) . . . . ? C36 C35 C40 C43 178.9(5) . . . . ? N1 C35 C40 C43 -8.5(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.208 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.092 # Attachment '- Hope_9.cif' data_04199 _database_code_depnum_ccdc_archive 'CCDC 723141' _publ_section_title_footnote # remove if not required . #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C37 H39 N2 O2 P Ir)+ (B F4)- 0.5(C H Cl3)' _chemical_formula_sum 'C37.50 H39.50 B Cl1.50 F4 Ir N2 O2 P' _chemical_formula_weight 913.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.472(13) _cell_length_b 15.20(2) _cell_length_c 16.07(2) _cell_angle_alpha 81.60(2) _cell_angle_beta 76.57(2) _cell_angle_gamma 76.53(2) _cell_volume 1948(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.97 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 3.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.467 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 3198 reflections (SADABS); Rint 0.120 before correction and 0.034 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16473 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8374 _reflns_number_gt 7761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disordered CHCl3 solvent was eliminated from the final least squares using the SQUEEZE option of Platon. The solvent accessible voids are 307 3 with an estimated 85e/cell to be added. One solvent CHCl3 molecule/unit cell accounting for 58e was included in the formula, FWt, (000) and density calculations. PLATON Reference : Spek, A.L. (1990), Acta Cryst. A46, C-34 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^)+(0.0661P)^2^+8.3942P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8374 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.92959(3) 0.751188(14) 0.741366(13) 0.02229(9) Uani 1 1 d . . . P1 P 0.8457(2) 0.90060(10) 0.77729(10) 0.0250(3) Uani 1 1 d . . . N1 N 0.9548(7) 0.5524(4) 0.8014(3) 0.0250(10) Uani 1 1 d . . . N2 N 1.0948(7) 0.5595(3) 0.6723(3) 0.0242(10) Uani 1 1 d . . . O1 O 1.2624(7) 0.7971(4) 0.6595(4) 0.0489(14) Uani 1 1 d . . . C1 C 1.1405(9) 0.7758(4) 0.6980(5) 0.0318(14) Uani 1 1 d . . . O2 O 0.5923(8) 0.7558(5) 0.7073(6) 0.071(2) Uani 1 1 d . . . C2 C 0.7140(10) 0.7507(5) 0.7271(5) 0.0412(17) Uani 1 1 d . . . C3 C 1.0023(8) 0.6121(4) 0.7346(4) 0.0260(13) Uani 1 1 d . . . C4 C 1.0157(9) 0.4635(4) 0.7824(4) 0.0307(13) Uani 1 1 d . . . H4 H 0.9985 0.4101 0.8190 0.037 Uiso 1 1 calc R . . C5 C 1.1052(9) 0.4683(4) 0.7006(4) 0.0326(14) Uani 1 1 d . . . H5 H 1.1639 0.4184 0.6688 0.039 Uiso 1 1 calc R . . C6 C 0.8592(8) 0.5810(4) 0.8825(4) 0.0286(13) Uani 1 1 d . . . C7 C 0.9362(8) 0.6107(4) 0.9377(4) 0.0249(12) Uani 1 1 d . . . C8 C 0.8364(9) 0.6458(5) 1.0122(4) 0.0311(14) Uani 1 1 d . . . H8 H 0.8858 0.6683 1.0498 0.037 Uiso 1 1 calc R . . C9 C 0.6683(9) 0.6488(5) 1.0331(4) 0.0343(15) Uani 1 1 d . . . C10 C 0.5968(9) 0.6143(6) 0.9789(4) 0.0373(16) Uani 1 1 d . . . H10 H 0.4818 0.6136 0.9943 0.045 Uiso 1 1 calc R . . C11 C 0.6901(10) 0.5805(5) 0.9023(5) 0.0364(15) Uani 1 1 d . . . C12 C 1.1222(8) 0.6022(5) 0.9192(4) 0.0311(13) Uani 1 1 d . . . H12A H 1.1771 0.5381 0.9161 0.047 Uiso 1 1 calc R . . H12B H 1.1531 0.6262 0.9653 0.047 Uiso 1 1 calc R . . H12C H 1.1571 0.6370 0.8643 0.047 Uiso 1 1 calc R . . C13 C 0.5646(12) 0.6872(7) 1.1157(5) 0.056(2) Uani 1 1 d . . . H13A H 0.5613 0.6381 1.1626 0.084 Uiso 1 1 calc R . . H13B H 0.4516 0.7143 1.1078 0.084 Uiso 1 1 calc R . . H13C H 0.6143 0.7337 1.1298 0.084 Uiso 1 1 calc R . . C14 C 0.6095(10) 0.5440(7) 0.8433(5) 0.047(2) Uani 1 1 d . . . H14A H 0.6419 0.5709 0.7842 0.070 Uiso 1 1 calc R . . H14B H 0.4886 0.5599 0.8619 0.070 Uiso 1 1 calc R . . H14C H 0.6459 0.4778 0.8456 0.070 Uiso 1 1 calc R . . C15 C 1.1734(7) 0.5921(4) 0.5887(4) 0.0232(11) Uani 1 1 d . . . C16 C 1.0837(8) 0.6139(4) 0.5231(4) 0.0273(13) Uani 1 1 d . . . C17 C 1.1651(9) 0.6407(5) 0.4415(4) 0.0327(14) Uani 1 1 d . . . H17 H 1.1071 0.6539 0.3958 0.039 Uiso 1 1 calc R . . C18 C 1.3315(10) 0.6489(5) 0.4249(4) 0.0375(16) Uani 1 1 d . . . C19 C 1.4152(9) 0.6278(5) 0.4916(5) 0.0362(15) Uani 1 1 d . . . H19 H 1.5278 0.6334 0.4806 0.043 Uiso 1 1 calc R . . C20 C 1.3406(8) 0.5987(4) 0.5746(4) 0.0292(13) Uani 1 1 d . . . C21 C 0.9064(9) 0.6088(5) 0.5393(5) 0.0369(15) Uani 1 1 d . . . H21A H 0.8383 0.6612 0.5687 0.055 Uiso 1 1 calc R . . H21B H 0.8894 0.5526 0.5754 0.055 Uiso 1 1 calc R . . H21C H 0.8741 0.6092 0.4845 0.055 Uiso 1 1 calc R . . C22 C 1.4154(13) 0.6810(7) 0.3372(6) 0.058(2) Uani 1 1 d . . . H22A H 1.5341 0.6739 0.3353 0.087 Uiso 1 1 calc R . . H22B H 1.3670 0.7452 0.3238 0.087 Uiso 1 1 calc R . . H22C H 1.4001 0.6449 0.2950 0.087 Uiso 1 1 calc R . . C23 C 1.4359(10) 0.5759(5) 0.6455(5) 0.0399(16) Uani 1 1 d . . . H23A H 1.5181 0.5192 0.6361 0.060 Uiso 1 1 calc R . . H23B H 1.3593 0.5685 0.7008 0.060 Uiso 1 1 calc R . . H23C H 1.4925 0.6251 0.6459 0.060 Uiso 1 1 calc R . . C24 C 0.9705(8) 0.9261(4) 0.8448(4) 0.0265(12) Uani 1 1 d . . . H24A H 1.0834 0.9273 0.8105 0.032 Uiso 1 1 calc R . . H24B H 0.9213 0.9873 0.8643 0.032 Uiso 1 1 calc R . . C25 C 0.9824(10) 0.8575(5) 0.9224(5) 0.0380(16) Uani 1 1 d . . . H25A H 0.8716 0.8589 0.9585 0.057 Uiso 1 1 calc R . . H25B H 1.0547 0.8725 0.9554 0.057 Uiso 1 1 calc R . . H25C H 1.0287 0.7966 0.9035 0.057 Uiso 1 1 calc R . . C26 C 0.6361(9) 0.9271(4) 0.8422(4) 0.0311(14) Uani 1 1 d . . . C27 C 0.5695(9) 0.8588(5) 0.8931(5) 0.0365(15) Uani 1 1 d . . . H27 H 0.6303 0.7978 0.8928 0.044 Uiso 1 1 calc R . . C28 C 0.4132(10) 0.8791(6) 0.9451(6) 0.0482(19) Uani 1 1 d . . . H28 H 0.3669 0.8318 0.9805 0.058 Uiso 1 1 calc R . . C29 C 0.3250(10) 0.9671(6) 0.9458(6) 0.051(2) Uani 1 1 d . . . H29 H 0.2176 0.9807 0.9813 0.061 Uiso 1 1 calc R . . C30 C 0.3930(10) 1.0366(6) 0.8943(6) 0.0461(19) Uani 1 1 d . . . H30 H 0.3323 1.0976 0.8943 0.055 Uiso 1 1 calc R . . C31 C 0.5473(9) 1.0162(5) 0.8440(5) 0.0374(15) Uani 1 1 d . . . H31 H 0.5949 1.0636 0.8096 0.045 Uiso 1 1 calc R . . C32 C 0.8492(9) 0.9860(4) 0.6857(4) 0.0277(13) Uani 1 1 d . . . C33 C 0.7955(13) 0.9729(6) 0.6147(6) 0.051(2) Uani 1 1 d . . . H33 H 0.7620 0.9179 0.6129 0.061 Uiso 1 1 calc R . . C34 C 0.7901(16) 1.0395(7) 0.5457(6) 0.067(3) Uani 1 1 d . . . H34 H 0.7434 1.0324 0.4994 0.080 Uiso 1 1 calc R . . C35 C 0.8516(15) 1.1150(6) 0.5444(6) 0.059(3) Uani 1 1 d . . . H35 H 0.8555 1.1583 0.4954 0.071 Uiso 1 1 calc R . . C36 C 0.9075(13) 1.1284(5) 0.6134(6) 0.054(2) Uani 1 1 d . . . H36 H 0.9462 1.1824 0.6131 0.064 Uiso 1 1 calc R . . C37 C 0.9087(11) 1.0642(5) 0.6842(6) 0.0444(18) Uani 1 1 d . . . H37 H 0.9501 1.0736 0.7316 0.053 Uiso 1 1 calc R . . B1 B 0.9405(14) 0.2344(6) 0.8434(6) 0.047(2) Uani 1 1 d . . . F1 F 0.9103(11) 0.2638(5) 0.7633(4) 0.085(2) Uani 1 1 d . . . F2 F 1.1043(10) 0.2296(6) 0.8423(6) 0.105(3) Uani 1 1 d . . . F3 F 0.8530(8) 0.2978(4) 0.8998(4) 0.0664(15) Uani 1 1 d . . . F4 F 0.8962(14) 0.1532(4) 0.8705(5) 0.114(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02446(14) 0.01996(14) 0.02348(14) -0.00609(9) -0.00600(9) -0.00313(9) P1 0.0271(8) 0.0209(7) 0.0272(7) -0.0081(6) -0.0067(6) -0.0012(6) N1 0.026(3) 0.034(3) 0.014(2) 0.0021(19) 0.0022(18) -0.011(2) N2 0.031(3) 0.019(2) 0.025(2) -0.0059(19) -0.008(2) -0.003(2) O1 0.041(3) 0.037(3) 0.069(4) -0.012(3) -0.006(3) -0.010(2) C1 0.033(4) 0.020(3) 0.047(4) -0.007(3) -0.019(3) 0.000(2) O2 0.043(4) 0.060(4) 0.129(7) -0.037(4) -0.045(4) 0.000(3) C2 0.037(4) 0.034(4) 0.053(4) -0.020(3) -0.001(3) -0.005(3) C3 0.035(3) 0.014(3) 0.034(3) -0.003(2) -0.020(3) 0.000(2) C4 0.043(4) 0.024(3) 0.027(3) 0.001(2) -0.007(3) -0.012(3) C5 0.045(4) 0.022(3) 0.031(3) -0.006(2) -0.005(3) -0.007(3) C6 0.031(3) 0.029(3) 0.027(3) -0.005(2) -0.007(3) -0.006(3) C7 0.026(3) 0.029(3) 0.018(3) 0.003(2) -0.001(2) -0.010(2) C8 0.043(4) 0.035(3) 0.018(3) -0.001(2) -0.007(3) -0.015(3) C9 0.033(4) 0.047(4) 0.019(3) -0.003(3) 0.002(2) -0.009(3) C10 0.028(3) 0.055(4) 0.026(3) 0.003(3) 0.002(3) -0.015(3) C11 0.043(4) 0.041(4) 0.032(3) -0.002(3) -0.019(3) -0.013(3) C12 0.030(3) 0.037(3) 0.030(3) 0.002(3) -0.011(3) -0.013(3) C13 0.055(5) 0.082(7) 0.031(4) -0.018(4) 0.004(4) -0.020(5) C14 0.042(4) 0.078(6) 0.031(4) -0.004(4) -0.007(3) -0.034(4) C15 0.025(3) 0.021(3) 0.023(3) -0.006(2) 0.001(2) -0.006(2) C16 0.033(3) 0.018(3) 0.033(3) -0.008(2) -0.011(3) -0.001(2) C17 0.044(4) 0.029(3) 0.025(3) -0.006(2) -0.009(3) -0.004(3) C18 0.047(4) 0.031(3) 0.028(3) -0.006(3) -0.002(3) -0.001(3) C19 0.035(4) 0.036(4) 0.035(4) -0.007(3) -0.002(3) -0.004(3) C20 0.032(3) 0.024(3) 0.033(3) -0.011(2) -0.010(3) -0.001(2) C21 0.036(4) 0.039(4) 0.042(4) -0.009(3) -0.018(3) -0.008(3) C22 0.058(6) 0.060(6) 0.044(5) 0.001(4) 0.002(4) -0.005(4) C23 0.036(4) 0.040(4) 0.048(4) -0.012(3) -0.019(3) -0.001(3) C24 0.023(3) 0.032(3) 0.025(3) -0.007(2) -0.001(2) -0.007(2) C25 0.053(5) 0.027(3) 0.038(4) -0.006(3) -0.022(3) -0.003(3) C26 0.037(4) 0.026(3) 0.032(3) -0.012(3) -0.013(3) 0.000(3) C27 0.031(4) 0.036(4) 0.038(4) -0.011(3) 0.005(3) -0.007(3) C28 0.038(4) 0.049(5) 0.060(5) -0.019(4) -0.004(4) -0.011(3) C29 0.032(4) 0.061(5) 0.063(5) -0.035(4) -0.006(4) -0.001(4) C30 0.035(4) 0.044(4) 0.053(5) -0.018(4) -0.006(3) 0.009(3) C31 0.036(4) 0.036(4) 0.036(4) -0.010(3) -0.001(3) -0.002(3) C32 0.038(3) 0.020(3) 0.021(3) -0.001(2) -0.003(2) -0.002(2) C33 0.076(6) 0.045(4) 0.044(4) -0.002(3) -0.028(4) -0.021(4) C34 0.110(9) 0.058(6) 0.038(4) 0.002(4) -0.035(5) -0.015(6) C35 0.093(8) 0.033(4) 0.047(5) 0.006(4) -0.023(5) -0.004(4) C36 0.079(7) 0.029(4) 0.059(5) 0.007(4) -0.028(5) -0.015(4) C37 0.064(5) 0.026(3) 0.049(4) -0.004(3) -0.025(4) -0.007(3) B1 0.071(7) 0.033(4) 0.047(5) -0.002(4) -0.025(5) -0.015(4) F1 0.141(7) 0.077(4) 0.055(3) 0.009(3) -0.052(4) -0.034(4) F2 0.084(5) 0.108(6) 0.142(7) -0.057(5) -0.058(5) 0.007(4) F3 0.091(4) 0.048(3) 0.069(4) -0.014(3) -0.023(3) -0.022(3) F4 0.239(11) 0.046(3) 0.069(4) -0.005(3) -0.016(5) -0.071(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.864(8) . ? Ir1 C2 1.895(9) . ? Ir1 C3 2.071(6) . ? Ir1 P1 2.331(4) . ? P1 C32 1.814(7) . ? P1 C24 1.815(7) . ? P1 C26 1.825(8) . ? N1 C3 1.351(8) . ? N1 C4 1.380(9) . ? N1 C6 1.434(8) . ? N2 C3 1.354(8) . ? N2 C5 1.383(8) . ? N2 C15 1.428(8) . ? O1 C1 1.164(9) . ? O2 C2 1.130(10) . ? C4 C5 1.358(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.392(9) . ? C6 C11 1.395(10) . ? C7 C8 1.393(9) . ? C7 C12 1.512(9) . ? C8 C9 1.377(10) . ? C8 H8 0.9500 . ? C9 C10 1.388(11) . ? C9 C13 1.523(10) . ? C10 C11 1.395(10) . ? C10 H10 0.9500 . ? C11 C14 1.519(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.397(9) . ? C15 C20 1.406(9) . ? C16 C17 1.383(10) . ? C16 C21 1.482(10) . ? C17 C18 1.404(11) . ? C17 H17 0.9500 . ? C18 C19 1.379(11) . ? C18 C22 1.491(11) . ? C19 C20 1.394(10) . ? C19 H19 0.9500 . ? C20 C23 1.500(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.512(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.370(10) . ? C26 C31 1.388(10) . ? C27 C28 1.385(11) . ? C27 H27 0.9500 . ? C28 C29 1.373(12) . ? C28 H28 0.9500 . ? C29 C30 1.392(13) . ? C29 H29 0.9500 . ? C30 C31 1.361(11) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.378(10) . ? C32 C37 1.390(10) . ? C33 C34 1.390(12) . ? C33 H33 0.9500 . ? C34 C35 1.362(15) . ? C34 H34 0.9500 . ? C35 C36 1.360(13) . ? C35 H35 0.9500 . ? C36 C37 1.388(11) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? B1 F4 1.356(11) . ? B1 F1 1.361(11) . ? B1 F2 1.368(13) . ? B1 F3 1.382(12) . ? 