# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sad _database_code_depnum_ccdc_archive 'CCDC 905534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H76 F18 N13 O P3 Pd3' _chemical_formula_weight 1713.42 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbam 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' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 23.388(3) _cell_length_b 28.553(5) _cell_length_c 10.7407(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7172.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8397 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70502 _diffrn_reflns_av_R_equivalents 0.1187 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.92 _reflns_number_total 8983 _reflns_number_gt 5590 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1368P)^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_number_reflns 8983 _refine_ls_number_parameters 470 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.059 _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 Pd1 Pd 0.35683(3) 0.17255(2) 0.5000 0.02716(19) Uani 1 2 d S . . Pd2 Pd 0.57565(3) 0.34358(2) 0.5000 0.0293(2) Uani 1 2 d S . . Pd3 Pd 0.65642(3) 0.11059(3) 0.5000 0.0310(2) Uani 1 2 d S . . C101 C 0.3176(5) 0.2411(4) 0.5000 0.050(3) Uani 1 2 d S . . H101 H 0.3362 0.2707 0.5000 0.060 Uiso 1 2 calc SR . . C102 C 0.3045(3) 0.2202(3) 0.3866(7) 0.0445(18) Uani 1 1 d . . . H10A H 0.2859 0.1906 0.3849 0.053 Uiso 1 1 calc R . . H10B H 0.3141 0.2354 0.3108 0.053 Uiso 1 1 calc R . . C201 C 0.6670(4) 0.3327(4) 0.5000 0.051(3) Uani 1 2 d S . . H201 H 0.6873 0.3038 0.5000 0.061 Uiso 1 2 calc SR . . C202 C 0.6526(3) 0.3531(3) 0.3858(8) 0.0461(19) Uani 1 1 d . . . H20A H 0.6323 0.3819 0.3840 0.055 Uiso 1 1 calc R . . H20B H 0.6631 0.3382 0.3101 0.055 Uiso 1 1 calc R . . C301 C 0.6135(6) 0.0435(4) 0.5000 0.062(3) Uani 1 2 d S . . H301 H 0.5739 0.0362 0.5000 0.074 Uiso 1 2 calc SR . . C302 C 0.6409(4) 0.0485(3) 0.3859(8) 0.052(2) Uani 1 1 d . . . H30A H 0.6805 0.0557 0.3830 0.062 Uiso 1 1 calc R . . H30B H 0.6199 0.0447 0.3107 0.062 Uiso 1 1 calc R . . C1 C 0.4862(3) 0.1713(2) 0.3271(6) 0.0274(13) Uani 1 1 d . . . C2 C 0.4663(3) 0.2177(2) 0.3289(6) 0.0301(14) Uani 1 1 d . . . H2 H 0.4265 0.2240 0.3299 0.036 Uiso 1 1 calc R . . C3 C 0.5055(3) 0.2541(2) 0.3292(6) 0.0288(13) Uani 1 1 d . . . C4 C 0.5645(3) 0.2447(2) 0.3271(6) 0.0301(14) Uani 1 1 d . . . H4 H 0.5912 0.2698 0.3275 0.036 Uiso 1 1 calc R . . C5 C 0.5834(3) 0.1986(2) 0.3243(6) 0.0288(13) Uani 1 1 d . . . C6 C 0.5448(3) 0.1614(2) 0.3265(6) 0.0295(14) Uani 1 1 d . . . H6 H 0.5581 0.1300 0.3276 0.035 Uiso 1 1 calc R . . N11 N 0.4462(2) 0.13350(19) 0.3110(5) 0.0314(12) Uani 1 1 d . . . C12 C 0.3920(3) 0.1317(2) 0.3606(6) 0.0298(14) Uani 1 1 d . . . N13 N 0.3680(2) 0.09339(19) 0.3080(6) 0.0359(13) Uani 1 1 d . . . C14 C 0.4052(3) 0.0713(3) 0.2264(8) 0.0442(18) Uani 1 1 d . . . H14 H 0.3975 0.0443 0.1778 0.053 Uiso 1 1 calc R . . C15 C 0.4551(3) 0.0960(3) 0.2295(8) 0.0445(18) Uani 1 1 d . . . H15 H 0.4892 0.0891 0.1851 0.053 Uiso 1 1 calc R . . C16 C 0.3086(3) 0.0780(3) 0.3276(8) 0.0430(18) Uani 1 1 d . . . H16A H 0.2900 0.0989 0.3890 0.052 Uiso 1 1 calc R . . H16B H 0.3086 0.0459 0.3625 0.052 Uiso 1 1 calc R . . C17 C 0.2747(4) 0.0784(4) 0.2092(10) 0.081(3) Uani 1 1 d . . . H17A H 0.2698 0.1107 0.1807 0.122 Uiso 1 1 calc R . . H17B H 0.2371 0.0643 0.2241 0.122 Uiso 1 1 calc R . . H17C H 0.2950 0.0603 0.1454 0.122 Uiso 1 1 calc R . . N21 N 0.4865(2) 0.30180(18) 0.3157(5) 0.0307(12) Uani 1 1 d . . . C22 C 0.5142(3) 0.3406(2) 0.3631(6) 0.0312(14) Uani 1 1 d . . . N23 N 0.4881(2) 0.3776(2) 0.3068(6) 0.0355(13) Uani 1 1 d . . . C24 C 0.4451(3) 0.3624(3) 0.2270(8) 0.0458(18) Uani 1 1 d . . . H24 H 0.4211 0.3818 0.1778 0.055 Uiso 1 1 calc R . . C25 C 0.4437(3) 0.3153(2) 0.2316(7) 0.0400(17) Uani 1 1 d . . . H25 H 0.4187 0.2952 0.1869 0.048 Uiso 1 1 calc R . . C26 C 0.5068(3) 0.4268(2) 0.3186(7) 0.0450(18) Uani 1 1 d . . . H26A H 0.5313 0.4302 0.3933 0.054 Uiso 1 1 calc R . . H26B H 0.4729 0.4472 0.3296 0.054 Uiso 1 1 calc R . . C27 C 0.5400(4) 0.4426(3) 0.2044(8) 0.051(2) Uani 1 1 d . . . H27A H 0.5716 0.4208 0.1890 0.076 Uiso 1 1 calc R . . H27B H 0.5552 0.4741 0.2185 0.076 Uiso 1 1 calc R . . H27C H 0.5145 0.4430 0.1320 0.076 Uiso 1 1 calc R . . N31 N 0.6435(2) 0.19056(19) 0.3049(5) 0.0313(12) Uani 1 1 d . . . C32 C 0.6767(3) 0.1562(2) 0.3580(6) 0.0311(14) Uani 1 1 d . . . N33 N 0.7281(2) 0.1609(2) 0.3001(6) 0.0345(13) Uani 1 1 d . . . C34 C 0.7274(3) 0.1962(3) 0.2144(7) 0.0397(17) Uani 1 1 d . . . H34 H 0.7587 0.2059 0.1643 0.048 Uiso 1 1 calc R . . C35 C 0.6741(3) 0.2152(2) 0.2131(6) 0.0348(15) Uani 1 1 d . . . H35 H 0.6605 0.2398 0.1614 0.042 Uiso 1 1 calc R . . C36 C 0.7773(3) 0.1290(3) 0.3206(7) 0.0465(19) Uani 1 1 d . . . H36A H 0.7682 0.1071 0.3893 0.056 Uiso 1 1 calc R . . H36B H 0.8112 0.1475 0.3455 0.056 Uiso 1 1 calc R . . C37 C 0.7909(4) 0.1016(4) 0.2051(9) 0.072(3) Uani 1 1 d . . . H37A H 0.7568 0.0843 0.1783 0.108 Uiso 1 1 calc R . . H37B H 0.8219 0.0795 0.2226 0.108 Uiso 1 1 calc R . . H37C H 0.8027 0.1231 0.1388 0.108 Uiso 1 1 calc R . . P1 P 0.84251(16) 0.28738(14) 0.0000 0.0580(9) Uani 1 2 d S . . F11 F 0.8456(7) 0.3412(6) 0.0000 0.194(7) Uani 1 2 d SU . . F12 F 0.8355(6) 0.2357(5) 0.0000 0.185(6) Uani 1 2 d SU . . F13 F 0.7879(4) 0.2937(4) 0.0925(11) 0.178(4) Uani 1 1 d U . . F14 F 0.8855(5) 0.2861(5) 0.0985(11) 0.205(5) Uani 1 1 d U . . P2 P 0.37592(15) -0.06228(13) 0.0000 0.0566(8) Uani 1 2 d S . . F21 F 0.3352(4) -0.0331(3) -0.0988(9) 0.147(3) Uani 1 1 d U . . F22 F 0.4097(5) -0.0849(4) -0.0973(10) 0.186(4) Uani 1 1 d U . . F23 F 0.3312(8) -0.0988(7) 0.0000 0.204(7) Uani 1 2 d SU . . F24 F 0.4138(8) -0.0197(7) 0.0000 0.220(8) Uani 1 2 d SU . . P3 P 0.65394(16) 0.50792(13) 0.5000 0.0656(10) Uani 1 2 d S . . F31 F 0.7163(4) 0.5290(3) 0.5000 0.105(3) Uani 1 2 d SU . . F32 F 0.5913(4) 0.4871(4) 0.5000 0.125(4) Uani 1 2 d SU . . F33 F 0.6306(4) 0.5583(4) 0.5000 0.121(4) Uani 1 2 d SU . . F34 F 0.6816(7) 0.4575(5) 0.5000 0.172(6) Uani 1 2 d SU . . F35 F 0.6536(4) 0.5060(4) 0.3567(9) 0.163(4) Uani 1 1 d U . . N801 N 0.9061(5) 0.0516(4) 0.0000 0.059(3) Uani 1 2 d S . . C802 C 0.8692(6) 0.0282(4) 0.0000 0.049(3) Uani 1 2 d S . . C803 C 0.8208(7) -0.0022(6) 0.0000 0.102(6) Uani 1 2 d S . . H80A H 0.8314 -0.0323 0.0374 0.153 Uiso 0.50 1 calc PR . . H80B H 0.8080 -0.0073 -0.0858 0.153 Uiso 0.50 1 calc PR . . H80C H 0.7898 0.0121 0.0484 0.153 Uiso 0.50 1 calc PR . . O901 O 0.5942(4) 0.2752(3) 0.0000 0.065(2) Uani 1 2 d S . . C902 C 0.5415(7) 0.2514(8) 0.0000 0.092(6) Uani 1 2 d S . . H90A H 0.5195 0.2612 -0.0744 0.110 Uiso 0.50 1 calc PR . . H90B H 0.5195 0.2612 0.0744 0.110 Uiso 0.50 1 calc PR . . C903 C 0.5459(9) 0.2008(5) 0.0000 0.088(5) Uani 1 2 d S . . H90C H 0.5367 0.1888 -0.0831 0.132 Uiso 0.50 1 calc PR . . H90D H 0.5190 0.1878 0.0608 0.132 Uiso 0.50 1 calc PR . . H90E H 0.5849 0.1916 0.0222 0.132 Uiso 0.50 1 calc PR . . C904 C 0.5893(8) 0.3227(6) 0.0000 0.087(5) Uani 1 2 d S . . H90F H 0.5683 0.3334 0.0749 0.105 Uiso 0.50 1 calc PR . . H90G H 0.5683 0.3334 -0.0749 0.105 Uiso 0.50 1 calc PR . . C905 C 0.6519(8) 0.3429(6) 0.0000 0.087(5) Uani 1 2 d S . . H90H H 0.6611 0.3550 0.0830 0.130 Uiso 0.50 1 calc PR . . H90I H 0.6547 0.3683 -0.0610 0.130 Uiso 0.50 1 calc PR . . H90J H 0.6789 0.3180 -0.0220 0.130 