Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Simon B. Duckett' _publ_contact_author_address ;Department of Chemistry, University of York, Heslington York YO10 5DD United Kingdom ; _publ_contact_author_email sbd3@york.ac.uk loop_ _publ_author_name _publ_author_address S.B.Duckett ;Department of Chemistry, University of York, Heslington York YO10 5DD United Kingdom ; J.P.Dunne ;Department of Chemistry, University of York, Heslington York YO10 5DD United Kingdom ; C.Godard ;Department of Chemistry, University of York, Heslington York YO10 5DD United Kingdom ; A.C.Whitwood ;Department of Chemistry, University of York, Heslington York YO10 5DD United Kingdom ; R.Malacea ; Laboratoire de Chimie de Coordination CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; ; J.-C.Daran ; ; Laboratoire de Chimie de Coordination CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; E.Manoury ; Laboratoire de Chimie de Coordination CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; R.Poli ; Laboratoire de Chimie de Coordination CNRS 205 Route de Narbonne 31077 Toulouse Cedex France ; _publ_section_title ; Parahydrogen studies of H2 addition to Ir(I) complexes containing chiral phosphine-thioether ligands: Implications for catalysis. ; data_StBu _database_code_depnum_ccdc_archive 'CCDC 258501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H29 Cl Fe Ir O P S' _chemical_formula_sum 'C28 H29 Cl Fe Ir O P S' _chemical_formula_weight 728.04 _chemical_compound_source 'synthesis as described' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6773(11) _cell_length_b 8.0559(6) _cell_length_c 21.5594(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.933(2) _cell_angle_gamma 90.00 _cell_volume 2535.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 8034 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.98 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 6.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03;(Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19647 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4479 _reflns_number_gt 4101 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 ' _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^)+(0.0233P)^2^+2.1478P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4479 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.704250(9) 0.295054(16) 0.810684(6) 0.01558(6) Uani 1 1 d . . . Cl1 Cl 0.70315(8) 0.13856(12) 0.71758(4) 0.0311(2) Uani 1 1 d . . . P1 P 0.73557(6) 0.42251(11) 0.90135(4) 0.01414(19) Uani 1 1 d . . . S2 S 0.74466(6) 0.52663(11) 0.74892(4) 0.01726(19) Uani 1 1 d . . . C11 C 0.6632(2) 0.1112(5) 0.84925(17) 0.0214(8) Uani 1 1 d . . . O11 O 0.6348(2) -0.0046(4) 0.87097(13) 0.0333(7) Uani 1 1 d . . . Fe1 Fe 0.95552(3) 0.50604(6) 0.86644(2) 0.01687(12) Uani 1 1 d . . . C1 C 0.8336(2) 0.5574(4) 0.90096(16) 0.0152(7) Uani 1 1 d . . . C2 C 0.8485(3) 0.6696(4) 0.85132(17) 0.0173(8) Uani 1 1 d . . . C3 C 0.9319(3) 0.7568(5) 0.86964(18) 0.0203(8) Uani 1 1 d . . . H3 H 0.9584 0.8403 0.8461 0.024 Uiso 1 1 calc R . . C4 C 0.9681(3) 0.6966(5) 0.92916(18) 0.0214(8) Uani 1 1 d . . . H4 H 1.0235 0.7323 0.9520 0.026 Uiso 1 1 calc R . . C5 C 0.9080(2) 0.5753(4) 0.94858(16) 0.0163(7) Uani 1 1 d . . . H5 H 0.9157 0.5157 0.9868 0.020 Uiso 1 1 calc R . . C6 C 0.9498(3) 0.2796(5) 0.8218(2) 0.0269(9) Uani 1 1 d . . . H6 H 0.8972 0.2115 0.8130 0.032 Uiso 1 1 calc R . . C7 C 0.9795(3) 0.4046(5) 0.78249(18) 0.0294(10) Uani 1 1 d . . . H7 H 0.9502 0.4360 0.7429 0.035 Uiso 1 1 calc R . . C8 C 1.0613(3) 0.4752(5) 0.81287(19) 0.0291(9) Uani 