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 C2 150.7(4) . . ? C1 Ir1 C3 95.6(3) . . ? C2 Ir1 C3 91.5(3) . . ? C1 Ir1 P1 87.2(2) . . ? C2 Ir1 P1 91.3(2) . . ? C3 Ir1 P1 168.95(18) . . ? C32 P1 C24 107.1(3) . . ? C32 P1 C26 105.3(3) . . ? C24 P1 C26 102.5(3) . . ? C32 P1 Ir1 114.4(2) . . ? C24 P1 Ir1 112.3(2) . . ? C26 P1 Ir1 114.2(2) . . ? C3 N1 C4 111.8(5) . . ? C3 N1 C6 122.3(6) . . ? C4 N1 C6 125.9(5) . . ? C3 N2 C5 110.7(5) . . ? C3 N2 C15 125.5(5) . . ? C5 N2 C15 123.8(5) . . ? O1 C1 Ir1 169.2(6) . . ? O2 C2 Ir1 170.4(9) . . ? N1 C3 N2 104.6(5) . . ? N1 C3 Ir1 121.6(5) . . ? N2 C3 Ir1 133.8(5) . . ? C5 C4 N1 105.8(5) . . ? C5 C4 H4 127.1 . . ? N1 C4 H4 127.1 . . ? C4 C5 N2 107.1(6) . . ? C4 C5 H5 126.5 . . ? N2 C5 H5 126.5 . . ? C7 C6 C11 122.2(6) . . ? C7 C6 N1 119.3(6) . . ? C11 C6 N1 118.5(6) . . ? C6 C7 C8 117.6(6) . . ? C6 C7 C12 121.4(6) . . ? C8 C7 C12 121.0(6) . . ? C9 C8 C7 122.0(6) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 118.9(6) . . ? C8 C9 C13 120.1(7) . . ? C10 C9 C13 121.1(7) . . ? C9 C10 C11 121.5(7) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 117.7(6) . . ? C10 C11 C14 120.8(7) . . ? C6 C11 C14 121.5(7) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 122.2(6) . . ? C16 C15 N2 119.2(6) . . ? C20 C15 N2 118.6(6) . . ? C17 C16 C15 118.1(6) . . ? C17 C16 C21 120.3(6) . . ? C15 C16 C21 121.6(6) . . ? C16 C17 C18 121.5(6) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 118.6(7) . . ? C19 C18 C22 120.7(8) . . ? C17 C18 C22 120.7(7) . . ? C18 C19 C20 122.3(7) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 117.2(6) . . ? C19 C20 C23 120.8(7) . . ? C15 C20 C23 122.0(6) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 P1 112.4(5) . . ? C25 C24 H24A 109.1 . . ? P1 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? P1 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 119.7(7) . . ? C27 C26 P1 119.5(5) . . ? C31 C26 P1 120.7(6) . . ? C26 C27 C28 119.7(7) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.3(9) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.0(8) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.3(8) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C26 121.0(8) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C33 C32 C37 118.6(7) . . ? C33 C32 P1 119.8(6) . . ? C37 C32 P1 121.6(5) . . ? C32 C33 C34 120.6(8) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.0(9) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.0(8) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.8(8) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C32 119.8(7) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? F4 B1 F1 110.2(8) . . ? F4 B1 F2 111.8(9) . . ? F1 B1 F2 109.4(10) . . ? F4 B1 F3 110.1(9) . . ? F1 B1 F3 109.7(8) . . ? F2 B1 F3 105.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C32 66.8(3) . . . . ? C2 Ir1 P1 C32 -83.9(4) . . . . ? C3 Ir1 P1 C32 171.6(10) . . . . ? C1 Ir1 P1 C24 -55.5(3) . . . . ? C2 Ir1 P1 C24 153.7(3) . . . . ? C3 Ir1 P1 C24 49.2(10) . . . . ? C1 Ir1 P1 C26 -171.7(3) . . . . ? C2 Ir1 P1 C26 37.5(4) . . . . ? C3 Ir1 P1 C26 -67.0(10) . . . . ? C2 Ir1 C1 O1 5(3) . . . . ? C3 Ir1 C1 O1 109(3) . . . . ? P1 Ir1 C1 O1 -82(3) . . . . ? C1 Ir1 C2 O2 -2(4) . . . . ? C3 Ir1 C2 O2 -106(4) . . . . ? P1 Ir1 C2 O2 85(4) . . . . ? C4 N1 C3 N2 0.1(7) . . . . ? C6 N1 C3 N2 177.3(5) . . . . ? C4 N1 C3 Ir1 179.2(4) . . . . ? C6 N1 C3 Ir1 -3.5(8) . . . . ? C5 N2 C3 N1 -0.4(7) . . . . ? C15 N2 C3 N1 -179.8(5) . . . . ? C5 N2 C3 Ir1 -179.4(5) . . . . ? C15 N2 C3 Ir1 1.2(10) . . . . ? C1 Ir1 C3 N1 132.1(5) . . . . ? C2 Ir1 C3 N1 -76.4(5) . . . . ? P1 Ir1 C3 N1 28.1(13) . . . . ? C1 Ir1 C3 N2 -49.1(6) . . . . ? C2 Ir1 C3 N2 102.4(7) . . . . ? P1 Ir1 C3 N2 -153.1(6) . . . . ? C3 N1 C4 C5 0.3(8) . . . . ? C6 N1 C4 C5 -176.8(6) . . . . ? N1 C4 C5 N2 -0.5(8) . . . . ? C3 N2 C5 C4 0.6(8) . . . . ? C15 N2 C5 C4 -180.0(6) . . . . ? C3 N1 C6 C7 -75.0(8) . . . . ? C4 N1 C6 C7 101.8(8) . . . . ? C3 N1 C6 C11 103.2(7) . . . . ? C4 N1 C6 C11 -80.0(9) . . . . ? C11 C6 C7 C8 -3.9(10) . . . . ? N1 C6 C7 C8 174.2(6) . . . . ? C11 C6 C7 C12 174.0(6) . . . . ? N1 C6 C7 C12 -7.9(9) . . . . ? C6 C7 C8 C9 2.1(10) . . . . ? C12 C7 C8 C9 -175.8(6) . . . . ? C7 C8 C9 C10 1.2(11) . . . . ? C7 C8 C9 C13 179.5(7) . . . . ? C8 C9 C10 C11 -2.9(11) . . . . ? C13 C9 C10 C11 178.8(8) . . . . ? C9 C10 C11 C6 1.2(11) . . . . ? C9 C10 C11 C14 -179.2(7) . . . . ? C7 C6 C11 C10 2.3(10) . . . . ? N1 C6 C11 C10 -175.8(6) . . . . ? C7 C6 C11 C14 -177.3(7) . . . . ? N1 C6 C11 C14 4.6(10) . . . . ? C3 N2 C15 C16 -86.7(7) . . . . ? C5 N2 C15 C16 94.0(7) . . . . ? C3 N2 C15 C20 95.2(7) . . . . ? C5 N2 C15 C20 -84.2(8) . . . . ? C20 C15 C16 C17 1.5(9) . . . . ? N2 C15 C16 C17 -176.6(5) . . . . ? C20 C15 C16 C21 -178.5(6) . . . . ? N2 C15 C16 C21 3.4(9) . . . . ? C15 C16 C17 C18 -2.0(9) . . . . ? C21 C16 C17 C18 178.0(6) . . . . ? C16 C17 C18 C19 1.2(10) . . . . ? C16 C17 C18 C22 -177.9(7) . . . . ? C17 C18 C19 C20 0.1(11) . . . . ? C22 C18 C19 C20 179.2(7) . . . . ? C18 C19 C20 C15 -0.6(10) . . . . ? C18 C19 C20 C23 179.7(7) . . . . ? C16 C15 C20 C19 -0.2(9) . . . . ? N2 C15 C20 C19 177.9(5) . . . . ? C16 C15 C20 C23 179.5(6) . . . . ? N2 C15 C20 C23 -2.4(9) . . . . ? C32 P1 C24 C25 -178.0(5) . . . . ? C26 P1 C24 C25 71.4(5) . . . . ? Ir1 P1 C24 C25 -51.6(5) . . . . ? C32 P1 C26 C27 152.3(6) . . . . ? C24 P1 C26 C27 -95.8(6) . . . . ? Ir1 P1 C26 C27 26.0(6) . . . . ? C32 P1 C26 C31 -31.2(6) . . . . ? C24 P1 C26 C31 80.7(6) . . . . ? Ir1 P1 C26 C31 -157.5(5) . . . . ? C31 C26 C27 C28 0.9(11) . . . . ? P1 C26 C27 C28 177.4(6) . . . . ? C26 C27 C28 C29 0.0(13) . . . . ? C27 C28 C29 C30 -0.3(13) . . . . ? C28 C29 C30 C31 -0.3(13) . . . . ? C29 C30 C31 C26 1.2(12) . . . . ? C27 C26 C31 C30 -1.5(11) . . . . ? P1 C26 C31 C30 -178.0(6) . . . . ? C24 P1 C32 C33 166.0(7) . . . . ? C26 P1 C32 C33 -85.4(7) . . . . ? Ir1 P1 C32 C33 40.8(7) . . . . ? C24 P1 C32 C37 -12.5(7) . . . . ? C26 P1 C32 C37 96.1(7) . . . . ? Ir1 P1 C32 C37 -137.7(6) . . . . ? C37 C32 C33 C34 -4.5(14) . . . . ? P1 C32 C33 C34 177.0(8) . . . . ? C32 C33 C34 C35 5.8(17) . . . . ? C33 C34 C35 C36 -4.7(18) . . . . ? C34 C35 C36 C37 2.5(17) . . . . ? C35 C36 C37 C32 -1.3(15) . . . . ? C33 C32 C37 C36 2.3(13) . . . . ? P1 C32 C37 C36 -179.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.844 _refine_diff_density_min -2.785 _refine_diff_density_rms 0.201 # Attachment '- Hope_6.cif' data_05042 _database_code_depnum_ccdc_archive 'CCDC 723142' _publ_section_title_footnote # remove if not required . #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C49 H51 Ir N2 P)+ (B F4)-' _chemical_formula_sum 'C49 H51 B F4 Ir N2 P' _chemical_formula_weight 977.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3704(17) _cell_length_b 13.371(2) _cell_length_c 15.841(3) _cell_angle_alpha 87.867(3) _cell_angle_beta 75.097(2) _cell_angle_gamma 89.756(3) _cell_volume 2121.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1022 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 28.25 _exptl_crystal_description red _exptl_crystal_colour plate _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 3.240 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 13220 reflections (SADABS); Rint 0.086 before correction and 0.022 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16617 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8227 _reflns_number_gt 7645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8227 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.516314(11) 0.815815(8) 0.709709(7) 0.02238(5) Uani 1 1 d . . . P1 P 0.29267(8) 0.80866(6) 0.78063(5) 0.02410(17) Uani 1 1 d . . . N1 N 0.5787(3) 0.6248(2) 0.81847(17) 0.0284(6) Uani 1 1 d . . . N2 N 0.5972(3) 0.6010(2) 0.68243(17) 0.0267(6) Uani 1 1 d . . . C1 C 0.5677(3) 0.6732(2) 0.74293(19) 0.0227(6) Uani 1 1 d . . . C2 C 0.6136(4) 0.5253(3) 0.8037(2) 0.0388(9) Uani 1 1 d . . . H2 H 0.6274 0.4769 0.8460 0.047 Uiso 1 1 calc R . . C3 C 0.6244(4) 0.5100(3) 0.7192(2) 0.0353(8) Uani 1 1 d . . . H3 H 0.6463 0.4490 0.6901 0.042 Uiso 1 1 calc R . . C4 C 0.5801(3) 0.6709(2) 0.8992(2) 0.0307(8) Uani 1 1 d . . . C5 C 0.4690(4) 0.6625(3) 0.9702(2) 0.0361(8) Uani 1 1 d . . . C6 C 0.4749(4) 0.7087(3) 1.0459(2) 0.0446(10) Uani 1 1 d . . . H6 H 0.3997 0.7046 1.0951 0.053 Uiso 1 1 calc R . . C7 C 0.5872(5) 0.7606(3) 1.0520(2) 0.0469(11) Uani 1 1 d . . . C8 C 0.6979(4) 0.7631(3) 0.9819(2) 0.0423(9) Uani 1 1 d . . . H8 H 0.7760 0.7971 0.9864 0.051 Uiso 1 1 calc R . . C9 C 0.6980(4) 0.7168(3) 0.9043(2) 0.0351(8) Uani 1 1 d . . . C10 C 0.3491(4) 0.6020(3) 0.9665(3) 0.0515(11) Uani 1 1 d . . . H10A H 0.3690 0.5306 0.9709 0.077 Uiso 1 1 calc R . . H10B H 0.3265 0.6171 0.9110 0.077 Uiso 1 1 calc R . . H10C H 0.2736 0.6189 1.0152 0.077 Uiso 1 1 calc R . . C11 C 0.5905(6) 0.8121(3) 1.1350(3) 0.0680(15) Uani 1 1 d . . . H11A H 0.5919 0.8848 1.1243 0.102 Uiso 1 1 calc R . . H11B H 0.6708 0.7918 1.1529 0.102 Uiso 1 1 calc R . . H11C H 0.5111 0.7931 1.1814 0.102 Uiso 1 1 calc R . . C12 C 0.8270(4) 0.7109(3) 0.8338(3) 0.0475(10) Uani 1 1 d . . . H12A H 0.8761 0.6511 0.8446 0.071 Uiso 1 1 calc R . . H12B H 0.8812 0.7707 0.8343 0.071 Uiso 1 1 calc R . . H12C H 0.8073 0.7073 0.7767 0.071 Uiso 1 1 calc R . . C13 C 0.6198(3) 0.6189(2) 0.5887(2) 0.0272(7) Uani 1 1 d . . . C14 C 0.7513(3) 0.6278(2) 0.5385(2) 0.0292(7) Uani 1 1 d . . . C15 C 0.7722(4) 0.6514(3) 0.4497(2) 0.0340(8) Uani 1 1 d . . . H15 H 0.8607 0.6605 0.4143 0.041 Uiso 1 1 calc R . . C16 C 0.6651(4) 0.6620(3) 0.4116(2) 0.0364(8) Uani 1 1 d . . . C17 C 0.5382(4) 0.6465(3) 0.4624(2) 0.0360(8) Uani 1 1 d . . . H17 H 0.4659 0.6516 0.4359 0.043 Uiso 1 1 calc R . . C18 C 0.5113(3) 0.6235(2) 0.5517(2) 0.0295(7) Uani 1 1 d . . . C19 C 0.8706(3) 0.6117(3) 0.5750(2) 0.0366(8) Uani 1 1 d . . . H19A H 0.8471 0.6280 0.6369 0.055 Uiso 1 1 calc R . . H19B H 0.9441 0.6551 0.5427 0.055 Uiso 1 1 calc R . . H19C H 0.8983 0.5416 0.5692 0.055 Uiso 1 1 calc R . . C20 C 0.6893(4) 0.6934(3) 0.3159(2) 0.0532(11) Uani 1 1 d . . . H20A H 0.6711 0.6367 0.2832 0.080 Uiso 1 1 d R . . H20B H 0.7825 0.7147 0.2930 0.080 Uiso 1 1 d R . . H20C H 0.6302 0.7490 0.3097 0.080 Uiso 1 1 d R . . C21 C 0.3711(3) 0.6038(3) 0.6040(2) 0.0375(8) Uani 1 1 d . . . H21A H 0.3711 0.5533 0.6505 0.056 Uiso 1 1 calc R . . H21B H 0.3183 0.5792 0.5658 0.056 Uiso 1 1 calc R . . H21C H 0.3320 0.6659 0.6301 0.056 Uiso 1 1 calc R . . C22 C 0.7297(3) 0.8452(2) 0.6461(2) 0.0261(7) Uani 1 1 d . . . H22 H 0.7440 0.7751 0.6491 0.031 Uiso 1 1 calc R . . C23 C 0.6910(3) 0.8954(3) 0.7250(2) 0.0299(7) Uani 1 1 d . . . H23 H 0.6799 0.8559 0.7774 0.036 Uiso 1 1 calc R . . C24 C 0.6657(4) 1.0053(3) 0.7342(2) 0.0364(8) Uani 1 1 d . . . H24A H 0.7522 1.0413 0.7206 0.044 Uiso 1 1 calc R . . H24B H 0.6186 1.0178 0.7956 0.044 Uiso 1 1 calc R . . C25 C 0.5822(4) 1.0468(3) 0.6740(2) 0.0357(8) Uani 1 1 d . . . H25A H 0.5383 1.1094 0.6977 0.043 Uiso 1 1 calc R . . H25B H 0.6415 1.0630 0.6154 0.043 Uiso 1 1 calc R . . C26 C 0.4776(3) 0.9724(2) 0.6660(2) 0.0312(7) Uani 1 1 d . . . H26 H 0.3949 0.9707 0.7093 0.037 Uiso 1 1 calc R . . C27 C 0.4962(3) 0.9061(2) 0.5981(2) 0.0276(7) Uani 1 1 d . . . H27 H 0.4240 0.8628 0.5977 0.033 Uiso 1 1 calc R . . C28 C 0.6211(3) 0.8976(3) 0.5258(2) 0.0323(8) Uani 1 1 d . . . H28A H 0.6254 0.9546 0.4835 0.039 Uiso 1 1 calc R . . H28B H 0.6161 0.8354 0.4947 0.039 Uiso 1 1 calc R . . C29 C 0.7498(3) 0.8961(3) 0.5564(2) 0.0322(8) Uani 1 1 d . . . H29A H 0.8200 0.8605 0.5138 0.039 Uiso 1 1 calc R . . H29B H 0.7809 0.9657 0.5584 0.039 Uiso 1 1 calc R . . C30 C 0.2068(3) 0.6923(2) 0.8006(2) 0.0278(7) Uani 1 1 d . . . C31 C 0.1544(3) 0.6126(3) 0.8098(2) 0.0299(7) Uani 1 1 d . . . C32 C 0.0888(3) 0.5166(2) 0.8194(2) 0.0330(8) Uani 1 1 d . . . C33 C 0.0248(4) 0.4879(3) 0.7566(3) 0.0436(9) Uani 1 1 d . . . H33 H 0.0277 0.5303 0.7067 0.052 Uiso 1 1 calc R . . C34 C -0.0429(4) 0.3970(3) 0.7673(3) 0.0542(11) Uani 1 1 d . . . H34 H -0.0872 0.3773 0.7249 0.065 Uiso 1 1 calc R . . C35 C -0.0457(4) 0.3357(3) 0.8395(3) 0.0584(13) Uani 1 1 d . . . H35 H -0.0928 0.2739 0.8470 0.070 Uiso 1 1 calc R . . C36 C 0.0183(5) 0.3627(3) 0.9004(3) 0.0577(12) Uani 1 1 d . . . H36 H 0.0171 0.3190 0.9493 0.069 Uiso 1 1 calc R . . C37 C 0.0846(4) 0.4527(3) 0.8913(3) 0.0435(9) Uani 1 1 d . . . H37 H 0.1278 0.4715 0.9345 0.052 Uiso 1 1 calc R . . C38 C 0.1793(3) 0.8816(2) 0.7306(2) 0.0265(7) Uani 1 1 d . . . C39 C 0.1446(3) 0.8454(3) 0.6587(2) 0.0325(8) Uani 1 1 d . . . H39 H 0.1720 0.7802 0.6397 0.039 Uiso 1 1 calc R . . C40 C 0.0703(3) 0.9031(3) 0.6137(2) 0.0380(8) Uani 1 1 d . . . H40 H 0.0467 0.8773 0.5646 0.046 Uiso 1 1 calc R . . C41 C 0.0311(3) 0.9975(3) 0.6407(2) 0.0375(9) Uani 1 1 d . . . H41 H -0.0185 1.0375 0.6095 0.045 Uiso 1 1 calc R . . C42 C 0.0635(4) 1.0344(3) 0.7129(2) 0.0398(9) Uani 1 1 d . . . H42 H 0.0349 1.0993 0.7320 0.048 Uiso 1 1 calc R . . C43 C 0.1375(3) 0.9769(3) 0.7573(2) 0.0335(8) Uani 1 1 d . . . H43 H 0.1601 1.0028 0.8067 0.040 Uiso 1 1 calc R . . C44 C 0.2561(3) 0.8565(2) 0.8909(2) 0.0270(7) Uani 1 1 d . . . C45 C 0.1257(3) 0.8554(3) 0.9428(2) 0.0362(8) Uani 1 1 d . . . H45 H 0.0568 0.8268 0.9218 0.043 Uiso 1 1 calc R . . C46 C 0.0952(4) 0.8959(3) 1.0252(2) 0.0411(9) Uani 1 1 d . . . H46 H 0.0057 0.8955 1.0600 0.049 Uiso 1 1 calc R . . C47 C 0.1953(4) 0.9367(3) 1.0561(2) 0.0404(9) Uani 1 1 d . . . H47 H 0.1750 0.9647 1.1122 0.048 Uiso 1 1 calc R . . C48 C 0.3237(4) 0.9365(3) 1.0058(2) 0.0440(9) Uani 1 1 d . . . H48 H 0.3926 0.9638 1.0277 0.053 Uiso 1 1 calc R . . C49 C 0.3555(3) 0.8973(3) 0.9232(2) 0.0342(8) Uani 1 1 d . . . H49 H 0.4453 0.8984 0.8889 0.041 Uiso 1 1 calc R . . B1 