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0225(3) 0.0281(4) 0.0309(4) 0.000 0.000 0.0001(3) Pd2 0.0276(4) 0.0248(4) 0.0356(4) 0.000 0.000 -0.0006(3) Pd3 0.0319(4) 0.0290(4) 0.0321(4) 0.000 0.000 0.0073(3) C101 0.043(6) 0.042(6) 0.066(8) 0.000 0.000 0.018(5) C102 0.041(4) 0.049(4) 0.043(4) 0.011(4) -0.004(3) 0.014(3) C201 0.024(5) 0.055(7) 0.074(9) 0.000 0.000 0.001(5) C202 0.036(4) 0.044(4) 0.058(5) 0.002(4) 0.014(4) 0.001(3) C301 0.072(9) 0.038(7) 0.075(10) 0.000 0.000 0.003(6) C302 0.074(6) 0.033(4) 0.047(5) -0.011(4) 0.001(4) -0.009(4) C1 0.026(3) 0.028(3) 0.028(3) -0.002(3) 0.001(2) 0.000(2) C2 0.024(3) 0.031(3) 0.035(4) -0.002(3) 0.001(3) 0.004(2) C3 0.032(3) 0.028(3) 0.027(3) -0.001(3) -0.001(3) 0.005(3) C4 0.031(3) 0.027(3) 0.033(3) -0.001(3) -0.004(3) -0.001(3) C5 0.029(3) 0.030(3) 0.028(3) -0.001(3) -0.003(3) 0.001(2) C6 0.032(3) 0.029(3) 0.027(3) 0.001(3) 0.000(3) 0.006(3) N11 0.031(3) 0.029(3) 0.035(3) -0.004(2) 0.002(2) -0.001(2) C12 0.025(3) 0.030(3) 0.034(4) 0.001(3) 0.001(3) -0.001(2) N13 0.034(3) 0.029(3) 0.044(3) -0.007(3) -0.001(3) -0.005(2) C14 0.044(4) 0.035(4) 0.054(5) -0.016(4) 0.006(4) -0.004(3) C15 0.039(4) 0.042(4) 0.053(5) -0.021(4) 0.007(3) 0.001(3) C16 0.032(4) 0.039(4) 0.058(5) -0.004(4) 0.004(3) -0.008(3) C17 0.048(5) 0.130(10) 0.066(7) -0.018(7) -0.006(5) -0.027(6) N21 0.028(3) 0.027(3) 0.037(3) 0.001(2) -0.002(2) 0.001(2) C22 0.032(3) 0.029(3) 0.033(4) 0.002(3) 0.003(3) 0.005(3) N23 0.039(3) 0.027(3) 0.040(3) 0.001(2) -0.001(3) 0.004(2) C24 0.046(4) 0.042(4) 0.049(5) 0.007(4) -0.011(4) 0.011(3) C25 0.036(4) 0.039(4) 0.045(4) -0.001(3) -0.017(3) 0.005(3) C26 0.057(5) 0.030(4) 0.048(5) 0.004(3) 0.007(4) 0.008(3) C27 0.065(5) 0.038(4) 0.049(5) 0.003(4) 0.002(4) -0.006(4) N31 0.027(3) 0.029(3) 0.038(3) 0.003(2) 0.004(2) 0.002(2) C32 0.028(3) 0.035(3) 0.030(3) -0.004(3) 0.000(3) 0.000(3) N33 0.026(3) 0.042(3) 0.036(3) -0.003(3) 0.000(2) 0.005(2) C34 0.030(3) 0.048(4) 0.041(4) 0.006(3) 0.006(3) -0.004(3) C35 0.030(3) 0.037(4) 0.037(4) 0.004(3) 0.004(3) -0.005(3) C36 0.033(4) 0.061(5) 0.045(4) -0.002(4) 0.001(3) 0.017(3) C37 0.056(5) 0.087(7) 0.072(7) -0.029(6) -0.005(5) 0.032(5) P1 0.073(2) 0.067(2) 0.0343(16) 0.000 0.000 -0.0230(18) F11 0.180(10) 0.169(10) 0.235(11) 0.000 0.000 -0.016(8) F12 0.155(9) 0.116(8) 0.284(11) 0.000 0.000 0.001(7) F13 0.136(6) 0.200(8) 0.197(8) 0.038(7) 0.040(6) 0.041(6) F14 0.195(8) 0.263(9) 0.156(7) 0.023(7) -0.091(6) -0.022(7) P2 0.060(2) 0.060(2) 0.0491(19) 0.000 0.000 -0.0189(16) F21 0.142(6) 0.158(7) 0.140(7) -0.002(5) -0.005(5) 0.056(5) F22 0.200(8) 0.222(8) 0.136(7) -0.042(6) 0.064(6) 0.075(7) F23 0.191(10) 0.177(10) 0.245(11) 0.000 0.000 -0.050(8) F24 0.197(11) 0.188(11) 0.276(12) 0.000 0.000 -0.040(8) P3 0.067(2) 0.051(2) 0.079(3) 0.000 0.000 -0.0287(17) F31 0.078(5) 0.097(6) 0.139(8) 0.000 0.000 -0.025(5) F32 0.104(6) 0.155(8) 0.116(7) 0.000 0.000 -0.082(6) F33 0.096(6) 0.101(7) 0.165(8) 0.000 0.000 0.009(5) F34 0.190(9) 0.122(8) 0.204(10) 0.000 0.000 -0.012(7) F35 0.165(7) 0.210(8) 0.114(6) -0.017(6) 0.009(5) -0.070(6) N801 0.059(6) 0.052(6) 0.066(7) 0.000 0.000 -0.008(5) C802 0.061(7) 0.046(7) 0.039(6) 0.000 0.000 0.002(6) C803 0.089(12) 0.082(12) 0.135(16) 0.000 0.000 -0.049(10) O901 0.074(6) 0.071(7) 0.048(5) 0.000 0.000 0.007(5) C902 0.067(10) 0.17(2) 0.036(7) 0.000 0.000 0.023(11) C903 0.154(17) 0.062(10) 0.049(9) 0.000 0.000 -0.017(10) C904 0.122(15) 0.084(12) 0.056(9) 0.000 0.000 0.033(11) C905 0.124(15) 0.065(10) 0.071(11) 0.000 0.000 0.013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C12 2.068(6) . ? Pd1 C12 2.068(6) 6_556 ? Pd1 C101 2.162(11) . ? Pd1 C102 2.198(7) . ? Pd1 C102 2.198(7) 6_556 ? Pd2 C22 2.057(7) . ? Pd2 C22 2.057(7) 6_556 ? Pd2 C201 2.160(10) . ? Pd2 C202 2.196(7) . ? Pd2 C202 2.196(7) 6_556 ? Pd3 C32 2.060(7) . ? Pd3 C32 2.060(7) 6_556 ? Pd3 C301 2.163(13) . ? Pd3 C302 2.186(8) . ? Pd3 C302 2.186(8) 6_556 ? C101 C102 1.392(10) . ? C101 C102 1.392(10) 6_556 ? C101 H101 0.9500 . ? C102 H10A 0.9500 . ? C102 H10B 0.9500 . ? C201 C202 1.400(10) . ? C201 C202 1.400(10) 6_556 ? C201 H201 0.9500 . ? C202 H20A 0.9500 . ? C202 H20B 0.9500 . ? C301 C302 1.390(10) . ? C301 C302 1.390(10) 6_556 ? C301 H301 0.9500 . ? C302 H30A 0.9500 . ? C302 H30B 0.9500 . ? C1 C6 1.400(8) . ? C1 C2 1.404(9) . ? C1 N11 1.438(8) . ? C2 C3 1.385(9) . ? C2 H2 0.9500 . ? C3 C4 1.406(9) . ? C3 N21 1.440(8) . ? C4 C5 1.390(9) . ? C4 H4 0.9500 . ? C5 C6 1.392(9) . ? C5 N31 1.440(8) . ? C6 H6 0.9500 . ? N11 C12 1.375(8) . ? N11 C15 1.398(9) . ? C12 N13 1.355(8) . ? N13 C14 1.386(9) . ? N13 C16 1.474(8) . ? C14 C15 1.363(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.499(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N21 C22 1.381(8) . ? N21 C25 1.402(8) . ? C22 N23 1.362(8) . ? N23 C24 1.390(9) . ? N23 C26 1.479(9) . ? C24 C25 1.346(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.519(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N31 C32 1.377(8) . ? N31 C35 1.407(8) . ? C32 N33 1.359(8) . ? N33 C34 1.364(9) . ? N33 C36 1.486(8) . ? C34 C35 1.358(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.501(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? P1 F14 1.460(10) . ? P1 F14 1.460(10) 6 ? P1 F12 1.485(15) . ? P1 F11 1.539(18) . ? P1 F13 1.628(10) 6 ? P1 F13 1.628(10) . ? P2 F22 1.460(8) . ? P2 F22 1.460(8) 6 ? P2 F23 1.478(17) . ? P2 F24 1.504(18) . ? P2 F21 1.651(9) . ? P2 F21 1.651(9) 6 ? P3 F33 1.538(12) . ? P3 F35 1.541(10) . ? P3 F35 1.541(10) 6_556 ? P3 F31 1.577(9) . ? P3 F34 1.579(16) . ? P3 F32 1.581(9) . ? N801 C802 1.092(15) . ? C802 C803 1.426(19) . ? C803 H80A 0.9800 . ? C803 H80B 0.9800 . ? C803 H80C 0.9800 . ? O901 C904 1.361(18) . ? O901 C902 1.407(19) . ? C902 C903 1.45(2) . ? C902 H90A 0.9900 . ? C902 H90B 0.9900 . ? C903 H90C 0.9800 . ? C903 H90D 0.9800 . ? C903 H90E 0.9800 . ? C904 C905 1.57(2) . ? C904 H90F 0.9900 . ? C904 H90G 0.9900 . ? C905 H90H 0.9800 . ? C905 H90I 0.9800 . ? C905 H90J 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Pd1 C12 92.7(4) . 6_556 ? C12 Pd1 C101 132.78(19) . . ? C12 Pd1 C101 132.78(19) 6_556 . ? C12 Pd1 C102 99.7(3) . . ? C12 Pd1 C102 166.3(3) 6_556 . ? C101 Pd1 C102 37.2(2) . . ? C12 Pd1 C102 166.3(3) . 6_556 ? C12 Pd1 C102 99.7(3) 6_556 6_556 ? C101 Pd1 C102 37.2(2) . 6_556 ? C102 Pd1 C102 67.3(4) . 6_556 ? C22 Pd2 C22 91.2(4) . 6_556 ? C22 Pd2 C201 133.22(19) . . ? C22 Pd2 C201 133.22(19) 6_556 . ? C22 Pd2 C202 100.3(3) . . ? C22 Pd2 C202 167.7(3) 6_556 . ? C201 Pd2 C202 37.5(2) . . ? C22 Pd2 C202 167.7(3) . 6_556 ? C22 Pd2 C202 100.3(3) 6_556 6_556 ? C201 Pd2 C202 37.5(2) . 6_556 ? C202 Pd2 C202 67.9(4) . 6_556 ? C32 Pd3 C32 95.5(4) . 6_556 ? C32 Pd3 C301 131.79(19) . . ? C32 Pd3 C301 131.79(19) 6_556 . ? C32 Pd3 C302 97.8(3) . . ? C32 Pd3 C302 164.9(3) 6_556 . ? C301 Pd3 C302 37.3(3) . . ? C32 Pd3 C302 164.9(3) . 6_556 ? C32 Pd3 C302 97.8(3) 6_556 6_556 ? C301 Pd3 C302 37.3(3) . 6_556 ? C302 Pd3 C302 68.2(4) . 6_556 ? C102 C101 C102 122.1(12) . 6_556 ? C102 C101 Pd1 72.8(5) . . ? C102 C101 Pd1 72.8(5) 6_556 . ? C102 C101 H101 118.9 . . ? C102 C101 H101 118.9 6_556 . ? Pd1 C101 H101 127.7 . . ? C101 C102 Pd1 70.0(5) . . ? C101 C102 H10A 120.0 . . ? Pd1 C102 H10A 73.4 . . ? C101 C102 H10B 120.0 . . ? Pd1 C102 H10B 128.8 . . ? H10A C102 H10B 120.0 . . ? C202 C201 C202 122.4(11) . 