# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_3 _database_code_depnum_ccdc_archive 'CCDC 914838' #TrackingRef '15993_web_deposit_cif_file_0_TomTeets_1354987002.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H43 Cl5 F24 Ir2 N4 O9 P4' _chemical_formula_weight 1733.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4031(11) _cell_length_b 12.5695(13) _cell_length_c 12.6361(13) _cell_angle_alpha 65.033(2) _cell_angle_beta 70.612(2) _cell_angle_gamma 84.392(2) _cell_volume 1411.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 175(2) _cell_measurement_reflns_used 1054 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 24.12 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 5.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4235 _exptl_absorpt_correction_T_max 0.6250 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 175(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8499 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 30.56 _reflns_number_total 8499 _reflns_number_gt 7197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0532P)^2^+7.6635P] 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 8499 _refine_ls_number_parameters 520 _refine_ls_number_restraints 1269 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.162 _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 -0.86578(2) -1.01086(2) -0.03013(2) 0.03667(9) Uani 1 1 d DU . . P1 P -0.85784(18) -1.06029(19) -0.18606(17) 0.0420(4) Uani 1 1 d U A . O1 O -0.8041(6) -1.1879(6) -0.1719(5) 0.0577(14) Uani 1 1 d U . . Cl1 Cl -0.7904(4) -0.7954(3) -0.1719(3) 0.0451(7) Uani 0.50 1 d PU A 1 N1 N -1.0054(6) -1.0733(6) -0.2042(6) 0.0460(14) Uani 1 1 d U . . C1 C -1.0107(9) -1.1148(10) -0.2960(10) 0.066(3) Uani 1 1 d U A . H1A H -1.1054 -1.1181 -0.2935 0.099 Uiso 0.50 1 calc PR . . H1B H -0.9746 -1.1934 -0.2769 0.099 Uiso 0.50 1 calc PR . . H1C H -0.9555 -1.0605 -0.3785 0.099 Uiso 0.50 1 calc PR . . H1D H -0.9183 -1.1299 -0.3391 0.099 Uiso 0.50 1 calc PR . . H1E H -1.0491 -1.0546 -0.3557 0.099 Uiso 0.50 1 calc PR . . H1F H -1.0682 -1.1875 -0.2541 0.099 Uiso 0.50 1 calc PR . . Cl1S Cl -0.4093(15) -0.4871(18) -0.515(4) 0.358(19) Uani 0.50 1 d PDU B -1 C1S C -0.462(3) -0.503(8) -0.622(5) 0.40(3) Uani 0.50 1 d PDU B -1 H1S1 H -0.4173 -0.5681 -0.6432 0.480 Uiso 0.50 1 calc PR B -1 H1S2 H -0.4483 -0.4297 -0.6976 0.480 Uiso 0.50 1 calc PR B -1 P2 P -0.85586(17) -0.97794(17) 0.13138(17) 0.0386(4) Uani 1 1 d U . . O2 O -0.7568(6) -0.9858(6) -0.3223(5) 0.0543(13) Uani 1 1 d U . . N2 N -0.9039(12) -1.2626(10) 0.1260(18) 0.043(3) Uani 0.50 1 d PDU A 1 N3 N -0.8626(13) -1.2739(9) 0.1231(16) 0.035(3) Uani 0.50 1 d PDU A 2 Cl2 Cl -0.6157(3) -0.9897(4) -0.1248(4) 0.0498(8) Uani 0.50 1 d PU A 2 Cl2S Cl -0.6293(14) -0.5368(9) -0.5342(8) 0.132(3) Uani 0.50 1 d PDU B -1 O3 O -0.8375(6) -1.0922(5) 0.2458(5) 0.0519(12) Uani 1 1 d U . . Cl3 Cl -0.6295(3) -1.0651(4) -0.0524(4) 0.0476(8) Uani 0.50 1 d PU A 1 O4 O -0.7362(6) -0.8976(6) 0.1141(7) 0.0655(17) Uani 1 1 d U . . O5 O -0.9082(9) -0.8400(9) -0.1231(9) 0.0408(19) Uani 0.50 1 d PU A 2 H5 H -0.8403 -0.7955 -0.1450 0.061 Uiso 0.50 1 calc PR A 2 C11 C -0.6647(10) -1.2120(11) -0.2101(13) 0.087(3) Uani 1 1 d DU A . H11W H -0.6241 -1.2213 -0.1463 0.104 Uiso 0.470(16) 1 calc PR C 1 H11X H -0.6151 -1.1455 -0.2875 0.104 Uiso 0.470(16) 1 calc PR C 1 H11Y H -0.6241 -1.2213 -0.1463 0.104 Uiso 0.530(16) 1 calc PR C 2 H11Z H -0.6151 -1.1455 -0.2875 0.104 Uiso 0.530(16) 1 calc PR C 2 C12 C -0.6518(9) -1.3172(10) -0.2294(10) 0.083(3) Uani 1 1 d DU . . C21 C -0.7529(15) -0.8656(10) -0.3827(10) 0.103(4) Uani 1 1 d DU A . H21W H -0.6678 -0.8322 -0.3875 0.124 Uiso 0.52(5) 1 calc PR D 1 H21X H -0.8309 -0.8346 -0.3354 0.124 Uiso 0.52(5) 1 calc PR D 1 H21Y H -0.6678 -0.8322 -0.3875 0.124 Uiso 0.48(5) 1 calc PR D 2 H21Z H -0.8309 -0.8346 -0.3354 0.124 Uiso 0.48(5) 1 calc PR D 2 C22 C -0.7587(14) -0.8297(9) -0.5037(12) 0.126(4) Uani 1 1 d DU . . C31 C -0.7131(11) -1.1448(10) 0.2541(10) 0.076(3) Uani 1 1 d DU A . H31W H -0.6357 -1.0881 0.1946 0.091 Uiso 0.34(10) 1 calc PR E 1 H31X H -0.7044 -1.2139 0.2342 0.091 Uiso 0.34(10) 1 calc PR E 1 H31Y H -0.6357 -1.0881 0.1946 0.091 Uiso 0.66(10) 1 calc PR E 2 H31Z H -0.7044 -1.2139 0.2342 0.091 Uiso 0.66(10) 1 calc PR E 2 C32 C -0.7108(12) -1.1812(10) 0.3799(12) 0.105(3) Uani 1 1 d DU . . C41 C -0.6520(13) -0.8084(11) 0.0043(13) 0.107(5) Uani 1 1 d DU A . H41A H -0.5568 -0.8330 -0.0141 0.128 Uiso 1 1 calc R . . H41B H -0.6835 -0.7965 -0.0656 0.128 Uiso 1 1 calc R . . F11 F -0.5274(17) -1.342(3) -0.279(3) 0.112(8) Uani 0.470(16) 1 d PDU A 1 F12 F -0.690(2) -1.3923(15) -0.1060(14) 0.134(7) Uani 0.470(16) 1 d PDU A 1 F13 