B 0.7990(5) 0.2669(3) 0.6106(3) 0.0449(11) Uani 1 1 d . . . F1 F 0.6928(3) 0.27143(19) 0.68165(18) 0.0777(9) Uani 1 1 d . . . F2 F 0.8412(3) 0.36295(18) 0.5857(2) 0.0792(9) Uani 1 1 d . . . F3 F 0.7554(3) 0.2223(2) 0.5453(2) 0.0939(11) Uani 1 1 d . . . F4 F 0.8987(4) 0.2139(2) 0.6254(3) 0.1306(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02036(7) 0.02299(8) 0.02237(7) 0.00204(5) -0.00337(5) 0.00300(5) P1 0.0215(4) 0.0249(4) 0.0244(4) 0.0008(3) -0.0035(3) 0.0036(3) N1 0.0353(15) 0.0275(15) 0.0218(14) 0.0008(11) -0.0063(12) 0.0095(12) N2 0.0299(14) 0.0271(15) 0.0230(14) -0.0003(11) -0.0065(11) 0.0048(11) C1 0.0208(15) 0.0246(16) 0.0209(15) 0.0004(12) -0.0021(12) 0.0027(12) C2 0.056(2) 0.030(2) 0.0298(19) 0.0044(15) -0.0107(17) 0.0160(17) C3 0.049(2) 0.0227(18) 0.0353(19) -0.0006(14) -0.0136(17) 0.0072(15) C4 0.041(2) 0.0303(18) 0.0215(16) 0.0005(14) -0.0101(15) 0.0141(15) C5 0.045(2) 0.037(2) 0.0229(17) 0.0090(15) -0.0048(15) 0.0148(16) C6 0.061(3) 0.045(2) 0.0206(18) 0.0063(16) 0.0006(17) 0.022(2) C7 0.080(3) 0.036(2) 0.0252(19) -0.0020(16) -0.016(2) 0.023(2) C8 0.056(2) 0.042(2) 0.035(2) -0.0040(17) -0.0230(19) 0.0113(19) C9 0.041(2) 0.038(2) 0.0271(18) -0.0004(15) -0.0107(16) 0.0134(16) C10 0.048(2) 0.064(3) 0.037(2) 0.013(2) -0.0030(19) 0.004(2) C11 0.122(5) 0.056(3) 0.028(2) -0.011(2) -0.023(3) 0.021(3) C12 0.033(2) 0.067(3) 0.045(2) -0.006(2) -0.0142(18) 0.0151(19) C13 0.0355(18) 0.0221(17) 0.0235(16) -0.0023(13) -0.0065(14) 0.0050(13) C14 0.0322(18) 0.0273(18) 0.0279(17) -0.0047(14) -0.0072(14) 0.0079(14) C15 0.0361(19) 0.035(2) 0.0282(18) -0.0029(15) -0.0027(15) 0.0068(15) C16 0.047(2) 0.036(2) 0.0258(18) -0.0053(15) -0.0086(16) 0.0117(17) C17 0.041(2) 0.040(2) 0.0305(18) -0.0078(16) -0.0149(16) 0.0102(16) C18 0.0330(18) 0.0268(18) 0.0291(17) -0.0079(14) -0.0077(14) 0.0078(14) C19 0.0329(19) 0.042(2) 0.0340(19) -0.0035(16) -0.0065(15) 0.0098(16) C20 0.058(3) 0.070(3) 0.029(2) 0.0031(19) -0.0087(19) 0.020(2) C21 0.0327(19) 0.046(2) 0.034(2) -0.0114(17) -0.0076(16) 0.0025(16) C22 0.0159(15) 0.0311(18) 0.0287(17) 0.0012(14) -0.0013(13) -0.0013(13) C23 0.0221(16) 0.0349(19) 0.0313(18) -0.0004(14) -0.0046(14) -0.0028(14) C24 0.0326(19) 0.038(2) 0.036(2) -0.0079(16) -0.0033(15) -0.0050(15) C25 0.038(2) 0.0260(18) 0.039(2) -0.0007(15) -0.0012(16) 0.0002(15) C26 0.0294(18) 0.0265(18) 0.0325(18) 0.0078(14) 0.0004(14) 0.0028(14) C27 0.0303(17) 0.0236(17) 0.0274(17) 0.0107(13) -0.0063(14) -0.0011(13) C28 0.0384(19) 0.0314(19) 0.0258(17) 0.0030(14) -0.0066(15) 0.0050(15) C29 0.0320(18) 0.0336(19) 0.0269(17) 0.0012(14) -0.0005(14) -0.0023(15) C30 0.0252(16) 0.0292(18) 0.0282(17) 0.0005(14) -0.0056(14) 0.0051(14) C31 0.0267(17) 0.0301(19) 0.0307(18) 0.0000(14) -0.0039(14) 0.0061(14) C32 0.0266(17) 0.0264(18) 0.042(2) -0.0023(15) -0.0020(15) 0.0014(14) C33 0.039(2) 0.036(2) 0.059(3) -0.0096(18) -0.0174(19) 0.0071(17) C34 0.041(2) 0.047(3) 0.079(3) -0.023(2) -0.020(2) 0.0029(19) C35 0.041(2) 0.036(2) 0.087(4) -0.010(2) 0.005(2) -0.0074(19) C36 0.063(3) 0.043(3) 0.057(3) 0.008(2) 0.002(2) -0.011(2) C37 0.044(2) 0.042(2) 0.039(2) 0.0022(17) -0.0026(18) -0.0086(18) C38 0.0204(15) 0.0291(18) 0.0281(17) 0.0031(13) -0.0036(13) 0.0034(13) C39 0.0254(17) 0.037(2) 0.0341(19) 0.0005(15) -0.0055(14) 0.0042(14) C40 0.0297(19) 0.052(2) 0.0321(19) 0.0047(17) -0.0088(15) 0.0009(16) C41 0.0228(17) 0.048(2) 0.038(2) 0.0135(17) -0.0044(15) 0.0069(16) C42 0.0314(19) 0.038(2) 0.045(2) 0.0047(17) -0.0012(17) 0.0128(16) C43 0.0280(18) 0.036(2) 0.0336(19) -0.0015(15) -0.0029(15) 0.0060(15) C44 0.0293(17) 0.0251(17) 0.0247(16) 0.0015(13) -0.0040(14) 0.0028(13) C45 0.0288(18) 0.043(2) 0.0338(19) -0.0037(16) -0.0026(15) -0.0015(15) C46 0.036(2) 0.051(2) 0.0298(19) -0.0028(17) 0.0038(16) 0.0028(17) C47 0.049(2) 0.039(2) 0.0284(19) -0.0046(16) -0.0018(17) 0.0004(17) C48 0.045(2) 0.052(2) 0.037(2) -0.0094(18) -0.0120(18) -0.0077(19) C49 0.0283(18) 0.040(2) 0.0316(19) -0.0020(15) -0.0020(15) -0.0007(15) B1 0.040(2) 0.031(2) 0.062(3) -0.011(2) -0.007(2) 0.0006(19) F1 0.089(2) 0.0522(16) 0.0691(18) -0.0164(14) 0.0233(15) -0.0198(15) F2 0.083(2) 0.0366(14) 0.093(2) -0.0062(14) 0.0220(16) -0.0115(13) F3 0.116(3) 0.091(2) 0.0659(19) -0.0264(17) -0.0033(18) -0.030(2) F4 0.096(3) 0.059(2) 0.260(5) -0.003(3) -0.089(3) 0.0302(19) _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 2.063(3) . ? Ir1 C27 2.157(3) . ? Ir1 C23 2.176(3) . ? Ir1 C22 2.213(3) . ? Ir1 C26 2.248(3) . ? Ir1 P1 2.3030(9) . ? P1 C30 1.773(3) . ? P1 C44 1.829(3) . ? P1 C38 1.837(3) . ? N1 C1 1.369(4) . ? N1 C2 1.390(4) . ? N1 C4 1.443(4) . ? N2 C1 1.364(4) . ? N2 C3 1.388(4) . ? N2 C13 1.453(4) . ? C2 C3 1.338(5) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.389(5) . ? C4 C9 1.392(5) . ? C5 C6 1.385(5) . ? C5 C10 1.500(5) . ? C6 C7 1.385(6) . ? C6 H6 0.9500 . ? C7 C8 1.377(6) . ? C7 C11 1.514(5) . ? C8 C9 1.397(5) . ? C8 H8 0.9500 . ? C9 C12 1.510(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 1.394(5) . ? C13 C18 1.396(5) . ? C14 C15 1.393(5) . ? C14 C19 1.506(5) . ? C15 C16 1.398(5) . ? C15 H15 0.9500 . ? C16 C17 1.366(5) . ? C16 C20 1.514(5) . ? C17 C18 1.393(5) . ? C17 H17 0.9500 . ? C18 C21 1.495(5) . ? 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 1.406(4) . ? C22 C29 1.516(4) . ? C22 H22 0.9500 . ? C23 C24 1.497(5) . ? C23 H23 0.9500 . ? C24 C25 1.532(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.508(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.393(5) . ? C26 H26 0.9500 . ? C27 C28 1.500(4) . ? C27 H27 0.9500 . ? C28 C29 1.533(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.186(5) . ? C31 C32 1.440(5) . ? C32 C37 1.389(5) . ? C32 C33 1.396(5) . ? C33 C34 1.389(6) . ? C33 H33 0.9500 . ? C34 C35 1.377(7) . ? C34 H34 0.9500 . ? C35 C36 1.363(7) . ? C35 H35 0.9500 . ? C36 C37 1.373(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.385(5) . ? C38 C43 1.390(5) . ? C39 C40 1.390(5) . ? C39 H39 0.9500 . ? C40 C41 1.374(5) . ? C40 H40 0.9500 . ? C41 C42 1.381(5) . ? C41 H41 0.9500 . ? C42 C43 1.382(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.385(5) . ? C44 C45 1.391(5) . ? C45 C46 1.391(5) . ? C45 H45 0.9500 . ? C46 C47 1.379(5) . ? C46 H46 0.9500 . ? C47 C48 1.366(5) . ? C47 H47 0.9500 . ? C48 C49 1.386(5) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? B1 F4 1.316(5) . ? B1 F1 1.360(5) . ? B1 F2 1.370(5) . ? B1 F3 1.384(5) . ? 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 141.02(12) . . ? C1 Ir1 C23 98.53(12) . . ? C27 Ir1 C23 94.98(13) . . ? C1 Ir1 C22 88.44(12) . . ? C27 Ir1 C22 80.56(12) . . ? C23 Ir1 C22 37.35(11) . . ? C1 Ir1 C26 175.19(11) . . ? C27 Ir1 C26 36.80(12) . . ? C23 Ir1 C26 78.31(13) . . ? C22 Ir1 C26 86.87(12) . . ? C1 Ir1 P1 98.30(9) . . ? C27 Ir1 P1 96.69(9) . . ? C23 Ir1 P1 136.26(9) . . ? C22 Ir1 P1 171.94(9) . . ? C26 Ir1 P1 86.46(9) . . ? C30 P1 C44 101.18(15) . . ? C30 P1 C38 100.16(15) . . ? C44 P1 C38 102.48(15) . . ? C30 P1 Ir1 120.52(11) . . ? C44 P1 Ir1 112.96(11) . . ? C38 P1 Ir1 116.85(11) . . ? C1 N1 C2 110.7(3) . . ? C1 N1 C4 126.3(3) . . ? C2 N1 C4 122.0(3) . . ? C1 N2 C3 111.7(3) . . ? C1 N2 C13 124.9(3) . . ? C3 N2 C13 122.7(3) . . ? N2 C1 N1 103.7(3) . . ? N2 C1 Ir1 121.1(2) . . ? N1 C1 Ir1 135.2(2) . . ? C3 C2 N1 107.5(3) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 106.4(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? C5 C4 C9 122.3(3) . . ? C5 C4 N1 119.7(3) . . ? C9 C4 N1 117.8(3) . . ? C6 C5 C4 117.6(4) . . ? C6 C5 C10 121.0(3) . . ? C4 C5 C10 121.4(3) . . ? C7 C6 C5 121.9(4) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C8 C7 C6 119.0(4) . . ? C8 C7 C11 120.0(4) . . ? C6 C7 C11 121.0(4) . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C4 C9 C8 117.5(3) . . ? C4 C9 C12 123.2(3) . . ? C8 C9 C12 119.1(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 122.4(3) . . ? C14 C13 N2 117.9(3) . . ? C18 C13 N2 119.7(3) . . ? C15 C14 C13 117.6(3) . . ? C15 C14 C19 118.8(3) . . ? C13 C14 C19 123.6(3) . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 119.1(3) . . ? C17 C16 C20 120.5(3) . . ? C15 C16 C20 120.3(3) . . ? C16 C17 C18 122.2(3) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C13 117.2(3) . . ? C17 C18 C21 120.3(3) . . ? C13 C18 C21 122.5(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 109.4 . . ? 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 124.0(3) . . ? C23 C22 Ir1 69.89(17) . . ? C29 C22 Ir1 112.0(2) . . ? C23 C22 H22 118.0 . . ? C29 C22 H22 118.0 . . ? Ir1 C22 H22 88.1 . . ? C22 C23 C24 126.3(3) . . ? C22 C23 Ir1 72.75(18) . . ? C24 C23 Ir1 111.7(2) . . ? C22 C23 H23 116.9 . . ? C24 C23 H23 116.9 . . ? Ir1 C23 H23 85.4 . . ? C23 C24 C25 112.6(3) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C24 111.2(3) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 123.2(3) . . ? C27 C26 Ir1 68.05(18) . . ? C25 C26 Ir1 113.4(2) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? Ir1 C26 H26 88.6 . . ? C26 C27 C28 125.2(3) . . ? C26 C27 Ir1 75.15(19) . . ? C28 C27 Ir1 109.0(2) . . ? C26 C27 H27 117.4 . . ? C28 C27 H27 117.4 . . ? Ir1 C27 H27 85.7 . . ? C27 C28 C29 114.1(3) . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C22 C29 C28 111.9(3) . . ? C22 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C22 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 P1 176.2(3) . . ? C30 C31 C32 178.6(4) . . ? C37 C32 C33 119.1(3) . . ? C37 C32 C31 121.4(3) . . ? C33 C32 C31 119.5(3) . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 120.8(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 120.3(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.4(4) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C39 C38 C43 118.5(3) . . ? C39 C38 P1 119.3(2) . . ? C43 C38 P1 121.8(3) . . ? C38 C39 C40 120.8(3) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 119.7(3) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.2(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 119.9(3) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C38 120.8(3) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? C49 C44 C45 118.8(3) . . ? C49 C44 P1 121.3(3) . . ? C45 C44 P1 119.9(3) . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 119.8(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C47 C46 119.7(3) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 121.2(3) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C44 C49 C48 119.9(3) . . ? C44 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? F4 B1 F1 113.4(5) . . ? F4 B1 F2 109.5(4) . . ? F1 B1 F2 107.6(3) . . ? F4 B1 F3 108.2(4) . . ? F1 B1 F3 107.5(4) . . ? F2 B1 F3 110.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C30 -26.14(15) . . . . ? C27 Ir1 P1 C30 117.77(15) . . . . ? C23 Ir1 P1 C30 -137.81(18) . . . . ? C22 Ir1 P1 C30 -172.7(6) . . . . ? C26 Ir1 P1 C30 153.19(16) . . . . ? C1 Ir1 P1 C44 93.48(14) . . . . ? C27 Ir1 P1 C44 -122.61(14) . . . . ? C23 Ir1 P1 C44 -18.20(18) . . . . ? C22 Ir1 P1 C44 -53.0(6) . . . . ? C26 Ir1 P1 C44 -87.20(15) . . . . ? C1 Ir1 P1 C38 -148.00(15) . . . . ? C27 Ir1 P1 C38 -4.09(15) . . . . ? C23 Ir1 P1 C38 100.32(18) . . . . ? C22 Ir1 P1 C38 65.5(6) . . . . ? C26 Ir1 P1 C38 31.32(15) . . . . ? C3 N2 C1 N1 0.6(4) . . . . ? C13 N2 C1 N1 -169.8(3) . . . . ? C3 N2 C1 Ir1 -177.9(2) . . . . ? C13 N2 C1 Ir1 11.8(4) . . . . ? C2 N1 C1 N2 -0.2(4) . . . . ? C4 N1 C1 N2 168.6(3) . . . . ? C2 N1 C1 Ir1 177.9(3) . . . . ? C4 N1 C1 Ir1 -13.3(5) . . . . ? C27 Ir1 C1 N2 -3.5(4) . . . . ? C23 Ir1 C1 N2 -112.4(2) . . . . ? C22 Ir1 C1 N2 -76.3(3) . . . . ? C26 Ir1 C1 N2 -63.9(14) . . . . ? P1 Ir1 C1 N2 108.1(2) . . . . ? C27 Ir1 C1 N1 178.7(3) . . . . ? C23 Ir1 C1 N1 69.7(3) . . . . ? C22 Ir1 C1 N1 105.8(3) . . . . ? C26 Ir1 C1 N1 118.3(13) . . . . ? P1 Ir1 C1 N1 -69.8(3) . . . . ? C1 N1 C2 C3 -0.3(4) . . . . ? C4 N1 C2 C3 -169.6(3) . . . . ? N1 C2 C3 N2 0.6(4) . . . . ? C1 N2 C3 C2 -0.8(4) . . . . ? C13 N2 C3 C2 169.8(3) . . . . ? C1 N1 C4 C5 106.5(4) . . . . ? C2 N1 C4 C5 -85.9(4) . . . . ? C1 N1 C4 C9 -77.7(4) . . . . ? C2 N1 C4 C9 89.9(4) . . . . ? C9 C4 C5 C6 5.0(5) . . . . ? N1 C4 C5 C6 -179.5(3) . . . . ? C9 C4 C5 C10 -172.5(3) . . . . ? N1 C4 C5 C10 3.1(5) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C10 C5 C6 C7 176.7(3) . . . . ? C5 C6 C7 C8 -2.5(6) . . . . ? C5 C6 C7 C11 178.9(3) . . . . ? C6 C7 C8 C9 1.7(6) . . . . ? C11 C7 C8 C9 -179.7(3) . . . . ? C5 C4 C9 C8 -5.7(5) . . . . ? N1 C4 C9 C8 178.7(3) . . . . ? C5 C4 C9 C12 168.8(3) . . . . ? N1 C4 C9 C12 -6.8(5) . . . . ? C7 C8 C9 C4 2.3(5) . . . . ? C7 C8 C9 C12 -172.5(4) . . . . ? C1 