Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Thomas Braun' _publ_contact_author_address ;Humboldt Universit\"at zu Berlin Department of Chemistry Brook-Taylor-Str. 2 12489 Berlin, germany ; _publ_contact_author_email thomas.braun@chemie.hu-berlin.de loop_ _publ_author_name _publ_author_address 'Thomas Braun' ;Humboldt Universit\"at zu Berlin Department of Chemistry Brook-Taylor-Str. 2 12489 Berlin, Germany ; P.Klaring ;Humboldt Universit\"at zu Berlin Department of Chemistry Brook-Taylor-Str. 2 12489 Berlin, Germany ; 'Anna Penner' ;Humboldt Universit\"at zu Berlin Department of Chemistry Brook-Taylor-Str. 2 12489 Berlin, Germany ; 'Stefanie Pahl' ;Universit\"at Bielefeld Department of Chemistry Postfach 100131 33501 Bielefeld, Germany ; data_c:\anna\paul1_compound2 _database_code_depnum_ccdc_archive 'CCDC 810896' #TrackingRef '- Braun_Klring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H43 F4 Ir N O P2' _chemical_formula_weight 679.72 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4183(3) _cell_length_b 17.6380(3) _cell_length_c 12.9846(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.300(2) _cell_angle_gamma 90.00 _cell_volume 2715.40(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27.50 _exptl_crystal_description lattice _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method none _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 5.078 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3465 _exptl_absorpt_correction_T_max 0.6335 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device_type 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,360 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6197 _diffrn_reflns_av_R_equivalents 0.1213 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6197 _reflns_number_gt 5311 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. ; _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^)+(0.0444P)^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 SHELXL _refine_ls_extinction_coef 0.00086(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6197 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9380(3) 0.19448(18) 0.1659(3) 0.0143(6) Uani 1 1 d . . . C2 C 0.9920(3) 0.2612(2) 0.2145(3) 0.0238(8) Uani 1 1 d . . . C3 C 1.0195(3) 0.3194(2) 0.1574(4) 0.0322(10) Uani 1 1 d . . . C4 C 0.9492(3) 0.2588(3) 0.0035(3) 0.0326(10) Uani 1 1 d . . . C5 C 0.9159(3) 0.1980(2) 0.0544(3) 0.0219(7) Uani 1 1 d . . . C6 C 0.6430(3) 0.16073(19) 0.0972(3) 0.0164(6) Uani 1 1 d . . . H6 H 0.6908 0.1969 0.0706 0.020 Uiso 1 1 calc R . . C7 C 0.6269(3) 0.0913(2) 0.0237(3) 0.0230(7) Uani 1 1 d . . . H7A H 0.5676 0.0590 0.0356 0.035 Uiso 1 1 calc R . . H7B H 0.6977 0.0627 0.0401 0.035 Uiso 1 1 calc R . . H7C H 0.6051 0.1078 -0.0518 0.035 Uiso 1 1 calc R . . C8 C 0.5291(3) 0.2007(2) 0.0808(3) 0.0250(8) Uani 1 1 d . . . H8A H 0.4962 0.2132 0.0043 0.037 Uiso 1 1 calc R . . H8B H 0.5406 0.2473 0.1237 0.037 Uiso 1 1 calc R . . H8C H 0.4779 0.1670 0.1038 0.037 Uiso 1 1 calc R . . C9 C 0.6945(3) 0.21854(18) 0.3173(3) 0.0140(6) Uani 1 1 d . . . H9 H 0.6108 0.2246 0.2987 0.017 Uiso 1 1 calc R . . C10 C 0.7437(3) 0.29218(18) 0.2878(3) 0.0192(6) Uani 1 1 d . . . H10A H 0.7211 0.3348 0.3251 0.029 Uiso 1 1 calc R . . H10B H 0.7153 0.3002 0.2097 0.029 Uiso 1 1 calc R . . H10C H 0.8262 0.2886 0.3097 0.029 Uiso 1 1 calc R . . C11 C 0.7410(3) 0.2044(2) 0.4390(3) 0.0218(7) Uani 1 1 d . . . H11A H 0.8213 0.1918 0.4575 0.033 Uiso 1 1 calc R . . H11B H 0.7001 0.1622 0.4593 0.033 Uiso 1 1 calc R . . H11C H 0.7313 0.2502 0.4781 0.033 Uiso 1 1 calc R . . C12 C 0.6605(3) 0.05726(18) 0.2899(3) 0.0155(6) Uani 1 1 d . . . H12 H 0.7020 0.0542 0.3686 0.019 Uiso 1 1 calc R . . C13 C 0.5373(3) 0.0662(2) 0.2840(3) 0.0242(8) Uani 1 1 d . . . H13A H 0.4907 0.0649 0.2085 0.036 Uiso 1 1 calc R . . H13B H 0.5265 0.1147 0.3163 0.036 Uiso 1 1 calc R . . H13C H 0.5150 0.0246 0.3235 0.036 Uiso 1 1 calc R . . C14 C 0.6799(3) -0.01984(19) 0.2431(3) 0.0226(7) Uani 1 1 d . . . H14A H 0.6625 -0.0607 0.2868 0.034 Uiso 1 1 calc R . . H14B H 0.7588 -0.0238 0.2439 0.034 Uiso 1 1 calc R . . H14C H 0.6307 -0.0242 0.1687 0.034 Uiso 1 1 calc R . . C15 C 1.1582(3) 0.0868(2) 0.1755(3) 0.0168(6) Uani 1 1 d . . . H15 H 1.0960 0.1007 0.1093 0.020 Uiso 1 1 calc R . . C16 C 1.2251(3) 0.1600(2) 0.2118(3) 0.0197(7) Uani 1 1 d . . . H16A H 1.2992 0.1476 0.2618 0.030 Uiso 1 1 calc R . . H16B H 1.1841 0.1928 0.2480 0.030 Uiso 1 1 calc R . . H16C H 1.2350 0.1863 0.1487 0.030 Uiso 1 1 calc R . . C17 C 1.2306(3) 0.0304(2) 0.1383(3) 0.0207(7) Uani 1 1 d . . . H17A H 1.2642 0.0551 0.0876 0.031 Uiso 1 1 calc R . . H17B H 1.1839 -0.0124 0.1025 0.031 Uiso 1 1 calc R . . H17C H 1.2907 0.0119 0.2008 0.031 Uiso 1 1 calc R . . C18 C 1.0652(3) -0.04970(19) 0.2415(3) 0.0154(6) Uani 1 1 d . . . H18 H 1.1382 -0.0710 0.2367 0.018 Uiso 1 1 calc R . . C19 C 0.9762(3) -0.0610(2) 0.1313(3) 0.0211(7) Uani 1 1 d . . . H19A H 0.9713 -0.1150 0.1124 0.032 Uiso 1 1 calc R . . H19B H 0.9980 -0.0320 0.0763 0.032 Uiso 1 1 calc R . . H19C H 0.9027 -0.0433 0.1352 0.032 Uiso 1 1 calc R . . C20 C 1.0297(3) -0.0952(2) 0.3258(3) 0.0226(7) Uani 1 1 d . . . H20A H 0.9601 -0.0738 0.3344 0.034 Uiso 1 1 calc R . . H20B H 1.0895 -0.0929 0.3948 0.034 Uiso 1 1 calc R . . H20C H 1.0168 -0.1481 0.3023 0.034 Uiso 1 1 calc R . . C21 C 1.1866(3) 0.0532(2) 0.4121(3) 0.0150(6) Uani 1 1 d . . . H21 H 1.1525 0.0193 0.4556 0.018 Uiso 1 1 calc R . . C22 C 1.3032(3) 0.0198(2) 0.4223(3) 0.0222(7) Uani 1 1 d . . . H22A H 1.3434 0.0529 0.3854 0.033 Uiso 1 1 calc R . . H22B H 1.2945 -0.0307 0.3893 0.033 Uiso 1 1 calc R . . H22C H 1.3463 0.0158 0.4987 0.033 Uiso 1 1 calc R . . C23 C 1.1960(3) 0.1313(2) 0.4656(3) 0.0218(7) Uani 1 1 d . . . H23A H 1.2394 0.1270 0.5419 0.033 Uiso 1 1 calc R . . H23B H 1.1203 0.1506 0.4596 0.033 Uiso 1 1 calc R . . H23C H 1.2343 0.1664 0.4296 0.033 Uiso 1 1 calc R . . F1 F 1.02325(19) 0.26808(13) 0.3232(2) 0.0294(5) Uani 1 1 d . . . F2 F 1.0727(3) 0.38089(14) 0.2109(3) 0.0514(8) Uani 1 1 d . . . F3 F 0.9294(3) 0.25598(19) -0.1037(2) 0.0485(8) Uani 1 1 d . . . F4 F 0.8636(2) 0.13949(14) -0.00841(17) 0.0280(5) Uani 1 1 d . . . Ir1 Ir 0.913621(9) 0.110018(6) 0.261473(8) 0.00931(5) Uani 1 1 d . . . N1 N 0.9994(3) 0.3195(2) 0.0524(4) 0.0382(10) Uani 1 1 d . . . O1 O 0.9132(2) 0.06279(15) 0.40350(19) 0.0195(5) Uani 1 1 d . . . H1 H 0.9781 0.0469 0.4361 0.029 Uiso 1 1 calc R . . P1 P 0.72421(6) 0.13808(5) 0.23885(6) 0.01080(15) Uani 1 1 d . . . P2 P 1.08693(6) 0.05254(4) 0.27400(6) 0.01052(15) 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 C1 0.0119(14) 0.0122(14) 0.0216(16) 0.0026(12) 0.0090(12) 0.0048(11) C2 0.0193(17) 0.0132(16) 0.044(2) 0.0015(15) 0.0175(16) -0.0019(13) C3 0.0262(19) 0.0126(16) 0.068(3) 0.0081(17) 0.030(2) 0.0031(14) C4 0.029(2) 0.042(2) 0.036(2) 0.0262(19) 0.0240(17) 0.0230(18) C5 0.0201(17) 0.0225(17) 0.0261(18) 0.0078(14) 0.0117(14) 0.0103(14) C6 0.0149(15) 0.0163(15) 0.0162(14) -0.0011(12) 0.0017(11) 0.0038(12) C7 0.0209(17) 0.0238(18) 0.0191(16) -0.0070(13) -0.0020(13) 0.0031(14) C8 0.0188(17) 0.0289(19) 0.0219(17) -0.0004(15) -0.0021(13) 0.0102(15) C9 0.0136(14) 0.0116(14) 0.0179(15) -0.0028(11) 0.0064(12) 0.0004(11) C10 0.0216(16) 0.0121(14) 0.0251(16) -0.0020(13) 0.0086(13) -0.0010(13) C11 0.0259(18) 0.0223(17) 0.0172(16) -0.0040(13) 0.0063(13) -0.0024(14) C12 0.0103(14) 0.0122(14) 0.0238(16) 0.0020(12) 0.0048(12) -0.0012(11) C13 0.0139(16) 0.0174(17) 0.043(2) 0.0018(15) 0.0112(15) -0.0006(13) C14 0.0180(16) 0.0127(15) 0.038(2) -0.0016(14) 0.0092(15) -0.0007(12) C15 0.0178(15) 0.0202(16) 0.0139(14) 0.0007(12) 0.0067(12) -0.0040(13) C16 0.0186(16) 0.0182(16) 0.0241(16) 0.0025(13) 0.0090(13) -0.0051(13) C17 0.0154(15) 0.0268(18) 0.0221(16) -0.0014(14) 0.0088(13) 0.0004(13) C18 0.0142(15) 0.0142(15) 0.0170(15) -0.0005(12) 0.0035(12) -0.0001(12) C19 0.0220(17) 0.0205(16) 0.0202(16) -0.0042(13) 0.0053(13) -0.0032(13) C20 0.0267(18) 0.0158(16) 0.0250(17) 0.0045(13) 0.0070(14) -0.0033(13) C21 0.0099(14) 0.0216(16) 0.0135(14) 0.0002(12) 0.0037(11) 0.0014(12) C22 0.0152(16) 0.034(2) 0.0178(16) 0.0055(14) 0.0046(12) 0.0075(14) C23 0.0169(16) 0.0277(18) 0.0182(16) -0.0078(14) 0.0010(13) -0.0011(13) F1 0.0263(12) 0.0222(11) 0.0409(13) -0.0148(10) 0.0121(10) -0.0104(9) F2 0.0458(17) 0.0158(12) 0.104(3) -0.0032(14) 0.0398(17) -0.0110(11) F3 0.0492(17) 0.068(2) 0.0378(14) 0.0371(14) 0.0275(13) 0.0296(15) F4 0.0296(12) 0.0385(13) 0.0151(10) 0.0007(9) 0.0056(8) 0.0083(10) Ir1 0.00796(7) 0.00972(7) 0.00999(7) 0.00050(4) 0.00229(4) -0.00114(4) N1 0.0325(19) 0.0218(17) 0.073(3) 0.0268(18) 0.0346(19) 0.0135(15) O1 0.0111(11) 0.0305(14) 0.0164(11) 0.0079(10) 0.0031(9) 0.0029(10) P1 0.0086(3) 0.0097(3) 0.0136(3) -0.0002(3) 0.0025(3) -0.0004(3) P2 0.0092(3) 0.0120(3) 0.0107(3) -0.0004(3) 0.0034(3) -0.0009(3) _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 C1 C5 1.393(5) . ? C1 C2 1.408(5) . ? C1 Ir1 2.019(3) . ? C2 F1 1.353(5) . ? C2 C3 1.367(5) . ? C3 N1 1.311(6) . ? C3 F2 1.349(5) . ? C4 N1 1.305(7) . ? C4 F3 1.341(5) . ? C4 C5 1.385(5) . ? C5 F4 1.355(5) . ? C6 C7 1.529(5) . ? C6 C8 1.538(5) . ? C6 P1 1.859(3) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.532(4) . ? C9 C11 1.533(5) . ? C9 P1 1.847(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.517(4) . ? C12 C14 1.538(5) . ? C12 P1 1.847(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.513(5) . ? C15 C16 1.531(5) . ? C15 P2 1.860(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.524(5) . ? C18 C19 1.538(5) . ? C18 P2 1.853(3) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.532(4) . ? C21 C23 1.532(5) . ? C21 P2 1.851(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Ir1 O1 2.025(2) . ? Ir1 P1 2.3351(8) . ? Ir1 P2 2.3406(8) . ? O1 H1 0.8400 . ? 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 C5 C1 C2 110.4(3) . . ? C5 C1 Ir1 130.8(3) . . ? C2 C1 Ir1 118.7(3) . . ? F1 C2 C3 117.3(4) . . ? F1 C2 C1 119.5(3) . . ? C3 C2 C1 123.2(4) . . ? N1 C3 F2 116.6(4) . . ? N1 C3 C2 124.3(4) . . ? F2 C3 C2 119.1(4) . . ? N1 C4 F3 116.7(4) . . ? N1 C4 C5 124.8(4) . . ? F3 C4 C5 118.5(4) . . ? F4 C5 C4 117.4(4) . . ? F4 C5 C1 120.2(3) . . ? C4 C5 C1 122.4(4) . . ? C7 C6 C8 109.6(3) . . ? C7 C6 P1 112.2(2) . . ? C8 C6 P1 116.2(2) . . ? C7 C6 H6 106.0 . . ? C8 C6 H6 106.0 . . ? P1 C6 H6 106.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 109.8(3) . . ? C10 C9 P1 110.7(2) . . ? C11 C9 P1 111.6(2) . . ? C10 C9 H9 108.2 . . ? C11 C9 H9 108.2 . . ? P1 C9 H9 108.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 110.3(3) . . ? C13 C12 P1 115.8(2) . . ? C14 C12 P1 114.0(2) . . ? C13 C12 H12 105.2 . . ? C14 C12 H12 105.2 . . ? P1 C12 H12 105.2 . . ? 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 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.4(3) . . ? C17 C15 P2 117.1(2) . . ? C16 C15 P2 112.8(2) . . ? C17 C15 H15 105.5 . . ? C16 C15 H15 105.5 . . ? P2 C15 H15 105.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 108.6(3) . . ? C20 C18 P2 113.7(2) . . ? C19 C18 P2 110.7(2) . . ? C20 C18 H18 107.9 . . ? C19 C18 H18 107.9 . . ? P2 C18 H18 107.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 111.4(3) . . ? C22 C21 P2 115.1(2) . . ? C23 C21 P2 112.6(2) . . ? C22 C21 H21 105.6 . . ? C23 C21 H21 105.6 . . ? P2 C21 H21 105.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 Ir1 O1 154.82(12) . . ? C1 Ir1 P1 95.52(9) . . ? O1 Ir1 P1 85.77(7) . . ? C1 Ir1 P2 93.40(9) . . ? O1 Ir1 P2 90.57(7) . . ? P1 Ir1 P2 166.30(3) . . ? C4 N1 C3 114.9(3) . . ? Ir1 O1 H1 109.5 . . ? C12 P1 C9 102.57(15) . . ? C12 P1 C6 110.90(15) . . ? C9 P1 C6 104.00(15) . . ? C12 P1 Ir1 108.33(11) . . ? C9 P1 Ir1 116.92(11) . . ? C6 P1 Ir1 113.56(11) . . ? C21 P2 C18 103.71(15) . . ? C21 P2 C15 110.25(15) . . ? C18 P2 C15 103.09(15) . . ? C21 P2 Ir1 113.64(11) . . ? C18 P2 Ir1 109.69(11) . . ? C15 P2 Ir1 115.28(11) . . ? 