1 1 d . . . H8 H 1.0963 0.5619 0.7971 0.035 Uiso 1 1 calc R . . C9 C 1.0809(3) 0.3933(5) 0.87047(19) 0.0280(9) Uani 1 1 d . . . H9 H 1.1318 0.4152 0.9002 0.034 Uiso 1 1 calc R . . C10 C 1.0123(3) 0.2735(5) 0.8766(2) 0.0282(9) Uani 1 1 d . . . H10 H 1.0085 0.2016 0.9112 0.034 Uiso 1 1 calc R . . C21 C 0.7841(3) 0.7084(4) 0.79510(18) 0.0219(8) Uani 1 1 d . . . H21A H 0.8147 0.7855 0.7681 0.026 Uiso 1 1 calc R . . H21B H 0.7300 0.7664 0.8086 0.026 Uiso 1 1 calc R . . C111 C 0.6484(2) 0.5562(4) 0.92973(16) 0.0157(7) Uani 1 1 d . . . C112 C 0.6706(3) 0.6878(4) 0.97071(18) 0.0209(8) Uani 1 1 d . . . H112 H 0.7328 0.7104 0.9848 0.025 Uiso 1 1 calc R . . C113 C 0.6011(3) 0.7855(5) 0.99075(19) 0.0264(9) Uani 1 1 d . . . H113 H 0.6162 0.8749 1.0187 0.032 Uiso 1 1 calc R . . C114 C 0.5109(3) 0.7538(5) 0.97050(19) 0.0271(9) Uani 1 1 d . . . H114 H 0.4638 0.8194 0.9852 0.033 Uiso 1 1 calc R . . C115 C 0.4887(3) 0.6254(5) 0.92847(18) 0.0263(9) Uani 1 1 d . . . H115 H 0.4266 0.6055 0.9133 0.032 Uiso 1 1 calc R . . C116 C 0.5569(2) 0.5271(5) 0.90885(17) 0.0214(8) Uani 1 1 d . . . H116 H 0.5414 0.4384 0.8807 0.026 Uiso 1 1 calc R . . C121 C 0.7705(2) 0.2825(4) 0.96671(17) 0.0158(8) Uani 1 1 d . . . C122 C 0.8183(2) 0.1369(4) 0.95553(17) 0.0183(8) Uani 1 1 d . . . H122 H 0.8312 0.1114 0.9143 0.022 Uiso 1 1 calc R . . C123 C 0.8468(3) 0.0296(5) 1.00377(18) 0.0230(8) Uani 1 1 d . . . H123 H 0.8793 -0.0686 0.9956 0.028 Uiso 1 1 calc R . . C124 C 0.8282(2) 0.0652(5) 1.06398(18) 0.0234(8) Uani 1 1 d . . . H124 H 0.8471 -0.0092 1.0970 0.028 Uiso 1 1 calc R . . C125 C 0.7819(3) 0.2098(5) 1.07599(18) 0.0228(9) Uani 1 1 d . . . H125 H 0.7699 0.2352 1.1174 0.027 Uiso 1 1 calc R . . C126 C 0.7530(2) 0.3176(5) 1.02770(17) 0.0197(8) Uani 1 1 d . . . H126 H 0.7210 0.4161 1.0363 0.024 Uiso 1 1 calc R . . C211 C 0.6402(2) 0.6149(5) 0.70203(17) 0.0209(8) Uani 1 1 d . . . C212 C 0.5742(3) 0.6912(6) 0.7437(2) 0.0356(11) Uani 1 1 d . . . H21C H 0.5181 0.7252 0.7183 0.053 Uiso 1 1 calc R . . H21D H 0.6028 0.7883 0.7651 0.053 Uiso 1 1 calc R . . H21E H 0.5592 0.6092 0.7747 0.053 Uiso 1 1 calc R . . C213 C 0.5939(3) 0.4750(5) 0.66403(18) 0.0265(9) Uani 1 1 d . . . H21F H 0.5669 0.3971 0.6919 0.040 Uiso 1 1 calc R . . H21G H 0.6391 0.4169 0.6416 0.040 Uiso 1 1 calc R . . H21H H 0.5456 0.5205 0.6340 0.040 Uiso 1 1 calc R . . C214 C 0.6763(3) 0.7409(5) 0.6582(2) 0.0301(10) Uani 1 1 d . . . H21I H 0.7177 0.6855 0.6318 0.045 Uiso 1 1 calc R . . H21J H 0.7097 0.8283 0.6826 0.045 Uiso 1 1 calc R . . H21K H 0.6249 0.7900 0.6318 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01610(9) 0.01599(9) 0.01447(9) -0.00132(5) 0.00079(6) -0.00051(6) Cl1 0.0501(6) 0.0230(5) 0.0204(5) -0.0060(4) 0.0047(4) 0.0002(5) P1 0.0123(4) 0.0157(4) 0.0144(4) -0.0005(4) 0.0012(3) 0.0007(4) S2 0.0172(4) 0.0195(5) 0.0146(4) 0.0015(4) -0.0006(3) 0.0012(4) C11 0.0200(19) 0.022(2) 0.020(2) -0.0050(17) -0.0059(15) -0.0004(17) O11 0.0352(17) 0.0286(16) 0.0350(17) 0.0081(13) -0.0021(13) -0.0133(14) Fe1 0.0129(3) 0.0223(3) 0.0156(3) -0.0009(2) 0.0021(2) 0.0006(2) C1 0.0128(17) 0.0164(17) 0.0164(18) -0.0035(14) 0.0020(14) 0.0005(14) C2 0.0190(19) 0.0151(17) 0.0178(19) 0.0001(14) 0.0013(15) 0.0014(15) C3 0.019(2) 0.0202(18) 0.023(2) -0.0028(16) 0.0034(16) -0.0046(16) C4 0.0154(19) 0.028(2) 0.020(2) -0.0069(16) 0.0000(15) -0.0014(16) C5 0.0157(18) 0.0212(18) 0.0123(17) -0.0010(14) 0.0021(14) 0.0022(15) C6 0.019(2) 0.030(2) 0.033(2) -0.0153(18) 0.0093(18) 0.0043(17) C7 0.025(2) 0.046(3) 0.018(2) -0.0109(19) 0.0056(17) 0.0086(19) C8 0.021(2) 0.038(2) 0.032(2) -0.0031(19) 0.0162(18) 