#Copyright The Royal Society of Chemistry, 1998 data_96111 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H16 F8 P2' _chemical_formula_weight 542.33 _chemical_melting_point ? _chemical_compound_source ? 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' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.372(1) _cell_length_b 9.458(1) _cell_length_c 9.846(1) _cell_angle_alpha 117.15(1) _cell_angle_beta 93.32(1) _cell_angle_gamma 98.07(1) _cell_volume 598.99(12) _cell_formula_units_Z 1 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method none _exptl_crystal_F_000 274 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method 'omega scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 2254 _diffrn_reflns_av_R_equivalents 0.0073 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 23.99 _reflns_number_total 1780 _reflns_number_observed 1566 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS (Fait,1991)' _computing_cell_refinement 'XSCANS (Fait,1991)' _computing_data_reduction 'XSCANS (Fait,1991)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics 'SHELXtl/pc (Sheldrick, 1990)' _computing_publication_material 'SHELXtl/pc (Sheldrick, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.3288P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1780 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_obs 0.0474 _refine_ls_wR_factor_all 0.1261 _refine_ls_wR_factor_obs 0.1209 _refine_ls_goodness_of_fit_all 1.175 _refine_ls_goodness_of_fit_obs 1.208 _refine_ls_restrained_S_all 1.175 _refine_ls_restrained_S_obs 1.208 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P -0.27361(11) -0.03553(9) 0.07063(8) 0.0536(3) Uani 1 d . . F12 F -0.0550(3) -0.0335(3) 0.3489(2) 0.1011(8) Uani 1 d . . F16 F -0.3782(4) -0.3817(3) -0.1432(4) 0.1441(13) Uani 1 d . . F22 F -0.5979(3) -0.1087(2) 0.1942(2) 0.0812(6) Uani 1 d . . F26 F -0.0973(3) 0.3188(2) 0.3414(3) 0.1005(8) Uani 1 d . . C1 C -0.0368(5) 0.0579(3) 0.0722(3) 0.0608(8) Uani 1 d . . H1A H 0.0427 0.0707 0.1594 0.073 Uiso 1 d R . H1B H -0.0339 0.1625 0.0784 0.073 Uiso 1 d R . C11 C -0.2217(4) -0.2014(3) 0.1043(3) 0.0555(7) Uani 1 d . . C12 C -0.1235(5) -0.1853(5) 0.2353(5) 0.0772(10) Uani 1 d . . C13 C -0.0929(8) -0.3137(9) 0.2567(8) 0.140(3) Uani 1 d . . H13A H -0.0280 -0.3074 0.3472 0.168 Uiso 1 d R . C14 C -0.1611(13) -0.4664(12) 0.1408(14) 0.192(6) Uani 1 d . . H14A H -0.1457 -0.5637 0.1446 0.231 Uiso 1 d R . C15 C -0.2536(10) -0.4895(6) 0.0099(12) 0.165(4) Uani 1 d . . H15A H -0.3031 -0.5931 -0.0767 0.198 Uiso 1 d R . C16 C -0.2855(6) -0.3599(4) -0.0100(6) 0.0922(13) Uani 1 d . . C21 C -0.3423(4) 0.0957(3) 0.2572(3) 0.0485(7) Uani 1 d . . C22 C -0.5068(4) 0.0430(4) 0.2937(3) 0.0571(7) Uani 1 d . . C23 C -0.5851(5) 0.1305(4) 0.4221(4) 0.0743(10) Uani 1 d . . H23A H -0.7009 0.0876 0.4414 0.089 Uiso 1 d R . C24 C -0.4953(5) 0.2855(4) 0.5220(4) 0.0795(10) Uani 1 d . . H24A H -0.5461 0.3492 0.6135 0.095 Uiso 1 d R . C25 C -0.3326(5) 0.3475(4) 0.4932(4) 0.0774(10) Uani 1 d . . H25A H -0.2676 0.4540 0.5654 0.093 Uiso 1 d R . C26 C -0.2604(4) 0.2525(4) 0.3635(4) 0.0624(8) Uani 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 P1 0.0592(5) 0.0632(5) 0.0380(4) 0.0205(3) 0.0112(3) 0.0200(4) F12 0.1095(18) 0.136(2) 0.0607(12) 0.0445(14) -0.0040(11) 0.0438(15) F16 0.121(2) 0.0970(19) 0.104(2) -0.0364(16) 0.0105(17) -0.0102(15) F22 0.0749(12) 0.0675(12) 0.0765(12) 0.0163(10) 0.0223(10) -0.0033(10) F26 0.0910(15) 0.0658(13) 0.0998(16) 0.0043(11) 0.0419(12) -0.0089(11) C1 0.081(2) 0.0521(17) 0.0606(18) 0.0308(15) 0.0327(16) 0.0205(15) C11 0.0545(16) 0.0490(17) 0.0617(17) 0.0227(14) 0.0247(14) 0.0117(13) C12 0.084(2) 0.094(3) 0.092(3) 0.064(2) 0.045(2) 0.047(2) C13 0.161(5) 0.190(6) 0.200(6) 0.165(6) 0.124(5) 0.128(5) C14 0.203(9) 0.163(8) 0.368(15) 0.209(11) 0.215(10) 0.141(8) C15 0.147(6) 0.045(3) 0.291(10) 0.052(4) 0.146(7) 0.029(3) C16 0.079(3) 0.054(2) 0.117(3) 0.015(2) 0.050(2) 0.0106(19) C21 0.0531(16) 0.0513(16) 0.0421(14) 0.0205(12) 0.0097(12) 0.0167(13) C22 0.0584(17) 0.0530(17) 0.0507(16) 0.0172(13) 0.0091(13) 0.0082(14) C23 0.065(2) 0.087(2) 0.064(2) 0.0257(18) 0.0266(16) 0.0184(18) C24 0.077(2) 0.081(2) 0.060(2) 0.0109(18) 0.0251(17) 0.0255(19) C25 0.079(2) 0.060(2) 0.065(2) 0.0037(16) 0.0170(17) 0.0160(17) C26 0.0610(18) 0.0558(18) 0.0607(18) 0.0185(15) 0.0173(14) 0.0101(15) _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 P1 C11 1.829(3) . ? P1 C21 1.837(3) . ? P1 C1 1.839(3) . ? F12 C12 1.354(5) . ? F16 C16 1.356(6) . ? F22 C22 1.357(3) . ? F26 C26 1.353(4) . ? C1 C1 1.533(5) 2 ? C11 C12 1.375(5) . ? C11 C16 1.391(5) . ? C12 C13 1.369(6) . ? C13 C14 1.366(11) . ? C14 C15 1.331(12) . ? C15 C16 1.376(8) . ? C21 C22 1.376(4) . ? C21 C26 1.385(4) . ? C22 C23 1.371(4) . ? C23 C24 1.375(5) . ? C24 C25 1.363(5) . ? C25 C26 1.373(4) . ? 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 C11 P1 C21 100.53(12) . . ? C11 P1 C1 99.09(13) . . ? C21 P1 C1 106.07(13) . . ? C1 C1 P1 108.3(3) 2 . ? C12 C11 C16 115.2(4) . . ? C12 C11 P1 125.9(2) . . ? C16 C11 P1 118.9(3) . . ? F12 C12 C13 118.8(5) . . ? F12 C12 C11 117.6(3) . . ? C13 C12 C11 123.6(5) . . ? C14 C13 C12 118.3(7) . . ? C15 C14 C13 120.8(7) . . ? C14 C15 C16 120.6(7) . . ? F16 C16 C15 121.2(5) . . ? F16 C16 C11 117.3(4) . . ? C15 C16 C11 121.5(6) . . ? C22 C21 C26 113.0(2) . . ? C22 C21 P1 118.0(2) . . ? C26 C21 P1 128.7(2) . . ? F22 C22 C23 117.6(3) . . ? F22 C22 C21 116.9(2) . . ? C23 C22 C21 125.5(3) . . ? C22 C23 C24 117.9(3) . . ? C25 C24 C23 120.2(3) . . ? C24 C25 C26 118.9(3) . . ? F26 C26 C25 116.6(3) . . ? F26 C26 C21 118.9(2) . . ? C25 C26 C21 124.5(3) . . ? _refine_diff_density_max 0.286 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.048 #=END data_9710 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H29 Cl2 F4 Ir O P' _chemical_formula_weight 727.56 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.983(2) _cell_length_b 16.220(5) _cell_length_c 16.605(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.95(3) _cell_angle_gamma 90.00 _cell_volume 2648.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method ? _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 5.350 _exptl_absorpt_correction_type 'Blessing Acta Cryst. A, 1995, 51,33.' _exptl_absorpt_correction_T_min 0.293 _exptl_absorpt_correction_T_max 0.498 _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(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 'Siemens P4 diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 6920 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5485 _reflns_number_observed 4276 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS (Fait, 1991)' _computing_cell_refinement 'XSCANS (Fait, 1991)' _computing_data_reduction 'XSCANS (Fait, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC ver5.0 (Sheldrick, 1996)' _computing_publication_material 'SHELXTL/PC ver5.0 (Sheldrick, 1996)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 19 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+78.9000P] 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 5466 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_obs 0.0617 _refine_ls_wR_factor_all 0.1902 _refine_ls_wR_factor_obs 0.1450 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.010 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.010 _refine_ls_shift/esd_max 0.021 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ir1 Ir 0.43032(4) 0.97176(3) 0.23888(2) 0.02490(15) Uani 1 d . . P1 P 0.4513(3) 