N2 C13 C14 97.3(4) . . . . ? C3 N2 C13 C14 -72.1(4) . . . . ? C1 N2 C13 C18 -84.6(4) . . . . ? C3 N2 C13 C18 106.0(4) . . . . ? C18 C13 C14 C15 6.1(5) . . . . ? N2 C13 C14 C15 -175.9(3) . . . . ? C18 C13 C14 C19 -172.9(3) . . . . ? N2 C13 C14 C19 5.2(5) . . . . ? C13 C14 C15 C16 -2.4(5) . . . . ? C19 C14 C15 C16 176.6(3) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C14 C15 C16 C20 176.6(3) . . . . ? C15 C16 C17 C18 2.0(5) . . . . ? C20 C16 C17 C18 -176.1(3) . . . . ? C16 C17 C18 C13 1.4(5) . . . . ? C16 C17 C18 C21 -178.0(3) . . . . ? C14 C13 C18 C17 -5.6(5) . . . . ? N2 C13 C18 C17 176.4(3) . . . . ? C14 C13 C18 C21 173.8(3) . . . . ? N2 C13 C18 C21 -4.3(5) . . . . ? C1 Ir1 C22 C23 -106.3(2) . . . . ? C27 Ir1 C22 C23 111.3(2) . . . . ? C26 Ir1 C22 C23 74.8(2) . . . . ? P1 Ir1 C22 C23 40.6(7) . . . . ? C1 Ir1 C22 C29 134.1(2) . . . . ? C27 Ir1 C22 C29 -8.3(2) . . . . ? C23 Ir1 C22 C29 -119.6(3) . . . . ? C26 Ir1 C22 C29 -44.8(2) . . . . ? P1 Ir1 C22 C29 -79.0(6) . . . . ? C29 C22 C23 C24 -1.0(5) . . . . ? Ir1 C22 C23 C24 -104.6(3) . . . . ? C29 C22 C23 Ir1 103.6(3) . . . . ? C1 Ir1 C23 C22 76.0(2) . . . . ? C27 Ir1 C23 C22 -67.3(2) . . . . ? C26 Ir1 C23 C22 -100.3(2) . . . . ? P1 Ir1 C23 C22 -172.41(14) . . . . ? C1 Ir1 C23 C24 -161.1(2) . . . . ? C27 Ir1 C23 C24 55.5(2) . . . . ? C22 Ir1 C23 C24 122.9(3) . . . . ? C26 Ir1 C23 C24 22.6(2) . . . . ? P1 Ir1 C23 C24 -49.5(3) . . . . ? C22 C23 C24 C25 44.6(4) . . . . ? Ir1 C23 C24 C25 -39.4(3) . . . . ? C23 C24 C25 C26 36.6(4) . . . . ? C24 C25 C26 C27 -95.0(4) . . . . ? C24 C25 C26 Ir1 -16.8(4) . . . . ? C1 Ir1 C26 C27 65.9(14) . . . . ? C23 Ir1 C26 C27 115.1(2) . . . . ? C22 Ir1 C26 C27 78.4(2) . . . . ? P1 Ir1 C26 C27 -106.11(19) . . . . ? C1 Ir1 C26 C25 -52.1(15) . . . . ? C27 Ir1 C26 C25 -118.0(3) . . . . ? C23 Ir1 C26 C25 -2.9(2) . . . . ? C22 Ir1 C26 C25 -39.6(2) . . . . ? P1 Ir1 C26 C25 135.9(2) . . . . ? C25 C26 C27 C28 1.3(5) . . . . ? Ir1 C26 C27 C28 -103.0(3) . . . . ? C25 C26 C27 Ir1 104.3(3) . . . . ? C1 Ir1 C27 C26 -173.01(18) . . . . ? C23 Ir1 C27 C26 -62.9(2) . . . . ? C22 Ir1 C27 C26 -97.5(2) . . . . ? P1 Ir1 C27 C26 74.90(19) . . . . ? C1 Ir1 C27 C28 -50.3(3) . . . . ? C23 Ir1 C27 C28 59.8(2) . . . . ? C22 Ir1 C27 C28 25.2(2) . . . . ? C26 Ir1 C27 C28 122.7(3) . . . . ? P1 Ir1 C27 C28 -162.4(2) . . . . ? C26 C27 C28 C29 45.5(4) . . . . ? Ir1 C27 C28 C29 -39.4(3) . . . . ? C23 C22 C29 C28 -90.1(4) . . . . ? Ir1 C22 C29 C28 -10.1(3) . . . . ? C27 C28 C29 C22 33.0(4) . . . . ? C44 P1 C30 C31 -154(5) . . . . ? C38 P1 C30 C31 101(5) . . . . ? Ir1 P1 C30 C31 -29(5) . . . . ? P1 C30 C31 C32 -86(17) . . . . ? C30 C31 C32 C37 -158(16) . . . . ? C30 C31 C32 C33 21(16) . . . . ? C37 C32 C33 C34 0.7(5) . . . . ? C31 C32 C33 C34 -177.6(3) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C33 C34 C35 C36 -0.6(7) . . . . ? C34 C35 C36 C37 1.3(7) . . . . ? C35 C36 C37 C32 -1.0(7) . . . . ? C33 C32 C37 C36 -0.1(6) . . . . ? C31 C32 C37 C36 178.2(4) . . . . ? C30 P1 C38 C39 -54.6(3) . . . . ? C44 P1 C38 C39 -158.6(3) . . . . ? Ir1 P1 C38 C39 77.4(3) . . . . ? C30 P1 C38 C43 131.9(3) . . . . ? C44 P1 C38 C43 27.9(3) . . . . ? Ir1 P1 C38 C43 -96.1(3) . . . . ? C43 C38 C39 C40 0.3(5) . . . . ? P1 C38 C39 C40 -173.4(3) . . . . ? C38 C39 C40 C41 0.3(5) . . . . ? C39 C40 C41 C42 -1.0(5) . . . . ? C40 C41 C42 C43 1.1(5) . . . . ? C41 C42 C43 C38 -0.4(5) . . . . ? C39 C38 C43 C42 -0.3(5) . . . . ? P1 C38 C43 C42 173.3(3) . . . . ? C30 P1 C44 C49 133.7(3) . . . . ? C38 P1 C44 C49 -123.1(3) . . . . ? Ir1 P1 C44 C49 3.4(3) . . . . ? C30 P1 C44 C45 -48.5(3) . . . . ? C38 P1 C44 C45 54.6(3) . . . . ? Ir1 P1 C44 C45 -178.8(2) . . . . ? C49 C44 C45 C46 0.9(5) . . . . ? P1 C44 C45 C46 -176.9(3) . . . . ? C44 C45 C46 C47 -0.6(6) . . . . ? C45 C46 C47 C48 -0.3(6) . . . . ? C46 C47 C48 C49 0.9(6) . . . . ? C45 C44 C49 C48 -0.4(5) . . . . ? P1 C44 C49 C48 177.5(3) . . . . ? C47 C48 C49 C44 -0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.369 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.092 # Attachment '- Hope_10.cif' data_05055 _database_code_depnum_ccdc_archive 'CCDC 723143' _publ_section_title_footnote # remove if not required . #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H29 N3 O2 Ir)+ (B F4)-' _chemical_formula_sum 'C28 H29 B F4 Ir N3 O2' _chemical_formula_weight 718.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8033(18) _cell_length_b 15.976(3) _cell_length_c 16.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2781.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26.94 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 4.857 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 16919 reflections (SADABS); Rint 0.117 before correction and 0.053 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23340 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6030 _reflns_number_gt 5485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(7) _refine_ls_number_reflns 6030 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 0.625769(17) 0.144088(10) 0.790051(10) 0.02396(5) Uani 1 1 d . . . N1 N 0.8653(4) 0.1372(2) 0.6835(2) 0.0252(7) Uani 1 1 d . . . N2 N 0.7234(3) 0.0626(2) 0.6280(2) 0.0227(7) Uani 1 1 d . . . N3 N 0.4853(3) 0.1694(2) 0.7025(3) 0.0279(9) Uani 1 1 d . . . O1 O 0.8063(3) 0.0987(3) 0.9216(2) 0.0536(11) Uani 1 1 d . . . O2 O 0.4433(3) 0.1970(3) 0.9227(2) 0.0497(10) Uani 1 1 d . . . C1 C 0.7419(4) 0.1179(3) 0.8696(3) 0.0310(11) Uani 1 1 d . . . C2 C 0.5106(4) 0.1756(3) 0.8729(3) 0.0313(11) Uani 1 1 d . . . C3 C 0.7460(4) 0.1121(3) 0.6947(3) 0.0225(10) Uani 1 1 d . . . C4 C 0.9131(4) 0.1049(3) 0.6105(3) 0.0297(11) Uani 1 1 d . . . H4 H 0.9935 0.1147 0.5887 0.036 Uiso 1 1 calc R . . C5 C 0.8254(4) 0.0577(3) 0.5767(3) 0.0286(10) Uani 1 1 d . . . H5 H 0.8318 0.0265 0.5267 0.034 Uiso 1 1 calc R . . C6 C 0.9396(4) 0.1849(3) 0.7422(3) 0.0237(10) Uani 1 1 d . . . C7 C 1.0237(4) 0.1399(3) 0.7904(3) 0.0290(9) Uani 1 1 d . . . C8 C 1.0957(4) 0.1847(3) 0.8467(3) 0.0333(11) Uani 1 1 d . . . H8 H 1.1540 0.1557 0.8802 0.040 Uiso 1 1 calc R . . C9 C 1.0840(4) 0.2706(3) 0.8547(3) 0.0313(11) Uani 1 1 d . . . C10 C 1.0003(4) 0.3123(3) 0.8044(3) 0.0334(11) Uani 1 1 d . . . H10 H 0.9930 0.3713 0.8095 0.040 Uiso 1 1 calc R . . C11 C 0.9267(4) 0.2710(3) 0.7467(3) 0.0298(10) Uani 1 1 d . . . C12 C 1.0355(4) 0.0460(3) 0.7850(4) 0.0355(11) Uani 1 1 d . . . H12A H 0.9572 0.0199 0.8015 0.053 Uiso 1 1 calc R . . H12B H 1.1017 0.0271 0.8221 0.053 Uiso 1 1 calc R . . H12C H 1.0554 0.0300 0.7278 0.053 Uiso 1 1 calc R . . C13 C 1.1602(5) 0.3172(3) 0.9182(3) 0.0413(14) Uani 1 1 d . . . H13A H 1.2445 0.3249 0.8971 0.062 Uiso 1 1 calc R . . H13B H 1.1630 0.2849 0.9699 0.062 Uiso 1 1 calc R . . H13C H 1.1227 0.3720 0.9289 0.062 Uiso 1 1 calc R . . C14 C 0.8345(4) 0.3178(3) 0.6953(3) 0.0395(13) Uani 1 1 d . . . H14A H 0.8360 0.2963 0.6383 0.059 Uiso 1 1 calc R . . H14B H 0.8554 0.3775 0.6951 0.059 Uiso 1 1 calc R . . H14C H 0.7515 0.3101 0.7187 0.059 Uiso 1 1 calc R . . C15 C 0.6126(4) 0.0135(2) 0.6152(2) 0.0240(9) Uani 1 1 d . . . C16 C 0.5864(4) -0.0511(3) 0.6704(3) 0.0281(10) Uani 1 1 d . . . C17 C 0.4780(4) -0.0960(3) 0.6571(3) 0.0336(11) Uani 1 1 d . . . H17 H 0.4570 -0.1399 0.6943 0.040 Uiso 1 1 calc R . . C18 C 0.4002(4) -0.0788(3) 0.5918(3) 0.0378(13) Uani 1 1 d . . . C19 C 0.4324(4) -0.0160(3) 0.5358(3) 0.0351(11) Uani 1 1 d . . . H19 H 0.3803 -0.0052 0.4895 0.042 Uiso 1 1 calc R . . C20 C 0.5390(4) 0.0311(3) 0.5464(3) 0.0284(10) Uani 1 1 d . . . C21 C 0.6706(4) -0.0745(3) 0.7417(3) 0.0355(11) Uani 1 1 d . . . H21A H 0.6415 -0.0474 0.7926 0.053 Uiso 1 1 calc R . . H21B H 0.7551 -0.0560 0.7295 0.053 Uiso 1 1 calc R . . H21C H 0.6697 -0.1354 0.7491 0.053 Uiso 1 1 calc R . . C22 C 0.2794(5) -0.1267(4) 0.5817(4) 0.0564(17) Uani 1 1 d . . . H22A H 0.2844 -0.1796 0.6122 0.085 Uiso 1 1 calc R . . H22B H 0.2652 -0.1382 0.5227 0.085 Uiso 1 1 calc R . . H22C H 0.2109 -0.0931 0.6035 0.085 Uiso 1 1 calc R . . C23 C 0.5718(5) 0.0980(3) 0.4851(3) 0.0381(13) Uani 1 1 d . . . H23A H 0.6064 0.1463 0.5144 0.057 Uiso 1 1 calc R . . H23B H 0.4973 0.1151 0.4548 0.057 Uiso 1 1 calc R . . H23C H 0.6331 0.0763 0.4458 0.057 Uiso 1 1 calc R . . C24 C 0.4909(5) 0.2351(3) 0.6514(3) 0.0346(11) Uani 1 1 d . . . H24 H 0.5617 0.2703 0.6530 0.042 Uiso 1 1 calc R . . C25 C 0.3969(5) 0.2533(3) 0.5964(3) 0.0432(13) Uani 1 1 d . . . H25 H 0.4030 0.3005 0.5608 0.052 Uiso 1 1 calc R . . C26 C 0.2949(5) 0.2027(4) 0.5935(4) 0.0477(15) Uani 1 1 d . . . H26 H 0.2294 0.2140 0.5558 0.057 Uiso 1 1 calc R . . C27 C 0.2886(4) 0.1351(4) 0.6464(4) 0.0463(14) Uani 1 1 d . . . H27 H 0.2189 0.0989 0.6451 0.056 Uiso 1 1 calc R . . C28 C 0.3839(5) 0.1200(3) 0.7012(3) 0.0387(11) Uani 1 1 d . . . H28 H 0.3782 0.0742 0.7386 0.046 Uiso 1 1 calc R . . B1 B 0.1012(5) 0.0372(4) 0.4266(4) 0.0423(15) Uani 1 1 d . . . F1 F 0.1852(3) -0.0120(3) 0.3903(3) 0.0771(12) Uani 1 1 d . A . F2 F 0.1286(12) 0.1233(6) 0.4406(7) 0.073(3) Uani 0.50 1 d P A 1 F3 F 0.1195(9) 0.0125(5) 0.5177(4) 0.073(2) Uani 0.50 1 d P A 1 F4 F -0.0195(11) 0.0314(8) 0.4182(8) 0.075(4) Uani 0.50 1 d P A 1 F2' F 0.1490(10) 0.0907(7) 0.4773(6) 0.071(3) Uani 0.50 1 d P A 2 F3' F 0.0696(8) 0.0795(5) 0.3503(5) 0.087(3) Uani 0.50 1 d P A 2 F4' F 0.0030(11) -0.0051(7) 0.4492(8) 0.078(4) Uani 0.50 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 0.02387(8) 0.02545(7) 0.02257(8) -0.00003(8) 0.00213(8) 0.00154(8) N1 0.0246(17) 0.0242(17) 0.0269(18) 0.0015(15) -0.0006(17) 0.003(2) N2 0.0216(18) 0.0263(18) 0.0202(19) 0.0017(16) 0.0003(15) 0.0006(15) N3 0.0223(18) 0.035(2) 0.026(2) -0.0026(19) 0.0016(17) 0.0027(15) O1 0.047(2) 0.085(3) 0.029(2) 0.006(2) 0.0012(17) 0.026(2) O2 0.044(2) 0.062(3) 0.043(2) -0.007(2) 0.0137(19) 0.0116(19) C1 0.031(3) 0.036(3) 0.026(3) 0.004(2) 0.008(2) 0.011(2) C2 0.027(2) 0.033(2) 0.033(3) 0.004(2) 0.000(2) 0.004(2) C3 0.022(2) 0.022(2) 0.024(3) 0.0049(18) 0.0004(17) 0.0001(17) C4 0.027(2) 0.033(2) 0.029(3) 0.005(2) 0.0052(18) -0.0017(19) C5 0.031(2) 0.032(3) 0.023(2) 0.002(2) 0.0058(18) 0.002(2) C6 0.021(2) 0.026(2) 0.024(2) 0.0013(19) 0.0032(18) -0.0034(18) C7 0.029(2) 0.025(2) 0.033(2) 0.000(3) 0.000(2) -0.0017(19) C8 0.025(3) 0.037(3) 0.038(3) 0.001(2) -0.0050(19) 0.0007(19) C9 0.030(2) 0.030(2) 0.035(3) -0.005(2) 0.0023(19) -0.0058(19) C10 0.032(2) 0.022(2) 0.046(3) 0.000(2) 0.003(2) -0.0044(19) C11 0.027(2) 0.029(2) 0.034(3) 0.005(2) 0.005(2) -0.0017(19) C12 0.036(3) 0.030(2) 0.040(3) -0.003(3) -0.008(2) 0.0042(19) C13 0.041(3) 0.039(3) 0.044(3) 0.000(2) -0.006(2) -0.009(2) C14 0.042(3) 0.031(2) 0.045(3) 0.006(2) -0.002(2) -0.002(2) C15 0.027(2) 0.0240(19) 0.021(2) -0.0025(16) 0.002(2) -0.003(2) C16 0.032(3) 0.026(2) 0.026(2) -0.002(2) 0.0025(18) 0.0011(19) C17 0.039(3) 0.032(3) 0.029(3) 0.004(2) 0.004(2) -0.008(2) C18 0.033(3) 0.044(3) 0.036(3) -0.004(2) 0.001(2) -0.014(2) C19 0.032(3) 0.044(3) 0.030(3) -0.004(2) -0.006(2) 0.000(2) C20 0.031(2) 0.033(3) 0.022(3) -0.004(2) -0.0007(19) 0.000(2) C21 0.044(3) 0.030(3) 0.033(3) 0.003(2) -0.001(2) -0.001(2) C22 0.042(3) 0.069(4) 0.058(4) 0.003(3) -0.007(3) -0.028(3) C23 0.040(3) 0.040(3) 0.034(3) 0.003(2) -0.004(2) -0.001(2) C24 0.036(3) 0.033(3) 0.035(3) -0.002(2) -0.001(2) 0.003(2) C25 0.049(4) 0.044(3) 0.038(3) 0.003(2) -0.011(2) 0.012(3) C26 0.036(3) 0.063(4) 0.044(4) -0.008(3) -0.013(2) 0.010(3) C27 0.025(2) 0.062(4) 0.052(4) -0.001(3) -0.008(2) 0.000(3) C28 0.027(2) 0.054(3) 0.035(3) -0.001(2) 0.000(3) 0.001(3) B1 0.030(4) 0.036(3) 0.060(4) -0.002(3) -0.001(3) 0.002(3) F1 0.063(2) 0.094(3) 0.074(3) -0.029(2) 0.019(2) 0.008(2) F2 0.077(6) 0.047(5) 0.094(8) 0.009(4) 0.002(7) -0.008(5) F3 0.082(5) 0.084(5) 0.052(4) 0.007(4) 0.008(5) 0.041(5) F4 0.041(5) 0.114(11) 0.071(8) -0.039(7) -0.011(5) 0.002(7) F2' 0.054(6) 0.087(8) 0.072(7) -0.047(6) -0.011(5) -0.010(6) F3' 0.107(6) 0.069(5) 0.085(6) 0.042(5) -0.037(5) 0.000(4) F4' 0.070(9) 0.066(7) 0.099(11) -0.041(6) 0.063(8) -0.024(6) _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 1.842(5) . ? Ir1 C2 1.894(5) . ? Ir1 C3 2.076(4) . ? Ir1 N3 2.112(4) . ? N1 C3 1.361(6) . ? N1 C4 1.384(6) . ? N1 C6 1.456(6) . ? N2 C3 1.357(6) . ? N2 C5 1.381(5) . ? N2 C15 1.446(6) . ? N3 C24 1.336(6) . ? N3 C28 1.349(6) . ? O1 C1 1.132(6) . ? O2 C2 1.135(6) . ? C4 C5 1.327(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.386(6) . ? C6 C7 1.394(6) . ? C7 C8 1.393(6) . ? C7 C12 1.508(6) . ? C8 C9 1.384(6) . ? C8 H8 0.9500 . ? C9 C10 1.385(6) . ? C9 C13 1.510(6) . ? C10 C11 1.389(6) . ? C10 H10 0.9500 . ? C11 C14 1.496(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.392(6) . ? C15 C20 1.394(6) . ? C16 C17 1.390(6) . ? C16 C21 1.512(6) . ? C17 C18 1.375(7) . ? C17 H17 0.9500 . ? C18 C19 1.394(7) . ? C18 C22 1.521(7) . ? C19 C20 1.387(7) . ? C19 H19 0.9500 . ? C20 C23 1.497(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.378(6) . ? C24 H24 0.9500 . ? C25 C26 1.368(8) . ? C25 H25 0.9500 . ? C26 C27 1.378(8) . ? C26 H26 0.9500 . ? C27 C28 1.377(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? B1 F2' 1.290(11) . ? B1 F4' 1.309(13) . ? B1 F4 1.314(13) . ? B1 F1 1.335(7) . ? B1 F2 1.425(11) . ? B1 F3' 1.444(9) . ? B1 F3 1.533(9) . ? 