# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chem. Commun.' _publ_contact_author_name 'Andrew S.Weller' _publ_contact_author_address ;Department of Chemistry University of Bath Bath, BA2 7AY United Kingdom ; _publ_contact_author_email a.s.weller@bath.ac.uk _publ_contact_author_phone '44 1225 38 3394' _publ_contact_author_fax '44 1225 82 6231' loop_ _publ_author_name _publ_author_address 'Eduardo Molinos' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Gabriele Kociok-Kohn' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Andrew S. Weller' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_section_title ; Polyethyl Substituted Weakly Coordinating Carborane Anions: A Sequential Dehydrogenative Borylation/Hydrogenation Route ; data_k04asw21 _database_code_depnum_ccdc_archive 'CCDC 268853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5' _chemical_melting_point ? _chemical_formula_moiety 'C44 H56 B11 P2 Rh' _chemical_formula_sum 'C44 H56 B11 P2 Rh' _chemical_formula_weight 868.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.8660(2) _cell_length_b 13.3420(4) _cell_length_c 17.7310(6) _cell_angle_alpha 83.5920(10) _cell_angle_beta 75.7420(10) _cell_angle_gamma 78.438(2) _cell_volume 2211.41(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31370 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26014 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.57 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9894 _reflns_number_gt 7320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SHELXS97-2 Program for Crystal Structure Solution. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _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^)+(0.0104P)^2^+2.2819P] 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 9894 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 Rh Rh 0.80874(3) 0.766559(19) 0.750856(16) 0.02566(8) Uani 1 1 d . . . P1 P 0.87815(8) 0.64203(6) 0.83677(5) 0.02462(18) Uani 1 1 d . . . P2 P 0.85443(9) 0.66698(6) 0.65255(5) 0.02763(19) Uani 1 1 d . . . C11 C 1.0128(3) 0.6889(2) 0.8707(2) 0.0297(7) Uani 1 1 d . . . C12 C 1.0041(4) 0.7018(3) 0.9490(2) 0.0371(8) Uani 1 1 d . . . H12 H 0.9277 0.6824 0.9884 0.045 Uiso 1 1 calc R . . C13 C 1.1093(5) 0.7437(3) 0.9689(3) 0.0492(11) Uani 1 1 d . . . H13 H 1.1032 0.7537 1.0219 0.059 Uiso 1 1 calc R . . C14 C 1.2208(5) 0.7702(3) 0.9122(3) 0.0544(12) Uani 1 1 d . . . H14 H 1.2912 0.7988 0.9262 0.065 Uiso 1 1 calc R . . C15 C 1.2316(4) 0.7559(3) 0.8354(3) 0.0506(11) Uani 1 1 d . . . H15 H 1.3104 0.7733 0.7966 0.061 Uiso 1 1 calc R . . C16 C 1.1283(4) 0.7164(3) 0.8142(2) 0.0402(9) Uani 1 1 d . . . H16 H 1.1356 0.7077 0.7608 0.048 Uiso 1 1 calc R . . C17 C 0.7432(3) 0.6202(2) 0.92468(19) 0.0276(7) Uani 1 1 d . . . C18 C 0.7695(4) 0.5372(3) 0.9781(2) 0.0366(8) Uani 1 1 d . . . H18 H 0.8572 0.4906 0.9676 0.044 Uiso 1 1 calc R . . C19 C 0.6684(4) 0.5226(3) 1.0463(2) 0.0402(8) Uani 1 1 d . . . H19 H 0.6871 0.4660 1.0821 0.048 Uiso 1 1 calc R . . C20 C 0.5414(4) 0.5896(3) 1.0621(2) 0.0412(9) Uani 1 1 d . . . H20 H 0.4723 0.5791 1.1087 0.049 Uiso 1 1 calc R . . C21 C 0.5136(4) 0.6721(3) 1.0106(2) 0.0418(9) Uani 1 1 d . . . H21 H 0.4257 0.7186 1.0222 0.050 Uiso 1 1 calc R . . C22 C 0.6127(4) 0.6879(3) 0.9420(2) 0.0343(8) Uani 1 1 d . . . H22 H 0.5923 0.7447 0.9067 0.041 Uiso 1 1 calc R . . C23 C 0.9618(3) 0.5094(2) 0.81617(19) 0.0277(7) Uani 1 1 d . . . C24 C 0.8767(4) 0.4404(3) 0.8091(2) 0.0343(8) Uani 1 1 d . . . H24 H 0.7776 0.4634 0.8137 0.041 Uiso 1 1 calc R . . C25 C 0.9354(4) 0.3386(3) 0.7955(2) 0.0433(9) Uani 1 1 d . . . H25 H 0.8766 0.2928 0.7901 0.052 Uiso 1 1 calc R . . C26 C 1.0787(5) 0.3039(3) 0.7897(3) 0.0509(11) Uani 1 1 d . . . H26 H 1.1188 0.2344 0.7798 0.061 Uiso 1 1 calc R . . C27 C 1.1634(4) 0.3702(3) 0.7983(3) 0.0498(10) Uani 1 1 d . . . H27 H 1.2615 0.3456 0.7959 0.060 Uiso 1 1 calc R . . C28 C 1.1071(4) 0.4722(3) 0.8104(2) 0.0376(8) Uani 1 1 d . . . H28 H 1.1673 0.5175 0.8149 0.045 Uiso 1 1 calc R . . C29 C 0.8083(4) 0.7315(3) 0.5630(2) 0.0340(8) Uani 1 1 d . . . C30 C 0.6657(4) 0.7799(3) 0.5683(3) 0.0453(9) Uani 1 1 d . . . H30 H 0.6000 0.7821 0.6175 0.054 Uiso 1 1 calc R . . C31 C 0.6210(5) 0.8244(3) 0.5019(3) 0.0581(12) Uani 1 1 d . . . H31 H 0.5249 0.8570 0.5057 0.070 Uiso 1 1 calc R . . C32 C 0.7171(6) 0.8210(4) 0.4301(3) 0.0658(14) Uani 1 1 d . . . H32 H 0.6859 0.8512 0.3848 0.079 Uiso 1 1 calc R . . C33 C 0.8570(6) 0.7746(4) 0.4235(3) 0.0630(13) Uani 1 1 d . . . H33 H 0.9221 0.7731 0.3741 0.076 Uiso 1 1 calc R . . C34 C 0.9023(5) 0.7296(3) 0.4904(2) 0.0460(9) Uani 1 1 d . . . H34 H 0.9986 0.6972 0.4860 0.055 Uiso 1 1 calc R . . C35 C 0.7507(3) 0.5650(2) 0.66502(19) 0.0285(7) Uani 1 1 d . . . C36 C 0.6251(4) 0.5723(3) 0.7226(2) 0.0339(8) Uani 1 1 d . . . H36 H 0.5986 0.6271 0.7562 0.041 Uiso 1 1 calc R . . C37 C 0.5384(4) 0.4999(3) 0.7312(2) 0.0420(9) Uani 1 1 d . . . H37 H 0.4517 0.5063 0.7697 0.050 Uiso 1 1 calc R . . C38 C 0.5775(5) 0.4187(3) 0.6840(3) 0.0472(10) Uani 1 1 d . . . H38 H 0.5202 0.3675 0.6918 0.057 Uiso 1 1 calc R . . C39 C 0.6998(5) 0.4117(3) 0.6253(3) 0.0475(10) Uani 1 1 d . . . H39 H 0.7257 0.3562 0.5923 0.057 Uiso 1 1 calc R . . C40 C 0.7851(4) 0.4858(3) 0.6143(2) 0.0381(8) Uani 1 1 d . . . H40 H 0.8668 0.4827 0.5724 0.046 Uiso 1 1 calc R . . C41 C 1.0438(4) 0.6156(3) 0.6206(2) 0.0335(8) Uani 1 1 d . . . C42 C 1.1050(4) 0.5123(3) 0.6207(2) 0.0440(9) Uani 1 1 d . . . H42 H 1.0470 0.4612 0.6353 0.053 Uiso 1 1 calc R . . C43 C 1.2539(5) 0.4841(4) 0.5991(3) 0.0582(12) Uani 1 1 d . . . H43 H 1.2965 0.4136 0.5986 0.070 Uiso 1 1 calc R . . C44 C 1.3378(4) 0.5577(4) 0.5786(3) 0.0598(13) Uani 1 1 d . . . H44 H 1.4382 0.5376 0.5647 0.072 Uiso 1 1 calc R . . C45 C 1.2785(4) 0.6598(4) 0.5781(3) 0.0527(11) Uani 1 1 d . . . H45 H 1.3375 0.7102 0.5634 0.063 Uiso 1 1 calc R . . C46 C 1.1330(4) 0.6888(3) 0.5990(2) 0.0446(9) Uani 1 1 d . . . H46 H 1.0923 0.7596 0.5988 0.053 Uiso 1 1 calc R . . C1 C 0.4439(4) 1.0289(3) 0.7994(2) 