# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year 2011 #TrackingRef '4400_web_deposit_cif_file_0_FernandoJ.Lahoz_1298577347.cif' # "Chemistry of eleven-vertex rhodathiaboranes: reactions with # monodentate phosphines" # # # by Beatriz Calvo, Martin Kess, Ramon Macias, Carmen Cunchillos # Fernando J. Lahoz, John D. Kennedy and Luis A. Oro # # Submitted to Dalton Transactions # Manuscript number ........... # ----------------------------------------------------------- # # Person for contact _publ_contact_author_name 'Dr. Fernando J. Lahoz' _publ_contact_author_address ; Dr. Fernando J. Lahoz Departamento de Qu\'imica Inorg\'anica - I.C.M.A. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_phone '+34 976 761147' _publ_contact_author_fax '+34 976 761187' _publ_contact_author_email lahoz@unizar.es _journal_volume ? _journal_page_first ? _journal_page_last ? loop_ _publ_author_name B.Calvo M.Kess R.Macias Cunchillos,C. F.J.Lahoz J.D.Kennedy ; L.A.Oro ; # ---------------------------------------------------------- # Data for compound_8 (local labelling as fjl29e) data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 814662' #TrackingRef '4400_web_deposit_cif_file_0_FernandoJ.Lahoz_1298577347.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_formula_moiety 'C9 H37 B9 P3 Rh S' _chemical_formula_sum 'C9 H37 B9 P3 Rh S' _chemical_formula_weight 470.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0035 0.0018 '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 0.0017 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1093 0.1021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -0.9982 0.9844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1327 0.1336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 16.3060(10) _cell_length_b 15.5790(10) _cell_length_c 17.4840(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4441.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 74697 _cell_measurement_theta_min 2.419 _cell_measurement_theta_max 29.449 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.105 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.049 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; Data were collected in the BM16 line in the ESRF synchrotron, Grenoble (France) ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.73780 _diffrn_radiation_monochromator 'Si 111 double crystal' _diffrn_source synchrotron _diffrn_source_type 'ESRF CRG BM16' _diffrn_measurement_device_type 'Single axis HUBER diffractometer' _diffrn_measurement_method phi-scans _diffrn_measurement_details '1 degree, 1 sec, detector distance 63.50 mm' _diffrn_detector 'CCD plate' _diffrn_detector_type 'ADSC Q210r CCD (binned mode)' _diffrn_detector_area_resol_mean 9.6 _diffrn_reflns_number 74697 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _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 3.55 _diffrn_reflns_theta_max 29.45 _reflns_number_total 5464 _reflns_number_gt 5211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Z. Otwinowski & W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski & W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.10,Bruker2000' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All non-hydrogen atoms, except those involved in disorder (see below), were refined with anisotropic displacement parameters. S(7a), the most abundant sulfur atom, has also refined anisotropically. After anisotropic refinement of a molecular model without disorder, the presence of a relatively low value of the displacement parameter for B(3) atom, together with the presence of a high residual in its close proximity, revealed the existence of a minor molecular static disorder involving a second different coordination of the thioborane to the metal. In fact, a model for the disorder was established assuming the exchange in the positions of the S(7) and B(3) atoms. A complementary occupancy factor was refined, ending with two very different values, 0.916 and 0.083(3). Hydrogen atoms of the terminal methyl groups were included in calculated positions and refined riding on their parent atoms. Hydrogen atoms of the borane cluster were refined from observed positions and refined as free isotropic atoms. ; _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^)+(0.0414P)^2^+4.5417P] 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 SHELXL _refine_ls_extinction_coef 0.0040(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5464 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Rh1 Rh 0.162532(7) 0.157844(7) 0.124406(6) 0.00379(6) Uani 1 1 d . . . P1 P 0.14868(3) 0.11787(3) -0.00762(2) 0.00710(9) Uani 1 1 d . . . P2 P 0.09841(2) 0.29319(3) 0.11304(2) 0.00719(9) Uani 1 1 d . . . P3 P 0.29522(2) 0.20243(3) 0.10975(2) 0.00808(9) Uani 1 1 d . . . C1 C 0.16778(12) 0.00551(12) -0.03120(11) 0.0174(4) Uani 1 1 d . . . H1A H 0.1584 -0.0036 -0.0860 0.026 Uiso 