# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_benzyl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H36 B9 Rh' _chemical_formula_sum 'C22 H36 B9 Rh' _chemical_formula_weight 500.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3802(7) _cell_length_b 17.2947(14) _cell_length_c 14.8255(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.867(2) _cell_angle_gamma 90.00 _cell_volume 2399.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1470 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 18.82 _exptl_crystal_description prism _exptl_crystal_colour gold _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \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 24285 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5771 _reflns_number_gt 3489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5771 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Rh3 Rh 0.84561(4) 0.23029(2) 0.97777(2) 0.02013(11) Uani 1 1 d . . . C1 C 0.9786(5) 0.1445(3) 0.9057(3) 0.0238(10) Uani 1 1 d . . . C2 C 0.9166(5) 0.2090(3) 0.8371(3) 0.0225(10) Uani 1 1 d . . . B4 B 1.0605(6) 0.1872(4) 1.0041(4) 0.0252(12) Uani 1 1 d . . . H4 H 1.070(4) 0.157(2) 1.068(3) 0.009(10) Uiso 1 1 d . . . B5 B 1.1607(6) 0.1467(4) 0.9170(4) 0.0268(12) Uani 1 1 d . . . H5 H 1.210(5) 0.095(3) 0.931(3) 0.041(15) Uiso 1 1 d . . . B6 B 1.0718(6) 0.1611(4) 0.8100(4) 0.0285(13) Uani 1 1 d . . . H6 H 1.060(5) 0.119(3) 0.764(4) 0.048(16) Uiso 1 1 d . . . B7 B 0.9487(6) 0.3025(4) 0.8808(4) 0.0284(13) Uani 1 1 d . . . H7 H 0.868(5) 0.350(3) 0.854(3) 0.028(13) Uiso 1 1 d . . . B8 B 1.0519(6) 0.2920(4) 0.9869(4) 0.0283(13) Uani 1 1 d . . . H8 H 1.062(4) 0.340(3) 1.044(3) 0.024(12) Uiso 1 1 d . . . B9 B 1.2075(6) 0.2387(4) 0.9636(4) 0.0307(13) Uani 1 1 d . . . H9 H 1.305(5) 0.244(2) 1.004(3) 0.017(11) Uiso 1 1 d . . . B10 B 1.2102(6) 0.2236(4) 0.8456(4) 0.0286(12) Uani 1 1 d . . . H10 H 1.313(4) 0.221(2) 0.811(3) 0.019(12) Uiso 1 1 d . . . B11 B 1.0496(6) 0.2606(3) 0.7930(4) 0.0252(12) Uani 1 1 d . . . H11 H 1.033(4) 0.280(2) 0.721(3) 0.017(11) Uiso 1 1 d . . . B12 B 1.1384(6) 0.3092(4) 0.8861(4) 0.0312(14) Uani 1 1 d . . . H12 H 1.184(5) 0.363(3) 0.879(3) 0.031(13) Uiso 1 1 d . . . C13 C 0.9120(4) 0.0648(3) 0.9050(3) 0.0218(10) Uani 1 1 d . . . H13A H 0.8907 0.0513 0.9676 0.026 Uiso 1 1 calc R . . H13B H 0.9833 0.0271 0.8856 0.026 Uiso 1 1 calc R . . C14 C 0.7763(5) 0.0556(3) 0.8445(3) 0.0226(10) Uani 1 1 d . . . C15 C 0.7081(5) -0.0167(3) 0.8461(3) 0.0275(11) Uani 1 1 d . . . H15A H 0.7498 -0.0568 0.8829 0.033 Uiso 1 1 calc R . . C16 C 0.5820(5) -0.0306(3) 0.7954(3) 0.0334(12) Uani 1 1 d . . . H16A H 0.5390 -0.0803 0.7956 0.040 Uiso 1 1 calc R . . C17 C 0.5190(5) 0.0284(3) 0.7445(3) 0.0354(13) Uani 1 1 d . . . H17A H 0.4298 0.0200 0.7116 0.043 Uiso 1 1 calc R . . C18 C 0.5845(5) 0.0990(3) 0.7411(3) 0.0288(11) Uani 1 1 d . . . H18A H 0.5401 0.1391 0.7056 0.035 Uiso 1 1 calc R . . C19 C 0.7156(5) 0.1131(3) 0.7890(3) 0.0241(10) Uani 1 1 d . . . C20 C 0.7886(5) 0.1891(3) 0.7725(3) 0.0230(10) Uani 1 1 d . . . H20A H 0.7170 0.2309 0.7757 0.028 Uiso 1 1 calc R . . H20B H 0.8205 0.1886 0.7102 0.028 Uiso 1 1 calc R . . C01 C 0.8267(5) 0.2396(3) 1.1192(3) 0.0249(11) Uani 1 1 d . . . H01A H 0.781(5) 0.287(3) 1.135(3) 0.029(14) Uiso 1 1 d . . . H01B H 0.900(5) 0.227(3) 1.156(3) 0.027(13) Uiso 1 1 d . . . C02 C 0.7426(5) 0.1741(3) 1.0913(3) 0.0222(10) Uani 1 1 d . . . C03 C 0.6346(4) 0.1799(3) 1.0194(3) 0.0221(10) Uani 1 1 d . . . C04 C 0.6100(5) 0.2480(3) 0.9657(3) 0.0269(12) Uani 1 1 d . . . H04 H 0.558(4) 0.240(2) 0.913(3) 0.013(11) Uiso 1 1 d . . . C05 C 0.6588(5) 0.3220(3) 0.9857(3) 0.0251(11) Uani 1 1 d . . . H05 H 0.670(4) 0.334(2) 1.046(3) 0.009(11) Uiso 1 1 d . . . C06 C 0.6328(5) 