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 C2 91.0(2) . . ? C1 Ir1 C3 91.89(17) . . ? C2 Ir1 C3 177.12(19) . . ? C1 Ir1 N3 176.63(18) . . ? C2 Ir1 N3 87.05(17) . . ? C3 Ir1 N3 90.14(16) . . ? C3 N1 C4 110.9(4) . . ? C3 N1 C6 126.1(4) . . ? C4 N1 C6 122.8(4) . . ? C3 N2 C5 111.3(4) . . ? C3 N2 C15 125.3(4) . . ? C5 N2 C15 123.1(4) . . ? C24 N3 C28 119.1(4) . . ? C24 N3 Ir1 122.0(3) . . ? C28 N3 Ir1 118.8(3) . . ? O1 C1 Ir1 174.8(4) . . ? O2 C2 Ir1 177.7(4) . . ? N2 C3 N1 103.7(4) . . ? N2 C3 Ir1 128.1(3) . . ? N1 C3 Ir1 128.2(3) . . ? C5 C4 N1 107.1(4) . . ? C5 C4 H4 126.4 . . ? N1 C4 H4 126.4 . . ? C4 C5 N2 106.9(4) . . ? C4 C5 H5 126.5 . . ? N2 C5 H5 126.5 . . ? C11 C6 C7 123.3(4) . . ? C11 C6 N1 119.9(4) . . ? C7 C6 N1 116.9(4) . . ? C8 C7 C6 117.5(4) . . ? C8 C7 C12 120.1(4) . . ? C6 C7 C12 122.4(4) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 118.8(4) . . ? C8 C9 C13 120.1(4) . . ? C10 C9 C13 121.1(4) . . ? C9 C10 C11 122.5(4) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C6 C11 C10 116.7(4) . . ? C6 C11 C14 122.3(4) . . ? C10 C11 C14 121.0(4) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 122.9(4) . . ? C16 C15 N2 118.6(4) . . ? C20 C15 N2 118.5(4) . . ? C17 C16 C15 117.1(4) . . ? C17 C16 C21 119.7(4) . . ? C15 C16 C21 123.2(4) . . ? C18 C17 C16 122.0(4) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 C22 120.4(5) . . ? C19 C18 C22 120.4(5) . . ? C20 C19 C18 121.3(5) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C15 117.5(4) . . ? C19 C20 C23 120.2(5) . . ? C15 C20 C23 122.3(4) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C25 121.9(5) . . ? N3 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 119.4(5) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 118.8(5) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 119.8(5) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? N3 C28 C27 120.9(5) . . ? N3 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? F2' B1 F4' 119.3(9) . . ? F2' B1 F4 120.6(9) . . ? F4' B1 F4 35.8(6) . . ? F2' B1 F1 113.3(7) . . ? F4' B1 F1 111.6(7) . . ? F4 B1 F1 126.0(8) . . ? F2' B1 F2 34.6(5) . . ? F4' B1 F2 128.5(9) . . ? F4 B1 F2 106.9(9) . . ? F1 B1 F2 119.8(7) . . ? F2' B1 F3' 108.9(7) . . ? F4' B1 F3' 106.7(8) . . ? F4 B1 F3' 73.2(7) . . ? F1 B1 F3' 93.6(6) . . ? F2 B1 F3' 74.5(6) . . ? F2' B1 F3 60.8(6) . . ? F4' B1 F3 72.9(8) . . ? F4 B1 F3 102.0(8) . . ? F1 B1 F3 100.4(5) . . ? F2 B1 F3 94.0(7) . . ? F3' B1 F3 165.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 N3 C24 163(3) . . . . ? C2 Ir1 N3 C24 109.5(4) . . . . ? C3 Ir1 N3 C24 -69.9(4) . . . . ? C1 Ir1 N3 C28 -13(3) . . . . ? C2 Ir1 N3 C28 -67.0(4) . . . . ? C3 Ir1 N3 C28 113.6(4) . . . . ? C2 Ir1 C1 O1 46(5) . . . . ? C3 Ir1 C1 O1 -134(5) . . . . ? N3 Ir1 C1 O1 -7(8) . . . . ? C1 Ir1 C2 O2 85(11) . . . . ? C3 Ir1 C2 O2 -85(12) . . . . ? N3 Ir1 C2 O2 -98(11) . . . . ? C5 N2 C3 N1 -0.4(5) . . . . ? C15 N2 C3 N1 173.4(4) . . . . ? C5 N2 C3 Ir1 178.3(3) . . . . ? C15 N2 C3 Ir1 -7.8(6) . . . . ? C4 N1 C3 N2 1.2(5) . . . . ? C6 N1 C3 N2 -173.4(4) . . . . ? C4 N1 C3 Ir1 -177.5(3) . . . . ? C6 N1 C3 Ir1 7.9(6) . . . . ? C1 Ir1 C3 N2 131.6(4) . . . . ? C2 Ir1 C3 N2 -58(4) . . . . ? N3 Ir1 C3 N2 -45.7(4) . . . . ? C1 Ir1 C3 N1 -50.0(4) . . . . ? C2 Ir1 C3 N1 121(4) . . . . ? N3 Ir1 C3 N1 132.7(4) . . . . ? C3 N1 C4 C5 -1.6(5) . . . . ? C6 N1 C4 C5 173.2(4) . . . . ? N1 C4 C5 N2 1.3(5) . . . . ? C3 N2 C5 C4 -0.5(5) . . . . ? C15 N2 C5 C4 -174.6(4) . . . . ? C3 N1 C6 C11 -81.5(6) . . . . ? C4 N1 C6 C11 104.5(5) . . . . ? C3 N1 C6 C7 99.9(5) . . . . ? C4 N1 C6 C7 -74.1(5) . . . . ? C11 C6 C7 C8 1.3(7) . . . . ? N1 C6 C7 C8 179.8(4) . . . . ? C11 C6 C7 C12 179.5(5) . . . . ? N1 C6 C7 C12 -2.0(6) . . . . ? C6 C7 C8 C9 0.2(7) . . . . ? C12 C7 C8 C9 -178.1(5) . . . . ? C7 C8 C9 C10 -1.1(7) . . . . ? C7 C8 C9 C13 177.9(4) . . . . ? C8 C9 C10 C11 0.7(7) . . . . ? C13 C9 C10 C11 -178.4(4) . . . . ? C7 C6 C11 C10 -1.7(7) . . . . ? N1 C6 C11 C10 179.8(4) . . . . ? C7 C6 C11 C14 -179.0(4) . . . . ? N1 C6 C11 C14 2.5(7) . . . . ? C9 C10 C11 C6 0.7(7) . . . . ? C9 C10 C11 C14 178.1(4) . . . . ? C3 N2 C15 C16 -63.9(6) . . . . ? C5 N2 C15 C16 109.2(5) . . . . ? C3 N2 C15 C20 118.3(5) . . . . ? C5 N2 C15 C20 -68.5(6) . . . . ? C20 C15 C16 C17 -3.5(7) . . . . ? N2 C15 C16 C17 178.9(4) . . . . ? C20 C15 C16 C21 175.4(4) . . . . ? N2 C15 C16 C21 -2.2(6) . . . . ? C15 C16 C17 C18 1.0(7) . . . . ? C21 C16 C17 C18 -178.0(5) . . . . ? C16 C17 C18 C19 1.7(7) . . . . ? C16 C17 C18 C22 -177.1(5) . . . . ? C17 C18 C19 C20 -2.1(8) . . . . ? C22 C18 C19 C20 176.8(5) . . . . ? C18 C19 C20 C15 -0.2(7) . . . . ? C18 C19 C20 C23 179.7(5) . . . . ? C16 C15 C20 C19 3.1(7) . . . . ? N2 C15 C20 C19 -179.3(4) . . . . ? C16 C15 C20 C23 -176.8(4) . . . . ? N2 C15 C20 C23 0.8(7) . . . . ? C28 N3 C24 C25 -1.0(7) . . . . ? Ir1 N3 C24 C25 -177.5(4) . . . . ? N3 C24 C25 C26 -0.2(8) . . . . ? C24 C25 C26 C27 0.4(8) . . . . ? C25 C26 C27 C28 0.5(8) . . . . ? C24 N3 C28 C27 2.0(7) . . . . ? Ir1 N3 C28 C27 178.6(4) . . . . ? C26 C27 C28 N3 -1.8(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.846 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.101 # Attachment '- Hope_8.cif' data_05059 _database_code_depnum_ccdc_archive 'CCDC 723144' _publ_section_title_footnote # remove if not required . #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H49 N3 Ir)+ 2(B F4)- 3(C H2 Cl2)' _chemical_formula_sum 'C83 H104 B2 Cl6 F8 Ir2 N6' _chemical_formula_weight 1956.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0104(17) _cell_length_b 19.823(3) _cell_length_c 21.835(3) _cell_angle_alpha 66.828(2) _cell_angle_beta 78.610(2) _cell_angle_gamma 78.803(2) _cell_volume 4258.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 23.25 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 3.373 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details ; absorption correction based on 18238 reflections (SADABS); Rint 0.073 before correction and 0.023 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35820 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.00 _reflns_number_total 18210 _reflns_number_gt 15146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The asymmetric unit has two unique metal cations, two unique BF4- ions and three lattice CH2Cl2 molecules. One of the solvent molecules has Cl atoms disordered over three sites, the highest residual e density peak is associated with this disorder. 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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18210 _refine_ls_number_parameters 989 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.283883(14) 0.546473(9) 0.272634(8) 0.02255(5) Uani 1 1 d . . . N1 N 0.5020(3) 0.63874(19) 0.24673(17) 0.0219(7) Uani 1 1 d . . . N2 N 0.3286(3) 0.69359(18) 0.27825(17) 0.0213(7) Uani 1 1 d . . . N3 N 0.1682(4) 0.6100(2) 0.19835(19) 0.0306(9) Uani 1 1 d . . . C1 C 0.3782(4) 0.6321(2) 0.2626(2) 0.0214(9) Uani 1 1 d . . . C2 C 0.5285(4) 0.7012(2) 0.2525(2) 0.0257(9) Uani 1 1 d . . . H2 H 0.6069 0.7165 0.2441 0.031 Uiso 1 1 calc R . . C3 C 0.4203(4) 0.7354(2) 0.2723(2) 0.0263(9) Uani 1 1 d . . . H3 H 0.4087 0.7790 0.2806 0.032 Uiso 1 1 calc R . . C4 C 0.6054(4) 0.5925(2) 0.2228(2) 0.0245(9) Uani 1 1 d . . . C5 C 0.6145(4) 0.5936(2) 0.1575(2) 0.0280(10) Uani 1 1 d . . . C6 C 0.7221(4) 0.5554(3) 0.1347(3) 0.0352(11) Uani 1 1 d . . . H6 H 0.7324 0.5560 0.0912 0.042 Uiso 1 1 calc R . . C7 C 0.8142(4) 0.5167(3) 0.1751(3) 0.0376(12) Uani 1 1 d . . . H7 H 0.8848 0.4911 0.1590 0.045 Uiso 1 1 calc R . . C8 C 0.8011(4) 0.5161(3) 0.2388(3) 0.0342(11) Uani 1 1 d . . . H8 H 0.8627 0.4890 0.2659 0.041 Uiso 1 1 calc R . . C9 C 0.6980(4) 0.5552(2) 0.2646(2) 0.0270(10) Uani 1 1 d . . . C10 C 0.6887(4) 0.5540(3) 0.3354(2) 0.0297(10) Uani 1 1 d . . . H10 H 0.6047 0.5766 0.3475 0.036 Uiso 1 1 calc R . . C11 C 0.7094(5) 0.4750(3) 0.3871(3) 0.0452(13) Uani 1 1 d . . . H11A H 0.6525 0.4459 0.3839 0.068 Uiso 1 1 calc R . . H11B H 0.6951 0.4763 0.4315 0.068 Uiso 1 1 calc R . . H11C H 0.7937 0.4534 0.3783 0.068 Uiso 1 1 calc R . . C12 C 0.7846(4) 0.5986(3) 0.3401(3) 0.0373(12) Uani 1 1 d . . . H12A H 0.8673 0.5791 0.3259 0.056 Uiso 1 1 calc R . . H12B H 0.7787 0.5949 0.3858 0.056 Uiso 1 1 calc R . . H12C H 0.7673 0.6496 0.3116 0.056 Uiso 1 1 calc R . . C13 C 0.5182(4) 0.6369(3) 0.1115(2) 0.0328(11) Uani 1 1 d . . . H13 H 0.4376 0.6401 0.1395 0.039 Uiso 1 1 calc R . . C14 C 0.5489(6) 0.7151(3) 0.0717(3) 0.0637(18) Uani 1 1 d . . . H14A H 0.5589 0.7373 0.1021 0.096 Uiso 1 1 calc R . . H14B H 0.4822 0.7437 0.0462 0.096 Uiso 1 1 calc R . . H14C H 0.6250 0.7138 0.0417 0.096 Uiso 1 1 calc R . . C15 C 0.5036(5) 0.6001(3) 0.0643(3) 0.0495(14) Uani 1 1 d . . . H15A H 0.5765 0.6035 0.0313 0.074 Uiso 1 1 calc R . . H15B H 0.4313 0.6246 0.0422 0.074 Uiso 1 1 calc R . . H15C H 0.4940 0.5490 0.0897 0.074 Uiso 1 1 calc R . . C16 C 0.1983(4) 0.7235(2) 0.2849(2) 0.0227(9) Uani 1 1 d . . . C17 C 0.1226(4) 0.6972(2) 0.3469(2) 0.0244(9) Uani 1 1 d . . . C18 C -0.0023(4) 0.7276(3) 0.3496(2) 0.0351(11) Uani 1 1 d . . . H18 H -0.0555 0.7106 0.3896 0.042 Uiso 1 1 calc R . . C19 C -0.0489(5) 0.7822(3) 0.2944(3) 0.0423(13) Uani 1 1 d . . . H19 H -0.1333 0.8007 0.2971 0.051 Uiso 1 1 calc R . . C20 C 0.0287(5) 0.8093(3) 0.2355(3) 0.0376(12) Uani 1 1 d . . . H20 H -0.0037 0.8474 0.1991 0.045 Uiso 1 1 calc R . . C21 C 0.1544(4) 0.7816(2) 0.2286(2) 0.0284(10) Uani 1 1 d . . . C22 C 0.1742(4) 0.6432(2) 0.4100(2) 0.0282(10) Uani 1 1 d . . . H22 H 0.2558 0.6191 0.3966 0.034 Uiso 1 1 calc R . . C23 C 0.0923(6) 0.5840(3) 0.4506(3) 0.0533(15) Uani 1 1 d . . . H23A H 0.0156 0.6055 0.4693 0.080 Uiso 1 1 calc R . . H23B H 0.1345 0.5471 0.4863 0.080 Uiso 1 1 calc R . . H23C H 0.0743 0.5615 0.4222 0.080 Uiso 1 1 calc R . . C24 C 0.1939(6) 0.6845(3) 0.4524(3) 0.0502(15) Uani 1 1 d . . . H24A H 0.2452 0.7227 0.4256 0.075 Uiso 1 1 calc R . . H24B H 0.2344 0.6505 0.4901 0.075 Uiso 1 1 calc R . . H24C H 0.1145 0.7063 0.4683 0.075 Uiso 1 1 calc R . . C25 C 0.2382(5) 0.8154(3) 0.1635(2) 0.0360(11) Uani 1 1 d . . . H25 H 0.3196 0.7846 0.1671 0.043 Uiso 1 1 calc R . . C26 C 0.1905(6) 0.8162(3) 0.1027(3) 0.0557(16) Uani 1 1 d . . . H26A H 0.1813 0.7666 0.1089 0.084 Uiso 1 1 calc R . . H26B H 0.2489 0.8359 0.0633 0.084 Uiso 1 1 calc R . . H26C H 0.1110 0.8465 0.0975 0.084 Uiso 1 1 calc R . . C27 C 0.2590(7) 0.8932(3) 0.1550(3) 0.0669(19) Uani 1 1 d . . . H27A H 0.1810 0.9252 0.1504 0.100 Uiso 1 1 calc R . . H27B H 0.3176 0.9124 0.1155 0.100 Uiso 1 1 calc R . . H27C H 0.2913 0.8906 0.1937 0.100 Uiso 1 1 calc R . . C28 C 0.1875(5) 0.6042(3) 0.1378(2) 0.0424(13) Uani 1 1 d . . . H28 H 0.2628 0.5797 0.1248 0.051 Uiso 1 1 calc R . . C29 C 0.0976(6) 0.6341(3) 0.0940(3) 0.0529(16) Uani 1 1 d . . . H29 H 0.1138 0.6295 0.0523 0.063 Uiso 1 1 calc R . . C30 C -0.0122(6) 0.6694(4) 0.1119(3) 0.0545(16) Uani 1 1 d . . . H30 H -0.0727 0.6891 0.0830 0.065 Uiso 1 1 calc R . . C31 C -0.0335(5) 0.6759(3) 0.1735(3) 0.0480(14) Uani 1 1 d . . . H31 H -0.1088 0.7001 0.1869 0.058 Uiso 1 1 calc R . . C32 C 0.0570(4) 0.6464(3) 0.2150(2) 0.0352(11) Uani 1 1 d . . . H32 H 0.0417 0.6517 0.2564 0.042 Uiso 1 1 calc R . . C33 C 0.3355(4) 0.4791(3) 0.3703(2) 0.0319(11) Uani 1 1 d . . . C34 C 0.4321(4) 0.4700(2) 0.3205(3) 0.0327(11) Uani 1 1 d . . . C35 C 0.4612(5) 0.4049(3) 0.2979(3) 0.0471(14) Uani 1 1 d . . . H35A H 0.5024 0.3631 0.3316 0.057 Uiso 1 1 calc R . . H35B H 0.5189 0.4175 0.2565 0.057 Uiso 1 1 calc R . . C36 C 0.3454(5) 0.3819(3) 0.2863(3) 0.0484(14) Uani 1 1 d . . . H36A H 0.3696 0.3586 0.2533 0.058 Uiso 1 1 calc R . . H36B H 0.3111 0.3457 0.3280 0.058 Uiso 1 1 calc R . . C37 C 0.2450(5) 0.4476(3) 0.2618(3) 0.0373(12) Uani 1 1 d . . . C39 C 0.1295(5) 0.4311(3) 0.3804(3) 0.0386(12) Uani 1 1 d . . . H39A H 0.1030 0.3832 0.3922 0.046 Uiso 1 1 calc R . . H39B H 0.0633 0.4604 0.3991 0.046 Uiso 1 1 calc R . . C38 C 0.1476(4) 0.4689(3) 