# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chunhui Huang' _publ_contact_author_email CHHUANG@PKU.EDU.CN _publ_section_title ; Sensitised near-infrared emission from lanthanides using an iridium complex as a ligand in heteronuclear Ir2Ln arrays ; loop_ _publ_author_name 'Chunhui Huang.' 'Zu-Qiang Bian.' 'Jiang Bian.' 'Fang-Fang Chen.' ; Zhuqi Chen ; 'Zhong-Ning Chen.' 'Zhiwei Liu.' 'Bin Lou.' 'En Ma.' 'Dao-Bo Nie.' # Attachment 'Ir-ppy-phen5f.cif' data_61106c _database_code_depnum_ccdc_archive 'CCDC 631669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Iridium bis(2-phenylpyridinato-N,C2) (4,4,5,5,5-pentafluoro-1- (1,10-phenanthrolin-2-yl)pentane-1,3-dionate) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H24 F5 Ir N4 O2' _chemical_formula_weight 867.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.612(2) _cell_length_b 17.190(3) _cell_length_c 18.641(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.554(3) _cell_angle_gamma 90.00 _cell_volume 3996.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4775 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.85 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 3.400 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.704585 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 19499 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7008 _reflns_number_gt 3935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0479P)^2^+3.1411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7008 _refine_ls_number_parameters 523 _refine_ls_number_restraints 313 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.085 _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 -0.01728(3) 0.755021(19) 0.864383(18) 0.03921(12) Uani 1 1 d . . . O1 O 0.1509(6) 0.6419(4) 1.0221(4) 0.064(2) Uani 1 1 d . . . O2 O 0.3013(5) 0.8558(4) 0.9931(4) 0.074(2) Uani 1 1 d . A . N1 N -0.1028(6) 0.6712(4) 0.9106(4) 0.043(2) Uani 1 1 d . . . N2 N 0.0710(6) 0.8273(4) 0.8086(4) 0.0387(18) Uani 1 1 d . . . N3 N -0.1231(6) 0.8516(4) 0.8777(4) 0.0400(19) Uani 1 1 d . . . N4 N 0.0421(6) 0.7991(4) 0.9762(4) 0.0383(18) Uani 1 1 d . . . C1 C -0.1956(8) 0.6845(6) 0.9360(5) 0.055(3) Uani 1 1 d . . . H1 H -0.2241 0.7345 0.9340 0.065 Uiso 1 1 calc R . . C2 C -0.2487(9) 0.6255(6) 0.9648(6) 0.072(3) Uani 1 1 d . . . H2 H -0.3123 0.6353 0.9828 0.087 Uiso 1 1 calc R . . C3 C -0.2067(10) 0.5508(6) 0.9669(6) 0.068(3) Uani 1 1 d . . . H3 H -0.2415 0.5102 0.9869 0.082 Uiso 1 1 calc R . . C4 C -0.1137(9) 0.5373(6) 0.9393(6) 0.060(3) Uani 1 1 d . . . H4 H -0.0853 0.4873 0.9408 0.071 Uiso 1 1 calc R . . C5 C -0.0609(8) 0.5979(5) 0.9088(5) 0.046(2) Uani 1 1 d . . . C6 C 0.0353(7) 0.5911(5) 0.8755(5) 0.044(2) Uani 1 1 d . . . C7 C 0.0868(9) 0.5207(5) 0.8682(6) 0.060(3) Uani 1 1 d . . . H7 H 0.0591 0.4754 0.8853 0.072 Uiso 1 1 calc R . . C8 C 0.1773(10) 0.5171(6) 0.8362(6) 0.074(4) Uani 1 1 d . . . H8 H 0.2101 0.4696 0.8299 0.089 Uiso 1 1 calc R . . C9 C 0.2194(9) 0.5864(7) 0.8133(6) 0.068(3) Uani 1 1 d . . . H9 H 0.2817 0.5851 0.7922 0.081 Uiso 1 1 calc R . . C10 C 0.1696(8) 0.6569(6) 0.8217(5) 0.056(3) Uani 1 1 d . . . H10 H 0.1995 0.7024 0.8065 0.067 Uiso 1 1 calc R . . C11 C 0.0757(7) 0.6610(5) 0.8524(5) 0.042(2) Uani 1 1 d . . . C12 C 0.1555(8) 0.8672(5) 0.8387(6) 0.056(3) Uani 1 1 d . . . H12 H 0.1755 0.8648 0.8887 0.067 Uiso 1 1 calc R . . C13 C 0.2160(9) 0.9128(6) 0.7978(7) 0.067(3) Uani 1 1 d . . . H13 H 0.2730 0.9425 0.8205 0.080 Uiso 1 1 calc R . . C14 C 0.1898(9) 0.9130(7) 0.7237(7) 0.072(3) Uani 1 1 d . . . H14 H 0.2306 0.9414 0.6952 0.087 Uiso 1 1 calc R . . C15 C 0.1030(9) 0.8711(6) 0.6924(6) 0.063(3) Uani 1 1 d . . . H15 H 0.0841 0.8712 0.6423 0.075 Uiso 1 1 calc R . . C16 C 0.0423(8) 0.8277(5) 0.7356(5) 0.047(2) Uani 1 1 d . . . C17 C -0.0512(8) 0.7791(5) 0.7079(6) 0.051(3) Uani 1 1 d . . . C18 C -0.1004(9) 0.7784(6) 0.6368(6) 0.060(3) Uani 1 1 d . . . H18 H -0.0756 0.8107 0.6029 0.072 Uiso 1 1 calc R . . C19 C -0.1851(10) 0.7306(7) 0.6164(6) 0.073(3) Uani 1 1 d . . . H19 H -0.2189 0.7299 0.5685 0.088 Uiso 1 1 calc R . . C20 C -0.2212(9) 0.6821(7) 0.6686(6) 0.073(3) Uani 1 1 d . . . H20 H -0.2786 0.6486 0.6549 0.088 Uiso 1 1 calc R . . C21 C -0.1716(8) 0.6839(6) 0.7405(6) 0.059(3) Uani 1 1 d . . . H21 H -0.1956 0.6504 0.7739 0.070 Uiso 1 1 calc R . . C22 C -0.0888(7) 0.7332(5) 0.7634(6) 0.051(3) Uani 1 1 d . . . C23 C -0.2008(8) 0.8780(5) 0.8290(6) 0.054(3) Uani 1 1 d . . . H23 H -0.2139 0.8531 0.7843 0.065 Uiso 1 1 calc R . . C24 C -0.2633(8) 0.9400(6) 0.8405(6) 0.061(3) Uani 1 1 d . . . H24 H -0.3150 0.9577 0.8033 0.074 Uiso 1 1 calc R . . C25 C -0.2505(8) 0.9761(6) 0.9063(6) 0.061(3) Uani 1 1 d . . . H25 H -0.2941 1.0176 0.9153 0.074 Uiso 1 1 calc R . . C26 C -0.1698(8) 0.9490(5) 0.9597(6) 0.049(3) Uani 1 1 d . . . C27 C -0.1491(8) 0.9819(5) 1.0316(6) 0.058(3) Uani 1 1 d . . . H27 H -0.1916 1.0227 1.0436 0.069 Uiso 1 1 calc R . . C28 C -0.0709(8) 0.9554(5) 1.0810(6) 0.055(3) Uani 1 1 d . . . H28 H -0.0607 0.9775 1.1271 0.067 Uiso 1 1 calc R . . C29 C -0.0019(7) 0.8938(5) 1.0652(5) 0.044(2) Uani 1 1 d . . . C30 C 0.0821(8) 0.8661(5) 1.1157(5) 0.053(3) Uani 1 1 d . . . H30 H 0.0952 0.8868 1.1623 0.063 Uiso 1 1 calc R . . C31 C 0.1441(8) 0.8084(6) 1.0953(5) 0.056(3) Uani 1 1 d . . . H31 H 0.2018 0.7901 1.1279 0.067 Uiso 1 1 calc R . . C32 C 0.1223(7) 0.7750(5) 1.0241(5) 0.041(2) Uani 1 1 d . . . C33 C -0.0199(7) 0.8587(4) 0.9958(5) 0.040(2) Uani 1 1 d . . . C34 C -0.1069(7) 0.8867(5) 0.9440(5) 0.038(2) Uani 1 1 d . . . C35 C 0.1899(8) 0.7062(5) 1.0097(5) 0.048(3) Uani 1 1 d . . . C36 C 0.2941(8) 0.7179(6) 0.9910(6) 0.066(3) Uani 1 1 d . A . H36 H 0.3344 0.6743 0.9830 0.079 Uiso 1 1 calc R . . C37 C 0.3373(7) 0.7885(7) 0.9843(7) 0.071(3) Uani 1 1 d D . . C38 C 0.4488(10) 0.7910(10) 0.9584(9) 0.143(7) Uani 0.50 1 d PDU A 1 C39 C 0.5303(12) 0.8528(9) 0.9900(10) 0.171(8) Uani 0.50 1 d PDU A 1 F1 F 0.4467(17) 0.8328(13) 0.8941(10) 0.160(6) Uani 0.50 1 d PDU A 1 F2 F 0.5138(13) 0.7380(10) 1.0004(10) 0.125(5) Uani 0.50 1 d PDU A 1 F3 F 0.5168(17) 0.8243(14) 1.0567(11) 0.238(9) Uani 0.50 1 d PDU A 1 F4 F 0.6341(12) 0.8456(11) 0.9769(11) 0.159(7) Uani 0.50 1 d PDU A 1 F5 F 0.4889(15) 0.9255(9) 0.9726(12) 0.174(7) Uani 0.50 1 d PDU A 1 C38' C 0.4460(11) 0.7856(7) 0.9570(9) 0.150(7) Uani 0.50 1 d PDU A 2 C39' C 0.5214(11) 0.8560(8) 0.9623(7) 0.174(8) Uani 0.50 1 d PDU A 2 F1' F 0.4361(17) 0.7689(12) 0.8838(9) 0.168(6) Uani 0.50 1 d PDU A 2 F2' F 0.4868(13) 0.7149(7) 0.9446(11) 0.121(5) Uani 0.50 1 d PDU A 2 F3' F 0.5307(16) 0.8808(13) 1.0323(8) 0.188(7) Uani 0.50 1 d PDU A 2 F4' F 0.6031(14) 0.8150(11) 0.9397(10) 0.166(7) Uani 0.50 1 d PDU A 2 F5' F 0.4684(14) 0.9046(8) 0.9116(10) 0.161(6) Uani 0.50 1 d PDU 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 0.0487(2) 0.0342(2) 0.03587(18) -0.0014(2) 0.01028(13) 0.0035(2) O1 0.092(5) 0.042(4) 0.057(5) 0.001(4) 0.012(4) -0.003(4) O2 0.064(5) 0.060(4) 0.097(6) 0.004(5) 0.015(5) -0.003(4) N1 0.060(5) 0.022(4) 0.046(5) -0.003(4) 0.007(4) 0.004(3) N2 0.052(5) 0.032(4) 0.034(4) 0.005(4) 0.015(4) -0.001(4) N3 0.053(5) 0.031(4) 0.039(5) 0.009(4) 0.014(4) 0.006(4) N4 0.053(5) 0.024(4) 0.040(4) 0.002(3) 0.011(4) 0.002(3) C1 0.061(7) 0.047(6) 0.061(7) 0.000(5) 0.028(6) 0.001(5) C2 0.082(8) 0.063(7) 0.082(8) -0.010(7) 0.042(7) -0.013(6) C3 0.094(9) 0.055(7) 0.063(8) -0.001(6) 0.032(7) -0.026(6) C4 0.078(8) 0.044(6) 0.057(7) -0.001(5) 0.010(6) -0.006(5) C5 0.063(6) 0.032(5) 0.039(6) 0.000(5) -0.002(5) -0.005(5) C6 0.057(6) 0.037(5) 0.041(6) -0.007(4) 0.015(5) 0.007(4) C7 0.069(7) 0.043(6) 0.067(8) -0.012(6) 0.004(6) 0.004(5) C8 0.093(9) 0.052(7) 0.078(9) -0.013(6) 0.012(8) 0.027(6) C9 0.063(7) 0.075(8) 0.067(8) -0.016(7) 0.019(6) 0.016(6) C10 0.063(7) 0.059(6) 0.049(6) -0.007(5) 0.015(6) 0.007(5) C11 0.061(6) 0.035(5) 0.033(5) -0.009(4) 0.018(5) 0.009(4) C12 0.072(8) 0.039(6) 0.057(7) -0.002(5) 0.015(6) 0.008(5) C13 0.067(8) 0.055(7) 0.082(9) 0.009(7) 0.021(7) -0.009(6) C14 0.074(8) 0.075(8) 0.075(9) 0.022(7) 0.037(7) 0.001(7) C15 0.085(8) 0.063(7) 0.044(6) 0.016(6) 0.018(6) 0.017(6) C16 0.057(6) 0.041(5) 0.048(6) 0.007(5) 0.025(5) 0.019(5) C17 0.057(6) 0.048(6) 0.051(6) 0.003(5) 0.015(5) 0.018(5) C18 0.066(7) 0.072(7) 0.042(6) -0.003(5) 0.009(6) 0.018(6) C19 0.090(8) 0.083(8) 0.045(6) 0.004(6) 0.005(6) 0.020(7) C20 0.064(7) 0.084(8) 0.070(8) -0.023(7) 0.001(7) 0.000(6) C21 0.063(7) 0.066(7) 0.047(6) 0.006(6) 0.007(6) -0.001(6) C22 0.048(5) 0.039(5) 0.071(7) 0.001(5) 0.017(5) 0.014(5) C23 0.063(7) 0.050(6) 0.053(7) 0.007(5) 0.013(6) 0.013(5) C24 0.058(7) 0.056(6) 0.069(8) 0.010(6) 0.007(6) 0.013(5) C25 0.066(7) 0.047(6) 0.075(8) 0.002(6) 0.024(7) 0.021(5) C26 0.058(7) 0.031(5) 0.066(7) -0.004(5) 0.031(6) 0.001(5) C27 0.065(7) 0.043(6) 0.074(8) -0.015(6) 0.041(6) 0.003(5) C28 0.066(7) 0.050(6) 0.053(7) -0.014(5) 0.020(6) -0.001(5) C29 0.055(6) 0.035(5) 0.047(6) -0.006(5) 0.020(5) -0.005(5) C30 0.066(7) 0.050(6) 0.045(6) -0.012(5) 0.017(6) 0.000(5) C31 0.067(7) 0.052(6) 0.050(6) 0.006(5) 0.008(6) -0.004(5) C32 0.052(6) 0.033(5) 0.040(5) 0.004(4) 0.011(5) -0.007(4) C33 0.054(6) 0.023(4) 0.048(6) 0.007(4) 0.029(5) -0.007(4) C34 0.050(6) 0.032(5) 0.037(5) -0.001(4) 0.021(5) -0.007(4) C35 0.071(7) 0.032(5) 0.041(6) 0.001(5) 0.006(5) 0.005(5) C36 0.059(7) 0.054(6) 0.089(9) 0.005(6) 0.023(7) 0.012(5) C37 0.050(7) 0.081(8) 0.087(9) 0.008(7) 0.024(7) 0.018(6) C38 0.145(8) 0.142(8) 0.143(8) 0.002(5) 0.021(5) 0.001(5) C39 0.171(8) 0.174(9) 0.171(9) -0.001(5) 0.028(5) 0.002(5) F1 0.159(7) 0.163(7) 0.160(7) 0.002(5) 0.034(5) 0.000(5) F2 0.118(6) 0.128(6) 0.133(6) 0.002(5) 0.025(4) 0.009(4) F3 0.232(10) 0.243(10) 0.240(10) 0.003(5) 0.033(5) -0.003(5) F4 0.150(8) 0.165(8) 0.164(8) 0.000(5) 0.026(5) -0.001(5) F5 0.172(8) 0.174(8) 0.176(8) 0.004(5) 0.028(5) -0.003(5) C38' 0.151(8) 0.149(8) 0.149(8) 0.003(5) 0.022(5) 0.001(5) C39' 0.172(8) 0.175(8) 0.174(9) -0.003(5) 0.026(5) 0.002(5) F1' 0.168(7) 0.173(7) 0.168(7) -0.005(5) 0.037(5) -0.004(5) F2' 0.113(6) 0.123(6) 0.128(6) -0.008(4) 0.024(4) 0.009(4) F3' 0.184(8) 0.189(8) 0.188(8) 0.002(5) 0.022(5) -0.003(5) F4' 0.160(8) 0.168(8) 0.172(8) 0.000(5) 0.027(5) 0.001(5) F5' 0.161(7) 0.161(7) 0.161(8) 0.006(5) 0.026(5) 