Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Russell Hughes Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; _publ_contact_author_phone '+603 646 2763' _publ_contact_author_fax '+603 646 3946' _publ_contact_author_email rph@dartmouth.edu _publ_requested_journal 'J Chem Soc Dalton Trans' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Water, water, everywhere. Synthesis and Structures of Perfluoroalkyliridium(III) Compounds Containing Water Ligands. ; loop_ _publ_author_name _publ_author_address 'Hughes, Russell P.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Lindner, Danielle C.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Smith, Jeremy M.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Zhang, Donghui' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Incarvito, Christopher ' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Liable-Sands, Louise M.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Lam, Kin-Chung' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Sommer, Roger' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Rheingold, Arnold L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; # 3. Results data_rph50 _database_code_CSD 164768 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16.50 H27 B Cl F11 O P Rh' _chemical_formula_weight 630.52 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.70290(10) _cell_length_b 13.70290(10) _cell_length_c 25.88380(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4860.19(5) _cell_formula_units_Z 8 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method ? _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29356 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.45 _reflns_number_total 5929 _reflns_number_observed 4773 _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 1 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^)+(0.0300P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 5928 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_obs 0.0426 _refine_ls_wR_factor_all 0.0806 _refine_ls_wR_factor_obs 0.0737 _refine_ls_goodness_of_fit_all 1.091 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.120 _refine_ls_shift/esd_max 0.072 _refine_ls_shift/esd_mean 0.007 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 -0.27724(2) 0.80056(2) 0.745032(10) 0.03133(8) Uani 1 d . . P P -0.24224(8) 0.74773(9) 0.66106(4) 0.0518(3) Uani 1 d . . F1 F -0.2398(4) 1.0201(3) 0.7833(2) 0.129(2) Uani 1 d . . F2 F -0.3902(3) 1.0171(2) 0.79151(14) 0.112(2) Uani 1 d . . F3 F -0.3262(3) 1.1093(2) 0.73721(14) 0.1145(14) Uani 1 d . . F4 F -0.2605(2) 0.9737(2) 0.67995(9) 0.0574(7) Uani 1 d . . F5 F -0.4263(2) 0.8759(3) 0.65354(12) 0.0919(12) Uani 1 d . . F6 F -0.4475(3) 1.0236(3) 0.6700(2) 0.1072(13) Uani 1 d . . F7 F -0.4951(2) 0.9187(3) 0.72269(14) 0.0860(10) Uani 1 d . . F8 F 0.0204(6) 1.0372(5) 0.8245(3) 0.095(3) Uani 0.617(12) d P . F8' F 0.1036(9) 1.0099(8) 0.8351(5) 0.089(5) Uani 0.383(12) d P . F9 F 0.1265(4) 0.9394(7) 0.8634(3) 0.097(3) Uani 0.617(12) d P . F9' F 0.0406(10) 0.8678(6) 0.8602(4) 0.080(4) Uani 0.383(12) d P . F10 F -0.0142(5) 0.8816(5) 0.8344(3) 0.089(3) Uani 0.617(12) d P . F10' F -0.0490(8) 0.9839(9) 0.8217(4) 0.087(5) Uani 0.383(12) d P . F11 F -0.0050(3) 0.9895(3) 0.90354(12) 0.1107(12) Uani 1 d . . O O -0.1284(2) 0.8614(3) 0.7451(2) 0.0577(9) Uani 1 d . . H1 H -0.0966(49) 0.8815(48) 0.7241(25) 0.098(27) Uiso 1 d . . H2 H -0.1090(44) 0.8843(44) 0.7693(22) 0.080(22) Uiso 1 d . . C1 C -0.3934(3) 0.7092(3) 0.77217(14) 0.0404(9) Uani 1 d . . C2 C -0.3801(3) 0.7819(3) 0.81182(15) 0.0434(10) Uani 1 d . . C3 C -0.2850(3) 0.7755(3) 0.82930(13) 0.0489(10) Uani 1 d . . C4 C -0.2390(4) 0.6933(3) 0.8046(2) 0.0552(11) Uani 1 d . . C5 C -0.3073(3) 0.6496(3) 0.7721(2) 0.0492(11) Uani 1 d . . C6 C -0.4886(3) 0.6819(3) 0.7478(2) 0.0587(12) Uani 1 d . . H6A H -0.5354(3) 0.7341(3) 0.7530(2) 0.088 Uiso 1 calc R . H6B H -0.5130(3) 0.6224(3) 0.7635(2) 0.088 Uiso 1 calc R . H6C H -0.4791(3) 0.6715(3) 0.7110(2) 0.088 Uiso 1 calc R . C7 C -0.4611(4) 0.8411(4) 0.8351(2) 0.072(2) Uani 1 d . . H7A H -0.5202(4) 0.8319(4) 0.8150(2) 0.108 Uiso 1 calc R . H7B H -0.4432(4) 0.9095(4) 0.8349(2) 0.108 Uiso 1 calc R . H7C H -0.4723(4) 0.8200(4) 0.8703(2) 0.108 Uiso 1 calc R . C8 C -0.2414(5) 0.8362(4) 0.8715(2) 0.081(2) Uani 1 d . . H8A H -0.1737(5) 0.8178(4) 0.8764(2) 0.122 Uiso 1 calc R . H8B H -0.2772(5) 0.8255(4) 0.9033(2) 0.122 Uiso 1 calc R . H8C H -0.2450(5) 0.9046(4) 0.8620(2) 0.122 Uiso 1 calc R . C9 C -0.1384(5) 0.6576(5) 0.8165(2) 0.100(2) Uani 1 d . . H9A H -0.1070(5) 0.7024(5) 0.8403(2) 0.150 Uiso 1 calc R . H9B H -0.1007(5) 0.6540(5) 0.7848(2) 0.150 Uiso 1 calc R . H9C H -0.1421(5) 0.5934(5) 0.8321(2) 0.150 Uiso 1 calc R . C10 C -0.3012(4) 0.5496(3) 0.7497(2) 0.083(2) Uani 1 d . . H10A H -0.3583(4) 0.5373(3) 0.7286(2) 0.124 Uiso 1 calc R . H10B H -0.2984(4) 0.5020(3) 0.7775(2) 0.124 Uiso 1 calc R . H10C H -0.2429(4) 0.5444(3) 0.7287(2) 0.124 Uiso 1 calc R . C11 C -0.3215(4) 1.0198(3) 0.7568(2) 0.0662(14) Uani 1 d . . C12 C -0.3246(3) 0.9383(3) 0.7182(2) 0.0431(10) Uani 1 d . . C13 C -0.4242(4) 0.9400(4) 0.6915(2) 0.0554(12) Uani 1 d . . C14 C -0.1324(4) 0.6757(5) 0.6640(2) 0.098(2) Uani 1 d . . H14A H -0.0811(4) 0.7134(5) 0.6804(2) 0.147 Uiso 1 calc R . H14B H -0.1125(4) 0.6580(5) 0.6293(2) 0.147 Uiso 1 calc R . H14C H -0.1446(4) 0.6170(5) 0.6840(2) 0.147 Uiso 1 calc R . C15 C -0.2136(4) 0.8314(4) 0.6089(2) 0.080(2) Uani 1 d . . H15A H -0.2685(4) 0.8749(4) 0.6032(2) 0.120 Uiso 1 calc R . H15B H -0.2008(4) 0.7947(4) 0.5775(2) 0.120 Uiso 1 calc R . H15C H -0.1564(4) 0.8694(4) 0.6179(2) 0.120 Uiso 1 calc R . C16 C -0.3301(4) 0.6688(4) 0.6301(2) 0.0706(15) Uani 1 d . . H16A H -0.3919(4) 0.7027(4) 0.6269(2) 0.106 Uiso 1 calc R . H16B H -0.3389(4) 0.6104(4) 0.6507(2) 0.106 Uiso 1 calc R . H16C H -0.3066(4) 0.6510(4) 0.5960(2) 0.106 Uiso 1 calc R . C17 C -0.3364(3) 0.6636(3) 1.0000 0.077(2) Uani 1 d S . H17A H -0.3718(3) 0.6391(3) 0.9697 0.093 Uiso 1 calc R . Cl1 Cl -0.21572(11) 0.63689(15) 0.99257(9) 0.1148(6) Uani 1 d . . B B 0.0268(4) 0.9619(4) 0.8573(2) 0.0487(12) 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 Rh 0.0279(2) 0.0350(2) 0.03111(13) -0.00476(13) -0.00196(12) -0.00105(10) P 0.0436(7) 0.0679(9) 0.0439(6) -0.0235(5) 0.0041(5) 0.0002(6) F1 0.150(4) 0.082(3) 0.155(4) -0.068(3) -0.056(3) 0.004(3) F2 0.181(4) 0.068(2) 0.087(2) -0.019(2) 0.074(3) -0.015(3) F3 0.197(4) 0.032(2) 0.115(3) 0.005(2) 0.045(3) 0.000(2) F4 0.064(2) 0.056(2) 0.0531(15) 0.0107(12) 0.0169(13) -0.0165(13) F5 0.076(2) 0.121(3) 0.079(2) -0.022(2) -0.037(2) 0.025(2) F6 0.091(3) 0.087(3) 0.144(3) 0.065(2) -0.011(2) 0.016(2) F7 0.041(2) 0.118(3) 0.099(2) 0.035(2) 0.014(2) 0.011(2) F8 0.106(8) 0.089(5) 0.091(4) 0.041(4) 0.017(5) -0.013(5) F8' 0.078(8) 0.077(8) 0.112(8) 0.004(7) 0.031(7) -0.029(7) F9 0.051(4) 0.139(8) 0.101(5) -0.024(5) -0.016(3) 0.012(4) F9' 0.112(11) 0.040(5) 0.088(7) 0.022(5) 0.001(7) 0.002(5) F10 0.084(5) 0.076(5) 0.106(5) -0.005(4) -0.018(4) -0.030(4) F10' 0.091(9) 0.088(10) 0.084(6) -0.017(6) -0.047(6) 0.019(7) F11 0.126(3) 0.152(4) 0.054(2) -0.003(2) 0.021(2) 0.048(2) O 0.039(2) 0.085(3) 0.050(2) -0.009(2) 0.000(2) -0.017(2) C1 0.040(2) 0.037(2) 0.045(2) 0.008(2) -0.006(2) -0.011(2) C2 0.052(3) 0.041(2) 0.037(2) 0.007(2) 0.014(2) -0.006(2) C3 0.062(3) 0.054(3) 0.031(2) 0.007(2) -0.011(2) -0.016(3) C4 0.056(3) 0.053(3) 0.057(2) 0.015(2) -0.020(2) 0.000(2) C5 0.062(3) 0.033(2) 0.053(2) 0.004(2) -0.012(2) -0.003(2) C6 0.049(3) 0.054(3) 0.073(3) 0.011(3) -0.010(3) -0.021(2) C7 0.083(4) 0.071(4) 0.063(3) 0.008(3) 0.038(3) -0.003(3) C8 0.113(5) 0.098(4) 0.033(2) -0.002(3) -0.013(3) -0.031(4) C9 0.081(5) 0.107(5) 0.112(5) 0.022(4) -0.052(4) 0.029(4) C10 0.100(4) 0.037(2) 0.112(4) -0.007(3) -0.013(5) 0.006(3) C11 0.086(4) 0.040(3) 0.073(3) -0.004(3) 0.009(3) -0.007(2) C12 0.044(3) 0.045(2) 0.040(2) 0.006(2) 0.010(2) -0.006(2) C13 0.050(3) 0.049(3) 0.067(3) 0.022(3) 0.002(3) 0.009(2) C14 0.066(4) 0.119(6) 0.108(5) -0.049(4) 0.008(4) 0.034(4) C15 0.083(4) 0.107(5) 0.049(3) -0.017(3) 0.025(3) -0.020(4) C16 0.080(4) 0.072(4) 0.060(3) -0.027(3) -0.012(3) -0.011(3) C17 0.062(3) 0.062(3) 0.107(6) 0.003(4) -0.003(4) -0.015(3) Cl1 0.0581(9) 0.1286(14) 0.158(2) -0.0206(14) 0.0000(11) -0.0027(9) B 0.053(4) 0.043(3) 0.050(3) -0.001(3) 0.002(3) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C12 2.113(4) . ? Rh C1 2.143(4) . ? Rh C4 2.193(4) . ? Rh O 2.203(3) . ? Rh C3 2.210(3) . ? Rh C5 2.223(4) . ? Rh C2 2.245(4) . ? Rh P 2.3406(10) . ? P C14 1.801(6) . ? P C16 1.806(4) . ? P C15 1.815(5) . ? F1 C11 1.313(6) . ? F2 C11 1.302(6) . ? F3 C11 1.329(5) . ? F4 C12 1.409(4) . ? F5 C13 1.318(6) . ? F6 C13 1.312(5) . ? F7 C13 1.297(5) . ? F8 F10' 1.201(11) . ? F8 F8' 1.230(13) . ? F8 B 1.339(8) . ? F8' F9 1.253(12) . ? F8' B 1.368(10) . ? F9 B 1.409(8) . ? F9 F9' 1.535(12) . ? F9' F10 1.023(10) . ? F9' B 1.305(10) . ? F10 B 1.369(8) . ? F10 F10' 1.516(11) . ? F10' B 1.422(10) . ? F11 B 1.328(6) . ? C1 C5 1.435(6) . ? C1 C2 1.442(6) . ? C1 C6 1.497(5) . ? C2 C3 1.382(6) . ? C2 C7 1.500(7) . ? C3 C4 1.441(6) . ? C3 C8 1.496(6) . ? C4 C5 1.394(6) . ? C4 C9 1.495(7) . ? C5 C10 1.489(6) . ? C11 C12 1.500(7) . ? C12 C13 1.529(7) . ? C17 Cl1 1.705(4) 7_467 ? C17 Cl1 1.705(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 C12 Rh C1 113.7(2) . . ? C12 Rh C4 154.6(2) . . ? C1 Rh C4 63.6(2) . . ? C12 Rh O 86.9(2) . . ? C1 Rh O 155.2(2) . . ? C4 Rh O 91.8(2) . . ? C12 Rh C3 116.6(2) . . ? C1 Rh C3 63.28(15) . . ? C4 Rh C3 38.2(2) . . ? O Rh C3 95.8(2) . . ? C12 Rh C5 151.4(2) . . ? C1 Rh C5 38.3(2) . . ? C4 Rh C5 36.8(2) . . ? O Rh C5 121.6(2) . . ? C3 Rh C5 62.3(2) . . ? C12 Rh C2 99.3(2) . . ? C1 Rh C2 38.28(15) . . ? C4 Rh C2 62.1(2) . . ? O Rh C2 128.5(2) . . ? C3 Rh C2 36.1(2) . . ? C5 Rh C2 62.3(2) . . ? C12 Rh P 91.93(12) . . ? C1 Rh P 106.01(11) . . ? C4 Rh P 113.34(14) . . ? O Rh P 85.90(12) . . ? C3 Rh P 151.42(13) . . ? C5 Rh P 92.44(12) . . ? C2 Rh P 143.95(11) . . ? C14 P C16 104.3(3) . . ? C14 P C15 101.4(3) . . ? C16 P C15 101.1(2) . . ? C14 P Rh 107.5(2) . . ? C16 P Rh 117.4(2) . . ? C15 P Rh 122.7(2) . . ? F10' F8 F8' 124.2(9) . . ? F10' F8 B 67.8(6) . . ? F8' F8 B 64.2(6) . . ? F8 F8' F9 126.6(8) . . ? F8 F8' B 61.8(6) . . ? F9 F8' B 64.8(6) . . ? F8' F9 B 61.5(5) . . ? F8' F9 F9' 105.6(7) . . ? B F9 F9' 52.4(5) . . ? F10 F9' B 70.9(7) . . ? F10 F9' F9 118.6(9) . . ? B F9' F9 58.8(5) . . ? F9' F10 B 64.2(6) . . ? F9' F10 F10' 123.0(8) . . ? B F10 F10' 58.8(5) . . ? F8 F10' B 60.7(6) . . ? F8 F10' F10 107.4(8) . . ? B F10' F10 55.4(4) . . ? C5 C1 C2 106.9(3) . . ? C5 C1 C6 125.0(4) . . ? C2 C1 C6 125.7(4) . . ? C5 C1 Rh 73.9(2) . . ? C2 C1 Rh 74.7(2) . . ? C6 C1 Rh 130.9(3) . . ? C3 C2 C1 108.0(4) . . ? C3 C2 C7 126.9(4) . . ? C1 C2 C7 124.4(4) . . ? C3 C2 Rh 70.6(2) . . ? C1 C2 Rh 67.0(2) . . ? C7 C2 Rh 135.4(3) . . ? C2 C3 C4 108.5(4) . . ? C2 C3 C8 125.5(5) . . ? C4 C3 C8 125.7(5) . . ? C2 C3 Rh 73.3(2) . . ? C4 C3 Rh 70.2(2) . . ? C8 C3 Rh 127.9(3) . . ? C5 C4 C3 108.1(4) . . ? C5 C4 C9 127.1(5) . . ? C3 C4 C9 124.6(4) . . ? C5 C4 Rh 72.8(2) . . ? C3 C4 Rh 71.6(2) . . ? C9 C4 Rh 125.8(4) . . ? C4 C5 C1 107.8(4) . . ? C4 C5 C10 126.3(4) . . ? C1 C5 C10 124.8(4) . . ? C4 C5 Rh 70.4(2) . . ? C1 C5 Rh 67.8(2) . . ? C10 C5 Rh 136.3(4) . . ? F2 C11 F1 104.9(5) . . ? F2 C11 F3 104.7(4) . . ? F1 C11 F3 103.8(5) . . ? F2 C11 C12 114.7(4) . . ? F1 C11 C12 112.0(4) . . ? F3 C11 C12 115.6(5) . . ? F4 C12 C11 101.2(3) . . ? F4 C12 C13 103.5(3) . . ? C11 C12 C13 108.4(4) . . ? F4 C12 Rh 110.3(3) . . ? C11 C12 Rh 115.9(3) . . ? C13 C12 Rh 115.9(3) . . ? F7 C13 F6 106.1(4) . . ? F7 C13 F5 107.3(5) . . ? F6 C13 F5 105.1(4) . . ? F7 C13 C12 112.6(4) . . ? F6 C13 C12 115.0(4) . . ? F5 C13 C12 110.3(4) . . ? Cl1 C17 Cl1 115.4(4) 7_467 . ? F9' B F11 106.1(6) . . ? F9' B F8 143.8(7) . . ? F11 B F8 109.2(5) . . ? F9' B F8' 112.8(8) . . ? F11 B F8' 119.6(7) . . ? F8 B F8' 54.0(6) . . ? F9' B F10 44.9(5) . . ? F11 B F10 119.0(5) . . ? F8 B F10 108.5(6) . . ? F8' B F10 121.3(6) . . ? F9' B F9 68.7(7) . . ? F11 B F9 106.2(5) . . ? F8 B F9 107.6(6) . . ? F8' B F9 53.6(6) . . ? F10 B F9 105.7(6) . . ? F9' B F10' 110.7(8) . . ? F11 B F10' 106.5(6) . . ? F8 B F10' 51.4(5) . . ? F8' B F10' 100.7(8) . . ? F10 B F10' 65.8(5) . . ? F9 B F10' 145.8(7) . . ? _refine_diff_density_max 0.393 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.108 #===END data_rph69 _database_code_CSD 164769 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16.50 H27 B Cl F11 Ir O P' _chemical_formula_weight 719.81 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.7243(4) _cell_length_b 13.7243(4) _cell_length_c 26.0997(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4916.