0.0372(8) Uani 1 1 d . . . C2 C 0.2843(4) 1.0329(3) 0.8192(3) 0.0481(10) Uani 1 1 d . . . H2A H 0.2376 1.0892 0.8530 0.072 Uiso 1 1 calc R . . H2B H 0.2625 0.9679 0.8464 0.072 Uiso 1 1 calc R . . H2C H 0.2497 1.0442 0.7711 0.072 Uiso 1 1 calc R . . B2 B 0.5375(4) 1.0033(3) 0.7058(3) 0.0370(9) Uani 1 1 d . . . H2 H 0.4890 0.9887 0.6581 0.044 Uiso 1 1 calc R . . B3 B 0.5522(4) 0.9128(3) 0.7846(2) 0.0316(8) Uani 1 1 d . . . H3 H 0.5125 0.8389 0.7890 0.038 Uiso 1 1 calc R . . B4 B 0.5387(4) 0.9781(3) 0.8690(3) 0.0355(9) Uani 1 1 d . . . H4 H 0.4911 0.9468 0.9288 0.043 Uiso 1 1 calc R . . B5 B 0.5119(5) 1.1100(3) 0.8418(3) 0.0424(10) Uani 1 1 d . . . H5 H 0.4450 1.1670 0.8839 0.051 Uiso 1 1 calc R . . B6 B 0.5118(5) 1.1252(3) 0.7415(3) 0.0398(10) Uani 1 1 d . . . H6 H 0.4445 1.1926 0.7169 0.048 Uiso 1 1 calc R . . B7 B 0.7076(4) 0.9395(3) 0.7161(2) 0.0310(8) Uani 1 1 d . . . H7 H 0.763(3) 0.879(2) 0.6782(19) 0.020(8) Uiso 1 1 d . . . B8 B 0.7080(4) 0.9236(3) 0.8143(2) 0.0307(8) Uani 1 1 d . . . H8 H 0.776(3) 0.851(2) 0.8370(18) 0.015(7) Uiso 1 1 d . . . B9 B 0.6832(4) 1.0457(3) 0.8530(3) 0.0374(9) Uani 1 1 d . . . C3 C 0.7527(4) 1.0658(3) 0.9210(3) 0.0454(9) Uani 1 1 d . . . H3A H 0.8215 1.1123 0.8994 0.054 Uiso 1 1 calc R . . H3B H 0.6770 1.1015 0.9619 0.054 Uiso 1 1 calc R . . C4 C 0.8282(5) 0.9704(3) 0.9583(3) 0.0547(11) Uani 1 1 d . . . H4A H 0.8681 0.9896 0.9989 0.082 Uiso 1 1 calc R . . H4B H 0.9049 0.9350 0.9185 0.082 Uiso 1 1 calc R . . H4C H 0.7604 0.9247 0.9816 0.082 Uiso 1 1 calc R . . B10 B 0.6630(5) 1.1374(3) 0.7727(3) 0.0416(10) Uani 1 1 d . . . H10 H 0.6971 1.2134 0.7689 0.050 Uiso 1 1 calc R . . B11 B 0.6828(5) 1.0730(3) 0.6859(3) 0.0391(10) Uani 1 1 d . . . C5 C 0.7434(5) 1.1208(3) 0.6009(3) 0.0516(10) Uani 1 1 d . . . H5A H 0.6742 1.1820 0.5896 0.062 Uiso 1 1 calc R . . H5B H 0.8325 1.1442 0.6009 0.062 Uiso 1 1 calc R . . C6 C 0.7734(6) 1.0498(4) 0.5362(3) 0.0636(12) Uani 1 1 d . . . H6A H 0.8103 1.0858 0.4864 0.095 Uiso 1 1 calc R . . H6B H 0.6854 1.0277 0.5344 0.095 Uiso 1 1 calc R . . H6C H 0.8440 0.9897 0.5458 0.095 Uiso 1 1 calc R . . B12 B 0.7898(5) 1.0227(3) 0.7560(3) 0.0382(10) Uani 1 1 d . . . C7 C 0.9563(4) 1.0235(3) 0.7390(3) 0.0483(10) Uani 1 1 d . . . H7A H 0.9710 1.0946 0.7223 0.058 Uiso 1 1 calc R . . H7B H 0.9867 1.0051 0.7887 0.058 Uiso 1 1 calc R . . C8 C 1.0514(5) 0.9552(4) 0.6800(3) 0.0630(13) Uani 1 1 d . . . H8A H 1.1502 0.9625 0.6750 0.094 Uiso 1 1 calc R . . H8B H 1.0259 0.9740 0.6295 0.094 Uiso 1 1 calc R . . H8C H 1.0412 0.8840 0.6962 0.094 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 Rh 0.02768(13) 0.02451(13) 0.02547(14) 0.00162(9) -0.00990(10) -0.00336(9) P1 0.0260(4) 0.0242(4) 0.0250(4) -0.0001(3) -0.0097(3) -0.0035(3) P2 0.0282(4) 0.0303(4) 0.0245(5) 0.0015(3) -0.0093(3) -0.0034(3) C11 0.0342(17) 0.0242(15) 0.0345(19) 0.0001(14) -0.0172(15) -0.0037(13) C12 0.046(2) 0.0339(18) 0.037(2) -0.0022(15) -0.0209(17) -0.0057(16) C13 0.068(3) 0.040(2) 0.052(3) -0.0017(19) -0.041(2) -0.007(2) C14 0.063(3) 0.039(2) 0.079(3) 0.010(2) -0.046(3) -0.022(2) C15 0.050(2) 0.050(2) 0.064(3) 0.015(2) -0.031(2) -0.0259(19) C16 0.045(2) 0.044(2) 0.037(2) 0.0025(17) -0.0145(17) -0.0158(17) C17 0.0291(16) 0.0276(16) 0.0252(17) -0.0016(13) -0.0071(13) -0.0017(13) C18 0.0402(19) 0.0333(18) 0.031(2) 0.0049(15) -0.0067(16) -0.0008(15) C19 0.051(2) 0.0379(19) 0.029(2) 0.0078(16) -0.0100(17) -0.0058(17) C20 0.042(2) 0.052(2) 0.027(2) 0.0064(17) -0.0030(16) -0.0121(18) C21 0.0342(19) 0.046(2) 0.036(2) 0.0017(17) -0.0022(16) 0.0027(16) C22 0.0350(18) 0.0348(18) 0.031(2) 0.0039(15) -0.0081(15) -0.0046(15) C23 0.0315(16) 0.0261(15) 0.0261(17) 0.0010(13) -0.0111(14) -0.0023(13) C24 0.0401(19) 0.0300(17) 0.037(2) 0.0038(15) -0.0172(16) -0.0082(15) C25 0.062(2) 0.0297(18) 0.046(2) 0.0017(16) -0.026(2) -0.0102(17) C26 0.071(3) 0.0279(18) 0.053(3) -0.0063(18) -0.026(2) 0.0082(19) C27 0.046(2) 0.042(2) 0.057(3) -0.0080(19) -0.018(2) 0.0131(18) C28 0.0350(18) 0.0332(18) 0.045(2) -0.0019(16) -0.0145(17) -0.0015(15) C29 0.0418(19) 0.0348(18) 0.0296(19) 0.0017(15) -0.0154(16) -0.0093(15) C30 0.041(2) 0.048(2) 0.049(3) 0.0060(19) -0.0210(19) -0.0065(18) C31 0.065(3) 0.057(3) 0.063(3) 0.014(2) -0.042(3) -0.012(2) C32 0.099(4) 0.062(3) 0.052(3) 0.019(2) -0.052(3) -0.021(3) C33 0.095(4) 0.065(3) 0.031(2) 0.008(2) -0.019(2) -0.021(3) C34 0.058(2) 0.050(2) 0.032(2) 0.0002(18) -0.0140(19) -0.012(2) C35 0.0335(17) 0.0294(16) 0.0236(17) 0.0003(13) -0.0106(14) -0.0040(14) C36 0.0355(18) 0.0398(19) 0.0280(19) 0.0006(15) -0.0119(15) -0.0063(15) C37 0.0374(19) 0.052(2) 0.038(2) 0.0113(18) -0.0134(17) -0.0135(18) C38 0.057(2) 0.039(2) 0.056(3) 0.0143(19) -0.029(2) -0.0218(19) C39 0.065(3) 0.0322(19) 0.048(3) -0.0040(17) -0.019(2) -0.0085(19) C40 0.045(2) 0.0361(19) 0.033(2) -0.0037(15) -0.0108(17) -0.0043(16) C41 0.0312(17) 0.045(2) 0.0232(18) -0.0008(15) -0.0099(14) 0.0002(15) C42 0.042(2) 0.050(2) 0.031(2) 0.0037(17) -0.0049(16) 0.0045(18) C43 0.048(2) 0.072(3) 0.039(3) 0.006(2) -0.0066(19) 0.017(2) C44 0.034(2) 0.104(4) 0.034(2) 0.004(2) -0.0081(18) -0.001(2) C45 0.035(2) 0.080(3) 0.041(2) -0.007(2) -0.0029(17) -0.012(2) C46 0.038(2) 0.056(2) 0.041(2) -0.0051(19) -0.0090(17) -0.0125(18) C1 0.0345(18) 0.0282(17) 0.051(2) -0.0054(16) -0.0184(17) 0.0008(15) C2 0.036(2) 0.042(2) 0.066(3) 0.001(2) -0.0168(19) -0.0012(17) B2 0.038(2) 0.030(2) 0.046(3) -0.0020(18) -0.019(2) -0.0025(17) B3 0.0281(18) 0.0278(19) 0.040(2) -0.0024(16) -0.0124(17) -0.0011(15) B4 0.036(2) 0.034(2) 0.035(2) -0.0065(17) -0.0066(17) -0.0017(17) B5 0.048(2) 0.030(2) 0.053(3) -0.0077(19) -0.025(2) 0.0001(19) B6 0.044(2) 0.0270(19) 0.052(3) 0.0033(18) -0.021(2) -0.0055(18) B7 0.037(2) 0.0266(18) 0.031(2) 0.0025(16) -0.0119(17) -0.0062(16) B8 0.0333(19) 0.0265(18) 0.034(2) 0.0004(16) -0.0128(17) -0.0055(16) B9 0.040(2) 0.029(2) 0.047(3) -0.0084(18) -0.017(2) -0.0033(17) C3 0.050(2) 0.041(2) 0.050(3) -0.0127(18) -0.021(2) -0.0031(18) C4 0.064(3) 0.056(3) 0.052(3) -0.012(2) -0.032(2) -0.003(2) B10 