Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Danopoulos, Andreas' 'Hursthouse, M. B.' 'Winston, Scott' _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton Hants SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'ad1@soton.ac.uk' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; C-H activation with N-heterocyclic carbene complexes of iridium and rhodium ; _publ_section_references ; WINGX - L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838 ; data_compound1 _database_code_CSD 183891 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02sw031 _chemical_melting_point ? _chemical_formula_moiety 'C31 H43 Cl N3 Rh Si' _chemical_formula_sum 'C31 H43 Cl N3 Rh Si' _chemical_formula_weight 624.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3072(4) _cell_length_b 21.6566(8) _cell_length_c 14.1863(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.8830(10) _cell_angle_gamma 90.00 _cell_volume 3128.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13832 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.35 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9339 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details 'Sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16713 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5658 _reflns_number_gt 4032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+1.0338P] 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 5658 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1506(4) 0.14386(19) 0.2704(3) 0.0253(10) Uani 1 1 d . . . C2 C 0.0712(4) 0.1641(2) 0.4094(3) 0.0388(12) Uani 1 1 d . . . H2 H 0.0528 0.1600 0.4727 0.047 Uiso 1 1 calc R . . C3 C 0.0310(4) 0.2089(2) 0.3477(3) 0.0393(12) Uani 1 1 d . . . H3 H -0.0208 0.2434 0.3599 0.047 Uiso 1 1 calc R . . C4 C 0.2086(4) 0.07089(19) 0.4094(3) 0.0262(10) Uani 1 1 d . . . C5 C 0.2665(4) 0.0256(2) 0.3597(4) 0.0313(11) Uani 1 1 d . . . C6 C 0.3264(5) -0.0227(2) 0.4148(4) 0.0369(12) Uani 1 1 d . . . C7 C 0.3260(4) -0.0249(2) 0.5113(4) 0.0327(11) Uani 1 1 d . . . C8 C 0.2637(4) 0.0215(2) 0.5549(3) 0.0278(10) Uani 1 1 d . . . C9 C 0.0519(4) 0.23626(19) 0.1799(3) 0.0255(10) Uani 1 1 d . . . C10 C 0.1515(4) 0.2754(2) 0.1602(4) 0.0341(12) Uani 1 1 d . . . C11 C 0.1264(5) 0.3102(2) 0.0771(4) 0.0450(14) Uani 1 1 d . . . H11 H 0.1941 0.3356 0.0597 0.054 Uiso 1 1 calc R . . C12 C 0.0080(6) 0.3089(2) 0.0203(4) 0.0510(15) Uani 1 1 d . . . H12 H -0.0062 0.3332 -0.0362 0.061 Uiso 1 1 calc R . . C13 C -0.0907(5) 0.2729(2) 0.0436(4) 0.0464(14) Uani 1 1 d . . . H13 H -0.1737 0.2734 0.0038 0.056 Uiso 1 1 calc R . . C14 C -0.0730(4) 0.23534(19) 0.1246(3) 0.0303(11) Uani 1 1 d . . . C15 C 0.2781(4) 0.2837(2) 0.2293(5) 0.0548(17) Uani 1 1 d . . . H15 H 0.2938 0.2450 0.2680 0.066 Uiso 1 1 calc R . . C16 C 0.2599(6) 0.3366(3) 0.2972(5) 0.086(2) Uani 1 1 d . . . H16A H 0.3412 0.3425 0.3422 0.130 Uiso 1 1 calc R . . H16B H 0.1881 0.3266 0.3325 0.130 Uiso 1 1 calc R . . H16C H 0.2388 0.3746 0.2605 0.130 Uiso 1 1 calc R . . C17 C 0.3968(5) 0.2948(3) 0.1818(6) 0.096(3) Uani 1 1 d . . . H17A H 0.4744 0.2999 0.2306 0.143 Uiso 1 1 calc R . . H17B H 0.3835 0.3323 0.1428 0.143 Uiso 1 1 calc R . . H17C H 0.4097 0.2595 0.1410 0.143 Uiso 1 1 calc R . . C18 C -0.1846(4) 0.1979(2) 0.1521(4) 0.0429(14) Uani 1 1 d . . . H18 H -0.1468 0.1666 0.2004 0.052 Uiso 1 1 calc R . . C19 C -0.2632(4) 0.1633(2) 0.0666(4) 0.0603(18) Uani 1 1 d . . . H19A H -0.3344 0.1398 0.0882 0.090 Uiso 1 1 calc R . . H19B H -0.2048 0.1349 0.0394 0.090 Uiso 1 1 calc R . . H19C H -0.3004 0.1931 0.0179 0.090 Uiso 1 1 calc R . . C20 C -0.2762(4) 0.2400(3) 0.1984(5) 0.0587(17) Uani 1 1 d . . . H20A H -0.3488 0.2156 0.2161 0.088 Uiso 1 1 calc R . . H20B H -0.3114 0.2723 0.1531 0.088 Uiso 1 1 calc R . . H20C H -0.2271 0.2592 0.2556 0.088 Uiso 1 1 calc R . . C21 C 0.1097(5) 0.0747(2) 0.6998(4) 0.0465(14) Uani 1 1 d . . . H21A H 0.1010 0.0772 0.7675 0.070 Uiso 1 1 calc R . . H21B H 0.0293 0.0571 0.6639 0.070 Uiso 1 1 calc R . . H21C H 0.1238 0.1161 0.6756 0.070 Uiso 1 1 calc R . . C22 C 0.2211(5) -0.0542(2) 0.7281(4) 0.0509(14) Uani 1 1 d . . . H22A H 0.2956 -0.0809 0.7206 0.076 Uiso 1 1 calc R . . H22B H 0.1409 -0.0709 0.6906 0.076 Uiso 1 1 calc R . . H22C H 0.2107 -0.0525 0.7955 0.076 Uiso 1 1 calc R . . C23 C 0.4088(4) 0.0562(3) 0.7508(4) 0.0511(14) Uani 1 1 d . . . H23A H 0.4813 0.0288 0.7415 0.077 Uiso 1 1 calc R . . H23B H 0.4032 0.0591 0.8190 0.077 Uiso 1 1 calc R . . H23C H 0.4245 0.0974 0.7262 0.077 Uiso 1 1 calc R . . C31 C 0.3551(4) 0.1247(2) 0.0468(3) 0.0366(12) Uani 1 1 d . . . H31 H 0.4098 0.1550 0.0813 0.044 Uiso 1 1 calc R . . C32 C 0.3762(4) 0.0645(2) 0.0754(3) 0.0316(11) Uani 1 1 d . . . H32 H 0.4423 0.0568 0.1286 0.038 Uiso 1 1 calc R . . C33 C 0.3025(5) 0.0100(2) 0.0286(4) 0.0433(13) Uani 1 1 d . . . H33A H 0.3621 -0.0260 0.0323 0.052 Uiso 1 1 calc R . . H33B H 0.2731 0.0194 -0.0396 0.052 Uiso 1 1 calc R . . C34 C 0.1828(4) -0.0065(2) 0.0756(4) 0.0358(12) Uani 1 1 d . . . H34A H 0.1183 -0.0286 0.0286 0.043 Uiso 1 1 calc R . . H34B H 0.2109 -0.0350 0.1294 0.043 Uiso 1 1 calc R . . C35 C 0.1165(4) 0.0485(2) 0.1122(3) 0.0291(11) Uani 1 1 d . . . H35 H 0.0905 0.0445 0.1733 0.035 Uiso 1 1 calc R . . C36 C 0.0896(4) 0.1044(2) 0.0656(3) 0.0340(11) Uani 1 1 d . . . H36 H 0.0500 0.1359 0.0981 0.041 Uiso 1 1 calc R . . C37 C 0.1188(5) 0.1187(2) -0.0333(3) 0.0423(13) Uani 1 1 d . . . H37A H 0.0508 0.1473 -0.0652 0.051 Uiso 1 1 calc R . . H37B H 0.1131 0.0801 -0.0710 0.051 Uiso 1 1 calc R . . C38 C 0.2541(5) 0.1477(2) -0.0337(4) 0.0474(13) Uani 1 1 d . . . H38A H 0.2840 0.1383 -0.0952 0.057 Uiso 1 1 calc R . . H38B H 0.2467 0.1931 -0.0288 0.057 Uiso 1 1 calc R . . N1 N 0.0766(3) 0.19701(16) 0.2637(2) 0.0271(9) Uani 1 1 d . . . N2 N 0.1459(3) 0.12429(15) 0.3620(2) 0.0260(9) Uani 1 1 d . . . N3 N 0.2063(3) 0.06972(16) 0.5022(3) 0.0281(9) Uani 1 1 d . . . Si1 Si 0.25145(12) 0.02479(6) 0.68536(9) 0.0319(3) Uani 1 1 d . . . Rh1 Rh 0.25844(3) 0.113091(15) 0.17174(2) 0.02329(12) Uani 1 1 d . . . Cl1 Cl 0.45403(10) 0.14005(5) 0.27482(9) 