6_556 ? C202 C201 Pd2 72.6(5) . . ? C202 C201 Pd2 72.6(5) 6_556 . ? C202 C201 H201 118.8 . . ? C202 C201 H201 118.8 6_556 . ? Pd2 C201 H201 128.3 . . ? C201 C202 Pd2 69.9(5) . . ? C201 C202 H20A 120.0 . . ? Pd2 C202 H20A 73.1 . . ? C201 C202 H20B 120.0 . . ? Pd2 C202 H20B 129.4 . . ? H20A C202 H20B 120.0 . . ? C302 C301 C302 123.7(13) . 6_556 ? C302 C301 Pd3 72.3(6) . . ? C302 C301 Pd3 72.3(6) 6_556 . ? C302 C301 H301 118.1 . . ? C302 C301 H301 118.1 6_556 . ? Pd3 C301 H301 130.2 . . ? C301 C302 Pd3 70.4(6) . . ? C301 C302 H30A 120.0 . . ? Pd3 C302 H30A 71.3 . . ? C301 C302 H30B 120.0 . . ? Pd3 C302 H30B 130.9 . . ? H30A C302 H30B 120.0 . . ? C6 C1 C2 120.8(6) . . ? C6 C1 N11 119.1(5) . . ? C2 C1 N11 119.6(5) . . ? C3 C2 C1 119.4(6) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.4(6) . . ? C2 C3 N21 120.5(5) . . ? C4 C3 N21 118.7(6) . . ? C5 C4 C3 119.5(6) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 N31 117.7(6) . . ? C6 C5 N31 120.9(6) . . ? C5 C6 C1 118.8(6) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? C12 N11 C15 110.6(5) . . ? C12 N11 C1 125.4(5) . . ? C15 N11 C1 123.6(6) . . ? N13 C12 N11 104.4(5) . . ? N13 C12 Pd1 126.3(5) . . ? N11 C12 Pd1 128.8(5) . . ? C12 N13 C14 111.8(5) . . ? C12 N13 C16 124.9(6) . . ? C14 N13 C16 123.2(6) . . ? C15 C14 N13 106.7(6) . . ? C15 C14 H14 126.7 . . ? N13 C14 H14 126.7 . . ? C14 C15 N11 106.5(6) . . ? C14 C15 H15 126.8 . . ? N11 C15 H15 126.8 . . ? N13 C16 C17 112.1(7) . . ? N13 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N13 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 N21 C25 110.6(5) . . ? C22 N21 C3 125.2(5) . . ? C25 N21 C3 123.1(5) . . ? N23 C22 N21 104.3(6) . . ? N23 C22 Pd2 126.8(5) . . ? N21 C22 Pd2 128.7(5) . . ? C22 N23 C24 110.9(6) . . ? C22 N23 C26 124.5(6) . . ? C24 N23 C26 124.3(6) . . ? C25 C24 N23 107.8(6) . . ? C25 C24 H24 126.1 . . ? N23 C24 H24 126.1 . . ? C24 C25 N21 106.3(6) . . ? C24 C25 H25 126.8 . . ? N21 C25 H25 126.8 . . ? N23 C26 C27 111.3(6) . . ? N23 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? N23 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C32 N31 C35 111.1(5) . . ? C32 N31 C5 127.2(5) . . ? C35 N31 C5 121.3(5) . . ? N33 C32 N31 103.7(6) . . ? N33 C32 Pd3 127.3(5) . . ? N31 C32 Pd3 128.8(5) . . ? C32 N33 C34 111.9(6) . . ? C32 N33 C36 123.7(6) . . ? C34 N33 C36 124.3(6) . . ? C35 C34 N33 108.2(6) . . ? C35 C34 H34 125.9 . . ? N33 C34 H34 125.9 . . ? C34 C35 N31 105.0(6) . . ? C34 C35 H35 127.5 . . ? N31 C35 H35 127.5 . . ? N33 C36 C37 111.2(7) . . ? N33 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? N33 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? F14 P1 F14 92.8(11) . 6 ? F14 P1 F12 93.0(7) . . ? F14 P1 F12 93.0(7) 6 . ? F14 P1 F11 89.5(7) . . ? F14 P1 F11 89.5(7) 6 . ? F12 P1 F11 176.4(9) . . ? F14 P1 F13 170.1(7) . 6 ? F14 P1 F13 95.8(7) 6 6 ? F12 P1 F13 91.4(6) . 6 ? F11 P1 F13 85.8(7) . 6 ? F14 P1 F13 95.8(7) . . ? F14 P1 F13 170.1(7) 6 . ? F12 P1 F13 91.4(6) . . ? F11 P1 F13 85.8(7) . . ? F13 P1 F13 75.3(8) 6 . ? F22 P2 F22 91.4(10) . 6 ? F22 P2 F23 94.1(7) . . ? F22 P2 F23 94.1(7) 6 . ? F22 P2 F24 92.2(7) . . ? F22 P2 F24 92.2(7) 6 . ? F23 P2 F24 171.0(12) . . ? F22 P2 F21 94.3(6) . . ? F22 P2 F21 174.2(6) 6 . ? F23 P2 F21 87.0(7) . . ? F24 P2 F21 86.2(7) . . ? F22 P2 F21 174.2(6) . 6 ? F22 P2 F21 94.3(6) 6 6 ? F23 P2 F21 87.0(7) . 6 ? F24 P2 F21 86.2(7) . 6 ? F21 P2 F21 80.0(7) . 6 ? F33 P3 F35 91.8(5) . . ? F33 P3 F35 91.8(5) . 6_556 ? F35 P3 F35 175.8(9) . 6_556 ? F33 P3 F31 88.4(6) . . ? F35 P3 F31 91.1(4) . . ? F35 P3 F31 91.1(4) 6_556 . ? F33 P3 F34 176.6(8) . . ? F35 P3 F34 88.3(5) . . ? F35 P3 F34 88.3(5) 6_556 . ? F31 P3 F34 88.2(7) . . ? F33 P3 F32 91.2(7) . . ? F35 P3 F32 88.9(4) . . ? F35 P3 F32 88.9(4) 6_556 . ? F31 P3 F32 179.6(7) . . ? F34 P3 F32 92.2(8) . . ? N801 C802 C803 179.8(15) . . ? C802 C803 H80A 109.5 . . ? C802 C803 H80B 109.5 . . ? H80A C803 H80B 109.5 . . ? C802 C803 H80C 109.5 . . ? H80A C803 H80C 109.5 . . ? H80B C803 H80C 109.5 . . ? C904 O901 C902 114.1(14) . . ? O901 C902 C903 114.8(14) . . ? O901 C902 H90A 108.6 . . ? C903 C902 H90A 108.6 . . ? O901 C902 H90B 108.6 . . ? C903 C902 H90B 108.6 . . ? H90A C902 H90B 107.5 . . ? C902 C903 H90C 109.5 . . ? C902 C903 H90D 109.5 . . ? H90C C903 H90D 109.5 . . ? C902 C903 H90E 109.5 . . ? H90C C903 H90E 109.5 . . ? H90D C903 H90E 109.5 . . ? O901 C904 C905 106.7(14) . . ? O901 C904 H90F 110.4 . . ? C905 C904 H90F 110.4 . . ? O901 C904 H90G 110.4 . . ? C905 C904 H90G 110.4 . . ? H90F C904 H90G 108.6 . . ? C904 C905 H90H 109.5 . . ? C904 C905 H90I 109.5 . . ? H90H C905 H90I 109.5 . . ? C904 C905 H90J 109.5 . . ? H90H C905 H90J 109.5 . . ? H90I C905 H90J 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Pd1 C101 C102 33.2(8) . . . . ? C12 Pd1 C101 C102 -165.9(4) 6_556 . . . ? C102 Pd1 C101 C102 -132.8(11) 6_556 . . . ? C12 Pd1 C101 C102 165.9(4) . . . 6_556 ? C12 Pd1 C101 C102 -33.2(8) 6_556 . . 6_556 ? C102 Pd1 C101 C102 132.8(11) . . . 6_556 ? C102 C101 C102 Pd1 -55.9(9) 6_556 . . . ? C12 Pd1 C102 C101 -156.0(6) . . . . ? C12 Pd1 C102 C101 48.8(14) 6_556 . . . ? C102 Pd1 C102 C101 28.8(7) 6_556 . . . ? C22 Pd2 C201 C202 34.6(8) . . . . ? C22 Pd2 C201 C202 -167.9(4) 6_556 . . . ? C202 Pd2 C201 C202 -133.3(11) 6_556 . . . ? C22 Pd2 C201 C202 167.9(4) . . . 6_556 ? C22 Pd2 C201 C202 -34.6(8) 6_556 . . 6_556 ? C202 Pd2 C201 C202 133.3(11) . . . 6_556 ? C202 C201 C202 Pd2 -55.3(9) 6_556 . . . ? C22 Pd2 C202 C201 -155.1(6) . . . . ? C22 Pd2 C202 C201 45.9(15) 6_556 . . . ? C202 Pd2 C202 C201 28.6(7) 6_556 . . . ? C32 Pd3 C301 C302 29.0(9) . . . . ? C32 Pd3 C301 C302 -164.6(5) 6_556 . . . ? C302 Pd3 C301 C302 -135.6(12) 6_556 . . . ? C32 Pd3 C301 C302 164.6(5) . . . 6_556 ? C32 Pd3 C301 C302 -29.0(9) 6_556 . . 6_556 ? C302 Pd3 C301 C302 135.6(12) . . . 6_556 ? C302 C301 C302 Pd3 -53.3(11) 6_556 . . . ? C32 Pd3 C302 C301 -158.6(7) . . . . ? C32 Pd3 C302 C301 49.6(14) 6_556 . . . ? C302 Pd3 C302 C301 27.2(7) 6_556 . . . ? C6 C1 C2 C3 0.5(10) . . . . ? N11 C1 C2 C3 -172.2(6) . . . . ? C1 C2 C3 C4 0.3(10) . . . . ? C1 C2 C3 N21 172.3(6) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? N21 C3 C4 C5 -172.0(6) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? C3 C4 C5 N31 171.6(6) . . . . ? C4 C5 C6 C1 2.3(10) . . . . ? N31 C5 C6 C1 -170.6(6) . . . . ? C2 C1 C6 C5 -1.7(10) . . . . ? N11 C1 C6 C5 170.9(6) . . . . ? C6 C1 N11 C12 149.7(6) . . . . ? C2 C1 N11 C12 -37.5(9) . . . . ? C6 C1 N11 C15 -38.3(9) . . . . ? C2 C1 N11 C15 134.5(7) . . . . ? C15 N11 C12 N13 -0.7(8) . . . . ? C1 N11 C12 N13 172.2(6) . . . . ? C15 N11 C12 Pd1 172.5(5) . . . . ? C1 N11 C12 Pd1 -14.6(9) . . . . ? C12 Pd1 C12 N13 88.8(6) 6_556 . . . ? C101 Pd1 C12 N13 -105.1(7) . . . . ? C102 Pd1 C12 N13 -85.5(6) . . . . ? C102 Pd1 C12 N13 -66.8(14) 6_556 . . . ? C12 Pd1 C12 N11 -83.0(6) 6_556 . . . ? C101 Pd1 C12 N11 83.1(8) . . . . ? C102 Pd1 C12 N11 102.7(6) . . . . ? C102 Pd1 C12 N11 121.5(12) 6_556 . . . ? N11 C12 N13 C14 -0.4(8) . . . . ? Pd1 C12 N13 C14 -173.8(5) . . . . ? N11 C12 N13 C16 -176.9(6) . . . . ? Pd1 C12 N13 C16 9.7(10) . . . . ? C12 N13 C14 C15 1.3(9) . . . . ? C16 N13 C14 C15 177.9(7) . . . . ? N13 C14 C15 N11 -1.7(9) . . . . ? C12 N11 C15 C14 1.5(9) . . . . ? C1 N11 C15 C14 -171.5(6) . . . . ? C12 N13 C16 C17 117.7(9) . . . . ? C14 N13 C16 C17 -58.4(10) . . . . ? C2 C3 N21 C22 151.9(6) . . . . ? C4 C3 N21 C22 -36.0(9) . . . . ? C2 