F -0.7375(19) -1.345(2) -0.269(3) 0.121(5) Uani 0.470(16) 1 d PDU A 1 F11A F -0.5286(13) -1.361(2) -0.239(2) 0.082(5) Uani 0.530(16) 1 d PDU A 2 F12A F -0.7429(14) -1.4045(12) -0.165(2) 0.111(5) Uani 0.530(16) 1 d PDU A 2 F13A F -0.659(2) -1.2786(19) -0.3457(15) 0.127(6) Uani 0.530(16) 1 d PDU A 2 F21 F -0.733(4) -0.7147(12) -0.568(3) 0.230(10) Uani 0.52(5) 1 d PDU A 1 F22 F -0.891(2) -0.849(3) -0.489(3) 0.164(8) Uani 0.52(5) 1 d PDU A 1 F23 F -0.695(4) -0.882(2) -0.5737(19) 0.137(7) Uani 0.52(5) 1 d PDU A 1 F21A F -0.768(4) -0.7165(14) -0.562(3) 0.228(11) Uani 0.48(5) 1 d PDU A 2 F22A F -0.853(4) -0.887(3) -0.512(3) 0.151(7) Uani 0.48(5) 1 d PDU A 2 F23A F -0.642(3) -0.860(2) -0.568(2) 0.137(8) Uani 0.48(5) 1 d PDU A 2 F31 F -0.755(8) -1.103(4) 0.426(4) 0.132(8) Uani 0.34(10) 1 d PDU A 1 F32 F -0.784(7) -1.280(4) 0.454(4) 0.145(10) Uani 0.34(10) 1 d PDU A 1 F33 F -0.583(3) -1.200(7) 0.382(4) 0.127(9) Uani 0.34(10) 1 d PDU A 1 F31A F -0.708(5) -1.0911(17) 0.409(2) 0.134(6) Uani 0.66(10) 1 d PDU A 2 F32A F -0.816(3) -1.251(3) 0.4644(16) 0.131(7) Uani 0.66(10) 1 d PDU A 2 F33A F -0.600(3) -1.240(4) 0.397(3) 0.135(7) Uani 0.66(10) 1 d PDU A 2 F41 F -0.5757(10) -0.6172(7) -0.0808(10) 0.146(4) Uani 1 1 d DU A . F42 F -0.6135(10) -0.7120(8) 0.1082(10) 0.137(3) Uani 1 1 d DU A . F43 F -0.7785(8) -0.6589(8) 0.0410(10) 0.129(3) Uani 1 1 d DU A . C42 C -0.6572(10) -0.7018(10) 0.0181(11) 0.087(3) Uani 1 1 d DU . . C100 C -0.9504(15) -1.1672(11) 0.0875(12) 0.046(3) Uani 0.50 1 d PDU A 1 C101 C -0.9534(15) -1.3865(14) 0.2035(15) 0.058(4) Uani 0.50 1 d PDU A 1 C102 C -0.824(2) -1.4576(17) 0.214(2) 0.075(6) Uani 0.50 1 d PDU A 1 H10M H -0.7758 -1.4304 0.2533 0.112 Uiso 0.25 1 calc PR A 1 H10N H -0.7634 -1.4460 0.1310 0.112 Uiso 0.25 1 calc PR A 1 H10O H -0.8504 -1.5413 0.2631 0.112 Uiso 0.25 1 calc PR A 1 H10P H -0.8173 -1.5147 0.1783 0.112 Uiso 0.25 1 calc PR A 1 H10Q H -0.8297 -1.4991 0.3006 0.112 Uiso 0.25 1 calc PR A 1 H10R H -0.7427 -1.4038 0.1685 0.112 Uiso 0.25 1 calc PR A 1 C103 C -1.047(2) -1.393(2) 0.3320(18) 0.086(7) Uani 0.50 1 d PDU A 1 H10A H -0.9927 -1.3693 0.3698 0.130 Uiso 0.25 1 calc PR A 1 H10B H -1.0845 -1.4732 0.3854 0.130 Uiso 0.25 1 calc PR A 1 H10C H -1.1212 -1.3394 0.3212 0.130 Uiso 0.25 1 calc PR A 1 H10D H -1.1396 -1.4187 0.3478 0.130 Uiso 0.25 1 calc PR A 1 H10E H -1.0478 -1.3148 0.3322 0.130 Uiso 0.25 1 calc PR A 1 H10F H -1.0110 -1.4486 0.3964 0.130 Uiso 0.25 1 calc PR A 1 C104 C -1.035(3) -1.423(2) 0.140(3) 0.080(7) Uani 0.50 1 d PDU A 1 H12G H -1.1169 -1.3775 0.1385 0.119 Uiso 0.25 1 calc PR A 1 H12H H -1.0619 -1.5070 0.1862 0.119 Uiso 0.25 1 calc PR A 1 H10I H -0.9780 -1.4079 0.0554 0.119 Uiso 0.25 1 calc PR A 1 H10J H -0.9876 -1.4841 0.1149 0.119 Uiso 0.25 1 calc PR A 1 H10K H -1.0426 -1.3546 0.0672 0.119 Uiso 0.25 1 calc PR A 1 H10L H -1.1266 -1.4537 0.1980 0.119 Uiso 0.25 1 calc PR A 1 C105 C -0.8924(16) -1.4034(14) 0.2025(15) 0.056(4) Uani 0.50 1 d PDU A 2 C106 C -0.7523(19) -1.4632(17) 0.193(2) 0.079(6) Uani 0.50 1 d PDU A 2 H11I H -0.7047 -1.4507 0.1073 0.119 Uiso 0.25 1 calc PR A 2 H11J H -0.7681 -1.5477 0.2453 0.119 Uiso 0.25 1 calc PR A 2 H11K H -0.6965 -1.4288 0.2208 0.119 Uiso 0.25 1 calc PR A 2 H11L H -0.7415 -1.5008 0.2749 0.119 Uiso 0.25 1 calc PR A 2 H11M H -0.6781 -1.4037 0.1369 0.119 Uiso 0.25 1 calc PR A 2 H11N H -0.7497 -1.5227 0.1614 0.119 Uiso 0.25 1 calc PR A 2 C107 C -0.970(3) -1.421(2) 0.3379(16) 0.087(7) Uani 0.50 1 d PDU A 2 H10S H -1.0560 -1.3814 0.3419 0.130 Uiso 0.25 1 calc PR A 2 H10T H -0.9133 -1.3866 0.3657 0.130 Uiso 0.25 1 calc PR A 2 H10U H -0.9877 -1.5047 0.3913 0.130 Uiso 0.25 1 calc PR A 2 H10V H -0.9153 -1.4671 0.3907 0.130 Uiso 0.25 1 calc PR A 2 H10W H -1.0581 -1.4618 0.3669 0.130 Uiso 0.25 1 calc PR A 2 H10$ H -0.9837 -1.3437 0.3413 0.130 Uiso 0.25 1 calc PR A 2 C108 C -0.981(2) -1.452(2) 0.153(2) 0.073(6) Uani 0.50 1 d PDU A 2 H11C H -0.9301 -1.4402 0.0678 0.109 Uiso 0.25 1 calc PR A 2 H11D H -1.0659 -1.4110 0.1556 0.109 Uiso 0.25 1 calc PR A 2 H11E H -1.0017 -1.5365 0.2045 0.109 Uiso 0.25 1 calc PR A 2 H11F H -1.0683 -1.4850 0.2175 0.109 Uiso 0.25 1 calc PR A 2 H10G H -0.9326 -1.5141 0.1297 0.109 Uiso 0.25 1 calc PR A 2 H10H H -0.9968 -1.3886 0.0808 0.109 Uiso 0.25 1 calc PR A 2 C110 C -0.8644(12) -1.1777(11) 0.0690(12) 0.039(2) Uani 0.50 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02512(12) 0.05164(17) 0.03523(13) -0.01870(11) -0.01151(9) 0.00279(9) P1 0.0317(8) 0.0608(11) 0.0373(8) -0.0243(8) -0.0123(7) 0.0081(7) O1 0.055(3) 0.072(4) 0.050(3) -0.033(3) -0.018(3) 0.026(3) Cl1 0.0413(16) 0.0504(19) 0.0406(16) -0.0164(14) -0.0117(14) -0.0019(14) N1 0.033(3) 0.065(4) 0.052(3) -0.035(3) -0.016(2) 