Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Robert Waymouth' _publ_contact_author_address ; Department of Chemistry Stanford University Stanford CA 94305-5080 UNITED STATES OF AMERICA ; _publ_contact_author_email WAYMOUTH@STANFORD.EDU _publ_section_title ; New Bimetallic Complexes of Late Transition Metals Involving Pyrazole-Bridged Bis N-Heterocyclic Carbene Ligands ; loop_ _publ_author_name 'Robert Waymouth' 'Sang-Jin Jeon.' # Attachment '6-Ir2.cif' data_zzzs _database_code_depnum_ccdc_archive 'CCDC 648819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 07044 _chemical_melting_point ? _chemical_formula_moiety 'C51 H67 Ir2 N6, F6 P' _chemical_formula_sum 'C51 H67 F6 Ir2 N6 P' _chemical_formula_weight 1293.48 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 30.809(8) _cell_length_b 18.203(5) _cell_length_c 16.420(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.924(4) _cell_angle_gamma 90.00 _cell_volume 9204(4) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3447 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3828 _exptl_absorpt_coefficient_mu 4.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2164 _exptl_absorpt_correction_T_max 0.5575 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45218 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.08 _reflns_number_total 16290 _reflns_number_gt 14518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The function SQUEEZE, in the program PLATON (A. L. Spek, Acta. Cryst. A46, C34 (1990)), was used to model solvent accessible void space. A void space of 2309.3 angstroms^3^, containing 769 electrons per cell, was found. The sample was also modeled as a racemic twin, in the ratio 94:6. ; _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^)+(0.0764P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 7824 Friedel Pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.059(9) _refine_ls_number_reflns 16290 _refine_ls_number_parameters 935 _refine_ls_number_restraints 230 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.030 _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 0.542444(11) 0.79571(2) 0.40212(2) 0.03306(10) Uani 1 1 d . . . Ir2 Ir 0.808491(11) 0.83003(2) 0.24079(2) 0.03236(10) Uani 1 1 d . . . Ir3 Ir 0.846613(12) 0.71033(2) 0.03631(2) 0.03561(10) Uani 1 1 d . . . P1 P 0.53892(9) 0.40426(15) 0.35050(17) 0.0419(6) Uani 1 1 d . . . F1 F 0.5148(3) 0.3589(4) 0.2798(5) 0.083(3) Uani 1 1 d . . . F2 F 0.5205(3) 0.3547(5) 0.4212(6) 0.093(3) Uani 1 1 d . . . F3 F 0.5639(2) 0.4510(4) 0.4203(5) 0.067(2) Uani 1 1 d . . . F4 F 0.5596(3) 0.4531(5) 0.2838(5) 0.080(2) Uani 1 1 d . . . F5 F 0.4984(2) 0.4587(4) 0.3583(6) 0.076(2) Uani 1 1 d . . . F6 F 0.5784(3) 0.3485(4) 0.3460(5) 0.075(2) Uani 1 1 d . . . P2 P 0.5035(4) 0.5294(2) -0.0058(6) 0.0448(18) Uani 0.454(17) 1 d PD A -1 F7 F 0.4624(5) 0.5666(8) -0.0491(9) 0.096(5) Uani 0.454(17) 1 d PD A -1 F8 F 0.4835(5) 0.4507(6) -0.0244(11) 0.082(5) Uani 0.454(17) 1 d PD A -1 F9 F 0.4799(5) 0.5311(9) 0.0785(8) 0.067(4) Uani 0.454(17) 1 d PD A -1 F10 F 0.5235(5) 0.6079(5) 0.0130(11) 0.082(5) Uani 0.454(17) 1 d PD A -1 F11 F 0.5446(4) 0.4920(8) 0.0375(9) 0.096(5) Uani 0.454(17) 1 d PD A -1 F12 F 0.5271(4) 0.5277(9) -0.0900(7) 0.067(4) Uani 0.454(17) 1 d PD A -1 P2' P 0.5035(4) 0.5294(2) -0.0058(6) 0.0448(18) Uani 0.046(17) 1 d PD A -2 F7' F 0.470(3) 0.594(5) -0.017(8) 0.096(5) Uani 0.046(17) 1 d PD A -2 F8' F 0.475(3) 0.480(6) -0.066(5) 0.082(5) Uani 0.046(17) 1 d PD A -2 F9' F 0.477(3) 0.499(7) 0.068(4) 0.067(4) Uani 0.046(17) 1 d PD A -2 F10' F 0.532(3) 0.579(6) 0.055(6) 0.082(5) Uani 0.046(17) 1 d PD A -2 F11' F 0.537(3) 0.465(5) 0.005(8) 0.096(5) Uani 0.046(17) 1 d PD A -2 F12' F 0.530(3) 0.560(7) -0.080(5) 0.067(4) Uani 0.046(17) 1 d PD A -2 N1 N 0.5070(3) 0.7566(5) 0.2226(5) 0.0358(18) Uani 1 1 d . . . N2 N 0.5261(3) 0.6634(4) 0.2977(5) 0.0393(19) Uani 1 1 d . . . N3 N 0.5109(3) 0.7103(5) 0.4623(4) 0.0354(17) Uani 1 1 d . . . N4 N 0.8444(3) 0.7899(5) 0.4203(5) 0.044(2) Uani 1 1 d . . . N5 N 0.8866(3) 0.8544(4) 0.3485(5) 0.0368(19) Uani 1 1 d . . . N6 N 0.8661(2) 0.8225(5) 0.1773(5) 0.0349(17) Uani 1 1 d . . . N7 N 0.8735(2) 0.8012(5) 0.1005(5) 0.0337(17) Uani 1 1 d . . . N8 N 0.9005(2) 0.8053(5) -0.0683(5) 0.039(2) Uani 1 1 d . . . N9 N 0.8452(3) 0.7784(4) -0.1424(5) 0.0372(19) Uani 1 1 d . . . C1 C 0.5236(3) 0.7402(6) 0.2970(5) 0.034(2) Uani 1 1 d . . . C2 C 0.5011(4) 0.6900(8) 0.1777(7) 0.061(4) Uani 1 1 d . . . H2A H 0.4913 0.6868 0.1223 0.074 Uiso 1 1 calc R . . C3 C 0.5111(4) 0.6336(7) 0.2251(7) 0.052(3) Uani 1 1 d . . . H3A H 0.5086 0.5830 0.2119 0.063 Uiso 1 1 calc R . . C4 C 0.4999(2) 0.8248(4) 0.1872(4) 0.046(2) Uani 1 1 d GU B . C5 C 0.4631(2) 0.8641(5) 0.2075(5) 0.072(4) Uani 1 1 d GU . . C6 C 0.4561(3) 0.9341(6) 0.1758(7) 0.112(7) Uani 1 1 d GU B . H6 H 0.4310 0.9610 0.1896 0.134 Uiso 1 1 calc R . . C7 C 0.4859(4) 0.9647(4) 0.1238(7) 0.111(7) Uani 1 1 d GU . . H7 H 0.4811 1.0125 0.1021 0.133 Uiso 1 1 calc R B . C8 C 0.5227(3) 0.9254(4) 0.1036(5) 0.071(3) Uani 1 1 d GU B . H8 H 0.5430 0.9464 0.0681 0.085 Uiso 1 1 calc R . . C9 C 0.5297(2) 0.8555(4) 0.1353(4) 0.042(2) Uani 1 1 d GU . . C10 C 0.4277(4) 0.8299(9) 0.2614(7) 0.086(5) Uani 0.86(3) 1 d PDU B 1 H10 H 0.4425 0.8003 0.3053 0.103 Uiso 0.86(3) 1 calc PR B 1 C11 C 0.4002(9) 0.8873(17) 0.3010(12) 0.143(11) Uani 0.86(3) 1 d PDU B 1 H11A H 0.4189 0.9203 0.3338 0.215 Uiso 0.86(3) 1 calc PR B 1 H11B H 0.3794 0.8633 0.3362 0.215 Uiso 0.86(3) 1 calc PR B 1 H11C H 0.3844 0.9158 0.2589 0.215 Uiso 0.86(3) 1 calc PR B 1 C12 C 0.3989(6) 0.7797(16) 0.2118(16) 0.110(7) Uani 0.86(3) 1 d PDU B 1 H12A H 0.4165 0.7414 0.1871 0.165 Uiso 0.86(3) 1 calc PR B 1 H12B H 0.3836 0.8079 0.1688 0.165 Uiso 0.86(3) 1 calc PR B 1 H12C H 0.3776 0.7569 0.2470 0.165 Uiso 0.86(3) 1 calc PR B 1 C10' C 0.4277(4) 0.8299(9) 0.2614(7) 0.086(5) Uani 0.14(3) 1 d PD B 2 H10' H 0.4048 0.8626 0.2364 0.103 Uiso 0.14(3) 1 calc PR B 2 C11' C 0.405(4) 0.828(9) 0.341(4) 0.143(11) Uani 0.14(3) 1 d PD B 2 H11D H 0.4150 0.8689 0.3755 0.215 Uiso 0.14(3) 1 calc PR B 2 H11E H 0.4111 0.7814 0.3689 0.215 Uiso 0.14(3) 1 calc PR B 2 H11F H 0.3734 0.8325 0.3306 0.215 Uiso 0.14(3) 1 calc PR B 2 C12' C 0.412(5) 0.766(7) 0.210(10) 0.110(7) Uani 0.14(3) 1 d PD B 2 H12D H 0.4295 0.7639 0.1607 0.165 Uiso 0.14(3) 1 calc PR B 2 H12E H 0.3817 0.7727 0.1946 0.165 Uiso 0.14(3) 1 calc PR B 2 H12F H 0.4163 0.7206 0.2410 0.165 Uiso 0.14(3) 1 calc PR B 2 C13 C 0.5703(4) 0.8139(7) 0.1126(7) 0.059(3) Uani 0.19(5) 1 d PDU B 1 H13 H 0.5680 0.7712 0.1505 0.070 Uiso 0.19(5) 1 calc PR B 1 C14 C 0.6133(17) 0.849(6) 0.149(5) 0.098(7) Uani 0.19(5) 1 d PDU B 1 H14A H 0.6384 0.8216 0.1308 0.148 Uiso 0.19(5) 1 calc PR B 1 H14B H 0.6129 0.8483 0.2088 0.148 Uiso 0.19(5) 1 calc PR B 1 H14C H 0.6153 0.9004 0.1307 0.148 Uiso 0.19(5) 1 calc PR B 1 C15 C 0.580(3) 0.771(5) 0.032(4) 0.073(5) Uani 0.19(5) 1 d PDU B 1 H15A H 0.6086 0.7488 0.0363 0.109 Uiso 0.19(5) 1 calc PR B 1 H15B H 0.5785 0.8054 -0.0143 0.109 Uiso 0.19(5) 1 calc PR B 1 H15C H 0.5577 0.7327 0.0231 0.109 Uiso 0.19(5) 1 calc PR B 1 C13' C 0.5703(4) 0.8139(7) 0.1126(7) 0.059(3) Uani 0.81(5) 1 d PD B 2 H13' H 0.5756 0.7731 0.1525 0.070 Uiso 0.81(5) 1 calc PR B 2 C14' C 0.6104(5) 0.8657(14) 0.1149(15) 0.098(7) Uani 0.81(5) 1 d PD B 2 H14D H 0.6363 0.8379 0.1004 0.148 Uiso 0.81(5) 1 calc PR B 2 H14E H 0.6147 0.8861 0.1698 0.148 Uiso 0.81(5) 1 calc PR B 2 H14F H 0.6056 0.9058 0.0758 0.148 Uiso 0.81(5) 1 calc PR B 2 C15' C 0.5628(8) 0.7802(12) 0.0247(8) 0.073(5) Uani 0.81(5) 1 d PD B 2 H15D H 0.5888 0.7531 0.0094 0.109 Uiso 0.81(5) 1 calc PR B 2 H15E H 0.5571 0.8198 -0.0146 0.109 Uiso 0.81(5) 1 calc PR B 2 H15F H 0.5379 0.7467 0.0246 0.109 Uiso 0.81(5) 1 calc PR B 2 C16 C 0.5415(6) 0.6228(9) 0.3710(8) 0.073(4) Uani 1 1 d . . . H16A H 0.5381 0.5694 0.3613 0.087 Uiso 1 1 calc R . . H16B H 0.5727 0.6331 0.3815 0.087 Uiso 1 1 calc R . . C17 C 0.5174(4) 0.6438(6) 0.4418(6) 0.046(3) Uani 1 1 d . . . C18 C 0.5000 0.5947(9) 0.5000 0.053(4) Uani 1 2 d S . . H18A H 0.5000 0.5425 0.5000 0.064 Uiso 1 2 calc SR . . C19 C 0.5597(4) 0.8939(7) 0.3399(8) 0.059(3) Uani 1 1 d U . . H19A H 0.5462 0.9007 0.2842 0.071 Uiso 1 1 calc R . . C20 C 0.5948(4) 0.8500(8) 0.3448(7) 0.058(3) Uani 1 1 d U . . H20A H 0.6019 0.8275 0.2913 0.069 Uiso 1 1 calc R . . C21 C 0.6355(4) 0.8605(14) 0.4021(8) 0.108(7) Uani 1 1 d U . . H21A H 0.6390 0.9132 0.4158 0.130 Uiso 1 1 calc R . . H21B H 0.6617 0.8442 0.3741 0.130 Uiso 1 1 calc R . . C22 C 0.6305(4) 0.8141(13) 0.4838(8) 0.092(5) Uani 1 1 d U . . H22A H 0.6433 0.7648 0.4762 0.110 Uiso 1 1 calc R . . H22B H 0.6471 0.8387 0.5286 0.110 Uiso 1 1 calc R . . C23 C 0.5849(3) 0.8054(8) 0.5077(6) 0.054(3) Uani 1 1 d U . . H23A H 0.5806 0.7664 0.5495 0.065 Uiso 1 1 calc R . . C24 C 0.5549(4) 0.8627(6) 0.5104(6) 0.046(2) Uani 1 1 d U . . H24A H 0.5328 0.8566 0.5533 0.055 Uiso 1 1 calc R . . C25 C 0.5642(6) 0.9426(7) 0.4887(9) 0.077(4) Uani 1 1 d U . . H25A H 0.5460 0.9749 0.5222 0.093 Uiso 1 1 calc R . . H25B H 0.5950 0.9535 0.5029 0.093 Uiso 1 1 calc R . . C26 C 0.5554(6) 0.9605(7) 0.3999(9) 0.079(4) Uani 1 1 d U . . H26A H 0.5759 0.9994 0.3838 0.095 Uiso 1 1 calc R . . H26B H 0.5257 0.9806 0.3935 0.095 Uiso 1 1 calc R . . C27 C 0.8466(3) 0.8228(5) 0.3458(5) 0.0290(14) Uani 1 1 d . . . C28 C 0.8823(3) 0.8042(8) 0.4666(7) 0.055(3) Uani 1 1 d . . . H28A H 0.8889 0.7874 0.5204 0.066 Uiso 1 1 calc R . . C29 C 0.9075(3) 0.8461(7) 0.4211(7) 0.049(3) Uani 1 1 d . . . H29A H 0.9350 0.8661 0.4370 0.058 Uiso 1 1 calc R . . C30 C 0.9019(4) 0.9011(6) 0.2844(6) 0.045(3) Uani 1 1 d . . . H30A H 0.9320 0.9168 0.2981 0.054 Uiso 1 1 calc R . . H30B H 0.8835 0.9457 0.2804 0.054 Uiso 1 1 calc R . . C31 C 0.9008(3) 0.8630(5) 0.2049(6) 0.036(2) Uani 1 1 d . . . C32 C 0.9310(3) 0.8701(6) 0.1412(6) 0.039(2) Uani 1 1 d . . . H32A H 0.9571 0.8980 0.1408 0.046 Uiso 1 1 calc R . . C33 C 0.9126(3) 0.8258(7) 0.0796(6) 0.046(2) Uani 1 1 d . . . C34 C 0.9325(3) 0.8064(6) 0.0025(6) 0.045(2) Uani 1 1 d . . . H34A H 0.9461 0.7574 0.0081 0.054 Uiso 1 1 calc R . . H34B H 0.9557 0.8424 -0.0086 0.054 Uiso 1 1 calc R . . C35 C 0.9066(3) 0.8406(6) -0.1385(7) 0.047(3) Uani 1 1 d . . . H35A H 0.9306 0.8703 -0.1522 0.057 Uiso 1 1 calc R . . C36 C 0.8716(4) 0.8249(7) -0.1849(6) 0.046(3) Uani 1 1 d . . . H36A H 0.8657 0.8428 -0.2384 0.055 Uiso 1 1 calc R . . C37 C 0.8638(3) 0.7674(5) -0.0663(5) 0.0290(14) Uani 1 1 d . . . C38 C 0.8089(3) 0.7493(6) 0.4518(6) 0.041(2) Uani 1 1 d . C . C39 C 0.8058(5) 0.6724(7) 0.4341(8) 0.065(4) Uani 1 1 d . . . C40 C 0.7665(7) 0.6404(9) 0.4698(10) 0.089(6) Uani 1 1 d . C . H40A H 0.7597 0.5909 0.4561 0.107 Uiso 1 1 calc R . . C41 C 0.7405(6) 0.6735(9) 0.5180(9) 0.075(4) Uani 1 1 d . . . H41A H 0.7169 0.6478 0.5404 0.090 Uiso 1 1 calc R C . C42 C 0.7473(4) 0.7464(7) 0.5365(7) 0.052(3) Uani 1 1 d . C . H42A H 0.7276 0.7721 0.5696 0.063 Uiso 1 1 calc R . . C43 C 0.7830(3) 0.7820(6) 0.5064(6) 0.039(2) Uani 1 1 d . . . C44 C 0.8335(5) 0.6351(7) 0.3795(9) 0.081(4) Uani 0.67(4) 1 d PDU C 1 H44 H 0.8399 0.6733 0.3378 0.097 Uiso 0.67(4) 1 calc PR C 1 C45 C 0.8162(12) 0.5653(11) 0.3251(14) 0.075(6) Uani 0.67(4) 1 d PDU C 1 H45A H 0.8397 0.5473 0.2917 0.113 Uiso 0.67(4) 1 calc PR C 1 H45B H 0.7917 0.5808 0.2896 0.113 Uiso 0.67(4) 1 calc PR C 1 H45C H 0.8068 0.5260 0.3613 0.113 Uiso 0.67(4) 1 calc PR C 1 C46 C 0.8809(13) 0.621(2) 0.426(3) 0.149(14) Uani 0.67(4) 1 d PDU C 1 H46A H 0.9003 0.5959 0.3890 0.223 Uiso 0.67(4) 1 calc PR C 1 H46B H 0.8770 0.5907 0.4745 0.223 Uiso 0.67(4) 1 calc PR C 1 H46C H 0.8937 0.6684 0.4424 0.223 Uiso 0.67(4) 1 calc PR C 1 C44' C 0.8335(5) 0.6351(7) 0.3795(9) 0.081(4) Uani 0.33(4) 1 d PDU C 2 H44' H 0.8456 0.6723 0.3417 0.097 Uiso 0.33(4) 1 calc PR C 2 C45' C 0.7980(17) 0.585(3) 0.328(3) 0.075(6) Uani 0.33(4) 1 d PDU C 2 H45D H 0.8129 0.5562 0.2871 0.113 Uiso 0.33(4) 1 calc PR C 2 H45E H 0.7767 0.6176 0.3003 0.113 Uiso 0.33(4) 1 calc PR C 2 H45F H 0.7831 0.5524 0.3650 0.113 Uiso 0.33(4) 1 calc PR C 2 C46' C 0.874(3) 0.587(4) 0.419(7) 0.149(14) Uani 0.33(4) 1 d PDU C 2 H46D H 0.8971 0.5829 0.3795 0.223 Uiso 0.33(4) 1 calc PR C 2 H46E H 0.8639 0.5375 0.4330 0.223 Uiso 0.33(4) 1 calc PR C 2 H46F H 0.8856 0.6112 0.4685 0.223 Uiso 0.33(4) 1 calc PR C 2 C47 C 0.7866(4) 0.8636(6) 0.5290(7) 0.045(3) Uani 1 1 d . C . H47A H 0.8077 0.8864 0.4915 0.054 Uiso 1 1 calc R . . C48 C 0.8077(5) 0.8658(8) 0.6161(8) 0.066(4) Uani 1 1 d . . . H48A H 0.8355 0.8396 0.6167 0.099 Uiso 1 1 calc R C . H48B H 0.7882 0.8423 0.6543 0.099 Uiso 1 1 calc R . . H48C H 0.8126 0.9170 0.6325 0.099 Uiso 1 1 calc R . . C49 C 0.7458(5) 0.9071(9) 0.5221(10) 0.074(4) Uani 1 1 d . . . H49A H 0.7292 0.8924 0.4728 0.111 Uiso 1 1 calc R C . H49B H 0.7529 0.9595 0.5190 0.111 Uiso 1 1 calc R . . H49C H 0.7284 0.8981 0.5700 0.111 Uiso 1 1 calc R . . C50 C 0.8060(3) 0.7454(6) -0.1800(6) 0.043(2) Uani 1 1 d . . . C51 C 0.8122(4) 0.6853(6) -0.2322(6) 0.043(2) Uani 1 1 d . . . C52 C 0.7752(4) 0.6540(7) -0.2681(7) 0.053(3) Uani 1 1 d . . . H52A H 0.7776 0.6131 -0.3035 0.064 Uiso 1 1 calc R . . C53 C 0.7344(5) 0.6832(8) -0.2515(8) 0.068(4) Uani 1 1 d . . . H53A H 0.7093 0.6608 -0.2757 0.082 Uiso 1 1 calc R . . C54 C 0.7292(4) 0.7419(9) -0.2026(7) 0.060(3) Uani 1 1 d . . . H54A H 0.7009 0.7604 -0.1935 0.072 Uiso 1 1 calc R . . C55 C 0.7665(4) 0.7762(5) -0.1646(6) 0.041(2) Uani 1 1 d . . . C56 C 0.8559(4) 0.6555(6) -0.2503(7) 0.054(3) Uani 1 1 d . . . H56A H 0.8773 0.6775 -0.2100 0.065 Uiso 1 1 calc R . . C57 C 0.8708(6) 0.6744(9) -0.3346(8) 0.081(5) Uani 1 1 d . . . H57A H 0.9014 0.6606 -0.3392 0.122 Uiso 1 1 calc R . . H57B H 0.8676 0.7274 -0.3438 0.122 Uiso 1 1 calc R . . H57C H 0.8531 0.6476 -0.3754 0.122 Uiso 1 1 calc R . . C58 C 0.8599(5) 0.5686(8) -0.2430(10) 0.085(5) Uani 1 1 d . . . H58A H 0.8493 0.5527 -0.1902 0.128 Uiso 1 1 calc R . . H58B H 0.8903 0.5541 -0.2473 0.128 Uiso 1 1 calc R . . H58C H 0.8424 0.5455 -0.2869 0.128 Uiso 1 1 calc R . . C59 C 0.7607(4) 0.8430(7) -0.1120(8) 0.060(3) Uani 1 1 d . . . H59A H 0.7849 0.8427 -0.0699 0.072 Uiso 1 1 calc R . . C60 C 0.7182(4) 0.8436(12) -0.0660(8) 0.086(5) Uani 1 1 d . . . H60A H 0.7040 0.7956 -0.0716 0.129 Uiso 1 1 calc R . . H60B H 0.6989 0.8818 -0.0888 0.129 Uiso 1 1 calc R . . H60C H 0.7245 0.8538 -0.0082 0.129 Uiso 1 1 calc R . . C61 C 0.7667(5) 0.9147(7) -0.1657(10) 0.079(5) Uani 1 1 d . . . H61A H 0.7948 0.9128 -0.1918 0.118 Uiso 1 1 calc R . . H61B H 0.7655 0.9583 -0.1309 0.118 Uiso 1 1 calc R . . H61C H 0.7433 0.9173 -0.2077 0.118 Uiso 1 1 calc R . . C62 C 0.7585(4) 0.8806(7) 0.3053(9) 0.058(3) Uani 1 1 d U . . H62A H 0.7673 0.8934 0.3628 0.069 Uiso 1 1 calc R . . C63 C 0.7484(3) 0.8068(7) 0.2947(7) 0.048(2) Uani 1 1 d U . . H63A H 0.7506 0.7764 0.3454 0.058 Uiso 1 1 calc R . . C64 C 0.7152(4) 0.7814(10) 0.2328(8) 0.077(4) Uani 1 1 d U . . H64A H 0.7097 0.7287 0.2432 0.092 Uiso 1 1 calc R . . H64B H 0.6878 0.8079 0.2431 0.092 Uiso 1 1 calc R . . C65 C 0.7230(4) 0.7887(13) 0.1531(9) 0.101(6) Uani 1 1 d U . . H65A H 0.6998 0.8197 0.1280 0.121 Uiso 1 1 calc R . . H65B H 0.7206 0.7395 0.1275 0.121 Uiso 1 1 calc R . . C66 C 0.7678(3) 0.8225(8) 0.1311(6) 0.050(2) Uani 1 1 d U . . H66A H 0.7820 0.7975 0.0847 0.060 Uiso 1 1 calc R . . C67 C 0.7815(4) 0.8921(7) 0.1444(8) 0.055(3) Uani 1 1 d U . . H67A H 0.8030 0.9103 0.1048 0.066 Uiso 1 1 calc R . . C68 C 0.7521(6) 0.9543(9) 0.1824(11) 0.088(5) Uani 1 1 d U . . H68A H 0.7684 1.0011 0.1815 0.106 Uiso 1 1 calc R . . H68B H 0.7259 0.9605 0.1464 0.106 Uiso 1 1 calc R . . C69 C 0.7389(5) 0.9433(9) 0.2590(10) 0.080(4) Uani 1 1 d U . . H69A H 0.7070 0.9364 0.2565 0.096 Uiso 1 1 calc R . . H69B H 0.7449 0.9888 0.2906 0.096 Uiso 1 1 calc R . . C70 C 0.8178(4) 0.6601(6) 0.1416(7) 0.049(2) Uani 1 1 d U . . H70A H 0.8104 0.6942 0.1868 0.058 Uiso 1 1 calc R . . C71 C 0.8598(5) 0.6404(6) 0.1382(7) 0.056(3) Uani 1 1 d U . . H71A H 0.8781 0.6655 0.1813 0.067 Uiso 1 1 calc R . . C72 C 0.8793(9) 0.5703(11) 0.1128(11) 0.115(7) Uani 1 1 d U . . H72A H 0.9112 0.5766 0.1104 0.137 Uiso 1 1 calc R . . H72B H 0.8737 0.5324 0.1544 0.137 Uiso 1 1 calc R . . C73 C 0.8639(7) 0.5468(8) 0.0403(13) 0.103(5) Uani 1 1 d U . . H73A H 0.8392 0.5134 0.0498 0.124 Uiso 1 1 calc R . . H73B H 0.8868 0.5174 0.0149 0.124 Uiso 1 1 calc R . . C74 C 0.8481(5) 0.6073(7) -0.0226(7) 0.065(3) Uani 1 1 d U . . H74A H 0.8615 0.6062 -0.0771 0.078 Uiso 1 1 calc R . . C75 C 0.8055(5) 0.6310(6) -0.0211(8) 0.059(3) Uani 1 1 d U . . H75A H 0.7940 0.6474 -0.0758 0.071 Uiso 1 1 calc R . . C76 C 0.7693(5) 0.6045(10) 0.0347(9) 0.086(5) Uani 1 1 d U . . H76A H 0.7437 0.6371 0.0278 0.104 Uiso 1 1 calc R . . H76B H 0.7604 0.5541 0.0189 0.104 Uiso 1 1 calc R . . C77 C 0.7842(6) 0.6050(9) 0.1182(9) 0.079(4) Uani 1 1 d U . . H77A