0.0022(18) C9 0.0140(19) 0.038(2) 0.032(2) -0.0066(19) 0.0015(16) 0.0078(18) C10 0.025(2) 0.025(2) 0.035(2) -0.0013(18) 0.0059(19) 0.0110(17) C21 0.024(2) 0.019(2) 0.021(2) 0.0023(15) -0.0041(16) -0.0017(16) C111 0.0153(18) 0.0170(18) 0.0152(18) 0.0039(14) 0.0031(14) 0.0019(14) C112 0.020(2) 0.0218(19) 0.021(2) 0.0001(15) 0.0011(16) 0.0033(16) C113 0.038(2) 0.021(2) 0.021(2) 0.0018(16) 0.0047(18) 0.0077(17) C114 0.028(2) 0.030(2) 0.025(2) 0.0119(18) 0.0101(18) 0.0134(18) C115 0.0175(19) 0.034(2) 0.027(2) 0.0050(18) 0.0033(16) 0.0057(17) C116 0.0209(19) 0.026(2) 0.0181(19) -0.0018(16) 0.0042(15) -0.0008(16) C121 0.0137(18) 0.0178(18) 0.0155(18) -0.0013(14) -0.0012(14) -0.0038(14) C122 0.0148(18) 0.0195(19) 0.0199(19) -0.0036(15) -0.0011(15) -0.0005(15) C123 0.0197(19) 0.0172(18) 0.032(2) -0.0013(16) 0.0002(17) 0.0022(15) C124 0.0183(19) 0.024(2) 0.026(2) 0.0106(17) -0.0027(16) -0.0047(16) C125 0.020(2) 0.031(2) 0.019(2) 0.0053(16) 0.0068(16) -0.0031(16) C126 0.0156(18) 0.0211(19) 0.022(2) -0.0010(15) 0.0024(15) 0.0032(15) C211 0.0195(19) 0.023(2) 0.0188(19) 0.0015(16) -0.0032(15) 0.0066(16) C212 0.022(2) 0.056(3) 0.028(2) -0.011(2) -0.0059(18) 0.016(2) C213 0.023(2) 0.030(2) 0.025(2) -0.0004(17) -0.0049(17) 0.0013(17) C214 0.037(3) 0.023(2) 0.028(2) 0.0041(17) -0.0097(19) 0.0016(19) _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 1.830(4) . ? Ir1 P1 2.2137(9) . ? Ir1 Cl1 2.3690(9) . ? Ir1 S2 2.4018(9) . ? P1 C1 1.804(4) . ? P1 C111 1.826(3) . ? P1 C121 1.836(4) . ? S2 C21 1.831(4) . ? S2 C211 1.886(4) . ? C11 O11 1.142(5) . ? Fe1 C4 2.042(4) . ? Fe1 C8 2.043(4) . ? Fe1 C9 2.046(4) . ? Fe1 C5 2.047(3) . ? Fe1 C7 2.049(4) . ? Fe1 C2 2.050(4) . ? Fe1 C1 2.050(3) . ? Fe1 C3 2.052(4) . ? Fe1 C10 2.053(4) . ? Fe1 C6 2.060(4) . ? C1 C5 1.427(5) . ? C1 C2 1.435(5) . ? C2 C3 1.431(5) . ? C2 C21 1.491(5) . ? C3 C4 1.422(5) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.413(6) . ? C6 C10 1.420(6) . ? C6 H6 0.9500 . ? C7 C8 1.425(6) . ? C7 H7 0.9500 . ? C8 C9 1.409(6) . ? C8 H8 0.9500 . ? C9 C10 1.411(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C111 C116 1.391(5) . ? C111 C112 1.396(5) . ? C112 C113 1.392(5) . ? C112 H112 0.9500 . ? C113 C114 1.375(6) . ? C113 H113 0.9500 . ? C114 C115 1.391(6) . ? C114 H114 0.9500 . ? C115 C116 1.377(5) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.395(5) . ? C121 C122 1.400(5) . ? C122 C123 1.383(5) . ? C122 H122 0.9500 . ? C123 C124 1.384(5) . ? C123 H123 0.9500 . ? C124 C125 1.386(5) . ? C124 H124 0.9500 . ? C125 C126 1.388(5) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C213 1.513(5) . ? C211 C212 1.517(5) . ? C211 C214 1.519(6) . ? C212 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C213 H21F 0.9800 . ? C213 H21G 0.9800 . ? C213 H21H 0.9800 . ? C214 H21I 0.9800 . ? C214 H21J 0.9800 . ? C214 H21K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ir1 P1 91.27(11) . . ? C11 Ir1 Cl1 88.89(12) . . ? P1 Ir1 Cl1 167.85(4) . . ? C11 Ir1 S2 172.73(11) . . ? P1 Ir1 S2 95.08(3) . . ? Cl1 Ir1 S2 85.64(3) . . ? C1 P1 C111 103.48(16) . . ? C1 P1 C121 102.34(16) . . ? C111 P1 C121 104.78(16) . . ? C1 P1 Ir1 111.61(12) . . ? C111 P1 Ir1 118.74(12) . . ? C121 P1 Ir1 114.13(12) . . ? C21 S2 C211 100.57(17) . . ? C21 S2 Ir1 113.71(13) . . ? C211 S2 Ir1 110.88(12) . . ? O11 C11 Ir1 176.8(3) . . ? C4 Fe1 C8 116.34(17) . . ? C4 Fe1 C9 106.64(16) . . ? C8 Fe1 C9 40.33(17) . . ? C4 Fe1 C5 40.31(15) . . ? C8 Fe1 C5 150.31(16) . . ? C9 Fe1 C5 118.00(15) . . ? C4 Fe1 C7 150.79(17) . . ? C8 Fe1 C7 40.75(16) . . ? C9 Fe1 C7 67.95(16) . . ? C5 Fe1 C7 