0.050(3) 0.0260(19) 0.055(3) 0.0037(19) -0.026(2) -0.0085(18) B11 0.043(2) 0.032(2) 0.045(3) 0.0068(18) -0.017(2) -0.0093(18) C5 0.062(3) 0.042(2) 0.054(3) 0.0082(19) -0.020(2) -0.014(2) C6 0.085(3) 0.053(3) 0.045(3) 0.010(2) -0.009(2) -0.011(2) B12 0.040(2) 0.032(2) 0.048(3) 0.0038(18) -0.019(2) -0.0109(18) C7 0.040(2) 0.055(2) 0.053(3) 0.003(2) -0.0115(19) -0.0174(19) C8 0.045(2) 0.070(3) 0.075(4) -0.020(3) -0.009(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh P2 2.2129(9) . ? Rh P1 2.2457(8) . ? Rh B7 2.401(4) . ? Rh B8 2.405(4) . ? Rh H7 1.93(3) . ? Rh H8 1.93(3) . ? P1 C17 1.822(3) . ? P1 C11 1.825(3) . ? P1 C23 1.832(3) . ? P2 C35 1.824(3) . ? P2 C41 1.825(3) . ? P2 C29 1.834(3) . ? C11 C12 1.397(5) . ? C11 C16 1.400(5) . ? C12 C13 1.404(5) . ? C12 H12 0.9500 . ? C13 C14 1.370(7) . ? C13 H13 0.9500 . ? C14 C15 1.372(6) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.401(4) . ? C17 C22 1.403(5) . ? C18 C19 1.388(5) . ? C18 H18 0.9500 . ? C19 C20 1.372(5) . ? C19 H19 0.9500 . ? C20 C21 1.378(5) . ? C20 H20 0.9500 . ? C21 C22 1.385(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.398(4) . ? C23 C28 1.402(5) . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C25 C26 1.378(6) . ? C25 H25 0.9500 . ? C26 C27 1.376(6) . ? C26 H26 0.9500 . ? C27 C28 1.383(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.389(5) . ? C29 C30 1.410(5) . ? C30 C31 1.388(5) . ? C30 H30 0.9500 . ? C31 C32 1.387(7) . ? C31 H31 0.9500 . ? C32 C33 1.377(7) . ? C32 H32 0.9500 . ? C33 C34 1.400(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.393(5) . ? C35 C40 1.399(5) . ? C36 C37 1.386(5) . ? C36 H36 0.9500 . ? C37 C38 1.378(6) . ? C37 H37 0.9500 . ? C38 C39 1.380(6) . ? C38 H38 0.9500 . ? C39 C40 1.391(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.390(5) . ? C41 C46 1.403(5) . ? C42 C43 1.407(6) . ? C42 H42 0.9500 . ? C43 C44 1.370(7) . ? C43 H43 0.9500 . ? C44 C45 1.370(7) . ? C44 H44 0.9500 . ? C45 C46 1.377(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C1 C2 1.518(5) . ? C1 B6 1.693(6) . ? C1 B3 1.702(5) . ? C1 B5 1.705(5) . ? C1 B2 1.723(6) . ? C1 B4 1.728(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? B2 B3 1.757(6) . ? B2 B6 1.759(6) . ? B2 B7 1.766(5) . ? B2 B11 1.805(6) . ? B2 H2 1.1200 . ? B3 B7 1.777(6) . ? B3 B4 1.778(6) . ? B3 B8 1.779(5) . ? B3 H3 1.1200 . ? B4 B5 1.756(6) . ? B4 B8 1.769(6) . ? B4 B9 1.785(6) . ? B4 H4 1.1200 . ? B5 B10 1.754(7) . ? B5 B6 1.767(7) . ? B5 B9 1.783(6) . ? B5 H5 1.1200 . ? B6 B10 1.755(6) . ? B6 B11 1.779(7) . ? B6 H6 1.1200 . ? B7 B8 1.732(6) . ? B7 B11 1.787(5) . ? B7 B12 1.792(5) . ? B7 H7 1.08(3) . ? B8 B12 1.783(6) . ? B8 B9 1.786(5) . ? B8 H8 1.15(3) . ? B9 C3 1.596(5) . ? B9 B10 1.794(6) . ? B9 B12 1.804(7) . ? C3 C4 1.512(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? B10 B12 1.774(6) . ? B10 B11 1.796(7) . ? B10 H10 1.1200 . ? B11 C5 1.590(6) . ? B11 B12 1.813(6) . ? C5 C6 1.505(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? B12 C7 1.597(5) . ? C7 C8 1.481(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 P2 Rh P1 95.77(3) . . ? P2 Rh B7 111.71(10) . . ? P1 Rh B7 152.43(10) . . ? P2 Rh B8 153.47(9) . . ? P1 Rh B8 110.20(10) . . ? B7 Rh B8 42.24(14) . . ? P2 Rh H7 86.7(10) . . ? P1 Rh H7 174.7(8) . . ? B7 Rh H7 25.9(10) . . ? B8 Rh H7 67.9(10) . . ? P2 Rh H8 178.0(8) . . ? P1 Rh H8 82.9(9) . . ? B7 Rh H8 69.7(9) . . ? B8 Rh H8 28.1(8) . . ? H7 Rh H8 94.5(13) . . ? C17 P1 C11 104.90(15) . . ? C17 P1 C23 100.16(15) . . ? C11 P1 C23 102.81(14) . . ? C17 P1 Rh 115.69(10) . . ? C11 P1 Rh 104.50(10) . . ? C23 P1 Rh 126.47(11) . . ? C35 P2 C41 110.38(16) . . ? C35 P2 C29 98.12(15) . . ? C41 P2 C29 103.07(16) . . ? C35 P2 Rh 116.58(11) . . ? C41 P2 Rh 112.29(11) . . ? C29 P2 Rh 114.82(12) . . ? C12 C11 C16 118.9(3) . . ? C12 C11 P1 123.7(3) . . ? C16 C11 P1 117.4(3) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.6(4) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C18 C17 C22 118.3(3) . . ? C18 C17 P1 120.6(3) . . ? C22 C17 P1 121.0(2) . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.3(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 120.2(3) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C24 C23 C28 118.0(3) . . ? C24 C23 P1 119.0(2) . . ? C28 C23 P1 123.0(2) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 119.8(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C23 120.5(3) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C34 C29 C30 118.7(3) . . ? C34 C29 P2 124.0(3) . . ? C30 C29 P2 117.2(3) . . ? C31 C30 C29 120.3(4) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 119.8(4) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.3(5) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C29 C34 C33 120.9(4) . . ? C29 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C40 118.9(3) . . ? C36 C35 P2 118.3(3) . . ? C40 C35 P2 122.5(3) . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.3(4) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 120.1(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.1(4) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? C42 C41 C46 118.7(3) . . ? C42 C41 P2 125.6(3) . . ? C46 C41 P2 115.6(3) . . ? C41 C42 C43 119.3(4) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.4(4) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.8(4) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 119.6(4) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 121.2(4) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? C2 C1 B6 119.0(3) . . ? C2 C1 B3 118.3(3) . . ? B6 C1 B3 112.7(3) . . ? C2 C1 B5 119.0(3) . . ? B6 C1 B5 62.7(3) . . ? B3 C1 B5 113.1(3) . . ? C2 C1 B2 118.3(3) . . ? B6 C1 B2 62.0(3) . . ? B3 C1 B2 61.7(2) . . ? B5 C1 B2 113.6(3) . . ? C2 C1 B4 118.9(3) . . ? B6 C1 B4 112.9(3) . . ? B3 C1 B4 62.4(2) . . ? B5 C1 B4 61.5(2) . . ? B2 C1 B4 113.1(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 B2 B3 58.6(2) . . ? C1 B2 B6 58.2(2) . . ? B3 B2 B6 107.0(3) . . ? C1 B2 B7 