1 1 calc R . . H1B H 0.1305 -0.0311 -0.0017 0.026 Uiso 1 1 calc R . . H1C H 0.2246 -0.0091 -0.0186 0.026 Uiso 1 1 calc R . . C2 C 0.04423(11) 0.13004(12) -0.04361(10) 0.0157(3) Uani 1 1 d . . . H2A H 0.0296 0.1910 -0.0446 0.024 Uiso 1 1 calc R . . H2B H 0.0062 0.0991 -0.0101 0.024 Uiso 1 1 calc R . . H2C H 0.0408 0.1065 -0.0955 0.024 Uiso 1 1 calc R . . C3 C 0.20553(12) 0.16888(12) -0.08509(10) 0.0155(3) Uani 1 1 d . . . H3A H 0.1878 0.1448 -0.1342 0.023 Uiso 1 1 calc R . . H3B H 0.2643 0.1585 -0.0782 0.023 Uiso 1 1 calc R . . H3C H 0.1950 0.2308 -0.0846 0.023 Uiso 1 1 calc R . . C4 C 0.12558(11) 0.37745(11) 0.18100(10) 0.0146(3) Uani 1 1 d . . . H4A H 0.1842 0.3904 0.1766 0.022 Uiso 1 1 calc R . . H4B H 0.1135 0.3580 0.2331 0.022 Uiso 1 1 calc R . . H4C H 0.0936 0.4292 0.1698 0.022 Uiso 1 1 calc R . . C5 C -0.01255(12) 0.28580(13) 0.12876(11) 0.0184(4) Uani 1 1 d . . . H5A H -0.0363 0.3436 0.1290 0.028 Uiso 1 1 calc R . . H5B H -0.0231 0.2579 0.1780 0.028 Uiso 1 1 calc R . . H5C H -0.0375 0.2519 0.0876 0.028 Uiso 1 1 calc R . . C6 C 0.10260(13) 0.35449(12) 0.02490(11) 0.0186(4) Uani 1 1 d . . . H6A H 0.0678 0.4055 0.0297 0.028 Uiso 1 1 calc R . . H6B H 0.0829 0.3189 -0.0175 0.028 Uiso 1 1 calc R . . H6C H 0.1593 0.3721 0.0150 0.028 Uiso 1 1 calc R . . C7 C 0.36402(10) 0.11850(12) 0.07540(11) 0.0161(3) Uani 1 1 d . . . H7A H 0.4206 0.1396 0.0763 0.024 Uiso 1 1 calc R . . H7B H 0.3490 0.1028 0.0230 0.024 Uiso 1 1 calc R . . H7C H 0.3594 0.0680 0.1085 0.024 Uiso 1 1 calc R . . C8 C 0.34861(10) 0.24642(13) 0.19239(11) 0.0155(3) Uani 1 1 d . . . H8A H 0.3472 0.2047 0.2344 0.023 Uiso 1 1 calc R . . H8B H 0.3217 0.2996 0.2086 0.023 Uiso 1 1 calc R . . H8C H 0.4057 0.2586 0.1787 0.023 Uiso 1 1 calc R . . C9 C 0.31535(12) 0.29008(12) 0.04270(11) 0.0183(4) Uani 1 1 d . . . H9A H 0.2900 0.3429 0.0618 0.027 Uiso 1 1 calc R . . H9B H 0.2922 0.2757 -0.0074 0.027 Uiso 1 1 calc R . . H9C H 0.3747 0.2985 0.0378 0.027 Uiso 1 1 calc R . . S7A S 0.04364(4) 0.07355(5) 0.14665(2) 0.00667(15) Uani 0.917(2) 1 d P . . S7B S 0.1727(5) 0.0188(4) 0.1584(3) 0.0067(18) Uiso 0.083(2) 1 d P . . B1 B 0.16578(12) -0.00303(12) 0.26375(11) 0.0119(4) Uani 1 1 d . . . H1 H 0.1981(15) -0.0589(16) 0.2791(14) 0.021(6) Uiso 1 1 d . . . B2 B 0.06659(12) -0.01598(11) 0.22589(11) 0.0116(3) Uani 1 1 d . . . H2 H 0.0400(14) -0.0784(14) 0.2154(14) 0.018(6) Uiso 1 1 d . . . B3A B 0.1558(2) 0.01795(16) 0.16435(15) 0.0077(7) Uiso 0.917(2) 1 d P . . H3 H 0.1729(15) -0.0282(18) 0.1216(13) 0.011(6) Uiso 0.917(2) 1 d P . . B3B B 0.045(3) 0.075(3) 0.129(2) 0.0077(7) Uiso 0.083(2) 1 d P . . B4 B 0.21846(11) 0.08600(12) 0.22324(10) 0.0108(3) Uani 1 1 d . . . H4 H 0.2863(15) 0.0817(15) 0.2255(14) 0.020(6) Uiso 1 1 d . . . B5 B 0.17133(12) 0.09631(12) 0.31493(10) 0.0105(3) Uani 1 1 d . . . H5 H 0.2088(18) 0.0998(18) 0.3682(14) 0.028(7) Uiso 1 1 d . . . B6 B 0.07856(12) 0.03657(12) 0.31401(10) 0.0125(3) Uani 1 1 d . . . H6 H 0.0600(19) 0.0117(19) 0.3695(15) 0.035(8) Uiso 1 1 d . . . B9 B 0.16633(10) 0.18477(12) 0.24985(10) 0.0060(3) Uani 1 1 d . . . H9 H 0.1946(14) 0.2410(15) 0.2660(13) 0.016(5) Uiso 1 1 d . . . H910 H 0.0818(17) 0.1878(19) 0.2449(15) 0.033(7) Uiso 1 1 d . . . B10 B 0.07441(12) 0.14926(12) 0.30593(11) 0.0102(3) Uani 1 1 d . . . H10 H 0.0496(15) 0.1880(15) 0.3522(14) 0.016(5) Uiso 1 1 d . . . B11 B 0.00763(11) 0.08015(12) 0.25068(10) 0.0116(3) Uani 1 1 d . . . H11 H -0.0599(15) 0.0752(14) 0.2575(13) 0.017(6) 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 Rh1 0.00575(8) 0.00311(8) 0.00252(8) -0.00035(4) -0.00045(3) -0.00121(3) P1 0.01187(19) 0.00539(18) 0.00403(18) -0.00042(13) -0.00104(14) -0.00019(14) P2 0.00811(19) 0.00453(18) 0.00894(18) -0.00150(14) -0.00064(14) 0.00187(14) P3 0.00527(18) 0.00643(18) 0.01252(19) -0.00182(14) 0.00022(14) -0.00103(13) C1 0.0339(11) 0.0072(8) 0.0112(8) -0.0043(6) -0.0040(7) 0.0024(7) C2 0.0175(8) 0.0183(9) 0.0114(7) -0.0020(6) -0.0068(6) -0.0006(7) C3 0.0239(9) 0.0156(8) 0.0068(7) 0.0024(6) 0.0040(6) -0.0010(7) C4 0.0223(9) 0.0069(7) 0.0145(8) -0.0048(6) -0.0029(6) 0.0023(6) C5 0.0139(8) 0.0159(9) 0.0254(10) 0.0003(7) 0.0009(7) 0.0028(7) C6 0.0311(10) 0.0114(8) 0.0133(8) 0.0038(6) -0.0006(7) 0.0043(7) C7 0.0103(7) 0.0168(8) 0.0213(9) -0.0066(7) -0.0008(7) 0.0046(6) C8 0.0097(7) 0.0156(8) 0.0213(9) -0.0072(7) -0.0043(6) -0.0023(6) C9 0.0188(9) 0.0135(8) 0.0227(9) 0.0017(7) 0.0048(7) -0.0072(7) S7A 0.0082(2) 0.0062(2) 0.0056(3) 0.0004(2) -0.0003(2) -0.00195(14) B1 0.0207(10) 0.0076(8) 0.0074(8) 0.0019(7) -0.0002(6) 0.0025(6) B2 0.0188(9) 0.0063(8) 0.0097(8) 0.0028(6) 0.0012(7) -0.0032(6) B4 0.0126(8) 0.0108(8) 0.0091(8) 0.0010(6) -0.0023(6) 0.0016(6) B5 0.0157(8) 0.0101(8) 0.0056(8) -0.0003(6) -0.0010(6) 0.0026(6) B6 0.0202(9) 0.0096(8) 0.0076(8) 0.0024(6) 0.0022(7) -0.0017(7) B9 0.0086(7) 0.0067(8) 0.0026(7) -0.0007(6) -0.0009(5) -0.0006(6) B10 0.0124(8) 0.0114(8) 0.0066(8) -0.0011(6) 