0.3895(3) 0.9264(3) 0.0244(10) Uani 1 1 d . . . C07 C 0.6805(5) 0.4596(3) 0.9556(3) 0.0292(11) Uani 1 1 d . . . C08 C 0.7739(6) 0.4688(3) 1.0410(4) 0.0384(13) Uani 1 1 d . . . H08A H 0.8367 0.4237 1.0492 0.058 Uiso 1 1 calc R . . H08B H 0.7140 0.4730 1.0925 0.058 Uiso 1 1 calc R . . H08C H 0.8319 0.5156 1.0372 0.058 Uiso 1 1 calc R . . C09 C 0.7810(5) 0.0984(3) 1.1364(3) 0.0299(11) Uani 1 1 d . . . H09A H 0.7325 0.0942 1.1927 0.045 Uiso 1 1 calc R . . H09B H 0.8846 0.0960 1.1500 0.045 Uiso 1 1 calc R . . H09C H 0.7510 0.0558 1.0960 0.045 Uiso 1 1 calc R . . C010 C 0.5462(5) 0.1096(3) 0.9914(3) 0.0273(11) Uani 1 1 d . . . H01C H 0.4686 0.1035 1.0319 0.041 Uiso 1 1 calc R . . H01D H 0.6069 0.0634 0.9949 0.041 Uiso 1 1 calc R . . H01E H 0.5057 0.1162 0.9292 0.041 Uiso 1 1 calc R . . C011 C 0.5515(5) 0.3781(3) 0.8362(3) 0.0304(12) Uani 1 1 d . . . H01F H 0.5415 0.4278 0.8047 0.046 Uiso 1 1 calc R . . H01G H 0.4566 0.3571 0.8455 0.046 Uiso 1 1 calc R . . H01H H 0.6036 0.3418 0.7996 0.046 Uiso 1 1 calc R . . C012 C 0.6468(6) 0.5342(3) 0.9078(4) 0.0353(13) Uani 1 1 d . . . H01I H 0.5726 0.5255 0.8591 0.053 Uiso 1 1 calc R . . H01J H 0.7332 0.5541 0.8821 0.053 Uiso 1 1 calc R . . H01K H 0.6127 0.5719 0.9507 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh3 0.01804(17) 0.02350(19) 0.01880(18) -0.00018(18) 0.00079(12) -0.00080(18) C1 0.018(2) 0.027(3) 0.026(3) -0.005(2) -0.0006(19) -0.002(2) C2 0.018(2) 0.026(3) 0.023(2) -0.0022(19) -0.0006(19) -0.0029(18) B4 0.022(3) 0.034(3) 0.019(3) -0.004(2) 0.000(2) 0.000(2) B5 0.021(3) 0.031(3) 0.029(3) -0.006(3) 0.002(2) 0.001(2) B6 0.023(3) 0.029(3) 0.033(3) -0.009(3) 0.004(2) -0.002(2) B7 0.022(3) 0.028(3) 0.036(3) -0.001(3) 0.006(2) 0.000(2) B8 0.018(3) 0.039(4) 0.028(3) -0.009(3) 0.003(2) -0.008(2) B9 0.020(3) 0.042(4) 0.031(3) -0.013(3) 0.008(2) -0.004(3) B10 0.023(3) 0.036(3) 0.028(3) -0.002(3) 0.004(2) -0.002(3) B11 0.022(3) 0.029(3) 0.025(3) 0.002(2) 0.008(2) -0.003(2) B12 0.026(3) 0.030(3) 0.040(4) -0.012(3) 0.014(3) -0.013(3) C13 0.018(2) 0.020(2) 0.027(3) 0.000(2) -0.0038(19) 0.0023(18) C14 0.020(2) 0.025(3) 0.022(2) -0.003(2) -0.0020(19) -0.0003(19) C15 0.028(3) 0.032(3) 0.023(3) -0.002(2) 0.007(2) -0.003(2) C16 0.038(3) 0.032(3) 0.031(3) -0.009(2) 0.004(2) -0.016(2) C17 0.029(3) 0.054(4) 0.022(3) -0.002(2) -0.007(2) -0.015(3) C18 0.028(3) 0.039(3) 0.020(2) 0.003(2) -0.003(2) -0.001(2) C19 0.022(2) 0.035(3) 0.015(2) -0.004(2) 0.0022(19) 0.001(2) C20 0.026(2) 0.024(3) 0.019(2) -0.002(2) -0.0025(19) 0.000(2) C01 0.024(2) 0.037(3) 0.014(2) 0.002(2) 0.0020(19) 0.007(2) C02 0.016(2) 0.032(3) 0.019(2) 0.002(2) 0.0026(18) 0.0014(19) C03 0.014(2) 0.028(2) 0.025(2) -0.002(2) 0.0066(19) -0.0009(19) C04 0.016(2) 0.042(3) 0.021(2) -0.001(2) -0.0024(19) -0.003(2) C05 0.018(2) 0.037(3) 0.020(2) -0.003(2) 0.0021(19) 0.004(2) C06 0.024(2) 0.030(3) 0.019(2) 0.001(2) 0.0016(19) 0.001(2) C07 0.032(3) 0.031(3) 0.024(3) 0.002(2) 0.004(2) 0.005(2) C08 0.047(3) 0.027(3) 0.039(3) -0.003(2) -0.009(3) -0.002(3) C09 0.032(3) 0.034(3) 0.024(3) 0.007(2) -0.001(2) -0.003(2) C010 0.023(2) 0.031(3) 0.028(3) 0.005(2) 0.001(2) -0.004(2) C011 0.031(3) 0.029(3) 0.030(3) 0.001(2) -0.006(2) 0.002(2) C012 0.040(3) 0.028(3) 0.039(3) 0.006(2) 0.006(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh3 C01 2.122(5) . ? Rh3 B4 2.159(5) . ? Rh3 B7 2.179(6) . ? Rh3 B8 2.206(5) . ? Rh3 C02 2.221(4) . ? Rh3 C04 2.226(5) . ? Rh3 C1 2.253(5) . ? Rh3 C2 2.262(5) . ? Rh3 C03 2.286(4) . ? Rh3 C05 2.372(5) . ? C1 C13 1.514(6) . ? C1 C2 1.593(7) . ? C1 B5 1.706(7) . ? C1 B6 1.740(7) . ? C1 B4 1.764(7) . ? C2 C20 1.524(6) . ? C2 B11 1.700(7) . ? C2 B6 1.745(7) . ? C2 B7 1.759(7) . ? B4 B9 1.779(8) . ? B4 B5 1.792(8) . ? B4 B8 1.831(9) . ? B4 H4 1.09(4) . ? B5 