C3 N21 C25 -41.3(9) . . . . ? C4 C3 N21 C25 130.8(7) . . . . ? C25 N21 C22 N23 -0.3(7) . . . . ? C3 N21 C22 N23 168.0(6) . . . . ? C25 N21 C22 Pd2 174.3(5) . . . . ? C3 N21 C22 Pd2 -17.4(9) . . . . ? C22 Pd2 C22 N23 91.6(6) 6_556 . . . ? C201 Pd2 C22 N23 -104.5(7) . . . . ? C202 Pd2 C22 N23 -84.0(6) . . . . ? C202 Pd2 C22 N23 -67.7(15) 6_556 . . . ? C22 Pd2 C22 N21 -81.8(6) 6_556 . . . ? C201 Pd2 C22 N21 82.0(8) . . . . ? C202 Pd2 C22 N21 102.6(6) . . . . ? C202 Pd2 C22 N21 118.9(13) 6_556 . . . ? N21 C22 N23 C24 0.3(8) . . . . ? Pd2 C22 N23 C24 -174.5(5) . . . . ? N21 C22 N23 C26 -173.7(6) . . . . ? Pd2 C22 N23 C26 11.6(10) . . . . ? C22 N23 C24 C25 -0.2(9) . . . . ? C26 N23 C24 C25 173.8(7) . . . . ? N23 C24 C25 N21 0.0(9) . . . . ? C22 N21 C25 C24 0.2(8) . . . . ? C3 N21 C25 C24 -168.4(6) . . . . ? C22 N23 C26 C27 101.5(8) . . . . ? C24 N23 C26 C27 -71.7(9) . . . . ? C4 C5 N31 C32 143.4(7) . . . . ? C6 C5 N31 C32 -43.5(10) . . . . ? C4 C5 N31 C35 -44.6(9) . . . . ? C6 C5 N31 C35 128.5(7) . . . . ? C35 N31 C32 N33 1.5(7) . . . . ? C5 N31 C32 N33 174.1(6) . . . . ? C35 N31 C32 Pd3 177.8(5) . . . . ? C5 N31 C32 Pd3 -9.6(10) . . . . ? C32 Pd3 C32 N33 91.0(6) 6_556 . . . ? C301 Pd3 C32 N33 -99.2(8) . . . . ? C302 Pd3 C32 N33 -82.0(6) . . . . ? C302 Pd3 C32 N33 -61.0(14) 6_556 . . . ? C32 Pd3 C32 N31 -84.5(6) 6_556 . . . ? C301 Pd3 C32 N31 85.3(8) . . . . ? C302 Pd3 C32 N31 102.5(6) . . . . ? C302 Pd3 C32 N31 123.5(11) 6_556 . . . ? N31 C32 N33 C34 -0.3(8) . . . . ? Pd3 C32 N33 C34 -176.7(5) . . . . ? N31 C32 N33 C36 -175.7(6) . . . . ? Pd3 C32 N33 C36 7.9(10) . . . . ? C32 N33 C34 C35 -1.0(8) . . . . ? C36 N33 C34 C35 174.4(7) . . . . ? N33 C34 C35 N31 1.8(8) . . . . ? C32 N31 C35 C34 -2.1(8) . . . . ? C5 N31 C35 C34 -175.2(6) . . . . ? C32 N33 C36 C37 113.8(8) . . . . ? C34 N33 C36 C37 -61.0(10) . . . . ? C904 O901 C902 C903 180.0 . . . . ? C902 O901 C904 C905 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.236 _refine_diff_density_min -1.358 _refine_diff_density_rms 0.163 data_sad2 _database_code_depnum_ccdc_archive 'CCDC 905535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H53 Cl2 F6 Ir2 N6 P' _chemical_formula_weight 1230.16 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 26.9202(6) _cell_length_b 26.9202(6) _cell_length_c 34.3435(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21554.2(11) _cell_formula_units_Z 18 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 13959 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10764 _exptl_absorpt_coefficient_mu 5.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6255 _exptl_absorpt_correction_T_max 0.7618 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85000 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13959 _reflns_number_gt 11398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. One half PF6 anion was found disordered in the asymmetric unit. An unidentified disordered solvent molecule was found in the asymmetrical unit and could not be satisfactorily refined. The program SQUEEZE was therefore used to remove mathematically the effect of the solvent. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 373 102 ' ' 2 0.000 0.000 0.500 702 119 ' ' 3 0.757 0.011 0.196 9 0 ' ' 4 0.655 0.079 0.530 8 0 ' ' 5 0.413 0.091 0.137 8 0 ' ' 6 0.667 0.333 0.833 710 120 ' ' 7 0.667 0.333 0.333 376 102 ' ' 8 0.254 0.242 0.196 9 0 ' ' 9 0.011 0.254 0.804 9 0 ' ' 10 0.909 0.322 0.137 8 0 ' ' 11 0.424 0.345 0.530 8 0 ' ' 12 0.322 0.413 0.863 8 0 ' ' 13 0.079 0.424 0.470 8 0 ' ' 14 0.333 0.667 0.167 710 120 ' ' 15 0.333 0.667 0.667 376 102 ' ' 16 0.920 0.576 0.530 8 0 ' ' 17 0.678 0.587 0.137 8 0 ' ' 18 0.576 0.655 0.470 8 0 ' ' 19 0.091 0.678 0.863 8 0 ' ' 20 0.989 0.746 0.196 9 0 ' ' 21 0.746 0.757 0.804 9 0 ' ' 22 0.587 0.909 0.863 8 0 ' ' 23 0.345 0.920 0.470 8 0 ' ' 24 0.242 0.988 0.804 9 0 ' ' _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^)+(0.0439P)^2^+20.5691P] 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 13959 _refine_ls_number_parameters 527 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.150728(6) 0.347918(6) 0.135005(4) 0.02371(4) Uani 1 1 d . . . Ir2 Ir 0.158486(6) 0.363622(7) -0.042406(4) 0.02819(4) Uani 1 1 d . . . Cl2 Cl 0.18657(4) 0.29673(4) -0.06805(3) 0.0343(2) Uani 1 1 d . . . Cl1 Cl 0.21876(4) 0.31461(4) 0.14456(3) 0.03162(18) Uani 1 1 d . . . N1 N 0.02854(13) 0.23332(15) -0.02367(8) 0.0320(7) Uani 1 1 d . . . N2 N 0.00166(17) 0.1871(2) -0.07783(11) 0.0545(11) Uani 1 1 d . . . N3 N 0.05220(13) 0.23962(14) 0.11584(8) 0.0290(6) Uani 1 1 d . . . N4 N 0.06608(13) 0.23297(14) 0.17704(9) 0.0323(7) Uani 1 1 d . . . N5 N 0.20636(12) 0.37428(13) 0.03490(8) 0.0262(6) Uani 1 1 d . . . N6 N 0.27859(13) 0.41925(14) -0.00366(9) 0.0322(7) Uani 1 1 d . . . C1 C 0.04675(18) 0.2189(2) -0.05503(11) 0.0415(10) Uani 1 1 d . . . H1 H 0.0854 0.2294 -0.0604 0.050 Uiso 1 1 calc R . . C2 C -0.03032(17) 0.2089(2) -0.02550(12) 0.0413(10) Uani 1 1 d . . . H2 H -0.0545 0.2117 -0.0066 0.050 Uiso 1 1 calc R . . C3 C -0.0467(2) 0.1800(2) -0.05976(13) 0.0544(13) Uani 1 1 d . . . H3 H -0.0848 0.1587 -0.0694 0.065 Uiso 1 1 calc R . . C4 C 0.0045(3) 0.1632(3) -0.11603(16) 0.080(2) Uani 1 1 d . . . H4A H -0.0059 0.1821 -0.1366 0.095 Uiso 1 1 calc R . . H4B H 0.0446 0.1728 -0.1207 0.095 Uiso 1 1 calc R . . C5 C -0.0293(5) 0.1068(5) -0.1192(3) 0.187(6) Uani 1 1 d . . . H5A H -0.0058 0.0884 -0.1199 0.281 Uiso 1 1 calc R . . H5B H -0.0517 0.0980 -0.1433 0.281 Uiso 1 1 calc R . . H5C H -0.0554 0.0924 -0.0969 0.281 Uiso 1 1 calc R . . C6 C 0.06356(15) 0.26345(17) 0.00967(9) 0.0269(7) Uani 1 1 d . . . C7 C 0.04002(15) 0.23743(16) 0.04566(10) 0.0277(7) Uani 1 1 d . . . H7 H 0.0042 0.2028 0.0471 0.033 Uiso 1 1 calc R . . C8 C 0.07076(14) 0.26396(15) 0.07868(9) 0.0243(7) Uani 1 1 d . . . C9 C 0.08788(15) 0.26865(16) 0.14606(9) 0.0257(7) Uani 1 1 d . . . C10 C 0.01772(18) 0.1826(2) 0.16634(12) 0.0437(10) Uani 1 1 d . . . H10 H -0.0050 0.1510 0.1830 0.052 Uiso 1 1 calc R . . C11 C 0.00841(17) 0.18609(19) 0.12814(11) 0.0395(10) Uani 1 1 d . . . H11 H -0.0218 0.1578 0.1127 0.047 Uiso 1 1 calc R . . C12 C 0.09271(19) 0.2444(2) 0.21598(10) 0.0398(9) Uani 1 1 d . . . H12A H 0.0639 0.2394 0.2358 0.048 Uiso 1 1 calc R . . H12B H 0.1244 0.2846 0.2172 0.048 Uiso 1 1 calc R . . C13 C 0.1158(2) 0.2048(2) 0.22517(15) 0.0604(14) Uani 1 1 d . . . H13A H 0.0848 0.1648 0.2229 0.091 Uiso 1 1 calc R . . H13B H 0.1309 0.2119 0.2518 0.091 Uiso 1 1 calc R . . H13C H 0.1465 0.2118 0.2068 0.091 Uiso 1 1 calc R . . C14 C 0.12522(14) 0.31388(15) 0.07913(9) 0.0234(6) Uani 1 1 d . . . C15 C 0.14763(14) 0.33309(15) 0.04189(9) 0.0237(7) Uani 1 1 d . . . C16 C 0.22082(16) 0.38952(16) -0.00308(10) 0.0277(7) Uani 1 1 d . . . C17 C 0.25462(15) 0.39360(16) 0.05762(11) 0.0306(8) Uani 1 1 d . . . H17 H 0.2558 0.3880 0.0848 0.037 Uiso 1 1 calc R . . C18 C 0.30027(16) 0.42222(17) 0.03341(11) 0.0340(8) Uani 1 1 d . . . H18 H 0.3396 0.4408 0.0406 0.041 Uiso 1 1 calc R . . C19 C 0.31458(19) 0.43851(19) -0.03887(12) 0.0404(10) Uani 1 1 d . . . H19A H 0.3467 0.4780 -0.0348 0.048 Uiso 1 1 calc R . . H19B H 0.2914 0.4393 -0.0610 0.048 Uiso 1 1 calc R . . C20 C 0.33862(19) 0.3998(2) -0.04897(13) 0.0461(11) Uani 1 1 d . . . H20A H 0.3628 0.4001 -0.0275 0.069 Uiso 1 1 calc R . . H20B H 0.3616 0.4138 -0.0728 0.069 Uiso 1 1 calc R . . H20C H 0.3070 0.3606 -0.0531 0.069 Uiso 1 1 calc R . . C21 C 0.11695(15) 0.31251(16) 0.00604(9) 0.0250(7) Uani 1 1 d . . . C22 C 0.11273(17) 0.40074(17) 0.13466(11) 0.0328(8) Uani 1 1 d . . . C23 C 0.11813(18) 0.38906(18) 0.17514(11) 0.0345(8) Uani 1 1 d . . . C24 C 0.17704(18) 0.41250(18) 0.18356(11) 0.0347(8) Uani 1 1 d . . . C25 C 0.20937(18) 0.44183(17) 0.14893(11) 0.0343(8) Uani 1 1 d . . . C26 C 0.17032(18) 0.43668(17) 0.11998(11) 0.0330(8) Uani 1 1 d . . . C27 C 0.0578(2) 0.3863(2) 0.11447(14) 0.0500(12) Uani 1 1 d . . . H27A H 0.0436 0.4110 0.1244 0.075 Uiso 1 1 calc R . . H27B H 0.0293 0.3461 0.1194 0.075 Uiso 1 1 calc R . . H27C H 0.0647 0.3925 0.0864 0.075 Uiso 1 1 calc R . . C28 C 0.0690(2) 0.3587(2) 0.20285(13) 0.0492(12) Uani 1 1 d . . . H28A H 0.0816 0.3459 0.2256 0.074 Uiso 1 1 calc R . . H28B H 0.0376 0.3254 0.1899 0.074 Uiso 1 1 calc R . . H28C H 0.0558 0.3849 0.2112 0.074 Uiso 1 1 calc R . . C29 C 0.2034(2) 0.4133(2) 0.22244(12) 0.0521(12) Uani 1 1 d . . . H29A H 0.2194 0.4515 0.2341 0.078 Uiso 1 1 calc R . . H29B H 0.2340 0.4041 0.2188 0.078 Uiso 1 1 calc R . . H29C H 0.1739 0.3848 0.2397 0.078 Uiso 1 1 calc R . . C30 C 0.2734(2) 0.4751(2) 0.14703(15) 0.0530(12) Uani 1 1 d . . . H30A H 0.2855 0.4859 0.1200 0.080 Uiso 1 1 calc R . . H30B H 0.2889 0.4515 0.1569 0.080 Uiso 1 1 calc R . . H30C H 0.2877 0.5098 0.1630 0.080 Uiso 1 1 calc R . . C31 C 0.1844(2) 0.4660(2) 0.08128(12) 0.0479(11) Uani 1 1 d . . . H31A H 0.1780 0.4988 0.0822 0.072 Uiso 1 1 calc R . . H31B H 0.1598 0.4390 0.0612 0.072 Uiso 1 1 calc R . . H31C H 0.2247 0.4796 0.0750 0.072 Uiso 1 1 calc R . . C32 C 0.1841(2) 0.4486(2) -0.07025(12) 0.0451(11) Uani 1 1 d . . . C33 C 0.1686(2) 0.4075(2) -0.09998(11) 0.0455(11) Uani 1 1 d . . . C34 C 0.1090(2) 0.3643(2) -0.09538(10) 0.0425(11) Uani 1 1 d . . . C35 C 0.08767(19) 0.3783(2) -0.06142(11) 0.0373(9) Uani 1 1 d . . . C36 C 0.1352(2) 0.4294(2) -0.04426(10) 0.0383(10) Uani 1 1 d . . . C37 C 0.2385(2) 0.5047(2) -0.06527(16) 0.0588(14) Uani 1 1 d . . . H37A H 0.2666 0.5079 -0.0847 0.088 Uiso 1 1 calc R . . H37B H 0.2539 0.5067 -0.0391 0.088 Uiso 1 1 calc R . . H37C H 0.2306 0.5363 -0.0688 0.088 Uiso 1 1 calc R . . C38 C 0.2048(3) 0.4078(3) -0.13354(13) 0.0627(16) Uani 1 1 d . . . H38A H 0.1856 0.4062 -0.1581 0.094 Uiso 1 1 calc R . . H38B H 0.2102 0.3745 -0.1316 0.094 Uiso 1 1 calc R . . H38C H 0.2423 0.4431 -0.1327 0.094 Uiso 1 1 calc R . . C39 C 0.0747(3) 0.3161(3) -0.12386(13) 0.0599(15) Uani 1 1 d . . . H39A H 0.0352 0.2929 -0.1144 0.090 Uiso 1 1 calc R . . H39B H 0.0921 0.2918 -0.1262 0.090 Uiso 1 1 calc R . . H39C H 0.0745 0.3322 -0.1494 0.090 Uiso 1 1 calc R . . C40 C 0.0285(2) 0.3499(2) -0.04630(13) 0.0494(12) Uani 1 1 d . . . H40A H 0.0139 0.3767 -0.0472 0.074 Uiso 1 1 calc R . . H40B H 0.0282 0.3379 -0.0193 0.074 Uiso 1 1 calc R . . H40C H 0.0041 0.3162 -0.0623 0.074 Uiso 1 1 calc R . . C41 C 0.1302(2) 0.4645(2) -0.01222(12) 0.0513(13) Uani 1 1 d . . . H41A H 0.1664 0.4844 0.0021 0.077 Uiso 1 1 calc R . . H41B H 0.0993 0.4393 0.0056 0.077 Uiso 1 1 calc R . . H41C H 0.1215 0.4928 -0.0234 0.077 Uiso 1 1 calc R . . P1 P 0.5000 0.5000 0.0000 0.0327(3) Uani 1 2 d S . . F11 F 0.47558(13) 0.44667(11) -0.02911(8) 0.0569(7) Uani 1 1 d U . . F12 F 0.4545(2) 0.51486(18) -0.01368(17) 0.1343(19) Uani 1 1 d U . . F13 F 0.4569(2) 0.45832(16) 0.03086(11) 0.1274(18) Uani 1 1 d U . . P2 P 0.0000 0.0000 -0.20619(10) 0.0688(7) Uani 1 3 d S . . F21 F -0.0162(3) 0.0361(3) -0.2341(2) 0.185(3) Uani 1 1 d U . . F22 F -0.0550(3) -0.0155(3) -0.1866(2) 0.203(3) Uani 1 1 d U . . 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 0.02575(7) 0.03399(8) 0.01509(6) -0.00002(5) 0.00075(4) 0.01772(6) Ir2 0.03760(8) 0.04398(9) 0.01565(7) 0.00526(5) 0.00652(5) 0.02988(7) Cl2 0.0411(5) 0.0487(5) 0.0276(4) 0.0010(4) 0.0060(4) 0.0333(5) Cl1 0.0263(4) 0.0397(5) 0.0336(4) -0.0014(4) -0.0023(3) 0.0201(4) N1 0.0313(16) 0.049(2) 0.0202(14) -0.0060(13) -0.0049(12) 0.0238(15) N2 0.051(2) 0.091(3) 0.0330(19) -0.029(2) -0.0154(17) 0.045(2) N3 0.0264(15) 0.0401(18) 0.0188(14) 0.0034(12) 0.0009(11) 0.0153(14) N4 0.0306(16) 0.0419(18) 0.0208(14) 0.0065(13) 0.0020(12) 0.0155(14) N5 0.0246(14) 0.0363(16) 0.0192(13) 0.0035(12) 0.0057(11) 0.0164(13) N6 0.0310(16) 0.0412(18) 0.0285(16) 0.0077(13) 0.0101(13) 0.0212(15) C1 0.036(2) 0.068(3) 0.0258(19) -0.0098(19) -0.0050(16) 0.030(2) C2 0.029(2) 0.066(3) 0.032(2) -0.0116(19) -0.0084(16) 0.027(2) C3 0.038(2) 0.085(4) 0.041(2) -0.026(2) -0.0145(19) 0.031(3) C4 0.097(5) 0.121(6) 0.042(3) -0.047(3) -0.027(3) 0.070(5) C5 0.202(13) 0.153(10) 0.151(10) -0.080(8) 0.025(9) 0.047(9) C6 0.0279(17) 0.043(2) 0.0170(15) -0.0002(14) -0.0005(12) 0.0228(16) C7 0.0225(16) 0.037(2) 0.0231(16) -0.0010(14) -0.0003(13) 0.0150(15) C8 0.0223(16) 0.0366(19) 0.0173(15) 0.0024(13) 0.0032(12) 0.0171(15) C9 0.0259(17) 0.041(2) 0.0162(14) 0.0029(13) 0.0045(12) 0.0216(16) C10 0.035(2) 0.051(3) 0.031(2) 0.0116(18) 0.0042(16) 0.011(2) C11 0.029(2) 0.043(2) 0.0291(19) 0.0081(17) 0.0020(15) 0.0053(17) C12 0.047(2) 0.054(3) 0.0179(17) 0.0066(16) -0.0012(16) 0.026(2) C13 0.078(4) 0.068(3) 0.049(3) 0.002(2) -0.022(3) 0.047(3) C14 0.0243(16) 0.0320(18) 0.0182(15) 0.0025(13) 0.0013(12) 0.0173(14) C15 0.0231(16) 0.0322(18) 0.0198(15) -0.0003(13) 0.0020(12) 0.0170(14) C16 0.0362(19) 0.0350(19) 0.0195(16) 0.0069(13) 0.0084(14) 0.0235(16) C17 0.0259(18) 0.039(2) 0.0269(18) 0.0009(15) -0.0002(14) 0.0160(16) C18 0.0258(18) 0.037(2) 0.037(2) 0.0037(16) 0.0039(15) 0.0139(16) C19 0.043(2) 0.050(2) 0.032(2) 0.0162(18) 0.0194(17) 0.026(2) C20 0.040(2) 0.055(3) 0.048(3) 0.006(2) 0.0189(19) 0.027(2) C21 0.0276(17) 0.0393(19) 0.0172(15) 0.0006(13) 0.0030(12) 0.0237(16) C22 0.040(2) 0.041(2) 0.0277(18) -0.0050(15) -0.0006(15) 0.0287(19) C23 0.047(2) 0.046(2) 0.0243(18) -0.0020(15) 0.0056(16) 0.033(2) C24 0.048(2) 0.042(2) 0.0224(17) -0.0034(15) -0.0012(16) 0.0282(19) C25 0.042(2) 0.036(2) 0.0279(18) -0.0042(15) -0.0009(16) 0.0211(18) C26 0.046(2) 0.036(2) 0.0233(17) -0.0024(14) -0.0012(15) 0.0257(18) C27 0.053(3) 0.066(3) 0.053(3) -0.012(2) -0.012(2) 0.047(3) C28 0.062(3) 0.060(3) 0.042(2) 0.008(2) 0.023(2) 0.043(3) C29 0.067(3) 0.066(3) 0.030(2) -0.009(2) -0.014(2) 0.039(3) C30 0.042(3) 0.047(3) 0.059(3) -0.016(2) -0.007(2) 0.014(2) C31 0.079(3) 0.049(3) 0.031(2) 0.0075(18) 0.007(2) 0.042(3) C32 0.061(3) 0.058(3) 0.034(2) 0.018(2) 0.012(2) 0.044(3) C33 0.073(3) 0.067(3) 0.0230(19) 0.0171(19) 0.0161(19) 0.055(3) C34 0.067(3) 0.073(3) 0.0167(16) 0.0011(18) -0.0016(17) 0.057(3) C35 0.050(2) 0.062(3) 0.0227(17) 0.0075(17) 0.0027(16) 0.045(2) C36 0.061(3) 0.060(3) 0.0192(17) 0.0051(16) 0.0029(17) 0.049(2) C37 0.066(3) 0.049(3) 0.070(3) 0.021(3) 0.010(3) 0.035(3) C38 0.096(4) 0.097(4) 0.031(2) 0.026(2) 0.032(3) 0.075(4) C39 0.092(4) 0.093(4) 0.029(2) -0.012(2) -0.014(2) 0.072(4) C40 0.058(3) 0.082(4) 0.035(2) 0.008(2) 0.001(2) 0.054(3) C41 0.088(4) 0.072(3) 0.028(2) -0.003(2) -0.005(2) 0.065(3) P1 0.0330(7) 0.0301(7) 0.0262(7) 0.0055(5) 0.0041(5) 0.0091(6) F11 0.0624(18) 0.0446(15) 0.0461(15) -0.0069(12) 0.0024(13) 0.0135(13) F12 0.117(3) 0.085(3) 0.222(5) -0.065(3) -0.106(3) 0.066(2) F13 0.168(4) 0.062(2) 0.073(2) -0.0057(18) 0.073(2) -0.001(2) P2 0.0524(9) 0.0524(9) 0.102(2) 0.000 0.000 0.0262(4) F21 0.152(4) 0.161(5) 0.256(6) 0.056(4) -0.016(4) 0.087(4) F22 0.169(5) 0.225(6) 0.222(5) 0.023(4) 0.106(4) 