0.0361(3) Uani 1 1 d . . . H5 H 0.263(4) 0.0262(19) 0.291(3) 0.032(12) Uiso 1 1 d . . . H6 H 0.360(4) -0.053(2) 0.388(4) 0.048(16) Uiso 1 1 d . . . H7 H 0.365(4) -0.059(2) 0.552(3) 0.041(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(2) 0.024(3) 0.023(3) -0.005(2) 0.0004(19) -0.0023(19) C2 0.053(3) 0.046(3) 0.018(3) 0.002(2) 0.009(2) 0.023(2) C3 0.051(3) 0.040(3) 0.027(3) 0.001(2) 0.006(2) 0.023(2) C4 0.030(2) 0.028(3) 0.021(3) 0.000(2) 0.0024(19) 0.0016(19) C5 0.039(2) 0.034(3) 0.022(3) -0.001(2) 0.007(2) 0.003(2) C6 0.051(3) 0.029(3) 0.033(3) -0.002(3) 0.015(2) 0.006(2) C7 0.041(3) 0.029(3) 0.028(3) 0.008(2) 0.004(2) 0.006(2) C8 0.029(2) 0.026(3) 0.028(3) 0.002(2) 0.004(2) 0.002(2) C9 0.031(2) 0.022(2) 0.023(3) -0.001(2) 0.0019(19) -0.0001(19) C10 0.035(2) 0.021(3) 0.048(4) -0.007(2) 0.012(2) -0.003(2) C11 0.057(3) 0.028(3) 0.054(4) 0.002(3) 0.023(3) -0.011(2) C12 0.084(4) 0.035(3) 0.033(3) 0.014(3) 0.003(3) -0.013(3) C13 0.060(3) 0.037(3) 0.032(3) 0.007(3) -0.023(3) -0.006(3) C14 0.034(2) 0.025(3) 0.029(3) 0.004(2) -0.003(2) -0.001(2) C15 0.032(3) 0.027(3) 0.100(5) -0.005(3) -0.006(3) -0.003(2) C16 0.074(4) 0.062(4) 0.104(6) -0.036(4) -0.046(4) 0.007(3) C17 0.037(3) 0.050(4) 0.203(10) 0.015(5) 0.029(4) -0.009(3) C18 0.028(2) 0.038(3) 0.061(4) 0.014(3) 0.003(2) 0.000(2) C19 0.035(3) 0.046(3) 0.090(5) 0.010(3) -0.020(3) -0.014(2) C20 0.034(3) 0.057(4) 0.086(5) 0.015(3) 0.014(3) 0.009(3) C21 0.059(3) 0.056(4) 0.026(3) 0.003(3) 0.010(2) 0.017(3) C22 0.068(3) 0.044(3) 0.044(4) 0.008(3) 0.018(3) 0.013(3) C23 0.049(3) 0.073(4) 0.034(3) -0.006(3) 0.014(2) 0.001(3) C31 0.042(3) 0.044(3) 0.027(3) -0.002(2) 0.016(2) -0.008(2) C32 0.031(2) 0.040(3) 0.025(3) -0.008(2) 0.008(2) -0.002(2) C33 0.051(3) 0.038(3) 0.042(3) -0.003(3) 0.010(3) 0.008(2) C34 0.047(3) 0.026(3) 0.033(3) -0.006(2) 0.002(2) -0.006(2) C35 0.033(2) 0.037(3) 0.016(3) -0.002(2) 0.0022(19) -0.004(2) C36 0.030(2) 0.043(3) 0.027(3) -0.015(2) -0.003(2) -0.006(2) C37 0.050(3) 0.047(3) 0.027(3) -0.002(3) -0.005(2) 0.007(2) C38 0.066(3) 0.050(3) 0.027(3) 0.007(3) 0.009(3) 0.005(3) N1 0.0356(19) 0.032(2) 0.013(2) -0.0009(17) 0.0031(16) 0.0086(17) N2 0.0322(18) 0.031(2) 0.014(2) 0.0000(17) 0.0017(15) 0.0083(16) N3 0.0324(19) 0.031(2) 0.020(2) -0.0016(18) 0.0018(16) 0.0030(16) Si1 0.0417(7) 0.0310(7) 0.0242(8) 0.0044(6) 0.0087(6) 0.0092(6) Rh1 0.02438(17) 0.0262(2) 0.0188(2) -0.00181(16) 0.00175(13) -0.00110(15) Cl1 0.0295(6) 0.0413(7) 0.0345(7) -0.0062(6) -0.0046(5) -0.0018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.376(5) . ? C1 N2 1.376(5) . ? C1 Rh1 2.029(4) . ? C2 C3 1.329(6) . ? C2 N2 1.395(5) . ? C3 N1 1.371(6) . ? C4 N3 1.320(5) . ? C4 C5 1.395(6) . ? C4 N2 1.439(5) . ? C5 C6 1.392(7) . ? C6 C7 1.370(7) . ? C7 C8 1.388(6) . ? C8 N3 1.364(5) . ? C8 Si1 1.876(5) . ? C9 C10 1.392(6) . ? C9 C14 1.401(5) . ? C9 N1 1.452(5) . ? C10 C11 1.390(7) . ? C10 C15 1.516(6) . ? C11 C12 1.355(7) . ? C12 C13 1.363(7) . ? C13 C14 1.397(6) . ? C14 C18 1.506(6) . ? C15 C17 1.505(8) . ? C15 C16 1.528(8) . ? C18 C20 1.533(7) . ? C18 C19 1.546(7) . ? C21 Si1 1.854(5) . ? C22 Si1 1.857(5) . ? C23 Si1 1.869(5) . ? C31 C32 1.373(6) . ? C31 C38 1.506(6) . ? C31 Rh1 2.178(4) . ? C32 C33 1.502(6) . ? C32 Rh1 2.227(4) . ? C33 C34 1.532(6) . ? C34 C35 1.504(6) . ? C35 C36 1.386(6) . ? C35 Rh1 2.104(4) . ? C36 C37 1.513(7) . ? C36 Rh1 2.126(4) . ? C37 C38 1.530(6) . ? Rh1 Cl1 2.3734(10) . ? 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 N1 C1 N2 102.9(3) . . ? N1 C1 Rh1 125.7(3) . . ? N2 C1 Rh1 130.8(3) . . ? C3 C2 N2 105.8(4) . . ? C2 C3 N1 108.8(4) . . ? N3 C4 C5 124.4(4) . . ? N3 C4 N2 113.9(4) . . ? C5 C4 N2 121.7(4) . . ? C6 C5 C4 115.5(5) . . ? C7 C6 C5 121.2(5) . . ? C6 C7 C8 119.5(4) . . ? N3 C8 C7 120.1(4) . . ? N3 C8 Si1 115.0(3) . . ? C7 C8 Si1 124.9(3) . . ? C10 C9 C14 122.6(4) . . ? C10 C9 N1 118.6(4) . . ? C14 C9 N1 118.7(4) . . ? C11 C10 C9 117.0(4) . . ? C11 C10 C15 120.8(4) . . ? C9 C10 C15 122.0(5) . . ? C12 C11 C10 121.7(4) . . ? C11 C12 C13 120.3(5) . . ? C12 C13 C14 121.7(4) . . ? C13 C14 C9 116.4(4) . . ? C13 C14 C18 121.2(4) . . ? C9 C14 C18 122.4(4) . . ? C17 C15 C10 114.1(5) . . ? C17 C15 C16 110.5(5) . . ? C10 C15 C16 108.6(4) . . ? C14 C18 C20 109.6(4) . . ? C14 C18 C19 112.8(4) . . ? C20 C18 C19 110.0(4) . . ? C32 C31 C38 126.7(4) . . ? C32 C31 Rh1 73.8(3) . . ? C38 C31 Rh1 107.8(3) . . ? C31 C32 C33 124.7(4) . . ? C31 C32 Rh1 69.9(3) . . ? C33 C32 Rh1 110.8(3) . . ? C32 C33 C34 112.2(4) . . ? C35 C34 C33 113.9(4) . . ? C36 C35 C34 126.5(4) . . ? C36 C35 Rh1 71.7(2) . . ? C34 C35 Rh1 109.9(3) . . ? C35 C36 C37 124.6(4) . . ? C35 C36 Rh1 70.0(2) . . ? C37 C36 Rh1 112.4(3) . . ? C36 C37 C38 113.6(4) . . ? C31 C38 C37 112.6(4) . . ? C3 N1 C1 111.0(4) . . ? C3 N1 C9 124.2(4) . . ? C1 N1 C9 124.8(4) . . ? C1 N2 C2 111.6(3) . . ? C1 N2 C4 127.6(3) . . ? C2 N2 C4 120.8(4) . . ? C4 N3 C8 119.2(4) . . ? C21 Si1 C22 109.0(2) . . ? C21 Si1 C23 111.8(2) . . ? C22 Si1 C23 110.5(2) . . ? C21 Si1 C8 107.8(2) . . ? C22 Si1 C8 109.1(2) . . ? C23 Si1 C8 108.6(2) . . ? C1 Rh1 C35 94.27(16) . . ? C1 Rh1 C36 92.38(17) . . ? C35 Rh1 C36 38.24(16) . . ? C1 Rh1 C31 153.05(18) . . ? C35 Rh1 C31 97.29(18) . . ? C36 Rh1 C31 82.03(17) . . ? C1 Rh1 C32 170.64(18) . . ? C35 Rh1 C32 81.40(16) . . ? C36 Rh1 C32 89.31(17) . . ? C31 Rh1 C32 36.30(16) . . ? C1 Rh1 Cl1 89.89(11) . . ? C35 Rh1 Cl1 151.95(12) . . ? C36 Rh1 Cl1 169.26(13) . . ? C31 Rh1 Cl1 91.22(13) . . ? C32 Rh1 Cl1 90.15(11) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.641 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.093 #==END data_compound2 _database_code_CSD 183892 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02nts02 _chemical_melting_point ? _chemical_formula_moiety 'C70 H63 B F24 N3 Rh Si' _chemical_formula_sum 'C70 H63 B F24 N3 Rh Si' _chemical_formula_weight 1544.