1.0452(2) 0.1209(2) 0.0233(5) Uani 1 d . . Cl1 Cl 0.6660(3) 0.9446(2) 0.2377(2) 0.0389(7) Uani 1 d . . Cl2 Cl 0.3743(4) 0.8474(2) 0.1593(2) 0.0480(8) Uani 1 d . . C1 C 0.4914(12) 0.9786(7) 0.0403(7) 0.029(2) Uani 1 d . . H1A H 0.5767(12) 0.9488(7) 0.0616(7) 0.035 Uiso 1 calc R . H1B H 0.4183(12) 0.9370(7) 0.0278(7) 0.035 Uiso 1 calc R . C3 C 0.4646(12) 0.9722(8) 0.3739(7) 0.032(2) Uani 1 d . . C3A C 0.5974(14) 0.9510(10) 0.4281(8) 0.045(3) Uani 1 d . . H3AA H 0.6531(14) 1.0009(10) 0.4388(8) 0.068 Uiso 1 calc R . H3AB H 0.6460(14) 0.9100(10) 0.4008(8) 0.068 Uiso 1 calc R . H3AC H 0.5793(14) 0.9285(10) 0.4799(8) 0.068 Uiso 1 calc R . C4 C 0.4275(11) 1.0550(7) 0.3448(6) 0.025(2) Uani 1 d . . C4A C 0.5029(14) 1.1309(9) 0.3674(8) 0.045(3) Uani 1 d . . H4AA H 0.4541(14) 1.1775(9) 0.3383(8) 0.068 Uiso 1 calc R . H4AB H 0.5935(14) 1.1266(9) 0.3525(8) 0.068 Uiso 1 calc R . H4AC H 0.5119(14) 1.1396(9) 0.4265(8) 0.068 Uiso 1 calc R . C5 C 0.2916(12) 1.0464(8) 0.2952(7) 0.034(3) Uani 1 d . . C5A C 0.2032(13) 1.1181(9) 0.2630(8) 0.041(3) Uani 1 d . . H5AA H 0.2575(13) 1.1688(9) 0.2690(8) 0.062 Uiso 1 calc R . H5AB H 0.1285(13) 1.1233(9) 0.2939(8) 0.062 Uiso 1 calc R . H5AC H 0.1661(13) 1.1092(9) 0.2051(8) 0.062 Uiso 1 calc R . C6 C 0.2501(11) 0.9634(7) 0.2969(6) 0.026(2) Uani 1 d . . C6A C 0.1153(13) 0.9254(9) 0.2620(8) 0.044(3) Uani 1 d . . H6AA H 0.1182(13) 0.8661(9) 0.2735(8) 0.066 Uiso 1 calc R . H6AB H 0.0961(13) 0.9343(9) 0.2027(8) 0.066 Uiso 1 calc R . H6AC H 0.0436(13) 0.9510(9) 0.2870(8) 0.066 Uiso 1 calc R . C7 C 0.3586(12) 0.9162(8) 0.3455(7) 0.033(3) Uani 1 d . . C7A C 0.3535(14) 0.8264(8) 0.3642(9) 0.044(3) Uani 1 d . . H7AA H 0.2674(14) 0.8032(8) 0.3361(9) 0.065 Uiso 1 calc R . H7AB H 0.3604(14) 0.8187(8) 0.4234(9) 0.065 Uiso 1 calc R . H7AC H 0.4294(14) 0.7982(8) 0.3456(9) 0.065 Uiso 1 calc R . C11 C 0.3066(11) 1.1013(7) 0.0633(7) 0.030(2) Uani 1 d . . C12 C 0.3136(12) 1.1677(7) 0.0104(7) 0.033(2) Uani 1 d . . F12 F 0.4373(7) 1.2012(4) 0.0079(4) 0.038(2) Uani 1 d . . C13 C 0.2040(14) 1.2013(8) -0.0409(8) 0.042(3) Uani 1 d . . H13A H 0.2161(14) 1.2459(8) -0.0761(8) 0.051 Uiso 1 calc R . C14 C 0.0769(12) 1.1693(8) -0.0401(8) 0.042(3) Uani 1 d . . H14A H 0.0001(12) 1.1918(8) -0.0750(8) 0.050 Uiso 1 calc R . C15 C 0.0604(13) 1.1044(9) 0.0115(8) 0.041(3) Uani 1 d . . H15A H -0.0272(13) 1.0826(9) 0.0137(8) 0.049 Uiso 1 calc R . C16 C 0.1744(12) 1.0725(8) 0.0592(7) 0.035(3) Uani 1 d . . F16 F 0.1548(8) 1.0047(5) 0.1045(5) 0.049(2) Uani 1 d . . C21 C 0.5870(11) 1.1219(7) 0.1420(6) 0.027(2) Uani 1 d . . C22 C 0.7220(11) 1.1104(7) 0.1305(7) 0.030(2) Uani 1 d . . F22 F 0.7559(6) 1.0426(4) 0.0925(4) 0.035(2) Uani 1 d . . C23 C 0.8257(12) 1.1675(8) 0.1557(7) 0.035(3) Uani 1 d . . H23A H 0.9154(12) 1.1576(8) 0.1461(7) 0.043 Uiso 1 calc R . C24 C 0.7957(12) 1.2386(8) 0.1948(8) 0.038(3) Uani 1 d . . H24A H 0.8657(12) 1.2770(8) 0.2142(8) 0.046 Uiso 1 calc R . C25 C 0.6642(12) 1.2539(7) 0.2055(7) 0.034(3) Uani 1 d . . H25A H 0.6418(12) 1.3037(7) 0.2304(7) 0.041 Uiso 1 calc R . C26 C 0.5666(11) 1.1962(7) 0.1797(6) 0.028(2) Uani 1 d . . F26 F 0.4375(7) 1.2132(4) 0.1903(4) 0.037(2) Uani 1 d . . C8 C 0.4408(16) 1.3914(11) -0.0337(11) 0.058(4) Uani 1 d . . O1 O 0.3554(15) 1.4045(9) 0.0076(8) 0.085(4) Uani 1 d . . C10 C 0.4079(20) 1.3938(18) -0.1237(12) 0.103(9) Uani 1 d . . H10A H 0.3117(20) 1.4079(18) -0.1406(12) 0.155 Uiso 1 calc R . H10B H 0.4257(20) 1.3397(18) -0.1458(12) 0.155 Uiso 1 calc R . H10C H 0.4644(20) 1.4355(18) -0.1444(12) 0.155 Uiso 1 calc R . C9 C 0.5834(18) 1.3707(15) -0.0013(15) 0.102(8) Uani 1 d . . H9A H 0.5975(18) 1.3704(15) 0.0586(15) 0.154 Uiso 1 calc R . H9B H 0.6432(18) 1.4120(15) -0.0198(15) 0.154 Uiso 1 calc R . H9C H 0.6045(18) 1.3162(15) -0.0211(15) 0.154 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0248(2) 0.0262(2) 0.0243(2) 0.0007(2) 0.0057(2) -0.0007(2) P1 0.0233(13) 0.0272(14) 0.0202(12) 0.0001(10) 0.0057(10) -0.0024(11) Cl1 0.0313(14) 0.046(2) 0.042(2) 0.0122(14) 0.0138(12) 0.0163(13) Cl2 0.075(2) 0.0279(15) 0.045(2) -0.0080(13) 0.021(2) -0.013(2) C1 0.029(5) 0.025(5) 0.034(6) 0.005(5) 0.008(5) 0.002(4) C3 0.028(6) 0.046(7) 0.022(5) -0.001(5) 0.002(4) 0.000(5) C3A 0.042(7) 0.066(9) 0.026(6) 0.009(6) 0.000(5) 0.000(7) C4 0.028(5) 0.034(6) 0.016(5) -0.012(4) 0.008(4) 0.006(5) C4A 0.042(7) 0.056(9) 0.037(7) -0.010(6) 0.004(6) -0.017(7) C5 0.028(6) 0.038(7) 0.034(6) -0.001(5) 0.002(5) -0.012(5) C5A 0.030(6) 0.051(8) 0.046(7) 0.002(6) 0.015(6) 0.010(6) C6 0.024(5) 0.026(5) 0.027(5) 0.004(4) 0.004(4) -0.010(4) C6A 0.035(6) 0.056(9) 0.043(7) 0.009(6) 0.012(6) -0.001(6) C7 0.034(6) 0.044(7) 0.022(5) 0.000(5) 0.014(5) -0.001(5) C7A 0.048(8) 0.029(6) 0.056(8) 0.011(6) 0.017(6) 0.000(6) C11 0.025(5) 0.033(6) 0.030(6) -0.009(5) 0.004(4) -0.004(5) C12 0.036(6) 0.029(6) 0.033(6) -0.001(5) 0.004(5) -0.001(5) F12 0.037(4) 0.035(4) 0.041(4) 0.011(3) 0.006(3) -0.002(3) C13 0.046(7) 0.034(7) 0.043(7) 0.004(6) -0.002(6) 0.007(6) C14 0.028(6) 0.038(7) 0.052(8) 0.001(6) -0.013(6) 0.008(5) C15 0.030(6) 0.050(8) 0.040(7) -0.006(6) 0.000(5) 0.002(6) C16 0.030(6) 0.039(7) 0.035(6) 0.000(5) 0.004(5) 0.001(5) F16 0.037(4) 0.059(5) 0.047(4) 0.013(4) -0.003(3) -0.019(4) C21 0.031(6) 0.031(6) 0.021(5) 0.004(4) 0.008(4) 0.000(5) C22 0.026(5) 0.037(6) 0.027(5) -0.005(5) 0.004(4) -0.008(5) F22 0.028(3) 0.039(4) 0.041(4) -0.007(3) 0.013(3) 0.004(3) C23 0.030(6) 0.038(7) 0.038(6) 0.000(5) 0.006(5) -0.002(5) C24 0.028(6) 0.035(7) 0.049(7) -0.003(6) 0.000(5) -0.012(5) C25 0.034(6) 0.028(6) 0.039(6) -0.004(5) 0.002(5) -0.001(5) C26 0.028(5) 0.033(6) 0.024(5) 0.001(5) 0.005(4) 0.002(5) F26 0.030(3) 0.036(4) 0.046(4) -0.009(3) 0.009(3) -0.002(3) C8 0.047(9) 0.058(10) 0.068(11) 0.004(8) 0.003(8) -0.006(8) O1 0.093(10) 0.094(10) 0.075(9) 0.013(8) 0.039(8) 0.014(8) C10 0.059(12) 0.187(28) 0.065(13) 0.008(15) 0.016(10) 0.012(15) C9 0.047(10) 0.112(18) 0.133(20) 0.042(16) -0.026(12) -0.029(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C5 2.169(13) . ? Ir1 C6 2.187(10) . ? Ir1 C3 2.208(11) . ? Ir1 C7 2.213(11) . ? Ir1 C4 2.221(9) . ? Ir1 P1 2.334(3) . ? Ir1 Cl1 2.397(3) . ? Ir1 Cl2 2.423(3) . ? P1 C1 1.817(11) . ? P1 C21 1.828(12) . ? P1 C11 1.831(12) . ? C1 C1 1.54(2) 3_675 ? C3 C7 1.41(2) . ? C3 C4 1.45(2) . ? C3 C3A 1.51(2) . ? C4 C5 1.47(2) . ? C4 C4A 1.46(2) . ? C5 C6 1.41(2) . ? C5 C5A 1.50(2) . ? C6 C7 1.45(2) . ? C6 C6A 1.50(2) . ? C7 C7A 1.49(2) . ? C11 C16 1.39(2) . ? C11 C12 1.40(2) . ? C12 F12 1.356(14) . ? C12 C13 1.38(2) . ? C13 C14 1.37(2) . ? C14 C15 1.38(2) . ? C15 C16 1.37(2) . ? C16 F16 1.366(14) . ? C21 C26 1.39(2) . ? C21 C22 1.41(2) . ? C22 F22 1.340(13) . ? C22 C23 1.40(2) . ? C23 C24 1.38(2) . ? C24 C25 1.38(2) . ? C25 C26 1.37(2) . ? C26 F26 1.359(12) . ? C8 O1 1.20(2) . ? C8 C9 1.47(2) . ? C8 C10 1.47(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ir1 C6 37.8(4) . . ? C5 Ir1 C3 63.8(4) . . ? C6 Ir1 C3 63.1(4) . . ? C5 Ir1 C7 64.1(5) . . ? C6 Ir1 C7 38.5(4) . . ? C3 Ir1 C7 37.3(4) . . ? C5 Ir1 C4 39.0(4) . . ? C6 Ir1 C4 64.2(4) . . ? C3 Ir1 C4 38.3(4) . . ? C7 Ir1 C4 64.2(4) . . ? C5 Ir1 P1 103.5(3) . . ? C6 Ir1 P1 127.0(3) . . ? C3 Ir1 P1 146.1(3) . . ? C7 Ir1 P1 165.5(3) . . ? C4 Ir1 P1 111.7(3) . . ? C5 Ir1 Cl1 143.8(3) . . ? C6 Ir1 Cl1 151.1(3) . . ? C3 Ir1 Cl1 91.6(3) . . ? C7 Ir1 Cl1 112.7(3) . . ? C4 Ir1 Cl1 105.4(3) . . ? P1 Ir1 Cl1 81.73(10) . . ? C5 Ir1 Cl2 126.5(3) . . ? C6 Ir1 Cl2 93.4(3) . . ? C3 Ir1 Cl2 122.5(3) . . ? C7 Ir1 Cl2 91.2(3) . . ? C4 Ir1 Cl2 154.7(3) . . ? P1 Ir1 Cl2 