H 0.7959 0.5557 0.1316 0.095 Uiso 1 1 calc R . . H77B H 0.7588 0.6131 0.1524 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03329(19) 0.03258(19) 0.0332(2) -0.00238(16) -0.00001(14) 0.00014(15) Ir2 0.03093(18) 0.03016(18) 0.0358(2) 0.00125(16) -0.00164(14) 0.00090(15) Ir3 0.0393(2) 0.02883(18) 0.0389(2) 0.00147(16) 0.00394(16) 0.00009(16) P1 0.0407(14) 0.0387(15) 0.0463(15) -0.0035(12) 0.0018(11) 0.0041(11) F1 0.091(6) 0.065(5) 0.090(6) -0.035(4) -0.041(5) 0.006(4) F2 0.104(7) 0.089(6) 0.091(6) 0.023(5) 0.050(5) 0.001(5) F3 0.062(4) 0.071(5) 0.068(5) -0.015(4) -0.016(3) 0.011(4) F4 0.104(6) 0.072(5) 0.066(5) 0.012(4) 0.024(4) -0.006(5) F5 0.045(4) 0.061(5) 0.120(7) -0.023(4) -0.020(4) 0.013(3) F6 0.070(5) 0.070(5) 0.084(5) -0.010(4) 0.003(4) 0.034(4) P2 0.060(4) 0.034(2) 0.041(3) 0.012(5) 0.012(3) 0.003(5) F7 0.094(9) 0.128(13) 0.066(10) 0.052(8) 0.001(7) 0.021(9) F8 0.121(11) 0.055(7) 0.073(10) -0.014(7) 0.019(8) -0.042(7) F9 0.076(7) 0.073(9) 0.054(5) 0.005(11) 0.017(5) -0.015(12) F10 0.121(11) 0.055(7) 0.073(10) -0.014(7) 0.019(8) -0.042(7) F11 0.094(9) 0.128(13) 0.066(10) 0.052(8) 0.001(7) 0.021(9) F12 0.076(7) 0.073(9) 0.054(5) 0.005(11) 0.017(5) -0.015(12) P2' 0.060(4) 0.034(2) 0.041(3) 0.012(5) 0.012(3) 0.003(5) F7' 0.094(9) 0.128(13) 0.066(10) 0.052(8) 0.001(7) 0.021(9) F8' 0.121(11) 0.055(7) 0.073(10) -0.014(7) 0.019(8) -0.042(7) F9' 0.076(7) 0.073(9) 0.054(5) 0.005(11) 0.017(5) -0.015(12) F10' 0.121(11) 0.055(7) 0.073(10) -0.014(7) 0.019(8) -0.042(7) F11' 0.094(9) 0.128(13) 0.066(10) 0.052(8) 0.001(7) 0.021(9) F12' 0.076(7) 0.073(9) 0.054(5) 0.005(11) 0.017(5) -0.015(12) N1 0.040(4) 0.038(5) 0.030(4) 0.008(4) 0.000(3) 0.000(4) N2 0.057(5) 0.024(4) 0.036(5) -0.002(3) -0.003(4) 0.005(4) N3 0.044(4) 0.031(4) 0.032(4) -0.005(4) 0.002(3) 0.000(4) N4 0.053(5) 0.046(5) 0.035(4) -0.003(4) 0.001(4) 0.004(4) N5 0.036(4) 0.037(5) 0.036(4) -0.008(3) -0.006(3) -0.004(3) N6 0.028(4) 0.032(4) 0.044(5) -0.006(4) 0.000(3) -0.006(3) N7 0.028(4) 0.036(4) 0.038(4) 0.008(4) 0.001(3) 0.000(3) N8 0.033(4) 0.055(6) 0.029(4) 0.003(4) 0.007(3) 0.011(4) N9 0.050(5) 0.023(4) 0.038(5) -0.006(3) -0.007(4) -0.005(3) C1 0.055(6) 0.035(5) 0.013(4) -0.004(4) -0.001(4) -0.005(5) C2 0.052(7) 0.098(12) 0.034(6) -0.018(6) 0.004(5) -0.013(7) C3 0.077(8) 0.039(6) 0.042(6) -0.005(5) 0.013(6) 0.002(6) C4 0.050(5) 0.045(5) 0.043(6) 0.006(5) 0.000(4) 0.003(4) C5 0.061(7) 0.099(9) 0.056(8) 0.025(7) 0.006(5) 0.038(7) C6 0.111(12) 0.124(13) 0.103(13) 0.048(11) 0.032(9) 0.086(12) C7 0.169(17) 0.073(10) 0.093(12) 0.036(9) 0.041(11) 0.069(10) C8 0.074(8) 0.048(6) 0.090(10) 0.024(6) 0.007(6) 0.000(5) C9 0.047(5) 0.045(5) 0.032(5) 0.008(4) -0.005(4) 0.004(4) C10 0.047(6) 0.155(14) 0.056(8) 0.038(8) 0.000(5) 0.053(8) C11 0.136(19) 0.23(3) 0.066(13) 0.024(13) 0.039(12) 0.115(18) C12 0.048(12) 0.17(2) 0.108(14) 0.048(12) 0.014(11) 0.011(12) C10' 0.047(6) 0.155(14) 0.056(8) 0.038(8) 0.000(5) 0.053(8) C11' 0.136(19) 0.23(3) 0.066(13) 0.024(13) 0.039(12) 0.115(18) C12' 0.048(12) 0.17(2) 0.108(14) 0.048(12) 0.014(11) 0.011(12) C13 0.056(6) 0.073(10) 0.047(6) 0.018(5) 0.005(5) 0.012(6) C14 0.053(8) 0.20(2) 0.046(12) 0.071(11) 0.005(8) -0.006(10) C15 0.064(13) 0.106(14) 0.051(7) 0.031(7) 0.027(7) 0.054(10) C13' 0.056(6) 0.073(10) 0.047(6) 0.018(5) 0.005(5) 0.012(6) C14' 0.053(8) 0.20(2) 0.046(12) 0.071(11) 0.005(8) -0.006(10) C15' 0.064(13) 0.106(14) 0.051(7) 0.031(7) 0.027(7) 0.054(10) C16 0.111(12) 0.067(9) 0.041(7) 0.013(6) -0.001(7) 0.000(8) C17 0.075(7) 0.029(5) 0.031(5) -0.003(4) -0.012(5) 0.023(5) C18 0.093(13) 0.029(8) 0.037(8) 0.000 0.004(8) 0.000 C19 0.063(6) 0.055(7) 0.059(7) -0.003(5) 0.008(6) -0.032(5) C20 0.042(5) 0.091(9) 0.042(5) -0.013(6) 0.019(4) -0.035(5) C21 0.039(6) 0.23(2) 0.058(8) -0.023(9) 0.016(5) -0.040(9) C22 0.036(5) 0.173(18) 0.065(7) -0.021(8) -0.017(5) -0.013(8) C23 0.041(5) 0.087(8) 0.034(5) -0.011(6) -0.004(4) 0.001(5) C24 0.063(6) 0.045(5) 0.032(5) -0.013(4) 0.017(5) -0.029(4) C25 0.110(11) 0.048(6) 0.075(7) -0.017(6) 0.025(8) -0.045(7) C26 0.126(13) 0.029(6) 0.085(8) -0.003(5) 0.028(9) -0.029(7) C27 0.037(3) 0.023(3) 0.027(3) -0.008(3) 0.008(3) -0.001(3) C28 0.041(6) 0.077(9) 0.046(6) -0.008(6) -0.009(5) 0.015(6) C29 0.036(5) 0.065(8) 0.044(6) -0.005(5) -0.007(5) -0.005(5) C30 0.050(6) 0.051(7) 0.033(5) 0.013(5) -0.007(4) -0.015(5) C31 0.027(5) 0.025(5) 0.057(6) -0.006(4) -0.002(4) -0.001(4) C32 0.032(5) 0.042(6) 0.042(6) 0.002(4) 0.002(4) -0.013(4) C33 0.037(5) 0.056(6) 0.045(6) 0.007(5) 0.006(4) -0.008(5) C34 0.034(5) 0.052(7) 0.049(6) -0.005(5) 0.004(4) -0.001(4) C35 0.042(6) 0.047(7) 0.055(7) 0.004(5) 0.021(5) -0.007(5) C36 0.067(7) 0.044(6) 0.027(5) 0.010(5) 0.023(5) -0.004(6) C37 0.037(3) 0.023(3) 0.027(3) -0.008(3) 0.008(3) -0.001(3) C38 0.052(6) 0.050(6) 0.020(5) 0.004(4) -0.003(4) -0.003(5) C39 0.102(10) 0.044(7) 0.049(7) 0.004(6) -0.006(7) 0.026(7) C40 0.147(16) 0.054(9) 0.067(10) 0.013(7) -0.003(10) -0.051(10) C41 0.107(12) 0.064(9) 0.055(8) 0.026(8) 0.018(8) -0.028(9) C42 0.064(7) 0.058(8) 0.036(6) -0.001(5) 0.007(5) 0.002(6) C43 0.042(5) 0.048(6) 0.027(5) 0.001(4) 0.005(4) 0.001(5) C44 0.130(11) 0.030(6) 0.084(10) 0.005(6) 0.021(8) 0.026(6) C45 0.144(17) 0.020(9) 0.062(9) 0.023(8) 0.016(12) 0.019(9) C46 0.24(2) 0.09(2) 0.108(18) -0.04(2) -0.079(18) 0.08(2) C44' 0.130(11) 0.030(6) 0.084(10) 0.005(6) 0.021(8) 0.026(6) C45' 0.144(17) 0.020(9) 0.062(9) 0.023(8) 0.016(12) 0.019(9) C46' 0.24(2) 0.09(2) 0.108(18) -0.04(2) -0.079(18) 0.08(2) C47 0.052(6) 0.037(6) 0.047(6) -0.012(5) 0.012(5) -0.003(5) C48 0.078(9) 0.053(8) 0.068(9) -0.013(7) 0.009(7) 0.014(7) C49 0.063(8) 0.068(9) 0.090(11) 0.017(8) -0.015(7) 0.019(7) C50 0.039(5) 0.046(6) 0.044(6) 0.003(5) 0.005(4) -0.006(5) C51 0.057(6) 0.039(6) 0.032(5) 0.002(4) 0.006(4) -0.021(5) C52 0.061(7) 0.061(8) 0.037(6) -0.002(5) -0.004(5) -0.015(6) C53 0.073(9) 0.073(9) 0.058(8) -0.002(7) -0.011(7) -0.025(7) C54 0.035(6) 0.098(10) 0.047(7) -0.008(7) 0.002(5) 0.001(6) C55 0.056(6) 0.028(5) 0.040(6) 0.004(4) -0.004(5) -0.006(4) C56 0.065(7) 0.041(6) 0.057(7) -0.018(5) 0.026(6) -0.016(5) C57 0.125(13) 0.065(9) 0.055(8) -0.008(7) 0.030(8) -0.020(9) C58 0.089(10) 0.072(10) 0.098(11) -0.042(8) 0.057(9) -0.036(8) C59 0.051(6) 0.066(9) 0.063(7) -0.021(6) -0.005(5) 0.026(6) C60 0.062(8) 0.150(17) 0.047(7) -0.028(9) -0.003(6) 0.027(9) C61 0.096(10) 0.029(6) 0.114(12) -0.023(7) 0.045(9) 0.013(7) C62 0.037(6) 0.059(6) 0.078(8) 0.002(5) 0.012(5) 0.014(5) C63 0.033(5) 0.064(6) 0.048(5) 0.003(5) 0.000(4) -0.006(5) C64 0.052(7) 0.118(13) 0.061(7) 0.007(8) -0.002(5) -0.036(8) C65 0.046(7) 0.188(18) 0.069(6) -0.044(11) 0.008(6) -0.046(9) C66 0.022(4) 0.085(7) 0.043(6) -0.015(6) -0.005(4) 0.011(5) C67 0.051(6) 0.050(6) 0.064(7) 0.018(5) -0.004(5) 0.028(5) C68 0.089(10) 0.062(8) 0.117(11) 0.027(7) 0.031(9) 0.052(8) C69 0.074(9) 0.066(8) 0.101(10) -0.003(7) 0.018(8) 0.040(7) C70 0.074(6) 0.029(5) 0.043(6) 0.007(4) 0.003(5) -0.012(4) C71 0.086(7) 0.032(5) 0.048(6) 0.020(5) -0.001(6) 0.003(5) C72 0.19(2) 0.076(11) 0.081(9) 0.031(8) 0.038(10) 0.068(12) C73 0.144(15) 0.031(7) 0.138(12) -0.006(6) 0.039(10) 0.041(9) C74 0.110(8) 0.046(7) 0.042(6) -0.012(5) 0.041(6) -0.006(6) C75 0.095(7) 0.030(6) 0.051(6) 0.005(5) 0.001(6) -0.024(5) C76 0.082(9) 0.095(12) 0.082(8) 0.001(8) 0.001(7) -0.053(9) C77 0.099(10) 0.076(10) 0.064(7) -0.001(7) 0.015(7) -0.051(8) _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 2.067(9) . ? Ir1 N3 2.097(9) . ? Ir1 C19 2.136(12) . ? Ir1 C20 2.138(10) . ? Ir1 C23 2.144(10) . ? Ir1 C24 2.180(10) . ? Ir2 C27 2.056(9) . ? Ir2 N6 2.092(7) . ? Ir2 C67 2.093(11) . ? Ir2 C62 2.110(11) . ? Ir2 C63 2.121(10) . ? Ir2 C66 2.164(10) . ? Ir3 C37 2.063(9) . ? Ir3 C74 2.111(12) . ? Ir3 N7 2.115(8) . ? Ir3 C75 2.121(12) . ? Ir3 C71 2.131(10) . ? Ir3 C70 2.173(11) . ? P1 F4 1.563(8) . ? P1 F6 1.587(7) . ? P1 F1 1.589(7) . ? P1 F2 1.590(8) . ? P1 F3 1.603(7) . ? P1 F5 1.603(7) . ? P2 F10 1.583(6) . ? P2 F8 1.584(6) . ? P2 F7 1.585(6) . ? P2 F11 1.585(6) . ? P2 F12 1.585(6) . ? P2 F9 1.585(6) . ? N1 C1 1.342(12) . ? N1 C4 1.385(10) . ? N1 C2 1.428(16) . ? N2 C3 1.374(14) . ? N2 C1 1.399(13) . ? N2 C16 1.477(15) . ? N3 C17 1.274(13) . ? N3 N3 1.430(15) 2_656 ? N4 C27 1.367(12) . ? N4 C28 1.396(14) . ? N4 C38 1.433(14) . ? N5 C29 1.346(13) . ? N5 C27 1.360(12) . ? N5 C30 1.444(13) . ? N6 N7 1.347(11) . ? N6 C31 1.364(12) . ? N7 C33 1.342(12) . ? N8 C37 1.325(12) . ? N8 C35 1.338(13) . ? N8 C34 1.499(13) . ? N9 C37 1.372(12) . ? N9 C36 1.378(13) . ? N9 C50 1.467(13) . ? C2 C3 1.319(19) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 C10 1.559(16) . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 H7 0.9500 . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C13 1.520(13) . ? C10 C12 1.495(19) . ? C10 C11 1.506(18) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13 C14 1.57(2) . ? C13 C15 1.57(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16 C17 1.452(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.426(15) . ? C18 C17 1.426(15) 2_656 ? C18 H18A 0.9500 . ? C19 C20 1.345(19) . ? C19 C26 1.570(18) . ? C19 H19A 1.0000 . ? C20 C21 1.552(18) . ? C20 H20A 1.0000 . ? C21 C22 1.60(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.479(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.396(17) . ? C23 H23A 1.0000 . ? C24 C25 1.527(17) . ? C24 H24A 1.0000 . ? C25 C26 1.51(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C28 C29 1.334(17) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.477(15) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.431(14) . ? C32 C33 1.398(15) . ? C32 H32A 0.9500 . ? C33 C34 1.467(14) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.331(16) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C38 C43 1.357(15) . ? C38 C39 1.431(17) . ? C39 C44 1.43(2) . ? C39 C40 1.48(2) . ? C40 C41 1.29(2) . ? C40 H40A 0.9500 . ? C41 C42 1.38(2) . ? C41 H41A 0.9500 . ? C42 C43 1.382(16) . ? C42 H42A 0.9500 . ? C43 C47 1.535(15) . ? C44 C45 1.632(18) . ? C44 C46 1.65(2) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47 C49 1.488(17) . ? C47 C48 1.552(18) . ? C47 H47A 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.370(15) . ? C50 C51 1.407(15) . ? C51 C52 1.387(15) . ? C51 C56 1.491(17) . ? C52 C53 1.40(2) . ? C52 H52A 0.9500 . ? C53 C54 1.348(19) . ? C53 H53A 0.9500 . ? C54 C55 1.434(16) . ? C54 H54A 0.9500 . ? C55 C59 1.506(15) . ? C56 C57 1.512(17) . ? C56 C58 1.59(2) . ? C56 H56A 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.533(18) . ? C59 C61 1.59(2) . ? C59 H59A 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.388(18) . ? C62 C69 1.489(19) . ? C62 H62A 1.0000 . ? C63 C64 1.493(16) . ? C63 H63A 1.0000 . ? C64 C65 1.345(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.565(17) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.350(18) . ? C66 H66A 1.0000 . ? C67 C68 1.592(18) . ? C67 H67A 1.0000 . ? C68 C69 1.35(2) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.346(18) . ? C70 C77 1.482(17) . ? C70 H70A 1.0000 . ? C71 C72 1.48(2) . ? C71 H71A 1.0000 . ? C72 C73 1.34(3) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.58(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.38(2) . ? C74 H74A 1.0000 . ? C75 C76 1.543(19) . ? C75 H75A 1.0000 . ? C76 C77 1.43(2) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? 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 84.8(3) . . ? C1 Ir1 C19 94.4(4) . . ? N3 Ir1 C19 166.6(4) . . ? C1 Ir1 C20 93.1(4) . . ? N3 Ir1 C20 156.7(5) . . ? C19 Ir1 C20 36.7(5) . . ? C1 Ir1 C23 149.6(5) . . ? N3 Ir1 C23 87.7(4) . . ? C19 Ir1 C23 99.3(5) . . ? C20 Ir1 C23 82.4(5) . . ? C1 Ir1 C24 172.7(5) . . ? N3 Ir1 C24 95.8(3) . . ? C19 Ir1 C24 83.2(4) . . ? C20 Ir1 C24 89.2(4) . . ? C23 Ir1 C24 37.7(5) . . ? C27 Ir2 N6 86.8(3) . . ? C27 Ir2 C67 150.3(5) . . ? N6 Ir2 C67 88.8(4) . . ? C27 Ir2 C62 90.7(4) . . ? N6 Ir2 C62 157.6(4) . . ? C67 Ir2 C62 82.3(5) . . ? C27 Ir2 C63 96.8(4) . . ? N6 Ir2 C63 164.1(4) . . ? C67 Ir2 C63 95.4(5) . . ? C62 Ir2 C63 38.3(5) . . ? C27 Ir2 C66 172.7(5) . . ? N6 Ir2 C66 93.3(3) . . ? C67 Ir2 C66 36.9(5) . . ? C62 Ir2 C66 91.9(5) . . ? C63 Ir2 C66 81.1(4) . . ? C37 Ir3 C74 93.6(4) . . ? C37 Ir3 N7 84.6(3) . . ? C74 Ir3 N7 155.4(5) . . ? C37 Ir3 C75 98.4(4) . . ? C74 Ir3 C75 38.1(6) . . ? N7 Ir3 C75 166.3(4) . . ? C37 Ir3 C71 153.4(4) . . ? C74 Ir3 C71 79.8(5) . . ? N7 Ir3 C71 90.9(4) . . ? C75 Ir3 C71 92.2(5) . . ? C37 Ir3 C70 170.1(4) . . ? C74 Ir3 C70 90.4(4) . . ? N7 Ir3 C70 95.5(4) . . ? C75 Ir3 C70 79.2(4) . . ? C71 Ir3 C70 36.4(5) . . ? F4 P1 F6 90.0(5) . . ? F4 P1 F1 88.6(5) . . ? F6 P1 F1 88.5(4) . . ? F4 P1 F2 176.6(6) . . ? F6 P1 F2 87.9(5) . . ? F1 P1 F2 94.0(6) . . ? F4 P1 F3 90.0(5) . . ? F6 P1 F3 91.2(4) . . ? F1 P1 F3 178.6(5) . . ? F2 P1 F3 87.4(5) . . ? F4 P1 F5 92.4(5) . . ? F6 P1 F5 177.6(5) . . ? F1 P1 F5 91.9(4) . . ? F2 P1 F5 89.7(5) . . ? F3 P1 F5 88.4(4) . . ? F10 P2 F8 179.9(3) . . ? F10 P2 F7 90.0(2) . . ? F8 P2 F7 90.0(2) . . ? F10 P2 F11 90.0(2) . . ? F8 P2 F11 90.0(2) . . ? F7 P2 F11 179.9(3) . . ? F10 P2 F12 90.0(2) . . ? F8 P2 F12 90.1(2) . . ? F7 P2 F12 90.0(2) . . ? F11 P2 F12 90.0(2) . . ? F10 P2 F9 90.0(2) . . ? F8 P2 F9 90.0(2) . . ? F7 P2 F9 90.0(2) . . ? F11 P2 F9 90.0(2) . . ? F12 P2 F9 179.9(3) . . ? C1 N1 C4 129.1(8) . . ? C1 N1 C2 108.6(9) . . ? C4 N1 C2 122.0(8) . . ? C3 N2 C1 111.8(9) . . ? C3 N2 C16 126.7(10) . . ? C1 N2 C16 121.5(9) . . ? C17 N3 N3 108.1(6) . 2_656 ? C17 N3 Ir1 120.1(7) . . ? N3 N3 Ir1 130.3(3) 2_656 . ? C27 N4 C28 110.0(9) . . ? C27 N4 C38 127.5(8) . . ? C28 N4 C38 122.4(9) . . ? C29 N5 C27 112.9(8) . . ? C29 N5 C30 123.6(9) . . ? C27 N5 C30 122.9(8) . . ? N7 N6 C31 108.2(7) . . ? N7 N6 Ir2 131.2(5) . . ? C31 N6 Ir2 117.9(6) . . ? C33 N7 N6 108.9(8) . . ? C33 N7 Ir3 118.3(7) . . ? N6 N7 Ir3 128.1(6) . . ? C37 N8 C35 114.6(8) . . ? C37 N8 C34 121.7(8) . . ? C35 N8 C34 123.7(9) . . ? C37 N9 C36 108.4(8) . . ? C37 N9 C50 129.6(8) . . ? C36 N9 C50 121.9(9) . . ? N1 C1 N2 104.4(8) . . ? N1 C1 Ir1 137.7(8) . . ? N2 C1 Ir1 117.9(7) . . ? C3 C2 N1 109.4(10) . . ? C3 C2 H2A 125.3 . . ? N1 C2 H2A 125.3 . . ? C2 C3 N2 105.7(10) . . ? C2 C3 H3A 127.2 . . ? N2 C3 H3A 127.2 . . ? N1 C4 C5 118.7(6) . . ? N1 C4 C9 121.2(6) . . ? C5 C4 C9 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C10 121.5(7) . . ? C6 C5 C10 118.4(7) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 C13 118.9(6) . . ? C4 C9 C13 121.1(6) . . ? C12 C10 C11 109.2(17) . . ? C12 C10 C5 110.4(13) . . ? C11 C10 C5 112.5(16) . . ? C12 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C5 C10 H10 108.2 . . ? 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 . . ? H11D C11' H11E 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? H12D C12' H12E 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C9 C13 C14 113(4) . . ? C9 C13 C15 129(3) . . ? C14 C13 C15 111(3) . . ? C9 C13 H13 99.1 . . ? C14 C13 H13 99.1 . . ? C15 C13 H13 99.1 . . ? 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 . . ? H14D C14' H14E 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? H15D C15' H15E 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C17 C16 N2 111.2(12) . . ? C17 C16 H16A 109.4 . . ? N2 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? N2 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N3 C17 C18 110.7(10) . . ? N3 C17 C16 123.4(11) . . ? C18 C17 C16 125.9(11) . . ? C17 C18 C17 102.4(13) . 2_656 ? C17 C18 H18A 128.8 . . ? C17 C18 H18A 128.8 2_656 . ? C20 C19 C26 120.4(13) . . ? C20 C19 Ir1 71.7(7) . . ? C26 C19 Ir1 108.5(8) . . ? C20 C19 H19A 115.9 . . ? C26 C19 H19A 115.9 . . ? Ir1 C19 H19A 115.9 . . ? C19 C20 C21 126.4(13) . . ? C19 C20 Ir1 71.6(6) . . ? C21 C20 Ir1 113.3(9) . . ? C19 C20 H20A 112.9 . . ? C21 C20 H20A 112.9 . . ? Ir1 C20 H20A 112.9 . . ? C20 C21 C22 110.3(11) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 113.4(12) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 124.4(14) . . ? C24 C23 Ir1 72.6(6) . . ? C22 C23 Ir1 110.7(8) . . ? C24 C23 H23A 113.9 . . ? C22 C23 H23A 113.9 . . ? Ir1 C23 H23A 113.9 . . ? C23 C24 C25 125.0(12) . . ? C23 C24 Ir1 69.8(6) . . ? C25 C24 Ir1 111.8(8) . . ? C23 C24 H24A 114.0 . . ? C25 C24 H24A 114.0 . . ? Ir1 C24 H24A 114.0 . . ? C26 C25 C24 113.7(10) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C19 115.1(12) . . ? C25 C26 H26A 108.5 . . ? C19 C26 H26A 108.5 . . ? C25 C26 H26B 108.5 . . ? C19 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? N5 C27 N4 103.1(8) . . ? N5 C27 Ir2 119.4(6) . . ? N4 C27 Ir2 137.4(7) . . ? C29 C28 N4 107.1(10) . . ? C29 C28 H28A 126.5 . . ? N4 C28 H28A 126.5 . . ? C28 C29 N5 106.8(9) . . ? C28 C29 H29A 126.6 . . ? N5 C29 H29A 126.6 . . ? N5 C30 C31 111.7(9) . . ? N5 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N5 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? N6 C31 C32 109.2(8) . . ? N6 C31 C30 122.8(9) . . ? C32 C31 C30 127.4(9) . . ? C33 C32 C31 102.6(8) . . ? C33 C32 H32A 128.7 . . ? C31 C32 H32A 128.7 . . ? N7 C33 C32 110.8(9) . . ? N7 C33 C34 123.0(10) . . ? C32 C33 C34 126.3(9) . . ? C33 C34 N8 113.0(8) . . ? C33 C34 H34A 109.0 . . ? N8 C34 H34A 109.0 . . ? C33 C34 H34B 109.0 . . ? N8 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C36 C35 N8 104.8(9) . . ? C36 C35 H35A 127.6 . . ? N8 C35 H35A 127.6 . . ? C35 C36 N9 108.8(9) . . ? C35 C36 H36A 125.6 . . ? N9 C36 H36A 125.6 . . ? N8 C37 N9 103.4(8) . . ? N8 C37 Ir3 121.7(7) . . ? N9 C37 Ir3 134.9(7) . . ? C43 C38 C39 121.8(11) . . ? C43 C38 N4 119.0(10) . . ? C39 C38 N4 118.5(11) . . ? C44 C39 C38 123.7(14) . . ? C44 C39 C40 125.0(14) . . ? C38 C39 C40 110.7(12) . . ? C41 C40 C39 126.1(14) . . ? C41 C40 H40A 117.0 . . ? C39 C40 H40A 117.0 . . ? C40 C41 C42 119.5(13) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C41 C42 C43 119.3(13) . . ? C41 C42 H42A 120.3 . . ? C43 C42 H42A 120.3 . . ? C38 C43 C42 121.6(11) . . ? C38 C43 C47 123.0(10) . . ? C42 C43 C47 114.7(10) . . ? C39 C44 C45 121.5(18) . . ? C39 C44 C46 109(2) . . ? C45 C44 C46 113.7(15) . . ? C39 C44 H44 103.5 . . ? C45 C44 H44 103.5 . . ? C46 C44 H44 103.