0.007(3) C1 0.043(4) 0.105(8) 0.084(6) -0.069(6) -0.023(4) 0.009(4) Cl1S 0.096(8) 0.241(18) 0.80(6) -0.35(3) -0.039(16) -0.021(9) C1S 0.15(3) 0.35(6) 0.70(8) -0.29(7) -0.03(4) -0.05(5) P2 0.0279(7) 0.0528(10) 0.0412(8) -0.0226(8) -0.0144(6) 0.0018(7) O2 0.045(3) 0.075(4) 0.042(3) -0.028(2) -0.006(2) -0.002(3) N2 0.014(7) 0.067(6) 0.052(7) -0.026(5) -0.011(6) -0.001(5) N3 0.015(6) 0.055(5) 0.043(6) -0.026(4) -0.009(6) -0.002(4) Cl2 0.0267(14) 0.067(3) 0.064(2) -0.036(2) -0.0111(15) 0.0018(15) Cl2S 0.197(11) 0.110(6) 0.093(5) -0.054(5) -0.032(6) -0.002(7) O3 0.047(3) 0.071(3) 0.046(3) -0.027(2) -0.024(2) 0.013(2) Cl3 0.0273(14) 0.064(2) 0.068(2) -0.040(2) -0.0208(15) 0.0119(15) O4 0.043(3) 0.082(4) 0.087(4) -0.055(4) -0.010(3) -0.013(3) O5 0.025(4) 0.052(5) 0.041(4) -0.015(4) -0.009(4) -0.004(3) C11 0.055(5) 0.104(7) 0.145(10) -0.092(7) -0.039(6) 0.030(5) C12 0.071(6) 0.095(7) 0.108(7) -0.067(6) -0.037(6) 0.033(5) C21 0.141(11) 0.076(6) 0.072(5) -0.041(4) 0.021(5) -0.045(7) C22 0.160(10) 0.081(7) 0.071(6) -0.004(5) 0.008(7) 0.000(8) C31 0.082(6) 0.096(7) 0.089(5) -0.060(5) -0.060(5) 0.048(5) C32 0.131(9) 0.117(8) 0.106(8) -0.056(6) -0.088(7) 0.064(6) C41 0.080(7) 0.099(7) 0.122(9) -0.073(7) 0.040(7) -0.041(6) F11 0.091(8) 0.110(13) 0.135(16) -0.080(12) -0.006(9) 0.038(9) F12 0.124(13) 0.105(9) 0.125(9) -0.033(9) -0.014(8) 0.063(10) F13 0.109(10) 0.141(13) 0.174(14) -0.126(11) -0.039(10) 0.006(9) F11A 0.069(6) 0.087(9) 0.106(12) -0.061(9) -0.026(7) 0.031(6) F12A 0.082(7) 0.093(8) 0.183(13) -0.073(9) -0.058(9) 0.022(6) F13A 0.136(14) 0.194(16) 0.115(9) -0.114(9) -0.065(9) 0.058(11) F21 0.25(2) 0.083(7) 0.146(12) 0.033(8) 0.076(14) 0.026(10) F22 0.158(11) 0.174(17) 0.096(13) -0.008(11) -0.042(10) 0.063(11) F23 0.180(16) 0.144(11) 0.049(6) -0.032(7) -0.003(9) 0.005(12) F21A 0.26(2) 0.094(8) 0.131(12) 0.034(9) 0.064(14) 0.023(10) F22A 0.188(14) 0.174(14) 0.077(10) -0.024(10) -0.068(10) 0.029(12) F23A 0.191(14) 0.091(11) 0.061(8) -0.027(7) 0.048(11) -0.033(11) F31 0.14(2) 0.206(14) 0.137(13) -0.124(12) -0.109(14) 0.089(14) F32 0.154(17) 0.150(13) 0.109(13) -0.023(12) -0.070(14) 0.050(14) F33 0.148(10) 0.15(2) 0.146(15) -0.083(15) -0.123(11) 0.084(11) F31A 0.149(17) 0.204(10) 0.156(11) -0.138(9) -0.116(11) 0.083(9) F32A 0.152(10) 0.149(12) 0.091(7) -0.035(8) -0.073(7) 0.066(9) F33A 0.152(9) 0.146(16) 0.158(11) -0.068(11) -0.127(9) 0.083(10) F41 0.109(6) 0.085(5) 0.208(8) -0.045(6) -0.017(6) -0.029(5) F42 0.150(8) 0.108(6) 0.225(9) -0.088(6) -0.124(8) 0.005(5) F43 0.090(5) 0.106(6) 0.164(8) -0.037(6) -0.044(5) 0.042(4) C42 0.060(5) 0.079(6) 0.133(9) -0.051(6) -0.033(6) 0.000(5) C100 0.044(7) 0.062(6) 0.035(5) -0.023(5) -0.010(5) -0.009(5) C101 0.041(8) 0.063(7) 0.065(8) -0.018(7) -0.019(7) -0.008(7) C102 0.068(11) 0.057(10) 0.099(15) -0.021(10) -0.042(12) 0.002(9) C103 0.092(17) 0.068(15) 0.066(10) -0.011(9) 0.003(11) -0.027(12) C104 0.091(17) 0.053(12) 0.109(15) -0.023(11) -0.062(15) -0.005(10) C105 0.048(9) 0.062(7) 0.058(8) -0.024(7) -0.015(8) -0.004(7) C106 0.054(10) 0.054(10) 0.113(17) -0.015(11) -0.031(11) -0.003(8) C107 0.095(17) 0.087(17) 0.053(8) -0.013(8) -0.007(11) -0.020(14) C108 0.068(13) 0.063(13) 0.098(14) -0.033(12) -0.037(12) -0.010(10) C110 0.019(5) 0.061(5) 0.043(6) -0.024(4) -0.016(5) 0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C110 1.938(12) . ? Ir1 C100 1.962(12) . ? Ir1 O5 2.054(10) . ? Ir1 P1 2.2783(18) . ? Ir1 P2 2.2821(17) . ? Ir1 Cl3 2.442(3) . ? Ir1 Cl2 2.464(3) . ? Ir1 Cl1 2.559(4) . ? Ir1 Ir1 2.6584(5) 2_335 ? P1 O1 1.602(6) . ? P1 O2 1.604(6) . ? P1 N1 1.658(6) . ? O1 C11 1.414(11) . ? N1 C1 1.476(10) . ? N1 P2 1.668(6) 2_335 ? Cl1S C1S 1.70(2) . ? C1S Cl2S 1.71(2) . ? P2 O4 1.581(6) . ? P2 O3 1.602(6) . ? P2 N1 1.668(6) 2_335 ? O2 C21 1.373(13) . ? N2 C100 1.208(13) . ? N2 C101 1.477(17) . ? N3 C110 1.111(14) . ? N3 C105 1.505(17) . ? O3 C31 1.409(10) . ? O4 C41 1.421(13) . ? C11 C12 1.429(14) . ? C12 F13 1.290(12) . ? C12 F12A 1.305(12) . ? C12 F11 1.309(13) . ? C12 F11A 1.332(12) . ? C12 F13A 1.367(12) . ? C12 F12 1.378(13) . ? C21 C22 1.420(17) . ? C22 F23 1.295(14) . ? C22 F21A 1.310(13) . ? C22 F21 1.327(13) . ? C22 F22A 1.333(14) . ? C22 F23A 1.341(14) . ? C22 F22 1.352(14) . ? C31 C32 1.465(14) . ? C32 F32A 1.313(13) . ? C32 F31 1.317(14) . ? C32 F32 1.319(14) . ? C32 F33 1.334(14) . ? C32 F31A 1.334(13) . ? C32 F33A 1.336(12) . ? C41 C42 1.416(15) . ? F41 C42 1.327(11) . ? F42 C42 1.316(11) . ? F43 C42 1.312(10) . ? C101 C102 1.554(15) . ? C101 C104 1.555(15) . ? C101 C103 1.563(15) . ? C105 C107 1.558(15) . ? C105 C108 1.559(15) . ? C105 C106 1.565(15) . ? 