0.0023(6) -0.0001(6) B11 0.0134(8) 0.0119(8) 0.0095(8) 0.0004(7) 0.0037(6) -0.0033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 B9 2.2339(17) . ? Rh1 B4 2.2517(18) . ? Rh1 S7B 2.252(6) . ? Rh1 P3 2.2869(4) . ? Rh1 B3A 2.291(3) . ? Rh1 B3B 2.31(5) . ? Rh1 P2 2.3619(4) . ? Rh1 S7A 2.3736(7) . ? Rh1 P1 2.4016(4) . ? P1 C3 1.8235(18) . ? P1 C1 1.8252(18) . ? P1 C2 1.8254(18) . ? P2 C6 1.8143(18) . ? P2 C4 1.8251(17) . ? P2 C5 1.834(2) . ? P3 C8 1.8207(18) . ? P3 C7 1.8245(17) . ? P3 C9 1.8293(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? S7A B11 1.9140(19) . ? S7A B2 2.0012(19) . ? S7A B3A 2.047(3) . ? S7B B4 1.713(6) . ? S7B B1 1.876(6) . ? S7B B2 2.163(8) . ? S7B B3B 2.32(5) . ? S7B H3 0.98(3) . ? B1 B2 1.759(3) . ? B1 B3A 1.776(3) . ? B1 B4 1.779(3) . ? B1 B6 1.782(3) . ? B1 B5 1.790(3) . ? B1 H1 1.05(2) . ? B2 B6 1.756(3) . ? B2 B11 1.832(3) . ? B2 B3A 1.885(4) . ? B2 H2 1.08(2) . ? B3A B4 1.797(3) . ? B3A H3 1.07(3) . ? B4 B5 1.785(3) . ? B4 B9 1.818(3) . ? B4 H4 1.11(2) . ? B5 B6 1.776(3) . ? B5 B9 1.789(3) . ? B5 B10 1.790(3) . ? B5 H5 1.12(3) . ? B6 B11 1.739(3) . ? B6 B10 1.762(3) . ? B6 H6 1.09(3) . ? B9 B10 1.875(3) . ? B9 H9 1.03(2) . ? B9 H910 1.38(3) . ? B10 B11 1.811(3) . ? B10 H910 1.23(3) . ? B10 H10 1.09(2) . ? B11 H11 1.11(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B9 Rh1 B4 47.83(7) . . ? B9 Rh1 S7B 85.36(16) . . ? B4 Rh1 S7B 44.71(16) . . ? B9 Rh1 P3 91.53(4) . . ? B4 Rh1 P3 81.59(5) . . ? S7B Rh1 P3 104.6(2) . . ? B9 Rh1 B3A 83.15(8) . . ? B4 Rh1 B3A 46.58(8) . . ? S7B Rh1 B3A 7.38(18) . . ? P3 Rh1 B3A 111.62(8) . . ? B9 Rh1 B3B 95.4(10) . . ? B4 Rh1 B3B 91.9(11) . . ? S7B Rh1 B3B 61.1(12) . . ? P3 Rh1 B3B 163.3(12) . . ? B3A Rh1 B3B 54.5(12) . . ? B9 Rh1 P2 85.83(5) . . ? B4 Rh1 P2 133.44(5) . . ? S7B Rh1 P2 156.0(2) . . ? P3 Rh1 P2 97.946(15) . . ? B3A Rh1 P2 148.61(8) . . ? B3B Rh1 P2 97.7(12) . . ? B9 Rh1 S7A 88.04(4) . . ? B4 Rh1 S7A 85.99(5) . . ? S7B Rh1 S7A 59.0(2) . . ? P3 Rh1 S7A 163.57(2) . . ? B3A Rh1 S7A 52.02(8) . . ? B3B Rh1 S7A 7.5(10) . . ? P2 Rh1 S7A 98.40(2) . . ? B9 Rh1 P1 174.29(5) . . ? B4 Rh1 P1 130.31(5) . . ? S7B Rh1 P1 90.66(15) . . ? P3 Rh1 P1 93.443(15) . . ? B3A Rh1 P1 92.40(7) . . ? B3B Rh1 P1 79.0(10) . . ? P2 Rh1 P1 96.256(14) . . ? S7A Rh1 P1 86.400(15) . . ? C3 P1 C1 99.41(9) . . ? C3 P1 C2 99.96(9) . . ? C1 P1 C2 100.42(9) . . ? C3 P1 Rh1 123.58(6) . . ? C1 P1 Rh1 116.73(6) . . ? C2 P1 Rh1 113.09(6) . . ? C6 P2 C4 99.51(9) . . ? C6 P2 C5 101.38(9) . . ? C4 P2 C5 100.78(9) . . ? C6 P2 Rh1 121.65(6) . . ? C4 P2 Rh1 118.68(6) . . ? C5 P2 Rh1 111.61(7) . . ? C8 P3 C7 103.71(8) . . ? C8 P3 C9 98.15(9) . . ? C7 P3 C9 102.34(9) . . ? C8 P3 Rh1 118.54(6) . . ? C7 P3 Rh1 113.64(6) . . ? C9 P3 Rh1 117.92(7) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? B11 S7A B2 55.74(8) . . ? B11 S7A B3A 98.81(10) . . ? B2 S7A B3A 55.49(10) . . ? B11 S7A Rh1 112.12(6) . . ? B2 S7A Rh1 110.26(6) . . ? B3A S7A Rh1 61.91(8) . . ? B4 S7B B1 59.2(2) . . ? B4 S7B B2 98.1(3) . . ? B1 S7B B2 51.0(2) . . ? B4 S7B Rh1 67.6(2) . . ? B1 S7B Rh1 115.4(3) . . ? B2 S7B Rh1 109.0(3) . . ? B4 S7B B3B 107.9(12) . . ? B1 S7B B3B 103.5(10) . . ? B2 S7B B3B 59.9(11) . . ? Rh1 S7B B3B 60.7(12) . . ? B4 S7B H3 153.4(16) . . ? B1 S7B H3 120.8(15) . . ? B2 S7B H3 100.0(16) . . ? Rh1 S7B H3 123.2(15) . . ? B3B S7B H3 98.0(19) . . ? B2 B1 B3A 64.44(14) . . ? B2 B1 B4 112.56(13) . . ? B3A B1 B4 60.72(13) . . ? B2 B1 B6 59.44(11) . . ? B3A B1 B6 110.23(16) . . ? B4 B1 B6 108.17(13) . . ? B2 B1 B5 109.50(13) . . ? B3A B1 B5 109.55(14) . . ? B4 B1 B5 60.03(11) . . ? B6 B1 B5 59.63(11) . . ? B2 B1 S7B 73.0(3) . . ? B4 B1 S7B 55.8(2) . . ? B6 B1 S7B 118.0(3) . . ? B5 B1 S7B 109.3(2) . . ? B2 B1 H1 117.5(13) . . ? B3A B1 H1 116.6(14) . . ? B4 B1 H1 120.3(13) . . ? B6 B1 H1 124.1(14) . . ? B5 B1 H1 124.2(14) . . ? S7B B1 H1 111.7(14) . . ? B6 B2 B1 60.93(11) . . ? B6 B2 B11 57.95(10) . . ? B1 B2 B11 107.44(13) . . ? B6 B2 B3A 106.52(14) . . ? B1 B2 B3A 58.20(12) . . ? B11 B2 B3A 108.11(13) . . ? B6 B2 S7A 107.66(11) . . ? B1 B2 S7A 110.64(11) . . ? B11 B2 S7A 59.72(8) . . ? B3A B2 S7A 63.49(10) . . ? B6 B2 S7B 105.82(19) . . ? B1 B2 S7B 56.00(18) . . ? B11 B2 S7B 110.12(19) . . ? S7A B2 S7B 66.27(17) . . ? B6 B2 H2 127.8(13) . . ? B1 B2 H2 122.4(12) . . ? B11 B2 H2 124.5(12) . . ? B3A B2 H2 117.7(13) . . ? S7A B2 H2 115.8(13) . . ? S7B B2 H2 117.0(13) . . ? B1 B3A B4 59.71(12) . . ? B1 B3A B2 57.35(12) . . ? B4 B3A B2 106.10(16) . . ? B1 B3A S7A 107.92(17) . . ? B4 B3A S7A 110.18(14) . . ? B2 B3A S7A 61.02(12) . . ? B1 B3A Rh1 117.97(14) . . ? B4 B3A Rh1 65.55(10) . . ? B2 B3A Rh1 118.54(15) . . ? S7A B3A Rh1 66.06(8) . . ? B1 B3A H3 122.3(14) . . ? B4 B3A H3 130.3(14) . . ? B2 B3A H3 114.2(14) . . ? S7A B3A H3 114.2(13) . . ? Rh1 B3A H3 114.4(14) . . ? Rh1 B3B S7B 58.2(12) . . ? S7B B4 B1 65.0(2) . . ? S7B B4 B5 117.5(3) . . ? B1 B4 B5 60.30(11) . . ? B1 B4 B3A 