167.95(16) . . ? C4 Fe1 C2 68.73(15) . . ? C8 Fe1 C2 127.04(16) . . ? C9 Fe1 C2 164.36(16) . . ? C5 Fe1 C2 68.81(14) . . ? C7 Fe1 C2 108.33(15) . . ? C4 Fe1 C1 68.30(14) . . ? C8 Fe1 C1 166.49(16) . . ? C9 Fe1 C1 152.76(16) . . ? C5 Fe1 C1 40.77(13) . . ? C7 Fe1 C1 129.59(15) . . ? C2 Fe1 C1 40.98(14) . . ? C4 Fe1 C3 40.66(15) . . ? C8 Fe1 C3 106.23(16) . . ? C9 Fe1 C3 126.16(16) . . ? C5 Fe1 C3 68.20(15) . . ? C7 Fe1 C3 117.86(17) . . ? C2 Fe1 C3 40.82(15) . . ? C1 Fe1 C3 68.42(14) . . ? C4 Fe1 C10 127.42(16) . . ? C8 Fe1 C10 68.04(17) . . ? C9 Fe1 C10 40.27(16) . . ? C5 Fe1 C10 109.09(16) . . ? C7 Fe1 C10 68.02(17) . . ? C2 Fe1 C10 154.06(16) . . ? C1 Fe1 C10 120.33(16) . . ? C3 Fe1 C10 164.36(16) . . ? C4 Fe1 C6 166.39(17) . . ? C8 Fe1 C6 67.96(16) . . ? C9 Fe1 C6 67.65(16) . . ? C5 Fe1 C6 130.16(16) . . ? C7 Fe1 C6 40.22(17) . . ? C2 Fe1 C6 120.08(16) . . ? C1 Fe1 C6 110.71(15) . . ? C3 Fe1 C6 152.67(16) . . ? C10 Fe1 C6 40.40(17) . . ? C5 C1 C2 108.0(3) . . ? C5 C1 P1 127.5(3) . . ? C2 C1 P1 124.5(3) . . ? C5 C1 Fe1 69.49(19) . . ? C2 C1 Fe1 69.5(2) . . ? P1 C1 Fe1 127.36(18) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 C21 125.0(3) . . ? C1 C2 C21 127.2(3) . . ? C3 C2 Fe1 69.7(2) . . ? C1 C2 Fe1 69.52(19) . . ? C21 C2 Fe1 132.5(3) . . ? C4 C3 C2 108.1(3) . . ? C4 C3 Fe1 69.3(2) . . ? C2 C3 Fe1 69.5(2) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe1 C3 H3 126.8 . . ? C5 C4 C3 108.5(3) . . ? C5 C4 Fe1 70.0(2) . . ? C3 C4 Fe1 70.0(2) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 108.2(3) . . ? C4 C5 Fe1 69.7(2) . . ? C1 C5 Fe1 69.74(19) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe1 C5 H5 126.3 . . ? C7 C6 C10 108.1(4) . . ? C7 C6 Fe1 69.5(2) . . ? C10 C6 Fe1 69.5(2) . . ? C7 C6 H6 125.9 . . ? C10 C6 H6 125.9 . . ? Fe1 C6 H6 126.7 . . ? C6 C7 C8 107.8(4) . . ? C6 C7 Fe1 70.3(2) . . ? C8 C7 Fe1 69.4(2) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? Fe1 C7 H7 125.8 . . ? C9 C8 C7 107.7(4) . . ? C9 C8 Fe1 69.9(2) . . ? C7 C8 Fe1 69.8(2) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? Fe1 C8 H8 125.7 . . ? C8 C9 C10 108.7(4) . . ? C8 C9 Fe1 69.8(2) . . ? C10 C9 Fe1 70.1(2) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 126.0 . . ? C9 C10 C6 107.6(4) . . ? C9 C10 Fe1 69.6(2) . . ? C6 C10 Fe1 70.1(2) . . ? C9 C10 H10 126.2 . . ? C6 C10 H10 126.2 . . ? Fe1 C10 H10 125.7 . . ? C2 C21 S2 114.4(3) . . ? C2 C21 H21A 108.7 . . ? S2 C21 H21A 108.7 . . ? C2 C21 H21B 108.7 . . ? S2 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C116 C111 C112 119.1(3) . . ? C116 C111 P1 118.6(3) . . ? C112 C111 P1 122.3(3) . . ? C113 C112 C111 119.7(4) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C114 C113 C112 120.6(4) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.8(4) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C116 C115 C114 119.9(4) . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 C111 120.8(4) . . ? C115 C116 H116 119.6 . . ? C111 C116 H116 119.6 . . ? C126 C121 C122 118.4(3) . . ? C126 C121 P1 122.4(3) . . ? C122 C121 P1 119.2(3) . . ? C123 C122 C121 120.8(3) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 120.1(4) . . ? C122 C123 H123 119.9 . . ? C124 C123 H123 119.9 . . ? C123 C124 C125 119.8(3) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C124 C125 C126 120.2(4) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C126 C121 120.6(3) . . ? C125 C126 H126 119.7 . . ? C121 C126 H126 119.7 . . ? C213 C211 C212 110.1(3) . . ? C213 C211 C214 109.1(3) . . ? C212 C211 C214 112.5(3) . . ? C213 C211 S2 107.7(3) . . ? C212 C211 S2 111.6(3) . . ? C214 C211 S2 105.6(3) . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C211 C213 H21F 109.5 . . ? C211 C213 H21G 109.5 . . ? H21F C213 H21G 109.5 . . ? C211 C213 H21H 109.5 . . ? H21F C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C211 C214 H21I 109.5 . . ? C211 C214 H21J 109.5 . . ? H21I C214 H21J 109.5 . . ? C211 C214 H21K 109.5 . . ? H21I C214 H21K 109.5 . . ? H21J C214 H21K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.592 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.113 #====END data_SPh _database_code_depnum_ccdc_archive 'CCDC 297786' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H25 Cl Fe Ir O P S, 0.25(C Cl2)' _chemical_formula_sum 'C30.25 H25 Cl1.50 Fe Ir O P S' _chemical_formula_weight 768.79 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3886(11) _cell_length_b 10.4105(11) _cell_length_c 14.7920(14) _cell_angle_alpha 70.514(11) _cell_angle_beta 79.099(12) _cell_angle_gamma 66.987(12) _cell_volume 1384.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 26.04 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.1354 _exptl_absorpt_correction_T_max 0.1657 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 167 frames (3 min per frame) were obtained with 0 < \f < 250\% and with the crystals rotated through 1.5\% in \f. Coverage of the unique set was over 92.5% complete to at least 26.04\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 10375 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5064 _reflns_number_gt 4096 _reflns_threshold_expression >2\s(I) _computing_data_collection 'IPDS software, 2.93 (Stoe, 2000)' _computing_cell_refinement 'IPDS software, 2.93 (Stoe, 2000)' _computing_data_reduction 'Stoe, Xred-1.07, 1996' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5064 _refine_ls_number_parameters 344 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.42134(3) 0.43804(3) 0.27583(2) 0.02412(9) Uani 1 1 d . . . Fe1 Fe 0.08865(10) 0.36059(10) 0.19477(8) 0.0315(2) Uani 1 1 d . . . S2 S 0.31902(16) 0.27608(16) 0.39096(13) 0.0268(3) Uani 1 1 d . . . Cl1 Cl 0.63658(16) 0.25582(17) 0.33466(15) 0.0382(4) Uani 1 1 d . . . C1 C 0.0818(6) 0.5328(7) 0.2353(5) 0.0295(15) Uani 1 1 d . . . C2 C 0.0549(7) 0.4226(7) 0.3175(5) 0.0310(15) Uani 1 1 d . . . C3 C -0.0640(7) 0.4008(9) 0.3015(7) 0.0433(19) Uani 1 1 d . . . H3 H -0.1044 0.3334 0.3443 0.052 Uiso 1 1 calc R . . C4 C -0.1122(7) 0.4949(9) 0.2124(7) 0.043(2) Uani 1 1 d . . . H4 H -0.1908 0.5017 0.1846 0.052 Uiso 1 1 calc R . . C5 C -0.0251(7) 0.5784(8) 0.1700(6) 0.0366(17) Uani 1 1 d . . . H5 H -0.0353 0.6511 0.1097 0.044 Uiso 1 1 calc R . . C6 C 0.2840(8) 0.2592(9) 0.1395(7) 0.048(2) Uani 1 1 d . . . H6 H 0.3659 0.2791 0.1392 0.058 Uiso 1 1 calc R . . C7 C 0.2380(9) 0.1553(8) 0.2133(7) 0.049(2) Uani 1 1 d . . . H7 H 0.2830 0.0935 0.2706 0.058 Uiso 1 1 calc R . . C8 C 0.1119(9) 0.1613(8) 0.1854(6) 0.046(2) Uani 1 1 d . . . H8 H 0.0574 0.1036 0.2213 0.055 Uiso 1 1 calc R . . C9 C 0.0811(9) 0.2670(9) 0.0957(6) 0.0449(19) Uani 1 1 d . . . H9 H 0.0024 0.2929 0.0608 0.054 Uiso 1 1 calc R . . C10 C 0.1888(8) 0.3284(8) 0.0664(6) 0.0414(18) Uani 1 1 d . . . H10 H 0.1952 0.4019 0.0086 0.050 Uiso 1 1 calc R . . C11 C 0.5093(7) 0.5459(8) 0.1839(6) 0.0373(17) Uani 1 1 d . . . O11 O 0.5653(6) 0.6165(7) 0.1243(5) 0.064(2) Uani 1 1 d . . . C21 C 0.1288(7) 0.3596(8) 0.4085(6) 0.0351(16) Uani 1 1 d . . . H21A H 0.0919 0.2853 0.4534 0.042 Uiso 1 1 calc R . . H21B H 0.1073 0.4379 0.4389 0.042 Uiso 1 1 calc R . . C111 C 0.1317(6) 0.7337(6) 0.2963(5) 0.0265(14) Uani 1 1 d . . . C112 C -0.0124(7) 0.8126(7) 