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Rh' 'Rh' -1.1178 0.9187 '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' _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 13.1410(4) _cell_length_b 16.6819(4) _cell_length_c 18.5852(7) _cell_angle_alpha 72.2740(10) _cell_angle_beta 69.5560(10) _cell_angle_gamma 69.840(2) _cell_volume 3504.33(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31807 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.368 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9641 _exptl_absorpt_correction_T_max 0.9641 _exptl_absorpt_process_details 'Sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 396(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Chi scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37869 _diffrn_reflns_av_R_equivalents 0.1951 _diffrn_reflns_av_sigmaI/netI 0.2337 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13990 _reflns_number_gt 6714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^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 13990 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1890 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2194 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9349(5) 0.2610(4) 0.2565(4) 0.0232(15) Uani 1 1 d . . . C2 C 0.8954(5) 0.1342(4) 0.2702(4) 0.0322(17) Uani 1 1 d . . . H2 H 0.9033 0.0751 0.2760 0.039 Uiso 1 1 calc R . . C3 C 0.8035(5) 0.1997(4) 0.2641(4) 0.0299(16) Uani 1 1 d . . . H3 H 0.7347 0.1946 0.2652 0.036 Uiso 1 1 calc R . . C4 C 0.7504(5) 0.3636(4) 0.2448(4) 0.0301(17) Uani 1 1 d . . . C5 C 0.7627(5) 0.4112(4) 0.1673(4) 0.0270(15) Uani 1 1 d . . . C6 C 0.6926(5) 0.4964(4) 0.1571(4) 0.0332(17) Uani 1 1 d . . . H6 H 0.6987 0.5309 0.1067 0.040 Uiso 1 1 calc R . . C7 C 0.6152(5) 0.5301(5) 0.2194(5) 0.0372(18) Uani 1 1 d . . . H7 H 0.5710 0.5873 0.2111 0.045 Uiso 1 1 calc R . . C8 C 0.6024(5) 0.4793(4) 0.2952(4) 0.0324(17) Uani 1 1 d . . . H8 H 0.5487 0.5029 0.3368 0.039 Uiso 1 1 calc R . . C9 C 0.6694(5) 0.3929(4) 0.3097(4) 0.0303(16) Uani 1 1 d . . . C10 C 0.8477(6) 0.3775(5) 0.0980(4) 0.0418(19) Uani 1 1 d . . . H10 H 0.8747 0.3141 0.1148 0.050 Uiso 1 1 calc R . . C11 C 0.8014(9) 0.3946(7) 0.0280(5) 0.086(3) Uani 1 1 d . . . H11A H 0.8605 0.3709 -0.0140 0.130 Uiso 1 1 calc R . . H11B H 0.7733 0.4564 0.0105 0.130 Uiso 1 1 calc R . . H11C H 0.7413 0.3673 0.0437 0.130 Uiso 1 1 calc R . . C12 C 0.6506(5) 0.3365(5) 0.3908(4) 0.0353(18) Uani 1 1 d . . . H12 H 0.7215 0.2917 0.3937 0.042 Uiso 1 1 calc R . . C13 C 0.6185(6) 0.3864(5) 0.4554(5) 0.054(2) Uani 1 1 d . . . H13A H 0.6083 0.3469 0.5056 0.081 Uiso 1 1 calc R . . H13B H 0.5496 0.4314 0.4535 0.081 Uiso 1 1 calc R . . H13C H 0.6774 0.4123 0.4476 0.081 Uiso 1 1 calc R . . C14 C 0.5617(6) 0.2898(5) 0.4055(5) 0.050(2) Uani 1 1 d . . . H14A H 0.5512 0.2537 0.4574 0.075 Uiso 1 1 calc R . . H14B H 0.5861 0.2541 0.3676 0.075 Uiso 1 1 calc R . . H14C H 0.4918 0.3322 0.4009 0.075 Uiso 1 1 calc R . . C15 C 1.0922(5) 0.1334(4) 0.2609(4) 0.0258(15) Uani 1 1 d . . . C16 C 1.1324(5) 0.0445(4) 0.2837(4) 0.0330(17) Uani 1 1 d . . . H16 H 1.0841 0.0084 0.3059 0.040 Uiso 1 1 calc R . . C17 C 1.2472(5) 0.0109(4) 0.2726(4) 0.0381(18) Uani 1 1 d . . . H17 H 1.2782 -0.0481 0.2904 0.046 Uiso 1 1 calc R . . C18 C 1.3151(5) 0.0674(4) 0.2341(4) 0.0398(19) Uani 1 1 d . . . H18 H 1.3929 0.0449 0.2231 0.048 Uiso 1 1 calc R . . C19 C 1.2704(5) 0.1564(4) 0.2116(4) 0.0339(17) Uani 1 1 d . . . C20 C 1.4722(6) 0.1451(5) 0.0714(5) 0.054(2) Uani 1 1 d . . . H20A H 1.5140 0.0953 0.1015 0.081 Uiso 1 1 calc R . . H20B H 1.5233 0.1745 0.0299 0.081 Uiso 1 1 calc R . . H20C H 1.4306 0.1261 0.0493 0.081 Uiso 1 1 calc R . . C21 C 1.2943(6) 0.3164(4) 0.0745(4) 0.0436(19) Uani 1 1 d . . . H21A H 1.2423 0.3571 0.1064 0.065 Uiso 1 1 calc R . . H21B H 1.2537 0.2965 0.0524 0.065 Uiso 1 1 calc R . . H21C H 1.3467 0.3446 0.0329 0.065 Uiso 1 1 calc R . . C22 C 1.1624(6) 0.3171(4) 0.3242(5) 0.0373(19) Uani 1 1 d . . . H22 H 1.2007 0.2593 0.3212 0.045 Uiso 1 1 calc R . . C23 C 1.1774(5) 0.3789(4) 0.2558(4) 0.0309(17) Uani 1 1 d . . . H23 H 1.2224 0.3594 0.2100 0.037 Uiso 1 1 calc R . . C24 C 1.1269(5) 0.4759(4) 0.2491(5) 0.042(2) Uani 1 1 d . . . H24A H 1.1803 0.5063 0.2099 0.050 Uiso 1 1 calc R . . H24B H 1.1132 0.4905 0.2990 0.050 Uiso 1 1 calc R . . C25 C 1.0160(5) 0.5075(4) 0.2260(5) 0.042(2) Uani 1 1 d . . . H25A H 0.9732 0.5630 0.2410 0.051 Uiso 1 1 calc R . . H25B H 1.0328 0.5168 0.1694 0.051 Uiso 1 1 calc R . . C26 C 0.9452(5) 0.4441(4) 0.2639(5) 0.0311(17) Uani 1 1 d . . . H26 H 0.9082 0.4365 0.2329 0.037 Uiso 1 1 calc R . . C27 C 0.9292(5) 0.3963(4) 0.3391(5) 0.0371(18) Uani 1 1 d . . . H27 H 0.8861 0.3572 0.3532 0.045 Uiso 1 1 calc R . . C28 C 0.9751(6) 0.4006(5) 0.4025(5) 0.048(2) Uani 1 1 d . . . H28A H 0.9220 0.3890 0.4535 0.057 Uiso 1 1 calc R . . H28B H 0.9823 0.4590 0.3937 0.057 Uiso 1 1 calc R . . C29 C 1.0904(6) 0.3343(5) 0.4029(5) 0.046(2) Uani 1 1 d . . . H29A H 1.1307 0.3556 0.4248 0.055 Uiso 1 1 calc R . . H29B H 1.0782 0.2796 0.4372 0.055 Uiso 1 1 calc R . . C30 C 0.9486(7) 0.4142(5) 0.0705(5) 0.071(3) Uani 1 1 d . . . H30A H 1.0022 0.3907 0.0265 0.107 Uiso 1 1 calc R . . H30B H 0.9830 0.3986 0.1125 0.107 Uiso 1 1 calc R . . H30C H 0.9246 0.4767 0.0552 0.107 Uiso 1 1 calc R . . C31 C 1.4572(6) 0.2479(5) 0.1852(5) 0.057(2) Uani 1 1 d . . . H31A H 1.4080 0.2876 0.2188 0.085 Uiso 1 1 calc R . . H31B H 1.5130 0.2745 0.1458 0.085 Uiso 1 1 calc R . . H31C H 1.4936 0.1952 0.2158 0.085 Uiso 1 1 calc R . . C40 C 0.1745(5) 0.2832(4) 0.8961(4) 0.0307(16) Uani 1 1 d . . . C41 C 0.1704(5) 0.2742(4) 0.8204(4) 0.0223(15) Uani 1 1 d . . . C42 C 0.0987(5) 0.2314(4) 0.8173(4) 0.0256(15) Uani 1 1 d . . . H42 H 0.0550 0.2058 0.8643 0.031 Uiso 1 1 calc R . . C43 C 0.0894(5) 0.2251(4) 0.7463(4) 0.0258(15) Uani 1 1 d . . . C44 C 0.1553(5) 0.2668(4) 0.6777(4) 0.0258(15) Uani 1 1 d . . . H44 H 0.1502 0.2658 0.6293 0.031 Uiso 1 1 calc R . . C45 C 0.2290(5) 0.3103(4) 0.6796(4) 0.0247(15) Uani 1 1 d . . . C46 C 0.2363(5) 0.3132(4) 0.7513(4) 0.0272(16) Uani 1 1 d . . . H46 H 0.2852 0.3411 0.7531 0.033 Uiso 1 1 calc R . . C47 C 0.2926(5) 0.3554(4) 0.6042(5) 0.0369(18) Uani 1 1 d . . . C48 C 0.1840(7) -0.1031(5) 0.9118(6) 0.048(2) Uani 1 1 d . . . C49 