59.56(12) . . ? B5 B4 B3A 108.84(15) . . ? S7B B4 B9 118.9(3) . . ? B1 B4 B9 109.41(13) . . ? B5 B4 B9 59.53(10) . . ? B3A B4 B9 112.34(14) . . ? S7B B4 Rh1 67.7(2) . . ? B1 B4 Rh1 119.84(11) . . ? B5 B4 Rh1 118.04(11) . . ? B3A B4 Rh1 67.86(10) . . ? B9 B4 Rh1 65.57(8) . . ? S7B B4 H4 114.9(13) . . ? B1 B4 H4 114.8(12) . . ? B5 B4 H4 113.7(13) . . ? B3A B4 H4 123.5(12) . . ? B9 B4 H4 120.6(12) . . ? Rh1 B4 H4 117.5(13) . . ? B6 B5 B4 108.15(13) . . ? B6 B5 B9 111.05(13) . . ? B4 B5 B9 61.17(10) . . ? B6 B5 B10 59.24(11) . . ? B4 B5 B10 110.04(13) . . ? B9 B5 B10 63.18(10) . . ? B6 B5 B1 59.96(11) . . ? B4 B5 B1 59.67(10) . . ? B9 B5 B1 110.23(13) . . ? B10 B5 B1 108.06(13) . . ? B6 B5 H5 120.0(14) . . ? B4 B5 H5 121.2(15) . . ? B9 B5 H5 121.2(15) . . ? B10 B5 H5 122.3(15) . . ? B1 B5 H5 119.2(15) . . ? B11 B6 B2 63.22(11) . . ? B11 B6 B10 62.27(11) . . ? B2 B6 B10 112.95(13) . . ? B11 B6 B5 111.57(13) . . ? B2 B6 B5 110.30(13) . . ? B10 B6 B5 60.76(11) . . ? B11 B6 B1 110.60(13) . . ? B2 B6 B1 59.63(11) . . ? B10 B6 B1 109.63(13) . . ? B5 B6 B1 60.40(11) . . ? B11 B6 H6 121.5(16) . . ? B2 B6 H6 125.8(16) . . ? B10 B6 H6 114.6(16) . . ? B5 B6 H6 114.6(16) . . ? B1 B6 H6 122.6(16) . . ? B5 B9 B4 59.31(10) . . ? B5 B9 B10 58.42(10) . . ? B4 B9 B10 104.94(12) . . ? B5 B9 Rh1 118.75(11) . . ? B4 B9 Rh1 66.60(8) . . ? B10 B9 Rh1 115.84(10) . . ? B5 B9 H9 117.4(13) . . ? B4 B9 H9 125.5(13) . . ? B10 B9 H9 117.7(13) . . ? Rh1 B9 H9 116.2(13) . . ? B5 B9 H910 96.4(12) . . ? B4 B9 H910 118.6(12) . . ? Rh1 B9 H910 85.3(11) . . ? H9 B9 H910 115.8(17) . . ? B6 B10 B5 60.00(11) . . ? B6 B10 B11 58.24(11) . . ? B5 B10 B11 107.70(13) . . ? B6 B10 B9 107.77(13) . . ? B5 B10 B9 58.40(10) . . ? B11 B10 B9 112.17(12) . . ? B6 B10 H910 123.5(14) . . ? B5 B10 H910 102.4(13) . . ? B11 B10 H910 83.5(13) . . ? B9 B10 H910 47.4(13) . . ? B6 B10 H10 120.5(13) . . ? B5 B10 H10 121.3(13) . . ? B11 B10 H10 120.2(13) . . ? B9 B10 H10 121.5(13) . . ? H910 B10 H10 114.2(18) . . ? B6 B11 B10 59.49(11) . . ? B6 B11 B2 58.83(11) . . ? B10 B11 B2 107.26(13) . . ? B6 B11 S7A 112.33(12) . . ? B10 B11 S7A 110.76(11) . . ? B2 B11 S7A 64.54(9) . . ? B6 B11 H11 124.3(12) . . ? B10 B11 H11 125.5(12) . . ? B2 B11 H11 119.3(12) . . ? S7A B11 H11 113.8(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.786 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.090 # ---------------------------------------------------------- # Data for compound_9 (local labelling as fjl31es) data_compound_9 _database_code_depnum_ccdc_archive 'CCDC 814663' #TrackingRef '4400_web_deposit_cif_file_0_FernandoJ.Lahoz_1298577347.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_formula_moiety 'C39 H49 B9 P3 Rh S, 0.5 (C6 H14)' _chemical_formula_sum 'C42 H56 B9 P3 Rh S' _chemical_formula_weight 886.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0035 0.0018 '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 0.0017 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1093 0.1021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -0.9982 0.9844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1327 0.1336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4960(10) _cell_length_b 12.6030(10) _cell_length_c 17.1240(10) _cell_angle_alpha 75.9350(10) _cell_angle_beta 82.6070(10) _cell_angle_gamma 65.0700(10) _cell_volume 2181.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 43398 _cell_measurement_theta_min 1.892 _cell_measurement_theta_max 33.304 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9446 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995) A51, 33-38 ; _exptl_special_details ; Data were collected at the BM16 line in the ESRF ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.73780 _diffrn_radiation_monochromator 'Si 111 double crystal' _diffrn_source synchrotron _diffrn_source_type 'ESRF CRG BM16' _diffrn_measurement_device_type 'Single axis HUBER diffractometer' _diffrn_measurement_method phi-scans _diffrn_measurement_details '1 degree, 1 sec, detector distance 63.50 mm' _diffrn_detector 'CCD plate' _diffrn_detector_type 'ADSC Q210r CCD (binned mode)' _diffrn_detector_area_resol_mean 9.6 _diffrn_reflns_number 43398 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 33.30 _reflns_number_total 11291 _reflns_number_gt 10602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Z. Otwinowski & W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski & W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.10,Bruker2000' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters, except those atoms of the disordered phenyl ring and those of the highly disordered solvent molecule. All hydrogen atoms of the phenyl rings were included in calculated positions and refined riding on their carbon parent atoms. Those of the borane cluster has been included from the difference Fourier maps and refined as free iso- tropic atoms. The