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 C110 Ir1 C100 25.4(5) . . ? C110 Ir1 O5 168.7(4) . . ? C100 Ir1 O5 143.3(5) . . ? C110 Ir1 P1 86.6(4) . . ? C100 Ir1 P1 88.5(4) . . ? O5 Ir1 P1 92.9(3) . . ? C110 Ir1 P2 88.3(4) . . ? C100 Ir1 P2 88.8(4) . . ? O5 Ir1 P2 93.0(3) . . ? P1 Ir1 P2 173.28(6) . . ? C110 Ir1 Cl3 71.3(4) . . ? C100 Ir1 Cl3 96.7(4) . . ? O5 Ir1 Cl3 120.0(3) . . ? P1 Ir1 Cl3 89.48(10) . . ? P2 Ir1 Cl3 84.75(10) . . ? C110 Ir1 Cl2 93.3(4) . . ? C100 Ir1 Cl2 118.7(4) . . ? O5 Ir1 Cl2 97.9(3) . . ? P1 Ir1 Cl2 83.76(10) . . ? P2 Ir1 Cl2 92.18(10) . . ? Cl3 Ir1 Cl2 23.07(13) . . ? C110 Ir1 Cl1 162.7(4) . . ? C100 Ir1 Cl1 171.4(4) . . ? O5 Ir1 Cl1 28.6(3) . . ? P1 Ir1 Cl1 94.52(10) . . ? P2 Ir1 Cl1 89.07(10) . . ? Cl3 Ir1 Cl1 91.44(14) . . ? Cl2 Ir1 Cl1 69.73(14) . . ? C110 Ir1 Ir1 98.6(4) . 2_335 ? C100 Ir1 Ir1 73.2(4) . 2_335 ? O5 Ir1 Ir1 70.1(2) . 2_335 ? P1 Ir1 Ir1 92.92(5) . 2_335 ? P2 Ir1 Ir1 92.16(4) . 2_335 ? Cl3 Ir1 Ir1 169.51(12) . 2_335 ? Cl2 Ir1 Ir1 167.41(12) . 2_335 ? Cl1 Ir1 Ir1 98.54(8) . 2_335 ? O1 P1 O2 98.0(3) . . ? O1 P1 N1 98.6(3) . . ? O2 P1 N1 105.3(3) . . ? O1 P1 Ir1 115.5(2) . . ? O2 P1 Ir1 119.1(2) . . ? N1 P1 Ir1 117.0(2) . . ? C11 O1 P1 124.0(7) . . ? C1 N1 P1 120.5(5) . . ? C1 N1 P2 120.0(5) . 2_335 ? P1 N1 P2 119.0(4) . 2_335 ? Cl1S C1S Cl2S 96.4(17) . . ? O4 P2 O3 97.9(4) . . ? O4 P2 N1 103.0(3) . 2_335 ? O3 P2 N1 99.8(3) . 2_335 ? O4 P2 Ir1 120.5(3) . . ? O3 P2 Ir1 115.4(2) . . ? N1 P2 Ir1 116.8(2) 2_335 . ? C21 O2 P1 124.3(6) . . ? C100 N2 C101 138.7(12) . . ? C110 N3 C105 167.8(13) . . ? C31 O3 P2 125.6(6) . . ? C41 O4 P2 129.0(8) . . ? O1 C11 C12 109.8(8) . . ? F13 C12 F12A 54.7(12) . . ? F13 C12 F11 111.7(16) . . ? F12A C12 F11 116.8(18) . . ? F13 C12 F11A 123.1(16) . . ? F12A C12 F11A 108.4(13) . . ? F11 C12 F11A 19.8(19) . . ? F13 C12 F13A 49.0(12) . . ? F12A C12 F13A 103.1(13) . . ? F11 C12 F13A 84.3(16) . . ? F11A C12 F13A 103.8(13) . . ? F13 C12 F12 104.1(15) . . ? F12A C12 F12 49.6(12) . . ? F11 C12 F12 105.9(15) . . ? F11A C12 F12 86.9(13) . . ? F13A C12 F12 152.7(16) . . ? F13 C12 C11 120.4(11) . . ? F12A C12 C11 122.6(11) . . ? F11 C12 C11 116.0(16) . . ? F11A C12 C11 113.7(13) . . ? F13A C12 C11 102.8(11) . . ? F12 C12 C11 95.3(11) . . ? O2 C21 C22 111.5(9) . . ? F23 C22 F21A 115(3) . . ? F23 C22 F21 108.9(17) . . ? F21A C22 F21 15(3) . . ? F23 C22 F22A 73.0(18) . . ? F21A C22 F22A 109(2) . . ? F21 C22 F22A 122(3) . . ? F23 C22 F23A 29.5(18) . . ? F21A C22 F23A 107.7(18) . . ? F21 C22 F23A 96(2) . . ? F22A C22 F23A 102.4(16) . . ? F23 C22 F22 101.9(17) . . ? F21A C22 F22 90(2) . . ? F21 C22 F22 105.7(19) . . ? F22A C22 F22 29.9(17) . . ? F23A C22 F22 131(2) . . ? F23 C22 C21 122.5(16) . . ? F21A C22 C21 114.6(19) . . ? F21 C22 C21 110.8(18) . . ? F22A C22 C21 114.9(14) . . ? F23A C22 C21 106.9(16) . . ? F22 C22 C21 105.4(14) . . ? O3 C31 C32 108.6(8) . . ? F32A C32 F31 88(3) . . ? F32A C32 F32 22(3) . . ? F31 C32 F32 109(2) . . ? F32A C32 F33 123(3) . . ? F31 C32 F33 106.2(19) . . ? F32 C32 F33 107.9(19) . . ? F32A C32 F31A 106.5(15) . . ? F31 C32 F31A 21(3) . . ? F32 C32 F31A 125(3) . . ? F33 C32 F31A 88(3) . . ? F32A C32 F33A 106.3(14) . . ? F31 C32 F33A 121(3) . . ? F32 C32 F33A 88(3) . . ? F33 C32 F33A 21(3) . . ? F31A C32 F33A 105.5(13) . . ? F32A C32 C31 113.1(13) . . ? F31 C32 C31 114.1(19) . . ? F32 C32 C31 109.9(19) . . ? F33 C32 C31 109.6(18) . . ? F31A C32 C31 113.3(13) . . ? F33A C32 C31 111.6(14) . . ? C42 C41 O4 110.2(9) . . ? F43 C42 F42 105.6(10) . . ? F43 C42 F41 106.5(10) . . ? F42 C42 F41 104.1(10) . . ? F43 C42 C41 115.4(10) . . ? F42 C42 C41 112.2(11) . . ? F41 C42 C41 112.2(10) . . ? N2 C100 Ir1 132.6(11) . . ? N2 C101 C102 105.8(12) . . ? N2 C101 C104 108.2(13) . . ? C102 C101 C104 112.9(14) . . ? N2 C101 C103 106.9(14) . . ? C102 C101 C103 111.4(15) . . ? C104 C101 C103 111.2(14) . . ? N3 C105 C107 108.5(14) . . ? N3 C105 C108 108.6(13) . . ? C107 C105 C108 111.1(14) . . ? N3 C105 C106 107.4(12) . . ? C107 C105 C106 110.5(15) . . ? C108 C105 C106 110.6(14) . . ? N3 C110 Ir1 178.1(15) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.186 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.188 data_5 _database_code_depnum_ccdc_archive 'CCDC 914839' #TrackingRef '15993_web_deposit_cif_file_0_TomTeets_1354987002.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 Cl4 F24 Ir2 N4 O8 P4' _chemical_formula_weight 1666.72 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7559(9) _cell_length_b 19.5938(14) _cell_length_c 21.0181(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.9880(10) _cell_angle_gamma 90.00 _cell_volume 5202.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9693 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 30.