0.000(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 C22 1.998(11) . ? Ir1 C11 2.028(8) . ? Ir1 N2 2.052(7) . ? Ir1 N1 2.063(7) . ? Ir1 N3 2.166(7) . ? Ir1 N4 2.239(7) . ? O1 C35 1.245(10) . ? O2 C37 1.263(12) . ? N1 C1 1.346(11) . ? N1 C5 1.369(10) . ? N2 C12 1.320(11) . ? N2 C16 1.355(11) . ? N3 C23 1.314(11) . ? N3 C34 1.364(10) . ? N4 C32 1.313(11) . ? N4 C33 1.370(10) . ? C1 C2 1.368(12) . ? C1 H1 0.9300 . ? C2 C3 1.387(14) . ? C2 H2 0.9300 . ? C3 C4 1.369(14) . ? C3 H3 0.9300 . ? C4 C5 1.402(12) . ? C4 H4 0.9300 . ? C5 C6 1.448(12) . ? C6 C7 1.390(12) . ? C6 C11 1.398(12) . ? C7 C8 1.365(14) . ? C7 H7 0.9300 . ? C8 C9 1.396(15) . ? C8 H8 0.9300 . ? C9 C10 1.386(13) . ? C9 H9 0.9300 . ? C10 C11 1.391(12) . ? C10 H10 0.9300 . ? C12 C13 1.396(13) . ? C12 H12 0.9300 . ? C13 C14 1.372(15) . ? C13 H13 0.9300 . ? C14 C15 1.367(14) . ? C14 H14 0.9300 . ? C15 C16 1.405(12) . ? C15 H15 0.9300 . ? C16 C17 1.475(13) . ? C17 C18 1.377(14) . ? C17 C22 1.437(13) . ? C18 C19 1.358(15) . ? C18 H18 0.9300 . ? C19 C20 1.407(14) . ? C19 H19 0.9300 . ? C20 C21 1.393(14) . ? C20 H20 0.9300 . ? C21 C22 1.363(13) . ? C21 H21 0.9300 . ? C23 C24 1.360(12) . ? C23 H23 0.9300 . ? C24 C25 1.363(14) . ? C24 H24 0.9300 . ? C25 C26 1.394(13) . ? C25 H25 0.9300 . ? C26 C34 1.389(11) . ? C26 C27 1.443(13) . ? C27 C28 1.326(13) . ? C27 H27 0.9300 . ? C28 C29 1.428(12) . ? C28 H28 0.9300 . ? C29 C30 1.392(12) . ? C29 C33 1.415(12) . ? C30 C31 1.354(12) . ? C30 H30 0.9300 . ? C31 C32 1.435(12) . ? C31 H31 0.9300 . ? C32 C35 1.504(12) . ? C33 C34 1.433(12) . ? C35 C36 1.423(13) . ? C36 C37 1.344(14) . ? C36 H36 0.9300 . ? C37 C38' 1.533(9) . ? C37 C38 1.554(9) . ? C38 F2 1.387(9) . ? C38 F1 1.394(10) . ? C38 C39 1.533(10) . ? C39 F3 1.369(10) . ? C39 F4 1.372(9) . ? C39 F5 1.375(9) . ? C38' F2' 1.353(9) . ? C38' F1' 1.383(10) . ? C38' C39' 1.532(9) . ? C39' F5' 1.361(9) . ? C39' F3' 1.361(9) . ? C39' F4' 1.366(9) . ? F1' F2' 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Ir1 C11 86.2(3) . . ? C22 Ir1 N2 80.8(4) . . ? C11 Ir1 N2 93.5(3) . . ? C22 Ir1 N1 94.1(3) . . ? C11 Ir1 N1 80.6(3) . . ? N2 Ir1 N1 172.4(3) . . ? C22 Ir1 N3 93.0(3) . . ? C11 Ir1 N3 177.2(3) . . ? N2 Ir1 N3 89.1(3) . . ? N1 Ir1 N3 96.8(3) . . ? C22 Ir1 N4 169.1(3) . . ? C11 Ir1 N4 104.7(3) . . ? N2 Ir1 N4 97.8(3) . . ? N1 Ir1 N4 88.3(3) . . ? N3 Ir1 N4 76.1(3) . . ? C1 N1 C5 121.6(8) . . ? C1 N1 Ir1 124.4(6) . . ? C5 N1 Ir1 113.9(6) . . ? C12 N2 C16 120.1(9) . . ? C12 N2 Ir1 124.3(7) . . ? C16 N2 Ir1 115.4(6) . . ? C23 N3 C34 117.9(8) . . ? C23 N3 Ir1 126.5(6) . . ? C34 N3 Ir1 115.6(6) . . ? C32 N4 C33 117.8(8) . . ? C32 N4 Ir1 130.0(6) . . ? C33 N4 Ir1 112.1(6) . . ? N1 C1 C2 120.9(9) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 119.4(10) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.4(10) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.8(10) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 117.8(9) . . ? N1 C5 C6 115.8(8) . . ? C4 C5 C6 126.4(9) . . ? C7 C6 C11 121.4(9) . . ? C7 C6 C5 123.1(9) . . ? C11 C6 C5 115.5(8) . . ? C8 C7 C6 121.1(10) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 118.3(10) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 120.9(10) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 121.2(10) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 117.0(8) . . ? C10 C11 Ir1 128.8(7) . . ? C6 C11 Ir1 114.1(6) . . ? N2 C12 C13 122.1(10) . . ? N2 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 118.8(11) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 119.0(11) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.4(10) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? N2 C16 C15 119.4(9) . . ? N2 C16 C17 115.4(9) . . ? C15 C16 C17 125.1(10) . . ? C18 C17 C22 122.6(10) . . ? C18 C17 C16 124.3(10) . . ? C22 C17 C16 113.0(9) . . ? C19 C18 C17 119.9(11) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.2(11) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 120.4(11) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 121.9(11) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C17 115.8(10) . . ? C21 C22 Ir1 129.0(8) . . ? C17 C22 Ir1 115.1(7) . . ? N3 C23 C24 123.5(10) . . ? N3 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C25 120.4(10) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 117.7(9) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C34 C26 C25 119.1(9) . . ? C34 C26 C27 117.9(10) . . ? C25 C26 C27 122.9(9) . . ? C28 C27 C26 121.5(9) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 121.7(9) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C30 C29 C33 118.4(8) . . ? C30 C29 C28 122.6(9) . . ? C33 C29 C28 119.0(9) . . ? C31 C30 C29 118.3(9) . . ? C31 C30 H30 120.9 . . ? C29 C30 H30 120.9 . . ? C30 C31 C32 121.0(10) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? N4 C32 C31 121.7(8) . . ? N4 C32 C35 121.9(8) . . ? C31 C32 C35 116.3(9) . . ? N4 C33 C29 122.9(9) . . ? N4 C33 C34 118.7(8) . . ? C29 C33 C34 118.4(8) . . ? N3 C34 C26 121.3(9) . . ? N3 C34 C33 117.3(8) . . ? C26 C34 C33 121.4(9) . . ? O1 C35 C36 125.1(9) . . ? O1 C35 C32 114.5(9) . . ? C36 C35 C32 120.1(8) . . ? C37 C36 C35 123.5(9) . . ? C37 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? O2 C37 C36 131.1(8) . . ? O2 C37 C38' 115.4(10) . . ? C36 C37 C38' 113.4(10) . . ? O2 C37 C38 111.9(11) . . ? C36 C37 C38 116.9(11) . . ? C38' C37 C38 3.7(8) . . ? F2 C38 F1 139.3(16) . . ? F2 C38 C39 86.1(12) . . ? F1 C38 C39 84.3(14) . . ? F2 C38 C37 107.0(12) . . ? F1 C38 C37 112.3(13) . . ? C39 C38 C37 119.0(13) . . ? F3 C39 F4 112.3(12) . . ? F3 C39 F5 116.5(13) . . ? F4 C39 F5 112.2(11) . . ? F3 C39 C38 86.3(16) . . ? F4 C39 C38 118.1(15) . . ? F5 C39 C38 109.3(15) . . ? F2' C38' F1' 68.0(12) . . ? F2' C38' C39' 118.2(12) . . ? F1' C38' C39' 101.1(8) . . ? F2' C38' C37 117.8(12) . . ? F1' C38' C37 112.3(16) . . ? C39' C38' C37 122.0(11) . . ? F5' C39' F3' 115.9(10) . . ? F5' C39' F4' 114.6(11) . . ? F3' C39' F4' 119.7(11) . . ? F5' C39' C38' 101.8(8) . . ? F3' C39' C38' 105.9(15) . . ? F4' C39' C38' 93.5(12) . . ? C38' F1' F2' 55.1(7) . . ? C38' F2' F1' 56.9(8) . . ? 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 C22 Ir1 N1 C1 -92.0(8) . . . . ? C11 Ir1 N1 C1 -177.4(8) . . . . ? N2 Ir1 N1 C1 -139(2) . . . . ? N3 Ir1 N1 C1 1.5(8) . . . . ? N4 Ir1 N1 C1 77.4(8) . . . . ? C22 Ir1 N1 C5 83.5(6) . . . . ? C11 Ir1 N1 C5 -2.0(6) . . . . ? N2 Ir1 N1 C5 37(2) . . . . ? N3 Ir1 N1 C5 177.0(6) . . . . ? N4 Ir1 N1 C5 -107.2(6) . . . . ? C22 Ir1 N2 C12 -174.4(8) . . . . ? C11 Ir1 N2 C12 -88.8(7) . . . . ? N1 Ir1 N2 C12 -127(2) . . . . ? N3 Ir1 N2 C12 92.5(7) . . . . ? N4 Ir1 N2 C12 16.6(7) . . . . ? C22 Ir1 N2 C16 0.5(6) . . . . ? C11 Ir1 N2 C16 86.1(6) . . . . ? N1 Ir1 N2 C16 48(2) . . . . ? N3 Ir1 N2 C16 -92.6(6) . . . . ? N4 Ir1 N2 C16 -168.5(6) . . . . ? C22 Ir1 N3 C23 -1.1(8) . . . . ? C11 Ir1 N3 C23 -74(7) . . . . ? N2 Ir1 N3 C23 79.6(7) . . . . ? N1 Ir1 N3 C23 -95.6(8) . . . . ? N4 Ir1 N3 C23 177.9(8) . . . . ? C22 Ir1 N3 C34 177.9(6) . . . . ? C11 Ir1 N3 C34 105(6) . . . . ? N2 Ir1 N3 C34 -101.4(6) . . . . ? N1 Ir1 N3 C34 83.4(6) . . . . ? N4 Ir1 N3 C34 -3.2(6) . . . . ? C22 Ir1 N4 C32 -173.6(15) . . . . ? C11 Ir1 N4 C32 3.5(8) . . . . ? N2 Ir1 N4 C32 -92.2(7) . . . . ? N1 Ir1 N4 C32 83.4(7) . . . . ? N3 Ir1 N4 C32 -179.2(8) . . . . ? C22 Ir1 N4 C33 8.9(19) . . . . ? C11 Ir1 N4 C33 -174.0(5) . . . . ? N2 Ir1 N4 C33 90.3(5) . . . . ? N1 Ir1 N4 C33 -94.1(5) . . . . ? N3 Ir1 N4 C33 3.2(5) . . . . ? C5 N1 C1 C2 3.7(15) . . . . ? Ir1 N1 C1 C2 178.8(8) . . . . ? N1 C1 C2 C3 -0.9(17) . . . . ? C1 C2 C3 C4 -0.8(17) . . . . ? C2 C3 C4 C5 -0.2(17) . . . . ? C1 N1 C5 C4 -4.6(13) . . . . ? Ir1 N1 C5 C4 179.8(7) . . . . ? C1 N1 C5 C6 175.8(8) . . . . ? Ir1 N1 C5 C6 0.2(10) . . . . ? C3 C4 C5 N1 2.9(14) . . . . ? C3 C4 C5 C6 -177.6(10) . . . . ? N1 C5 C6 C7 -178.9(9) . . . . ? C4 C5 C6 C7 1.6(15) . . . . ? N1 C5 C6 C11 2.7(12) . . . . ? C4 C5 C6 C11 -176.8(9) . . . . ? C11 C6 C7 C8 -1.8(15) . . . . ? C5 C6 C7 C8 179.9(10) . . . . ? C6 C7 C8 C9 2.3(16) . . . . ? C7 C8 C9 C10 -1.1(17) . . . . ? C8 C9 C10 C11 -0.6(17) . . . . ? C9 C10 C11 C6 1.1(14) . . . . ? C9 C10 C11 Ir1 -175.5(8) . . . . ? C7 C6 C11 C10 0.0(14) . . . . ? C5 C6 C11 C10 178.5(8) . . . . ? C7 C6 C11 Ir1 177.2(7) . . . . ? C5 C6 C11 Ir1 -4.3(11) . . . . ? C22 Ir1 C11 C10 85.4(9) . . . . ? N2 Ir1 C11 C10 4.9(9) . . . . ? N1 Ir1 C11 C10 -179.8(9) . . . . ? N3 Ir1 C11 C10 159(6) . . . . ? N4 Ir1 C11 C10 -94.1(9) . . . . ? C22 Ir1 C11 C6 -91.4(7) . . . . ? N2 Ir1 C11 C6 -171.9(7) . . . . ? N1 Ir1 C11 C6 3.4(7) . . . . ? N3 Ir1 C11 C6 -18(7) . . . . ? N4 Ir1 C11 C6 89.2(7) . . . . ? C16 N2 C12 C13 2.2(13) . . . . ? Ir1 N2 C12 C13 176.9(7) . . . . ? N2 C12 C13 C14 -3.4(15) . . . . ? C12 C13 C14 C15 2.5(17) . . . . ? C13 C14 C15 C16 -0.7(16) . . . . ? C12 N2 C16 C15 -0.3(12) . . . . ? Ir1 N2 C16 C15 -175.4(6) . . . . ? C12 N2 C16 C17 178.0(8) . . . . ? Ir1 N2 C16 C17 2.9(10) . . . . ? C14 C15 C16 N2 -0.5(14) . . . . ? C14 C15 C16 C17 -178.6(9) . . . . ? N2 C16 C17 C18 172.2(9) . . . . ? C15 C16 C17 C18 -9.7(15) . . . . ? N2 C16 C17 C22 -6.0(11) . . . . ? C15 C16 C17 C22 172.1(8) . . . . ? C22 C17 C18 C19 -3.0(15) . . . . ? C16 C17 C18 C19 179.0(9) . . . . ? C17 C18 C19 C20 -0.1(16) . . . . ? C18 C19 C20 C21 0.9(16) . . . . ? C19 C20 C21 C22 1.5(17) . . . . ? C20 C21 C22 C17 -4.3(14) . . . . ? C20 C21 C22 Ir1 172.1(8) . . . . ? C18 C17 C22 C21 5.1(13) . . . . ? C16 C17 C22 C21 -176.6(8) . . . . ? C18 C17 C22 Ir1 -171.8(7) . . . . ? C16 C17 C22 Ir1 6.5(10) . . . . ? C11 Ir1 C22 C21 85.5(9) . . . . ? N2 Ir1 C22 C21 179.7(9) . . . . ? N1 Ir1 C22 C21 5.2(9) . . . . ? N3 Ir1 C22 C21 -91.8(9) . . . . ? N4 Ir1 C22 C21 -97.2(18) . . . . ? C11 Ir1 C22 C17 -98.1(7) . . . . ? N2 Ir1 C22 C17 -3.9(6) . . . . ? N1 Ir1 C22 C17 -178.4(6) . . . . ? N3 Ir1 C22 C17 84.6(6) . . . . ? N4 Ir1 C22 C17 79.1(18) . . . . ? C34 N3 C23 C24 2.3(13) . . . . ? Ir1 N3 C23 C24 -178.8(7) . . . . ? N3 C23 C24 C25 -3.0(16) . . . . ? C23 C24 C25 C26 1.9(15) . . . . ? C24 C25 C26 C34 -0.3(14) . . . . ? C24 C25 C26 C27 -179.4(9) . . . . ? C34 C26 C27 C28 1.8(14) . . . . ? C25 C26 C27 C28 -179.2(10) . . . . ? C26 C27 C28 C29 1.1(15) . . . . ? C27 C28 C29 C30 178.6(9) . . . . ? C27 C28 C29 C33 -2.0(14) . . . . ? C33 C29 C30 C31 1.7(13) . . . . ? C28 C29 C30 C31 -179.0(9) . . . . ? C29 C30 C31 C32 -1.7(14) . . . . ? C33 N4 C32 C31 1.1(12) . . . . ? Ir1 N4 C32 C31 -176.3(6) . . . . ? C33 N4 C32 C35 175.5(8) . . . . ? Ir1 N4 C32 C35 -1.9(12) . . . . ? C30 C31 C32 N4 0.3(14) . . . . ? C30 C31 C32 C35 -174.4(9) . . . . ? C32 N4 C33 C29 -1.0(11) . . . . ? Ir1 N4 C33 C29 176.8(6) . . . . ? C32 N4 C33 C34 179.1(7) . . . . ? Ir1 N4 C33 C34 -3.0(9) . . . . ? C30 C29 C33 N4 -0.4(12) . . . . ? C28 C29 C33 N4 -179.7(8) . . . . ? C30 C29 C33 C34 179.5(8) . . . . ? C28 C29 C33 C34 0.1(12) . . . . ? C23 N3 C34 C26 -0.6(12) . . . . ? Ir1 N3 C34 C26 -179.6(6) . . . . ? C23 N3 C34 C33 -178.2(8) . . . . ? Ir1 N3 C34 C33 2.7(9) . . . . ? C25 C26 C34 N3 -0.4(13) . . . . ? C27 C26 C34 N3 178.7(8) . . . . ? C25 C26 C34 C33 177.2(8) . . . . ? C27 C26 C34 C33 -3.7(12) . . . . ? N4 C33 C34 N3 0.3(11) . . . . ? C29 C33 C34 N3 -179.5(7) . . . . ? N4 C33 C34 C26 -177.4(8) . . . . ? C29 C33 C34 C26 2.8(12) . . . . ? N4 C32 C35 O1 -82.7(11) . . . . ? C31 C32 C35 O1 92.0(10) . . . . ? N4 C32 C35 C36 103.3(11) . . . . ? C31 C32 C35 C36 -82.0(11) . . . . ? O1 C35 C36 C37 -173.9(11) . . . . ? C32 C35 C36 C37 -0.7(17) . . . . ? C35 C36 C37 O2 1(2) . . . . ? C35 C36 C37 C38' -174.8(11) . . . . ? C35 C36 C37 C38 -176.0(11) . . . . ? O2 C37 C38 F2 133.7(15) . . . . ? C36 C37 C38 F2 -48.6(19) . . . . ? C38' C37 C38 F2 -67(14) . . . . ? O2 C37 C38 F1 -57(2) . . . . ? C36 C37 C38 F1 120.4(17) . . . . ? C38' C37 C38 F1 102(14) . . . . ? O2 C37 C38 C39 38.6(17) . . . . ? C36 C37 C38 C39 -143.6(14) . . . . ? C38' C37 C38 C39 -162(14) . . . . ? F2 C38 C39 F3 -52.3(12) . . . . ? F1 C38 C39 F3 167.3(14) . . . . ? C37 C38 C39 F3 55.0(14) . . . . ? F2 C38 C39 F4 61.1(16) . . . . ? F1 C38 C39 F4 -79.3(17) . . . . ? C37 C38 C39 F4 168.4(13) . . . . ? F2 C38 C39 F5 -169.1(14) . . . . ? F1 C38 C39 F5 50.5(15) . . . . ? C37 C38 C39 F5 -61.8(17) . . . . ? O2 C37 C38' F2' -178.1(15) . . . . ? C36 C37 C38' F2' -1(2) . . . . ? C38 C37 C38' F2' 161(15) . . . . ? O2 C37 C38' F1' -102.1(14) . . . . ? C36 C37 C38' F1' 74.6(16) . . . . ? C38 C37 C38' F1' -123(14) . . . . ? O2 C37 C38' C39' 18.1(19) . . . . ? C36 C37 C38' C39' -165.2(12) . . . . ? C38 C37 C38' C39' -3(13) . . . . ? F2' C38' C39' F5' 125.1(16) . . . . ? F1' C38' C39' F5' 54.3(15) . . . . ? C37 C38' C39' F5' -71.2(16) . . . . ? F2' C38' C39' F3' -113.3(17) . . . . ? F1' C38' C39' F3' 175.9(15) . . . . ? C37 C38' C39' F3' 50.4(16) . . . . ? F2' C38' C39' F4' 9.0(17) . . . . ? F1' C38' C39' F4' -61.8(15) . . . . ? C37 C38' C39' F4' 172.7(14) . . . . ? C39' C38' F1' F2' 116.1(13) . . . . ? C37 C38' F1' F2' -112.2(13) . . . . ? C39' C38' F2' F1' -91.1(12) . . . . ? C37 C38' F2' F1' 104.5(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.405 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.136 # Attachment 'Ir2-Nd.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 648231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis(Iridium bis(2-phenylpyridinato-N,C2) (4,4,5,5,5- pentafluoro-1-(1,10-phenanthrolin-2-yl)pentane-1,3-dionate)) Neodymium nitrate ; _chemical_melting_point ? _chemical_formula_moiety 'C87 H65.50 F10 Ir2 N13.50 Nd O14' _chemical_formula_sum 'C87 H65.50 F10 Ir2 N13.50 Nd O14' _chemical_formula_weight 2242.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4979(18) _cell_length_b 17.028(2) _cell_length_c 34.616(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.743(7) _cell_angle_gamma 90.00 _cell_volume 9134.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16328 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4392 _exptl_absorpt_coefficient_mu 3.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5085 _exptl_absorpt_correction_T_max 0.6001 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65277 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15938 _reflns_number_gt 13186 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0838P)^2^+70.7919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15938 _refine_ls_number_parameters 1231 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.1974 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.009 _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 0.73870(3) 0.40183(3) 0.568752(11) 0.03718(15) Uani 1 1 d . . . Ir2 Ir 0.59416(3) -0.04955(2) 0.316201(12) 0.03943(15) Uani 1 1 d . . . Nd1 Nd 0.72174(5) 0.23952(4) 0.407986(16) 0.04224(19) Uani 1 1 d . . . N1 N 0.8281(8) 0.4981(6) 0.5782(3) 0.050(3) Uani 1 1 d . . . N2 N 0.8548(7) 0.3643(6) 0.5377(2) 0.046(2) Uani 1 1 d . . . N3 N 0.7803(7) 0.3317(6) 0.6140(2) 0.043(2) Uani 1 1 d . . . N4 N 0.6789(7) 0.4686(5) 0.5269(2) 0.040(2) Uani 1 1 d . . . N5 N 0.5749(7) -0.1650(5) 0.3379(3) 0.047(3) Uani 1 1 d . . . N6 N 0.7020(7) -0.0622(6) 0.3575(2) 0.044(2) Uani 1 1 d . . . N7 N 0.5050(8) -0.0065(5) 0.3543(2) 0.046(3) Uani 1 1 d . . . N8 N 0.6760(6) -0.0798(5) 0.2722(2) 0.038(2) Uani 1 1 d . . . N9 N 0.6991(7) 0.4016(6) 0.3766(3) 0.051(3) Uani 1 1 d . . . N10 N 0.9107(9) 0.2043(7) 0.4176(3) 0.055(3) Uani 1 1 d . . . N11 N 0.5327(8) 0.2580(6) 0.4210(3) 0.052(3) Uani 1 1 d . . . O1 O 0.7640(6) 0.2880(5) 0.4717(2) 0.048(2) Uani 1 1 d . . . O2 O 0.6841(6) 0.1444(5) 0.4584(2) 0.052(2) Uani 1 1 d . A . O3 O 0.7063(6) 0.1109(5) 0.3771(2) 0.045(2) Uani 1 1 d . . . O4 O 0.7917(6) 0.2392(5) 0.34400(19) 0.045(2) Uani 1 1 d . . . O5 O 0.6563(6) 0.3451(5) 0.3631(2) 0.047(2) Uani 1 1 d . . . O6 O 0.7517(6) 0.3869(5) 0.4042(2) 0.049(2) Uani 1 1 d . . . O7 O 0.6935(6) 0.4697(5) 0.3649(2) 0.055(2) Uani 1 1 d . . . O8 O 0.8851(6) 0.2744(5) 0.4119(2) 0.053(2) Uani 1 1 d . . . O9 O 0.8545(6) 0.1514(5) 0.4223(2) 0.054(2) Uani 1 1 d . . . O10 O 0.9888(8) 0.1892(6) 0.4194(3) 0.072(3) Uani 1 1 d . . . O11 O 0.5871(6) 0.3006(5) 0.4388(2) 0.048(2) Uani 1 1 d . . . O12 O 0.5639(6) 0.2118(5) 0.3958(2) 0.048(2) Uani 1 1 d . . . O13 O 0.4550(7) 0.2605(6) 0.4273(3) 0.064(3) Uani 1 1 d . . . F1 F 0.5944(11) 0.0539(13) 0.5045(10) 0.126(13) Uani 0.56(2) 1 d PDU A 1 F2 F 0.7012(13) 0.0460(8) 0.5454(3) 0.045(4) Uani 0.56(2) 1 d PDU A 1 F3 F 0.689(3) -0.0837(9) 0.5062(10) 0.19(3) Uani 0.56(2) 1 d PD A 1 F4 F 0.8004(12) -0.0218(15) 0.4877(8) 0.090(7) Uani 0.56(2) 1 d PDU A 1 F5 F 0.678(2) -0.0193(14) 0.4500(5) 0.081(10) Uani 0.56(2) 1 d PD A 1 C16 C 0.6816(11) 0.0531(6) 0.5073(4) 0.072(12) Uani 0.56(2) 1 d PD A 1 C17 C 0.7134(12) -0.0192(8) 0.4861(4) 0.076(11) Uani 0.56(2) 1 d PD A 1 F1' F 0.7977(10) 0.0059(10) 0.4905(8) 0.060(7) Uani 0.44(2) 1 d PDU A 2 F2' F 0.7353(16) 0.0368(11) 0.5429(4) 0.050(6) Uani 0.44(2) 1 d PDU A 2 F3' F 0.654(2) -0.0779(11) 0.5041(10) 0.079(10) Uani 0.44(2) 1 d PD A 2 F4' F 0.5761(10) 0.0374(10) 0.4996(5) 0.036(5) Uani 0.44(2) 1 d PDU A 2 F5' F 0.655(3) -0.018(2) 0.4519(5) 0.104(18) Uani 0.44(2) 1 d PD A 2 C16' C 0.7270(9) 0.0426(7) 0.5040(4) 0.047(10) Uani 0.44(2) 1 d PD A 2 C17' C 0.6479(9) -0.0033(8) 0.4905(5) 0.049(10) Uani 0.44(2) 1 d PD A 2 F6 F 0.8589(6) 0.2792(5) 0.2768(2) 0.071(2) Uani 1 1 d . . . F7 F 0.8922(6) 0.1584(5) 0.2633(2) 0.068(2) Uani 1 1 d . . . F8 F 1.0303(6) 0.2456(7) 0.2770(3) 0.096(3) Uani 1 1 d . . . F9 F 0.9867(6) 0.2747(6) 0.3335(2) 0.084(3) Uani 1 1 d . . . F10 F 1.0131(6) 0.1551(7) 0.3195(3) 0.096(3) Uani 1 1 d . . . C1 C 0.8098(9) 0.5654(7) 0.5956(3) 0.051(3) Uani 1 1 d . . . H1 H 0.7526 0.5727 0.6045 0.061 Uiso 1 1 calc R . . C2 C 0.8680(10) 0.6251(8) 0.6016(4) 0.059(4) Uani 1 1 d . . . H2 H 0.8521 0.6723 0.6143 0.071 Uiso 1 1 calc R . . C3 C 0.9502(11) 0.6135(8) 0.5884(4) 0.061(4) Uani 1 1 d . . . H3 H 0.9928 0.6529 0.5923 0.073 Uiso 1 1 calc R . . C4 C 0.9724(9) 0.5418(9) 0.5685(3) 0.057(4) Uani 1 1 d . . . C5 C 1.0577(10) 0.5241(11) 0.5576(4) 0.070(4) Uani 1 1 d . . . H5 H 1.1030 0.5608 0.5621 0.083 Uiso 1 1 calc R . . C6 C 1.0742(10) 0.4535(11) 0.5404(5) 0.074(5) Uani 1 1 d . . . H6 H 1.1315 0.4424 0.5325 0.089 Uiso 1 1 calc R . . C7 C 1.0087(9) 0.3957(10) 0.5337(4) 0.063(4) Uani 1 1 d . . . C8 C 1.0224(10) 0.3208(11) 0.5166(4) 0.067(4) Uani 1 1 d . . . H8 H 1.0791 0.3041 0.5105 0.081 Uiso 1 1 calc R . . C9 C 0.9534(10) 0.2732(10) 0.5091(4) 0.066(4) Uani 1 1 d . . . H9 H 0.9615 0.2233 0.4974 0.079 Uiso 1 1 calc R . . C10 C 0.8702(8) 0.2989(8) 0.5188(3) 0.048(3) Uani 1 1 d . . . C11 C 0.9233(8) 0.4134(8) 0.5456(3) 0.047(3) Uani 1 1 d . . . C12 C 0.9069(9) 0.4856(7) 0.5646(3) 0.046(3) Uani 1 1 d . . . C13 C 0.7970(8) 0.2520(7) 0.4994(3) 0.045(3) Uani 1 1 d . . . C14 C 0.7780(9) 0.1767(7) 0.5114(3) 0.049(3) Uani 1 1 d . A . H14 H 0.8047 0.1575 0.5343 0.059 Uiso 1 1 calc R . . C15 C 0.7210(9) 0.1277(6) 0.4912(3) 0.060(4) Uani 1 1 d D . . C18 C 0.8454(8) 0.3532(8) 0.6387(3) 0.045(3) Uani 1 1 d . . . H18 H 0.8775 0.3998 0.6341 0.054 Uiso 1 1 calc R . . C19 C 0.8643(9) 0.3075(9) 0.6702(3) 0.054(3) Uani 1 1 d . . . H19 H 0.9080 0.3235 0.6879 0.065 Uiso 1 1 calc R . . C20 C 0.8207(12) 0.2388(9) 0.6763(4) 0.072(5) Uani 1 1 d . . . H20 H 0.8353 0.2063 0.6977 0.086 Uiso 1 1 calc R . . C21 C 0.7557(10) 0.2174(8) 0.6511(3) 0.058(4) Uani 1 1 d . . . H21 H 0.7246 0.1702 0.6553 0.069 Uiso 1 1 calc R . . C22 C 0.7345(10) 0.2656(7) 0.6188(3) 0.052(3) Uani 1 1 d . . . C23 C 0.6659(9) 0.2517(7) 0.5905(3) 0.046(3) Uani 1 1 d . . . C24 C 0.6588(8) 0.3087(7) 0.5618(3) 0.044(3) Uani 1 1 d . . . C25 C 0.5939(8) 0.2985(7) 0.5340(3) 0.045(3) Uani 1 1 d . . . H25 H 0.5846 0.3376 0.5148 0.055 Uiso 1 1 calc R . . C26 C 0.5433(9) 0.2324(8) 0.5340(4) 0.059(4) Uani 1 1 d . . . H26 H 0.5017 0.2252 0.5139 0.070 Uiso 1 1 calc R . . C27 C 0.5513(11) 0.1753(8) 0.5630(4) 0.066(4) Uani 1 1 d . . . H27 H 0.5139 0.1311 0.5635 0.079 Uiso 1 1 calc R . . C28 C 0.6142(10) 0.1850(7) 0.5903(3) 0.056(4) Uani 1 1 d . . . H28 H 0.6229 0.1458 0.6095 0.067 Uiso 1 1 calc R . . C29 C 0.6993(8) 0.4680(7) 0.4889(3) 0.040(3) Uani 1 1 d . . . H29 H 0.7434 0.4338 0.4803 0.048 Uiso 1 1 calc R . . C30 C 0.6575(8) 0.5162(7) 0.4626(3) 0.045(3) Uani 1 1 d . . . H30 H 0.6720 0.5149 0.4360 0.054 Uiso 1 1 calc R . . C31 C 0.5937(9) 0.5667(7) 0.4757(3) 0.044(3) Uani 1 1 d . . . H31 H 0.5650 0.6011 0.4582 0.053 Uiso 1 1 