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 C5 C1 C2 F1 -178.4(3) . . . . ? Ir1 C1 C2 F1 -1.8(4) . . . . ? C5 C1 C2 C3 -1.2(5) . . . . ? Ir1 C1 C2 C3 175.3(3) . . . . ? F1 C2 C3 N1 176.9(3) . . . . ? C1 C2 C3 N1 -0.3(6) . . . . ? F1 C2 C3 F2 -1.8(5) . . . . ? C1 C2 C3 F2 -179.0(3) . . . . ? N1 C4 C5 F4 179.4(3) . . . . ? F3 C4 C5 F4 -0.9(5) . . . . ? N1 C4 C5 C1 -3.0(6) . . . . ? F3 C4 C5 C1 176.8(3) . . . . ? C2 C1 C5 F4 -179.7(3) . . . . ? Ir1 C1 C5 F4 4.3(5) . . . . ? C2 C1 C5 C4 2.7(5) . . . . ? Ir1 C1 C5 C4 -173.3(3) . . . . ? C5 C1 Ir1 O1 -175.5(2) . . . . ? C2 C1 Ir1 O1 8.8(4) . . . . ? C5 C1 Ir1 P1 -83.7(3) . . . . ? C2 C1 Ir1 P1 100.6(3) . . . . ? C5 C1 Ir1 P2 85.9(3) . . . . ? C2 C1 Ir1 P2 -89.8(3) . . . . ? F3 C4 N1 C3 -178.6(3) . . . . ? C5 C4 N1 C3 1.2(6) . . . . ? F2 C3 N1 C4 179.2(3) . . . . ? C2 C3 N1 C4 0.4(6) . . . . ? C13 C12 P1 C9 54.5(3) . . . . ? C14 C12 P1 C9 -176.1(2) . . . . ? C13 C12 P1 C6 -56.1(3) . . . . ? C14 C12 P1 C6 73.4(3) . . . . ? C13 C12 P1 Ir1 178.7(2) . . . . ? C14 C12 P1 Ir1 -51.8(3) . . . . ? C10 C9 P1 C12 178.8(2) . . . . ? C11 C9 P1 C12 56.2(3) . . . . ? C10 C9 P1 C6 -65.6(3) . . . . ? C11 C9 P1 C6 171.8(2) . . . . ? C10 C9 P1 Ir1 60.5(3) . . . . ? C11 C9 P1 Ir1 -62.1(3) . . . . ? C7 C6 P1 C12 -53.1(3) . . . . ? C8 C6 P1 C12 74.1(3) . . . . ? C7 C6 P1 C9 -162.7(3) . . . . ? C8 C6 P1 C9 -35.4(3) . . . . ? C7 C6 P1 Ir1 69.1(3) . . . . ? C8 C6 P1 Ir1 -163.6(2) . . . . ? C1 Ir1 P1 C12 166.54(15) . . . . ? O1 Ir1 P1 C12 -38.70(14) . . . . ? P2 Ir1 P1 C12 36.18(17) . . . . ? C1 Ir1 P1 C9 -78.29(15) . . . . ? O1 Ir1 P1 C9 76.47(14) . . . . ? P2 Ir1 P1 C9 151.34(15) . . . . ? C1 Ir1 P1 C6 42.86(15) . . . . ? O1 Ir1 P1 C6 -162.37(14) . . . . ? P2 Ir1 P1 C6 -87.50(16) . . . . ? C22 C21 P2 C18 64.0(3) . . . . ? C23 C21 P2 C18 -166.9(2) . . . . ? C22 C21 P2 C15 -45.8(3) . . . . ? C23 C21 P2 C15 83.3(3) . . . . ? C22 C21 P2 Ir1 -176.9(2) . . . . ? C23 C21 P2 Ir1 -47.8(3) . . . . ? C20 C18 P2 C21 53.0(3) . . . . ? C19 C18 P2 C21 175.6(2) . . . . ? C20 C18 P2 C15 168.0(2) . . . . ? C19 C18 P2 C15 -69.4(3) . . . . ? C20 C18 P2 Ir1 -68.7(3) . . . . ? C19 C18 P2 Ir1 53.9(2) . . . . ? C17 C15 P2 C21 80.7(3) . . . . ? C16 C15 P2 C21 -47.6(3) . . . . ? C17 C15 P2 C18 -29.4(3) . . . . ? C16 C15 P2 C18 -157.8(2) . . . . ? C17 C15 P2 Ir1 -148.9(2) . . . . ? C16 C15 P2 Ir1 82.7(3) . . . . ? C1 Ir1 P2 C21 115.06(16) . . . . ? O1 Ir1 P2 C21 -40.06(14) . . . . ? P1 Ir1 P2 C21 -114.38(16) . . . . ? C1 Ir1 P2 C18 -129.38(14) . . . . ? O1 Ir1 P2 C18 75.49(13) . . . . ? P1 Ir1 P2 C18 1.18(17) . . . . ? C1 Ir1 P2 C15 -13.59(15) . . . . ? O1 Ir1 P2 C15 -168.72(14) . . . . ? P1 Ir1 P2 C15 116.97(16) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.679 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.134 data_d:\x-data\paul5_compound4 _database_code_depnum_ccdc_archive 'CCDC 810897' #TrackingRef '- Braun_Klring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 F4 Ir N O P2' _chemical_formula_weight 690.73 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6289(2) _cell_length_b 16.0526(2) _cell_length_c 36.1516(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.0450(10) _cell_angle_gamma 90.00 _cell_volume 5584.35(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 4.940 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3188 _exptl_absorpt_correction_T_max 0.8269 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _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 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,360 exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10913 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10913 _reflns_number_gt 7878 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. ; _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^)+(0.0469P)^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 SHELXL _refine_ls_extinction_coef 0.00085(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10913 _refine_ls_number_parameters 620 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.867 _refine_ls_shift/su_max 0.011 _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 C1 C 0.6870(6) 0.1678(4) 1.24861(16) 0.0336(12) Uani 1 1 d . . . H1 H 0.6196 0.2037 1.2617 0.040 Uiso 1 1 calc R . . C2 C 0.6043(7) 0.0936(4) 1.23372(19) 0.0440(15) Uani 1 1 d . . . H2A H 0.5480 0.0707 1.2534 0.053 Uiso 1 1 calc R . . H2B H 0.6683 0.0507 1.2253 0.053 Uiso 1 1 calc R . . H2C H 0.5432 0.1115 1.2130 0.053 Uiso 1 1 calc R . . C3 C 0.7943(7) 0.1386(5) 1.27811(18) 0.0482(17) Uani 1 1 d . . . H3C H 0.8469 0.1867 1.2877 0.058 Uiso 1 1 calc R . . H3B H 0.8582 0.0989 1.2671 0.058 Uiso 1 1 calc R . . H3A H 0.7466 0.1115 1.2984 0.058 Uiso 1 1 calc R . . C4 C 0.8882(6) 0.2970(4) 1.23408(19) 0.0432(14) Uani 1 1 d . . . H4 H 0.9555 0.2583 1.2469 0.052 Uiso 1 1 calc R . . C5 C 0.8267(7) 0.3522(4) 1.26371(19) 0.0477(16) Uani 1 1 d . . . H5A H 0.7687 0.3954 1.2518 0.057 Uiso 1 1 calc R . . H5B H 0.9020 0.3785 1.2785 0.057 Uiso 1 1 calc R . . H5C H 0.7699 0.3182 1.2799 0.057 Uiso 1 1 calc R . . C6 C 0.9694(9) 0.3495(6) 1.2076(2) 0.074(3) Uani 1 1 d . . . H6A H 1.0134 0.3132 1.1896 0.089 Uiso 1 1 calc R . . H6B H 1.0410 0.3811 1.2215 0.089 Uiso 1 1 calc R . . H6C H 0.9062 0.3882 1.1945 0.089 Uiso 1 1 calc R . . C7 C 0.8573(6) 0.1663(4) 1.18011(17) 0.0370(13) Uani 1 1 d . . . H7 H 0.9072 0.2059 1.1639 0.044 Uiso 1 1 calc R . . C8 C 0.9710(8) 0.1135(5) 1.1989(2) 0.060(2) Uani 1 1 d . . . H8A H 1.0353 0.0940 1.1804 0.072 Uiso 1 1 calc R . . H8B H 0.9290 0.0655 1.2110 0.072 Uiso 1 1 calc R . . H8C H 1.0218 0.1472 1.2175 0.072 Uiso 1 1 calc R . . C9 C 0.7687(7) 0.1113(4) 1.15335(18) 0.0448(15) Uani 1 1 d . . . H9A H 0.6888 0.1433 1.1436 0.054 Uiso 1 1 calc R . . H9B H 0.7357 0.0623 1.1666 0.054 Uiso 1 1 calc R . . H9C H 0.8253 0.0933 1.1328 0.054 Uiso 1 1 calc R . . C10 C 0.5184(9) 0.4545(5) 1.1068(2) 0.059(2) Uani 1 1 d . . . H10A H 0.5794 0.4194 1.0913 0.070 Uiso 1 1 calc R . . C11 C 0.6191(9) 0.5128(5) 1.1290(3) 0.071(2) Uani 1 1 d . . . H11A H 0.5655 0.5542 1.1423 0.086 Uiso 1 1 calc R . . H11B H 0.6802 0.5412 1.1119 0.086 Uiso 1 1 calc R . . H11C H 0.6754 0.4798 1.1467 0.086 Uiso 1 1 calc R . . C12 C 0.4294(10) 0.5044(6) 1.0794(2) 0.078(3) Uani 1 1 d . . . H12A H 0.3650 0.4669 1.0660 0.094 Uiso 1 1 calc R . . H12B H 0.4891 0.5322 1.0618 0.094 Uiso 1 1 calc R . . H12C H 0.3764 0.5462 1.0927 0.094 Uiso 1 1 calc R . . C13 C 0.3368(8) 0.3087(4) 1.10374(17) 0.0544(19) Uani 1 1 d . . . H13 H 0.2730 0.3432 1.0876 0.065 Uiso 1 1 calc R . . C14 C 0.4341(11) 0.2631(6) 1.0789(2) 0.088(3) Uani 1 1 d . . . H14A H 0.3800 0.2284 1.0614 0.105 Uiso 1 1 calc R . . H14B H 0.4968 0.2278 1.0940 0.105 Uiso 1 1 calc R . . H14C H 0.4887 0.3035 1.0653 0.105 Uiso 1 1 calc R . . C15 C 0.2476(9) 0.2461(4) 1.1243(2) 0.063(2) Uani 1 1 d . . . H15A H 0.1880 0.2760 1.1412 0.076 Uiso 1 1 calc R . . H15B H 0.3081 0.2076 1.1384 0.076 Uiso 1 1 calc R . . H15C H 0.1897 0.2147 1.1063 0.076 Uiso 1 1 calc R . . C16 C 0.2839(6) 0.4347(3) 1.15882(16) 0.0355(13) Uani 1 1 d . . . H16 H 0.2523 0.3963 1.1786 0.043 Uiso 1 1 calc R . . C17 C 0.3330(7) 0.5140(4) 1.17894(18) 0.0437(15) Uani 1 1 d . . . H17A H 0.2649 0.5300 1.1971 0.052 Uiso 1 1 calc R . . H17B H 0.3425 0.5591 1.1609 0.052 Uiso 1 1 calc R . . H17C H 0.4231 0.5037 1.1916 0.052 Uiso 1 1 calc R . . C18 C 0.1541(7) 0.4533(4) 1.13443(18) 0.0423(14) Uani 1 1 d . . . H18A H 0.1151 0.4010 1.1247 0.051 Uiso 1 1 calc R . . H18B H 0.1793 0.4892 1.1138 0.051 Uiso 1 1 calc R . . H18C H 0.0849 0.4816 1.1492 0.051 Uiso 1 1 calc R . . C19 C 0.7103(7) 0.3098(4) 1.13666(18) 0.0455(15) Uani 1 1 d . . . C20 C 0.4537(5) 0.3108(3) 1.22007(15) 0.0306(11) Uani 1 1 d . . . C21 C 0.3559(6) 0.2511(4) 1.22884(16) 0.0356(13) Uani 1 1 d . . . C22 C 0.2802(6) 0.2552(4) 1.26090(18) 0.0435(15) Uani 1 1 d . . . C23 C 0.3764(7) 0.3733(4) 1.27710(17) 0.0436(15) Uani 1 1 d . . . C24 C 0.4578(6) 0.3746(4) 1.24666(14) 0.0314(12) Uani 1 1 d . . . C25 C 0.8576(7) 0.3341(4) 1.01835(16) 0.0372(13) Uani 1 1 d . . . H25 H 0.7913 0.3009 1.0331 0.045 Uiso 1 1 calc R . . C26 C 0.7680(8) 0.3986(4) 0.99756(19) 0.0471(16) Uani 1 1 d . . . H26A H 0.8278 0.4415 0.9873 0.057 Uiso 1 1 calc R . . H26B H 0.7040 0.4245 1.0147 0.057 Uiso 1 1 calc R . . H26C H 0.7145 0.3712 0.9774 0.057 Uiso 1 1 calc R . . C27 C 0.9558(8) 0.3760(4) 1.04699(19) 0.0491(17) Uani 1 1 d . . . H27A H 1.0078 0.3332 1.0610 0.059 Uiso 1 1 calc R . . H27B H 0.9016 0.4094 1.0640 0.059 Uiso 1 1 calc R . . H27C H 1.0209 0.4121 1.0343 0.059 Uiso 1 1 calc R . . C28 C 1.0133(7) 0.1795(4) 1.01983(17) 0.0424(15) Uani 1 1 d . . . H28 H 1.0870 0.2076 1.0355 0.051 Uiso 1 1 calc R . . C29 C 0.9099(8) 0.1423(5) 1.04539(19) 0.0537(18) Uani 1 1 d . . . H29A H 0.9561 0.1002 1.0611 0.064 Uiso 1 1 calc R . . H29B H 0.8341 0.1162 1.0307 0.064 Uiso 1 1 calc R . . H29C H 0.8721 0.1862 1.0609 0.064 Uiso 1 1 calc R . . C30 C 1.0837(9) 0.1116(5) 0.9976(2) 0.061(2) Uani 1 1 d . . . H30A H 1.1519 0.1370 0.9816 0.074 Uiso 1 1 calc R . . H30B H 1.0136 0.0818 0.9824 0.074 Uiso 1 1 calc R . . H30C H 1.1308 0.0724 1.0146 0.074 Uiso 1 1 calc R . . C31 C 1.0949(6) 0.3059(5) 0.96716(17) 0.0451(15) Uani 1 1 d . . . H31 H 1.1215 0.2678 0.9467 0.054 Uiso 1 1 calc R . . C32 C 1.2264(7) 0.3148(6) 0.9926(2) 0.066(2) Uani 1 1 d . . . H32A H 1.2065 0.3515 1.0134 0.079 Uiso 1 1 calc R . . H32B H 1.3019 0.3386 0.9785 0.079 Uiso 1 1 calc R . . H32C H 1.2543 0.2598 1.0021 0.079 Uiso 1 1 calc R . . C33 C 1.0608(9) 0.3890(4) 0.9488(2) 0.060(2) Uani 1 1 d . . . H33C H 0.9715 0.3848 0.9350 0.072 Uiso 1 1 calc R . . H33B H 1.1338 0.4034 0.9317 0.072 Uiso 1 1 calc R . . H33A H 1.0549 0.4324 0.9677 0.072 Uiso 1 1 calc R . . C34 C 0.6898(6) 0.0640(3) 0.86980(16) 0.0341(12) Uani 1 1 d . . . H34A H 0.7551 0.1035 0.8580 0.041 Uiso 1 1 calc R . . C35 C 0.7788(7) -0.0099(4) 0.88276(19) 0.0443(15) Uani 1 1 d . . . H35A H 0.8374 -0.0279 0.8626 0.053 Uiso 1 1 calc R . . H35B H 0.7183 -0.0559 0.8898 0.053 Uiso 1 1 calc R . . H35C H 0.8377 0.0068 0.9041 0.053 Uiso 1 1 calc R . . C36 C 0.5862(8) 0.0368(5) 0.83878(18) 0.0531(18) Uani 1 1 d . . . H36A H 0.5366 0.0857 0.8289 0.064 Uiso 1 1 calc R . . H36B H 0.5195 -0.0027 0.8487 0.064 Uiso 1 1 calc R . . H36C H 0.6367 0.0100 0.8189 0.064 Uiso 1 1 calc R . . C37 C 0.4799(6) 0.1862(4) 0.88698(16) 0.0369(13) Uani 1 1 d . . . H37A H 0.4163 0.1479 0.8726 0.044 Uiso 1 1 calc R . . C38 C 0.5374(7) 0.2481(4) 0.8598(2) 0.0495(17) Uani 1 1 d . . . H38A H 0.5909 0.2909 0.8733 0.059 Uiso 1 1 calc R . . H38B H 0.4604 0.2743 0.8456 0.059 Uiso 1 1 calc R . . H38C H 0.5979 0.2190 0.8428 0.059 Uiso 1 1 calc R . . C39 C 0.3934(7) 0.2310(5) 0.9150(2) 0.0495(16) Uani 1 1 d . . . H39A H 0.3496 0.1901 0.9309 0.059 Uiso 1 1 calc R . . H39B H 0.3214 0.2641 0.9019 0.059 Uiso 1 1 calc R . . H39C H 0.4533 0.2679 0.9301 0.059 Uiso 1 1 calc R . . C40 C 0.5214(6) 0.0481(4) 0.93794(15) 0.0327(12) Uani 1 1 d . . . H40A H 0.4713 0.0838 0.9558 0.039 Uiso 1 1 calc R . . C41 C 0.4083(7) -0.0047(4) 0.91814(18) 0.0439(15) Uani 1 1 d . . . H41A H 0.3543 -0.0341 0.9366 0.053 Uiso 1 1 calc R . . H41B H 0.4520 -0.0454 0.9020 0.053 Uiso 1 1 calc R . . H41C H 0.3467 0.0316 0.9032 0.053 Uiso 1 1 calc R . . C42 C 0.6171(6) -0.0082(3) 0.96185(17) 0.0366(13) Uani 1 1 d . . . H42A H 0.6645 -0.0478 0.9459 0.044 Uiso 1 1 calc R . . H42B H 0.5617 -0.0389 0.9795 0.044 Uiso 1 1 calc R . . H42C H 0.6863 0.0260 0.9753 0.044 Uiso 1 1 calc R . . C43 C 0.6536(6) 0.1949(4) 0.98282(16) 0.0374(13) Uani 1 1 d . . . C44 C 0.9155(5) 0.2097(3) 0.90084(14) 0.0258(11) Uani 1 1 d . . . C45 C 1.0150(5) 0.1529(3) 0.89022(14) 0.0262(11) Uani 1 1 d . . . C46 C 1.0898(5) 0.1638(3) 0.85904(15) 0.0293(11) Uani 1 1 d . . . C47 C 0.9879(6) 0.2842(3) 0.84706(15) 0.0325(12) Uani 1 1 d . . . C48 C 0.9070(5) 0.2786(3) 0.87760(15) 0.0286(11) Uani 1 1 d . . . F1 F 0.3329(4) 0.1852(2) 1.20631(10) 0.0453(8) Uani 1 1 d . . . F2 F 0.1921(4) 0.1929(3) 1.26820(11) 0.0560(10) Uani 1 1 d . . . F3 F 0.3894(5) 0.4363(3) 1.30187(10) 0.0579(11) Uani 1 1 d . . . F4 F 0.5438(4) 0.4404(2) 1.24300(9) 0.0389(8) Uani 1 1 d . . . F5 F 0.8191(3) 0.34077(19) 0.88409(9) 0.0363(7) Uani 1 1 d . . . F6 F 0.9756(4) 0.3517(2) 0.82482(10) 0.0484(9) Uani 1 1 d . . . F7 F 1.1812(3) 0.1047(2) 0.84947(9) 0.0371(7) Uani 1 1 d . . . F8 F 1.0423(3) 0.0834(2) 0.91075(9) 0.0363(7) Uani 1 1 d . . . Ir1 Ir 0.58752(2) 0.309144(12) 1.175621(5) 0.02599(6) Uani 1 1 d . . . Ir2 Ir 0.780457(18) 0.196750(12) 0.945659(5) 0.02230(6) Uani 1 1 d . . . N1 N 0.2888(5) 0.3149(4) 1.28481(15) 0.0452(13) Uani 1 1 d . . . N2 N 1.0794(5) 0.2282(3) 0.83723(13) 0.0326(10) Uani 1 1 d . . . O1 O 0.7869(7) 0.3121(4) 1.11453(16) 0.082(2) Uani 1 1 d . . . O2 O 0.5727(5) 0.1973(3) 1.00538(12) 0.0502(11) Uani 1 1 d . . . P1 P 0.75416(14) 0.23255(8) 1.21043(4) 0.0254(3) Uani 1 1 d . . . P2 P 0.42830(17) 0.38008(9) 1.13673(4) 0.0329(3) Uani 1 1 d . . . P3 P 0.93940(14) 0.25793(8) 0.98748(4) 0.0270(3) Uani 1 1 d . . . P4 P 0.61837(13) 0.12156(8) 0.90891(4) 0.0244(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(3) 0.034(3) 0.033(3) 0.001(2) 0.000(2) 0.011(2) C2 0.048(4) 0.026(3) 0.058(4) 0.014(3) 0.006(3) -0.002(3) C3 