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? H45D C45' H45E 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? H46D C46' H46E 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C49 C47 C43 116.3(11) . . ? C49 C47 C48 112.5(10) . . ? C43 C47 C48 105.9(9) . . ? C49 C47 H47A 107.3 . . ? C43 C47 H47A 107.3 . . ? C48 C47 H47A 107.3 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 124.8(10) . . ? C55 C50 N9 118.6(10) . . ? C51 C50 N9 116.6(9) . . ? C52 C51 C50 116.8(11) . . ? C52 C51 C56 120.0(10) . . ? C50 C51 C56 123.2(9) . . ? C51 C52 C53 119.5(12) . . ? C51 C52 H52A 120.3 . . ? C53 C52 H52A 120.3 . . ? C54 C53 C52 122.8(12) . . ? C54 C53 H53A 118.6 . . ? C52 C53 H53A 118.6 . . ? C53 C54 C55 119.6(12) . . ? C53 C54 H54A 120.2 . . ? C55 C54 H54A 120.2 . . ? C50 C55 C54 116.5(10) . . ? C50 C55 C59 124.1(10) . . ? C54 C55 C59 119.5(11) . . ? C51 C56 C57 113.7(12) . . ? C51 C56 C58 114.5(10) . . ? C57 C56 C58 105.7(10) . . ? C51 C56 H56A 107.5 . . ? C57 C56 H56A 107.5 . . ? C58 C56 H56A 107.5 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 C59 C60 114.1(12) . . ? C55 C59 C61 109.0(10) . . ? C60 C59 C61 112.6(12) . . ? C55 C59 H59A 106.9 . . ? C60 C59 H59A 106.9 . . ? C61 C59 H59A 106.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 C69 126.4(13) . . ? C63 C62 Ir2 71.3(7) . . ? C69 C62 Ir2 111.6(9) . . ? C63 C62 H62A 113.3 . . ? C69 C62 H62A 113.3 . . ? Ir2 C62 H62A 113.3 . . ? C62 C63 C64 122.1(12) . . ? C62 C63 Ir2 70.4(7) . . ? C64 C63 Ir2 111.5(8) . . ? C62 C63 H63A 115.0 . . ? C64 C63 H63A 115.0 . . ? Ir2 C63 H63A 115.0 . . ? C65 C64 C63 119.4(11) . . ? C65 C64 H64A 107.5 . . ? C63 C64 H64A 107.5 . . ? C65 C64 H64B 107.5 . . ? C63 C64 H64B 107.5 . . ? H64A C64 H64B 107.0 . . ? C64 C65 C66 116.8(11) . . ? C64 C65 H65A 108.1 . . ? C66 C65 H65A 108.1 . . ? C64 C65 H65B 108.1 . . ? C66 C65 H65B 108.1 . . ? H65A C65 H65B 107.3 . . ? C67 C66 C65 127.3(12) . . ? C67 C66 Ir2 68.7(6) . . ? C65 C66 Ir2 108.9(8) . . ? C67 C66 H66A 114.0 . . ? C65 C66 H66A 114.0 . . ? Ir2 C66 H66A 114.0 . . ? C66 C67 C68 123.4(12) . . ? C66 C67 Ir2 74.4(7) . . ? C68 C67 Ir2 107.7(9) . . ? C66 C67 H67A 114.6 . . ? C68 C67 H67A 114.6 . . ? Ir2 C67 H67A 114.6 . . ? C69 C68 C67 117.0(12) . . ? C69 C68 H68A 108.1 . . ? C67 C68 H68A 108.1 . . ? C69 C68 H68B 108.1 . . ? C67 C68 H68B 108.1 . . ? H68A C68 H68B 107.3 . . ? C68 C69 C62 117.4(11) . . ? C68 C69 H69A 107.9 . . ? C62 C69 H69A 107.9 . . ? C68 C69 H69B 107.9 . . ? C62 C69 H69B 107.9 . . ? H69A C69 H69B 107.2 . . ? C71 C70 C77 118.3(12) . . ? C71 C70 Ir3 70.1(7) . . ? C77 C70 Ir3 112.2(8) . . ? C71 C70 H70A 116.0 . . ? C77 C70 H70A 116.0 . . ? Ir3 C70 H70A 116.0 . . ? C70 C71 C72 130.0(16) . . ? C70 C71 Ir3 73.5(7) . . ? C72 C71 Ir3 111.3(10) . . ? C70 C71 H71A 111.7 . . ? C72 C71 H71A 111.7 . . ? Ir3 C71 H71A 111.7 . . ? C73 C72 C71 113.1(16) . . ? C73 C72 H72A 109.0 . . ? C71 C72 H72A 109.0 . . ? C73 C72 H72B 109.0 . . ? C71 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? C72 C73 C74 116.9(13) . . ? C72 C73 H73A 108.1 . . ? C74 C73 H73A 108.1 . . ? C72 C73 H73B 108.1 . . ? C74 C73 H73B 108.1 . . ? H73A C73 H73B 107.3 . . ? C75 C74 C73 118.6(12) . . ? C75 C74 Ir3 71.3(7) . . ? C73 C74 Ir3 109.4(9) . . ? C75 C74 H74A 116.4 . . ? C73 C74 H74A 116.4 . . ? Ir3 C74 H74A 116.4 . . ? C74 C75 C76 128.2(13) . . ? C74 C75 Ir3 70.5(7) . . ? C76 C75 Ir3 112.4(9) . . ? C74 C75 H75A 112.6 . . ? C76 C75 H75A 112.6 . . ? Ir3 C75 H75A 112.6 . . ? C77 C76 C75 110.6(12) . . ? C77 C76 H76A 109.5 . . ? C75 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 108.1 . . ? C76 C77 C70 116.8(11) . . ? C76 C77 H77A 108.1 . . ? C70 C77 H77A 108.1 . . ? C76 C77 H77B 108.1 . . ? C70 C77 H77B 108.1 . . ? H77A C77 H77B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 N3 C17 46.1(8) . . . . ? C19 Ir1 N3 C17 133.5(17) . . . . ? C20 Ir1 N3 C17 -39.6(13) . . . . ? C23 Ir1 N3 C17 -104.4(8) . . . . ? C24 Ir1 N3 C17 -141.3(8) . . . . ? C1 Ir1 N3 N3 -149.6(10) . . . 2_656 ? C19 Ir1 N3 N3 -62(2) . . . 2_656 ? C20 Ir1 N3 N3 124.7(11) . . . 2_656 ? C23 Ir1 N3 N3 59.9(10) . . . 2_656 ? C24 Ir1 N3 N3 23.1(10) . . . 2_656 ? C27 Ir2 N6 N7 157.4(9) . . . . ? C67 Ir2 N6 N7 -51.9(9) . . . . ? C62 Ir2 N6 N7 -118.5(12) . . . . ? C63 Ir2 N6 N7 53.8(18) . . . . ? C66 Ir2 N6 N7 -15.2(9) . . . . ? C27 Ir2 N6 C31 -43.8(7) . . . . ? C67 Ir2 N6 C31 106.8(8) . . . . ? C62 Ir2 N6 C31 40.3(15) . . . . ? C63 Ir2 N6 C31 -147.4(12) . . . . ? C66 Ir2 N6 C31 143.5(8) . . . . ? C31 N6 N7 C33 1.5(11) . . . . ? Ir2 N6 N7 C33 161.8(8) . . . . ? C31 N6 N7 Ir3 156.4(6) . . . . ? Ir2 N6 N7 Ir3 -43.3(11) . . . . ? C37 Ir3 N7 C33 -47.8(8) . . . . ? C74 Ir3 N7 C33 39.1(13) . . . . ? C75 Ir3 N7 C33 -151.2(16) . . . . ? C71 Ir3 N7 C33 106.0(8) . . . . ? C70 Ir3 N7 C33 142.2(8) . . . . ? C37 Ir3 N7 N6 159.4(7) . . . . ? C74 Ir3 N7 N6 -113.7(10) . . . . ? C75 Ir3 N7 N6 56.0(19) . . . . ? C71 Ir3 N7 N6 -46.8(8) . . . . ? C70 Ir3 N7 N6 -10.6(8) . . . . ? C4 N1 C1 N2 -176.0(9) . . . . ? C2 N1 C1 N2 -2.0(11) . . . . ? C4 N1 C1 Ir1 6.5(17) . . . . ? C2 N1 C1 Ir1 -179.5(9) . . . . ? C3 N2 C1 N1 -0.3(12) . . . . ? C16 N2 C1 N1 -177.9(10) . . . . ? C3 N2 C1 Ir1 177.8(7) . . . . ? C16 N2 C1 Ir1 0.2(15) . . . . ? N3 Ir1 C1 N1 137.4(11) . . . . ? C19 Ir1 C1 N1 -29.2(12) . . . . ? C20 Ir1 C1 N1 -65.9(12) . . . . ? C23 Ir1 C1 N1 -146.2(11) . . . . ? C24 Ir1 C1 N1 42(4) . . . . ? N3 Ir1 C1 N2 -39.9(8) . . . . ? C19 Ir1 C1 N2 153.5(9) . . . . ? C20 Ir1 C1 N2 116.8(9) . . . . ? C23 Ir1 C1 N2 36.5(13) . . . . ? C24 Ir1 C1 N2 -135(3) . . . . ? C1 N1 C2 C3 3.8(13) . . . . ? C4 N1 C2 C3 178.3(10) . . . . ? N1 C2 C3 N2 -3.8(13) . . . . ? C1 N2 C3 C2 2.6(14) . . . . ? C16 N2 C3 C2 -180.0(12) . . . . ? C1 N1 C4 C5 -80.0(11) . . . . ? C2 N1 C4 C5 106.7(9) . . . . ? C1 N1 C4 C9 97.2(11) . . . . ? C2 N1 C4 C9 -76.1(11) . . . . ? N1 C4 C5 C6 177.2(8) . . . . ? C9 C4 C5 C6 0.0 . . . . ? N1 C4 C5 C10 -6.5(11) . . . . ? C9 C4 C5 C10 176.4(10) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C10 C5 C6 C7 -176.5(10) . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C4 0.0 . . . . ? C7 C8 C9 C13 -179.6(9) . . . . ? N1 C4 C9 C8 -177.1(9) . . . . ? C5 C4 C9 C8 0.0 . . . . ? N1 C4 C9 C13 2.4(10) . . . . ? C5 C4 C9 C13 179.5(9) . . . . ? C4 C5 C10 C12 -78.9(15) . . . . ? C6 C5 C10 C12 97.6(14) . . . . ? C4 C5 C10 C11 158.9(12) . . . . ? C6 C5 C10 C11 -24.7(15) . . . . ? C8 C9 C13 C14 68(4) . . . . ? C4 C9 C13 C14 -112(4) . . . . ? C8 C9 C13 C15 -79(5) . . . . ? C4 C9 C13 C15 102(5) . . . . ? C3 N2 C16 C17 -123.8(13) . . . . ? C1 N2 C16 C17 53.4(17) . . . . ? N3 N3 C17 C18 1.0(12) 2_656 . . . ? Ir1 N3 C17 C18 168.5(5) . . . . ? N3 N3 C17 C16 -175.7(11) 2_656 . . . ? Ir1 N3 C17 C16 -8.2(15) . . . . ? N2 C16 C17 N3 -49.3(18) . . . . ? N2 C16 C17 C18 134.5(11) . . . . ? N3 C17 C18 C17 -0.4(5) . . . 2_656 ? C16 C17 C18 C17 176.2(15) . . . 2_656 ? C1 Ir1 C19 C20 -89.2(7) . . . . ? N3 Ir1 C19 C20 -175.4(14) . . . . ? C23 Ir1 C19 C20 63.6(8) . . . . ? C24 Ir1 C19 C20 97.8(8) . . . . ? C1 Ir1 C19 C26 154.0(10) . . . . ? N3 Ir1 C19 C26 68(2) . . . . ? C20 Ir1 C19 C26 -116.8(13) . . . . ? C23 Ir1 C19 C26 -53.2(11) . . . . ? C24 Ir1 C19 C26 -19.0(10) . . . . ? C26 C19 C20 C21 -4.6(19) . . . . ? Ir1 C19 C20 C21 -105.8(13) . . . . ? C26 C19 C20 Ir1 101.2(11) . . . . ? C1 Ir1 C20 C19 93.3(8) . . . . ? N3 Ir1 C20 C19 177.3(8) . . . . ? C23 Ir1 C20 C19 -116.9(8) . . . . ? C24 Ir1 C20 C19 -79.7(8) . . . . ? C1 Ir1 C20 C21 -144.2(13) . . . . ? N3 Ir1 C20 C21 -60.2(16) . . . . ? C19 Ir1 C20 C21 122.5(15) . . . . ? C23 Ir1 C20 C21 5.6(12) . . . . ? C24 Ir1 C20 C21 42.8(13) . . . . ? C19 C20 C21 C22 95(2) . . . . ? Ir1 C20 C21 C22 10.9(19) . . . . ? C20 C21 C22 C23 -30(2) . . . . ? C21 C22 C23 C24 -47.6(19) . . . . ? C21 C22 C23 Ir1 35.0(19) . . . . ? C1 Ir1 C23 C24 -178.3(7) . . . . ? N3 Ir1 C23 C24 -102.6(6) . . . . ? C19 Ir1 C23 C24 65.9(7) . . . . ? C20 Ir1 C23 C24 98.6(7) . . . . ? C1 Ir1 C23 C22 60.7(17) . . . . ? N3 Ir1 C23 C22 136.4(13) . . . . ? C19 Ir1 C23 C22 -55.1(13) . . . . ? C20 Ir1 C23 C22 -22.4(13) . . . . ? C24 Ir1 C23 C22 -121.0(15) . . . . ? C22 C23 C24 C25 0.5(18) . . . . ? Ir1 C23 C24 C25 -103.0(11) . . . . ? C22 C23 C24 Ir1 103.5(11) . . . . ? C1 Ir1 C24 C23 173(3) . . . . ? N3 Ir1 C24 C23 78.6(7) . . . . ? C19 Ir1 C24 C23 -114.9(8) . . . . ? C20 Ir1 C24 C23 -78.6(8) . . . . ? C1 Ir1 C24 C25 -66(3) . . . . ? N3 Ir1 C24 C25 -160.7(10) . . . . ? C19 Ir1 C24 C25 5.9(10) . . . . ? C20 Ir1 C24 C25 42.2(11) . . . . ? C23 Ir1 C24 C25 120.8(13) . . . . ? C23 C24 C25 C26 89.7(18) . . . . ? Ir1 C24 C25 C26 9.7(17) . . . . ? C24 C25 C26 C19 -27(2) . . . . ? C20 C19 C26 C25 -48.5(18) . . . . ? Ir1 C19 C26 C25 30.8(16) . . . . ? C29 N5 C27 N4 -3.4(11) . . . . ? C30 N5 C27 N4 -174.7(9) . . . . ? C29 N5 C27 Ir2 179.3(7) . . . . ? C30 N5 C27 Ir2 7.9(12) . . . . ? C28 N4 C27 N5 1.8(11) . . . . ? C38 N4 C27 N5 178.7(10) . . . . ? C28 N4 C27 Ir2 178.4(8) . . . . ? C38 N4 C27 Ir2 -4.7(17) . . . . ? N6 Ir2 C27 N5 35.1(7) . . . . ? C67 Ir2 C27 N5 -46.9(12) . . . . ? C62 Ir2 C27 N5 -122.6(8) . . . . ? C63 Ir2 C27 N5 -160.5(7) . . . . ? C66 Ir2 C27 N5 126(3) . . . . ? N6 Ir2 C27 N4 -141.1(10) . . . . ? C67 Ir2 C27 N4 136.9(11) . . . . ? C62 Ir2 C27 N4 61.3(11) . . . . ? C63 Ir2 C27 N4 23.3(11) . . . . ? C66 Ir2 C27 N4 -50(3) . . . . ? C27 N4 C28 C29 0.4(13) . . . . ? C38 N4 C28 C29 -176.8(10) . . . . ? N4 C28 C29 N5 -2.4(13) . . . . ? C27 N5 C29 C28 3.7(13) . . . . ? C30 N5 C29 C28 175.0(10) . . . . ? C29 N5 C30 C31 132.4(10) . . . . ? C27 N5 C30 C31 -57.2(13) . . . . ? N7 N6 C31 C32 2.3(11) . . . . ? Ir2 N6 C31 C32 -161.0(7) . . . . ? N7 N6 C31 C30 174.2(9) . . . . ? Ir2 N6 C31 C30 10.9(13) . . . . ? N5 C30 C31 N6 45.5(13) . . . . ? N5 C30 C31 C32 -144.2(10) . . . . ? N6 C31 C32 C33 -5.0(11) . . . . ? C30 C31 C32 C33 -176.4(10) . . . . ? N6 N7 C33 C32 -5.0(12) . . . . ? Ir3 N7 C33 C32 -162.6(7) . . . . ? N6 N7 C33 C34 174.2(10) . . . . ? Ir3 N7 C33 C34 16.5(14) . . . . ? C31 C32 C33 N7 6.0(12) . . . . ? C31 C32 C33 C34 -173.1(11) . . . . ? N7 C33 C34 N8 39.9(15) . . . . ? C32 C33 C34 N8 -141.1(11) . . . . ? C37 N8 C34 C33 -51.8(13) . . . . ? C35 N8 C34 C33 129.3(11) . . . . ? C37 N8 C35 C36 0.2(13) . . . . ? C34 N8 C35 C36 179.2(9) . . . . ? N8 C35 C36 N9 -1.6(12) . . . . ? C37 N9 C36 C35 2.4(12) . . . . ? C50 N9 C36 C35 -174.1(10) . . . . ? C35 N8 C37 N9 1.2(11) . . . . ? C34 N8 C37 N9 -177.8(8) . . . . ? C35 N8 C37 Ir3 -178.6(7) . . . . ? C34 N8 C37 Ir3 2.5(12) . . . . ? C36 N9 C37 N8 -2.1(10) . . . . ? C50 N9 C37 N8 174.0(10) . . . . ? C36 N9 C37 Ir3 177.6(8) . . . . ? C50 N9 C37 Ir3 -6.3(15) . . . . ? C74 Ir3 C37 N8 -117.0(9) . . . . ? N7 Ir3 C37 N8 38.3(7) . . . . ? C75 Ir3 C37 N8 -155.1(8) . . . . ? C71 Ir3 C37 N8 -42.7(13) . . . . ? C70 Ir3 C37 N8 130(2) . . . . ? C74 Ir3 C37 N9 63.3(10) . . . . ? N7 Ir3 C37 N9 -141.4(9) . . . . ? C75 Ir3 C37 N9 25.2(10) . . . . ? C71 Ir3 C37 N9 137.6(11) . . . . ? C70 Ir3 C37 N9 -50(3) . . . . ? C27 N4 C38 C43 -102.5(12) . . . . ? C28 N4 C38 C43 74.1(14) . . . . ? C27 N4 C38 C39 86.7(14) . . . . ? C28 N4 C38 C39 -96.7(13) . . . . ? C43 C38 C39 C44 -177.5(12) . . . . ? N4 C38 C39 C44 -7.0(18) . . . . ? C43 C38 C39 C40 11.0(16) . . . . ? N4 C38 C39 C40 -178.5(10) . . . . ? C44 C39 C40 C41 -178.5(16) . . . . ? C38 C39 C40 C41 -7(2) . . . . ? C39 C40 C41 C42 3(3) . . . . ? C40 C41 C42 C43 -3(2) . . . . ? C39 C38 C43 C42 -12.0(17) . . . . ? N4 C38 C43 C42 177.6(10) . . . . ? C39 C38 C43 C47 177.7(11) . . . . ? N4 C38 C43 C47 7.3(15) . . . . ? C41 C42 C43 C38 7.3(18) . . . . ? C41 C42 C43 C47 178.4(12) . . . . ? C38 C39 C44 C45 -147.8(15) . . . . ? C40 C39 C44 C45 23(2) . . . . ? C38 C39 C44 C46 77(3) . . . . ? C40 C39 C44 C46 -112(2) . . . . ? C38 C43 C47 C49 127.4(12) . . . . ? C42 C43 C47 C49 -43.5(15) . . . . ? C38 C43 C47 C48 -106.9(11) . . . . ? C42 C43 C47 C48 82.2(12) . . . . ? C37 N9 C50 C55 84.3(13) . . . . ? C36 N9 C50 C55 -100.1(12) . . . . ? C37 N9 C50 C51 -98.0(12) . . . . ? C36 N9 C50 C51 77.7(13) . . . . ? C55 C50 C51 C52 -2.3(16) . . . . ? N9 C50 C51 C52 -179.9(9) . . . . ? C55 C50 C51 C56 177.2(10) . . . . ? N9 C50 C51 C56 -0.4(15) . . . . ? C50 C51 C52 C53 0.4(16) . . . . ? C56 C51 C52 C53 -179.1(11) . . . . ? C51 C52 C53 C54 1(2) . . . . ? C52 C53 C54 C55 -1(2) . . . . ? C51 C50 C55 C54 2.6(16) . . . . ? N9 C50 C55 C54 -179.8(10) . . . . ? C51 C50 C55 C59 -176.7(11) . . . . ? N9 C50 C55 C59 0.9(16) . . . . ? C53 C54 C55 C50 -1.0(17) . . . . ? C53 C54 C55 C59 178.3(12) . . . . ? C52 C51 C56 C57 73.4(14) . . . . ? C50 C51 C56 C57 -106.1(13) . . . . ? C52 C51 C56 C58 -48.3(16) . . . . ? C50 C51 C56 C58 132.2(12) . . . . ? C50 C55 C59 C60 -148.2(12) . . . . ? C54 C55 C59 C60 32.6(16) . . . . ? C50 C55 C59 C61 84.9(13) . . . . ? C54 C55 C59 C61 -94.3(13) . . . . ? C27 Ir2 C62 C63 -100.1(7) . . . . ? N6 Ir2 C62 C63 176.6(8) . . . . ? C67 Ir2 C62 C63 108.8(8) . . . . ? C66 Ir2 C62 C63 73.1(8) . . . . ? C27 Ir2 C62 C69 137.2(11) . . . . ? N6 Ir2 C62 C69 53.9(17) . . . . ? C67 Ir2 C62 C69 -13.8(11) . . . . ? C63 Ir2 C62 C69 -122.7(14) . . . . ? C66 Ir2 C62 C69 -49.6(11) . . . . ? C69 C62 C63 C64 0(2) . . . . ? Ir2 C62 C63 C64 -103.6(11) . . . . ? C69 C62 C63 Ir2 103.4(13) . . . . ? C27 Ir2 C63 C62 82.5(8) . . . . ? N6 Ir2 C63 C62 -175.2(12) . . . . ? C67 Ir2 C63 C62 -70.4(8) . . . . ? C66 Ir2 C63 C62 -104.6(8) . . . . ? C27 Ir2 C63 C64 -159.8(10) . . . . ? N6 Ir2 C63 C64 -57.5(19) . . . . ? C67 Ir2 C63 C64 47.3(11) . . . . ? C62 Ir2 C63 C64 117.7(14) . . . . ? C66 Ir2 C63 C64 13.1(10) . . . . ? C62 C63 C64 C65 68(2) . . . . ? Ir2 C63 C64 C65 -12(2) . . . . ? C63 C64 C65 C66 1(3) . . . . ? C64 C65 C66 C67 -67(2) . . . . ? C64 C65 C66 Ir2 10(2) . . . . ? C27 Ir2 C66 C67 -175(3) . . . . ? N6 Ir2 C66 C67 -83.6(7) . . . . ? C62 Ir2 C66 C67 74.6(8) . . . . ? C63 Ir2 C66 C67 111.4(8) . . . . ? C27 Ir2 C66 C65 62(3) . . . . ? N6 Ir2 C66 C65 152.8(11) . . . . ? C67 Ir2 C66 C65 -123.6(14) . . . . ? C62 Ir2 C66 C65 -49.1(12) . . . . ? C63 Ir2 C66 C65 -12.2(11) . . . . ? C65 C66 C67 C68 -3(2) . . . . ? Ir2 C66 C67 C68 -101.1(12) . . . . ? C65 C66 C67 Ir2 98.1(13) . . . . ? C27 Ir2 C67 C66 178.6(7) . . . . ? N6 Ir2 C67 C66 97.1(7) . . . . ? C62 Ir2 C67 C66 -103.6(8) . . . . ? C63 Ir2 C67 C66 -67.5(7) . . . . ? C27 Ir2 C67 C68 -60.7(14) . . . . ? N6 Ir2 C67 C68 -142.2(10) . . . . ? C62 Ir2 C67 C68 17.2(10) . . . . ? C63 Ir2 C67 C68 53.2(11) . . . . ? C66 Ir2 C67 C68 120.7(13) . . . . ? C66 C67 C68 C69 63(2) . . . . ? Ir2 C67 C68 C69 -20(2) . . . . ? C67 C68 C69 C62 9(3) . . . . ? C63 C62 C69 C68 -76(2) . . . . ? Ir2 C62 C69 C68 6(2) . . . . ? C37 Ir3 C70 C71 -174(2) . . . . ? C74 Ir3 C70 C71 72.1(8) . . . . ? N7 Ir3 C70 C71 -83.9(7) . . . . ? C75 Ir3 C70 C71 108.8(8) . . . . ? C37 Ir3 C70 C77 72(3) . . . . ? C74 Ir3 C70 C77 -41.2(11) . . . . ? N7 Ir3 C70 C77 162.7(11) . . . . ? C75 Ir3 C70 C77 -4.5(11) . . . . ? C71 Ir3 C70 C77 -113.3(14) . . . . ? C77 C70 C71 C72 1(2) . . . . ? Ir3 C70 C71 C72 -104.2(14) . . . . ? C77 C70 C71 Ir3 105.2(10) . . . . ? C37 Ir3 C71 C70 177.8(8) . . . . ? C74 Ir3 C71 C70 -104.7(8) . . . . ? N7 Ir3 C71 C70 98.2(7) . . . . ? C75 Ir3 C71 C70 -68.5(8) . . . . ? C37 Ir3 C71 C72 -55.1(18) . . . . ? C74 Ir3 C71 C72 22.4(14) . . . . ? N7 Ir3 C71 C72 -134.7(14) . . . . ? C75 Ir3 C71 C72 58.6(15) . . . . ? C70 Ir3 C71 C72 127.1(17) . . . . ? C70 C71 C72 C73 51(3) . . . . ? Ir3 C71 C72 C73 -35(2) . . . . ? C71 C72 C73 C74 29(3) . . . . ? C72 C73 C74 C75 -88(2) . . . . ? C72 C73 C74 Ir3 -10(2) . . . . ? C37 Ir3 C74 C75 -99.0(7) . . . . ? N7 Ir3 C74 C75 176.1(8) . . . . ? C71 Ir3 C74 C75 106.9(8) . . . . ? C70 Ir3 C74 C75 71.9(8) . . . . ? C37 Ir3 C74 C73 146.4(11) . . . . ? N7 Ir3 C74 C73 61.4(15) . . . . ? C75 Ir3 C74 C73 -114.6(13) . . . . ? C71 Ir3 C74 C73 -7.7(12) . . . . ? C70 Ir3 C74 C73 -42.7(12) . . . . ? C73 C74 C75 C76 -1(2) . . . . ? Ir3 C74 C75 C76 -103.7(13) . . . . ? C73 C74 C75 Ir3 102.4(12) . . . . ? C37 Ir3 C75 C74 85.1(7) . . . . ? N7 Ir3 C75 C74 -173.0(14) . . . . ? C71 Ir3 C75 C74 -70.4(8) . . . . ? C70 Ir3 C75 C74 -104.7(8) . . . . ? C37 Ir3 C75 C76 -150.6(11) . . . . ? C74 Ir3 C75 C76 124.3(14) . . . . ? N7 Ir3 C75 C76 -49(2) . . . . ? C71 Ir3 C75 C76 53.9(12) . . . . ? C70 Ir3 C75 C76 19.6(11) . . . . ? C74 C75 C76 C77 50(2) . . . . ? Ir3 C75 C76 C77 -32.3(18) . . . . ? C75 C76 C77 C70 29(2) . . . . ? C71 C70 C77 C76 -91.6(18) . . . . ? Ir3 C70 C77 C76 -13(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.350 _refine_diff_density_min -1.661 _refine_diff_density_rms 0.160 data_07006a _database_code_depnum_ccdc_archive 'CCDC 648820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 07006a _chemical_melting_point ? _chemical_formula_moiety 'C70 H86 N12 Ni2, 2(C4 H8 O), 2(F6 P)' _chemical_formula_sum 'C78 H102 F12 N12 Ni2 O2 P2' _chemical_formula_weight 1647.