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method ? _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 5.696 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15628 _diffrn_reflns_av_R_equivalents 0.1173 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3857 _reflns_number_observed 2863 _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 13 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^)+(0.0300P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 3844 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_obs 0.0517 _refine_ls_wR_factor_all 0.1004 _refine_ls_wR_factor_obs 0.0868 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.091 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.045 _refine_ls_shift/esd_mean 0.003 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 0.30037(4) 0.77736(4) -0.00438(2) 0.0387(2) Uani 1 d . . P1 P 0.2481(4) 0.7410(3) -0.0872(2) 0.0679(13) Uani 1 d . . O1 O 0.3643(7) 0.6263(6) -0.0038(4) 0.062(3) Uani 1 d . . F1 F 0.4754(6) 0.7566(7) -0.0688(3) 0.072(3) Uani 1 d . . F2 F 0.6113(7) 0.8217(10) -0.0114(4) 0.129(5) Uani 1 d . . F3 F 0.5197(8) 0.8837(11) 0.0425(5) 0.125(5) Uani 1 d . . F4 F 0.5210(9) 0.7339(10) 0.0343(5) 0.132(5) Uani 1 d . . F5 F 0.4200(8) 0.9920(7) -0.0266(4) 0.093(4) Uani 1 d . . F6 F 0.5302(9) 0.9423(8) -0.0767(6) 0.124(5) Uani 1 d . . F7 F 0.3800(10) 0.9247(9) -0.0965(5) 0.107(4) Uani 1 d . . C1 C 0.2744(12) 0.7851(13) 0.0796(5) 0.064(5) Uani 1 d . . C2 C 0.1961(11) 0.7401(12) 0.0540(6) 0.055(4) Uani 1 d . . C3 C 0.1496(9) 0.8034(14) 0.0247(6) 0.064(5) Uani 1 d . . C4 C 0.2074(11) 0.8957(10) 0.0230(5) 0.054(4) Uani 1 d . . C5 C 0.2843(11) 0.8831(11) 0.0613(5) 0.047(4) Uani 1 d . . C6 C 0.3377(13) 0.7367(14) 0.1231(5) 0.094(7) Uani 1 d . . H6A H 0.3848(13) 0.7842(14) 0.1362(5) 0.140 Uiso 1 calc R . H6B H 0.3726(13) 0.6803(14) 0.1091(5) 0.140 Uiso 1 calc R . H6C H 0.2951(13) 0.7153(14) 0.1511(5) 0.140 Uiso 1 calc R . C7 C 0.1602(14) 0.6375(15) 0.0666(7) 0.101(8) Uani 1 d . . H7A H 0.2073(14) 0.6053(15) 0.0892(7) 0.151 Uiso 1 calc R . H7B H 0.1534(14) 0.6000(15) 0.0349(7) 0.151 Uiso 1 calc R . H7C H 0.0969(14) 0.6416(15) 0.0839(7) 0.151 Uiso 1 calc R . C8 C 0.0482(10) 0.8050(13) 0.0012(8) 0.099(7) Uani 1 d . . H8A H 0.0403(10) 0.8643(13) -0.0193(8) 0.148 Uiso 1 calc R . H8B H -0.0007(10) 0.8040(13) 0.0285(8) 0.148 Uiso 1 calc R . H8C H 0.0397(10) 0.7478(13) -0.0208(8) 0.148 Uiso 1 calc R . C9 C 0.1813(10) 0.9882(10) -0.0001(7) 0.066(5) Uani 1 d . . H9A H 0.1273(10) 0.9785(10) -0.0242(7) 0.099 Uiso 1 calc R . H9B H 0.2377(10) 1.0146(10) -0.0185(7) 0.099 Uiso 1 calc R . H9C H 0.1613(10) 1.0341(10) 0.0267(7) 0.099 Uiso 1 calc R . C10 C 0.3428(14) 0.9640(13) 0.0834(7) 0.084(7) Uani 1 d . . H10A H 0.3366(14) 1.0218(13) 0.0616(7) 0.126 Uiso 1 calc R . H10B H 0.4114(14) 0.9444(13) 0.0852(7) 0.126 Uiso 1 calc R . H10C H 0.3189(14) 0.9791(13) 0.1179(7) 0.126 Uiso 1 calc R . C11 C 0.4378(11) 0.8176(10) -0.0313(6) 0.050(4) Uani 1 d . . C12 C 0.5213(11) 0.8152(16) 0.0087(7) 0.070(5) Uani 1 d . . C13 C 0.4458(14) 0.9172(15) -0.0573(9) 0.076(6) Uani 1 d . . C14 C 0.1696(15) 0.8287(15) -0.1185(6) 0.084(6) Uani 1 d . . H14A H 0.2031(15) 0.8916(15) -0.1207(6) 0.126 Uiso 1 calc R . H14B H 0.1095(15) 0.8362(15) -0.0987(6) 0.126 Uiso 1 calc R . H14C H 0.1538(15) 0.8057(15) -0.1531(6) 0.126 Uiso 1 calc R . C15 C 0.3302(14) 0.7089(14) -0.1396(6) 0.099(8) Uani 1 d . . H15A H 0.3781(14) 0.6612(14) -0.1275(6) 0.148 Uiso 1 calc R . H15B H 0.3640(14) 0.7675(14) -0.1516(6) 0.148 Uiso 1 calc R . H15C H 0.2925(14) 0.6807(14) -0.1679(6) 0.148 Uiso 1 calc R . C16 C 0.1730(18) 0.6296(13) -0.0856(8) 0.129(10) Uani 1 d . . H16A H 0.2096(18) 0.5772(13) -0.0688(8) 0.193 Uiso 1 calc R . H16B H 0.1565(18) 0.6101(13) -0.1206(8) 0.193 Uiso 1 calc R . H16C H 0.1130(18) 0.6424(13) -0.0663(8) 0.193 Uiso 1 calc R . B11 B 0.4718(16) 0.4623(22) -0.1047(8) 0.059(6) Uani 1 d . . F11 F 0.5073(10) 0.4891(11) -0.1507(4) 0.129(4) Uani 1 d . . F12 F 0.4752(25) 0.5304(21) -0.0713(10) 0.111(10) Uani 0.55 d P 1 F13 F 0.3732(21) 0.4371(23) -0.1101(11) 0.101(10) Uani 0.55 d P 1 F14 F 0.5199(20) 0.3872(23) -0.0814(11) 0.102(10) Uani 0.55 d P 1 F12' F 0.5425(28) 0.4915(27) -0.0676(14) 0.134(16) Uani 0.45 d P 2 F13' F 0.3907(23) 0.5043(31) -0.0928(16) 0.113(11) Uani 0.45 d P 2 F14' F 0.4644(45) 0.3669(25) -0.1084(17) 0.160(22) Uani 0.45 d P 2 C21 C 0.3375(11) 0.3375(11) 0.0000 0.103(10) Uani 1 d S . H21A H 0.3626(11) 0.3728(11) 0.0304 0.123 Uiso 1 calc R . H21B H 0.3728(11) 0.3625(11) -0.0304 0.123 Uiso 0.00 calc PR . Cl21 Cl 0.2156(3) 0.3642(4) -0.0069(3) 0.125(2) 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 Ir1 0.0448(3) 0.0364(3) 0.0350(3) 0.0030(3) -0.0065(3) 0.0005(2) P1 0.091(4) 0.053(3) 0.060(3) -0.006(2) -0.034(2) 0.003(2) O1 0.093(8) 0.042(6) 0.049(7) 0.004(6) -0.008(8) 0.014(4) F1 0.073(6) 0.086(7) 0.059(6) -0.019(5) 0.016(5) 0.019(5) F2 0.043(6) 0.228(14) 0.115(10) -0.026(11) 0.005(6) 0.002(7) F3 0.083(9) 0.207(15) 0.084(9) -0.070(10) -0.017(7) -0.005(9) F4 0.114(10) 0.124(11) 0.158(13) 0.028(10) -0.091(9) -0.011(8) F5 0.126(9) 0.052(6) 0.100(10) -0.007(6) 0.043(7) -0.014(6) F6 0.103(10) 0.114(10) 0.156(13) 0.020(9) 0.084(9) -0.016(7) F7 0.151(12) 0.093(9) 0.076(9) 0.045(7) -0.009(9) -0.028(8) C1 0.065(11) 0.100(14) 0.026(7) 0.010(9) 0.014(8) 0.052(12) C2 0.031(8) 0.076(11) 0.059(10) 0.024(9) -0.010(8) -0.010(7) C3 0.024(8) 0.097(14) 0.071(12) -0.011(10) 0.004(7) 0.023(10) C4 0.067(11) 0.044(9) 0.051(10) 0.020(7) 0.003(9) 0.030(9) C5 0.056(10) 0.059(10) 0.026(8) 0.002(7) 0.013(8) 0.024(9) C6 0.142(18) 0.110(17) 0.029(10) 0.012(10) -0.019(10) 0.037(13) C7 0.101(17) 0.125(19) 0.076(14) 0.055(14) 0.010(12) -0.049(14) C8 0.050(9) 0.113(15) 0.133(18) 0.064(18) -0.014(13) -0.010(9) C9 0.068(10) 0.074(10) 0.056(11) -0.010(11) 0.026(11) 0.029(8) C10 0.098(16) 0.087(14) 0.067(14) -0.048(12) 0.006(11) -0.013(12) C11 0.061(10) 0.042(9) 0.046(10) 0.006(8) 0.025(8) 0.032(8) C12 0.047(10) 0.110(15) 0.054(13) -0.010(14) -0.001(10) 0.007(10) C13 0.060(13) 0.090(15) 0.079(16) -0.011(13) 0.028(13) -0.023(10) C14 0.106(16) 0.098(15) 0.048(11) -0.002(11) -0.032(11) 0.033(10) C15 0.143(19) 0.107(17) 0.046(11) -0.034(11) -0.030(11) 0.039(15) C16 0.198(26) 0.067(14) 0.121(19) 0.003(13) -0.091(19) -0.069(15) B11 0.037(15) 0.095(21) 0.044(14) 0.029(15) 0.020(11) 0.006(11) F11 0.159(16) 0.153(16) 0.075(8) 0.008(8) 0.024(8) -0.044(8) F12 0.121(27) 0.141(24) 0.071(17) -0.043(16) -0.032(16) 0.068(18) F13 0.094(21) 0.097(20) 0.112(21) -0.031(17) -0.036(15) -0.017(17) F14 0.089(19) 0.072(22) 0.145(25) -0.004(17) -0.029(17) 0.027(15) F12' 0.128(29) 0.107(26) 0.167(32) 0.072(24) -0.106(26) -0.061(21) F13' 0.053(22) 0.157(36) 0.130(32) 0.030(27) 0.008(21) 0.037(22) F14' 0.277(60) 0.054(22) 0.148(37) -0.023(24) 0.149(38) -0.083(32) C21 0.084(11) 0.084(11) 0.140(28) -0.021(18) 0.021(18) -0.026(13) Cl21 0.066(3) 0.147(5) 0.163(6) 0.025(5) 0.004(5) -0.005(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 Ir1 C11 2.087(15) . ? Ir1 C2 2.151(14) . ? Ir1 C4 2.186(13) . ? Ir1 C3 2.232(12) . ? Ir1 C1 2.224(12) . ? Ir1 C5 2.257(13) . ? Ir1 O1 2.251(7) . ? Ir1 P1 2.332(4) . ? P1 C14 1.809(14) . ? P1 C16 1.84(2) . ? P1 C15 1.83(2) . ? F1 C11 1.389(14) . ? F2 C12 1.34(2) . ? F3 C12 1.29(2) . ? F4 C12 1.30(2) . ? F5 C13 1.35(2) . ? F6 C13 1.31(2) . ? F7 C13 1.37(2) . ? C1 C2 1.41(2) . ? C1 C5 1.43(2) . ? C1 C6 1.58(2) . ? C2 C3 1.32(2) . ? C2 C7 1.53(2) . ? C3 C4 1.50(2) . ? C3 C8 1.52(2) . ? C4 C9 1.45(2) . ? C4 C5 1.46(2) . ? C5 C10 1.49(2) . ? C11 C13 1.53(2) . ? C11 C12 1.55(2) . ? B11 F12 1.28(3) . ? B11 F13' 1.29(4) . ? B11 F14' 1.32(4) . ? B11 F11 1.35(2) . ? B11 F13 1.40(3) . ? B11 F14 1.37(3) . ? B11 F12' 1.43(4) . ? C21 Cl21 1.722(12) . ? C21 Cl21 1.722(12) 7 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ir1 C2 154.4(6) . . ? C11 Ir1 C4 116.2(5) . . ? C2 Ir1 C4 63.7(5) . . ? C11 Ir1 C3 155.5(6) . . ? C2 Ir1 C3 35.0(5) . . ? C4 Ir1 C3 39.5(5) . . ? C11 Ir1 C1 117.6(7) . . ? C2 Ir1 C1 37.5(5) . . ? C4 Ir1 C1 63.2(5) . . ? C3 Ir1 C1 60.6(6) . . ? C11 Ir1 C5 100.0(6) . . ? C2 Ir1 C5 63.2(6) . . ? C4 Ir1 C5 38.4(5) . . ? C3 Ir1 C5 63.2(6) . . ? C1 Ir1 C5 37.3(5) . . ? C11 Ir1 O1 83.9(5) . . ? C2 Ir1 O1 92.1(5) . . ? C4 Ir1 O1 155.5(5) . . ? C3 Ir1 O1 120.4(6) . . ? C1 Ir1 O1 95.8(5) . . ? C5 Ir1 O1 128.7(4) . . ? C11 Ir1 P1 91.3(5) . . ? C2 Ir1 P1 113.7(5) . . ? C4 Ir1 P1 106.4(4) . . ? C3 Ir1 P1 93.7(4) . . ? C1 Ir1 P1 151.0(5) . . ? C5 Ir1 P1 144.3(4) . . ? O1 Ir1 P1 85.9(3) . . ? C14 P1 C16 103.2(10) . . ? C14 P1 C15 100.9(8) . . ? C16 P1 C15 99.3(11) . . ? C14 P1 Ir1 117.4(6) . . ? C16 P1 Ir1 109.1(7) . . ? C15 P1 Ir1 123.8(6) . . ? C2 C1 C5 109.0(13) . . ? C2 C1 C6 125.3(16) . . ? C5 C1 C6 125.7(17) . . ? C2 C1 Ir1 68.4(8) . . ? C5 C1 Ir1 72.6(7) . . ? C6 C1 Ir1 126.9(9) . . ? C3 C2 C1 110.8(15) . . ? C3 C2 C7 125.1(16) . . ? C1 C2 C7 123.2(15) . . ? C3 C2 Ir1 75.8(9) . . ? C1 C2 Ir1 74.1(8) . . ? C7 C2 Ir1 125.9(13) . . ? C2 C3 C4 108.5(13) . . ? C2 C3 C8 133.3(17) . . ? C4 C3 C8 117.4(15) . . ? C2 C3 Ir1 69.1(8) . . ? C4 C3 Ir1 68.6(7) . . ? C8 C3 Ir1 135.5(13) . . ? C9 C4 C5 124.4(15) . . ? C9 C4 C3 128.6(15) . . ? C5 C4 C3 105.2(11) . . ? C9 C4 Ir1 131.2(10) . . ? C5 C4 Ir1 73.4(7) . . ? C3 C4 Ir1 71.9(7) . . ? C1 C5 C4 105.7(14) . . ? C1 C5 C10 128.5(15) . . ? C4 C5 C10 124.5(14) . . ? C1 C5 Ir1 70.1(7) . . ? C4 C5 Ir1 68.2(8) . . ? C10 C5 Ir1 136.2(11) . . ? F1 C11 C13 101.4(12) . . ? F1 C11 C12 100.8(11) . . ? C13 C11 C12 105.4(16) . . ? F1 C11 Ir1 114.4(11) . . ? C13 C11 Ir1 116.8(10) . . ? C12 C11 Ir1 115.9(10) . . ? F4 C12 F3 106.0(17) . . ? F4 C12 F2 105.1(16) . . ? F3 C12 F2 103.5(16) . . ? F4 C12 C11 111.1(15) . . ? F3 C12 C11 115.6(15) . . ? F2 C12 C11 114.5(15) . . ? F6 C13 F7 106.1(17) . . ? F6 C13 F5 105.1(15) . . ? F7 C13 F5 102.3(17) . . ? F6 C13 C11 118.0(18) . . ? F7 C13 C11 110.6(15) . . ? F5 C13 C11 113.3(16) . . ? F13' B11 F14' 113.3(32) . . ? F12 B11 F11 113.3(26) . . ? F13' B11 F11 113.9(26) . . ? F14' B11 F11 103.4(24) . . ? F12 B11 F13 106.5(25) . . ? F11 B11 F13 109.0(21) . . ? F12 B11 F14 103.4(24) . . ? F11 B11 F14 115.3(24) . . ? F13 B11 F14 108.9(25) . . ? F13' B11 F12' 107.4(37) . . ? F14' B11 F12' 112.5(36) . . ? F11 B11 F12' 106.3(21) . . ? Cl21 C21 Cl21 115.1(13) . 7 ? _refine_diff_density_max 0.661 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.147 #===END data_rph111 _database_code_CSD 164770 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 F8 Ir O4 P S' _chemical_formula_weight 689.60 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8926(2) _cell_length_b 8.4162(2) _cell_length_c 32.0068(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.5855(5) _cell_angle_gamma 90.00 _cell_volume 4752.50(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 5.855 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details DIFABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20916 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8861 _reflns_number_gt 7782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8861 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.367 _refine_ls_restrained_S_all 1.367 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.740300(17) 0.25195(4) 0.249484(10) 0.01820(14) Uani 1 1 d . . . P1 P 0.86414(12) 0.2777(3) 0.28723(8) 0.0248(5) Uani 1 1 d . . . O1 O 0.7577(3) 0.4828(8) 0.22000(18) 0.0259(14) Uani 1 1 d . . . F1 F 0.7558(3) 0.5046(7) 0.31554(17) 0.0358(13) Uani 1 1 d . . . F2 F 0.6962(3) 0.2933(7) 0.33307(17) 0.0381(13) Uani 1 1 d . . . F3 F 0.6202(3) 0.5806(8) 0.32010(19) 0.0526(18) Uani 1 1 d . . . F4 F 0.5691(3) 0.3859(8) 0.28132(19) 0.0414(14) Uani 1 1 d . . . F5 F 0.6264(3) 0.5745(7) 0.25363(17) 0.0385(14) Uani 1 1 d . . . C1 C 0.7528(5) 0.0306(12) 0.2102(3) 0.027(2) Uani 1 1 d . . . C2 C 0.7290(5) -0.0054(11) 0.2497(3) 0.029(2) Uani 1 1 d . . . C3 C 0.6544(5) 0.0615(11) 0.2489(3) 0.0268(19) Uani 1 1 d . . . C4 C 0.6352(4) 0.1496(12) 0.2101(3) 0.026(2) Uani 1 1 d . . . C5 C 0.6978(5) 0.1274(10) 0.1870(3) 0.0239(18) Uani 1 1 d . . . C6 C 0.8191(6) -0.0488(13) 0.1937(3) 0.041(3) Uani 1 1 d . . . H6A H 0.8011 -0.1445 0.1777 0.062 Uiso 1 1 calc R . . H6B H 0.8582 -0.0779 0.2177 0.062 Uiso 1 1 calc R . . H6C H 0.8404 0.0252 0.1752 0.062 Uiso 1 1 calc R . . C7 C 0.7671(5) -0.1202(13) 0.2845(3) 0.038(2) Uani 1 1 d . . . H7A H 0.7521 -0.2296 0.2767 0.056 Uiso 1 1 calc R . . H7B H 0.7512 -0.0935 0.3115 0.056 Uiso 1 1 calc R . . H7C H 0.8223 -0.1104 0.2874 0.056 Uiso 1 1 calc R . . C8 C 0.6025(5) 0.0250(13) 0.2810(3) 0.036(2) Uani 1 1 d . . . H8A H 0.5709 -0.0674 0.2715 0.053 Uiso 1 1 calc R . . H8B H 0.5700 0.1170 