0.050(4) 0.060(4) 0.034(3) 0.011(3) -0.006(3) 0.020(3) C4 0.027(3) 0.047(3) 0.055(4) -0.011(3) -0.005(3) -0.003(3) C5 0.040(4) 0.056(4) 0.047(4) -0.021(3) -0.011(3) -0.002(3) C6 0.063(5) 0.088(6) 0.074(6) -0.021(5) 0.019(4) -0.042(5) C7 0.036(3) 0.035(3) 0.040(3) -0.006(2) 0.005(3) 0.006(2) C8 0.051(4) 0.064(5) 0.065(5) -0.004(4) 0.002(4) 0.022(4) C9 0.054(4) 0.037(3) 0.043(3) -0.009(3) 0.002(3) 0.012(3) C10 0.072(5) 0.052(4) 0.054(4) 0.026(3) 0.019(4) 0.021(4) C11 0.069(5) 0.060(5) 0.086(6) 0.033(4) 0.021(5) -0.003(4) C12 0.104(7) 0.081(6) 0.051(5) 0.035(4) 0.020(5) 0.043(5) C13 0.082(5) 0.050(4) 0.031(3) -0.010(3) -0.014(3) 0.036(4) C14 0.118(8) 0.098(7) 0.044(4) -0.032(5) -0.026(5) 0.059(6) C15 0.094(6) 0.033(3) 0.060(5) -0.010(3) -0.036(4) 0.000(4) C16 0.045(3) 0.028(3) 0.033(3) 0.000(2) -0.009(2) 0.003(2) C17 0.058(4) 0.031(3) 0.041(3) -0.008(3) -0.012(3) 0.013(3) C18 0.045(4) 0.036(3) 0.045(4) -0.001(3) -0.014(3) 0.010(3) C19 0.049(4) 0.045(3) 0.043(3) 0.012(3) 0.008(3) 0.018(3) C20 0.028(3) 0.032(3) 0.031(3) 0.010(2) -0.009(2) 0.008(2) C21 0.023(3) 0.047(3) 0.036(3) 0.013(3) 0.001(2) 0.007(2) C22 0.025(3) 0.059(4) 0.046(4) 0.017(3) -0.002(3) 0.007(3) C23 0.047(4) 0.053(4) 0.031(3) 0.002(3) 0.003(3) 0.019(3) C24 0.027(3) 0.043(3) 0.025(3) 0.003(2) 0.004(2) 0.010(2) C25 0.043(3) 0.035(3) 0.034(3) -0.006(2) 0.002(3) -0.001(3) C26 0.058(4) 0.035(3) 0.048(4) -0.006(3) 0.000(3) 0.010(3) C27 0.053(4) 0.052(4) 0.042(4) -0.019(3) 0.003(3) -0.009(3) C28 0.043(3) 0.044(3) 0.039(3) -0.001(3) -0.016(3) 0.010(3) C29 0.070(5) 0.053(4) 0.038(4) 0.014(3) -0.009(3) 0.004(4) C30 0.074(5) 0.066(5) 0.043(4) 0.005(3) -0.011(4) 0.035(4) C31 0.037(3) 0.062(4) 0.036(3) -0.013(3) -0.002(3) -0.015(3) C32 0.036(4) 0.109(7) 0.052(4) -0.028(4) -0.003(3) -0.024(4) C33 0.083(6) 0.052(4) 0.047(4) -0.006(3) 0.012(4) -0.035(4) C34 0.030(3) 0.033(3) 0.040(3) -0.005(2) 0.000(2) -0.006(2) C35 0.047(4) 0.037(3) 0.050(4) -0.008(3) 0.016(3) 0.004(3) C36 0.052(4) 0.074(5) 0.033(3) -0.016(3) 0.002(3) -0.025(4) C37 0.026(3) 0.045(3) 0.039(3) 0.005(3) -0.008(2) 0.000(3) C38 0.037(4) 0.057(4) 0.053(4) 0.019(3) -0.014(3) 0.005(3) C39 0.028(3) 0.056(4) 0.065(4) 0.008(3) -0.002(3) 0.011(3) C40 0.030(3) 0.040(3) 0.028(3) -0.001(2) 0.003(2) -0.004(2) C41 0.035(3) 0.051(4) 0.045(4) 0.000(3) -0.002(3) -0.021(3) C42 0.036(3) 0.032(3) 0.042(3) 0.003(2) 0.002(3) -0.001(2) C43 0.032(3) 0.042(3) 0.038(3) -0.008(3) -0.004(3) -0.006(3) C44 0.022(2) 0.026(3) 0.029(3) -0.005(2) 0.000(2) -0.002(2) C45 0.022(3) 0.026(2) 0.030(3) 0.002(2) 0.001(2) -0.003(2) C46 0.018(2) 0.034(3) 0.035(3) -0.004(2) -0.001(2) 0.001(2) C47 0.037(3) 0.032(3) 0.028(3) 0.006(2) 0.000(2) -0.003(2) C48 0.023(3) 0.027(2) 0.036(3) 0.004(2) -0.001(2) 0.000(2) F1 0.0396(19) 0.045(2) 0.052(2) 0.0033(17) 0.0000(16) -0.0041(16) F2 0.0327(19) 0.069(3) 0.067(3) 0.025(2) 0.0082(17) -0.0074(19) F3 0.072(3) 0.066(3) 0.036(2) -0.0063(18) 0.0163(18) 0.011(2) F4 0.047(2) 0.0362(18) 0.0335(17) -0.0054(14) 0.0060(15) 0.0054(15) F5 0.0409(19) 0.0296(16) 0.0392(18) 0.0057(14) 0.0099(15) 0.0100(14) F6 0.058(2) 0.043(2) 0.045(2) 0.0177(16) 0.0136(17) 0.0071(17) F7 0.0249(16) 0.0447(19) 0.0420(18) -0.0082(15) 0.0062(14) 0.0100(14) F8 0.0331(17) 0.0317(16) 0.0443(18) 0.0071(14) 0.0024(14) 0.0103(14) Ir1 0.02859(12) 0.02511(10) 0.02436(11) 0.00106(8) 0.00223(8) 0.00468(8) Ir2 0.02013(10) 0.02367(10) 0.02301(10) -0.00071(8) -0.00069(7) 0.00051(8) N1 0.033(3) 0.060(3) 0.044(3) 0.017(3) 0.011(2) 0.007(3) N2 0.029(2) 0.039(3) 0.030(2) -0.002(2) 0.0033(19) 0.000(2) O1 0.101(5) 0.086(4) 0.062(4) 0.026(3) 0.041(3) 0.039(4) O2 0.042(2) 0.070(3) 0.039(2) -0.015(2) 0.017(2) -0.013(2) P1 0.0218(6) 0.0264(6) 0.0278(7) -0.0036(5) -0.0015(5) 0.0035(5) P2 0.0442(9) 0.0281(7) 0.0261(7) 0.0032(6) -0.0011(6) 0.0128(6) P3 0.0252(7) 0.0295(7) 0.0260(7) -0.0033(5) -0.0046(5) -0.0024(5) P4 0.0199(6) 0.0294(6) 0.0238(6) -0.0015(5) -0.0014(5) -0.0026(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 C1 C2 1.521(9) . ? C1 C3 1.532(8) . ? C1 P1 1.862(6) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3B 0.9800 . ? C3 H3A 0.9800 . ? C4 C6 1.514(10) . ? C4 C5 1.526(9) . ? C4 P1 1.841(6) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.525(9) . ? C7 C9 1.544(9) . ? C7 P1 1.843(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.515(10) . ? C10 C11 1.550(12) . ? C10 P2 1.849(7) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.509(10) . ? C13 C15 1.531(12) . ? C13 P2 1.854(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.533(8) . ? C16 C17 1.533(8) . ? C16 P2 1.849(6) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O1 1.108(8) . ? C19 Ir1 1.871(7) . ? C20 C21 1.389(8) . ? C20 C24 1.404(8) . ? C20 Ir1 2.096(6) . ? C21 F1 1.349(7) . ? C21 C22 1.392(9) . ? C22 N1 1.291(9) . ? C22 F2 1.344(7) . ? C23 N1 1.298(9) . ? C23 F3 1.353(8) . ? C23 C24 1.374(8) . ? C24 F4 1.352(7) . ? C25 C26 1.528(9) . ? C25 C27 1.533(8) . ? C25 P3 1.850(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.506(10) . ? C28 C30 1.526(9) . ? C28 P3 1.844(6) . ? C28 H28 1.0000 . ? 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 C33 1.521(10) . ? C31 C32 1.546(9) . ? C31 P3 1.858(6) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? C34 C35 1.527(8) . ? C34 C36 1.537(8) . ? C34 P4 1.842(6) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.515(9) . ? C37 C38 1.517(9) . ? C37 P4 1.845(6) . ? C37 H37A 1.0000 . ? 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 C42 1.536(8) . ? C40 C41 1.537(8) . ? C40 P4 1.853(6) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 O2 1.149(7) . ? C43 Ir2 1.848(6) . ? C44 C45 1.388(7) . ? C44 C48 1.389(7) . ? C44 Ir2 2.123(5) . ? C45 F8 1.360(6) . ? C45 C46 1.370(7) . ? C46 N2 1.303(7) . ? C46 F7 1.347(6) . ? C47 N2 1.316(7) . ? C47 F6 1.352(6) . ? C47 C48 1.377(8) . ? C48 F5 1.335(6) . ? Ir1 P2 2.3387(14) . ? Ir1 P1 2.3507(13) . ? Ir2 P3 2.3297(13) . ? Ir2 P4 2.3473(13) . ? 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 C2 C1 C3 109.8(5) . . ? C2 C1 P1 111.5(4) . . ? C3 C1 P1 116.3(5) . . ? C2 C1 H1 106.2 . . ? C3 C1 H1 106.2 . . ? P1 C1 H1 106.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? C1 C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? C6 C4 C5 110.1(6) . . ? C6 C4 P1 112.8(5) . . ? C5 C4 P1 111.7(4) . . ? C6 C4 H4 107.3 . . ? C5 C4 H4 107.3 . . ? P1 C4 H4 107.3 . . ? 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 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 109.5(5) . . ? C8 C7 P1 116.7(5) . . ? C9 C7 P1 113.9(4) . . ? C8 C7 H7 105.2 . . ? C9 C7 H7 105.2 . . ? P1 C7 H7 105.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.4(7) . . ? C12 C10 P2 117.2(6) . . ? C11 C10 P2 112.7(5) . . ? C12 C10 H10A 105.1 . . ? C11 C10 H10A 105.1 . . ? P2 C10 H10A 105.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 109.9(7) . . ? C14 C13 P2 113.1(6) . . ? C15 C13 P2 110.8(4) . . ? C14 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? P2 C13 H13 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 110.0(5) . . ? C18 C16 P2 117.0(4) . . ? C17 C16 P2 112.0(4) . . ? C18 C16 H16 105.6 . . ? C17 C16 H16 105.6 . . ? P2 C16 H16 105.6 . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 Ir1 177.0(8) . . ? C21 C20 C24 110.5(5) . . ? C21 C20 Ir1 127.4(4) . . ? C24 C20 Ir1 122.1(4) . . ? F1 C21 C20 120.1(5) . . ? F1 C21 C22 117.4(6) . . ? C20 C21 C22 122.5(6) . . ? N1 C22 F2 116.5(6) . . ? N1 C22 C21 124.7(6) . . ? F2 C22 C21 118.8(6) . . ? N1 C23 F3 116.3(6) . . ? N1 C23 C24 125.2(6) . . ? F3 C23 C24 118.4(6) . . ? F4 C24 C23 117.4(5) . . ? F4 C24 C20 120.3(5) . . ? C23 C24 C20 122.3(6) . . ? C26 C25 C27 111.0(5) . . ? C26 C25 P3 113.3(4) . . ? C27 C25 P3 115.6(5) . . ? C26 C25 H25 105.3 . . ? C27 C25 H25 105.3 . . ? P3 C25 H25 105.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 110.8(6) . . ? C29 C28 P3 114.3(5) . . ? C30 C28 P3 108.8(4) . . ? C29 C28 H28 107.6 . . ? C30 C28 H28 107.6 . . ? P3 C28 H28 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 109.9(6) . . ? C33 C31 P3 111.8(5) . . ? C32 C31 P3 117.2(5) . . ? C33 C31 H31 105.7 . . ? C32 C31 H31 105.7 . . ? P3 C31 H31 105.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C31 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C35 C34 C36 110.2(5) . . ? C35 C34 P4 112.0(4) . . ? C36 C34 P4 116.9(4) . . ? C35 C34 H34A 105.6 . . ? C36 C34 H34A 105.6 . . ? P4 C34 H34A 105.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 110.1(6) . . ? C39 C37 P4 112.7(4) . . ? C38 C37 P4 111.9(4) . . ? C39 C37 H37A 107.3 . . ? C38 C37 H37A 107.3 . . ? P4 C37 H37A 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C41 109.7(5) . . ? C42 C40 P4 112.9(4) . . ? C41 C40 P4 116.8(4) . . ? C42 C40 H40A 105.5 . . ? C41 C40 H40A 105.5 . . ? P4 C40 H40A 105.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O2 C43 Ir2 176.9(6) . . ? C45 C44 C48 112.5(5) . . ? C45 C44 Ir2 126.5(4) . . ? C48 C44 Ir2 121.0(4) . . ? F8 C45 C46 117.1(5) . . ? F8 C45 C44 120.7(5) . . ? C46 C45 C44 122.2(5) . . ? N2 C46 F7 116.1(5) . . ? N2 C46 C45 124.6(5) . . ? F7 C46 C45 119.3(5) . . ? N2 C47 F6 115.6(5) . . ? N2 C47 C48 125.1(5) . . ? F6 C47 C48 119.3(5) . . ? F5 C48 C47 118.2(5) . . ? F5 C48 C44 120.8(5) . . ? C47 C48 C44 121.0(5) . . ? C19 Ir1 C20 178.4(3) . . ? C19 Ir1 P2 87.9(2) . . ? C20 Ir1 P2 92.68(14) . . ? C19 Ir1 P1 88.18(19) . . ? C20 Ir1 P1 91.32(13) . . ? P2 Ir1 P1 175.38(5) . . ? C43 Ir2 C44 174.2(2) . . ? C43 Ir2 P3 88.33(18) . . ? C44 Ir2 P3 92.74(14) . . ? C43 Ir2 P4 87.70(18) . . ? C44 Ir2 P4 91.80(14) . . ? P3 Ir2 P4 172.85(5) . . ? C22 N1 C23 114.7(5) . . ? C46 N2 C47 114.6(5) . . ? C4 P1 C7 102.6(3) . . ? C4 P1 C1 103.0(3) . . ? C7 P1 C1 109.1(3) . . ? C4 P1 Ir1 114.1(2) . . ? C7 P1 Ir1 110.8(2) . . ? C1 P1 Ir1 116.13(19) . . ? C10 P2 C16 108.8(3) . . ? C10 P2 C13 104.2(4) . . ? C16 P2 C13 102.9(3) . . ? C10 P2 Ir1 110.8(3) . . ? C16 P2 Ir1 117.26(19) . . ? C13 P2 Ir1 111.8(2) . . ? C28 P3 C25 103.4(3) . . ? C28 P3 C31 103.6(3) . . ? C25 P3 C31 109.3(3) . . ? C28 P3 Ir2 110.7(2) . . ? C25 P3 Ir2 112.7(2) . . ? C31 P3 Ir2 115.99(19) . . ? C34 P4 C37 103.6(3) . . ? C34 P4 C40 109.0(3) . . ? C37 P4 C40 103.3(3) . . ? C34 P4 Ir2 115.67(19) . . ? C37 P4 Ir2 114.2(2) . . ? C40 P4 Ir2 110.17(18) . . ? 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 C24 C20 C21 F1 178.4(5) . . . . ? Ir1 C20 C21 F1 -4.3(7) . . . . ? C24 C20 C21 C22 -2.8(7) . . . . ? Ir1 C20 C21 C22 174.5(4) . . . . ? F1 C21 C22 N1 -178.8(5) . . . . ? C20 C21 C22 N1 2.4(9) . . . . ? F1 C21 C22 F2 1.8(8) . . . . ? C20 C21 C22 F2 -177.0(5) . . . . ? N1 C23 C24 F4 -179.8(5) . . . . ? F3 C23 C24 F4 -1.6(8) . . . . ? N1 C23 C24 C20 0.1(9) . . . . ? F3 C23 C24 C20 178.3(5) . . . . ? C21 C20 C24 F4 -178.4(5) . . . . ? Ir1 C20 C24 F4 4.2(7) . . . . ? C21 C20 C24 C23 1.6(7) . . . . ? Ir1 C20 C24 C23 -175.8(4) . . . . ? C48 C44 C45 F8 177.0(4) . . . . ? Ir2 C44 C45 F8 -5.4(7) . . . . ? C48 C44 C45 C46 -3.0(7) . . . . ? Ir2 C44 C45 C46 174.6(4) . . . . ? F8 C45 C46 N2 -177.5(5) . . . . ? C44 C45 C46 N2 2.4(9) . . . . ? F8 C45 C46 F7 2.6(7) . . . . ? C44 C45 C46 F7 -177.5(5) . . . . ? N2 C47 C48 F5 179.7(5) . . . . ? F6 C47 C48 F5 -0.2(8) . . . . ? N2 C47 C48 C44 -1.0(9) . . . . ? F6 C47 C48 C44 179.2(5) . . . . ? C45 C44 C48 F5 -178.4(5) . . . . ? Ir2 C44 C48 F5 3.9(7) . . . . ? C45 C44 C48 C47 2.3(7) . . . . ? Ir2 C44 C48 C47 -175.5(4) . . . . ? O1 C19 Ir1 C20 10(18) . . . . ? O1 C19 Ir1 P2 120(12) . . . . ? O1 C19 Ir1 P1 -63(12) . . . . ? C21 C20 Ir1 C19 -159(8) . . . . ? C24 C20 Ir1 C19 18(8) . . . . ? C21 C20 Ir1 P2 90.7(4) . . . . ? C24 C20 Ir1 P2 -92.3(4) . . . . ? C21 C20 Ir1 P1 -87.0(4) . . . . ? C24 C20 Ir1 P1 90.0(4) . . . . ? O2 C43 Ir2 C44 -9(11) . . . . ? O2 C43 Ir2 P3 91(10) . . . . ? O2 C43 Ir2 P4 -95(10) . . . . ? C45 C44 Ir2 C43 -171(2) . . . . ? C48 C44 Ir2 C43 7(2) . . . . ? C45 C44 Ir2 P3 88.9(4) . . . . ? C48 C44 Ir2 P3 -93.7(4) . . . . ? C45 C44 Ir2 P4 -85.6(4) . . . . ? C48 C44 Ir2 P4 91.8(4) . . . . ? F2 C22 N1 C23 179.0(5) . . . . ? C21 C22 N1 C23 -0.4(9) . . . . ? F3 C23 N1 C22 -179.1(5) . . . . ? C24 C23 N1 C22 -0.8(9) . . . . ? F7 C46 N2 C47 179.1(5) . . . . ? C45 C46 N2 C47 -0.8(8) . . . . ? F6 C47 N2 C46 179.9(5) . . . . ? C48 C47 N2 C46 0.1(8) . . . . ? C6 C4 P1 C7 60.7(6) . . . . ? C5 C4 P1 C7 -174.7(5) . . . . ? C6 C4 P1 C1 174.0(6) . . . . ? C5 C4 P1 C1 -61.4(5) . . . . ? C6 C4 P1 Ir1 -59.2(6) . . . . ? C5 C4 P1 Ir1 65.4(5) . . . . ? C8 C7 P1 C4 57.2(6) . . . . ? C9 C7 P1 C4 -173.7(5) . . . . ? C8 C7 P1 C1 -51.6(6) . . . . ? C9 