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8499(18) _cell_length_b 17.6914(15) _cell_length_c 23.633(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.251(1) _cell_angle_gamma 90.00 _cell_volume 7948.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2961 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.46 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7753 _exptl_absorpt_correction_T_max 0.9539 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details 'S-J. Jeon / Prof. R. Waymouth - Stanford Univ.' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 37711 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9020 _reflns_number_gt 7198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0705P)^2^+13.4573P] 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 9020 _refine_ls_number_parameters 495 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.090 _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 Ni1 Ni 0.565173(14) 0.763056(16) 0.215154(13) 0.01961(9) Uani 1 1 d . . . N1 N 0.63178(10) 0.65019(12) 0.17043(10) 0.0275(4) Uani 1 1 d . . . N2 N 0.52974(10) 0.68168(11) 0.10136(9) 0.0263(4) Uani 1 1 d . . . N3 N 0.46627(10) 0.74973(10) 0.17600(9) 0.0214(4) Uani 1 1 d . . . N4 N 0.42050(9) 0.77440(10) 0.20053(9) 0.0211(4) Uani 1 1 d . . . N5 N 0.30811(10) 0.84635(11) 0.21961(9) 0.0248(4) Uani 1 1 d . . . N6 N 0.36030(10) 0.88165(11) 0.31486(9) 0.0273(4) Uani 1 1 d . . . C1 C 0.69001(12) 0.64005(13) 0.23093(12) 0.0285(5) Uani 1 1 d . . . C2 C 0.67635(13) 0.60405(14) 0.27764(12) 0.0299(5) Uani 1 1 d . . . C3 C 0.73158(14) 0.59884(15) 0.33651(13) 0.0357(6) Uani 1 1 d . . . H3A H 0.7235 0.5768 0.3696 0.043 Uiso 1 1 calc R . . C4 C 0.79767(14) 0.62540(16) 0.34700(14) 0.0394(6) Uani 1 1 d . . . H4B H 0.8344 0.6224 0.3875 0.047 Uiso 1 1 calc R . . C5 C 0.81110(14) 0.65619(16) 0.29951(14) 0.0392(6) Uani 1 1 d . . . H5A H 0.8575 0.6719 0.3072 0.047 Uiso 1 1 calc R . . C6 C 0.75753(13) 0.66464(14) 0.24011(13) 0.0326(5) Uani 1 1 d . . . C7 C 0.57842(12) 0.70134(13) 0.15760(11) 0.0238(5) Uani 1 1 d . . . C8 C 0.61486(14) 0.59960(15) 0.12113(13) 0.0362(6) Uani 1 1 d . . . H8A H 0.6431 0.5588 0.1184 0.043 Uiso 1 1 calc R . . C9 C 0.55161(14) 0.61919(15) 0.07848(12) 0.0342(6) Uani 1 1 d . . . H9A H 0.5264 0.5949 0.0398 0.041 Uiso 1 1 calc R . . C10 C 0.46303(13) 0.72202(14) 0.07064(11) 0.0278(5) Uani 1 1 d . . . H10A H 0.4301 0.6901 0.0368 0.033 Uiso 1 1 calc R . . H10B H 0.4713 0.7689 0.0518 0.033 Uiso 1 1 calc R . . C11 C 0.42967(12) 0.74217(13) 0.11417(11) 0.0236(5) Uani 1 1 d . . . C12 C 0.35975(12) 0.76119(14) 0.09795(11) 0.0264(5) Uani 1 1 d . . . H12A H 0.3224 0.7607 0.0577 0.032 Uiso 1 1 calc R . . C13 C 0.35633(11) 0.78091(13) 0.15326(11) 0.0233(5) Uani 1 1 d . . . C14 C 0.29176(12) 0.80273(14) 0.16250(11) 0.0265(5) Uani 1 1 d . . . H14A H 0.2606 0.8331 0.1265 0.032 Uiso 1 1 calc R . . H14B H 0.2659 0.7564 0.1640 0.032 Uiso 1 1 calc R . . C15 C 0.36082(12) 0.82765(13) 0.27381(11) 0.0236(5) Uani 1 1 d . . . C16 C 0.27393(13) 0.91081(15) 0.22542(13) 0.0329(6) Uani 1 1 d . . . H16A H 0.2349 0.9347 0.1936 0.040 Uiso 1 1 calc R . . C17 C 0.30650(14) 0.93314(15) 0.28467(13) 0.0359(6) Uani 1 1 d . . . H17A H 0.2950 0.9761 0.3027 0.043 Uiso 1 1 calc R . . C18 C 0.41368(13) 0.89049(14) 0.37824(12) 0.0302(5) Uani 1 1 d . . . C19 C 0.47853(14) 0.92295(14) 0.38678(12) 0.0324(5) Uani 1 1 d . . . C20 C 0.52914(15) 0.92897(16) 0.44778(13) 0.0409(6) Uani 1 1 d . . . H20A H 0.5741 0.9492 0.4554 0.049 Uiso 1 1 calc R . . C21 C 0.51476(17) 0.90589(18) 0.49728(14) 0.0465(7) Uani 1 1 d . . . H21A H 0.5501 0.9099 0.5384 0.056 Uiso 1 1 calc R . . C22 C 0.45030(17) 0.87739(17) 0.48765(13) 0.0444(7) Uani 1 1 d . . . H22A H 0.4411 0.8630 0.5223 0.053 Uiso 1 1 calc R . . C23 C 0.39759(15) 0.86890(15) 0.42792(12) 0.0347(6) Uani 1 1 d . . . C24 C 0.60673(13) 0.56584(15) 0.26516(13) 0.0330(5) Uani 1 1 d . . . H24A H 0.5685 0.5953 0.2324 0.040 Uiso 1 1 calc R . . C25 C 0.59005(16) 0.56126(17) 0.32206(14) 0.0416(6) Uani 1 1 d . . . H25A H 0.5930 0.6118 0.3398 0.062 Uiso 1 1 calc R . . H25B H 0.6240 0.5278 0.3530 0.062 Uiso 1 1 calc R . . H25C H 0.5424 0.5412 0.3100 0.062 Uiso 1 1 calc R . . C26 C 0.60743(18) 0.48589(18) 0.24036(17) 0.0507(8) Uani 1 1 d . . . H26A H 0.6135 0.4889 0.2015 0.076 Uiso 1 1 calc R . . H26B H 0.5628 0.4606 0.2328 0.076 Uiso 1 1 calc R . . H26C H 0.6464 0.4570 0.2710 0.076 Uiso 1 1 calc R . . C27 C 0.77419(14) 0.69575(16) 0.18818(14) 0.0390(6) Uani 1 1 d . . . H27A H 0.7288 0.7104 0.1534 0.047 Uiso 1 1 calc R . . C28 C 0.82090(17) 0.76629(19) 0.20779(18) 0.0523(8) Uani 1 1 d . . . H28A H 0.8255 0.7880 0.1715 0.078 Uiso 1 1 calc R . . H28B H 0.8675 0.7523 0.2390 0.078 Uiso 1 1 calc R . . H28C H 0.7995 0.8036 0.2254 0.078 Uiso 1 1 calc R . . C29 C 0.80873(18) 0.6343(2) 0.16381(17) 0.0539(8) Uani 1 1 d . . . H29A H 0.7777 0.5901 0.1506 0.081 Uiso 1 1 calc R . . H29B H 0.8539 0.6195 0.1969 0.081 Uiso 1 1 calc R . . H29C H 0.8166 0.6541 0.1285 0.081 Uiso 1 1 calc R . . C30 C 0.49291(13) 0.95668(15) 0.33399(13) 0.0340(6) Uani 1 1 d . . . H30A H 0.4686 0.9249 0.2962 0.041 Uiso 1 1 calc R . . C31 C 0.46143(17) 1.03679(17) 0.32023(16) 0.0472(7) Uani 1 1 d . . . H31A H 0.4699 1.0587 0.2858 0.071 Uiso 1 1 calc R . . H31B H 0.4837 1.0685 0.3572 0.071 Uiso 1 1 calc R . . H31C H 0.4107 1.0342 0.3089 0.071 Uiso 1 1 calc R . . C32 C 0.57085(15) 0.96015(16) 0.34735(16) 0.0427(7) Uani 1 1 d . . . H32A H 0.5762 0.9736 0.3093 0.064 Uiso 1 1 calc R . . H32B H 0.5925 0.9107 0.3620 0.064 Uiso 1 1 calc R . . H32C H 0.5940 0.9983 0.3793 0.064 Uiso 1 1 calc R . . C33 C 0.32523(16) 0.84114(17) 0.41943(14) 0.0410(6) Uani 1 1 d . . . H33A H 0.2990 0.8262 0.3750 0.049 Uiso 1 1 calc R . . C34 C 0.3284(2) 0.7724(2) 0.45965(17) 0.0566(9) Uani 1 1 d . . . H34A H 0.3553 0.7320 0.4510 0.085 Uiso 1 1 calc R . . H34B H 0.2805 0.7546 0.4501 0.085 Uiso 1 1 calc R . . H34C H 0.3514 0.7866 0.5036 0.085 Uiso 1 1 calc R . . C35 C 0.2845(2) 0.9059(2) 0.4333(2) 0.0628(10) Uani 1 1 d . . . H35A H 0.2805 0.9485 0.4056 0.094 Uiso 1 1 calc R . . H35B H 0.3098 0.9222 0.4765 0.094 Uiso 1 1 calc R . . H35C H 0.2374 0.8883 0.4267 0.094 Uiso 1 1 calc R . . P1 P 0.67813(4) 0.45375(4) 0.02208(3) 0.04034(19) Uani 1 1 d . . . F1 F 0.6458(2) 0.44650(16) 0.07140(17) 0.1393(16) Uani 1 1 d . . . F2 F 0.75221(19) 0.45894(16) 0.07784(14) 0.1381(16) Uani 1 1 d . . . F3 F 0.68458(11) 0.36365(10) 0.02397(9) 0.0612(6) Uani 1 1 d . . . F4 F 0.67152(14) 0.54315(11) 0.02115(11) 0.0747(7) Uani 1 1 d . . . F5 F 0.60386(12) 0.44621(14) -0.03352(13) 0.0904(9) Uani 1 1 d . . . F6 F 0.71252(16) 0.45926(15) -0.02489(14) 0.0909(8) Uani 1 1 d . . . O1 O 0.47687(18) 0.7653(2) 0.87197(17) 0.0924(10) Uani 1 1 d D . . C37 C 0.5297(2) 0.7439(3) 0.8510(2) 0.0850(14) Uani 1 1 d D . . H37A H 0.5728 0.7742 0.8732 0.102 Uiso 1 1 calc R . . H37B H 0.5128 0.7546 0.8061 0.102 Uiso 1 1 calc R . . C38 C 0.5460(3) 0.6651(3) 0.8620(3) 0.115(2) Uani 1 1 d D . . H38A H 0.5975 0.6572 0.8831 0.138 Uiso 1 1 calc R . . H38B H 0.5277 0.6365 0.8225 0.138 Uiso 1 1 calc R . . C39 C 0.5101(4) 0.6398(3) 0.9032(3) 0.112(2) Uani 1 1 d D . . H39A H 0.4839 0.5921 0.8875 0.135 Uiso 1 1 calc R . . H39B H 0.5452 0.6316 0.9463 0.135 Uiso 1 1 calc R . . C40 C 0.4627(3) 0.6998(3) 0.9011(3) 0.1061(19) Uani 1 1 d D . . H40A H 0.4687 0.7127 0.9438 0.127 Uiso 1 1 calc R . . H40B H 0.4135 0.6832 0.8774 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01945(15) 0.01930(15) 0.02059(16) -0.00281(11) 0.00872(11) -0.00275(10) N1 0.0274(10) 0.0283(10) 0.0299(11) -0.0063(8) 0.0147(9) -0.0010(8) N2 0.0282(10) 0.0281(10) 0.0245(10) -0.0062(8) 0.0126(8) -0.0038(8) N3 0.0211(9) 0.0213(9) 0.0216(9) -0.0003(7) 0.0085(8) -0.0021(7) N4 0.0194(9) 0.0223(9) 0.0212(9) 0.0005(7) 0.0081(7) -0.0002(7) N5 0.0210(9) 0.0245(10) 0.0277(10) 0.0023(8) 0.0088(8) 0.0032(7) N6 0.0270(10) 0.0263(10) 0.0283(10) -0.0012(8) 0.0110(8) 0.0049(8) C1 0.0263(11) 0.0243(11) 0.0350(13) -0.0056(10) 0.0127(10) 0.0038(9) C2 0.0291(12) 0.0247(12) 0.0365(14) -0.0028(10) 0.0142(11) 0.0052(9) C3 0.0373(14) 0.0286(13) 0.0379(14) -0.0001(11) 0.0122(12) 0.0088(11) C4 0.0308(13) 0.0359(14) 0.0410(15) -0.0018(12) 0.0042(12) 0.0095(11) C5 0.0245(12) 0.0335(14) 0.0559(18) -0.0056(13) 0.0126(12) 0.0035(10) C6 0.0277(12) 0.0265(12) 0.0455(15) -0.0050(11) 0.0171(11) 0.0030(10) C7 0.0245(11) 0.0237(11) 0.0264(11) -0.0006(9) 0.0135(9) -0.0033(9) C8 0.0388(14) 0.0342(14) 0.0399(15) -0.0128(11) 0.0204(12) 0.0004(11) C9 0.0395(14) 0.0357(14) 0.0316(13) -0.0135(11) 0.0190(11) -0.0052(11) C10 0.0289(12) 0.0323(13) 0.0215(11) -0.0030(9) 0.0097(9) -0.0028(10) C11 0.0250(11) 0.0242(11) 0.0205(11) -0.0009(9) 0.0081(9) -0.0048(9) C12 0.0220(11) 0.0299(12) 0.0225(11) -0.0002(9) 0.0044(9) -0.0037(9) C13 0.0206(10) 0.0213(10) 0.0250(11) 0.0016(9) 0.0065(9) -0.0015(8) C14 0.0201(10) 0.0283(12) 0.0272(12) -0.0002(9) 0.0058(9) 0.0003(9) C15 0.0227(10) 0.0221(11) 0.0273(12) 0.0011(9) 0.0118(9) 0.0009(8) C16 0.0277(12) 0.0307(13) 0.0380(14) 0.0043(11) 0.0111(11) 0.0113(10) C17 0.0328(13) 0.0318(13) 0.0425(15) 0.0003(11) 0.0149(12) 0.0128(11) C18 0.0327(12) 0.0261(12) 0.0297(13) -0.0047(10) 0.0109(10) 0.0084(10) C19 0.0330(13) 0.0258(12) 0.0350(14) -0.0058(10) 0.0105(11) 0.0066(10) C20 0.0369(14) 0.0388(15) 0.0395(15) -0.0107(12) 0.0080(12) 0.0035(12) C21 0.0475(17) 0.0501(18) 0.0307(14) -0.0095(13) 0.0048(13) 0.0112(14) C22 0.0585(19) 0.0447(16) 0.0302(14) -0.0015(12) 0.0184(13) 0.0136(14) C23 0.0417(14) 0.0298(13) 0.0334(14) -0.0024(11) 0.0163(12) 0.0085(11) C24 0.0297(12) 0.0326(13) 0.0385(14) 0.0018(11) 0.0157(11) 0.0034(10) C25 0.0454(16) 0.0373(15) 0.0489(17) 0.0042(13) 0.0264(14) 0.0055(12) C26 0.0518(18) 0.0391(16) 0.069(2) -0.0163(15) 0.0323(17) -0.0098(14) C27 0.0292(13) 0.0398(15) 0.0512(17) 0.0016(13) 0.0197(12) 0.0033(11) C28 0.0408(16) 0.0476(18) 0.072(2) 0.0017(16) 0.0263(16) -0.0069(14) C29 0.0549(19) 0.057(2) 0.062(2) -0.0066(16) 0.0363(17) 0.0055(16) C30 0.0316(13) 0.0314(13) 0.0372(14) -0.0049(11) 0.0125(11) 0.0029(10) C31 0.0500(17) 0.0375(16) 0.0567(19) 0.0082(14) 0.0246(15) 0.0133(13) C32 0.0370(14) 0.0340(14) 0.0576(19) -0.0072(13) 0.0201(14) -0.0012(12) C33 0.0489(16) 0.0416(15) 0.0391(15) -0.0006(12) 0.0247(13) 0.0040(13) C34 0.071(2) 0.057(2) 0.049(2) 0.0063(16) 0.0329(18) -0.0018(17) C35 0.060(2) 0.062(2) 0.079(3) -0.0025(19) 0.041(2) 0.0132(18) P1 0.0575(5) 0.0341(4) 0.0287(4) -0.0034(3) 0.0169(3) -0.0028(3) F1 0.293(5) 0.0640(17) 0.158(3) -0.0065(17) 0.191(4) -0.003(2) F2 0.156(3) 0.0702(17) 0.0849(19) 0.0133(14) -0.0550(19) -0.0497(18) F3 0.0680(13) 0.0368(10) 0.0539(12) -0.0057(8) -0.0003(10) 0.0009(9) F4 0.118(2) 0.0331(10) 0.0804(16) 0.0006(10) 0.0489(15) -0.0003(11) F5 0.0519(13) 0.0654(15) 0.115(2) 0.0277(14) -0.0046(13) -0.0034(11) F6 0.112(2) 0.0874(18) 0.112(2) -0.0113(15) 0.0848(18) -0.0143(15) O1 0.084(2) 0.102(3) 0.104(3) 0.031(2) 0.052(2) 0.0188(18) C37 0.070(3) 0.123(4) 0.073(3) 0.009(3) 0.040(2) -0.005(3) C38 0.131(5) 0.070(3) 0.177(6) -0.019(4) 0.097(5) -0.016(3) C39 0.165(6) 0.077(3) 0.084(4) -0.001(3) 0.041(4) -0.021(4) C40 0.101(4) 0.127(5) 0.125(5) 0.047(4) 0.083(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C15 1.851(2) 2_655 ? Ni1 C7 1.851(2) . ? Ni1 N3 1.8966(19) . ? Ni1 N4 1.9000(19) 2_655 ? N1 C7 1.368(3) . ? N1 C8 1.395(3) . ? N1 C1 1.458(3) . ? N2 C7 1.345(3) . ? N2 C9 1.387(3) . ? N2 C10 1.463(3) . ? N3 C11 1.349(3) . ? N3 N4 1.375(3) . ? N4 C13 1.350(3) . ? N4 Ni1 1.9000(19) 2_655 ? N5 C15 1.342(3) . ? N5 C16 1.381(3) . ? N5 C14 1.468(3) . ? N6 C15 1.365(3) . ? N6 C17 1.393(3) . ? N6 C18 1.462(3) . ? C1 C2 1.401(4) . ? C1 C6 1.403(3) . ? C2 C3 1.398(4) . ? C2 C24 1.516(3) . ? C3 C4 1.378(4) . ? C3 H3A 0.9500 . ? C4 C5 1.376(4) . ? C4 H4B 0.9500 . ? C5 C6 1.397(4) . ? C5 H5A 0.9500 . ? C6 C27 1.510(4) . ? C8 C9 1.335(4) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.502(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.388(3) . ? C12 C13 1.383(3) . ? C12 H12A 0.9500 . ? C13 C14 1.500(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 Ni1 1.851(2) 2_655 ? C16 C17 1.340(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C23 1.400(4) . ? C18 C19 1.405(4) . ? C19 C20 1.398(4) . ? C19 C30 1.520(4) . ? C20 C21 1.383(4) . ? C20 H20A 0.9500 . ? C21 C22 1.364(5) . ? C21 H21A 0.9500 . ? C22 C23 1.396(4) . ? C22 H22A 0.9500 . ? C23 C33 1.520(4) . ? C24 C25 1.523(4) . ? C24 C26 1.533(4) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.533(4) . ? C27 C29 1.541(4) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.524(4) . ? C30 C31 1.539(4) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.527(4) . ? C33 C35 1.539(4) . ? C33 H33A 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? P1 F6 1.552(2) . ? P1 F2 1.568(3) . ? P1 F5 1.572(2) . ? P1 F1 1.574(3) . ? P1 F4 1.587(2) . ? P1 F3 1.599(2) . ? O1 C37 1.432(4) . ? O1 C40 1.438(4) . ? C37 C38 1.435(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.520(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.438(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 C15 Ni1 C7 95.75(10) 2_655 . ? C15 Ni1 N3 145.30(9) 2_655 . ? C7 Ni1 N3 91.65(9) . . ? C15 Ni1 N4 91.38(9) 2_655 2_655 ? C7 Ni1 N4 145.70(9) . 2_655 ? N3 Ni1 N4 101.30(8) . 2_655 ? C7 N1 C8 109.6(2) . . ? C7 N1 C1 124.94(19) . . ? C8 N1 C1 124.3(2) . . ? C7 N2 C9 110.8(2) . . ? C7 N2 C10 122.8(2) . . ? C9 N2 C10 126.4(2) . . ? C11 N3 N4 107.84(18) . . ? C11 N3 Ni1 123.97(16) . . ? N4 N3 Ni1 123.95(14) . . ? C13 N4 N3 107.54(18) . . ? C13 N4 Ni1 123.52(15) . 2_655 ? N3 N4 Ni1 124.81(14) . 2_655 ? C15 N5 C16 111.2(2) . . ? C15 N5 C14 122.53(19) . . ? C16 N5 C14 126.2(2) . . ? C15 N6 C17 109.5(2) . . ? C15 N6 C18 125.33(19) . . ? C17 N6 C18 124.7(2) . . ? C2 C1 C6 122.3(2) . . ? C2 C1 N1 118.2(2) . . ? C6 C1 N1 119.5(2) . . ? C3 C2 C1 117.6(2) . . ? C3 C2 C24 119.7(2) . . ? C1 C2 C24 122.5(2) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4B 119.6 . . ? C3 C4 H4B 119.6 . . ? C4 C5 C6 121.0(2) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 117.4(3) . . ? C5 C6 C27 120.0(2) . . ? C1 C6 C27 122.6(2) . . ? N2 C7 N1 105.2(2) . . ? N2 C7 Ni1 126.78(17) . . ? N1 C7 Ni1 125.49(17) . . ? C9 C8 N1 107.2(2) . . ? C9 C8 H8A 126.4 . . ? N1 C8 H8A 126.4 . . ? C8 C9 N2 107.1(2) . . ? C8 C9 H9A 126.5 . . ? N2 C9 H9A 126.5 . . ? N2 C10 C11 112.90(19) . . ? N2 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N3 C11 C12 109.7(2) . . ? N3 C11 C10 123.4(2) . . ? C12 C11 C10 126.7(2) . . ? C13 C12 C11 104.8(2) . . ? C13 C12 H12A 127.6 . . ? C11 C12 H12A 127.6 . . ? N4 C13 C12 110.0(2) . . ? N4 C13 C14 123.0(2) . . ? C12 C13 C14 126.9(2) . . ? N5 C14 C13 112.68(18) . . ? N5 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? N5 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N5 C15 N6 105.28(19) . . ? N5 C15 Ni1 126.52(17) . 2_655 ? N6 C15 Ni1 125.57(17) . 2_655 ? C17 C16 N5 106.6(2) . . ? C17 C16 H16A 126.7 . . ? N5 C16 H16A 126.7 . . ? C16 C17 N6 107.4(2) . . ? C16 C17 H17A 126.3 . . ? N6 C17 H17A 126.3 . . ? C23 C18 C19 122.6(2) . . ? C23 C18 N6 119.1(2) . . ? C19 C18 N6 118.3(2) . . ? C20 C19 C18 117.0(3) . . ? C20 C19 C30 119.8(3) . . ? C18 C19 C30 123.0(2) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 121.4(3) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C18 117.3(3) . . ? C22 C23 C33 119.7(3) . . ? C18 C23 C33 123.0(2) . . ? C2 C24 C25 113.5(2) . . ? C2 C24 C26 109.1(2) . . ? C25 C24 C26 109.2(2) . . ? C2 C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? C26 C24 H24A 108.3 . . ? 