B6 1.759(8) . ? B5 B9 1.778(8) . ? B5 B10 1.781(9) . ? B5 H5 1.01(5) . ? B6 B10 1.744(8) . ? B6 B11 1.749(9) . ? B6 H6 1.00(5) . ? B7 B12 1.780(8) . ? B7 B8 1.800(8) . ? B7 B11 1.812(8) . ? B7 H7 1.17(4) . ? B8 B12 1.773(8) . ? B8 B9 1.780(8) . ? B8 H8 1.19(4) . ? B9 B12 1.768(9) . ? B9 B10 1.770(8) . ? B9 H9 1.06(4) . ? B10 B12 1.748(9) . ? B10 B11 1.769(8) . ? B10 H10 1.12(4) . ? B11 B12 1.775(8) . ? B11 H11 1.11(4) . ? B12 H12 1.03(5) . ? C13 C14 1.515(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.387(6) . ? C14 C15 1.405(6) . ? C15 C16 1.379(6) . ? C15 H15A 0.9500 . ? C16 C17 1.379(7) . ? C16 H16A 0.9500 . ? C17 C18 1.369(7) . ? C17 H17A 0.9500 . ? C18 C19 1.400(6) . ? C18 H18A 0.9500 . ? C19 C20 1.510(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C01 C02 1.426(7) . ? C01 H01A 0.96(5) . ? C01 H01B 0.87(5) . ? C02 C03 1.424(6) . ? C02 C09 1.501(6) . ? C03 C04 1.431(7) . ? C03 C010 1.514(6) . ? C04 C05 1.385(7) . ? C04 H04 0.90(4) . ? C05 C06 1.473(7) . ? C05 H05 0.92(4) . ? C06 C07 1.353(7) . ? C06 C011 1.507(6) . ? C07 C012 1.495(7) . ? C07 C08 1.499(7) . ? C08 H08A 0.9800 . ? C08 H08B 0.9800 . ? C08 H08C 0.9800 . ? C09 H09A 0.9800 . ? C09 H09B 0.9800 . ? C09 H09C 0.9800 . ? C010 H01C 0.9800 . ? C010 H01D 0.9800 . ? C010 H01E 0.9800 . ? C011 H01F 0.9800 . ? C011 H01G 0.9800 . ? C011 H01H 0.9800 . ? C012 H01I 0.9800 . ? C012 H01J 0.9800 . ? C012 H01K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C01 Rh3 B4 89.2(2) . . ? C01 Rh3 B7 132.8(2) . . ? B4 Rh3 B7 82.3(2) . . ? C01 Rh3 B8 92.0(2) . . ? B4 Rh3 B8 49.6(2) . . ? B7 Rh3 B8 48.5(2) . . ? C01 Rh3 C02 38.25(18) . . ? B4 Rh3 C02 99.24(19) . . ? B7 Rh3 C02 170.4(2) . . ? B8 Rh3 C02 126.17(19) . . ? C01 Rh3 C04 85.43(19) . . ? B4 Rh3 C04 166.2(2) . . ? B7 Rh3 C04 110.5(2) . . ? B8 Rh3 C04 143.2(2) . . ? C02 Rh3 C04 68.94(17) . . ? C01 Rh3 C1 127.16(19) . . ? B4 Rh3 C1 47.07(18) . . ? B7 Rh3 C1 77.3(2) . . ? B8 Rh3 C1 80.58(19) . . ? C02 Rh3 C1 110.74(18) . . ? C04 Rh3 C1 129.09(17) . . ? C01 Rh3 C2 166.60(18) . . ? B4 Rh3 C2 77.37(18) . . ? B7 Rh3 C2 46.63(19) . . ? B8 Rh3 C2 79.84(19) . . ? C02 Rh3 C2 142.93(18) . . ? C04 Rh3 C2 107.49(17) . . ? C1 Rh3 C2 41.32(17) . . ? C01 Rh3 C03 68.32(18) . . ? B4 Rh3 C03 129.4(2) . . ? B7 Rh3 C03 145.85(19) . . ? B8 Rh3 C03 160.07(19) . . ? C02 Rh3 C03 36.80(15) . . ? C04 Rh3 C03 36.96(17) . . ? C1 Rh3 C03 113.20(16) . . ? C2 Rh3 C03 120.07(16) . . ? C01 Rh3 C05 77.83(19) . . ? B4 Rh3 C05 154.8(2) . . ? B7 Rh3 C05 90.7(2) . . ? B8 Rh3 C05 108.7(2) . . ? C02 Rh3 C05 83.94(17) . . ? C04 Rh3 C05 34.87(17) . . ? C1 Rh3 C05 153.89(17) . . ? C2 Rh3 C05 114.75(17) . . ? C03 Rh3 C05 65.51(17) . . ? C13 C1 C2 120.1(4) . . ? C13 C1 B5 115.5(4) . . ? C2 C1 B5 111.5(4) . . ? C13 C1 B6 112.0(4) . . ? C2 C1 B6 63.0(3) . . ? B5 C1 B6 61.4(3) . . ? C13 C1 B4 122.9(4) . . ? C2 C1 B4 110.8(4) . . ? B5 C1 B4 62.1(3) . . ? B6 C1 B4 113.0(4) . . ? C13 C1 Rh3 111.2(3) . . ? C2 C1 Rh3 69.6(2) . . ? B5 C1 Rh3 121.5(3) . . ? B6 C1 Rh3 127.1(3) . . ? B4 C1 Rh3 63.7(2) . . ? C20 C2 C1 118.7(4) . . ? C20 C2 B11 116.4(4) . . ? C1 C2 B11 111.6(4) . . ? C20 C2 B6 112.5(4) . . ? C1 C2 B6 62.6(3) . . ? B11 C2 B6 61.0(3) . . ? C20 C2 B7 123.2(4) . . ? C1 C2 B7 111.2(4) . . ? B11 C2 B7 63.1(3) . . ? B6 C2 B7 113.3(4) . . ? C20 C2 Rh3 110.3(3) . . ? C1 C2 Rh3 69.0(2) . . ? B11 C2 Rh3 122.6(3) . . ? B6 C2 Rh3 126.3(3) . . ? B7 C2 Rh3 64.2(2) . . ? C1 B4 B9 103.6(4) . . ? C1 B4 B5 57.3(3) . . ? B9 B4 B5 59.7(3) . . ? C1 B4 B8 106.7(4) . . ? B9 B4 B8 59.1(3) . . ? B5 B4 B8 107.9(4) . . ? C1 B4 Rh3 69.3(2) . . ? B9 B4 Rh3 120.1(4) . . ? B5 B4 Rh3 122.3(3) . . ? B8 B4 Rh3 66.5(3) . . ? C1 B4 H4 122(2) . . ? B9 B4 H4 121(2) . . ? B5 B4 H4 115(2) . . ? B8 B4 H4 127(2) . . ? Rh3 B4 