0.2959(6) 0.0343(16) Uani 1 1 d . . . H112 H -0.0691 0.7958 0.2608 0.041 Uiso 1 1 calc R . . C113 C -0.0730(8) 0.9145(7) 0.3461(6) 0.0384(18) Uani 1 1 d . . . H113 H -0.1707 0.9690 0.3447 0.046 Uiso 1 1 calc R . . C114 C 0.0076(9) 0.9368(8) 0.3975(6) 0.0434(19) Uani 1 1 d . . . H114 H -0.0347 1.0086 0.4309 0.052 Uiso 1 1 calc R . . C115 C 0.1496(9) 0.8579(8) 0.4026(6) 0.0439(19) Uani 1 1 d . . . H115 H 0.2037 0.8727 0.4407 0.053 Uiso 1 1 calc R . . C116 C 0.2122(7) 0.7565(7) 0.3510(6) 0.0355(16) Uani 1 1 d . . . H116 H 0.3100 0.7026 0.3529 0.043 Uiso 1 1 calc R . . P1 P 0.21649(16) 0.60429(16) 0.22595(13) 0.0244(4) Uani 1 1 d . A . C11A C 0.2188(7) 0.7179(8) 0.1026(6) 0.0385(17) Uani 1 1 d D . . C12A C 0.261(3) 0.6701(17) 0.0223(10) 0.050(2) Uani 0.50 1 d PD A 1 H12A H 0.2871 0.5691 0.0301 0.060 Uiso 0.50 1 calc PR A 1 C13A C 0.269(3) 0.7622(18) -0.0700(12) 0.050(2) Uani 0.50 1 d PD A 1 H13A H 0.2766 0.7294 -0.1242 0.060 Uiso 0.50 1 calc PR A 1 C14A C 0.264(2) 0.9014(16) -0.0827(12) 0.050(2) Uani 0.50 1 d PD A 1 H14A H 0.2779 0.9619 -0.1451 0.060 Uiso 0.50 1 calc PR A 1 C15A C 0.2398(19) 0.9510(15) -0.0035(11) 0.050(2) Uani 0.50 1 d PD A 1 H15A H 0.2338 1.0477 -0.0119 0.060 Uiso 0.50 1 calc PR A 1 C16A C 0.224(2) 0.8620(15) 0.0885(11) 0.050(2) Uani 0.50 1 d PD A 1 H16A H 0.2164 0.8948 0.1427 0.060 Uiso 0.50 1 calc PR A 1 C12B C 0.282(3) 0.6427(15) 0.0354(10) 0.0426(18) Uani 0.50 1 d PD A 2 H12B H 0.3216 0.5394 0.0562 0.051 Uiso 0.50 1 calc PR A 2 C13B C 0.288(2) 0.7150(16) -0.0617(11) 0.0426(18) Uani 0.50 1 d PD A 2 H13B H 0.3445 0.6640 -0.1062 0.051 Uiso 0.50 1 calc PR A 2 C14B C 0.2120(16) 0.8612(16) -0.0930(11) 0.0426(18) Uani 0.50 1 d PD A 2 H14B H 0.2154 0.9130 -0.1592 0.051 Uiso 0.50 1 calc PR A 2 C15B C 0.1303(16) 0.9316(14) -0.0265(10) 0.0426(18) Uani 0.50 1 d PD A 2 H15B H 0.0739 1.0317 -0.0482 0.051 Uiso 0.50 1 calc PR A 2 C16B C 0.1284(16) 0.8602(14) 0.0709(11) 0.0426(18) Uani 0.50 1 d PD A 2 H16B H 0.0661 0.9082 0.1152 0.051 Uiso 0.50 1 calc PR A 2 C211 C 0.3647(7) 0.2555(7) 0.5062(5) 0.0304(15) Uani 1 1 d . . . C212 C 0.3642(8) 0.3742(8) 0.5312(6) 0.0405(18) Uani 1 1 d . . . H212 H 0.3419 0.4678 0.4855 0.049 Uiso 1 1 calc R . . C213 C 0.3966(9) 0.3549(9) 0.6230(7) 0.050(2) Uani 1 1 d . . . H213 H 0.3982 0.4348 0.6397 0.060 Uiso 1 1 calc R . . C214 C 0.4261(8) 0.2197(11) 0.6899(7) 0.053(2) Uani 1 1 d . . . H214 H 0.4459 0.2070 0.7531 0.064 Uiso 1 1 calc R . . C215 C 0.4270(8) 0.1027(9) 0.6649(6) 0.047(2) Uani 1 1 d . . . H215 H 0.4497 0.0094 0.7109 0.056 Uiso 1 1 calc R . . C216 C 0.3954(6) 0.1194(8) 0.5742(6) 0.0330(16) Uani 1 1 d . . . H216 H 0.3947 0.0386 0.5582 0.040 Uiso 1 1 calc R . . C100 C 0.417(3) 0.967(5) 0.028(4) 0.070(12) Uiso 0.25 1 d PD A -1 Cl11 Cl 0.3468(12) 1.1027(10) -0.0869(8) 0.078(3) Uani 0.25 1 d PD A -1 Cl12 Cl 0.5710(12) 0.9882(13) 0.0411(11) 0.084(4) Uani 0.25 1 d PD A -1 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 0.02338(13) 0.01950(12) 0.02925(17) -0.00809(9) -0.00361(9) -0.00563(8) Fe1 0.0320(5) 0.0372(5) 0.0343(7) -0.0141(4) -0.0034(4) -0.0178(4) S2 0.0304(8) 0.0250(7) 0.0264(10) -0.0079(6) -0.0038(6) -0.0101(6) Cl1 0.0253(8) 0.0284(8) 0.0506(13) -0.0056(7) -0.0070(7) -0.0015(6) C1 0.024(3) 0.030(3) 0.033(5) -0.014(3) -0.002(3) -0.004(3) C2 0.028(3) 0.039(4) 0.030(5) -0.013(3) -0.001(3) -0.014(3) C3 0.030(4) 0.063(5) 0.049(6) -0.026(4) 0.005(3) -0.023(4) C4 0.021(3) 0.060(5) 0.057(6) -0.025(4) -0.006(3) -0.014(3) C5 0.029(3) 0.035(4) 0.043(5) -0.013(3) -0.011(3) -0.004(3) C6 0.033(4) 0.052(4) 0.077(7) -0.044(5) 0.005(4) -0.015(3) C7 0.066(5) 0.036(4) 