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 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C6 C27 C28 112.4(3) . . ? C6 C27 C29 110.2(2) . . ? C28 C27 C29 110.6(2) . . ? C6 C27 H27A 107.8 . . ? C28 C27 H27A 107.8 . . ? C29 C27 H27A 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C19 C30 C32 113.5(2) . . ? C19 C30 C31 108.9(2) . . ? C32 C30 C31 109.4(2) . . ? C19 C30 H30A 108.3 . . ? C32 C30 H30A 108.3 . . ? C31 C30 H30A 108.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C23 C33 C34 112.8(3) . . ? C23 C33 C35 109.6(3) . . ? C34 C33 C35 110.3(3) . . ? C23 C33 H33A 108.0 . . ? C34 C33 H33A 108.0 . . ? C35 C33 H33A 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? F6 P1 F2 90.7(2) . . ? F6 P1 F5 89.62(17) . . ? F2 P1 F5 178.47(14) . . ? F6 P1 F1 177.9(2) . . ? F2 P1 F1 87.5(2) . . ? F5 P1 F1 92.1(2) . . ? F6 P1 F4 89.45(14) . . ? F2 P1 F4 90.18(15) . . ? F5 P1 F4 91.32(14) . . ? F1 P1 F4 91.73(14) . . ? F6 P1 F3 91.39(14) . . ? F2 P1 F3 89.57(13) . . ? F5 P1 F3 88.94(12) . . ? F1 P1 F3 87.41(14) . . ? F4 P1 F3 179.12(13) . . ? C37 O1 C40 107.0(4) . . ? O1 C37 C38 110.6(3) . . ? O1 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? O1 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 105.1(3) . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38B 110.7 . . ? C39 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C40 C39 C38 105.8(3) . . ? C40 C39 H39A 110.6 . . ? C38 C39 H39A 110.6 . . ? C40 C39 H39B 110.6 . . ? C38 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? C39 C40 O1 109.8(3) . . ? C39 C40 H40A 109.7 . . ? O1 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? O1 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? 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 C15 Ni1 N3 C11 67.9(2) 2_655 . . . ? C7 Ni1 N3 C11 -34.68(19) . . . . ? N4 Ni1 N3 C11 177.27(17) 2_655 . . . ? C15 Ni1 N3 N4 -86.1(2) 2_655 . . . ? C7 Ni1 N3 N4 171.29(17) . . . . ? N4 Ni1 N3 N4 23.24(15) 2_655 . . . ? C11 N3 N4 C13 0.5(2) . . . . ? Ni1 N3 N4 C13 158.11(15) . . . . ? C11 N3 N4 Ni1 158.26(15) . . . 2_655 ? Ni1 N3 N4 Ni1 -44.2(2) . . . 2_655 ? C7 N1 C1 C2 73.5(3) . . . . ? C8 N1 C1 C2 -92.9(3) . . . . ? C7 N1 C1 C6 -108.0(3) . . . . ? C8 N1 C1 C6 85.6(3) . . . . ? C6 C1 C2 C3 5.4(4) . . . . ? N1 C1 C2 C3 -176.1(2) . . . . ? C6 C1 C2 C24 -169.6(2) . . . . ? N1 C1 C2 C24 8.9(3) . . . . ? C1 C2 C3 C4 -2.8(4) . . . . ? C24 C2 C3 C4 172.4(2) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C3 C4 C5 C6 3.0(4) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C4 C5 C6 C27 -177.6(2) . . . . ? C2 C1 C6 C5 -3.9(4) . . . . ? N1 C1 C6 C5 177.7(2) . . . . ? C2 C1 C6 C27 173.2(2) . . . . ? N1 C1 C6 C27 -5.2(4) . . . . ? C9 N2 C7 N1 -0.2(3) . . . . ? C10 N2 C7 N1 179.1(2) . . . . ? C9 N2 C7 Ni1 -162.88(18) . . . . ? C10 N2 C7 Ni1 16.4(3) . . . . ? C8 N1 C7 N2 0.3(3) . . . . ? C1 N1 C7 N2 -167.9(2) . . . . ? C8 N1 C7 Ni1 163.25(18) . . . . ? C1 N1 C7 Ni1 -4.9(3) . . . . ? C15 Ni1 C7 N2 -127.6(2) 2_655 . . . ? N3 Ni1 C7 N2 18.5(2) . . . . ? N4 Ni1 C7 N2 131.4(2) 2_655 . . . ? C15 Ni1 C7 N1 73.1(2) 2_655 . . . ? N3 Ni1 C7 N1 -140.9(2) . . . . ? N4 Ni1 C7 N1 -27.9(3) 2_655 . . . ? C7 N1 C8 C9 -0.2(3) . . . . ? C1 N1 C8 C9 168.0(2) . . . . ? N1 C8 C9 N2 0.1(3) . . . . ? C7 N2 C9 C8 0.0(3) . . . . ? C10 N2 C9 C8 -179.2(2) . . . . ? C7 N2 C10 C11 -42.0(3) . . . . ? C9 N2 C10 C11 137.2(2) . . . . ? N4 N3 C11 C12 -0.5(2) . . . . ? Ni1 N3 C11 C12 -158.08(16) . . . . ? N4 N3 C11 C10 175.1(2) . . . . ? Ni1 N3 C11 C10 17.5(3) . . . . ? N2 C10 C11 N3 24.0(3) . . . . ? N2 C10 C11 C12 -161.2(2) . . . . ? N3 C11 C12 C13 0.3(3) . . . . ? C10 C11 C12 C13 -175.1(2) . . . . ? N3 N4 C13 C12 -0.4(2) . . . . ? Ni1 N4 C13 C12 -158.45(16) 2_655 . . . ? N3 N4 C13 C14 176.7(2) . . . . ? Ni1 N4 C13 C14 18.7(3) 2_655 . . . ? C11 C12 C13 N4 0.1(3) . . . . ? C11 C12 C13 C14 -176.9(2) . . . . ? C15 N5 C14 C13 -43.6(3) . . . . ? C16 N5 C14 C13 135.4(2) . . . . ? N4 C13 C14 N5 24.7(3) . . . . ? C12 C13 C14 N5 -158.7(2) . . . . ? C16 N5 C15 N6 -0.3(3) . . . . ? C14 N5 C15 N6 178.8(2) . . . . ? C16 N5 C15 Ni1 -162.60(18) . . . 2_655 ? C14 N5 C15 Ni1 16.5(3) . . . 2_655 ? C17 N6 C15 N5 0.0(3) . . . . ? C18 N6 C15 N5 -172.0(2) . . . . ? C17 N6 C15 Ni1 162.56(18) . . . 2_655 ? C18 N6 C15 Ni1 -9.5(3) . . . 2_655 ? C15 N5 C16 C17 0.4(3) . . . . ? C14 N5 C16 C17 -178.6(2) . . . . ? N5 C16 C17 N6 -0.4(3) . . . . ? C15 N6 C17 C16 0.2(3) . . . . ? C18 N6 C17 C16 172.3(2) . . . . ? C15 N6 C18 C23 -106.2(3) . . . . ? C17 N6 C18 C23 82.9(3) . . . . ? C15 N6 C18 C19 76.0(3) . . . . ? C17 N6 C18 C19 -94.9(3) . . . . ? C23 C18 C19 C20 3.8(4) . . . . ? N6 C18 C19 C20 -178.5(2) . . . . ? C23 C18 C19 C30 -171.1(2) . . . . ? N6 C18 C19 C30 6.6(3) . . . . ? C18 C19 C20 C21 -1.9(4) . . . . ? C30 C19 C20 C21 173.2(3) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 1.5(5) . . . . ? C21 C22 C23 C18 0.3(4) . . . . ? C21 C22 C23 C33 -176.5(3) . . . . ? C19 C18 C23 C22 -3.0(4) . . . . ? N6 C18 C23 C22 179.2(2) . . . . ? C19 C18 C23 C33 173.7(2) . . . . ? N6 C18 C23 C33 -4.1(4) . . . . ? C3 C2 C24 C25 30.4(3) . . . . ? C1 C2 C24 C25 -154.7(2) . . . . ? C3 C2 C24 C26 -91.7(3) . . . . ? C1 C2 C24 C26 83.2(3) . . . . ? C5 C6 C27 C28 -46.3(3) . . . . ? C1 C6 C27 C28 136.7(3) . . . . ? C5 C6 C27 C29 77.5(3) . . . . ? C1 C6 C27 C29 -99.5(3) . . . . ? C20 C19 C30 C32 27.8(3) . . . . ? C18 C19 C30 C32 -157.4(2) . . . . ? C20 C19 C30 C31 -94.4(3) . . . . ? C18 C19 C30 C31 80.4(3) . . . . ? C22 C23 C33 C34 -46.6(4) . . . . ? C18 C23 C33 C34 136.8(3) . . . . ? C22 C23 C33 C35 76.7(3) . . . . ? C18 C23 C33 C35 -99.9(3) . . . . ? C40 O1 C37 C38 4.2(7) . . . . ? O1 C37 C38 C39 -10.8(7) . . . . ? C37 C38 C39 C40 13.2(7) . . . . ? C38 C39 C40 O1 -11.2(7) . . . . ? C37 O1 C40 C39 4.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.259 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.072 # Attachment '5-Rh2.cif' data_07066s _database_code_depnum_ccdc_archive 'CCDC 648821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 07066s _chemical_melting_point ? _chemical_formula_moiety 'C51 H67 N6 Rh2, F6 P' _chemical_formula_sum 'C51 H67 F6 N6 P Rh2' _chemical_formula_weight 1114.90 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' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 30.849(4) _cell_length_b 18.153(2) _cell_length_c 16.475(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.222(2) _cell_angle_gamma 90.00 _cell_volume 9219.1(19) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3958 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7486 _exptl_absorpt_correction_T_max 0.7911 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45510 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.04 _reflns_number_total 16350 _reflns_number_gt 15285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The function SQUEEZE, in the program PLATON (A. L. Spek, Acta. Cryst. A46, C34 (1990)) was used to model solvent accessible void space. A void space of 2332.0 angstroms^3^, containing 773 electrons per cell, was found. ; _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^)+(0.0591P)^2^+20.5158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 7886 Friedel Pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_number_reflns 16350 _refine_ls_number_parameters 959 _refine_ls_number_restraints 347 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.048 _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 Rh1 Rh 0.457471(11) 0.20401(2) 0.59773(2) 0.03240(9) Uani 1 1 d . . . Rh2 Rh 0.192238(11) 0.16964(2) 0.76204(2) 0.03096(9) Uani 1 1 d . . . Rh3 Rh 0.154936(12) 0.28981(2) 0.96667(2) 0.03326(9) Uani 1 1 d . . . P1 P 0.46154(4) 0.59731(7) 0.64836(8) 0.0385(3) Uani 1 1 d . . . F1 F 0.48519(16) 0.6412(3) 0.7204(3) 0.1049(18) Uani 1 1 d . . . F2 F 0.48274(18) 0.6459(2) 0.5825(3) 0.1060(18) Uani 1 1 d . . . F3 F 0.43600(13) 0.5494(2) 0.5807(2) 0.0710(11) Uani 1 1 d . . . F4 F 0.43839(16) 0.5471(2) 0.7136(3) 0.0830(12) Uani 1 1 d . . . F5 F 0.50094(11) 0.5415(2) 0.6431(3) 0.0731(11) Uani 1 1 d . . . F6 F 0.42280(13) 0.6531(2) 0.6527(2) 0.0719(11) Uani 1 1 d . . . P2 P 0.5025(2) 0.47051(12) 0.9933(4) 0.0445(10) Uani 0.458(13) 1 d PD A -1 F7 F 0.5257(3) 0.4708(4) 0.9098(5) 0.0699(16) Uani 0.458(13) 1 d PD A -1 F8 F 0.5428(3) 0.5109(6) 1.0349(6) 0.081(5) Uani 0.458(13) 1 d PD A -1 F9 F 0.4814(4) 0.5476(3) 0.9718(7) 0.086(4) Uani 0.458(13) 1 d PD A -1 F10 F 0.4620(3) 0.4307(6) 0.9515(5) 0.100(6) Uani 0.458(13) 1 d PD A -1 F11 F 0.5232(4) 0.3933(4) 1.0143(5) 0.084(4) Uani 0.458(13) 1 d PD A -1 F12 F 0.4792(3) 0.4705(5) 1.0766(5) 0.0699(16) Uani 0.458(13) 1 d PD A -1 P2' P 0.5025(2) 0.47051(12) 0.9933(4) 0.0445(10) Uani 0.042(13) 1 d PD A -2 F7' F 0.531(2) 0.467(5) 0.916(3) 0.0699(16) Uani 0.042(13) 1 d PD A -2 F8' F 0.508(3) 0.5568(7) 0.996(6) 0.081(5) Uani 0.042(13) 1 d PD A -2 F9' F 0.4604(17) 0.480(6) 0.937(4) 0.086(4) Uani 0.042(13) 1 d PD A -2 F10' F 0.497(3) 0.3843(8) 0.991(6) 0.100(6) Uani 0.042(13) 1 d PD A -2 F11' F 0.5445(17) 0.461(6) 1.050(5) 0.084(4) Uani 0.042(13) 1 d PD A -2 F12' F 0.474(2) 0.474(5) 1.070(3) 0.0699(16) Uani 0.042(13) 1 d PD A -2 N1 N 0.49361(13) 0.2446(2) 0.7786(2) 0.0361(9) Uani 1 1 d . . . N2 N 0.47477(15) 0.3348(2) 0.7012(2) 0.0421(10) Uani 1 1 d . . . N3 N 0.48962(13) 0.2872(2) 0.5356(2) 0.0349(8) Uani 1 1 d . . . N4 N 0.15574(13) 0.2120(3) 0.5834(2) 0.0383(9) Uani 1 1 d . . . N5 N 0.11449(13) 0.1462(2) 0.6545(2) 0.0371(9) Uani 1 1 d . . . N6 N 0.13467(11) 0.1775(2) 0.8246(2) 0.0339(8) Uani 1 1 d . . . N7 N 0.12749(12) 0.2011(2) 0.9014(2) 0.0359(8) Uani 1 1 d . . . N8 N 0.10028(13) 0.1944(2) 1.0668(2) 0.0378(9) Uani 1 1 d . . . N9 N 0.15505(13) 0.2204(2) 1.1452(2) 0.0357(9) Uani 1 1 d . . . C1 C 0.47714(15) 0.2604(3) 0.7019(3) 0.0314(10) Uani 1 1 d . . . C2 C 0.50029(19) 0.3092(3) 0.8233(3) 0.0489(14) Uani 1 1 d . . . H2A H 0.5110 0.3125 0.8780 0.059 Uiso 1 1 calc R . . C3 C 0.4886(2) 0.3675(4) 0.7736(3) 0.0543(14) Uani 1 1 d . . . H3A H 0.4898 0.4186 0.7862 0.065 Uiso 1 1 calc R . . C4 C 0.50095(17) 0.1738(3) 0.8132(3) 0.0454(11) Uani 1 1 d U B . C5 C 0.5385(2) 0.1364(4) 0.7937(4) 0.0648(17) Uani 1 1 d DU . . C6 C 0.5450(3) 0.0674(5) 0.8288(5) 0.098(3) Uani 1 1 d U B . H6A H 0.5712 0.0418 0.8193 0.118 Uiso 1 1 calc R . . C7 C 0.5159(3) 0.0359(5) 0.8751(5) 0.087(2) Uani 1 1 d U . . H7A H 0.5198 -0.0134 0.8931 0.104 Uiso 1 1 calc R B . C8 C 0.4801(2) 0.0755(4) 0.8966(4) 0.0643(16) Uani 1 1 d U B . H8A H 0.4608 0.0545 0.9337 0.077 Uiso 1 1 calc R . . C9 C 0.47139(18) 0.1445(3) 0.8659(3) 0.0460(12) Uani 1 1 d U . . C10 C 0.5736(2) 0.1729(4) 0.7408(4) 0.0784(17) Uani 0.779(16) 1 d PDU B 1 H10 H 0.5582 0.2010 0.6961 0.094 Uiso 0.779(16) 1 calc PR B 1 C11 C 0.6063(4) 0.1254(7) 0.7035(7) 0.094(2) Uani 0.779(16) 1 d PDU B 1 H11A H 0.6238 0.1008 0.7463 0.141 Uiso 0.779(16) 1 calc PR B 1 H11B H 0.6251 0.1556 0.6704 0.141 Uiso 0.779(16) 1 calc PR B 1 H11C H 0.5916 0.0883 0.6691 0.141 Uiso 0.779(16) 1 calc PR B 1 C12 C 0.5995(4) 0.2263(7) 0.7905(6) 0.082(2) Uani 0.779(16) 1 d PDU B 1 H12A H 0.6143 0.2004 0.8359 0.123 Uiso 0.779(16) 1 calc PR B 1 H12B H 0.5802 0.2639 0.8118 0.123 Uiso 0.779(16) 1 calc PR B 1 H12C H 0.6210 0.2498 0.7569 0.123 Uiso 0.779(16) 1 calc PR B 1 C10' C 0.5736(2) 0.1729(4) 0.7408(4) 0.0784(17) Uani 0.221(16) 1 d PDU B 2 H10' H 0.5652 0.2156 0.7051 0.094 Uiso 0.221(16) 1 calc PR B 2 C11' C 0.5868(13) 0.1026(12) 0.703(2) 0.094(2) Uani 0.221(16) 1 d PDU B 2 H11D H 0.6056 0.1131 0.6575 0.141 Uiso 0.221(16) 1 calc PR B 2 H11E H 0.5609 0.0762 0.6824 0.141 Uiso 0.221(16) 1 calc PR B 2 H11F H 0.6025 0.0722 0.7432 0.141 Uiso 0.221(16) 1 calc PR B 2 C12' C 0.6060(8) 0.184(2) 0.8080(14) 0.082(2) Uani 0.221(16) 1 d PDU B 2 H12D H 0.5926 0.1747 0.8599 0.123 Uiso 0.221(16) 1 calc PR B 2 H12E H 0.6166 0.2350 0.8069 0.123 Uiso 0.221(16) 1 calc PR B 2 H12F H 0.6304 0.1502 0.8017 0.123 Uiso 0.221(16) 1 calc PR B 2 C13 C 0.43066(16) 0.1846(4) 0.8882(3) 0.0595(19) Uani 1 1 d . B . H13A H 0.4264 0.2256 0.8483 0.071 Uiso 1 1 calc R . . C14 C 0.3896(3) 0.1397(8) 0.8847(7) 0.139(5) Uani 1 1 d . . . H14A H 0.3878 0.1118 0.8338 0.209 Uiso 1 1 calc R B . H14B H 0.3645 0.1726 0.8874 0.209 Uiso 1 1 calc R . . H14C H 0.3899 0.1054 0.9307 0.209 Uiso 1 1 calc R . . C15 C 0.4372(2) 0.2214(4) 0.9751(4) 0.0709(19) Uani 1 1 d . . . H15A H 0.4616 0.2559 0.9748 0.106 Uiso 1 1 calc R B . H15B H 0.4431 0.1831 1.0159 0.106 Uiso 1 1 calc R . . H15C H 0.4107 0.2481 0.9884 0.106 Uiso 1 1 calc R . . C16 C 0.4582(3) 0.3769(3) 0.6325(3) 0.0617(17) Uani 1 1 d . . . H16A H 0.4613 0.4302 0.6442 0.074 Uiso 1 1 calc R . . H16B H 0.4270 0.3661 0.6226 0.074 Uiso 1 1 calc R . . C17 C 0.48318(19) 0.3575(3) 0.5567(3) 0.0419(12) Uani 1 1 d . . . C18 C 0.5000 0.4047(4) 0.5000 0.056(2) Uani 1 2 d S . . H18A H 0.5000 0.4570 0.5000 0.067 Uiso 1 2 calc SR . . C19 C 0.4385(2) 0.1052(4) 0.6580(4) 0.0628(15) Uani 1 1 d U . . H19A H 0.4523 0.0990 0.7136 0.075 Uiso 1 1 calc R . . C20 C 0.4042(2) 0.1533(4) 0.6551(4) 0.0633(16) Uani 1 1 d U . . H20A H 0.3978 0.1753 0.7089 0.076 Uiso 1 1 calc R . . C21 C 0.3634(3) 0.1451(5) 0.5972(5) 0.082(2) Uani 1 1 d U . . H21A H 0.3579 0.0922 0.5866 0.099 Uiso 1 1 calc R . . H21B H 0.3379 0.1658 0.6238 0.099 Uiso 1 1 calc R . . C22 C 0.3695(3) 0.1846(5) 0.5173(5) 0.085(2) Uani 1 1 d U . . H22A H 0.3529 0.1575 0.4741 0.102 Uiso 1 1 calc R . . H22B H 0.3563 0.2342 0.5210 0.102 Uiso 1 1 calc R . . C23 C 0.41447(18) 0.1934(4) 0.4915(3) 0.0597(15) Uani 1 1 d U . . H23A H 0.4183 0.2324 0.4495 0.072 Uiso 1 1 calc R . . C24 C 0.4440(2) 0.1365(3) 0.4887(3) 0.0507(13) Uani 1 1 d U . . H24A H 0.4658 0.1427 0.4459 0.061 Uiso 1 1 calc R . . C25 C 0.4357(3) 0.0579(4) 0.5107(4) 0.0709(17) Uani 1 1 d U . . H25A H 0.4538 0.0258 0.4773 0.085 Uiso 1 1 calc R . . H25B H 0.4049 0.0462 0.4967 0.085 Uiso 1 1 calc R . . C26 C 0.4451(3) 0.0396(5) 0.6017(5) 0.081(2) Uani 1 1 d U . . H26A H 0.4259 -0.0010 0.6178 0.098 Uiso 1 1 calc R . . H26B H 0.4755 0.0223 0.6089 0.098 Uiso 1 1 calc R . . C27 C 0.15385(15) 0.1795(3) 0.6570(3) 0.0336(10) Uani 1 1 d . . . C28 C 0.11833(15) 0.1983(3) 0.5358(3) 0.0441(12) Uani 1 1 d . . . H28A H 0.1121 0.2155 0.4821 0.053 Uiso 1 1 calc R . . C29 C 0.09265(16) 0.1560(3) 0.5809(3) 0.0449(13) Uani 1 1 d . . . H29A H 0.0650 0.1368 0.5650 0.054 Uiso 1 1 calc R . . C30 C 0.09902(17) 0.0988(3) 0.7189(3) 0.0422(12) Uani 1 1 d . . . H30A H 0.1174 0.0541 0.7227 0.051 Uiso 1 1 calc R . . H30B H 0.0689 0.0831 0.7047 0.051 Uiso 1 1 calc R . . C31 C 0.09993(16) 0.1366(3) 0.7994(3) 0.0354(10) Uani 1 1 d . . . C32 C 0.07037(15) 0.1336(3) 0.8580(3) 0.0388(11) Uani 1 1 d . . . H32A H 0.0432 0.1089 0.8557 0.047 Uiso 1 1 calc R . . C33 C 0.08845(14) 0.1746(3) 0.9222(3) 0.0386(10) Uani 1 1 d . . . C34 C 0.06898(16) 0.1947(4) 0.9991(3) 0.0490(13) Uani 1 1 d . . . H34A H 0.0560 0.2445 0.9938 0.059 Uiso 1 1 calc R . . H34B H 0.0454 0.1597 1.0102 0.059 Uiso 1 1 calc R . . C35 C 0.09365(16) 0.1573(3) 1.1402(3) 0.0426(12) Uani 1 1 d . . . H35A H 0.0698 0.1267 1.1529 0.051 Uiso 1 1 calc R . . C36 C 0.12836(17) 0.1744(3) 1.1884(3) 0.0410(11) Uani 1 1 d . . . H36A H 0.1337 0.1580 1.2426 0.049 Uiso 1 1 calc R . . C37 C 0.13735(16) 0.2333(3) 1.0682(3) 0.0357(10) Uani 1 1 d . . . C38 C 0.19228(17) 0.2520(3) 0.5519(3) 0.0397(11) Uani 1 1 d . C . C39 C 0.1981(2) 0.3271(3) 0.5724(3) 0.0527(15) Uani 1 1 d . . . C40 C 0.2337(3) 0.3622(4) 0.5406(4) 0.072(2) Uani 1 1 d . C . H40A H 0.2395 0.4121 0.5544 0.086 Uiso 1 1 calc R . . C41 C 0.2607(3) 0.3256(4) 0.4891(5) 0.0698(19) Uani 1 1 d . . . H41A H 0.2849 0.3509 0.4684 0.084 Uiso 1 1 calc R C . C42 C 0.25367(19) 0.2543(4) 0.4674(4) 0.0548(15) Uani 1 1 d . C . H42A H 0.2725 0.2306 0.4312 0.066 Uiso 1 1 calc R . . C43 C 0.21823(17) 0.2153(3) 0.4986(3) 0.0423(12) Uani 1 1 d . . . C44 C 0.1683(2) 0.3657(3) 0.6289(4) 0.0649(16) Uani 0.28(3) 1 d PDU C 1 H44 H 0.1532 0.3315 0.6661 0.078 Uiso 0.28(3) 1 calc PR C 1 C45 C 0.1361(13) 0.4085(17) 0.5664(19) 0.095(3) Uani 0.28(3) 1 d PDU C 1 H45A H 0.1148 0.4363 0.5967 0.143 Uiso 0.28(3) 1 calc PR C 1 H45B H 0.1211 0.3729 0.5306 0.143 Uiso 0.28(3) 1 calc PR C 1 H45C H 0.1529 0.4426 0.5337 0.143 Uiso 0.28(3) 1 calc PR C 1 C46 C 0.2045(10) 0.4162(18) 0.674(2) 0.070(3) Uani 0.28(3) 1 d PDU C 1 H46A H 0.1908 0.4469 0.7151 0.104 Uiso 0.28(3) 1 calc PR C 1 H46B H 0.2182 0.4479 0.6347 0.104 Uiso 0.28(3) 1 calc PR C 1 H46C H 0.2265 0.3847 0.7012 0.104 Uiso 0.28(3) 1 calc PR C 1 C44' C 0.1683(2) 0.3657(3) 0.6289(4) 0.0649(16) Uani 0.72(3) 1 d PD C 2 H44' H 0.1616 0.3282 0.6711 