H4 110(2) . . ? C1 B5 B6 60.3(3) . . ? C1 B5 B9 106.0(4) . . ? B6 B5 B9 108.2(4) . . ? C1 B5 B10 104.9(4) . . ? B6 B5 B10 59.0(3) . . ? B9 B5 B10 59.6(3) . . ? C1 B5 B4 60.5(3) . . ? B6 B5 B4 110.7(4) . . ? B9 B5 B4 59.8(3) . . ? B10 B5 B4 107.8(4) . . ? C1 B5 H5 116(3) . . ? B6 B5 H5 119(3) . . ? B9 B5 H5 127(3) . . ? B10 B5 H5 130(3) . . ? B4 B5 H5 117(3) . . ? C1 B6 B10 105.1(4) . . ? C1 B6 C2 54.4(3) . . ? B10 B6 C2 104.6(4) . . ? C1 B6 B11 102.6(4) . . ? B10 B6 B11 60.8(3) . . ? C2 B6 B11 58.2(3) . . ? C1 B6 B5 58.3(3) . . ? B10 B6 B5 61.1(3) . . ? C2 B6 B5 102.3(4) . . ? B11 B6 B5 108.3(4) . . ? C1 B6 H6 113(3) . . ? B10 B6 H6 135(3) . . ? C2 B6 H6 117(3) . . ? B11 B6 H6 128(3) . . ? B5 B6 H6 122(3) . . ? C2 B7 B12 102.8(4) . . ? C2 B7 B8 107.4(4) . . ? B12 B7 B8 59.4(3) . . ? C2 B7 B11 56.8(3) . . ? B12 B7 B11 59.2(3) . . ? B8 B7 B11 108.2(4) . . ? C2 B7 Rh3 69.2(2) . . ? B12 B7 Rh3 119.7(4) . . ? B8 B7 Rh3 66.6(3) . . ? B11 B7 Rh3 121.5(4) . . ? C2 B7 H7 116(2) . . ? B12 B7 H7 126(2) . . ? B8 B7 H7 131(2) . . ? B11 B7 H7 113(2) . . ? Rh3 B7 H7 109(2) . . ? B12 B8 B9 59.7(3) . . ? B12 B8 B7 59.8(3) . . ? B9 B8 B7 106.4(4) . . ? B12 B8 B4 105.3(4) . . ? B9 B8 B4 59.0(3) . . ? B7 B8 B4 103.7(4) . . ? B12 B8 Rh3 118.6(3) . . ? B9 B8 Rh3 117.7(4) . . ? B7 B8 Rh3 65.0(2) . . ? B4 B8 Rh3 63.9(2) . . ? B12 B8 H8 117(2) . . ? B9 B8 H8 118(2) . . ? B7 B8 H8 124(2) . . ? B4 B8 H8 127(2) . . ? Rh3 B8 H8 114(2) . . ? B12 B9 B10 59.2(3) . . ? B12 B9 B5 107.1(4) . . ? B10 B9 B5 60.3(3) . . ? B12 B9 B4 107.8(4) . . ? B10 B9 B4 108.9(4) . . ? B5 B9 B4 60.5(3) . . ? B12 B9 B8 60.0(3) . . ? B10 B9 B8 109.6(4) . . ? B5 B9 B8 110.8(4) . . ? B4 B9 B8 61.9(3) . . ? B12 B9 H9 125(2) . . ? B10 B9 H9 120(2) . . ? B5 B9 H9 118(2) . . ? B4 B9 H9 120(2) . . ? B8 B9 H9 122(2) . . ? B6 B10 B12 109.4(4) . . ? B6 B10 B11 59.7(3) . . ? B12 B10 B11 60.6(3) . . ? B6 B10 B9 109.3(4) . . ? B12 B10 B9 60.3(4) . . ? B11 B10 B9 108.3(4) . . ? B6 B10 B5 59.9(3) . . ? B12 B10 B5 107.9(4) . . ? B11 B10 B5 106.5(4) . . ? B9 B10 B5 60.1(3) . . ? B6 B10 H10 119(2) . . ? B12 B10 H10 123(2) . . ? B11 B10 H10 123(2) . . ? B9 B10 H10 122(2) . . ? B5 B10 H10 120(2) . . ? C2 B11 B6 60.8(3) . . ? C2 B11 B10 105.4(4) . . ? B6 B11 B10 59.4(3) . . ? C2 B11 B12 105.5(4) . . ? B6 B11 B12 108.0(4) . . ? B10 B11 B12 59.1(3) . . ? C2 B11 B7 60.0(3) . . ? B6 B11 B7 110.6(4) . . ? B10 B11 B7 107.3(4) . . ? B12 B11 B7 59.5(3) . . ? C2 B11 H11 118(2) . . ? B6 B11 H11 116(2) . . ? B10 B11 H11 126(2) . . ? B12 B11 H11 129(2) . . ? B7 B11 H11 121(2) . . ? B10 B12 B9 60.4(3) . . ? B10 B12 B8 110.9(4) . . ? B9 B12 B8 60.4(3) . . ? B10 B12 B11 60.3(3) . . ? B9 B12 B11 108.1(4) . . ? B8 B12 B11 111.0(4) . . ? B10 B12 B7 109.7(4) . . ? B9 B12 B7 107.8(4) . . ? B8 B12 B7 60.9(3) . . ? B11 B12 B7 61.3(3) . . ? B10 B12 H12 124(3) . . ? B9 B12 H12 124(3) . . ? B8 B12 H12 117(3) . . ? B11 B12 H12 121(3) . . ? B7 B12 H12 118(3) . . ? C1 C13 C14 115.4(4) . . ? C1 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? C1 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C19 C14 C15 118.6(4) . . ? C19 C14 C13 124.8(4) . . ? C15 C14 C13 116.6(4) . . ? C16 C15 C14 121.4(5) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 121.2(5) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C14 C19 C18 119.2(4) . . ? C14 C19 C20 123.2(4) . . ? C18 C19 C20 117.5(4) . . ? C19 C20 C2 116.2(4) . . ? C19 C20 H20A 108.2 . . ? C2 C20 H20A 108.2 . . ? C19 C20 H20B 108.2 . . ? C2 C20 H20B 108.2 . . ? H20A C20 H20B 107.4 . . ? C02 C01 Rh3 74.6(3) . . ? C02 C01 H01A 120(3) . . ? Rh3 C01 H01A 112(3) . . ? C02 C01 H01B 112(3) . . ? Rh3 C01 H01B 119(3) . . ? H01A C01 H01B 114(4) . . ? C03 C02 C01 120.9(4) . . ? C03 C02 C09 122.2(4) . . ? C01 C02 