calc R . . C32 C 0.5723(9) 0.5664(6) 0.5140(3) 0.045(3) Uani 1 1 d . . . H32 H 0.5293 0.6014 0.5231 0.054 Uiso 1 1 calc R . . C33 C 0.6137(7) 0.5150(6) 0.5398(3) 0.035(2) Uani 1 1 d . . . C34 C 0.5942(8) 0.5048(6) 0.5806(3) 0.039(3) Uani 1 1 d . . . C35 C 0.6474(7) 0.4515(6) 0.6008(3) 0.032(2) Uani 1 1 d . . . C36 C 0.6317(9) 0.4433(7) 0.6407(3) 0.045(3) Uani 1 1 d . . . H36 H 0.6658 0.4072 0.6552 0.054 Uiso 1 1 calc R . . C37 C 0.5696(9) 0.4852(7) 0.6590(3) 0.047(3) Uani 1 1 d . . . H37 H 0.5615 0.4790 0.6860 0.057 Uiso 1 1 calc R . . C38 C 0.5197(9) 0.5354(7) 0.6388(3) 0.049(3) Uani 1 1 d . . . H38 H 0.4763 0.5639 0.6519 0.059 Uiso 1 1 calc R . . C39 C 0.5293(8) 0.5472(7) 0.5993(3) 0.041(3) Uani 1 1 d . . . H39 H 0.4932 0.5828 0.5855 0.049 Uiso 1 1 calc R . . C40 C 0.5112(10) -0.2142(7) 0.3288(5) 0.062(4) Uani 1 1 d . . . H40 H 0.4670 -0.1966 0.3116 0.075 Uiso 1 1 calc R . . C41 C 0.5063(11) -0.2916(9) 0.3434(5) 0.070(4) Uani 1 1 d . . . H41 H 0.4615 -0.3263 0.3355 0.084 Uiso 1 1 calc R . . C42 C 0.5680(12) -0.3143(9) 0.3693(4) 0.074(5) Uani 1 1 d . . . H42 H 0.5640 -0.3647 0.3808 0.088 Uiso 1 1 calc R . . C43 C 0.6353(11) -0.2667(8) 0.3791(4) 0.059(4) Uani 1 1 d . . . C44 C 0.7011(13) -0.2898(11) 0.4038(6) 0.092(6) Uani 1 1 d . . . H44 H 0.7027 -0.3419 0.4136 0.111 Uiso 1 1 calc R . . C45 C 0.7622(14) -0.2388(11) 0.4136(5) 0.091(6) Uani 1 1 d . . . H45 H 0.8049 -0.2549 0.4319 0.109 Uiso 1 1 calc R . . C46 C 0.7676(10) -0.1602(8) 0.3981(4) 0.063(4) Uani 1 1 d . . . C47 C 0.8370(12) -0.1074(10) 0.4054(5) 0.087(6) Uani 1 1 d . . . H47 H 0.8849 -0.1234 0.4209 0.105 Uiso 1 1 calc R . . C48 C 0.8344(12) -0.0337(9) 0.3901(5) 0.077(5) Uani 1 1 d . . . H48 H 0.8794 0.0028 0.3951 0.093 Uiso 1 1 calc R . . C49 C 0.7634(10) -0.0133(8) 0.3667(3) 0.053(3) Uani 1 1 d . . . C50 C 0.7027(9) -0.1368(7) 0.3731(3) 0.052(3) Uani 1 1 d . . . C51 C 0.6358(8) -0.1901(7) 0.3631(3) 0.043(3) Uani 1 1 d . . . C52 C 0.7583(8) 0.0742(7) 0.3571(3) 0.042(3) Uani 1 1 d . . . C53 C 0.8148(9) 0.1023(7) 0.3288(3) 0.049(3) Uani 1 1 d . . . H53 H 0.8461 0.0666 0.3133 0.059 Uiso 1 1 calc R . . C54 C 0.8247(8) 0.1833(8) 0.3238(3) 0.047(3) Uani 1 1 d . . . C55 C 0.8881(9) 0.2103(8) 0.2928(3) 0.053(3) Uani 1 1 d . . . C56 C 0.9806(11) 0.2211(10) 0.3058(5) 0.069(4) Uani 1 1 d . . . C57 C 0.5236(10) 0.0257(7) 0.3894(4) 0.057(4) Uani 1 1 d . . . H57 H 0.5818 0.0259 0.3984 0.069 Uiso 1 1 calc R . . C58 C 0.4617(11) 0.0579(6) 0.4123(4) 0.059(4) Uani 1 1 d . . . H58 H 0.4759 0.0790 0.4370 0.070 Uiso 1 1 calc R . . C59 C 0.3762(11) 0.0585(8) 0.3980(4) 0.064(4) Uani 1 1 d . . . H59 H 0.3320 0.0808 0.4133 0.077 Uiso 1 1 calc R . . C60 C 0.3561(11) 0.0287(9) 0.3636(3) 0.063(4) Uani 1 1 d . . . H60 H 0.2981 0.0305 0.3545 0.076 Uiso 1 1 calc R . . C61 C 0.4215(9) -0.0061(7) 0.3402(4) 0.053(3) Uani 1 1 d . . . C62 C 0.4068(9) -0.0384(6) 0.3025(3) 0.046(3) Uani 1 1 d . . . C63 C 0.4869(9) -0.0569(6) 0.2834(4) 0.047(3) Uani 1 1 d . . . C64 C 0.4797(9) -0.0857(7) 0.2456(3) 0.050(3) Uani 1 1 d . . . H64 H 0.5302 -0.0973 0.2314 0.060 Uiso 1 1 calc R . . C65 C 0.3969(9) -0.0977(7) 0.2284(4) 0.053(3) Uani 1 1 d . . . H65 H 0.3920 -0.1162 0.2025 0.063 Uiso 1 1 calc R . . C66 C 0.3240(8) -0.0824(7) 0.2494(4) 0.051(3) Uani 1 1 d . . . H66 H 0.2692 -0.0942 0.2382 0.061 Uiso 1 1 calc R . . C67 C 0.3274(9) -0.0518(7) 0.2847(4) 0.050(3) Uani 1 1 d . . . H67 H 0.2756 -0.0391 0.2977 0.060 Uiso 1 1 calc R . . C68 C 0.7084(8) -0.1532(7) 0.2676(3) 0.044(3) Uani 1 1 d . . . H68 H 0.6909 -0.1937 0.2847 0.052 Uiso 1 1 calc R . . C69 C 0.7659(9) -0.1708(7) 0.2389(3) 0.049(3) Uani 1 1 d . . . H69 H 0.7856 -0.2231 0.2354 0.059 Uiso 1 1 calc R . . C70 C 0.7948(9) -0.1105(8) 0.2148(3) 0.054(3) Uani 1 1 d . . . H70 H 0.8345 -0.1210 0.1948 0.065 Uiso 1 1 calc R . . C71 C 0.7648(9) -0.0370(8) 0.2207(4) 0.053(3) Uani 1 1 d . . . H71 H 0.7842 0.0049 0.2049 0.064 Uiso 1 1 calc R . . C72 C 0.7051(9) -0.0219(6) 0.2502(3) 0.044(3) Uani 1 1 d . . . C73 C 0.6699(8) 0.0559(6) 0.2599(3) 0.042(3) Uani 1 1 d . . . C74 C 0.6171(8) 0.0569(6) 0.2929(3) 0.039(3) Uani 1 1 d . . . C75 C 0.5830(8) 0.1289(7) 0.3050(3) 0.044(3) Uani 1 1 d . . . H75 H 0.5473 0.1315 0.3271 0.052 Uiso 1 1 calc R . . C76 C 0.6022(9) 0.1966(7) 0.2844(3) 0.051(3) Uani 1 1 d . . . H76 H 0.5778 0.2452 0.2922 0.061 Uiso 1 1 calc R . . C77 C 0.6568(9) 0.1950(7) 0.2523(3) 0.046(3) Uani 1 1 d . . . H77 H 0.6709 0.2425 0.2394 0.056 Uiso 1 1 calc R . . C78 C 0.6898(8) 0.1249(7) 0.2396(3) 0.043(3) Uani 1 1 d . . . H78 H 0.7255 0.1231 0.2175 0.052 Uiso 1 1 calc R . . C79 C 0.3153(14) 0.2433(11) 0.3465(5) 0.079(5) Uani 1 1 d . . . C80 C 0.4038(11) 0.2678(11) 0.3347(5) 0.079(5) Uani 1 1 d . . . H80A H 0.4055 0.3250 0.3317 0.119 Uiso 1 1 calc R . . H80B H 0.4180 0.2428 0.3101 0.119 Uiso 1 1 calc R . . H80C H 0.4458 0.2517 0.3546 0.119 Uiso 1 1 calc R . . C81 C 0.0282(11) 0.5219(10) 0.6710(4) 0.067(4) Uani 1 1 d . . . C82 C 0.1116(12) 0.5584(13) 0.6638(7) 0.111(7) Uani 1 1 d . . . H82A H 0.1069 0.5926 0.6411 0.167 Uiso 1 1 calc R . . H82B H 0.1547 0.5176 0.6592 0.167 Uiso 1 1 calc R . . H82C H 0.1291 0.5897 0.6864 0.167 Uiso 1 1 calc R . . C83 C 0.3771(16) 0.3658(11) 0.7401(5) 0.104(7) Uani 1 1 d . . . H83A H 0.3595 0.3708 0.7671 0.156 Uiso 1 1 calc R . . H83B H 0.4266 0.4001 0.7355 0.156 Uiso 1 1 calc R . . H83C H 0.3932 0.3112 0.7349 0.156 Uiso 1 1 calc R . . C84 C 0.3077(17) 0.3878(9) 0.7155(6) 0.109(8) Uani 1 1 d . . . H84A H 0.2754 0.4306 0.7282 0.131 Uiso 1 1 calc R . . H84B H 0.3318 0.4093 0.6914 0.131 Uiso 1 1 calc R . . C85 C 0.179(2) 0.3474(17) 0.6822(8) 0.171(14) Uani 1 1 d . . . H85A H 0.2004 0.3659 0.6569 0.205 Uiso 1 1 calc R . . H85B H 0.1467 0.3908 0.6942 0.205 Uiso 1 1 calc R . . C86 C 0.1171(16) 0.2743(18) 0.6757(7) 0.140(11) Uani 1 1 d . . . H86A H 0.1493 0.2311 0.6639 0.210 Uiso 1 1 calc R . . H86B H 0.0692 0.2896 0.6585 0.210 Uiso 1 1 calc R . . H86C H 0.0942 0.2572 0.7006 0.210 Uiso 1 1 calc R . . N12 N 0.2474(13) 0.2253(12) 0.3555(6) 0.117(7) Uani 1 1 d . . . N13 N -0.0353(10) 0.4948(9) 0.6757(4) 0.077(4) Uani 1 1 d . . . O14 O 0.2502(9) 0.3285(7) 0.7059(3) 0.092(4) Uani 1 1 d . . . C87 C 0.7540(19) 0.7135(16) 0.5221(7) 0.065(8) Uani 0.50 1 d PDU . . N14 N 0.7731(15) 0.6608(14) 0.5052(7) 0.068(6) Uani 0.50 1 d PDU . . C88 C 0.744(3) 0.776(2) 0.5520(12) 0.137(18) Uani 0.50 1 d PDU . . H88A H 0.6835 0.7807 0.5591 0.206 Uiso 0.50 1 calc PR . . H88B H 0.7641 0.8266 0.5415 0.206 Uiso 0.50 1 calc PR . . H88C H 0.7791 0.7629 0.5749 0.206 Uiso 0.50 1 calc PR . . 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 0.0532(3) 0.0379(3) 0.0204(2) 0.00157(16) -0.00094(18) -0.0092(2) Ir2 0.0606(3) 0.0304(2) 0.0276(2) -0.00155(16) 0.0117(2) -0.0072(2) Nd1 0.0643(5) 0.0382(3) 0.0243(3) 0.0001(2) -0.0007(3) -0.0129(3) N1 0.069(8) 0.045(6) 0.035(5) 0.008(4) -0.007(5) -0.015(5) N2 0.067(7) 0.052(6) 0.019(4) -0.001(4) -0.006(4) -0.006(5) N3 0.064(7) 0.043(6) 0.023(4) -0.003(4) 0.004(4) -0.003(5) N4 0.057(6) 0.041(5) 0.022(4) 0.009(4) -0.009(4) -0.014(5) N5 0.063(7) 0.028(5) 0.051(6) 0.001(4) 0.013(5) -0.009(5) N6 0.067(7) 0.042(5) 0.022(4) 0.000(4) 0.006(4) -0.006(5) N7 0.088(9) 0.024(5) 0.027(5) -0.005(4) 0.011(5) -0.014(5) N8 0.061(6) 0.025(5) 0.028(4) -0.010(3) 0.010(4) -0.017(4) N9 0.072(8) 0.054(7) 0.026(5) 0.010(4) 0.003(5) -0.012(6) N10 0.068(9) 0.068(8) 0.028(5) -0.010(5) 0.002(5) -0.005(7) N11 0.073(9) 0.045(6) 0.039(6) 0.003(5) 0.003(6) 0.015(6) O1 0.084(6) 0.040(4) 0.020(4) -0.004(3) -0.004(4) -0.014(4) O2 0.083(7) 0.044(5) 0.030(4) 0.002(3) 0.009(4) -0.014(4) O3 0.069(6) 0.043(4) 0.023(4) -0.001(3) 0.000(4) -0.008(4) O4 0.068(6) 0.051(5) 0.018(3) -0.004(3) 0.009(4) -0.016(4) O5 0.061(6) 0.056(5) 0.025(4) 0.005(3) -0.008(4) -0.016(4) O6 0.070(6) 0.049(5) 0.028(4) 0.008(3) -0.011(4) -0.015(4) O7 0.078(7) 0.042(5) 0.044(5) 0.013(4) -0.002(4) -0.008(4) O8 0.066(6) 0.048(5) 0.044(5) -0.001(4) -0.002(4) -0.009(5) O9 0.071(6) 0.047(5) 0.044(5) 0.004(4) -0.010(4) -0.014(5) O10 0.081(8) 0.073(7) 0.062(6) -0.007(5) 0.003(5) 0.003(6) O11 0.067(6) 0.049(5) 0.027(4) -0.002(3) -0.002(4) -0.013(4) O12 0.059(6) 0.042(5) 0.044(5) -0.008(4) 0.005(4) -0.006(4) O13 0.067(7) 0.069(6) 0.057(6) -0.011(5) 0.018(5) -0.001(5) F1 0.130(15) 0.124(15) 0.125(15) 0.000(9) 0.010(9) -0.021(9) F2 0.053(8) 0.049(7) 0.033(6) 0.005(5) 0.002(5) -0.003(6) F3 0.42(7) 0.063(18) 0.09(2) 0.012(15) -0.08(3) -0.09(3) F4 0.100(10) 0.082(11) 0.089(10) 0.001(9) -0.002(8) -0.002(8) F5 0.16(2) 0.038(12) 0.043(14) -0.017(10) -0.005(12) -0.009(13) C16 0.12(3) 0.07(2) 0.022(12) 0.015(12) 0.019(15) 0.03(2) C17 0.14(3) 0.065(19) 0.021(12) 0.026(12) -0.016(15) -0.03(2) F1' 0.066(10) 0.043(9) 0.072(10) 0.002(8) -0.005(7) 0.004(7) F2' 0.053(10) 0.049(9) 0.048(9) -0.006(6) 0.004(7) -0.006(7) F3' 0.117(19) 0.069(19) 0.050(16) 0.032(13) -0.023(13) -0.036(13) F4' 0.040(8) 0.028(7) 0.041(7) 0.008(6) 0.015(6) -0.012(6) F5' 0.15(3) 0.11(3) 0.05(2) 0.054(17) -0.031(16) -0.09(2) C16' 0.09(3) 0.036(16) 0.018(13) -0.004(11) 0.007(14) 0.024(17) C17' 0.10(3) 0.018(13) 0.031(15) -0.005(11) 0.035(16) -0.009(15) F6 0.091(6) 0.078(6) 0.044(4) 0.013(4) 0.016(4) -0.022(5) F7 0.085(6) 0.085(6) 0.035(4) -0.007(4) 0.016(4) -0.018(5) F8 0.084(7) 0.136(9) 0.070(6) 0.002(6) 0.025(5) -0.034(6) F9 0.087(7) 0.113(8) 0.051(5) -0.017(5) -0.002(4) -0.033(6) F10 0.079(7) 0.103(8) 0.106(8) 0.014(6) -0.002(6) -0.011(6) C1 0.063(9) 0.050(7) 0.039(6) 0.000(6) 0.001(6) -0.012(6) C2 0.084(11) 0.053(8) 0.040(7) 0.001(6) -0.018(7) -0.023(8) C3 0.077(11) 0.054(8) 0.052(8) -0.005(6) -0.004(7) -0.023(8) C4 0.056(9) 0.085(10) 0.032(6) 0.013(6) -0.007(6) -0.010(8) C5 0.072(11) 0.106(13) 0.030(7) -0.003(7) -0.002(6) -0.028(9) C6 0.043(9) 0.116(14) 0.063(9) -0.009(9) -0.005(7) -0.009(9) C7 0.054(9) 0.102(12) 0.035(7) -0.007(7) -0.001(6) -0.006(8) C8 0.048(9) 0.114(13) 0.040(7) 0.002(8) -0.006(6) 0.014(9) C9 0.074(11) 0.091(11) 0.032(7) -0.015(7) 0.000(6) 0.017(9) C10 0.049(8) 0.055(8) 0.041(6) 0.004(6) -0.004(6) 0.007(6) C11 0.046(8) 0.066(8) 0.029(6) 0.008(5) -0.006(5) -0.008(6) C12 0.065(9) 0.041(7) 0.032(6) -0.006(5) -0.003(6) -0.015(6) C13 0.061(8) 0.052(7) 0.021(5) -0.003(5) -0.005(5) 0.002(6) C14 0.071(9) 0.036(6) 0.040(6) -0.004(5) -0.002(6) 