0.078 Uiso 0.72(3) 1 calc PR C 2 C45' C 0.1224(4) 0.3841(11) 0.5838(9) 0.095(3) Uani 0.72(3) 1 d PD C 2 H45D H 0.1036 0.4091 0.6218 0.143 Uiso 0.72(3) 1 calc PR C 2 H45E H 0.1086 0.3382 0.5650 0.143 Uiso 0.72(3) 1 calc PR C 2 H45F H 0.1270 0.4163 0.5372 0.143 Uiso 0.72(3) 1 calc PR C 2 C46' C 0.1895(6) 0.4337(6) 0.6785(8) 0.070(3) Uani 0.72(3) 1 d PD C 2 H46D H 0.1680 0.4549 0.7139 0.104 Uiso 0.72(3) 1 calc PR C 2 H46E H 0.1989 0.4713 0.6402 0.104 Uiso 0.72(3) 1 calc PR C 2 H46F H 0.2146 0.4164 0.7115 0.104 Uiso 0.72(3) 1 calc PR C 2 C47 C 0.21234(18) 0.1360(3) 0.4731(3) 0.0469(13) Uani 1 1 d . C . H47A H 0.1919 0.1127 0.5112 0.056 Uiso 1 1 calc R . . C48 C 0.1909(2) 0.1326(4) 0.3873(4) 0.0680(19) Uani 1 1 d . . . H48A H 0.1652 0.1642 0.3848 0.102 Uiso 1 1 calc R C . H48B H 0.1823 0.0817 0.3748 0.102 Uiso 1 1 calc R . . H48C H 0.2115 0.1495 0.3475 0.102 Uiso 1 1 calc R . . C49 C 0.2529(3) 0.0918(4) 0.4760(5) 0.072(2) Uani 1 1 d . . . H49A H 0.2707 0.1054 0.5243 0.109 Uiso 1 1 calc R C . H49B H 0.2692 0.1015 0.4272 0.109 Uiso 1 1 calc R . . H49C H 0.2457 0.0393 0.4785 0.109 Uiso 1 1 calc R . . C50 C 0.19407(16) 0.2532(3) 1.1820(3) 0.0351(10) Uani 1 1 d . . . C51 C 0.18855(17) 0.3132(3) 1.2343(3) 0.0391(11) Uani 1 1 d . . . C52 C 0.2263(2) 0.3433(3) 1.2714(3) 0.0488(14) Uani 1 1 d . . . H52A H 0.2240 0.3837 1.3076 0.059 Uiso 1 1 calc R . . C53 C 0.2658(2) 0.3161(4) 1.2565(4) 0.0587(16) Uani 1 1 d . . . H53A H 0.2909 0.3385 1.2811 0.070 Uiso 1 1 calc R . . C54 C 0.27059(19) 0.2550(4) 1.2053(4) 0.0540(14) Uani 1 1 d . . . H54A H 0.2987 0.2360 1.1964 0.065 Uiso 1 1 calc R . . C55 C 0.23415(18) 0.2219(3) 1.1672(3) 0.0451(12) Uani 1 1 d . . . C56 C 0.14451(18) 0.3447(3) 1.2509(3) 0.0470(13) Uani 1 1 d . . . H56A H 0.1233 0.3252 1.2087 0.056 Uiso 1 1 calc R . . C57 C 0.1285(3) 0.3216(5) 1.3359(4) 0.084(2) Uani 1 1 d . . . H57A H 0.1030 0.3509 1.3488 0.125 Uiso 1 1 calc R . . H57B H 0.1517 0.3303 1.3772 0.125 Uiso 1 1 calc R . . H57C H 0.1209 0.2692 1.3351 0.125 Uiso 1 1 calc R . . C58 C 0.1429(2) 0.4292(4) 1.2475(5) 0.0694(19) Uani 1 1 d . . . H58A H 0.1509 0.4459 1.1935 0.104 Uiso 1 1 calc R . . H58B H 0.1633 0.4497 1.2887 0.104 Uiso 1 1 calc R . . H58C H 0.1134 0.4460 1.2581 0.104 Uiso 1 1 calc R . . C59 C 0.23933(18) 0.1538(3) 1.1146(4) 0.0517(14) Uani 1 1 d . . . H59A H 0.2151 0.1548 1.0725 0.062 Uiso 1 1 calc R . . C60 C 0.2810(2) 0.1541(5) 1.0697(4) 0.077(2) Uani 1 1 d . . . H60A H 0.2865 0.2038 1.0493 0.116 Uiso 1 1 calc R . . H60B H 0.2785 0.1196 1.0239 0.116 Uiso 1 1 calc R . . H60C H 0.3050 0.1389 1.1066 0.116 Uiso 1 1 calc R . . C61 C 0.2328(3) 0.0851(4) 1.1660(5) 0.0690(18) Uani 1 1 d . . . H61A H 0.2058 0.0897 1.1950 0.104 Uiso 1 1 calc R . . H61B H 0.2573 0.0798 1.2053 0.104 Uiso 1 1 calc R . . H61C H 0.2312 0.0417 1.1307 0.104 Uiso 1 1 calc R . . C62 C 0.24122(19) 0.1173(4) 0.6965(4) 0.0550(14) Uani 1 1 d U . . H62A H 0.2324 0.1059 0.6389 0.066 Uiso 1 1 calc R . . C63 C 0.25308(16) 0.1883(3) 0.7091(3) 0.0466(12) Uani 1 1 d U . . H63A H 0.2510 0.2192 0.6588 0.056 Uiso 1 1 calc R . . C64 C 0.2870(2) 0.2146(4) 0.7704(4) 0.0654(16) Uani 1 1 d U . . H64A H 0.3146 0.1894 0.7592 0.078 Uiso 1 1 calc R . . H64B H 0.2915 0.2679 0.7616 0.078 Uiso 1 1 calc R . . C65 C 0.2780(3) 0.2034(5) 0.8549(5) 0.0832(19) Uani 1 1 d U . . H65A H 0.2815 0.2512 0.8832 0.100 Uiso 1 1 calc R . . H65B H 0.3004 0.1697 0.8785 0.100 Uiso 1 1 calc R . . C66 C 0.23290(17) 0.1718(5) 0.8740(3) 0.0633(15) Uani 1 1 d U . . H66A H 0.2190 0.1958 0.9211 0.076 Uiso 1 1 calc R . . C67 C 0.2203(2) 0.1037(5) 0.8601(4) 0.0677(17) Uani 1 1 d U . . H67A H 0.1988 0.0848 0.8989 0.081 Uiso 1 1 calc R . . C68 C 0.2485(3) 0.0450(5) 0.8250(6) 0.094(2) Uani 1 1 d U . . H68A H 0.2756 0.0422 0.8590 0.112 Uiso 1 1 calc R . . H68B H 0.2334 -0.0028 0.8303 0.112 Uiso 1 1 calc R . . C69 C 0.2601(3) 0.0526(5) 0.7429(5) 0.0791(19) Uani 1 1 d U . . H69A H 0.2513 0.0070 0.7135 0.095 Uiso 1 1 calc R . . H69B H 0.2921 0.0559 0.7419 0.095 Uiso 1 1 calc R . . C70 C 0.1847(2) 0.3412(4) 0.8613(4) 0.0600(15) Uani 1 1 d U . . H70A H 0.1931 0.3059 0.8180 0.072 Uiso 1 1 calc R . . C71 C 0.1429(3) 0.3583(4) 0.8602(4) 0.0663(16) Uani 1 1 d U . . H71A H 0.1254 0.3331 0.8159 0.080 Uiso 1 1 calc R . . C72 C 0.1228(3) 0.4284(6) 0.8887(6) 0.100(2) Uani 1 1 d U . . H72A H 0.1312 0.4686 0.8519 0.119 Uiso 1 1 calc R . . H72B H 0.0908 0.4232 0.8830 0.119 Uiso 1 1 calc R . . C73 C 0.1332(4) 0.4493(6) 0.9664(6) 0.103(2) Uani 1 1 d U . . H73A H 0.1064 0.4685 0.9902 0.123 Uiso 1 1 calc R . . H73B H 0.1537 0.4910 0.9638 0.123 Uiso 1 1 calc R . . C74 C 0.1534(3) 0.3912(3) 1.0271(4) 0.0692(17) Uani 1 1 d U . . H74A H 0.1400 0.3898 1.0813 0.083 Uiso 1 1 calc R . . C75 C 0.1951(3) 0.3704(3) 1.0276(4) 0.0626(16) Uani 1 1 d U . . H75A H 0.2067 0.3541 1.0822 0.075 Uiso 1 1 calc R . . C76 C 0.2305(2) 0.3983(4) 0.9712(4) 0.0716(17) Uani 1 1 d U . . H76A H 0.2367 0.4506 0.9840 0.086 Uiso 1 1 calc R . . H76B H 0.2574 0.3699 0.9827 0.086 Uiso 1 1 calc R . . C77 C 0.2193(3) 0.3925(6) 0.8888(5) 0.093(2) Uani 1 1 d U . . H77A H 0.2459 0.3786 0.8606 0.111 Uiso 1 1 calc R . . H77B H 0.2109 0.4422 0.8693 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.03101(18) 0.03296(18) 0.03318(19) -0.00247(15) 0.00058(14) -0.00109(15) Rh2 0.02821(17) 0.03489(18) 0.02944(17) 0.00213(15) -0.00321(13) -0.00009(15) Rh3 0.03381(19) 0.03337(18) 0.03264(19) 0.00288(15) 0.00184(14) -0.00094(16) P1 0.0384(7) 0.0378(7) 0.0392(7) -0.0028(5) 0.0017(5) 0.0037(5) F1 0.099(3) 0.088(3) 0.123(4) -0.060(3) -0.054(3) 0.007(3) F2 0.129(4) 0.067(3) 0.127(4) 0.025(3) 0.078(3) 0.001(3) F3 0.071(2) 0.071(2) 0.069(2) -0.0161(19) -0.0301(19) 0.0136(19) F4 0.117(3) 0.064(2) 0.070(3) 0.018(2) 0.030(2) 0.000(2) F5 0.0426(18) 0.066(2) 0.110(3) -0.029(2) -0.0130(19) 0.0187(17) F6 0.067(2) 0.067(3) 0.082(3) -0.009(2) 0.0101(19) 0.0287(19) P2 0.0631(19) 0.0384(10) 0.033(2) 0.003(2) 0.0089(16) -0.003(3) F7 0.077(3) 0.089(3) 0.045(3) -0.002(5) 0.017(3) 0.005(7) F8 0.084(7) 0.087(10) 0.073(7) -0.051(7) 0.006(5) -0.018(6) F9 0.124(11) 0.044(5) 0.093(9) 0.007(5) 0.036(8) 0.019(6) F10 0.081(8) 0.162(17) 0.058(7) -0.042(8) 0.008(5) -0.038(10) F11 0.105(11) 0.073(7) 0.072(7) 0.016(5) 0.004(6) 0.051(6) F12 0.077(3) 0.089(3) 0.045(3) -0.002(5) 0.017(3) 0.005(7) P2' 0.0631(19) 0.0384(10) 0.033(2) 0.003(2) 0.0089(16) -0.003(3) F7' 0.077(3) 0.089(3) 0.045(3) -0.002(5) 0.017(3) 0.005(7) F8' 0.084(7) 0.087(10) 0.073(7) -0.051(7) 0.006(5) -0.018(6) F9' 0.124(11) 0.044(5) 0.093(9) 0.007(5) 0.036(8) 0.019(6) F10' 0.081(8) 0.162(17) 0.058(7) -0.042(8) 0.008(5) -0.038(10) F11' 0.105(11) 0.073(7) 0.072(7) 0.016(5) 0.004(6) 0.051(6) F12' 0.077(3) 0.089(3) 0.045(3) -0.002(5) 0.017(3) 0.005(7) N1 0.035(2) 0.038(2) 0.035(2) -0.0022(18) -0.0001(17) -0.0027(18) N2 0.061(3) 0.033(2) 0.032(2) -0.0082(17) 0.0029(19) -0.004(2) N3 0.041(2) 0.0320(19) 0.0320(18) -0.0013(18) 0.0021(16) 0.0004(19) N4 0.037(2) 0.048(2) 0.0293(19) -0.0026(18) -0.0029(16) 0.0030(19) N5 0.037(2) 0.038(2) 0.036(2) -0.0034(17) -0.0027(17) -0.0007(17) N6 0.0279(18) 0.043(2) 0.0306(19) -0.0031(17) -0.0003(14) -0.0077(17) N7 0.0333(19) 0.042(2) 0.032(2) -0.0002(18) -0.0034(15) -0.0041(19) N8 0.036(2) 0.047(3) 0.0306(19) -0.0021(18) 0.0060(16) -0.0046(18) N9 0.039(2) 0.044(2) 0.0248(19) -0.0009(16) -0.0027(16) -0.0032(17) C1 0.032(2) 0.033(2) 0.029(2) -0.0029(19) -0.0042(18) 0.0016(19) C2 0.058(3) 0.054(4) 0.034(3) -0.004(2) -0.002(2) -0.017(3) C3 0.067(4) 0.052(3) 0.045(3) -0.008(3) 0.011(3) -0.007(3) C4 0.048(3) 0.050(3) 0.037(3) 0.000(2) -0.008(2) 0.003(2) C5 0.061(4) 0.084(4) 0.049(3) 0.012(3) -0.004(3) 0.034(3) C6 0.107(6) 0.098(6) 0.090(6) 0.026(5) 0.016(4) 0.076(5) C7 0.089(3) 0.081(3) 0.090(3) 0.0046(19) 0.0015(19) 0.0108(18) C8 0.065(2) 0.062(2) 0.066(2) 0.0048(17) -0.0020(17) 0.0014(17) C9 0.048(3) 0.053(3) 0.036(3) 0.012(2) -0.013(2) 0.001(2) C10 0.076(2) 0.082(2) 0.077(2) 0.0047(14) 0.0035(13) 0.0036(14) C11 0.093(3) 0.095(3) 0.094(3) -0.0011(14) 0.0047(14) 0.0031(14) C12 0.080(3) 0.084(3) 0.082(3) 0.0049(14) 0.0033(14) 0.0013(14) C10' 0.076(2) 0.082(2) 0.077(2) 0.0047(14) 0.0035(13) 0.0036(14) C11' 0.093(3) 0.095(3) 0.094(3) -0.0011(14) 0.0047(14) 0.0031(14) C12' 0.080(3) 0.084(3) 0.082(3) 0.0049(14) 0.0033(14) 0.0013(14) C13 0.031(3) 0.099(6) 0.049(3) 0.031(3) 0.002(2) 0.012(3) C14 0.090(7) 0.197(13) 0.133(9) 0.089(9) 0.047(6) -0.013(7) C15 0.070(4) 0.083(5) 0.061(4) 0.002(3) 0.014(3) 0.015(4) C16 0.098(5) 0.044(3) 0.044(3) 0.012(3) 0.011(3) 0.027(3) C17 0.060(3) 0.031(3) 0.035(3) 0.000(2) 0.001(2) 0.009(2) C18 0.103(7) 0.026(4) 0.038(4) 0.000 0.009(4) 0.000 C19 0.080(4) 0.056(4) 0.053(3) 0.007(3) 0.011(3) -0.036(3) C20 0.050(3) 0.098(5) 0.044(3) -0.018(3) 0.016(2) -0.027(3) C21 0.077(2) 0.093(3) 0.078(2) -0.0015(18) 0.0079(18) -0.0043(19) C22 0.077(2) 0.096(3) 0.082(2) -0.0025(19) 0.0014(18) -0.0032(19) C23 0.040(3) 0.097(4) 0.041(3) -0.015(3) -0.010(2) -0.016(3) C24 0.057(3) 0.057(3) 0.039(3) -0.016(2) 0.009(2) -0.020(3) C25 0.076(2) 0.069(2) 0.068(2) -0.0063(18) 0.0081(18) -0.0110(18) C26 0.090(3) 0.074(2) 0.081(2) 0.0015(18) 0.0070(19) -0.0081(19) C27 0.034(2) 0.033(2) 0.034(2) -0.0043(19) 0.0025(18) 0.0039(19) C28 0.032(2) 0.063(3) 0.036(2) -0.001(2) -0.008(2) 0.006(2) C29 0.034(2) 0.063(4) 0.036(3) -0.009(2) -0.011(2) 0.001(2) C30 0.043(3) 0.051(3) 0.033(3) -0.001(2) -0.005(2) -0.013(2) C31 0.041(3) 0.033(2) 0.032(2) -0.0013(19) -0.005(2) -0.007(2) C32 0.026(2) 0.051(3) 0.038(3) 0.001(2) -0.0033(19) -0.014(2) C33 0.031(2) 0.048(3) 0.037(2) 0.008(2) 0.0019(18) -0.003(2) C34 0.030(2) 0.071(4) 0.046(3) -0.002(3) 0.006(2) -0.008(2) C35 0.039(3) 0.045(3) 0.044(3) 0.002(2) 0.012(2) -0.006(2) C36 0.054(3) 0.037(2) 0.033(2) 0.001(2) 0.006(2) -0.010(2) C37 0.036(3) 0.031(2) 0.040(3) 0.001(2) 0.004(2) -0.005(2) C38 0.041(3) 0.050(3) 0.028(2) 0.002(2) -0.003(2) 0.002(2) C39 0.080(4) 0.037(3) 0.041(3) 0.010(2) -0.007(3) 0.004(3) C40 0.114(6) 0.048(4) 0.054(4) 0.011(3) 0.005(4) -0.026(4) C41 0.078(5) 0.063(4) 0.069(4) 0.015(4) 0.009(4) -0.021(4) C42 0.043(3) 0.074(4) 0.048(3) 0.003(3) 0.012(2) -0.004(3) C43 0.047(3) 0.048(3) 0.032(2) 0.005(2) 0.001(2) 0.000(2) C44 0.098(5) 0.028(3) 0.069(4) 0.002(3) 0.014(3) 0.013(3) C45 0.096(4) 0.093(4) 0.096(4) 0.003(2) 0.0034(19) 0.006(2) C46 0.138(9) 0.022(5) 0.050(4) -0.007(4) 0.021(6) -0.005(5) C44' 0.098(5) 0.028(3) 0.069(4) 0.002(3) 0.014(3) 0.013(3) C45' 0.096(4) 0.093(4) 0.096(4) 0.003(2) 0.0034(19) 0.006(2) C46' 0.138(9) 0.022(5) 0.050(4) -0.007(4) 0.021(6) -0.005(5) C47 0.042(3) 0.054(3) 0.045(3) -0.006(3) 0.006(2) -0.003(2) C48 0.074(4) 0.084(5) 0.045(3) -0.024(3) -0.008(3) 0.012(4) C49 0.079(5) 0.066(4) 0.071(4) -0.008(4) -0.010(4) 0.021(4) C50 0.039(3) 0.034(2) 0.032(2) 0.006(2) -0.0011(19) -0.004(2) C51 0.052(3) 0.032(3) 0.034(2) -0.001(2) 0.003(2) -0.012(2) C52 0.063(4) 0.046(3) 0.037(3) -0.005(2) -0.006(2) -0.021(3) C53 0.061(4) 0.063(4) 0.051(3) -0.004(3) -0.009(3) -0.022(3) C54 0.042(3) 0.067(4) 0.053(3) 0.010(3) -0.004(2) -0.005(3) C55 0.051(3) 0.049(3) 0.035(3) 0.002(2) -0.002(2) -0.003(2) C56 0.043(3) 0.049(3) 0.051(3) -0.015(2) 0.019(2) -0.015(2) C57 0.121(7) 0.067(4) 0.065(4) -0.008(4) 0.033(4) -0.029(5) C58 0.081(5) 0.049(4) 0.080(5) -0.024(3) 0.025(4) -0.015(3) C59 0.046(3) 0.055(4) 0.054(3) -0.010(3) -0.007(2) 0.017(3) C60 0.061(4) 0.113(6) 0.057(4) -0.015(4) -0.003(3) 0.028(4) C61 0.082(5) 0.049(4) 0.076(4) -0.004(3) 0.008(4) 0.016(3) C62 0.045(3) 0.062(3) 0.058(3) -0.001(3) 0.005(3) 0.029(3) C63 0.040(3) 0.062(3) 0.037(2) 0.003(2) -0.001(2) 0.002(2) C64 0.061(2) 0.071(2) 0.064(2) 0.0067(18) -0.0021(17) -0.0072(18) C65 0.077(2) 0.096(3) 0.077(2) -0.0068(19) 0.0039(18) -0.0054(19) C66 0.033(2) 0.128(5) 0.028(2) -0.004(3) -0.0085(19) 0.018(3) C67 0.060(4) 0.085(4) 0.058(4) 0.034(3) -0.001(3) 0.018(3) C68 0.095(3) 0.092(3) 0.094(3) 0.0092(19) 0.0044(19) 0.0120(19) C69 0.082(3) 0.074(2) 0.081(2) 0.0036(18) 0.0053(18) 0.0129(19) C70 0.089(4) 0.054(4) 0.037(3) 0.004(3) 0.007(3) -0.027(3) C71 0.091(4) 0.051(3) 0.057(4) 0.026(3) -0.002(3) 0.005(3) C72 0.102(3) 0.096(3) 0.101(3) 0.0035(19) 0.0029(19) 0.0069(19) C73 0.107(3) 0.098(3) 0.104(3) 0.0005(19) 0.0095(19) 0.0105(19) C74 0.116(5) 0.030(3) 0.065(4) -0.008(3) 0.039(4) -0.001(3) C75 0.093(4) 0.046(3) 0.047(3) 0.015(3) -0.012(3) -0.035(3) C76 0.073(2) 0.072(2) 0.069(2) 0.0045(18) -0.0021(18) -0.0145(18) C77 0.094(3) 0.095(3) 0.089(3) -0.0043(19) 0.0070(19) -0.0124(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 Rh1 C1 2.069(4) . ? Rh1 N3 2.095(4) . ? Rh1 C20 2.137(6) . ? Rh1 C19 2.142(6) . ? Rh1 C23 2.163(5) . ? Rh1 C24 2.200(5) . ? Rh2 C27 2.067(5) . ? Rh2 N6 2.093(4) . ? Rh2 C62 2.116(5) . ? Rh2 C63 2.128(5) . ? Rh2 C67 2.165(6) . ? Rh2 C66 2.191(5) . ? Rh3 C37 2.054(5) . ? Rh3 C74 2.094(6) . ? Rh3 N7 2.097(4) . ? Rh3 C75 2.141(6) . ? Rh3 C71 2.171(6) . ? Rh3 C70 2.203(6) . ? P1 F2 1.561(4) . ? P1 F6 1.570(4) . ? P1 F1 1.584(4) . ? P1 F5 1.587(3) . ? P1 F3 1.598(4) . ? P1 F4 1.599(4) . ? P2 F11 1.574(4) . ? P2 F12 1.574(4) . ? P2 F7 1.575(4) . ? P2 F10 1.576(4) . ? P2 F9 1.577(4) . ? P2 F8 1.578(4) . ? N1 C1 1.374(6) . ? N1 C2 1.396(7) . ? N1 C4 1.420(7) . ? N2 C1 1.351(6) . ? N2 C3 1.386(7) . ? N2 C16 1.443(7) . ? N3 C17 1.340(6) . ? N3 N3 1.359(7) 2_656 ? N4 C27 1.351(6) . ? N4 C28 1.392(6) . ? N4 C38 1.454(7) . ? N5 C27 1.355(6) . ? N5 C29 1.376(6) . ? N5 C30 1.460(6) . ? N6 C31 1.355(6) . ? N6 N7 1.361(5) . ? N7 C33 1.354(6) . ? N8 C37 1.344(6) . ? N8 C35 1.405(6) . ? N8 C34 1.447(6) . ? N9 C37 1.380(6) . ? N9 C36 1.388(6) . ? N9 C50 1.455(6) . ? C2 C3 1.376(9) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.389(8) . ? C4 C5 1.390(8) . ? C5 C6 1.390(11) . ? C5 C10 1.565(11) . ? C6 C7 1.329(12) . ? C6 H6A 0.9500 . ? C7 C8 1.375(11) . ? C7 H7A 0.9500 . ? C8 C9 1.373(9) . ? C8 H8A 0.9500 . ? C9 C13 1.510(8) . ? C10 C11 1.477(8) . ? C10 C12 1.482(8) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13 C14 1.504(12) . ? C13 C15 1.586(10) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.533(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.383(7) . ? C18 C17 1.383(7) 2_656 ? C18 H18A 0.9500 . ? C19 C20 1.372(10) . ? C19 C26 1.527(11) . ? C19 H19A 1.0000 . ? C20 C21 1.554(10) . ? C20 H20A 1.0000 . ? C21 C22 1.517(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.476(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.379(9) . ? C23 H23A 1.0000 . ? C24 C25 1.498(10) . ? C24 H24A 1.0000 . ? C25 C26 1.553(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C28 C29 1.347(8) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.493(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.354(7) . ? C32 C33 1.393(7) . ? C32 H32A 0.9500 . ? C33 C34 1.469(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.345(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C38 C43 1.382(7) . ? C38 C39 1.414(8) . ? C39 C40 1.390(10) . ? C39 C44 1.505(9) . ? C40 C41 1.383(11) . ? C40 H40A 0.9500 . ? C41 C42 1.358(10) . ? C41 H41A 0.9500 . ? C42 C43 1.416(8) . ? C42 H42A 0.9500 . ? C43 C47 1.509(8) . ? C44 C45 1.604(8) . ? C44 C46 1.607(8) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47 C49 1.486(9) . ? C47 C48 1.539(8) . ? C47 H47A 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.391(7) . ? C50 C51 1.402(7) . ? C51 C52 1.406(7) . ? C51 C56 1.509(8) . ? C52 C53 1.346(9) . ? C52 H52A 0.9500 . ? C53 C54 1.404(9) . ? C53 H53A 0.9500 . ? C54 C55 1.401(8) . ? C54 H54A 0.9500 . ? C55 C59 1.522(8) . ? C56 C58 1.536(9) . ? C56 C57 1.560(9) . ? C56 H56A 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.507(9) . ? C59 C61 1.525(9) . ? C59 H59A 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.354(9) . ? C62 C69 1.507(10) . ? C62 H62A 1.0000 . ? C63 C64 1.502(8) . ? C63 H63A 1.0000 . ? C64 C65 1.445(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.549(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.312(11) . ? C66 H66A 1.0000 . ? C67 C68 1.506(12) . ? C67 H67A 1.0000 . ? C68 C69 1.419(11) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.327(10) . ? C70 C77 1.475(11) . ? C70 H70A 1.0000 . ? C71 C72 1.499(12) . ? C71 H71A 1.0000 . ? C72 C73 1.361(13) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.566(12) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.338(10) . ? C74 H74A 1.0000 . ? C75 C76 1.547(10) . ? C75 H75A 1.0000 . ? C76 C77 1.392(11) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? 