104.7(3) . . ? B3 B2 B7 60.6(2) . . ? B6 B2 B7 106.4(3) . . ? C1 B2 B11 105.7(3) . . ? B3 B2 B11 109.4(3) . . ? B6 B2 B11 59.9(2) . . ? B7 B2 B11 60.1(2) . . ? C1 B2 H2 124.6 . . ? B3 B2 H2 121.1 . . ? B6 B2 H2 122.8 . . ? B7 B2 H2 122.8 . . ? B11 B2 H2 121.3 . . ? C1 B3 B2 59.7(2) . . ? C1 B3 B7 105.0(3) . . ? B2 B3 B7 59.9(2) . . ? C1 B3 B4 59.5(2) . . ? B2 B3 B4 109.0(3) . . ? B7 B3 B4 106.6(3) . . ? C1 B3 B8 104.9(3) . . ? B2 B3 B8 107.0(3) . . ? B7 B3 B8 58.3(2) . . ? B4 B3 B8 59.6(2) . . ? C1 B3 H3 123.8 . . ? B2 B3 H3 121.0 . . ? B7 B3 H3 123.4 . . ? B4 B3 H3 121.4 . . ? B8 B3 H3 123.4 . . ? C1 B4 B5 58.6(2) . . ? C1 B4 B8 104.3(3) . . ? B5 B4 B8 107.1(3) . . ? C1 B4 B3 58.1(2) . . ? B5 B4 B3 107.1(3) . . ? B8 B4 B3 60.2(2) . . ? C1 B4 B9 106.2(3) . . ? B5 B4 B9 60.5(2) . . ? B8 B4 B9 60.3(2) . . ? B3 B4 B9 109.4(3) . . ? C1 B4 H4 124.7 . . ? B5 B4 H4 122.2 . . ? B8 B4 H4 122.8 . . ? B3 B4 H4 121.5 . . ? B9 B4 H4 120.9 . . ? C1 B5 B10 105.6(3) . . ? C1 B5 B4 59.9(2) . . ? B10 B5 B4 108.7(3) . . ? C1 B5 B6 58.3(2) . . ? B10 B5 B6 59.8(3) . . ? B4 B5 B6 108.0(3) . . ? C1 B5 B9 107.3(3) . . ? B10 B5 B9 61.0(3) . . ? B4 B5 B9 60.6(2) . . ? B6 B5 B9 109.0(3) . . ? C1 B5 H5 123.6 . . ? B10 B5 H5 122.0 . . ? B4 B5 H5 121.1 . . ? B6 B5 H5 121.9 . . ? B9 B5 H5 120.9 . . ? C1 B6 B10 106.1(3) . . ? C1 B6 B2 59.9(2) . . ? B10 B6 B2 109.4(3) . . ? C1 B6 B5 59.0(2) . . ? B10 B6 B5 59.7(3) . . ? B2 B6 B5 108.8(3) . . ? C1 B6 B11 108.1(3) . . ? B10 B6 B11 61.1(3) . . ? B2 B6 B11 61.3(2) . . ? B5 B6 B11 109.6(3) . . ? C1 B6 H6 123.2 . . ? B10 B6 H6 121.9 . . ? B2 B6 H6 120.6 . . ? B5 B6 H6 121.4 . . ? B11 B6 H6 120.3 . . ? B8 B7 B2 108.8(3) . . ? B8 B7 B3 60.9(2) . . ? B2 B7 B3 59.4(2) . . ? B8 B7 B11 109.8(3) . . ? B2 B7 B11 61.0(2) . . ? B3 B7 B11 109.3(3) . . ? B8 B7 B12 60.8(2) . . ? B2 B7 B12 109.7(3) . . ? B3 B7 B12 109.9(3) . . ? B11 B7 B12 60.9(2) . . ? B8 B7 Rh 69.02(18) . . ? B2 B7 Rh 135.0(2) . . ? B3 B7 Rh 84.50(19) . . ? B11 B7 Rh 163.9(2) . . ? B12 B7 Rh 107.3(2) . . ? B8 B7 H7 119.9(16) . . ? B2 B7 H7 118.5(16) . . ? B3 B7 H7 115.6(16) . . ? B11 B7 H7 124.3(17) . . ? B12 B7 H7 125.4(16) . . ? Rh B7 H7 51.6(16) . . ? B7 B8 B4 109.1(3) . . ? B7 B8 B3 60.8(2) . . ? B4 B8 B3 60.1(2) . . ? B7 B8 B12 61.3(2) . . ? B4 B8 B12 109.2(3) . . ? B3 B8 B12 110.2(3) . . ? B7 B8 B9 110.0(3) . . ? B4 B8 B9 60.3(2) . . ? B3 B8 B9 109.3(3) . . ? B12 B8 B9 60.7(2) . . ? B7 B8 Rh 68.74(19) . . ? B4 B8 Rh 135.7(2) . . ? B3 B8 Rh 84.32(19) . . ? B12 B8 Rh 107.4(2) . . ? B9 B8 Rh 164.0(3) . . ? B7 B8 H8 119.1(15) . . ? B4 B8 H8 122.1(16) . . ? B3 B8 H8 119.5(14) . . ? B12 B8 H8 120.8(15) . . ? B9 B8 H8 122.5(14) . . ? Rh B8 H8 52.2(15) . . ? C3 B9 B5 123.4(3) . . ? C3 B9 B4 123.4(4) . . ? B5 B9 B4 59.0(2) . . ? C3 B9 B8 123.9(3) . . ? B5 B9 B8 105.2(3) . . ? B4 B9 B8 59.4(2) . . ? C3 B9 B10 122.7(3) . . ? B5 B9 B10 58.7(3) . . ? B4 B9 B10 105.7(3) . . ? B8 B9 B10 105.0(3) . . ? C3 B9 B12 121.2(3) . . ? B5 B9 B12 106.4(3) . . ? B4 B9 B12 107.6(3) . . ? B8 B9 B12 59.6(2) . . ? B10 B9 B12 59.1(3) . . ? C4 C3 B9 114.8(3) . . ? C4 C3 H3A 108.6 . . ? B9 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? B9 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? B5 B10 B6 60.5(3) . . ? B5 B10 B12 109.0(3) . . ? B6 B10 B12 108.7(3) . . ? B5 B10 B9 60.3(2) . . ? B6 B10 B9 109.0(3) . . ? B12 B10 B9 60.7(2) . . ? B5 B10 B11 109.5(3) . . ? B6 B10 B11 60.1(2) . . ? B12 B10 B11 61.0(2) . . ? B9 B10 B11 110.3(3) . . ? B5 B10 H10 121.1 . . ? B6 B10 H10 121.5 . . ? B12 B10 H10 121.1 . . ? B9 B10 H10 120.7 . . ? B11 B10 H10 120.4 . . ? C5 B11 B6 121.0(3) . . ? C5 B11 B7 125.6(4) . . ? B6 B11 B7 104.7(3) . . ? C5 B11 B10 122.7(3) . . ? B6 B11 B10 58.8(2) . . ? B7 B11 B10 105.0(3) . . ? C5 B11 B2 121.8(3) . . ? B6 B11 B2 58.8(2) . . ? B7 B11 B2 58.9(2) . . ? B10 B11 B2 105.6(3) . . ? C5 B11 B12 124.2(3) . . ? B6 B11 B12 105.9(3) . . ? B7 B11 B12 59.7(2) . . ? B10 B11 B12 58.9(2) . . ? B2 B11 B12 107.0(3) . . ? C6 C5 B11 115.3(3) . . ? C6 C5 H5A 108.4 . . ? B11 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? B11 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 B12 B10 121.1(3) . . ? C7 B12 B8 123.4(3) . . ? B10 B12 B8 105.9(3) . . ? C7 B12 B7 126.1(4) . . ? B10 B12 B7 105.7(3) . . ? B8 B12 B7 57.9(2) . . ? C7 B12 B9 118.6(3) . . ? B10 B12 B9 60.2(3) . . ? B8 B12 B9 59.7(2) . . ? B7 B12 B9 106.5(3) . . ? C7 B12 B11 123.1(3) . . ? B10 B12 B11 60.1(2) . . ? B8 B12 B11 106.3(3) . . ? B7 B12 B11 59.4(2) . . ? B9 B12 B11 109.0(3) . . ? C8 C7 B12 117.4(3) . . ? C8 C7 H7A 108.0 . . ? B12 C7 H7A 108.0 . . ? C8 C7 H7B 108.0 . . ? B12 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.452 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.080 #===END data_k05asw1 _database_code_depnum_ccdc_archive 'CCDC 268854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4' _chemical_melting_point ? _chemical_formula_moiety '[(C43 H38 P2 Rh)+(C11 H32 B11)-]' _chemical_formula_sum 'C54 H70 B11 P2 Rh' _chemical_formula_weight 1002.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 16.7380(2) _cell_length_b 18.0910(2) _cell_length_c 18.5710(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.6180(10) _cell_angle_gamma 90.00 _cell_volume 5227.88(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 89758 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 76466 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11940 _reflns_number_gt 9750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _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. One phenyl group of the cation shows disorder in the ratio 80:20. Three ethyl groups of the anion are disordered in the ratio 60:40. C54 and C54A are isotropically refined. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+6.4736P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11940 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Rh Rh 0.276568(14) 0.183944(12) 0.197604(11) 0.02903(7) Uani 1 1 d . . . P1 P 0.29124(5) 0.16285(4) 0.32525(4) 0.03162(16) Uani 1 1 d . B . P2 P 0.15809(5) 0.10724(4) 0.13555(4) 0.03159(16) Uani 1 1 d . . . C2 C 0.2971(2) 0.31347(17) 0.12336(18) 0.0431(7) Uani 1 1 d . . . H2 H 0.2596 0.3577 0.1038 0.052 Uiso 1 1 calc R . . C3 C 0.2620(2) 0.23853(17) 0.08703(16) 0.0375(6) Uani 1 1 d . . . H3 H 0.2038 0.2268 0.0576 0.045 Uiso 1 1 calc R . . C4 C 0.3308(2) 0.19198(17) 0.10527(16) 0.0383(6) Uani 1 1 d . . . H4 H 0.3293 0.1413 0.0913 0.046 Uiso 1 1 calc R . . C5 C 0.4105(2) 0.23622(19) 0.15215(18) 0.0450(7) Uani 1 1 d . . . H5 H 0.4676 0.2158 0.1564 0.054 Uiso 1 1 calc R . . C6 C 0.3950(2) 0.24912(18) 0.22781(17) 0.0413(7) Uani 1 1 d . . . H6 H 0.4269 0.2284 0.2771 0.050 Uiso 1 1 calc R . . C7 C 0.3265(2) 0.29603(16) 0.21057(17) 0.0397(7) Uani 1 1 d . . . H7 H 0.3018 0.3144 0.2456 0.048 Uiso 1 1 calc R . . C8 C 0.3850(2) 0.3129(2) 0.1139(2) 0.0514(8) Uani 1 1 d . . . H8A H 0.4237 0.3529 0.1433 0.062 Uiso 1 1 calc R . . H8B H 0.3798 0.3137 0.0591 0.062 Uiso 1 1 calc R . . C11 C 0.19576(19) 0.18058(16) 0.34854(16) 0.0356(6) Uani 1 1 d . . . C12 C 0.1409(2) 0.2352(2) 0.3070(2) 0.0528(9) Uani 1 1 d . . . H12 H 0.1537 0.2617 0.2684 0.063 Uiso 1 1 calc R . . C13 C 0.0669(3) 0.2522(2) 0.3210(3) 0.0696(11) Uani 1 1 d . . . H13 H 0.0296 0.2900 0.2919 0.083 Uiso 1 1 calc R . . C14 C 0.0474(2) 0.2149(2) 0.3760(2) 0.0601(10) Uani 1 1 d . . . H14 H -0.0036 0.2262 0.3849 0.072 Uiso 1 1 calc R . . C15 C 0.1018(3) 0.1610(2) 0.4183(2) 0.0604(10) Uani 1 1 d . . . H15 H 0.0888 0.1355 0.4573 0.072 Uiso 1 1 calc R . . C16 C 0.1763(2) 0.1432(2) 0.40488(19) 0.0521(8) Uani 1 1 d . . . H16 H 0.2135 0.1054 0.4344 0.063 Uiso 1 1 calc R . . C17 C 0.3719(2) 0.22278(16) 0.39401(15) 0.0355(6) Uani 1 1 d . . . C18 C 0.3490(2) 0.29277(18) 0.41191(18) 0.0432(7) Uani 1 1 d . . . H18 H 0.2905 0.3077 0.3918 0.052 Uiso 1 1 calc R . . C19 C 0.4115(3) 0.3405(2) 0.4591(2) 0.0548(9) Uani 1 1 d . . . H19 H 0.3957 0.3883 0.4703 0.066 Uiso 1 1 calc R . . C20 C 0.4965(3) 0.3189(2) 0.4896(2) 0.0581(10) Uani 1 1 d . . . H20 H 0.5390 0.3513 0.5224 0.070 Uiso 1 1 calc R . . C21 C 0.5196(2) 0.2498(2) 0.4722(2) 0.0565(9) Uani 1 1 d . . . H21 H 0.5781 0.2350 0.4931 0.068 Uiso 1 1 calc R . . C22 C 0.4580(2) 0.20187(19) 0.42448(18) 0.0461(7) Uani 1 1 d . . . H22 H 0.4747 0.1546 0.4126 0.055 Uiso 1 1 calc R . . C23 C 0.3312(2) 0.06985(16) 0.35647(17) 0.0379(6) Uani 1 1 d . . . C26 C 0.3975(3) -0.0719(2) 0.3974(3) 0.0702(12) Uani 1 1 d . . . H26 H 0.4186 -0.1207 0.4112 0.084 Uiso 1 1 calc R A 1 C24 C 0.3427(3) 0.0209(3) 0.3041(3) 0.0426(11) Uani 0.858(7) 1 d P B 1 H24 H 0.3271 0.0359 0.2517 0.051 Uiso 0.858(7) 1 calc PR B 1 C25 C 0.3763(4) -0.0495(3) 0.3253(3) 0.0540(13) Uani 0.858(7) 1 d P B 1 H25 H 0.3840 -0.0815 0.2878 0.065 Uiso 0.858(7) 1 calc PR B 1 C27 C 0.3893(4) -0.0244(3) 0.4546(3) 0.0661(15) Uani 0.858(7) 1 d P B 1 H27 H 0.4049 -0.0409 0.5066 0.079 Uiso 0.858(7) 1 calc PR B 1 C28 C 0.3583(3) 0.0465(2) 0.4344(2) 0.0528(12) Uani 0.858(7) 1 d P B 1 H28 H 0.3552 0.0796 0.4730 0.063 Uiso 0.858(7) 1 calc PR B 1 C24A C 0.379(2) 0.0455(15) 0.3186(17) 0.038(6) Uani 0.142(7) 1 d P B 2 H24A H 0.3913 0.0762 0.2824 0.046 Uiso 0.142(7) 1 calc PR B 2 C25A C 0.409(2) -0.0218(17) 0.3323(19) 0.050(8) Uani 0.142(7) 1 d P B 2 H25A H 0.4391 -0.0413 0.3019 0.060 Uiso 0.142(7) 1 calc PR B 2 C27A C 0.322(2) -0.0516(13) 0.4012(15) 0.064(10) Uani 0.142(7) 1 d P B 2 H27A H 0.2886 -0.0885 0.4139 0.077 Uiso 0.142(7) 1 calc PR B 2 C28A C 0.2878(15) 0.0210(12) 0.3875(12) 0.042(6) Uani 0.142(7) 1 d P B 2 H28A H 0.2390 0.0355 0.3985 0.050 Uiso 0.142(7) 1 calc PR B 2 C29 C 0.05939(18) 0.16194(17) 0.09933(17) 0.0366(6) Uani 1 1 d . . . C30 C -0.0203(2) 0.1282(2) 0.06789(19) 0.0475(8) Uani 1 1 d . . . H30 H -0.0244 0.0758 0.0671 0.057 Uiso 1 1 calc R . . C31 C -0.0941(2) 0.1706(2) 0.0376(2) 0.0565(9) Uani 1 1 d . . . H31 H -0.1486 0.1472 0.0160 0.068 Uiso 1 1 calc R . . C32 C -0.0887(2) 0.2466(2) 0.0386(2) 0.0569(9) Uani 1 1 d . . . H32 H -0.1394 0.2754 0.0172 0.068 Uiso 1 1 calc R . . C33 C -0.0098(2) 0.2810(2) 0.0708(2) 0.0520(8) Uani 1 1 d . . . H33 H -0.0063 0.3334 0.0718 0.062 Uiso 1 1 calc R . . C34 C 0.0644(2) 0.23891(17) 0.10152(19) 0.0433(7) Uani 1 1 d . . . H34 H 0.1186 0.2626 0.1241 0.052 Uiso 1 1 calc R . . C35 C 0.16752(19) 0.06757(16) 0.04874(17) 0.0372(6) Uani 1 1 d . . . C36 C 0.1088(2) 0.08112(19) -0.02544(18) 0.0462(8) Uani 1 1 d . . . H36 H 0.0602 0.1115 -0.0325 0.055 Uiso 1 1 calc R . . C37 C 0.1207(3) 0.0505(2) -0.0895(2) 0.0600(10) Uani 1 1 d . . . H37 H 0.0800 0.0598 -0.1401 0.072 Uiso 1 1 calc R . . C38 C 0.1911(3) 0.0066(2) -0.0801(2) 0.0609(10) Uani 1 1 d . . . H38 H 0.1985 -0.0147 -0.1240 0.073 Uiso 1 1 calc R . . C39 C 0.2512(2) -0.0064(2) -0.0067(2) 0.0534(9) Uani 1 1 d . . . H39 H 0.3001 -0.0361 -0.0003 0.064 Uiso 1 1 calc R . . C40 C 0.2402(2) 0.02385(18) 0.05734(19) 0.0434(7) Uani 1 1 d . . . H40 H 0.2819 0.0151 0.1076 0.052 Uiso 1 1 calc R . . C41 C 0.12806(18) 0.02901(16) 0.18253(17) 0.0374(6) Uani 1 1 d . . . C42 C 0.0890(2) 0.04371(19) 0.23542(18) 0.0471(8) Uani 1 1 d . . . H42 H 0.0733 0.0929 0.2422 0.056 Uiso 1 1 calc R . . C43 C 0.0728(3) -0.0133(2) 0.2785(2) 0.0593(10) Uani 1 1 d . . . H43 H 0.0471 -0.0028 0.3152 0.071 Uiso 1 1 calc R . . C44 C 0.0940(3) -0.0851(2) 0.2680(2) 0.0656(11) Uani 1 1 d . . . H44 H 0.0843 -0.1238 0.2984 0.079 Uiso 1 1 calc R . . C45 C 0.1286(3) -0.1003(2) 0.2142(3) 0.0728(13) Uani 1 1 d . . . H45 H 0.1409 -0.1501 0.2057 0.087 Uiso 1 1 calc R . . C46 C 0.1463(2) -0.04396(19) 0.1711(2) 0.0565(9) Uani 1 1 d . . . H46 H 0.1709 -0.0555 0.1338 0.068 Uiso 1 1 calc R . . C1 C 0.6420(4) 0.0569(3) 0.3413(3) 0.0862(15) Uani 1 1 d . . . H1A H 0.6039 0.0277 0.3712 0.103 Uiso 1 1 calc R . . B2 B 0.5990(3) 0.0668(3) 0.2409(3) 0.0706(13) Uani 1 1 d . E . B3 B 0.6875(3) 0.0090(2) 0.2861(3) 0.0576(11) Uani 1 1 d . . . H3A H 0.6813 -0.0524 0.2782 0.069 Uiso 1 1 calc R . . B4 B 0.7536(4) 0.0487(3) 0.3761(3) 0.0627(12) Uani 1 1 d . E . B5 B 0.7065(3) 0.1315(3) 0.3852(3) 0.0623(12) Uani 1 1 d . E . H5A H 0.7133 0.1519 0.4442 0.075 Uiso 1 1 calc R . . B6 B 0.6138(3) 0.1413(3) 0.3023(3) 0.0675(13) Uani 1 1 d . E . H6A H 0.5560 0.1699 0.3058 0.081 Uiso 1 1 calc R . . B7 B 0.6882(3) 0.0683(2) 0.2106(2) 0.0485(9) Uani 1 1 d . . . H7A H 0.6832 0.0468 0.1526 0.058 Uiso 1 1 calc R . . B8 B 0.7842(3) 0.0564(2) 0.2935(2) 0.0494(9) Uani 1 1 d . . . B9 B 0.7919(3) 0.1354(3) 0.3537(2) 0.0572(11) Uani 1 1 d . E . H9A H 0.8556 0.1593 0.3906 0.069 Uiso 1 1 calc R . . B10 B 0.7023(4) 0.1934(3) 0.3098(3) 0.0664(13) Uani 1 1 d . . . B11 B 0.6391(3) 0.1509(3) 0.2216(3) 0.0614(12) Uani 1 1 d . E . H11A H 0.6003 0.1850 0.1703 0.074 Uiso 1 1 calc R . . B12 B 0.7522(3) 0.1465(2) 0.2515(2) 0.0488(9) Uani 1 1 d . E . C51 C 0.5025(3) 0.0379(4) 0.1896(4) 0.108(2) Uani 1 1 d . . . H51A H 0.4649 0.0498 0.2185 0.130 Uiso 1 1 calc R C 1 H51B H 0.4815 0.0670 0.1411 0.130 Uiso 1 1 calc R C 1 C53 C 0.8048(4) 0.0012(3) 0.4495(3) 0.0953(17) Uani 1 1 d . . . H53A H 0.7656 -0.0101 0.4770 0.114 Uiso 1 1 calc R D 1 H53B H 0.8199 -0.0464 0.4315 0.114 Uiso 1 1 calc R D 1 C55 C 0.8671(2) 0.0136(2) 0.2934(2) 0.0582(9) Uani 1 1 d . . . H55A H 0.8851 0.0357 0.2530 0.070 Uiso 1 1 calc R . . H55B H 0.9142 0.0219 0.3440 0.070 Uiso 1 1 calc R . . C56 C 0.8564(3) -0.0698(2) 0.2791(3) 0.0716(12) Uani 1 1 d . . . H56A H 0.9107 -0.0910 0.2802 0.107 Uiso 1 1 calc R . . H56B H 0.8113 -0.0790 0.2283 0.107 Uiso 1 1 calc R . . H56C H 0.8402 -0.0928 0.3195 0.107 Uiso 1 1 calc R . . C52 C 0.4916(9) -0.0334(8) 0.1705(13) 0.137(7) Uani 0.576(15) 1 d P E 1 H52A H 0.4310 -0.0428 0.1395 0.206 Uiso 0.576(15) 1 calc PR E 1 H52B H 0.5092 -0.0636 0.2176 0.206 Uiso 0.576(15) 1 calc PR E 1 H52C H 0.5267 -0.0464 0.1402 0.206 Uiso 0.576(15) 1 calc PR E 1 C54 C 0.8886(7) 0.0349(6) 0.5094(6) 0.089(3) Uiso 0.576(15) 1 d P E 1 H54A H 0.9151 -0.0007 0.5512 0.133 Uiso 0.576(15) 1 calc PR E 1 H54B H 0.8747 0.0804 0.5310 0.133 Uiso 0.576(15) 1 calc PR E 1 H54C H 0.9288 0.0463 0.4837 0.133 Uiso 0.576(15) 1 calc PR E 1 C57 C 0.6909(18) 0.2805(9) 0.3115(14) 0.180(11) Uani 0.576(15) 1 d P E 1 H57A H 0.7409 0.3036 0.3039 0.216 Uiso 0.576(15) 1 calc PR E 1 H57B H 0.6393 0.2940 0.2661 0.216 Uiso 0.576(15) 1 calc PR E 1 C58 C 0.6833(12) 0.3117(7) 0.3737(9) 0.112(5) Uani 0.576(15) 1 d P E 1 H58A H 0.6702 0.3644 0.3637 0.168 Uiso 0.576(15) 1 calc PR E 1 H58B H 0.7373 0.3060 0.4182 0.168 Uiso 0.576(15) 1 calc PR E 1 H58C H 0.6367 0.2876 0.3849 0.168 Uiso 0.576(15) 1 calc PR E 1 C52A C 0.4945(10) -0.0068(10) 0.1218(11) 0.089(5) Uani 0.424(15) 1 d P E 2 H52D H 0.4344 -0.0214 0.0952 0.134 Uiso 0.424(15) 1 calc PR E 2 H52E H 0.5304 -0.0511 0.1382 0.134 Uiso 0.424(15) 1 calc PR E 2 H52F H 0.5135 0.0222 0.0864 0.134 Uiso 0.424(15) 1 calc PR E 2 C54A C 0.8404(12) 0.0519(8) 0.5205(9) 0.107(5) Uiso 0.424(15) 1 d P E 2 H54D H 0.8717 0.0222 0.5664 0.160 Uiso 0.424(15) 1 calc PR E 2 H54E H 0.7927 0.0775 0.5285 0.160 Uiso 0.424(15) 1 calc PR E 2 H54F H 0.8793 0.0883 0.5120 0.160 Uiso 0.424(15) 1 calc PR E 2 C57A C 0.7170(7) 0.2811(9) 0.3285(10) 0.054(4) Uani 0.424(15) 1 d P E 2 H57C H 0.7674 0.2882 0.3770 0.065 Uiso 0.424(15) 1 calc PR E 2 H57D H 0.7293 0.3059 0.2861 0.065 Uiso 0.424(15) 1 calc PR E 2 C58A C 0.6359(11) 0.3175(8) 0.3371(11) 0.078(5) Uani 0.424(15) 1 d P E 2 H58D H 0.6471 0.3700 0.3494 0.117 Uiso 0.424(15) 1 calc PR E 2 H58E H 0.6236 0.2929 0.3788 0.117 Uiso 0.424(15) 1 calc PR E 2 H58F H 0.5865 0.3122 0.2884 0.117 Uiso 0.424(15) 1 calc PR E 2 C59 C 0.8049(3) 0.1910(2) 0.2088(2) 0.0586(9) Uani 1 1 d . . . H59A H 0.8404 0.2291 0.2447 0.070 Uiso 1 1 calc R E . H59B H 0.8446 0.1562 0.1977 0.070 Uiso 1 1 calc R . . C60 C 0.7502(3) 0.2287(3) 0.1334(3) 0.0830(14) Uani 1 1 d . E . H60A H 0.7876 0.2544 0.1115 0.125 Uiso 1 1 calc R . . H60B H 0.7117 0.2645 0.1437 0.125 Uiso 1 1 calc R . . H60C H 0.7160 0.1915 0.0966 0.125 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 Rh 0.03270(12) 0.03012(12) 0.02594(11) 0.00188(8) 0.01274(8) 0.00240(9) P1 0.0397(4) 0.0298(4) 0.0280(3) 0.0008(3) 0.0156(3) 0.0014(3) P2 0.0325(4) 0.0314(4) 0.0300(3) 0.0008(3) 0.0105(3) 0.0049(3) C2 0.060(2) 0.0339(16) 0.0375(15) 0.0091(13) 0.0209(14) 0.0062(14) C3 0.0413(16) 0.0445(17) 0.0279(14) 0.0068(12) 0.0141(12) 0.0003(13) C4 0.0489(17) 0.0391(16) 0.0329(14) 0.0032(12) 0.0220(13) 0.0020(13) C5 0.0390(17) 0.059(2) 0.0424(17) 0.0036(15) 0.0214(14) -0.0019(14) C6 0.0412(17) 0.0497(18) 0.0330(15) 0.0054(13) 0.0136(13) -0.0084(14) C7 0.0535(19) 0.0351(15) 0.0351(15) 0.0003(12) 0.0219(14) -0.0052(13) C8 0.063(2) 0.055(2) 0.0415(17) 0.0043(15) 0.0253(16) -0.0125(17) C11 0.0436(16) 0.0348(15) 0.0337(14) -0.0077(12) 0.0204(13) -0.0063(12) C12 0.062(2) 0.050(2) 0.060(2) 0.0118(16) 0.0379(18) 0.0189(17) C13 0.067(3) 0.072(3) 0.084(3) 0.013(2) 0.044(2) 0.027(2) C14 0.047(2) 0.073(3) 0.070(2) -0.010(2) 0.0329(19) 0.0004(18) C15 0.058(2) 0.082(3) 0.054(2) -0.0013(19) 0.0359(19) -0.015(2) C16 0.052(2) 0.068(2) 0.0402(17) 0.0043(16) 0.0209(15) -0.0045(17) C17 0.0457(17) 0.0371(16) 0.0259(13) 0.0006(11) 0.0158(12) -0.0048(12) C18 0.0521(19) 0.0430(17) 0.0413(16) -0.0057(13) 0.0251(15) -0.0049(14) C19 0.077(3) 0.0459(19) 0.051(2) -0.0129(16) 0.0358(19) -0.0180(18) C20 0.069(3) 0.063(2) 0.0398(18) -0.0070(16) 0.0176(17) -0.029(2) C21 0.051(2) 0.067(2) 0.0424(18) 0.0067(17) 0.0061(16) -0.0088(17) C22 0.0477(18) 0.0476(18) 0.0374(16) 0.0042(14) 0.0090(14) 0.0008(14) C23 0.0487(18) 0.0304(15) 0.0385(15) 0.0036(12) 0.0207(14) 0.0031(12) C26 0.092(3) 0.038(2) 0.086(3) 0.012(2) 0.038(3) 0.017(2) C24 0.048(3) 0.041(3) 0.035(2) 0.0006(19) 0.011(2) 0.010(2) C25 0.067(4) 0.037(3) 0.052(3) -0.007(2) 0.015(3) 0.016(2) C27 0.097(4) 0.053(3) 0.048(3) 0.019(2) 0.025(3) 0.019(3) C28 0.078(3) 0.044(2) 0.039(2) 0.0075(17) 0.024(2) 0.016(2) C24A 0.058(19) 0.024(14) 0.045(15) 0.007(11) 0.032(15) 0.021(12) C25A 0.07(2) 0.031(16) 0.053(16) -0.014(13) 0.028(16) -0.004(13) C27A 0.13(3) 0.036(13) 0.054(16) -0.021(11) 0.060(18) -0.034(15) C28A 0.043(13) 0.042(12) 0.032(11) -0.007(9) 0.005(9) 0.011(9) C29 