0.2836 0.053 Uiso 1 1 calc R . . H8C H 0.6334 0.0020 0.3086 0.053 Uiso 1 1 calc R . . C9 C 0.5599(5) 0.2306(12) 0.1928(4) 0.037(3) Uani 1 1 d . . . H9A H 0.5254 0.1532 0.1768 0.056 Uiso 1 1 calc R . . H9B H 0.5688 0.3181 0.1740 0.056 Uiso 1 1 calc R . . H9C H 0.5372 0.2723 0.2163 0.056 Uiso 1 1 calc R . . C10 C 0.6989(5) 0.1922(13) 0.1436(3) 0.031(2) Uani 1 1 d . . . H10A H 0.6771 0.1139 0.1224 0.047 Uiso 1 1 calc R . . H10B H 0.7513 0.2149 0.1403 0.047 Uiso 1 1 calc R . . H10C H 0.6690 0.2903 0.1398 0.047 Uiso 1 1 calc R . . C11 C 0.7042(4) 0.3856(11) 0.2974(3) 0.0249(18) Uani 1 1 d . . . C12 C 0.6293(5) 0.4815(12) 0.2879(3) 0.029(2) Uani 1 1 d . . . C13 C 0.9077(5) 0.4728(13) 0.2879(4) 0.042(3) Uani 1 1 d . . . H13A H 0.9589 0.4685 0.3045 0.063 Uiso 1 1 calc R . . H13B H 0.8771 0.5496 0.3008 0.063 Uiso 1 1 calc R . . H13C H 0.9105 0.5056 0.2589 0.063 Uiso 1 1 calc R . . C14 C 0.9354(5) 0.1567(14) 0.2668(3) 0.038(3) Uani 1 1 d . . . H14A H 0.9852 0.1743 0.2842 0.058 Uiso 1 1 calc R . . H14B H 0.9372 0.1870 0.2374 0.058 Uiso 1 1 calc R . . H14C H 0.9218 0.0441 0.2679 0.058 Uiso 1 1 calc R . . C15 C 0.8764(5) 0.2214(13) 0.3434(3) 0.033(2) Uani 1 1 d . . . H15A H 0.9295 0.2360 0.3564 0.049 Uiso 1 1 calc R . . H15B H 0.8622 0.1097 0.3458 0.049 Uiso 1 1 calc R . . H15C H 0.8440 0.2884 0.3579 0.049 Uiso 1 1 calc R . . S1 S 0.89504(11) 0.4769(4) 0.13999(7) 0.0355(6) Uani 1 1 d . . . F6 F 0.9985(5) 0.3801(17) 0.0988(3) 0.130(5) Uani 1 1 d . . . F7 F 0.9514(5) 0.1913(11) 0.1318(4) 0.098(4) Uani 1 1 d . . . F8 F 1.0306(3) 0.3534(9) 0.1647(3) 0.067(2) Uani 1 1 d . . . O2 O 0.8371(4) 0.4430(12) 0.1042(2) 0.062(2) Uani 1 1 d . . . O3 O 0.8775(4) 0.4234(14) 0.1798(3) 0.075(3) Uani 1 1 d . . . O4 O 0.9272(4) 0.6333(11) 0.1402(3) 0.068(3) Uani 1 1 d . . . C20 C 0.9728(6) 0.3427(16) 0.1339(3) 0.045(3) Uani 1 1 d . . . Ir1' Ir 0.755296(18) 0.72706(4) -0.012781(11) 0.02193(14) Uani 1 1 d . . . P1' P 0.63100(12) 0.6603(3) -0.04228(7) 0.0296(5) Uani 1 1 d . . . O1' O 0.7405(3) 0.5670(8) 0.03883(18) 0.0293(14) Uani 1 1 d . . . F1' F 0.7866(4) 0.5375(10) -0.0853(2) 0.074(2) Uani 1 1 d . . . F2' F 0.7371(4) 0.3951(10) -0.0448(3) 0.080(3) Uani 1 1 d . . . F3' F 0.8762(4) 0.4164(11) 0.0146(2) 0.084(3) Uani 1 1 d . . . F4' F 0.9205(4) 0.5307(10) -0.0338(3) 0.082(3) Uani 1 1 d . . . F5' F 0.8718(4) 0.2985(9) -0.0460(3) 0.066(2) Uani 1 1 d . . . C1' C 0.8628(5) 0.8686(13) 0.0058(4) 0.042(3) Uani 1 1 d . . . C2' C 0.8283(5) 0.8995(12) -0.0379(3) 0.036(2) Uani 1 1 d . . . C3' C 0.7547(5) 0.9687(12) -0.0388(3) 0.028(2) Uani 1 1 d . . . C4' C 0.7436(5) 0.9862(12) 0.0048(3) 0.032(2) Uani 1 1 d . . . C5' C 0.8094(5) 0.9230(11) 0.0310(3) 0.030(2) Uani 1 1 d . . . C6' C 0.9434(5) 0.8216(15) 0.0226(4) 0.056(3) Uani 1 1 d . . . H6'A H 0.9751 0.9171 0.0272 0.085 Uiso 1 1 calc R . . H6'B H 0.9624 0.7524 0.0021 0.085 Uiso 1 1 calc R . . H6'C H 0.9453 0.7648 0.0495 0.085 Uiso 1 1 calc R . . C7' C 0.8658(7) 0.8825(16) -0.0780(5) 0.065(4) Uani 1 1 d . . . H7'A H 0.8953 0.9783 -0.0815 0.098 Uiso 1 1 calc R . . H7'B H 0.8264 0.8686 -0.1029 0.098 Uiso 1 1 calc R . . H7'C H 0.8994 0.7898 -0.0749 0.098 Uiso 1 1 calc R . . C8' C 0.7061(6) 1.0380(12) -0.0773(3) 0.041(3) Uani 1 1 d . . . H8'A H 0.7197 1.1497 -0.0803 0.062 Uiso 1 1 calc R . . H8'B H 0.6526 1.0306 -0.0742 0.062 Uiso 1 1 calc R . . H8'C H 0.7143 0.9787 -0.1025 0.062 Uiso 1 1 calc R . . C9' C 0.6804(6) 1.0767(14) 0.0209(3) 0.045(3) Uani 1 1 d . . . H9'A H 0.6951 1.1884 0.0253 0.068 Uiso 1 1 calc R . . H9'B H 0.6717 1.0304 0.0477 0.068 Uiso 1 1 calc R . . H9'C H 0.6339 1.0696 0.0000 0.068 Uiso 1 1 calc R . . C10' C 0.8202(6) 0.9201(14) 0.0789(3) 0.045(3) Uani 1 1 d . . . H10D H 0.8451 1.0184 0.0902 0.068 Uiso 1 1 calc R . . H10E H 0.8518 0.8288 0.0896 0.068 Uiso 1 1 calc R . . H10F H 0.7707 0.9110 0.0880 0.068 Uiso 1 1 calc R . . C11' C 0.7885(6) 0.5239(14) -0.0439(3) 0.039(2) Uani 1 1 d . . . C12' C 0.8608(7) 0.4380(17) -0.0261(4) 0.062(4) Uani 1 1 d . . . C13' C 0.5931(6) 0.4839(15) -0.0202(4) 0.052(3) Uani 1 1 d . . . H13D H 0.5410 0.4657 -0.0345 0.077 Uiso 1 1 calc R . . H13E H 0.5935 0.4996 0.0102 0.077 Uiso 1 1 calc R . . H13F H 0.6245 0.3917 -0.0244 0.077 Uiso 1 1 calc R . . C14' C 0.5587(6) 0.8086(16) -0.0336(5) 0.064(4) Uani 1 1 d . . . H14D H 0.5085 0.7715 -0.0469 0.096 Uiso 1 1 calc R . . H14E H 0.5698 0.9103 -0.0462 0.096 Uiso 1 1 calc R . . H14F H 0.5597 0.8226 -0.0031 0.096 Uiso 1 1 calc R . . C15' C 0.6108(6) 0.6305(16) -0.0998(3) 0.048(3) Uani 1 1 d . . . H15D H 0.5571 0.6032 -0.1084 0.071 Uiso 1 1 calc R . . H15E H 0.6423 0.5439 -0.1077 0.071 Uiso 1 1 calc R . . H15F H 0.6220 0.7284 -0.1142 0.071 Uiso 1 1 calc R . . S1' S 0.61311(11) 0.6385(3) 0.11634(7) 0.0298(5) Uani 1 1 d . . . F6' F 0.5604(5) 0.9105(11) 0.1382(4) 0.104(4) Uani 1 1 d . . . F7' F 0.4957(5) 0.8109(13) 0.0830(4) 0.111(4) Uani 1 1 d . . . F8' F 0.4855(6) 0.7141(13) 0.1412(5) 0.114(5) Uani 1 1 d . . . O2' O 0.6502(5) 0.6217(13) 0.1593(3) 0.076(3) Uani 1 1 d . . . O3' O 0.6548(5) 0.7256(11) 0.0893(4) 0.072(3) Uani 1 1 d . . . O4' O 0.5759(4) 0.4977(9) 0.0970(3) 0.051(2) Uani 1 1 d . . . C20' C 0.5361(7) 0.7787(16) 0.1217(5) 0.051(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 Ir1 0.0146(2) 0.0224(2) 0.0175(2) -0.00044(11) 0.00243(13) 0.00046(11) P1 0.0143(10) 0.0346(14) 0.0246(11) -0.0008(9) 0.0006(8) 0.0006(9) O1 0.024(3) 0.032(4) 0.021(3) -0.001(3) 0.001(2) -0.005(3) F1 0.032(3) 0.041(4) 0.031(3) -0.009(2) -0.004(2) 0.002(2) F2 0.048(3) 0.046(4) 0.022(3) 0.003(3) 0.010(2) 0.011(3) F3 0.046(3) 0.067(5) 0.041(3) -0.025(3) -0.003(3) 0.027(3) F4 0.017(2) 0.059(4) 0.049(3) -0.003(3) 0.008(2) -0.001(2) F5 0.031(3) 0.045(4) 0.037(3) 0.008(3) 0.001(2) 0.018(3) C1 0.028(4) 0.030(6) 0.021(4) -0.003(4) 0.001(3) 0.004(4) C2 0.026(4) 0.014(5) 0.047(6) -0.004(4) 0.004(4) 0.003(3) C3 0.025(4) 0.023(5) 0.032(5) -0.001(4) 0.005(4) -0.005(4) C4 0.016(4) 0.039(6) 0.021(4) -0.010(4) -0.008(3) -0.005(4) C5 0.026(4) 0.019(5) 0.026(4) -0.009(3) 0.004(3) -0.003(3) C6 0.042(5) 0.036(6) 0.049(6) -0.013(5) 0.014(5) 0.015(5) C7 0.038(5) 0.032(6) 0.041(6) 0.003(4) 0.000(4) -0.002(4) C8 0.019(4) 0.042(6) 0.047(6) 0.007(5) 0.009(4) -0.008(4) C9 0.022(5) 0.039(6) 0.048(6) -0.014(5) 0.000(4) 0.003(4) C10 0.033(5) 0.044(6) 0.015(4) -0.005(4) 0.000(3) 0.007(4) C11 0.019(4) 0.030(5) 0.023(4) 0.004(4) -0.004(3) 0.000(4) C12 0.027(4) 0.039(6) 0.022(4) -0.003(4) 0.006(3) 0.013(4) C13 0.021(4) 0.048(7) 0.055(6) 0.006(5) 0.000(4) -0.014(4) C14 0.015(4) 0.063(8) 0.038(5) 0.011(5) 0.006(4) 0.012(4) C15 0.025(4) 0.051(7) 0.020(4) 0.001(4) -0.001(4) 0.003(4) S1 0.0164(10) 0.0675(19) 0.0216(11) 0.0123(11) 0.0001(8) 0.0062(10) F6 0.100(7) 0.212(14) 0.092(7) 0.047(8) 0.065(6) 0.085(8) F7 0.065(5) 0.053(6) 0.156(10) -0.014(6) -0.041(6) -0.001(4) F8 0.028(3) 0.061(5) 0.103(6) -0.007(4) -0.021(3) 0.008(3) O2 0.043(4) 0.103(8) 0.034(4) 0.017(4) -0.010(3) 0.001(5) O3 0.035(4) 0.153(10) 0.042(5) 0.039(6) 0.019(4) 0.023(5) O4 0.038(4) 0.057(6) 0.101(8) 0.019(5) -0.008(4) 0.008(4) C20 0.026(5) 0.069(9) 0.038(6) 0.011(6) 0.000(4) 0.008(5) Ir1' 0.0211(2) 0.0263(2) 0.0176(2) -0.00064(12) 0.00086(14) 0.00115(13) P1' 0.0222(11) 0.0372(16) 0.0260(11) 0.0049(10) -0.0062(9) -0.0031(10) O1' 0.023(3) 0.040(4) 0.022(3) 0.009(3) -0.005(2) -0.001(3) F1' 0.095(5) 0.096(6) 0.026(3) -0.018(4) -0.005(3) 0.048(5) F2' 0.061(4) 0.050(5) 0.128(8) -0.021(5) 0.012(5) -0.011(4) F3' 0.093(5) 0.116(8) 0.045(4) 0.022(4) 0.020(4) 0.071(5) F4' 0.049(4) 0.086(7) 0.114(7) -0.004(5) 0.027(4) -0.008(4) F5' 0.058(4) 0.046(4) 0.096(6) -0.020(4) 0.018(4) 0.019(3) C1' 0.015(4) 0.034(6) 0.076(8) -0.010(5) 0.004(4) -0.014(4) C2' 0.041(5) 0.031(6) 0.037(5) -0.004(4) 0.010(4) -0.015(4) C3' 0.030(5) 0.031(6) 0.020(4) 0.001(4) -0.007(4) -0.008(4) C4' 0.037(5) 0.035(6) 0.022(4) -0.008(4) 0.000(4) 0.000(4) C5' 0.033(5) 0.026(5) 0.025(5) -0.006(4) -0.016(4) -0.002(4) C6' 0.024(5) 0.052(8) 0.088(10) 0.006(7) -0.008(5) -0.002(5) C7' 0.066(8) 0.053(9) 0.086(10) -0.003(7) 0.043(8) -0.013(7) C8' 0.071(7) 0.026(6) 0.023(5) 0.014(4) -0.006(5) -0.015(5) C9' 0.045(6) 0.046(7) 0.041(6) -0.009(5) -0.003(5) 0.016(5) C10' 0.053(6) 0.051(7) 0.025(5) -0.004(5) -0.014(4) -0.008(5) C11' 0.038(5) 0.042(7) 0.041(6) -0.005(5) 0.015(5) 0.010(5) C12' 0.063(8) 0.058(9) 0.058(8) -0.021(7) -0.007(6) 0.024(7) C13' 0.037(6) 0.058(8) 0.055(7) 0.015(6) -0.007(5) -0.010(5) C14' 0.028(5) 0.058(9) 0.102(11) -0.025(8) -0.003(6) 0.013(6) C15' 0.040(5) 0.081(9) 0.017(4) 0.001(5) -0.010(4) -0.014(6) S1' 0.0203(10) 0.0419(15) 0.0264(11) 0.0048(9) 0.0016(8) 0.0047(9) F6' 0.074(5) 0.062(6) 0.170(10) -0.074(7) -0.002(6) -0.002(4) F7' 0.088(6) 0.100(8) 0.124(9) -0.022(7) -0.044(6) 0.055(6) F8' 0.093(7) 0.098(8) 0.178(13) -0.020(8) 0.098(9) -0.001(6) O2' 0.073(6) 0.099(8) 0.045(5) 0.014(5) -0.024(4) 0.032(6) O3' 0.070(6) 0.063(6) 0.099(9) 0.019(5) 0.061(6) 0.009(5) O4' 0.044(4) 0.034(5) 0.072(6) -0.019(4) -0.001(4) 0.001(3) C20' 0.025(6) 0.054(8) 0.075(10) -0.007(7) 0.007(6) 0.004(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 C11 2.090(9) . ? Ir1 C2 2.176(9) . ? Ir1 O1 2.205(6) . ? Ir1 C3 2.218(8) . ? Ir1 C4 2.253(7) . ? Ir1 C5 2.275(8) . ? Ir1 C1 2.280(9) . ? Ir1 P1 2.350(2) . ? P1 C13 1.816(10) . ? P1 C14 1.835(9) . ? P1 C15 1.836(9) . ? O1 O3 2.724(9) . ? O1 O2' 2.756(10) . ? F1 C11 1.420(10) . ? F2 C11 1.407(10) . ? F3 C12 1.356(10) . ? F4 C12 1.333(11) . ? F5 C12 1.342(11) . ? C1 C5 1.393(12) . ? C1 C2 1.435(13) . ? C1 C6 1.528(12) . ? C2 C3 1.444(12) . ? C2 C7 1.545(13) . ? C3 C4 1.436(12) . ? C3 C8 1.527(12) . ? C4 C5 1.454(11) . ? C4 C9 1.530(12) . ? C5 C10 1.494(12) . ? C11 C12 1.550(11) . ? S1 O3 1.435(8) . ? S1 O4 1.437(9) . ? S1 O2 1.438(8) . ? S1 C20 1.827(12) . ? F6 C20 1.321(13) . ? F7 C20 1.329(16) . ? F8 C20 1.309(11) . ? O2 O1' 2.694(9) . ? Ir1' C11' 2.114(10) . ? Ir1' O1' 2.182(6) . ? Ir1' C2' 2.193(9) . ? Ir1' C3' 2.196(10) . ? Ir1' C1' 2.257(8) . ? Ir1' C4' 2.271(10) . ? Ir1' C5' 2.275(9) . ? Ir1' P1' 2.335(2) . ? P1' C13' 1.822(11) . ? P1' C15' 1.835(9) . ? P1' C14' 1.852(11) . ? O1' O3' 2.750(12) . ? F1' C11' 1.325(12) . ? F2' C11' 1.419(13) . ? F3' C12' 1.298(15) . ? F4' C12' 1.377(16) . ? F5' C12' 1.366(14) . ? C1' C5' 1.426(14) . ? C1' C2' 1.455(15) . ? C1' C6' 1.506(13) . ? C2' C3' 1.436(13) . ? C2' C7' 1.549(14) . ? C3' C4' 1.449(12) . ? C3' C8' 1.504(12) . ? C4' C5' 1.430(12) . ? C4' C9' 1.522(13) . ? C5' C10' 1.513(12) . ? C11' C12' 1.509(15) . ? S1' O2' 1.431(8) . ? S1' O3' 1.435(9) . ? S1' O4' 1.447(8) . ? S1' C20' 1.843(12) . ? F6' C20' 1.273(15) . ? F7' C20' 1.352(17) . ? F8' C20' 1.302(17) . ? 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 Ir1 C2 119.5(4) . . ? C11 Ir1 O1 85.6(3) . . ? C2 Ir1 O1 154.0(3) . . ? C11 Ir1 C3 95.6(3) . . ? C2 Ir1 C3 38.4(3) . . ? O1 Ir1 C3 141.3(3) . . ? C11 Ir1 C4 106.6(3) . . ? C2 Ir1 C4 63.4(3) . . ? O1 Ir1 C4 105.2(3) . . ? C3 Ir1 C4 37.5(3) . . ? C11 Ir1 C5 142.6(3) . . ? C2 Ir1 C5 61.8(3) . . ? O1 Ir1 C5 94.6(3) . . ? C3 Ir1 C5 61.9(3) . . ? C4 Ir1 C5 37.5(3) . . ? C11 Ir1 C1 156.3(3) . . ? C2 Ir1 C1 37.5(3) . . ? O1 Ir1 C1 116.7(3) . . ? C3 Ir1 C1 62.4(3) . . ? C4 Ir1 C1 61.9(3) . . ? C5 Ir1 C1 35.6(3) . . ? C11 Ir1 P1 87.3(2) . . ? C2 Ir1 P1 99.8(2) . . ? O1 Ir1 P1 87.16(16) . . ? C3 Ir1 P1 131.6(2) . . ? C4 Ir1 P1 161.9(2) . . ? C5 Ir1 P1 130.0(2) . . ? C1 Ir1 P1 100.9(2) . . ? C13 P1 C14 100.6(5) . . ? C13 P1 C15 103.9(5) . . ? C14 P1 C15 103.2(4) . . ? C13 P1 Ir1 117.1(3) . . ? C14 P1 Ir1 114.7(3) . . ? C15 P1 Ir1 115.3(3) . . ? Ir1 O1 O3 102.6(3) . . ? Ir1 O1 O2' 122.9(3) . . ? O3 O1 O2' 104.9(3) . . ? C5 C1 C2 107.9(8) . . ? C5 C1 C6 126.3(8) . . ? C2 C1 C6 124.9(8) . . ? C5 C1 Ir1 72.0(5) . . ? C2 C1 Ir1 67.3(5) . . ? C6 C1 Ir1 134.4(7) . . ? C1 C2 C3 108.0(8) . . ? C1 C2 C7 127.5(8) . . ? C3 C2 C7 123.6(8) . . ? C1 C2 Ir1 75.2(6) . . ? C3 C2 Ir1 72.4(5) . . ? C7 C2 Ir1 126.5(7) . . ? C4 C3 C2 107.8(7) . . ? C4 C3 C8 126.9(8) . . ? C2 C3 C8 124.9(8) . . ? C4 C3 Ir1 72.6(5) . . ? C2 C3 Ir1 69.2(5) . . ? C8 C3 Ir1 129.6(7) . . ? C3 C4 C5 106.3(7) . . ? C3 C4 C9 127.8(8) . . ? C5 C4 C9 125.3(8) . . ? C3 C4 Ir1 70.0(4) . . ? C5 C4 Ir1 72.1(4) . . ? C9 C4 Ir1 129.5(7) . . ? C1 C5 C4 109.8(8) . . ? C1 C5 C10 126.2(8) . . ? C4 C5 C10 123.9(8) . . ? C1 C5 Ir1 72.4(5) . . ? C4 C5 Ir1 70.5(4) . . ? C10 C5 Ir1 126.5(6) . . ? F2 C11 F1 101.8(6) . . ? F2 C11 C12 104.2(6) . . ? F1 C11 C12 101.3(7) . . ? F2 C11 Ir1 112.6(6) . . ? F1 C11 Ir1 114.8(5) . . ? C12 C11 Ir1 120.0(6) . . ? F4 C12 F5 107.6(7) . . ? F4 C12 F3 107.2(7) . . ? F5 C12 F3 105.6(8) . . ? F4 C12 C11 111.5(8) . . ? F5 C12 C11 112.2(7) . . ? F3 C12 C11 112.4(7) . . ? O3 S1 O4 115.4(7) . . ? O3 S1 O2 114.2(5) . . ? O4 S1 O2 114.8(5) . . ? O3 S1 C20 100.6(5) . . ? O4 