0.001(6) C15 0.097(11) 0.055(8) 0.027(6) 0.005(5) 0.007(6) -0.003(8) C18 0.052(8) 0.062(8) 0.023(5) -0.004(5) -0.001(5) 0.009(6) C19 0.068(9) 0.072(9) 0.022(5) -0.002(6) -0.004(5) 0.017(7) C20 0.118(14) 0.073(10) 0.025(6) 0.009(6) 0.003(7) 0.033(10) C21 0.093(11) 0.048(7) 0.032(6) 0.008(5) -0.006(7) -0.003(7) C22 0.089(10) 0.044(7) 0.023(5) -0.006(5) 0.004(6) -0.001(7) C23 0.073(9) 0.035(6) 0.032(6) 0.001(5) 0.010(6) -0.011(6) C24 0.064(8) 0.040(6) 0.029(6) 0.001(5) 0.003(5) -0.013(6) C25 0.073(9) 0.045(7) 0.018(5) -0.002(4) 0.008(5) -0.013(6) C26 0.060(9) 0.070(9) 0.046(7) -0.018(7) 0.000(6) -0.009(7) C27 0.099(12) 0.044(8) 0.054(8) -0.009(6) 0.021(8) -0.028(8) C28 0.100(11) 0.040(7) 0.028(6) 0.005(5) 0.013(6) -0.025(7) C29 0.055(8) 0.037(6) 0.028(5) -0.003(4) -0.003(5) -0.014(5) C30 0.066(8) 0.036(6) 0.032(6) 0.006(5) -0.003(5) -0.019(6) C31 0.068(9) 0.042(6) 0.022(5) 0.009(5) -0.006(5) -0.009(6) C32 0.066(9) 0.027(6) 0.043(7) 0.002(5) -0.005(6) 0.003(6) C33 0.044(7) 0.033(6) 0.027(5) 0.005(4) -0.003(5) -0.011(5) C34 0.053(7) 0.035(6) 0.029(5) 0.002(4) -0.010(5) -0.016(5) C35 0.047(7) 0.031(5) 0.019(5) -0.004(4) -0.002(4) -0.021(5) C36 0.064(8) 0.050(7) 0.021(5) 0.007(5) 0.000(5) -0.010(6) C37 0.074(9) 0.044(7) 0.023(5) -0.005(5) 0.000(6) -0.020(7) C38 0.065(9) 0.052(7) 0.030(6) -0.008(5) 0.010(6) -0.013(7) C39 0.042(7) 0.044(7) 0.037(6) 0.003(5) 0.004(5) -0.005(5) C40 0.063(9) 0.030(6) 0.094(11) 0.015(7) 0.018(8) -0.005(6) C41 0.075(11) 0.049(8) 0.085(11) 0.011(8) 0.011(9) -0.009(8) C42 0.119(14) 0.049(8) 0.053(8) 0.013(7) 0.031(9) -0.026(9) C43 0.091(11) 0.042(7) 0.043(7) 0.013(6) -0.002(7) -0.011(7) C44 0.115(16) 0.060(10) 0.102(14) 0.039(10) -0.017(12) -0.019(11) C45 0.135(17) 0.082(12) 0.055(9) 0.032(9) -0.005(10) 0.031(12) C46 0.084(11) 0.047(8) 0.057(8) 0.006(6) -0.021(8) -0.008(7) C47 0.086(12) 0.082(12) 0.093(13) 0.025(10) -0.051(10) 0.002(10) C48 0.101(13) 0.066(10) 0.063(9) -0.001(8) -0.028(9) -0.021(9) C49 0.086(10) 0.051(7) 0.022(5) -0.001(5) -0.010(6) -0.012(7) C50 0.077(10) 0.045(7) 0.034(6) 0.014(5) -0.011(6) -0.005(7) C51 0.059(8) 0.044(7) 0.026(5) 0.004(5) -0.001(5) -0.004(6) C52 0.058(8) 0.042(6) 0.027(5) -0.008(5) -0.004(5) -0.012(6) C53 0.073(9) 0.054(8) 0.021(5) 0.000(5) -0.006(5) -0.021(7) C54 0.048(7) 0.065(8) 0.029(6) 0.005(6) -0.001(5) -0.018(6) C55 0.068(9) 0.063(8) 0.028(6) 0.005(6) -0.009(6) -0.016(7) C56 0.073(11) 0.072(10) 0.063(9) 0.005(8) 0.019(8) -0.008(9) C57 0.081(10) 0.038(7) 0.055(8) -0.005(6) 0.030(7) -0.019(7) C58 0.106(13) 0.025(6) 0.045(7) -0.010(5) 0.040(8) -0.010(7) C59 0.081(12) 0.056(9) 0.056(9) 0.010(7) 0.024(8) -0.007(8) C60 0.092(11) 0.070(9) 0.027(6) 0.006(6) 0.011(6) -0.002(8) C61 0.064(9) 0.039(7) 0.057(8) 0.007(6) 0.021(7) 0.000(6) C62 0.075(9) 0.031(6) 0.032(6) 0.010(5) 0.004(6) 0.006(6) C63 0.059(8) 0.027(6) 0.054(7) 0.005(5) 0.012(6) -0.008(6) C64 0.073(9) 0.038(6) 0.039(6) 0.000(5) -0.001(6) -0.007(6) C65 0.067(9) 0.047(7) 0.045(7) -0.004(6) -0.007(6) -0.001(7) C66 0.040(7) 0.051(7) 0.061(8) 0.019(6) -0.009(6) -0.016(6) C67 0.054(8) 0.050(7) 0.046(7) 0.013(6) -0.010(6) -0.004(6) C68 0.062(8) 0.039(6) 0.029(6) 0.010(5) 0.001(5) -0.001(6) C69 0.065(9) 0.043(7) 0.038(6) -0.004(5) 0.000(6) -0.003(6) C70 0.072(9) 0.056(8) 0.034(6) -0.005(6) 0.010(6) 0.013(7) C71 0.058(9) 0.060(8) 0.041(7) 0.001(6) 0.018(6) 0.000(7) C72 0.074(9) 0.031(6) 0.028(5) -0.003(4) 0.002(5) -0.006(6) C73 0.065(8) 0.032(6) 0.028(5) -0.006(4) -0.001(5) 0.003(5) C74 0.056(8) 0.036(6) 0.026(5) 0.000(4) 0.009(5) -0.008(5) C75 0.052(8) 0.042(6) 0.036(6) 0.002(5) 0.017(5) -0.004(6) C76 0.073(9) 0.034(6) 0.046(7) 0.002(5) 0.016(6) 0.004(6) C77 0.067(9) 0.034(6) 0.038(6) 0.004(5) 0.006(6) -0.004(6) C78 0.048(7) 0.049(7) 0.032(6) 0.004(5) 0.008(5) -0.008(6) C79 0.100(15) 0.083(12) 0.054(9) 0.011(8) -0.003(9) 0.014(11) C80 0.089(13) 0.087(12) 0.062(10) 0.005(8) 0.015(9) 0.018(10) C81 0.066(11) 0.083(11) 0.054(9) 0.009(8) 0.004(7) -0.001(9) C82 0.063(12) 0.104(15) 0.17(2) 0.012(14) 0.005(13) -0.034(11) C83 0.18(2) 0.071(12) 0.064(11) 0.001(9) -0.016(12) 0.009(13) C84 0.20(2) 0.035(9) 0.098(15) -0.018(9) 0.008(15) 0.018(12) C85 0.26(4) 0.13(2) 0.13(2) -0.033(18) -0.06(2) 0.07(3) C86 0.117(19) 0.20(3) 0.098(17) -0.047(18) -0.018(14) 0.07(2) N12 0.112(15) 0.124(15) 0.115(15) 0.033(11) 0.044(12) 0.009(12) N13 0.071(9) 0.096(10) 0.063(8) 0.005(7) 0.012(7) -0.020(8) O14 0.139(11) 0.077(8) 0.061(7) 0.014(6) -0.028(7) 0.022(8) C87 0.068(11) 0.070(11) 0.057(10) 0.006(8) 0.010(8) -0.006(9) N14 0.061(10) 0.073(10) 0.069(10) 0.003(8) -0.005(8) -0.014(8) C88 0.14(2) 0.14(2) 0.14(2) 0.007(10) 0.003(10) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C35 1.996(11) . ? Ir1 C24 2.024(12) . ? Ir1 N4 2.054(9) . ? Ir1 N3 2.065(9) . ? Ir1 N1 2.168(10) . ? Ir1 N2 2.204(11) . ? Ir2 C63 2.004(14) . ? Ir2 C74 2.016(11) . ? Ir2 N7 2.058(10) . ? Ir2 N8 2.060(9) . ? Ir2 N5 2.127(9) . ? Ir2 N6 2.195(10) . ? Nd1 O1 2.436(7) . ? Nd1 O3 2.447(8) . ? Nd1 O2 2.458(8) . ? Nd1 O4 2.479(7) . ? Nd1 O12 2.522(9) . ? Nd1 O6 2.556(8) . ? Nd1 O11 2.575(9) . ? Nd1 O5 2.576(8) . ? Nd1 O9 2.589(9) . ? Nd1 O8 2.603(9) . ? Nd1 N9 2.986(10) . ? Nd1 N11 2.987(13) . ? N1 C1 1.327(16) . ? N1 C12 1.331(16) . ? N2 C10 1.314(16) . ? N2 C11 1.376(16) . ? N3 C22 1.343(16) . ? N3 C18 1.364(15) . ? N4 C29 1.356(14) . ? N4 C33 1.362(15) . ? N5 C40 1.331(17) . ? N5 C51 1.346(15) . ? N6 C49 1.302(16) . ? N6 C50 1.380(15) . ? N7 C57 1.361(16) . ? N7 C61 1.378(18) . ? N8 C72 1.328(14) . ? N8 C68 1.359(15) . ? N9 O7 1.231(13) . ? N9 O5 1.256(12) . ? N9 O6 1.272(13) . ? N10 O10 1.237(15) . ? N10 O9 1.265(14) . ? N10 O8 1.272(14) . ? N11 O13 1.227(14) . ? N11 O11 1.265(14) . ? N11 O12 1.277(13) . ? O1 C13 1.243(13) . ? O2 C15 1.294(14) . ? O3 C52 1.239(14) . ? O4 C54 1.289(15) . ? F1 C16 1.353(10) . ? F2 C16 1.354(9) . ? F3 C17 1.355(10) . ? F4 C17 1.350(10) . ? F5 C17 1.361(10) . ? C16 C17 1.519(10) . ? C16 C15 1.520(9) . ? F1' C16' 1.352(10) . ? F2' C16' 1.354(10) . ? F3' C17' 1.358(10) . ? F4' C17' 1.351(9) . ? F5' C17' 1.364(10) . ? C16' C15 1.518(9) . ? C16' C17' 1.523(10) . ? F6 C55 1.372(16) . ? F7 C55 1.353(15) . ? F8 C56 1.333(16) . ? F9 C56 1.327(18) . ? F10 C56 1.319(19) . ? C1 C2 1.373(18) . ? C1 H1 0.9500 . ? C2 C3 1.37(2) . ? C2 H2 0.9500 . ? C3 C4 1.44(2) . ? C3 H3 0.9500 . ? C4 C12 1.401(18) . ? C4 C5 1.41(2) . ? C5 C6 1.37(2) . ? C5 H5 0.9500 . ? C6 C7 1.43(2) . ? C6 H6 0.9500 . ? C7 C8 1.42(2) . ? C7 C11 1.424(19) . ? C8 C9 1.36(2) . ? C8 H8 0.9500 . ? C9 C10 1.406(19) . ? C9 H9 0.9500 . ? C10 C13 1.536(18) . ? C11 C12 1.418(18) . ? C13 C14 1.381(17) . ? C14 C15 1.396(17) . ? C14 H14 0.9500 . ? C18 C19 1.367(17) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 C21 1.37(2) . ? C20 H20 0.9500 . ? C21 C22 1.423(17) . ? C21 H21 0.9500 . ? C22 C23 1.455(18) . ? C23 C28 1.389(17) . ? C23 C24 1.392(16) . ? C24 C25 1.396(17) . ? C25 C26 1.371(18) . ? C25 H25 0.9500 . ? C26 C27 1.40(2) . ? C26 H26 0.9500 . ? C27 C28 1.36(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.382(16) . ? C29 H29 0.9500 . ? C30 C31 1.391(18) . ? C30 H30 0.9500 . ? C31 C32 1.371(16) . ? C31 H31 0.9500 . ? C32 C33 1.400(15) . ? C32 H32 0.9500 . ? C33 C34 1.457(14) . ? C34 C39 1.404(17) . ? C34 C35 1.406(16) . ? C35 C36 1.412(14) . ? C36 C37 1.364(18) . ? C36 H36 0.9500 . ? C37 C38 1.343(18) . ? C37 H37 0.9500 . ? C38 C39 1.390(16) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.414(19) . ? C40 H40 0.9500 . ? C41 C42 1.36(2) . ? C41 H41 0.9500 . ? C42 C43 1.36(2) . ? C42 H42 0.9500 . ? C43 C44 1.38(2) . ? C43 C51 1.417(17) . ? C44 C45 1.33(3) . ? C44 H44 0.9500 . ? C45 C46 1.44(2) . ? C45 H45 0.9500 . ? C46 C50 1.377(18) . ? C46 C47 1.42(2) . ? C47 C48 1.36(2) . ? C47 H47 0.9500 . ? C48 C49 1.40(2) . ? C48 H48 0.9500 . ? C49 C52 1.527(17) . ? C50 C51 1.417(17) . ? C52 C53 1.406(17) . ? C53 C54 1.399(18) . ? C53 H53 0.9500 . ? C54 C55 1.535(17) . ? C55 C56 1.51(2) . ? C57 C58 1.365(18) . ? C57 H57 0.9500 . ? C58 C59 1.41(2) . ? C58 H58 0.9500 . ? C59 C60 1.33(2) . ? C59 H59 0.9500 . ? C60 C61 1.434(19) . ? C60 H60 0.9500 . ? C61 C62 1.431(18) . ? C62 C67 1.389(18) . ? C62 C63 1.449(18) . ? C63 C64 1.403(17) . ? C64 C65 1.421(19) . ? C64 H64 0.9500 . ? C65 C66 1.377(19) . ? C65 H65 0.9500 . ? C66 C67 1.330(18) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.376(17) . ? C68 H68 0.9500 . ? C69 C70 1.398(17) . ? C69 H69 0.9500 . ? C70 C71 1.352(18) . ? C70 H70 0.9500 . ? C71 C72 1.409(16) . ? C71 H71 0.9500 . ? C72 C73 1.474(16) . ? C73 C78 1.407(16) . ? C73 C74 1.414(15) . ? C74 C75 1.402(16) . ? C75 C76 1.391(16) . ? C75 H75 0.9500 . ? C76 C77 1.404(16) . ? C76 H76 0.9500 . ? C77 C78 1.374(17) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 N12 1.14(2) . ? C79 C80 1.49(3) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 N13 1.101(18) . ? C81 C82 1.46(2) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.41(3) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 O14 1.39(2) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 O14 1.40(3) . ? C85 C86 1.59(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 N14 1.111(9) . ? C87 C88 1.499(9) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 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 C35 Ir1 C24 87.7(4) . . ? C35 Ir1 N4 80.8(4) . . ? C24 Ir1 N4 94.6(4) . . ? C35 Ir1 N3 92.3(4) . . ? C24 Ir1 N3 79.7(4) . . ? N4 Ir1 N3 171.3(4) . . ? C35 Ir1 N1 93.0(4) . . ? C24 Ir1 N1 177.1(4) . . ? N4 Ir1 N1 88.2(4) . . ? N3 Ir1 N1 97.5(4) . . ? C35 Ir1 N2 169.5(4) . . ? C24 Ir1 N2 102.5(4) . . ? N4 Ir1 N2 100.4(4) . . ? N3 Ir1 N2 87.3(4) . . ? N1 Ir1 N2 76.6(4) . . ? C63 Ir2 C74 88.8(5) . . ? C63 Ir2 N7 80.0(5) . . ? C74 Ir2 N7 93.4(4) . . ? C63 Ir2 N8 94.6(4) . . ? C74 Ir2 N8 79.4(4) . . ? N7 Ir2 N8 171.1(4) . . ? C63 Ir2 N5 91.4(4) . . ? C74 Ir2 N5 176.3(4) . . ? N7 Ir2 N5 90.2(4) . . ? N8 Ir2 N5 97.0(4) . . ? C63 Ir2 N6 168.9(4) . . ? C74 Ir2 N6 102.2(4) . . ? N7 Ir2 N6 97.4(4) . . ? N8 Ir2 N6 89.2(4) . . ? N5 Ir2 N6 77.8(4) . . ? O1 Nd1 O3 136.2(3) . . ? O1 Nd1 O2 69.1(3) . . ? O3 Nd1 O2 72.4(3) . . ? O1 Nd1 O4 133.9(3) . . ? O3 Nd1 O4 69.4(3) . . ? O2 Nd1 O4 138.1(3) . . ? O1 Nd1 O12 117.7(3) . . ? O3 