# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Macropolyhedral boron-containing cluster chemistry. The unique nido-five-vertex-B2-nido-ten-vertex conjuncto structure of [(eta5-C5Me5)2Rh2B11H15] via an unexpected cluster-dismantling ; loop_ _publ_author_name J.Kennedy M.J.Carr W.Clegg T.Jelinek C.Kilner S.D.Perera ; B.Stibr ; _publ_contact_author_name 'J. Kennedy' _publ_contact_author_email J.D.KENNEDY@LEEDS.AC.UK data_mc101b _database_code_depnum_ccdc_archive 'CCDC 644825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H44.83 B11 Cl0.17 Rh2' _chemical_formula_sum 'C20 H44.83 B11 Cl0.17 Rh2' _chemical_formula_weight 616.15 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8255(5) _cell_length_b 9.9185(6) _cell_length_c 17.9003(10) _cell_angle_alpha 89.867(1) _cell_angle_beta 79.475(1) _cell_angle_gamma 68.194(1) _cell_volume 1426.63(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 625 _exptl_absorpt_coefficient_mu 1.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9114 _exptl_absorpt_correction_T_max 0.9768 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6932 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9949 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 29.22 _reflns_number_total 7239 _reflns_number_gt 6095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; enCIFer (CCDC, 2002) ; _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 'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.3050P] 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 7239 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Rh4' Rh 0.10061(3) 1.16845(2) 0.367077(11) 0.03096(7) Uani 1 1 d . A . Rh7 Rh 0.47281(2) 0.79038(2) 0.143140(9) 0.02446(7) Uani 1 1 d . . . Cl5' Cl -0.0302(6) 1.2119(6) 0.1773(3) 0.0494(11) Uani 0.17 1 d P A 2 C41 C -0.1152(5) 1.3648(4) 0.40497(17) 0.0485(8) Uani 1 1 d . . . C42 C 0.0242(7) 1.4021(4) 0.3903(3) 0.0751(16) Uani 1 1 d . . . C43 C 0.1315(5) 1.3214(6) 0.4419(3) 0.087(2) Uani 1 1 d . . . C44 C 0.0443(5) 1.2459(4) 0.4898(2) 0.0568(10) Uani 1 1 d . . . C45 C -0.1053(4) 1.2749(3) 0.46741(16) 0.0419(7) Uani 1 1 d . . . C46 C -0.2652(7) 1.4202(6) 0.3673(3) 0.0946(19) Uani 1 1 d . . . H46A H -0.3529 1.5031 0.3987 0.142 Uiso 1 1 calc R . . H46B H -0.3064 1.3423 0.3620 0.142 Uiso 1 1 calc R . . H46C H -0.2333 1.4512 0.3168 0.142 Uiso 1 1 calc R . . C47 C 0.0561(12) 1.5036(6) 0.3329(4) 0.181(5) Uani 1 1 d . . . H47A H 0.0455 1.4728 0.2828 0.271 Uiso 1 1 calc R . . H47B H 0.1687 1.5018 0.3304 0.271 Uiso 1 1 calc R . . H47C H -0.0252 1.6027 0.3482 0.271 Uiso 1 1 calc R . . C48 C 0.2963(7) 1.3252(10) 0.4520(6) 0.211(6) Uani 1 1 d . . . H48A H 0.2776 1.3957 0.4943 0.316 Uiso 1 1 calc R . . H48B H 0.3495 1.3539 0.4051 0.316 Uiso 1 1 calc R . . H48C H 0.3687 1.2284 0.4632 0.316 Uiso 1 1 calc R . . C49 C 0.1008(11) 1.1520(6) 0.5543(3) 0.138(3) Uani 1 1 d . . . H49A H 0.0436 1.2076 0.6033 0.207 Uiso 1 1 calc R . . H49B H 0.2213 1.1230 0.5496 0.207 Uiso 1 1 calc R . . H49C H 0.0740 1.0649 0.5517 0.207 Uiso 1 1 calc R . . C50 C -0.2425(6) 1.2263(5) 0.5033(3) 0.0809(15) Uani 1 1 d . . . H50A H -0.1966 1.1400 0.5312 0.121 Uiso 1 1 calc R . . H50B H -0.2933 1.2024 0.4635 0.121 Uiso 1 1 calc R . . H50C H -0.3270 1.3048 0.5386 0.121 Uiso 1 1 calc R . . C71 C 0.3694(4) 0.7546(3) 0.04475(16) 0.0386(6) Uani 1 1 d . . . C72 C 0.3334(3) 0.6660(3) 0.10391(15) 0.0323(5) Uani 1 1 d . . . C73 C 0.4874(3) 0.5658(3) 0.11796(15) 0.0318(5) Uani 1 1 d . . . C74 C 0.6178(4) 0.5925(3) 0.06738(16) 0.0375(6) Uani 1 1 d . . . C75 C 0.5459(4) 0.7068(4) 0.02156(15) 0.0407(7) Uani 1 1 d . . . C76 C 0.2396(6) 0.8724(4) 0.0115(2) 0.0623(11) Uani 1 1 d . . . H76A H 0.2077 0.8289 -0.0291 0.093 Uiso 1 1 calc R . . H76B H 0.2855 0.9437 -0.0094 0.093 Uiso 1 1 calc R . . H76C H 0.1415 0.9210 0.0516 0.093 Uiso 1 1 calc R . . C77 C 0.1638(4) 0.6763(4) 0.1436(2) 0.0486(8) Uani 1 1 d . . . H77A H 0.1368 0.5995 0.1217 0.073 Uiso 1 1 calc R . . H77B H 0.0810 0.7717 0.1369 0.073 Uiso 1 1 calc R . . H77C H 0.1628 0.6644 0.1980 0.073 Uiso 1 1 calc R . . C78 C 0.5088(5) 0.4499(4) 0.1728(2) 0.0477(7) Uani 1 1 d . . . H78A H 0.4130 0.4812 0.2153 0.072 Uiso 1 1 calc R . . H78B H 0.6108 0.4324 0.1922 0.072 Uiso 1 1 calc R . . H78C H 0.5165 0.3600 0.1469 0.072 Uiso 1 1 calc R . . C79 C 0.7999(4) 0.5030(4) 0.0604(2) 0.0579(10) Uani 1 1 d . . . H79A H 0.8294 0.4134 0.0285 0.087 Uiso 1 1 calc R . . H79B H 0.8242 0.4784 0.1111 0.087 Uiso 1 1 calc R . . H79C H 0.8651 0.5589 0.0370 0.087 Uiso 1 1 calc R . . C80 C 0.6406(6) 0.7616(5) -0.04153(18) 0.0679(13) Uani 1 1 d . . . H80A H 0.7441 0.7586 -0.0276 0.102 Uiso 1 1 calc R . . H80B H 0.5727 0.8621 -0.0496 0.102 Uiso 1 1 calc R . . H80C H 0.6669 0.6999 -0.0885 0.102 Uiso 1 1 calc R . . B1 B 0.5469(4) 0.8598(4) 0.31559(17) 0.0369(7) Uani 1 1 d . . . B1' B 0.2476(4) 1.1420(3) 0.25710(16) 0.0307(6) Uani 1 1 d . A . B2 B 0.4080(4) 0.8131(3) 0.26824(16) 0.0312(6) Uani 1 1 d . . . B3 B 0.6271(4) 0.7440(4) 0.23076(16) 0.0349(6) Uani 1 1 d . . . B4 B 0.7240(4) 0.8652(5) 0.25221(19) 0.0428(8) Uani 1 1 d . . . B5 B 0.3573(4) 0.9990(3) 0.30666(15) 0.0269(5) Uani 1 1 d . . . B5' B 0.0800(4) 1.0941(4) 0.2512(2) 0.0400(7) Uani 1 1 d . . . B6 B 0.2913(4) 0.9678(3) 0.22241(16) 0.0281(5) Uani 1 1 d . A . B8 B 0.6910(4) 0.8454(4) 0.15684(17) 0.0351(7) Uani 1 1 d . . . B9 B 0.6782(5) 1.0156(5) 0.2002(2) 0.0437(8) Uani 1 1 d . . . B10 B 0.5593(4) 1.0287(4) 0.29510(18) 0.0382(7) Uani 1 1 d . . . H1 H 0.562(5) 0.820(4) 0.371(2) 0.054(10) Uiso 1 1 d . . . H1' H 0.282(4) 1.228(3) 0.2292(17) 0.030(8) Uiso 1 1 d . . . H2 H 0.349(4) 0.743(4) 0.2950(18) 0.034(8) Uiso 1 1 d . . . H3 H 0.693(4) 0.629(4) 0.2301(17) 0.035(8) Uiso 1 1 d . . . H4 H 0.848(5) 0.833(4) 0.267(2) 0.053(10) Uiso 1 1 d . . . H8 H 0.797(4) 0.795(4) 0.1106(17) 0.035(8) Uiso 1 1 d . . . H9 H 0.770(4) 1.074(4) 0.1777(19) 0.043(9) Uiso 1 1 d . . . H10 H 0.572(5) 1.112(4) 0.336(2) 0.055(11) Uiso 1 1 d . . . H45A H 0.253(4) 1.007(4) 0.3676(19) 0.041(9) Uiso 1 1 d . . . H45B H 0.015(5) 1.068(5) 0.323(2) 0.063(12) Uiso 1 1 d . . . H56 H 0.142(4) 0.962(4) 0.2378(17) 0.034(8) Uiso 1 1 d . . . H67 H 0.361(4) 0.963(3) 0.1511(16) 0.024(7) Uiso 1 1 d . . . H89 H 0.622(4) 0.978(4) 0.1475(18) 0.036(8) Uiso 1 1 d . . . H910 H 0.549(5) 1.088(4) 0.233(2) 0.050(10) Uiso 1 1 d . . . H5' H -0.024(6) 1.136(5) 0.219(3) 0.057(13) Uiso 0.83 1 d P B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh4' 0.02867(12) 0.02857(12) 0.02995(12) -0.00433(8) 0.00139(8) -0.00763(9) Rh7 0.02346(10) 0.02930(12) 0.01896(10) 0.00057(7) -0.00149(6) -0.00930(8) Cl5' 