90.75(11) . . ? Cl1 Ir1 Cl2 88.66(13) . . ? C1 P1 C21 107.2(5) . . ? C1 P1 C11 99.5(5) . . ? C21 P1 C11 104.7(5) . . ? C1 P1 Ir1 112.2(4) . . ? C21 P1 Ir1 110.9(3) . . ? C11 P1 Ir1 121.0(4) . . ? C1 C1 P1 116.3(10) 3_675 . ? C7 C3 C4 110.5(10) . . ? C7 C3 C3A 125.7(12) . . ? C4 C3 C3A 123.8(11) . . ? C7 C3 Ir1 71.5(6) . . ? C4 C3 Ir1 71.3(6) . . ? C3A C3 Ir1 124.9(8) . . ? C3 C4 C5 104.9(10) . . ? C3 C4 C4A 127.2(10) . . ? C5 C4 C4A 127.6(11) . . ? C3 C4 Ir1 70.4(6) . . ? C5 C4 Ir1 68.6(6) . . ? C4A C4 Ir1 129.8(8) . . ? C6 C5 C4 109.0(10) . . ? C6 C5 C5A 126.2(11) . . ? C4 C5 C5A 123.8(11) . . ? C6 C5 Ir1 71.8(7) . . ? C4 C5 Ir1 72.4(6) . . ? C5A C5 Ir1 131.2(9) . . ? C5 C6 C7 108.8(10) . . ? C5 C6 C6A 129.1(11) . . ? C7 C6 C6A 122.0(10) . . ? C5 C6 Ir1 70.4(6) . . ? C7 C6 Ir1 71.7(6) . . ? C6A C6 Ir1 127.3(8) . . ? C3 C7 C6 106.8(10) . . ? C3 C7 C7A 127.5(12) . . ? C6 C7 C7A 125.6(11) . . ? C3 C7 Ir1 71.2(6) . . ? C6 C7 Ir1 69.7(6) . . ? C7A C7 Ir1 126.3(9) . . ? C16 C11 C12 112.2(11) . . ? C16 C11 P1 121.0(9) . . ? C12 C11 P1 126.1(9) . . ? F12 C12 C13 117.0(11) . . ? F12 C12 C11 118.2(10) . . ? C13 C12 C11 124.9(12) . . ? C12 C13 C14 118.8(12) . . ? C13 C14 C15 120.1(12) . . ? C16 C15 C14 118.0(12) . . ? F16 C16 C15 116.1(11) . . ? F16 C16 C11 117.9(10) . . ? C15 C16 C11 126.0(12) . . ? C26 C21 C22 113.3(10) . . ? C26 C21 P1 121.0(8) . . ? C22 C21 P1 125.4(9) . . ? F22 C22 C23 116.8(10) . . ? F22 C22 C21 119.9(10) . . ? C23 C22 C21 123.3(11) . . ? C24 C23 C22 119.0(11) . . ? C25 C24 C23 120.0(11) . . ? C26 C25 C24 118.7(11) . . ? F26 C26 C25 117.5(10) . . ? F26 C26 C21 116.8(10) . . ? C25 C26 C21 125.7(11) . . ? O1 C8 C9 124.6(19) . . ? O1 C8 C10 121.2(16) . . ? C9 C8 C10 114.2(18) . . ? _refine_diff_density_max 4.399 _refine_diff_density_min -2.595 _refine_diff_density_rms 0.283 #=END data_fecp1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H46 Cl4 F20 Ir2 O2 P2' _chemical_formula_weight 1671.03 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.149(2) _cell_length_b 12.650(3) _cell_length_c 19.663(4) _cell_angle_alpha 86.30(2) _cell_angle_beta 79.36(2) _cell_angle_gamma 78.87(2) _cell_volume 2913.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 12.54 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .52 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method ? _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 4.906 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6313 _exptl_absorpt_correction_T_max 0.9081 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.99 _diffrn_reflns_number 10772 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10249 _reflns_number_observed 8006 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+20.6024P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10247 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_obs 0.0429 _refine_ls_wR_factor_all 0.0916 _refine_ls_wR_factor_obs 0.0827 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 1.122 _refine_ls_shift/esd_max -0.541 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ir1 Ir -0.97991(2) 0.19805(2) -0.154966(14) 0.02205(8) Uani 1 d . . P1 P -0.8875(2) 0.08924(14) -0.07643(9) 0.0197(4) Uani 1 d . . Cl2 Cl -0.9413(2) 0.0350(2) -0.21704(10) 0.0366(5) Uani 1 d . . Cl1 Cl -1.1585(2) 0.1493(2) -0.10103(11) 0.0371(5) Uani 1 d . . F12 F -0.8125(4) -0.1476(3) -0.1321(2) 0.0337(10) Uani 1 d . . F26 F -1.0298(4) 0.2678(3) 0.0110(2) 0.0346(10) Uani 1 d . . F16 F -0.6638(4) 0.1674(4) -0.1132(2) 0.0387(11) Uani 1 d . . C3 C -1.0432(7) 0.3705(6) -0.1475(4) 0.029(2) Uani 1 d . . F22 F -0.6774(4) 0.0280(4) 0.0039(2) 0.0407(12) Uani 1 d . . F14 F -0.4423(4) -0.1271(5) -0.2360(3) 0.057(2) Uani 1 d . . F15 F -0.4651(4) 0.0737(5) -0.1848(3) 0.0538(14) Uani 1 d . . F13 F -0.6181(4) -0.2335(4) -0.2068(3) 0.0537(14) Uani 1 d . . F25 F -0.9933(5) 0.3599(4) 0.1197(2) 0.0526(14) Uani 1 d . . C7 C -1.0686(7) 0.3369(6) -0.2112(4) 0.029(2) Uani 1 d . . F23 F -0.6399(5) 0.1261(5) 0.1094(3) 0.063(2) Uani 1 d . . C6 C -0.9633(7) 0.2954(6) -0.2545(4) 0.033(2) Uani 1 d . . C4 C -0.9212(7) 0.3509(6) -0.1525(4) 0.030(2) Uani 1 d . . C16 C -0.6566(6) 0.0678(6) -0.1368(4) 0.030(2) Uani 1 d . . C26 C -0.9302(7) 0.2316(6) 0.0326(4) 0.027(2) Uani 1 d . . C12 C -0.7318(6) -0.0876(6) -0.1451(4) 0.030(2) Uani 1 d . . C21 C -0.8518(6) 0.1481(5) -0.0011(3) 0.0214(15) Uani 1 d . . C22 C -0.7565(7) 0.1118(6) 0.0292(4) 0.033(2) Uani 1 d . . C5 C -0.8714(7) 0.2983(6) -0.2177(4) 0.034(2) Uani 1 d . . C11 C -0.7487(6) 0.0165(6) -0.1206(4) 0.022(2) Uani 1 d . . C15 C -0.5526(6) 0.0210(7) -0.1743(4) 0.037(2) Uani 1 d . . C14 C -0.5403(7) -0.0803(7) -0.1986(4) 0.039(2) Uani 1 d . . C25 C -0.9129(8) 0.2795(6) 0.0895(4) 0.036(2) Uani 1 d . . C13 C -0.6295(7) -0.1332(7) -0.1843(4) 0.038(2) Uani 1 d . . C4A C -0.8570(7) 0.3897(6) -0.1045(5) 0.039(2) Uani 1 d . . H4A1 H -0.9066(14) 0.4074(41) -0.0612(11) 0.058 Uiso 1 calc R . H4A2 H -0.8286(40) 0.4526(27) -0.1246(13) 0.058 Uiso 1 calc R . H4A3 H -0.7942(28) 0.3341(17) -0.0968(23) 0.058 Uiso 1 calc R . C1 C -0.9569(6) -0.0193(6) -0.0321(4) 0.026(2) Uani 1 d . . H12 H -0.9953(6) -0.0478(6) -0.0639(4) 0.032 Uiso 1 calc R . H11 H -0.8992(6) -0.0772(6) -0.0188(4) 0.032 Uiso 1 calc R . C23 C -0.7355(8) 0.1620(7) 0.0848(4) 0.039(2) Uani 1 d . . F24 F -0.7946(6) 0.2942(4) 0.1685(3) 0.065(2) Uani 1 d . . C7A C -1.1850(8) 0.3537(7) -0.2291(5) 0.050(2) Uani 1 d . . H7A1 H -1.2186(22) 0.4289(10) -0.2264(32) 0.075 Uiso 1 calc R . H7A2 H -1.2314(17) 0.3128(40) -0.1971(20) 0.075 Uiso 1 calc R . H7A3 H -1.1799(9) 0.3303(47) -0.2752(13) 0.075 Uiso 1 calc R . C6A C -0.9482(9) 0.2535(8) -0.3258(4) 0.052(3) Uani 1 d . . H6A1 H -0.9114(50) 0.1792(16) -0.3262(9) 0.078 Uiso 1 calc R . H6A2 H -0.9021(45) 0.2947(34) -0.3579(7) 0.078 Uiso 1 calc R . H6A3 H -1.0213(9) 0.2598(48) -0.3392(14) 0.078 Uiso 1 calc R . O5S O -0.1918(6) -0.0175(6) -0.3854(4) 0.069(2) Uani 1 d . . C5S C -0.1913(7) -0.0027(8) -0.3262(5) 0.045(2) Uani 1 d . . C6S C -0.2109(9) 0.1078(9) -0.2978(6) 0.063(3) Uani 1 d . . H6S1 H -0.1506(34) 0.1130(21) -0.2735(33) 0.094 Uiso 1 calc R . H6S2 H -0.2825(30) 0.1207(24) -0.2666(29) 0.094 Uiso 1 calc R . H6S3 H -0.2120(62) 0.1605(9) -0.3352(6) 0.094 Uiso 1 calc R . C4S C -0.1682(8) -0.0940(9) -0.2753(6) 0.067(3) Uani 1 d . . H4S1 H -0.2304(32) -0.0883(36) -0.2369(20) 0.100 Uiso 1 calc R . H4S2 H -0.0991(37) -0.0911(37) -0.2590(31) 0.100 Uiso 1 calc R . H4S3 H -0.1602(65) -0.1613(9) -0.2974(12) 0.100 Uiso 1 calc R . C2S C -0.4738(13) -0.3345(12) 0.0108(8) 0.098(5) Uani 1 d . . C3S C -0.5235(14) -0.3395(18) 0.0833(9) 0.152(8) Uani 1 d . . H3S1 H -0.5591(118) -0.4016(71) 0.0927(19) 0.228 Uiso 1 calc R . H3S2 H -0.5794(98) -0.2756(59) 0.0947(20) 0.228 Uiso 1 calc R . H3S3 H -0.4648(26) -0.3447(133) 0.1107(9) 0.228 Uiso 1 calc R . C24 C -0.8140(9) 0.2457(7) 0.1146(4) 0.043(2) Uani 1 d . . C5A C -0.7478(7) 0.2728(7) -0.2498(4) 0.042(2) Uani 1 d . . H5A1 H -0.7335(12) 0.3197(32) -0.2895(18) 0.063 Uiso 1 calc R . H5A2 H -0.7286(13) 0.1993(16) -0.2638(27) 0.063 Uiso 1 calc R . H5A3 H -0.7022(7) 0.2832(44) -0.2167(11) 0.063 Uiso 1 calc R . C3A C -1.1320(7) 0.4282(6) -0.0914(4) 0.038(2) Uani 1 d . . H3A1 H -1.0957(9) 0.4449(39) -0.0550(14) 0.057 Uiso 1 calc R . H3A2 H -1.1859(27) 0.3827(18) -0.0731(20) 0.057 Uiso 1 calc R . H3A3 H -1.1708(33) 0.4936(23) -0.1103(8) 0.057 Uiso 1 calc R . O1S O -0.3715(9) -0.3539(9) -0.0097(6) 0.120(4) Uani 1 d . . C1S C -0.5577(18) -0.3085(21) -0.0369(10) 0.208(13) Uani 1 d . . H1S1 H -0.5996(132) -0.2365(68) -0.0293(81) 0.312 Uiso 1 calc R . H1S2 H -0.6095(121) -0.3583(114) -0.0281(81) 0.312 Uiso 1 calc R . H1S3 H -0.5183(24) -0.3139(179) -0.0839(11) 0.312 Uiso 1 calc R . Ir2 Ir -0.82310(3) -0.35766(2) -0.44018(2) 0.03833(11) Uani 1 d . . Cl3 Cl -0.7844(3) -0.5518(2) -0.44331(14) 0.0693(9) Uani 1 d . . P2 P -0.6299(2) -0.3580(2) -0.45955(14) 0.0596(9) Uani 1 d . . C57 C -0.9365(8) -0.3554(6) -0.3412(4) 0.041(2) Uani 1 d . . Cl4 Cl -0.7905(2) -0.3521(2) -0.56462(11) 0.0454(6) Uani 1 d . . C56 C -0.8897(7) -0.2597(6) -0.3501(4) 0.032(2) Uani 1 d . . C55 C -0.9233(7) -0.1999(6) -0.4093(4) 0.033(2) Uani 1 d . . C54 C -0.9956(7) -0.2594(6) -0.4362(4) 0.035(2) Uani 1 d . . C53 C -1.0041(8) -0.3544(6) -0.3955(4) 0.040(2) Uani 1 d . . C57A C -0.9318(10) -0.4383(7) -0.2833(5) 0.060(3) Uani 1 d . . H571 H -0.9170(61) -0.5090(7) -0.3018(6) 0.089 Uiso 1 calc R . H572 H -1.0033(22) -0.4276(36) -0.2519(20) 0.089 Uiso 1 calc R . H573 H -0.8720(40) -0.4314(38) -0.2590(23) 0.089 Uiso 1 calc R . C56A C -0.8316(8) -0.2217(6) -0.2974(4) 0.044(2) Uani 1 d . . H561 H -0.8870(11) -0.1978(44) -0.2573(13) 0.066 Uiso 1 calc R . H562 H -0.7951(42) -0.1631(32) -0.3171(11) 0.066 Uiso 1 calc R . H563 H -0.7755(36) -0.2799(15) -0.2842(23) 0.066 Uiso 1 calc R . C55A C -0.9068(7) -0.0895(6) -0.4346(4) 0.038(2) Uani 1 d . . H551 H -0.9791(9) -0.0413(11) -0.4284(26) 0.056 Uiso 1 calc R . H552 H -0.8736(43) -0.0910(10) -0.4829(8) 0.056 Uiso 1 calc R . H553 H -0.8571(37) -0.0650(18) -0.4089(19) 0.056 Uiso 1 calc R . C54A C -1.0556(8) -0.2228(7) -0.4964(4) 0.042(2) Uani 1 d . . H541 H -1.0061(19) -0.1900(42) -0.5317(13) 0.063 Uiso 1 calc R . H542 H -1.1235(27) -0.1713(35) -0.4811(7) 0.063 Uiso 1 calc R . H543 H -1.0755(44) -0.2837(10) -0.5147(19) 0.063 Uiso 1 calc R . C53A C -1.0702(9) -0.4392(7) -0.4022(5) 0.053(3) Uani 1 d . . H531 H -1.1270(37) -0.4418(36) -0.3614(15) 0.080 Uiso 1 calc R . H532 H -1.0198(12) -0.5077(11) -0.4075(34) 0.080 Uiso 1 calc R . H533 H -1.1066(46) -0.4228(28) -0.4420(20) 0.080 Uiso 1 calc R . C61A C -0.5338(14) -0.3469(12) -0.3976(8) 0.025(4) Uiso 0.526(8) d P 1 C62A C -0.5583(13) -0.4122(12) -0.3384(9) 0.025(3) Uiso 0.526(8) d P 1 F62A F -0.6420(9) -0.4674(7) -0.3297(5) 0.030(2) Uiso 0.526(8) d P 1 C63A C -0.4911(15) -0.4283(12) -0.2856(8) 0.029(3) Uiso 0.526(8) d P 1 F63A F -0.5188(9) -0.4892(8) -0.2297(5) 0.044(3) Uiso 0.526(8) d P 1 C64A C -0.4067(12) -0.3743(12) -0.2913(9) 0.020(3) Uiso 0.526(8) d P 1 F64A F -0.3423(8) -0.3842(7) -0.2401(5) 0.040(2) Uiso 0.526(8) d P 1 C65A C -0.3784(15) -0.3096(14) -0.3501(9) 0.033(4) Uiso 0.526(8) d P 1 F65A F -0.2905(8) -0.2600(7) -0.3544(5) 0.037(2) Uiso 0.526(8) d P 1 C66A C -0.4401(13) -0.3004(12) -0.4004(10) 0.019(3) Uiso 0.526(8) d P 1 F66A F -0.4055(8) -0.2402(8) -0.4573(5) 0.036(2) Uiso 0.526(8) d P 1 C61B C -0.5637(14) -0.3746(14) -0.3782(10) 0.022(4) Uiso 0.474(8) d P 2 C62B C -0.6003(18) -0.4350(15) -0.3171(10) 0.030(4) Uiso 0.474(8) d P 2 F62B F -0.6927(10) -0.4819(8) -0.3117(6) 0.036(3) Uiso 0.474(8) d P 2 F63B F -0.5818(11) -0.5062(9) -0.2065(6) 0.056(3) Uiso 0.474(8) d P 2 C63B C -0.5425(17) -0.4477(15) -0.2640(11) 0.037(4) Uiso 0.474(8) d P 2 F64B F -0.3922(11) -0.4170(10) -0.2131(6) 0.056(3) Uiso 0.474(8) d P 2 C64B C -0.4481(19) -0.4049(16) -0.2684(11) 0.038(4) Uiso 0.474(8) d P 2 F65B F -0.3177(11) -0.3066(10) -0.3276(7) 0.055(3) Uiso 0.474(8) d P 2 C65B C -0.4042(16) -0.3474(17) -0.3266(12) 0.034(4) Uiso 0.474(8) d P 2 F66B F -0.4227(10) -0.2824(10) -0.4361(8) 0.042(3) Uiso 0.474(8) d P 2 C66B C -0.4688(17) -0.3337(16) -0.3803(10) 0.034(4) Uiso 0.474(8) d P 2 C73B C -0.6170(19) -0.0164(24) -0.5139(12) 0.038(6) Uiso 0.474(8) d P 2 F73B F -0.6523(14) 0.0583(13) -0.4698(9) 0.050(5) Uiso 0.474(8) d P 2 C74B C -0.5802(18) -0.0134(20) -0.5793(12) 0.045(5) Uiso 0.474(8) d P 2 F74B F -0.5694(10) 0.0752(11) -0.6126(6) 0.053(3) Uiso 0.474(8) d P 2 C75B C -0.5501(13) -0.1056(16) -0.6171(9) 0.021(4) Uiso 0.474(8) d P 2 F75B F -0.5083(9) -0.1044(10) -0.6855(5) 0.045(3) Uiso 0.474(8) d P 2 C76B C -0.5536(15) -0.2063(18) -0.5877(10) 0.029(4) Uiso 0.474(8) d P 2 F76B F -0.5255(8) -0.2929(8) -0.6264(5) 0.033(2) Uiso 0.474(8) d P 2 C71B C -0.5986(9) -0.2348(8) -0.5110(5) 0.053(2) Uiso 0.474(8) d P 2 C72B C -0.6201(19) -0.1223(22) -0.4822(13) 0.033(6) Uiso 0.474(8) d P 2 F72B F -0.6491(12) -0.1252(12) -0.4165(8) 0.040(4) Uiso 0.474(8) d P 2 C71A C -0.5986(9) -0.2348(8) -0.5110(5) 0.053(2) Uiso 0.526(8) d P 1 C72A C -0.6265(18) -0.1522(19) -0.4746(11) 0.038(7) Uiso 0.526(8) d P 1 F72A F -0.6632(11) -0.1441(10) -0.4044(7) 0.037(4) Uiso 0.526(8) d P 1 C73A C -0.6130(18) -0.0574(22) -0.5151(12) 0.044(6) Uiso 0.526(8) d P 1 F73A F -0.6382(17) 0.0432(18) -0.4882(11) 0.084(7) Uiso 0.526(8) d P 1 C74A C -0.5736(17) -0.0652(20) -0.5813(12) 0.049(5) Uiso 0.526(8) d P 1 F74A F -0.5526(13) 0.0209(14) -0.6257(9) 0.092(5) Uiso 0.526(8) d P 1 C75A C -0.5440(15) -0.1593(20) -0.6155(11) 0.041(4) Uiso 0.526(8) d P 1 F75A F -0.5038(11) -0.1723(12) -0.6833(7) 0.076(4) Uiso 0.526(8) d P 1 C76A C -0.5631(15) -0.2565(16) -0.5770(9) 0.038(4) Uiso 0.526(8) d P 1 F76A F -0.5371(8) -0.3513(9) -0.6124(5) 0.046(3) Uiso 0.526(8) d P 1 C51A C -0.5192(12) -0.4502(11) -0.5207(7) 0.027(3) Uiso 0.526(8) d P 1 H52A H -0.5521(12) -0.4684(11) -0.5588(7) 0.033 Uiso 0.526(8) calc PR 1 H51A H -0.4553(12) -0.4152(11) -0.5395(7) 0.033 Uiso 0.526(8) calc PR 1 C51B C -0.5644(12) -0.4941(11) -0.4935(7) 0.018(3) Uiso 0.474(8) d P 2 H52B H -0.5876(12) -0.5492(11) -0.4603(7) 0.022 Uiso 0.474(8) calc PR 2 H51B H -0.5900(12) -0.5033(11) -0.5363(7) 0.022 Uiso 0.474(8) calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0257(2) 0.0214(2) 0.01798(15) 0.00126(11) -0.00575(12) -0.00059(12) P1 0.0213(9) 0.0188(9) 0.0179(9) 0.0016(7) -0.0017(7) -0.0035(7) Cl2 0.0491(12) 0.0312(10) 0.0302(10) -0.0082(8) -0.0188(9) 0.0042(9) Cl1 0.0258(10) 0.0432(12) 0.0419(12) 0.0065(9) -0.0093(9) -0.0054(9) F12 0.038(3) 0.028(2) 0.035(3) -0.007(2) -0.006(2) -0.005(2) F26 0.039(3) 0.032(2) 0.031(2) -0.006(2) -0.006(2) 0.001(2) F16 0.036(3) 0.035(3) 0.044(3) 0.004(2) -0.005(2) -0.010(2) C3 0.033(4) 0.017(4) 0.034(4) 0.009(3) -0.003(4) -0.004(3) F22 0.038(3) 0.046(3) 0.038(3) 0.004(2) -0.018(2) 0.002(2) F14 0.025(3) 0.093(4) 0.046(3) -0.026(3) -0.001(2) 0.011(3) F15 0.027(3) 0.077(4) 0.056(3) 0.002(3) 0.000(2) -0.016(3) F13 0.049(3) 0.055(3) 0.052(3) -0.030(3) -0.009(3) 0.010(3) F25 0.085(4) 0.035(3) 0.037(3) -0.013(2) -0.013(3) -0.003(3) C7 0.035(4) 0.030(4) 0.021(4) 0.003(3) -0.009(3) -0.002(3) F23 0.066(4) 0.075(4) 0.058(4) -0.003(3) -0.048(3) -0.005(3) C6 0.046(5) 0.030(4) 0.022(4) 0.012(3) -0.009(4) -0.004(4) C4 0.045(5) 0.018(4) 0.028(4) 0.009(3) -0.007(4) -0.011(3) C16 0.029(4) 0.034(4) 0.024(4) 0.003(3) -0.006(3) -0.002(3) C26 0.038(5) 0.020(4) 0.026(4) 0.004(3) -0.008(3) -0.008(3) C12 0.029(4) 0.034(4) 0.026(4) 0.003(3) -0.009(3) 0.000(3) C21 0.028(4) 0.022(4) 0.016(3) 0.006(3) -0.002(3) -0.013(3) C22 0.038(5) 0.033(4) 0.028(4) 0.008(3) -0.009(4) -0.009(4) C5 0.038(5) 0.027(4) 0.030(4) 0.011(3) -0.001(4) -0.002(4) C11 0.019(4) 0.027(4) 0.021(4) 0.005(3) -0.005(3) -0.005(3) C15 0.021(4) 0.053(5) 0.035(5) 0.008(4) -0.001(4) -0.010(4) C14 0.029(5) 0.058(6) 0.025(4) -0.010(4) -0.003(4) 0.006(4) C25 0.060(6) 0.027(4) 0.023(4) -0.003(3) -0.010(4) -0.009(4) C13 0.039(5) 0.042(5) 0.030(5) -0.012(4) -0.013(4) 0.012(4) C4A 0.044(5) 0.023(4) 0.049(5) 0.003(4) -0.007(4) -0.010(4) C1 0.036(4) 0.022(4) 0.024(4) 0.001(3) -0.008(3) -0.010(3) C23 0.047(5) 