C 0.0808(6) -0.0432(4) 0.8902(4) 0.0325(17) Uani 1 1 d . . . C50 C 0.0825(5) 0.0359(4) 0.8376(4) 0.0283(16) Uani 1 1 d . . . H50 H 0.1498 0.0520 0.8179 0.034 Uiso 1 1 calc R . . C51 C -0.0112(5) 0.0933(4) 0.8123(4) 0.0242(15) Uani 1 1 d . . . C52 C -0.1088(5) 0.0637(4) 0.8457(4) 0.0305(16) Uani 1 1 d . . . H52 H -0.1736 0.0978 0.8305 0.037 Uiso 1 1 calc R . . C53 C -0.1134(5) -0.0148(4) 0.9009(4) 0.0286(16) Uani 1 1 d . . . C54 C -0.0184(5) -0.0688(4) 0.9226(4) 0.0320(16) Uani 1 1 d . . . H54 H -0.0206 -0.1216 0.9583 0.038 Uiso 1 1 calc R . . C56 C 0.3009(7) 0.0272(6) 0.5293(8) 0.077(3) Uani 1 1 d . . . C57 C 0.1801(5) 0.0707(4) 0.5614(4) 0.0361(18) Uani 1 1 d . . . C58 C 0.1450(5) 0.1028(4) 0.6294(4) 0.0341(17) Uani 1 1 d . . . H58 H 0.1986 0.0936 0.6552 0.041 Uiso 1 1 calc R . . C59 C 0.0346(5) 0.1480(4) 0.6613(4) 0.0246(15) Uani 1 1 d . . . C60 C -0.0427(5) 0.1573(4) 0.6187(4) 0.0270(16) Uani 1 1 d . . . H60 H -0.1187 0.1843 0.6375 0.032 Uiso 1 1 calc R . . C61 C -0.0061(5) 0.1268(4) 0.5502(4) 0.0304(16) Uani 1 1 d . . . C62 C 0.1042(6) 0.0838(4) 0.5207(4) 0.0369(18) Uani 1 1 d . . . H62 H 0.1269 0.0641 0.4743 0.044 Uiso 1 1 calc R . . C63 C -0.0940(6) 0.1417(5) 0.5095(4) 0.0385(18) Uani 1 1 d . . . C64 C -0.2559(5) 0.4654(4) 0.6248(4) 0.0328(17) Uani 1 1 d . . . C65 C -0.2370(5) 0.3989(4) 0.6958(4) 0.0233(14) Uani 1 1 d . . . C66 C -0.1433(5) 0.3270(4) 0.6900(4) 0.0245(15) Uani 1 1 d . . . H66 H -0.0927 0.3230 0.6408 0.029 Uiso 1 1 calc R . . C67 C -0.1210(5) 0.2606(4) 0.7539(4) 0.0212(14) Uani 1 1 d . . . C68 C -0.1993(5) 0.2712(4) 0.8265(4) 0.0272(15) Uani 1 1 d . . . H68 H -0.1873 0.2293 0.8712 0.033 Uiso 1 1 calc R . . C69 C -0.2944(5) 0.3419(4) 0.8344(4) 0.0257(15) Uani 1 1 d . . . C70 C -0.3141(5) 0.4065(4) 0.7684(4) 0.0276(16) Uani 1 1 d . . . H70 H -0.3778 0.4537 0.7731 0.033 Uiso 1 1 calc R . . C71 C -0.3790(6) 0.3520(5) 0.9121(4) 0.0407(19) Uani 1 1 d . . . C85 C -0.2206(6) -0.0417(5) 0.9366(5) 0.0406(19) Uani 1 1 d . . . C901 C 0.5313(8) 0.1767(6) 0.8106(6) 0.071(3) Uani 1 1 d . . . H901 H 0.5263 0.1752 0.8621 0.085 Uiso 1 1 calc R . . C902 C 0.5975(7) 0.2248(5) 0.7472(6) 0.053(2) Uani 1 1 d . . . H902 H 0.6382 0.2548 0.7563 0.063 Uiso 1 1 calc R . . C903 C 0.6014(7) 0.2269(5) 0.6750(6) 0.059(2) Uani 1 1 d . . . H903 H 0.6427 0.2611 0.6338 0.070 Uiso 1 1 calc R . . C904 C 0.5457(7) 0.1797(5) 0.6574(6) 0.062(3) Uani 1 1 d . . . H904 H 0.5520 0.1806 0.6057 0.075 Uiso 1 1 calc R . . C905 C 0.4826(7) 0.1329(5) 0.7185(8) 0.066(3) Uani 1 1 d . . . C906 C 0.4748(7) 0.1323(5) 0.7945(6) 0.057(2) Uani 1 1 d . . . H906 H 0.4299 0.1009 0.8358 0.069 Uiso 1 1 calc R . . C907 C 0.4202(7) 0.0822(6) 0.7021(8) 0.111(5) Uani 1 1 d . . . H90A H 0.3790 0.0530 0.7508 0.166 Uiso 1 1 calc R . . H90B H 0.4733 0.0398 0.6723 0.166 Uiso 1 1 calc R . . H90C H 0.3687 0.1216 0.6726 0.166 Uiso 1 1 calc R . . N1 N 0.8284(4) 0.2772(3) 0.2557(3) 0.0245(12) Uani 1 1 d . . . N2 N 0.9769(4) 0.1721(3) 0.2661(3) 0.0225(12) Uani 1 1 d . . . N3 N 1.1550(4) 0.1912(3) 0.2313(3) 0.0295(13) Uani 1 1 d . . . Si1 Si 1.37265(15) 0.22116(12) 0.13627(14) 0.0399(5) Uani 1 1 d . . . B1 B -0.0029(6) 0.1820(5) 0.7431(5) 0.0248(17) Uani 1 1 d . . . Rh1 Rh 1.04923(4) 0.31454(3) 0.26083(3) 0.02823(19) Uani 1 1 d . . . F1 F 0.3738(3) 0.3808(3) 0.6112(3) 0.0586(13) Uani 1 1 d . . . F2 F 0.3436(4) 0.3044(3) 0.5521(3) 0.0776(16) Uani 1 1 d . . . F3 F 0.2282(4) 0.4259(3) 0.5708(3) 0.0785(17) Uani 1 1 d . . . F4 F 0.2740(3) 0.2415(3) 0.9116(2) 0.0541(12) Uani 1 1 d . . . F5 F 0.0978(3) 0.2529(2) 0.9577(2) 0.0389(10) Uani 1 1 d . . . F6 F 0.1563(3) 0.3668(2) 0.8980(2) 0.0469(11) Uani 1 1 d . . . F7 F 0.2755(5) -0.0789(5) 0.8715(5) 0.178(4) Uani 1 1 d . . . F8 F 0.1858(6) -0.1081(5) 0.9804(4) 0.147(4) Uani 1 1 d . . . F9 F 0.2101(5) -0.1795(4) 0.9020(5) 0.126(3) Uani 1 1 d . . . F10 F -0.2494(4) -0.0570(3) 1.0152(3) 0.0587(12) Uani 1 1 d . . . F11 F -0.2123(3) -0.1168(2) 0.9183(2) 0.0465(11) Uani 1 1 d . . . F12 F -0.3089(3) 0.0171(3) 0.9146(3) 0.0631(14) Uani 1 1 d . . . F13 F -0.3437(3) 0.2952(3) 0.9724(2) 0.0456(11) Uani 1 1 d . . . F14 F -0.4754(3) 0.3370(3) 0.9168(2) 0.0641(14) Uani 1 1 d . . . F15 F -0.4050(4) 0.4312(3) 0.9252(3) 0.0744(15) Uani 1 1 d . . . F16 F -0.3063(4) 0.4441(3) 0.5851(2) 0.0542(12) Uani 1 1 d . . . F17 F -0.1588(3) 0.4796(2) 0.5737(2) 0.0401(10) Uani 1 1 d . . . F18 F -0.3192(3) 0.5437(2) 0.6404(2) 0.0474(11) Uani 1 1 d . . . F19 F -0.1455(4) 0.2270(3) 0.4912(3) 0.0657(14) Uani 1 1 d . . . F20 F -0.0512(4) 0.1134(3) 0.4425(3) 0.0612(13) Uani 1 1 d . . . F21 F -0.1750(3) 0.1028(3) 0.5528(2) 0.0495(11) Uani 1 1 d . . . F22 F 0.3245(5) -0.0068(8) 0.4737(6) 0.212(6) Uani 1 1 d . . . F23 F 0.3374(6) -0.0411(6) 0.5846(6) 0.208(6) Uani 1 1 d . . . F24 F 0.3694(4) 0.0668(5) 0.5210(5) 0.151(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(3) 0.019(3) 0.032(4) -0.008(3) -0.002(3) -0.007(3) C2 0.031(4) 0.030(4) 0.036(5) -0.008(3) 0.002(3) -0.020(3) C3 0.024(3) 0.033(4) 0.034(4) -0.005(3) -0.004(3) -0.016(3) C4 0.016(3) 0.026(4) 0.051(5) -0.004(4) -0.013(3) -0.009(3) C5 0.029(4) 0.033(4) 0.027(4) -0.003(3) -0.011(3) -0.017(3) C6 0.039(4) 0.037(4) 0.025(4) -0.004(3) -0.004(3) -0.018(3) C7 0.030(4) 0.034(4) 0.051(5) 0.002(4) -0.020(4) -0.014(3) C8 0.022(3) 0.033(4) 0.044(5) -0.012(4) -0.008(3) -0.008(3) C9 0.018(3) 0.035(4) 0.039(5) -0.006(4) -0.004(3) -0.013(3) C10 0.055(5) 0.037(4) 0.036(5) -0.005(4) -0.011(4) -0.019(4) C11 0.128(9) 0.085(8) 0.052(7) -0.018(6) -0.046(6) -0.009(7) C12 0.020(3) 0.044(4) 0.036(5) -0.005(4) -0.002(3) -0.010(3) C13 0.053(5) 0.061(6) 0.042(5) -0.009(5) -0.014(4) -0.008(4) C14 0.032(4) 0.050(5) 0.050(6) -0.002(4) 0.005(4) -0.015(4) C15 0.027(3) 0.023(3) 0.028(4) -0.012(3) -0.003(3) -0.006(3) C16 0.030(4) 0.024(4) 0.039(5) -0.007(3) -0.005(3) -0.004(3) C17 0.034(4) 0.025(4) 0.040(5) 0.000(3) -0.007(3) 0.002(3) C18 0.014(3) 0.037(4) 0.063(6) -0.011(4) -0.010(3) 0.000(3) C19 0.023(4) 0.023(4) 0.056(5) -0.008(3) -0.011(3) -0.006(3) C20 0.033(4) 0.047(5) 0.072(6) -0.016(5) 0.009(4) -0.020(4) C21 0.039(4) 