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 5.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2140 _exptl_absorpt_correction_T_max 0.3364 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 117116 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.03 _reflns_number_total 15213 _reflns_number_gt 12283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0317P)^2^+20.0826P] 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 15213 _refine_ls_number_parameters 695 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.647487(12) 0.701831(8) 0.265345(7) 0.01817(4) Uani 1 1 d . . . Ir2 Ir 0.713623(12) 0.730872(8) 0.393043(7) 0.01746(4) Uani 1 1 d . . . P1 P 0.81024(9) 0.73116(6) 0.24189(5) 0.0210(2) Uani 1 1 d . . . P2 P 0.88329(8) 0.70910(5) 0.37626(5) 0.0191(2) Uani 1 1 d . . . P3 P 0.48398(9) 0.67554(6) 0.29257(5) 0.0251(2) Uani 1 1 d . . . P4 P 0.54296(9) 0.74931(6) 0.41116(5) 0.0203(2) Uani 1 1 d . . . Cl1 Cl 0.58147(8) 0.81599(5) 0.24797(5) 0.0245(2) Uani 1 1 d . . . Cl2 Cl 0.58590(8) 0.67852(6) 0.15062(5) 0.0250(2) Uani 1 1 d . . . Cl3 Cl 0.69184(8) 0.61364(5) 0.42193(5) 0.02318(19) Uani 1 1 d . . . Cl4 Cl 0.77597(8) 0.75947(5) 0.50714(5) 0.02351(19) Uani 1 1 d . . . N1 N 0.9095(3) 0.7198(2) 0.30164(18) 0.0256(8) Uani 1 1 d . . . N2 N 0.4478(3) 0.7224(2) 0.35349(18) 0.0265(8) Uani 1 1 d . . . N3 N 0.7120(3) 0.55084(18) 0.27475(17) 0.0245(7) Uani 1 1 d . . . N4 N 0.7374(3) 0.88474(18) 0.37302(17) 0.0238(7) Uani 1 1 d . . . O1 O 0.8307(3) 0.80924(16) 0.22438(15) 0.0259(6) Uani 1 1 d . . . O2 O 0.8550(3) 0.69711(17) 0.18215(16) 0.0296(7) Uani 1 1 d . . . O3 O 0.9304(2) 0.63476(16) 0.39201(15) 0.0259(6) Uani 1 1 d . . . O4 O 0.9767(2) 0.75061(16) 0.41868(15) 0.0253(6) Uani 1 1 d . . . O5 O 0.4694(3) 0.59662(17) 0.31000(16) 0.0342(8) Uani 1 1 d . . . O6 O 0.3821(3) 0.68019(19) 0.23948(16) 0.0337(7) Uani 1 1 d . . . O7 O 0.5023(3) 0.71722(18) 0.47328(15) 0.0299(7) Uani 1 1 d . . . O8 O 0.5068(2) 0.82688(16) 0.41641(15) 0.0258(6) Uani 1 1 d . . . C1 C 1.0212(4) 0.7213(3) 0.2883(3) 0.0396(12) Uani 1 1 d . . . H1A H 1.0591 0.7586 0.3125 0.059 Uiso 1 1 calc R . . H1B H 1.0223 0.7283 0.2423 0.059 Uiso 1 1 calc R . . H1C H 1.0556 0.6778 0.3015 0.059 Uiso 1 1 calc R . . C2 C 0.3354(4) 0.7338(3) 0.3622(3) 0.0356(11) Uani 1 1 d . . . H2A H 0.3247 0.7197 0.4055 0.053 Uiso 1 1 calc R . . H2B H 0.2893 0.7069 0.3304 0.053 Uiso 1 1 calc R . . H2C H 0.3182 0.7823 0.3563 0.053 Uiso 1 1 calc R . . C11 C 0.7899(4) 0.8357(2) 0.1627(2) 0.0282(9) Uani 1 1 d . . . H11A H 0.7286 0.8659 0.1660 0.034 Uiso 1 1 calc R . . H11B H 0.7663 0.7980 0.1328 0.034 Uiso 1 1 calc R . . C12 C 0.8765(5) 0.8750(3) 0.1387(2) 0.0359(11) Uani 1 1 d . . . C21 C 0.8254(4) 0.6351(2) 0.1486(2) 0.0286(9) Uani 1 1 d . . . H21A H 0.7871 0.6453 0.1054 0.034 Uiso 1 1 calc R . . H21B H 0.7782 0.6080 0.1725 0.034 Uiso 1 1 calc R . . C22 C 0.9231(5) 0.5959(3) 0.1427(3) 0.0480(15) Uani 1 1 d . . . C31 C 0.9555(4) 0.6125(2) 0.4575(2) 0.0291(9) Uani 1 1 d . . . H31A H 0.9082 0.5746 0.4662 0.035 Uiso 1 1 calc R . . H31B H 0.9460 0.6506 0.4871 0.035 Uiso 1 1 calc R . . C32 C 1.0682(5) 0.5892(3) 0.4670(3) 0.0443(13) Uani 1 1 d . . . C41 C 0.9738(4) 0.8228(3) 0.4271(3) 0.0363(11) Uani 1 1 d . . . H41A H 0.9284 0.8344 0.4601 0.044 Uiso 1 1 calc R . . H41B H 0.9442 0.8451 0.3862 0.044 Uiso 1 1 calc R . . C42 C 1.0835(5) 0.8466(3) 0.4476(3) 0.0425(13) Uani 1 1 d . . . C51 C 0.4402(4) 0.5706(3) 0.3678(2) 0.0356(11) Uani 1 1 d . . . H51A H 0.4358 0.6084 0.3986 0.043 Uiso 1 1 calc R . . H51B H 0.4947 0.5380 0.3874 0.043 Uiso 1 1 calc R . . C52 C 0.3353(4) 0.5352(3) 0.3549(3) 0.0383(12) Uani 1 1 d . . . C61 C 0.3581(4) 0.7341(3) 0.1944(3) 0.0454(14) Uani 1 1 d DU A . H61A H 0.4061 0.7320 0.1613 0.054 Uiso 0.644(12) 1 calc PR A 1 H61B H 0.3682 0.7787 0.2165 0.054 Uiso 0.644(12) 1 calc PR A 1 H61C H 0.4061 0.7320 0.1613 0.054 Uiso 0.356(12) 1 calc PR A 2 H61D H 0.3682 0.7787 0.2165 0.054 Uiso 0.356(12) 1 calc PR A 2 C62 C 0.2486(5) 0.7270(3) 0.1644(3) 0.0525(15) Uani 1 1 d DU . . C71 C 0.5576(4) 0.6855(2) 0.5295(2) 0.0261(9) Uani 1 1 d . . . H71A H 0.5815 0.7202 0.5626 0.031 Uiso 1 1 calc R . . H71B H 0.6203 0.6604 0.5189 0.031 Uiso 1 1 calc R . . C72 C 0.4802(4) 0.6374(3) 0.5531(2) 0.0347(11) Uani 1 1 d . . . C81 C 0.5323(4) 0.8656(2) 0.4742(2) 0.0305(10) Uani 1 1 d . . . H81A H 0.5841 0.9018 0.4679 0.037 Uiso 1 1 calc R . . H81B H 0.5637 0.8356 0.5097 0.037 Uiso 1 1 calc R . . C82 C 0.4320(5) 0.8969(4) 0.4901(3) 0.0515(16) Uani 1 1 d . . . C100 C 0.6900(3) 0.6082(2) 0.27533(19) 0.0215(8) Uani 1 1 d . . . C101 C 0.7332(4) 0.4774(2) 0.2820(2) 0.0311(10) Uani 1 1 d U . . C102 C 0.8436(7) 