0.041(2) 0.047(3) 0.060(3) 0.008(2) -0.024(2) -0.009(2) C41 0.056(2) 0.0350(17) 0.0330(15) -0.0017(12) -0.0012(13) 0.0043(14) C42 0.099(4) 0.0323(19) 0.069(3) -0.0168(17) 0.040(3) -0.023(2) C43 0.0397(19) 0.079(3) 0.128(4) -0.079(3) 0.018(2) -0.023(2) C44 0.061(2) 0.044(2) 0.0484(19) -0.0199(15) -0.0211(16) 0.0053(17) C45 0.0433(17) 0.0381(16) 0.0316(14) -0.0059(11) 0.0016(11) -0.0049(13) C46 0.091(4) 0.080(3) 0.060(3) -0.008(2) -0.031(2) 0.035(3) C47 0.295(11) 0.049(3) 0.136(6) -0.035(3) 0.143(7) -0.080(5) C48 0.053(3) 0.234(9) 0.317(12) -0.239(10) 0.037(5) -0.056(5) C49 0.211(8) 0.073(3) 0.078(3) -0.028(3) -0.096(4) 0.037(4) C50 0.078(3) 0.070(3) 0.074(3) -0.017(2) 0.039(2) -0.029(2) C71 0.0530(18) 0.0387(16) 0.0298(13) 0.0004(11) -0.0174(12) -0.0194(14) C72 0.0272(13) 0.0385(15) 0.0302(12) -0.0054(10) -0.0022(9) -0.0128(11) C73 0.0302(13) 0.0320(14) 0.0301(12) -0.0017(10) -0.0021(9) -0.0101(11) C74 0.0294(13) 0.0460(17) 0.0331(13) -0.0136(12) 0.0062(10) -0.0153(13) C75 0.0545(19) 0.0530(19) 0.0217(12) -0.0056(11) 0.0020(11) -0.0328(16) C76 0.095(3) 0.052(2) 0.053(2) 0.0116(16) -0.049(2) -0.025(2) C77 0.0282(14) 0.062(2) 0.0536(18) -0.0125(15) 0.0028(12) -0.0198(15) C78 0.057(2) 0.0335(17) 0.0522(18) 0.0092(13) -0.0157(15) -0.0145(15) C79 0.0291(15) 0.058(2) 0.072(2) -0.0291(19) 0.0061(15) -0.0072(15) C80 0.105(3) 0.096(3) 0.0258(15) -0.0035(17) 0.0063(17) -0.074(3) B1 0.0359(16) 0.0416(18) 0.0234(13) 0.0002(12) -0.0093(11) -0.0018(14) B1' 0.0341(15) 0.0303(15) 0.0265(13) 0.0033(10) -0.0076(10) -0.0099(12) B2 0.0322(15) 0.0301(15) 0.0244(13) 0.0023(10) -0.0009(10) -0.0062(12) B3 0.0335(15) 0.0358(17) 0.0242(13) 0.0019(11) -0.0079(11) 0.0008(13) B4 0.0271(15) 0.062(2) 0.0333(15) -0.0092(14) -0.0093(12) -0.0078(15) B5 0.0257(13) 0.0317(15) 0.0199(11) 0.0013(10) -0.0028(9) -0.0078(11) B5' 0.0294(15) 0.0419(19) 0.0419(17) -0.0083(14) -0.0096(12) -0.0046(14) B6 0.0255(13) 0.0318(15) 0.0260(13) 0.0007(10) -0.0050(10) -0.0097(12) B8 0.0248(13) 0.051(2) 0.0268(13) -0.0038(12) -0.0033(10) -0.0126(14) B9 0.0355(17) 0.061(2) 0.0387(17) -0.0060(15) -0.0027(13) -0.0251(17) B10 0.0309(15) 0.051(2) 0.0313(14) -0.0058(13) -0.0061(11) -0.0136(15) _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 Rh4' B1' 2.108(3) . ? Rh4' C43 2.150(3) . ? Rh4' C41 2.159(3) . ? Rh4' C42 2.177(4) . ? Rh4' C44 2.233(3) . ? Rh4' C45 2.243(3) . ? Rh4' B5' 2.264(3) . ? Rh4' B5 2.326(3) . ? Rh4' H45A 1.66(4) . ? Rh4' H45B 1.72(4) . ? Rh7 B6 2.182(3) . ? Rh7 B2 2.198(3) . ? Rh7 B3 2.199(3) . ? Rh7 C74 2.200(3) . ? Rh7 C71 2.212(3) . ? Rh7 C75 2.222(3) . ? Rh7 C73 2.225(3) . ? Rh7 C72 2.231(2) . ? Rh7 B8 2.240(3) . ? Rh7 H67 1.62(3) . ? Cl5' B5' 1.917(6) . ? Cl5' H5' 1.05(5) . ? C41 C42 1.393(6) . ? C41 C45 1.423(4) . ? C41 C46 1.514(6) . ? C42 C43 1.463(8) . ? C42 C47 1.500(6) . ? C43 C44 1.440(7) . ? C43 C48 1.512(6) . ? C44 C45 1.377(5) . ? C44 C49 1.520(6) . ? C45 C50 1.503(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C71 C75 1.428(5) . ? C71 C72 1.440(4) . ? C71 C76 1.510(5) . ? C72 C73 1.421(4) . ? C72 C77 1.501(4) . ? C73 C74 1.435(4) . ? C73 C78 1.491(4) . ? C74 C75 1.419(5) . ? C74 C79 1.501(5) . ? C75 C80 1.503(4) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? B1 B10 1.753(5) . ? B1 B5 1.764(4) . ? B1 B3 1.771(4) . ? B1 B4 1.774(5) . ? B1 B2 1.800(5) . ? B1 H1 1.08(4) . ? B1' B6 1.715(4) . ? B1' B5' 1.733(5) . ? B1' B5 1.739(4) . ? B1' H1' 1.10(3) . ? B2 B3 1.790(4) . ? B2 B6 1.793(4) . ? B2 B5 1.831(4) . ? B2 H2 1.08(3) . ? B3 B4 1.791(5) . ? B3 B8 1.795(5) . ? B3 H3 1.07(3) . ? B4 B9 1.714(6) . ? B4 B10 1.783(5) . ? B4 B8 1.806(4) . ? B4 H4 1.11(4) . ? B5 B6 1.780(4) . ? B5 B10 1.888(4) . ? B5 H45A 1.27(3) . ? B5' B6 1.797(5) . ? B5' H45B 1.37(4) . ? B5' H56 1.22(3) . ? B5' H5' 1.12(5) . ? B6 H56 1.32(3) . ? B6 H67 1.31(3) . ? B8 B9 1.816(5) . ? B8 H8 1.09(3) . ? B8 H89 1.25(3) . ? B9 B10 1.803(5) . ? B9 H9 1.18(3) . ? B9 H89 1.26(3) . ? B9 H910 1.15(4) . ? B10 H10 1.15(4) . ? B10 H910 1.25(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1' Rh4' C43 112.92(17) . . ? B1' Rh4' C41 121.20(12) . . ? C43 Rh4' C41 63.87(16) . . ? B1' Rh4' C42 99.91(13) . . ? C43 Rh4' C42 39.5(2) . . ? C41 Rh4' C42 37.47(17) . . ? B1' Rh4' C44 149.54(15) . . ? C43 Rh4' C44 38.31(19) . . ? C41 Rh4' C44 62.65(13) . . ? C42 Rh4' C44 64.24(17) . . ? B1' Rh4' C45 158.87(12) . . ? C43 Rh4' C45 62.21(14) . . ? C41 Rh4' C45 37.67(12) . . ? C42 Rh4' C45 62.69(13) . . ? C44 Rh4' C45 35.82(13) . . ? B1' Rh4' B5' 46.54(12) . . ? C43 Rh4' B5' 151.6(2) . . ? C41 Rh4' B5' 106.86(13) . . ? C42 Rh4' B5' 116.40(19) . . ? C44 Rh4' B5' 163.23(15) . . ? C45 Rh4' B5' 128.00(13) . . ? B1' Rh4' B5 45.85(11) . . ? C43 Rh4' B5 110.89(13) . . ? C41 Rh4' B5 164.75(12) . . ? C42 Rh4' B5 129.24(15) . . ? C44 Rh4' B5 123.13(12) . . ? C45 Rh4' B5 154.68(11) . . ? B5' Rh4' B5 70.57(11) . . ? B1' Rh4' H45A 77.3(11) . . ? C43 Rh4' H45A 108.2(12) . . ? C41 Rh4' H45A 161.3(11) . . ? C42 Rh4' H45A 144.4(12) . . ? C44 Rh4' H45A 100.3(11) . . ? C45 Rh4' H45A 123.8(11) . . ? B5' Rh4' H45A 87.8(12) . . ? B5 Rh4' H45A 32.1(11) . . ? B1' Rh4' H45B 81.8(14) . . ? C43 Rh4' H45B 162.5(14) . . ? C41 Rh4' H45B 100.9(15) . . ? C42 Rh4' H45B 131.7(15) . . ? C44 Rh4' H45B 128.5(14) . . ? C45 Rh4' H45B 100.6(14) . . ? B5' Rh4' H45B 37.3(13) . . ? B5 Rh4' H45B 86.0(14) . . ? H45A Rh4' H45B 83.6(19) . . ? B6 Rh7 B2 48.33(11) . . ? B6 Rh7 B3 86.44(11) . . ? B2 Rh7 B3 48.03(12) . . ? B6 Rh7 C74 168.59(10) . . ? B2 Rh7 C74 128.84(12) . . ? B3 Rh7 C74 97.95(12) . . ? B6 Rh7 C71 111.59(11) . . ? B2 Rh7 C71 139.46(12) . . ? B3 Rh7 C71 159.78(12) . . ? C74 Rh7 C71 62.63(12) . . ? B6 Rh7 C75 142.99(12) . . ? B2 Rh7 C75 164.80(12) . . ? B3 Rh7 C75 128.48(13) . . ? C74 Rh7 C75 37.42(12) . . ? C71 Rh7 C75 37.58(12) . . ? B6 Rh7 C73 131.20(10) . . ? B2 Rh7 C73 101.96(11) . . ? B3 Rh7 C73 98.69(12) . . ? C74 Rh7 C73 37.84(10) . . ? C71 Rh7 C73 62.81(11) . . ? C75 Rh7 C73 63.00(11) . . ? B6 Rh7 C72 106.54(10) . . ? B2 Rh7 C72 106.88(11) . . ? B3 Rh7 C72 130.01(12) . . ? C74 Rh7 C72 62.63(10) . . ? C71 Rh7 C72 37.83(10) . . ? C75 Rh7 C72 62.95(10) . . ? C73 Rh7 C72 37.19(10) . . ? B6 Rh7 B8 94.84(11) . . ? B2 Rh7 B8 85.57(11) . . ? B3 Rh7 B8 47.70(12) . . ? C74 Rh7 B8 95.90(11) . . ? C71 Rh7 B8 134.69(11) . . ? C75 Rh7 B8 100.96(11) . . ? C73 Rh7 B8 124.18(12) . . ? C72 Rh7 B8 158.52(11) . . ? B6 Rh7 H67 36.5(10) . . ? B2 Rh7 H67 83.3(10) . . ? B3 Rh7 H67 108.2(10) . . ? C74 Rh7 H67 147.7(10) . . ? C71 Rh7 H67 92.0(10) . . ? C75 Rh7 H67 110.4(10) . . ? C73 Rh7 H67 147.2(10) . . ? C72 Rh7 H67 110.1(10) . . ? B8 Rh7 H67 88.3(10) . . ? B5' Cl5' H5' 29(3) . . ? C42 C41 C45 109.5(4) . . ? C42 C41 C46 127.0(4) . . ? C45 C41 C46 123.3(4) . . ? C42 C41 Rh4' 72.0(2) . . ? C45 C41 Rh4' 74.40(18) . . ? C46 C41 Rh4' 124.6(3) . . ? C41 C42 C43 105.8(3) . . ? C41 C42 C47 126.4(7) . . ? C43 C42 C47 127.7(6) . . ? C41 C42 Rh4' 70.6(2) . . ? C43 C42 Rh4' 69.2(2) . . ? C47 C42 Rh4' 124.5(3) . . ? C44 C43 C42 107.7(3) . . ? C44 C43 C48 123.6(7) . . ? C42 C43 C48 128.3(7) . . ? C44 C43 Rh4' 74.0(2) . . ? C42 C43 Rh4' 71.2(2) . . ? C48 C43 Rh4' 125.4(3) . . ? C45 C44 C43 107.4(4) . . ? C45 C44 C49 124.7(5) . . ? C43 C44 C49 127.8(5) . . ? C45 C44 Rh4' 72.49(18) . . ? C43 C44 Rh4' 67.7(2) . . ? C49 C44 Rh4' 125.7(3) . . ? C44 C45 C41 109.3(3) . . ? C44 C45 C50 126.9(4) . . ? C41 C45 C50 123.7(4) . . ? C44 C45 Rh4' 71.68(19) . . ? C41 C45 Rh4' 67.93(17) . . ? C50 C45 Rh4' 128.2(2) . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C75 C71 C72 108.3(3) . . ? C75 C71 C76 126.9(3) . . ? C72 C71 C76 124.7(3) . . ? C75 C71 Rh7 71.61(16) . . ? C72 C71 Rh7 71.81(14) . . ? C76 C71 Rh7 124.6(2) . . ? C73 C72 C71 107.8(2) . . ? C73 C72 C77 125.8(3) . . ? C71 C72 C77 126.4(3) . . ? C73 C72 Rh7 71.18(15) . . ? C71 C72 Rh7 70.36(14) . . ? C77 C72 Rh7 124.30(19) . . ? C72 C73 C74 107.5(3) . . ? C72 C73 C78 126.0(3) . . ? C74 C73 C78 126.4(3) . . ? C72 C73 Rh7 71.64(16) . . ? C74 C73 Rh7 70.15(16) . . ? C78 C73 Rh7 125.7(2) . . ? C75 C74 C73 109.0(3) . . ? C75 C74 C79 126.4(3) . . ? C73 C74 C79 124.4(3) . . ? C75 C74 Rh7 72.14(16) . . ? C73 C74 Rh7 72.01(15) . . ? C79 C74 Rh7 126.2(2) . . ? C74 C75 C71 107.3(2) . . ? C74 C75 C80 125.5(3) . . ? C71 C75 C80 127.2(4) . . ? C74 C75 Rh7 70.45(15) . . ? C71 C75 Rh7 70.82(15) . . ? C80 C75 Rh7 125.8(2) . . ? C71 C76 H76A 109.5 . . ? C71 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C71 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C74 C79 H79A 109.5 . . ? C74 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C74 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C75 C80 H80A 109.5 . . ? C75 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C75 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? B10 B1 B5 64.93(19) . . ? B10 B1 B3 108.4(2) . . ? B5 B1 B3 108.9(2) . . ? B10 B1 B4 60.7(2) . . ? B5 B1 B4 114.4(2) . . ? B3 B1 B4 60.70(19) . . ? B10 B1 B2 114.7(2) . . ? B5 B1 B2 61.84(17) . . ? B3 B1 B2 60.15(18) . . ? B4 B1 B2 113.2(2) . . ? B10 B1 H1 119(2) . . ? B5 B1 H1 119(2) . . ? B3 B1 H1 123(2) . . ? B4 B1 H1 118(2) . . ? B2 B1 H1 118(2) . . ? B6 B1' B5' 62.80(18) . . ? B6 B1' B5 62.02(17) . . ? B5' B1' B5 99.6(2) . . ? B6 B1' Rh4' 106.52(18) . . ? B5' B1' Rh4' 71.48(16) . . ? B5 B1' Rh4' 73.72(14) . . ? B6 B1' H1' 129.1(16) . . ? B5' B1' H1' 128.9(17) . . ? B5 B1' H1' 130.8(17) . . ? Rh4' B1' H1' 124.3(16) . . ? B3 B2 B6 113.8(2) . . ? B3 B2 B1 59.14(18) . . ? B6 B2 B1 109.3(2) . . ? B3 B2 B5 105.2(2) . . ? B6 B2 B5 58.80(16) . . ? B1 B2 B5 58.12(17) . . ? B3 B2 Rh7 66.02(13) . . ? B6 B2 Rh7 65.38(13) . . ? B1 B2 Rh7 115.79(18) . . ? B5 B2 Rh7 112.46(17) . . ? B3 B2 H2 120.7(18) . . ? B6 B2 H2 119.9(18) . . ? B1 B2 H2 118.9(17) . . ? B5 B2 H2 122.7(17) . . ? Rh7 B2 H2 116.3(17) . . ? B1 B3 B2 60.71(18) . . ? B1 B3 B4 59.73(19) . . ? B2 B3 B4 112.9(2) . . ? B1 B3 B8 107.4(2) . . ? B2 B3 B8 114.5(2) . . ? B4 B3 B8 60.48(19) . . ? B1 B3 Rh7 117.00(19) . . ? B2 B3 Rh7 65.95(14) . . ? B4 B3 Rh7 120.8(2) . . ? B8 B3 Rh7 67.35(13) . . ? B1 B3 H3 123.0(17) . . ? B2 B3 H3 117.0(17) . . ? B4 B3 H3 119.6(17) . . ? B8 B3 H3 120.2(17) . . ? Rh7 B3 H3 109.3(17) . . ? B9 B4 B1 112.8(3) . . ? B9 B4 B10 62.0(2) . . ? B1 B4 B10 59.05(19) . . ? B9 B4 B3 113.2(2) . . ? B1 B4 B3 59.57(19) . . ? B10 B4 B3 106.2(2) . . ? B9 B4 B8 62.0(2) . . ? B1 B4 B8 106.8(2) . . ? B10 B4 B8 105.7(2) . . ? B3 B4 B8 59.87(18) . . ? B9 B4 H4 112.3(19) . . ? B1 B4 H4 123.2(19) . . ? B10 B4 H4 120(2) . . ? B3 B4 H4 126(2) . . ? B8 B4 H4 124.1(19) . . ? B1' B5 B1 149.3(2) . . ? B1' B5 B6 58.34(16) . . ? B1 B5 B6 111.6(2) . . ? B1' B5 B2 117.9(2) . . ? B1 B5 B2 60.04(18) . . ? B6 B5 B2 59.53(17) . . ? B1' B5 B10 99.6(2) . . ? B1 B5 B10 57.25(19) . . ? B6 B5 B10 117.62(19) . . ? B2 B5 B10 107.1(2) . . ? B1' B5 Rh4' 60.43(14) . . ? B1 B5 Rh4' 147.74(17) . . ? B6 B5 Rh4' 95.99(15) . . ? B2 B5 Rh4' 128.62(17) . . ? B10 B5 Rh4' 124.15(18) . . ? B1' B5 H45A 103.4(16) . . ? B1 B5 H45A 106.9(16) . . ? B6 B5 H45A 113.8(16) . . ? B2 B5 H45A 101.7(15) . . ? B10 B5 H45A 128.4(16) . . ? Rh4' B5 H45A 44.0(16) . . ? B1' B5' B6 58.12(18) . . ? B1' B5' Cl5' 106.3(3) . . ? B6 B5' Cl5' 119.4(3) . . ? B1' B5' Rh4' 61.99(14) . . ? B6 B5' Rh4' 97.69(17) . . ? Cl5' B5' Rh4' 127.7(2) . . ? B1' B5' H45B 108.0(18) . . ? B6 B5' H45B 109.6(19) . . ? Cl5' B5' H45B 129.8(19) . . ? Rh4' B5' H45B 49.3(17) . . ? B1' B5' H56 104.2(15) . . ? B6 B5' H56 47.3(15) . . ? Cl5' B5' H56 118.6(15) . . ? Rh4' B5' H56 113.6(15) . . ? H45B B5' H56 87(2) . . ? B1' B5' H5' 133(2) . . ? B6 B5' H5' 131(2) . . ? Cl5' B5' H5' 27(2) . . ? Rh4' B5' H5' 130(3) . . ? H45B B5' H5' 108(3) . . ? H56 B5' H5' 107(3) . . ? B1' B6 B5 59.64(17) . . ? B1' B6 B2 121.3(2) . . ? B5 B6 B2 61.66(17) . . ? B1' B6 B5' 59.08(19) . . ? B5 B6 B5' 95.7(2) . . ? B2 B6 B5' 129.8(2) . . ? B1' B6 Rh7 142.88(19) . . ? B5 B6 Rh7 115.38(17) . . ? B2 B6 Rh7 66.29(14) . . ? B5' B6 Rh7 148.14(19) . . ? B1' B6 H56 100.8(14) . . ? B5 B6 H56 111.7(14) . . ? B2 B6 H56 101.3(14) . . ? B5' B6 H56 42.8(14) . . ? Rh7 B6 H56 113.7(14) . . ? B1' B6 H67 104.3(13) . . ? B5 B6 H67 129.7(13) . . ? B2 B6 H67 111.4(14) . . ? B5' B6 H67 116.8(14) . . ? Rh7 B6 H67 47.6(13) . . ? H56 B6 H67 118.3(19) . . ? B3 B8 B4 59.65(19) . . ? B3 B8 B9 108.3(2) . . ? B4 B8 B9 56.5(2) . . ? B3 B8 Rh7 64.95(14) . . ? B4 B8 Rh7 118.02(19) . . ? B9 B8 Rh7 125.3(2) . . ? B3 B8 H8 122.8(17) . . ? B4 B8 H8 119.9(17) . . ? B9 B8 H8 115.1(17) . . ? Rh7 B8 H8 111.9(17) . . ? B3 B8 H89 127.7(15) . . ? B4 B8 H89 97.6(15) . . ? B9 B8 H89 43.8(15) . . ? Rh7 B8 H89 94.9(15) . . ? H8 B8 H89 109(2) . . ? B4 B9 B10 60.8(2) . . ? B4 B9 B8 61.5(2) . . ? B10 B9 B8 104.4(2) . . ? B4 B9 H9 125.2(18) . . ? B10 B9 H9 128.3(17) . . ? B8 B9 H9 123.5(17) . . ? B4 B9 H89 102.2(15) . . ? B10 B9 H89 115.7(15) . . ? B8 B9 H89 43.6(15) . . ? H9 B9 H89 112(2) . . ? B4 B9 H910 101.4(18) . . ? B10 B9 H910 43.6(18) . . ? B8 B9 H910 115.0(18) . . ? H9 B9 H910 117(3) . . ? H89 B9 H910 94(2) . . ? B1 B10 B4 60.2(2) . . ? B1 B10 B9 109.5(2) . . ? B4 B10 B9 57.1(2) . . ? B1 B10 B5 57.81(18) . . ? B4 B10 B5 108.2(2) . . ? B9 B10 