C09 116.8(4) . . ? C03 C02 Rh3 74.1(3) . . ? C01 C02 Rh3 67.1(3) . . ? C09 C02 Rh3 128.0(3) . . ? C02 C03 C04 123.6(4) . . ? C02 C03 C010 119.8(4) . . ? C04 C03 C010 116.3(4) . . ? C02 C03 Rh3 69.1(2) . . ? C04 C03 Rh3 69.2(2) . . ? C010 C03 Rh3 134.5(3) . . ? C05 C04 C03 127.1(5) . . ? C05 C04 Rh3 78.4(3) . . ? C03 C04 Rh3 73.8(3) . . ? C05 C04 H04 118(3) . . ? C03 C04 H04 115(3) . . ? Rh3 C04 H04 122(3) . . ? C04 C05 C06 124.5(4) . . ? C04 C05 Rh3 66.8(3) . . ? C06 C05 Rh3 126.4(3) . . ? C04 C05 H05 115(3) . . ? C06 C05 H05 114(3) . . ? Rh3 C05 H05 99(2) . . ? C07 C06 C05 118.8(4) . . ? C07 C06 C011 122.6(4) . . ? C05 C06 C011 118.6(4) . . ? C06 C07 C012 124.5(5) . . ? C06 C07 C08 121.8(4) . . ? C012 C07 C08 113.7(4) . . ? C07 C08 H08A 109.5 . . ? C07 C08 H08B 109.5 . . ? H08A C08 H08B 109.5 . . ? C07 C08 H08C 109.5 . . ? H08A C08 H08C 109.5 . . ? H08B C08 H08C 109.5 . . ? C02 C09 H09A 109.5 . . ? C02 C09 H09B 109.5 . . ? H09A C09 H09B 109.5 . . ? C02 C09 H09C 109.5 . . ? H09A C09 H09C 109.5 . . ? H09B C09 H09C 109.5 . . ? C03 C010 H01C 109.5 . . ? C03 C010 H01D 109.5 . . ? H01C C010 H01D 109.5 . . ? C03 C010 H01E 109.5 . . ? H01C C010 H01E 109.5 . . ? H01D C010 H01E 109.5 . . ? C06 C011 H01F 109.5 . . ? C06 C011 H01G 109.5 . . ? H01F C011 H01G 109.5 . . ? C06 C011 H01H 109.5 . . ? H01F C011 H01H 109.5 . . ? H01G C011 H01H 109.5 . . ? C07 C012 H01I 109.5 . . ? C07 C012 H01J 109.5 . . ? H01I C012 H01J 109.5 . . ? C07 C012 H01K 109.5 . . ? H01I C012 H01K 109.5 . . ? H01J C012 H01K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.657 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.130 _database_code_depnum_ccdc_archive 'CCDC 965360' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_phme _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 B9 Rh' _chemical_formula_sum 'C21 H36 B9 Rh' _chemical_formula_weight 488.70 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.575(5) _cell_length_b 15.128(9) _cell_length_c 16.401(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2376(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5590 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 32.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \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 30387 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6881 _reflns_number_gt 6505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0379P)^2^+0.7033P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _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 0.46(2) _refine_ls_number_reflns 6881 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Rh3 Rh 0.146266(16) 0.280296(10) 0.850755(9) 0.01140(4) Uani 1 1 d . . . C1 C 0.0193(2) 0.34026(16) 0.75132(13) 0.0158(4) Uani 1 1 d . . . C2 C 0.0807(2) 0.24548(15) 0.72164(13) 0.0146(4) Uani 1 1 d . . . B4 B -0.0640(2) 0.33245(16) 0.84738(19) 0.0161(4) Uani 1 1 d . . . H4 H -0.073(3) 0.391(2) 0.8795(17) 0.021(7) Uiso 1 1 d . . . B5 B -0.1583(3) 0.33932(18) 0.75309(15) 0.0180(5) Uani 1 1 d . . . H5 H -0.204(3) 0.3977(18) 0.7396(16) 0.015(7) Uiso 1 1 d . . . B6 B -0.0685(3) 0.2839(2) 0.67469(15) 0.0186(5) Uani 1 1 d . . . H6 H -0.052(3) 0.305(2) 0.6116(19) 0.024(8) Uiso 1 1 d . . . B7 B 0.0451(3) 0.16525(18) 0.79815(16) 0.0171(5) Uani 1 1 d . . . H7 H 0.099(3) 0.107(2) 0.8005(17) 0.019(7) Uiso 1 1 d . . . B8 B -0.0569(3) 0.2167(2) 0.87726(15) 0.0164(4) Uani 1 1 d . . . H8 H -0.075(4) 0.192(2) 0.939(2) 0.031(9) Uiso 1 1 d . . . B9 B -0.2087(3) 0.26099(18) 0.82781(16) 0.0190(5) Uani 1 1 d . . . H9 H -0.298(3) 0.2700(18) 0.8634(17) 0.020(7) Uiso 1 1 d . . . B10 B -0.2089(3) 0.2303(2) 0.72360(17) 0.0210(5) Uani 1 1 d . . . H10 H -0.296(3) 0.221(2) 0.6840(18) 0.030(8) Uiso 1 1 d . . . B11 B -0.0502(3) 