S1 C20 104.8(5) . . ? O2 S1 C20 104.6(5) . . ? S1 O2 O1' 145.7(6) . . ? S1 O3 O1 131.9(5) . . ? F8 C20 F6 106.4(10) . . ? F8 C20 F7 106.7(9) . . ? F6 C20 F7 109.0(12) . . ? F8 C20 S1 113.4(9) . . ? F6 C20 S1 108.9(9) . . ? F7 C20 S1 112.3(8) . . ? C11' Ir1' O1' 86.4(4) . . ? C11' Ir1' C2' 97.5(4) . . ? O1' Ir1' C2' 147.3(3) . . ? C11' Ir1' C3' 123.7(4) . . ? O1' Ir1' C3' 149.9(3) . . ? C2' Ir1' C3' 38.2(4) . . ? C11' Ir1' C1' 104.9(4) . . ? O1' Ir1' C1' 109.4(3) . . ? C2' Ir1' C1' 38.1(4) . . ? C3' Ir1' C1' 64.0(4) . . ? C11' Ir1' C4' 159.8(4) . . ? O1' Ir1' C4' 112.2(3) . . ? C2' Ir1' C4' 62.6(4) . . ? C3' Ir1' C4' 37.8(3) . . ? C1' Ir1' C4' 62.4(4) . . ? C11' Ir1' C5' 138.9(4) . . ? O1' Ir1' C5' 94.2(3) . . ? C2' Ir1' C5' 61.8(4) . . ? C3' Ir1' C5' 62.4(3) . . ? C1' Ir1' C5' 36.7(4) . . ? C4' Ir1' C5' 36.7(3) . . ? C11' Ir1' P1' 86.4(3) . . ? O1' Ir1' P1' 85.97(16) . . ? C2' Ir1' P1' 126.6(3) . . ? C3' Ir1' P1' 97.2(2) . . ? C1' Ir1' P1' 161.1(3) . . ? C4' Ir1' P1' 102.2(2) . . ? C5' Ir1' P1' 134.7(2) . . ? C13' P1' C15' 104.7(6) . . ? C13' P1' C14' 100.2(6) . . ? C15' P1' C14' 102.5(6) . . ? C13' P1' Ir1' 115.5(3) . . ? C15' P1' Ir1' 117.0(3) . . ? C14' P1' Ir1' 114.8(4) . . ? Ir1' O1' O2 133.2(3) . . ? Ir1' O1' O3' 107.1(3) . . ? O2 O1' O3' 94.6(4) . . ? C5' C1' C2' 105.7(8) . . ? C5' C1' C6' 125.0(11) . . ? C2' C1' C6' 128.2(10) . . ? C5' C1' Ir1' 72.3(5) . . ? C2' C1' Ir1' 68.5(5) . . ? C6' C1' Ir1' 132.8(8) . . ? C3' C2' C1' 109.4(8) . . ? C3' C2' C7' 122.9(10) . . ? C1' C2' C7' 127.3(10) . . ? C3' C2' Ir1' 71.0(5) . . ? C1' C2' Ir1' 73.3(5) . . ? C7' C2' Ir1' 127.5(8) . . ? C2' C3' C4' 107.1(8) . . ? C2' C3' C8' 125.1(9) . . ? C4' C3' C8' 126.7(9) . . ? C2' C3' Ir1' 70.8(6) . . ? C4' C3' Ir1' 73.9(6) . . ? C8' C3' Ir1' 129.5(6) . . ? C5' C4' C3' 107.2(8) . . ? C5' C4' C9' 125.0(8) . . ? C3' C4' C9' 127.2(9) . . ? C5' C4' Ir1' 71.8(6) . . ? C3' C4' Ir1' 68.3(5) . . ? C9' C4' Ir1' 132.0(7) . . ? C1' C5' C4' 110.5(8) . . ? C1' C5' C10' 125.8(9) . . ? C4' C5' C10' 123.7(9) . . ? C1' C5' Ir1' 71.0(5) . . ? C4' C5' Ir1' 71.5(5) . . ? C10' C5' Ir1' 125.6(7) . . ? F1' C11' F2' 98.0(9) . . ? F1' C11' C12' 107.3(9) . . ? F2' C11' C12' 98.8(10) . . ? F1' C11' Ir1' 116.1(8) . . ? F2' C11' Ir1' 113.3(6) . . ? C12' C11' Ir1' 120.0(8) . . ? F3' C12' F5' 109.0(12) . . ? F3' C12' F4' 102.5(10) . . ? F5' C12' F4' 103.1(10) . . ? F3' C12' C11' 118.2(10) . . ? F5' C12' C11' 114.6(10) . . ? F4' C12' C11' 107.6(11) . . ? O2' S1' O3' 115.3(7) . . ? O2' S1' O4' 115.9(6) . . ? O3' S1' O4' 114.1(6) . . ? O2' S1' C20' 102.0(6) . . ? O3' S1' C20' 101.6(6) . . ? O4' S1' C20' 105.4(5) . . ? S1' O2' O1 151.2(6) . . ? S1' O3' O1' 120.2(5) . . ? F6' C20' F8' 112.4(13) . . ? F6' C20' F7' 107.3(12) . . ? F8' C20' F7' 102.3(12) . . ? F6' C20' S1' 112.8(9) . . ? F8' C20' S1' 111.6(10) . . ? F7' C20' S1' 109.8(10) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.602 _refine_diff_density_min -1.759 _refine_diff_density_rms 0.204 #===END data_rph130 _database_code_CSD 164771 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H26 F10 O4 P Rh S' _chemical_formula_weight 650.32 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9856(2) _cell_length_b 10.2371(2) _cell_length_c 15.1273(4) _cell_angle_alpha 83.2160(10) _cell_angle_beta 85.286(2) _cell_angle_gamma 82.0550(10) _cell_volume 1213.47(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Difabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7315 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5461 _reflns_number_gt 5334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+4.4342P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5461 _refine_ls_number_parameters 315 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.37700(3) 0.25792(3) 0.248169(17) 0.01826(9) Uani 1 1 d . . . C1 C 0.6402(4) 0.1719(4) 0.2009(2) 0.0255(7) Uani 1 1 d . . . C2 C 0.5896(5) 0.1169(4) 0.2911(2) 0.0248(7) Uani 1 1 d . . . C3 C 0.4524(5) 0.0404(4) 0.2837(3) 0.0267(7) Uani 1 1 d . . . C4 C 0.4058(5) 0.0634(4) 0.1951(3) 0.0250(7) Uani 1 1 d . . . C5 C 0.5247(5) 0.1433(4) 0.1436(2) 0.0241(7) Uani 1 1 d . . . C6 C 0.7997(5) 0.2318(5) 0.1753(3) 0.0337(9) Uani 1 1 d . . . H6A H 0.8899 0.1630 0.1575 0.051 Uiso 1 1 calc R . . H6B H 0.8330 0.2708 0.2263 0.051 Uiso 1 1 calc R . . H6C H 0.7809 0.3011 0.1253 0.051 Uiso 1 1 calc R . . C7 C 0.6948(5) 0.1100(5) 0.3694(3) 0.0362(9) Uani 1 1 d . . . H7A H 0.7813 0.0321 0.3692 0.054 Uiso 1 1 calc R . . H7B H 0.6220 0.1028 0.4247 0.054 Uiso 1 1 calc R . . H7C H 0.7500 0.1904 0.3656 0.054 Uiso 1 1 calc R . . C8 C 0.3845(6) -0.0553(4) 0.3560(3) 0.0384(10) Uani 1 1 d . . . H8A H 0.4483 -0.1437 0.3525 0.058 Uiso 1 1 calc R . . H8B H 0.2645 -0.0589 0.3484 0.058 Uiso 1 1 calc R . . H8C H 0.3962 -0.0260 0.4143 0.058 Uiso 1 1 calc R . . C9 C 0.2667(6) 0.0061(4) 0.1581(3) 0.0349(9) Uani 1 1 d . . . H9A H 0.3109 -0.0810 0.1389 0.052 Uiso 1 1 calc R . . H9B H 0.2239 0.0655 0.1069 0.052 Uiso 1 1 calc R . . H9C H 0.1743 -0.0037 0.2042 0.052 Uiso 1 1 calc R . . C10 C 0.5300(5) 0.1786(5) 0.0441(3) 0.0333(9) Uani 1 1 d . . . H10A H 0.6055 0.1102 0.0150 0.050 Uiso 1 1 calc R . . H10B H 0.5723 0.2644 0.0289 0.050 Uiso 1 1 calc R . . H10C H 0.4157 0.1841 0.0236 0.050 Uiso 1 1 calc R . . C11 C 0.5104(6) 0.5313(5) 0.1371(3) 0.0378(10) Uani 1 1 d . . . H11A H 0.5407 0.6210 0.1362 0.057 Uiso 1 1 calc R . . H11B H 0.4165 0.5335 0.0990 0.057 Uiso 1 1 calc R . . H11C H 0.6085 0.4726 0.1151 0.057 Uiso 1 1 calc R . . C12 C 0.6163(6) 0.4895(5) 0.3186(3) 0.0406(10) Uani 1 1 d . . . H12A H 0.6322 0.5834 0.3137 0.061 Uiso 1 1 calc R . . H12B H 0.7214 0.4374 0.2977 0.061 Uiso 1 1 calc R . . H12C H 0.5872 0.4585 0.3810 0.061 Uiso 1 1 calc R . . C13 C 0.2813(6) 0.6007(4) 0.2807(3) 0.0391(10) Uani 1 1 d . . . H13A H 0.3299 0.6839 0.2788 0.059 Uiso 1 1 calc R . . H13B H 0.2325 0.5770 0.3411 0.059 Uiso 1 1 calc R . . H13C H 0.1924 0.6118 0.2384 0.059 Uiso 1 1 calc R . . C14 C 0.1859(5) 0.2782(4) 0.3494(2) 0.0256(7) Uani 1 1 d . . . C15 C 0.2235(5) 0.2800(4) 0.4472(3) 0.0307(8) Uani 1 1 d . . . C16 C 0.0756(7) 0.2712(6) 0.5187(3) 0.0477(12) Uani 1 1 d . . . C17 C -0.1407(6) 0.8204(4) 0.1381(3) 0.0377(9) Uani 1 1 d . . . P1 P 0.44637(13) 0.46961(10) 0.25071(7) 0.0262(2) Uani 1 1 d . . . F1 F 0.0931(3) 0.1713(3) 0.35180(17) 0.0357(5) Uani 1 1 d . . . F2 F 0.0675(3) 0.3872(3) 0.33123(16) 0.0351(5) Uani 1 1 d . . . F3 F 0.3439(4) 0.1800(3) 0.47166(17) 0.0465(7) Uani 1 1 d . . . F4 F 0.2863(4) 0.3951(3) 0.45439(18) 0.0490(7) Uani 1 1 d . . . F5 F 0.1253(6) 0.2899(5) 0.5970(2) 0.0808(13) Uani 1 1 d . . . F6 F 0.0266(5) 0.1524(4) 0.5281(2) 0.0694(10) Uani 1 1 d . . . F7 F -0.0577(5) 0.3578(4) 0.4997(2) 0.0751(12) Uani 1 1 d . . . F8 F -0.1300(5) 0.9303(3) 0.0829(3) 0.0701(10) Uani 1 1 d . . . F9 F -0.0642(5) 0.8331(3) 0.2108(2) 0.0577(8) Uani 1 1 d . . . F10 F -0.3037(4) 0.8154(3) 0.1628(2) 0.0568(8) Uani 1 1 d . . . O1 O 0.1752(4) 0.3446(3) 0.16272(18) 0.0290(6) Uani 1 1 d D . . H1A H 0.106(5) 0.412(3) 0.174(3) 0.036(13) Uiso 1 1 d D . . H1B H 0.188(7) 0.336(6) 0.1075(11) 0.051(16) Uiso 1 1 d D . . O2 O -0.1529(5) 0.6770(4) 0.0129(2) 0.0524(10) Uani 1 1 d . . . O3 O 0.1248(4) 0.6964(4) 0.0620(3) 0.0550(10) Uani 1 1 d . . . O4 O -0.0676(4) 0.5671(3) 0.1556(2) 0.0336(6) Uani 1 1 d . . . S1 S -0.04657(12) 0.67343(11) 0.08565(6) 0.0299(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 Rh1 0.01403(13) 0.02269(15) 0.01666(14) 0.00216(9) -0.00028(9) -0.00150(9) C1 0.0179(16) 0.0313(19) 0.0240(17) 0.0000(14) 0.0028(13) 0.0031(14) C2 0.0207(16) 0.0266(18) 0.0238(17) 0.0023(14) -0.0011(13) 0.0040(14) C3 0.0267(18) 0.0233(17) 0.0280(19) -0.0011(14) 0.0024(14) -0.0001(14) C4 0.0217(17) 0.0217(17) 0.0301(19) -0.0034(14) 0.0019(14) 0.0012(13) C5 0.0203(16) 0.0252(17) 0.0249(18) -0.0028(14) 0.0021(13) 0.0021(13) C6 0.0178(17) 0.047(2) 0.035(2) -0.0037(18) 0.0014(15) -0.0022(16) C7 0.029(2) 0.049(3) 0.028(2) 0.0044(18) -0.0080(16) 0.0014(18) C8 0.047(3) 0.029(2) 0.037(2) 0.0063(17) 0.0020(19) -0.0074(18) C9 0.034(2) 0.038(2) 0.036(2) -0.0100(18) -0.0006(17) -0.0112(18) C10 0.0286(19) 0.048(2) 0.0218(18) -0.0057(17) 0.0026(15) -0.0018(17) C11 0.042(2) 0.035(2) 0.036(2) 0.0087(17) -0.0043(18) -0.0129(19) C12 0.037(2) 0.045(3) 0.043(3) -0.003(2) -0.0131(19) -0.014(2) C13 0.044(2) 0.026(2) 0.048(3) -0.0081(18) -0.009(2) -0.0002(18) C14 0.0188(16) 0.036(2) 0.0213(17) -0.0021(14) 0.0023(13) -0.0027(14) C15 0.031(2) 0.037(2) 0.0217(18) -0.0035(15) 0.0028(15) 0.0013(16) C16 0.049(3) 0.062(3) 0.026(2) 0.000(2) 0.0110(19) 0.004(2) C17 0.039(2) 0.031(2) 0.043(2) -0.0019(18) -0.0055(19) -0.0069(18) P1 0.0267(5) 0.0244(5) 0.0282(5) -0.0003(4) -0.0061(4) -0.0055(4) F1 0.0280(12) 0.0465(15) 0.0337(13) -0.0026(11) 0.0064(10) -0.0147(11) F2 0.0264(11) 0.0445(14) 0.0293(12) -0.0031(10) 0.0016(9) 0.0099(10) F3 0.0424(15) 0.0646(19) 0.0256(12) 0.0001(12) -0.0053(11) 0.0155(13) F4 0.0623(19) 0.0580(18) 0.0319(14) -0.0113(12) -0.0045(13) -0.0195(15) F5 0.093(3) 0.128(4) 0.0206(14) -0.0163(18) 0.0125(16) -0.015(3) F6 0.076(2) 0.077(2) 0.0496(19) 0.0085(17) 0.0262(17) -0.022(2) F7 0.059(2) 0.095(3) 0.052(2) 0.0037(18) 0.0254(16) 0.033(2) F8 0.094(3) 0.0353(16) 0.076(2) 0.0134(16) -0.008(2) -0.0048(17) F9 0.070(2) 0.0568(19) 0.0528(19) -0.0171(15) -0.0180(16) -0.0153(16) F10 0.0359(15) 0.0512(18) 0.084(2) -0.0314(17) 0.0083(15) 0.0033(13) O1 0.0260(14) 0.0355(15) 0.0234(13) -0.0054(11) -0.0075(11) 0.0090(11) O2 0.053(2) 0.070(2) 0.0312(17) -0.0165(16) -0.0159(15) 0.0185(18) O3 0.0281(16) 0.075(3) 0.051(2) 0.0166(19) 0.0132(15) -0.0001(16) O4 0.0296(14) 0.0318(15) 0.0355(15) 0.0022(12) -0.0008(12) 0.0041(12) S1 0.0238(4) 0.0393(5) 0.0224(4) 0.0009(4) 0.0001(3) 0.0059(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 Rh1 C14 2.078(4) . ? Rh1 C2 2.161(4) . ? Rh1 O1 2.175(3) . ? Rh1 C4 2.209(4) . ? Rh1 C3 2.238(4) . ? Rh1 C5 2.240(4) . ? Rh1 C1 2.257(3) . ? Rh1 P1 2.3151(10) . ? C1 C5 1.397(5) . ? C1 C2 1.461(5) . ? C1 C6 1.493(5) . ? C2 C3 1.451(5) . ? C2 C7 1.497(5) . ? C3 C4 1.404(5) . ? C3 C8 1.499(5) . ? C4 C5 1.456(5) . ? C4 C9 1.501(5) . ? C5 C10 1.504(5) . ? C11 P1 1.817(4) . ? C12 P1 1.815(4) . ? C13 P1 1.816(5) . ? C14 F2 1.376(4) . ? C14 F1 1.400(5) . ? C14 C15 1.536(5) . ? C15 F3 1.344(5) . ? C15 F4 1.362(5) . ? C15 C16 1.539(6) . ? C16 F7 1.316(6) . ? C16 F6 1.317(7) . ? C16 F5 1.322(6) . ? C17 F8 1.328(5) . ? C17 F9 1.329(6) . ? C17 F10 1.331(6) . ? C17 S1 1.824(5) . ? O2 S1 1.439(3) . ? O3 S1 1.430(3) . ? O4 S1 1.443(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Rh1 C2 111.62(14) . . ? C14 Rh1 O1 83.42(13) . . ? C2 Rh1 O1 156.33(13) . . ? C14 Rh1 C4 113.30(15) . . ? C2 Rh1 C4 63.73(14) . . ? O1 Rh1 C4 93.90(13) . . ? C14 Rh1 C3 95.58(15) . . ? C2 Rh1 C3 38.46(14) . . ? O1 Rh1 C3 125.27(13) . . ? C4 Rh1 C3 36.81(14) . . ? C14 Rh1 C5 151.40(15) . . ? C2 Rh1 C5 63.24(14) . . ? O1 Rh1 C5 94.64(12) . . ? C4 Rh1 C5 38.19(13) . . ? C3 Rh1 C5 62.34(14) . . ? C14 Rh1 C1 149.98(14) . . ? C2 Rh1 C1 38.55(13) . . ? O1 Rh1 C1 125.60(12) . . ? C4 Rh1 C1 62.48(14) . . ? C3 Rh1 C1 62.76(14) . . ? C5 Rh1 C1 36.19(14) . . ? C14 Rh1 P1 93.82(12) . . ? C2 Rh1 P1 108.28(11) . . ? O1 Rh1 P1 88.00(9) . . ? C4 Rh1 P1 152.87(10) . . ? C3 Rh1 P1 146.23(11) . . ? C5 Rh1 P1 114.67(10) . . ? C1 Rh1 P1 94.65(11) . . ? C5 C1 C2 107.7(3) . . ? C5 C1 C6 127.2(3) . . ? C2 C1 C6 124.7(3) . . ? C5 C1 Rh1 71.2(2) . . ? C2 C1 Rh1 67.17(19) . . ? C6 C1 Rh1 132.7(3) . . ? C3 C2 C1 107.0(3) . . ? C3 C2 C7 126.8(3) . . ? C1 C2 C7 124.0(3) . . ? C3 C2 Rh1 73.6(2) . . ? C1 C2 Rh1 74.3(2) . . ? C7 C2 Rh1 130.9(3) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 C8 126.4(4) . . ? C2 C3 C8 125.6(4) . . ? C4 C3 Rh1 70.5(2) . . ? C2 C3 Rh1 67.9(2) . . ? C8 C3 Rh1 131.2(3) . . ? C3 C4 C5 108.2(3) . . ? C3 C4 C9 125.9(4) . . ? C5 C4 C9 125.6(4) . . ? C3 C4 Rh1 72.7(2) . . ? C5 C4 Rh1 72.0(2) . . ? C9 C4 Rh1 125.0(3) . . ? C1 C5 C4 108.6(3) . . ? C1 C5 C10 126.1(3) . . ? C4 C5 C10 125.2(4) . . ? C1 C5 Rh1 72.6(2) . . ? C4 C5 Rh1 69.8(2) . . ? C10 C5 Rh1 127.4(3) . . ? F2 C14 F1 103.4(3) . . ? F2 C14 C15 105.2(3) . . ? F1 C14 C15 103.9(3) . . ? F2 C14 Rh1 112.6(2) . . ? F1 C14 Rh1 107.5(2) . . ? C15 C14 Rh1 122.3(3) . . ? F3 C15 F4 107.0(4) . . ? F3 C15 C14 110.5(3) . . ? F4 C15 C14 108.2(3) . . ? F3 C15 C16 106.1(4) . . ? F4 C15 C16 106.5(4) . . ? C14 C15 C16 117.9(4) . . ? F7 C16 F6 107.4(5) . . ? F7 C16 F5 109.0(5) . . ? F6 C16 F5 106.6(4) . . ? F7 C16 C15 112.8(4) . . ? F6 C16 C15 110.9(4) . . ? F5 C16 C15 109.9(5) . . ? F8 C17 F9 107.2(4) . . ? F8 C17 F10 107.7(4) . . ? F9 C17 F10 107.0(4) . . ? F8 C17 S1 111.4(4) . . ? F9 C17 S1 111.9(3) . . ? F10 C17 S1 111.4(3) . . ? C12 P1 C11 106.2(2) . . ? C12 P1 C13 102.7(2) . . ? C11 