B5 118.4(2) . . ? B1 B10 H10 127.7(19) . . ? B4 B10 H10 125(2) . . ? B9 B10 H10 113.1(18) . . ? B5 B10 H10 119.9(19) . . ? B1 B10 H910 127.0(17) . . ? B4 B10 H910 93.6(17) . . ? B9 B10 H910 39.1(17) . . ? B5 B10 H910 96.2(17) . . ? H10 B10 H910 105(2) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 1.227 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.112 # Attachment 'B709470A CCDC 644826 mod.cif' data_mc105c _database_code_depnum_ccdc_archive 'CCDC 644826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H49 B16 Cl Rh2' _chemical_formula_sum 'C20 H49 B16 Cl Rh2' _chemical_formula_weight 703.82 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 11.4055(2) _cell_length_b 10.4608(2) _cell_length_c 14.3232(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.5450(10) _cell_angle_gamma 90.00 _cell_volume 1610.44(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5119 _exptl_absorpt_correction_T_max 0.6627 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Fine-focus Sealed tube' _diffrn_radiation_collimation miracol _diffrn_radiation_polarisn_norm ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15502 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5977 _reflns_number_gt 5940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; enCIFer (CCDC, 2002) ; _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^)+(0.0468P)^2^+0.8303P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 5977 _refine_ls_number_parameters 439 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 Rh7' Rh 1.056040(19) 0.83830(3) 1.008262(17) 0.02136(8) Uani 1 1 d . A . Rh9 Rh 0.60576(2) 0.70536(3) 0.74444(2) 0.02319(8) Uani 1 1 d . . . Cl2' Cl 0.91432(10) 0.81892(11) 0.75053(8) 0.0288(2) Uani 0.91 1 d P A 1 Cl8 Cl 0.7845(14) 0.5640(16) 0.9547(10) 0.055(4) Uani 0.09 1 d P A 2 C11 C 1.1947(4) 0.7529(4) 1.1401(3) 0.0301(8) Uani 1 1 d . . . C12 C 1.2538(4) 0.7770(4) 1.0672(3) 0.0287(8) Uani 1 1 d . . . C13 C 1.1920(4) 0.7023(4) 0.9811(3) 0.0293(9) Uani 1 1 d . . . C14 C 1.0982(4) 0.6280(4) 1.0005(3) 0.0316(9) Uani 1 1 d . . . C15 C 1.0984(4) 0.6596(4) 1.0978(3) 0.0325(9) Uani 1 1 d . . . C16 C 1.2311(5) 0.8089(6) 1.2418(4) 0.0475(13) Uani 1 1 d . . . H16A H 1.2812 0.7468 1.2900 0.071 Uiso 1 1 calc R . . H16B H 1.1560 0.8297 1.2576 0.071 Uiso 1 1 calc R . . H16C H 1.2798 0.8868 1.2445 0.071 Uiso 1 1 calc R . . C17 C 1.3683(4) 0.8558(5) 1.0806(4) 0.0408(11) Uani 1 1 d . . . H17A H 1.4384 0.7992 1.0850 0.061 Uiso 1 1 calc R . . H17B H 1.3874 0.9060 1.1417 0.061 Uiso 1 1 calc R . . H17C H 1.3537 0.9135 1.0240 0.061 Uiso 1 1 calc R . . C18 C 1.2283(5) 0.6940(5) 0.8898(4) 0.0417(11) Uani 1 1 d . . . H18A H 1.2736 0.7715 0.8840 0.063 Uiso 1 1 calc R . . H18B H 1.1533 0.6859 0.8314 0.063 Uiso 1 1 calc R . . H18C H 1.2816 0.6192 0.8944 0.063 Uiso 1 1 calc R . . C19 C 1.0236(5) 0.5277(5) 0.9332(4) 0.0469(12) Uani 1 1 d . . . H19A H 0.9599 0.4955 0.9591 0.070 Uiso 1 1 calc R . . H19B H 1.0783 0.4572 0.9289 0.070 Uiso 1 1 calc R . . H19C H 0.9834 0.5640 0.8671 0.070 Uiso 1 1 calc R . . C20 C 1.0174(5) 0.6016(5) 1.1497(4) 0.0497(13) Uani 1 1 d . . . H20A H 0.9347 0.5848 1.1016 0.074 Uiso 1 1 calc R . . H20B H 1.0100 0.6608 1.2004 0.074 Uiso 1 1 calc R . . H20C H 1.0544 0.5212 1.1810 0.074 Uiso 1 1 calc R . . C21 C 0.4362(4) 0.6124(4) 0.6543(3) 0.0287(8) Uani 1 1 d . . . C22 C 0.5205(4) 0.5179(4) 0.7143(3) 0.0312(9) Uani 1 1 d . . . C23 C 0.6289(4) 0.5164(4) 0.6859(3) 0.0325(9) Uani 1 1 d . . . C24 C 0.6127(4) 0.6077(4) 0.6086(3) 0.0320(9) Uani 1 1 d . . . C25 C 0.4933(4) 0.6664(4) 0.5883(3) 0.0301(9) Uani 1 1 d . . . C26 C 0.3073(4) 0.6389(5) 0.6543(4) 0.0407(11) Uani 1 1 d . . . H26A H 0.2851 0.7276 0.6342 0.061 Uiso 1 1 calc R . . H26B H 0.3039 0.6252 0.7211 0.061 Uiso 1 1 calc R . . H26C H 0.2486 0.5811 0.6077 0.061 Uiso 1 1 calc R . . C27 C 0.4933(6) 0.4303(5) 0.7873(4) 0.0466(12) Uani 1 1 d . . . H27A H 0.4431 0.3581 0.7521 0.070 Uiso 1 1 calc R . . H27B H 0.4474 0.4772 0.8233 0.070 Uiso 1 1 calc R . . H27C H 0.5717 0.3985 0.8344 0.070 Uiso 1 1 calc R . . C28 C 0.7371(5) 0.4287(5) 0.7270(4) 0.0507(14) Uani 1 1 d . . . H28A H 0.7481 0.4098 0.7964 0.076 Uiso 1 1 calc R . . H28B H 0.8124 0.4697 0.7228 0.076 Uiso 1 1 calc R . . H28C H 0.7219 0.3491 0.6888 0.076 Uiso 1 1 calc R . . C29 C 0.7037(5) 0.6306(6) 0.5551(4) 0.0474(12) Uani 1 1 d . . . H29A H 0.6977 0.5611 0.5078 0.071 Uiso 1 1 calc R . . H29B H 0.7883 0.6336 0.6031 0.071 Uiso 1 1 calc R . . H29C H 0.6846 0.7121 0.5194 0.071 Uiso 1 1 calc R . . C30 C 0.4362(5) 0.7649(5) 0.5114(4) 0.0455(12) Uani 1 1 d . . . H30A H 0.3888 0.7227 0.4491 0.068 Uiso 1 1 calc R . . H30B H 0.5019 0.8176 0.5011 0.068 Uiso 1 1 calc R . . H30C H 0.3804 0.8192 0.5333 0.068 Uiso 1 1 calc R . . B1 B 0.5898(4) 0.9211(5) 0.9180(4) 0.0309(9) Uani 1 1 d . A . B1' B 0.9343(4) 1.0773(4) 0.8458(3) 0.0268(9) Uani 1 1 d . A . B2 B 0.7414(4) 0.9844(4) 0.9702(3) 0.0268(9) Uani 1 1 d . A . B2' B 0.9306(4) 0.9067(4) 0.8641(3) 0.0242(8) Uani 1 1 d . . . H2' H 0.9172 0.8390 0.8008 0.029 Uiso 0.09 1 calc PR A 2 B3 B 0.7173(4) 0.8171(5) 0.9829(3) 0.0272(9) Uani 1 1 d . . . B3' B 1.0735(4) 0.9946(4) 0.9121(3) 0.0264(9) Uani 1 1 d . A . H3' H 1.1481 0.9728 0.8798 0.032 Uiso 1 1 calc R . . B4 B 0.5848(4) 0.7567(5) 0.8866(4) 0.0279(9) Uani 1 1 d . A . B4' B 1.0536(5) 1.1571(4) 0.9408(4) 0.0287(10) Uani 1 1 d . . . B5 B 0.6431(4) 1.0306(4) 0.8483(4) 0.0302(9) Uani 1 1 d . . . B6 B 0.8114(4) 1.0124(4) 0.8809(3) 0.0247(8) Uani 1 1 d . A . B7 B 0.8497(4) 0.8679(4) 0.9517(3) 0.0235(8) Uani 1 1 d . A . B8 B 0.7413(4) 0.7101(4) 0.8992(3) 0.0247(9) Uani 1 1 d . A . H8 H 0.7991 0.6232 0.9003 0.030 Uiso 0.91 1 calc PR B 1 B8' B 1.1155(4) 1.0445(5) 1.0395(3) 0.0279(9) Uani 1 1 d . A . B9' B 1.0147(5) 1.1739(5) 1.0467(4) 0.0305(10) Uani 1 1 d . A . B10 B 0.5334(4) 0.8824(5) 0.7929(4) 0.0304(9) Uani 1 1 d . A . B10' B 0.8951(5) 1.1767(5) 0.9288(4) 0.0296(9) Uani 1 1 d . A . H1 H 0.521(5) 0.958(6) 0.949(4) 0.045(15) Uiso 1 1 d . . . H1' H 0.900(4) 1.104(5) 0.771(4) 0.035(13) Uiso 1 1 d . . . H2 H 0.762(4) 1.045(5) 1.037(4) 0.034(12) Uiso 1 1 d . . . H3 H 0.735(5) 0.782(5) 1.058(4) 0.029(12) Uiso 1 1 d . . . H4 H 0.520(5) 0.702(5) 0.911(4) 0.030(12) Uiso 1 1 d . . . H4' H 1.105(5) 1.229(5) 0.920(4) 0.028(12) Uiso 1 1 d . . . H5 H 0.608(5) 1.127(6) 0.828(4) 0.041(15) Uiso 1 1 d . . . H8' H 1.209(5) 1.048(5) 1.091(4) 0.032(12) Uiso 1 1 d . . . H9' H 1.034(6) 1.250(8) 1.102(5) 0.07(2) Uiso 1 1 d . . . H10 H 0.437(5) 0.915(6) 0.754(4) 0.046(15) Uiso 1 1 d . . . H10' H 0.838(5) 1.270(6) 0.903(4) 0.043(15) Uiso 1 1 d . . . H67 H 0.710(4) 1.006(4) 0.803(3) 0.024(11) Uiso 1 1 d . . . H67' H 0.937(4) 0.881(4) 1.036(3) 0.018(10) Uiso 1 1 d . . . H89 H 0.750(4) 0.730(4) 0.822(3) 0.022(11) Uiso 1 1 d . . . H89' H 1.042(5) 1.069(6) 1.085(4) 0.046(15) Uiso 1 1 d . . . H91 H 0.593(5) 0.876(5) 0.736(4) 0.029(11) Uiso 1 1 d . . . H91' H 0.900(6) 1.151(6) 1.023(5) 0.050(16) 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 Rh7' 0.02075(13) 0.02238(15) 0.02092(14) 0.00061(11) 0.00692(10) -0.00013(10) Rh9 0.02214(14) 0.02301(15) 0.02242(14) 0.00039(11) 0.00479(10) 0.00031(11) Cl2' 0.0328(5) 0.0336(5) 0.0219(5) -0.0036(4) 0.0118(4) -0.0041(4) Cl8 0.054(8) 0.058(8) 0.040(7) 0.000(6) -0.003(6) -0.002(7) C11 0.0281(19) 0.036(2) 0.0226(19) 0.0049(17) 0.0033(15) 0.0086(17) C12 0.0193(18) 0.034(2) 0.030(2) -0.0025(16) 0.0060(15) 0.0022(16) C13 0.0251(19) 0.032(2) 0.031(2) -0.0001(16) 0.0103(17) 0.0078(15) C14 0.0278(19) 0.0229(18) 0.042(2) 0.0006(18) 0.0088(17) 0.0048(16) C15 0.029(2) 0.030(2) 0.040(2) 0.0149(17) 0.0134(18) 0.0098(16) C16 0.043(3) 0.069(3) 0.027(2) -0.001(2) 0.006(2) 0.016(2) C17 0.024(2) 0.047(3) 0.052(3) -0.010(2) 0.013(2) -0.0048(19) C18 0.041(3) 0.055(3) 0.033(2) -0.009(2) 0.016(2) 0.007(2) C19 0.038(2) 0.028(2) 0.068(4) -0.008(2) 0.009(2) 0.0000(19) C20 0.050(3) 0.046(3) 0.060(3) 0.028(2) 0.028(2) 0.007(2) C21 0.0261(19) 0.029(2) 0.027(2) -0.0031(16) 0.0030(15) -0.0040(16) C22 0.037(2) 0.027(2) 0.0255(19) -0.0014(16) 0.0045(16) -0.0018(16) C23 0.032(2) 0.028(2) 0.030(2) -0.0054(16) 0.0012(16) 0.0031(17) C24 0.0297(19) 0.038(2) 0.0282(19) -0.0048(17) 0.0097(16) -0.0027(17) C25 0.032(2) 0.032(2) 0.0204(19) -0.0020(16) 0.0000(16) -0.0015(17) C26 0.026(2) 0.048(3) 0.046(3) -0.008(2) 0.0098(19) -0.001(2) C27 0.066(3) 0.034(2) 0.038(2) 0.004(2) 0.014(2) -0.014(2) C28 0.049(3) 0.044(3) 0.047(3) -0.010(2) 0.001(2) 0.020(2) C29 0.042(3) 0.065(3) 0.040(3) -0.014(2) 0.021(2) -0.005(2) C30 0.053(3) 0.041(3) 0.032(2) 0.013(2) 0.000(2) 0.001(2) B1 0.022(2) 0.032(2) 0.039(2) -0.0038(19) 0.0101(18) 0.0002(17) B1' 0.032(2) 0.026(2) 0.025(2) 0.0047(17) 0.0136(17) -0.0021(17) B2 0.025(2) 0.029(2) 0.029(2) -0.0021(17) 0.0131(17) -0.0010(17) B2' 0.026(2) 0.024(2) 0.0216(19) 0.0016(16) 0.0077(16) -0.0022(16) B3 0.026(2) 0.032(2) 0.025(2) -0.0021(17) 0.0094(17) -0.0053(17) B3' 0.029(2) 0.022(2) 0.028(2) 0.0024(17) 0.0106(17) -0.0027(17) B4 0.023(2) 0.029(2) 0.034(2) -0.0033(18) 0.0120(17) -0.0045(17) B4' 0.029(2) 0.025(2) 0.033(2) 0.0024(17) 0.0118(19) -0.0023(17) B5 0.028(2) 0.025(2) 0.036(2) -0.0023(18) 0.0080(18) 0.0031(17) B6 0.0233(19) 0.026(2) 0.023(2) 0.0015(17) 0.0058(16) -0.0002(17) B7 0.0211(19) 0.026(2) 0.0228(19) 0.0024(16) 0.0062(15) -0.0016(16) B8 0.019(2) 0.026(2) 0.026(2) 0.0024(16) 0.0040(16) 0.0013(15) B8' 0.028(2) 0.027(2) 0.029(2) -0.0047(18) 0.0111(18) -0.0046(18) B9' 0.028(2) 0.027(2) 0.038(3) -0.0047(18) 0.012(2) -0.0048(17) B10 0.025(2) 0.026(2) 0.035(2) -0.0033(18) 0.0035(18) 0.0041(18) B10' 0.030(2) 0.025(2) 0.035(3) 0.0005(18) 0.012(2) -0.0012(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh7' B3' 2.190(4) . ? Rh7' B2' 2.201(4) . ? Rh7' C11 2.206(4) . ? Rh7' C12 2.222(4) . ? Rh7' C15 2.226(4) . ? Rh7' C13 2.233(4) . ? Rh7' B7 2.240(4) . ? Rh7' B8' 2.260(5) . ? Rh7' C14 2.263(4) . ? Rh7' H67' 1.61(4) . ? Rh9 C21 2.163(4) . ? Rh9 C22 2.167(4) . ? Rh9 B4 2.195(5) . ? Rh9 C23 2.197(4) . ? Rh9 C25 2.212(4) . ? Rh9 C24 2.222(4) . ? Rh9 B10 2.231(5) . ? Rh9 B8 2.239(5) . ? Rh9 H89 1.67(5) . ? Rh9 H91 1.79(5) . ? Cl2' B2' 1.823(4) . ? Cl8 B8 1.717(17) . ? C11 C12 1.441(6) . ? C11 C15 1.443(7) . ? C11 C16 1.495(7) . ? C12 C13 1.431(6) . ? C12 C17 1.501(6) . ? C13 C14 1.423(6) . ? C13 C18 1.499(6) . ? C14 C15 1.432(7) . ? C14 C19 1.485(6) . ? C15 C20 1.494(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.431(6) . ? C21 C22 1.444(6) . ? C21 C26 1.496(6) . ? C22 C23 1.424(7) . ? C22 C27 1.500(6) . ? C23 C24 1.427(6) . ? C23 C28 1.492(6) . ? C24 C25 1.433(6) . ? C24 C29 1.501(7) . ? C25 C30 1.490(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? B1 B10 1.737(7) . ? B1 B5 1.756(7) . ? B1 B2 1.767(6) . ? B1 B4 1.774(7) . ? B1 B3 1.805(7) . ? B1 H1 1.09(6) . ? B1' B10' 1.746(7) . ? B1' B6 1.775(6) . ? B1' B4' 1.778(7) . ? B1' B3' 1.778(6) . ? B1' B2' 1.806(6) . ? B1' H1' 1.04(5) . ? B2 B6 1.745(6) . ? B2 B3 1.790(7) . ? B2 B5 1.797(7) . ? B2 B7 1.817(6) . ? B2 H2 1.11(5) . ? B2' B3' 1.796(6) . ? B2' B6 1.829(6) . ? B2' B7 1.835(6) . ? B2' H2' 1.1200 . ? B3 B8 1.728(7) . ? B3 B4 1.786(6) . ? B3 B7 1.793(6) . ? B3 H3 1.09(5) . ? B3' B4' 1.781(6) . ? B3' B8' 1.802(6) . ? B3' H3' 1.1200 . ? B4 B8 1.800(6) . ? B4 B10 1.830(7) . ? B4 H4 1.09(5) . ? B4' B9' 1.726(7) . ? B4' B10' 1.770(7) . ? B4' B8' 1.794(7) . ? B4' H4' 1.05(5) . ? B5 B6 1.827(6) . ? B5 B10 1.983(7) . ? B5 H5 1.09(6) . ? B5 H67 1.18(5) . ? B6 B7 1.791(6) . ? B6 B10' 1.974(6) . ? B6 H67 1.32(4) . ? B7 B8 2.049(6) . ? B7 H67' 1.29(4) . ? B8 H8 1.1200 . ? B8 H89 1.17(5) . ? B8' B9' 1.801(7) . ? B8' H8' 1.08(5) . ? B8' H89' 1.25(6) . ? B9' B10' 1.781(7) . ? B9' H9' 1.09(8) . ? B9' H89' 1.22(6) . ? B9' H91' 1.26(6) . ? B10 H10 1.11(5) . ? B10 H91 1.23(5) . ? B10' H10' 1.16(6) . ? B10' H91' 1.36(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 B3' Rh7' B2' 48.29(16) . . ? B3' Rh7' C11 130.58(17) . . ? B2' Rh7' C11 171.64(16) . . ? B3' Rh7' C12 99.19(17) . . ? B2' Rh7' C12 135.13(16) . . ? C11 Rh7' C12 38.00(16) . . ? B3' Rh7' C15 160.30(17) . . ? B2' Rh7' C15 139.55(17) . . ? C11 Rh7' C15 37.99(17) . . ? C12 Rh7' C15 62.75(16) . . ? B3' Rh7' C13 98.70(17) . . ? B2' Rh7' C13 108.36(16) . . ? C11 Rh7' C13 63.28(16) . . ? C12 Rh7' C13 37.48(16) . . ? C15 Rh7' C13 62.37(16) . . ? B3' Rh7' B7 88.59(16) . . ? B2' Rh7' B7 48.80(15) . . ? C11 Rh7' B7 137.00(16) . . ? C12 Rh7' B7 171.00(18) . . ? C15 Rh7' B7 108.86(16) . . ? C13 Rh7' B7 137.07(17) . . ? B3' Rh7' B8' 47.74(16) . . ? B2' Rh7' B8' 86.17(17) . . ? C11 Rh7' B8' 97.76(17) . . ? C12 Rh7' B8' 90.04(16) . . ? C15 Rh7' B8' 133.95(17) . . ? C13 Rh7' B8' 117.56(16) . . ? B7 Rh7' B8' 98.58(17) . . ? B3' Rh7' C14 129.01(17) . . ? B2' Rh7' C14 110.61(16) . . ? C11 Rh7' C14 62.95(16) . . ? C12 Rh7' C14 62.16(15) . . ? C15 Rh7' C14 37.21(17) . . ? C13 Rh7' C14 36.91(16) . . ? B7 Rh7' C14 109.35(16) . . ? B8' Rh7' C14 152.00(17) . . ? B3' Rh7' H67' 102.2(16) . . ? B2' Rh7' H67' 78.7(15) . . ? C11 Rh7' H67' 108.9(15) . . ? C12 Rh7' H67' 145.4(15) . . ? C15 Rh7' H67' 97.4(16) . . ? C13 Rh7' H67' 156.6(16) . . ? B7 Rh7' H67' 34.5(15) . . ? B8' Rh7' H67' 84.6(16) . . ? C14 Rh7' H67' 119.8(16) . . ? C21 