C7 P1 C1 77.6(5) . . . . ? C8 C7 P1 Ir1 179.3(5) . . . . ? C9 C7 P1 Ir1 -51.5(5) . . . . ? C2 C1 P1 C4 -164.1(4) . . . . ? C3 C1 P1 C4 -37.2(5) . . . . ? C2 C1 P1 C7 -55.7(5) . . . . ? C3 C1 P1 C7 71.3(5) . . . . ? C2 C1 P1 Ir1 70.4(4) . . . . ? C3 C1 P1 Ir1 -162.7(4) . . . . ? C19 Ir1 P1 C4 84.2(3) . . . . ? C20 Ir1 P1 C4 -94.2(3) . . . . ? P2 Ir1 P1 C4 115.9(7) . . . . ? C19 Ir1 P1 C7 -30.9(3) . . . . ? C20 Ir1 P1 C7 150.6(3) . . . . ? P2 Ir1 P1 C7 0.7(7) . . . . ? C19 Ir1 P1 C1 -156.1(3) . . . . ? C20 Ir1 P1 C1 25.4(3) . . . . ? P2 Ir1 P1 C1 -124.5(7) . . . . ? C12 C10 P2 C16 -50.8(7) . . . . ? C11 C10 P2 C16 78.9(6) . . . . ? C12 C10 P2 C13 58.5(7) . . . . ? C11 C10 P2 C13 -171.8(5) . . . . ? C12 C10 P2 Ir1 178.9(6) . . . . ? C11 C10 P2 Ir1 -51.4(6) . . . . ? C18 C16 P2 C10 75.0(5) . . . . ? C17 C16 P2 C10 -53.4(5) . . . . ? C18 C16 P2 C13 -35.2(5) . . . . ? C17 C16 P2 C13 -163.5(4) . . . . ? C18 C16 P2 Ir1 -158.4(4) . . . . ? C17 C16 P2 Ir1 73.3(4) . . . . ? C14 C13 P2 C10 60.1(6) . . . . ? C15 C13 P2 C10 -176.0(5) . . . . ? C14 C13 P2 C16 173.6(6) . . . . ? C15 C13 P2 C16 -62.4(5) . . . . ? C14 C13 P2 Ir1 -59.6(6) . . . . ? C15 C13 P2 Ir1 64.3(5) . . . . ? C19 Ir1 P2 C10 -36.3(4) . . . . ? C20 Ir1 P2 C10 142.2(3) . . . . ? P1 Ir1 P2 C10 -67.9(7) . . . . ? C19 Ir1 P2 C16 -161.9(3) . . . . ? C20 Ir1 P2 C16 16.5(3) . . . . ? P1 Ir1 P2 C16 166.4(6) . . . . ? C19 Ir1 P2 C13 79.5(4) . . . . ? C20 Ir1 P2 C13 -102.0(3) . . . . ? P1 Ir1 P2 C13 47.9(7) . . . . ? C29 C28 P3 C25 55.0(5) . . . . ? C30 C28 P3 C25 179.4(5) . . . . ? C29 C28 P3 C31 169.1(5) . . . . ? C30 C28 P3 C31 -66.5(6) . . . . ? C29 C28 P3 Ir2 -65.9(5) . . . . ? C30 C28 P3 Ir2 58.5(6) . . . . ? C26 C25 P3 C28 -170.6(5) . . . . ? C27 C25 P3 C28 59.6(5) . . . . ? C26 C25 P3 C31 79.5(5) . . . . ? C27 C25 P3 C31 -50.2(5) . . . . ? C26 C25 P3 Ir2 -51.0(5) . . . . ? C27 C25 P3 Ir2 179.2(4) . . . . ? C33 C31 P3 C28 -162.6(4) . . . . ? C32 C31 P3 C28 -34.5(6) . . . . ? C33 C31 P3 C25 -52.9(5) . . . . ? C32 C31 P3 C25 75.2(6) . . . . ? C33 C31 P3 Ir2 75.9(5) . . . . ? C32 C31 P3 Ir2 -156.0(5) . . . . ? C43 Ir2 P3 C28 76.9(3) . . . . ? C44 Ir2 P3 C28 -108.8(3) . . . . ? P4 Ir2 P3 C28 20.6(5) . . . . ? C43 Ir2 P3 C25 -38.3(3) . . . . ? C44 Ir2 P3 C25 136.0(3) . . . . ? P4 Ir2 P3 C25 -94.7(4) . . . . ? C43 Ir2 P3 C31 -165.4(3) . . . . ? C44 Ir2 P3 C31 8.9(3) . . . . ? P4 Ir2 P3 C31 138.2(4) . . . . ? C35 C34 P4 C37 -164.6(4) . . . . ? C36 C34 P4 C37 -36.1(5) . . . . ? C35 C34 P4 C40 -55.1(5) . . . . ? C36 C34 P4 C40 73.4(5) . . . . ? C35 C34 P4 Ir2 69.6(4) . . . . ? C36 C34 P4 Ir2 -161.9(4) . . . . ? C39 C37 P4 C34 172.5(5) . . . . ? C38 C37 P4 C34 -62.8(5) . . . . ? C39 C37 P4 C40 58.8(5) . . . . ? C38 C37 P4 C40 -176.5(5) . . . . ? C39 C37 P4 Ir2 -60.8(5) . . . . ? C38 C37 P4 Ir2 63.9(5) . . . . ? C42 C40 P4 C34 75.2(4) . . . . ? C41 C40 P4 C34 -53.4(5) . . . . ? C42 C40 P4 C37 -175.1(4) . . . . ? C41 C40 P4 C37 56.3(5) . . . . ? C42 C40 P4 Ir2 -52.8(4) . . . . ? C41 C40 P4 Ir2 178.7(4) . . . . ? C43 Ir2 P4 C34 -159.2(3) . . . . ? C44 Ir2 P4 C34 26.6(3) . . . . ? P3 Ir2 P4 C34 -102.8(4) . . . . ? C43 Ir2 P4 C37 80.6(3) . . . . ? C44 Ir2 P4 C37 -93.6(3) . . . . ? P3 Ir2 P4 C37 137.0(4) . . . . ? C43 Ir2 P4 C40 -35.1(3) . . . . ? C44 Ir2 P4 C40 150.7(2) . . . . ? P3 Ir2 P4 C40 21.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.475 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.124 data_klaer1_copound5_C6D6 _database_code_depnum_ccdc_archive 'CCDC 810898' #TrackingRef '- Braun_Klring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 F4 Ir N O3 P2, 3(C6 H6)' _chemical_formula_sum 'C42 H62 F4 Ir N O3 P2' _chemical_formula_weight 959.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0103(8) _cell_length_b 13.5035(7) _cell_length_c 14.5047(7) _cell_angle_alpha 103.313(4) _cell_angle_beta 107.097(4) _cell_angle_gamma 108.962(4) _cell_volume 2148.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 140932 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 29.65 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 3.236 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5784 _exptl_absorpt_correction_T_max 0.7379 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,319 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 76554 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 29.42 _reflns_number_total 11605 _reflns_number_gt 10648 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, 1990' _computing_publication_material 'PLATON, 1990' _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^)+(0.0259P)^2^+17.4388P] 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 SHELXL _refine_ls_extinction_coef 0.0054(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11605 _refine_ls_number_parameters 458 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 C1 C 0.8353(4) 0.7059(4) 0.7043(4) 0.0208(9) Uani 1 1 d . . . C2 C 0.7931(5) 0.7062(4) 0.6047(4) 0.0252(10) Uani 1 1 d . . . C3 C 0.7229(5) 0.7610(4) 0.5764(4) 0.0280(11) Uani 1 1 d . . . C4 C 0.7319(5) 0.8218(4) 0.7348(4) 0.0269(11) Uani 1 1 d . . . C5 C 0.8004(5) 0.7685(4) 0.7693(4) 0.0266(10) Uani 1 1 d . . . C6 C 1.0272(4) 0.5102(4) 0.6419(4) 0.0196(9) Uani 1 1 d . . . C7 C 0.6563(5) 0.3773(4) 0.5902(4) 0.0247(10) Uani 1 1 d . . . H7 H 0.5980 0.3135 0.5979 0.030 Uiso 1 1 calc R . . C8 C 0.5906(6) 0.4423(5) 0.5468(5) 0.0369(14) Uani 1 1 d . . . H8A H 0.6426 0.4991 0.5294 0.055 Uiso 1 1 calc R . . H8B H 0.5676 0.4792 0.5986 0.055 Uiso 1 1 calc R . . H8C H 0.5195 0.3904 0.4844 0.055 Uiso 1 1 calc R . . C9 C 0.7010(6) 0.3272(6) 0.5131(5) 0.0372(13) Uani 1 1 d . . . H9A H 0.6343 0.2813 0.4460 0.056 Uiso 1 1 calc R . . H9B H 0.7373 0.2804 0.5386 0.056 Uiso 1 1 calc R . . H9C H 0.7600 0.3880 0.5052 0.056 Uiso 1 1 calc R . . C10 C 0.6981(5) 0.5013(4) 0.7994(4) 0.0240(10) Uani 1 1 d . . . H10 H 0.6825 0.5646 0.7835 0.029 Uiso 1 1 calc R . . C11 C 0.5759(5) 0.4105(5) 0.7754(5) 0.0350(13) Uani 1 1 d . . . H11A H 0.5855 0.3469 0.7922 0.053 Uiso 1 1 calc R . . H11B H 0.5255 0.3850 0.7018 0.053 Uiso 1 1 calc R . . H11C H 0.5389 0.4417 0.8170 0.053 Uiso 1 1 calc R . . C12 C 0.7722(6) 0.5479(5) 0.9160(4) 0.0307(12) Uani 1 1 d . . . H12A H 0.7360 0.5873 0.9522 0.046 Uiso 1 1 calc R . . H12B H 0.8529 0.6002 0.9312 0.046 Uiso 1 1 calc R . . H12C H 0.7752 0.4859 0.9394 0.046 Uiso 1 1 calc R . . C13 C 0.8315(5) 0.3607(4) 0.7555(4) 0.0257(10) Uani 1 1 d . . . H13 H 0.8670 0.3398 0.7058 0.031 Uiso 1 1 calc R . . C14 C 0.7353(6) 0.2503(5) 0.7419(5) 0.0364(13) Uani 1 1 d . . . H14A H 0.7707 0.1984 0.7550 0.055 Uiso 1 1 calc R . . H14B H 0.6745 0.2171 0.6711 0.055 Uiso 1 1 calc R . . H14C H 0.6989 0.2647 0.7909 0.055 Uiso 1 1 calc R . . C15 C 0.9319(5) 0.4090(5) 0.8627(4) 0.0285(11) Uani 1 1 d . . . H15A H 0.8991 0.4146 0.9154 0.043 Uiso 1 1 calc R . . H15B H 0.9884 0.4838 0.8736 0.043 Uiso 1 1 calc R . . H15C H 0.9726 0.3596 0.8677 0.043 Uiso 1 1 calc R . . C16 C 1.1083(5) 0.9085(4) 0.9001(4) 0.0262(10) Uani 1 1 d . . . H16 H 1.0326 0.9121 0.8622 0.031 Uiso 1 1 calc R . . C17 C 1.2068(6) 1.0253(5) 0.9303(5) 0.0353(13) Uani 1 1 d . . . H17A H 1.1927 1.0820 0.9741 0.053 Uiso 1 1 calc R . . H17B H 1.2067 1.0412 0.8676 0.053 Uiso 1 1 calc R . . H17C H 1.2838 1.0272 0.9682 0.053 Uiso 1 1 calc R . . C18 C 1.0991(5) 0.8896(5) 0.9975(4) 0.0325(12) Uani 1 1 d . . . H18A H 1.1780 0.9069 1.0473 0.049 Uiso 1 1 calc R . . H18B H 1.0463 0.8110 0.9797 0.049 Uiso 1 1 calc R . . H18C H 1.0671 0.9385 1.0281 0.049 Uiso 1 1 calc R . . C19 C 1.2416(5) 0.7616(4) 0.8770(4) 0.0248(10) Uani 1 1 d . . . H19 H 1.2413 0.6999 0.8232 0.030 Uiso 1 1 calc R . . C20 C 1.2241(5) 0.7144(5) 0.9598(4) 0.0286(11) Uani 1 1 d . . . H20A H 1.2799 0.6809 0.9788 0.043 Uiso 1 1 calc R . . H20B H 1.1427 0.6570 0.9330 0.043 Uiso 1 1 calc R . . H20C H 1.2385 0.7751 1.0210 0.043 Uiso 1 1 calc R . . C21 C 1.3654(5) 0.8579(5) 0.9189(5) 0.0343(13) Uani 1 1 d . . . H21A H 1.3763 0.9167 0.9797 0.051 Uiso 1 1 calc R . . H21B H 1.3734 0.8891 0.8654 0.051 Uiso 1 1 calc R . . H21C H 1.4258 0.8294 0.9383 0.051 Uiso 1 1 calc R . . C22 C 1.1648(5) 0.8550(4) 0.7222(4) 0.0254(10) Uani 1 1 d . . . H22 H 1.2387 0.9249 0.7674 0.031 Uiso 1 1 calc R . . C23 C 1.0756(6) 0.8917(6) 0.6624(5) 0.0382(14) Uani 1 1 d . . . H23A H 1.1122 0.9400 0.6293 0.057 Uiso 1 1 calc R . . H23B H 1.0513 0.9334 0.7101 0.057 Uiso 1 1 calc R . . H23C H 1.0059 0.8254 0.6095 0.057 Uiso 1 1 calc R . . C24 C 1.1983(6) 0.7820(5) 0.6501(5) 0.0355(13) Uani 1 1 d . . . H24A H 1.1277 0.7131 0.6027 0.053 Uiso 1 1 calc R . . H24B H 1.2582 0.7627 0.6910 0.053 Uiso 1 1 calc R . . H24C H 1.2304 0.8233 0.6102 0.053 Uiso 1 1 calc R . . F1 F 0.8170(3) 0.6501(3) 0.5297(2) 0.0287(7) Uani 1 1 d . . . F2 F 0.6830(3) 0.7552(3) 0.4780(3) 0.0389(8) Uani 1 1 d . . . F3 F 0.7014(3) 0.8821(3) 0.8012(3) 0.0366(8) Uani 1 1 d . . . F4 F 0.8326(3) 0.7800(3) 0.8705(2) 0.0282(7) Uani 1 1 d . . . Ir1 Ir 0.938293(17) 0.624599(15) 0.739077(14) 0.01814(7) Uani 1 1 d . . . H1 H 0.9067 0.6577 0.8198 0.06(2) Uiso 1 1 d R . . N1 N 0.6916(4) 0.8198(4) 0.6393(4) 0.0309(10) Uani 1 1 d . . . O1 O 0.9610(3) 0.5479(3) 0.5900(3) 0.0211(7) Uani 1 1 d . . . O2 O 1.0433(3) 0.5272(3) 0.7353(3) 0.0201(7) Uani 1 1 d . . . O3 O 1.0777(3) 0.4540(3) 0.6001(3) 0.0248(7) Uani 1 1 d . . . H3 H 1.0581 0.4473 0.5376 0.037 Uiso 1 1 calc R . . P1 P 0.77784(12) 0.46387(10) 0.71937(9) 0.0198(2) Uani 1 1 d . . . P2 P 1.11464(12) 0.79016(10) 0.80903(9) 0.0202(2) Uani 1 1 d . . . C25 C 1.5597(6) 0.6872(6) 0.8833(5) 0.0409(14) Uani 1 1 d . . . H25 H 1.6388 0.7417 0.9068 0.049 Uiso 1 1 calc R . . C26 C 1.4822(6) 0.6510(6) 0.7818(6) 0.0419(15) Uani 1 1 d . . . H26 H 1.5080 0.6811 0.7354 0.050 Uiso 1 1 calc R . . C29 C 1.4045(7) 0.5631(7) 0.9147(6) 0.0496(18) Uani 1 1 d . . . H29 H 1.3773 0.5324 0.9602 0.060 Uiso 1 1 calc R . . C28 C 1.3294(6) 0.5288(6) 0.8133(6) 0.0458(17) Uani 1 1 d . . . H28 H 1.2500 0.4747 0.7889 0.055 Uiso 1 1 calc R . . C27 C 1.3682(6) 0.5720(6) 0.7472(6) 0.0442(15) Uani 1 1 d . . . H27 H 1.3160 0.5471 0.6769 0.053 Uiso 1 1 calc R . . C30 C 1.5212(7) 0.6433(7) 0.9511(6) 0.0469(17) Uani 1 1 d . . . H30 H 1.5736 0.6676 1.0213 0.056 Uiso 1 1 calc R . . C31 C 1.4649(6) 1.0887(6) 0.7927(6) 0.0465(15) Uani 1 1 d U . . H31 H 1.4803 1.1203 0.8637 0.056 Uiso 1 1 calc R . . C32 C 1.5187(6) 1.0230(6) 0.7636(6) 0.0441(15) Uani 1 1 d U . . H32 H 1.5710 1.0088 0.8147 0.053 Uiso 1 1 calc R . . C33 C 1.4986(7) 0.9773(6) 0.6622(6) 0.0513(17) Uani 1 1 d U . . H33 H 1.5373 0.9324 0.6429 0.062 Uiso 1 1 calc R . . C35 C 1.3660(8) 1.0637(7) 0.6180(8) 0.071(3) Uani 1 1 d U . . H35 H 1.3124 1.0776 0.5676 0.085 Uiso 1 1 calc R . . C34 C 1.4210(8) 0.9971(7) 0.5875(6) 0.065(2) Uani 1 1 d U . . H34 H 1.4057 0.9656 0.5165 0.078 Uiso 1 1 calc R . . C36 C 1.3890(7) 1.1090(6) 0.7201(8) 0.061(2) Uani 1 1 d U . . H36 H 1.3520 1.1551 0.7407 0.073 Uiso 1 1 calc R . . C37 C 1.0583(9) 0.1803(9) 0.8255(9) 0.0728(11) Uiso 1 1 d . . . H37 H 1.0857 0.1948 0.8977 0.087 Uiso 1 1 calc R . . C38 C 1.1339(10) 0.2389(9) 0.7899(8) 0.0728(11) Uiso 1 1 d . . . H38 H 1.2128 0.2912 0.8352 0.087 Uiso 1 1 calc R . . C42 C 0.9492(10) 0.1044(9) 0.7660(8) 0.0728(11) Uiso 1 1 d . . . H42 H 0.9025 0.0641 0.7958 0.087 Uiso 1 1 calc R . . C41 C 0.9042(10) 0.0837(9) 0.6671(8) 0.0728(11) Uiso 1 1 d . . . H41 H 0.8250 0.0289 0.6266 0.087 Uiso 1 1 calc R . . C39 C 1.0915(10) 0.2194(9) 0.6839(8) 0.0728(11) Uiso 1 1 d . . . H39 H 1.1405 0.2568 0.6541 0.087 Uiso 1 1 calc R . . C40 C 0.9666(9) 0.1375(9) 0.6205(9) 0.0728(11) Uiso 1 1 d . . . H40 H 0.9314 0.1235 0.5486 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(2) 0.017(2) 0.029(2) 0.0113(19) 0.008(2) 0.0167(19) C2 0.031(3) 0.022(2) 0.026(2) 0.010(2) 0.011(2) 0.015(2) C3 0.029(3) 0.020(2) 0.027(3) 0.006(2) 0.002(2) 0.011(2) C4 0.026(3) 0.018(2) 0.035(3) 0.004(2) 0.012(2) 0.012(2) C5 0.026(3) 0.023(2) 0.025(2) 0.008(2) 0.009(2) 0.006(2) C6 0.023(2) 0.014(2) 0.018(2) 0.0030(17) 0.0081(18) 0.0064(18) C7 0.025(2) 0.020(2) 0.020(2) 0.0047(19) 0.0042(19) 0.006(2) C8 0.036(3) 0.029(3) 0.030(3) 0.010(2) -0.004(2) 0.010(3) C9 0.034(3) 0.039(3) 0.026(3) 0.003(2) 0.010(2) 0.008(3) C10 0.026(2) 0.022(2) 0.027(2) 0.008(2) 0.017(2) 0.007(2) C11 0.032(3) 0.027(3) 0.045(3) 0.007(3) 0.026(3) 0.006(2) C12 0.039(3) 0.030(3) 0.026(3) 0.008(2) 0.017(2) 0.015(2) C13 0.031(3) 0.020(2) 0.027(2) 0.011(2) 0.010(2) 0.011(2) C14 0.036(3) 0.022(3) 0.048(4) 0.017(3) 0.012(3) 0.009(2) C15 0.035(3) 0.028(3) 0.024(2) 0.012(2) 0.009(2) 0.015(2) C16 0.026(3) 0.015(2) 