0.3046(3) 0.0345(11) Uani 1 1 d . . . C40 C 0.2486(5) 0.4203(3) 0.4125(3) 0.0389(12) Uani 1 1 d . . . H40A H 0.2245 0.4225 0.4569 0.047 Uiso 1 1 calc R . . H40B H 0.2936 0.3716 0.4176 0.047 Uiso 1 1 calc R . . Ir1A Ir 0.876456(14) 0.219615(8) 0.270840(8) 0.01886(5) Uani 1 1 d . . . N1A N 0.9600(3) 0.06761(18) 0.25118(17) 0.0202(7) Uani 1 1 d . . . N2A N 0.7624(3) 0.09924(18) 0.25325(16) 0.0198(7) Uani 1 1 d . . . N3A N 0.8166(3) 0.29766(19) 0.18051(17) 0.0231(8) Uani 1 1 d . . . C1A C 0.8687(4) 0.1248(2) 0.25356(19) 0.0181(8) Uani 1 1 d . . . C3A C 0.7862(4) 0.0286(2) 0.2524(2) 0.0237(9) Uani 1 1 d . . . H3A H 0.7278 0.0003 0.2527 0.028 Uiso 1 1 calc R . . C2A C 0.9097(4) 0.0091(2) 0.2509(2) 0.0253(9) Uani 1 1 d . . . H2A H 0.9535 -0.0357 0.2498 0.030 Uiso 1 1 calc R . . C4A C 1.0953(4) 0.0660(2) 0.2417(2) 0.0238(9) Uani 1 1 d . . . C5A C 1.1526(4) 0.1098(3) 0.1787(2) 0.0304(10) Uani 1 1 d . . . C6A C 1.2815(4) 0.1037(3) 0.1700(3) 0.0414(13) Uani 1 1 d . . . H6A H 1.3231 0.1328 0.1295 0.050 Uiso 1 1 calc R . . C7A C 1.3501(5) 0.0554(3) 0.2204(3) 0.0470(14) Uani 1 1 d . . . H7A H 1.4367 0.0524 0.2134 0.056 Uiso 1 1 calc R . . C8A C 1.2912(4) 0.0120(3) 0.2803(3) 0.0411(13) Uani 1 1 d . . . H8A H 1.3388 -0.0210 0.3132 0.049 Uiso 1 1 calc R . . C9A C 1.1617(4) 0.0163(2) 0.2930(2) 0.0283(10) Uani 1 1 d . . . C10A C 1.1015(4) -0.0340(2) 0.3610(2) 0.0318(10) Uani 1 1 d . . . H10A H 1.0110 -0.0187 0.3641 0.038 Uiso 1 1 calc R . . C11A C 1.1473(5) -0.0285(3) 0.4200(3) 0.0454(13) Uani 1 1 d . . . H11D H 1.0998 -0.0562 0.4612 0.068 Uiso 1 1 calc R . . H11E H 1.1370 0.0224 0.4154 0.068 Uiso 1 1 calc R . . H11F H 1.2341 -0.0483 0.4207 0.068 Uiso 1 1 calc R . . C12A C 1.1250(5) -0.1137(3) 0.3664(3) 0.0454(13) Uani 1 1 d . . . H12D H 1.0950 -0.1175 0.3296 0.068 Uiso 1 1 calc R . . H12E H 1.0819 -0.1438 0.4081 0.068 Uiso 1 1 calc R . . H12F H 1.2130 -0.1304 0.3649 0.068 Uiso 1 1 calc R . . C13A C 1.0795(5) 0.1570(3) 0.1211(2) 0.0338(11) Uani 1 1 d . . . H13A H 0.9980 0.1764 0.1395 0.041 Uiso 1 1 calc R . . C14A C 1.1449(5) 0.2228(3) 0.0694(3) 0.0488(14) Uani 1 1 d . . . H14D H 1.1724 0.2483 0.0925 0.073 Uiso 1 1 calc R . . H14E H 1.0873 0.2562 0.0397 0.073 Uiso 1 1 calc R . . H14F H 1.2156 0.2049 0.0438 0.073 Uiso 1 1 calc R . . C15A C 1.0581(5) 0.1083(3) 0.0858(3) 0.0480(14) Uani 1 1 d . . . H15D H 1.1373 0.0876 0.0686 0.072 Uiso 1 1 calc R . . H15E H 1.0110 0.1375 0.0494 0.072 Uiso 1 1 calc R . . H15F H 1.0127 0.0691 0.1173 0.072 Uiso 1 1 calc R . . C16A C 0.6429(4) 0.1439(2) 0.2408(2) 0.0224(9) Uani 1 1 d . . . C17A C 0.6189(4) 0.1767(2) 0.1738(2) 0.0274(10) Uani 1 1 d . . . C18A C 0.5036(4) 0.2210(3) 0.1617(3) 0.0336(11) Uani 1 1 d . . . H18A H 0.4847 0.2443 0.1179 0.040 Uiso 1 1 calc R . . C19A C 0.4180(4) 0.2301(3) 0.2141(3) 0.0370(12) Uani 1 1 d . . . H19A H 0.3429 0.2606 0.2052 0.044 Uiso 1 1 calc R . . C20A C 0.4428(4) 0.1947(3) 0.2790(3) 0.0340(11) Uani 1 1 d . . . H20A H 0.3829 0.2006 0.3136 0.041 Uiso 1 1 calc R . . C21A C 0.5557(4) 0.1497(2) 0.2947(2) 0.0251(9) Uani 1 1 d . . . C22A C 0.5749(4) 0.1038(3) 0.3665(2) 0.0308(10) Uani 1 1 d . . . H22A H 0.6646 0.0871 0.3675 0.037 Uiso 1 1 calc R . . C23A C 0.5328(6) 0.1459(3) 0.4131(3) 0.0496(14) Uani 1 1 d . . . H23D H 0.5730 0.1898 0.3960 0.074 Uiso 1 1 calc R . . H23E H 0.5547 0.1153 0.4570 0.074 Uiso 1 1 calc R . . H23F H 0.4439 0.1594 0.4160 0.074 Uiso 1 1 calc R . . C24A C 0.5081(5) 0.0349(3) 0.3917(3) 0.0419(12) Uani 1 1 d . . . H24D H 0.4206 0.0497 0.3883 0.063 Uiso 1 1 calc R . . H24E H 0.5193 0.0062 0.4377 0.063 Uiso 1 1 calc R . . H24F H 0.5426 0.0056 0.3647 0.063 Uiso 1 1 calc R . . C25A C 0.7090(5) 0.1629(3) 0.1164(2) 0.0311(10) Uani 1 1 d . . . H25A H 0.7867 0.1354 0.1341 0.037 Uiso 1 1 calc R . . C26A C 0.6537(6) 0.1142(3) 0.0920(3) 0.0561(17) Uani 1 1 d . . . H26D H 0.6320 0.0705 0.1294 0.084 Uiso 1 1 calc R . . H26E H 0.7142 0.1004 0.0594 0.084 Uiso 1 1 calc R . . H26F H 0.5803 0.1413 0.0718 0.084 Uiso 1 1 calc R . . C27A C 0.7415(5) 0.2330(3) 0.0572(2) 0.0372(12) Uani 1 1 d . . . H27D H 0.6667 0.2610 0.0391 0.056 Uiso 1 1 calc R . . H27E H 0.7984 0.2198 0.0231 0.056 Uiso 1 1 calc R . . H27F H 0.7800 0.2623 0.0721 0.056 Uiso 1 1 calc R . . C28A C 0.8977(4) 0.3352(2) 0.1292(2) 0.0280(10) Uani 1 1 d . . . H28A H 0.9827 0.3202 0.1312 0.034 Uiso 1 1 calc R . . C29A C 0.8612(5) 0.3942(2) 0.0744(2) 0.0328(11) Uani 1 1 d . . . H29A H 0.9205 0.4186 0.0401 0.039 Uiso 1 1 calc R . . C30A C 0.7353(5) 0.4171(3) 0.0704(2) 0.0352(11) Uani 1 1 d . . . H30A H 0.7083 0.4567 0.0333 0.042 Uiso 1 1 calc R . . C31A C 0.6511(5) 0.3801(3) 0.1223(2) 0.0336(11) Uani 1 1 d . . . H31A H 0.5658 0.3947 0.1210 0.040 Uiso 1 1 calc R . . C32A C 0.6931(4) 0.3216(2) 0.1762(2) 0.0275(10) Uani 1 1 d . . . H32A H 0.6349 0.2972 0.2111 0.033 Uiso 1 1 calc R . . C33A C 1.0008(4) 0.1548(3) 0.3412(2) 0.0289(10) Uani 1 1 d . . . C34A C 0.8805(4) 0.1582(2) 0.3764(2) 0.0247(9) Uani 1 1 d . . . C35A C 0.8366(4) 0.2045(3) 0.4202(2) 0.0316(10) Uani 1 1 d . . . H35C H 0.9072 0.2080 0.4387 0.038 Uiso 1 1 calc R . . H35D H 0.7760 0.1800 0.4574 0.038 Uiso 1 1 calc R . . C36A C 0.7768(5) 0.2833(3) 0.3800(2) 0.0370(11) Uani 1 1 d . . . H36C H 0.6871 0.2836 0.3858 0.044 Uiso 1 1 calc R . . H36D H 0.7926 0.3172 0.3988 0.044 Uiso 1 1 calc R . . C37A C 0.8238(4) 0.3108(2) 0.3064(2) 0.0291(10) Uani 1 1 d . . . C38A C 0.9507(5) 0.3094(3) 0.2798(2) 0.0328(11) Uani 1 1 d . . . C39A C 1.0560(5) 0.2800(3) 0.3236(3) 0.0428(13) Uani 1 1 d . . . H39C H 1.1251 0.3085 0.3014 0.051 Uiso 1 1 calc R . . H39D H 1.0264 0.2866 0.3661 0.051 Uiso 1 1 calc R . . C40A C 1.1021(5) 0.1987(3) 0.3374(3) 0.0428(13) Uani 1 1 d . . . H40C H 1.1686 0.1947 0.3021 0.051 Uiso 1 1 calc R . . H40D H 1.1368 0.1772 0.3795 0.051 Uiso 1 1 calc R . . B1 B 0.5971(6) 0.8691(3) 0.2863(4) 0.0421(15) Uani 1 1 d . . . F1 F 0.6016(3) 0.9347(2) 0.23162(19) 0.0680(10) Uani 1 1 d . . . F2 F 0.6604(3) 0.8715(2) 0.33355(18) 0.0654(10) Uani 1 1 d . . . F3 F 0.6560(3) 0.81121(19) 0.2670(2) 0.0641(10) Uani 1 1 d . . . F4 F 0.4752(3) 0.8578(2) 0.3131(2) 0.0688(11) Uani 1 1 d . . . B2 B 0.2082(6) 0.4177(3) 0.0971(3) 0.0381(13) Uani 1 1 d . . . F5 F 0.3152(4) 0.4428(3) 0.0950(2) 0.0924(15) Uani 1 1 d . . . F6 F 0.1785(4) 0.3617(2) 0.1529(2) 0.0948(16) Uani 1 1 d . . . F7 F 0.1981(6) 0.4090(3) 0.0412(2) 0.137(2) Uani 1 1 d . . . F8 F 0.1137(5) 0.4721(3) 0.0998(4) 0.156(3) Uani 1 1 d . . . C41 C 0.2228(6) 0.1337(3) 0.5533(3) 0.0547(15) Uani 1 1 d . . . H41A H 0.1743 0.1258 0.5972 0.066 Uiso 1 1 calc R . . H41B H 0.3101 0.1288 0.5581 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.17732(16) 0.22286(9) 0.49823(8) 0.0608(4) Uani 1 1 d . . . Cl2 Cl 0.20139(15) 0.06559(9) 0.52465(8) 0.0555(4) Uani 1 1 d . . . C42 C 0.4402(6) 0.2944(4) 0.5644(3) 0.0627(18) Uani 1 1 d . . . H42A H 0.4715 0.2695 0.6074 0.075 Uiso 1 1 calc R . . H42B H 0.3505 0.2938 0.5721 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.47302(16) 0.38732(10) 0.52917(8) 0.0684(5) Uani 1 1 d . . . Cl4 Cl 0.50834(19) 0.24747(13) 0.51187(11) 0.0929(7) Uani 1 1 d . . . C43 C 0.7393(12) 0.9146(5) 0.0929(4) 0.131(4) Uani 1 1 d . . . H43 H 0.7008 0.9157 0.1370 0.157 Uiso 1 1 calc R . . Cl5 Cl 0.8696(2) 0.95739(17) 0.06868(16) 0.0801(8) Uani 0.67 1 d P . . Cl6 Cl 0.7667(4) 0.82923(15) 0.09841(14) 0.1015(12) Uani 0.67 1 d P . . Cl7 Cl 0.6301(3) 0.9642(2) 0.03355(16) 0.0942(10) Uani 0.67 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 0.02168(9) 0.02192(9) 0.02669(10) -0.01135(7) 0.00018(7) -0.00723(7) N1 0.0207(17) 0.0204(18) 0.0251(19) -0.0090(15) 0.0006(14) -0.0060(14) N2 0.0218(17) 0.0187(18) 0.0226(18) -0.0078(15) 0.0001(14) -0.0039(14) N3 0.037(2) 0.033(2) 0.026(2) -0.0110(18) -0.0007(17) -0.0184(18) C1 0.025(2) 0.019(2) 0.022(2) -0.0075(17) -0.0024(17) -0.0058(17) C2 0.024(2) 0.022(2) 0.034(2) -0.0116(19) -0.0026(19) -0.0075(17) C3 0.029(2) 0.020(2) 0.033(2) -0.0110(19) -0.0068(19) -0.0058(18) C4 0.020(2) 0.019(2) 0.035(2) -0.0122(19) 0.0027(18) -0.0039(16) C5 0.027(2) 0.023(2) 0.033(3) -0.011(2) 0.0041(19) -0.0083(18) C6 0.035(3) 0.035(3) 0.040(3) -0.022(2) 0.007(2) -0.010(2) C7 0.028(2) 0.037(3) 0.056(3) -0.030(3) 0.005(2) -0.005(2) C8 0.025(2) 0.030(3) 0.053(3) -0.021(2) -0.008(2) -0.0034(19) C9 0.022(2) 0.024(2) 0.037(3) -0.012(2) -0.0018(19) -0.0082(18) C10 0.021(2) 0.030(2) 0.038(3) -0.014(2) -0.0034(19) -0.0038(18) C11 0.040(3) 0.041(3) 0.048(3) -0.003(3) -0.015(3) -0.009(2) C12 0.032(3) 0.039(3) 0.045(3) -0.018(2) -0.006(2) -0.009(2) C13 0.033(3) 0.034(3) 0.028(2) -0.010(2) 0.000(2) -0.003(2) C14 0.073(4) 0.043(4) 0.060(4) -0.001(3) -0.011(3) -0.011(3) C15 0.048(3) 0.058(4) 0.042(3) -0.023(3) -0.011(3) 0.008(3) C16 0.024(2) 0.023(2) 0.025(2) -0.0124(18) -0.0045(17) -0.0020(17) C17 0.025(2) 0.026(2) 0.024(2) -0.0124(19) -0.0007(18) -0.0050(18) C18 0.030(2) 0.044(3) 0.033(3) -0.019(2) 0.003(2) -0.006(2) C19 0.027(3) 0.056(4) 0.054(3) -0.035(3) -0.007(2) 0.005(2) C20 0.041(3) 0.036(3) 0.033(3) -0.013(2) -0.015(2) 0.010(2) C21 0.031(2) 0.027(2) 0.030(2) -0.015(2) -0.0055(19) -0.0018(19) C22 0.033(2) 0.027(2) 0.025(2) -0.010(2) -0.0017(19) -0.0054(19) C23 0.068(4) 0.050(4) 0.039(3) -0.007(3) -0.001(3) -0.026(3) C24 0.076(4) 0.037(3) 0.043(3) -0.013(3) -0.029(3) -0.001(3) C25 0.046(3) 0.030(3) 0.024(2) -0.003(2) -0.003(2) -0.002(2) C26 0.074(4) 0.061(4) 0.027(3) -0.008(3) -0.010(3) -0.012(3) C27 0.107(6) 0.041(4) 0.045(4) -0.005(3) 0.001(4) -0.026(4) C28 0.054(3) 0.048(3) 0.030(3) -0.018(2) 0.006(2) -0.024(3) C29 0.076(4) 0.069(4) 0.024(3) -0.015(3) -0.009(3) -0.034(4) C30 0.058(4) 0.070(4) 0.034(3) -0.004(3) -0.019(3) -0.025(3) C31 0.042(3) 0.063(4) 0.034(3) -0.007(3) -0.013(2) -0.011(3) C32 0.035(3) 0.040(3) 0.029(3) -0.008(2) -0.004(2) -0.013(2) C33 0.030(2) 0.025(2) 0.038(3) -0.007(2) -0.011(2) -0.0020(19) C34 0.025(2) 0.018(2) 0.046(3) -0.003(2) -0.006(2) -0.0008(18) C35 0.034(3) 0.036(3) 0.069(4) -0.023(3) 0.004(3) -0.003(2) C36 0.051(3) 0.033(3) 0.069(4) -0.031(3) 0.007(3) -0.010(2) C37 0.039(3) 0.031(3) 0.054(3) -0.026(2) 0.000(2) -0.017(2) C39 0.037(3) 0.032(3) 0.047(3) -0.013(2) 0.003(2) -0.015(2) C38 0.031(2) 0.027(2) 0.049(3) -0.014(2) -0.002(2) -0.015(2) C40 0.042(3) 0.029(3) 0.040(3) -0.007(2) -0.001(2) -0.010(2) Ir1A 0.02022(9) 0.01761(9) 0.02012(9) -0.00786(7) -0.00176(6) -0.00466(6) N1A 0.0174(16) 0.0203(18) 0.0252(18) -0.0108(15) -0.0015(14) -0.0042(14) N2A 0.0219(17) 0.0199(18) 0.0196(17) -0.0086(15) -0.0018(14) -0.0057(14) N3A 0.0279(19) 0.0209(18) 0.0217(18) -0.0077(15) -0.0019(15) -0.0080(15) C1A 0.021(2) 0.018(2) 0.0140(19) -0.0049(16) 0.0023(16) -0.0064(16) C3A 0.028(2) 0.020(2) 0.025(2) -0.0091(18) -0.0023(18) -0.0085(17) C2A 0.032(2) 0.017(2) 0.029(2) -0.0092(18) -0.0030(19) -0.0053(18) C4A 0.018(2) 0.021(2) 0.036(2) -0.017(2) 0.0010(18) -0.0029(16) C5A 0.028(2) 0.028(2) 0.039(3) -0.018(2) 0.004(2) -0.0070(19) C6A 0.028(3) 0.041(3) 0.053(3) -0.019(3) 0.010(2) -0.012(2) C7A 0.024(2) 0.047(3) 0.068(4) -0.023(3) 0.001(3) -0.004(2) C8A 0.026(2) 0.034(3) 0.065(4) -0.020(3) -0.011(2) -0.001(2) C9A 0.026(2) 0.020(2) 0.042(3) -0.016(2) -0.004(2) -0.0037(18) C10A 0.031(2) 0.026(2) 0.036(3) -0.009(2) -0.008(2) 0.0006(19) C11A 0.057(3) 0.035(3) 0.041(3) -0.005(2) -0.022(3) -0.002(2) C12A 0.048(3) 0.027(3) 0.058(4) -0.009(3) -0.009(3) -0.008(2) C13A 0.036(3) 0.034(3) 0.025(2) -0.009(2) 0.007(2) -0.007(2) C14A 0.052(3) 0.041(3) 0.040(3) -0.007(3) 0.016(3) -0.015(3) C15A 0.053(3) 0.054(4) 0.039(3) -0.022(3) 0.002(3) -0.011(3) C16A 0.021(2) 0.024(2) 0.028(2) -0.0117(19) -0.0053(17) -0.0077(17) C17A 0.028(2) 0.025(2) 0.031(2) -0.009(2) -0.0078(19) -0.0077(18) C18A 0.036(3) 0.026(2) 0.040(3) -0.006(2) -0.019(2) -0.004(2) C19A 0.025(2) 0.029(3) 0.060(3) -0.018(3) -0.010(2) -0.003(2) C20A 0.023(2) 0.038(3) 0.047(3) -0.023(2) 0.001(2) -0.008(2) C21A 0.020(2) 0.025(2) 0.035(2) -0.015(2) -0.0004(18) -0.0085(17) C22A 0.027(2) 0.042(3) 0.026(2) -0.013(2) 0.0025(19) -0.014(2) C23A 0.065(4) 0.056(4) 0.037(3) -0.028(3) 0.007(3) -0.020(3) C24A 0.052(3) 0.042(3) 0.033(3) -0.012(2) 0.000(2) -0.018(3) C25A 0.039(3) 0.029(2) 0.024(2) -0.006(2) -0.004(2) -0.008(2) C26A 0.096(5) 0.052(4) 0.030(3) -0.023(3) 0.012(3) -0.038(3) C27A 0.055(3) 0.034(3) 0.026(2) -0.009(2) -0.004(2) -0.017(2) C28A 0.032(2) 0.031(2) 0.026(2) -0.017(2) 0.0022(19) -0.0101(19) C29A 0.049(3) 0.026(2) 0.024(2) -0.007(2) -0.001(2) -0.014(2) C30A 0.054(3) 0.021(2) 0.031(3) -0.006(2) -0.015(2) -0.003(2) C31A 0.037(3) 0.026(2) 0.039(3) -0.013(2) -0.011(2) 0.001(2) C32A 0.030(2) 0.024(2) 0.032(2) -0.013(2) -0.003(2) -0.0063(19) C33A 0.030(2) 0.033(3) 