P1 C13 101.5(2) . . ? C12 P1 Rh1 117.97(17) . . ? C11 P1 Rh1 107.63(16) . . ? C13 P1 Rh1 119.03(16) . . ? O3 S1 O2 116.3(2) . . ? O3 S1 O4 115.1(2) . . ? O2 S1 O4 114.1(2) . . ? O3 S1 C17 104.0(2) . . ? O2 S1 C17 101.9(2) . . ? O4 S1 C17 102.8(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.284 _refine_diff_density_min -1.666 _refine_diff_density_rms 0.114 #===END data_rph103r _database_code_CSD 164772 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H26 F10 Ir O4 P S' _chemical_formula_weight 739.61 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7018(2) _cell_length_b 11.1491(2) _cell_length_c 13.5780(2) _cell_angle_alpha 80.5213(5) _cell_angle_beta 76.3566(5) _cell_angle_gamma 81.7157(7) _cell_volume 1255.02(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7756 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 5.561 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details DIFABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8600 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4388 _reflns_number_gt 4275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4388 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2764 _refine_ls_wR_factor_gt 0.2745 _refine_ls_goodness_of_fit_ref 2.518 _refine_ls_restrained_S_all 2.518 _refine_ls_shift/su_max 5.281 _refine_ls_shift/su_mean 0.187 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir -0.34117(6) 0.73062(5) 1.75111(4) 0.0409(3) Uani 1 1 d . . . P1 P -0.3855(5) 0.5614(4) 1.6894(3) 0.0429(9) Uani 1 1 d . . . F1 F -0.628(2) 0.5960(17) 1.8831(16) 0.133(6) Uiso 1 1 d . . . F2 F -0.559(4) 0.607(3) 1.957(3) 0.264(12) Uiso 1 1 d . A . F3 F -0.770(3) 0.795(2) 1.7981(18) 0.065(5) Uiso 0.50 1 d P A 1 F3' F -0.573(4) 0.787(3) 1.987(3) 0.118(10) Uiso 0.50 1 d P A 2 F4 F -0.6427(16) 0.9135(11) 1.8562(10) 0.078(3) Uiso 1 1 d . . . F5 F -0.761(3) 0.798(2) 2.0492(19) 0.070(6) Uiso 0.50 1 d P B 1 F5' F -0.877(5) 0.896(4) 1.997(4) 0.128(12) Uiso 0.50 1 d P B 2 F6 F -0.894(3) 0.688(2) 1.9847(19) 0.064(5) Uiso 0.50 1 d P B 1 F6' F -0.869(4) 0.705(3) 2.032(3) 0.086(7) Uiso 0.50 1 d P B 2 F7 F -0.939(3) 0.8826(19) 1.9605(17) 0.056(4) Uiso 0.50 1 d P B 1 F7' F -0.913(3) 0.817(3) 1.890(2) 0.089(7) Uiso 0.50 1 d P B 2 O1 O -0.4783(19) 0.8372(11) 1.6445(13) 0.074(4) Uani 1 1 d . . . C1 C -0.1019(19) 0.6614(19) 1.7802(15) 0.060(5) Uani 1 1 d . . . C2 C -0.0789(19) 0.7540(14) 1.6913(13) 0.044(3) Uani 1 1 d . . . C3 C -0.157(2) 0.8615(18) 1.722(2) 0.074(7) Uani 1 1 d . . . C4 C -0.237(3) 0.844(3) 1.829(2) 0.091(9) Uani 1 1 d . . . C5 C -0.198(2) 0.709(2) 1.8632(14) 0.071(6) Uani 1 1 d . . . C6 C -0.024(3) 0.538(2) 1.787(3) 0.096(9) Uani 1 1 d . . . H6A H 0.0814 0.5377 1.8014 0.143 Uiso 1 1 calc R . . H6B H -0.0115 0.5069 1.7216 0.143 Uiso 1 1 calc R . . H6C H -0.0877 0.4858 1.8417 0.143 Uiso 1 1 calc R . . C7 C 0.028(3) 0.737(3) 1.5868(19) 0.090(8) Uani 1 1 d . . . H7A H 0.1359 0.7542 1.5857 0.135 Uiso 1 1 calc R . . H7B H -0.0139 0.7940 1.5337 0.135 Uiso 1 1 calc R . . H7C H 0.0309 0.6530 1.5738 0.135 Uiso 1 1 calc R . . C8 C -0.160(3) 0.987(2) 1.645(3) 0.118(13) Uani 1 1 d . . . H8A H -0.0698 1.0300 1.6449 0.176 Uiso 1 1 calc R . . H8B H -0.2598 1.0387 1.6669 0.176 Uiso 1 1 calc R . . H8C H -0.1538 0.9691 1.5755 0.176 Uiso 1 1 calc R . . C9 C -0.311(4) 0.939(5) 1.900(4) 0.19(3) Uani 1 1 d . . . H9A H -0.2277 0.9669 1.9257 0.285 Uiso 1 1 calc R . . H9B H -0.3886 0.9027 1.9580 0.285 Uiso 1 1 calc R . . H9C H -0.3646 1.0087 1.8625 0.285 Uiso 1 1 calc R . . C10 C -0.234(4) 0.653(5) 1.9717(18) 0.15(2) Uani 1 1 d . . . H10A H -0.1439 0.6561 2.0026 0.227 Uiso 1 1 calc R . . H10B H -0.2524 0.5672 1.9756 0.227 Uiso 1 1 calc R . . H10C H -0.3294 0.6977 2.0087 0.227 Uiso 1 1 calc R . . C11 C -0.561(2) 0.7034(15) 1.858(2) 0.069(6) Uani 1 1 d . A . C12 C -0.696(3) 0.803(3) 1.870(2) 0.034(5) Uiso 0.50 1 d P A 1 C12' C -0.675(9) 0.764(7) 1.910(6) 0.11(2) Uiso 0.50 1 d P A 2 C13 C -0.819(2) 0.7919(15) 1.9669(17) 0.062(5) Uani 1 1 d . . . C14 C -0.392(3) 0.423(2) 1.7782(15) 0.073(6) Uani 1 1 d . . . H14A H -0.4117 0.3567 1.7455 0.109 Uiso 1 1 calc R . . H14B H -0.4778 0.4351 1.8383 0.109 Uiso 1 1 calc R . . H14C H -0.2902 0.4027 1.7993 0.109 Uiso 1 1 calc R . . C15 C -0.572(2) 0.5789(19) 1.6385(17) 0.065(5) Uani 1 1 d . . . H15A H -0.5812 0.5030 1.6138 0.097 Uiso 1 1 calc R . . H15B H -0.5677 0.6465 1.5821 0.097 Uiso 1 1 calc R . . H15C H -0.6649 0.5965 1.6932 0.097 Uiso 1 1 calc R . . C16 C -0.234(2) 0.5196(15) 1.5812(15) 0.061(4) Uani 1 1 d . . . H16A H -0.2602 0.4473 1.5588 0.092 Uiso 1 1 calc R . . H16B H -0.1309 0.5012 1.6008 0.092 Uiso 1 1 calc R . . H16C H -0.2288 0.5877 1.5251 0.092 Uiso 1 1 calc R . . C17 C -0.166(5) 0.812(3) 1.269(3) 0.112(11) Uani 1 1 d . . . S1 S -0.3504(9) 0.8262(4) 1.3671(4) 0.0760(16) Uani 1 1 d . . . O2 O -0.405(4) 0.7078(14) 1.3842(18) 0.139(10) Uani 1 1 d . . . O3 O -0.299(3) 0.848(2) 1.4536(16) 0.119(8) Uani 1 1 d . . . O4 O -0.447(2) 0.9231(14) 1.3263(13) 0.084(4) Uani 1 1 d . . . F8 F -0.059(4) 0.736(3) 1.301(3) 0.211(17) Uani 1 1 d . . . F9 F -0.196(4) 0.790(4) 1.186(2) 0.198(15) Uani 1 1 d . . . F10 F -0.106(3) 0.928(3) 1.238(3) 0.183(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0344(4) 0.0507(4) 0.0415(4) -0.0183(3) -0.0077(3) -0.0046(3) P1 0.046(2) 0.0419(19) 0.044(2) -0.0118(15) -0.0110(16) -0.0059(15) O1 0.085(10) 0.039(6) 0.108(12) -0.024(6) -0.037(9) 0.010(6) C1 0.034(8) 0.083(12) 0.055(10) 0.023(9) -0.015(7) -0.006(8) C2 0.052(8) 0.046(7) 0.053(9) -0.026(6) -0.027(7) -0.021(6) C3 0.042(10) 0.051(10) 0.14(2) -0.016(11) -0.019(11) -0.018(8) C4 0.046(11) 0.14(2) 0.11(2) -0.078(18) -0.005(12) -0.020(12) C5 0.054(10) 0.125(17) 0.045(9) -0.001(10) -0.022(8) -0.044(11) C6 0.067(13) 0.062(12) 0.16(2) 0.023(14) -0.052(15) -0.002(10) C7 0.053(12) 0.15(2) 0.064(14) -0.028(14) 0.018(10) -0.027(13) C8 0.051(13) 0.074(14) 0.21(4) 0.019(18) -0.009(16) -0.012(10) C9 0.090(19) 0.29(5) 0.25(5) -0.25(5) -0.03(3) 0.02(3) C10 0.10(2) 0.33(6) 0.052(12) 0.00(2) -0.051(14) -0.10(3) C11 0.058(11) 0.035(8) 0.111(17) -0.001(9) -0.013(11) -0.012(7) C13 0.048(10) 0.041(8) 0.095(15) -0.025(8) -0.001(9) -0.005(7) C14 0.089(15) 0.089(14) 0.047(10) 0.012(10) -0.027(10) -0.039(12) C15 0.041(9) 0.070(12) 0.083(14) -0.018(10) -0.002(9) -0.018(8) C16 0.078(13) 0.042(8) 0.067(11) -0.023(7) -0.020(9) 0.008(7) C17 0.14(3) 0.100(19) 0.11(3) -0.039(18) -0.06(2) 0.038(19) S1 0.136(5) 0.036(2) 0.067(3) -0.0058(19) -0.050(3) 0.000(2) O2 0.27(3) 0.038(8) 0.127(17) 0.016(9) -0.082(19) -0.040(12) O3 0.17(2) 0.127(16) 0.085(13) -0.046(11) -0.074(14) 0.009(14) O4 0.095(11) 0.067(9) 0.082(10) -0.002(7) -0.013(8) 0.002(7) F8 0.19(3) 0.23(3) 0.21(3) -0.09(3) -0.10(2) 0.14(3) F9 0.20(3) 0.28(4) 0.13(2) -0.10(2) -0.06(2) 0.06(3) F10 0.115(18) 0.20(3) 0.24(3) 0.00(2) -0.08(2) -0.019(18) _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 C11 2.13(2) . ? Ir1 C5 2.147(17) . ? Ir1 C4 2.19(2) . ? Ir1 O1 2.184(14) . ? Ir1 C1 2.216(16) . ? Ir1 C3 2.246(18) . ? Ir1 C2 2.272(16) . ? Ir1 P1 2.300(4) . ? P1 C16 1.80(2) . ? P1 C14 1.79(2) . ? P1 C15 1.88(2) . ? F1 F2 1.31(4) . ? F1 C11 1.37(3) . ? F1 C12' 1.94(8) . ? F2 C11 1.58(4) . ? F3 C12 1.31(4) . ? F3' C12' 1.60(8) . ? F4 C12 1.34(3) . ? F4 C12' 1.74(7) . ? F5 C13 1.35(3) . ? F5' C13 1.29(5) . ? F6 C13 1.37(3) . ? F6' C13 1.25(3) . ? F7 C13 1.35(3) . ? F7' C13 1.44(4) . ? O1 O3 2.69(3) . ? C1 C5 1.37(3) . ? C1 C2 1.45(2) . ? C1 C6 1.44(3) . ? C2 C3 1.36(3) . ? C2 C7 1.53(3) . ? C3 C4 1.46(4) . ? C3 C8 1.60(3) . ? C4 C5 1.51(4) . ? C4 C9 1.52(3) . ? C5 C10 1.48(3) . ? C11 C12' 1.26(8) . ? C11 C12 1.50(3) . ? C12 C13 1.49(3) . ? C12' C13 1.33(8) . ? C17 F9 1.28(4) . ? C17 F8 1.27(3) . ? C17 F10 1.42(5) . ? C17 S1 1.83(4) . ? S1 O4 1.393(15) . ? S1 O2 1.433(18) . ? S1 O3 1.422(18) . ? 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 Ir1 C5 96.1(9) . . ? C11 Ir1 C4 101.0(9) . . ? C5 Ir1 C4 40.9(11) . . ? C11 Ir1 O1 88.2(8) . . ? C5 Ir1 O1 154.2(8) . . ? C4 Ir1 O1 113.3(10) . . ? C11 Ir1 C1 125.1(8) . . ? C5 Ir1 C1 36.5(9) . . ? C4 Ir1 C1 63.4(10) . . ? O1 Ir1 C1 146.7(7) . . ? C11 Ir1 C3 136.2(9) . . ? C5 Ir1 C3 64.4(9) . . ? C4 Ir1 C3 38.4(11) . . ? O1 Ir1 C3 95.1(8) . . ? C1 Ir1 C3 61.0(8) . . ? C11 Ir1 C2 159.3(8) . . ? C5 Ir1 C2 63.4(6) . . ? C4 Ir1 C2 62.9(7) . . ? O1 Ir1 C2 109.6(6) . . ? C1 Ir1 C2 37.6(6) . . ? C3 Ir1 C2 35.2(7) . . ? C11 Ir1 P1 84.5(6) . . ? C5 Ir1 P1 119.6(7) . . ? C4 Ir1 P1 159.8(9) . . ? O1 Ir1 P1 86.1(4) . . ? C1 Ir1 P1 97.5(6) . . ? C3 Ir1 P1 139.2(7) . . ? C2 Ir1 P1 106.5(4) . . ? C16 P1 C14 103.3(11) . . ? C16 P1 C15 102.2(10) . . ? C14 P1 C15 105.8(10) . . ? C16 P1 Ir1 113.7(6) . . ? C14 P1 Ir1 115.3(8) . . ? C15 P1 Ir1 115.1(7) . . ? F2 F1 C11 72(2) . . ? F2 F1 C12' 72(3) . . ? C11 F1 C12' 40(2) . . ? F1 F2 C11 55.5(18) . . ? C12 F4 C12' 21(3) . . ? Ir1 O1 O3 109.3(8) . . ? C5 C1 C2 111.1(19) . . ? C5 C1 C6 123(2) . . ? C2 C1 C6 126(2) . . ? C5 C1 Ir1 69.0(10) . . ? C2 C1 Ir1 73.3(9) . . ? C6 C1 Ir1 129.5(16) . . ? C3 C2 C1 107.1(19) . . ? C3 C2 C7 126(2) . . ? C1 C2 C7 126.1(19) . . ? C3 C2 Ir1 71.4(10) . . ? C1 C2 Ir1 69.1(9) . . ? C7 C2 Ir1 129.9(13) . . ? C2 C3 C4 111(2) . . ? C2 C3 C8 123(3) . . ? C4 C3 C8 126(2) . . ? C2 C3 Ir1 73.5(10) . . ? C4 C3 Ir1 68.6(12) . . ? C8 C3 Ir1 123.5(17) . . ? C3 C4 C5 104.1(19) . . ? C3 C4 C9 129(4) . . ? C5 C4 C9 125(3) . . ? C3 C4 Ir1 73.0(12) . . ? C5 C4 Ir1 68.2(11) . . ? C9 C4 Ir1 132.0(18) . . ? C1 C5 C4 106.6(17) . . ? C1 C5 C10 129(3) . . ? C4 C5 C10 123(3) . . ? C1 C5 Ir1 74.5(10) . . ? C4 C5 Ir1 70.9(12) . . ? C10 C5 Ir1 129.2(14) . . ? C12' C11 F1 95(4) . . ? C12' C11 C12 27(3) . . ? F1 C11 C12 106.1(18) . . ? C12' C11 F2 88(4) . . ? F1 C11 F2 52.2(15) . . ? C12 C11 F2 114(2) . . ? C12' C11 Ir1 140(4) . . ? F1 C11 Ir1 125.1(16) . . ? C12 C11 Ir1 121.6(15) . . ? F2 C11 Ir1 118.6(17) . . ? F3 C12 F4 111(2) . . ? F3 C12 C13 105(2) . . ? F4 C12 C13 109(2) . . ? F3 C12 C11 104(2) . . ? F4 C12 C11 111(2) . . ? C13 C12 C11 117(2) . . ? C11 C12' C13 159(7) . . ? C11 C12' F3' 94(5) . . ? C13 C12' F3' 98(5) . . ? C11 C12' F1 45(3) . . ? C13 C12' F1 115(5) . . ? F3' C12' F1 109(4) . . ? C11 C12' F4 102(5) . . ? C13 C12' F4 96(4) . . ? F3' C12' F4 84(4) . . ? F1 C12' F4 143(5) . . ? F6' C13 F5' 111(3) . . ? F6' C13 F7 110(2) . . ? F5' C13 F7 38(2) . . ? F6' C13 F6 34.7(16) . . ? F5' C13 F6 127(3) . . ? F7 C13 F6 103.4(18) . . ? F6' C13 F5 74(2) . . ? F5' C13 F5 73(3) . . ? F7 C13 F5 108.8(19) . . ? F6 C13 F5 109(2) . . ? F6' C13 F7' 110(2) . . ? F5' C13 F7' 90(3) . . ? F7 C13 F7' 53.5(16) . . ? F6 C13 F7' 78.7(19) . . ? F5 C13 F7' 162(2) . . ? F6' C13 C12' 114(4) . . ? F5' C13 C12' 127(4) . . ? F7 C13 C12' 135(4) . . ? F6 C13 C12' 106(4) . . ? F5 C13 C12' 93(4) . . ? F7' C13 C12' 101(4) . . ? F6' C13 C12 135(2) . . ? F5' C13 C12 113(3) . . ? F7 C13 C12 109(2) . . ? F6 C13 C12 114(2) . . ? F5 C13 C12 112(2) . . ? F7' C13 C12 77(2) . . ? C12' C13 C12 27(3) . . ? F9 C17 F8 114(3) . . ? F9 C17 F10 102(4) . . ? F8 C17 F10 108(4) . . ? F9 C17 S1 110(3) . . ? F8 C17 S1 112(3) . . ? F10 C17 S1 109(2) . . ? O4 S1 O2 116.4(14) . . ? O4 S1 O3 114.7(13) . . ? O2 S1 O3 110.9(14) . . ? O4 S1 C17 105.3(13) . . ? O2 S1 C17 104.0(17) . . ? O3 S1 C17 103.9(16) . . ? S1 O3 O1 124.6(16) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.570 _refine_diff_density_min -2.733 _refine_diff_density_rms 0.219 #===END data_rph85 _database_code_CSD 164773 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H41 B Cl2 F31 Ir O1.50 P' _chemical_formula_weight 1547.70 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.9162(3) _cell_length_b 34.8748(6) _cell_length_c 13.2920(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.6911(3) _cell_angle_gamma 90.00 _cell_volume 5918.