0.027(2) 0.0006(19) 0.008(2) 0.0029(19) C17 0.041(3) 0.017(2) 0.038(3) -0.000(2) 0.015(3) 0.008(2) C18 0.034(3) 0.031(3) 0.025(3) 0.002(2) 0.011(2) 0.011(2) C19 0.025(2) 0.022(2) 0.025(2) 0.010(2) 0.007(2) 0.008(2) C20 0.030(3) 0.030(3) 0.025(2) 0.013(2) 0.008(2) 0.011(2) C21 0.027(3) 0.032(3) 0.042(3) 0.019(3) 0.010(2) 0.009(2) C22 0.028(3) 0.021(2) 0.023(2) 0.0095(19) 0.011(2) 0.004(2) C23 0.037(3) 0.044(4) 0.035(3) 0.026(3) 0.011(3) 0.014(3) C24 0.048(4) 0.025(3) 0.029(3) 0.006(2) 0.023(3) 0.005(3) F1 0.0369(18) 0.0311(17) 0.0218(14) 0.0109(13) 0.0102(13) 0.0191(15) F2 0.045(2) 0.041(2) 0.0321(18) 0.0173(16) 0.0060(16) 0.0252(18) F3 0.0372(19) 0.0277(17) 0.0412(19) 0.0036(15) 0.0132(16) 0.0176(15) F4 0.0347(17) 0.0266(16) 0.0227(15) 0.0041(12) 0.0131(13) 0.0141(14) Ir1 0.02355(11) 0.01582(10) 0.01456(9) 0.00548(6) 0.00698(7) 0.00832(7) N1 0.031(2) 0.019(2) 0.038(3) 0.0073(19) 0.006(2) 0.0136(19) O1 0.0277(18) 0.0197(16) 0.0191(16) 0.0083(13) 0.0088(14) 0.0133(15) O2 0.0258(17) 0.0208(17) 0.0185(15) 0.0082(13) 0.0103(14) 0.0134(14) O3 0.032(2) 0.0270(19) 0.0173(16) 0.0083(14) 0.0097(15) 0.0156(16) P1 0.0237(6) 0.0175(6) 0.0171(5) 0.0060(4) 0.0076(5) 0.0081(5) P2 0.0251(6) 0.0169(6) 0.0166(5) 0.0059(4) 0.0076(5) 0.0074(5) C25 0.031(3) 0.033(3) 0.047(4) 0.005(3) 0.012(3) 0.010(3) C26 0.040(4) 0.039(3) 0.046(4) 0.016(3) 0.017(3) 0.015(3) C29 0.063(5) 0.061(5) 0.067(5) 0.042(4) 0.047(4) 0.045(4) C28 0.034(3) 0.042(4) 0.071(5) 0.028(4) 0.023(3) 0.019(3) C27 0.035(3) 0.043(4) 0.048(4) 0.015(3) 0.010(3) 0.015(3) C30 0.048(4) 0.057(4) 0.040(3) 0.011(3) 0.014(3) 0.035(4) C31 0.041(4) 0.036(3) 0.054(4) 0.018(3) 0.018(3) 0.006(3) C32 0.039(3) 0.038(3) 0.046(3) 0.021(3) 0.010(3) 0.008(3) C33 0.048(4) 0.036(4) 0.062(4) 0.014(3) 0.029(4) 0.005(3) C35 0.053(5) 0.041(4) 0.080(5) 0.041(4) -0.013(4) -0.004(3) C34 0.069(5) 0.046(4) 0.040(4) 0.017(3) 0.008(3) -0.013(3) C36 0.042(4) 0.031(4) 0.093(6) 0.025(4) 0.011(4) 0.008(3) _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 C1 C2 1.389(7) . ? C1 C5 1.393(7) . ? C1 Ir1 2.018(4) . ? C2 F1 1.351(6) . ? C2 C3 1.381(7) . ? C3 N1 1.313(8) . ? C3 F2 1.342(6) . ? C4 N1 1.319(7) . ? C4 F3 1.350(6) . ? C4 C5 1.373(7) . ? C5 F4 1.358(6) . ? C6 O2 1.261(6) . ? C6 O1 1.284(6) . ? C6 O3 1.311(6) . ? C6 Ir1 2.613(5) . ? C7 C8 1.524(8) . ? C7 C9 1.527(8) . ? C7 P1 1.851(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.531(8) . ? C10 C11 1.537(7) . ? C10 P1 1.860(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.527(7) . ? C13 C14 1.528(8) . ? C13 P1 1.859(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.523(8) . ? C16 C17 1.536(8) . ? C16 P2 1.867(5) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.523(7) . ? C19 C21 1.534(8) . ? C19 P2 1.865(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.525(8) . ? C22 C24 1.526(8) . ? C22 P2 1.844(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Ir1 O2 2.186(3) . ? Ir1 O1 2.320(3) . ? Ir1 P2 2.3547(13) . ? Ir1 P1 2.3599(13) . ? Ir1 H1 1.3799 . ? O3 H3 0.8400 . ? C25 C26 1.377(10) . ? C25 C30 1.390(11) . ? C25 H25 0.9500 . ? C26 C27 1.370(10) . ? C26 H26 0.9500 . ? C29 C28 1.371(11) . ? C29 C30 1.398(11) . ? C29 H29 0.9500 . ? C28 C27 1.366(10) . ? C28 H28 0.9500 . ? C27 H27 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.363(11) . ? C31 C32 1.364(11) . ? C31 H31 0.9500 . ? C32 C33 1.365(11) . ? C32 H32 0.9500 . ? C33 C34 1.389(12) . ? C33 H33 0.9500 . ? C35 C36 1.364(14) . ? C35 C34 1.393(15) . ? C35 H35 0.9500 . ? C34 H34 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.318(14) . ? C37 C38 1.358(14) . ? C37 H37 0.9500 . ? C38 C39 1.398(14) . ? C38 H38 0.9500 . ? C42 C41 1.301(14) . ? C42 H42 0.9500 . ? C41 C40 1.346(14) . ? C41 H41 0.9500 . ? C39 C40 1.482(15) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 C2 C1 C5 111.8(4) . . ? C2 C1 Ir1 119.5(4) . . ? C5 C1 Ir1 128.6(4) . . ? F1 C2 C3 116.7(5) . . ? F1 C2 C1 121.1(4) . . ? C3 C2 C1 122.2(5) . . ? N1 C3 F2 116.4(5) . . ? N1 C3 C2 124.8(5) . . ? F2 C3 C2 118.8(5) . . ? N1 C4 F3 115.3(5) . . ? N1 C4 C5 125.1(5) . . ? F3 C4 C5 119.6(5) . . ? F4 C5 C4 116.4(5) . . ? F4 C5 C1 121.6(5) . . ? C4 C5 C1 122.0(5) . . ? O2 C6 O1 119.0(4) . . ? O2 C6 O3 119.4(4) . . ? O1 C6 O3 121.7(4) . . ? O2 C6 Ir1 56.5(2) . . ? O1 C6 Ir1 62.5(2) . . ? O3 C6 Ir1 175.6(4) . . ? C8 C7 C9 109.7(5) . . ? C8 C7 P1 112.4(4) . . ? C9 C7 P1 111.8(4) . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? P1 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 109.0(5) . . ? C12 C10 P1 114.0(4) . . ? C11 C10 P1 116.6(4) . . ? C12 C10 H10 105.4 . . ? C11 C10 H10 105.4 . . ? P1 C10 H10 105.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 110.2(4) . . ? C15 C13 P1 114.2(4) . . ? C14 C13 P1 115.5(4) . . ? C15 C13 H13 105.3 . . ? C14 C13 H13 105.3 . . ? P1 C13 H13 105.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 109.4(5) . . ? C18 C16 P2 114.1(4) . . ? C17 C16 P2 115.6(4) . . ? C18 C16 H16 105.6 . . ? C17 C16 H16 105.6 . . ? P2 C16 H16 105.6 . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 110.9(4) . . ? C20 C19 P2 112.8(4) . . ? C21 C19 P2 116.1(4) . . ? C20 C19 H19 105.3 . . ? C21 C19 H19 105.3 . . ? P2 C19 H19 105.3 . . ? 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 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 111.5(5) . . ? C23 C22 P2 111.9(4) . . ? C24 C22 P2 113.2(4) . . ? C23 C22 H22 106.6 . . ? C24 C22 H22 106.6 . . ? P2 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C1 Ir1 O2 165.31(17) . . ? C1 Ir1 O1 107.18(17) . . ? O2 Ir1 O1 58.13(12) . . ? C1 Ir1 P2 92.82(15) . . ? O2 Ir1 P2 88.97(10) . . ? O1 Ir1 P2 95.76(10) . . ? C1 Ir1 P1 92.93(15) . . ? O2 Ir1 P1 89.39(10) . . ? O1 Ir1 P1 97.31(9) . . ? P2 Ir1 P1 163.48(4) . . ? C1 Ir1 C6 136.58(18) . . ? O2 Ir1 C6 28.73(13) . . ? O1 Ir1 C6 29.41(13) . . ? P2 Ir1 C6 92.11(11) . . ? P1 Ir1 C6 94.32(11) . . ? C1 Ir1 H1 70.0 . . ? O2 Ir1 H1 124.5 . . ? O1 Ir1 H1 171.0 . . ? P2 Ir1 H1 92.9 . . ? P1 Ir1 H1 74.6 . . ? C6 Ir1 H1 152.6 . . ? C3 N1 C4 114.1(5) . . ? C6 O1 Ir1 88.1(3) . . ? C6 O2 Ir1 94.8(3) . . ? C6 O3 H3 109.5 . . ? C7 P1 C13 102.4(2) . . ? C7 P1 C10 102.8(3) . . ? C13 P1 C10 109.8(2) . . ? C7 P1 Ir1 119.77(18) . . ? C13 P1 Ir1 110.20(18) . . ? C10 P1 Ir1 111.20(17) . . ? C22 P2 C19 103.1(2) . . ? C22 P2 C16 102.1(2) . . ? C19 P2 C16 109.8(3) . . ? C22 P2 Ir1 119.67(18) . . ? C19 P2 Ir1 109.15(17) . . ? C16 P2 Ir1 112.36(18) . . ? C26 C25 C30 119.4(7) . . ? C26 C25 H25 120.3 . . ? C30 C25 H25 120.3 . . ? C27 C26 C25 120.7(7) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C29 C30 120.0(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C27 C28 C29 120.3(7) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C27 C26 120.3(7) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C25 C30 C29 119.2(7) . . ? C25 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C36 C31 C32 120.0(8) . . ? C36 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 121.1(7) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C34 119.4(8) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C36 C35 C34 120.0(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C33 C34 C35 119.1(8) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C31 C36 C35 120.4(9) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C42 C37 C38 123.9(11) . . ? C42 C37 H37 118.1 . . ? C38 C37 H37 118.1 . . ? C37 C38 C39 117.6(11) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? C41 C42 C37 121.4(11) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? C42 C41 C40 121.9(11) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C38 C39 C40 116.8(10) . . ? C38 C39 H39 121.6 . . ? C40 C39 H39 121.6 . . ? C41 C40 C39 118.3(10) . . ? C41 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 F1 -179.8(5) . . . . ? Ir1 C1 C2 F1 2.0(7) . . . . ? C5 C1 C2 C3 -1.4(8) . . . . ? Ir1 C1 C2 C3 -179.6(4) . . . . ? F1 C2 C3 N1 -179.7(5) . . . . ? C1 C2 C3 N1 1.9(9) . . . . ? F1 C2 C3 F2 0.1(8) . . . . ? C1 C2 C3 F2 -178.3(5) . . . . ? N1 C4 C5 F4 -179.6(5) . . . . ? F3 C4 C5 F4 0.5(8) . . . . ? N1 C4 C5 C1 0.5(9) . . . . ? F3 C4 C5 C1 -179.5(5) . . . . ? C2 C1 C5 F4 -179.6(5) . . . . ? Ir1 C1 C5 F4 -1.6(8) . . . . ? C2 C1 C5 C4 0.4(8) . . . . ? Ir1 C1 C5 C4 178.3(4) . . . . ? C2 C1 Ir1 O2 0.6(10) . . . . ? C5 C1 Ir1 O2 -177.2(5) . . . . ? C2 C1 Ir1 O1 0.4(5) . . . . ? C5 C1 Ir1 O1 -177.4(4) . . . . ? C2 C1 Ir1 P2 97.3(4) . . . . ? C5 C1 Ir1 P2 -80.5(5) . . . . ? C2 C1 Ir1 P1 -98.2(4) . . . . ? C5 C1 Ir1 P1 84.0(5) . . . . ? C2 C1 Ir1 C6 1.2(6) . . . . ? C5 C1 Ir1 C6 -176.6(4) . . . . ? O2 C6 Ir1 C1 -179.7(3) . . . . ? O1 C6 Ir1 C1 -1.7(4) . . . . ? O3 C6 Ir1 C1 161(5) . . . . ? O1 C6 Ir1 O2 178.0(5) . . . . ? O3 C6 Ir1 O2 -19(5) . . . . ? O2 C6 Ir1 O1 -178.0(5) . . . . ? O3 C6 Ir1 O1 163(5) . . . . ? O2 C6 Ir1 P2 84.0(3) . . . . ? O1 C6 Ir1 P2 -98.0(3) . . . . ? O3 C6 Ir1 P2 65(5) . . . . ? O2 C6 Ir1 P1 -80.8(3) . . . . ? O1 C6 Ir1 P1 97.2(3) . . . . ? O3 C6 Ir1 P1 -100(5) . . . . ? F2 C3 N1 C4 179.2(5) . . . . ? C2 C3 N1 C4 -0.9(8) . . . . ? F3 C4 N1 C3 179.7(5) . . . . ? C5 C4 N1 C3 -0.2(8) . . . . ? O2 C6 O1 Ir1 1.9(4) . . . . ? O3 C6 O1 Ir1 -178.5(4) . . . . ? C1 Ir1 O1 C6 178.8(3) . . . . ? O2 Ir1 O1 C6 -1.1(3) . . . . ? P2 Ir1 O1 C6 84.1(3) . . . . ? P1 Ir1 O1 C6 -85.8(3) . . . . ? O1 C6 O2 Ir1 -2.0(5) . . . . ? O3 C6 O2 Ir1 178.4(4) . . . . ? C1 Ir1 O2 C6 0.9(8) . . . . ? O1 Ir1 O2 C6 1.1(3) . . . . ? P2 Ir1 O2 C6 -96.3(3) . . . . ? P1 Ir1 O2 C6 100.2(3) . . . . ? C8 C7 P1 C13 175.6(4) . . . . ? C9 C7 P1 C13 -60.6(5) . . . . ? C8 C7 P1 C10 61.6(5) . . . . ? C9 C7 P1 C10 -174.5(4) . . . . ? C8 C7 P1 Ir1 -62.2(5) . . . . ? C9 C7 P1 Ir1 61.6(4) . . . . ? C15 C13 P1 C7 -178.3(4) . . . . ? C14 C13 P1 C7 -49.1(5) . . . . ? C15 C13 P1 C10 -69.6(5) . . . . ? C14 C13 P1 C10 59.6(5) . . . . ? C15 C13 P1 Ir1 53.2(4) . . . . ? C14 C13 P1 Ir1 -177.6(4) . . . . ? C12 C10 P1 C7 165.2(4) . . . . ? C11 C10 P1 C7 36.9(5) . . . . ? C12 C10 P1 C13 56.8(4) . . . . ? C11 C10 P1 C13 -71.6(5) . . . . ? C12 C10 P1 Ir1 -65.5(4) . . . . ? C11 C10 P1 Ir1 166.2(4) . . . . ? C1 Ir1 P1 C7 66.4(3) . . . . ? O2 Ir1 P1 C7 -99.0(2) . . . . ? O1 Ir1 P1 C7 -41.3(2) . . . . ? P2 Ir1 P1 C7 176.7(2) . . . . ? C6 Ir1 P1 C7 -70.7(2) . . . . ? C1 Ir1 P1 C13 -175.3(2) . . . . ? O2 Ir1 P1 C13 19.3(2) . . . . ? O1 Ir1 P1 C13 77.0(2) . . . . ? P2 Ir1 P1 C13 -65.0(3) . . . . ? C6 Ir1 P1 C13 47.6(2) . . . . ? C1 Ir1 P1 C10 -53.3(2) . . . . ? O2 Ir1 P1 C10 141.3(2) . . . . ? O1 Ir1 P1 C10 -161.0(2) . . . . ? P2 Ir1 P1 C10 57.0(3) . . . . ? C6 Ir1 P1 C10 169.6(2) . . . . ? C23 C22 P2 C19 -176.8(4) . . . . ? C24 C22 P2 C19 56.2(5) . . . . ? C23 C22 P2 C16 -62.8(5) . . . . ? C24 C22 P2 C16 170.1(4) . . . . ? C23 C22 P2 Ir1 61.9(5) . . . . ? C24 C22 P2 Ir1 -65.2(5) . . . . ? C20 C19 P2 C22 176.0(4) . . . . ? C21 C19 P2 C22 46.4(5) . . . . ? C20 C19 P2 C16 67.8(4) . . . . ? C21 C19 P2 C16 -61.8(5) . . . . ? C20 C19 P2 Ir1 -55.8(4) . . . . ? C21 C19 P2 Ir1 174.6(4) . . . . ? C18 C16 P2 C22 -165.5(4) . . . . ? C17 C16 P2 C22 -37.4(5) . . . . ? C18 C16 P2 C19 -56.6(5) . . . . ? C17 C16 P2 C19 71.5(5) . . . . ? C18 C16 P2 Ir1 65.1(4) . . . . ? C17 C16 P2 Ir1 -166.8(4) . . . . ? C1 Ir1 P2 C22 -72.3(3) . . . . ? O2 Ir1 P2 C22 93.1(2) . . . . ? O1 Ir1 P2 C22 35.3(2) . . . . ? P1 Ir1 P2 C22 177.5(2) . . . . ? C6 Ir1 P2 C22 64.5(2) . . . . ? C1 Ir1 P2 C19 169.4(2) . . . . ? O2 Ir1 P2 C19 -25.1(2) . . . . ? O1 Ir1 P2 C19 -83.0(2) . . . . ? P1 Ir1 P2 C19 59.2(3) . . . . ? C6 Ir1 P2 C19 -53.7(2) . . . . ? C1 Ir1 P2 C16 47.4(2) . . . . ? O2 Ir1 P2 C16 -147.2(2) . . . . ? O1 Ir1 P2 C16 155.0(2) . . . . ? P1 Ir1 P2 C16 -62.9(3) . . . . ? C6 Ir1 P2 C16 -175.8(2) . . . . ? C30 C25 C26 C27 -0.4(11) . . . . ? C30 C29 C28 C27 0.5(11) . . . . ? C29 C28 C27 C26 -0.8(11) . . . . ? C25 C26 C27 C28 0.7(11) . . . . ? C26 C25 C30 C29 0.1(10) . . . . ? C28 C29 C30 C25 -0.2(10) . . . . ? C36 C31 C32 C33 0.5(11) . . . . ? C31 C32 C33 C34 -0.8(11) . . . . ? C32 C33 C34 C35 0.4(11) . . . . ? C36 C35 C34 C33 0.3(12) . . . . ? C32 C31 C36 C35 0.3(11) . . . . ? C34 C35 C36 C31 -0.6(12) . . . . ? C42 C37 C38 C39 1.9(17) . . . . ? C38 C37 C42 C41 -2.9(18) . . . . ? C37 C42 C41 C40 0.6(18) . . . . ? C37 C38 C39 C40 1.1(15) . . . . ? C42 C41 C40 C39 2.4(17) . . . . ? C38 C39 C40 C41 -3.