Nd1 O12 70.7(3) . . ? O2 Nd1 O12 76.0(3) . . ? O4 Nd1 O12 106.5(3) . . ? O1 Nd1 O6 70.6(2) . . ? O3 Nd1 O6 150.8(2) . . ? O2 Nd1 O6 136.8(3) . . ? O4 Nd1 O6 82.8(3) . . ? O12 Nd1 O6 110.6(3) . . ? O1 Nd1 O11 72.4(3) . . ? O3 Nd1 O11 117.8(3) . . ? O2 Nd1 O11 76.8(3) . . ? O4 Nd1 O11 137.5(3) . . ? O12 Nd1 O11 49.9(3) . . ? O6 Nd1 O11 76.9(3) . . ? O1 Nd1 O5 114.1(3) . . ? O3 Nd1 O5 109.0(3) . . ? O2 Nd1 O5 142.5(3) . . ? O4 Nd1 O5 68.6(3) . . ? O12 Nd1 O5 69.9(3) . . ? O6 Nd1 O5 49.8(2) . . ? O11 Nd1 O5 69.7(3) . . ? O1 Nd1 O9 79.6(3) . . ? O3 Nd1 O9 68.8(3) . . ? O2 Nd1 O9 71.2(3) . . ? O4 Nd1 O9 79.3(3) . . ? O12 Nd1 O9 133.6(3) . . ? O6 Nd1 O9 115.8(3) . . ? O11 Nd1 O9 143.3(3) . . ? O5 Nd1 O9 145.6(3) . . ? O1 Nd1 O8 68.0(3) . . ? O3 Nd1 O8 108.4(3) . . ? O2 Nd1 O8 110.7(3) . . ? O4 Nd1 O8 67.0(3) . . ? O12 Nd1 O8 172.9(3) . . ? O6 Nd1 O8 66.5(3) . . ? O11 Nd1 O8 132.8(3) . . ? O5 Nd1 O8 104.3(3) . . ? O9 Nd1 O8 49.6(3) . . ? O1 Nd1 N9 92.6(3) . . ? O3 Nd1 N9 131.1(3) . . ? O2 Nd1 N9 147.2(3) . . ? O4 Nd1 N9 74.2(3) . . ? O12 Nd1 N9 90.2(3) . . ? O6 Nd1 N9 25.0(3) . . ? O11 Nd1 N9 71.7(3) . . ? O5 Nd1 N9 24.7(3) . . ? O9 Nd1 N9 134.0(3) . . ? O8 Nd1 N9 85.3(3) . . ? O1 Nd1 N11 94.6(3) . . ? O3 Nd1 N11 94.0(3) . . ? O2 Nd1 N11 73.7(3) . . ? O4 Nd1 N11 125.2(3) . . ? O12 Nd1 N11 25.0(3) . . ? O6 Nd1 N11 94.8(3) . . ? O11 Nd1 N11 24.9(3) . . ? O5 Nd1 N11 68.8(3) . . ? O9 Nd1 N11 144.2(3) . . ? O8 Nd1 N11 157.5(3) . . ? N9 Nd1 N11 81.2(3) . . ? C1 N1 C12 120.0(11) . . ? C1 N1 Ir1 125.5(10) . . ? C12 N1 Ir1 114.4(8) . . ? C10 N2 C11 118.1(11) . . ? C10 N2 Ir1 130.0(9) . . ? C11 N2 Ir1 111.0(8) . . ? C22 N3 C18 122.3(10) . . ? C22 N3 Ir1 114.7(8) . . ? C18 N3 Ir1 122.8(8) . . ? C29 N4 C33 120.4(9) . . ? C29 N4 Ir1 124.8(9) . . ? C33 N4 Ir1 114.8(7) . . ? C40 N5 C51 117.8(11) . . ? C40 N5 Ir2 127.2(9) . . ? C51 N5 Ir2 115.0(8) . . ? C49 N6 C50 119.4(11) . . ? C49 N6 Ir2 130.1(8) . . ? C50 N6 Ir2 110.3(8) . . ? C57 N7 C61 120.1(12) . . ? C57 N7 Ir2 125.5(10) . . ? C61 N7 Ir2 114.2(7) . . ? C72 N8 C68 119.1(10) . . ? C72 N8 Ir2 117.2(7) . . ? C68 N8 Ir2 123.3(7) . . ? O7 N9 O5 124.4(10) . . ? O7 N9 O6 118.3(10) . . ? O5 N9 O6 117.3(9) . . ? O7 N9 Nd1 176.5(9) . . ? O5 N9 Nd1 59.0(5) . . ? O6 N9 Nd1 58.2(5) . . ? O10 N10 O9 121.3(13) . . ? O10 N10 O8 120.4(12) . . ? O9 N10 O8 118.3(12) . . ? O10 N10 Nd1 176.6(8) . . ? O9 N10 Nd1 59.0(7) . . ? O8 N10 Nd1 59.6(7) . . ? O13 N11 O11 122.9(10) . . ? O13 N11 O12 121.6(12) . . ? O11 N11 O12 115.5(11) . . ? O13 N11 Nd1 175.7(9) . . ? O11 N11 Nd1 59.0(6) . . ? O12 N11 Nd1 56.7(6) . . ? C13 O1 Nd1 129.3(7) . . ? C15 O2 Nd1 131.4(8) . . ? C52 O3 Nd1 129.5(8) . . ? C54 O4 Nd1 131.8(7) . . ? N9 O5 Nd1 96.2(6) . . ? N9 O6 Nd1 96.7(6) . . ? N10 O8 Nd1 95.5(8) . . ? N10 O9 Nd1 96.3(8) . . ? N11 O11 Nd1 96.1(7) . . ? N11 O12 Nd1 98.3(7) . . ? F1 C16 F2 106(2) . . ? F1 C16 C17 107.7(11) . . ? F2 C16 C17 109.2(10) . . ? F1 C16 C15 111.8(11) . . ? F2 C16 C15 110.2(10) . . ? C17 C16 C15 111.4(11) . . ? F4 C17 F3 103(3) . . ? F4 C17 F5 116(2) . . ? F3 C17 F5 111(3) . . ? F4 C17 C16 109.7(11) . . ? F3 C17 C16 108.4(12) . . ? F5 C17 C16 108.3(10) . . ? F1' C16' F2' 104(2) . . ? F1' C16' C15 112.7(11) . . ? F2' C16' C15 111.5(10) . . ? F1' C16' C17' 108.0(10) . . ? F2' C16' C17' 109.5(10) . . ? C15 C16' C17' 110.7(11) . . ? F4' C17' F3' 117(2) . . ? F4' C17' F5' 113(2) . . ? F3' C17' F5' 99(2) . . ? F4' C17' C16' 109.1(11) . . ? F3' C17' C16' 108.7(11) . . ? F5' C17' C16' 108.7(12) . . ? N1 C1 C2 124.4(14) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 116.9(14) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? C2 C3 C4 120.5(13) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C12 C4 C5 120.5(14) . . ? C12 C4 C3 116.5(13) . . ? C5 C4 C3 122.5(14) . . ? C6 C5 C4 119.1(14) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.6(15) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C11 117.1(14) . . ? C8 C7 C6 125.0(14) . . ? C11 C7 C6 117.8(14) . . ? C9 C8 C7 119.4(14) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.3(14) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 123.7(13) . . ? N2 C10 C13 121.4(11) . . ? C9 C10 C13 114.1(12) . . ? N2 C11 C12 118.5(12) . . ? N2 C11 C7 122.0(12) . . ? C12 C11 C7 119.4(12) . . ? N1 C12 C4 121.6(12) . . ? N1 C12 C11 118.2(11) . . ? C4 C12 C11 120.2(13) . . ? O1 C13 C14 127.1(11) . . ? O1 C13 C10 112.0(10) . . ? C14 C13 C10 120.7(11) . . ? C13 C14 C15 122.7(11) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? O2 C15 C14 125.2(9) . . ? O2 C15 C16' 119.4(11) . . ? C14 C15 C16' 112.8(10) . . ? O2 C15 C16 109.3(10) . . ? C14 C15 C16 124.8(10) . . ? C16' C15 C16 28.1(9) . . ? N3 C18 C19 119.7(13) . . ? N3 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 120.6(13) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 119.3(12) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 120.4(13) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? N3 C22 C21 117.7(12) . . ? N3 C22 C23 115.9(10) . . ? C21 C22 C23 126.4(12) . . ? C28 C23 C24 121.7(12) . . ? C28 C23 C22 123.6(11) . . ? C24 C23 C22 114.6(11) . . ? C23 C24 C25 117.1(11) . . ? C23 C24 Ir1 114.8(9) . . ? C25 C24 Ir1 127.9(9) . . ? C26 C25 C24 120.6(11) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 121.6(13) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 118.0(12) . . ? C28 C27 H27 121.0 . . ? C26 C27 H27 121.0 . . ? C27 C28 C23 120.7(12) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? N4 C29 C30 121.5(12) . . ? N4 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C31 118.7(11) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 119.7(11) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.3(12) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? N4 C33 C32 119.3(10) . . ? N4 C33 C34 114.3(9) . . ? C32 C33 C34 126.4(11) . . ? C39 C34 C35 121.4(10) . . ? C39 C34 C33 123.1(10) . . ? C35 C34 C33 115.5(10) . . ? C34 C35 C36 116.3(11) . . ? C34 C35 Ir1 114.4(7) . . ? C36 C35 Ir1 129.3(9) . . ? C37 C36 C35 122.4(11) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C38 C37 C36 119.6(11) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 122.5(12) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C38 C39 C34 117.8(11) . . ? C38 C39 H39 121.1 . . ? C34 C39 H39 121.1 . . ? N5 C40 C41 123.0(15) . . ? N5 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C42 C41 C40 117.5(15) . . ? C42 C41 H41 121.3 . . ? C40 C41 H41 121.3 . . ? C41 C42 C43 121.8(13) . . ? C41 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C42 C43 C44 123.0(14) . . ? C42 C43 C51 117.2(13) . . ? C44 C43 C51 119.8(14) . . ? C45 C44 C43 119.5(15) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 123.7(16) . . ? C44 C45 H45 118.1 . . ? C46 C45 H45 118.1 . . ? C50 C46 C47 118.2(12) . . ? C50 C46 C45 117.2(14) . . ? C47 C46 C45 124.5(15) . . ? C48 C47 C46 119.6(14) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 118.2(15) . . ? C47 C48 H48 120.9 . . ? C49 C48 H48 120.9 . . ? N6 C49 C48 123.2(12) . . ? N6 C49 C52 122.4(12) . . ? C48 C49 C52 114.0(12) . . ? C46 C50 N6 121.0(12) . . ? C46 C50 C51 119.5(11) . . ? N6 C50 C51 119.5(11) . . ? N5 C51 C50 117.3(10) . . ? N5 C51 C43 122.6(12) . . ? C50 C51 C43 120.2(11) . . ? O3 C52 C53 129.2(12) . . ? O3 C52 C49 113.7(10) . . ? C53 C52 C49 116.9(11) . . ? C54 C53 C52 119.5(12) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? O4 C54 C53 128.0(11) . . ? O4 C54 C55 114.8(11) . . ? C53 C54 C55 117.0(12) . . ? F7 C55 F6 105.8(9) . . ? F7 C55 C56 104.5(12) . . ? F6 C55 C56 108.9(11) . . ? F7 C55 C54 111.6(10) . . ? F6 C55 C54 109.1(11) . . ? C56 C55 C54 116.3(10) . . ? F10 C56 F9 107.6(14) . . ? F10 C56 F8 108.4(14) . . ? F9 C56 F8 106.8(13) . . ? F10 C56 C55 111.1(13) . . ? F9 C56 C55 110.9(13) . . ? F8 C56 C55 111.8(13) . . ? N7 C57 C58 122.5(15) . . ? N7 C57 H57 118.8 . . ? C58 C57 H57 118.8 . . ? C57 C58 C59 117.7(14) . . ? C57 C58 H58 121.1 . . ? C59 C58 H58 121.1 . . ? C60 C59 C58 121.3(15) . . ? C60 C59 H59 119.3 . . ? C58 C59 H59 119.3 . . ? C59 C60 C61 120.4(16) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? N7 C61 C62 117.3(11) . . ? N7 C61 C60 118.0(13) . . ? C62 C61 C60 124.7(14) . . ? C67 C62 C61 126.6(13) . . ? C67 C62 C63 121.4(11) . . ? C61 C62 C63 111.9(12) . . ? C64 C63 C62 116.4(12) . . ? C64 C63 Ir2 127.3(10) . . ? C62 C63 Ir2 115.9(9) . . ? C63 C64 C65 120.2(13) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 119.6(12) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C67 C66 C65 122.5(12) . . ? C67 C66 H66 118.7 . . ? C65 C66 H66 118.7 . . ? C66 C67 C62 119.8(13) . . ? C66 C67 H67 120.1 . . ? C62 C67 H67 120.1 . . ? N8 C68 C69 121.9(10) . . ? N8 C68 H68 119.0 . . ? C69 C68 H68 119.0 . . ? C68 C69 C70 119.1(12) . . ? C68 C69 H69 120.4 . . ? C70 C69 H69 120.4 . . ? C71 C70 C69 118.4(12) . . ? C71 C70 H70 120.8 . . ? C69 C70 H70 120.8 . . ? C70 C71 C72 120.5(12) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? N8 C72 C71 120.8(11) . . ? N8 C72 C73 113.9(10) . . ? C71 C72 C73 125.3(11) . . ? C78 C73 C74 121.9(10) . . ? C78 C73 C72 123.5(11) . . ? C74 C73 C72 114.5(10) . . ? C75 C74 C73 118.4(10) . . ? C75 C74 Ir2 126.7(8) . . ? C73 C74 Ir2 114.8(8) . . ? C76 C75 C74 119.2(10) . . ? C76 C75 H75 120.4 . . ? C74 C75 H75 120.4 . . ? C75 C76 C77 121.7(11) . . ? C75 C76 H76 119.1 . . ? C77 C76 H76 119.1 . . ? C78 C77 C76 120.1(11) . . ? C78 C77 H77 119.9 . . ? C76 C77 H77 119.9 . . ? C77 C78 C73 118.6(10) . . ? C77 C78 H78 120.7 . . ? C73 C78 H78 120.7 . . ? N12 C79 C80 179(2) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N13 C81 C82 178.5(19) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O14 C84 C83 115.7(16) . . ? O14 C84 H84A 108.3 . . ? C83 C84 H84A 108.3 . . ? O14 C84 H84B 108.3 . . ? C83 C84 H84B 108.3 . . ? H84A C84 H84B 107.4 . . ? O14 C85 C86 112(2) . . ? O14 C85 H85A 109.2 . . ? C86 C85 H85A 109.2 . . ? O14 C85 H85B 109.2 . . ? C86 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C84 O14 C85 118.1(18) . . ? N14 C87 C88 166(3) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? 