0.042(5) 0.034(5) 0.008(4) -0.021(4) -0.014(4) F24 0.112(5) 0.054(3) 0.046(3) -0.010(3) -0.045(3) -0.022(3) C7A 0.050(6) 0.048(5) 0.050(6) 0.001(4) -0.026(5) 0.014(4) C6A 0.075(7) 0.052(6) 0.020(4) 0.007(4) -0.009(4) 0.007(5) O5S 0.061(5) 0.092(6) 0.055(5) -0.015(4) -0.018(4) -0.001(4) C5S 0.019(4) 0.068(7) 0.047(6) -0.005(5) -0.006(4) -0.005(4) C6S 0.054(7) 0.070(7) 0.069(7) -0.006(6) -0.025(6) -0.006(5) C4S 0.031(5) 0.092(8) 0.070(7) 0.023(6) 0.001(5) -0.010(5) C2S 0.071(9) 0.111(11) 0.100(11) 0.048(9) 0.002(8) -0.023(8) C3S 0.093(12) 0.243(24) 0.120(15) 0.045(15) 0.003(11) -0.069(14) C24 0.075(7) 0.036(5) 0.027(4) 0.000(4) -0.020(5) -0.023(5) C5A 0.042(5) 0.039(5) 0.035(5) 0.016(4) 0.012(4) -0.007(4) C3A 0.049(5) 0.021(4) 0.040(5) -0.005(3) -0.004(4) 0.003(4) O1S 0.086(7) 0.130(9) 0.128(9) 0.036(7) 0.007(7) -0.020(7) C1S 0.139(18) 0.334(35) 0.133(18) 0.103(21) -0.050(15) -0.009(20) Ir2 0.0621(2) 0.0229(2) 0.0308(2) -0.01204(13) -0.0312(2) 0.0159(2) Cl3 0.119(2) 0.0252(11) 0.071(2) -0.0211(11) -0.067(2) 0.0231(13) P2 0.059(2) 0.060(2) 0.056(2) -0.0419(13) -0.0441(14) 0.0423(13) C57 0.078(7) 0.023(4) 0.026(4) -0.001(3) -0.026(4) -0.001(4) Cl4 0.0529(13) 0.0503(13) 0.0314(11) -0.0159(9) -0.0235(10) 0.0142(10) C56 0.046(5) 0.018(4) 0.032(4) -0.008(3) -0.013(4) 0.005(3) C55 0.045(5) 0.015(4) 0.032(4) -0.007(3) -0.005(4) 0.010(3) C54 0.054(5) 0.020(4) 0.031(4) -0.004(3) -0.021(4) 0.011(4) C53 0.069(6) 0.018(4) 0.033(5) -0.009(3) -0.021(4) 0.002(4) C57A 0.123(10) 0.024(4) 0.037(5) 0.004(4) -0.041(6) -0.004(5) C56A 0.072(7) 0.026(4) 0.036(5) -0.015(4) -0.025(5) 0.004(4) C55A 0.039(5) 0.031(4) 0.041(5) 0.000(4) -0.012(4) 0.001(4) C54A 0.054(6) 0.038(5) 0.033(5) -0.003(4) -0.022(4) 0.008(4) C53A 0.078(7) 0.033(5) 0.054(6) -0.011(4) -0.029(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C5 2.170(8) . ? Ir1 C3 2.174(7) . ? Ir1 C4 2.192(7) . ? Ir1 C7 2.221(7) . ? Ir1 C6 2.242(7) . ? Ir1 P1 2.304(2) . ? Ir1 Cl2 2.388(2) . ? Ir1 Cl1 2.407(2) . ? P1 C1 1.837(7) . ? P1 C11 1.846(7) . ? P1 C21 1.855(7) . ? F12 C12 1.331(9) . ? F26 C26 1.343(8) . ? F16 C16 1.353(9) . ? C3 C4 1.440(11) . ? C3 C7 1.452(11) . ? C3 C3A 1.508(11) . ? F22 C22 1.339(9) . ? F14 C14 1.331(9) . ? F15 C15 1.339(9) . ? F13 C13 1.344(9) . ? F25 C25 1.349(9) . ? C7 C6 1.426(11) . ? C7 C7A 1.491(11) . ? F23 C23 1.328(9) . ? C6 C5 1.445(11) . ? C6 C6A 1.499(11) . ? C4 C5 1.456(11) . ? C4 C4A 1.491(11) . ? C16 C11 1.377(10) . ? C16 C15 1.383(11) . ? C26 C25 1.374(10) . ? C26 C21 1.390(10) . ? C12 C13 1.377(11) . ? C12 C11 1.396(10) . ? C21 C22 1.386(10) . ? C22 C23 1.386(11) . ? C5 C5A 1.499(11) . ? C15 C14 1.368(12) . ? C14 C13 1.359(12) . ? C25 C24 1.365(12) . ? C1 C1 1.524(14) 2_355 ? C23 C24 1.363(12) . ? F24 C24 1.336(9) . ? O5S C5S 1.192(11) . ? C5S C4S 1.498(13) . ? C5S C6S 1.499(14) . ? C2S O1S 1.216(15) . ? C2S C3S 1.45(2) . ? C2S C1S 1.49(2) . ? Ir2 C57 2.166(9) . ? Ir2 C56 2.167(7) . ? Ir2 C55 2.187(7) . ? Ir2 C53 2.206(10) . ? Ir2 C54 2.212(8) . ? Ir2 P2 2.306(3) . ? Ir2 Cl4 2.404(2) . ? Ir2 Cl3 2.412(2) . ? P2 C51B 1.862(14) . ? P2 C71A 1.865(10) . ? P2 C71B 1.865(10) . ? P2 C61A 1.87(2) . ? P2 C51A 1.896(14) . ? P2 C61B 1.90(2) . ? C57 C56 1.422(11) . ? C57 C53 1.460(11) . ? C57 C57A 1.499(11) . ? C56 C55 1.427(10) . ? C56 C56A 1.507(11) . ? C55 C54 1.448(11) . ? C55 C55A 1.490(11) . ? C54 C53 1.410(11) . ? C54 C54A 1.505(10) . ? C53 C53A 1.484(12) . ? C61A C66A 1.37(2) . ? C61A C62A 1.40(2) . ? C62A F62A 1.32(2) . ? C62A C63A 1.42(2) . ? C63A C64A 1.32(2) . ? C63A F63A 1.33(2) . ? C64A F64A 1.37(2) . ? C64A C65A 1.40(2) . ? C65A F65A 1.33(2) . ? C65A C66A 1.33(2) . ? C66A F66A 1.36(2) . ? C61B C66B 1.34(3) . ? C61B C62B 1.43(3) . ? C62B C63B 1.35(3) . ? C62B F62B 1.35(2) . ? F63B C63B 1.37(2) . ? C63B C64B 1.35(3) . ? F64B C64B 1.37(2) . ? C64B C65B 1.39(3) . ? F65B C65B 1.25(2) . ? C65B C66B 1.41(3) . ? F66B C66B 1.33(2) . ? C73B F73B 1.28(4) . ? C73B C74B 1.28(3) . ? C73B C72B 1.44(3) . ? C74B F74B 1.28(3) . ? C74B C75B 1.38(3) . ? C75B F75B 1.35(2) . ? C75B C76B 1.37(3) . ? C76B F76B 1.33(2) . ? C76B C71B 1.55(2) . ? C71B C72B 1.52(3) . ? C72B F72B 1.28(3) . ? C71A C72A 1.26(2) . ? C71A C76A 1.32(2) . ? C72A F72A 1.37(3) . ? C72A C73A 1.42(3) . ? C73A C74A 1.30(3) . ? C73A F73A 1.37(3) . ? C74A C75A 1.36(3) . ? C74A F74A 1.39(3) . ? C75A F75A 1.34(2) . ? C75A C76A 1.44(3) . ? C76A F76A 1.38(2) . ? C51A C51A 1.50(3) 2_444 ? C51B C51B 1.52(3) 2_444 ? 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 Ir1 C3 65.1(3) . . ? C5 Ir1 C4 39.0(3) . . ? C3 Ir1 C4 38.5(3) . . ? C5 Ir1 C7 64.2(3) . . ? C3 Ir1 C7 38.6(3) . . ? C4 Ir1 C7 64.1(3) . . ? C5 Ir1 C6 38.2(3) . . ? C3 Ir1 C6 63.6(3) . . ? C4 Ir1 C6 63.6(3) . . ? C7 Ir1 C6 37.3(3) . . ? C5 Ir1 P1 112.2(2) . . ? C3 Ir1 P1 126.1(2) . . ? C4 Ir1 P1 103.2(2) . . ? C7 Ir1 P1 164.6(2) . . ? C6 Ir1 P1 146.9(2) . . ? C5 Ir1 Cl2 103.9(2) . . ? C3 Ir1 Cl2 151.0(2) . . ? C4 Ir1 Cl2 142.2(2) . . ? C7 Ir1 Cl2 112.5(2) . . ? C6 Ir1 Cl2 90.8(2) . . ? P1 Ir1 Cl2 82.77(7) . . ? C5 Ir1 Cl1 155.4(2) . . ? C3 Ir1 Cl1 94.5(2) . . ? C4 Ir1 Cl1 129.1(2) . . ? C7 Ir1 Cl1 91.4(2) . . ? C6 Ir1 Cl1 121.6(2) . . ? P1 Ir1 Cl1 90.63(7) . . ? Cl2 Ir1 Cl1 87.45(8) . . ? C1 P1 C11 103.3(3) . . ? C1 P1 C21 99.9(3) . . ? C11 P1 C21 103.8(3) . . ? C1 P1 Ir1 117.3(2) . . ? C11 P1 Ir1 110.0(2) . . ? C21 P1 Ir1 120.5(2) . . ? C4 C3 C7 108.1(7) . . ? C4 C3 C3A 127.7(7) . . ? C7 C3 C3A 123.8(7) . . ? C4 C3 Ir1 71.4(4) . . ? C7 C3 Ir1 72.5(4) . . ? C3A C3 Ir1 127.5(5) . . ? C6 C7 C3 107.9(7) . . ? C6 C7 C7A 127.3(7) . . ? C3 C7 C7A 124.6(7) . . ? C6 C7 Ir1 72.2(4) . . ? C3 C7 Ir1 69.0(4) . . ? C7A C7 Ir1 128.6(6) . . ? C7 C6 C5 108.7(7) . . ? C7 C6 C6A 126.5(8) . . ? C5 C6 C6A 124.7(8) . . ? C7 C6 Ir1 70.6(4) . . ? C5 C6 Ir1 68.2(4) . . ? C6A C6 Ir1 126.3(6) . . ? C3 C4 C5 107.5(7) . . ? C3 C4 C4A 126.3(7) . . ? C5 C4 C4A 125.7(7) . . ? C3 C4 Ir1 70.1(4) . . ? C5 C4 Ir1 69.7(4) . . ? C4A C4 Ir1 131.4(5) . . ? F16 C16 C11 119.8(7) . . ? F16 C16 C15 116.7(7) . . ? C11 C16 C15 123.4(7) . . ? F26 C26 C25 116.6(7) . . ? F26 C26 C21 120.3(6) . . ? C25 C26 C21 123.1(7) . . ? F12 C12 C13 116.7(7) . . ? F12 C12 C11 122.2(7) . . ? C13 C12 C11 121.1(8) . . ? C22 C21 C26 115.1(7) . . ? C22 C21 P1 126.2(6) . . ? C26 C21 P1 118.5(5) . . ? F22 C22 C23 116.6(7) . . ? F22 C22 C21 121.0(7) . . ? C23 C22 C21 122.4(8) . . ? C6 C5 C4 107.5(7) . . ? C6 C5 C5A 123.7(7) . . ? C4 C5 C5A 127.5(8) . . ? C6 C5 Ir1 73.6(4) . . ? C4 C5 Ir1 71.3(4) . . ? C5A C5 Ir1 130.5(5) . . ? C16 C11 C12 115.7(7) . . ? C16 C11 P1 120.3(6) . . ? C12 C11 P1 123.8(5) . . ? F15 C15 C14 121.0(7) . . ? F15 C15 C16 120.0(8) . . ? C14 C15 C16 119.0(8) . . ? F14 C14 C13 119.9(8) . . ? F14 C14 C15 120.8(8) . . ? C13 C14 C15 119.3(7) . . ? F25 C25 C24 120.7(7) . . ? F25 C25 C26 119.7(7) . . ? C24 C25 C26 119.6(8) . . ? F13 C13 C14 120.0(7) . . ? F13 C13 C12 118.5(8) . . ? C14 C13 C12 121.4(8) . . ? C1 C1 P1 112.3(6) 2_355 . ? F23 C23 C24 120.9(8) . . ? F23 C23 C22 119.3(8) . . ? C24 C23 C22 119.8(8) . . ? O5S C5S C4S 122.0(10) . . ? O5S C5S C6S 122.7(10) . . ? C4S C5S C6S 115.3(9) . . ? O1S C2S C3S 122.5(15) . . ? O1S C2S C1S 122.7(16) . . ? C3S C2S C1S 114.7(14) . . ? F24 C24 C23 120.2(8) . . ? F24 C24 C25 120.0(8) . . ? C23 C24 C25 119.8(7) . . ? C57 Ir2 C56 38.3(3) . . ? C57 Ir2 C55 64.5(3) . . ? C56 Ir2 C55 38.3(3) . . ? C57 Ir2 C53 39.0(3) . . ? C56 Ir2 C53 64.2(3) . . ? C55 Ir2 C53 64.1(3) . . ? C57 Ir2 C54 63.8(3) . . ? C56 Ir2 C54 63.6(3) . . ? C55 Ir2 C54 38.4(3) . . ? C53 Ir2 