0.4711(4) 0.3158(5) 0.094(3) Uani 1 1 d U . . H10A H 0.8925 0.4940 0.2907 0.141 Uiso 1 1 calc R . . H10B H 0.8626 0.4227 0.3207 0.141 Uiso 1 1 calc R . . H10C H 0.8484 0.4923 0.3583 0.141 Uiso 1 1 calc R . . C103 C 0.7212(9) 0.4460(4) 0.2171(4) 0.091(3) Uani 1 1 d U . . H10D H 0.6475 0.4504 0.1968 0.137 Uiso 1 1 calc R . . H10E H 0.7403 0.3976 0.2209 0.137 Uiso 1 1 calc R . . H10F H 0.7678 0.4693 0.1907 0.137 Uiso 1 1 calc R . . C104 C 0.6548(7) 0.4491(3) 0.3226(4) 0.072(2) Uani 1 1 d U . . H10G H 0.6569 0.4763 0.3619 0.108 Uiso 1 1 calc R . . H10H H 0.6731 0.4016 0.3339 0.108 Uiso 1 1 calc R . . H10I H 0.5835 0.4509 0.2983 0.108 Uiso 1 1 calc R . . C200 C 0.7268(3) 0.8261(2) 0.37575(19) 0.0211(8) Uani 1 1 d . . . C201 C 0.7438(4) 0.9589(2) 0.3636(2) 0.0258(9) Uani 1 1 d . . . C202 C 0.8217(4) 0.9714(3) 0.3164(3) 0.0386(12) Uani 1 1 d . . . H20A H 0.8924 0.9562 0.3353 0.058 Uiso 1 1 calc R . . H20B H 0.8237 1.0203 0.3066 0.058 Uiso 1 1 calc R . . H20C H 0.7993 0.9459 0.2767 0.058 Uiso 1 1 calc R . . C203 C 0.6329(4) 0.9836(2) 0.3378(2) 0.0306(10) Uani 1 1 d . . . H20D H 0.6075 0.9597 0.2976 0.046 Uiso 1 1 calc R . . H20E H 0.6346 1.0329 0.3297 0.046 Uiso 1 1 calc R . . H20F H 0.5851 0.9743 0.3694 0.046 Uiso 1 1 calc R . . C204 C 0.7840(5) 0.9907(3) 0.4293(3) 0.0428(13) Uani 1 1 d . . . H20G H 0.7356 0.9790 0.4599 0.064 Uiso 1 1 calc R . . H20H H 0.7873 1.0404 0.4249 0.064 Uiso 1 1 calc R . . H20I H 0.8548 0.9730 0.4448 0.064 Uiso 1 1 calc R . . F11 F 0.9107(3) 0.92724(17) 0.17779(16) 0.0512(9) Uani 1 1 d . . . F12 F 0.9616(3) 0.83679(18) 0.13265(17) 0.0485(8) Uani 1 1 d . . . F13 F 0.8420(3) 0.90160(16) 0.08076(15) 0.0496(9) Uani 1 1 d . . . F21 F 0.9743(4) 0.5782(2) 0.2012(3) 0.0873(16) Uani 1 1 d . . . F22 F 0.8995(3) 0.5383(2) 0.1118(2) 0.0791(14) Uani 1 1 d . . . F23 F 0.9928(3) 0.6297(2) 0.1141(2) 0.0744(13) Uani 1 1 d . . . F31 F 1.0936(3) 0.5655(2) 0.5269(2) 0.0694(12) Uani 1 1 d . . . F32 F 1.0839(3) 0.53810(19) 0.4274(2) 0.0640(11) Uani 1 1 d . . . F33 F 1.1364(3) 0.63822(19) 0.4574(2) 0.0577(10) Uani 1 1 d . . . F41 F 1.1255(3) 0.8155(2) 0.5026(2) 0.0724(12) Uani 1 1 d . . . F42 F 1.1491(3) 0.8337(2) 0.4067(2) 0.0691(12) Uani 1 1 d . . . F43 F 1.0847(3) 0.91298(18) 0.4602(2) 0.0581(10) Uani 1 1 d . . . F51 F 0.2581(3) 0.5748(2) 0.3282(2) 0.0605(10) Uani 1 1 d . . . F52 F 0.3103(3) 0.50887(19) 0.40917(17) 0.0546(9) Uani 1 1 d . . . F53 F 0.3404(3) 0.48270(18) 0.31396(16) 0.0499(8) Uani 1 1 d . . . F61 F 0.1791(5) 0.7102(6) 0.1992(4) 0.077(3) Uani 0.644(12) 1 d PDU A 1 F62 F 0.2516(6) 0.6667(3) 0.1260(3) 0.063(2) Uani 0.644(12) 1 d PDU A 1 F61A F 0.2073(12) 0.7692(8) 0.2144(7) 0.092(5) Uani 0.356(12) 1 d PDU A 2 F62A F 0.1895(13) 0.6768(8) 0.1683(9) 0.098(7) Uani 0.356(12) 1 d PDU A 2 F63 F 0.2188(3) 0.7740(2) 0.1217(2) 0.0635(11) Uani 1 1 d DU A . F71 F 0.3936(3) 0.6694(2) 0.56735(18) 0.0560(10) Uani 1 1 d . . . F72 F 0.4470(3) 0.58783(19) 0.51247(16) 0.0574(10) Uani 1 1 d . . . F73 F 0.5270(3) 0.60750(18) 0.60736(15) 0.0483(8) Uani 1 1 d . . . F81 F 0.3830(4) 0.9338(3) 0.4414(2) 0.0912(18) Uani 1 1 d . . . F82 F 0.3657(3) 0.8509(3) 0.5058(2) 0.0843(15) Uani 1 1 d . . . F83 F 0.4551(4) 0.9397(2) 0.53996(17) 0.0720(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01996(8) 0.01713(7) 0.01764(7) 0.00006(5) 0.00340(5) 0.00027(5) Ir2 0.01799(7) 0.01695(7) 0.01792(7) -0.00091(5) 0.00412(5) -0.00058(5) P1 0.0205(5) 0.0233(5) 0.0202(5) -0.0002(4) 0.0061(4) -0.0006(4) P2 0.0186(5) 0.0185(5) 0.0207(5) 0.0000(4) 0.0043(4) 0.0006(4) P3 0.0251(6) 0.0272(5) 0.0233(5) -0.0019(4) 0.0044(4) -0.0035(4) P4 0.0195(5) 0.0217(5) 0.0205(5) -0.0010(4) 0.0056(4) -0.0003(4) Cl1 0.0254(5) 0.0200(4) 0.0274(5) 0.0011(4) 0.0013(4) 0.0018(4) Cl2 0.0267(5) 0.0293(5) 0.0190(4) 0.0004(4) 0.0030(4) 0.0038(4) Cl3 0.0284(5) 0.0191(4) 0.0229(4) 0.0007(4) 0.0064(4) -0.0019(4) Cl4 0.0250(5) 0.0259(5) 0.0198(4) -0.0026(4) 0.0036(4) -0.0030(4) N1 0.0171(17) 0.036(2) 0.0242(17) 0.0015(15) 0.0049(14) 0.0007(15) N2 0.0198(18) 0.034(2) 0.0268(18) -0.0013(16) 0.0053(14) -0.0011(15) N3 0.030(2) 0.0202(17) 0.0237(17) -0.0004(14) 0.0047(15) 0.0006(14) N4 0.0237(18) 0.0214(17) 0.0254(17) -0.0032(14) 0.0001(14) 0.0003(14) O1 0.0291(17) 0.0239(15) 0.0247(15) 0.0016(12) 0.0036(12) -0.0063(12) O2 0.0311(17) 0.0309(17) 0.0286(16) -0.0041(13) 0.0106(13) -0.0012(13) O3 0.0277(16) 0.0233(15) 0.0268(15) 0.0013(12) 0.0045(12) 0.0047(12) O4 0.0192(15) 0.0237(15) 0.0328(16) -0.0035(13) 0.0030(12) -0.0005(12) O5 0.045(2) 0.0275(17) 0.0328(18) -0.0026(14) 0.0146(15) -0.0072(15) O6 0.0292(18) 0.0382(19) 0.0330(18) -0.0019(15) 0.0019(14) -0.0041(15) O7 0.0263(17) 0.0387(18) 0.0267(16) 0.0083(14) 0.0103(13) 