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 C35 Ir1 N1 C1 -7.6(10) . . . . ? C24 Ir1 N1 C1 -113(9) . . . . ? N4 Ir1 N1 C1 73.1(10) . . . . ? N3 Ir1 N1 C1 -100.4(10) . . . . ? N2 Ir1 N1 C1 174.2(10) . . . . ? C35 Ir1 N1 C12 172.7(8) . . . . ? C24 Ir1 N1 C12 68(9) . . . . ? N4 Ir1 N1 C12 -106.6(8) . . . . ? N3 Ir1 N1 C12 79.9(8) . . . . ? N2 Ir1 N1 C12 -5.5(8) . . . . ? C35 Ir1 N2 C10 167.9(18) . . . . ? C24 Ir1 N2 C10 0.6(11) . . . . ? N4 Ir1 N2 C10 -96.5(10) . . . . ? N3 Ir1 N2 C10 79.5(10) . . . . ? N1 Ir1 N2 C10 177.8(10) . . . . ? C35 Ir1 N2 C11 -1(2) . . . . ? C24 Ir1 N2 C11 -167.9(8) . . . . ? N4 Ir1 N2 C11 95.0(7) . . . . ? N3 Ir1 N2 C11 -89.0(8) . . . . ? N1 Ir1 N2 C11 9.3(7) . . . . ? C35 Ir1 N3 C22 83.0(9) . . . . ? C24 Ir1 N3 C22 -4.3(9) . . . . ? N4 Ir1 N3 C22 45(3) . . . . ? N1 Ir1 N3 C22 176.3(8) . . . . ? N2 Ir1 N3 C22 -107.6(9) . . . . ? C35 Ir1 N3 C18 -92.7(9) . . . . ? C24 Ir1 N3 C18 -180.0(10) . . . . ? N4 Ir1 N3 C18 -130(2) . . . . ? N1 Ir1 N3 C18 0.7(9) . . . . ? N2 Ir1 N3 C18 76.8(9) . . . . ? C35 Ir1 N4 C29 -175.8(9) . . . . ? C24 Ir1 N4 C29 -88.9(9) . . . . ? N3 Ir1 N4 C29 -138(2) . . . . ? N1 Ir1 N4 C29 90.8(9) . . . . ? N2 Ir1 N4 C29 14.8(9) . . . . ? C35 Ir1 N4 C33 3.3(7) . . . . ? C24 Ir1 N4 C33 90.3(8) . . . . ? N3 Ir1 N4 C33 42(3) . . . . ? N1 Ir1 N4 C33 -90.0(8) . . . . ? N2 Ir1 N4 C33 -166.0(7) . . . . ? C63 Ir2 N5 C40 0.7(11) . . . . ? C74 Ir2 N5 C40 -92(7) . . . . ? N7 Ir2 N5 C40 80.7(11) . . . . ? N8 Ir2 N5 C40 -94.1(11) . . . . ? N6 Ir2 N5 C40 178.3(12) . . . . ? C63 Ir2 N5 C51 179.4(9) . . . . ? C74 Ir2 N5 C51 87(7) . . . . ? N7 Ir2 N5 C51 -100.6(9) . . . . ? N8 Ir2 N5 C51 84.6(9) . . . . ? N6 Ir2 N5 C51 -3.0(8) . . . . ? C63 Ir2 N6 C49 -168(2) . . . . ? C74 Ir2 N6 C49 3.2(11) . . . . ? N7 Ir2 N6 C49 -91.9(11) . . . . ? N8 Ir2 N6 C49 82.1(11) . . . . ? N5 Ir2 N6 C49 179.4(11) . . . . ? C63 Ir2 N6 C50 16(3) . . . . ? C74 Ir2 N6 C50 -172.8(8) . . . . ? N7 Ir2 N6 C50 92.1(8) . . . . ? N8 Ir2 N6 C50 -93.8(8) . . . . ? N5 Ir2 N6 C50 3.5(8) . . . . ? C63 Ir2 N7 C57 -172.8(10) . . . . ? C74 Ir2 N7 C57 -84.6(10) . . . . ? N8 Ir2 N7 C57 -120(2) . . . . ? N5 Ir2 N7 C57 95.9(9) . . . . ? N6 Ir2 N7 C57 18.2(9) . . . . ? C63 Ir2 N7 C61 1.8(8) . . . . ? C74 Ir2 N7 C61 90.0(8) . . . . ? N8 Ir2 N7 C61 55(3) . . . . ? N5 Ir2 N7 C61 -89.6(8) . . . . ? N6 Ir2 N7 C61 -167.2(8) . . . . ? C63 Ir2 N8 C72 88.1(9) . . . . ? C74 Ir2 N8 C72 0.2(9) . . . . ? N7 Ir2 N8 C72 36(3) . . . . ? N5 Ir2 N8 C72 -180.0(9) . . . . ? N6 Ir2 N8 C72 -102.4(9) . . . . ? C63 Ir2 N8 C68 -99.5(9) . . . . ? C74 Ir2 N8 C68 172.6(10) . . . . ? N7 Ir2 N8 C68 -152(2) . . . . ? N5 Ir2 N8 C68 -7.5(10) . . . . ? N6 Ir2 N8 C68 70.0(9) . . . . ? O1 Nd1 N9 O7 35(14) . . . . ? O3 Nd1 N9 O7 -143(14) . . . . ? O2 Nd1 N9 O7 89(14) . . . . ? O4 Nd1 N9 O7 -100(14) . . . . ? O12 Nd1 N9 O7 153(14) . . . . ? O6 Nd1 N9 O7 7(14) . . . . ? O11 Nd1 N9 O7 106(14) . . . . ? O5 Nd1 N9 O7 -173(15) . . . . ? O9 Nd1 N9 O7 -43(14) . . . . ? O8 Nd1 N9 O7 -33(14) . . . . ? N11 Nd1 N9 O7 129(14) . . . . ? O1 Nd1 N9 O5 -151.7(7) . . . . ? O3 Nd1 N9 O5 30.2(8) . . . . ? O2 Nd1 N9 O5 -97.7(8) . . . . ? O4 Nd1 N9 O5 73.1(6) . . . . ? O12 Nd1 N9 O5 -34.0(7) . . . . ? O6 Nd1 N9 O5 -179.6(11) . . . . ? O11 Nd1 N9 O5 -81.2(7) . . . . ? O9 Nd1 N9 O5 130.2(6) . . . . ? O8 Nd1 N9 O5 140.6(7) . . . . ? N11 Nd1 N9 O5 -57.5(7) . . . . ? O1 Nd1 N9 O6 27.8(7) . . . . ? O3 Nd1 N9 O6 -150.3(6) . . . . ? O2 Nd1 N9 O6 81.8(9) . . . . ? O4 Nd1 N9 O6 -107.3(7) . . . . ? O12 Nd1 N9 O6 145.5(7) . . . . ? O11 Nd1 N9 O6 98.4(7) . . . . ? O5 Nd1 N9 O6 179.6(11) . . . . ? O9 Nd1 N9 O6 -50.2(8) . . . . ? O8 Nd1 N9 O6 -39.9(7) . . . . ? N11 Nd1 N9 O6 122.1(7) . . . . ? O1 Nd1 N10 O10 -163(17) . . . . ? O3 Nd1 N10 O10 57(17) . . . . ? O2 Nd1 N10 O10 129(17) . . . . ? O4 Nd1 N10 O10 -12(17) . . . . ? O12 Nd1 N10 O10 73(17) . . . . ? O6 Nd1 N10 O10 -94(17) . . . . ? O11 Nd1 N10 O10 -162(16) . . . . ? O5 Nd1 N10 O10 -55(17) . . . . ? O9 Nd1 N10 O10 96(17) . . . . ? O8 Nd1 N10 O10 -90(17) . . . . ? N9 Nd1 N10 O10 -76(17) . . . . ? N11 Nd1 N10 O10 153(16) . . . . ? O1 Nd1 N10 O9 101.0(6) . . . . ? O3 Nd1 N10 O9 -39.0(6) . . . . ? O2 Nd1 N10 O9 33.3(6) . . . . ? O4 Nd1 N10 O9 -108.0(6) . . . . ? O12 Nd1 N10 O9 -22.6(10) . . . . ? O6 Nd1 N10 O9 170.2(6) . . . . ? O11 Nd1 N10 O9 101.9(7) . . . . ? O5 Nd1 N10 O9 -150.8(6) . . . . ? O8 Nd1 N10 O9 174.0(10) . . . . ? N9 Nd1 N10 O9 -172.2(6) . . . . ? N11 Nd1 N10 O9 57.4(14) . . . . ? O1 Nd1 N10 O8 -73.1(6) . . . . ? O3 Nd1 N10 O8 147.0(6) . . . . ? O2 Nd1 N10 O8 -140.7(6) . . . . ? O4 Nd1 N10 O8 78.0(6) . . . . ? O12 Nd1 N10 O8 163.4(7) . . . . ? O6 Nd1 N10 O8 -3.8(6) . . . . ? O11 Nd1 N10 O8 -72.1(8) . . . . ? O5 Nd1 N10 O8 35.2(7) . . . . ? O9 Nd1 N10 O8 -174.0(10) . . . . ? N9 Nd1 N10 O8 13.8(6) . . . . ? N11 Nd1 N10 O8 -116.6(12) . . . . ? O1 Nd1 N11 O13 -90(11) . . . . ? O3 Nd1 N11 O13 47(11) . . . . ? O2 Nd1 N11 O13 -24(11) . . . . ? O4 Nd1 N11 O13 114(11) . . . . ? O12 Nd1 N11 O13 68(11) . . . . ? O6 Nd1 N11 O13 -161(11) . . . . ? O11 Nd1 N11 O13 -117(12) . . . . ? O5 Nd1 N11 O13 155(12) . . . . ? O9 Nd1 N11 O13 -12(12) . . . . ? O8 Nd1 N11 O13 -129(11) . . . . ? N9 Nd1 N11 O13 178(100) . . . . ? O1 Nd1 N11 O11 26.9(6) . . . . ? O3 Nd1 N11 O11 163.9(6) . . . . ? O2 Nd1 N11 O11 93.6(6) . . . . ? O4 Nd1 N11 O11 -128.5(6) . . . . ? O12 Nd1 N11 O11 -174.8(10) . . . . ? O6 Nd1 N11 O11 -43.9(6) . . . . ? O5 Nd1 N11 O11 -87.2(6) . . . . ? O9 Nd1 N11 O11 105.5(7) . . . . ? O8 Nd1 N11 O11 -11.3(11) . . . . ? N9 Nd1 N11 O11 -65.0(6) . . . . ? O1 Nd1 N11 O12 -158.3(6) . . . . ? O3 Nd1 N11 O12 -21.2(6) . . . . ? O2 Nd1 N11 O12 -91.6(7) . . . . ? O4 Nd1 N11 O12 46.4(7) . . . . ? O6 Nd1 N11 O12 130.9(6) . . . . ? O11 Nd1 N11 O12 174.8(10) . . . . ? O5 Nd1 N11 O12 87.6(7) . . . . ? O9 Nd1 N11 O12 -79.7(8) . . . . ? O8 Nd1 N11 O12 163.6(7) . . . . ? N9 Nd1 N11 O12 109.8(7) . . . . ? O3 Nd1 O1 C13 10.5(12) . . . . ? O2 Nd1 O1 C13 40.6(10) . . . . ? O4 Nd1 O1 C13 -97.0(11) . . . . ? O12 Nd1 O1 C13 101.0(11) . . . . ? O6 Nd1 O1 C13 -155.3(11) . . . . ? O11 Nd1 O1 C13 122.7(11) . . . . ? O5 Nd1 O1 C13 -179.9(10) . . . . ? O9 Nd1 O1 C13 -33.1(11) . . . . ? O8 Nd1 O1 C13 -83.6(11) . . . . ? N9 Nd1 O1 C13 -167.4(11) . . . . ? N11 Nd1 O1 C13 111.2(11) . . . . ? O1 Nd1 O2 C15 -32.3(10) . . . . ? O3 Nd1 O2 C15 126.4(11) . . . . ? O4 Nd1 O2 C15 101.1(10) . . . . ? O12 Nd1 O2 C15 -159.7(11) . . . . ? O6 Nd1 O2 C15 -54.5(12) . . . . ? O11 Nd1 O2 C15 -108.3(10) . . . . ? O5 Nd1 O2 C15 -135.1(10) . . . . ? O9 Nd1 O2 C15 53.5(10) . . . . ? O8 Nd1 O2 C15 22.8(11) . . . . ? N9 Nd1 O2 C15 -92.2(12) . . . . ? N11 Nd1 O2 C15 -133.9(11) . . . . ? O1 Nd1 O3 C52 -95.3(10) . . . . ? O2 Nd1 O3 C52 -124.7(10) . . . . ? O4 Nd1 O3 C52 37.5(9) . . . . ? O12 Nd1 O3 C52 154.4(10) . . . . ? O6 Nd1 O3 C52 56.5(12) . . . . ? O11 Nd1 O3 C52 171.3(9) . . . . ? O5 Nd1 O3 C52 94.8(9) . . . . ? O9 Nd1 O3 C52 -48.6(9) . . . . ? O8 Nd1 O3 C52 -18.2(10) . . . . ? N9 Nd1 O3 C52 81.9(10) . . . . ? N11 Nd1 O3 C52 163.7(9) . . . . ? O1 Nd1 O4 C54 108.9(10) . . . . ? O3 Nd1 O4 C54 -26.3(10) . . . . ? O2 Nd1 O4 C54 -0.5(12) . . . . ? O12 Nd1 O4 C54 -87.7(10) . . . . ? O6 Nd1 O4 C54 162.9(10) . . . . ? O11 Nd1 O4 C54 -135.6(10) . . . . ? O5 Nd1 O4 C54 -147.6(11) . . . . ? O9 Nd1 O4 C54 44.8(10) . . . . ? O8 Nd1 O4 C54 95.4(10) . . . . ? N9 Nd1 O4 C54 -173.1(11) . . . . ? N11 Nd1 O4 C54 -106.4(10) . . . . ? O7 N9 O5 Nd1 179.5(10) . . . . ? O6 N9 O5 Nd1 -0.4(11) . . . . ? O1 Nd1 O5 N9 31.2(7) . . . . ? O3 Nd1 O5 N9 -156.4(6) . . . . ? O2 Nd1 O5 N9 118.0(7) . . . . ? O4 Nd1 O5 N9 -98.6(7) . . . . ? O12 Nd1 O5 N9 143.4(7) . . . . ? O6 Nd1 O5 N9 0.2(6) . . . . ? O11 Nd1 O5 N9 90.0(7) . . . . ? O9 Nd1 O5 N9 -76.5(8) . . . . ? O8 Nd1 O5 N9 -40.8(7) . . . . ? N11 Nd1 O5 N9 116.7(7) . . . . ? O7 N9 O6 Nd1 -179.5(9) . . . . ? O5 N9 O6 Nd1 0.4(11) . . . . ? O1 Nd1 O6 N9 -150.4(7) . . . . ? O3 Nd1 O6 N9 49.9(10) . . . . ? O2 Nd1 O6 N9 -128.4(7) . . . . ? O4 Nd1 O6 N9 67.8(7) . . . . ? O12 Nd1 O6 N9 -37.2(7) . . . . ? O11 Nd1 O6 N9 -74.6(7) . . . . ? O5 Nd1 O6 N9 -0.2(6) . . . . ? O9 Nd1 O6 N9 142.1(6) . . . . ? O8 Nd1 O6 N9 135.9(7) . . . . ? N11 Nd1 O6 N9 -57.2(7) . . . . ? O10 N10 O8 Nd1 176.0(9) . . . . ? O9 N10 O8 Nd1 -5.8(10) . . . . ? O1 Nd1 O8 N10 98.3(6) . . . . ? O3 Nd1 O8 N10 -35.0(6) . . . . ? O2 Nd1 O8 N10 42.6(6) . . . . ? O4 Nd1 O8 N10 -92.1(6) . . . . ? O12 Nd1 O8 N10 -117(2) . . . . ? O6 Nd1 O8 N10 175.9(7) . . . . ? O11 Nd1 O8 N10 133.5(6) . . . . ? O5 Nd1 O8 N10 -151.0(6) . . . . ? O9 Nd1 O8 N10 3.3(5) . . . . ? N9 Nd1 O8 N10 -166.9(6) . . . . ? N11 Nd1 O8 N10 140.0(7) . . . . ? O10 N10 O9 Nd1 -176.0(9) . . . . ? O8 N10 O9 Nd1 5.9(10) . . . . ? O1 Nd1 O9 N10 -73.2(6) . . . . ? O3 Nd1 O9 N10 137.6(7) . . . . ? O2 Nd1 O9 N10 -144.5(7) . . . . ? O4 Nd1 O9 N10 65.6(6) . . . . ? O12 Nd1 O9 N10 168.3(5) . . . . ? O6 Nd1 O9 N10 -10.9(7) . . . . ? O11 Nd1 O9 N10 -113.9(7) . . . . ? O5 Nd1 O9 N10 44.7(8) . . . . ? O8 Nd1 O9 N10 -3.3(5) . . . . ? N9 Nd1 O9 N10 10.3(8) . . . . ? N11 Nd1 O9 N10 -156.6(6) . . . . ? O13 N11 O11 Nd1 175.4(10) . . . . ? O12 N11 O11 Nd1 -4.8(10) . . . . ? O1 Nd1 O11 N11 -151.8(7) . . . . ? O3 Nd1 O11 N11 -18.2(7) . . . . ? O2 Nd1 O11 N11 -79.8(6) . . . . ? O4 Nd1 O11 N11 71.2(7) . . . . ? O12 Nd1 O11 N11 2.8(6) . . . . ? O6 Nd1 O11 N11 134.8(6) . . . . ? O5 Nd1 O11 N11 83.2(6) . . . . ? O9 Nd1 O11 N11 -109.5(7) . . . . ? O8 Nd1 O11 N11 174.1(6) . . . . ? N9 Nd1 O11 N11 109.3(6) . . . . ? O13 N11 O12 Nd1 -175.3(10) . . . . ? O11 N11 O12 Nd1 4.9(10) . . . . ? O1 Nd1 O12 N11 24.6(7) . . . . ? O3 Nd1 O12 N11 157.5(7) . . . . ? O2 Nd1 O12 N11 81.6(6) . . . . ? O4 Nd1 O12 N11 -141.9(6) . . . . ? O6 Nd1 O12 N11 -53.6(7) . . . . ? O11 Nd1 O12 N11 -2.8(6) . . . . ? O5 Nd1 O12 N11 -82.8(6) . . . . ? O9 Nd1 O12 N11 127.3(6) . . . . ? O8 Nd1 O12 N11 -118(2) . . . . ? N9 Nd1 O12 N11 -68.4(7) . . . . ? F1 C16 C17 F4 179(2) . . . . ? F2 C16 C17 F4 -66(2) . . . . ? C15 C16 C17 F4 56.2(19) . . . . ? F1 C16 C17 F3 -69(3) . . . . ? F2 C16 C17 F3 47(3) . . . . ? C15 C16 C17 F3 168(2) . . . . ? F1 C16 C17 F5 52(2) . . . . ? F2 C16 C17 F5 167(2) . . . . ? C15 C16 C17 F5 -71(2) . . . . ? F1' C16' C17' F4' -172.4(17) . . . . ? F2' C16' C17' F4' 74.7(18) . . . . ? C15 C16' C17' F4' -48.6(16) . . . . ? F1' C16' C17' F3' 