hydride ligand was also included from observed positions. At this point, we observed several residual peaks of high intensity clearly far away of the metal complex. We interpreted these residuals as part of a highly disordered solvent molecule. We hardly tried to model this molecule bearing in mind the solvents used in the crystallization process (CH2Cl2 and hexane) with no success. We carried out an estimation of the residual electron density in this solvent region running the squeeze program; a total of 17e/cell was estimated. We assumed that this region was occupated by half an hexane molecule (18e due to the carbon atoms) and we decided to include the highest intensity residual peaks to account for the disordered electron density of the solvent molecule. The occupancy factors of these peaks were refined to give similar thermal parameters; constraining the sum of their occupancies to be 3 carbon atoms. At the end of the refinement only one peak over 1e/A3 was observed in the difference Fourier map (1.28 e/A3), localized in the region of the disordered solvent ; _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^)+(0.0688P)^2^+1.7632P] 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 SHELXL _refine_ls_extinction_coef 0.0382(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11291 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.883377(12) 0.297537(12) 0.705621(8) 0.01380(7) Uani 1 1 d . . . H1H H 0.850(3) 0.216(3) 0.7818(19) 0.038(8) Uiso 1 1 d . . . S7 S 0.92971(5) 0.43507(4) 0.59410(3) 0.01992(11) Uani 1 1 d . . . P1 P 1.07053(5) 0.22497(5) 0.77587(3) 0.02150(11) Uani 1 1 d . A . P2 P 0.93138(5) 0.14891(4) 0.63432(3) 0.01466(10) Uani 1 1 d . . . P3 P 0.55293(5) 0.32336(4) 0.70281(3) 0.01575(10) Uani 1 1 d . . . C1 C 1.1991(2) 0.2641(3) 0.72097(17) 0.0344(5) Uani 1 1 d . . . H1A H 1.218(3) 0.237(3) 0.676(2) 0.040(9) Uiso 1 1 d . . . H1B H 1.275(3) 0.233(3) 0.751(2) 0.043(9) Uiso 1 1 d . . . H1C H 1.166(3) 0.347(3) 0.7101(19) 0.036(8) Uiso 1 1 d . . . C2 C 1.1469(3) 0.0635(2) 0.81497(17) 0.0389(6) Uani 1 1 d . . . C3A C 1.1083(7) 0.0060(6) 0.8681(4) 0.0272(13) Uiso 0.422(9) 1 d P A 1 H3A H 1.0303 0.0495 0.8939 0.033 Uiso 0.422(9) 1 calc PR A 1 C4A C 1.1621(8) -0.1169(7) 0.8977(4) 0.0345(15) Uiso 0.422(9) 1 d P A 1 H4A H 1.1230 -0.1545 0.9412 0.041 Uiso 0.422(9) 1 calc PR A 1 C5A C 1.2760(8) -0.1819(7) 0.8604(5) 0.0400(17) Uiso 0.422(9) 1 d P A 1 H5A H 1.3141 -0.2666 0.8767 0.048 Uiso 0.422(9) 1 calc PR A 1 C6A C 1.3349(8) -0.1248(7) 0.7997(5) 0.0420(18) Uiso 0.422(9) 1 d P A 1 H6A H 1.4149 -0.1706 0.7768 0.050 Uiso 0.422(9) 1 calc PR A 1 C7A C 1.2786(7) -0.0016(6) 0.7720(4) 0.0315(14) Uiso 0.422(9) 1 d P A 1 H7A H 1.3166 0.0398 0.7304 0.038 Uiso 0.422(9) 1 calc PR A 1 C3B C 1.0733(5) 0.0173(4) 0.8870(3) 0.0259(9) Uiso 0.578(9) 1 d P A 2 H3B H 0.9995 0.0716 0.9103 0.031 Uiso 0.578(9) 1 calc PR A 2 C4B C 1.1166(6) -0.1049(5) 0.9173(3) 0.0365(11) Uiso 0.578(9) 1 d P A 2 H4B H 1.0724 -0.1359 0.9612 0.044 Uiso 0.578(9) 1 calc PR A 2 C5B C 1.2256(6) -0.1813(5) 0.8824(3) 0.0430(13) Uiso 0.578(9) 1 d P A 2 H5B H 1.2555 -0.2649 0.9037 0.052 Uiso 0.578(9) 1 calc PR A 2 C6B C 1.2923(6) -0.1407(5) 0.8180(4) 0.0432(13) Uiso 0.578(9) 1 d P A 2 H6B H 1.3673 -0.1945 0.7953 0.052 Uiso 0.578(9) 1 calc PR A 2 C7B C 1.2451(6) -0.0171(5) 0.7875(3) 0.0355(11) Uiso 0.578(9) 1 d P A 2 H7B H 1.2898 0.0099 0.7420 0.043 Uiso 0.578(9) 1 calc PR A 2 C8 C 1.0588(2) 0.2754(2) 0.86994(13) 0.0264(4) Uani 1 1 d . . . C9 C 1.1694(3) 0.2508(3) 0.90855(17) 0.0423(6) Uani 1 1 d . A . H9 H 1.2513 0.2088 0.8860 0.051 Uiso 1 1 calc R . . C10 C 1.1599(4) 0.2880(3) 0.98041(19) 0.0514(8) Uani 1 1 d . . . H10 H 1.2358 0.2714 1.0064 0.062 Uiso 1 1 calc R A . C11 C 1.0416(4) 0.3487(2) 1.01413(16) 0.0454(8) Uani 1 1 d . A . H11 H 1.0359 0.3738 1.0630 0.054 Uiso 1 1 calc R . . C12 C 0.9324(4) 0.3724(3) 0.97658(17) 0.0499(8) Uani 1 1 d . . . H12 H 0.8506 0.4135 0.9998 0.060 Uiso 1 1 calc R A . C13 C 0.9409(3) 0.3362(3) 0.90395(16) 0.0404(6) Uani 1 1 d . A . H13 H 0.8647 0.3538 0.8780 0.049 Uiso 1 1 calc R . . C14 C 0.8717(2) 0.20780(19) 0.53147(12) 0.0219(4) Uani 1 1 d . . . H14A H 0.903(3) 0.267(3) 0.5073(17) 0.030(7) Uiso 1 1 d . . . H14B H 0.909(3) 0.143(3) 0.5004(18) 0.031(7) Uiso 1 1 d . . . H14C H 0.781(3) 0.240(3) 0.5317(16) 0.024(7) Uiso 1 1 d . . . C15 C 1.10080(19) 0.06540(18) 0.60868(11) 0.0186(3) Uani 1 1 d . . . C16 C 1.1629(2) -0.05920(19) 0.62660(12) 0.0224(4) Uani 1 1 d . . . H16 H 1.1175 -0.1058 0.6545 0.027 Uiso 1 1 calc R . . C17 C 1.2914(2) -0.1154(2) 0.60359(15) 0.0298(5) Uani 1 1 d . . . H17 H 1.3337 -0.2003 0.6158 0.036 Uiso 1 1 calc R . . C18 C 1.3575(2) -0.0473(2) 0.56286(17) 0.0370(6) Uani 1 1 d . . . H18 H 1.4451 -0.0858 0.5474 0.044 Uiso 1 1 calc R . . C19 C 1.2967(2) 0.0762(2) 0.54466(16) 0.0346(5) Uani 1 1 d . . . H19 H 1.3424 0.1224 0.5166 0.042 Uiso 1 1 calc R . . C20 C 1.1691(2) 