0.0011(14) O8 0.0272(16) 0.0240(15) 0.0271(15) -0.0030(12) 0.0073(12) 0.0062(12) C1 0.021(2) 0.066(4) 0.033(3) 0.000(2) 0.0093(19) 0.000(2) C2 0.022(2) 0.047(3) 0.038(3) -0.008(2) 0.0068(19) 0.003(2) C11 0.032(2) 0.026(2) 0.026(2) 0.0051(18) 0.0043(18) 0.0012(18) C12 0.048(3) 0.030(2) 0.034(3) 0.001(2) 0.018(2) -0.001(2) C21 0.031(2) 0.028(2) 0.028(2) -0.0009(18) 0.0077(18) 0.0021(18) C22 0.037(3) 0.040(3) 0.068(4) -0.015(3) 0.012(3) 0.008(2) C31 0.027(2) 0.029(2) 0.031(2) 0.0068(19) 0.0008(18) 0.0046(18) C32 0.037(3) 0.039(3) 0.055(3) 0.016(3) 0.001(3) 0.009(2) C41 0.027(2) 0.031(2) 0.050(3) -0.008(2) 0.004(2) -0.007(2) C42 0.036(3) 0.035(3) 0.055(3) -0.005(3) 0.001(3) -0.010(2) C51 0.038(3) 0.034(3) 0.037(3) 0.001(2) 0.011(2) -0.010(2) C52 0.038(3) 0.038(3) 0.040(3) -0.002(2) 0.011(2) -0.010(2) C61 0.027(2) 0.044(3) 0.063(4) 0.016(3) 0.000(2) 0.000(2) C62 0.037(3) 0.070(4) 0.048(3) 0.021(3) 0.000(2) -0.010(3) C71 0.031(2) 0.028(2) 0.0192(19) 0.0001(17) 0.0041(17) -0.0022(18) C72 0.041(3) 0.038(3) 0.025(2) 0.001(2) 0.007(2) -0.009(2) C81 0.035(3) 0.028(2) 0.030(2) -0.0045(19) 0.0089(19) 0.0008(19) C82 0.050(4) 0.067(4) 0.038(3) -0.015(3) 0.006(3) 0.028(3) C100 0.022(2) 0.026(2) 0.0165(17) -0.0003(15) 0.0015(15) -0.0026(16) C101 0.044(3) 0.0158(19) 0.034(2) 0.0013(17) 0.010(2) 0.0024(18) C102 0.074(5) 0.045(4) 0.149(9) 0.016(5) -0.034(5) 0.018(4) C103 0.186(10) 0.036(3) 0.055(4) -0.015(3) 0.028(5) 0.005(5) C104 0.099(6) 0.030(3) 0.096(6) 0.005(3) 0.050(5) -0.005(3) C200 0.0153(18) 0.027(2) 0.0211(18) -0.0059(16) 0.0024(14) 0.0017(15) C201 0.030(2) 0.0152(18) 0.031(2) -0.0025(17) 0.0025(18) -0.0021(16) C202 0.036(3) 0.031(3) 0.050(3) 0.009(2) 0.011(2) -0.004(2) C203 0.036(3) 0.024(2) 0.031(2) -0.0007(18) 0.0026(19) 0.0029(19) C204 0.055(4) 0.026(2) 0.044(3) -0.010(2) -0.009(3) 0.001(2) F11 0.069(2) 0.0398(18) 0.0493(19) -0.0080(15) 0.0234(17) -0.0270(17) F12 0.0450(19) 0.049(2) 0.057(2) 0.0071(16) 0.0272(16) 0.0008(15) F13 0.081(3) 0.0346(17) 0.0374(17) 0.0099(14) 0.0230(17) 0.0031(16) F21 0.079(3) 0.063(3) 0.109(4) -0.002(3) -0.025(3) 0.039(2) F22 0.069(3) 0.053(2) 0.121(4) -0.048(3) 0.035(3) 0.003(2) F23 0.046(2) 0.084(3) 0.103(3) -0.038(3) 0.042(2) -0.010(2) F31 0.060(3) 0.072(3) 0.070(3) 0.033(2) -0.014(2) 0.012(2) F32 0.047(2) 0.047(2) 0.100(3) 0.001(2) 0.018(2) 0.0241(17) F33 0.0322(18) 0.052(2) 0.085(3) 0.019(2) -0.0039(17) -0.0030(15) F41 0.058(3) 0.074(3) 0.074(3) 0.001(2) -0.029(2) -0.008(2) F42 0.036(2) 0.075(3) 0.103(3) -0.027(2) 0.028(2) -0.0204(19) F43 0.050(2) 0.0386(18) 0.083(3) -0.0149(18) -0.0012(19) -0.0183(16) F51 0.0364(19) 0.060(2) 0.085(3) 0.003(2) 0.0088(19) -0.0026(17) F52 0.061(2) 0.060(2) 0.0470(19) 0.0000(17) 0.0222(17) -0.0269(18) F53 0.058(2) 0.0462(19) 0.0447(19) -0.0070(15) 0.0046(16) -0.0183(16) F61 0.022(3) 0.132(10) 0.077(5) 0.018(5) 0.006(3) -0.012(4) F62 0.080(5) 0.054(3) 0.047(4) -0.006(3) -0.022(3) -0.014(3) F61A 0.066(9) 0.104(12) 0.117(9) 0.026(8) 0.050(8) 0.038(8) F62A 0.075(11) 0.113(11) 0.095(15) 0.016(9) -0.025(11) -0.054(10) F63 0.040(2) 0.072(3) 0.073(3) 0.018(2) -0.0150(18) 0.0053(18) F71 0.0387(19) 0.073(3) 0.062(2) 0.0176(19) 0.0257(17) -0.0005(17) F72 0.078(3) 0.052(2) 0.0404(18) -0.0044(16) 0.0035(18) -0.0340(19) F73 0.061(2) 0.051(2) 0.0331(16) 0.0113(15) 0.0065(15) -0.0093(17) F81 0.111(4) 0.101(4) 0.053(2) -0.022(2) -0.016(2) 0.080(3) F82 0.045(2) 0.141(5) 0.074(3) -0.028(3) 0.034(2) -0.001(3) F83 0.097(3) 0.077(3) 0.0405(19) -0.0248(19) 0.003(2) 0.046(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 Ir1 C100 1.915(4) . ? Ir1 P1 2.2733(11) . ? Ir1 P3 2.2967(12) . ? Ir1 Cl1 2.4001(10) . ? Ir1 Cl2 2.4725(10) . ? Ir1 Ir2 2.7586(3) . ? Ir2 C200 1.912(4) . ? Ir2 P2 2.2809(11) . ? Ir2 P4 2.2902(11) . ? Ir2 Cl3 2.4019(10) . ? Ir2 Cl4 2.4833(10) . ? P1 O2 1.596(3) . ? P1 O1 1.603(3) . ? P1 N1 1.670(4) . ? P2 O3 1.593(3) . ? P2 O4 1.606(3) . ? P2 N1 1.662(4) . ? P3 O6 1.594(4) . ? P3 O5 1.606(4) . ? P3 N2 1.691(4) . ? P4 O8 1.597(3) . ? P4 O7 1.599(3) . ? P4 N2 1.677(4) . ? N1 C1 1.489(6) . ? N2 C2 1.488(6) . ? N3 C100 1.160(5) . ? N3 C101 1.468(6) . ? N4 C200 1.160(5) . ? N4 C201 1.469(5) . ? O1 C11 1.426(5) . ? O2 C21 1.429(6) . ? O3 C31 1.436(5) . ? O4 C41 1.426(6) . ? O5 C51 1.415(6) . ? O6 C61 1.423(6) . ? O7 C71 1.431(5) . ? O8 C81 1.431(5) . ? C11 C12 1.491(7) . ? C12 F12 1.339(6) . ? C12 F13 1.341(6) . ? C12 F11 1.347(6) . ? C21 C22 1.484(7) . ? C22 F22 1.317(7) . ? C22 F23 1.319(7) . ? C22 F21 1.354(8) . ? C31 C32 1.496(7) . ? C32 F33 1.330(7) . ? C32 F32 1.334(7) . ? C32 F31 1.338(7) . ? C41 C42 1.481(7) . ? C42 F42 1.305(7) . ? C42 F43 1.327(6) . ? C42 F41 1.351(7) . ? C51 C52 1.498(7) . ? C52 F51 1.317(7) . ? C52 F52 1.331(6) . ? C52 F53 1.348(6) . ? C61 C62 1.457(8) . ? C62 F62A 1.249(11) . ? C62 F61 1.269(8) . ? C62 F63 1.306(6) . ? C62 F62 1.434(8) . ? C62 F61A 1.489(11) . ? C71 C72 1.498(7) . ? C72 F72 1.324(6) . ? C72 F71 1.340(6) . ? C72 F73 1.347(6) . ? C81 C82 1.498(7) . ? C82 F82 1.309(9) . ? C82 F81 1.335(7) . ? C82 F83 1.343(7) . ? C101 C103 1.486(8) . ? C101 C102 1.493(9) . ? C101 C104 1.507(8) . ? C201 C202 1.519(7) . ? C201 C203 1.523(7) . ? C201 C204 1.537(7) . ? 