0.17254(18) 0.70358(18) 0.0196(5) Uani 1 1 d . . . H11 H -0.035(3) 0.119(2) 0.6581(19) 0.026(8) Uiso 1 1 d . . . B12 B -0.1415(3) 0.15712(17) 0.79802(16) 0.0197(4) Uani 1 1 d . . . H12 H -0.191(3) 0.097(2) 0.8121(17) 0.023(8) Uiso 1 1 d . . . C13 C 0.0824(3) 0.42828(15) 0.72580(15) 0.0197(4) Uani 1 1 d . . . H13A H 0.0405 0.4474 0.6742 0.030 Uiso 1 1 calc R . . H13B H 0.1835 0.4215 0.7188 0.030 Uiso 1 1 calc R . . H13C H 0.0638 0.4727 0.7680 0.030 Uiso 1 1 calc R . . C14 C 0.2070(2) 0.23899(16) 0.66650(12) 0.0173(5) Uani 1 1 d . . . C15 C 0.2335(3) 0.29958(18) 0.60424(14) 0.0241(5) Uani 1 1 d . . . H15A H 0.1703 0.3469 0.5948 0.029 Uiso 1 1 calc R . . C16 C 0.3528(3) 0.2910(2) 0.55573(15) 0.0315(6) Uani 1 1 d . . . H16A H 0.3702 0.3329 0.5138 0.038 Uiso 1 1 calc R . . C17 C 0.4453(3) 0.2228(3) 0.56785(15) 0.0320(6) Uani 1 1 d . . . H17A H 0.5275 0.2184 0.5356 0.038 Uiso 1 1 calc R . . C18 C 0.4173(3) 0.1603(2) 0.62771(16) 0.0279(6) Uani 1 1 d . . . H18A H 0.4797 0.1123 0.6359 0.033 Uiso 1 1 calc R . . C19 C 0.2985(3) 0.16782(18) 0.67555(15) 0.0220(5) Uani 1 1 d . . . H19A H 0.2790 0.1237 0.7152 0.026 Uiso 1 1 calc R . . C01 C 0.1686(2) 0.33944(16) 0.96908(13) 0.0188(4) Uani 1 1 d . . . H01A H 0.203(3) 0.300(2) 1.0037(19) 0.023 Uiso 1 1 d . . . H01B H 0.078(3) 0.3710(19) 0.9877(18) 0.023 Uiso 1 1 d . . . C02 C 0.2581(2) 0.38833(16) 0.91631(14) 0.0184(4) Uani 1 1 d . . . C03 C 0.3562(3) 0.34535(15) 0.86521(13) 0.0175(4) Uani 1 1 d . . . C04 C 0.3745(2) 0.24991(16) 0.86346(14) 0.0168(4) Uani 1 1 d . . . H04 H 0.424(3) 0.228(2) 0.8176(19) 0.030(8) Uiso 1 1 d . . . C05 C 0.3227(2) 0.18638(16) 0.91522(14) 0.0156(4) Uani 1 1 d . . . H05 H 0.291(3) 0.204(2) 0.957(2) 0.028(8) Uiso 1 1 d . . . C06 C 0.3516(3) 0.09115(15) 0.90519(13) 0.0188(4) Uani 1 1 d . . . C07 C 0.2850(3) 0.03135(16) 0.95243(16) 0.0212(5) Uani 1 1 d . . . C08 C 0.1663(3) 0.05481(17) 1.00829(16) 0.0259(5) Uani 1 1 d . . . H08A H 0.1453 0.1180 1.0031 0.039 Uiso 1 1 calc R . . H08B H 0.1926 0.0416 1.0647 0.039 Uiso 1 1 calc R . . H08C H 0.0836 0.0202 0.9934 0.039 Uiso 1 1 calc R . . C09 C 0.2358(3) 0.48745(17) 0.91031(18) 0.0280(6) Uani 1 1 d . . . H09A H 0.2980 0.5176 0.9487 0.042 Uiso 1 1 calc R . . H09B H 0.1386 0.5015 0.9236 0.042 Uiso 1 1 calc R . . H09C H 0.2566 0.5072 0.8547 0.042 Uiso 1 1 calc R . . C010 C 0.4432(3) 0.39616(18) 0.80438(16) 0.0239(5) Uani 1 1 d . . . H01C H 0.5290 0.4169 0.8308 0.036 Uiso 1 1 calc R . . H01D H 0.3899 0.4470 0.7844 0.036 Uiso 1 1 calc R . . H01E H 0.4672 0.3575 0.7585 0.036 Uiso 1 1 calc R . . C011 C 0.4665(3) 0.06308(17) 0.84719(19) 0.0271(5) Uani 1 1 d . . . H01F H 0.5223 0.0162 0.8725 0.041 Uiso 1 1 calc R . . H01G H 0.5266 0.1139 0.8351 0.041 Uiso 1 1 calc R . . H01H H 0.4250 0.0410 0.7965 0.041 Uiso 1 1 calc R . . C012 C 0.3216(3) -0.06569(16) 0.95290(18) 0.0274(6) Uani 1 1 d . . . H01I H 0.3918 -0.0775 0.9108 0.041 Uiso 1 1 calc R . . H01J H 0.2376 -0.1007 0.9418 0.041 Uiso 1 1 calc R . . H01K H 0.3592 -0.0819 1.0064 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh3 0.00999(6) 0.01282(6) 0.01139(6) -0.00007(6) -0.00023(6) 0.00035(6) C1 0.0139(9) 0.0186(10) 0.0149(9) -0.0002(8) -0.0021(8) 0.0002(8) C2 0.0120(9) 0.0187(10) 0.0131(9) -0.0025(7) -0.0016(8) -0.0013(8) B4 0.0136(9) 0.0174(11) 0.0173(11) -0.0011(11) -0.0021(11) 0.0027(9) B5 0.0127(10) 0.0221(11) 0.0193(11) -0.0002(9) -0.0047(10) 0.0035(10) B6 0.0134(10) 0.0242(12) 0.0181(10) 0.0012(11) -0.0028(8) -0.0016(11) B7 0.0121(11) 0.0182(12) 0.0208(12) -0.0004(10) 0.0018(9) 0.0004(9) B8 0.0127(10) 0.0175(11) 0.0190(10) 0.0027(11) 0.0011(8) -0.0001(11) B9 0.0120(11) 0.0236(14) 0.0214(12) 0.0012(9) -0.0011(9) 0.0033(9) B10 0.0140(11) 0.0234(14) 0.0256(13) -0.0020(11) -0.0051(9) -0.0022(10) B11 