0.13231(19) 0.56740(13) 0.0239(4) Uani 1 1 d . . . H20 H 1.1276 0.2172 0.5548 0.029 Uiso 1 1 calc R . . C21 C 0.87723(18) 0.02949(17) 0.67524(11) 0.0171(3) Uani 1 1 d . . . C22 C 0.8319(2) -0.02043(19) 0.62806(13) 0.0241(4) Uani 1 1 d . . . H22 H 0.8241 0.0106 0.5717 0.029 Uiso 1 1 calc R . . C23 C 0.7980(2) -0.1156(2) 0.66370(15) 0.0298(5) Uani 1 1 d . . . H23 H 0.7648 -0.1479 0.6318 0.036 Uiso 1 1 calc R . . C24 C 0.8128(2) -0.1635(2) 0.74565(15) 0.0288(5) Uani 1 1 d . . . H24 H 0.7915 -0.2297 0.7695 0.035 Uiso 1 1 calc R . . C25 C 0.8582(2) -0.11513(19) 0.79259(13) 0.0257(4) Uani 1 1 d . . . H25 H 0.8687 -0.1483 0.8486 0.031 Uiso 1 1 calc R . . C26 C 0.8887(2) -0.01782(18) 0.75779(12) 0.0207(4) Uani 1 1 d . . . H26 H 0.9175 0.0167 0.7906 0.025 Uiso 1 1 calc R . . C27 C 0.5367(2) 0.2653(2) 0.61994(12) 0.0222(4) Uani 1 1 d . . . H27A H 0.528(3) 0.325(3) 0.5696(19) 0.037(8) Uiso 1 1 d . . . H27B H 0.608(3) 0.187(3) 0.6206(16) 0.022(6) Uiso 1 1 d . . . H27C H 0.460(3) 0.255(3) 0.628(2) 0.044(9) Uiso 1 1 d . . . C28 C 0.58437(19) 0.20336(18) 0.79110(12) 0.0197(4) Uani 1 1 d . . . C29 C 0.5470(2) 0.11014(19) 0.79500(14) 0.0249(4) Uani 1 1 d . . . H29 H 0.5115 0.1056 0.7494 0.030 Uiso 1 1 calc R . . C30 C 0.5618(2) 0.0241(2) 0.86568(16) 0.0343(5) Uani 1 1 d . . . H30 H 0.5348 -0.0384 0.8686 0.041 Uiso 1 1 calc R . . C31 C 0.6153(2) 0.0287(3) 0.93131(15) 0.0384(6) Uani 1 1 d . . . H31 H 0.6261 -0.0311 0.9792 0.046 Uiso 1 1 calc R . . C32 C 0.6533(2) 0.1201(3) 0.92800(14) 0.0352(5) Uani 1 1 d . . . H32 H 0.6903 0.1229 0.9736 0.042 Uiso 1 1 calc R . . C33 C 0.6375(2) 0.2084(2) 0.85796(13) 0.0265(4) Uani 1 1 d . . . H33 H 0.6630 0.2716 0.8559 0.032 Uiso 1 1 calc R . . C34 C 0.39253(18) 0.43030(18) 0.72247(12) 0.0192(4) Uani 1 1 d . . . C35 C 0.3498(2) 0.4419(2) 0.80048(14) 0.0318(5) Uani 1 1 d . . . H35 H 0.4038 0.3920 0.8442 0.038 Uiso 1 1 calc R . . C36 C 0.2286(3) 0.5259(3) 0.81524(17) 0.0440(7) Uani 1 1 d . . . H36 H 0.1998 0.5332 0.8690 0.053 Uiso 1 1 calc R . . C37 C 0.1495(2) 0.5990(3) 0.75215(17) 0.0382(6) Uani 1 1 d . . . H37 H 0.0666 0.6568 0.7624 0.046 Uiso 1 1 calc R . . C38 C 0.1912(2) 0.5877(3) 0.67452(16) 0.0369(6) Uani 1 1 d . . . H38 H 0.1364 0.6372 0.6311 0.044 Uiso 1 1 calc R . . C39 C 0.3127(2) 0.5045(2) 0.65904(14) 0.0291(5) Uani 1 1 d . . . H39 H 0.3413 0.4982 0.6051 0.035 Uiso 1 1 calc R . . B1 B 0.7154(3) 0.6017(2) 0.69164(19) 0.0313(6) Uani 1 1 d . . . H1D H 0.696(3) 0.669(3) 0.726(2) 0.049(9) Uiso 1 1 d . . . B2 B 0.8215(2) 0.5996(2) 0.60733(19) 0.0298(5) Uani 1 1 d . . . H2D H 0.867(3) 0.660(3) 0.5909(19) 0.041(9) Uiso 1 1 d . . . B3 B 0.8680(2) 0.4809(2) 0.70453(15) 0.0232(4) Uani 1 1 d . . . H3D H 0.943(3) 0.485(3) 0.7383(18) 0.032(8) Uiso 1 1 d . . . B4 B 0.7259(2) 0.4555(2) 0.74350(15) 0.0214(4) Uani 1 1 d . . . H4D H 0.700(3) 0.448(3) 0.8058(16) 0.024(7) Uiso 1 1 d . . . B5 B 0.5995(2) 0.5519(2) 0.67448(18) 0.0275(5) Uani 1 1 d . . . H5D H 0.505(3) 0.590(3) 0.6986(17) 0.027(7) Uiso 1 1 d . . . B6 B 0.6606(3) 0.6320(2) 0.5927(2) 0.0338(6) Uani 1 1 d . . . H6D H 0.599(3) 0.716(3) 0.557(2) 0.043(9) Uiso 1 1 d . . . B9 B 0.6772(2) 0.39487(19) 0.67710(13) 0.0176(4) Uani 1 1 d . . . H910 H 0.714(3) 0.397(3) 0.6039(16) 0.026(7) Uiso 1 1 d . . . B10 B 0.6369(2) 0.5076(2) 0.57981(16) 0.0257(5) Uani 1 1 d . . . H10D H 0.558(3) 0.521(3) 0.5448(18) 0.034(8) Uiso 1 1 d . . . B11 B 0.7749(2) 0.5367(2) 0.53561(16) 0.0278(5) Uani 1 1 d . . . H11D H 0.794(3) 0.560(3) 0.4705(19) 0.036(8) Uiso 1 1 d . . . C91 C 0.5366(9) 0.5278(14) 0.9595(6) 0.034(3) Uiso 0.34(3) 1 d P . . C92 C 0.5493(5) 0.4822(9) 0.9742(4) 0.0658(16) Uiso 0.99(3) 1 d P . . C93 C 0.5737(5) 0.6195(5) 0.9666(3) 0.0661(17) Uiso 0.872(15) 1 d P . . C94 C 0.6339(6) 0.6654(6) 0.8928(3) 0.0400(18) Uiso 0.494(12) 1 d P . . C95 C 0.5503(4) 0.7061(4) 0.9660(3) 0.0309(14) Uiso 0.544(12) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.01178(9) 0.00851(9) 0.01994(9) -0.00235(5) 0.00194(5) -0.00402(7) S7 0.0142(2) 0.0121(2) 0.0293(2) 0.00161(16) 0.00280(16) -0.0055(2) P1 0.0198(2) 0.0152(3) 0.0286(3) -0.00376(18) -0.00495(19) -0.0056(2) P2 0.0144(2) 0.0095(2) 0.0177(2) -0.00183(15) 0.00250(15) -0.0039(2) P3 0.0122(2) 0.0119(2) 0.0212(2) -0.00014(16) 0.00145(15) -0.0053(2) C1 0.0173(10) 0.0457(17) 0.0437(14) -0.0152(11) 0.0011(9) -0.0136(12) C2 0.0456(15) 0.0167(12) 0.0487(14) -0.0043(9) -0.0313(12) -0.0001(12) C8 0.0376(12) 0.0190(10) 0.0259(9) 0.0001(7) -0.0087(8) -0.0150(10) C9 0.0461(16) 0.0449(17) 0.0419(14) -0.0074(11) -0.0160(11) -0.0210(14) C10 0.073(2) 0.0493(19) 0.0431(15) -0.0012(13) -0.0274(15) -0.0335(19) C11 0.088(2) 0.0245(13) 0.0291(12) 0.0006(9) -0.0177(13) -0.0265(16) C12 0.067(2) 0.0456(18) 0.0336(13) -0.0181(12) -0.0064(13) -0.0128(17) C13 0.0477(16) 0.0449(17) 0.0305(12) -0.0157(11) -0.0054(10) -0.0150(14) C14 0.0241(10) 0.0190(10) 0.0195(8) -0.0015(7) -0.0004(7) -0.0073(9) C15 0.0160(8) 0.0151(10) 0.0208(8) -0.0045(6) 