0.105(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C9 1.987(4) . ? Ir1 C14 2.089(3) . ? Ir1 C22 2.127(4) . ? Ir1 C23 2.206(3) . ? Ir1 C26 2.235(4) . ? Ir1 C24 2.252(4) . ? Ir1 C25 2.263(4) . ? Ir1 Cl1 2.4305(9) . ? Ir2 C16 1.989(4) . ? Ir2 C21 2.091(3) . ? Ir2 C36 2.155(4) . ? Ir2 C35 2.230(4) . ? Ir2 C32 2.247(4) . ? Ir2 C33 2.249(4) . ? Ir2 C34 2.261(4) . ? Ir2 Cl2 2.4395(9) . ? N1 C1 1.319(5) . ? N1 C2 1.380(5) . ? N1 C6 1.447(4) . ? N2 C1 1.334(5) . ? N2 C3 1.367(6) . ? N2 C4 1.481(6) . ? N3 C9 1.364(4) . ? N3 C11 1.395(5) . ? N3 C8 1.407(4) . ? N4 C9 1.355(4) . ? N4 C10 1.380(5) . ? N4 C12 1.475(5) . ? N5 C16 1.364(4) . ? N5 C17 1.375(4) . ? N5 C15 1.426(4) . ? N6 C16 1.347(5) . ? N6 C18 1.386(5) . ? N6 C19 1.472(4) . ? C1 H1 0.9500 . ? C2 C3 1.357(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.327(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C21 1.388(5) . ? C6 C7 1.406(5) . ? C7 C8 1.375(5) . ? C7 H7 0.9500 . ? C8 C14 1.409(5) . ? C10 C11 1.348(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.511(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.398(4) . ? C15 C21 1.431(5) . ? C17 C18 1.360(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.516(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 C26 1.447(6) . ? C22 C23 1.449(5) . ? C22 C27 1.497(6) . ? C23 C24 1.413(6) . ? C23 C28 1.497(6) . ? C24 C25 1.452(5) . ? C24 C29 1.507(5) . ? C25 C26 1.402(5) . ? C25 C30 1.494(6) . ? C26 C31 1.495(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.407(7) . ? C32 C36 1.455(6) . ? C32 C37 1.498(7) . ? C33 C34 1.446(7) . ? C33 C38 1.506(5) . ? C34 C35 1.432(5) . ? C34 C39 1.514(7) . ? C35 C36 1.455(6) . ? C35 C40 1.474(6) . ? C36 C41 1.500(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? P1 F12 1.539(4) 10_665 ? P1 F12 1.539(4) . ? P1 F13 1.558(3) . ? P1 F13 1.558(3) 10_665 ? P1 F11 1.597(3) 10_665 ? P1 F11 1.597(3) . ? P2 F22 1.482(6) 3 ? P2 F22 1.482(6) . ? P2 F22 1.482(6) 2 ? P2 F21 1.575(6) 2 ? P2 F21 1.575(6) . ? P2 F21 1.575(6) 3 ? 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 C9 Ir1 C14 77.76(13) . . ? C9 Ir1 C22 106.45(15) . . ? C14 Ir1 C22 97.22(13) . . ? C9 Ir1 C23 94.64(15) . . ? C14 Ir1 C23 131.92(14) . . ? C22 Ir1 C23 39.01(14) . . ? C9 Ir1 C26 144.22(14) . . ? C14 Ir1 C26 96.14(13) . . ? C22 Ir1 C26 38.66(15) . . ? C23 Ir1 C26 63.13(14) . . ? C9 Ir1 C24 117.23(14) . . ? C14 Ir1 C24 157.84(14) . . ? C22 Ir1 C24 63.82(14) . . ? C23 Ir1 C24 36.93(15) . . ? C26 Ir1 C24 62.00(14) . . ? C9 Ir1 C25 154.55(14) . . ? C14 Ir1 C25 125.23(13) . . ? C22 Ir1 C25 63.54(15) . . ? C23 Ir1 C25 62.46(15) . . ? C26 Ir1 C25 36.33(14) . . ? C24 Ir1 C25 37.51(14) . . ? C9 Ir1 Cl1 88.40(10) . . ? C14 Ir1 Cl1 96.04(9) . . ? C22 Ir1 Cl1 161.88(11) . . ? C23 Ir1 Cl1 131.52(11) . . ? C26 Ir1 Cl1 127.38(11) . . ? C24 Ir1 Cl1 100.40(10) . . ? C25 Ir1 Cl1 98.63(10) . . ? C16 Ir2 C21 76.72(14) . . ? C16 Ir2 C36 105.84(15) . . ? C21 Ir2 C36 106.54(14) . . ? C16 Ir2 C35 141.53(15) . . ? C21 Ir2 C35 97.26(14) . . ? C36 Ir2 C35 38.70(16) . . ? C16 Ir2 C32 98.99(16) . . ? C21 Ir2 C32 143.09(14) . . ? C36 Ir2 C32 38.53(15) . . ? C35 Ir2 C32 63.18(17) . . ? C16 Ir2 C33 123.60(17) . . ? C21 Ir2 C33 158.38(16) . . ? C36 Ir2 C33 63.32(14) . . ? C35 Ir2 C33 62.56(15) . . ? C32 Ir2 C33 36.49(16) . . ? C16 Ir2 C34 160.26(17) . . ? C21 Ir2 C34 121.45(16) . . ? C36 Ir2 C34 63.58(15) . . ? C35 Ir2 C34 37.18(13) . . ? C32 Ir2 C34 62.08(18) . . ? C33 Ir2 C34 37.40(18) . . ? C16 Ir2 Cl2 89.16(10) . . ? C21 Ir2 Cl2 93.60(9) . . ? C36 Ir2 Cl2 157.05(10) . . ? C35 Ir2 Cl2 129.30(11) . . ? C32 Ir2 Cl2 123.19(11) . . ? C33 Ir2 Cl2 93.97(11) . . ? C34 Ir2 Cl2 96.69(10) . . ? C1 N1 C2 109.2(3) . . ? C1 N1 C6 125.2(3) . . ? C2 N1 C6 125.1(3) . . ? C1 N2 C3 108.7(3) . . ? C1 N2 C4 124.8(4) . . ? C3 N2 C4 126.5(4) . . ? C9 N3 C11 110.5(3) . . ? C9 N3 C8 116.0(3) . . ? C11 N3 C8 132.5(3) . . ? C9 N4 C10 110.4(3) . . ? C9 N4 C12 124.8(3) . . ? C10 N4 C12 124.6(3) . . ? C16 N5 C17 110.8(3) . . ? C16 N5 C15 115.7(3) . . ? C17 N5 C15 132.0(3) . . ? C16 N6 C18 110.4(3) . . ? C16 N6 C19 125.6(3) . . ? C18 N6 C19 123.4(3) . . ? N1 C1 N2 108.4(4) . . ? N1 C1 H1 125.8 . . ? N2 C1 H1 125.8 . . ? C3 C2 N1 106.3(4) . . ? C3 C2 H2 126.9 . . ? N1 C2 H2 126.9 . . ? C2 C3 N2 107.4(4) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C5 C4 N2 114.6(7) . . ? C5 C4 H4A 108.6 . . ? N2 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? N2 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C21 C6 C7 123.2(3) . . ? C21 C6 N1 122.5(3) . . ? C7 C6 N1 114.3(3) . . ? C8 C7 C6 117.5(3) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 N3 121.7(3) . . ? C7 C8 C14 125.0(3) . . ? N3 C8 C14 113.1(3) . . ? N4 C9 N3 105.1(3) . . ? N4 C9 Ir1 138.2(3) . . ? N3 C9 Ir1 116.6(2) . . ? C11 C10 N4 107.9(4) . . ? C11 C10 H10 126.1 . . ? N4 C10 H10 126.1 . . ? C10 C11 N3 106.1(4) . . ? C10 C11 H11 127.0 . . ? N3 C11 H11 127.0 . . ? N4 C12 C13 111.8(4) . . ? N4 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N4 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C8 113.2(3) . . ? C15 C14 Ir1 133.8(3) . . ? C8 C14 Ir1 112.7(2) . . ? C14 C15 N5 123.2(3) . . ? C14 C15 C21 125.8(3) . . ? N5 C15 C21 110.9(3) . . ? N6 C16 N5 105.3(3) . . ? N6 C16 Ir2 136.0(3) . . ? N5 C16 Ir2 118.7(3) . . ? C18 C17 N5 106.4(3) . . ? C18 C17 H17 126.8 . . ? N5 C17 H17 126.8 . . ? C17 C18 N6 107.1(3) . . ? C17 C18 H18 126.5 . . ? N6 C18 H18 126.5 . . ? N6 C19 C20 112.2(3) . . ? N6 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N6 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 C21 C15 114.4(3) . . ? C6 C21 Ir2 131.0(2) . . ? C15 C21 Ir2 114.5(2) . . ? C26 C22 C23 106.8(3) . . ? C26 C22 C27 126.9(4) . . ? C23 C22 C27 125.5(4) . . ? C26 C22 Ir1 74.7(2) . . ? C23 C22 Ir1 73.5(2) . . ? C27 C22 Ir1 124.9(3) . . ? C24 C23 C22 108.1(3) . . ? C24 C23 C28 127.0(4) . . ? C22 C23 C28 124.9(4) . . ? C24 C23 Ir1 73.3(2) . . ? C22 C23 Ir1 67.53(19) . . ? C28 C23 Ir1 126.0(3) . . ? C23 C24 C25 108.0(3) . . ? C23 C24 C29 127.1(4) . . ? C25 C24 C29 124.6(4) . . ? C23 C24 Ir1 69.8(2) . . ? C25 C24 Ir1 71.6(2) . . ? C29 C24 Ir1 129.1(3) . . ? C26 C25 C24 108.1(4) . . ? C26 C25 C30 127.7(4) . . ? C24 C25 C30 124.1(4) . . ? C26 C25 Ir1 70.7(2) . . ? C24 C25 Ir1 70.8(2) . . ? C30 C25 Ir1 127.7(3) . . ? C25 C26 C22 108.6(3) . . ? C25 C26 C31 126.8(4) . . ? C22 C26 C31 124.5(4) . . ? C25 C26 Ir1 72.9(2) . . ? C22 C26 Ir1 66.6(2) . . ? C31 C26 Ir1 129.2(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C36 107.8(4) . . ? C33 C32 C37 129.2(4) . . ? C36 C32 C37 122.9(4) . . ? C33 C32 Ir2 71.8(2) . . ? C36 C32 Ir2 67.3(2) . . ? C37 C32 Ir2 128.7(3) . . ? C32 C33 C34 109.1(4) . . ? C32 C33 C38 127.9(5) . . ? C34 C33 C38 122.9(5) . . ? C32 C33 Ir2 71.7(2) . . ? C34 C33 Ir2 71.8(2) . . ? C38 C33 Ir2 125.7(3) . . ? C35 C34 C33 107.8(4) . . ? C35 C34 C39 126.8(4) . . ? C33 C34 C39 125.1(4) . . ? C35 C34 Ir2 70.2(2) . . ? C33 C34 Ir2 70.8(2) . . ? C39 C34 Ir2 128.5(3) . . ? C34 C35 C36 107.5(4) . . ? C34 C35 C40 128.4(4) . . ? C36 C35 C40 124.0(4) . . ? C34 C35 Ir2 72.6(2) . . ? C36 C35 Ir2 67.9(2) . . ? C40 C35 Ir2 127.0(3) . . ? C35 C36 C32 107.4(3) . . ? C35 C36 C41 125.4(4) . . ? C32 C36 C41 125.2(4) . . ? C35 C36 Ir2 73.4(2) . . ? C32 C36 Ir2 74.2(2) . . ? C41 C36 Ir2 130.6(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? F12 P1 F12 180.0(5) 10_665 . ? F12 P1 F13 90.4(3) 10_665 . ? F12 P1 F13 89.6(3) . . ? F12 P1 F13 89.6(3) 10_665 10_665 ? F12 P1 F13 90.4(3) . 