Rh9 C22 38.95(16) . . ? C21 Rh9 B4 108.09(16) . . ? C22 Rh9 B4 103.04(17) . . ? C21 Rh9 C23 64.24(16) . . ? C22 Rh9 C23 38.09(18) . . ? B4 Rh9 C23 129.67(18) . . ? C21 Rh9 C25 38.16(17) . . ? C22 Rh9 C25 64.00(16) . . ? B4 Rh9 C25 140.94(17) . . ? C23 Rh9 C25 63.35(16) . . ? C21 Rh9 C24 63.75(16) . . ? C22 Rh9 C24 63.55(17) . . ? B4 Rh9 C24 166.32(17) . . ? C23 Rh9 C24 37.68(17) . . ? C25 Rh9 C24 37.70(16) . . ? C21 Rh9 B10 102.06(16) . . ? C22 Rh9 B10 128.71(18) . . ? B4 Rh9 B10 48.84(18) . . ? C23 Rh9 B10 165.88(16) . . ? C25 Rh9 B10 108.51(16) . . ? C24 Rh9 B10 141.17(17) . . ? C21 Rh9 B8 141.60(16) . . ? C22 Rh9 B8 109.43(16) . . ? B4 Rh9 B8 47.89(17) . . ? C23 Rh9 B8 105.45(15) . . ? C25 Rh9 B8 168.46(16) . . ? C24 Rh9 B8 131.46(16) . . ? B10 Rh9 B8 83.02(17) . . ? C21 Rh9 H89 162.3(16) . . ? C22 Rh9 H89 123.5(16) . . ? B4 Rh9 H89 74.6(17) . . ? C23 Rh9 H89 100.2(16) . . ? C25 Rh9 H89 144.1(17) . . ? C24 Rh9 H89 109.7(17) . . ? B10 Rh9 H89 92.8(16) . . ? B8 Rh9 H89 30.5(17) . . ? C21 Rh9 H91 111.8(16) . . ? C22 Rh9 H91 150.2(16) . . ? B4 Rh9 H91 77.9(17) . . ? C23 Rh9 H91 152.5(17) . . ? C25 Rh9 H91 96.2(16) . . ? C24 Rh9 H91 115.0(17) . . ? B10 Rh9 H91 33.4(16) . . ? B8 Rh9 H91 93.4(16) . . ? H89 Rh9 H91 86(2) . . ? C12 C11 C15 106.8(4) . . ? C12 C11 C16 126.4(4) . . ? C15 C11 C16 126.7(4) . . ? C12 C11 Rh7' 71.6(2) . . ? C15 C11 Rh7' 71.8(2) . . ? C16 C11 Rh7' 124.2(3) . . ? C13 C12 C11 108.3(4) . . ? C13 C12 C17 124.5(4) . . ? C11 C12 C17 126.9(4) . . ? C13 C12 Rh7' 71.7(2) . . ? C11 C12 Rh7' 70.4(2) . . ? C17 C12 Rh7' 128.3(3) . . ? C14 C13 C12 108.4(4) . . ? C14 C13 C18 125.7(4) . . ? C12 C13 C18 125.7(4) . . ? C14 C13 Rh7' 72.7(2) . . ? C12 C13 Rh7' 70.8(2) . . ? C18 C13 Rh7' 126.8(3) . . ? C13 C14 C15 107.9(4) . . ? C13 C14 C19 124.4(4) . . ? C15 C14 C19 127.5(5) . . ? C13 C14 Rh7' 70.4(2) . . ? C15 C14 Rh7' 70.0(2) . . ? C19 C14 Rh7' 129.4(3) . . ? C14 C15 C11 108.5(4) . . ? C14 C15 C20 126.2(5) . . ? C11 C15 C20 125.3(5) . . ? C14 C15 Rh7' 72.8(2) . . ? C11 C15 Rh7' 70.2(2) . . ? C20 C15 Rh7' 125.2(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 107.7(4) . . ? C25 C21 C26 126.2(4) . . ? C22 C21 C26 125.8(4) . . ? C25 C21 Rh9 72.7(2) . . ? C22 C21 Rh9 70.7(2) . . ? C26 C21 Rh9 126.8(3) . . ? C23 C22 C21 107.9(4) . . ? C23 C22 C27 126.4(4) . . ? C21 C22 C27 125.5(4) . . ? C23 C22 Rh9 72.1(2) . . ? C21 C22 Rh9 70.4(2) . . ? C27 C22 Rh9 126.7(3) . . ? C22 C23 C24 108.3(4) . . ? C22 C23 C28 125.2(4) . . ? C24 C23 C28 126.4(4) . . ? C22 C23 Rh9 69.8(2) . . ? C24 C23 Rh9 72.1(2) . . ? C28 C23 Rh9 126.3(3) . . ? C23 C24 C25 108.1(4) . . ? C23 C24 C29 124.8(4) . . ? C25 C24 C29 127.0(4) . . ? C23 C24 Rh9 70.2(2) . . ? C25 C24 Rh9 70.7(2) . . ? C29 C24 Rh9 127.4(3) . . ? C21 C25 C24 108.0(4) . . ? C21 C25 C30 125.4(4) . . ? C24 C25 C30 126.6(4) . . ? C21 C25 Rh9 69.1(2) . . ? C24 C25 Rh9 71.6(2) . . ? C30 C25 Rh9 125.6(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? B10 B1 B5 69.2(3) . . ? B10 B1 B2 119.7(3) . . ? B5 B1 B2 61.3(3) . . ? B10 B1 B4 62.8(3) . . ? B5 B1 B4 118.4(3) . . ? B2 B1 B4 114.5(3) . . ? B10 B1 B3 110.3(3) . . ? B5 B1 B3 108.2(3) . . ? B2 B1 B3 60.1(2) . . ? B4 B1 B3 59.9(3) . . ? B10 B1 H1 116(3) . . ? B5 B1 H1 116(3) . . ? B2 B1 H1 115(3) . . ? B4 B1 H1 118(3) . . ? B3 B1 H1 124(3) . . ? B10' B1' B6 68.2(3) . . ? B10' B1' B4' 60.3(3) . . ? B6 B1' B4' 116.0(3) . . ? B10' B1' B3' 108.2(3) . . ? B6 B1' B3' 108.1(3) . . ? B4' B1' B3' 60.1(3) . . ? B10' B1' B2' 117.7(3) . . ? B6 B1' B2' 61.4(2) . . ? B4' B1' B2' 113.7(3) . . ? B3' B1' B2' 60.1(2) . . ? B10' B1' H1' 116(3) . . ? B6 B1' H1' 110(3) . . ? B4' B1' H1' 126(3) . . ? B3' B1' H1' 130(3) . . ? B2' B1' H1' 113(3) . . ? B6 B2 B1 112.0(3) . . ? B6 B2 B3 111.2(3) . . ? B1 B2 B3 61.0(3) . . ? B6 B2 B5 62.1(3) . . ? B1 B2 B5 59.0(3) . . ? B3 B2 B5 107.1(3) . . ? B6 B2 B7 60.3(2) . . ? B1 B2 B7 107.6(3) . . ? B3 B2 B7 59.6(3) . . ? B5 B2 B7 105.8(3) . . ? B6 B2 H2 122(3) . . ? B1 B2 H2 118(3) . . ? B3 B2 H2 118(3) . . ? B5 B2 H2 125(3) . . ? B7 B2 H2 124(3) . . ? B3' B2' B1' 59.2(2) . . ? B3' B2' Cl2' 114.1(3) . . ? B1' B2' Cl2' 111.6(3) . . ? B3' B2' B6 105.1(3) . . ? B1' B2' B6 58.5(2) . . ? Cl2' B2' B6 124.3(3) . . ? B3' B2' B7 116.8(3) . . ? B1' B2' B7 111.1(3) . . ? Cl2' B2' B7 125.0(3) . . ? B6 B2' B7 58.5(2) . . ? B3' B2' Rh7' 65.51(19) . . ? B1' B2' Rh7' 114.7(3) . . ? Cl2' B2' Rh7' 120.9(2) . . ? B6 B2' Rh7' 110.6(2) . . ? B7 B2' Rh7' 66.69(18) . . ? B3' B2' H2' 119.6 . . ? B1' B2' H2' 120.7 . . ? Cl2' B2' H2' 9.4 . . ? B6 B2' H2' 125.6 . . ? B7 B2' H2' 116.7 . . ? Rh7' B2' H2' 115.0 . . ? B8 B3 B4 61.6(3) . . ? B8 B3 B2 119.8(3) . . ? B4 B3 B2 112.7(3) . . ? B8 B3 B7 71.1(3) . . ? B4 B3 B7 118.5(3) . . ? B2 B3 B7 60.9(3) . . ? B8 B3 B1 108.7(3) . . ? B4 B3 B1 59.2(3) . . ? B2 B3 B1 58.9(3) . . ? B7 B3 B1 107.1(3) . . ? B8 B3 H3 116(3) . . ? B4 B3 H3 118(3) . . ? B2 B3 H3 117(3) . . ? B7 B3 H3 117(3) . . ? B1 B3 H3 125(3) . . ? B1' B3' B4' 59.9(3) . . ? B1' B3' B2' 60.7(2) . . ? B4' B3' B2' 114.0(3) . . ? B1' B3' B8' 106.7(3) . . ? B4' B3' B8' 60.1(3) . . ? B2' B3' B8' 115.8(3) . . ? B1' B3' Rh7' 116.5(3) . . ? B4' B3' Rh7' 121.5(3) . . ? B2' B3' Rh7' 66.20(19) . . ? B8' B3' Rh7' 68.2(2) . . ? B1' B3' H3' 123.0 . . ? B4' B3' H3' 117.6 . . ? B2' B3' H3' 117.1 . . ? B8' B3' H3' 119.8 . . ? Rh7' B3' H3' 110.4 . . ? B1 B4 B3 60.9(3) . . ? B1 B4 B8 106.9(3) . . ? B3 B4 B8 57.6(3) . . ? B1 B4 B10 57.6(3) . . ? B3 B4 B10 107.0(3) . . ? B8 B4 B10 109.4(3) . . ? B1 B4 Rh9 117.9(3) . . ? B3 B4 Rh9 118.5(3) . . ? B8 B4 Rh9 67.3(2) . . ? B10 B4 Rh9 66.6(2) . . ? B1 B4 H4 114(3) . . ? B3 B4 H4 115(3) . . ? B8 B4 H4 126(3) . . ? B10 B4 H4 122(3) . . ? Rh9 B4 H4 118(3) . . ? B9' B4' B10' 61.2(3) . . ? B9' B4' B1' 111.4(3) . . ? B10' B4' B1' 59.0(3) . . ? B9' B4' B3' 113.0(3) . . ? B10' B4' B3' 107.0(3) . . ? B1' B4' B3' 60.0(3) . . ? B9' B4' B8' 61.5(3) . . ? B10' B4' B8' 105.8(3) . . ? B1' B4' B8' 107.1(3) . . ? B3' B4' B8' 60.5(2) . . ? B9' B4' H4' 120(3) . . ? B10' B4' H4' 123(3) . . ? B1' B4' H4' 119(3) . . ? B3' B4' H4' 119(3) . . ? B8' B4' H4' 125(3) . . ? B1 B5 B2 59.6(3) . . ? B1 B5 B6 108.7(3) . . ? B2 B5 B6 57.5(2) . . ? B1 B5 B10 55.0(3) . . ? B2 B5 B10 106.5(3) . . ? B6 B5 B10 119.3(3) . . ? B1 B5 H5 126(3) . . ? B2 B5 H5 124(3) . . ? B6 B5 H5 115(3) . . ? B10 B5 H5 119(3) . . ? B1 B5 H67 126(2) . . ? B2 B5 H67 100(2) . . ? B6 B5 H67 46(2) . . ? B10 B5 H67 93(2) . . ? H5 B5 H67 107(4) . . ? B2 B6 B1' 150.5(3) . . ? B2 B6 B7 61.8(2) . . ? B1' B6 B7 114.7(3) . . ? B2 B6 B5 60.4(3) . . ? B1' B6 B5 