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 Rh1 N3 85.36(17) . . ? C1 Rh1 C20 93.0(2) . . ? N3 Rh1 C20 156.0(2) . . ? C1 Rh1 C19 96.1(2) . . ? N3 Rh1 C19 166.6(2) . . ? C20 Rh1 C19 37.4(3) . . ? C1 Rh1 C23 150.0(2) . . ? N3 Rh1 C23 87.5(2) . . ? C20 Rh1 C23 82.0(2) . . ? C19 Rh1 C23 97.5(3) . . ? C1 Rh1 C24 173.0(2) . . ? N3 Rh1 C24 94.62(18) . . ? C20 Rh1 C24 89.8(2) . . ? C19 Rh1 C24 82.3(2) . . ? C23 Rh1 C24 36.8(2) . . ? C27 Rh2 N6 86.38(16) . . ? C27 Rh2 C62 90.5(2) . . ? N6 Rh2 C62 156.7(2) . . ? C27 Rh2 C63 97.39(19) . . ? N6 Rh2 C63 166.00(19) . . ? C62 Rh2 C63 37.2(2) . . ? C27 Rh2 C67 150.8(3) . . ? N6 Rh2 C67 89.6(2) . . ? C62 Rh2 C67 81.9(3) . . ? C63 Rh2 C67 93.4(2) . . ? C27 Rh2 C66 174.0(3) . . ? N6 Rh2 C66 93.06(17) . . ? C62 Rh2 C66 92.3(2) . . ? C63 Rh2 C66 81.8(2) . . ? C67 Rh2 C66 35.1(3) . . ? C37 Rh3 C74 92.3(2) . . ? C37 Rh3 N7 85.44(17) . . ? C74 Rh3 N7 154.6(3) . . ? C37 Rh3 C75 97.2(2) . . ? C74 Rh3 C75 36.8(3) . . ? N7 Rh3 C75 168.5(3) . . ? C37 Rh3 C71 154.5(2) . . ? C74 Rh3 C71 82.8(3) . . ? N7 Rh3 C71 88.4(2) . . ? C75 Rh3 C71 93.8(3) . . ? C37 Rh3 C70 170.1(3) . . ? C74 Rh3 C70 91.2(2) . . ? N7 Rh3 C70 95.32(19) . . ? C75 Rh3 C70 80.2(2) . . ? C71 Rh3 C70 35.3(3) . . ? F2 P1 F6 90.4(3) . . ? F2 P1 F1 92.5(3) . . ? F6 P1 F1 88.3(2) . . ? F2 P1 F5 88.9(3) . . ? F6 P1 F5 179.3(3) . . ? F1 P1 F5 91.8(2) . . ? F2 P1 F3 91.8(3) . . ? F6 P1 F3 91.6(2) . . ? F1 P1 F3 175.7(3) . . ? F5 P1 F3 88.4(2) . . ? F2 P1 F4 178.0(3) . . ? F6 P1 F4 88.6(2) . . ? F1 P1 F4 89.3(3) . . ? F5 P1 F4 92.1(3) . . ? F3 P1 F4 86.4(3) . . ? F11 P2 F12 90.1(2) . . ? F11 P2 F7 90.0(2) . . ? F12 P2 F7 179.9(3) . . ? F11 P2 F10 89.8(2) . . ? F12 P2 F10 90.0(2) . . ? F7 P2 F10 90.0(2) . . ? F11 P2 F9 179.6(4) . . ? F12 P2 F9 89.9(2) . . ? F7 P2 F9 89.9(2) . . ? F10 P2 F9 89.8(2) . . ? F11 P2 F8 90.6(4) . . ? F12 P2 F8 90.0(2) . . ? F7 P2 F8 90.0(2) . . ? F10 P2 F8 179.6(4) . . ? F9 P2 F8 89.7(2) . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C4 127.3(4) . . ? C2 N1 C4 122.1(4) . . ? C1 N2 C3 113.9(5) . . ? C1 N2 C16 123.6(5) . . ? C3 N2 C16 122.4(5) . . ? C17 N3 N3 107.6(3) . 2_656 ? C17 N3 Rh1 118.9(3) . . ? N3 N3 Rh1 132.05(14) 2_656 . ? C27 N4 C28 111.3(4) . . ? C27 N4 C38 126.9(4) . . ? C28 N4 C38 121.6(4) . . ? C27 N5 C29 112.1(4) . . ? C27 N5 C30 124.0(4) . . ? C29 N5 C30 123.6(4) . . ? C31 N6 N7 107.6(4) . . ? C31 N6 Rh2 119.2(3) . . ? N7 N6 Rh2 130.6(3) . . ? C33 N7 N6 107.6(4) . . ? C33 N7 Rh3 119.2(3) . . ? N6 N7 Rh3 129.9(3) . . ? C37 N8 C35 112.9(4) . . ? C37 N8 C34 123.5(4) . . ? C35 N8 C34 123.4(4) . . ? C37 N9 C36 110.6(4) . . ? C37 N9 C50 127.2(4) . . ? C36 N9 C50 122.0(4) . . ? N2 C1 N1 103.6(4) . . ? N2 C1 Rh1 118.2(3) . . ? N1 C1 Rh1 138.2(4) . . ? C3 C2 N1 107.6(5) . . ? C3 C2 H2A 126.2 . . ? N1 C2 H2A 126.2 . . ? C2 C3 N2 104.3(5) . . ? C2 C3 H3A 127.8 . . ? N2 C3 H3A 127.8 . . ? C9 C4 C5 122.0(6) . . ? C9 C4 N1 119.9(5) . . ? C5 C4 N1 118.1(5) . . ? C4 C5 C6 116.9(7) . . ? C4 C5 C10 121.5(6) . . ? C6 C5 C10 121.4(6) . . ? C7 C6 C5 122.4(7) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C8 119.4(8) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 121.9(7) . . ? C9 C8 H8A 119.0 . . ? C7 C8 H8A 119.0 . . ? C8 C9 C4 117.1(6) . . ? C8 C9 C13 120.2(6) . . ? C4 C9 C13 122.7(5) . . ? C11 C10 C12 104.5(8) . . ? C11 C10 C5 118.9(8) . . ? C12 C10 C5 109.8(7) . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C5 C10 H10 107.8 . . ? 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 . . ? H11D C11' H11E 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? H12D C12' H12E 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C14 C13 C9 115.9(8) . . ? C14 C13 C15 109.9(7) . . ? C9 C13 C15 110.2(5) . . ? C14 C13 H13A 106.8 . . ? C9 C13 H13A 106.8 . . ? C15 C13 H13A 106.8 . . ? 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 . . ? N2 C16 C17 110.1(5) . . ? N2 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? N2 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? N3 C17 C18 110.6(5) . . ? N3 C17 C16 120.9(5) . . ? C18 C17 C16 128.4(5) . . ? C17 C18 C17 103.5(6) 2_656 . ? C17 C18 H18A 128.2 2_656 . ? C17 C18 H18A 128.2 . . ? C20 C19 C26 126.5(7) . . ? C20 C19 Rh1 71.1(4) . . ? C26 C19 Rh1 109.0(5) . . ? C20 C19 H19A 113.9 . . ? C26 C19 H19A 113.9 . . ? Rh1 C19 H19A 113.9 . . ? C19 C20 C21 124.5(6) . . ? C19 C20 Rh1 71.5(3) . . ? C21 C20 Rh1 112.8(4) . . ? C19 C20 H20A 113.6 . . ? C21 C20 H20A 113.6 . . ? Rh1 C20 H20A 113.6 . . ? C22 C21 C20 111.4(6) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C21 116.7(7) . . ? C23 C22 H22A 108.1 . . ? C21 C22 H22A 108.1 . . ? C23 C22 H22B 108.1 . . ? C21 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C24 C23 C22 124.0(7) . . ? C24 C23 Rh1 73.0(3) . . ? C22 C23 Rh1 109.3(4) . . ? C24 C23 H23A 114.3 . . ? C22 C23 H23A 114.3 . . ? Rh1 C23 H23A 114.3 . . ? C23 C24 C25 125.9(6) . . ? C23 C24 Rh1 70.1(3) . . ? C25 C24 Rh1 111.3(4) . . ? C23 C24 H24A 113.8 . . ? C25 C24 H24A 113.8 . . ? Rh1 C24 H24A 113.8 . . ? C24 C25 C26 114.1(6) . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C19 C26 C25 113.3(7) . . ? C19 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C19 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? N4 C27 N5 103.7(4) . . ? N4 C27 Rh2 138.2(4) . . ? N5 C27 Rh2 118.0(3) . . ? C29 C28 N4 106.5(4) . . ? C29 C28 H28A 126.8 . . ? N4 C28 H28A 126.8 . . ? C28 C29 N5 106.3(4) . . ? C28 C29 H29A 126.8 . . ? N5 C29 H29A 126.8 . . ? N5 C30 C31 112.3(4) . . ? N5 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? N5 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? C32 C31 N6 110.5(4) . . ? C32 C31 C30 128.7(4) . . ? N6 C31 C30 120.7(4) . . ? C31 C32 C33 105.0(4) . . ? C31 C32 H32A 127.5 . . ? C33 C32 H32A 127.5 . . ? N7 C33 C32 109.3(4) . . ? N7 C33 C34 121.9(5) . . ? C32 C33 C34 128.6(4) . . ? N8 C34 C33 112.4(4) . . ? N8 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? N8 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C36 C35 N8 105.0(4) . . ? C36 C35 H35A 127.5 . . ? N8 C35 H35A 127.5 . . ? C35 C36 N9 108.1(4) . . ? C35 C36 H36A 126.0 . . ? N9 C36 H36A 126.0 . . ? N8 C37 N9 103.4(4) . . ? N8 C37 Rh3 120.0(3) . . ? N9 C37 Rh3 136.5(3) . . ? C43 C38 C39 123.1(5) . . ? C43 C38 N4 117.5(5) . . ? C39 C38 N4 119.3(5) . . ? C40 C39 C38 116.5(6) . . ? C40 C39 C44 122.0(6) . . ? C38 C39 C44 121.4(6) . . ? C41 C40 C39 121.1(6) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C42 C41 C40 121.7(6) . . ? C42 C41 H41A 119.2 . . ? C40 C41 H41A 119.2 . . ? C41 C42 C43 119.9(6) . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C38 C43 C42 117.7(5) . . ? C38 C43 C47 124.8(5) . . ? C42 C43 C47 117.5(5) . . ? C39 C44 C45 101.9(15) . . ? C39 C44 C46 97.2(15) . . ? C45 C44 C46 115.1(10) . . ? C39 C44 H44 113.6 . . ? C45 C44 H44 113.6 . . ? C46 C44 H44 113.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? H45D C45' H45E 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? H46D C46' H46E 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C49 C47 C43 114.5(5) . . ? C49 C47 C48 109.8(5) . . ? C43 C47 C48 109.8(5) . . ? C49 C47 H47A 107.5 . . ? C43 C47 H47A 107.5 . . ? C48 C47 H47A 107.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 123.7(5) . . ? C55 C50 N9 119.1(4) . . ? C51 C50 N9 117.2(4) . . ? C50 C51 C52 116.8(5) . . ? C50 C51 C56 122.5(4) . . ? C52 C51 C56 120.7(5) . . ? C53 C52 C51 121.2(5) . . ? C53 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? C52 C53 C54 121.1(5) . . ? C52 C53 H53A 119.4 . . ? C54 C53 H53A 119.4 . . ? C55 C54 C53 120.4(6) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C50 C55 C54 116.7(5) . . ? C50 C55 C59 123.1(5) . . ? C54 C55 C59 120.2(5) . . ? C51 C56 C58 113.6(5) . . ? C51 C56 C57 112.3(6) . . ? C58 C56 C57 106.8(5) . . ? C51 C56 H56A 108.0 . . ? C58 C56 H56A 108.0 . . ? C57 C56 H56A 108.0 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C55 112.8(6) . . ? C60 C59 C61 114.1(6) . . ? C55 C59 C61 109.2(5) . . ? C60 C59 H59A 106.7 . . ? C55 C59 H59A 106.7 . . ? C61 C59 H59A 106.7 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 C69 124.7(6) . . ? C63 C62 Rh2 71.9(3) . . ? C69 C62 Rh2 111.2(5) . . ? C63 C62 H62A 113.9 . . ? C69 C62 H62A 113.9 . . ? Rh2 C62 H62A 113.9 . . ? C62 C63 C64 125.5(5) . . ? C62 C63 Rh2 70.9(3) . . ? C64 C63 Rh2 112.1(4) . . ? C62 C63 H63A 113.5 . . ? C64 C63 H63A 113.5 . . ? Rh2 C63 H63A 113.5 . . ? C65 C64 C63 116.7(6) . . ? C65 C64 H64A 108.1 . . ? C63 C64 H64A 108.1 . . ? C65 C64 H64B 108.1 . . ? C63 C64 H64B 108.1 . . ? H64A C64 H64B 107.3 . . ? C64 C65 C66 117.0(6) . . ? C64 C65 H65A 108.0 . . ? C66 C65 H65A 108.0 . . ? C64 C65 H65B 108.0 . . ? C66 C65 H65B 108.0 . . ? H65A C65 H65B 107.3 . . ? C67 C66 C65 125.0(7) . . ? C67 C66 Rh2 71.4(4) . . ? C65 C66 Rh2 109.0(4) . . ? C67 C66 H66A 114.3 . . ? C65 C66 H66A 114.3 . . ? Rh2 C66 H66A 114.3 . . ? C66 C67 C68 124.3(7) . . ? C66 C67 Rh2 73.5(4) . . ? C68 C67 Rh2 109.0(5) . . ? C66 C67 H67A 114.2 . . ? C68 C67 H67A 114.2 . . ? Rh2 C67 H67A 114.2 . . ? C69 C68 C67 117.9(7) . . ? C69 C68 H68A 107.8 . . ? C67 C68 H68A 107.8 . . ? C69 C68 H68B 107.8 . . ? C67 C68 H68B 107.8 . . ? H68A C68 H68B 107.2 . . ? C68 C69 C62 116.9(7) . . ? C68 C69 H69A 108.1 . . ? C62 C69 H69A 108.1 . . ? C68 C69 H69B 108.1 . . ? C62 C69 H69B 108.1 . . ? H69A C69 H69B 107.3 . . ? C71 C70 C77 123.2(7) . . ? C71 C70 Rh3 71.0(4) . . ? C77 C70 Rh3 110.1(5) . . ? C71 C70 H70A 114.8 . . ? C77 C70 H70A 114.8 . . ? Rh3 C70 H70A 114.8 . . ? C70 C71 C72 127.5(8) . . ? C70 C71 Rh3 73.7(4) . . ? C72 C71 Rh3 107.0(5) . . ? C70 C71 H71A 113.5 . . ? C72 C71 H71A 113.5 . . ? Rh3 C71 H71A 113.5 . . ? C73 C72 C71 116.5(9) . . ? C73 C72 H72A 108.2 . . ? C71 C72 H72A 108.2 . . ? C73 C72 H72B 108.2 . . ? C71 C72 H72B 108.2 . . ? H72A C72 H72B 107.3 . . ? C72 C73 C74 119.1(9) . . ? C72 C73 H73A 107.5 . . ? C74 C73 H73A 107.5 . . ? C72 C73 H73B 107.5 . . ? C74 C73 H73B 107.5 . . ? H73A C73 H73B 107.0 . . ? C75 C74 C73 123.6(7) . . ? C75 C74 Rh3 73.5(4) . . ? C73 C74 Rh3 107.7(5) . . ? C75 C74 H74A 114.7 . . ? C73 C74 H74A 114.7 . . ? Rh3 C74 H74A 114.7 . . ? C74 C75 C76 127.1(6) . . ? C74 C75 Rh3 69.7(4) . . ? C76 C75 Rh3 110.5(4) . . ? C74 C75 H75A 113.6 . . ? C76 C75 H75A 113.6 . . ? Rh3 C75 H75A 113.6 . . ? C77 C76 C75 114.0(6) . . ? C77 C76 H76A 108.7 . . ? C75 C76 H76A 108.7 . . ? C77 C76 H76B 108.7 . . ? C75 C76 H76B 108.7 . . ? H76A C76 H76B 107.6 . . ? C76 C77 C70 119.8(7) . . ? C76 C77 H77A 107.4 . . ? C70 C77 H77A 107.4 . . ? C76 C77 H77B 107.4 . . ? C70 C77 H77B 107.4 . . ? H77A C77 H77B 106.9 . . ? 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 Rh1 N3 C17 -46.1(4) . . . . ? C20 Rh1 N3 C17 40.9(7) . . . . ? C19 Rh1 N3 C17 -142.9(9) . . . . ? C23 Rh1 N3 C17 104.7(4) . . . . ? C24 Rh1 N3 C17 140.9(4) . . . . ? C1 Rh1 N3 N3 149.6(5) . . . 2_656 ? C20 Rh1 N3 N3 -123.4(6) . . . 2_656 ? C19 Rh1 N3 N3 52.7(12) . . . 2_656 ? C23 Rh1 N3 N3 -59.6(5) . . . 2_656 ? C24 Rh1 N3 N3 -23.5(6) . . . 2_656 ? C27 Rh2 N6 C31 46.6(4) . . . . ? C62 Rh2 N6 C31 -36.3(7) . . . . ? C63 Rh2 N6 C31 152.8(7) . . . . ? C67 Rh2 N6 C31 -104.5(4) . . . . ? C66 Rh2 N6 C31 -139.4(4) . . . . ? C27 Rh2 N6 N7 -154.3(4) . . . . ? C62 Rh2 N6 N7 122.8(6) . . . . ? C63 Rh2 N6 N7 -48.2(9) . . . . ? C67 Rh2 N6 N7 54.6(5) . . . . ? C66 Rh2 N6 N7 19.7(5) . . . . ? C31 N6 N7 C33 -0.1(5) . . . . ? Rh2 N6 N7 C33 -161.0(4) . . . . ? C31 N6 N7 Rh3 -159.0(3) . . . . ? Rh2 N6 N7 Rh3 40.1(6) . . . . ? C37 Rh3 N7 C33 45.3(4) . . . . ? C74 Rh3 N7 C33 -40.5(7) . . . . ? C75 Rh3 N7 C33 149.1(9) . . . . ? C71 Rh3 N7 C33 -109.9(4) . . . . ? C70 Rh3 N7 C33 -144.5(4) . . . . ? C37 Rh3 N7 N6 -157.9(4) . . . . ? C74 Rh3 N7 N6 116.3(6) . . . . ? C75 Rh3 N7 N6 -54.1(11) . . . . ? C71 Rh3 N7 N6 46.9(4) . . . . ? C70 Rh3 N7 N6 12.3(4) . . . . ? C3 N2 C1 N1 -0.4(6) . . . . ? C16 N2 C1 N1 -178.6(5) . . . . ? C3 N2 C1 Rh1 180.0(4) . . . . ? C16 N2 C1 Rh1 1.7(7) . . . . ? C2 N1 C1 N2 0.9(6) . . . . ? C4 N1 C1 N2 177.1(5) . . . . ? C2 N1 C1 Rh1 -179.6(4) . . . . ? C4 N1 C1 Rh1 -3.4(8) . . . . ? N3 Rh1 C1 N2 41.4(4) . . . . ? C20 Rh1 C1 N2 -114.7(4) . . . . ? C19 Rh1 C1 N2 -152.1(4) . . . . ? C23 Rh1 C1 N2 -35.4(7) . . . . ? C24 Rh1 C1 N2 131.5(16) . . . . ? N3 Rh1 C1 N1 -138.1(5) . . . . ? C20 Rh1 C1 N1 65.8(6) . . . . ? C19 Rh1 C1 N1 28.4(6) . . . . ? C23 Rh1 C1 N1 145.1(5) . . . . ? C24 Rh1 C1 N1 -48(2) . . . . ? C1 N1 C2 C3 -1.1(6) . . . . ? C4 N1 C2 C3 -177.5(5) . . . . ? N1 C2 C3 N2 0.8(6) . . . . ? C1 N2 C3 C2 -0.3(7) . . . . ? C16 N2 C3 C2 178.0(5) . . . . ? C1 N1 C4 C9 -100.4(6) . . . . ? C2 N1 C4 C9 75.4(7) . . . . ? C1 N1 C4 C5 80.6(7) . . . . ? C2 N1 C4 C5 -103.6(6) . . . . ? C9 C4 C5 C6 0.7(10) . . . . ? N1 C4 C5 C6 179.7(7) . . . . ? C9 C4 C5 C10 -174.3(5) . . . . ? N1 C4 C5 C10 4.7(9) . . . . ? C4 C5 C6 C7 3.9(13) . . . . ? C10 C5 C6 C7 178.8(8) . . . . ? C5 C6 C7 C8 -7.1(15) . . . . ? C6 C7 C8 C9 5.8(13) . . . . ? C7 C8 C9 C4 -1.4(10) . . . . ? C7 C8 C9 C13 177.3(7) . . . . ? C5 C4 C9 C8 -1.8(8) . . . . ? N1 C4 C9 C8 179.2(5) . . . . ? C5 C4 C9 C13 179.6(6) . . . . ? N1 C4 C9 C13 0.6(8) . . . . ? C4 C5 C10 C11 -163.5(8) . . . . ? C6 C5 C10 C11 21.8(12) . . . . ? C4 C5 C10 C12 76.4(9) . . . . ? C6 C5 C10 C12 -98.4(10) . . . . ? C8 C9 C13 C14 -45.3(8) . . . . ? C4 C9 C13 C14 133.3(7) . . . . ? C8 C9 C13 C15 80.3(8) . . . . ? C4 C9 C13 C15 -101.1(6) . . . . ? C1 N2 C16 C17 -55.7(8) . . . . ? C3 N2 C16 C17 126.2(6) . . . . ? N3 N3 C17 C18 -0.6(6) 2_656 . . . ? Rh1 N3 C17 C18 -168.5(3) . . . . ? N3 N3 C17 C16 176.7(5) 2_656 . . . ? Rh1 N3 C17 C16 8.8(7) . . . . ? N2 C16 C17 N3 48.9(8) . . . . ? N2 C16 C17 C18 -134.3(5) . . . . ? N3 C17 C18 C17 0.2(2) . . . 2_656 ? C16 C17 C18 C17 -176.8(7) . . . 2_656 ? C1 Rh1 C19 C20 87.0(4) . . . . ? N3 Rh1 C19 C20 -177.5(7) . . . . ? C23 Rh1 C19 C20 -66.2(4) . . . . ? C24 Rh1 C19 C20 -99.8(4) . . . . ? C1 Rh1 C19 C26 -149.8(5) . . . . ? N3 Rh1 C19 C26 -54.3(12) . . . . ? C20 Rh1 C19 C26 123.1(7) . . . . ? C23 Rh1 C19 C26 57.0(6) . . . . ? C24 Rh1 C19 C26 23.3(5) . . . . ? C26 C19 C20 C21 5.4(10) . . . . ? Rh1 C19 C20 C21 105.4(6) . . . . ? C26 C19 C20 Rh1 -100.0(6) . . . . ? C1 Rh1 C20 C19 -96.1(4) . . . . ? N3 Rh1 C20 C19 178.5(4) . . . . ? C23 Rh1 C20 C19 113.7(4) . . . . ? C24 Rh1 C20 C19 77.6(4) . . . . ? C1 Rh1 C20 C21 143.4(5) . . . . ? N3 Rh1 C20 C21 58.0(8) . . . . ? C19 Rh1 C20 C21 -120.5(7) . . . . ? C23 Rh1 C20 C21 -6.8(6) . . . . ? C24 Rh1 C20 C21 -43.0(6) . . . . ? C19 C20 C21 C22 -90.3(9) . . . . ? Rh1 C20 C21 C22 -7.7(9) . . . . ? C20 C21 C22 C23 26.6(10) . . . . ? C21 C22 C23 C24 50.4(10) . . . . ? C21 C22 C23 Rh1 -31.8(9) . . . . ? C1 Rh1 C23 C24 177.4(4) . . . . ? N3 Rh1 C23 C24 101.1(4) . . . . ? C20 Rh1 C23 C24 -100.5(4) . . . . ? C19 Rh1 C23 C24 -66.3(4) . . . . ? C1 Rh1 C23 C22 -61.8(8) . . . . ? N3 Rh1 C23 C22 -138.1(6) . . . . ? C20 Rh1 C23 C22 20.3(6) . . . . ? C19 Rh1 C23 C22 54.5(6) . . . . ? C24 Rh1 C23 C22 120.8(7) . . . . ? C22 C23 C24 C25 0.2(10) . . . . ? Rh1 C23 C24 C25 102.4(6) . . . . ? C22 C23 C24 Rh1 -102.2(6) . . . . ? C1 Rh1 C24 C23 -169.1(16) . . . . ? N3 Rh1 C24 C23 -79.5(4) . . . . ? C20 Rh1 C24 C23 76.9(4) . . . . ? C19 Rh1 C24 C23 113.6(4) . . . . ? C1 Rh1 C24 C25 69.1(18) . . . . ? N3 Rh1 C24 C25 158.6(5) . . . . ? C20 Rh1 C24 C25 -45.0(5) . . . . ? C19 Rh1 C24 C25 -8.2(5) . . . . ? C23 Rh1 C24 C25 -121.9(6) . . . . ? C23 C24 C25 C26 -89.1(8) . . . . ? Rh1 C24 C25 C26 -8.8(8) . . . . ? C20 C19 C26 C25 45.0(10) . . . . ? Rh1 C19 C26 C25 -35.1(8) . . . . ? C24 C25 C26 C19 29.4(10) . . . . ? C28 N4 C27 N5 -0.7(5) . . . . ? C38 N4 C27 N5 -176.2(4) . . . . ? C28 N4 C27 Rh2 179.8(4) . . . . ? C38 N4 C27 Rh2 4.2(8) . . . . ? C29 N5 C27 N4 1.4(5) . . . . ? C30 N5 C27 N4 175.1(4) . . . . ? C29 N5 C27 Rh2 -179.0(3) . . . . ? C30 N5 C27 Rh2 -5.3(6) . . . . ? N6 Rh2 C27 N4 142.3(5) . . . . ? C62 Rh2 C27 N4 -60.8(5) . . . . ? C63 Rh2 C27 N4 -24.2(6) . . . . ? C67 Rh2 C27 N4 -135.0(6) . . . . ? C66 Rh2 C27 N4 58(2) . . . . ? N6 Rh2 C27 N5 -37.2(4) . . . . ? C62 Rh2 C27 N5 119.7(4) . . . . ? C63 Rh2 C27 N5 156.4(4) . . . . ? C67 Rh2 C27 N5 45.5(6) . . . . ? C66 Rh2 C27 N5 -121.9(18) . . . . ? C27 N4 C28 C29 -0.2(6) . . . . ? C38 N4 C28 C29 175.6(5) . . . . ? N4 C28 C29 N5 1.1(6) . . . . ? C27 N5 C29 C28 -1.6(6) . . . . ? C30 N5 C29 C28 -175.3(5) . . . . ? C27 N5 C30 C31 56.0(6) . . . . ? C29 N5 C30 C31 -131.1(5) . . . . ? N7 N6 C31 C32 0.4(6) . . . . ? Rh2 N6 C31 C32 163.8(3) . . . . ? N7 N6 C31 C30 -176.4(4) . . . . ? Rh2 N6 C31 C30 -12.9(6) . . . . ? N5 C30 C31 C32 139.8(5) . . . . ? N5 C30 C31 N6 -44.1(6) . . . . ? N6 C31 C32 C33 -0.4(6) . . . . ? C30 C31 C32 C33 176.0(5) . . . . ? N6 N7 C33 C32 -0.1(6) . . . . ? Rh3 N7 C33 C32 161.4(3) . . . . ? N6 N7 C33 C34 -174.9(5) . . . . ? Rh3 N7 C33 C34 -13.4(7) . . . . ? C31 C32 C33 N7 0.3(6) . . . . ? C31 C32 C33 C34 174.6(6) . . . . ? C37 N8 C34 C33 55.1(7) . . . . ? C35 N8 C34 C33 -129.4(5) . . . . ? N7 C33 C34 N8 -42.7(7) . . . . ? C32 C33 C34 N8 143.6(5) . . . . ? C37 N8 C35 C36 -0.1(6) . . . . ? C34 N8 C35 C36 -176.0(5) . . . . ? N8 C35 C36 N9 -0.1(6) . . . . ? C37 N9 C36 