0.0053(6) -0.0037(8) C16 0.0218(9) 0.0147(10) 0.0266(9) -0.0040(7) 0.0042(7) -0.0051(9) C17 0.0239(11) 0.0162(11) 0.0390(12) -0.0058(8) 0.0052(9) 0.0002(10) C18 0.0196(10) 0.0260(14) 0.0520(15) -0.0076(10) 0.0134(9) -0.0010(11) C19 0.0229(11) 0.0253(13) 0.0467(13) -0.0047(10) 0.0166(9) -0.0077(11) C20 0.0193(9) 0.0148(10) 0.0309(10) -0.0029(7) 0.0081(7) -0.0042(9) C21 0.0158(8) 0.0098(9) 0.0239(8) -0.0045(6) 0.0042(6) -0.0043(8) C22 0.0288(11) 0.0171(10) 0.0285(10) -0.0076(7) 0.0027(8) -0.0108(10) C23 0.0330(12) 0.0199(11) 0.0427(12) -0.0098(9) 0.0017(9) -0.0156(11) C24 0.0260(11) 0.0153(10) 0.0452(12) -0.0040(8) 0.0056(9) -0.0115(10) C25 0.0253(10) 0.0160(10) 0.0308(10) 0.0018(7) 0.0038(8) -0.0086(9) C26 0.0215(9) 0.0134(9) 0.0250(9) -0.0013(7) 0.0019(7) -0.0073(9) C27 0.0209(9) 0.0212(11) 0.0254(9) -0.0044(7) 0.0014(7) -0.0103(9) C28 0.0132(8) 0.0153(10) 0.0249(9) 0.0011(7) 0.0021(6) -0.0040(8) C29 0.0181(9) 0.0162(10) 0.0355(11) 0.0024(7) 0.0013(7) -0.0071(9) C30 0.0285(12) 0.0195(12) 0.0451(13) 0.0077(9) 0.0046(9) -0.0096(11) C31 0.0291(12) 0.0324(14) 0.0335(12) 0.0137(9) 0.0029(9) -0.0055(12) C32 0.0295(12) 0.0411(15) 0.0250(10) 0.0055(9) -0.0018(8) -0.0113(12) C33 0.0229(10) 0.0284(12) 0.0249(9) -0.0004(8) 0.0006(7) -0.0106(10) C34 0.0136(8) 0.0138(9) 0.0278(9) -0.0019(7) 0.0017(7) -0.0051(8) C35 0.0242(10) 0.0322(14) 0.0296(11) -0.0112(9) -0.0009(8) 0.0000(11) C36 0.0328(13) 0.0464(18) 0.0385(13) -0.0211(12) 0.0052(10) 0.0023(14) C37 0.0213(11) 0.0291(14) 0.0497(15) -0.0091(11) 0.0052(10) 0.0024(11) C38 0.0202(10) 0.0335(15) 0.0389(13) 0.0050(10) 0.0008(9) -0.0011(11) C39 0.0167(9) 0.0294(13) 0.0281(10) 0.0033(8) 0.0012(7) -0.0024(10) B1 0.0217(12) 0.0135(12) 0.0591(17) -0.0124(10) 0.0096(11) -0.0082(11) B2 0.0189(11) 0.0103(11) 0.0553(16) 0.0006(9) 0.0034(10) -0.0065(10) B3 0.0187(10) 0.0153(11) 0.0368(12) -0.0080(8) 0.0038(8) -0.0080(10) B4 0.0176(10) 0.0137(11) 0.0342(11) -0.0105(8) 0.0074(8) -0.0068(9) B5 0.0167(10) 0.0102(11) 0.0501(15) -0.0034(9) 0.0045(9) -0.0035(10) B6 0.0170(11) 0.0103(12) 0.0632(18) 0.0062(10) 0.0008(11) -0.0031(11) B9 0.0149(9) 0.0118(10) 0.0245(9) -0.0012(7) 0.0037(7) -0.0066(9) B10 0.0173(10) 0.0165(12) 0.0351(12) 0.0092(8) -0.0041(8) -0.0061(10) B11 0.0191(11) 0.0188(12) 0.0370(12) 0.0110(9) -0.0036(9) -0.0080(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh B9 2.218(2) . ? Rh B4 2.224(2) . ? Rh B3 2.238(2) . ? Rh P2 2.3175(5) . ? Rh P1 2.3206(6) . ? Rh S7 2.4172(5) . ? S7 B11 1.930(3) . ? S7 B2 1.970(3) . ? S7 B3 2.062(2) . ? P1 C1 1.828(3) . ? P1 C2 1.828(3) . ? P1 C8 1.840(2) . ? P2 C21 1.8189(18) . ? P2 C14 1.836(2) . ? P2 C15 1.836(2) . ? P3 C28 1.809(2) . ? P3 C27 1.809(2) . ? P3 C34 1.815(2) . ? P3 B9 1.943(2) . ? C2 C3A 1.181(8) . ? C2 C7B 1.287(6) . ? C2 C3B 1.542(6) . ? C2 C7A 1.571(8) . ? C3A C4A 1.389(10) . ? C4A C5A 1.388(11) . ? C5A C6A 1.387(10) . ? C6A C7A 1.388(10) . ? C3B C4B 1.386(7) . ? C4B C5B 1.387(8) . ? C5B C6B 1.380(8) . ? C6B C7B 1.400(8) . ? C8 C13 1.379(4) . ? C8 C9 1.391(3) . ? C9 C10 1.396(4) . ? C10 C11 1.380(5) . ? C11 C12 1.370(5) . ? C12 C13 1.404(3) . ? C15 C16 1.395(3) . ? C15 C20 1.398(3) . ? C16 C17 1.395(3) . ? C17 C18 1.386(3) . ? C18 C19 1.382(4) . ? C19 C20 1.384(3) . ? C21 C26 1.394(3) . ? C21 C22 1.397(3) . ? C22 C23 1.393(3) . ? C23 C24 1.388(3) . ? C24 C25 1.381(3) . ? C25 C26 1.391(3) . ? C28 C33 1.391(3) . ? C28 C29 1.396(3) . ? C29 C30 1.389(3) . ? C30 C31 1.373(4) . ? C31 C32 1.381(4) . ? C32 C33 1.395(3) . ? C34 C35 1.383(3) . ? C34 C39 1.391(3) . ? C35 C36 1.387(3) . ? C36 C37 1.380(4) . ? C37 C38 1.374(4) . ? C38 C39 1.388(3) . ? B1 B2 1.764(4) . ? B1 B3 1.769(4) . ? B1 B5 1.775(4) . ? B1 B6 1.781(5) . ? B1 B4 1.801(3) . ? B2 B6 1.756(4) . ? B2 B11 1.851(4) . ? B2 B3 1.907(4) . ? B3 B4 1.809(3) . ? B4 B9 1.772(3) . ? B4 B5 1.800(4) . ? B5 B6 1.769(4) . ? B5 B10 1.784(4) . ? B5 B9 1.787(3) . ? B6 B11 1.742(4) . ? B6 B10 1.768(4) . ? B9 B10 1.871(3) . ? B10 B11 1.808(3) . ? C91 C92 0.532(10) . ? C91 C92 1.424(11) 2_667 ? C91 C93 1.424(13) . ? C91 C91 1.69(2) 2_667 ? C92 C92 1.333(10) 2_667 ? C92 C91 1.424(11) 2_667 ? C92 C93 1.838(10) . ? C93 C95 1.005(7) . ? C93 C94 1.473(7) . ? C94 C95 1.532(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B9 Rh B4 47.01(8) . . ? B9 Rh B3 83.07(8) . . ? B4 Rh B3 47.83(8) . . ? B9 Rh P2 97.34(6) . . ? B4 Rh P2 144.25(6) . . ? B3 Rh P2 147.57(6) . . ? B9 Rh P1 159.43(6) . . ? B4 Rh P1 113.93(6) . . ? B3 Rh P1 86.74(7) . . ? P2 Rh P1 100.810(19) . . ? B9 Rh S7 88.79(5) . . ? B4 Rh S7 87.75(6) . . ? B3 Rh S7 52.42(6) . . ? P2 Rh S7 95.149(18) . . ? P1 Rh S7 99.077(19) . . ? B11 S7 B2 56.65(13) . . ? B11 S7 B3 98.70(12) . . ? B2 S7 B3 56.41(11) . . ? B11 S7 Rh 109.06(7) . . ? B2 S7 Rh 108.49(8) . . ? B3 S7 Rh 59.33(6) . . ? C1 P1 C2 104.81(15) . . ? C1 P1 C8 101.36(11) . . ? C2 P1 C8 98.62(11) . . ? C1 P1 Rh 115.06(9) . . ? C2 P1 Rh 117.35(8) . . ? C8 