0.0160(11) 0.0184(13) 0.0246(13) -0.0063(10) -0.0003(10) -0.0037(10) B12 0.0138(10) 0.0195(11) 0.0259(12) -0.0009(9) 0.0015(11) -0.0028(11) C13 0.0207(11) 0.0180(11) 0.0203(11) 0.0048(8) -0.0039(9) -0.0010(9) C14 0.0133(9) 0.0278(12) 0.0107(9) -0.0060(8) -0.0004(7) -0.0040(8) C15 0.0184(11) 0.0376(16) 0.0162(11) 0.0020(9) -0.0009(9) -0.0019(10) C16 0.0254(11) 0.0521(17) 0.0170(10) 0.0032(11) 0.0036(11) -0.0055(15) C17 0.0186(10) 0.0586(18) 0.0187(11) -0.0102(14) 0.0024(9) -0.0053(15) C18 0.0171(11) 0.0410(15) 0.0255(13) -0.0133(11) 0.0019(9) 0.0020(11) C19 0.0185(10) 0.0279(13) 0.0195(11) -0.0087(9) 0.0013(8) -0.0015(10) C01 0.0204(12) 0.0209(10) 0.0150(9) -0.0031(8) -0.0027(8) 0.0043(9) C02 0.0157(10) 0.0196(11) 0.0200(11) -0.0038(9) -0.0071(9) -0.0003(9) C03 0.0127(8) 0.0211(10) 0.0189(11) 0.0023(8) -0.0044(9) -0.0023(9) C04 0.0128(10) 0.0210(9) 0.0165(11) -0.0014(8) -0.0004(8) 0.0008(8) C05 0.0138(11) 0.0189(10) 0.0142(10) -0.0010(8) -0.0009(8) 0.0029(8) C06 0.0171(9) 0.0201(10) 0.0192(10) -0.0029(8) -0.0040(10) 0.0012(10) C07 0.0198(11) 0.0213(11) 0.0225(11) 0.0000(9) -0.0060(9) -0.0008(9) C08 0.0214(13) 0.0249(12) 0.0314(13) 0.0034(10) 0.0037(10) -0.0031(10) C09 0.0306(14) 0.0184(12) 0.0350(15) -0.0069(11) -0.0071(12) 0.0038(10) C010 0.0174(11) 0.0266(12) 0.0278(13) 0.0085(10) 0.0009(10) -0.0053(10) C011 0.0310(13) 0.0230(11) 0.0273(12) -0.0004(12) 0.0060(12) 0.0079(9) C012 0.0316(14) 0.0178(11) 0.0328(13) 0.0014(10) -0.0072(11) 0.0005(9) _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 Rh3 C01 2.148(2) . ? Rh3 B4 2.164(3) . ? Rh3 B7 2.170(3) . ? Rh3 B8 2.213(3) . ? Rh3 C1 2.227(2) . ? Rh3 C02 2.230(2) . ? Rh3 C04 2.243(3) . ? Rh3 C03 2.251(3) . ? Rh3 C2 2.271(2) . ? Rh3 C05 2.447(2) . ? C1 C13 1.521(3) . ? C1 C2 1.624(3) . ? C1 B5 1.700(3) . ? C1 B6 1.736(4) . ? C1 B4 1.770(4) . ? C2 C14 1.513(3) . ? C2 B11 1.696(4) . ? C2 B6 1.724(3) . ? C2 B7 1.779(4) . ? B4 B9 1.786(4) . ? B4 B5 1.793(4) . ? B4 B8 1.819(4) . ? B4 H4 1.04(3) . ? B5 B6 1.759(4) . ? B5 B9 1.772(4) . ? B5 B10 1.785(4) . ? B5 H5 1.01(3) . ? B6 B11 1.758(4) . ? B6 B10 1.762(4) . ? B6 H6 1.09(3) . ? B7 B12 1.791(4) . ? B7 B8 1.801(4) . ? B7 B11 1.803(4) . ? B7 H7 1.02(3) . ? B8 B12 1.777(4) . ? B8 B9 1.794(4) . ? B8 H8 1.09(3) . ? B9 B12 1.767(4) . ? B9 B10 1.771(4) . ? B9 H9 1.04(3) . ? B10 B12 1.770(4) . ? B10 B11 1.784(4) . ? B10 H10 1.07(3) . ? B11 B12 1.794(4) . ? B11 H11 1.11(3) . ? B12 H12 1.05(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.396(3) . ? C14 C19 1.396(4) . ? C15 C16 1.398(4) . ? C15 H15A 0.9500 . ? C16 C17 1.374(5) . ? C16 H16A 0.9500 . ? C17 C18 1.389(4) . ? C17 H17A 0.9500 . ? C18 C19 1.386(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C01 C02 1.425(3) . ? C01 H01A 0.89(3) . ? C01 H01B 1.03(3) . ? C02 C03 1.417(3) . ? C02 C09 1.518(4) . ? C03 C04 1.455(4) . ? C03 C010 1.510(3) . ? C04 C05 1.375(3) . ? C04 H04 0.95(3) . ? C05 C06 1.476(3) . ? C05 H05 0.79(3) . ? C06 C07 1.351(3) . ? C06 C011 1.516(4) . ? C07 C08 1.502(4) . ? C07 C012 1.509(4) . ? C08 H08A 0.9800 . ? C08 H08B 0.9800 . ? C08 H08C 0.9800 . ? C09 H09A 0.9800 . ? C09 H09B 0.9800 . ? C09 H09C 0.9800 . ? C010 H01C 0.9800 . ? C010 H01D 0.9800 . ? C010 H01E 0.9800 . ? C011 H01F 0.9800 . ? C011 H01G 0.9800 . ? C011 H01H 0.9800 . ? C012 H01I 0.9800 . ? C012 H01J 0.9800 . ? C012 H01K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C01 Rh3 B4 87.92(10) . . ? C01 Rh3 B7 137.53(10) . . ? B4 Rh3 B7 82.36(10) . . ? C01 Rh3 B8 95.22(10) . . ? B4 Rh3 B8 49.10(11) . . ? B7 Rh3 B8 48.51(10) . . ? C01 Rh3 C1 123.11(9) . . ? B4 Rh3 C1 47.52(10) . . ? B7 Rh3 C1 78.00(10) . . ? B8 Rh3 C1 80.85(10) . . ? C01 Rh3 C02 37.94(9) . . ? B4 Rh3 C02 101.07(10) . . ? B7 Rh3 C02 173.44(10) . . ? B8 Rh3 C02 