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.962 _refine_diff_density_min -4.271 _refine_diff_density_rms 0.198 data_test_h_compound5Tol _database_code_depnum_ccdc_archive 'CCDC 810899' #TrackingRef '- Braun_Klring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C24 H44 F4 Ir N O3 P2), 5(C7 H8)' _chemical_formula_sum 'C131 H216 F16 Ir4 N4 O12 P8' _chemical_formula_weight 3359.64 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4793(3) _cell_length_b 29.9800(6) _cell_length_c 17.1589(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.9110(10) _cell_angle_gamma 90.00 _cell_volume 7162.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 177314 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 29.58 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3396 _exptl_absorpt_coefficient_mu 3.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4104 _exptl_absorpt_correction_T_max 0.4697 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,319 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 197025 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 29.23 _reflns_number_total 19347 _reflns_number_gt 17150 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, 1990' _computing_publication_material 'PLATON, 1990' _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^)+(0.0300P)^2^+38.0375P] 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 19347 _refine_ls_number_parameters 813 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.005 _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 C1 C -0.1045(3) 0.20945(15) 0.6801(3) 0.0227(9) Uani 1 1 d . . . C2 C -0.0461(4) 0.24663(16) 0.7163(3) 0.0280(10) Uani 1 1 d . . . C3 C -0.0674(5) 0.28803(18) 0.6781(4) 0.0409(14) Uani 1 1 d . . . C4 C -0.2014(4) 0.2631(2) 0.5716(4) 0.0391(14) Uani 1 1 d . . . C5 C -0.1859(4) 0.22076(18) 0.6058(3) 0.0290(10) Uani 1 1 d . . . C6 C -0.2801(3) 0.17578(17) 0.7453(3) 0.0243(9) Uani 1 1 d . . . H6 H -0.2727 0.2019 0.7125 0.029 Uiso 1 1 calc R . . C7 C -0.3408(4) 0.1421(2) 0.6759(3) 0.0342(11) Uani 1 1 d . . . H7A H -0.3616 0.1182 0.7028 0.051 Uiso 1 1 calc R . . H7B H -0.3024 0.1294 0.6487 0.051 Uiso 1 1 calc R . . H7C H -0.3973 0.1571 0.6319 0.051 Uiso 1 1 calc R . . C8 C -0.3375(4) 0.1931(2) 0.7919(3) 0.0381(13) Uani 1 1 d . . . H8A H -0.3984 0.2056 0.7495 0.057 Uiso 1 1 calc R . . H8B H -0.3006 0.2164 0.8332 0.057 Uiso 1 1 calc R . . H8C H -0.3504 0.1686 0.8230 0.057 Uiso 1 1 calc R . . C9 C -0.1565(3) 0.10246(16) 0.8675(3) 0.0239(9) Uani 1 1 d . . . H9 H -0.0878 0.0952 0.9057 0.029 Uiso 1 1 calc R . . C10 C -0.1951(4) 0.06322(17) 0.8039(3) 0.0308(10) Uani 1 1 d . . . H10A H -0.1792 0.0351 0.8362 0.046 Uiso 1 1 calc R . . H10B H -0.1658 0.0637 0.7636 0.046 Uiso 1 1 calc R . . H10C H -0.2650 0.0658 0.7713 0.046 Uiso 1 1 calc R . . C11 C -0.2065(4) 0.10357(19) 0.9270(4) 0.0354(12) Uani 1 1 d . . . H11A H -0.2743 0.1114 0.8932 0.053 Uiso 1 1 calc R . . H11B H -0.1756 0.1259 0.9725 0.053 Uiso 1 1 calc R . . H11C H -0.2018 0.0742 0.9535 0.053 Uiso 1 1 calc R . . C12 C -0.1153(3) 0.19521(17) 0.9077(3) 0.0253(9) Uani 1 1 d . . . H12 H -0.1636 0.1931 0.9317 0.030 Uiso 1 1 calc R . . C13 C -0.1138(5) 0.24374(19) 0.8818(4) 0.0415(14) Uani 1 1 d . . . H13A H -0.1076 0.2633 0.9298 0.062 Uiso 1 1 calc R . . H13B H -0.1737 0.2506 0.8307 0.062 Uiso 1 1 calc R . . H13C H -0.0592 0.2485 0.8683 0.062 Uiso 1 1 calc R . . C14 C -0.0184(4) 0.1826(2) 0.9810(3) 0.0378(13) Uani 1 1 d . . . H14A H 0.0319 0.1860 0.9613 0.057 Uiso 1 1 calc R . . H14B H -0.0204 0.1516 0.9981 0.057 Uiso 1 1 calc R . . H14C H -0.0045 0.2023 1.0307 0.057 Uiso 1 1 calc R . . C15 C -0.0900(3) 0.14153(17) 0.5223(3) 0.0257(9) Uani 1 1 d . . . H10 H -0.1132 0.1725 0.5235 0.031 Uiso 1 1 calc R . . C16 C -0.0488(4) 0.14233(19) 0.4552(3) 0.0338(12) Uani 1 1 d . . . H16A H -0.0229 0.1129 0.4524 0.051 Uiso 1 1 calc R . . H16B H 0.0026 0.1646 0.4723 0.051 Uiso 1 1 calc R . . H16C H -0.0998 0.1501 0.3981 0.051 Uiso 1 1 calc R . . C17 C -0.1794(4) 0.1120(2) 0.4888(3) 0.0381(13) Uani 1 1 d . . . H17A H -0.2314 0.1267 0.4395 0.057 Uiso 1 1 calc R . . H17B H -0.1994 0.1073 0.5351 0.057 Uiso 1 1 calc R . . H17C H -0.1649 0.0832 0.4703 0.057 Uiso 1 1 calc R . . C18 C 0.0247(4) 0.06826(16) 0.6459(3) 0.0262(9) Uani 1 1 d . . . H18 H 0.0770 0.0643 0.7059 0.031 Uiso 1 1 calc R . . C19 C 0.0664(5) 0.0505(2) 0.5852(4) 0.0394(13) Uani 1 1 d . . . H19A H 0.0935 0.0207 0.6043 0.059 Uiso 1 1 calc R . . H19B H 0.1170 0.0707 0.5868 0.059 Uiso 1 1 calc R . . H19C H 0.0153 0.0488 0.5259 0.059 Uiso 1 1 calc R . . C20 C -0.0576(4) 0.03821(18) 0.6411(4) 0.0353(11) Uani 1 1 d . . . H20A H -0.1037 0.0340 0.5804 0.053 Uiso 1 1 calc R . . H20B H -0.0900 0.0522 0.6727 0.053 Uiso 1 1 calc R . . H20C H -0.0318 0.0092 0.6671 0.053 Uiso 1 1 calc R . . C21 C 0.1080(3) 0.15471(17) 0.6439(3) 0.0247(9) Uani 1 1 d . . . H21 H 0.1195 0.1432 0.5945 0.030 Uiso 1 1 calc R . . C22 C 0.1001(4) 0.20556(19) 0.6353(4) 0.0374(12) Uani 1 1 d . . . H22A H 0.1025 0.2184 0.6887 0.056 Uiso 1 1 calc R . . H22B H 0.0391 0.2136 0.5864 0.056 Uiso 1 1 calc R . . H22C H 0.1535 0.2172 0.6253 0.056 Uiso 1 1 calc R . . C23 C 0.1949(4) 0.1417(2) 0.7275(3) 0.0379(13) Uani 1 1 d . . . H23A H 0.2524 0.1565 0.7297 0.057 Uiso 1 1 calc R . . H23B H 0.2036 0.1093 0.7290 0.057 Uiso 1 1 calc R . . H23C H 0.1843 0.1510 0.7774 0.057 Uiso 1 1 calc R . . C24 C 0.0754(3) 0.11102(15) 0.8677(3) 0.0194(8) Uani 1 1 d . . . C25 C 0.4798(3) 0.07223(15) 1.1954(3) 0.0203(8) Uani 1 1 d . . . C26 C 0.5697(3) 0.05923(17) 1.2577(3) 0.0249(9) Uani 1 1 d . . . C27 C 0.5952(4) 0.01480(19) 1.2756(3) 0.0326(11) Uani 1 1 d . . . C28 C 0.4523(4) -0.00816(17) 1.1812(4) 0.0335(11) Uani 1 1 d . . . C29 C 0.4209(4) 0.03532(15) 1.1573(3) 0.0241(9) Uani 1 1 d . . . C30 C 0.2599(3) 0.12401(18) 1.2430(3) 0.0265(9) Uani 1 1 d . . . H30 H 0.2516 0.1305 1.2965 0.032 Uiso 1 1 calc R . . C31 C 0.1758(4) 0.1461(2) 1.1668(4) 0.0403(13) Uani 1 1 d . . . H31A H 0.1829 0.1414 1.1134 0.060 Uiso 1 1 calc R . . H31B H 0.1755 0.1782 1.1778 0.060 Uiso 1 1 calc R . . H31C H 0.1152 0.1329 1.1606 0.060 Uiso 1 1 calc R . . C32 C 0.2557(4) 0.0737(2) 1.2314(4) 0.0418(13) Uani 1 1 d . . . H32A H 0.1963 0.0623 1.2313 0.063 Uiso 1 1 calc R . . H32B H 0.3111 0.0601 1.2790 0.063 Uiso 1 1 calc R . . H32C H 0.2568 0.0664 1.1762 0.063 Uiso 1 1 calc R . . C33 C 0.3633(4) 0.20736(17) 1.2696(3) 0.0296(10) Uani 1 1 d . . . H33 H 0.3119 0.2166 1.2119 0.035 Uiso 1 1 calc R . . C34 C 0.3260(5) 0.2211(2) 1.3353(4) 0.0411(13) Uani 1 1 d . . . H34A H 0.3733 0.2129 1.3938 0.062 Uiso 1 1 calc R . . H34B H 0.2653 0.2057 1.3220 0.062 Uiso 1 1 calc R . . H34C H 0.3154 0.2534 1.3323 0.062 Uiso 1 1 calc R . . C35 C 0.4517(5) 0.23518(19) 1.2821(4) 0.0402(13) Uani 1 1 d . . . H35A H 0.4331 0.2666 1.2693 0.060 Uiso 1 1 calc R . . H35B H 0.4778 0.2243 1.2428 0.060 Uiso 1 1 calc R . . H35C H 0.5007 0.2324 1.3421 0.060 Uiso 1 1 calc R . . C36 C 0.4608(3) 0.12279(18) 1.3668(3) 0.0269(9) Uani 1 1 d . . . H36 H 0.4780 0.0924 1.3540 0.032 Uiso 1 1 calc R . . C37 C 0.4193(4) 0.1155(2) 1.4325(3) 0.0383(13) Uani 1 1 d . . . H37A H 0.4684 0.1021 1.4854 0.058 Uiso 1 1 calc R . . H37B H 0.3637 0.0955 1.4075 0.058 Uiso 1 1 calc R . . H37C H 0.3992 0.1442 1.4465 0.058 Uiso 1 1 calc R . . C38 C 0.5561(4) 0.1481(2) 1.4109(3) 0.0373(13) Uani 1 1 d . . . H38A H 0.5455 0.1763 1.4342 0.056 Uiso 1 1 calc R . . H38B H 0.5812 0.1542 1.3685 0.056 Uiso 1 1 calc R . . H38C H 0.6024 0.1300 1.4582 0.056 Uiso 1 1 calc R . . C39 C 0.4382(3) 0.13636(17) 0.9520(3) 0.0259(9) Uani 1 1 d . . . H39 H 0.3922 0.1614 0.9434 0.031 Uiso 1 1 calc R . . C40 C 0.3762(4) 0.09395(18) 0.9229(3) 0.0328(11) Uani 1 1 d . . . H40A H 0.3151 0.1010 0.8732 0.049 Uiso 1 1 calc R . . H40B H 0.3638 0.0828 0.9707 0.049 Uiso 1 1 calc R . . H40C H 0.4103 0.0711 0.9062 0.049 Uiso 1 1 calc R . . C41 C 0.4844(4) 0.1464(2) 0.8914(3) 0.0362(12) Uani 1 1 d . . . H41A H 0.5244 0.1210 0.8913 0.054 Uiso 1 1 calc R . . H41B H 0.5244 0.1731 0.9115 0.054 Uiso 1 1 calc R . . H41C H 0.4341 0.1513 0.8326 0.054 Uiso 1 1 calc R . . C42 C 0.5912(4) 0.18719(16) 1.0893(3) 0.0268(9) Uani 1 1 d . . . H42 H 0.6281 0.1847 1.0539 0.032 Uiso 1 1 calc R . . C43 C 0.6654(4) 0.1905(2) 1.1839(3) 0.0352(12) Uani 1 1 d . . . H43A H 0.7092 0.2153 1.1905 0.053 Uiso 1 1 calc R . . H43B H 0.7020 0.1626 1.2012 0.053 Uiso 1 1 calc R . . H43C H 0.6325 0.1957 1.2206 0.053 Uiso 1 1 calc R . . C44 C 0.5330(5) 0.23023(18) 1.0612(4) 0.0398(13) Uani 1 1 d . . . H44A H 0.5028 0.2363 1.0998 0.060 Uiso 1 1 calc R . . H44B H 0.4833 0.2270 1.0016 0.060 Uiso 1 1 calc R . . H44C H 0.5757 0.2550 1.0642 0.060 Uiso 1 1 calc R . . C45 C 0.6125(3) 0.09219(15) 1.0916(3) 0.0208(8) Uani 1 1 d . . . H45 H 0.6455 0.0884 1.1559 0.025 Uiso 1 1 calc R . . C46 C 0.5713(4) 0.04625(16) 1.0542(3) 0.0271(9) Uani 1 1 d . . . H46A H 0.5512 0.0462 0.9916 0.041 Uiso 1 1 calc R . . H46B H 0.5158 0.0398 1.0656 0.041 Uiso 1 1 calc R . . H46C H 0.6206 0.0234 1.0816 0.041 Uiso 1 1 calc R . . C47 C 0.6911(3) 0.10403(18) 1.0637(3) 0.0280(10) Uani 1 1 d . . . H47A H 0.7340 0.0784 1.0738 0.042 Uiso 1 1 calc R . . H47B H 0.7279 0.1296 1.0974 0.042 Uiso 1 1 calc R . . H47C H 0.6616 0.1116 1.0019 0.042 Uiso 1 1 calc R . . C48 C 0.2907(3) 0.17687(15) 1.0332(3) 0.0202(8) Uani 1 1 d . . . C49 C 0.0425(5) -0.0165(2) 0.9124(4) 0.0426(14) Uani 1 1 d . . . H49A H 0.0942 -0.0039 0.9648 0.064 Uiso 1 1 calc R . . H49B H 0.0148 -0.0424 0.9281 0.064 Uiso 1 1 calc R . . H49C H -0.0074 0.0061 0.8848 0.064 Uiso 1 1 calc R . . C50 C 0.0824(4) -0.03068(18) 0.8506(3) 0.0305(10) Uani 1 1 d . . . C51 C 0.1495(4) -0.00457(18) 0.8382(3) 0.0322(11) Uani 1 1 d . . . H51 H 0.1714 0.0223 0.8704 0.039 Uiso 1 1 calc R . . C52 C 0.1852(4) -0.01686(19) 0.7799(4) 0.0332(11) Uani 1 1 d . . . H52 H 0.2303 0.0016 0.7717 0.040 Uiso 1 1 calc R . . C53 C 0.1545(4) -0.0564(2) 0.7337(3) 0.0351(11) Uani 1 1 d . . . H53 H 0.1788 -0.0651 0.6939 0.042 Uiso 1 1 calc R . . C54 C 0.0886(4) -0.0828(2) 0.7458(4) 0.0379(12) Uani 1 1 d . . . H54 H 0.0674 -0.1098 0.7141 0.046 Uiso 1 1 calc R . . C55 C 0.0528(4) -0.07018(19) 0.8042(4) 0.0358(11) Uani 1 1 d . . . H55 H 0.0077 -0.0888 0.8123 0.043 Uiso 1 1 calc R . . C56 C 0.1858(10) 0.0668(4) 1.4459(9) 0.114(4) Uiso 1 1 d . . . H56A H 0.2273 0.0534 1.4225 0.170 Uiso 1 1 calc R . . H56B H 0.1229 0.0734 1.3983 0.170 Uiso 1 1 calc R . . H56C H 0.1779 0.0459 1.4862 0.170 Uiso 1 1 calc R . . C57 C 0.2283(6) 0.1069(3) 1.4903(5) 0.0600(18) Uiso 1 1 d . . . C58 C 0.3020(6) 0.1083(3) 1.5668(5) 0.0613(19) Uiso 1 1 d . . . H58 H 0.3274 0.0812 1.5971 0.074 Uiso 1 1 calc R . . C59 C 0.3451(9) 0.1502(4) 1.6056(8) 0.095(3) Uiso 1 1 d . . . H59 H 0.4001 0.1521 1.6599 0.114 Uiso 1 1 calc R . . C60 C 0.2994(7) 0.1877(3) 1.5568(6) 0.076(2) Uiso 1 1 d . . . H60 H 0.3225 0.2167 1.5787 0.092 Uiso 1 1 calc R . . C61 C 0.2226(7) 0.1834(3) 1.4790(6) 0.074(2) Uiso 1 1 d . . . H61 H 0.1949 0.2103 1.4491 0.089 Uiso 1 1 calc R . . C62 C 0.1827(7) 0.1463(3) 1.4404(7) 0.076(2) Uiso 1 1 d . . . H62 H 0.1290 0.1452 1.3851 0.091 Uiso 1 1 calc R . . C63 C 0.339(2) 0.5214(8) -0.0778(13) 0.075(9) Uani 0.50 1 d PD A -1 H63A H 0.2962 0.5070 -0.0571 0.113 Uiso 0.50 1 calc PR A -1 H63B H 0.3178 0.5144 -0.1392 0.113 Uiso 0.50 1 calc PR A -1 H63C H 0.3376 0.5538 -0.0704 0.113 Uiso 0.50 1 calc PR A -1 C64 C 0.4378(11) 0.5049(4) -0.0275(7) 0.045(3) Uani 0.50 1 d PD A -1 C65 C 0.4713(13) 0.4929(7) 0.0585(9) 0.042(5) Uani 0.50 1 d PD A -1 H65 H 0.4294 0.4956 0.0855 0.050 Uiso 0.50 1 calc PR A -1 C66 C 0.5637(8) 0.4771(5) 0.1071(7) 0.044(3) Uani 0.50 1 d PD A -1 H66 H 0.5839 0.4687 0.1659 0.053 Uiso 0.50 1 calc PR A -1 C67 C 0.6261(15) 0.4738(9) 0.0697(11) 0.051(6) Uani 0.50 1 d PD A -1 H67 H 0.6901 0.4637 0.1023 0.061 Uiso 0.50 1 calc PR A -1 C68 C 0.5934(10) 0.4854(5) -0.0160(8) 0.055(4) Uani 0.50 1 d PD A -1 H68 H 0.6353 0.4825 -0.0429 0.066 Uiso 0.50 1 calc PR A -1 C69 C 0.5015(12) 0.5011(9) -0.0637(13) 0.052(7) Uani 0.50 1 d PD A -1 H69 H 0.4817 0.5094 -0.1225 0.062 Uiso 0.50 1 calc PR A -1 F1 F 0.0372(2) 0.24247(11) 0.7891(2) 0.0357(7) Uani 1 1 d . . . F2 F -0.0075(3) 0.32210(12) 0.7154(3) 0.0614(12) Uani 1 1 d . . . F3 F -0.2796(3) 0.27126(14) 0.4969(2) 0.0535(11) Uani 1 1 d . . . F4 F -0.2540(2) 0.18999(11) 0.56148(18) 0.0344(7) Uani 1 1 d . . . F5 F 0.6380(2) 0.08971(11) 1.30197(18) 0.0314(6) Uani 1 1 d . . . F6 F 0.6841(3) 0.00470(13) 1.3352(2) 0.0466(9) Uani 1 1 d . . . F7 F 0.3923(3) -0.04187(11) 1.1417(3) 0.0495(9) Uani 1 1 d . . . F8 F 0.3321(2) 0.04090(11) 1.0924(2) 0.0336(7) Uani 1 1 d . . . Ir1 Ir -0.064605(11) 0.149096(5) 0.735179(9) 0.01625(4) Uani 1 1 d . . . H1 H -0.1525 0.1470 0.6635 0.024 Uiso 1 1 d R . . Ir2 Ir 0.434630(11) 0.134317(5) 1.155057(10) 0.01632(4) Uani 1 1 d . . . H2 H 0.5235 0.1342 