0.053(6) -0.022(4) -0.005(4) -0.019(4) C8 0.068(5) 0.046(4) 0.042(6) -0.017(4) 0.004(4) -0.038(4) C9 0.061(5) 0.050(4) 0.041(6) -0.019(4) -0.006(4) -0.032(4) C10 0.056(5) 0.044(4) 0.037(5) -0.019(4) 0.009(4) -0.029(4) C11 0.028(3) 0.036(4) 0.045(5) -0.007(3) -0.011(3) -0.008(3) O11 0.042(3) 0.072(4) 0.065(5) 0.018(3) -0.014(3) -0.032(3) C21 0.031(3) 0.040(4) 0.036(5) -0.012(3) 0.000(3) -0.015(3) C111 0.031(3) 0.023(3) 0.022(4) -0.006(3) 0.002(3) -0.008(3) C112 0.038(4) 0.031(3) 0.031(5) -0.010(3) 0.002(3) -0.010(3) C113 0.041(4) 0.028(3) 0.037(5) -0.006(3) 0.004(3) -0.007(3) C114 0.059(5) 0.034(4) 0.033(5) -0.021(3) 0.007(4) -0.007(3) C115 0.058(5) 0.039(4) 0.044(6) -0.024(4) -0.005(4) -0.016(4) C116 0.037(4) 0.034(4) 0.036(5) -0.013(3) -0.003(3) -0.010(3) P1 0.0224(8) 0.0205(7) 0.0284(11) -0.0087(7) -0.0035(7) -0.0036(6) C11A 0.035(4) 0.033(4) 0.034(5) -0.008(3) -0.001(3) 0.000(3) C12A 0.077(6) 0.038(4) 0.035(6) -0.004(3) 0.007(4) -0.030(4) C13A 0.077(6) 0.038(4) 0.035(6) -0.004(3) 0.007(4) -0.030(4) C14A 0.077(6) 0.038(4) 0.035(6) -0.004(3) 0.007(4) -0.030(4) C15A 0.077(6) 0.038(4) 0.035(6) -0.004(3) 0.007(4) -0.030(4) C16A 0.077(6) 0.038(4) 0.035(6) -0.004(3) 0.007(4) -0.030(4) C12B 0.056(5) 0.034(4) 0.034(5) -0.004(3) -0.004(3) -0.016(4) C13B 0.056(5) 0.034(4) 0.034(5) -0.004(3) -0.004(3) -0.016(4) C14B 0.056(5) 0.034(4) 0.034(5) -0.004(3) -0.004(3) -0.016(4) C15B 0.056(5) 0.034(4) 0.034(5) -0.004(3) -0.004(3) -0.016(4) C16B 0.056(5) 0.034(4) 0.034(5) -0.004(3) -0.004(3) -0.016(4) C211 0.030(3) 0.030(3) 0.033(5) -0.010(3) -0.005(3) -0.011(3) C212 0.050(4) 0.040(4) 0.041(5) -0.018(3) -0.008(4) -0.019(3) C213 0.055(5) 0.054(5) 0.056(7) -0.028(4) -0.012(4) -0.021(4) C214 0.041(4) 0.082(6) 0.036(6) -0.020(5) -0.013(4) -0.015(4) C215 0.039(4) 0.052(5) 0.037(6) -0.006(4) -0.007(3) -0.007(3) C216 0.026(3) 0.040(4) 0.030(5) -0.008(3) -0.002(3) -0.010(3) Cl11 0.117(9) 0.051(5) 0.061(8) 0.003(5) -0.010(6) -0.039(6) Cl12 0.086(8) 0.072(7) 0.095(12) -0.025(7) -0.020(7) -0.023(6) _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 1.805(8) . ? Ir1 P1 2.2205(16) . ? Ir1 S2 2.3820(17) . ? Ir1 Cl1 2.3820(16) . ? Fe1 C4 2.033(7) . ? Fe1 C3 2.039(8) . ? Fe1 C9 2.040(8) . ? Fe1 C8 2.042(7) . ? Fe1 C6 2.043(7) . ? Fe1 C1 2.045(6) . ? Fe1 C5 2.047(7) . ? Fe1 C2 2.049(7) . ? Fe1 C10 2.051(8) . ? Fe1 C7 2.056(8) . ? S2 C211 1.778(8) . ? S2 C21 1.828(7) . ? C1 C2 1.437(10) . ? C1 C5 1.443(10) . ? C1 P1 1.789(7) . ? C2 C3 1.412(9) . ? C2 C21 1.497(10) . ? C3 C4 1.398(13) . ? C4 C5 1.415(11) . ? C6 C10 1.412(13) . ? C6 C7 1.418(13) . ? C7 C8 1.418(12) . ? C8 C9 1.410(12) . ? C9 C10 1.428(10) . ? C11 O11 1.168(9) . ? C111 C116 1.396(10) . ? C111 C112 1.398(9) . ? C111 P1 1.826(7) . ? C112 C113 1.379(10) . ? C113 C114 1.358(12) . ? C114 C115 1.382(11) . ? C115 C116 1.390(10) . ? P1 C11A 1.815(8) . ? C11A C12A 1.370(15) . ? C11A C12B 1.378(15) . ? C11A C16B 1.383(14) . ? C11A C16A 1.466(14) . ? C12A C13A 1.390(17) . ? C13A C14A 1.381(18) . ? C14A C15A 1.38(2) . ? C15A C16A 1.391(18) . ? C15A Cl11 2.192(17) . ? C12B C13B 1.385(16) . ? C13B C14B 1.372(17) . ? C14B C15B 1.379(19) . ? C15B C16B 1.384(18) . ? C211 C216 1.392(10) . ? C211 C212 1.400(9) . ? C212 C213 1.391(12) . ? C213 C214 1.379(13) . ? C214 C215 1.382(13) . ? C215 C216 1.380(12) . ? C100 Cl12 1.749(10) . ? C100 Cl11 1.87(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 C11 Ir1 P1 89.4(2) . . ? C11 Ir1 S2 174.3(2) . . ? P1 Ir1 S2 93.99(6) . . ? C11 Ir1 Cl1 92.7(2) . . ? P1 Ir1 Cl1 177.85(7) . . ? S2 Ir1 Cl1 83.97(6) . . ? C4 Fe1 C3 40.1(4) . . ? C4 Fe1 