0.034(4) 0.048(5) -0.004(4) -0.001(4) -0.013(3) C22 0.040(4) 0.026(4) 0.060(6) -0.013(4) -0.030(4) -0.007(3) C23 0.026(4) 0.028(4) 0.045(5) -0.016(4) -0.003(3) -0.014(3) C24 0.030(4) 0.031(4) 0.072(6) -0.012(4) -0.012(4) -0.017(3) C25 0.038(4) 0.016(3) 0.074(6) -0.003(4) -0.026(4) -0.003(3) C26 0.023(3) 0.015(3) 0.058(5) -0.016(4) -0.006(3) -0.007(3) C27 0.040(4) 0.026(4) 0.057(6) -0.021(4) -0.012(4) -0.013(3) C28 0.045(4) 0.051(5) 0.054(6) -0.031(4) -0.003(4) -0.013(4) C29 0.051(5) 0.032(4) 0.062(6) -0.010(4) -0.019(4) -0.016(4) C30 0.076(6) 0.047(5) 0.076(7) -0.036(5) 0.034(5) -0.035(5) C31 0.030(4) 0.049(5) 0.088(7) -0.012(5) -0.018(4) -0.008(4) C40 0.029(4) 0.025(4) 0.046(5) -0.011(3) -0.013(4) -0.010(3) C41 0.019(3) 0.013(3) 0.036(4) -0.011(3) -0.007(3) -0.001(2) C42 0.020(3) 0.019(3) 0.032(4) -0.002(3) -0.005(3) -0.003(3) C43 0.021(3) 0.017(3) 0.033(4) 0.000(3) -0.007(3) -0.001(3) C44 0.020(3) 0.021(3) 0.031(4) -0.007(3) -0.007(3) 0.001(3) C45 0.016(3) 0.017(3) 0.034(4) 0.000(3) -0.006(3) -0.002(3) C46 0.019(3) 0.014(3) 0.048(5) -0.005(3) -0.008(3) -0.005(3) C47 0.024(4) 0.031(4) 0.050(5) -0.006(4) -0.004(4) -0.009(3) C48 0.050(5) 0.033(5) 0.064(6) 0.000(4) -0.033(5) -0.007(4) C49 0.041(4) 0.022(4) 0.040(5) -0.006(3) -0.021(4) -0.006(3) C50 0.025(3) 0.020(3) 0.042(5) -0.008(3) -0.012(3) -0.004(3) C51 0.027(3) 0.016(3) 0.036(4) -0.010(3) -0.014(3) -0.003(3) C52 0.022(3) 0.024(4) 0.040(5) -0.002(3) -0.011(3) 0.000(3) C53 0.030(4) 0.021(3) 0.033(4) 0.000(3) -0.006(3) -0.011(3) C54 0.042(4) 0.018(3) 0.035(5) 0.001(3) -0.016(3) -0.007(3) C56 0.047(6) 0.054(6) 0.151(11) -0.067(7) -0.033(7) 0.007(5) C57 0.027(4) 0.032(4) 0.048(5) -0.023(4) 0.002(4) -0.005(3) C58 0.025(4) 0.026(4) 0.053(5) -0.009(4) -0.013(4) -0.006(3) C59 0.027(3) 0.017(3) 0.029(4) -0.002(3) -0.008(3) -0.007(3) C60 0.023(3) 0.018(3) 0.038(5) 0.000(3) -0.005(3) -0.012(3) C61 0.036(4) 0.021(4) 0.038(5) -0.011(3) -0.007(3) -0.012(3) C62 0.046(4) 0.024(4) 0.044(5) -0.009(4) -0.011(4) -0.012(3) C63 0.051(5) 0.046(5) 0.029(5) -0.017(4) -0.013(4) -0.016(4) C64 0.029(4) 0.029(4) 0.039(5) -0.004(4) -0.010(4) -0.008(3) C65 0.024(3) 0.024(4) 0.024(4) 0.001(3) -0.011(3) -0.008(3) C66 0.029(3) 0.024(3) 0.026(4) -0.007(3) -0.009(3) -0.010(3) C67 0.025(3) 0.020(3) 0.021(4) 0.003(3) -0.008(3) -0.014(3) C68 0.030(4) 0.025(4) 0.028(4) 0.001(3) -0.014(3) -0.008(3) C69 0.030(4) 0.023(4) 0.026(4) -0.006(3) -0.006(3) -0.011(3) C70 0.023(3) 0.024(4) 0.039(5) -0.002(3) -0.014(3) -0.009(3) C71 0.041(4) 0.042(5) 0.036(5) -0.001(4) -0.017(4) -0.006(4) C85 0.034(4) 0.030(4) 0.054(6) 0.003(4) -0.013(4) -0.012(3) C901 0.079(7) 0.046(6) 0.074(8) -0.019(5) -0.024(6) 0.007(5) C902 0.051(5) 0.031(5) 0.089(8) -0.012(5) -0.038(5) -0.008(4) C903 0.046(5) 0.038(5) 0.072(7) 0.005(5) -0.015(5) -0.003(4) C904 0.056(6) 0.046(5) 0.083(8) -0.009(5) -0.037(6) 0.005(4) C905 0.034(5) 0.039(5) 0.127(10) -0.034(6) -0.032(6) 0.013(4) C906 0.047(5) 0.029(5) 0.073(7) -0.015(5) 0.005(5) -0.001(4) C907 0.061(6) 0.059(6) 0.258(16) -0.059(8) -0.101(8) 0.011(5) N1 0.021(3) 0.018(3) 0.032(3) -0.002(2) -0.004(2) -0.009(2) N2 0.025(3) 0.017(3) 0.025(3) -0.005(2) -0.005(2) -0.006(2) N3 0.023(3) 0.028(3) 0.039(4) -0.008(3) -0.008(3) -0.007(2) Si1 0.0238(10) 0.0299(11) 0.0608(16) -0.0097(11) -0.0054(10) -0.0072(8) B1 0.018(4) 0.024(4) 0.030(5) -0.006(4) -0.005(3) -0.004(3) Rh1 0.0214(3) 0.0187(3) 0.0453(4) -0.0088(3) -0.0084(2) -0.0050(2) F1 0.054(3) 0.073(3) 0.052(3) 0.008(2) -0.006(2) -0.047(2) F2 0.093(4) 0.082(4) 0.052(3) -0.033(3) 0.037(3) -0.058(3) F3 0.046(3) 0.074(4) 0.067(4) 0.040(3) -0.010(2) -0.011(2) F4 0.039(2) 0.078(3) 0.051(3) -0.024(3) -0.023(2) -0.002(2) F5 0.048(2) 0.039(2) 0.034(3) -0.0016(19) -0.006(2) -0.0274(19) F6 0.075(3) 0.032(2) 0.040(3) -0.013(2) -0.006(2) -0.027(2) F7 0.058(4) 0.137(6) 0.241(10) 0.116(6) -0.070(5) -0.016(4) F8 0.130(5) 0.176(7) 0.120(6) -0.097(6) -0.101(5) 0.103(5) F9 0.128(5) 0.061(4) 0.239(8) -0.074(5) -0.148(6) 0.050(3) F10 0.078(3) 0.054(3) 0.037(3) -0.008(2) 0.010(2) -0.036(2) F11 0.050(2) 0.037(2) 0.055(3) 0.000(2) -0.009(2) -0.030(2) F12 0.031(2) 0.043(3) 0.095(4) 0.012(3) -0.010(2) -0.016(2) F13 0.043(2) 0.058(3) 0.027(3) -0.004(2) -0.010(2) -0.007(2) F14 0.026(2) 0.115(4) 0.044(3) -0.009(3) -0.003(2) -0.023(2) F15 0.105(4) 0.035(3) 0.052(3) -0.017(2) 0.008(3) -0.004(3) F16 0.071(3) 0.058(3) 0.055(3) 0.011(2) -0.044(3) -0.035(2) F17 0.038(2) 0.036(2) 0.036(3) 0.0056(19) -0.0073(19) -0.0110(18) F18 0.052(2) 0.025(2) 0.046(3) 0.002(2) -0.014(2) 0.0051(18) F19 0.088(3) 0.033(3) 0.092(4) 0.000(3) -0.064(3) -0.007(2) F20 0.061(3) 0.092(4) 0.042(3) -0.023(3) -0.012(2) -0.029(3) F21 0.049(2) 0.066(3) 0.045(3) -0.004(2) -0.018(2) -0.031(2) F22 0.044(4) 0.383(14) 0.294(12) -0.306(13) -0.033(5) 0.034(5) F23 0.086(5) 0.138(7) 0.214(10) 0.024(7) 0.036(5) 0.063(5) F24 0.034(3) 0.170(7) 0.276(10) -0.152(8) 0.014(4) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(7) . ? C1 N2 1.372(7) . ? C1 Rh1 2.028(6) . ? C2 C3 1.333(8) . ? C2 N2 1.391(7) . ? C3 N1 1.391(7) . ? C4 C9 1.390(9) . ? C4 C5 1.401(9) . ? C4 N1 1.455(7) . ? C5 C6 1.400(9) . ? C5 C10 1.492(9) . ? C6 C7 1.368(9) . ? C7 C8 1.390(9) . ? C8 C9 1.408(9) . ? C9 C12 1.501(9) . ? C10 C30 1.513(10) . ? C10 C11 1.532(10) . ? C12 C14 1.524(9) . ? C12 C13 1.524(10) . ? C15 N3 1.349(7) . ? C15 C16 1.376(8) . ? C15 N2 1.408(7) . ? C16 C17 1.378(8) . ? C17 C18 1.385(9) . ? C18 C19 1.384(9) . ? C19 N3 1.381(7) . ? C19 Si1 1.923(7) . ? C20 Si1 1.861(8) . ? C21 Si1 1.868(7) . ? C22 C23 1.373(9) . ? C22 C29 1.489(10) . ? C22 Rh1 2.214(6) . ? C23 C24 1.506(9) . ? C23 Rh1 2.254(5) . ? C24 C25 1.535(8) . ? C25 C26 1.499(8) . ? C26 C27 1.366(9) . ? C26 Rh1 2.128(6) . ? C27 C28 1.528(9) . ? C27 Rh1 2.142(7) . ? C28 C29 1.538(9) . ? C31 Si1 1.885(8) . ? C40 F5 1.333(7) . ? C40 F4 1.338(7) . ? C40 F6 1.340(7) . ? C40 C41 1.481(9) . ? C41 C42 1.388(8) . ? C41 C46 1.388(8) . ? C42 C43 1.406(9) . ? C43 C44 1.400(8) . ? C43 B1 1.633(9) . ? C44 C45 1.412(8) . ? C45 C46 1.384(9) . ? C45 C47 1.484(9) . ? C47 F3 1.312(7) . ? C47 