C54 37.2(3) . . ? C57 Ir2 P2 127.2(2) . . ? C56 Ir2 P2 104.2(2) . . ? C55 Ir2 P2 112.1(2) . . ? C53 Ir2 P2 166.2(2) . . ? C54 Ir2 P2 146.2(2) . . ? C57 Ir2 Cl4 151.0(2) . . ? C56 Ir2 Cl4 143.3(2) . . ? C55 Ir2 Cl4 105.5(2) . . ? C53 Ir2 Cl4 112.1(2) . . ? C54 Ir2 Cl4 91.2(2) . . ? P2 Ir2 Cl4 81.65(9) . . ? C57 Ir2 Cl3 93.4(2) . . ? C56 Ir2 Cl3 127.2(2) . . ? C55 Ir2 Cl3 155.3(2) . . ? C53 Ir2 Cl3 91.9(2) . . ? C54 Ir2 Cl3 123.2(2) . . ? P2 Ir2 Cl3 89.73(10) . . ? Cl4 Ir2 Cl3 88.49(9) . . ? C51B P2 C71B 120.1(6) . . ? C71A P2 C61A 93.7(6) . . ? C71A P2 C51A 92.4(6) . . ? C61A P2 C51A 95.6(6) . . ? C51B P2 C61B 96.5(6) . . ? C71B P2 C61B 111.0(7) . . ? C51B P2 Ir2 104.1(5) . . ? C71A P2 Ir2 110.1(3) . . ? C71B P2 Ir2 110.1(3) . . ? C61A P2 Ir2 130.3(5) . . ? C51A P2 Ir2 124.9(5) . . ? C61B P2 Ir2 114.6(6) . . ? C56 C57 C53 107.5(7) . . ? C56 C57 C57A 128.3(7) . . ? C53 C57 C57A 123.9(8) . . ? C56 C57 Ir2 70.9(5) . . ? C53 C57 Ir2 72.0(5) . . ? C57A C57 Ir2 127.8(7) . . ? C57 C56 C55 109.2(7) . . ? C57 C56 C56A 123.5(7) . . ? C55 C56 C56A 126.6(7) . . ? C57 C56 Ir2 70.8(5) . . ? C55 C56 Ir2 71.6(4) . . ? C56A C56 Ir2 131.6(6) . . ? C56 C55 C54 106.7(7) . . ? C56 C55 C55A 129.0(7) . . ? C54 C55 C55A 123.6(7) . . ? C56 C55 Ir2 70.1(4) . . ? C54 C55 Ir2 71.7(4) . . ? C55A C55 Ir2 130.5(6) . . ? C53 C54 C55 109.3(7) . . ? C53 C54 C54A 125.7(8) . . ? C55 C54 C54A 124.9(7) . . ? C53 C54 Ir2 71.2(5) . . ? C55 C54 Ir2 69.8(4) . . ? C54A C54 Ir2 127.0(6) . . ? C54 C53 C57 107.3(7) . . ? C54 C53 C53A 128.8(8) . . ? C57 C53 C53A 123.9(7) . . ? C54 C53 Ir2 71.6(5) . . ? C57 C53 Ir2 69.0(5) . . ? C53A C53 Ir2 125.9(6) . . ? C66A C61A C62A 115.0(16) . . ? C66A C61A P2 134.7(14) . . ? C62A C61A P2 109.8(13) . . ? F62A C62A C61A 122.4(15) . . ? F62A C62A C63A 115.2(16) . . ? C61A C62A C63A 122.3(15) . . ? C64A C63A F63A 121.5(18) . . ? C64A C63A C62A 117.9(16) . . ? F63A C63A C62A 120.3(17) . . ? C63A C64A F64A 119.9(17) . . ? C63A C64A C65A 121.4(17) . . ? F64A C64A C65A 118.7(13) . . ? F65A C65A C66A 121.9(17) . . ? F65A C65A C64A 119.1(14) . . ? C66A C65A C64A 119.0(18) . . ? C65A C66A F66A 116.2(15) . . ? C65A C66A C61A 124.2(19) . . ? F66A C66A C61A 119.7(14) . . ? C66B C61B C62B 117.0(19) . . ? C66B C61B P2 117.4(16) . . ? C62B C61B P2 125.4(14) . . ? C63B C62B F62B 118.6(18) . . ? C63B C62B C61B 120.6(21) . . ? F62B C62B C61B 120.8(16) . . ? C62B C63B C64B 120.3(22) . . ? C62B C63B F63B 118.1(19) . . ? C64B C63B F63B 121.6(19) . . ? C63B C64B F64B 119.1(19) . . ? C63B C64B C65B 123.2(21) . . ? F64B C64B C65B 117.7(21) . . ? F65B C65B C64B 120.9(23) . . ? F65B C65B C66B 124.3(23) . . ? C64B C65B C66B 114.7(19) . . ? F66B C66B C61B 122.2(18) . . ? F66B C66B C65B 113.4(19) . . ? C61B C66B C65B 124.2(20) . . ? F73B C73B C74B 131.9(27) . . ? F73B C73B C72B 112.1(19) . . ? C74B C73B C72B 116.0(27) . . ? F74B C74B C73B 121.7(25) . . ? F74B C74B C75B 116.7(20) . . ? C73B C74B C75B 121.6(25) . . ? F75B C75B C76B 114.6(18) . . ? F75B C75B C74B 122.4(17) . . ? C76B C75B C74B 122.8(19) . . ? F76B C76B C75B 120.7(20) . . ? F76B C76B C71B 111.8(18) . . ? C75B C76B C71B 127.3(15) . . ? C72B C71B C76B 98.4(14) . . ? C72B C71B P2 124.9(12) . . ? C76B C71B P2 136.6(10) . . ? F72B C72B C73B 115.6(20) . . ? F72B C72B C71B 110.9(22) . . ? C73B C72B C71B 133.4(23) . . ? C72A C71A C76A 137.1(16) . . ? C72A C71A P2 111.6(13) . . ? C76A C71A P2 110.8(11) . . ? C71A C72A F72A 129.5(20) . . ? C71A C72A C73A 111.5(18) . . ? F72A C72A C73A 118.9(19) . . ? C74A C73A F73A 117.6(25) . . ? C74A C73A C72A 119.2(23) . . ? F73A C73A C72A 123.2(20) . . ? C73A C74A C75A 124.7(23) . . ? C73A C74A F74A 124.5(25) . . ? C75A C74A F74A 110.8(23) . . ? F75A C75A C74A 127.4(24) . . ? F75A C75A C76A 114.8(17) . . ? C74A C75A C76A 117.8(20) . . ? C71A C76A F76A 132.7(17) . . ? C71A C76A C75A 109.5(16) . . ? F76A C76A C75A 117.7(15) . . ? C51A C51A P2 106.8(13) 2_444 . ? C51B C51B P2 109.3(13) 2_444 . ? _refine_diff_density_max 1.572 _refine_diff_density_min -3.247 _refine_diff_density_rms 0.148 #=END data_gcs1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H37 B Cl F12 O P2 Rh' _chemical_formula_weight 960.80 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9380(10) _cell_length_b 20.915(2) _cell_length_c 17.3520(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.68 _cell_angle_gamma 90.00 _cell_volume 3887.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max .52 _exptl_crystal_size_mid .475 _exptl_crystal_size_min .375 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method ? _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type 'empirical (psi scans)' _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.967 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7641 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6831 _reflns_number_observed 5789 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+16.9668P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6825 _refine_ls_number_parameters 567 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_obs 0.0422 _refine_ls_wR_factor_all 0.1040 _refine_ls_wR_factor_obs 0.0931 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.099 _refine_ls_restrained_S_obs 1.083 _refine_ls_shift/esd_max -0.046 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.20101(3) 0.636151(15) 0.66832(2) 0.01902(10) Uani 1 d . . Cl Cl 0.14072(10) 0.56460(5) 0.56027(6) 0.0311(2) Uani 1 d . . P1 P 0.20647(11) 0.54192(5) 0.74042(6) 0.0263(2) Uani 0.50 d PD 1 C1 C 0.3504(11) 0.4951(5) 0.7260(7) 0.027(3) Uani 0.50 d PD 1 H1A H 0.4098(11) 0.4926(5) 0.7772(7) 0.033 Uiso 0.50 calc PR 1 H1B H 0.3245(11) 0.4510(5) 0.7099(7) 0.033 Uiso 0.50 calc PR 1 C2 C 0.4185(8) 0.5234(4) 0.6651(6) 0.023(2) Uani 0.50 d PD 1 H2A H 0.3804(8) 0.5073(4) 0.6121(6) 0.028 Uiso 0.50 calc PR 1 H2B H 0.5072(8) 0.5101(4) 0.6773(6) 0.028 Uiso 0.50 calc PR 1 P2 P 0.40860(10) 0.60843(6) 0.66662(8) 0.0343(3) Uani 0.50 d PD 1 P1' P 0.20647(11) 0.54192(5) 0.74042(6) 0.0263(2) Uani 0.50 d PD 2 C1' C 0.3054(10) 0.4888(5) 0.7006(6) 0.019(2) Uani 0.50 d PD 2 H1'1 H 0.3123(10) 0.4470(5) 0.7278(6) 0.023 Uiso 0.50 calc PR 2 H1'2 H 0.2737(10) 0.4820(5) 0.6436(6) 0.023 Uiso 0.50 calc PR 2 C2' C 0.4311(7) 0.5236(4) 0.7156(6) 0.023(2) Uani 0.50 d PD 2 H2'1 H 0.4924(7) 0.4987(4) 0.6931(6) 0.028 Uiso 0.50 calc PR 2 H2'2 H 0.4633(7) 0.5280(4) 0.7729(6) 0.028 Uiso 0.50 calc PR 2 P2' P 0.40860(10) 0.60843(6) 0.66662(8) 0.0343(3) Uani 0.50 d PD 2 C3 C 0.1047(4) 0.7005(2) 0.7394(3) 0.0293(10) Uani 1 d . . C4 C 0.2034(4) 0.7344(2) 0.7161(3) 0.0335(11) Uani 1 d . . C5 C 0.1764(5) 0.7401(2) 0.6316(3) 0.0348(11) Uani 1 d . . C6 C 0.0642(4) 0.7070(2) 0.6033(3) 0.0345(11) Uani 1 d . . C7 C 0.0203(4) 0.6807(2) 0.6693(3) 0.0342(11) Uani 1 d . . C3A C 0.0825(5) 0.6968(2) 0.8207(3) 0.0392(12) Uani 1 d . . H3A1 H 0.0241(25) 0.6619(11) 0.8243(6) 0.059 Uiso 1 calc R . H3A2 H 0.0469(30) 0.7373(6) 0.8343(8) 0.059 Uiso 1 calc R . H3A3 H 0.1617(7) 0.6888(17) 0.8574(4) 0.059 Uiso 1 calc R . C4A C 0.3027(5) 0.7716(2) 0.7707(4) 0.053(2) Uani 1 d . . H4A1 H 0.2679(12) 0.8123(9) 0.7843(20) 0.080 Uiso 1 calc R . H4A2 H 0.3727(18) 0.7800(17) 0.7447(10) 0.080 Uiso 1 calc R . H4A3 H 0.3323(27) 0.7468(9) 0.8188(11) 0.080 Uiso 1 calc R . C5A C 0.2350(6) 0.7854(2) 0.5826(4) 0.054(2) Uani 1 d . . H5A1 H 0.3201(15) 0.7956(15) 0.6102(11) 0.080 Uiso 1 calc R . H5A2 H 0.1855(22) 0.8247(8) 0.5738(21) 0.080 Uiso 1 calc R . H5A3 H 0.2377(35) 0.7654(8) 0.5319(10) 0.080 Uiso 1 calc R . C6A C -0.0037(6) 0.7026(3) 