C9 104.3(3) . . ? C3 Fe1 C9 123.7(3) . . ? C4 Fe1 C8 115.6(3) . . ? C3 Fe1 C8 105.9(3) . . ? C9 Fe1 C8 40.4(3) . . ? C4 Fe1 C6 164.5(4) . . ? C3 Fe1 C6 155.3(4) . . ? C9 Fe1 C6 68.0(3) . . ? C8 Fe1 C6 67.9(3) . . ? C4 Fe1 C1 68.8(3) . . ? C3 Fe1 C1 68.7(3) . . ? C9 Fe1 C1 152.8(3) . . ? C8 Fe1 C1 166.6(3) . . ? C6 Fe1 C1 111.5(3) . . ? C4 Fe1 C5 40.6(3) . . ? C3 Fe1 C5 68.2(3) . . ? C9 Fe1 C5 116.4(3) . . ? C8 Fe1 C5 149.6(3) . . ? C6 Fe1 C5 129.4(3) . . ? C1 Fe1 C5 41.3(3) . . ? C4 Fe1 C2 68.0(3) . . ? C3 Fe1 C2 40.4(3) . . ? C9 Fe1 C2 162.4(3) . . ? C8 Fe1 C2 127.1(3) . . ? C6 Fe1 C2 123.1(3) . . ? C1 Fe1 C2 41.1(3) . . ? C5 Fe1 C2 68.8(3) . . ? C4 Fe1 C10 125.3(4) . . ? C3 Fe1 C10 161.8(3) . . ? C9 Fe1 C10 40.9(3) . . ? C8 Fe1 C10 68.3(3) . . ? C6 Fe1 C10 40.3(4) . . ? C1 Fe1 C10 120.6(3) . . ? C5 Fe1 C10 107.5(3) . . ? C2 Fe1 C10 156.3(3) . . ? C4 Fe1 C7 150.9(3) . . ? C3 Fe1 C7 119.3(4) . . ? C9 Fe1 C7 68.2(4) . . ? C8 Fe1 C7 40.5(3) . . ? C6 Fe1 C7 40.5(4) . . ? C1 Fe1 C7 130.3(3) . . ? C5 Fe1 C7 168.2(3) . . ? C2 Fe1 C7 110.3(3) . . ? C10 Fe1 C7 68.3(4) . . ? C211 S2 C21 98.7(3) . . ? C211 S2 Ir1 107.4(2) . . ? C21 S2 Ir1 112.6(2) . . ? C2 C1 C5 106.9(6) . . ? C2 C1 P1 124.1(5) . . ? C5 C1 P1 128.8(5) . . ? C2 C1 Fe1 69.6(4) . . ? C5 C1 Fe1 69.4(4) . . ? P1 C1 Fe1 129.7(3) . . ? C3 C2 C1 107.9(7) . . ? C3 C2 C21 126.9(7) . . ? C1 C2 C21 124.7(6) . . ? C3 C2 Fe1 69.4(5) . . ? C1 C2 Fe1 69.3(4) . . ? C21 C2 Fe1 133.3(5) . . ? C4 C3 C2 108.7(7) . . ? C4 C3 Fe1 69.7(5) . . ? C2 C3 Fe1 70.2(4) . . ? C3 C4 C5 109.1(6) . . ? C3 C4 Fe1 70.2(4) . . ? C5 C4 Fe1 70.2(4) . . ? C4 C5 C1 107.4(7) . . ? C4 C5 Fe1 69.2(4) . . ? C1 C5 Fe1 69.3(4) . . ? C10 C6 C7 109.2(7) . . ? C10 C6 Fe1 70.1(4) . . ? C7 C6 Fe1 70.2(5) . . ? C6 C7 C8 107.0(8) . . ? C6 C7 Fe1 69.3(4) . . ? C8 C7 Fe1 69.2(5) . . ? C9 C8 C7 108.6(7) . . ? C9 C8 Fe1 69.7(4) . . ? C7 C8 Fe1 70.3(4) . . ? C8 C9 C10 108.1(7) . . ? C8 C9 Fe1 69.9(5) . . ? C10 C9 Fe1 70.0(4) . . ? C6 C10 C9 107.1(7) . . ? C6 C10 Fe1 69.5(5) . . ? C9 C10 Fe1 69.2(5) . . ? O11 C11 Ir1 179.5(7) . . ? C2 C21 S2 113.8(5) . . ? C116 C111 C112 118.8(6) . . ? C116 C111 P1 119.6(5) . . ? C112 C111 P1 121.6(5) . . ? C113 C112 C111 120.5(7) . . ? C114 C113 C112 119.7(7) . . ? C113 C114 C115 121.8(7) . . ? C114 C115 C116 119.0(7) . . ? C115 C116 C111 120.2(7) . . ? C1 P1 C11A 104.8(4) . . ? C1 P1 C111 100.6(3) . . ? C11A P1 C111 104.4(3) . . ? C1 P1 Ir1 114.7(2) . . ? C11A P1 Ir1 115.9(2) . . ? C111 P1 Ir1 114.7(2) . . ? C12A C11A C12B 12.9(13) . . ? C12A C11A C16B 105.1(11) . . ? C12B C11A C16B 117.9(11) . . ? C12A C11A C16A 114.0(11) . . ? C12B C11A C16A 121.1(12) . . ? C16B C11A C16A 44.5(9) . . ? C12A C11A P1 126.1(8) . . ? C12B C11A P1 114.9(8) . . ? C16B C11A P1 123.9(8) . . ? C16A C11A P1 116.3(8) . . ? C11A C12A C13A 123.3(13) . . ? C14A C13A C12A 119.9(15) . . ? C15A C14A C13A 119.0(13) . . ? C14A C15A C16A 121.1(13) . . ? C14A C15A Cl11 87.5(10) . . ? C16A C15A Cl11 142.2(14) . . ? C15A C16A C11A 120.4(13) . . ? C11A C12B C13B 121.3(12) . . ? C14B C13B C12B 119.2(14) . . ? C13B C14B C15B 118.9(13) . . ? C14B C15B C16B 121.7(13) . . ? C11A C16B C15B 118.8(13) . . ? C216 C211 C212 119.6(7) . . ? C216 C211 S2 118.8(5) . . ? C212 C211 S2 121.5(6) . . ? C213 C212 C211 119.9(7) . . ? C214 C213 C212 120.0(8) . . ? C213 C214 C215 119.9(9) . . ? C216 C215 C214 121.0(8) . . ? C215 C216 C211 119.5(7) . . ? Cl12 C100 Cl11 107(2) . . ? C100 Cl11 C15A 60.5(8) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.480 _refine_diff_density_min -2.342 _refine_diff_density_rms 0.162 #====END