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_coefficient_mu 2.508 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4739 _exptl_absorpt_correction_T_max 0.7048 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27462 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10390 _reflns_number_gt 8110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10390 _refine_ls_number_parameters 871 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2607 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 1.824 _refine_ls_restrained_S_all 1.824 _refine_ls_shift/su_max 0.214 _refine_ls_shift/su_mean 0.019 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.51373(4) 0.167374(11) 0.38330(4) 0.0545(2) Uani 1 1 d . . . P1 P 0.6208(4) 0.16385(10) 0.2543(3) 0.0761(11) Uani 1 1 d . . . F1 F 0.3978(7) 0.2075(2) 0.2032(6) 0.095(3) Uani 1 1 d . . . F2 F 0.4266(8) 0.2828(2) 0.2693(8) 0.105(3) Uani 1 1 d . . . F3 F 0.5695(8) 0.2517(2) 0.2730(8) 0.106(3) Uani 1 1 d . . . F4 F 0.5128(7) 0.2646(2) 0.4104(7) 0.095(3) Uani 1 1 d . . . F5 F 0.2667(6) 0.1877(3) 0.3452(9) 0.110(3) Uani 1 1 d . . . F6 F 0.3254(8) 0.2365(3) 0.4344(9) 0.107(3) Uani 1 1 d . . . F7 F 0.2541(7) 0.2425(3) 0.2786(9) 0.124(4) Uani 1 1 d . . . O1 O 0.3976(9) 0.1322(3) 0.2772(8) 0.099(4) Uani 1 1 d . . . C1 C 0.5157(5) 0.18221(15) 0.5505(5) 0.074(4) Uani 1 1 d G . . C2 C 0.6206(4) 0.17642(16) 0.5338(5) 0.082(4) Uani 1 1 d G . . C3 C 0.6304(4) 0.13779(17) 0.5028(5) 0.073(4) Uani 1 1 d G . . C4 C 0.5316(4) 0.11969(14) 0.5005(5) 0.063(3) Uani 1 1 d G . . C5 C 0.4607(4) 0.14715(16) 0.5299(5) 0.063(3) Uani 1 1 d G . . C6 C 0.4707(7) 0.21914(18) 0.5843(8) 0.128(7) Uani 1 1 d G . . H6A H 0.4775 0.2196 0.6580 0.191 Uiso 1 1 calc R . . H6B H 0.3972 0.2209 0.5553 0.191 Uiso 1 1 calc R . . H6C H 0.5083 0.2407 0.5613 0.191 Uiso 1 1 calc R . . C7 C 0.7066(6) 0.2061(2) 0.5466(8) 0.105(6) Uani 1 1 d G . . H7A H 0.7422 0.2058 0.6163 0.158 Uiso 1 1 calc R . . H7B H 0.6765 0.2313 0.5310 0.158 Uiso 1 1 calc R . . H7C H 0.7563 0.2004 0.5008 0.158 Uiso 1 1 calc R . . C8 C 0.7286(5) 0.1192(2) 0.4770(8) 0.104(6) Uani 1 1 d G . . H8A H 0.7675 0.1078 0.5378 0.156 Uiso 1 1 calc R . . H8B H 0.7716 0.1384 0.4505 0.156 Uiso 1 1 calc R . . H8C H 0.7099 0.0995 0.4261 0.156 Uiso 1 1 calc R . . C9 C 0.5063(7) 0.07851(15) 0.4716(8) 0.109(6) Uani 1 1 d G . . H9A H 0.5195 0.0625 0.5319 0.163 Uiso 1 1 calc R . . H9B H 0.5500 0.0701 0.4226 0.163 Uiso 1 1 calc R . . H9C H 0.4332 0.0765 0.4419 0.163 Uiso 1 1 calc R . . C10 C 0.3469(4) 0.1403(2) 0.5380(8) 0.111(6) Uani 1 1 d G . . H10A H 0.3405 0.1324 0.6067 0.166 Uiso 1 1 calc R . . H10B H 0.3194 0.1203 0.4906 0.166 Uiso 1 1 calc R . . H10C H 0.3075 0.1637 0.5217 0.166 Uiso 1 1 calc R . . C11 C 0.572(2) 0.1782(6) 0.1249(13) 0.129(8) Uani 1 1 d . . . H11A H 0.6263 0.1748 0.0829 0.193 Uiso 1 1 calc R . . H11B H 0.5509 0.2049 0.1241 0.193 Uiso 1 1 calc R . . H11C H 0.5118 0.1625 0.0985 0.193 Uiso 1 1 calc R . . C12 C 0.7461(14) 0.1871(6) 0.2770(16) 0.119(6) Uani 1 1 d . . . H12A H 0.7818 0.1835 0.2185 0.179 Uiso 1 1 calc R . . H12B H 0.7878 0.1760 0.3368 0.179 Uiso 1 1 calc R . . H12C H 0.7364 0.2143 0.2879 0.179 Uiso 1 1 calc R . . C13 C 0.6549(19) 0.1140(5) 0.2325(13) 0.128(8) Uani 1 1 d . . . H13A H 0.6991 0.1129 0.1797 0.192 Uiso 1 1 calc R . . H13B H 0.5915 0.0994 0.2113 0.192 Uiso 1 1 calc R . . H13C H 0.6923 0.1032 0.2949 0.192 Uiso 1 1 calc R . . C14 C 0.4259(10) 0.2153(3) 0.3115(10) 0.064(3) Uani 1 1 d . . . C15 C 0.4821(11) 0.2538(3) 0.3161(11) 0.066(3) Uani 1 1 d . . . C16 C 0.3149(11) 0.2206(4) 0.3455(15) 0.087(5) Uani 1 1 d . . . B1 B 0.9700(9) -0.0925(3) 0.2501(8) 0.039(2) Uani 1 1 d . . . F21 F 0.9609(8) 0.0441(3) 0.0586(7) 0.102(3) Uani 1 1 d . . . F22 F 0.8478(10) 0.0156(3) -0.0415(6) 0.130(4) Uani 1 1 d . . . F23 F 0.8071(10) 0.0642(3) 0.0501(9) 0.142(5) Uani 1 1 d . . . F24 F 0.588(2) 0.0166(7) 0.282(3) 0.141(16) Uani 0.60 1 d P A 1 F25 F 0.6716(15) -0.0119(14) 0.4080(16) 0.160(15) Uani 0.60 1 d P A 1 F26 F 0.5789(13) -0.0448(5) 0.293(2) 0.099(7) Uani 0.60 1 d P A 1 F24' F 0.561(3) 0.000(2) 0.241(4) 0.24(4) Uani 0.40 1 d P A 2 F25' F 0.649(7) 0.0123(18) 0.363(6) 0.28(6) Uani 0.40 1 d P A 2 F26' F 0.624(3) -0.0383(10) 0.360(4) 0.107(11) Uani 0.40 1 d P A 2 F31 F 1.097(3) -0.0802(6) 0.7034(17) 0.113(10) Uani 0.60 1 d P B 1 F32 F 1.045(5) -0.0341(7) 0.605(2) 0.17(2) Uani 0.60 1 d P B 1 F33 F 0.9527(18) -0.0618(8) 0.691(2) 0.115(10) Uani 0.60 1 d P B 1 F31' F 1.122(3) -0.0601(17) 0.661(6) 0.18(3) Uani 0.40 1 d P B 2 F32' F 0.996(4) -0.0309(11) 0.611(3) 0.103(17) Uani 0.40 1 d P B 2 F33' F 0.968(8) -0.0739(12) 0.710(3) 0.26(5) Uani 0.40 1 d P B 2 F34 F 0.946(2) -0.2111(9) 0.6014(19) 0.081(8) Uani 0.50 1 d P C 1 F35 F 1.0358(18) -0.2204(8) 0.485(3) 0.072(10) Uani 0.50 1 d P C 1 F36 F 0.860(3) -0.2149(10) 0.464(3) 0.063(6) Uani 0.50 1 d P C 1 F34' F 0.992(2) -0.2108(9) 0.618(3) 0.092(10) Uani 0.50 1 d P C 2 F35' F 1.025(3) -0.2243(11) 0.458(3) 0.098(13) Uani 0.50 1 d P C 2 F36' F 0.886(4) -0.2176(14) 0.480(5) 0.13(2) Uani 0.50 1 d P C 2 F41 F 1.049(4) -0.166(2) -0.084(2) 0.22(2) Uani 0.50 1 d P D 1 F42 F 0.905(5) -0.1807(15) -0.166(3) 0.19(3) Uani 0.50 1 d P D 1 F43 F 0.951(8) -0.1271(10) -0.160(3) 0.21(3) Uani 0.50 1 d P D 1 F41' F 1.019(3) -0.1378(11) -0.116(2) 0.112(11) Uani 0.50 1 d P D 2 F42' F 0.926(5) -0.1907(9) -0.141(3) 0.142(19) Uani 0.50 1 d P D 2 F43' F 0.862(2) -0.1366(14) -0.181(2) 0.137(14) Uani 0.50 1 d P D 2 F44 F 0.640(2) -0.2097(10) 0.046(2) 0.182(17) Uani 0.60 1 d P E 1 F45 F 0.6088(16) -0.1690(7) 0.158(2) 0.124(10) Uani 0.60 1 d P E 1 F46 F 0.7051(12) -0.2117(5) 0.2041(17) 0.097(8) Uani 0.60 1 d P E 1 F44' F 0.666(4) -0.2221(10) 0.077(5) 0.21(3) Uani 0.40 1 d P E 2 F45' F 0.5878(14) -0.1710(9) 0.108(2) 0.089(9) Uani 0.40 1 d P E 2 F46' F 0.658(3) -0.189(2) 0.212(2) 0.24(3) Uani 0.40 1 d P E 2 F51 F 1.253(3) 0.0214(6) 0.2458(19) 0.155(13) Uani 0.60 1 d P F 1 F52 F 1.252(2) 0.0115(8) 0.3960(18) 0.124(9) Uani 0.60 1 d P F 1 F53 F 1.382(3) -0.0014(12) 0.334(4) 0.21(2) Uani 0.60 1 d P F 1 F51' F 1.335(3) 0.0157(13) 0.239(3) 0.18(3) Uani 0.40 1 d P F 2 F52' F 1.234(2) 0.0197(14) 0.338(7) 0.29(5) Uani 0.40 1 d P F 2 F53' F 1.388(3) -0.0056(12) 0.376(2) 0.065(7) Uani 0.40 1 d P F 2 F54 F 1.437(2) -0.1246(8) 0.192(2) 0.146(10) Uiso 0.50 1 d P G 1 F55 F 1.3284(14) -0.1670(4) 0.2358(14) 0.074(4) Uiso 0.50 1 d P G 1 F56 F 1.3060(18) -0.1449(7) 0.0870(17) 0.108(6) Uiso 0.50 1 d P G 1 F54' F 1.4345(14) -0.1357(5) 0.2397(14) 0.081(5) Uiso 0.50 1 d P G 2 F55' F 1.2981(18) -0.1726(6) 0.1937(18) 0.097(6) Uiso 0.50 1 d P G 2 F56' F 1.3557(15) -0.1295(5) 0.0919(14) 0.085(5) Uiso 0.50 1 d P G 2 C21 C 0.9102(4) -0.02657(16) 0.1547(4) 0.043(2) Uani 1 1 d G . . H21A H 0.9687 -0.0295 0.1211 0.051 Uiso 1 1 calc R . . C22 C 0.8418(5) 0.00394(15) 0.1303(4) 0.049(3) Uani 1 1 d G . . C23 C 0.7552(4) 0.00824(14) 0.1800(5) 0.047(2) Uani 1 1 d G . . H23A H 0.7089 0.0289 0.1634 0.057 Uiso 1 1 calc R . . C24 C 0.7371(4) -0.01798(17) 0.2541(5) 0.050(3) Uani 1 1 d G A . C25 C 0.8055(4) -0.04849(14) 0.2786(4) 0.040(2) Uani 1 1 d G . . H25A H 0.7932 -0.0662 0.3287 0.048 Uiso 1 1 calc R . . C26 C 0.8920(4) -0.05278(13) 0.2289(4) 0.0313(18) Uani 1 1 d G . . C27 C 0.8619(14) 0.0322(4) 0.0505(11) 0.080(4) Uani 1 1 d . . . C28 C 0.6413(13) -0.0143(5) 0.3063(14) 0.081(4) Uani 1 1 d . . . C31 C 0.9871(5) -0.08254(11) 0.4487(4) 0.042(2) Uani 1 1 d G . . H31A H 0.9925 -0.0563 0.4339 0.050 Uiso 1 1 calc R . . C32 C 0.9961(5) -0.09474(15) 0.5492(4) 0.045(2) Uani 1 1 d G B . C33 C 0.9881(5) -0.13351(17) 0.5710(3) 0.048(2) Uani 1 1 d G . . H33A H 0.9942 -0.1418 0.6389 0.058 Uiso 1 1 calc R . . C34 C 0.9710(5) -0.16008(12) 0.4923(4) 0.042(2) Uani 1 1 d G C . C35 C 0.9619(5) -0.14788(13) 0.3918(4) 0.039(2) Uani 1 1 d G . . H35A H 0.9504 -0.1658 0.3385 0.046 Uiso 1 1 calc R . . C36 C 0.9700(5) -0.10911(14) 0.3700(3) 0.039(2) Uani 1 1 d G . . C37 C 1.0220(13) -0.0655(4) 0.6341(10) 0.072(4) Uani 1 1 d . . . C38 C 0.9632(11) -0.2014(4) 0.5128(10) 0.061(3) Uani 1 1 d . . . C41 C 0.9506(5) -0.12710(18) 0.0673(5) 0.048(2) Uani 1 1 d G . . H41A H 1.0102 -0.1132 0.0559 0.057 Uiso 1 1 calc R . . C42 C 0.9006(6) -0.1514(2) -0.0077(4) 0.065(3) Uani 1 1 d G D . C43 C 0.8125(6) -0.17184(18) 0.0093(4) 0.063(4) Uani 1 1 d G . . H43A H 0.7787 -0.1882 -0.0414 0.076 Uiso 1 1 calc R . . C44 C 0.7745(4) -0.16807(17) 0.1012(5) 0.052(3) Uani 1 1 d G E . C45 C 0.8245(5) -0.14380(17) 0.1761(4) 0.043(2) Uani 1 1 d G . . H45A H 0.7988 -0.1413 0.2383 0.051 Uiso 1 1 calc R . . C46 C 0.9126(5) -0.12332(16) 0.1592(4) 0.043(2) Uani 1 1 d G . . C47 C 0.937(2) -0.1545(5) -0.1095(13) 0.106(7) Uani 1 1 d . . . C48 C 0.6806(10) -0.1906(4) 0.1201(13) 0.073(4) Uani 1 1 d . . . C51 C 1.1379(4) -0.04770(15) 0.2763(5) 0.045(2) Uani 1 1 d G . . H51A H 1.0946 -0.0282 0.2957 0.054 Uiso 1 1 calc R . . C52 C 1.2444(5) -0.04111(15) 0.2789(6) 0.052(3) Uani 1 1 d G F . C53 C 1.3083(4) -0.0699(2) 0.2502(6) 0.065(3) Uani 1 1 d G . . H53A H 1.3803 -0.0655 0.2519 0.078 Uiso 1 1 calc R . . C54 C 1.2656(5) -0.10535(18) 0.2189(5) 0.056(3) Uani 1 1 d G G . C55 C 1.1591(5) -0.11194(14) 0.2163(5) 0.048(2) Uani 1 1 d G . . H55A H 1.1303 -0.1359 0.1951 0.057 Uiso 1 1 calc R . . C56 C 1.0952(3) -0.08311(17) 0.2450(5) 0.042(2) Uani 1 1 d G . . C57 C 1.2892(11) -0.0033(4) 0.3157(16) 0.085(5) Uani 1 1 d . . . C58 C 1.3347(12) -0.1363(4) 0.1827(11) 0.077(4) Uani 1 1 d . . . C61 C 0.404(3) 0.0575(9) 0.068(2) 0.101(8) Uiso 0.60 1 d P H 1 H61A H 0.3744 0.0316 0.0672 0.121 Uiso 0.60 1 calc PR H 1 H61B H 0.4392 0.0623 0.1371 0.121 Uiso 0.60 1 calc PR H 1 C61' C 0.394(4) 0.0757(14) -0.055(4) 0.105(13) Uiso 0.40 1 d P H 2 H61C H 0.3539 0.0593 -0.1060 0.126 Uiso 0.40 1 calc PR H 2 H61D H 0.4030 0.1008 -0.0854 0.126 Uiso 0.40 1 calc PR H 2 Cl1 Cl 0.5073(15) 0.0568(6) -0.0173(12) 0.365(9) Uani 1 1 d . . . Cl2 Cl 0.3256(14) 0.0811(4) 0.0508(13) 0.336(8) Uani 1 1 d . . . O2 O 0.2486(19) 0.1008(8) 0.348(3) 0.141(11) Uani 0.50 1 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 Ir1 0.0547(3) 0.0454(3) 0.0632(3) 0.00573(19) 0.0076(2) 0.00284(18) P1 0.100(3) 0.070(2) 0.0589(19) 0.0014(15) 0.013(2) 0.0206(18) F1 0.116(7) 0.084(5) 0.075(5) 0.007(4) -0.015(5) 0.024(5) F2 0.122(7) 0.068(5) 0.125(7) 0.032(5) 0.023(6) 0.017(5) F3 0.127(8) 0.055(5) 0.146(8) 0.003(5) 0.058(7) -0.007(4) F4 0.122(7) 0.062(5) 0.102(6) -0.012(4) 0.020(6) -0.029(4) F5 0.064(5) 0.082(6) 0.183(11) 0.026(6) 0.010(6) -0.011(4) F6 0.091(6) 0.113(7) 0.124(8) -0.015(6) 0.037(6) 0.005(5) F7 0.092(6) 0.111(7) 0.166(10) 0.060(7) 0.013(6) 0.041(5) O1 0.120(8) 0.065(6) 0.097(7) -0.014(5) -0.031(6) -0.008(5) C1 0.094(10) 0.066(8) 0.063(7) 0.021(6) 0.014(7) 0.015(7) C2 0.071(9) 0.083(9) 0.092(10) -0.022(8) 0.016(8) -0.006(7) C3 0.068(8) 0.090(10) 0.061(8) 0.010(7) 0.011(7) 0.021(7) C4 0.064(7) 0.049(6) 0.074(8) 0.009(5) 0.006(7) 0.003(5) C5 0.065(7) 0.052(7) 0.078(8) 0.014(6) 0.032(7) 0.008(5) C6 0.18(2) 0.080(12) 0.136(16) -0.015(11) 0.051(15) 0.015(12) C7 0.130(14) 0.110(12) 0.070(9) -0.007(8) -0.001(9) -0.060(11) C8 0.074(10) 0.126(14) 0.114(13) 0.019(11) 0.021(10) 0.047(9) C9 0.124(14) 0.044(7) 0.163(18) 0.007(9) 0.037(13) -0.001(8) C10 0.088(11) 0.100(12) 0.163(17) 0.029(12) 0.078(13) 0.013(9) C11 0.20(2) 0.114(13) 0.074(10) -0.002(10) 0.040(13) 0.057(15) C12 0.101(13) 0.143(17) 0.124(16) 0.022(13) 0.048(12) 0.024(12) C13 0.21(2) 0.092(12) 0.088(11) -0.007(9) 0.037(13) 0.075(13) C14 0.065(7) 0.053(6) 0.069(7) 0.006(5) -0.005(6) 0.008(5) C15 0.068(8) 0.049(7) 0.085(9) 0.007(6) 0.025(8) -0.006(5) C16 0.058(8) 0.077(10) 0.117(13) 0.033(9) -0.010(9) 0.006(7) B1 0.048(6) 0.031(5) 0.035(5) -0.003(4) -0.006(5) 0.008(4) F21 0.105(7) 0.100(6) 0.101(6) 0.039(5) 0.019(6) -0.028(5) F22 0.200(12) 0.136(8) 0.050(5) 0.022(5) 0.003(6) -0.043(8) F23 0.184(10) 0.102(7) 0.165(10) 0.090(7) 0.102(9) 0.090(7) F24 0.15(3) 0.087(12) 0.23(4) 0.086(18) 0.16(3) 0.071(13) F25 0.065(11) 0.35(5) 0.072(12) -0.07(2) 0.037(9) -0.006(19) F26 0.048(9) 0.093(11) 0.17(2) -0.009(13) 0.057(11) -0.032(9) F24' 0.063(18) 0.46(10) 0.19(4) 0.18(6) 0.03(2) 0.12(4) F25' 0.42(12) 0.17(5) 0.31(9) 0.06(5) 0.33(9) 0.13(6) F26' 0.07(2) 0.11(2) 0.17(4) 0.03(3) 0.08(2) 0.027(18) F31 0.17(3) 0.084(14) 0.066(10) -0.035(9) -0.043(13) 0.031(14) F32 0.39(7) 0.058(16) 0.070(14) -0.020(12) 0.06(3) -0.09(2) F33 0.124(15) 0.13(2) 0.10(2) -0.058(17) 0.041(13) 0.018(12) F31' 0.066(16) 0.17(5) 0.28(7) -0.17(4) -0.05(3) 0.02(2) F32' 0.19(3) 0.08(2) 0.037(13) -0.035(14) 0.012(17) 0.06(2) F33' 0.69(16) 0.060(18) 0.060(17) -0.003(13) 0.18(4) -0.03(4) F34 0.12(2) 0.082(12) 0.032(9) 0.028(8) -0.002(13) -0.002(15) F35 0.047(9) 0.031(10) 0.15(3) 0.026(13) 0.046(14) 0.019(7) F36 0.040(12) 0.045(13) 0.102(14) 0.021(11) 0.003(11) -0.011(10) F34' 0.12(2) 0.063(10) 0.080(17) 0.047(10) -0.034(13) -0.026(13) F35' 0.17(3) 0.055(14) 0.072(13) -0.010(10) 0.017(14) 0.007(14) F36' 0.09(3) 0.061(15) 0.23(5) 0.065(19) 0.00(2) 0.015(17) F41 0.15(3) 0.46(8) 0.065(17) 0.03(3) 0.09(2) 0.00(4) F42 0.33(6) 0.20(5) 0.067(19) -0.09(3) 0.06(2) -0.15(5) F43 0.48(10) 0.13(2) 0.06(2) 0.04(2) 0.10(4) 0.01(5) F41' 0.18(3) 0.14(2) 0.026(12) -0.022(12) 0.041(14) -0.05(2) F42' 0.29(5) 0.065(12) 0.09(2) 0.007(13) 0.11(3) 0.04(2) F43' 0.13(2) 0.20(4) 0.069(15) 0.047(18) -0.004(15) 0.00(2) F44 0.15(2) 0.27(4) 0.126(16) -0.11(2) 0.015(14) -0.16(2) F45 0.073(14) 0.121(15) 0.15(2) -0.018(15) -0.066(14) -0.037(10) F46 0.057(10) 0.086(10) 0.149(19) 0.058(12) 0.013(10) -0.017(7) F44' 0.24(5) 0.067(16) 0.39(8) -0.12(3) 0.24(5) -0.10(2) F45' 0.003(7) 0.16(2) 0.11(2) -0.014(18) 0.002(11) 0.013(10) F46' 0.07(2) 0.61(9) 0.043(14) -0.07(3) 0.039(16) -0.14(4) F51 0.29(4) 0.053(10) 0.118(16) 0.002(10) 