0.5192(3) 0.060(2) Uani 1 d . . H6A1 H -0.0669(29) 0.7364(14) 0.5084(8) 0.091 Uiso 1 calc R . H6A2 H -0.0445(35) 0.6607(9) 0.5100(7) 0.091 Uiso 1 calc R . H6A3 H 0.0558(9) 0.7077(22) 0.4844(3) 0.091 Uiso 1 calc R . C7A C -0.1031(4) 0.6481(3) 0.6636(4) 0.057(2) Uani 1 d . . H7A1 H -0.1072(16) 0.6107(12) 0.6290(20) 0.085 Uiso 1 calc R . H7A2 H -0.1704(5) 0.6779(7) 0.6419(24) 0.085 Uiso 1 calc R . H7A3 H -0.1123(18) 0.6343(18) 0.7161(5) 0.085 Uiso 1 calc R . C11 C 0.2574(4) 0.5375(2) 0.8483(3) 0.0300(10) Uani 1 d . . C12 C 0.2428(5) 0.4821(3) 0.8906(3) 0.0474(14) Uani 1 d . . F12 F 0.1829(3) 0.4315(2) 0.8512(2) 0.0594(9) Uani 1 d . . C13 C 0.2862(6) 0.4759(4) 0.9698(4) 0.070(2) Uani 1 d . . H13 H 0.2719(6) 0.4376(4) 0.9961(4) 0.083 Uiso 1 calc R . C14 C 0.3511(6) 0.5259(4) 1.0114(4) 0.075(2) Uani 1 d . . H14 H 0.3804(6) 0.5222(4) 1.0666(4) 0.089 Uiso 1 calc R . C15 C 0.3737(5) 0.5813(3) 0.9728(3) 0.053(2) Uani 1 d . . H15 H 0.4196(5) 0.6157(3) 1.0005(3) 0.064 Uiso 1 calc R . C16 C 0.3271(4) 0.5849(3) 0.8928(3) 0.0390(12) Uani 1 d . . F16 F 0.3541(3) 0.63894(14) 0.8558(2) 0.0429(7) Uani 1 d . . C21 C 0.0602(5) 0.4970(2) 0.7225(3) 0.0400(12) Uani 1 d . . C22 C 0.0270(8) 0.4480(3) 0.6677(3) 0.067(2) Uani 1 d . . F22 F 0.1100(5) 0.4282(2) 0.6251(2) 0.0859(15) Uani 1 d . . C23 C -0.0897(10) 0.4184(3) 0.6550(4) 0.098(4) Uani 1 d . . H23 H -0.1113(10) 0.3875(3) 0.6144(4) 0.118 Uiso 1 calc R . C24 C -0.1711(9) 0.4336(4) 0.7003(4) 0.102(4) Uani 1 d . . H24 H -0.2486(9) 0.4117(4) 0.6933(4) 0.122 Uiso 1 calc R . C25 C -0.1441(6) 0.4803(3) 0.7566(4) 0.064(2) Uani 1 d . . H25 H -0.2019(6) 0.4915(3) 0.7886(4) 0.077 Uiso 1 calc R . C26 C -0.0307(5) 0.5105(2) 0.7652(3) 0.0434(13) Uani 1 d . . F26 F -0.0058(3) 0.55596(14) 0.8218(2) 0.0431(7) Uani 1 d . . C31 C 0.4704(4) 0.6105(3) 0.5760(3) 0.054(2) Uani 1 d . . C32 C 0.4117(4) 0.6368(3) 0.5050(4) 0.052(2) Uani 1 d . . F32 F 0.3015(3) 0.66647(14) 0.5000(2) 0.0453(7) Uani 1 d . . C33 C 0.4597(5) 0.6358(4) 0.4375(4) 0.069(2) Uani 1 d . . H33 H 0.4145(5) 0.6539(4) 0.3900(4) 0.083 Uiso 1 calc R . C34 C 0.5745(6) 0.6080(5) 0.4405(4) 0.114(4) Uani 1 d . . H34 H 0.6094(6) 0.6072(5) 0.3946(4) 0.136 Uiso 1 calc R . C35 C 0.6389(6) 0.5815(5) 0.5088(4) 0.119(4) Uani 1 d . . H35 H 0.7182(6) 0.5623(5) 0.5109(4) 0.143 Uiso 1 calc R . C36 C 0.5869(5) 0.5831(4) 0.5739(4) 0.085(3) Uani 1 d . . F36 F 0.6536(3) 0.5585(2) 0.6415(2) 0.091(2) Uani 1 d . . C41 C 0.5347(4) 0.6506(2) 0.7328(2) 0.0240(9) Uani 1 d . . C42 C 0.6055(5) 0.6293(3) 0.8037(3) 0.0506(15) Uani 1 d . . F42 F 0.5832(4) 0.5708(2) 0.8297(3) 0.123(2) Uani 1 d . . C43 C 0.6985(5) 0.6642(4) 0.8493(3) 0.064(2) Uani 1 d . . H43 H 0.7443(5) 0.6471(4) 0.8972(3) 0.076 Uiso 1 calc R . C44 C 0.7250(5) 0.7239(3) 0.8255(3) 0.056(2) Uani 1 d . . H44 H 0.7896(5) 0.7486(3) 0.8567(3) 0.067 Uiso 1 calc R . C45 C 0.6583(5) 0.7480(3) 0.7569(4) 0.054(2) Uani 1 d . . H45 H 0.6749(5) 0.7897(3) 0.7400(4) 0.065 Uiso 1 calc R . C46 C 0.5669(4) 0.7110(2) 0.7126(3) 0.0304(10) Uani 1 d . . F46 F 0.5000(3) 0.7357(2) 0.6443(2) 0.0531(9) Uani 1 d . . O O 0.4496(4) 0.8129(3) 0.4780(2) 0.093(2) Uani 1 d . . C8 C 0.6590(6) 0.7846(4) 0.5273(4) 0.076(2) Uani 1 d . . H8A H 0.6957(30) 0.7798(20) 0.5834(4) 0.114 Uiso 1 calc R . H8B H 0.7217(22) 0.8019(13) 0.4999(26) 0.114 Uiso 1 calc R . H8C H 0.6309(10) 0.7427(8) 0.5051(28) 0.114 Uiso 1 calc R . C9 C 0.5495(5) 0.8294(4) 0.5175(3) 0.070(2) Uani 1 d . . C10 C 0.5706(8) 0.8917(5) 0.5556(7) 0.121(4) Uani 1 d . . H10A H 0.6594(15) 0.9026(18) 0.5637(44) 0.181 Uiso 1 calc R . H10B H 0.5450(70) 0.8902(12) 0.6065(21) 0.181 Uiso 1 calc R . H10C H 0.5214(59) 0.9242(8) 0.5222(22) 0.181 Uiso 1 calc R . B B -0.4508(5) 0.3598(3) 0.8027(3) 0.0303(11) Uani 1 d . . F1 F -0.5413(6) 0.3840(4) 0.8382(4) 0.066(3) Uani 0.508(9) d P . F2 F -0.3962(7) 0.3097(4) 0.8377(7) 0.078(4) Uani 0.508(9) d P . F3 F -0.5073(11) 0.3471(4) 0.7248(4) 0.078(3) Uani 0.508(9) d P . F4 F -0.3875(4) 0.4157(2) 0.8040(2) 0.0828(13) Uani 1 d . . F1A F -0.4515(7) 0.3365(4) 0.8798(3) 0.051(3) Uani 0.492(9) d P . F2A F -0.3722(7) 0.3183(4) 0.7731(5) 0.063(3) Uani 0.492(9) d P . F3A F -0.5676(6) 0.3532(3) 0.7592(5) 0.049(2) Uani 0.492(9) d P . 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 Rh 0.0163(2) 0.0171(2) 0.0238(2) 0.00112(13) 0.00451(11) 0.00032(13) Cl 0.0348(6) 0.0350(6) 0.0204(5) -0.0015(4) -0.0018(4) -0.0084(5) P1 0.0409(6) 0.0185(5) 0.0205(5) 0.0010(4) 0.0087(5) 0.0034(5) C1 0.035(8) 0.020(5) 0.024(7) -0.004(5) 0.000(5) 0.005(6) C2 0.027(5) 0.023(5) 0.019(5) -0.002(4) 0.001(4) 0.002(3) P2 0.0166(5) 0.0224(6) 0.0643(9) -0.0143(6) 0.0089(5) -0.0023(4) P1' 0.0409(6) 0.0185(5) 0.0205(5) 0.0010(4) 0.0087(5) 0.0034(5) C1' 0.029(6) 0.015(5) 0.011(5) -0.003(4) 0.000(4) -0.006(4) C2' 0.016(4) 0.016(4) 0.032(6) -0.001(4) -0.007(4) 0.001(4) P2' 0.0166(5) 0.0224(6) 0.0643(9) -0.0143(6) 0.0089(5) -0.0023(4) C3 0.031(2) 0.024(2) 0.037(3) 0.004(2) 0.017(2) 0.011(2) C4 0.037(3) 0.018(2) 0.052(3) -0.002(2) 0.023(2) 0.006(2) C5 0.044(3) 0.017(2) 0.053(3) 0.009(2) 0.031(2) 0.013(2) C6 0.032(2) 0.034(3) 0.042(3) 0.013(2) 0.016(2) 0.018(2) C7 0.025(2) 0.039(3) 0.042(3) 0.014(2) 0.013(2) 0.015(2) C3A 0.048(3) 0.036(3) 0.038(3) 0.008(2) 0.021(2) 0.012(2) C4A 0.061(4) 0.030(3) 0.075(4) -0.030(3) 0.031(3) -0.016(3) C5A 0.073(4) 0.029(3) 0.072(4) 0.014(3) 0.047(3) 0.007(3) C6A 0.060(4) 0.081(5) 0.040(3) 0.027(3) 0.010(3) 0.036(3) C7A 0.020(2) 0.086(5) 0.064(4) 0.027(3) 0.009(2) 0.006(3) C11 0.028(2) 0.039(3) 0.023(2) 0.007(2) 0.006(2) 0.012(2) C12 0.044(3) 0.058(4) 0.041(3) 0.022(3) 0.011(2) 0.018(3) F12 0.065(2) 0.045(2) 0.068(2) 0.034(2) 0.011(2) 0.004(2) C13 0.057(4) 0.104(6) 0.050(4) 0.048(4) 0.016(3) 0.030(4) C14 0.061(4) 0.136(7) 0.027(3) 0.028(4) 0.011(3) 0.041(5) C15 0.038(3) 0.090(5) 0.028(3) -0.006(3) -0.002(2) 0.022(3) C16 0.030(2) 0.062(3) 0.025(2) -0.001(2) 0.004(2) 0.016(2) F16 0.042(2) 0.048(2) 0.0334(15) -0.0080(14) -0.0055(12) -0.0007(14) C21 0.067(3) 0.029(3) 0.022(2) 0.006(2) 0.004(2) -0.020(2) C22 0.143(7) 0.034(3) 0.020(3) 0.003(2) 0.007(3) -0.038(4) F22 0.193(5) 0.033(2) 0.036(2) -0.0148(15) 0.032(2) -0.028(2) C23 0.184(9) 0.057(4) 0.034(4) 0.009(3) -0.025(5) -0.080(6) C24 0.137(8) 0.105(7) 0.044(4) 0.035(4) -0.028(5) -0.091(6) C25 0.062(4) 0.073(4) 0.049(4) 0.030(3) -0.007(3) -0.037(3) C26 0.055(3) 0.040(3) 0.030(3) 0.011(2) -0.004(2) -0.019(2) F26 0.037(2) 0.049(2) 0.045(2) -0.0023(14) 0.0116(13) -0.0093(13) C31 0.017(2) 0.084(4) 0.062(4) -0.059(3) 0.007(2) -0.008(2) C32 0.019(2) 0.068(4) 0.071(4) -0.050(3) 0.014(2) -0.011(2) F32 0.039(2) 0.038(2) 0.065(2) -0.0096(14) 0.0268(14) -0.0004(13) C33 0.032(3) 0.117(6) 0.059(4) -0.065(4) 0.012(3) -0.010(3) C34 0.033(3) 0.239(11) 0.070(5) -0.108(6) 0.011(3) -0.002(5) C35 0.028(3) 0.246(12) 0.080(5) -0.108(7) 0.000(3) 0.025(5) C36 0.017(3) 0.159(7) 0.074(4) -0.084(5) -0.005(3) 0.008(3) F36 0.021(2) 0.157(4) 0.087(3) -0.074(3) -0.009(2) 0.025(2) C41 0.018(2) 0.025(2) 0.030(2) -0.004(2) 0.007(2) -0.002(2) C42 0.033(3) 0.066(4) 0.054(3) 0.032(3) 0.013(2) 0.003(3) F42 0.058(2) 0.116(4) 0.190(5) 0.125(4) 0.010(3) 0.005(2) C43 0.035(3) 0.120(6) 0.031(3) 0.011(3) -0.004(2) 0.013(3) C44 0.035(3) 0.073(4) 0.050(3) -0.033(3) -0.011(3) 0.003(3) C45 0.041(3) 0.032(3) 0.080(4) -0.010(3) -0.009(3) -0.010(2) C46 0.029(2) 0.030(2) 0.029(2) 0.001(2) -0.003(2) -0.003(2) F46 0.047(2) 0.054(2) 0.050(2) 0.027(2) -0.0100(14) -0.0187(15) O 0.036(2) 0.197(6) 0.041(2) 0.034(3) -0.008(2) -0.027(3) C8 0.042(3) 0.114(6) 0.062(4) 0.034(4) -0.012(3) -0.026(4) C9 