P1 Rh 117.13(8) . . ? C21 P2 C14 104.45(9) . . ? C21 P2 C15 102.15(9) . . ? C14 P2 C15 97.88(9) . . ? C21 P2 Rh 118.89(6) . . ? C14 P2 Rh 112.97(7) . . ? C15 P2 Rh 117.66(7) . . ? C28 P3 C27 106.84(10) . . ? C28 P3 C34 103.86(9) . . ? C27 P3 C34 105.07(10) . . ? C28 P3 B9 115.89(10) . . ? C27 P3 B9 111.62(9) . . ? C34 P3 B9 112.68(9) . . ? C7B C2 C3B 115.9(4) . . ? C3A C2 C7A 118.6(5) . . ? C3A C2 P1 127.1(4) . . ? C7B C2 P1 129.9(4) . . ? C3B C2 P1 113.9(3) . . ? C7A C2 P1 114.3(3) . . ? C2 C3A C4A 128.5(7) . . ? C5A C4A C3A 116.5(7) . . ? C6A C5A C4A 120.9(7) . . ? C5A C6A C7A 120.9(7) . . ? C6A C7A C2 114.5(6) . . ? C4B C3B C2 118.8(4) . . ? C3B C4B C5B 118.9(5) . . ? C6B C5B C4B 122.7(6) . . ? C5B C6B C7B 117.3(5) . . ? C2 C7B C6B 126.4(5) . . ? C13 C8 C9 118.9(2) . . ? C13 C8 P1 120.86(18) . . ? C9 C8 P1 120.2(2) . . ? C8 C9 C10 120.0(3) . . ? C11 C10 C9 120.7(3) . . ? C12 C11 C10 119.5(3) . . ? C11 C12 C13 120.2(3) . . ? C8 C13 C12 120.7(3) . . ? C16 C15 C20 119.08(18) . . ? C16 C15 P2 123.88(15) . . ? C20 C15 P2 117.02(15) . . ? C17 C16 C15 120.08(19) . . ? C18 C17 C16 119.9(2) . . ? C19 C18 C17 120.4(2) . . ? C18 C19 C20 119.9(2) . . ? C19 C20 C15 120.7(2) . . ? C26 C21 C22 119.09(17) . . ? C26 C21 P2 117.20(14) . . ? C22 C21 P2 123.62(15) . . ? C23 C22 C21 120.0(2) . . ? C24 C23 C22 120.2(2) . . ? C25 C24 C23 120.08(19) . . ? C24 C25 C26 120.0(2) . . ? C25 C26 C21 120.58(19) . . ? C33 C28 C29 119.56(19) . . ? C33 C28 P3 119.80(16) . . ? C29 C28 P3 120.46(16) . . ? C30 C29 C28 119.8(2) . . ? C31 C30 C29 120.4(2) . . ? C30 C31 C32 120.2(2) . . ? C31 C32 C33 120.2(2) . . ? C28 C33 C32 119.7(2) . . ? C35 C34 C39 119.2(2) . . ? C35 C34 P3 120.42(17) . . ? C39 C34 P3 120.39(16) . . ? C34 C35 C36 120.4(2) . . ? C37 C36 C35 120.3(2) . . ? C38 C37 C36 119.6(2) . . ? C37 C38 C39 120.5(2) . . ? C38 C39 C34 120.0(2) . . ? B2 B1 B3 65.36(15) . . ? B2 B1 B5 109.9(2) . . ? B3 B1 B5 110.23(17) . . ? B2 B1 B6 59.39(16) . . ? B3 B1 B6 110.97(19) . . ? B5 B1 B6 59.68(15) . . ? B2 B1 B4 113.70(17) . . ? B3 B1 B4 60.90(14) . . ? B5 B1 B4 60.46(14) . . ? B6 B1 B4 108.79(17) . . ? B6 B2 B1 60.79(17) . . ? B6 B2 B11 57.70(16) . . ? B1 B2 B11 106.60(17) . . ? B6 B2 B3 105.88(16) . . ? B1 B2 B3 57.45(15) . . ? B11 B2 B3 107.47(15) . . ? B6 B2 S7 109.30(16) . . ? B1 B2 S7 111.65(15) . . ? B11 B2 S7 60.59(12) . . ? B3 B2 S7 64.25(11) . . ? B1 B3 B4 60.42(13) . . ? B1 B3 B2 57.19(15) . . ? B4 B3 B2 106.80(17) . . ? B1 B3 S7 107.32(17) . . ? B4 B3 S7 112.38(14) . . ? B2 B3 S7 59.34(11) . . ? B1 B3 Rh 118.47(14) . . ? B4 B3 Rh 65.68(10) . . ? B2 B3 Rh 118.65(14) . . ? S7 B3 Rh 68.25(7) . . ? B9 B4 B5 60.02(14) . . ? B9 B4 B1 108.06(18) . . ? B5 B4 B1 59.07(14) . . ? B9 B4 B3 111.21(16) . . ? B5 B4 B3 107.30(17) . . ? B1 B4 B3 58.68(13) . . ? B9 B4 Rh 66.30(10) . . ? B5 B4 Rh 118.48(14) . . ? B1 B4 Rh 117.70(13) . . ? B3 B4 Rh 66.49(10) . . ? B6 B5 B1 60.32(16) . . ? B6 B5 B10 59.66(16) . . ? B1 B5 B10 108.46(17) . . ? B6 B5 B9 110.60(18) . . ? B1 B5 B9 108.53(17) . . ? B10 B5 B9 63.20(14) . . ? B6 B5 B4 109.32(17) . . ? B1 B5 B4 60.48(15) . . ? B10 B5 B4 109.92(17) . . ? B9 B5 B4 59.20(13) . . ? B11 B6 B2 63.88(16) . . ? B11 B6 B10 62.00(16) . . ? B2 B6 B10 113.31(19) . . ? B11 B6 B5 111.42(18) . . ? B2 B6 B5 110.6(2) . . ? B10 B6 B5 60.59(14) . . ? B11 B6 B1 110.71(19) . . ? B2 B6 B1 59.82(16) . . ? B10 B6 B1 108.94(17) . . ? B5 B6 B1 60.00(16) . . ? B4 B9 B5 60.78(14) . . ? B4 B9 B10 107.31(15) . . ? B5 B9 B10 58.33(14) . . ? B4 B9 P3 125.65(13) . . ? B5 B9 P3 110.24(13) . . ? B10 B9 P3 109.87(13) . . ? B4 B9 Rh 66.69(10) . . ? B5 B9 Rh 119.45(13) . . ? B10 B9 Rh 116.72(12) . . ? P3 B9 Rh 124.17(11) . . ? B6 B10 B5 59.75(16) . . ? B6 B10 B11 58.31(15) . . ? B5 B10 B11 107.74(18) . . ? B6 B10 B9 106.88(18) . . ? B5 B10 B9 58.47(13) . . ? B11 B10 B9 111.17(16) . . ? B6 B11 B10 59.69(15) . . ? B6 B11 B2 58.42(16) . . ? B10 B11 B2 107.13(19) . . ? B6 B11 S7 111.73(18) . . ? B10 B11 S7 113.12(14) . . ? B2 B11 S7 62.76(12) . . ? C92 C91 C92 69.3(15) . 2_667 ? C92 C91 C93 134.8(15) . . ? C92 C91 C93 106.4(8) 2_667 . ? C92 C91 C91 52.2(12) . 2_667 ? C93 C91 C91 117.4(8) . 2_667 ? C91 C92 C92 88.8(15) . 2_667 ? C91 C92 C91 110.7(15) . 2_667 ? C92 C92 C93 90.6(8) 2_667 . ? C91 C92 C93 108.7(8) 2_667 . ? C95 C93 C91 149.6(8) . . ? C95 C93 C94 73.6(5) . . ? C91 C93 C94 114.0(6) . . ? C95 C93 C92 157.9(6) . . ? C94 C93 C92 119.3(4) . . ? C93 C95 C94 67.3(4) . . ? _diffrn_measured_fraction_theta_max 0.749 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.935 _diffrn_special_details ; Data were collected to a completeness of 0.935 to theta = 27.50, measuring a total of 43398 reflections. Once symmetry equivalent reflections were merged the ratio reflections/parameters was statistically satisfactory 19.6 (11291/576 ref./par.) ; _refine_diff_density_max 1.279 _refine_diff_density_min -1.886 _refine_diff_density_rms 0.094