138.5(3) . . ? B7 B6 B5 105.6(3) . . ? B2 B6 B2' 122.5(3) . . ? B1' B6 B2' 60.1(2) . . ? B7 B6 B2' 60.9(2) . . ? B5 B6 B2' 142.4(3) . . ? B2 B6 B10' 100.2(3) . . ? B1' B6 B10' 55.2(2) . . ? B7 B6 B10' 122.7(3) . . ? B5 B6 B10' 110.0(3) . . ? B2' B6 B10' 106.1(3) . . ? B2 B6 H67 97(2) . . ? B1' B6 H67 109(2) . . ? B7 B6 H67 115(2) . . ? B5 B6 H67 40(2) . . ? B2' B6 H67 110(2) . . ? B10' B6 H67 122(2) . . ? B6 B7 B3 109.0(3) . . ? B6 B7 B2 57.8(2) . . ? B3 B7 B2 59.5(3) . . ? B6 B7 B2' 60.6(2) . . ? B3 B7 B2' 153.5(3) . . ? B2 B7 B2' 118.2(3) . . ? B6 B7 B8 118.0(3) . . ? B3 B7 B8 53.0(2) . . ? B2 B7 B8 103.8(3) . . ? B2' B7 B8 107.9(3) . . ? B6 B7 Rh7' 110.4(2) . . ? B3 B7 Rh7' 137.7(3) . . ? B2 B7 Rh7' 136.3(3) . . ? B2' B7 Rh7' 64.51(18) . . ? B8 B7 Rh7' 117.0(2) . . ? B6 B7 H67' 114(2) . . ? B3 B7 H67' 104.3(19) . . ? B2 B7 H67' 97.9(19) . . ? B2' B7 H67' 102.2(19) . . ? B8 B7 H67' 128(2) . . ? Rh7' B7 H67' 44.8(19) . . ? Cl8 B8 B3 110.1(6) . . ? Cl8 B8 B4 114.2(6) . . ? B3 B8 B4 60.8(3) . . ? Cl8 B8 B7 120.2(5) . . ? B3 B8 B7 55.9(2) . . ? B4 B8 B7 106.0(3) . . ? Cl8 B8 Rh9 115.8(5) . . ? B3 B8 Rh9 119.0(3) . . ? B4 B8 Rh9 64.8(2) . . ? B7 B8 Rh9 120.9(2) . . ? Cl8 B8 H8 36.4 . . ? B3 B8 H8 138.2 . . ? B4 B8 H8 141.4 . . ? B7 B8 H8 111.6 . . ? Rh9 B8 H8 101.8 . . ? Cl8 B8 H89 120(2) . . ? B3 B8 H89 129(2) . . ? B4 B8 H89 105(2) . . ? B7 B8 H89 88(2) . . ? Rh9 B8 H89 47(2) . . ? H8 B8 H89 85.6 . . ? B4' B8' B9' 57.4(3) . . ? B4' B8' B3' 59.4(3) . . ? B9' B8' B3' 108.5(3) . . ? B4' B8' Rh7' 117.2(3) . . ? B9' B8' Rh7' 125.0(3) . . ? B3' B8' Rh7' 64.1(2) . . ? B4' B8' H8' 124(3) . . ? B9' B8' H8' 116(3) . . ? B3' B8' H8' 125(3) . . ? Rh7' B8' H8' 109(3) . . ? B4' B8' H89' 97(3) . . ? B9' B8' H89' 43(3) . . ? B3' B8' H89' 126(3) . . ? Rh7' B8' H89' 95(3) . . ? H8' B8' H89' 108(4) . . ? B4' B9' B10' 60.6(3) . . ? B4' B9' B8' 61.1(3) . . ? B10' B9' B8' 105.0(3) . . ? B4' B9' H9' 131(4) . . ? B10' B9' H9' 126(4) . . ? B8' B9' H9' 127(4) . . ? B4' B9' H89' 101(3) . . ? B10' B9' H89' 116(3) . . ? B8' B9' H89' 44(3) . . ? H9' B9' H89' 112(5) . . ? B4' B9' H91' 107(3) . . ? B10' B9' H91' 50(3) . . ? B8' B9' H91' 118(3) . . ? H9' B9' H91' 106(5) . . ? H89' B9' H91' 92(4) . . ? B1 B10 B4 59.6(3) . . ? B1 B10 B5 55.9(3) . . ? B4 B10 B5 105.3(3) . . ? B1 B10 Rh9 117.8(3) . . ? B4 B10 Rh9 64.6(2) . . ? B5 B10 Rh9 121.6(3) . . ? B1 B10 H10 114(3) . . ? B4 B10 H10 127(3) . . ? B5 B10 H10 111(3) . . ? Rh9 B10 H10 120(3) . . ? B1 B10 H91 127(2) . . ? B4 B10 H91 110(2) . . ? B5 B10 H91 84(2) . . ? Rh9 B10 H91 53(2) . . ? H10 B10 H91 111(4) . . ? B1' B10' B4' 60.7(3) . . ? B1' B10' B9' 110.3(3) . . ? B4' B10' B9' 58.2(3) . . ? B1' B10' B6 56.6(2) . . ? B4' B10' B6 107.0(3) . . ? B9' B10' B6 116.3(3) . . ? B1' B10' H10' 122(3) . . ? B4' B10' H10' 125(3) . . ? B9' B10' H10' 119(3) . . ? B6 B10' H10' 118(3) . . ? B1' B10' H91' 129(3) . . ? B4' B10' H91' 101(3) . . ? B9' B10' H91' 45(3) . . ? B6 B10' H91' 92(3) . . ? H10' B10' H91' 108(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.591 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.060 # Attachment 'B709470A CCDC 644827.cif' data_mc37b1 _database_code_depnum_ccdc_archive 'CCDC 644827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H28 B9 Rh' _chemical_formula_sum 'C10 H28 B9 Rh' _chemical_formula_weight 348.52 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' B B 0.0013 0.0007 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.0218(5) _cell_length_b 11.5559(5) _cell_length_c 13.4953(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1718.85(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9090 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _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_collimation miracol _diffrn_radiation_polarisn_norm ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10060 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1762 _reflns_number_gt 1497 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; 'enCIFer (CCDC, 2002)' ; _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. Cage hydrogen atoms not located due to the disorder associated with the boron cage itself. Disorder across the plane containing Rh5, B7 and B8, which is a crystallographic mirror plane but only a pseudo-mirror plane for the molecule. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+3.7852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1762 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 Rh5 Rh 0.18483(4) 0.2500 0.55698(4) 0.0395(2) Uani 1 2 d S . . C11 C 0.2522(4) 0.1878(4) 0.7010(3) 0.0459(11) Uani 1 1 d . . . C12 C 0.3336(4) 0.1496(4) 0.6244(4) 0.0472(11) Uani 1 1 d . . . C13 C 0.3834(6) 0.2500 0.5779(5) 0.0483(16) Uani 1 2 d S . . C14 C 0.1865(5) 0.1113(5) 0.7722(4) 0.0686(15) Uani 1 1 d . . . H14A H 0.2385 0.0958 0.8296 0.103 Uiso 1 1 calc R . . H14B H 0.1658 0.0382 0.7396 0.103 Uiso 1 1 calc R . . H14C H 0.1120 0.1498 0.7943 0.103 Uiso 1 1 calc R . . C15 C 0.3665(5) 0.0277(5) 0.6009(5) 0.0671(15) Uani 1 1 d . . . H15A H 0.3788 0.0197 0.5293 0.101 Uiso 1 1 calc R . . H15B H 0.3008 -0.0239 0.6221 0.101 Uiso 1 1 calc R . . H15C H 0.4414 0.0070 0.6357 0.101 Uiso 1 1 calc R . . C16 C 0.4767(7) 0.2500 0.4963(7) 0.066(2) Uani 1 2 d S . . H16A H 0.5552 0.2253 0.5230 0.099 Uiso 0.50 1 calc PR . . H16B H 0.4842 0.3282 0.4689 0.099 Uiso 0.50 1 calc PR . . H16C H 0.4514 0.1965 0.4439 0.099 Uiso 0.50 1 calc PR . . B1 B 0.0643(18) 0.3818(13) 0.5094(14) 0.097(6) Uani 0.50 1 d P . . B3 B 0.023(2) 0.3683(19) 0.3678(19) 0.123(11) Uani 0.50 1 d P . . B4 B -0.067(5) 0.366(2) 0.455(4) 0.30(4) Uani 0.50 1 d P . . B7 B 0.0718(11) 0.2500 0.3247(8) 0.099(5) Uani 1 2 d S . . B8 B -0.0863(11) 0.2500 0.3717(8) 0.088(3) Uani 1 2 d S . . B9 B -0.1115(14) 0.218(4) 0.4975(11) 0.17(2) Uani 0.50 1 d P . . B10 B -0.0110(9) 0.2825(19) 0.5812(9) 0.078(10) Uani 0.50 1 d P . . B16 B 0.1722(8) 0.3216(9) 0.4048(6) 0.091(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh5 0.0389(3) 0.0314(3) 0.0483(3) 0.000 -0.0060(2) 0.000 C11 0.042(2) 0.047(2) 0.048(2) 0.005(2) -0.009(2) -0.001(2) C12 0.041(2) 0.037(2) 0.063(3) 0.001(2) -0.013(2) 0.0028(19) C13 0.036(3) 0.049(4) 0.059(4) 0.000 0.001(3) 0.000 C14 0.074(4) 0.072(4) 0.060(3) 0.020(3) -0.007(3) -0.012(3) C15 0.058(3) 0.041(3) 0.102(4) -0.003(3) -0.014(3) 0.010(2) C16 0.049(4) 0.070(5) 0.080(5) 0.000 0.009(4) 0.000 B1 0.128(14) 0.052(8) 0.110(12) -0.014(8) -0.069(12) 0.024(9) B3 0.16(2) 0.075(13) 0.137(18) 0.060(14) -0.118(17) -0.045(14) B4 0.45(8) 0.067(16) 0.38(7) -0.03(3) -0.34(7) 0.07(3) B7 