0.026(2) -0.011(2) -0.0117(19) -0.002(2) C34A 0.029(2) 0.020(2) 0.022(2) -0.0031(18) -0.0117(18) 0.0004(18) C35A 0.037(3) 0.032(3) 0.024(2) -0.012(2) 0.003(2) -0.005(2) C36A 0.046(3) 0.029(3) 0.036(3) -0.017(2) -0.004(2) 0.004(2) C37A 0.044(3) 0.018(2) 0.029(2) -0.0125(19) -0.006(2) -0.0041(19) C38A 0.049(3) 0.027(2) 0.033(3) -0.016(2) -0.008(2) -0.015(2) C39A 0.044(3) 0.052(3) 0.041(3) -0.018(3) -0.003(2) -0.027(3) C40A 0.030(3) 0.064(4) 0.043(3) -0.023(3) -0.007(2) -0.013(2) B1 0.038(3) 0.029(3) 0.069(4) -0.025(3) -0.020(3) 0.000(3) F1 0.075(3) 0.050(2) 0.077(3) -0.010(2) -0.024(2) -0.0173(18) F2 0.065(2) 0.084(3) 0.065(2) -0.040(2) -0.0138(19) -0.020(2) F3 0.0436(19) 0.056(2) 0.116(3) -0.056(2) -0.0094(19) -0.0080(16) F4 0.0374(18) 0.059(2) 0.127(3) -0.055(2) -0.003(2) -0.0081(16) B2 0.044(3) 0.041(3) 0.032(3) -0.014(3) -0.002(3) -0.013(3) F5 0.066(3) 0.132(4) 0.088(3) -0.033(3) 0.005(2) -0.063(3) F6 0.072(3) 0.098(3) 0.073(3) 0.034(2) -0.024(2) -0.044(2) F7 0.193(6) 0.190(6) 0.068(3) -0.069(4) 0.038(3) -0.130(5) F8 0.099(4) 0.110(5) 0.273(9) -0.101(5) -0.032(5) 0.026(3) C41 0.069(4) 0.058(4) 0.043(3) -0.021(3) -0.012(3) -0.013(3) Cl1 0.0735(11) 0.0498(9) 0.0562(9) -0.0209(8) -0.0046(8) -0.0032(8) Cl2 0.0637(9) 0.0553(9) 0.0530(9) -0.0234(7) -0.0036(7) -0.0175(7) C42 0.068(4) 0.076(5) 0.047(4) -0.035(4) 0.015(3) -0.011(4) Cl3 0.0688(11) 0.0780(12) 0.0531(10) -0.0190(9) 0.0040(8) -0.0208(9) Cl4 0.0869(14) 0.1281(19) 0.0943(15) -0.0842(15) 0.0352(11) -0.0388(13) C43 0.264(14) 0.089(7) 0.048(5) -0.030(5) -0.010(7) -0.045(8) Cl5 0.0528(15) 0.089(2) 0.100(2) -0.0375(18) -0.0210(15) 0.0035(14) Cl6 0.176(3) 0.0472(16) 0.0557(17) -0.0149(13) 0.0182(19) 0.0016(18) Cl7 0.077(2) 0.111(3) 0.084(2) -0.0201(19) -0.0387(17) 0.0062(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.076(4) . ? Ir1 N3 2.103(4) . ? Ir1 C34 2.126(4) . ? Ir1 C33 2.143(5) . ? Ir1 C38 2.178(4) . ? Ir1 C37 2.194(4) . ? N1 C1 1.357(5) . ? N1 C2 1.384(5) . ? N1 C4 1.465(5) . ? N2 C1 1.377(5) . ? N2 C3 1.383(5) . ? N2 C16 1.444(5) . ? N3 C28 1.342(6) . ? N3 C32 1.357(6) . ? C2 C3 1.335(6) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.400(6) . ? C4 C9 1.402(6) . ? C5 C6 1.393(6) . ? C5 C13 1.504(6) . ? C6 C7 1.383(7) . ? C6 H6 0.9300 . ? C7 C8 1.365(7) . ? C7 H7 0.9300 . ? C8 C9 1.398(6) . ? C8 H8 0.9300 . ? C9 C10 1.520(6) . ? C10 C11 1.533(6) . ? C10 C12 1.544(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.516(7) . ? C13 C15 1.523(7) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.402(6) . ? C16 C21 1.406(6) . ? C17 C18 1.390(6) . ? C17 C22 1.509(6) . ? C18 C19 1.374(7) . ? C18 H18 0.9300 . ? C19 C20 1.369(7) . ? C19 H19 0.9300 . ? C20 C21 1.389(6) . ? C20 H20 0.9300 . ? C21 C25 1.513(6) . ? C22 C23 1.501(7) . ? C22 C24 1.524(6) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.515(7) . ? C25 C27 1.536(7) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.396(8) . ? C28 H28 0.9300 . ? C29 C30 1.342(8) . ? C29 H29 0.9300 . ? C30 C31 1.372(8) . ? C30 H30 0.9300 . ? C31 C32 1.367(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.402(7) . ? C33 C40 1.537(6) . ? C34 C35 1.515(7) . ? C35 C36 1.529(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.527(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.393(7) . ? C39 C38 1.514(7) . ? C39 C40 1.546(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? Ir1A C1A 2.077(4) . ? Ir1A N3A 2.106(3) . ? Ir1A C33A 2.117(4) . ? Ir1A C34A 2.146(4) . ? Ir1A C37A 2.175(4) . ? Ir1A C38A 2.187(4) . ? N1A C1A 1.371(5) . ? N1A C2A 1.383(5) . ? N1A C4A 1.459(5) . ? N2A C1A 1.365(5) . ? N2A C3A 1.380(5) . ? N2A C16A 1.445(5) . ? N3A C28A 1.346(5) . ? N3A C32A 1.359(5) . ? C3A C2A 1.337(6) . ? C3A H3A 0.9300 . ? C2A H2A 0.9300 . ? C4A C9A 1.391(6) . ? C4A C5A 1.406(6) . ? C5A C6A 1.382(6) . ? C5A C13A 1.512(7) . ? C6A C7A 1.383(7) . ? C6A H6A 0.9300 . ? C7A C8A 1.367(8) . ? C7A H7A 0.9300 . ? C8A C9A 1.391(6) . ? C8A H8A 0.9300 . ? C9A C10A 1.529(6) . ? C10A C12A 1.511(6) . ? C10A C11A 1.523(7) . ? C10A H10A 0.9800 . ? C11A H11D 0.9600 . ? C11A H11E 0.9600 . ? C11A H11F 0.9600 . ? C12A H12D 0.9600 . ? C12A H12E 0.9600 . ? C12A H12F 0.9600 . ? C13A C15A 1.524(7) . ? C13A C14A 1.542(6) . ? C13A H13A 0.9800 . ? C14A H14D 0.9600 . ? C14A H14E 0.9600 . ? C14A H14F 0.9600 . ? C15A H15D 0.9600 . ? C15A H15E 0.9600 . ? C15A H15F 0.9600 . ? C16A C21A 1.392(6) . ? C16A C17A 1.403(6) . ? C17A C18A 1.402(6) . ? C17A C25A 1.517(6) . ? C18A C19A 1.378(7) . ? C18A H18A 0.9300 . ? C19A C20A 1.367(7) . ? C19A H19A 0.9300 . ? C20A C21A 1.398(6) . ? C20A H20A 0.9300 . ? C21A C22A 1.506(6) . ? C22A C23A 1.510(6) . ? C22A C24A 1.532(6) . ? C22A H22A 0.9800 . ? C23A H23D 0.9600 . ? C23A H23E 0.9600 . ? C23A H23F 0.9600 . ? C24A H24D 0.9600 . ? C24A H24E 0.9600 . ? C24A H24F 0.9600 . ? C25A C27A 1.525(6) . ? C25A C26A 1.533(7) . ? C25A H25A 0.9800 . ? C26A H26D 0.9600 . ? C26A H26E 0.9600 . ? C26A H26F 0.9600 . ? C27A H27D 0.9600 . ? C27A H27E 0.9600 . ? C27A H27F 0.9600 . ? C28A C29A 1.367(6) . ? C28A H28A 0.9300 . ? C29A C30A 1.381(7) . ? C29A H29A 0.9300 . ? C30A C31A 1.370(7) . ? C30A H30A 0.9300 . ? C31A C32A 1.370(6) . ? C31A H31A 0.9300 . ? C32A H32A 0.9300 . ? C33A C34A 1.397(6) . ? C33A C40A 1.513(6) . ? C34A C35A 1.526(6) . ? C35A C36A 1.546(6) . ? C35A H35C 0.9700 . ? C35A H35D 0.9700 . ? C36A C37A 1.496(6) . ? C36A H36C 0.9700 . ? C36A H36D 0.9700 . ? C37A C38A 1.402(7) . ? C38A C39A 1.528(7) . ? C39A C40A 1.519(7) . ? C39A H39C 0.9700 . ? C39A H39D 0.9700 . ? C40A H40C 0.9700 . ? C40A H40D 0.9700 . ? B1 F2 1.374(7) . ? B1 F3 1.377(6) . ? B1 F4 1.377(7) . ? B1 F1 1.378(7) . ? B2 F6 1.320(7) . ? B2 F7 1.327(7) . ? B2 F5 1.351(7) . ? B2 F8 1.356(8) . ? C41 Cl1 1.744(6) . ? C41 Cl2 1.765(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 Cl4 1.724(6) . ? C42 Cl3 1.775(7) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 Cl6 1.619(9) . ? C43 Cl5 1.696(11) . ? C43 Cl7 1.801(11) . ? C43 H43 0.9800 . ? 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 N3 96.12(15) . . ? C1 Ir1 C34 88.73(17) . . ? N3 Ir1 C34 160.26(18) . . ? C1 Ir1 C33 93.57(17) . . ? N3 Ir1 C33 158.80(17) . . ? C34 Ir1 C33 38.35(18) . . ? C1 Ir1 C38 162.86(18) . . ? N3 Ir1 C38 83.86(16) . . ? C34 Ir1 C38 97.06(18) . . ? C33 Ir1 C38 81.39(18) . . ? C1 Ir1 C37 159.84(18) . . ? N3 Ir1 C37 87.86(17) . . ? C34 Ir1 C37 81.38(19) . . ? C33 Ir1 C37 89.52(19) . . ? C38 Ir1 C37 37.16(18) . . ? C1 N1 C2 112.1(3) . . ? C1 N1 C4 130.0(3) . . ? C2 N1 C4 117.9(3) . . ? C1 N2 C3 111.5(3) . . ? C1 N2 C16 126.8(3) . . ? C3 N2 C16 120.3(4) . . ? C28 N3 C32 116.8(4) . . ? C28 N3 Ir1 121.9(4) . . ? C32 N3 Ir1 119.9(3) . . ? N1 C1 N2 102.8(3) . . ? N1 C1 Ir1 130.2(3) . . ? N2 C1 Ir1 126.7(3) . . ? C3 C2 N1 106.9(4) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 106.8(4) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C5 C4 C9 123.1(4) . . ? C5 C4 N1 119.3(4) . . ? C9 C4 N1 117.2(4) . . ? C6 C5 C4 116.8(4) . . ? C6 C5 C13 120.1(4) . . ? C4 C5 C13 123.0(4) . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 119.8(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 122.0(5) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C4 116.6(4) . . ? C8 C9 C10 120.1(4) . . ? C4 C9 C10 123.3(4) . . ? C9 C10 C11 112.0(4) . . ? C9 C10 C12 111.6(4) . . ? C11 C10 C12 108.2(4) . . ? C9 C10 H10 108.3 . . ? C11 C10 H10 108.3 . . ? C12 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 C14 110.2(4) . . ? C5 C13 C15 112.9(4) . . ? C14 C13 C15 110.5(5) . . ? C5 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.6(4) . . ? C17 C16 N2 119.9(4) . . ? C21 C16 N2 117.4(4) . . ? C18 C17 C16 117.0(4) . . ? C18 C17 C22 120.3(4) . . ? C16 C17 C22 122.5(4) . . ? C19 C18 C17 121.5(5) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 120.1(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.9(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C16 116.8(4) . . ? C20 C21 C25 120.2(4) . . ? C16 C21 C25 123.0(4) . . ? C23 C22 C17 112.6(4) . . ? C23 C22 C24 110.3(4) . . ? C17 C22 C24 109.9(4) . . ? C23 C22 H22 108.0 . . ? C17 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.9(4) . . ? C21 C25 C27 110.3(4) . . ? C26 C25 C27 111.5(5) . . ? C21 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 121.8(5) . . ? N3 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 120.2(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 118.8(5) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C32 C31 C30 119.4(6) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? N3 C32 C31 122.9(5) . . ? N3 C32 H32 118.5 . . ? C31 C32 H32 118.5 . . ? C34 C33 C40 123.4(4) . . ? C34 C33 Ir1 70.2(3) . . ? C40 C33 Ir1 114.0(3) . . ? C33 C34 C35 125.9(4) . . ? C33 C34 Ir1 71.5(3) . . ? C35 C34 Ir1 110.5(3) . . ? C34 C35 C36 113.5(4) . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 112.2(4) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C36 123.5(5) . . ? C38 C37 Ir1 70.8(3) . . ? C36 C37 Ir1 112.0(3) . . ? C38 C39 C40 113.5(4) . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C37 C38 C39 124.5(5) . . ? C37 C38 Ir1 72.0(3) . . ? C39 C38 Ir1 110.5(3) . . ? C33 C40 C39 112.4(4) . . ? C33 C40 H40A 109.1 . . ? C39 C40 H40A 109.1 . . ? C33 C40 H40B 109.1 . . ? C39 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C1A Ir1A N3A 97.63(14) . . ? C1A Ir1A C33A 87.83(16) . . ? N3A Ir1A C33A 158.46(16) . . ? C1A Ir1A C34A 91.87(15) . . ? N3A Ir1A C34A 160.45(15) . . ? C33A Ir1A C34A 38.26(17) . . ? C1A Ir1A C37A 161.08(17) . . ? N3A Ir1A C37A 84.56(15) . . ? C33A Ir1A C37A 97.01(17) . . ? C34A Ir1A C37A 81.05(16) . . ? C1A Ir1A C38A 160.89(18) . . ? N3A Ir1A C38A 87.02(16) . . ? C33A Ir1A C38A 81.54(18) . . ? C34A Ir1A C38A 89.56(17) . . ? C37A Ir1A C38A 37.51(18) . . ? C1A N1A C2A 111.2(3) . . ? C1A N1A C4A 128.5(3) . . ? C2A N1A C4A 119.8(3) . . ? C1A N2A C3A 112.0(3) . . ? C1A N2A C16A 125.3(3) . . ? C3A N2A C16A 121.4(3) . . ? C28A N3A C32A 116.7(4) . . ? C28A N3A Ir1A 121.5(3) . . ? C32A N3A Ir1A 120.8(3) . . ? N2A C1A N1A 102.9(3) . . ? N2A C1A Ir1A 125.8(3) . . ? N1A C1A Ir1A 130.5(3) . . ? C2A C3A N2A 106.5(4) . . ? C2A C3A H3A 126.7 . . ? N2A C3A H3A 126.7 . . ? C3A C2A N1A 107.3(4) . . ? C3A C2A H2A 126.4 . . ? N1A C2A H2A 126.4 . . ? C9A C4A C5A 123.4(4) . . ? C9A C4A N1A 118.4(4) . . ? C5A C4A N1A 117.9(4) . . ? C6A C5A C4A 116.5(4) . . ? C6A C5A C13A 120.9(4) . . ? C4A C5A C13A 122.4(4) . . ? C5A C6A C7A 121.4(5) . . ? C5A C6A H6A 119.3 . . ? C7A C6A H6A 119.3 . . ? C8A C7A C6A 120.4(5) . . ? C8A C7A H7A 119.8 . . ? C6A C7A H7A 119.8 . . ? C7A C8A C9A 121.3(5) . . ? C7A C8A H8A 119.3 . . ? C9A C8A H8A 119.3 . . ? C4A C9A C8A 116.9(4) . . ? C4A C9A C10A 124.2(4) . . ? C8A C9A C10A 118.8(4) . . ? C12A C10A C11A 109.2(4) . . ? C12A C10A C9A 110.9(4) . . ? C11A C10A C9A 112.6(4) . . ? C12A C10A H10A 108.0 . . ? C11A C10A H10A 108.0 . . ? C9A C10A H10A 108.0 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C5A C13A C15A 108.6(4) . . ? C5A C13A C14A 113.4(4) . . ? C15A C13A C14A 109.3(4) . . ? C5A C13A H13A 108.4 . . ? C15A C13A H13A 108.4 . . ? C14A C13A H13A 108.4 . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C13A C15A H15D 109.5 . . ? C13A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C21A C16A C17A 123.2(4) . . ? C21A C16A N2A 119.6(4) . . ? C17A C16A N2A 117.2(4) . . ? C18A C17A C16A 117.0(4) . . ? C18A C17A C25A 120.4(4) . . ? C16A C17A C25A 122.5(4) . . ? C19A C18A C17A 120.7(4) . . ? C19A C18A H18A 119.7 . . ? C17A C18A H18A 119.7 . . ? C20A C19A C18A 120.5(4) . . ? C20A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C19A C20A C21A 121.8(5) . . ? C19A C20A H20A 119.1 . . ? C21A C20A H20A 119.1 . . ? C16A C21A C20A 116.6(4) . . ? C16A C21A C22A 122.1(4) . . ? C20A C21A C22A 120.9(4) . . ? C21A C22A C23A 113.4(4) . . ? C21A C22A C24A 109.7(4) . . ? C23A C22A C24A 110.3(4) . . ? C21A C22A H22A 107.7 . . ? C23A C22A H22A 107.7 . . ? C24A C22A H22A 107.7 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C17A C25A C27A 114.4(4) . . ? C17A C25A C26A 108.9(4) . . ? C27A C25A C26A 109.5(4) . . ? C17A C25A H25A 107.9 . . ? C27A C25A H25A 107.9 . . ? C26A C25A H25A 107.9 . . ? C25A C26A H26D 109.5 . . ? C25A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C25A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C25A C27A H27D 109.5 . . ? C25A C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C25A C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? N3A C28A C29A 123.3(4) . . ? N3A C28A H28A 118.4 . . ? C29A C28A H28A 118.4 . . ? C28A C29A C30A 119.2(4) . . ? C28A C29A H29A 120.4 . . ? C30A C29A H29A 120.4 . . ? C31A C30A C29A 118.5(4) . . ? C31A C30A H30A 120.7 . . ? C29A C30A H30A 120.7 . . ? C32A C31A C30A 119.6(5) . . ? C32A C31A H31A 120.2 . . ? C30A C31A H31A 120.2 . . ? N3A C32A C31A 122.6(4) . . ? N3A C32A H32A 118.7 . . ? C31A C32A H32A 118.7 . . ? C34A C33A C40A 125.9(4) . . ? C34A C33A Ir1A 72.0(2) . . ? C40A C33A Ir1A 110.4(3) . . ? C33A C34A C35A 123.4(4) . . ? C33A C34A Ir1A 69.7(3) . . ? C35A C34A Ir1A 114.3(3) . . ? C34A C35A C36A 111.9(4) . . ? C34A C35A H35C 109.2 . . ? C36A C35A H35C 109.2 . . ? C34A C35A H35D 109.2 . . ? C36A C35A H35D 109.2 . . ? H35C C35A H35D 107.9 . . ? C37A C36A C35A 114.3(4) . . ? C37A C36A H36C 108.7 . . ? C35A C36A H36C 108.7 . . ? C37A C36A H36D 108.7 . . ? C35A C36A H36D 108.7 . . ? H36C C36A H36D 107.6 . . ? C38A C37A C36A 124.1(4) . . ? C38A C37A Ir1A 71.7(3) . . ? C36A C37A Ir1A 110.8(3) . . ? C37A C38A C39A 123.1(4) . . ? C37A C38A Ir1A 70.8(2) . . ? C39A C38A Ir1A 111.6(3) . . ? C40A C39A C38A 112.4(4) . . ? C40A C39A H39C 109.1 . . ? C38A C39A H39C 109.1 . . ? C40A C39A H39D 109.1 . . ? C38A C39A H39D 109.1 . . ? H39C C39A H39D 107.9 . . ? C33A C40A C39A 113.4(4) . . ? C33A C40A H40C 108.9 . . ? C39A C40A H40C 108.9 . . ? C33A C40A H40D 108.9 . . ? C39A C40A H40D 108.9 . . ? H40C C40A H40D 107.7 . . ? F2 B1 F3 108.0(5) . . ? F2 B1 F4 110.3(6) . . ? F3 B1 F4 109.4(4) . . ? F2 B1 F1 108.7(4) . . ? F3 B1 F1 109.7(6) . . ? F4 B1 F1 110.7(5) . . ? F6 B2 F7 114.3(5) . . ? F6 B2 F5 114.3(5) . . ? F7 B2 F5 114.0(5) . . ? F6 B2 F8 102.7(6) . . ? F7 B2 F8 102.9(6) . . ? F5 B2 F8 106.8(6) . . ? Cl1 C41 Cl2 111.8(3) . . ? Cl1 C41 H41A 109.3 . . ? Cl2 C41 H41A 109.3 . . ? Cl1 C41 H41B 109.3 . . ? Cl2 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? Cl4 C42 Cl3 111.1(3) . . ? Cl4 C42 H42A 109.4 . . ? Cl3 C42 H42A 109.4 . . ? Cl4 C42 H42B 109.4 . . ? Cl3 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? Cl6 C43 Cl5 113.5(7) . . ? Cl6 C43 Cl7 108.6(5) . . ? Cl5 C43 Cl7 109.3(5) . . ? Cl6 C43 H43 108.5 . . ? Cl5 C43 H43 108.5 . . ? Cl7 C43 H43 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 N3 C28 105.6(4) . . . . ? C34 Ir1 N3 C28 2.1(7) . . . . ? C33 Ir1 N3 C28 -137.7(5) . . . . ? C38 Ir1 N3 C28 -91.7(4) . . . . ? C37 Ir1 N3 C28 -54.6(4) . . . . ? C1 Ir1 N3 C32 -88.2(4) . . . . ? C34 Ir1 N3 C32 168.3(4) . . . . ? C33 Ir1 N3 C32 28.5(6) . . . . ? C38 Ir1 N3 C32 74.6(4) . . . . ? C37 Ir1 N3 C32 111.6(4) . . . . ? C2 N1 C1 N2 0.2(5) . . . . ? C4 N1 C1 N2 -177.0(4) . . . . ? C2 N1 C1 Ir1 -173.3(3) . . . . ? C4 N1 C1 Ir1 9.5(7) . . . . ? C3 N2 C1 N1 -0.4(5) . . . . ? C16 N2 C1 N1 165.7(4) . . . . ? C3 N2 C1 Ir1 173.4(3) . . . . ? C16 N2 C1 Ir1 -20.5(6) . . . . ? N3 Ir1 C1 N1 -121.0(4) . . . . ? C34 Ir1 C1 N1 39.8(4) . . . . ? C33 Ir1 C1 N1 77.9(4) . . . . ? C38 Ir1 C1 N1 150.0(5) . . . . ? C37 Ir1 C1 N1 -20.5(8) . . . . ? N3 Ir1 C1 N2 66.9(4) . . . . ? C34 Ir1 C1 N2 -132.2(4) . . . . ? C33 Ir1 C1 N2 -94.2(4) . . . . ? C38 Ir1 C1 N2 -22.1(8) . . . . ? C37 Ir1 C1 N2 167.5(5) . . . . ? C1 N1 C2 C3 0.0(5) . . . . ? C4 N1 C2 C3 177.6(4) . . . . ? N1 C2 C3 N2 -0.2(5) . . . . ? C1 N2 C3 C2 0.4(5) . . . . ? C16 N2 C3 C2 -166.7(4) . . . . ? C1 N1 C4 C5 70.5(6) . . . . ? C2 N1 C4 C5 -106.6(5) . . . . ? C1 N1 C4 C9 -116.2(5) . . . . ? C2 N1 C4 C9 66.8(5) . . . . ? C9 C4 C5 C6 -0.2(6) . . . . ? N1 C4 C5 C6 172.8(4) . . . . ? C9 C4 C5 C13 -176.8(4) . . . . ? N1 C4 C5 C13 -3.8(6) . . . . ? C4 C5 C6 C7 1.6(7) . . . . ? C13 C5 C6 C7 178.3(4) . . . . ? C5 C6 C7 C8 -0.8(7) . . . . ? C6 C7 C8 C9 -1.5(7) . . . . ? C7 C8 C9 C4 2.7(7) . . . . ? C7 C8 C9 C10 -178.9(4) . . . . ? C5 C4 C9 C8 -1.9(6) . . . . ? N1 C4 C9 C8 -175.0(4) . . . . ? C5 C4 C9 C10 179.8(4) . . . . ? N1 C4 C9 C10 6.7(6) . . . . ? C8 C9 C10 C11 -50.6(6) . . . . ? C4 C9 C10 C11 127.6(5) . . . . ? C8 C9 C10 C12 70.9(5) . . . . ? C4 C9 C10 C12 -110.9(5) . . . . ? C6 C5 C13 C14 -88.3(6) . . . . ? C4 C5 C13 C14 88.2(6) . . . . ? C6 C5 C13 C15 35.8(6) . . . . ? C4 C5 C13 C15 -147.7(5) . . . . ? C1 N2 C16 C17 87.5(5) . . . . ? C3 N2 C16 C17 -107.5(5) . . . . ? C1 N2 C16 C21 -95.9(5) . . . . ? C3 N2 C16 C21 69.1(5) . . . . ? C21 C16 C17 C18 4.4(6) . . . . ? N2 C16 C17 C18 -179.1(4) . . . . ? C21 C16 C17 C22 -170.5(4) . . . . ? N2 C16 C17 C22 6.0(6) . . . . ? C16 C17 C18 C19 -1.5(7) . . . . ? C22 C17 C18 C19 173.6(4) . . . . ? C17 C18 C19 C20 -1.7(8) . . . . ? C18 C19 C20 C21 2.2(8) . . . . ? C19 C20 C21 C16 0.7(7) . . . . ? C19 C20 C21 C25 -177.3(5) . . . . ? C17 C16 C21 C20 -4.0(6) . . . . ? N2 C16 C21 C20 179.4(4) . . . . ? C17 C16 C21 C25 173.9(4) . . . . ? N2 C16 C21 C25 -2.7(6) . . . . ? C18 C17 C22 C23 47.3(6) . . . . ? C16 C17 C22 C23 -138.0(5) . . . . ? C18 C17 C22 C24 -76.2(5) . . . . ? C16 C17 C22 C24 98.6(5) . . . . ? C20 C21 C25 C26 -55.6(6) . . . . ? C16 C21 C25 C26 126.6(5) . . . . ? C20 C21 C25 C27 69.9(6) . . . . ? C16 C21 C25 C27 -108.0(5) . . . . ? C32 N3 C28 C29 -0.2(7) . . . . ? Ir1 N3 C28 C29 166.4(4) . . . . ? N3 C28 C29 C30 -0.4(8) . . . . ? C28 C29 C30 C31 0.5(9) . . . . ? C29 C30 C31 C32 0.0(9) . . . . ? C28 N3 C32 C31 0.7(7) . . . . ? Ir1 N3 C32 C31 -166.2(4) . . . . ? C30 C31 C32 N3 -0.6(8) . . . . ? C1 Ir1 C33 C34 -83.4(3) . . . . ? N3 Ir1 C33 C34 159.5(4) . . . . ? C38 Ir1 C33 C34 113.1(3) . . . . ? C37 Ir1 C33 C34 76.6(3) . . . . ? C1 Ir1 C33 C40 157.9(4) . . . . ? N3 Ir1 C33 C40 40.8(7) . . . . ? C34 Ir1 C33 C40 -118.7(5) . . . . ? C38 Ir1 C33 C40 -5.6(4) . . . . ? C37 Ir1 C33 C40 -42.0(4) . . . . ? C40 C33 C34 C35 3.8(8) . . . . ? Ir1 C33 C34 C35 -102.4(5) . . . . ? C40 C33 C34 Ir1 106.2(4) . . . . ? C1 Ir1 C34 C33 97.4(3) . . . . ? N3 Ir1 C34 C33 -157.9(4) . . . . ? C38 Ir1 C34 C33 -66.4(3) . . . . ? C37 Ir1 C34 C33 -100.2(3) . . . . ? C1 Ir1 C34 C35 -140.3(4) . . . . ? N3 Ir1 C34 C35 -35.6(7) . . . . ? C33 Ir1 C34 C35 122.3(5) . . . . ? C38 Ir1 C34 C35 55.9(4) . . . . ? C37 Ir1 C34 C35 22.1(3) . . . . ? C33 C34 C35 C36 45.5(7) . . . . ? Ir1 C34 C35 C36 -36.0(6) . . . . ? C34 C35 C36 C37 31.8(7) . . . . ? C35 C36 C37 C38 -93.2(6) . . . . ? C35 C36 C37 Ir1 -12.4(6) . . . . ? C1 Ir1 C37 C38 175.4(4) . . . . ? N3 Ir1 C37 C38 -82.7(3) . . . . ? C34 Ir1 C37 C38 113.9(3) . . . . ? C33 Ir1 C37 C38 76.3(3) . . . . ? C1 Ir1 C37 C36 56.0(7) . . . . ? N3 Ir1 C37 C36 158.0(4) . . . . ? C34 Ir1 C37 C36 -5.4(4) . . . . ? C33 Ir1 C37 C36 -43.0(4) . . . . ? C38 Ir1 C37 C36 -119.3(5) . . . . ? C36 C37 C38 C39 1.2(7) . . . . ? Ir1 C37 C38 C39 -103.0(4) . . . . ? C36 C37 C38 Ir1 104.1(4) . . . . ? C40 C39 C38 C37 50.0(6) . . . . ? C40 C39 C38 Ir1 -31.8(5) . . . . ? C1 Ir1 C38 C37 -174.6(5) . . . . ? N3 Ir1 C38 C37 94.6(3) . . . . ? C34 Ir1 C38 C37 -65.6(3) . . . . ? C33 Ir1 C38 C37 -100.7(3) . . . . ? C1 Ir1 C38 C39 -53.6(7) . . . . ? N3 Ir1 C38 C39 -144.4(4) . . . . ? C34 Ir1 C38 C39 55.4(4) . . . . ? C33 Ir1 C38 C39 20.3(3) . . . . ? C37 Ir1 C38 C39 121.0(5) . . . . ? C34 C33 C40 C39 -91.2(6) . . . . ? Ir1 C33 C40 C39 -9.9(5) . . . . ? C38 C39 C40 C33 27.6(6) . . . . ? C1A Ir1A N3A C28A -102.8(3) . . . . ? C33A Ir1A N3A C28A 0.8(6) . . . . ? C34A Ir1A N3A C28A 138.8(4) . . . . ? C37A Ir1A N3A C28A 96.1(3) . . . . ? C38A Ir1A N3A C28A 58.6(3) . . . . ? C1A Ir1A N3A C32A 89.0(3) . . . . ? C33A Ir1A N3A C32A -167.4(4) . . . . ? C34A Ir1A N3A C32A -29.4(6) . . . . ? C37A Ir1A N3A C32A -72.1(3) . . . . ? C38A Ir1A N3A C32A -109.7(3) . . . . ? C3A N2A C1A N1A 1.4(4) . . . . ? C16A N2A C1A N1A -165.9(4) . . . . ? C3A N2A C1A Ir1A -169.1(3) . . . . ? C16A N2A C1A Ir1A 23.6(5) . . . . ? C2A N1A C1A N2A -1.2(4) . . . . ? C4A N1A C1A N2A 171.4(4) . . . . ? C2A N1A C1A Ir1A 168.6(3) . . . . ? C4A N1A C1A Ir1A -18.7(6) . . . . ? N3A Ir1A C1A N2A -70.2(3) . . . . ? C33A Ir1A C1A N2A 130.7(3) . . . . ? C34A Ir1A C1A N2A 92.7(3) . . . . ? C37A Ir1A C1A N2A 25.3(7) . . . . ? C38A Ir1A C1A N2A -173.3(4) . . . . ? N3A Ir1A C1A N1A 122.0(4) . . . . ? C33A Ir1A C1A N1A -37.1(4) . . . . ? C34A Ir1A C1A N1A -75.1(4) . . . . ? C37A Ir1A C1A N1A -142.5(5) . . . . ? C38A Ir1A C1A N1A 18.9(7) . . . . ? C1A N2A C3A C2A -1.1(5) . . . . ? C16A N2A C3A C2A 166.8(4) . . . . ? N2A C3A C2A N1A 0.3(5) . . . . ? C1A N1A C2A C3A 0.6(5) . . . . ? C4A N1A C2A C3A -172.7(4) . . . . ? C1A N1A C4A C9A 117.7(5) . . . . ? C2A N1A C4A C9A -70.2(5) . . . . ? C1A N1A C4A C5A -68.3(6) . . . . ? C2A N1A C4A C5A 103.8(5) . . . . ? C9A C4A C5A C6A -2.7(7) . . . . ? N1A C4A C5A C6A -176.4(4) . . . . ? C9A C4A C5A C13A 172.9(4) . . . . ? N1A C4A C5A C13A -0.7(6) . . . . ? C4A C5A C6A C7A 1.9(7) . . . . ? C13A C5A C6A C7A -173.8(5) . . . . ? C5A C6A C7A C8A 0.1(8) . . . . ? C6A C7A C8A C9A -1.5(8) . . . . ? C5A C4A C9A C8A 1.5(7) . . . . ? N1A C4A C9A C8A 175.1(4) . . . . ? C5A C4A C9A C10A -177.6(4) . . . . ? N1A C4A C9A C10A -3.9(6) . . . . ? C7A C8A C9A C4A 0.7(7) . . . . ? C7A C8A C9A C10A 179.8(5) . . . . ? C4A C9A C10A C12A 108.6(5) . . . . ? C8A C9A C10A C12A -70.4(5) . . . . ? C4A C9A C10A C11A -128.8(5) . . . . ? C8A C9A C10A C11A 52.2(6) . . . . ? C6A C5A C13A C15A 92.9(5) . . . . ? C4A C5A C13A C15A -82.5(5) . . . . ? C6A C5A C13A C14A -28.9(6) . . . . ? C4A C5A C13A C14A 155.7(4) . . . . ? C1A N2A C16A C21A -93.3(5) . . . . ? C3A N2A C16A C21A 100.5(5) . . . . ? C1A N2A C16A C17A 89.6(5) . . . . ? C3A N2A C16A C17A -76.7(5) . . . . ? C21A C16A C17A C18A 3.9(6) . . . . ? N2A C16A C17A C18A -179.0(4) . . . . ? C21A C16A C17A C25A -173.0(4) . . . . ? N2A C16A C17A C25A 4.0(6) . . . . ? C16A C17A C18A C19A -1.0(7) . . . . ? C25A C17A C18A C19A 176.0(4) . . . . ? C17A C18A C19A C20A -1.7(7) . . . . ? C18A C19A C20A C21A 1.6(7) . . . . ? C17A C16A C21A C20A -4.0(6) . . . . ? N2A C16A C21A C20A 179.0(4) . . . . ? C17A C16A C21A C22A 169.4(4) . . . . ? N2A C16A C21A C22A -7.6(6) . . . . ? C19A C20A C21A C16A 1.1(7) . . . . ? C19A C20A C21A C22A -172.3(4) . . . . ? C16A C21A C22A C23A 140.6(4) . . . . ? C20A C21A C22A C23A -46.4(6) . . . . ? C16A C21A C22A C24A -95.6(5) . . . . ? C20A C21A C22A C24A 77.5(5) . . . . ? C18A C17A C25A C27A 54.2(6) . . . . ? C16A C17A C25A C27A -129.0(4) . . . . ? C18A C17A C25A C26A -68.8(6) . . . . ? C16A C17A C25A C26A 108.1(5) . . . . ? C32A N3A C28A C29A -0.6(6) . . . . ? Ir1A N3A C28A C29A -169.3(3) . . . . ? N3A C28A C29A C30A -0.2(7) . . . . ? C28A C29A C30A C31A 0.8(7) . . . . ? C29A C30A C31A C32A -0.5(7) . . . . ? C28A N3A C32A C31A 0.9(6) . . . . ? Ir1A N3A C32A C31A 169.7(3) . . . . ? C30A C31A C32A N3A -0.4(7) . . . . ? C1A Ir1A C33A C34A -95.8(3) . . . . ? N3A Ir1A C33A C34A 158.8(4) . . . . ? C37A Ir1A C33A C34A 65.9(3) . . . . ? C38A Ir1A C33A C34A 100.1(3) . . . . ? C1A Ir1A C33A C40A 141.7(3) . . . . ? N3A Ir1A C33A C40A 36.3(6) . . . . ? C34A Ir1A C33A C40A -122.5(5) . . . . ? C37A Ir1A C33A C40A -56.6(4) . . . . ? C38A Ir1A C33A C40A -22.4(3) . . . . ? C40A C33A C34A C35A -3.8(7) . . . . ? Ir1A C33A C34A C35A -106.4(4) . . . . ? C40A C33A C34A Ir1A 102.5(5) . . . . ? C1A Ir1A C34A C33A 84.1(3) . . . . ? N3A Ir1A C34A C33A -156.6(4) . . . . ? C37A Ir1A C34A C33A -113.5(3) . . . . ? C38A Ir1A C34A C33A -76.8(3) . . . . ? C1A Ir1A C34A C35A -157.4(3) . . . . ? N3A Ir1A C34A C35A -38.2(6) . . . . ? C33A Ir1A C34A C35A 118.5(4) . . . . ? C37A Ir1A C34A C35A 4.9(3) . . . . ? C38A Ir1A C34A C35A 41.6(3) . . . . ? C33A C34A C35A C36A 91.0(5) . . . . ? Ir1A C34A C35A C36A 10.0(5) . . . . ? C34A C35A C36A C37A -27.1(6) . . . . ? C35A C36A C37A C38A -50.6(6) . . . . ? C35A C36A C37A Ir1A 30.9(5) . . . . ? C1A Ir1A C37A C38A 170.1(4) . . . . ? N3A Ir1A C37A C38A -92.2(3) . . . . ? C33A Ir1A C37A C38A 66.2(3) . . . . ? C34A Ir1A C37A C38A 101.1(3) . . . . ? C1A Ir1A C37A C36A 49.7(7) . . . . ? N3A Ir1A C37A C36A 147.4(3) . . . . ? C33A Ir1A C37A C36A -54.2(4) . . . . ? C34A Ir1A C37A C36A -19.3(3) . . . . ? C38A Ir1A C37A C36A -120.4(5) . . . . ? C36A C37A C38A C39A -0.6(7) . . . . ? Ir1A C37A C38A C39A -103.8(4) . . . . ? C36A C37A C38A Ir1A 103.1(4) . . . . ? C1A Ir1A C38A C37A -170.2(4) . . . . ? N3A Ir1A C38A C37A 84.9(3) . . . . ? C33A Ir1A C38A C37A -113.4(3) . . . . ? C34A Ir1A C38A C37A -75.8(3) . . . . ? C1A Ir1A C38A C39A -51.3(7) . . . . ? N3A Ir1A C38A C39A -156.2(4) . . . . ? C33A Ir1A C38A C39A 5.5(3) . . . . ? C34A Ir1A C38A C39A 43.1(4) . . . . ? C37A Ir1A C38A C39A 118.9(5) . . . . ? C37A C38A C39A C40A 93.0(6) . . . . ? Ir1A C38A C39A C40A 12.5(5) . . . . ? C34A C33A C40A C39A -45.7(7) . . . . ? Ir1A C33A C40A C39A 36.4(5) . . . . ? C38A C39A C40A C33A -32.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.467 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.118