10_665 ? F13 P1 F13 180.0(4) . 10_665 ? F12 P1 F11 91.10(19) 10_665 10_665 ? F12 P1 F11 88.90(19) . 10_665 ? F13 P1 F11 92.59(17) . 10_665 ? F13 P1 F11 87.41(17) 10_665 10_665 ? F12 P1 F11 88.90(19) 10_665 . ? F12 P1 F11 91.10(19) . . ? F13 P1 F11 87.41(17) . . ? F13 P1 F11 92.59(17) 10_665 . ? F11 P1 F11 180.0(2) 10_665 . ? F22 P2 F22 101.1(4) 3 . ? F22 P2 F22 101.1(4) 3 2 ? F22 P2 F22 101.1(4) . 2 ? F22 P2 F21 169.3(5) 3 2 ? F22 P2 F21 86.7(4) . 2 ? F22 P2 F21 84.5(4) 2 2 ? F22 P2 F21 86.7(4) 3 . ? F22 P2 F21 84.5(4) . . ? F22 P2 F21 169.3(5) 2 . ? F21 P2 F21 86.8(5) 2 . ? F22 P2 F21 84.5(4) 3 3 ? F22 P2 F21 169.3(5) . 3 ? F22 P2 F21 86.7(4) 2 3 ? F21 P2 F21 86.8(5) 2 3 ? F21 P2 F21 86.8(5) . 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 C2 N1 C1 N2 1.8(5) . . . . ? C6 N1 C1 N2 174.2(4) . . . . ? C3 N2 C1 N1 -1.7(6) . . . . ? C4 N2 C1 N1 179.3(5) . . . . ? C1 N1 C2 C3 -1.2(5) . . . . ? C6 N1 C2 C3 -173.6(4) . . . . ? N1 C2 C3 N2 0.1(6) . . . . ? C1 N2 C3 C2 0.9(6) . . . . ? C4 N2 C3 C2 180.0(5) . . . . ? C1 N2 C4 C5 125.0(9) . . . . ? C3 N2 C4 C5 -53.9(11) . . . . ? C1 N1 C6 C21 47.7(6) . . . . ? C2 N1 C6 C21 -141.0(4) . . . . ? C1 N1 C6 C7 -129.7(4) . . . . ? C2 N1 C6 C7 41.6(5) . . . . ? C21 C6 C7 C8 3.1(5) . . . . ? N1 C6 C7 C8 -179.5(3) . . . . ? C6 C7 C8 N3 -176.6(3) . . . . ? C6 C7 C8 C14 -2.9(5) . . . . ? C9 N3 C8 C7 176.8(3) . . . . ? C11 N3 C8 C7 9.1(6) . . . . ? C9 N3 C8 C14 2.5(4) . . . . ? C11 N3 C8 C14 -165.2(4) . . . . ? C10 N4 C9 N3 0.1(4) . . . . ? C12 N4 C9 N3 175.6(3) . . . . ? C10 N4 C9 Ir1 175.6(3) . . . . ? C12 N4 C9 Ir1 -8.8(6) . . . . ? C11 N3 C9 N4 0.0(4) . . . . ? C8 N3 C9 N4 -170.3(3) . . . . ? C11 N3 C9 Ir1 -176.7(3) . . . . ? C8 N3 C9 Ir1 13.0(4) . . . . ? C14 Ir1 C9 N4 168.4(4) . . . . ? C22 Ir1 C9 N4 -97.6(4) . . . . ? C23 Ir1 C9 N4 -59.7(4) . . . . ? C26 Ir1 C9 N4 -108.2(4) . . . . ? C24 Ir1 C9 N4 -29.0(4) . . . . ? C25 Ir1 C9 N4 -35.1(6) . . . . ? Cl1 Ir1 C9 N4 71.8(4) . . . . ? C14 Ir1 C9 N3 -16.4(3) . . . . ? C22 Ir1 C9 N3 77.6(3) . . . . ? C23 Ir1 C9 N3 115.5(3) . . . . ? C26 Ir1 C9 N3 67.1(4) . . . . ? C24 Ir1 C9 N3 146.2(2) . . . . ? C25 Ir1 C9 N3 140.2(3) . . . . ? Cl1 Ir1 C9 N3 -112.9(3) . . . . ? C9 N4 C10 C11 -0.1(5) . . . . ? C12 N4 C10 C11 -175.7(4) . . . . ? N4 C10 C11 N3 0.1(5) . . . . ? C9 N3 C11 C10 -0.1(5) . . . . ? C8 N3 C11 C10 168.1(4) . . . . ? C9 N4 C12 C13 -110.5(5) . . . . ? C10 N4 C12 C13 64.4(5) . . . . ? C7 C8 C14 C15 -3.5(5) . . . . ? N3 C8 C14 C15 170.7(3) . . . . ? C7 C8 C14 Ir1 170.3(3) . . . . ? N3 C8 C14 Ir1 -15.6(4) . . . . ? C9 Ir1 C14 C15 -170.8(4) . . . . ? C22 Ir1 C14 C15 83.9(3) . . . . ? C23 Ir1 C14 C15 104.0(4) . . . . ? C26 Ir1 C14 C15 45.0(4) . . . . ? C24 Ir1 C14 C15 54.1(6) . . . . ? C25 Ir1 C14 C15 21.3(4) . . . . ? Cl1 Ir1 C14 C15 -83.8(3) . . . . ? C9 Ir1 C14 C8 17.2(2) . . . . ? C22 Ir1 C14 C8 -88.1(3) . . . . ? C23 Ir1 C14 C8 -68.0(3) . . . . ? C26 Ir1 C14 C8 -127.1(3) . . . . ? C24 Ir1 C14 C8 -117.9(4) . . . . ? C25 Ir1 C14 C8 -150.7(2) . . . . ? Cl1 Ir1 C14 C8 104.2(2) . . . . ? C8 C14 C15 N5 -165.4(3) . . . . ? Ir1 C14 C15 N5 22.6(5) . . . . ? C8 C14 C15 C21 10.6(5) . . . . ? Ir1 C14 C15 C21 -161.4(3) . . . . ? C16 N5 C15 C14 -178.2(3) . . . . ? C17 N5 C15 C14 17.4(6) . . . . ? C16 N5 C15 C21 5.2(4) . . . . ? C17 N5 C15 C21 -159.2(4) . . . . ? C18 N6 C16 N5 0.6(4) . . . . ? C19 N6 C16 N5 171.8(3) . . . . ? C18 N6 C16 Ir2 -177.2(3) . . . . ? C19 N6 C16 Ir2 -6.0(6) . . . . ? C17 N5 C16 N6 -0.9(4) . . . . ? C15 N5 C16 N6 -168.5(3) . . . . ? C17 N5 C16 Ir2 177.3(2) . . . . ? C15 N5 C16 Ir2 9.7(4) . . . . ? C21 Ir2 C16 N6 163.0(4) . . . . ? C36 Ir2 C16 N6 -93.3(4) . . . . ? C35 Ir2 C16 N6 -112.1(4) . . . . ? C32 Ir2 C16 N6 -54.4(4) . . . . ? C33 Ir2 C16 N6 -25.1(4) . . . . ? C34 Ir2 C16 N6 -38.6(7) . . . . ? Cl2 Ir2 C16 N6 69.1(4) . . . . ? C21 Ir2 C16 N5 -14.5(3) . . . . ? C36 Ir2 C16 N5 89.2(3) . . . . ? C35 Ir2 C16 N5 70.4(4) . . . . ? C32 Ir2 C16 N5 128.1(3) . . . . ? C33 Ir2 C16 N5 157.4(3) . . . . ? C34 Ir2 C16 N5 143.8(4) . . . . ? Cl2 Ir2 C16 N5 -108.4(3) . . . . ? C16 N5 C17 C18 0.8(4) . . . . ? C15 N5 C17 C18 165.8(4) . . . . ? N5 C17 C18 N6 -0.4(4) . . . . ? C16 N6 C18 C17 -0.1(4) . . . . ? C19 N6 C18 C17 -171.5(4) . . . . ? C16 N6 C19 C20 -100.5(5) . . . . ? C18 N6 C19 C20 69.5(5) . . . . ? C7 C6 C21 C15 3.0(5) . . . . ? N1 C6 C21 C15 -174.2(3) . . . . ? C7 C6 C21 Ir2 -173.7(3) . . . . ? N1 C6 C21 Ir2 9.1(5) . . . . ? C14 C15 C21 C6 -10.5(5) . . . . ? N5 C15 C21 C6 166.0(3) . . . . ? C14 C15 C21 Ir2 166.8(3) . . . . ? N5 C15 C21 Ir2 -16.8(4) . . . . ? C16 Ir2 C21 C6 -166.4(4) . . . . ? C36 Ir2 C21 C6 90.8(3) . . . . ? C35 Ir2 C21 C6 52.3(3) . . . . ? C32 Ir2 C21 C6 106.3(4) . . . . ? C33 Ir2 C21 C6 32.2(6) . . . . ? C34 Ir2 C21 C6 22.0(4) . . . . ? Cl2 Ir2 C21 C6 -78.1(3) . . . . ? C16 Ir2 C21 C15 16.9(2) . . . . ? C36 Ir2 C21 C15 -85.9(3) . . . . ? C35 Ir2 C21 C15 -124.4(3) . . . . ? C32 Ir2 C21 C15 -70.4(4) . . . . ? C33 Ir2 C21 C15 -144.5(4) . . . . ? C34 Ir2 C21 C15 -154.7(2) . . . . ? Cl2 Ir2 C21 C15 105.2(2) . . . . ? C9 Ir1 C22 C26 -170.1(2) . . . . ? C14 Ir1 C22 C26 -90.8(2) . . . . ? C23 Ir1 C22 C26 113.2(3) . . . . ? C24 Ir1 C22 C26 77.1(2) . . . . ? C25 Ir1 C22 C26 35.1(2) . . . . ? Cl1 Ir1 C22 C26 45.9(4) . . . . ? C9 Ir1 C22 C23 76.7(2) . . . . ? C14 Ir1 C22 C23 156.0(2) . . . . ? C26 Ir1 C22 C23 -113.2(3) . . . . ? C24 Ir1 C22 C23 -36.1(2) . . . . ? C25 Ir1 C22 C23 -78.1(2) . . . . ? Cl1 Ir1 C22 C23 -67.3(4) . . . . ? C9 Ir1 C22 C27 -45.5(4) . . . . ? C14 Ir1 C22 C27 33.8(4) . . . . ? C23 Ir1 C22 C27 -122.2(5) . . . . ? C26 Ir1 C22 C27 124.6(4) . . . . ? C24 Ir1 C22 C27 -158.2(4) . . . . ? C25 Ir1 C22 C27 159.7(4) . . . . ? Cl1 Ir1 C22 C27 170.6(3) . . . . ? C26 C22 C23 C24 -5.4(4) . . . . ? C27 C22 C23 C24 -176.2(4) . . . . ? Ir1 C22 C23 C24 62.4(3) . . . . ? C26 C22 C23 C28 173.0(4) . . . . ? C27 C22 C23 C28 2.3(6) . . . . ? Ir1 C22 C23 C28 -119.1(4) . . . . ? C26 C22 C23 Ir1 -67.8(2) . . . . ? C27 C22 C23 Ir1 121.4(4) . . . . ? C9 Ir1 C23 C24 131.0(2) . . . . ? C14 Ir1 C23 C24 -151.3(2) . . . . ? C22 Ir1 C23 C24 -118.4(3) . . . . ? C26 Ir1 C23 C24 -78.4(2) . . . . ? C25 Ir1 C23 C24 -37.3(2) . . . . ? Cl1 Ir1 C23 C24 39.0(3) . . . . ? C9 Ir1 C23 C22 -110.6(2) . . . . ? C14 Ir1 C23 C22 -32.9(3) . . . . ? C26 Ir1 C23 C22 40.1(2) . . . . ? C24 Ir1 C23 C22 118.4(3) . . . . ? C25 Ir1 C23 C22 81.1(3) . . . . ? Cl1 Ir1 C23 C22 157.47(19) . . . . ? C9 Ir1 C23 C28 7.1(4) . . . . ? C14 Ir1 C23 C28 84.8(4) . . . . ? C22 Ir1 C23 C28 117.6(5) . . . . ? C26 Ir1 C23 C28 157.7(4) . . . . ? C24 Ir1 C23 C28 -123.9(5) . . . . ? C25 Ir1 C23 C28 -161.3(4) . . . . ? Cl1 Ir1 C23 C28 -84.9(4) . . . . ? C22 C23 C24 C25 3.0(4) . . . . ? C28 C23 C24 C25 -175.4(4) . . . . ? Ir1 C23 C24 C25 61.8(3) . . . . ? C22 C23 C24 C29 176.8(4) . . . . ? C28 C23 C24 C29 -1.6(7) . . . . ? Ir1 C23 C24 C29 -124.4(4) . . . . ? C22 C23 C24 Ir1 -58.8(3) . . . . ? C28 C23 C24 Ir1 122.8(4) . . . . ? C9 Ir1 C24 C23 -57.8(3) . . . . ? C14 Ir1 C24 C23 71.4(4) . . . . ? C22 Ir1 C24 C23 38.1(2) . . . . ? C26 Ir1 C24 C23 81.7(2) . . . . ? C25 Ir1 C24 C23 118.0(3) . . . . ? Cl1 Ir1 C24 C23 -151.3(2) . . . . ? C9 Ir1 C24 C25 -175.8(2) . . . . ? C14 Ir1 C24 C25 -46.6(5) . . . . ? C22 Ir1 C24 C25 -79.9(2) . . . . ? C23 Ir1 C24 C25 -118.0(3) . . . . ? C26 Ir1 C24 C25 -36.3(2) . . . . ? Cl1 Ir1 C24 C25 90.7(2) . . . . ? C9 Ir1 C24 C29 64.1(4) . . . . ? C14 Ir1 C24 C29 -166.7(4) . . . . ? C22 Ir1 C24 C29 160.0(5) . . . . ? C23 Ir1 C24 C29 121.9(5) . . . . ? C26 Ir1 C24 C29 -156.4(5) . . . . ? C25 Ir1 C24 C29 -120.1(5) . . . . ? Cl1 Ir1 C24 C29 -29.4(4) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C29 C24 C25 C26 -173.4(4) . . . . ? Ir1 C24 C25 C26 61.2(3) . . . . ? C23 C24 C25 C30 176.2(4) . . . . ? C29 C24 C25 C30 2.2(6) . . . . ? Ir1 C24 C25 C30 -123.2(4) . . . . ? C23 C24 C25 Ir1 -60.6(3) . . . . ? C29 C24 C25 Ir1 125.4(4) . . . . ? C9 Ir1 C25 C26 -109.2(3) . . . . ? C14 Ir1 C25 C26 42.4(3) . . . . ? C22 Ir1 C25 C26 -37.3(2) . . . . ? C23 Ir1 C25 C26 -81.3(2) . . . . ? C24 Ir1 C25 C26 -118.0(3) . . . . ? Cl1 Ir1 C25 C26 146.1(2) . . . . ? C9 Ir1 C25 C24 8.8(4) . . . . ? C14 Ir1 C25 C24 160.4(2) . . . . ? C22 Ir1 C25 C24 80.7(2) . . . . ? C23 Ir1 C25 C24 36.7(2) . . . . ? C26 Ir1 C25 C24 118.0(3) . . . . ? Cl1 Ir1 C25 C24 -95.9(2) . . . . ? C9 Ir1 C25 C30 127.5(4) . . . . ? C14 Ir1 C25 C30 -80.9(4) . . . . ? C22 Ir1 C25 C30 -160.5(4) . . . . ? C23 Ir1 C25 C30 155.5(4) . . . . ? C26 Ir1 C25 C30 -123.2(5) . . . . ? C24 Ir1 C25 C30 118.7(5) . . . . ? Cl1 Ir1 C25 C30 22.9(4) . . . . ? C24 C25 C26 C22 -4.0(4) . . . . ? C30 C25 C26 C22 -179.4(4) . . . . ? Ir1 C25 C26 C22 57.3(3) . . . . ? C24 C25 C26 C31 172.1(4) . . . . ? C30 C25 C26 C31 -3.3(7) . . . . ? Ir1 C25 C26 C31 -126.6(4) . . . . ? C24 C25 C26 Ir1 -61.3(3) . . . . ? C30 C25 C26 Ir1 123.3(4) . . . . ? C23 C22 C26 C25 5.8(4) . . . . ? C27 C22 C26 C25 176.5(4) . . . . ? Ir1 C22 C26 C25 -61.2(3) . . . . ? C23 C22 C26 C31 -170.4(4) . . . . ? C27 C22 C26 C31 0.2(6) . . . . ? Ir1 C22 C26 C31 122.6(4) . . . . ? C23 C22 C26 Ir1 67.0(2) . . . . ? C27 C22 C26 Ir1 -122.4(4) . . . . ? C9 Ir1 C26 C25 136.0(3) . . . . ? C14 Ir1 C26 C25 -146.4(2) . . . . ? C22 Ir1 C26 C25 119.7(3) . . . . ? C23 Ir1 C26 C25 79.3(2) . . . . ? C24 Ir1 C26 C25 37.5(2) . . . . ? Cl1 Ir1 C26 C25 -43.9(3) . . . . ? C9 Ir1 C26 C22 16.3(3) . . . . ? C14 Ir1 C26 C22 93.9(2) . . . . ? C23 Ir1 C26 C22 -40.4(2) . . . . ? C24 Ir1 C26 C22 -82.2(2) . . . . ? C25 Ir1 C26 C22 -119.7(3) . . . . ? Cl1 Ir1 C26 C22 -163.67(17) . . . . ? C9 Ir1 C26 C31 -100.0(4) . . . . ? C14 Ir1 C26 C31 -22.5(4) . . . . ? C22 Ir1 C26 C31 -116.4(5) . . . . ? C23 Ir1 C26 C31 -156.8(5) . . . . ? C24 Ir1 C26 C31 161.4(5) . . . . ? C25 Ir1 C26 C31 123.9(5) . . . . ? Cl1 Ir1 C26 C31 80.0(4) . . . . ? C16 Ir2 C32 C33 136.7(3) . . . . ? C21 Ir2 C32 C33 -143.4(3) . . . . ? C36 Ir2 C32 C33 -119.1(4) . . . . ? C35 Ir2 C32 C33 -79.3(3) . . . . ? C34 Ir2 C32 C33 -37.3(3) . . . . ? Cl2 Ir2 C32 C33 41.8(3) . . . . ? C16 Ir2 C32 C36 -104.2(3) . . . . ? C21 Ir2 C32 C36 -24.3(4) . . . . ? C35 Ir2 C32 C36 39.7(2) . . . . ? C33 Ir2 C32 C36 119.1(4) . . . . ? C34 Ir2 C32 C36 81.8(3) . . . . ? Cl2 Ir2 C32 C36 160.9(2) . . . . ? C16 Ir2 C32 C37 10.6(4) . . . . ? C21 Ir2 C32 C37 90.5(5) . . . . ? C36 Ir2 C32 C37 114.8(5) . . . . ? C35 Ir2 C32 C37 154.5(5) . . . . ? C33 Ir2 C32 C37 -126.1(5) . . . . ? C34 Ir2 C32 C37 -163.4(5) . . . . ? Cl2 Ir2 C32 C37 -84.3(4) . . . . ? C36 C32 C33 C34 4.5(4) . . . . ? C37 C32 C33 C34 -172.0(4) . . . . ? Ir2 C32 C33 C34 62.4(3) . . . . ? C36 C32 C33 C38 -179.3(4) . . . . ? C37 C32 C33 C38 4.1(7) . . . . ? Ir2 C32 C33 C38 -121.5(4) . . . . ? C36 C32 C33 Ir2 -57.9(3) . . . . ? C37 C32 C33 Ir2 125.6(5) . . . . ? C16 Ir2 C33 C32 -54.4(3) . . . . ? C21 Ir2 C33 C32 103.8(5) . . . . ? C36 Ir2 C33 C32 37.5(3) . . . . ? C35 Ir2 C33 C32 81.2(3) . . . . ? C34 Ir2 C33 C32 118.2(4) . . . . ? Cl2 Ir2 C33 C32 -146.0(3) . . . . ? C16 Ir2 C33 C34 -172.5(2) . . . . ? C21 Ir2 C33 C34 -14.4(5) . . . . ? C36 Ir2 C33 C34 -80.6(3) . . . . ? C35 Ir2 C33 C34 -37.0(2) . . . . ? C32 Ir2 C33 C34 -118.2(4) . . . . ? Cl2 Ir2 C33 C34 95.8(2) . . . . ? C16 Ir2 C33 C38 69.6(5) . . . . ? C21 Ir2 C33 C38 -132.3(5) . . . . ? C36 Ir2 C33 C38 161.5(5) . . . . ? C35 Ir2 C33 C38 -154.8(5) . . . . ? C32 Ir2 C33 C38 124.0(6) . . . . ? C34 Ir2 C33 C38 -117.9(6) . . . . ? Cl2 Ir2 C33 C38 -22.0(5) . . . . ? C32 C33 C34 C35 -1.5(4) . . . . ? C38 C33 C34 C35 -177.9(4) . . . . ? Ir2 C33 C34 C35 60.8(3) . . . . ? C32 C33 C34 C39 173.5(4) . . . . ? C38 C33 C34 C39 -2.9(6) . . . . ? Ir2 C33 C34 C39 -124.1(4) . . . . ? C32 C33 C34 Ir2 -62.3(3) . . . . ? C38 C33 C34 Ir2 121.3(4) . . . . ? C16 Ir2 C34 C35 -99.3(5) . . . . ? C21 Ir2 C34 C35 55.9(3) . . . . ? C36 Ir2 C34 C35 -38.1(3) . . . . ? C32 Ir2 C34 C35 -81.6(3) . . . . ? C33 Ir2 C34 C35 -118.0(4) . . . . ? Cl2 Ir2 C34 C35 154.2(3) . . . . ? C16 Ir2 C34 C33 18.7(5) . . . . ? C21 Ir2 C34 C33 173.8(2) . . . . ? C36 Ir2 C34 C33 79.9(3) . . . . ? C35 Ir2 C34 C33 118.0(4) . . . . ? C32 Ir2 C34 C33 36.4(2) . . . . ? Cl2 Ir2 C34 C33 -87.8(2) . . . . ? C16 Ir2 C34 C39 138.8(5) . . . . ? C21 Ir2 C34 C39 -66.1(4) . . . . ? C36 Ir2 C34 C39 -160.0(5) . . . . ? C35 Ir2 C34 C39 -121.9(6) . . . . ? C32 Ir2 C34 C39 156.5(5) . . . . ? C33 Ir2 C34 C39 120.1(5) . . . . ? Cl2 Ir2 C34 C39 32.3(4) . . . . ? C33 C34 C35 C36 -2.1(4) . . . . ? C39 C34 C35 C36 -177.0(4) . . . . ? Ir2 C34 C35 C36 59.1(2) . . . . ? C33 C34 C35 C40 175.0(4) . . . . ? C39 C34 C35 C40 0.0(7) . . . . ? Ir2 C34 C35 C40 -123.8(4) . . . . ? C33 C34 C35 Ir2 -61.2(3) . . . . ? C39 C34 C35 Ir2 123.9(4) . . . . ? C16 Ir2 C35 C34 147.6(3) . . . . ? C21 Ir2 C35 C34 -134.6(3) . . . . ? C36 Ir2 C35 C34 117.9(4) . . . . ? C32 Ir2 C35 C34 78.4(3) . . . . ? C33 Ir2 C35 C34 37.2(3) . . . . ? Cl2 Ir2 C35 C34 -33.9(3) . . . . ? C16 Ir2 C35 C36 29.7(3) . . . . ? C21 Ir2 C35 C36 107.5(2) . . . . ? C32 Ir2 C35 C36 -39.6(2) . . . . ? C33 Ir2 C35 C36 -80.7(3) . . . . ? C34 Ir2 C35 C36 -117.9(4) . . . . ? Cl2 Ir2 C35 C36 -151.83(18) . . . . ? C16 Ir2 C35 C40 -87.1(5) . . . . ? C21 Ir2 C35 C40 -9.3(4) . . . . ? C36 Ir2 C35 C40 -116.7(5) . . . . ? C32 Ir2 C35 C40 -156.3(4) . . . . ? C33 Ir2 C35 C40 162.5(5) . . . . ? C34 Ir2 C35 C40 125.3(5) . . . . ? Cl2 Ir2 C35 C40 91.4(4) . . . . ? C34 C35 C36 C32 4.8(4) . . . . ? C40 C35 C36 C32 -172.4(4) . . . . ? Ir2 C35 C36 C32 66.9(3) . . . . ? C34 C35 C36 C41 169.4(4) . . . . ? C40 C35 C36 C41 -7.8(6) . . . . ? Ir2 C35 C36 C41 -128.5(4) . . . . ? C34 C35 C36 Ir2 -62.1(3) . . . . ? C40 C35 C36 Ir2 120.7(4) . . . . ? C33 C32 C36 C35 -5.7(4) . . . . ? C37 C32 C36 C35 171.1(4) . . . . ? Ir2 C32 C36 C35 -66.4(3) . . . . ? C33 C32 C36 C41 -170.4(4) . . . . ? C37 C32 C36 C41 6.4(6) . . . . ? Ir2 C32 C36 C41 128.9(4) . . . . ? C33 C32 C36 Ir2 60.7(3) . . . . ? C37 C32 C36 Ir2 -122.5(4) . . . . ? C16 Ir2 C36 C35 -161.3(2) . . . . ? C21 Ir2 C36 C35 -80.8(2) . . . . ? C32 Ir2 C36 C35 114.2(3) . . . . ? C33 Ir2 C36 C35 78.6(2) . . . . ? C34 Ir2 C36 C35 36.6(2) . . . . ? Cl2 Ir2 C36 C35 69.5(4) . . . . ? C16 Ir2 C36 C32 84.5(3) . . . . ? C21 Ir2 C36 C32 165.0(3) . . . . ? C35 Ir2 C36 C32 -114.2(3) . . . . ? C33 Ir2 C36 C32 -35.6(3) . . . . ? C34 Ir2 C36 C32 -77.6(3) . . . . ? Cl2 Ir2 C36 C32 -44.6(5) . . . . ? C16 Ir2 C36 C41 -38.6(5) . . . . ? C21 Ir2 C36 C41 41.9(5) . . . . ? C35 Ir2 C36 C41 122.7(5) . . . . ? C32 Ir2 C36 C41 -123.1(6) . . . . ? C33 Ir2 C36 C41 -158.7(5) . . . . ? C34 Ir2 C36 C41 159.3(5) . . . . ? Cl2 Ir2 C36 C41 -167.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.101 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.125