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 C100 Ir1 P1 90.72(13) . . ? C100 Ir1 P3 90.64(13) . . ? P1 Ir1 P3 177.54(4) . . ? C100 Ir1 Cl1 175.47(13) . . ? P1 Ir1 Cl1 92.47(4) . . ? P3 Ir1 Cl1 86.29(4) . . ? C100 Ir1 Cl2 88.67(12) . . ? P1 Ir1 Cl2 90.64(4) . . ? P3 Ir1 Cl2 91.44(4) . . ? Cl1 Ir1 Cl2 88.09(4) . . ? C100 Ir1 Ir2 92.71(12) . . ? P1 Ir1 Ir2 89.65(3) . . ? P3 Ir1 Ir2 88.25(3) . . ? Cl1 Ir1 Ir2 90.53(3) . . ? Cl2 Ir1 Ir2 178.59(3) . . ? C200 Ir2 P2 92.44(12) . . ? C200 Ir2 P4 89.34(12) . . ? P2 Ir2 P4 178.19(4) . . ? C200 Ir2 Cl3 175.73(12) . . ? P2 Ir2 Cl3 90.33(4) . . ? P4 Ir2 Cl3 87.87(4) . . ? C200 Ir2 Cl4 86.48(12) . . ? P2 Ir2 Cl4 90.47(4) . . ? P4 Ir2 Cl4 89.32(4) . . ? Cl3 Ir2 Cl4 90.26(3) . . ? C200 Ir2 Ir1 92.25(12) . . ? P2 Ir2 Ir1 88.82(3) . . ? P4 Ir2 Ir1 91.44(3) . . ? Cl3 Ir2 Ir1 91.04(2) . . ? Cl4 Ir2 Ir1 178.52(3) . . ? O2 P1 O1 97.51(17) . . ? O2 P1 N1 102.67(19) . . ? O1 P1 N1 99.72(19) . . ? O2 P1 Ir1 120.14(14) . . ? O1 P1 Ir1 118.29(13) . . ? N1 P1 Ir1 115.04(14) . . ? O3 P2 O4 96.81(17) . . ? O3 P2 N1 101.07(18) . . ? O4 P2 N1 103.23(19) . . ? O3 P2 Ir2 118.51(13) . . ? O4 P2 Ir2 117.76(12) . . ? N1 P2 Ir2 116.24(14) . . ? O6 P3 O5 96.1(2) . . ? O6 P3 N2 102.57(19) . . ? O5 P3 N2 107.31(19) . . ? O6 P3 Ir1 119.56(14) . . ? O5 P3 Ir1 114.25(14) . . ? N2 P3 Ir1 114.81(14) . . ? O8 P4 O7 100.85(18) . . ? O8 P4 N2 99.36(19) . . ? O7 P4 N2 100.50(19) . . ? O8 P4 Ir2 116.87(13) . . ? O7 P4 Ir2 119.83(13) . . ? N2 P4 Ir2 116.06(14) . . ? C1 N1 P2 120.2(3) . . ? C1 N1 P1 120.1(3) . . ? P2 N1 P1 119.7(2) . . ? C2 N2 P4 118.5(3) . . ? C2 N2 P3 122.9(3) . . ? P4 N2 P3 118.2(2) . . ? C100 N3 C101 172.2(4) . . ? C200 N4 C201 174.4(4) . . ? C11 O1 P1 120.3(3) . . ? C21 O2 P1 130.2(3) . . ? C31 O3 P2 120.3(3) . . ? C41 O4 P2 122.7(3) . . ? C51 O5 P3 126.6(3) . . ? C61 O6 P3 126.0(3) . . ? C71 O7 P4 131.7(3) . . ? C81 O8 P4 122.0(3) . . ? O1 C11 C12 107.5(4) . . ? F12 C12 F13 107.4(4) . . ? F12 C12 F11 106.5(5) . . ? F13 C12 F11 107.2(4) . . ? F12 C12 C11 113.1(4) . . ? F13 C12 C11 110.1(5) . . ? F11 C12 C11 112.3(4) . . ? O2 C21 C22 108.3(4) . . ? F22 C22 F23 109.1(5) . . ? F22 C22 F21 106.1(5) . . ? F23 C22 F21 105.8(5) . . ? F22 C22 C21 110.4(5) . . ? F23 C22 C21 113.9(5) . . ? F21 C22 C21 111.2(5) . . ? O3 C31 C32 107.7(4) . . ? F33 C32 F32 106.8(5) . . ? F33 C32 F31 108.4(5) . . ? F32 C32 F31 106.7(5) . . ? F33 C32 C31 113.3(4) . . ? F32 C32 C31 111.7(5) . . ? F31 C32 C31 109.6(5) . . ? O4 C41 C42 108.0(4) . . ? F42 C42 F43 109.3(5) . . ? F42 C42 F41 105.2(5) . . ? F43 C42 F41 106.1(5) . . ? F42 C42 C41 114.5(5) . . ? F43 C42 C41 110.6(5) . . ? F41 C42 C41 110.7(5) . . ? O5 C51 C52 110.2(4) . . ? F51 C52 F52 109.9(5) . . ? F51 C52 F53 106.2(5) . . ? F52 C52 F53 106.9(4) . . ? F51 C52 C51 113.6(5) . . ? F52 C52 C51 109.7(5) . . ? F53 C52 C51 110.4(5) . . ? O6 C61 C62 108.8(4) . . ? F62A C62 F61 44.0(9) . . ? F62A C62 F63 118.7(9) . . ? F61 C62 F63 114.8(7) . . ? F62A C62 F62 56.7(10) . . ? F61 C62 F62 100.7(7) . . ? F63 C62 F62 102.8(5) . . ? F62A C62 C61 126.7(10) . . ? F61 C62 C61 118.7(6) . . ? F63 C62 C61 113.6(5) . . ? F62 C62 C61 102.9(5) . . ? F62A C62 F61A 96.6(11) . . ? F61 C62 F61A 52.7(7) . . ? F63 C62 F61A 89.7(7) . . ? F62 C62 F61A 153.3(8) . . ? C61 C62 F61A 93.1(7) . . ? O7 C71 C72 105.9(4) . . ? F72 C72 F71 106.7(5) . . ? F72 C72 F73 106.9(4) . . ? F71 C72 F73 107.2(4) . . ? F72 C72 C71 114.5(4) . . ? F71 C72 C71 112.5(4) . . ? F73 C72 C71 108.6(4) . . ? O8 C81 C82 107.8(4) . . ? F82 C82 F81 108.4(6) . . ? F82 C82 F83 108.3(5) . . ? F81 C82 F83 106.8(5) . . ? F82 C82 C81 112.1(5) . . ? F81 C82 C81 111.9(5) . . ? F83 C82 C81 109.1(5) . . ? N3 C100 Ir1 173.0(4) . . ? N3 C101 C103 108.5(5) . . ? N3 C101 C102 106.2(5) . . ? C103 C101 C102 111.9(7) . . ? N3 C101 C104 107.0(4) . . ? C103 C101 C104 112.0(6) . . ? C102 C101 C104 110.9(6) . . ? N4 C200 Ir2 171.9(4) . . ? N4 C201 C202 107.6(4) . . ? N4 C201 C203 107.3(4) . . ? C202 C201 C203 112.0(4) . . ? N4 C201 C204 107.3(4) . . ? C202 C201 C204 110.7(4) . . ? C203 C201 C204 111.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.457 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.156