1.2257 0.024 Uiso 1 1 d R . . N1 N 0.5382(4) -0.01904(16) 1.2389(3) 0.0390(11) Uani 1 1 d . . . N2 N -0.1448(4) 0.29734(17) 0.6055(4) 0.0450(14) Uani 1 1 d . . . O1 O 0.0035(2) 0.09100(10) 0.81243(19) 0.0210(6) Uani 1 1 d . . . O2 O 0.0861(2) 0.15268(11) 0.85805(19) 0.0217(6) Uani 1 1 d . . . O3 O 0.1362(2) 0.08841(11) 0.9345(2) 0.0263(7) Uani 1 1 d . . . H3 H 0.1809 0.1053 0.9666 0.040 Uiso 1 1 calc R . . O4 O 0.3633(2) 0.19606(11) 1.0910(2) 0.0217(6) Uani 1 1 d . . . O5 O 0.2841(2) 0.13454(10) 1.0355(2) 0.0214(6) Uani 1 1 d . . . O6 O 0.2251(2) 0.20161(11) 0.9730(2) 0.0278(7) Uani 1 1 d . . . H6A H 0.1809 0.1852 0.9386 0.042 Uiso 1 1 calc R . . P1 P -0.15485(8) 0.15619(4) 0.81500(7) 0.0187(2) Uani 1 1 d . . . P2 P -0.00413(8) 0.12869(4) 0.63559(7) 0.0193(2) Uani 1 1 d . . . P3 P 0.37851(8) 0.14656(4) 1.26040(7) 0.0198(2) Uani 1 1 d . . . P4 P 0.51912(8) 0.13562(4) 1.06981(7) 0.0182(2) 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 C1 0.033(2) 0.019(2) 0.024(2) 0.0032(16) 0.0194(19) 0.0053(17) C2 0.034(3) 0.024(2) 0.033(2) 0.0007(18) 0.021(2) 0.0037(19) C3 0.062(4) 0.022(3) 0.064(4) 0.006(2) 0.051(3) 0.003(2) C4 0.050(3) 0.044(3) 0.038(3) 0.021(2) 0.033(3) 0.028(3) C5 0.034(3) 0.038(3) 0.023(2) 0.0044(19) 0.020(2) 0.009(2) C6 0.018(2) 0.036(3) 0.021(2) 0.0029(17) 0.0101(17) 0.0061(18) C7 0.020(2) 0.047(3) 0.029(2) -0.002(2) 0.0047(19) -0.000(2) C8 0.028(3) 0.062(4) 0.029(2) 0.006(2) 0.017(2) 0.017(2) C9 0.025(2) 0.029(2) 0.021(2) 0.0032(17) 0.0130(17) 0.0006(18) C10 0.032(3) 0.029(3) 0.034(3) 0.000(2) 0.017(2) -0.004(2) C11 0.045(3) 0.037(3) 0.039(3) 0.008(2) 0.033(3) 0.003(2) C12 0.025(2) 0.034(3) 0.020(2) -0.0066(17) 0.0121(18) -0.0003(18) C13 0.066(4) 0.031(3) 0.033(3) -0.010(2) 0.026(3) -0.008(3) C14 0.025(2) 0.059(4) 0.026(2) -0.015(2) 0.007(2) 0.001(2) C15 0.025(2) 0.037(3) 0.0146(18) 0.0011(17) 0.0089(17) 0.0094(19) C16 0.044(3) 0.044(3) 0.019(2) 0.0036(19) 0.019(2) 0.012(2) C17 0.027(3) 0.058(4) 0.023(2) -0.008(2) 0.004(2) 0.003(2) C18 0.035(3) 0.026(2) 0.021(2) 0.0002(17) 0.0149(19) 0.0065(19) C19 0.057(4) 0.035(3) 0.037(3) 0.003(2) 0.030(3) 0.016(3) C20 0.044(3) 0.028(3) 0.032(3) -0.005(2) 0.015(2) -0.002(2) C21 0.021(2) 0.035(3) 0.021(2) 0.0009(17) 0.0113(17) 0.0014(18) C22 0.037(3) 0.038(3) 0.045(3) -0.002(2) 0.026(3) -0.004(2) C23 0.018(2) 0.067(4) 0.026(2) 0.004(2) 0.0076(19) 0.001(2) C24 0.0175(19) 0.026(2) 0.0150(17) -0.0008(15) 0.0079(15) 0.0015(16) C25 0.025(2) 0.022(2) 0.0184(18) 0.0000(15) 0.0131(17) 0.0005(16) C26 0.029(2) 0.030(2) 0.021(2) 0.0040(17) 0.0153(18) 0.0022(18) C27 0.040(3) 0.038(3) 0.031(2) 0.015(2) 0.025(2) 0.015(2) C28 0.051(3) 0.023(2) 0.041(3) 0.000(2) 0.033(3) -0.005(2) C29 0.033(2) 0.019(2) 0.027(2) -0.0007(16) 0.0192(19) -0.0007(18) C30 0.018(2) 0.041(3) 0.025(2) -0.0033(19) 0.0130(17) -0.0026(18) C31 0.019(2) 0.070(4) 0.033(3) 0.003(3) 0.012(2) -0.000(2) C32 0.039(3) 0.042(3) 0.053(3) -0.010(3) 0.028(3) -0.015(3) C33 0.037(3) 0.027(2) 0.029(2) -0.0052(18) 0.018(2) -0.000(2) C34 0.056(4) 0.039(3) 0.039(3) -0.006(2) 0.031(3) 0.004(3) C35 0.054(4) 0.029(3) 0.044(3) -0.015(2) 0.029(3) -0.013(2) C36 0.026(2) 0.039(3) 0.0173(19) 0.0006(18) 0.0102(17) 0.0051(19) C37 0.040(3) 0.058(4) 0.022(2) 0.008(2) 0.018(2) 0.009(3) C38 0.023(2) 0.065(4) 0.021(2) -0.005(2) 0.0063(19) 0.001(2) C39 0.027(2) 0.037(3) 0.0139(18) 0.0033(17) 0.0093(17) 0.0041(19) C40 0.031(3) 0.039(3) 0.020(2) -0.0045(19) 0.0031(19) 0.000(2) C41 0.041(3) 0.052(3) 0.021(2) 0.009(2) 0.018(2) 0.005(2) C42 0.031(2) 0.024(2) 0.033(2) -0.0012(18) 0.022(2) -0.0055(18) C43 0.035(3) 0.042(3) 0.033(3) -0.012(2) 0.019(2) -0.016(2) C44 0.048(3) 0.022(3) 0.060(4) 0.002(2) 0.033(3) -0.004(2) C45 0.023(2) 0.023(2) 0.0199(19) 0.0023(15) 0.0122(17) 0.0021(16) C46 0.033(2) 0.023(2) 0.031(2) -0.0034(18) 0.020(2) 0.0005(19) C47 0.024(2) 0.035(3) 0.030(2) 0.0069(19) 0.0161(19) 0.0050(19) C48 0.0179(19) 0.025(2) 0.0180(18) -0.0011(15) 0.0077(15) 0.0003(16) C49 0.051(4) 0.041(3) 0.045(3) 0.006(2) 0.030(3) 0.015(3) C50 0.032(3) 0.031(3) 0.031(2) 0.0059(19) 0.016(2) 0.011(2) C51 0.033(3) 0.029(3) 0.034(3) 0.004(2) 0.015(2) 0.006(2) C52 0.031(3) 0.034(3) 0.038(3) 0.007(2) 0.018(2) 0.004(2) C53 0.040(3) 0.041(3) 0.026(2) 0.003(2) 0.017(2) 0.009(2) C54 0.045(3) 0.037(3) 0.032(3) -0.004(2) 0.018(2) -0.001(2) C55 0.038(3) 0.036(3) 0.037(3) 0.002(2) 0.021(2) -0.002(2) C63 0.09(2) 0.08(2) 0.045(10) 0.008(10) 0.022(12) 0.039(15) C64 0.069(9) 0.037(6) 0.028(5) -0.000(5) 0.021(6) 0.001(6) C65 0.062(11) 0.044(10) 0.036(9) 0.005(7) 0.036(9) 0.010(9) C66 0.047(7) 0.060(8) 0.028(5) 0.002(5) 0.020(5) 0.002(6) C67 0.052(13) 0.061(11) 0.039(9) -0.004(8) 0.019(9) -0.001(10) C68 0.057(9) 0.070(10) 0.048(8) -0.004(7) 0.032(7) -0.013(8) C69 0.070(14) 0.061(12) 0.029(8) 0.003(7) 0.027(8) -0.002(11) F1 0.0349(17) 0.0328(17) 0.0402(17) -0.0086(13) 0.0172(14) -0.0078(13) F2 0.087(3) 0.0226(17) 0.103(3) -0.0012(19) 0.067(3) -0.0077(18) F3 0.061(2) 0.072(3) 0.0417(19) 0.0335(18) 0.0350(18) 0.044(2) F4 0.0283(15) 0.0471(19) 0.0236(14) 0.0037(12) 0.0074(12) 0.0106(13) F5 0.0257(14) 0.0410(18) 0.0219(13) -0.0003(11) 0.0052(11) 0.0025(12) F6 0.045(2) 0.060(2) 0.0413(18) 0.0259(17) 0.0253(16) 0.0262(17) F7 0.072(3) 0.0267(17) 0.071(3) -0.0118(16) 0.051(2) -0.0165(17) F8 0.0309(15) 0.0362(17) 0.0331(15) -0.0073(12) 0.0133(13) -0.0118(13) Ir1 0.01628(7) 0.01916(8) 0.01328(7) -0.00040(5) 0.00642(6) 0.00069(5) Ir2 0.01576(7) 0.01972(8) 0.01368(7) -0.00138(5) 0.00662(6) -0.00157(5) N1 0.055(3) 0.031(2) 0.048(3) 0.011(2) 0.039(3) 0.008(2) N2 0.068(4) 0.030(3) 0.064(3) 0.021(2) 0.054(3) 0.022(2) O1 0.0204(15) 0.0218(16) 0.0175(14) 0.0010(11) 0.0052(12) 0.0011(12) O2 0.0244(15) 0.0220(16) 0.0190(14) -0.0004(11) 0.0098(12) -0.0007(12) O3 0.0287(17) 0.0226(17) 0.0196(15) 0.0021(12) 0.0029(13) -0.0003(13) O4 0.0195(15) 0.0220(16) 0.0204(14) 0.0013(11) 0.0057(12) 0.0013(12) O5 0.0231(15) 0.0195(15) 0.0192(14) -0.0004(11) 0.0070(12) -0.0000(12) O6 0.0246(16) 0.0238(17) 0.0250(16) 0.0013(13) 0.0017(13) 0.0001(13) P1 0.0186(5) 0.0233(5) 0.0149(4) -0.0004(4) 0.0080(4) 0.0009(4) P2 0.0187(5) 0.0250(6) 0.0140(4) -0.0002(4) 0.0071(4) 0.0024(4) P3 0.0180(5) 0.0255(6) 0.0177(5) -0.0020(4) 0.0095(4) -0.0013(4) P4 0.0204(5) 0.0202(5) 0.0157(4) 0.0002(4) 0.0095(4) -0.0012(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 C1 C5 1.387(7) . ? C1 C2 1.398(7) . ? C1 Ir1 2.010(4) . ? C2 F1 1.354(6) . ? C2 C3 1.374(7) . ? C3 N2 1.327(9) . ? C3 F2 1.339(7) . ? C4 N2 1.310(9) . ? C4 F3 1.346(7) . ? C4 C5 1.374(7) . ? C5 F4 1.356(6) . ? C6 C8 1.523(6) . ? C6 C7 1.530(7) . ? C6 P1 1.874(5) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.528(6) . ? C9 C10 1.537(7) . ? C9 P1 1.851(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.525(8) . ? C12 C14 1.524(7) . ? C12 P1 1.850(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.528(8) . ? C15 C16 1.542(6) . ? C15 P2 1.853(5) . ? C15 H10 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.533(7) . ? C18 C19 1.540(6) . ? C18 P2 1.856(5) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.527(7) . ? C21 C22 1.531(7) . ? C21 P2 1.850(5) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O1 1.256(5) . ? C24 O2 1.280(6) . ? C24 O3 1.310(5) . ? C24 Ir1 2.620(4) . ? C25 C26 1.389(6) . ? C25 C29 1.401(6) . ? C25 Ir2 2.002(4) . ? C26 F5 1.352(6) . ? C26 C27 1.385(7) . ? C27 N1 1.311(8) . ? C27 F6 1.342(6) . ? C28 N1 1.306(8) . ? C28 F7 1.339(6) . ? C28 C29 1.389(7) . ? C29 F8 1.349(6) . ? C30 C32 1.518(8) . ? C30 C31 1.534(7) . ? C30 P3 1.855(5) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.530(7) . ? C33 C35 1.536(8) . ? C33 P3 1.854(5) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.532(7) . ? C36 C37 1.539(6) . ? C36 P3 1.852(5) . ? C36 H36 1.0000 . ? 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 C41 1.527(6) . ? C39 C40 1.539(7) . ? C39 P4 1.855(4) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.526(7) . ? C42 C43 1.528(7) . ? C42 P4 1.850(5) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.531(6) . ? C45 C46 1.536(6) . ? C45 P4 1.858(4) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 O4 1.266(5) . ? C48 O5 1.275(5) . ? C48 O6 1.316(5) . ? C48 Ir2 2.625(4) . ? C49 C50 1.503(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.389(8) . ? C50 C51 1.389(8) . ? C51 C52 1.387(7) . ? C51 H51 0.9500 . ? C52 C53 1.389(8) . ? C52 H52 0.9500 . ? C53 C54 1.378(8) . ? C53 H53 0.9500 . ? C54 C55 1.392(7) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.422(14) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.310(11) . ? C57 C62 1.448(12) . ? C58 C59 1.442(14) . ? C58 H58 0.9500 . ? C59 C60 1.398(14) . ? C59 H59 0.9500 . ? C60 C61 1.351(13) . ? C60 H60 0.9500 . ? C61 C62 1.305(13) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.47(3) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.381(13) . ? C64 C69 1.382(13) . ? C65 C66 1.387(14) . ? C65 H65 0.9500 . ? C66 C67 1.377(14) . ? C66 H66 0.9500 . ? C67 C68 1.374(15) . ? C67 H67 0.9500 . ? C68 C69 1.377(14) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? Ir1 O1 2.163(3) . ? Ir1 P1 2.3546(10) . ? Ir1 P2 2.3598(10) . ? Ir1 O2 2.366(3) . ? Ir1 H1 1.3802 . ? Ir2 O4 2.189(3) . ? Ir2 O5 2.337(3) . ? Ir2 P4 2.3502(10) . ? Ir2 P3 2.3513(10) . ? Ir2 H2 1.3801 . ? O3 H3 0.8400 . ? O6 H6A 0.8400 . ? 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 C5 C1 C2 111.4(4) . . ? C5 C1 Ir1 128.4(4) . . ? C2 C1 Ir1 120.2(4) . . ? F1 C2 C3 117.2(5) . . ? F1 C2 C1 120.4(4) . . ? C3 C2 C1 122.3(5) . . ? N2 C3 F2 116.1(5) . . ? N2 C3 C2 124.6(6) . . ? F2 C3 C2 119.3(6) . . ? N2 C4 F3 115.4(5) . . ? N2 C4 C5 125.2(6) . . ? F3 C4 C5 119.4(6) . . ? F4 C5 C4 116.1(5) . . ? F4 C5 C1 121.3(4) . . ? C4 C5 C1 122.5(5) . . ? C8 C6 C7 109.5(4) . . ? C8 C6 P1 116.7(3) . . ? C7 C6 P1 113.7(3) . . ? C8 C6 H6 105.3 . . ? C7 C6 H6 105.3 . . ? P1 C6 H6 105.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 109.7(4) . . ? C11 C9 P1 115.2(3) . . ? C10 C9 P1 113.9(3) . . ? C11 C9 H9 105.7 . . ? C10 C9 H9 105.7 . . ? P1 C9 H9 105.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 110.0(5) . . ? C13 C12 P1 113.2(3) . . ? C14 C12 P1 112.9(3) . . ? C13 C12 H12 106.7 . . ? C14 C12 H12 106.7 . . ? P1 C12 H12 106.7 . . ? 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 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.3(4) . . ? C17 C15 P2 113.0(4) . . ? C16 C15 P2 116.5(3) . . ? C17 C15 H10 105.7 . . ? C16 C15 H10 105.7 . . ? P2 C15 H10 105.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 110.2(4) . . ? C20 C18 P2 114.1(4) . . ? C19 C18 P2 115.3(3) . . ? C20 C18 H18 105.4 . . ? C19 C18 H18 105.4 . . ? P2 C18 H18 105.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 110.2(5) . . ? C23 C21 P2 112.1(3) . . ? C22 C21 P2 112.3(3) . . ? C23 C21 H21 107.3 . . ? C22 C21 H21 107.3 . . ? P2 C21 H21 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 O2 119.4(4) . . ? O1 C24 O3 118.3(4) . . ? O2 C24 O3 122.3(4) . . ? O1 C24 Ir1 55.1(2) . . ? O2 C24 Ir1 64.4(2) . . ? O3 C24 Ir1 172.1(3) . . ? C26 C25 C29 111.5(4) . . ? C26 C25 Ir2 127.4(4) . . ? C29 C25 Ir2 121.0(3) . . ? F5 C26 C27 116.6(4) . . ? F5 C26 C25 121.1(4) . . ? C27 C26 C25 122.2(5) . . ? N1 C27 F6 116.2(5) . . ? N1 C27 C26 124.8(5) . . ? F6 C27 C26 119.0(5) . . ? N1 C28 F7 116.5(5) . . ? N1 C28 C29 124.6(5) . . ? F7 C28 C29 118.9(5) . . ? F8 C29 C28 117.3(5) . . ? F8 C29 C25 120.5(4) . . ? C28 C29 C25 122.1(5) . . ? C32 C30 C31 110.2(5) . . ? C32 C30 P3 111.4(3) . . ? C31 C30 P3 113.1(4) . . ? C32 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? P3 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 110.6(4) . . ? C34 C33 P3 115.5(4) . . ? C35 C33 P3 114.0(4) . . ? C34 C33 H33 105.2 . . ? C35 C33 H33 105.2 . . ? P3 C33 H33 105.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 109.2(4) . . ? C38 C36 P3 113.3(4) . . ? C37 C36 P3 116.7(3) . . ? C38 C36 H36 105.6 . . ? C37 C36 H36 105.6 . . ? P3 C36 H36 105.6 . . ? 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 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 110.6(4) . . ? C41 C39 P4 116.8(4) . . ? C40 C39 P4 111.9(3) . . ? C41 C39 H39 105.5 . . ? C40 C39 H39 105.5 . . ? P4 C39 H39 105.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 110.2(5) . . ? C44 C42 P4 115.0(4) . . ? C43 C42 P4 111.1(3) . . ? C44 C42 H42 106.7 . . ? C43 C42 H42 106.7 . . ? P4 C42 H42 106.