0.0319(14) 0.0427(16) 0.0349(15) 0.0057(12) 0.0119(12) 0.0088(12) C30 0.0382(17) 0.0500(19) 0.0527(19) 0.0072(15) 0.0149(15) 0.0054(14) C31 0.0344(17) 0.068(2) 0.063(2) 0.0118(18) 0.0123(16) 0.0067(16) C32 0.0419(19) 0.068(2) 0.063(2) 0.0240(19) 0.0216(17) 0.0207(17) C33 0.052(2) 0.0462(19) 0.065(2) 0.0172(17) 0.0294(18) 0.0165(16) C34 0.0408(17) 0.0414(17) 0.0507(18) 0.0084(14) 0.0203(14) 0.0088(13) C35 0.0402(16) 0.0371(16) 0.0361(15) -0.0046(12) 0.0163(13) -0.0027(12) C36 0.0445(18) 0.058(2) 0.0341(16) -0.0036(14) 0.0115(14) -0.0012(15) C37 0.059(2) 0.084(3) 0.0334(17) -0.0059(17) 0.0129(16) -0.006(2) C38 0.069(3) 0.074(3) 0.048(2) -0.0229(18) 0.0309(19) -0.013(2) C39 0.058(2) 0.050(2) 0.058(2) -0.0168(16) 0.0283(18) -0.0010(16) C40 0.0425(17) 0.0452(18) 0.0416(17) -0.0058(14) 0.0146(14) 0.0045(14) C41 0.0333(15) 0.0375(16) 0.0363(15) 0.0035(12) 0.0067(12) -0.0010(12) C42 0.054(2) 0.0455(18) 0.0414(17) -0.0035(14) 0.0179(15) -0.0119(15) C43 0.065(2) 0.069(3) 0.0417(18) -0.0016(17) 0.0172(17) -0.0271(19) C44 0.055(2) 0.062(3) 0.068(3) 0.026(2) 0.010(2) -0.0155(19) C45 0.060(2) 0.042(2) 0.119(4) 0.024(2) 0.036(3) 0.0049(17) C46 0.051(2) 0.0385(18) 0.087(3) 0.0101(18) 0.033(2) 0.0060(15) C1 0.107(4) 0.100(4) 0.067(3) -0.004(3) 0.050(3) -0.021(3) B2 0.057(3) 0.103(4) 0.060(3) -0.001(3) 0.030(2) -0.011(3) B3 0.081(3) 0.046(2) 0.053(2) -0.0061(18) 0.033(2) -0.008(2) B4 0.092(4) 0.055(3) 0.045(2) 0.0014(19) 0.030(2) 0.003(2) B5 0.087(3) 0.065(3) 0.046(2) -0.007(2) 0.037(2) -0.007(2) B6 0.064(3) 0.086(4) 0.065(3) 0.006(2) 0.037(2) 0.019(3) B7 0.048(2) 0.060(2) 0.0385(19) -0.0077(17) 0.0169(17) -0.0004(18) B8 0.055(2) 0.051(2) 0.0394(19) -0.0012(16) 0.0142(17) 0.0065(18) B9 0.063(3) 0.071(3) 0.042(2) -0.0138(19) 0.0235(19) -0.013(2) B10 0.098(4) 0.054(3) 0.065(3) 0.003(2) 0.051(3) 0.016(2) B11 0.053(2) 0.083(3) 0.054(2) 0.010(2) 0.027(2) 0.020(2) B12 0.057(2) 0.052(2) 0.043(2) 0.0002(17) 0.0251(18) -0.0008(18) C51 0.065(3) 0.149(6) 0.115(5) -0.008(4) 0.038(3) -0.018(3) C53 0.136(5) 0.081(3) 0.060(3) 0.005(2) 0.025(3) -0.019(3) C55 0.053(2) 0.063(2) 0.052(2) 0.0019(17) 0.0123(17) 0.0007(17) C56 0.079(3) 0.057(2) 0.089(3) 0.006(2) 0.043(3) 0.011(2) C52 0.075(7) 0.097(10) 0.190(18) -0.040(10) -0.009(10) -0.021(7) C57 0.38(3) 0.059(9) 0.215(19) 0.048(10) 0.24(2) 0.070(14) C58 0.139(12) 0.054(6) 0.128(11) -0.036(7) 0.033(9) -0.012(7) C52A 0.065(7) 0.084(10) 0.113(13) -0.025(9) 0.026(8) -0.035(7) C57A 0.035(5) 0.061(8) 0.065(7) -0.030(6) 0.016(4) -0.014(4) C58A 0.101(11) 0.051(6) 0.126(13) 0.009(8) 0.094(10) 0.014(7) C59 0.065(2) 0.058(2) 0.063(2) 0.0031(18) 0.0354(19) 0.0013(18) C60 0.082(3) 0.105(4) 0.077(3) 0.037(3) 0.048(3) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C7 2.173(3) . ? Rh C6 2.194(3) . ? Rh C3 2.210(3) . ? Rh C4 2.221(3) . ? Rh P1 2.3229(7) . ? Rh P2 2.3458(8) . ? P1 C23 1.824(3) . ? P1 C11 1.831(3) . ? P1 C17 1.833(3) . ? P2 C35 1.824(3) . ? P2 C41 1.827(3) . ? P2 C29 1.828(3) . ? C2 C3 1.532(4) . ? C2 C7 1.542(4) . ? C2 C8 1.544(5) . ? C3 C4 1.365(4) . ? C4 C5 1.523(4) . ? C5 C6 1.537(4) . ? C5 C8 1.545(5) . ? C6 C7 1.366(4) . ? C11 C12 1.377(4) . ? C11 C16 1.382(4) . ? C12 C13 1.390(5) . ? C13 C14 1.360(6) . ? C14 C15 1.368(6) . ? C15 C16 1.397(5) . ? C17 C22 1.393(4) . ? C17 C18 1.398(4) . ? C18 C19 1.390(5) . ? C19 C20 1.380(6) . ? C20 C21 1.380(6) . ? C21 C22 1.388(5) . ? C23 C24A 1.32(3) . ? C23 C24 1.379(6) . ? C23 C28A 1.40(2) . ? C23 C28 1.412(5) . ? C26 C25 1.317(7) . ? C26 C27A 1.35(3) . ? C26 C27 1.413(6) . ? C26 C25A 1.58(3) . ? C24 C25 1.390(8) . ? C27 C28 1.382(6) . ? C24A C25A 1.31(4) . ? C27A C28A 1.42(4) . ? C29 C30 1.386(4) . ? C29 C34 1.395(4) . ? C30 C31 1.385(5) . ? C31 C32 1.377(5) . ? C32 C33 1.382(5) . ? C33 C34 1.387(4) . ? C35 C36 1.388(4) . ? C35 C40 1.409(4) . ? C36 C37 1.392(5) . ? C37 C38 1.378(6) . ? C38 C39 1.383(5) . ? C39 C40 1.382(4) . ? C41 C46 1.389(5) . ? C41 C42 1.391(4) . ? C42 C43 1.392(5) . ? C43 C44 1.379(6) . ? C44 C45 1.354(6) . ? C45 C46 1.394(5) . ? C1 B6 1.681(7) . ? C1 B3 1.722(6) . ? C1 B5 1.732(7) . ? C1 B2 1.743(7) . ? C1 B4 1.744(8) . ? B2 C51 1.630(7) . ? B2 B6 1.723(8) . ? B2 B11 1.753(8) . ? B2 B3 1.754(7) . ? B2 B7 1.779(6) . ? B3 B7 1.768(6) . ? B3 B4 1.782(6) . ? B3 B8 1.790(6) . ? B4 C53 1.572(7) . ? B4 B5 1.730(7) . ? B4 B8 1.791(6) . ? B4 B9 1.800(7) . ? B5 B9 1.735(6) . ? B5 B6 1.746(7) . ? B5 B10 1.776(6) . ? B6 B11 1.709(6) . ? B6 B10 1.718(8) . ? B7 B11 1.752(6) . ? B7 B12 1.769(6) . ? B7 B8 1.782(6) . ? B8 C55 1.589(6) . ? B8 B9 1.791(6) . ? B8 B12 1.802(6) . ? B9 B10 1.764(7) . ? B9 B12 1.776(6) . ? B10 C57 1.588(16) . ? B10 C57A 1.623(16) . ? B10 B11 1.766(7) . ? B10 B12 1.804(6) . ? B11 B12 1.767(6) . ? B12 C59 1.605(5) . ? C51 C52 1.333(14) . ? C51 C52A 1.461(17) . ? C53 C54A 1.534(15) . ? C53 C54 1.558(11) . ? C55 C56 1.533(5) . ? C57 C58 1.33(2) . ? C57A C58A 1.57(2) . ? C59 C60 1.522(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Rh C6 36.45(12) . . ? C7 Rh C3 65.92(11) . . ? C6 Rh C3 77.13(11) . . ? C7 Rh C4 76.96(11) . . ? C6 Rh C4 64.81(11) . . ? C3 Rh C4 35.88(11) . . ? C7 Rh P1 98.54(8) . . ? C6 Rh P1 94.67(8) . . ? C3 Rh P1 162.89(8) . . ? C4 Rh P1 151.51(8) . . ? C7 Rh P2 145.87(9) . . ? C6 Rh P2 164.59(8) . . ? C3 Rh P2 91.39(8) . . ? C4 Rh P2 99.88(8) . . ? P1 Rh P2 99.01(3) . . ? C23 P1 C11 109.65(14) . . ? C23 P1 C17 103.55(14) . . ? C11 P1 C17 102.41(13) . . ? C23 P1 Rh 111.36(10) . . ? C11 P1 Rh 116.03(10) . . ? C17 P1 Rh 112.81(9) . . ? C35 P2 C41 104.23(14) . . ? C35 P2 C29 104.39(14) . . ? C41 P2 C29 102.98(14) . . ? C35 P2 Rh 109.52(10) . . ? C41 P2 Rh 123.72(9) . . ? C29 P2 Rh 110.26(10) . . ? C3 C2 C7 101.8(2) . . ? C3 C2 C8 99.8(3) . . ? C7 C2 C8 99.7(3) . . ? C4 C3 C2 106.6(3) . . ? C4 C3 Rh 72.52(16) . . ? C2 C3 Rh 95.35(17) . . ? C3 C4 C5 107.3(3) . . ? C3 C4 Rh 71.60(16) . . ? C5 C4 Rh 96.52(18) . . ? C4 C5 C6 101.3(2) . . ? C4 C5 C8 100.0(3) . . ? C6 C5 C8 99.9(3) . . ? C7 C6 C5 106.8(3) . . ? C7 C6 Rh 70.92(18) . . ? C5 C6 Rh 