F2 1.328(8) . ? C47 F1 1.332(7) . ? C48 F9 1.253(8) . ? C48 F8 1.259(9) . ? C48 F7 1.300(9) . ? C48 C49 1.484(9) . ? C49 C50 1.385(9) . ? C49 C54 1.387(9) . ? C50 C51 1.406(8) . ? C51 C52 1.403(8) . ? C51 B1 1.645(9) . ? C52 C53 1.402(8) . ? C53 C54 1.373(8) . ? C53 C85 1.492(9) . ? C56 F22 1.223(11) . ? C56 F24 1.233(9) . ? C56 F23 1.357(13) . ? C56 C57 1.486(10) . ? C57 C62 1.375(9) . ? C57 C58 1.390(9) . ? C58 C59 1.394(8) . ? C59 C60 1.435(8) . ? C59 B1 1.639(10) . ? C60 C61 1.381(9) . ? C61 C62 1.372(9) . ? C61 C63 1.505(9) . ? C63 F21 1.327(8) . ? C63 F20 1.334(8) . ? C63 F19 1.343(8) . ? C64 F16 1.332(7) . ? C64 F18 1.340(7) . ? C64 F17 1.345(7) . ? C64 C65 1.476(9) . ? C65 C70 1.387(9) . ? C65 C66 1.391(8) . ? C66 C67 1.392(8) . ? C67 C68 1.401(8) . ? C67 B1 1.646(9) . ? C68 C69 1.392(8) . ? C69 C70 1.399(8) . ? C69 C71 1.498(9) . ? C71 F15 1.322(8) . ? C71 F13 1.335(7) . ? C71 F14 1.342(7) . ? C85 F12 1.333(7) . ? C85 F10 1.340(8) . ? C85 F11 1.355(8) . ? C901 C906 1.363(12) . ? C901 C902 1.405(12) . ? C902 C903 1.314(11) . ? C903 C904 1.410(11) . ? C904 C905 1.354(12) . ? C905 C906 1.377(12) . ? C905 C907 1.515(11) . ? N3 Rh1 2.156(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 N1 C1 N2 105.1(5) . . ? N1 C1 Rh1 144.2(4) . . ? N2 C1 Rh1 110.2(4) . . ? C3 C2 N2 106.0(5) . . ? C2 C3 N1 108.2(5) . . ? C9 C4 C5 124.6(6) . . ? C9 C4 N1 119.4(6) . . ? C5 C4 N1 116.0(6) . . ? C6 C5 C4 116.1(6) . . ? C6 C5 C10 119.9(6) . . ? C4 C5 C10 123.9(6) . . ? C7 C6 C5 121.6(6) . . ? C6 C7 C8 120.5(6) . . ? C7 C8 C9 121.0(7) . . ? C4 C9 C8 116.0(6) . . ? C4 C9 C12 123.1(6) . . ? C8 C9 C12 120.9(6) . . ? C5 C10 C30 111.4(6) . . ? C5 C10 C11 114.3(7) . . ? C30 C10 C11 108.8(7) . . ? C9 C12 C14 110.6(5) . . ? C9 C12 C13 113.4(6) . . ? C14 C12 C13 110.0(6) . . ? N3 C15 C16 125.6(6) . . ? N3 C15 N2 113.6(5) . . ? C16 C15 N2 120.8(5) . . ? C15 C16 C17 117.4(6) . . ? C16 C17 C18 118.3(6) . . ? C19 C18 C17 121.9(6) . . ? N3 C19 C18 119.6(6) . . ? N3 C19 Si1 122.6(5) . . ? C18 C19 Si1 116.5(5) . . ? C23 C22 C29 125.8(6) . . ? C23 C22 Rh1 73.7(4) . . ? C29 C22 Rh1 106.8(4) . . ? C22 C23 C24 125.2(7) . . ? C22 C23 Rh1 70.5(3) . . ? C24 C23 Rh1 110.5(4) . . ? C23 C24 C25 112.1(5) . . ? C26 C25 C24 112.8(6) . . ? C27 C26 C25 126.8(6) . . ? C27 C26 Rh1 71.9(4) . . ? C25 C26 Rh1 109.7(4) . . ? C26 C27 C28 126.7(6) . . ? C26 C27 Rh1 70.8(4) . . ? C28 C27 Rh1 113.1(4) . . ? C27 C28 C29 111.9(6) . . ? C22 C29 C28 114.6(6) . . ? F5 C40 F4 105.9(5) . . ? F5 C40 F6 106.1(5) . . ? F4 C40 F6 105.6(5) . . ? F5 C40 C41 113.2(5) . . ? F4 C40 C41 113.4(5) . . ? F6 C40 C41 111.9(5) . . ? C42 C41 C46 119.8(6) . . ? C42 C41 C40 121.5(6) . . ? C46 C41 C40 118.6(5) . . ? C41 C42 C43 122.7(6) . . ? C44 C43 C42 115.9(5) . . ? C44 C43 B1 121.4(6) . . ? C42 C43 B1 122.3(6) . . ? C43 C44 C45 122.2(6) . . ? C46 C45 C44 119.5(6) . . ? C46 C45 C47 121.9(6) . . ? C44 C45 C47 118.5(6) . . ? C45 C46 C41 119.9(5) . . ? F3 C47 F2 106.4(7) . . ? F3 C47 F1 105.9(6) . . ? F2 C47 F1 105.6(5) . . ? F3 C47 C45 112.8(5) . . ? F2 C47 C45 111.9(5) . . ? F1 C47 C45 113.6(6) . . ? F9 C48 F8 107.6(8) . . ? F9 C48 F7 102.2(8) . . ? F8 C48 F7 100.1(8) . . ? F9 C48 C49 115.9(6) . . ? F8 C48 C49 114.9(7) . . ? F7 C48 C49 114.2(7) . . ? C50 C49 C54 120.0(6) . . ? C50 C49 C48 121.5(6) . . ? C54 C49 C48 118.6(6) . . ? C49 C50 C51 124.0(6) . . ? C52 C51 C50 113.8(6) . . ? C52 C51 B1 123.4(5) . . ? C50 C51 B1 122.5(5) . . ? C53 C52 C51 123.2(5) . . ? C54 C53 C52 120.3(6) . . ? C54 C53 C85 118.8(6) . . ? C52 C53 C85 120.9(5) . . ? C53 C54 C49 118.8(6) . . ? F22 C56 F24 112.0(11) . . ? F22 C56 F23 102.6(9) . . ? F24 C56 F23 95.6(9) . . ? F22 C56 C57 117.0(8) . . ? F24 C56 C57 116.6(7) . . ? F23 C56 C57 109.8(10) . . ? C62 C57 C58 119.9(6) . . ? C62 C57 C56 119.5(7) . . ? C58 C57 C56 120.4(7) . . ? C57 C58 C59 124.1(6) . . ? C58 C59 C60 114.1(6) . . ? C58 C59 B1 122.0(6) . . ? C60 C59 B1 123.8(5) . . ? C61 C60 C59 121.1(6) . . ? C62 C61 C60 122.3(6) . . ? C62 C61 C63 121.0(6) . . ? C60 C61 C63 116.6(6) . . ? C61 C62 C57 118.3(7) . . ? F21 C63 F20 106.3(5) . . ? F21 C63 F19 106.1(6) . . ? F20 C63 F19 106.4(6) . . ? F21 C63 C61 113.4(6) . . ? F20 C63 C61 112.9(6) . . ? F19 C63 C61 111.2(5) . . ? F16 C64 F18 106.3(5) . . ? F16 C64 F17 106.2(6) . . ? F18 C64 F17 105.2(5) . . ? F16 C64 C65 113.4(5) . . ? F18 C64 C65 113.1(6) . . ? F17 C64 C65 112.0(5) . . ? C70 C65 C66 119.5(6) . . ? C70 C65 C64 120.2(5) . . ? C66 C65 C64 120.3(6) . . ? C65 C66 C67 123.7(6) . . ? C66 C67 C68 115.4(6) . . ? C66 C67 B1 120.4(6) . . ? C68 C67 B1 123.9(5) . . ? C69 C68 C67 122.5(6) . . ? C68 C69 C70 120.0(6) . . ? C68 C69 C71 122.3(6) . . ? C70 C69 C71 117.7(6) . . ? C65 C70 C69 118.9(6) . . ? F15 C71 F13 107.4(6) . . ? F15 C71 F14 107.2(6) . . ? F13 C71 F14 105.3(6) . . ? F15 C71 C69 112.3(6) . . ? F13 C71 C69 112.7(6) . . ? F14 C71 C69 111.5(6) . . ? F12 C85 F10 106.4(6) . . ? F12 C85 F11 106.1(6) . . ? F10 C85 F11 105.7(5) . . ? F12 C85 C53 114.2(6) . . ? F10 C85 C53 111.8(6) . . ? F11 C85 C53 112.1(6) . . ? C906 C901 C902 118.2(9) . . ? C903 C902 C901 119.5(8) . . ? C902 C903 C904 122.9(8) . . ? C905 C904 C903 117.5(9) . . ? C904 C905 C906 120.2(8) . . ? C904 C905 C907 119.1(11) . . ? C906 C905 C907 120.7(11) . . ? C901 C906 C905 121.6(9) . . ? C1 N1 C3 110.3(5) . . ? C1 N1 C4 125.1(5) . . ? C3 N1 C4 124.6(5) . . ? C1 N2 C2 110.5(5) . . ? C1 N2 C15 119.9(5) . . ? C2 N2 C15 129.1(5) . . ? C15 N3 C19 116.2(5) . . ? C15 N3 Rh1 108.1(4) . . ? C19 N3 Rh1 132.4(4) . . ? C20 Si1 C21 107.4(4) . . ? C20 Si1 C31 107.6(3) . . ? C21 Si1 C31 115.5(3) . . ? C20 Si1 C19 104.8(3) . . ? C21 Si1 C19 109.6(3) . . ? C31 Si1 C19 111.3(4) . . ? C43 B1 C59 111.8(5) . . ? C43 B1 C51 111.2(5) . . ? C59 B1 C51 104.1(5) . . ? C43 B1 C67 103.9(5) . . ? C59 B1 C67 113.3(5) . . ? C51 B1 C67 112.8(5) . . ? C1 Rh1 C26 98.5(2) . . ? C1 Rh1 C27 94.4(2) . . ? C26 Rh1 C27 37.3(2) . . ? C1 Rh1 N3 78.4(2) . . ? C26 Rh1 N3 167.6(3) . . ? C27 Rh1 N3 154.1(3) . . ? C1 Rh1 C22 148.5(3) . . ? C26 Rh1 C22 96.6(3) . . ? C27 Rh1 C22 81.3(3) . . ? N3 Rh1 C22 91.9(2) . . ? C1 Rh1 C23 175.6(3) . . ? C26 Rh1 C23 80.4(2) . . ? C27 Rh1 C23 87.3(2) . . ? N3 Rh1 C23 101.7(2) . . ? C22 Rh1 C23 35.8(2) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.031 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.114 #==END data_compound3 _database_code_CSD 183893 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02sw047 _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Cl Ir N3 Si' _chemical_formula_sum 'C31 H42 Cl Ir N3 Si' _chemical_formula_weight 712.