0.036(3) 0.134(7) 0.038(3) 0.031(4) 0.006(3) -0.021(4) C10 0.056(5) 0.144(9) 0.167(10) -0.029(8) 0.031(6) -0.012(6) B 0.027(2) 0.030(3) 0.033(3) 0.003(2) 0.005(2) -0.001(2) F1 0.048(4) 0.086(6) 0.072(5) -0.018(4) 0.032(4) 0.000(4) F2 0.052(5) 0.049(5) 0.124(10) 0.035(5) -0.006(5) 0.015(4) F3 0.107(8) 0.087(6) 0.037(4) -0.013(4) 0.011(4) -0.018(5) F4 0.107(3) 0.055(2) 0.078(3) 0.011(2) -0.003(2) -0.047(2) F1A 0.071(5) 0.052(5) 0.027(3) -0.002(3) 0.002(3) -0.030(4) F2A 0.062(5) 0.053(5) 0.086(6) -0.006(4) 0.040(4) 0.020(3) F3A 0.035(4) 0.038(4) 0.063(6) 0.011(3) -0.018(3) -0.006(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 Rh C7 2.188(4) . ? Rh C4 2.213(4) . ? Rh C3 2.228(4) . ? Rh C6 2.241(4) . ? Rh C5 2.266(4) . ? Rh P1' 2.3286(11) . ? Rh P1 2.3286(11) . ? Rh P2 2.3495(12) . ? Rh P2' 2.3495(12) . ? Rh Cl 2.3851(11) . ? P1 C21 1.826(5) . ? P1 C11 1.843(4) . ? P1 C1 1.913(11) . ? C1 C2 1.529(13) . ? C2 P2 1.782(8) . ? P2 C41 1.833(4) . ? P2 C31 1.833(6) . ? P1' C1' 1.784(11) . ? P1' C21 1.826(5) . ? P1' C11 1.843(4) . ? C1' C2' 1.530(11) . ? C2' P2' 1.961(8) . ? P2' C41 1.833(4) . ? P2' C31 1.833(6) . ? C3 C4 1.417(6) . ? C3 C7 1.431(7) . ? C3 C3A 1.483(6) . ? C4 C5 1.439(7) . ? C4 C4A 1.507(7) . ? C5 C6 1.409(7) . ? C5 C5A 1.500(6) . ? C6 C7 1.438(6) . ? C6 C6A 1.500(7) . ? C7 C7A 1.497(7) . ? C11 C16 1.387(7) . ? C11 C12 1.397(7) . ? C12 F12 1.355(7) . ? C12 C13 1.368(8) . ? C13 C14 1.380(11) . ? C14 C15 1.386(10) . ? C15 C16 1.380(7) . ? C16 F16 1.362(6) . ? C21 C26 1.385(8) . ? C21 C22 1.396(7) . ? C22 F22 1.347(8) . ? C22 C23 1.395(11) . ? C23 C24 1.340(13) . ? C24 C25 1.371(11) . ? C25 C26 1.372(7) . ? C26 F26 1.354(6) . ? C31 C32 1.384(9) . ? C31 C36 1.404(7) . ? C32 F32 1.344(6) . ? C32 C33 1.376(8) . ? C33 C34 1.375(9) . ? C34 C35 1.369(13) . ? C35 C36 1.364(10) . ? C36 F36 1.351(9) . ? C41 C46 1.376(6) . ? C41 C42 1.387(7) . ? C42 F42 1.343(7) . ? C42 C43 1.366(9) . ? C43 C44 1.365(9) . ? C44 C45 1.360(8) . ? C45 C46 1.371(7) . ? C46 F46 1.363(5) . ? O C9 1.216(7) . ? C8 C9 1.503(10) . ? C9 C10 1.458(12) . ? B F2 1.293(8) . ? B F3A 1.353(8) . ? B F4 1.357(6) . ? B F1 1.365(8) . ? B F2A 1.391(8) . ? B F3 1.393(9) . ? B F1A 1.426(8) . ? F1 F1A 1.478(11) . ? F1 F3A 1.488(11) . ? F2 F1A 1.179(11) . ? F2 F2A 1.215(12) . ? F3 F3A 0.983(9) . ? F3 F2A 1.658(12) . ? 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 C7 Rh C4 62.9(2) . . ? C7 Rh C3 37.8(2) . . ? C4 Rh C3 37.2(2) . . ? C7 Rh C6 37.9(2) . . ? C4 Rh C6 62.0(2) . . ? C3 Rh C6 62.4(2) . . ? C7 Rh C5 62.5(2) . . ? C4 Rh C5 37.5(2) . . ? C3 Rh C5 62.2(2) . . ? C6 Rh C5 36.4(2) . . ? C7 Rh P1' 106.31(13) . . ? C4 Rh P1' 125.97(13) . . ? C3 Rh P1' 100.22(11) . . ? C6 Rh P1' 140.51(13) . . ? C5 Rh P1' 162.10(12) . . ? C7 Rh P1 106.31(13) . . ? C4 Rh P1 125.97(13) . . ? C3 Rh P1 100.22(11) . . ? C6 Rh P1 140.51(13) . . ? C5 Rh P1 162.10(12) . . ? C7 Rh P2 169.11(14) . . ? C4 Rh P2 107.19(12) . . ? C3 Rh P2 136.24(13) . . ? C6 Rh P2 134.85(12) . . ? C5 Rh P2 107.05(12) . . ? P1 Rh P2 83.00(5) . . ? C7 Rh P2' 169.11(14) . . ? C4 Rh P2' 107.19(12) . . ? C3 Rh P2' 136.24(13) . . ? C6 Rh P2' 134.85(12) . . ? C5 Rh P2' 107.05(12) . . ? P1' Rh P2' 83.00(5) . . ? C7 Rh Cl 99.60(14) . . ? C4 Rh Cl 148.98(14) . . ? C3 Rh Cl 136.67(13) . . ? C6 Rh Cl 88.22(14) . . ? C5 Rh Cl 112.53(14) . . ? P1' Rh Cl 82.20(4) . . ? P1 Rh Cl 82.20(4) . . ? P2 Rh Cl 87.10(4) . . ? P2' Rh Cl 87.10(4) . . ? C21 P1 C11 102.8(2) . . ? C21 P1 C1 115.5(4) . . ? C11 P1 C1 91.1(4) . . ? C21 P1 Rh 114.7(2) . . ? C11 P1 Rh 123.9(2) . . ? C1 P1 Rh 107.2(3) . . ? C2 C1 P1 114.9(7) . . ? C1 C2 P2 109.7(6) . . ? C2 P2 C41 116.6(3) . . ? C2 P2 C31 88.7(4) . . ? C41 P2 C31 99.5(2) . . ? C2 P2 Rh 108.0(3) . . ? C41 P2 Rh 118.70(14) . . ? C31 P2 Rh 122.0(2) . . ? C1' P1' C21 101.1(4) . . ? C1' P1' C11 106.2(4) . . ? C21 P1' C11 102.8(2) . . ? C1' P1' Rh 105.7(3) . . ? C21 P1' Rh 114.7(2) . . ? C11 P1' Rh 123.9(2) . . ? C2' C1' P1' 103.4(7) . . ? C1' C2' P2' 109.1(6) . . ? C41 P2' C31 99.5(2) . . ? C41 P2' C2' 98.7(3) . . ? C31 P2' C2' 110.9(4) . . ? C41 P2' Rh 118.70(14) . . ? C31 P2' Rh 122.0(2) . . ? C2' P2' Rh 104.7(3) . . ? C4 C3 C7 107.5(4) . . ? C4 C3 C3A 125.4(5) . . ? C7 C3 C3A 126.3(4) . . ? C4 C3 Rh 70.8(2) . . ? C7 C3 Rh 69.6(2) . . ? C3A C3 Rh 133.1(3) . . ? C3 C4 C5 108.7(4) . . ? C3 C4 C4A 125.0(5) . . ? C5 C4 C4A 124.8(4) . . ? C3 C4 Rh 72.0(2) . . ? C5 C4 Rh 73.3(3) . . ? C4A C4 Rh 131.9(3) . . ? C6 C5 C4 107.4(4) . . ? C6 C5 C5A 123.7(5) . . ? C4 C5 C5A 127.3(5) . . ? C6 C5 Rh 70.8(2) . . ? C4 C5 Rh 69.3(2) . . ? C5A C5 Rh 136.4(3) . . ? C5 C6 C7 108.6(4) . . ? C5 C6 C6A 126.5(5) . . ? C7 C6 C6A 124.8(5) . . ? C5 C6 Rh 72.8(3) . . ? C7 C6 Rh 69.1(2) . . ? C6A C6 Rh 126.7(4) . . ? C3 C7 C6 107.7(4) . . ? C3 C7 C7A 127.3(4) . . ? C6 C7 C7A 124.3(5) . . ? C3 C7 Rh 72.6(2) . . ? C6 C7 Rh 73.0(2) . . ? C7A C7 Rh 127.5(4) . . ? C16 C11 C12 114.0(4) . . ? C16 C11 P1 123.3(4) . . ? C12 C11 P1 122.1(4) . . ? C16 C11 P1' 123.3(4) . . ? C12 C11 P1' 122.1(4) . . ? F12 C12 C13 117.8(6) . . ? F12 C12 C11 118.5(4) . . ? C13 C12 C11 123.6(6) . . ? C12 C13 C14 119.4(6) . . ? C13 C14 C15 120.3(5) . . ? C16 C15 C14 117.7(6) . . ? F16 C16 C15 116.6(5) . . ? F16 C16 C11 118.5(4) . . ? C15 C16 C11 124.9(6) . . ? C26 C21 C22 113.5(5) . . ? C26 C21 P1 120.2(4) . . ? C22 C21 P1 126.3(5) . . ? C26 C21 P1' 120.2(4) . . ? C22 C21 P1' 126.3(5) . . ? F22 C22 C23 118.3(6) . . ? F22 C22 C21 119.2(6) . . ? C23 C22 C21 122.5(7) . . ? C24 C23 C22 119.8(6) . . ? C23 C24 C25 121.0(7) . . ? C24 C25 C26 117.7(7) . . ? F26 C26 C25 116.5(6) . . ? F26 C26 C21 118.0(4) . . ? C25 C26 C21 125.4(6) . . ? C32 C31 C36 113.5(5) . . ? C32 C31 P2' 126.0(4) . . ? C36 C31 P2' 120.5(5) . . ? C32 C31 P2 126.0(4) . . ? C36 C31 P2 120.5(5) . . ? F32 C32 C33 116.3(6) . . ? F32 C32 C31 119.3(5) . . ? C33 C32 C31 124.3(5) . . ? C34 C33 C32 118.5(7) . . ? C35 C34 C33 120.7(6) . . ? C36 C35 C34 118.7(6) . . ? F36 C36 C35 117.8(6) . . ? F36 C36 C31 117.8(6) . . ? C35 C36 C31 124.3(8) . . ? C46 C41 C42 113.2(4) . . ? C46 C41 P2 118.7(3) . . ? C42 C41 P2 128.1(4) . . ? C46 C41 P2' 118.7(3) . . ? C42 C41 P2' 128.1(4) . . ? F42 C42 C43 117.2(5) . . ? F42 C42 C41 118.8(5) . . ? C43 C42 C41 124.0(5) . . ? C44 C43 C42 119.5(5) . . ? C45 C44 C43 119.6(5) . . ? C44 C45 C46 118.9(5) . . ? F46 C46 C45 118.4(4) . . ? F46 C46 C41 116.8(4) . . ? C45 C46 C41 124.8(5) . . ? O C9 C10 123.4(8) . . ? O C9 C8 119.4(8) . . ? C10 C9 C8 117.2(6) . . ? F2 B F3A 118.3(6) . . ? F2 B F4 120.3(5) . . ? F3A B F4 121.2(5) . . ? F2 B F1 113.3(7) . . ? F3A B F1 66.4(6) . . ? F4 B F1 95.0(5) . . ? F2 B F2A 53.7(6) . . ? F3A B F2A 108.4(6) . . ? F4 B F2A 101.1(5) . . ? F1 B F2A 163.2(6) . . ? F2 B F3 112.0(7) . . ? F3A B F3 41.9(4) . . ? F4 B F3 107.7(6) . . ? F1 B F3 106.8(7) . . ? F2A B F3 73.1(6) . . ? F2 B F1A 51.1(6) . . ? F3A B F1A 107.8(6) . . ? F4 B F1A 112.2(5) . . ? F1 B F1A 63.9(5) . . ? F2A B F1A 104.8(7) . . ? F3 B F1A 139.5(6) . . ? B F1 F1A 60.0(4) . . ? B F1 F3A 56.4(4) . . ? F1A F1 F3A 98.3(5) . . ? F1A F2 F2A 137.4(8) . . ? F1A F2 B 70.3(6) . . ? F2A F2 B 67.2(6) . . ? F3A F3 B 66.8(6) . . ? F3A F3 F2A 112.3(8) . . ? B F3 F2A 53.4(5) . . ? F2 F1A B 58.6(5) . . ? F2 F1A F1 112.9(6) . . ? B F1A F1 56.0(4) . . ? F2 F2A B 59.1(5) . . ? F2 F2A F3 100.5(6) . . ? B F2A F3 53.5(4) . . ? F3 F3A B 71.2(7) . . ? F3 F3A F1 125.9(8) . . ? B F3A F1 57.2(4) . . ? _refine_diff_density_max 0.966 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.099 #=END