97.19(19) . . ? C6 C7 C2 106.8(3) . . ? C6 C7 Rh 72.63(18) . . ? C2 C7 Rh 96.53(19) . . ? C2 C8 C5 93.8(2) . . ? C12 C11 C16 118.8(3) . . ? C12 C11 P1 117.0(2) . . ? C16 C11 P1 124.2(3) . . ? C11 C12 C13 120.6(3) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 119.4(3) . . ? C14 C15 C16 120.8(3) . . ? C11 C16 C15 119.8(3) . . ? C22 C17 C18 118.9(3) . . ? C22 C17 P1 120.6(2) . . ? C18 C17 P1 120.3(2) . . ? C19 C18 C17 120.2(3) . . ? C20 C19 C18 120.4(3) . . ? C19 C20 C21 119.7(3) . . ? C20 C21 C22 120.6(4) . . ? C21 C22 C17 120.2(3) . . ? C24A C23 C24 30.9(14) . . ? C24A C23 C28A 121.3(16) . . ? C24 C23 C28A 96.5(9) . . ? C24A C23 C28 114.7(13) . . ? C24 C23 C28 117.0(3) . . ? C28A C23 C28 53.7(8) . . ? C24A C23 P1 111.2(12) . . ? C24 C23 P1 119.9(3) . . ? C28A C23 P1 121.9(9) . . ? C28 C23 P1 122.9(2) . . ? C25 C26 C27A 93.7(12) . . ? C25 C26 C27 120.9(4) . . ? C27A C26 C27 56.0(11) . . ? C25 C26 C25A 26.8(11) . . ? C27A C26 C25A 105.5(18) . . ? C27 C26 C25A 107.5(11) . . ? C23 C24 C25 122.4(5) . . ? C26 C25 C24 119.9(5) . . ? C28 C27 C26 119.4(4) . . ? C27 C28 C23 120.2(4) . . ? C25A C24A C23 118(3) . . ? C24A C25A C26 122(3) . . ? C26 C27A C28A 124(2) . . ? C23 C28A C27A 115.3(19) . . ? C30 C29 C34 119.4(3) . . ? C30 C29 P2 121.1(2) . . ? C34 C29 P2 119.6(2) . . ? C31 C30 C29 120.2(3) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 120.2(3) . . ? C32 C33 C34 120.0(3) . . ? C33 C34 C29 120.0(3) . . ? C36 C35 C40 118.5(3) . . ? C36 C35 P2 123.2(2) . . ? C40 C35 P2 118.2(2) . . ? C35 C36 C37 120.4(3) . . ? C38 C37 C36 120.4(3) . . ? C37 C38 C39 120.0(3) . . ? C40 C39 C38 120.2(3) . . ? C39 C40 C35 120.5(3) . . ? C46 C41 C42 118.5(3) . . ? C46 C41 P2 123.3(3) . . ? C42 C41 P2 118.2(2) . . ? C41 C42 C43 120.4(3) . . ? C44 C43 C42 120.1(4) . . ? C45 C44 C43 119.8(4) . . ? C44 C45 C46 120.9(4) . . ? C41 C46 C45 120.1(4) . . ? B6 C1 B3 108.4(3) . . ? B6 C1 B5 61.5(3) . . ? B3 C1 B5 109.7(3) . . ? B6 C1 B2 60.4(3) . . ? B3 C1 B2 60.8(3) . . ? B5 C1 B2 111.3(4) . . ? B6 C1 B4 109.2(4) . . ? B3 C1 B4 61.9(3) . . ? B5 C1 B4 59.7(3) . . ? B2 C1 B4 111.6(3) . . ? C51 B2 B6 120.5(4) . . ? C51 B2 C1 121.5(4) . . ? B6 B2 C1 58.0(3) . . ? C51 B2 B11 122.1(4) . . ? B6 B2 B11 58.9(3) . . ? C1 B2 B11 105.6(4) . . ? C51 B2 B3 124.7(5) . . ? B6 B2 B3 105.0(3) . . ? C1 B2 B3 59.0(3) . . ? B11 B2 B3 107.2(3) . . ? C51 B2 B7 125.9(4) . . ? B6 B2 B7 105.3(3) . . ? C1 B2 B7 106.0(3) . . ? B11 B2 B7 59.5(2) . . ? B3 B2 B7 60.1(3) . . ? C1 B3 B2 60.2(3) . . ? C1 B3 B7 107.5(3) . . ? B2 B3 B7 60.7(3) . . ? C1 B3 B4 59.7(3) . . ? B2 B3 B4 109.4(3) . . ? B7 B3 B4 108.4(3) . . ? C1 B3 B8 107.4(3) . . ? B2 B3 B8 109.4(3) . . ? B7 B3 B8 60.1(2) . . ? B4 B3 B8 60.2(3) . . ? C53 B4 B5 120.7(4) . . ? C53 B4 C1 122.3(4) . . ? B5 B4 C1 59.8(3) . . ? C53 B4 B3 123.0(4) . . ? B5 B4 B3 107.1(4) . . ? C1 B4 B3 58.4(3) . . ? C53 B4 B8 123.3(4) . . ? B5 B4 B8 107.6(3) . . ? C1 B4 B8 106.3(3) . . ? B3 B4 B8 60.1(2) . . ? C53 B4 B9 123.4(4) . . ? B5 B4 B9 58.8(3) . . ? C1 B4 B9 105.3(3) . . ? B3 B4 B9 106.6(3) . . ? B8 B4 B9 59.8(2) . . ? B4 B5 C1 60.5(3) . . ? B4 B5 B9 62.6(3) . . ? C1 B5 B9 108.8(3) . . ? B4 B5 B6 106.9(3) . . ? C1 B5 B6 57.8(3) . . ? B9 B5 B6 105.8(3) . . ? B4 B5 B10 110.8(3) . . ? C1 B5 B10 106.5(3) . . ? B9 B5 B10 60.3(3) . . ? B6 B5 B10 58.4(3) . . ? C1 B6 B11 110.5(4) . . ? C1 B6 B10 111.6(4) . . ? B11 B6 B10 62.0(3) . . ? C1 B6 B2 61.6(3) . . ? B11 B6 B2 61.4(3) . . ? B10 B6 B2 113.1(3) . . ? C1 B6 B5 60.7(3) . . ? B11 B6 B5 110.9(3) . . ? B10 B6 B5 61.7(3) . . ? B2 B6 B5 111.6(4) . . ? B11 B7 B3 106.6(3) . . ? B11 B7 B12 60.2(3) . . ? B3 B7 B12 109.0(3) . . ? B11 B7 B2 59.5(3) . . ? B3 B7 B2 59.3(3) . . ? B12 B7 B2 108.8(3) . . ? B11 B7 B8 108.3(3) . . ? B3 B7 B8 60.6(2) . . ? B12 B7 B8 61.0(2) . . ? B2 B7 B8 108.6(3) . . ? C55 B8 B7 124.6(3) . . ? C55 B8 B3 122.1(3) . . ? B7 B8 B3 59.3(2) . . ? C55 B8 B9 121.8(3) . . ? B7 B8 B9 106.1(3) . . ? B3 B8 B9 106.6(3) . . ? C55 B8 B4 119.2(3) . . ? B7 B8 B4 107.3(3) . . ? B3 B8 B4 59.7(3) . . ? B9 B8 B4 60.3(2) . . ? C55 B8 B12 124.0(3) . . ? B7 B8 B12 59.1(2) . . ? B3 B8 B12 106.5(3) . . ? B9 B8 B12 59.3(2) . . ? B4 B8 B12 107.9(3) . . ? B5 B9 B10 61.0(3) . . ? B5 B9 B12 109.6(3) . . ? B10 B9 B12 61.2(2) . . ? B5 B9 B8 107.4(3) . . ? B10 B9 B8 109.4(3) . . ? B12 B9 B8 60.7(2) . . ? B5 B9 B4 58.6(3) . . ? B10 B9 B4 108.1(3) . . ? B12 B9 B4 108.7(3) . . ? B8 B9 B4 59.9(2) . . ? C57 B10 C57A 15.5(13) . . ? C57 B10 B6 116.1(10) . . ? C57A B10 B6 127.7(6) . . ? C57 B10 B9 131.9(12) . . ? C57A B10 B9 116.5(6) . . ? B6 B10 B9 105.7(3) . . ? C57 B10 B11 114.6(11) . . ? C57A B10 B11 128.1(7) . . ? B6 B10 B11 58.7(3) . . ? B9 B10 B11 106.6(3) . . ? C57 B10 B5 125.4(8) . . ? C57A B10 B5 119.3(7) . . ? B6 B10 B5 59.9(3) . . ? B9 B10 B5 58.7(3) . . ? B11 B10 B5 107.0(4) . . ? C57 B10 B12 124.4(7) . . ? C57A B10 B12 121.4(7) . . ? B6 B10 B12 105.6(3) . . ? B9 B10 B12 59.7(2) . . ? B11 B10 B12 59.3(2) . . ? B5 B10 B12 106.5(3) . . ? B6 B11 B7 107.1(3) . . ? B6 B11 B2 59.7(3) . . ? B7 B11 B2 61.0(3) . . ? B6 B11 B10 59.3(3) . . ? B7 B11 B10 109.5(3) . . ? B2 B11 B10 109.5(3) . . ? B6 B11 B12 107.6(3) . . ? B7 B11 B12 60.3(2) . . ? B2 B11 B12 110.1(3) . . ? B10 B11 B12 61.4(3) . . ? C59 B12 B11 122.9(3) . . ? C59 B12 B7 123.1(3) . . ? B11 B12 B7 59.4(3) . . ? C59 B12 B9 121.9(3) . . ? B11 B12 B9 106.1(3) . . ? B7 B12 B9 107.3(3) . . ? C59 B12 B8 122.6(3) . . ? B11 B12 B8 106.8(3) . . ? B7 B12 B8 59.9(2) . . ? B9 B12 B8 60.1(2) . . ? C59 B12 B10 121.4(3) . . ? B11 B12 B10 59.3(3) . . ? B7 B12 B10 107.1(3) . . ? B9 B12 B10 59.1(3) . . ? B8 B12 B10 107.2(3) . . ? C52 C51 C52A 43.5(9) . . ? C52 C51 B2 118.3(8) . . ? C52A C51 B2 115.9(7) . . ? C54A C53 C54 36.0(6) . . ? C54A C53 B4 109.5(7) . . ? C54 C53 B4 117.7(5) . . ? C56 C55 B8 115.7(3) . . ? C58 C57 B10 119.2(14) . . ? C58A C57A B10 111.3(10) . . ? C60 C59 B12 115.2(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.645 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.066