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 8.1132(16) _cell_length_b 14.308(3) _cell_length_c 25.784(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.99 _cell_angle_gamma 90.00 _cell_volume 2985.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34375 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.68 _exptl_crystal_description Needle _exptl_crystal_colour Green _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 4.626 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8737 _exptl_absorpt_correction_T_max 0.9552 _exptl_absorpt_process_details 'Sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius Fr591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10106 _diffrn_reflns_av_R_equivalents 0.1444 _diffrn_reflns_av_sigmaI/netI 0.2539 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.77 _reflns_number_total 4213 _reflns_number_gt 2053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^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 4213 _refine_ls_number_parameters 341 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1941 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2595(18) 0.8356(15) 0.0818(6) 0.029(4) Uani 1 1 d U . . C2 C 0.4610(17) 0.9024(14) 0.0377(6) 0.024(5) Uani 1 1 d . . . H2 H 0.5415 0.9108 0.0131 0.029 Uiso 1 1 calc R . . C3 C 0.4299(17) 0.9579(14) 0.0772(6) 0.026(5) Uani 1 1 d . . . H3 H 0.4877 1.0139 0.0864 0.032 Uiso 1 1 calc R . . C4 C 0.2289(18) 0.9672(14) 0.1455(5) 0.029(4) Uani 1 1 d U . . C5 C 0.0942(19) 1.0243(15) 0.1338(6) 0.032(4) Uani 1 1 d U . . C6 C 0.0321(19) 1.0705(15) 0.1746(6) 0.041(6) Uani 1 1 d . . . H6 H -0.0563 1.1135 0.1685 0.049 Uiso 1 1 calc R . . C7 C 0.0990(18) 1.0544(14) 0.2252(6) 0.033(6) Uani 1 1 d . . . H7 H 0.0510 1.0852 0.2531 0.040 Uiso 1 1 calc R . . C8 C 0.2309(19) 0.9960(14) 0.2363(6) 0.030(4) Uani 1 1 d U . . H8 H 0.2787 0.9905 0.2709 0.036 Uiso 1 1 calc R . . C9 C 0.2931(18) 0.9452(14) 0.1961(6) 0.030(4) Uani 1 1 d U . . C10 C 0.4443(18) 0.8837(14) 0.2066(5) 0.032(6) Uani 1 1 d . . . H10 H 0.4469 0.8392 0.1768 0.038 Uiso 1 1 calc R . . C11 C 0.6037(18) 0.9410(14) 0.2076(6) 0.038(6) Uani 1 1 d . . . H11A H 0.6143 0.9693 0.1734 0.057 Uiso 1 1 calc R . . H11B H 0.6986 0.9001 0.2162 0.057 Uiso 1 1 calc R . . H11C H 0.6002 0.9904 0.2339 0.057 Uiso 1 1 calc R . . C12 C 0.4378(19) 0.8238(14) 0.2568(5) 0.036(5) Uani 1 1 d . . . H12A H 0.5398 0.7873 0.2622 0.053 Uiso 1 1 calc R . . H12B H 0.3430 0.7813 0.2532 0.053 Uiso 1 1 calc R . . H12C H 0.4264 0.8650 0.2867 0.053 Uiso 1 1 calc R . . C13 C 0.0276(18) 1.0440(14) 0.0789(6) 0.031(6) Uani 1 1 d . . . H13 H 0.0696 0.9930 0.0568 0.037 Uiso 1 1 calc R . . C14 C 0.090(2) 1.1336(17) 0.0580(7) 0.065(8) Uani 1 1 d . . . H14A H 0.0530 1.1394 0.0212 0.097 Uiso 1 1 calc R . . H14B H 0.2110 1.1341 0.0619 0.097 Uiso 1 1 calc R . . H14C H 0.0469 1.1861 0.0774 0.097 Uiso 1 1 calc R . . C15 C -0.157(2) 1.0386(15) 0.0732(6) 0.044(6) Uani 1 1 d . . . H15A H -0.2038 1.0918 0.0910 0.066 Uiso 1 1 calc R . . H15B H -0.1933 0.9802 0.0886 0.066 Uiso 1 1 calc R . . H15C H -0.1940 1.0402 0.0362 0.066 Uiso 1 1 calc R . . C16 C 0.3325(17) 0.7496(14) 0.0074(6) 0.027(6) Uani 1 1 d . . . C17 C 0.2098(18) 0.6917(15) 0.0234(6) 0.029(4) Uani 1 1 d U . . C18 C 0.3964(18) 0.6721(17) -0.0650(6) 0.037(6) Uani 1 1 d . . . C19 C 0.2836(19) 0.6051(16) -0.0533(6) 0.049(7) Uani 1 1 d . . . H19 H 0.2668 0.5525 -0.0755 0.059 Uiso 1 1 calc R . . C20 C 0.193(2) 0.6130(16) -0.0096(6) 0.044(7) Uani 1 1 d . . . H20 H 0.1195 0.5644 -0.0017 0.053 Uiso 1 1 calc R . . C21 C 0.7307(19) 0.6221(16) -0.1015(6) 0.053(7) Uani 1 1 d . . . H21A H 0.7196 0.5565 -0.0913 0.079 Uiso 1 1 calc R . . H21B H 0.7769 0.6584 -0.0717 0.079 Uiso 1 1 calc R . . H21C H 0.8045 0.6264 -0.1299 0.079 Uiso 1 1 calc R . . C22 C 0.4246(19) 0.5901(15) -0.1719(6) 0.044(6) Uani 1 1 d . . . H22A H 0.3045 0.5980 -0.1726 0.066 Uiso 1 1 calc R . . H22B H 0.4534 0.5253 -0.1628 0.066 Uiso 1 1 calc R . . H22C H 0.4623 0.6046 -0.2063 0.066 Uiso 1 1 calc R . . C23 C 0.5348(18) 0.7883(14) -0.1510(6) 0.039(6) Uani 1 1 d . . . H23A H 0.5873 0.7857 -0.1841 0.058 Uiso 1 1 calc R . . H23B H 0.5995 0.8288 -0.1266 0.058 Uiso 1 1 calc R . . H23C H 0.4226 0.8134 -0.1569 0.058 Uiso 1 1 calc R . . C30 C -0.118(2) 0.6427(15) 0.0649(6) 0.041(6) Uani 1 1 d . . . H30 H -0.0779 0.6428 0.0312 0.050 Uiso 1 1 calc R . . C31 C -0.0348(19) 0.5967(15) 0.1020(6) 0.036(6) Uani 1 1 d . . . H31 H 0.0656 0.5690 0.0928 0.043 Uiso 1 1 calc R . . C32 C -0.0776(19) 0.5820(15) 0.1570(6) 0.042(6) Uani 1 1 d . . . H32A H -0.0301 0.5218 0.1697 0.051 Uiso 1 1 calc R . . H32B H -0.1992 0.5778 0.1578 0.051 Uiso 1 1 calc R . . C33 C -0.011(2) 0.6635(16) 0.1951(6) 0.042(7) Uani 1 1 d . . . H33A H -0.0938 0.6752 0.2209 0.051 Uiso 1 1 calc R . . H33B H 0.0920 0.6424 0.2143 0.051 Uiso 1 1 calc R . . C34 C 0.020(2) 0.7499(14) 0.1687(6) 0.036(7) Uani 1 1 d . . . H34 H 0.1275 0.7767 0.1740 0.043 Uiso 1 1 calc R . . C35 C -0.0990(18) 0.7978(14) 0.1351(5) 0.035(6) Uani 1 1 d . . . H35 H -0.0703 0.8561 0.1205 0.042 Uiso 1 1 calc R . . C36 C -0.2673(19) 0.7590(15) 0.1222(6) 0.042(6) Uani 1 1 d . . . H36A H -0.3465 0.8112 0.1163 0.050 Uiso 1 1 calc R . . H36B H -0.3015 0.7222 0.1521 0.050 Uiso 1 1 calc R . . C37 C -0.275(2) 0.6957(15) 0.0732(6) 0.047(6) Uani 1 1 d . . . H37A H -0.3657 0.6501 0.0758 0.056 Uiso 1 1 calc R . . H37B H -0.3024 0.7351 0.0423 0.056 Uiso 1 1 calc R . . N1 N 0.2993(15) 0.9211(12) 0.1030(5) 0.033(5) Uani 1 1 d . . . N2 N 0.3536(15) 0.8324(14) 0.0404(5) 