C35 0.2(6) . . . . ? C50 N9 C36 C35 175.6(5) . . . . ? C35 N8 C37 N9 0.2(5) . . . . ? C34 N8 C37 N9 176.1(4) . . . . ? C35 N8 C37 Rh3 178.2(3) . . . . ? C34 N8 C37 Rh3 -5.9(7) . . . . ? C36 N9 C37 N8 -0.2(5) . . . . ? C50 N9 C37 N8 -175.3(4) . . . . ? C36 N9 C37 Rh3 -177.8(4) . . . . ? C50 N9 C37 Rh3 7.2(8) . . . . ? C74 Rh3 C37 N8 118.7(5) . . . . ? N7 Rh3 C37 N8 -35.9(4) . . . . ? C75 Rh3 C37 N8 155.4(4) . . . . ? C71 Rh3 C37 N8 40.6(8) . . . . ? C70 Rh3 C37 N8 -130.7(12) . . . . ? C74 Rh3 C37 N9 -64.1(6) . . . . ? N7 Rh3 C37 N9 141.3(5) . . . . ? C75 Rh3 C37 N9 -27.4(6) . . . . ? C71 Rh3 C37 N9 -142.1(6) . . . . ? C70 Rh3 C37 N9 46.5(16) . . . . ? C27 N4 C38 C43 100.4(6) . . . . ? C28 N4 C38 C43 -74.8(6) . . . . ? C27 N4 C38 C39 -83.6(7) . . . . ? C28 N4 C38 C39 101.3(6) . . . . ? C43 C38 C39 C40 -4.4(8) . . . . ? N4 C38 C39 C40 179.8(5) . . . . ? C43 C38 C39 C44 178.3(5) . . . . ? N4 C38 C39 C44 2.5(8) . . . . ? C38 C39 C40 C41 2.4(10) . . . . ? C44 C39 C40 C41 179.7(6) . . . . ? C39 C40 C41 C42 0.2(11) . . . . ? C40 C41 C42 C43 -1.0(11) . . . . ? C39 C38 C43 C42 3.7(8) . . . . ? N4 C38 C43 C42 179.6(5) . . . . ? C39 C38 C43 C47 -178.1(5) . . . . ? N4 C38 C43 C47 -2.2(7) . . . . ? C41 C42 C43 C38 -0.9(9) . . . . ? C41 C42 C43 C47 -179.3(6) . . . . ? C40 C39 C44 C45 83.4(17) . . . . ? C38 C39 C44 C45 -99.4(16) . . . . ? C40 C39 C44 C46 -34.2(15) . . . . ? C38 C39 C44 C46 143.0(15) . . . . ? C38 C43 C47 C49 -133.2(6) . . . . ? C42 C43 C47 C49 45.0(7) . . . . ? C38 C43 C47 C48 102.8(6) . . . . ? C42 C43 C47 C48 -79.0(6) . . . . ? C37 N9 C50 C55 -84.8(6) . . . . ? C36 N9 C50 C55 100.6(6) . . . . ? C37 N9 C50 C51 98.3(6) . . . . ? C36 N9 C50 C51 -76.3(6) . . . . ? C55 C50 C51 C52 1.6(7) . . . . ? N9 C50 C51 C52 178.3(4) . . . . ? C55 C50 C51 C56 -178.3(5) . . . . ? N9 C50 C51 C56 -1.6(7) . . . . ? C50 C51 C52 C53 0.6(8) . . . . ? C56 C51 C52 C53 -179.5(5) . . . . ? C51 C52 C53 C54 -2.0(9) . . . . ? C52 C53 C54 C55 1.2(9) . . . . ? C51 C50 C55 C54 -2.3(8) . . . . ? N9 C50 C55 C54 -179.0(5) . . . . ? C51 C50 C55 C59 176.0(5) . . . . ? N9 C50 C55 C59 -0.7(7) . . . . ? C53 C54 C55 C50 0.9(8) . . . . ? C53 C54 C55 C59 -177.4(5) . . . . ? C50 C51 C56 C58 -134.6(5) . . . . ? C52 C51 C56 C58 45.5(7) . . . . ? C50 C51 C56 C57 104.0(6) . . . . ? C52 C51 C56 C57 -75.8(6) . . . . ? C50 C55 C59 C60 147.8(5) . . . . ? C54 C55 C59 C60 -34.0(7) . . . . ? C50 C55 C59 C61 -84.2(6) . . . . ? C54 C55 C59 C61 94.0(6) . . . . ? C27 Rh2 C62 C63 101.6(4) . . . . ? N6 Rh2 C62 C63 -176.4(4) . . . . ? C67 Rh2 C62 C63 -106.7(4) . . . . ? C66 Rh2 C62 C63 -73.1(4) . . . . ? C27 Rh2 C62 C69 -137.4(5) . . . . ? N6 Rh2 C62 C69 -55.4(8) . . . . ? C63 Rh2 C62 C69 121.0(7) . . . . ? C67 Rh2 C62 C69 14.3(5) . . . . ? C66 Rh2 C62 C69 47.9(6) . . . . ? C69 C62 C63 C64 0.4(10) . . . . ? Rh2 C62 C63 C64 104.1(6) . . . . ? C69 C62 C63 Rh2 -103.6(6) . . . . ? C27 Rh2 C63 C62 -81.0(4) . . . . ? N6 Rh2 C63 C62 174.1(6) . . . . ? C67 Rh2 C63 C62 71.8(4) . . . . ? C66 Rh2 C63 C62 105.0(4) . . . . ? C27 Rh2 C63 C64 157.4(4) . . . . ? N6 Rh2 C63 C64 52.5(10) . . . . ? C62 Rh2 C63 C64 -121.6(6) . . . . ? C67 Rh2 C63 C64 -49.8(5) . . . . ? C66 Rh2 C63 C64 -16.6(5) . . . . ? C62 C63 C64 C65 -64.9(9) . . . . ? Rh2 C63 C64 C65 16.9(8) . . . . ? C63 C64 C65 C66 -5.2(11) . . . . ? C64 C65 C66 C67 71.6(10) . . . . ? C64 C65 C66 Rh2 -8.6(10) . . . . ? C27 Rh2 C66 C67 169.3(17) . . . . ? N6 Rh2 C66 C67 84.9(4) . . . . ? C62 Rh2 C66 C67 -72.4(4) . . . . ? C63 Rh2 C66 C67 -108.1(4) . . . . ? C27 Rh2 C66 C65 -69(2) . . . . ? N6 Rh2 C66 C65 -153.4(6) . . . . ? C62 Rh2 C66 C65 49.3(6) . . . . ? C63 Rh2 C66 C65 13.5(6) . . . . ? C67 Rh2 C66 C65 121.7(7) . . . . ? C65 C66 C67 C68 1.5(11) . . . . ? Rh2 C66 C67 C68 102.0(7) . . . . ? C65 C66 C67 Rh2 -100.6(6) . . . . ? C27 Rh2 C67 C66 -177.7(4) . . . . ? N6 Rh2 C67 C66 -95.9(4) . . . . ? C62 Rh2 C67 C66 105.9(4) . . . . ? C63 Rh2 C67 C66 70.4(4) . . . . ? C27 Rh2 C67 C68 61.0(8) . . . . ? N6 Rh2 C67 C68 142.8(6) . . . . ? C62 Rh2 C67 C68 -15.4(6) . . . . ? C63 Rh2 C67 C68 -50.9(6) . . . . ? C66 Rh2 C67 C68 -121.3(8) . . . . ? C66 C67 C68 C69 -68.1(11) . . . . ? Rh2 C67 C68 C69 14.6(11) . . . . ? C67 C68 C69 C62 -3.0(13) . . . . ? C63 C62 C69 C68 71.4(10) . . . . ? Rh2 C62 C69 C68 -10.6(10) . . . . ? C37 Rh3 C70 C71 173.6(12) . . . . ? C74 Rh3 C70 C71 -75.8(5) . . . . ? N7 Rh3 C70 C71 79.6(4) . . . . ? C75 Rh3 C70 C71 -111.1(5) . . . . ? C37 Rh3 C70 C77 -67.0(15) . . . . ? C74 Rh3 C70 C77 43.7(6) . . . . ? N7 Rh3 C70 C77 -161.0(6) . . . . ? C75 Rh3 C70 C77 8.4(6) . . . . ? C71 Rh3 C70 C77 119.4(8) . . . . ? C77 C70 C71 C72 -2.9(12) . . . . ? Rh3 C70 C71 C72 99.2(8) . . . . ? C77 C70 C71 Rh3 -102.1(7) . . . . ? C37 Rh3 C71 C70 -177.4(5) . . . . ? C74 Rh3 C71 C70 102.4(5) . . . . ? N7 Rh3 C71 C70 -101.6(4) . . . . ? C75 Rh3 C71 C70 67.1(5) . . . . ? C37 Rh3 C71 C72 57.6(9) . . . . ? C74 Rh3 C71 C72 -22.6(6) . . . . ? N7 Rh3 C71 C72 133.4(6) . . . . ? C75 Rh3 C71 C72 -57.9(6) . . . . ? C70 Rh3 C71 C72 -125.0(8) . . . . ? C70 C71 C72 C73 -54.5(13) . . . . ? Rh3 C71 C72 C73 27.7(11) . . . . ? C71 C72 C73 C74 -17.0(15) . . . . ? C72 C73 C74 C75 78.0(13) . . . . ? C72 C73 C74 Rh3 -3.5(12) . . . . ? C37 Rh3 C74 C75 98.9(4) . . . . ? N7 Rh3 C74 C75 -176.8(4) . . . . ? C71 Rh3 C74 C75 -106.2(4) . . . . ? C70 Rh3 C74 C75 -71.8(4) . . . . ? C37 Rh3 C74 C73 -140.3(6) . . . . ? N7 Rh3 C74 C73 -56.1(8) . . . . ? C75 Rh3 C74 C73 120.8(7) . . . . ? C71 Rh3 C74 C73 14.5(6) . . . . ? C70 Rh3 C74 C73 48.9(6) . . . . ? C73 C74 C75 C76 0.4(11) . . . . ? Rh3 C74 C75 C76 100.9(7) . . . . ? C73 C74 C75 Rh3 -100.6(7) . . . . ? C37 Rh3 C75 C74 -84.2(4) . . . . ? N7 Rh3 C75 C74 173.1(8) . . . . ? C71 Rh3 C75 C74 72.7(4) . . . . ? C70 Rh3 C75 C74 105.4(4) . . . . ? C37 Rh3 C75 C76 152.5(5) . . . . ? C74 Rh3 C75 C76 -123.2(7) . . . . ? N7 Rh3 C75 C76 49.9(12) . . . . ? C71 Rh3 C75 C76 -50.6(5) . . . . ? C70 Rh3 C75 C76 -17.8(5) . . . . ? C74 C75 C76 C77 -53.7(11) . . . . ? Rh3 C75 C76 C77 25.9(9) . . . . ? C75 C76 C77 C70 -20.1(12) . . . . ? C71 C70 C77 C76 84.2(11) . . . . ? Rh3 C70 C77 C76 4.2(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.736 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.073 # Attachment 'I2salt.cif' data_07065 _database_code_depnum_ccdc_archive 'CCDC 648822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 07065 _chemical_melting_point ? _chemical_formula_moiety 'C35 H46 N6, 2(I)' _chemical_formula_sum 'C35 H46 I2 N6' _chemical_formula_weight 804.58 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' I I -0.4742 1.8119 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7975(7) _cell_length_b 17.8932(17) _cell_length_c 13.1964(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.196(2) _cell_angle_gamma 90.00 _cell_volume 1830.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4052 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.02 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5413 _exptl_absorpt_correction_T_max 0.7793 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details 'S.-J. Jeon/Prof. R. Waymouth-Stanford University' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14689 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3247 _reflns_number_gt 2974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHEXTL, Bruker' _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^)+(0.0587P)^2^+7.8687P] 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 3247 _refine_ls_number_parameters 209 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.009 _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 I1 I 0.63932(5) 0.58677(2) 0.77568(3) 0.04955(16) Uani 1 1 d . . . N1 N 0.3165(4) 0.74674(19) 0.5329(3) 0.0253(7) Uani 1 1 d . . . N2 N 0.1552(5) 0.66423(19) 0.5934(3) 0.0273(8) Uani 1 1 d . A . C1 C 0.3171(6) 0.6861(2) 0.5915(3) 0.0276(9) Uani 1 1 d . . . H1 H 0.4162 0.6627 0.6258 0.033 Uiso 1 1 calc R . . C2 C 0.0481(6) 0.7109(3) 0.5338(3) 0.0327(10) Uani 1 1 d . . . H2 H -0.0740 0.7074 0.5217 0.039 Uiso 1 1 calc R . . C3 C 0.1483(6) 0.7626(2) 0.4955(3) 0.0306(9) Uani 1 1 d . . . H3 H 0.1105 0.8025 0.4511 0.037 Uiso 1 1 calc R . . C4 C 0.4689(5) 0.7869(2) 0.5079(3) 0.0265(9) Uani 1 1 d . . . C5 C 0.5499(5) 0.7601(2) 0.4261(3) 0.0300(9) Uani 1 1 d . . . C6 C 0.6938(6) 0.8010(3) 0.4026(4) 0.0353(10) Uani 1 1 d . . . H6 H 0.7545 0.7854 0.3477 0.042 Uiso 1 1 calc R . . C7 C 0.7488(6) 0.8638(3) 0.4582(4) 0.0370(11) Uani 1 1 d . . . H7 H 0.8461 0.8908 0.4404 0.044 Uiso 1 1 calc R . . C8 C 0.6653(6) 0.8876(3) 0.5385(4) 0.0355(10) Uani 1 1 d . . . H8 H 0.7061 0.9306 0.5760 0.043 Uiso 1 1 calc R . . C9 C 0.5202(6) 0.8493(2) 0.5659(3) 0.0295(9) Uani 1 1 d . . . C10 C 0.4889(6) 0.6904(3) 0.3673(3) 0.0352(10) Uani 1 1 d . . . H10 H 0.3686 0.6797 0.3828 0.042 Uiso 1 1 calc R . . C11 C 0.6005(8) 0.6230(3) 0.4024(5) 0.0517(14) Uani 1 1 d . . . H11A H 0.5581 0.5786 0.3641 0.078 Uiso 1 1 calc R . . H11B H 0.5946 0.6146 0.4753 0.078 Uiso 1 1 calc R . . H11C H 0.7203 0.6327 0.3903 0.078 Uiso 1 1 calc R . . C12 C 0.4831(8) 0.7016(4) 0.2521(4) 0.0534(14) Uani 1 1 d . . . H12A H 0.4049 0.7430 0.2309 0.080 Uiso 1 1 calc R . . H12B H 0.4417 0.6558 0.2169 0.080 Uiso 1 1 calc R . . H12C H 0.5991 0.7133 0.2346 0.080 Uiso 1 1 calc R . . C13 C 0.4268(6) 0.8762(3) 0.6540(4) 0.0337(10) Uani 1 1 d . . . H13 H 0.3277 0.8415 0.6597 0.040 Uiso 1 1 calc R . . C14 C 0.3528(9) 0.9542(3) 0.6339(5) 0.0597(16) Uani 1 1 d . . . H14A H 0.2793 0.9673 0.6870 0.090 Uiso 1 1 calc R . . H14B H 0.2842 0.9553 0.5671 0.090 Uiso 1 1 calc R . . H14C H 0.4473 0.9904 0.6346 0.090 Uiso 1 1 calc R . . C15 C 0.5418(8) 0.8729(4) 0.7539(4) 0.0596(16) Uani 1 1 d . . . H15A H 0.4752 0.8871 0.8098 0.089 Uiso 1 1 calc R . . H15B H 0.6387 0.9075 0.7515 0.089 Uiso 1 1 calc R . . H15C H 0.5858 0.8219 0.7652 0.089 Uiso 1 1 calc R . . C16 C 0.1058(7) 0.5938(2) 0.6404(4) 0.0385(11) Uani 1 1 d . . . H16A H 0.0133 0.6029 0.6813 0.046 Uiso 1 1 d R A . H16B H 0.2018 0.5738 0.6836 0.046 Uiso 1 1 d R . . C17 C 0.0731(11) 0.5387(7) 0.5445(7) 0.0289(16) Uani 0.50 1 d PDU A -1 C18 C -0.0713(10) 0.4957(5) 0.5102(7) 0.0352(19) Uani 0.50 1 d PDU A -1 H18A H -0.1822 0.4942 0.5355 0.042 Uiso 0.50 1 d PR A -1 C19 C -0.0230(11) 0.4596(7) 0.4254(7) 0.0289(16) Uani 0.50 1 d PDU . -1 N3 N 0.2035(9) 0.5312(4) 0.4882(5) 0.0340(12) Uani 0.50 1 d PDU A -1 N4 N 0.1404(8) 0.4815(4) 0.4161(5) 0.0340(12) Uani 0.50 1 d PDU A -1 H4A H 0.1956 0.4630 0.3652 0.041 Uiso 0.50 1 d PR A -1 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 I1 0.0453(2) 0.0571(3) 0.0462(2) 0.00017(16) 0.00505(16) 0.01528(16) N1 0.0268(17) 0.0221(17) 0.0278(17) 0.0022(14) 0.0066(14) -0.0016(14) N2 0.036(2) 0.0192(17) 0.0272(18) -0.0014(14) 0.0064(15) -0.0056(14) C1 0.032(2) 0.024(2) 0.027(2) 0.0002(16) 0.0057(17) 0.0006(17) C2 0.028(2) 0.036(2) 0.034(2) -0.0020(19) 0.0024(18) -0.0030(18) C3 0.029(2) 0.030(2) 0.033(2) 0.0027(18) 0.0015(17) 0.0036(18) C4 0.022(2) 0.025(2) 0.033(2) 0.0086(17) 0.0047(16) -0.0005(16) C5 0.027(2) 0.033(2) 0.030(2) 0.0064(18) 0.0047(17) 0.0045(18) C6 0.031(2) 0.042(3) 0.035(2) 0.010(2) 0.0131(19) 0.005(2) C7 0.028(2) 0.035(2) 0.050(3) 0.015(2) 0.010(2) -0.0020(19) C8 0.033(2) 0.030(2) 0.044(3) 0.005(2) 0.007(2) -0.0038(19) C9 0.028(2) 0.028(2) 0.033(2) 0.0065(18) 0.0052(17) 0.0023(17) C10 0.034(2) 0.042(3) 0.031(2) -0.004(2) 0.0098(19) 0.000(2) C11 0.058(3) 0.037(3) 0.061(3) -0.009(3) 0.007(3) 0.006(2) C12 0.053(3) 0.076(4) 0.034(3) -0.006(3) 0.015(2) -0.002(3) C13 0.035(2) 0.029(2) 0.038(2) -0.0036(19) 0.0127(19) -0.0072(19) C14 0.069(4) 0.040(3) 0.074(4) -0.005(3) 0.023(3) 0.015(3) C15 0.053(3) 0.085(5) 0.042(3) -0.004(3) 0.009(3) 0.000(3) C16 0.047(3) 0.029(2) 0.043(3) 0.0053(19) 0.018(2) -0.007(2) C17 0.037(5) 0.021(3) 0.031(6) 0.004(4) 0.014(3) -0.004(4) C18 0.040(4) 0.025(5) 0.044(5) 0.002(4) 0.015(4) -0.003(4) C19 0.037(5) 0.021(3) 0.031(6) 0.004(4) 0.014(3) -0.004(4) N3 0.038(3) 0.027(3) 0.039(3) -0.008(2) 0.016(2) -0.006(2) N4 0.038(3) 0.027(3) 0.039(3) -0.008(2) 0.016(2) -0.006(2) _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 N1 C1 1.332(5) . ? N1 C3 1.380(6) . ? N1 C4 1.457(5) . ? N2 C1 1.324(6) . ? N2 C2 1.368(6) . ? N2 C16 1.473(5) . ? C1 H1 0.9500 . ? C2 C3 1.344(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.387(6) . ? C4 C5 1.393(6) . ? C5 C6 1.402(6) . ? C5 C10 1.518(6) . ? C6 C7 1.383(7) . ? C6 H6 0.9500 . ? C7 C8 1.370(7) . ? C7 H7 0.9500 . ? C8 C9 1.404(6) . ? C8 H8 0.9500 . ? C9 C13 1.515(6) . ? C10 C12 1.529(7) . ? C10 C11 1.530(7) . ? C10 H10 1.0000 . ? 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 C15 1.514(7) . ? C13 C14 1.524(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.401(10) 3_566 ? C16 C17 1.603(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 N3 1.330(5) . ? C17 C18 1.397(5) . ? C18 C19 1.380(5) . ? C18 H18A 0.9600 . ? C19 N4 1.351(5) . ? C19 C16 1.401(10) 3_566 ? N3 N4 1.355(5) . ? N4 H4A 0.9001 . ? 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 N1 C3 108.5(4) . . ? C1 N1 C4 125.6(4) . . ? C3 N1 C4 125.8(3) . . ? C1 N2 C2 109.4(4) . . ? C1 N2 C16 123.6(4) . . ? C2 N2 C16 126.3(4) . . ? N2 C1 N1 108.0(4) . . ? N2 C1 H1 126.0 . . ? N1 C1 H1 126.0 . . ? C3 C2 N2 107.0(4) . . ? C3 C2 H2 126.5 . . ? N2 C2 H2 126.5 . . ? C2 C3 N1 107.1(4) . . ? C2 C3 H3 126.5 . . ? N1 C3 H3 126.5 . . ? C9 C4 C5 125.2(4) . . ? C9 C4 N1 117.7(4) . . ? C5 C4 N1 117.0(4) . . ? C4 C5 C6 115.6(4) . . ? C4 C5 C10 122.4(4) . . ? C6 C5 C10 122.0(4) . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 121.1(4) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 120.7(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C4 C9 C8 116.3(4) . . ? C4 C9 C13 123.0(4) . . ? C8 C9 C13 120.6(4) . . ? C5 C10 C12 112.0(4) . . ? C5 C10 C11 110.8(4) . . ? C12 C10 C11 111.1(4) . . ? C5 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? 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 . . ? C15 C13 C9 111.6(4) . . ? C15 C13 C14 111.4(5) . . ? C9 C13 C14 111.3(4) . . ? C15 C13 H13 107.5 . . ? C9 C13 H13 107.5 . . ? C14 C13 H13 107.5 . . ? 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 . . ? C19 C16 N2 116.5(6) 3_566 . ? C19 C16 C17 21.2(3) 3_566 . ? N2 C16 C17 102.8(5) . . ? C19 C16 H16A 98.1 3_566 . ? N2 C16 H16A 109.7 . . ? C17 C16 H16A 118.9 . . ? C19 C16 H16B 113.0 3_566 . ? N2 C16 H16B 110.3 . . ? C17 C16 H16B 106.6 . . ? H16A C16 H16B 108.3 . . ? N3 C17 C18 113.7(7) . . ? N3 C17 C16 115.9(6) . . ? C18 C17 C16 130.4(6) . . ? C19 C18 C17 103.9(7) . . ? C19 C18 H18A 127.1 . . ? C17 C18 H18A 128.9 . . ? N4 C19 C18 106.3(7) . . ? N4 C19 C16 121.2(6) . 3_566 ? C18 C19 C16 132.4(6) . 3_566 ? C17 N3 N4 102.5(7) . . ? C19 N4 N3 113.7(7) . . ? C19 N4 H4A 119.5 . . ? N3 N4 H4A 126.8 . . ? 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 C2 N2 C1 N1 0.9(5) . . . . ? C16 N2 C1 N1 172.4(4) . . . . ? C3 N1 C1 N2 -1.0(5) . . . . ? C4 N1 C1 N2 -177.8(4) . . . . ? C1 N2 C2 C3 -0.5(5) . . . . ? C16 N2 C2 C3 -171.7(4) . . . . ? N2 C2 C3 N1 -0.2(5) . . . . ? C1 N1 C3 C2 0.7(5) . . . . ? C4 N1 C3 C2 177.5(4) . . . . ? C1 N1 C4 C9 -96.5(5) . . . . ? C3 N1 C4 C9 87.2(5) . . . . ? C1 N1 C4 C5 84.6(5) . . . . ? C3 N1 C4 C5 -91.7(5) . . . . ? C9 C4 C5 C6 -0.3(6) . . . . ? N1 C4 C5 C6 178.6(4) . . . . ? C9 C4 C5 C10 178.7(4) . . . . ? N1 C4 C5 C10 -2.5(6) . . . . ? C4 C5 C6 C7 -0.1(6) . . . . ? C10 C5 C6 C7 -179.0(4) . . . . ? C5 C6 C7 C8 0.5(7) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C5 C4 C9 C8 0.1(6) . . . . ? N1 C4 C9 C8 -178.7(4) . . . . ? C5 C4 C9 C13 179.7(4) . . . . ? N1 C4 C9 C13 0.9(6) . . . . ? C7 C8 C9 C4 0.3(7) . . . . ? C7 C8 C9 C13 -179.3(4) . . . . ? C4 C5 C10 C12 135.4(5) . . . . ? C6 C5 C10 C12 -45.7(6) . . . . ? C4 C5 C10 C11 -100.0(5) . . . . ? C6 C5 C10 C11 78.9(5) . . . . ? C4 C9 C13 C15 117.3(5) . . . . ? C8 C9 C13 C15 -63.1(6) . . . . ? C4 C9 C13 C14 -117.6(5) . . . . ? C8 C9 C13 C14 61.9(6) . . . . ? C1 N2 C16 C19 -115.3(6) . . . 3_566 ? C2 N2 C16 C19 54.7(7) . . . 3_566 ? C1 N2 C16 C17 -98.1(6) . . . . ? C2 N2 C16 C17 71.9(6) . . . . ? C19 C16 C17 N3 -171(3) 3_566 . . . ? N2 C16 C17 N3 55.6(11) . . . . ? C19 C16 C17 C18 7.8(17) 3_566 . . . ? N2 C16 C17 C18 -125.3(12) . . . . ? N3 C17 C18 C19 -0.3(17) . . . . ? C16 C17 C18 C19 -179.5(8) . . . . ? C17 C18 C19 N4 0.9(16) . . . . ? C17 C18 C19 C16 176.5(9) . . . 3_566 ? C18 C17 N3 N4 -0.4(13) . . . . ? C16 C17 N3 N4 179.0(8) . . . . ? C18 C19 N4 N3 -1.2(13) . . . . ? C16 C19 N4 N3 -177.4(9) 3_566 . . . ? C17 N3 N4 C19 1.0(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 I1 0.95 2.84 3.750(4) 161.9 . N4 H4A I1 0.90 2.53 3.434(6) 178.0 3_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.020 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.099