0.071(7) 0.178(16) 0.048(5) 0.000 -0.011(5) 0.000 B8 0.081(7) 0.113(9) 0.068(6) 0.000 -0.038(6) 0.000 B9 0.056(8) 0.39(6) 0.059(8) 0.059(19) -0.025(7) -0.14(2) B10 0.028(4) 0.15(3) 0.060(6) -0.029(10) 0.000(4) 0.018(8) B16 0.086(5) 0.116(7) 0.071(4) 0.032(5) -0.022(4) -0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh5 B1 2.120(14) 8_565 ? Rh5 B1 2.120(14) . ? Rh5 C11 2.201(4) 8_565 ? Rh5 C11 2.201(4) . ? Rh5 C12 2.205(4) 8_565 ? Rh5 C12 2.205(4) . ? Rh5 C13 2.207(7) . ? Rh5 B10 2.215(11) 8_565 ? Rh5 B10 2.215(11) . ? Rh5 B16 2.219(8) 8_565 ? Rh5 B16 2.219(8) . ? C11 C11 1.438(9) 8_565 ? C11 C12 1.438(7) . ? C11 C14 1.493(7) . ? C12 C13 1.428(6) . ? C12 C15 1.489(7) . ? C13 C12 1.428(6) 8_565 ? C13 C16 1.507(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? B1 B4 1.63(4) . ? B1 B10 1.72(3) . ? B1 B3 1.97(3) . ? B1 B16 1.97(2) . ? B3 B4 1.54(7) . ? B3 B7 1.58(3) . ? B3 B16 1.80(3) . ? B3 B8 1.82(2) . ? B4 B9 1.22(7) 8_565 ? B4 B8 1.76(4) . ? B4 B9 1.87(6) . ? B4 B10 2.05(4) . ? B7 B3 1.58(3) 8_565 ? B7 B16 1.754(12) . ? B7 B16 1.754(12) 8_565 ? B7 B8 1.855(17) . ? B8 B4 1.76(4) 8_565 ? B8 B9 1.762(19) 8_565 ? B8 B9 1.762(19) . ? B8 B3 1.82(2) 8_565 ? B9 B9 0.75(9) 8_565 ? B9 B4 1.22(7) 8_565 ? B9 B10 1.582(18) 8_565 ? B9 B10 1.75(2) . ? B10 B10 0.75(4) 8_565 ? B10 B9 1.582(18) 8_565 ? B16 B16 1.65(2) 8_565 ? 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 B1 Rh5 B1 91.8(9) 8_565 . ? B1 Rh5 C11 135.5(5) 8_565 8_565 ? B1 Rh5 C11 104.1(4) . 8_565 ? B1 Rh5 C11 104.1(4) 8_565 . ? B1 Rh5 C11 135.5(5) . . ? C11 Rh5 C11 38.1(2) 8_565 . ? B1 Rh5 C12 165.6(4) 8_565 8_565 ? B1 Rh5 C12 102.3(5) . 8_565 ? C11 Rh5 C12 38.09(18) 8_565 8_565 ? C11 Rh5 C12 63.67(18) . 8_565 ? B1 Rh5 C12 102.3(5) 8_565 . ? B1 Rh5 C12 165.6(4) . . ? C11 Rh5 C12 63.67(18) 8_565 . ? C11 Rh5 C12 38.09(18) . . ? C12 Rh5 C12 63.5(2) 8_565 . ? B1 Rh5 C13 131.3(6) 8_565 . ? B1 Rh5 C13 131.3(6) . . ? C11 Rh5 C13 63.4(2) 8_565 . ? C11 Rh5 C13 63.4(2) . . ? C12 Rh5 C13 37.77(15) 8_565 . ? C12 Rh5 C13 37.77(15) . . ? B1 Rh5 B10 46.6(8) 8_565 8_565 ? B1 Rh5 B10 63.6(8) . 8_565 ? C11 Rh5 B10 104.7(4) 8_565 8_565 ? C11 Rh5 B10 98.2(4) . 8_565 ? C12 Rh5 B10 138.8(5) 8_565 8_565 ? C12 Rh5 B10 125.1(5) . 8_565 ? C13 Rh5 B10 161.3(4) . 8_565 ? B1 Rh5 B10 63.6(8) 8_565 . ? B1 Rh5 B10 46.6(8) . . ? C11 Rh5 B10 98.2(4) 8_565 . ? C11 Rh5 B10 104.7(4) . . ? C12 Rh5 B10 125.1(5) 8_565 . ? C12 Rh5 B10 138.8(5) . . ? C13 Rh5 B10 161.3(4) . . ? B10 Rh5 B10 19.5(11) 8_565 . ? B1 Rh5 B16 54.0(6) 8_565 8_565 ? B1 Rh5 B16 87.0(5) . 8_565 ? C11 Rh5 B16 163.8(2) 8_565 8_565 ? C11 Rh5 B16 135.8(3) . 8_565 ? C12 Rh5 B16 128.7(3) 8_565 8_565 ? C12 Rh5 B16 103.5(3) . 8_565 ? C13 Rh5 B16 100.4(3) . 8_565 ? B10 Rh5 B16 90.7(4) 8_565 8_565 ? B10 Rh5 B16 98.0(4) . 8_565 ? B1 Rh5 B16 87.0(5) 8_565 . ? B1 Rh5 B16 54.0(6) . . ? C11 Rh5 B16 135.8(3) 8_565 . ? C11 Rh5 B16 163.8(2) . . ? C12 Rh5 B16 103.5(3) 8_565 . ? C12 Rh5 B16 128.7(3) . . ? C13 Rh5 B16 100.4(3) . . ? B10 Rh5 B16 98.0(4) 8_565 . ? B10 Rh5 B16 90.7(4) . . ? B16 Rh5 B16 43.8(6) 8_565 . ? C11 C11 C12 107.8(3) 8_565 . ? C11 C11 C14 126.3(3) 8_565 . ? C12 C11 C14 125.7(4) . . ? C11 C11 Rh5 70.94(12) 8_565 . ? C12 C11 Rh5 71.1(3) . . ? C14 C11 Rh5 126.7(3) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 C15 125.5(5) . . ? C11 C12 C15 126.5(5) . . ? C13 C12 Rh5 71.2(3) . . ? C11 C12 Rh5 70.8(2) . . ? C15 C12 Rh5 126.2(4) . . ? C12 C13 C12 108.6(6) 8_565 . ? C12 C13 C16 125.7(3) 8_565 . ? C12 C13 C16 125.7(3) . . ? C12 C13 Rh5 71.1(3) 8_565 . ? C12 C13 Rh5 71.1(3) . . ? C16 C13 Rh5 125.7(5) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? B4 B1 B10 75(2) . . ? B4 B1 B3 50(2) . . ? B10 B1 B3 112.6(12) . . ? B4 B1 B16 100(2) . . ? B10 B1 B16 117.4(10) . . ? B3 B1 B16 54.3(11) . . ? B4 B1 Rh5 127.5(13) . . ? B10 B1 Rh5 69.6(7) . . ? B3 B1 Rh5 112.4(12) . . ? B16 B1 Rh5 65.5(6) . . ? B4 B3 B7 118.8(17) . . ? B4 B3 B16 111.7(16) . . ? B7 B3 B16 62.2(12) . . ? B4 B3 B8 62.3(16) . . ? B7 B3 B8 65.6(10) . . ? B16 B3 B8 111.8(11) . . ? B4 B3 B1 53.8(16) . . ? B7 B3 B1 110.4(11) . . ? B16 B3 B1 62.9(8) . . ? B8 B3 B1 100.6(13) . . ? B9 B4 B3 129(3) 8_565 . ? B9 B4 B1 104(2) 8_565 . ? B3 B4 B1 77(3) . . ? B9 B4 B8 69.8(19) 8_565 . ? B3 B4 B8 67(2) . . ? B1 B4 B8 119(3) . . ? B9 B4 B9 14.4(19) 8_565 . ? B3 B4 B9 115(3) . . ? B1 B4 B9 101.6(16) . . ? B8 B4 B9 58.0(13) . . ? B9 B4 B10 50.4(16) 8_565 . ? B3 B4 B10 117(3) . . ? B1 B4 B10 54.1(12) . . ? B8 B4 B10 102.3(14) . . ? B9 B4 B10 52.8(12) . . ? B3 B7 B3 119.9(19) 8_565 . ? B3 B7 B16 113.3(9) 8_565 . ? B3 B7 B16 65.1(8) . . ? B3 B7 B16 65.1(8) 8_565 8_565 ? B3 B7 B16 113.3(9) . 8_565 ? B16 B7 B16 56.3(7) . 8_565 ? B3 B7 B8 63.6(10) 8_565 . ? B3 B7 B8 63.6(10) . . ? B16 B7 B8 112.5(7) . . ? B16 B7 B8 112.5(7) 8_565 . ? B4 B8 B4 99(3) . 8_565 ? B4 B8 B9 41(2) . 8_565 ? B4 B8 B9 64(2) 8_565 8_565 ? B4 B8 B9 64(2) . . ? B4 B8 B9 41(2) 8_565 . ? B9 B8 B9 25(3) 8_565 . ? B4 B8 B3 51(2) . . ? B4 B8 B3 120.4(13) 8_565 . ? B9 B8 B3 88.4(17) 8_565 . ? B9 B8 B3 107.0(13) . . ? B4 B8 B3 120.4(13) . 8_565 ? B4 B8 B3 51(2) 8_565 8_565 ? B9 B8 B3 107.0(13) 8_565 8_565 ? B9 B8 B3 88.4(17) . 8_565 ? B3 B8 B3 97(2) . 8_565 ? B4 B8 B7 96(2) . . ? B4 B8 B7 96(2) 8_565 . ? B9 B8 B7 118.5(8) 8_565 . ? B9 B8 B7 118.5(8) . . ? B3 B8 B7 50.8(11) . . ? B3 B8 B7 50.8(11) 8_565 . ? B9 B9 B4 142(3) 8_565 8_565 ? B9 B9 B10 90.0(18) 8_565 8_565 ? B4 B9 B10 93(3) 8_565 8_565 ? B9 B9 B10 64.6(16) 8_565 . ? B4 B9 B10 113(2) 8_565 . ? B10 B9 B10 25.4(15) 8_565 . ? B9 B9 B8 77.7(15) 8_565 . ? B4 B9 B8 70(2) 8_565 . ? B10 B9 B8 125.3(9) 8_565 . ? B10 B9 B8 115.5(13) . . ? B9 B9 B4 24(2) 8_565 . ? B4 B9 B4 118(5) 8_565 . ? B10 B9 B4 92.0(18) 8_565 . ? B10 B9 B4 68.9(16) . . ? B8 B9 B4 57.8(18) . . ? B10 B10 B9 90.0(18) 8_565 8_565 ? B10 B10 B1 132.0(8) 8_565 . ? B9 B10 B1 86.3(17) 8_565 . ? B10 B10 B9 64.6(16) 8_565 . ? B9 B10 B9 25(3) 8_565 . ? B1 B10 B9 103.2(11) . . ? B10 B10 B4 117.9(10) 8_565 . ? B9 B10 B4 37(2) 8_565 . ? B1 B10 B4 50.4(17) . . ? B9 B10 B4 58.3(16) . . ? B10 B10 Rh5 80.3(6) 8_565 . ? B9 B10 Rh5 125.2(8) 8_565 . ? B1 B10 Rh5 63.8(6) . . ? B9 B10 Rh5 116.7(12) . . ? B4 B10 Rh5 104(2) . . ? B16 B16 B7 61.9(4) 8_565 . ? B16 B16 B3 107.5(7) 8_565 . ? B7 B16 B3 52.8(9) . . ? B16 B16 B1 110.6(6) 8_565 . ? B7 B16 B1 103.1(7) . . ? B3 B16 B1 62.8(11) . . ? B16 B16 Rh5 68.1(3) 8_565 . ? B7 B16 Rh5 115.7(5) . . ? B3 B16 Rh5 115.2(9) . . ? B1 B16 Rh5 60.4(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.568 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.086