0.01(2) -0.069(16) F52 0.11(2) 0.143(18) 0.114(14) -0.056(13) 0.020(13) -0.073(15) F53 0.08(2) 0.16(3) 0.38(7) -0.10(4) 0.01(3) -0.05(2) F51' 0.16(3) 0.21(4) 0.15(3) 0.10(3) -0.07(3) -0.16(3) F52' 0.033(11) 0.18(4) 0.61(12) -0.30(6) -0.08(3) 0.035(18) F53' 0.040(12) 0.076(15) 0.070(11) -0.013(9) -0.019(9) -0.006(10) C21 0.044(5) 0.041(5) 0.043(5) -0.001(4) 0.008(4) 0.004(4) C22 0.066(7) 0.039(5) 0.044(5) 0.006(4) 0.010(5) 0.015(5) C23 0.041(5) 0.048(6) 0.050(6) -0.001(4) 0.001(5) 0.006(4) C24 0.055(6) 0.036(5) 0.064(6) 0.005(5) 0.025(6) 0.008(4) C25 0.042(5) 0.028(4) 0.051(5) -0.001(4) 0.015(5) -0.005(3) C26 0.034(4) 0.027(4) 0.031(4) -0.001(3) 0.000(4) -0.002(3) C27 0.112(12) 0.055(7) 0.075(9) 0.022(6) 0.021(9) 0.019(7) C28 0.078(10) 0.071(9) 0.103(12) 0.015(9) 0.040(10) 0.021(8) C31 0.050(5) 0.032(4) 0.041(5) 0.001(4) -0.001(4) 0.006(4) C32 0.050(6) 0.053(6) 0.033(4) -0.001(4) 0.007(4) 0.004(4) C33 0.051(6) 0.060(6) 0.033(5) 0.014(4) 0.005(5) 0.004(5) C34 0.040(5) 0.044(5) 0.044(5) 0.005(4) 0.014(5) 0.005(4) C35 0.044(5) 0.033(5) 0.040(5) -0.002(4) 0.010(4) 0.000(4) C36 0.039(5) 0.033(4) 0.045(5) 0.006(4) 0.008(4) 0.000(4) C37 0.089(10) 0.073(9) 0.049(7) -0.018(6) -0.002(7) 0.013(8) C38 0.064(9) 0.060(7) 0.058(7) 0.016(6) 0.009(7) -0.004(6) C41 0.062(7) 0.040(5) 0.042(5) 0.001(4) 0.009(5) -0.004(4) C42 0.108(10) 0.053(6) 0.033(5) -0.011(5) 0.008(6) -0.015(6) C43 0.099(10) 0.049(6) 0.034(5) -0.002(4) -0.012(6) 0.000(6) C44 0.044(6) 0.043(5) 0.062(7) 0.000(5) -0.012(5) 0.003(4) C45 0.040(5) 0.042(5) 0.045(5) -0.002(4) 0.001(4) 0.004(4) C46 0.050(6) 0.037(5) 0.039(5) -0.002(4) -0.009(4) 0.006(4) C47 0.19(2) 0.078(10) 0.064(10) -0.019(8) 0.052(14) -0.047(14) C48 0.047(7) 0.054(7) 0.117(12) -0.014(8) 0.011(8) -0.004(6) C51 0.042(5) 0.047(5) 0.043(5) 0.006(4) 0.002(5) 0.008(4) C52 0.053(6) 0.047(6) 0.058(6) 0.009(5) 0.015(5) 0.000(5) C53 0.043(6) 0.078(8) 0.079(8) 0.014(7) 0.022(6) 0.008(5) C54 0.049(6) 0.067(7) 0.055(6) 0.014(5) 0.018(5) 0.020(5) C55 0.049(6) 0.044(5) 0.049(6) 0.011(4) 0.007(5) 0.003(4) C56 0.048(5) 0.040(5) 0.040(5) 0.008(4) 0.011(5) 0.004(4) C57 0.057(9) 0.053(8) 0.142(16) 0.005(9) 0.010(10) -0.013(6) C58 0.071(9) 0.084(10) 0.076(9) 0.006(7) 0.015(8) 0.008(7) Cl1 0.35(2) 0.45(3) 0.290(17) -0.006(16) 0.030(16) -0.045(18) Cl2 0.39(2) 0.243(13) 0.364(19) 0.043(13) 0.009(16) 0.088(14) O2 0.081(15) 0.12(2) 0.22(3) -0.03(2) 0.035(19) -0.019(14) _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 C14 2.160(11) . ? Ir1 O1 2.258(9) . ? Ir1 C3 2.266(6) . ? Ir1 C4 2.266(6) . ? Ir1 C2 2.274(6) . ? Ir1 C5 2.273(6) . ? Ir1 C1 2.278(6) . ? Ir1 P1 2.363(4) . ? P1 C12 1.79(2) . ? P1 C11 1.812(18) . ? P1 C13 1.827(15) . ? F1 C14 1.456(14) . ? F2 C15 1.339(14) . ? F3 C15 1.343(16) . ? F4 C15 1.312(15) . ? F5 C16 1.306(16) . ? F6 C16 1.295(19) . ? F7 C16 1.334(15) . ? C1 C5 1.4200 . ? C1 C2 1.4200 . ? C1 C6 1.5095 . ? C2 C3 1.4200 . ? C2 C7 1.5095 . ? C3 C4 1.4200 . ? C3 C8 1.5095 . ? C4 C5 1.4200 . ? C4 C9 1.5095 . ? C5 C10 1.5095 . ? C14 C15 1.521(16) . ? C14 C16 1.58(2) . ? B1 C56 1.662(12) . ? B1 C36 1.695(11) . ? B1 C46 1.701(10) . ? B1 C26 1.712(10) . ? F21 C27 1.332(18) . ? F22 C27 1.340(17) . ? F23 C27 1.321(15) . ? F24 C28 1.29(3) . ? F25 C28 1.35(3) . ? F26 C28 1.33(2) . ? F24' C28 1.34(3) . ? F25' C28 1.19(8) . ? F26' C28 1.14(3) . ? F31 C37 1.33(2) . ? F32 C37 1.22(3) . ? F33 C37 1.26(3) . ? F31' C37 1.30(3) . ? F32' C37 1.28(4) . ? F33' C37 1.34(6) . ? F34 C38 1.28(3) . ? F35 C38 1.25(3) . ? F36 C38 1.47(4) . ? F34' C38 1.43(3) . ? F35' C38 1.40(4) . ? F36' C38 1.17(5) . ? F41 C47 1.50(5) . ? F42 C47 1.21(3) . ? F43 C47 1.20(3) . ? F41' C47 1.23(3) . ? F42' C47 1.33(4) . ? F43' C47 1.40(4) . ? F44 C48 1.24(2) . ? F45 C48 1.35(3) . ? F46 C48 1.33(2) . ? F44' C48 1.24(3) . ? F45' C48 1.37(3) . ? F45' F46' 1.66(6) . ? F46' C48 1.30(3) . ? F51 C57 1.30(3) . ? F52 C57 1.34(3) . ? F53 C57 1.19(4) . ? F51' C57 1.42(4) . ? F52' C57 1.14(3) . ? F53' C57 1.40(3) . ? F54 C58 1.37(3) . ? F55 C58 1.29(2) . ? F56 C58 1.31(2) . ? F54' C58 1.39(2) . ? F55' C58 1.36(2) . ? F56' C58 1.30(2) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.500(14) . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C24 C28 1.512(18) . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 C37 1.519(12) . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C34 C38 1.474(13) . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 C47 1.501(18) . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C44 C48 1.499(14) . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 C57 1.492(14) . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C54 C58 1.525(15) . ? C55 C56 1.3900 . ? C61 Cl2 1.30(3) . ? C61 Cl1 1.88(3) . ? C61' Cl1 1.61(5) . ? C61' Cl2 1.78(5) . ? 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 C14 Ir1 O1 83.6(4) . . ? C14 Ir1 C3 155.7(4) . . ? O1 Ir1 C3 120.0(3) . . ? C14 Ir1 C4 149.7(4) . . ? O1 Ir1 C4 91.2(3) . . ? C3 Ir1 C4 36.52(8) . . ? C14 Ir1 C2 119.3(4) . . ? O1 Ir1 C2 151.9(3) . . ? C3 Ir1 C2 36.45(8) . . ? C4 Ir1 C2 60.81(12) . . ? C14 Ir1 C5 114.4(4) . . ? O1 Ir1 C5 96.3(4) . . ? C3 Ir1 C5 60.81(12) . . ? C4 Ir1 C5 36.46(9) . . ? C2 Ir1 C5 60.70(13) . . ? C14 Ir1 C1 100.5(4) . . ? O1 Ir1 C1 129.9(4) . . ? C3 Ir1 C1 60.73(13) . . ? C4 Ir1 C1 60.74(13) . . ? C2 Ir1 C1 36.35(9) . . ? C5 Ir1 C1 36.35(10) . . ? C14 Ir1 P1 92.6(4) . . ? O1 Ir1 P1 85.7(4) . . ? C3 Ir1 P1 94.87(17) . . ? C4 Ir1 P1 116.78(17) . . ? C2 Ir1 P1 107.53(19) . . ? C5 Ir1 P1 153.00(16) . . ? C1 Ir1 P1 142.93(19) . . ? C12 P1 C11 102.3(11) . . ? C12 P1 C13 102.9(11) . . ? C11 P1 C13 99.8(8) . . ? C12 P1 Ir1 117.8(7) . . ? C11 P1 Ir1 121.0(8) . . ? C13 P1 Ir1 110.2(7) . . ? C5 C1 C2 108.0 . . ? C5 C1 C6 126.0 . . ? C2 C1 C6 126.0 . . ? C5 C1 Ir1 71.63(19) . . ? C2 C1 Ir1 71.7(2) . . ? C6 C1 Ir1 122.40(18) . . ? C3 C2 C1 108.0 . . ? C3 C2 C7 126.0 . . ? C1 C2 C7 126.0 . . ? C3 C2 Ir1 71.5(2) . . ? C1 C2 Ir1 72.0(2) . . ? C7 C2 Ir1 122.22(18) . . ? C2 C3 C4 108.0 . . ? C2 C3 C8 126.0 . . ? C4 C3 C8 126.0 . . ? C2 C3 Ir1 72.1(2) . . ? C4 C3 Ir1 71.7(2) . . ? C8 C3 Ir1 121.9(2) . . ? C3 C4 C5 108.0 . . ? C3 C4 C9 126.0 . . ? C5 C4 C9 126.0 . . ? C3 C4 Ir1 71.8(2) . . ? C5 C4 Ir1 72.1(2) . . ? C9 C4 Ir1 121.89(19) . . ? C1 C5 C4 108.0 . . ? C1 C5 C10 126.0 . . ? C4 C5 C10 126.0 . . ? C1 C5 Ir1 72.0(2) . . ? C4 C5 Ir1 71.5(2) . . ? C10 C5 Ir1 122.19(18) . . ? F1 C14 C15 104.5(10) . . ? F1 C14 C16 101.7(10) . . ? C15 C14 C16 109.5(11) . . ? F1 C14 Ir1 109.1(7) . . ? C15 C14 Ir1 116.7(8) . . ? C16 C14 Ir1 113.8(8) . . ? F4 C15 F2 106.8(11) . . ? F4 C15 F3 105.7(11) . . ? F2 C15 F3 105.5(11) . . ? F4 C15 C14 111.4(11) . . ? F2 C15 C14 115.5(11) . . ? F3 C15 C14 111.2(11) . . ? F6 C16 F5 111.3(15) . . ? F6 C16 F7 109.5(15) . . ? F5 C16 F7 105.6(12) . . ? F6 C16 C14 109.7(11) . . ? F5 C16 C14 110.5(13) . . ? F7 C16 C14 110.2(13) . . ? C56 B1 C36 104.2(6) . . ? C56 B1 C46 114.7(7) . . ? C36 B1 C46 113.0(7) . . ? C56 B1 C26 112.6(7) . . ? C36 B1 C26 110.3(7) . . ? C46 B1 C26 102.2(6) . . ? C48 F45' F46' 49.9(18) . . ? C48 F46' F45' 53(2) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 C27 120.2(7) . . ? C21 C22 C27 119.8(7) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 C28 119.5(7) . . ? C23 C24 C28 120.5(7) . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 B1 120.3(5) . . ? C21 C26 B1 119.4(5) . . ? F23 C27 F21 104.2(13) . . ? F23 C27 F22 111.3(12) . . ? F21 C27 F22 101.8(13) . . ? F23 C27 C22 114.1(12) . . ? F21 C27 C22 114.4(11) . . ? F22 C27 C22 110.3(11) . . ? F26' C28 F25' 100(4) . . ? F26' C28 F24 129(2) . . ? F25' C28 F24 60(4) . . ? F26' C28 F26 48(2) . . ? F25' C28 F26 134(4) . . ? F24 C28 F26 110(2) . . ? F26' C28 F24' 118(4) . . ? F25' C28 F24' 96(5) . . ? F24 C28 F24' 37(4) . . ? F26 C28 F24' 79(4) . . ? F26' C28 F25 58(3) . . ? F25' C28 F25 48(4) . . ? F24 C28 F25 105(3) . . ? F26 C28 F25 105(3) . . ? F24' C28 F25 134(4) . . ? F26' C28 C24 118.2(18) . . ? F25' C28 C24 111(4) . . ? F24 C28 C24 113.2(16) . . ? F26 C28 C24 113.3(15) . . ? F24' C28 C24 110(3) . . ? F25 C28 C24 109.4(14) . . ? C32 C31 C36 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 C37 120.8(7) . . ? C31 C32 C37 119.0(7) . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 C38 118.6(6) . . ? C33 C34 C38 121.4(6) . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 B1 122.6(5) . . ? C31 C36 B1 117.2(5) . . ? F32 C37 F33 109(3) . . ? F32 C37 F32' 30(4) . . ? F33 C37 F32' 82(3) . . ? F32 C37 F31' 71(3) . . ? F33 C37 F31' 126(3) . . ? F32' C37 F31' 98(4) . . ? F32 C37 F31 112(3) . . ? F33 C37 F31 97(2) . . ? F32' C37 F31 132(2) . . ? F31' C37 F31 44(3) . . ? F32 C37 F33' 128(3) . . ? F33 C37 F33' 23(3) . . ? F32' C37 F33' 104(3) . . ? F31' C37 F33' 116(4) . . ? F31 C37 F33' 78(4) . . ? F32 C37 C32 114.0(17) . . ? F33 C37 C32 114.7(15) . . ? F32' C37 C32 115.7(19) . . ? F31' C37 C32 113(2) . . ? F31 C37 C32 108.1(13) . . ? F33' C37 C32 109(3) . . ? F36' C38 F35 106(3) . . ? F36' C38 F34 88(3) . . ? F35 C38 F34 112(2) . . ? F36' C38 F35' 93(4) . . ? F35 C38 F35' 15(3) . . ? F34 C38 F35' 121(3) . . ? F36' C38 F34' 110(3) . . ? F35 C38 F34' 94(2) . . ? F34 C38 F34' 25.1(19) . . ? F35' C38 F34' 107(2) . . ? F36' C38 F36 10(3) . . ? F35 C38 F36 112(2) . . ? F34 C38 F36 93(2) . . ? F35' C38 F36 98(2) . . ? F34' C38 F36 117(2) . . ? F36' C38 C34 118(2) . . ? F35 C38 C34 112.7(16) . . ? F34 C38 C34 117.2(18) . . ? F35' C38 C34 114(2) . . ? F34' C38 C34 112.9(15) . . ? F36 C38 C34 108.3(17) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 C47 121.2(9) . . ? C43 C42 C47 118.8(9) . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 C48 120.0(7) . . ? C45 C44 C48 120.0(7) . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 B1 119.3(6) . . ? C41 C46 B1 120.7(6) . . ? F43 C47 F42 109(3) . . ? F43 C47 F41' 51(4) . . ? F42 C47 F41' 122(3) . . ? F43 C47 F42' 127(3) . . ? F42 C47 F42' 24(4) . . ? F41' C47 F42' 118(3) . . ? F43 C47 F43' 54(4) . . ? F42 C47 F43' 77(3) . . ? F41' C47 F43' 105(3) . . ? F42' C47 F43' 101(3) . . ? F43 C47 F41 97(5) . . ? F42 C47 F41 99(4) . . ? F41' C47 F41 48(2) . . ? F42' C47 F41 82(3) . . ? F43' C47 F41 146(2) . . ? F43 C47 C42 123(2) . . ? F42 C47 C42 119(3) . . ? F41' C47 C42 114.8(17) . . ? F42' C47 C42 109(2) . . ? F43' C47 C42 108(2) . . ? F41 C47 C42 103.5(18) . . ? F44 C48 F44' 31(4) . . ? F44 C48 F46' 130(3) . . ? F44' C48 F46' 116(4) . . ? F44 C48 F46 113(2) . . ? F44' C48 F46 84(3) . . ? F46' C48 F46 46(3) . . ? F44 C48 F45 111(2) . . ? F44' C48 F45 127(2) . . ? F46' C48 F45 50(3) . . ? F46 C48 F45 94.8(19) . . ? F44 C48 F45' 85(2) . . ? F44' C48 F45' 108(3) . . ? F46' C48 F45' 77(3) . . ? F46 C48 F45' 118(2) . . ? F45 C48 F45' 29.3(13) . . ? F44 C48 C44 114.0(18) . . ? F44' C48 C44 117(2) . . ? F46' C48 C44 116(2) . . ? F46 C48 C44 109.5(11) . . ? F45 C48 C44 112.9(13) . . ? F45' C48 C44 115.6(17) . . ? C52 C51 C56 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 C57 119.2(8) . . ? C53 C52 C57 120.8(8) . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 C58 119.9(7) . . ? C53 C54 C58 120.0(8) . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 B1 119.4(5) . . ? C51 C56 B1 120.5(5) . . ? F52' C57 F53 124(3) . . ? F52' C57 F51 63(5) . . ? F53 C57 F51 111(3) . . ? F52' C57 F52 38(5) . . ? F53 C57 F52 107(3) . . ? F51 C57 F52 100(2) . . ? F52' C57 F53' 116(3) . . ? F53 C57 F53' 24(4) . . ? F51 C57 F53' 130(2) . . ? F52 C57 F53' 88(2) . . ? F52' C57 F51' 102(6) . . ? F53 C57 F51' 66(3) . . ? F51 C57 F51' 47(2) . . ? F52 C57 F51' 129(3) . . ? F53' C57 F51' 90(2) . . ? F52' C57 C52 119(2) . . ? F53 C57 C52 117(2) . . ? F51 C57 C52 105.6(16) . . ? F52 C57 C52 115.7(15) . . ? F53' C57 C52 114.4(19) . . ? F51' C57 C52 111(2) . . ? F55 C58 F56' 134.4(17) . . ? F55 C58 F56 108.1(18) . . ? F56' C58 F56 37.3(11) . . ? F55 C58 F54 109.8(18) . . ? F56' C58 F54 72.3(17) . . ? F56 C58 F54 107(2) . . ? F55 C58 F55' 28.7(11) . . ? F56' C58 F55' 113.2(17) . . ? F56 C58 F55' 80.8(17) . . ? F54 C58 F55' 127.8(19) . . ? F55 C58 F54' 81.2(14) . . ? F56' C58 F54' 101.3(16) . . ? F56 C58 F54' 129.6(18) . . ? F54 C58 F54' 31.3(13) . . ? F55' C58 F54' 105.3(15) . . ? F55 C58 C54 109.0(14) . . ? F56' C58 C54 112.2(13) . . ? F56 C58 C54 112.2(14) . . ? F54 C58 C54 111.0(17) . . ? F55' C58 C54 113.2(15) . . ? F54' C58 C54 110.7(12) . . ? Cl2 C61 Cl1 121(2) . . ? Cl1 C61' Cl2 110(3) . . ? C61' Cl1 C61 59(2) . . ? C61 Cl2 C61' 66(2) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.656 _refine_diff_density_min -1.645 _refine_diff_density_rms 0.148 #===END data_rph77 _database_code_CSD 164774 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 B F11 Ir O2 P' _chemical_formula_weight 881.56 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.3292(2) _cell_length_b 35.4589(7) _cell_length_c 10.4739(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.0288(7) _cell_angle_gamma 90.00 _cell_volume 3312.90(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 4.165 _exptl_absorpt_correction_type 'Empirical from DIFABS' _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13618 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4988 _reflns_number_gt 4632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4988 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.550 _refine_ls_shift/su_mean 0.032 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir -0.81230(2) 0.138111(6) 0.429132(18) 0.02005(14) Uani 1 1 d . . . P1 P -0.89373(14) 0.10204(4) 0.23208(12) 0.0200(3) Uani 1 1 d . . . O1 O -0.6226(4) 0.15772(11) 0.3621(4) 0.0304(9) Uani 1 1 d . . . O2 O -0.4045(6) 0.20610(15) 0.4826(5) 0.0576(13) Uani 1 1 d . . . F1 F -0.7201(3) 0.05773(10) 0.4877(3) 0.0354(8) Uani 1 1 d . . . F2 F -0.6819(5) 0.09161(11) 0.6661(3) 0.0459(9) Uani 1 1 d . . . F3 F -0.4466(4) 0.12705(11) 0.6100(3) 0.0385(8) Uani 1 1 d . . . F4 F -0.4762(4) 0.09050(11) 0.4343(3) 0.0383(8) Uani 1 1 d . . . F5 F -0.2661(4) 0.06716(14) 0.6494(5) 0.0723(14) Uani 1 1 d . . . F6 F -0.4510(4) 0.02846(12) 0.5968(4) 0.0588(11) Uani 1 1 d . . . F7 F -0.4152(5) 0.06362(13) 0.7682(3) 0.0586(11) Uani 1 1 d . . . C1 C -1.0377(6) 0.15398(18) 0.4410(6) 0.0326(14) Uani 1 1 d . . . C2 C -0.9425(8) 0.14408(17) 0.5720(7) 0.0330(15) Uani 1 1 d . . . C3 C -0.8220(6) 0.17160(16) 0.6068(5) 0.0283(12) Uani 1 1 d . . . C4 C -0.8458(6) 0.19774(16) 0.4980(5) 0.0283(12) Uani 1 1 d . . . C5 C -0.9790(6) 0.18656(16) 0.3946(5) 0.0274(12) Uani 1 1 d . . . C6 C -1.1917(7) 0.13599(19) 0.3728(9) 0.048(2) Uani 1 1 d . . . H6A H -1.2698 0.1497 0.3992 0.073 Uiso 1 1 calc R . . H6B H -1.1908 0.1095 0.4002 0.073 Uiso 1 1 calc R . . H6C H -1.2122 0.1373 0.2756 0.073 Uiso 1 1 calc R . . C7 C -0.9803(9) 0.1160(2) 0.6657(7) 0.0493(18) Uani 1 1 d . . . H7A H -1.0280 0.1292 0.7248 0.074 Uiso 1 1 calc R . . H7B H -0.8883 0.1037 0.7193 0.074 Uiso 1 1 calc R . . H7C H -1.0492 0.0970 0.6138 0.074 Uiso 1 1 calc R . . C8 C -0.7044(8) 0.1759(2) 0.7423(6) 0.0452(17) Uani 1 1 d . . . H8A H -0.7431 0.1926 0.7992 0.068 Uiso 1 1 calc R . . H8B H -0.6129 0.1868 0.7299 0.068 Uiso 1 1 calc R . . H8C H -0.6818 0.1511 0.7849 0.068 Uiso 1 1 calc R . . C9 C -0.7537(8) 0.23151(19) 0.4927(7) 0.0438(16) Uani 1 1 d . . . H9A H -0.7931 0.2533 0.5292 0.066 Uiso 1 1 calc R . . H9B H -0.7574 0.2366 0.3998 0.066 Uiso 1 1 calc R . . H9C H -0.6497 0.2269 0.5456 0.066 Uiso 1 1 calc R . . C10 C -1.0580(8) 0.2103(2) 0.2735(6) 0.0469(17) Uani 1 1 d . . . H10A H -1.1233 0.2287 0.2985 0.070 Uiso 1 1 calc R . . H10B H -1.1185 0.1939 0.2027 0.070 Uiso 1 1 calc R . . H10C H -0.9833 0.2235 0.2411 0.070 Uiso 1 1 calc R . . C11 C -1.1644(4) 0.12034(9) 0.0300(4) 0.0336(13) Uani 1 1 d G . . H11A H -1.2051 0.0984 0.0582 0.040 Uiso 1 1 calc R . . C12 C -1.2525(3) 0.14209(11) -0.0740(4) 0.0443(18) Uani 1 1 d G . . H12A H -1.3533 0.1350 -0.1169 0.053 Uiso 1 1 calc R . . C13 C -1.1930(4) 0.17422(10) -0.1152(3) 0.0434(16) Uani 1 1 d G . . H13A H -1.2532 0.1891 -0.1862 0.052 Uiso 1 1 calc R . . C14 C -1.0455(4) 0.18459(9) -0.0524(4) 0.0364(14) Uani 1 1 d G . . H14A H -1.0048 0.2065 -0.0806 0.044 Uiso 1 1 calc R . . C15 C -0.9574(3) 0.16283(10) 0.0516(3) 0.0300(13) Uani 1 1 d G . . H15A H -0.8566 0.1699 0.0945 0.036 Uiso 1 1 calc R . . C16 C -1.0169(4) 0.13071(10) 0.0928(3) 0.0253(12) Uani 1 1 d G . . C17 C -0.6793(4) 0.04844(10) 0.2084(4) 0.0332(14) Uani 1 1 d G . . H17A H -0.7135 0.0344 0.2710 0.040 Uiso 1 1 calc R . . C18 C -0.5640(4) 0.03445(9) 0.1628(4) 0.0374(15) Uani 1 1 d G . . H18A H -0.5194 0.0108 0.1943 0.045 Uiso 1 1 calc R . . C19 C -0.5140(4) 0.05500(13) 0.0711(4) 0.0437(17) Uani 1 1 d G . . H19A H -0.4352 0.0454 0.0400 0.052 Uiso 1 1 calc R . . C20 C -0.5793(5) 0.08954(13) 0.0251(5) 0.075(3) Uani 1 1 d G . . H20A H -0.5452 0.1036 -0.0376 0.090 Uiso 1 1 calc R . . C21 C -0.6946(5) 0.10353(10) 0.0707(4) 0.053(2) Uani 1 1 d G . . H21A H -0.7393 0.1271 0.0392 0.063 Uiso 1 1 calc R . . C22 C -0.7446(4) 0.08298(11) 0.1623(3) 0.0256(12) Uani 1 1 d G . . C23 C -1.0441(4) 0.04971(10) 0.3520(3) 0.0296(12) Uani 1 1 d G . . H23A H -1.0132 0.0655 0.4285 0.035 Uiso 1 1 calc R . . C24 C -1.1278(4) 0.01747(11) 0.3549(3) 0.0372(14) Uani 1 1 d G . . H24A H -1.1542 0.0112 0.4333 0.045 Uiso 1 1 calc R . . C25 C -1.1730(4) -0.00562(9) 0.2430(4) 0.0397(15) Uani 1 1 d G . . H25A H -1.2303 -0.0277 0.2449 0.048 Uiso 1 1 calc R . . C26 C -1.1344(4) 0.00352(10) 0.1283(3) 0.0380(15) Uani 1 1 d G . . H26A H -1.1653 -0.0123 0.0518 0.046 Uiso 1 1 calc R . . C27 C -1.0507(4) 0.03576(10) 0.1254(3) 0.0298(12) Uani 1 1 d G . . H27A H -1.0243 0.0420 0.0470 0.036 Uiso 1 1 calc R . . C28 C -1.0055(4) 0.05886(8) 0.2373(3) 0.0231(11) Uani 1 1 d G . . C29 C -0.6759(6) 0.09360(15) 0.5327(5) 0.0243(11) Uani 1 1 d . . . C30 C -0.5034(6) 0.09325(18) 0.5554(5) 0.0314(13) Uani 1 1 d . . . C31 C -0.4092(6) 0.06250(18) 0.6424(6) 0.0360(14) Uani 1 1 d . . . B1 B -0.5825(9) 0.2366(3) 0.1403(8) 0.051(2) Uani 1 1 d . . . F10 F -0.4418(6) 0.23949(15) 0.2319(5) 0.0728(13) Uiso 1 1 d . A . F11 F -0.590(3) 0.2259(5) 0.0249(16) 0.131(9) Uani 0.60 1 d P A 1 F12 F -0.6175(8) 0.2772(2) 0.1318(7) 0.0589(18) Uani 0.60 1 d P A 1 F13 F -0.6791(7) 0.2206(2) 0.1978(6) 0.0476(17) Uani 0.60 1 d P A 1 F11' F -0.593(2) 0.2405(7) 0.014(2) 0.083(8) Uani 0.40 1 d P A 2 F12' F -0.7097(18) 0.2473(5) 0.1791(17) 0.101(6) Uani 0.40 1 d P A 2 F13' F -0.6002(16) 0.1930(4) 0.1462(12) 0.078(4) Uani 0.40 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0207(2) 0.0216(2) 0.0192(2) -0.00213(6) 0.00796(13) -0.00264(7) P1 0.0184(6) 0.0231(8) 0.0195(6) -0.0026(5) 0.0071(5) 0.0004(5) O1 0.033(2) 0.024(2) 0.038(2) 0.0014(17) 0.0155(17) -0.0083(17) O2 0.055(3) 0.044(3) 0.068(3) -0.004(2) 0.009(2) -0.016(2) F1 0.0287(17) 0.027(2) 0.049(2) 0.0018(15) 0.0087(14) -0.0037(14) F2 0.060(2) 0.054(3) 0.0311(19) 0.0127(16) 0.0242(17) 0.0107(18) F3 0.038(2) 0.034(2) 0.0344(19) 0.0028(16) -0.0038(15) -0.0119(17) F4 0.0282(18) 0.057(3) 0.0325(18) 0.0015(16) 0.0137(14) -0.0044(16) F5 0.023(2) 0.082(4) 0.102(4) 0.039(3) 0.004(2) 0.002(2) F6 0.046(2) 0.039(3) 0.076(3) -0.005(2) -0.004(2) 0.0083(18) F7 0.075(3) 0.054(3) 0.035(2) 0.0127(18) -0.0032(18) 0.008(2) C1 0.028(3) 0.031(4) 0.045(4) -0.013(3) 0.021(3) 0.003(3) C2 0.040(4) 0.028(4) 0.042(4) -0.004(3) 0.028(3) -0.003(3) C3 0.041(3) 0.028(3) 0.018(2) -0.012(2) 0.014(2) -0.002(2) C4 0.038(3) 0.020(3) 0.031(3) -0.009(2) 0.018(2) 0.004(2) C5 0.031(3) 0.027(3) 0.028(3) -0.005(2) 0.016(2) 0.006(2) C6 0.020(4) 0.059(5) 0.072(5) -0.029(3) 0.022(4) -0.006(3) C7 0.074(5) 0.041(4) 0.048(4) 0.003(3) 0.042(4) -0.009(4) C8 0.064(4) 0.042(4) 0.026(3) -0.008(3) 0.007(3) 0.002(3) C9 0.053(4) 0.029(4) 0.055(4) -0.009(3) 0.024(3) 0.000(3) C10 0.048(4) 0.044(4) 0.045(4) 0.002(3) 0.008(3) 0.028(3) C11 0.034(3) 0.031(4) 0.033(3) -0.002(3) 0.006(2) 0.000(3) C12 0.034(4) 0.049(5) 0.044(4) -0.003(3) 0.002(3) 0.007(3) C13 0.050(4) 0.046(4) 0.028(3) 0.004(3) 0.002(3) 0.016(3) C14 0.055(4) 0.021(3) 0.036(3) 0.004(2) 0.018(3) 0.010(3) C15 0.034(3) 0.029(3) 0.028(3) -0.007(2) 0.009(2) 0.003(2) C16 0.026(3) 0.025(3) 0.024(3) -0.003(2) 0.005(2) 0.001(2) C17 0.030(3) 0.042(4) 0.029(3) -0.004(3) 0.011(2) 0.003(3) C18 0.037(3) 0.038(4) 0.040(3) -0.001(3) 0.017(3) 0.011(3) C19 0.042(4) 0.046(4) 0.051(4) 0.004(3) 0.026(3) 0.018(3) C20 0.077(6) 0.094(7) 0.083(6) 0.051(5) 0.069(5) 0.041(5) C21 0.054(5) 0.052(6) 0.066(5) 0.032(3) 0.039(4) 0.025(3) C22 0.017(3) 0.040(4) 0.021(3) -0.002(2) 0.007(2) -0.003(2) C23 0.022(3) 0.033(4) 0.034(3) -0.004(2) 0.008(2) -0.001(2) C24 0.032(3) 0.041(4) 0.039(3) 0.014(3) 0.011(3) 0.001(3) C25 0.033(3) 0.030(4) 0.053(4) 0.007(3) 0.008(3) -0.007(3) C26 0.027(3) 0.033(4) 0.051(4) -0.013(3) 0.007(3) -0.004(3) C27 0.027(3) 0.031(3) 0.036(3) -0.004(2) 0.017(2) -0.006(2) C28 0.018(2) 0.024(3) 0.026(3) 0.001(2) 0.004(2) 0.004(2) C29 0.031(3) 0.018(3) 0.024(2) 0.001(2) 0.008(2) -0.006(2) C30 0.026(3) 0.041(4) 0.025(3) -0.002(2) 0.003(2) -0.006(2) C31 0.024(3) 0.041(4) 0.040(3) -0.003(3) 0.005(2) -0.005(3) B1 0.040(4) 0.079(7) 0.035(4) 0.013(4) 0.013(3) -0.003(4) F11 0.228(17) 0.123(15) 0.067(9) -0.058(10) 0.083(10) -0.090(12) F12 0.049(4) 0.050(5) 0.080(5) 0.010(4) 0.023(4) -0.010(3) F13 0.036(4) 0.058(5) 0.044(4) 0.021(3) 0.005(3) -0.013(3) F11' 0.070(9) 0.13(2) 0.044(8) 0.035(11) 0.007(6) -0.061(10) F12' 0.098(11) 0.115(14) 0.105(11) 0.020(10) 0.054(9) 0.064(11) F13' 0.099(9) 0.054(8) 0.075(8) 0.008(6) 0.016(7) -0.032(7) _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 C29 2.116(5) . ? Ir1 C2 2.196(6) . ? Ir1 O1 2.200(4) . ? Ir1 C1 2.215(5) . ? Ir1 C3 2.232(5) . ? Ir1 C5 2.274(5) . ? Ir1 C4 2.285(5) . ? Ir1 P1 2.3568(13) . ? P1 C28 1.862(3) . ? P1 C16 1.871(3) . ? P1 C22 1.876(3) . ? F1 C29 1.377(6) . ? F2 C29 1.416(6) . ? F3 C30 1.366(7) . ? F4 C30 1.367(6) . ? F5 C31 1.326(7) . ? F6 C31 1.314(7) . ? F7 C31 1.336(7) . ? C1 C5 1.424(9) . ? C1 C2 1.443(9) . ? C1 C6 1.542(9) . ? C2 C3 1.452(8) . ? C2 C7 1.510(9) . ? C3 C4 1.435(8) . ? C3 C8 1.526(8) . ? C4 C5 1.444(8) . ? C4 C9 1.485(8) . ? C5 C10 1.521(8) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.557(8) . ? C30 C31 1.524(9) . ? B1 F11 1.249(18) . ? B1 F11' 1.30(2) . ? B1 F13 1.348(10) . ? B1 F10 1.385(9) . ? B1 F12' 1.415(16) . ? B1 F12 1.474(12) . ? B1 F13' 1.558(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 Ir1 C2 95.3(2) . . ? C29 Ir1 O1 88.88(18) . . ? C2 Ir1 O1 147.6(2) . . ? C29 Ir1 C1 126.8(2) . . ? C2 Ir1 C1 38.2(2) . . ? O1 Ir1 C1 143.5(2) . . ? C29 Ir1 C3 97.7(2) . . ? C2 Ir1 C3 38.3(2) . . ? O1 Ir1 C3 109.34(18) . . ? C1 Ir1 C3 63.1(2) . . ? C29 Ir1 C5 157.7(2) . . ? C2 Ir1 C5 63.1(2) . . ? O1 Ir1 C5 106.68(18) . . ? C1 Ir1 C5 37.0(2) . . ? C3 Ir1 C5 62.5(2) . . ? C29 Ir1 C4 130.2(2) . . ? C2 Ir1 C4 62.7(2) . . ? O1 Ir1 C4 90.32(17) . . ? C1 Ir1 C4 61.8(2) . . ? C3 Ir1 C4 37.0(2) . . ? C5 Ir1 C4 36.93(19) . . ? C29 Ir1 P1 92.03(15) . . ? C2 Ir1 P1 123.24(18) . . ? O1 Ir1 P1 88.57(11) . . ? C1 Ir1 P1 96.84(16) . . ? C3 Ir1 P1 159.65(15) . . ? C5 Ir1 P1 103.92(14) . . ? C4 Ir1 P1 137.71(14) . . ? C28 P1 C16 104.38(16) . . ? C28 P1 C22 101.57(17) . . ? C16 P1 C22 104.35(17) . . ? C28 P1 Ir1 117.41(11) . . ? C16 P1 Ir1 110.79(13) . . ? C22 P1 Ir1 116.80(14) . . ? C5 C1 C2 109.3(5) . . ? C5 C1 C6 125.2(6) . . ? C2 C1 C6 124.8(6) . . ? C5 C1 Ir1 73.8(3) . . ? C2 C1 Ir1 70.2(3) . . ? C6 C1 Ir1 129.7(4) . . ? C1 C2 C3 106.9(5) . . ? C1 C2 C7 125.6(6) . . ? C3 C2 C7 126.2(6) . . ? C1 C2 Ir1 71.6(3) . . ? C3 C2 Ir1 72.2(3) . . ? C7 C2 Ir1 131.3(5) . . ? C4 C3 C2 107.8(5) . . ? C4 C3 C8 125.2(5) . . ? C2 C3 C8 126.4(6) . . ? C4 C3 Ir1 73.5(3) . . ? C2 C3 Ir1 69.5(3) . . ? C8 C3 Ir1 129.4(4) . . ? C3 C4 C5 108.5(5) . . ? C3 C4 C9 126.4(5) . . ? C5 C4 C9 125.0(5) . . ? C3 C4 Ir1 69.5(3) . . ? C5 C4 Ir1 71.1(3) . . ? C9 C4 Ir1 126.9(4) . . ? C1 C5 C4 107.4(5) . . ? C1 C5 C10 126.3(6) . . ? C4 C5 C10 125.0(5) . . ? C1 C5 Ir1 69.3(3) . . ? C4 C5 Ir1 72.0(3) . . ? C10 C5 Ir1 133.8(4) . . ? C12 C11 C16 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 P1 118.5(2) . . ? C11 C16 P1 121.5(2) . . ? C18 C17 C22 120.0 . . ? C19 C18 C17 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C21 C22 P1 121.13(19) . . ? C17 C22 P1 118.81(19) . . ? C24 C23 C28 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 P1 119.60(18) . . ? C23 C28 P1 120.40(18) . . ? F1 C29 F2 101.4(4) . . ? F1 C29 C30 103.7(4) . . ? F2 C29 C30 100.8(4) . . ? F1 C29 Ir1 116.0(3) . . ? F2 C29 Ir1 110.6(4) . . ? C30 C29 Ir1 121.6(4) . . ? F4 C30 F3 107.3(4) . . ? F4 C30 C31 105.8(5) . . ? F3 C30 C31 107.0(4) . . ? F4 C30 C29 108.9(4) . . ? F3 C30 C29 108.3(5) . . ? C31 C30 C29 119.1(5) . . ? F6 C31 F5 108.8(5) . . ? F6 C31 F7 107.0(5) . . ? F5 C31 F7 105.9(5) . . ? F6 C31 C30 112.5(5) . . ? F5 C31 C30 109.8(5) . . ? F7 C31 C30 112.7(5) . . ? F11 B1 F11' 23.7(16) . . ? F11 B1 F13 116.8(11) . . ? F11' B1 F13 129.5(10) . . ? F11 B1 F10 117.7(13) . . ? F11' B1 F10 118.0(10) . . ? F13 B1 F10 110.1(6) . . ? F11 B1 F12' 123.1(14) . . ? F11' B1 F12' 116.2(14) . . ? F13 B1 F12' 42.1(8) . . ? F10 B1 F12' 119.1(10) . . ? F11 B1 F12 106.8(11) . . ? F11' B1 F12 83.4(13) . . ? F13 B1 F12 105.8(8) . . ? F10 B1 F12 96.7(7) . . ? F12' B1 F12 64.2(9) . . ? F11 B1 F13' 76.2(11) . . ? F11' B1 F13' 99.7(13) . . ? F13 B1 F13' 58.1(7) . . ? F10 B1 F13' 97.8(7) . . ? F12' B1 F13' 98.5(11) . . ? F12 B1 F13' 161.4(9) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.944 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.152 #===END