59(2) . . . . ? F2' C16' C17' F3' -54(2) . . . . ? C15 C16' C17' F3' -177(2) . . . . ? F1' C16' C17' F5' -48(3) . . . . ? F2' C16' C17' F5' -161(2) . . . . ? C15 C16' C17' F5' 75(2) . . . . ? C12 N1 C1 C2 -1.2(19) . . . . ? Ir1 N1 C1 C2 179.2(9) . . . . ? N1 C1 C2 C3 0.3(19) . . . . ? C1 C2 C3 C4 1.1(19) . . . . ? C2 C3 C4 C12 -1.5(19) . . . . ? C2 C3 C4 C5 -174.1(13) . . . . ? C12 C4 C5 C6 5(2) . . . . ? C3 C4 C5 C6 177.2(14) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C5 C6 C7 C8 -178.8(15) . . . . ? C5 C6 C7 C11 0(2) . . . . ? C11 C7 C8 C9 6.2(19) . . . . ? C6 C7 C8 C9 -175.0(14) . . . . ? C7 C8 C9 C10 -1(2) . . . . ? C11 N2 C10 C9 5.4(17) . . . . ? Ir1 N2 C10 C9 -162.4(10) . . . . ? C11 N2 C10 C13 -163.5(10) . . . . ? Ir1 N2 C10 C13 28.7(16) . . . . ? C8 C9 C10 N2 -5(2) . . . . ? C8 C9 C10 C13 164.1(12) . . . . ? C10 N2 C11 C12 177.5(10) . . . . ? Ir1 N2 C11 C12 -12.4(12) . . . . ? C10 N2 C11 C7 0.7(16) . . . . ? Ir1 N2 C11 C7 170.7(9) . . . . ? C8 C7 C11 N2 -6.4(18) . . . . ? C6 C7 C11 N2 174.7(12) . . . . ? C8 C7 C11 C12 176.8(12) . . . . ? C6 C7 C11 C12 -2.1(18) . . . . ? C1 N1 C12 C4 0.7(17) . . . . ? Ir1 N1 C12 C4 -179.6(9) . . . . ? C1 N1 C12 C11 -179.0(11) . . . . ? Ir1 N1 C12 C11 0.7(14) . . . . ? C5 C4 C12 N1 173.3(11) . . . . ? C3 C4 C12 N1 0.6(17) . . . . ? C5 C4 C12 C11 -7.0(18) . . . . ? C3 C4 C12 C11 -179.8(11) . . . . ? N2 C11 C12 N1 8.3(16) . . . . ? C7 C11 C12 N1 -174.8(11) . . . . ? N2 C11 C12 C4 -171.3(10) . . . . ? C7 C11 C12 C4 5.6(17) . . . . ? Nd1 O1 C13 C14 -38.8(19) . . . . ? Nd1 O1 C13 C10 136.9(8) . . . . ? N2 C10 C13 O1 67.2(15) . . . . ? C9 C10 C13 O1 -102.7(13) . . . . ? N2 C10 C13 C14 -116.7(14) . . . . ? C9 C10 C13 C14 73.4(16) . . . . ? O1 C13 C14 C15 5(2) . . . . ? C10 C13 C14 C15 -170.4(12) . . . . ? Nd1 O2 C15 C14 20.8(19) . . . . ? Nd1 O2 C15 C16' -139.7(9) . . . . ? Nd1 O2 C15 C16 -168.6(8) . . . . ? C13 C14 C15 O2 4(2) . . . . ? C13 C14 C15 C16' 165.9(12) . . . . ? C13 C14 C15 C16 -164.9(13) . . . . ? F1' C16' C15 O2 87.0(17) . . . . ? F2' C16' C15 O2 -156.2(16) . . . . ? C17' C16' C15 O2 -34.0(15) . . . . ? F1' C16' C15 C14 -75.8(17) . . . . ? F2' C16' C15 C14 41.0(16) . . . . ? C17' C16' C15 C14 163.1(11) . . . . ? F1' C16' C15 C16 162(2) . . . . ? F2' C16' C15 C16 -80.8(19) . . . . ? C17' C16' C15 C16 41.3(16) . . . . ? F1 C16 C15 O2 -45.2(18) . . . . ? F2 C16 C15 O2 -163.4(14) . . . . ? C17 C16 C15 O2 75.3(12) . . . . ? F1 C16 C15 C14 125.4(18) . . . . ? F2 C16 C15 C14 7.3(19) . . . . ? C17 C16 C15 C14 -114.1(14) . . . . ? F1 C16 C15 C16' -162(2) . . . . ? F2 C16 C15 C16' 80(2) . . . . ? C17 C16 C15 C16' -41.5(16) . . . . ? C22 N3 C18 C19 -1.5(17) . . . . ? Ir1 N3 C18 C19 173.8(9) . . . . ? N3 C18 C19 C20 2.5(19) . . . . ? C18 C19 C20 C21 -2(2) . . . . ? C19 C20 C21 C22 1(2) . . . . ? C18 N3 C22 C21 0.2(18) . . . . ? Ir1 N3 C22 C21 -175.5(10) . . . . ? C18 N3 C22 C23 178.6(11) . . . . ? Ir1 N3 C22 C23 2.9(14) . . . . ? C20 C21 C22 N3 0(2) . . . . ? C20 C21 C22 C23 -178.1(13) . . . . ? N3 C22 C23 C28 177.6(12) . . . . ? C21 C22 C23 C28 -4(2) . . . . ? N3 C22 C23 C24 1.2(17) . . . . ? C21 C22 C23 C24 179.5(13) . . . . ? C28 C23 C24 C25 3.7(19) . . . . ? C22 C23 C24 C25 -179.8(11) . . . . ? C28 C23 C24 Ir1 178.6(10) . . . . ? C22 C23 C24 Ir1 -4.9(15) . . . . ? C35 Ir1 C24 C23 -87.9(10) . . . . ? N4 Ir1 C24 C23 -168.4(10) . . . . ? N3 Ir1 C24 C23 4.9(9) . . . . ? N1 Ir1 C24 C23 17(10) . . . . ? N2 Ir1 C24 C23 89.8(10) . . . . ? C35 Ir1 C24 C25 86.4(11) . . . . ? N4 Ir1 C24 C25 5.8(12) . . . . ? N3 Ir1 C24 C25 179.2(12) . . . . ? N1 Ir1 C24 C25 -168(9) . . . . ? N2 Ir1 C24 C25 -95.9(11) . . . . ? C23 C24 C25 C26 -3.8(18) . . . . ? Ir1 C24 C25 C26 -177.9(10) . . . . ? C24 C25 C26 C27 4(2) . . . . ? C25 C26 C27 C28 -3(2) . . . . ? C26 C27 C28 C23 3(2) . . . . ? C24 C23 C28 C27 -4(2) . . . . ? C22 C23 C28 C27 -179.8(13) . . . . ? C33 N4 C29 C30 2.5(16) . . . . ? Ir1 N4 C29 C30 -178.3(8) . . . . ? N4 C29 C30 C31 0.6(17) . . . . ? C29 C30 C31 C32 -1.4(17) . . . . ? C30 C31 C32 C33 -0.8(18) . . . . ? C29 N4 C33 C32 -4.7(15) . . . . ? Ir1 N4 C33 C32 176.0(8) . . . . ? C29 N4 C33 C34 175.1(9) . . . . ? Ir1 N4 C33 C34 -4.1(11) . . . . ? C31 C32 C33 N4 3.9(17) . . . . ? C31 C32 C33 C34 -175.9(11) . . . . ? N4 C33 C34 C39 179.9(10) . . . . ? C32 C33 C34 C39 -0.2(17) . . . . ? N4 C33 C34 C35 2.5(13) . . . . ? C32 C33 C34 C35 -177.6(10) . . . . ? C39 C34 C35 C36 0.0(15) . . . . ? C33 C34 C35 C36 177.5(9) . . . . ? C39 C34 C35 Ir1 -177.2(8) . . . . ? C33 C34 C35 Ir1 0.3(11) . . . . ? C24 Ir1 C35 C34 -96.9(8) . . . . ? N4 Ir1 C35 C34 -1.9(7) . . . . ? N3 Ir1 C35 C34 -176.5(7) . . . . ? N1 Ir1 C35 C34 85.9(7) . . . . ? N2 Ir1 C35 C34 96(2) . . . . ? C24 Ir1 C35 C36 86.3(10) . . . . ? N4 Ir1 C35 C36 -178.6(10) . . . . ? N3 Ir1 C35 C36 6.7(10) . . . . ? N1 Ir1 C35 C36 -90.9(10) . . . . ? N2 Ir1 C35 C36 -81(2) . . . . ? C34 C35 C36 C37 -0.9(16) . . . . ? Ir1 C35 C36 C37 175.8(9) . . . . ? C35 C36 C37 C38 1.3(18) . . . . ? C36 C37 C38 C39 -0.6(19) . . . . ? C37 C38 C39 C34 -0.3(18) . . . . ? C35 C34 C39 C38 0.6(16) . . . . ? C33 C34 C39 C38 -176.7(10) . . . . ? C51 N5 C40 C41 -2(2) . . . . ? Ir2 N5 C40 C41 176.8(11) . . . . ? N5 C40 C41 C42 3(2) . . . . ? C40 C41 C42 C43 -4(2) . . . . ? C41 C42 C43 C44 -176.6(17) . . . . ? C41 C42 C43 C51 4(2) . . . . ? C42 C43 C44 C45 -176.5(18) . . . . ? C51 C43 C44 C45 3(3) . . . . ? C43 C44 C45 C46 -4(3) . . . . ? C44 C45 C46 C50 3(3) . . . . ? C44 C45 C46 C47 -174(2) . . . . ? C50 C46 C47 C48 5(3) . . . . ? C45 C46 C47 C48 -178.3(18) . . . . ? C46 C47 C48 C49 -1(3) . . . . ? C50 N6 C49 C48 4(2) . . . . ? Ir2 N6 C49 C48 -171.5(11) . . . . ? C50 N6 C49 C52 -167.9(11) . . . . ? Ir2 N6 C49 C52 16.4(17) . . . . ? C47 C48 C49 N6 -3(2) . . . . ? C47 C48 C49 C52 169.4(15) . . . . ? C47 C46 C50 N6 -4(2) . . . . ? C45 C46 C50 N6 178.8(14) . . . . ? C47 C46 C50 C51 175.7(15) . . . . ? C45 C46 C50 C51 -1(2) . . . . ? C49 N6 C50 C46 -0.3(19) . . . . ? Ir2 N6 C50 C46 176.2(11) . . . . ? C49 N6 C50 C51 179.8(12) . . . . ? Ir2 N6 C50 C51 -3.7(14) . . . . ? C40 N5 C51 C50 -179.2(12) . . . . ? Ir2 N5 C51 C50 2.0(14) . . . . ? C40 N5 C51 C43 1.7(18) . . . . ? Ir2 N5 C51 C43 -177.1(10) . . . . ? C46 C50 C51 N5 -178.6(13) . . . . ? N6 C50 C51 N5 1.3(18) . . . . ? C46 C50 C51 C43 1(2) . . . . ? N6 C50 C51 C43 -179.6(12) . . . . ? C42 C43 C51 N5 -3(2) . . . . ? C44 C43 C51 N5 177.8(15) . . . . ? C42 C43 C51 C50 178.2(13) . . . . ? C44 C43 C51 C50 -1(2) . . . . ? Nd1 O3 C52 C53 -39.4(17) . . . . ? Nd1 O3 C52 C49 137.0(8) . . . . ? N6 C49 C52 O3 72.5(14) . . . . ? C48 C49 C52 O3 -100.3(15) . . . . ? N6 C49 C52 C53 -110.6(14) . . . . ? C48 C49 C52 C53 76.6(15) . . . . ? O3 C52 C53 C54 8.1(19) . . . . ? C49 C52 C53 C54 -168.2(11) . . . . ? Nd1 O4 C54 C53 14.6(19) . . . . ? Nd1 O4 C54 C55 -160.0(7) . . . . ? C52 C53 C54 O4 5(2) . . . . ? C52 C53 C54 C55 179.3(11) . . . . ? O4 C54 C55 F7 -154.1(11) . . . . ? C53 C54 C55 F7 30.7(16) . . . . ? O4 C54 C55 F6 -37.6(14) . . . . ? C53 C54 C55 F6 147.3(11) . . . . ? O4 C54 C55 C56 86.1(15) . . . . ? C53 C54 C55 C56 -89.1(15) . . . . ? F7 C55 C56 F10 -64.0(14) . . . . ? F6 C55 C56 F10 -176.6(11) . . . . ? C54 C55 C56 F10 59.6(17) . . . . ? F7 C55 C56 F9 176.4(11) . . . . ? F6 C55 C56 F9 63.8(15) . . . . ? C54 C55 C56 F9 -60.0(17) . . . . ? F7 C55 C56 F8 57.3(16) . . . . ? F6 C55 C56 F8 -55.4(16) . . . . ? C54 C55 C56 F8 -179.1(13) . . . . ? C61 N7 C57 C58 1.4(17) . . . . ? Ir2 N7 C57 C58 175.6(9) . . . . ? N7 C57 C58 C59 -1.4(18) . . . . ? C57 C58 C59 C60 0(2) . . . . ? C58 C59 C60 C61 1(2) . . . . ? C57 N7 C61 C62 177.8(10) . . . . ? Ir2 N7 C61 C62 2.9(13) . . . . ? C57 N7 C61 C60 -0.2(17) . . . . ? Ir2 N7 C61 C60 -175.1(9) . . . . ? C59 C60 C61 N7 -0.9(19) . . . . ? C59 C60 C61 C62 -178.7(12) . . . . ? N7 C61 C62 C67 172.3(11) . . . . ? C60 C61 C62 C67 -10(2) . . . . ? N7 C61 C62 C63 -7.8(15) . . . . ? C60 C61 C62 C63 170.1(11) . . . . ? C67 C62 C63 C64 2.6(16) . . . . ? C61 C62 C63 C64 -177.3(10) . . . . ? C67 C62 C63 Ir2 -170.8(9) . . . . ? C61 C62 C63 Ir2 9.2(12) . . . . ? C74 Ir2 C63 C64 87.6(10) . . . . ? N7 Ir2 C63 C64 -178.7(11) . . . . ? N8 Ir2 C63 C64 8.4(10) . . . . ? N5 Ir2 C63 C64 -88.7(10) . . . . ? N6 Ir2 C63 C64 -101(2) . . . . ? C74 Ir2 C63 C62 -99.8(8) . . . . ? N7 Ir2 C63 C62 -6.1(8) . . . . ? N8 Ir2 C63 C62 -179.0(8) . . . . ? N5 Ir2 C63 C62 83.9(8) . . . . ? N6 Ir2 C63 C62 72(2) . . . . ? C62 C63 C64 C65 -1.9(16) . . . . ? Ir2 C63 C64 C65 170.6(9) . . . . ? C63 C64 C65 C66 -1.4(18) . . . . ? C64 C65 C66 C67 4.5(19) . . . . ? C65 C66 C67 C62 -3.8(19) . . . . ? C61 C62 C67 C66 -179.9(12) . . . . ? C63 C62 C67 C66 0.2(18) . . . . ? C72 N8 C68 C69 -4.9(17) . . . . ? Ir2 N8 C68 C69 -177.2(9) . . . . ? N8 C68 C69 C70 2.9(19) . . . . ? C68 C69 C70 C71 0(2) . . . . ? C69 C70 C71 C72 -1(2) . . . . ? C68 N8 C72 C71 4.0(18) . . . . ? Ir2 N8 C72 C71 176.7(9) . . . . ? C68 N8 C72 C73 -175.6(10) . . . . ? Ir2 N8 C72 C73 -2.9(14) . . . . ? C70 C71 C72 N8 -1(2) . . . . ? C70 C71 C72 C73 178.3(13) . . . . ? N8 C72 C73 C78 -178.0(11) . . . . ? C71 C72 C73 C78 2(2) . . . . ? N8 C72 C73 C74 5.1(16) . . . . ? C71 C72 C73 C74 -174.5(12) . . . . ? C78 C73 C74 C75 1.0(18) . . . . ? C72 C73 C74 C75 178.0(11) . . . . ? C78 C73 C74 Ir2 178.0(9) . . . . ? C72 C73 C74 Ir2 -5.0(14) . . . . ? C63 Ir2 C74 C75 84.5(12) . . . . ? N7 Ir2 C74 C75 4.6(11) . . . . ? N8 Ir2 C74 C75 179.4(12) . . . . ? N5 Ir2 C74 C75 177(18) . . . . ? N6 Ir2 C74 C75 -93.8(11) . . . . ? C63 Ir2 C74 C73 -92.2(10) . . . . ? N7 Ir2 C74 C73 -172.1(9) . . . . ? N8 Ir2 C74 C73 2.7(9) . . . . ? N5 Ir2 C74 C73 0(8) . . . . ? N6 Ir2 C74 C73 89.5(9) . . . . ? C73 C74 C75 C76 -0.1(19) . . . . ? Ir2 C74 C75 C76 -176.7(10) . . . . ? C74 C75 C76 C77 -2(2) . . . . ? C75 C76 C77 C78 3(2) . . . . ? C76 C77 C78 C73 -1.8(19) . . . . ? C74 C73 C78 C77 0.0(19) . . . . ? C72 C73 C78 C77 -176.7(12) . . . . ? C83 C84 O14 C85 179(2) . . . . ? C86 C85 O14 C84 -176.9(19) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 561.7 87.5 2 0.000 1.000 0.500 561.8 87.3 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.331 _refine_diff_density_min -2.486 _refine_diff_density_rms 0.182