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C46 108.6(4) . . ? C47 C45 P4 115.4(3) . . ? C46 C45 P4 113.6(3) . . ? C47 C45 H45 106.2 . . ? C46 C45 H45 106.2 . . ? P4 C45 H45 106.2 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 O5 118.9(4) . . ? O4 C48 O6 118.4(4) . . ? O5 C48 O6 122.7(4) . . ? O4 C48 Ir2 56.2(2) . . ? O5 C48 Ir2 62.8(2) . . ? O6 C48 Ir2 173.9(3) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 118.3(5) . . ? C55 C50 C49 120.8(5) . . ? C51 C50 C49 120.9(5) . . ? C52 C51 C50 121.4(5) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C53 119.6(5) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C54 C53 C52 119.7(5) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 120.3(5) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C50 C55 C54 120.7(5) . . ? C50 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C56 124.0(9) . . ? C58 C57 C62 123.6(9) . . ? C56 C57 C62 112.4(9) . . ? C57 C58 C59 120.9(9) . . ? C57 C58 H58 119.5 . . ? C59 C58 H58 119.5 . . ? C60 C59 C58 114.5(11) . . ? C60 C59 H59 122.8 . . ? C58 C59 H59 122.8 . . ? C61 C60 C59 120.8(11) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C62 C61 C60 126.8(10) . . ? C62 C61 H61 116.6 . . ? C60 C61 H61 116.6 . . ? C61 C62 C57 113.3(10) . . ? C61 C62 H62 123.3 . . ? C57 C62 H62 123.3 . . ? C65 C64 C69 116.8(13) . . ? C65 C64 C63 121.5(11) . . ? C69 C64 C63 121.8(11) . . ? C64 C65 C66 122.6(15) . . ? C64 C65 H65 118.7 . . ? C66 C65 H65 118.7 . . ? C67 C66 C65 119.6(15) . . ? C67 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C68 C67 C66 118.4(17) . . ? C68 C67 H67 120.8 . . ? C66 C67 H67 120.8 . . ? C67 C68 C69 121.6(15) . . ? C67 C68 H68 119.2 . . ? C69 C68 H68 119.2 . . ? C68 C69 C64 121.0(14) . . ? C68 C69 H69 119.5 . . ? C64 C69 H69 119.5 . . ? C1 Ir1 O1 168.63(17) . . ? C1 Ir1 P1 93.08(12) . . ? O1 Ir1 P1 88.29(9) . . ? C1 Ir1 P2 91.75(12) . . ? O1 Ir1 P2 89.65(8) . . ? P1 Ir1 P2 165.58(4) . . ? C1 Ir1 O2 111.04(16) . . ? O1 Ir1 O2 57.60(11) . . ? P1 Ir1 O2 94.71(8) . . ? P2 Ir1 O2 96.22(8) . . ? C1 Ir1 C24 140.20(17) . . ? O1 Ir1 C24 28.44(13) . . ? P1 Ir1 C24 90.58(9) . . ? P2 Ir1 C24 94.38(9) . . ? O2 Ir1 C24 29.19(12) . . ? C1 Ir1 H1 69.0 . . ? O1 Ir1 H1 122.4 . . ? P1 Ir1 H1 85.3 . . ? P2 Ir1 H1 83.8 . . ? O2 Ir1 H1 180.0 . . ? C24 Ir1 H1 150.8 . . ? C25 Ir2 O4 169.36(15) . . ? C25 Ir2 O5 111.71(15) . . ? O4 Ir2 O5 57.73(11) . . ? C25 Ir2 P4 91.43(12) . . ? O4 Ir2 P4 88.24(9) . . ? O5 Ir2 P4 93.79(8) . . ? C25 Ir2 P3 94.03(12) . . ? O4 Ir2 P3 88.81(9) . . ? O5 Ir2 P3 96.48(8) . . ? P4 Ir2 P3 165.66(4) . . ? C25 Ir2 C48 140.69(16) . . ? O4 Ir2 C48 28.71(13) . . ? O5 Ir2 C48 29.04(12) . . ? P4 Ir2 C48 90.32(9) . . ? P3 Ir2 C48 93.81(9) . . ? C25 Ir2 H2 68.3 . . ? O4 Ir2 H2 122.3 . . ? O5 Ir2 H2 180.0 . . ? P4 Ir2 H2 86.2 . . ? P3 Ir2 H2 83.5 . . ? C48 Ir2 H2 151.0 . . ? C28 N1 C27 114.8(5) . . ? C4 N2 C3 114.0(5) . . ? C24 O1 Ir1 96.4(3) . . ? C24 O2 Ir1 86.5(2) . . ? C24 O3 H3 109.5 . . ? C48 O4 Ir2 95.1(3) . . ? C48 O5 Ir2 88.1(2) . . ? C48 O6 H6A 109.5 . . ? C12 P1 C9 101.6(2) . . ? C12 P1 C6 102.3(2) . . ? C9 P1 C6 110.7(2) . . ? C12 P1 Ir1 119.97(15) . . ? C9 P1 Ir1 110.02(15) . . ? C6 P1 Ir1 111.62(14) . . ? C21 P2 C15 102.2(2) . . ? C21 P2 C18 103.1(2) . . ? C15 P2 C18 109.6(2) . . ? C21 P2 Ir1 119.35(15) . . ? C15 P2 Ir1 112.09(15) . . ? C18 P2 Ir1 109.83(14) . . ? C36 P3 C33 110.7(2) . . ? C36 P3 C30 103.0(2) . . ? C33 P3 C30 102.6(2) . . ? C36 P3 Ir2 111.81(15) . . ? C33 P3 Ir2 108.83(16) . . ? C30 P3 Ir2 119.45(15) . . ? C42 P4 C39 104.7(2) . . ? C42 P4 C45 101.2(2) . . ? C39 P4 C45 108.8(2) . . ? C42 P4 Ir2 110.94(15) . . ? C39 P4 Ir2 112.59(15) . . ? C45 P4 Ir2 117.30(14) . . ? 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 C5 C1 C2 F1 -179.8(4) . . . . ? Ir1 C1 C2 F1 -0.7(6) . . . . ? C5 C1 C2 C3 -3.0(6) . . . . ? Ir1 C1 C2 C3 176.0(4) . . . . ? F1 C2 C3 N2 178.2(4) . . . . ? C1 C2 C3 N2 1.4(8) . . . . ? F1 C2 C3 F2 -2.0(7) . . . . ? C1 C2 C3 F2 -178.9(4) . . . . ? N2 C4 C5 F4 179.1(4) . . . . ? F3 C4 C5 F4 -1.8(6) . . . . ? N2 C4 C5 C1 -2.4(8) . . . . ? F3 C4 C5 C1 176.6(4) . . . . ? C2 C1 C5 F4 -178.1(4) . . . . ? Ir1 C1 C5 F4 3.0(6) . . . . ? C2 C1 C5 C4 3.5(6) . . . . ? Ir1 C1 C5 C4 -175.4(4) . . . . ? C29 C25 C26 F5 179.5(4) . . . . ? Ir2 C25 C26 F5 2.7(6) . . . . ? C29 C25 C26 C27 1.8(6) . . . . ? Ir2 C25 C26 C27 -174.9(3) . . . . ? F5 C26 C27 N1 180.0(4) . . . . ? C25 C26 C27 N1 -2.2(7) . . . . ? F5 C26 C27 F6 0.6(6) . . . . ? C25 C26 C27 F6 178.4(4) . . . . ? N1 C28 C29 F8 175.6(4) . . . . ? F7 C28 C29 F8 -2.7(6) . . . . ? N1 C28 C29 C25 -1.4(7) . . . . ? F7 C28 C29 C25 -179.6(4) . . . . ? C26 C25 C29 F8 -177.0(4) . . . . ? Ir2 C25 C29 F8 -0.0(5) . . . . ? C26 C25 C29 C28 -0.2(6) . . . . ? Ir2 C25 C29 C28 176.8(3) . . . . ? C55 C50 C51 C52 1.2(8) . . . . ? C49 C50 C51 C52 -178.6(5) . . . . ? C50 C51 C52 C53 -0.9(8) . . . . ? C51 C52 C53 C54 0.3(8) . . . . ? C52 C53 C54 C55 -0.1(9) . . . . ? C51 C50 C55 C54 -1.0(8) . . . . ? C49 C50 C55 C54 178.9(5) . . . . ? C53 C54 C55 C50 0.4(9) . . . . ? C56 C57 C58 C59 176.1(10) . . . . ? C62 C57 C58 C59 -2.0(14) . . . . ? C57 C58 C59 C60 2.5(14) . . . . ? C58 C59 C60 C61 -1.6(15) . . . . ? C59 C60 C61 C62 0.0(17) . . . . ? C60 C61 C62 C57 0.7(15) . . . . ? C58 C57 C62 C61 0.4(13) . . . . ? C56 C57 C62 C61 -177.9(9) . . . . ? C69 C64 C65 C66 -1(3) . . . . ? C63 C64 C65 C66 179.7(15) . . . . ? C64 C65 C66 C67 1(3) . . . . ? C65 C66 C67 C68 -2(3) . . . . ? C66 C67 C68 C69 2(3) . . . . ? C67 C68 C69 C64 -1(3) . . . . ? C65 C64 C69 C68 1(3) . . . . ? C63 C64 C69 C68 -179.7(18) . . . . ? C5 C1 Ir1 O1 177.2(5) . . . . ? C2 C1 Ir1 O1 -1.6(10) . . . . ? C5 C1 Ir1 P1 -86.1(4) . . . . ? C2 C1 Ir1 P1 95.0(3) . . . . ? C5 C1 Ir1 P2 80.3(4) . . . . ? C2 C1 Ir1 P2 -98.6(3) . . . . ? C5 C1 Ir1 O2 177.6(4) . . . . ? C2 C1 Ir1 O2 -1.2(4) . . . . ? C5 C1 Ir1 C24 179.2(3) . . . . ? C2 C1 Ir1 C24 0.4(5) . . . . ? O1 C24 Ir1 C1 -179.2(3) . . . . ? O2 C24 Ir1 C1 -3.1(3) . . . . ? O3 C24 Ir1 C1 145(2) . . . . ? O2 C24 Ir1 O1 176.0(4) . . . . ? O3 C24 Ir1 O1 -36(2) . . . . ? O1 C24 Ir1 P1 85.3(2) . . . . ? O2 C24 Ir1 P1 -98.6(2) . . . . ? O3 C24 Ir1 P1 49(2) . . . . ? O1 C24 Ir1 P2 -81.1(2) . . . . ? O2 C24 Ir1 P2 94.9(2) . . . . ? O3 C24 Ir1 P2 -117(2) . . . . ? O1 C24 Ir1 O2 -176.0(4) . . . . ? O3 C24 Ir1 O2 148(2) . . . . ? C26 C25 Ir2 O4 165.4(6) . . . . ? C29 C25 Ir2 O4 -11.1(10) . . . . ? C26 C25 Ir2 O5 172.0(3) . . . . ? C29 C25 Ir2 O5 -4.5(4) . . . . ? C26 C25 Ir2 P4 77.4(4) . . . . ? C29 C25 Ir2 P4 -99.1(3) . . . . ? C26 C25 Ir2 P3 -89.4(4) . . . . ? C29 C25 Ir2 P3 94.1(3) . . . . ? C26 C25 Ir2 C48 169.6(3) . . . . ? C29 C25 Ir2 C48 -6.9(5) . . . . ? O4 C48 Ir2 C25 -178.4(3) . . . . ? O5 C48 Ir2 C25 4.6(4) . . . . ? O6 C48 Ir2 C25 -151(3) . . . . ? O5 C48 Ir2 O4 -177.0(4) . . . . ? O6 C48 Ir2 O4 27(3) . . . . ? O4 C48 Ir2 O5 177.0(4) . . . . ? O6 C48 Ir2 O5 -156(3) . . . . ? O4 C48 Ir2 P4 -85.7(2) . . . . ? O5 C48 Ir2 P4 97.3(2) . . . . ? O6 C48 Ir2 P4 -59(3) . . . . ? O4 C48 Ir2 P3 80.5(2) . . . . ? O5 C48 Ir2 P3 -96.5(2) . . . . ? O6 C48 Ir2 P3 108(3) . . . . ? F7 C28 N1 C27 179.4(4) . . . . ? C29 C28 N1 C27 1.1(7) . . . . ? F6 C27 N1 C28 -180.0(4) . . . . ? C26 C27 N1 C28 0.6(7) . . . . ? F3 C4 N2 C3 -178.7(4) . . . . ? C5 C4 N2 C3 0.4(7) . . . . ? F2 C3 N2 C4 -179.6(4) . . . . ? C2 C3 N2 C4 0.1(8) . . . . ? O2 C24 O1 Ir1 -4.1(4) . . . . ? O3 C24 O1 Ir1 174.7(3) . . . . ? C1 Ir1 O1 C24 2.7(8) . . . . ? P1 Ir1 O1 C24 -94.4(2) . . . . ? P2 Ir1 O1 C24 99.9(2) . . . . ? O2 Ir1 O1 C24 2.3(2) . . . . ? O1 C24 O2 Ir1 3.7(4) . . . . ? O3 C24 O2 Ir1 -175.0(4) . . . . ? C1 Ir1 O2 C24 177.9(2) . . . . ? O1 Ir1 O2 C24 -2.2(2) . . . . ? P1 Ir1 O2 C24 82.7(2) . . . . ? P2 Ir1 O2 C24 -87.9(2) . . . . ? O5 C48 O4 Ir2 3.0(4) . . . . ? O6 C48 O4 Ir2 -176.8(3) . . . . ? C25 Ir2 O4 C48 5.5(9) . . . . ? O5 Ir2 O4 C48 -1.7(2) . . . . ? P4 Ir2 O4 C48 93.9(2) . . . . ? P3 Ir2 O4 C48 -100.1(2) . . . . ? O4 C48 O5 Ir2 -2.8(4) . . . . ? O6 C48 O5 Ir2 177.0(4) . . . . ? C25 Ir2 O5 C48 -176.9(2) . . . . ? O4 Ir2 O5 C48 1.7(2) . . . . ? P4 Ir2 O5 C48 -83.8(2) . . . . ? P3 Ir2 O5 C48 86.2(2) . . . . ? C13 C12 P1 C9 -176.1(4) . . . . ? C14 C12 P1 C9 58.0(4) . . . . ? C13 C12 P1 C6 -61.7(4) . . . . ? C14 C12 P1 C6 172.5(4) . . . . ? C13 C12 P1 Ir1 62.4(4) . . . . ? C14 C12 P1 Ir1 -63.4(4) . . . . ? C11 C9 P1 C12 47.4(4) . . . . ? C10 C9 P1 C12 175.4(3) . . . . ? C11 C9 P1 C6 -60.6(4) . . . . ? C10 C9 P1 C6 67.4(4) . . . . ? C11 C9 P1 Ir1 175.6(3) . . . . ? C10 C9 P1 Ir1 -56.4(4) . . . . ? C8 C6 P1 C12 -35.2(5) . . . . ? C7 C6 P1 C12 -164.1(4) . . . . ? C8 C6 P1 C9 72.4(5) . . . . ? C7 C6 P1 C9 -56.5(4) . . . . ? C8 C6 P1 Ir1 -164.7(4) . . . . ? C7 C6 P1 Ir1 66.4(4) . . . . ? C1 Ir1 P1 C12 -71.6(2) . . . . ? O1 Ir1 P1 C12 97.1(2) . . . . ? P2 Ir1 P1 C12 179.0(2) . . . . ? O2 Ir1 P1 C12 39.8(2) . . . . ? C24 Ir1 P1 C12 68.8(2) . . . . ? C1 Ir1 P1 C9 171.2(2) . . . . ? O1 Ir1 P1 C9 -20.12(18) . . . . ? P2 Ir1 P1 C9 61.8(2) . . . . ? O2 Ir1 P1 C9 -77.40(18) . . . . ? C24 Ir1 P1 C9 -48.47(19) . . . . ? C1 Ir1 P1 C6 47.9(2) . . . . ? O1 Ir1 P1 C6 -143.4(2) . . . . ? P2 Ir1 P1 C6 -61.5(2) . . . . ? O2 Ir1 P1 C6 159.33(19) . . . . ? C24 Ir1 P1 C6 -171.7(2) . . . . ? C23 C21 P2 C15 -170.1(4) . . . . ? C22 C21 P2 C15 65.2(4) . . . . ? C23 C21 P2 C18 -56.3(4) . . . . ? C22 C21 P2 C18 179.0(3) . . . . ? C23 C21 P2 Ir1 65.7(4) . . . . ? C22 C21 P2 Ir1 -59.1(4) . . . . ? C17 C15 P2 C21 162.0(4) . . . . ? C16 C15 P2 C21 34.2(4) . . . . ? C17 C15 P2 C18 53.2(4) . . . . ? C16 C15 P2 C18 -74.6(4) . . . . ? C17 C15 P2 Ir1 -69.0(4) . . . . ? C16 C15 P2 Ir1 163.2(3) . . . . ? C20 C18 P2 C21 -180.0(3) . . . . ? C19 C18 P2 C21 -51.0(4) . . . . ? C20 C18 P2 C15 -71.7(4) . . . . ? C19 C18 P2 C15 57.3(5) . . . . ? C20 C18 P2 Ir1 51.8(4) . . . . ? C19 C18 P2 Ir1 -179.2(4) . . . . ? C1 Ir1 P2 C21 71.7(2) . . . . ? O1 Ir1 P2 C21 -97.0(2) . . . . ? P1 Ir1 P2 C21 -178.7(2) . . . . ? O2 Ir1 P2 C21 -39.7(2) . . . . ? C24 Ir1 P2 C21 -68.9(2) . . . . ? C1 Ir1 P2 C15 -47.6(2) . . . . ? O1 Ir1 P2 C15 143.6(2) . . . . ? P1 Ir1 P2 C15 61.9(3) . . . . ? O2 Ir1 P2 C15 -159.0(2) . . . . ? C24 Ir1 P2 C15 171.7(2) . . . . ? C1 Ir1 P2 C18 -169.7(2) . . . . ? O1 Ir1 P2 C18 21.58(19) . . . . ? P1 Ir1 P2 C18 -60.2(2) . . . . ? O2 Ir1 P2 C18 78.91(19) . . . . ? C24 Ir1 P2 C18 49.6(2) . . . . ? C38 C36 P3 C33 -51.3(4) . . . . ? C37 C36 P3 C33 76.8(5) . . . . ? C38 C36 P3 C30 -160.3(4) . . . . ? C37 C36 P3 C30 -32.2(5) . . . . ? C38 C36 P3 Ir2 70.2(4) . . . . ? C37 C36 P3 Ir2 -161.7(4) . . . . ? C34 C33 P3 C36 -57.3(5) . . . . ? C35 C33 P3 C36 72.3(4) . . . . ? C34 C33 P3 C30 52.0(5) . . . . ? C35 C33 P3 C30 -178.4(4) . . . . ? C34 C33 P3 Ir2 179.4(4) . . . . ? C35 C33 P3 Ir2 -50.9(4) . . . . ? C32 C30 P3 C36 -66.4(4) . . . . ? C31 C30 P3 C36 168.8(4) . . . . ? C32 C30 P3 C33 178.6(4) . . . . ? C31 C30 P3 C33 53.8(4) . . . . ? C32 C30 P3 Ir2 58.2(4) . . . . ? C31 C30 P3 Ir2 -66.5(4) . . . . ? C25 Ir2 P3 C36 39.9(2) . . . . ? O4 Ir2 P3 C36 -150.3(2) . . . . ? O5 Ir2 P3 C36 152.3(2) . . . . ? P4 Ir2 P3 C36 -72.2(3) . . . . ? C48 Ir2 P3 C36 -178.6(2) . . . . ? C25 Ir2 P3 C33 162.5(2) . . . . ? O4 Ir2 P3 C33 -27.8(2) . . . . ? O5 Ir2 P3 C33 -85.1(2) . . . . ? P4 Ir2 P3 C33 50.3(3) . . . . ? C48 Ir2 P3 C33 -56.1(2) . . . . ? C25 Ir2 P3 C30 -80.3(2) . . . . ? O4 Ir2 P3 C30 89.4(2) . . . . ? O5 Ir2 P3 C30 32.1(2) . . . . ? P4 Ir2 P3 C30 167.5(2) . . . . ? C48 Ir2 P3 C30 61.1(2) . . . . ? C44 C42 P4 C39 56.4(4) . . . . ? C43 C42 P4 C39 -177.5(3) . . . . ? C44 C42 P4 C45 169.5(4) . . . . ? C43 C42 P4 C45 -64.4(4) . . . . ? C44 C42 P4 Ir2 -65.3(4) . . . . ? C43 C42 P4 Ir2 60.8(4) . . . . ? C41 C39 P4 C42 47.8(4) . . . . ? C40 C39 P4 C42 176.6(3) . . . . ? C41 C39 P4 C45 -59.8(4) . . . . ? C40 C39 P4 C45 69.1(4) . . . . ? C41 C39 P4 Ir2 168.4(3) . . . . ? C40 C39 P4 Ir2 -62.8(4) . . . . ? C47 C45 P4 C42 -35.7(4) . . . . ? C46 C45 P4 C42 -162.0(3) . . . . ? C47 C45 P4 C39 74.2(4) . . . . ? C46 C45 P4 C39 -52.1(4) . . . . ? C47 C45 P4 Ir2 -156.5(3) . . . . ? C46 C45 P4 Ir2 77.2(3) . . . . ? C25 Ir2 P4 C42 -131.1(2) . . . . ? O4 Ir2 P4 C42 59.6(2) . . . . ? O5 Ir2 P4 C42 117.1(2) . . . . ? P3 Ir2 P4 C42 -18.6(3) . . . . ? C48 Ir2 P4 C42 88.2(2) . . . . ? C25 Ir2 P4 C39 112.0(2) . . . . ? O4 Ir2 P4 C39 -57.4(2) . . . . ? O5 Ir2 P4 C39 0.1(2) . . . . ? P3 Ir2 P4 C39 -135.6(2) . . . . ? C48 Ir2 P4 C39 -28.7(2) . . . . ? C25 Ir2 P4 C45 -15.5(2) . . . . ? O4 Ir2 P4 C45 175.15(19) . . . . ? O5 Ir2 P4 C45 -127.35(18) . . . . ? P3 Ir2 P4 C45 96.9(2) . . . . ? C48 Ir2 P4 C45 -156.21(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.844 _refine_diff_density_min -2.047 _refine_diff_density_rms 0.148