0.040(5) Uani 1 1 d . . . N3 N 0.4234(14) 0.7480(12) -0.0331(5) 0.030(3) Uani 1 1 d U . . Si1 Si 0.5251(6) 0.6693(5) -0.12337(17) 0.0374(17) Uani 1 1 d . . . Cl1 Cl 0.3347(5) 0.6483(4) 0.13750(15) 0.0397(15) Uani 1 1 d . . . Ir1 Ir 0.09932(8) 0.72891(6) 0.08819(2) 0.0319(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(4) 0.029(4) 0.029(4) 0.0001(10) 0.0023(11) -0.0001(10) C2 0.011(9) 0.016(18) 0.044(12) 0.004(9) -0.005(7) -0.004(9) C3 0.016(9) 0.013(18) 0.050(12) 0.012(9) 0.005(7) -0.007(9) C4 0.029(4) 0.029(4) 0.029(4) 0.0001(10) 0.0022(11) -0.0003(10) C5 0.032(4) 0.032(5) 0.032(4) 0.0001(10) 0.0023(11) -0.0003(10) C6 0.027(10) 0.06(2) 0.036(12) -0.005(10) 0.009(8) -0.005(10) C7 0.026(10) 0.04(2) 0.037(11) 0.004(9) 0.011(7) -0.017(10) C8 0.030(4) 0.030(4) 0.030(4) -0.0003(10) 0.0022(11) 0.0000(10) C9 0.031(4) 0.030(4) 0.031(4) 0.0000(10) 0.0023(11) -0.0003(10) C10 0.039(11) 0.035(19) 0.021(10) 0.004(9) -0.002(7) 0.001(10) C11 0.038(11) 0.04(2) 0.035(11) 0.005(9) -0.001(7) 0.002(10) C12 0.055(12) 0.010(18) 0.039(11) 0.003(9) -0.018(8) 0.007(11) C13 0.030(10) 0.021(19) 0.043(11) 0.004(9) 0.010(7) 0.023(10) C14 0.070(15) 0.08(3) 0.047(13) 0.022(13) -0.007(10) -0.021(15) C15 0.058(14) 0.03(2) 0.048(12) 0.005(10) 0.001(8) -0.008(12) C16 0.020(9) 0.02(2) 0.046(11) 0.006(9) 0.016(7) 0.016(9) C17 0.028(4) 0.029(4) 0.029(4) 0.0002(10) 0.0021(11) -0.0004(10) C18 0.014(9) 0.06(2) 0.034(10) -0.008(10) -0.003(7) 0.004(10) C19 0.033(11) 0.07(2) 0.043(12) -0.030(11) 0.010(8) -0.021(12) C20 0.041(11) 0.05(2) 0.042(12) -0.007(10) 0.005(8) -0.017(11) C21 0.042(12) 0.05(2) 0.073(14) -0.006(12) 0.017(9) 0.006(11) C22 0.045(11) 0.04(2) 0.049(12) -0.016(10) 0.019(8) -0.016(11) C23 0.035(10) 0.03(2) 0.050(11) -0.006(10) 0.004(7) -0.008(10) C30 0.069(14) 0.04(2) 0.021(11) -0.010(10) 0.019(9) -0.032(12) C31 0.028(10) 0.06(2) 0.023(11) 0.000(10) 0.007(7) -0.020(10) C32 0.032(11) 0.04(2) 0.060(13) -0.005(11) 0.012(8) 0.009(11) C33 0.050(12) 0.06(2) 0.021(11) -0.013(10) 0.010(7) 0.001(12) C34 0.051(11) 0.02(2) 0.042(11) 0.017(9) 0.014(8) -0.009(10) C35 0.041(11) 0.03(2) 0.037(11) 0.014(9) 0.010(8) -0.005(10) C36 0.044(11) 0.05(2) 0.032(11) -0.007(10) -0.004(7) -0.004(11) C37 0.053(12) 0.04(2) 0.051(12) 0.006(11) 0.022(9) 0.012(12) N1 0.033(9) 0.028(16) 0.037(9) -0.010(8) -0.002(6) 0.015(8) N2 0.027(9) 0.06(2) 0.036(10) 0.000(9) 0.004(6) -0.008(9) N3 0.030(4) 0.030(4) 0.030(4) -0.0001(10) 0.0025(10) 0.0002(10) Si1 0.038(3) 0.038(6) 0.037(3) -0.005(3) 0.011(2) -0.001(3) Cl1 0.033(3) 0.039(5) 0.048(3) 0.007(2) 0.0034(18) 0.000(2) Ir1 0.0324(4) 0.0302(7) 0.0335(4) 0.0004(4) 0.0050(2) -0.0015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.355(17) . ? C1 N1 1.37(2) . ? C1 Ir1 2.019(19) . ? C2 C3 1.33(2) . ? C2 N2 1.33(2) . ? C3 N1 1.393(19) . ? C4 C5 1.38(2) . ? C4 C9 1.41(2) . ? C4 N1 1.432(19) . ? C5 C6 1.37(2) . ? C5 C13 1.51(2) . ? C6 C7 1.40(2) . ? C7 C8 1.37(2) . ? C8 C9 1.39(2) . ? C9 C10 1.52(2) . ? C10 C11 1.53(2) . ? C10 C12 1.56(2) . ? C13 C14 1.49(3) . ? C13 C15 1.49(2) . ? C16 N3 1.318(17) . ? C16 C17 1.38(2) . ? C16 N2 1.46(2) . ? C17 C20 1.41(3) . ? C17 Ir1 2.022(15) . ? C18 C19 1.37(3) . ? C18 N3 1.37(2) . ? C18 Si1 1.890(15) . ? C19 C20 1.39(2) . ? C21 Si1 1.852(17) . ? C22 Si1 1.837(16) . ? C23 Si1 1.850(19) . ? C30 C31 1.31(2) . ? C30 C37 1.51(2) . ? C30 Ir1 2.201(17) . ? C31 C32 1.50(2) . ? C31 Ir1 2.223(18) . ? C32 C33 1.59(2) . ? C33 C34 1.44(2) . ? C34 C35 1.43(2) . ? C34 Ir1 2.234(16) . ? C35 C36 1.49(2) . ? C35 Ir1 2.301(16) . ? C36 C37 1.55(2) . ? Cl1 Ir1 2.501(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 N2 C1 N1 102.4(16) . . ? N2 C1 Ir1 116.1(15) . . ? N1 C1 Ir1 141.1(12) . . ? C3 C2 N2 104.4(14) . . ? C2 C3 N1 109.4(17) . . ? C5 C4 C9 124.9(14) . . ? C5 C4 N1 117.2(13) . . ? C9 C4 N1 117.7(16) . . ? C6 C5 C4 116.5(14) . . ? C6 C5 C13 120.3(17) . . ? C4 C5 C13 122.9(14) . . ? C5 C6 C7 119.9(18) . . ? C8 C7 C6 122.9(16) . . ? C7 C8 C9 118.7(14) . . ? C8 C9 C4 116.4(17) . . ? C8 C9 C10 120.0(13) . . ? C4 C9 C10 122.6(14) . . ? C9 C10 C11 111.3(16) . . ? C9 C10 C12 113.2(12) . . ? C11 C10 C12 111.0(12) . . ? C14 C13 C15 111.8(16) . . ? C14 C13 C5 113.0(16) . . ? C15 C13 C5 112.0(12) . . ? N3 C16 C17 132.9(18) . . ? N3 C16 N2 115.2(16) . . ? C17 C16 N2 111.7(13) . . ? C16 C17 C20 109.8(14) . . ? C16 C17 Ir1 117.4(14) . . ? C20 C17 Ir1 132.8(14) . . ? C19 C18 N3 120.1(14) . . ? C19 C18 Si1 125.0(15) . . ? N3 C18 Si1 114.9(14) . . ? C18 C19 C20 121.2(19) . . ? C19 C20 C17 121.3(19) . . ? C31 C30 C37 123.2(15) . . ? C31 C30 Ir1 73.7(11) . . ? C37 C30 Ir1 110.3(14) . . ? C30 C31 C32 128.3(17) . . ? C30 C31 Ir1 71.9(12) . . ? C32 C31 Ir1 114.7(12) . . ? C31 C32 C33 113.1(16) . . ? C34 C33 C32 113.5(14) . . ? C35 C34 C33 124.1(16) . . ? C35 C34 Ir1 74.2(9) . . ? C33 C34 Ir1 113.3(14) . . ? C34 C35 C36 121.9(17) . . ? C34 C35 Ir1 69.1(9) . . ? C36 C35 Ir1 112.8(12) . . ? C35 C36 C37 112.5(13) . . ? C30 C37 C36 115.0(14) . . ? C1 N1 C3 108.2(13) . . ? C1 N1 C4 128.5(15) . . ? C3 N1 C4 123.3(16) . . ? C2 N2 C1 115.0(17) . . ? C2 N2 C16 129.0(14) . . ? C1 N2 C16 115.9(17) . . ? C16 N3 C18 114.5(16) . . ? C22 Si1 C23 109.5(8) . . ? C22 Si1 C21 109.3(9) . . ? C23 Si1 C21 113.1(9) . . ? C22 Si1 C18 108.2(8) . . ? C23 Si1 C18 109.1(9) . . ? C21 Si1 C18 107.5(7) . . ? C1 Ir1 C17 78.8(7) . . ? C1 Ir1 C30 155.4(7) . . ? C17 Ir1 C30 91.2(6) . . ? C1 Ir1 C31 168.9(7) . . ? C17 Ir1 C31 99.1(7) . . ? C30 Ir1 C31 34.4(6) . . ? C1 Ir1 C34 101.6(7) . . ? C17 Ir1 C34 167.3(7) . . ? C30 Ir1 C34 93.0(6) . . ? C31 Ir1 C34 77.9(6) . . ? C1 Ir1 C35 101.3(7) . . ? C17 Ir1 C35 156.0(6) . . ? C30 Ir1 C35 78.9(7) . . ? C31 Ir1 C35 85.0(7) . . ? C34 Ir1 C35 36.7(6) . . ? C1 Ir1 Cl1 85.3(5) . . ? C17 Ir1 Cl1 86.1(5) . . ? C30 Ir1 Cl1 116.7(6) . . ? C31 Ir1 Cl1 83.7(5) . . ? C34 Ir1 Cl1 81.2(5) . . ? C35 Ir1 Cl1 117.9(4) . . ? _diffrn_measured_fraction_theta_max 0.737 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.737 _refine_diff_density_max 1.760 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.214 #==END