130.23(10) . . ? C1 Rh3 C02 108.46(9) . . ? C01 Rh3 C04 84.52(9) . . ? B4 Rh3 C04 169.74(9) . . ? B7 Rh3 C04 107.90(9) . . ? B8 Rh3 C04 138.52(11) . . ? C1 Rh3 C04 133.11(8) . . ? C02 Rh3 C04 68.75(9) . . ? C01 Rh3 C03 68.52(9) . . ? B4 Rh3 C03 132.42(10) . . ? B7 Rh3 C03 142.27(9) . . ? B8 Rh3 C03 162.63(8) . . ? C1 Rh3 C03 112.74(9) . . ? C02 Rh3 C03 36.87(8) . . ? C04 Rh3 C03 37.77(9) . . ? C01 Rh3 C2 165.21(8) . . ? B4 Rh3 C2 78.66(10) . . ? B7 Rh3 C2 47.15(9) . . ? B8 Rh3 C2 80.75(9) . . ? C1 Rh3 C2 42.33(9) . . ? C02 Rh3 C2 138.79(9) . . ? C04 Rh3 C2 107.97(8) . . ? C03 Rh3 C2 116.53(8) . . ? C01 Rh3 C05 77.46(9) . . ? B4 Rh3 C05 149.90(10) . . ? B7 Rh3 C05 90.81(10) . . ? B8 Rh3 C05 105.64(10) . . ? C1 Rh3 C05 158.36(8) . . ? C02 Rh3 C05 83.44(9) . . ? C04 Rh3 C05 33.74(8) . . ? C03 Rh3 C05 65.91(9) . . ? C2 Rh3 C05 117.33(8) . . ? C13 C1 C2 123.13(19) . . ? C13 C1 B5 114.15(19) . . ? C2 C1 B5 111.08(18) . . ? C13 C1 B6 115.06(19) . . ? C2 C1 B6 61.62(15) . . ? B5 C1 B6 61.57(14) . . ? C13 C1 B4 118.84(18) . . ? C2 C1 B4 111.78(17) . . ? B5 C1 B4 62.19(14) . . ? B6 C1 B4 113.15(17) . . ? C13 C1 Rh3 109.95(14) . . ? C2 C1 Rh3 70.26(11) . . ? B5 C1 Rh3 121.99(15) . . ? B6 C1 Rh3 126.46(16) . . ? B4 C1 Rh3 64.35(11) . . ? C14 C2 C1 121.71(18) . . ? C14 C2 B11 116.35(18) . . ? C1 C2 B11 111.05(18) . . ? C14 C2 B6 114.67(18) . . ? C1 C2 B6 62.39(15) . . ? B11 C2 B6 61.87(16) . . ? C14 C2 B7 122.02(18) . . ? C1 C2 B7 108.76(17) . . ? B11 C2 B7 62.47(15) . . ? B6 C2 B7 112.72(17) . . ? C14 C2 Rh3 110.58(14) . . ? C1 C2 Rh3 67.41(11) . . ? B11 C2 Rh3 121.21(15) . . ? B6 C2 Rh3 124.58(15) . . ? B7 C2 Rh3 63.46(11) . . ? C1 B4 B9 103.30(19) . . ? C1 B4 B5 56.99(15) . . ? B9 B4 B5 59.34(15) . . ? C1 B4 B8 106.69(16) . . ? B9 B4 B8 59.67(14) . . ? B5 B4 B8 107.87(17) . . ? C1 B4 Rh3 68.13(11) . . ? B9 B4 Rh3 120.38(15) . . ? B5 B4 Rh3 120.75(17) . . ? B8 B4 Rh3 66.88(11) . . ? C1 B4 H4 115.6(16) . . ? B9 B4 H4 123.1(17) . . ? B5 B4 H4 110.3(16) . . ? B8 B4 H4 133.7(16) . . ? Rh3 B4 H4 112.1(17) . . ? C1 B5 B6 60.22(14) . . ? C1 B5 B9 106.86(18) . . ? B6 B5 B9 108.6(2) . . ? C1 B5 B10 105.93(18) . . ? B6 B5 B10 59.61(16) . . ? B9 B5 B10 59.72(16) . . ? C1 B5 B4 60.81(14) . . ? B6 B5 B4 110.92(18) . . ? B9 B5 B4 60.13(15) . . ? B10 B5 B4 108.46(18) . . ? C1 B5 H5 115.0(16) . . ? B6 B5 H5 118.0(15) . . ? B9 B5 H5 128.1(16) . . ? B10 B5 H5 129.1(16) . . ? B4 B5 H5 117.2(16) . . ? C2 B6 C1 55.99(13) . . ? C2 B6 B11 58.28(14) . . ? C1 B6 B11 103.14(17) . . ? C2 B6 B5 103.82(17) . . ? C1 B6 B5 58.21(14) . . ? B11 B6 B5 107.98(19) . . ? C2 B6 B10 105.91(19) . . ? C1 B6 B10 105.41(18) . . ? B11 B6 B10 60.89(17) . . ? B5 B6 B10 60.93(16) . . ? C2 B6 H6 113.7(16) . . ? C1 B6 H6 118.2(17) . . ? B11 B6 H6 121.3(16) . . ? B5 B6 H6 128.4(16) . . ? B10 B6 H6 132.3(16) . . ? C2 B7 B12 103.71(18) . . ? C2 B7 B8 108.48(19) . . ? B12 B7 B8 59.29(14) . . ? C2 B7 B11 56.52(14) . . ? B12 B7 B11 59.87(15) . . ? B8 B7 B11 108.57(18) . . ? C2 B7 Rh3 69.38(12) . . ? B12 B7 Rh3 120.04(16) . . ? B8 B7 Rh3 66.99(13) . . ? B11 B7 Rh3 121.25(16) . . ? C2 B7 H7 121.2(16) . . ? B12 B7 H7 116.4(16) . . ? B8 B7 H7 128.3(16) . . ? B11 B7 H7 110.0(16) . . ? Rh3 B7 H7 116.8(16) . . ? B12 B8 B9 59.32(15) . . ? B12 B8 B7 60.07(16) . . ? B9 B8 B7 105.98(18) . . ? B12 B8 B4 105.92(17) . . ? B9 B8 B4 59.25(15) . . ? B7 B8 B4 104.03(17) . . ? B12 B8 Rh3 118.51(15) . . ? B9 B8 Rh3 117.47(18) . . ? B7 B8 Rh3 64.50(11) . . ? B4 B8 Rh3 64.02(11) . . ? B12 B8 H8 115.9(17) . . ? B9 B8 H8 114.8(18) . . ? B7 B8 H8 127.4(17) . . ? B4 B8 H8 124.7(17) . . ? Rh3 B8 H8 117.8(18) . . ? B12 B9 B10 60.04(15) . . ? B12 B9 B5 107.70(19) . . ? B10 B9 B5 60.51(16) . . ? B12 B9 B4 107.77(18) . . ? B10 B9 B4 109.42(19) . . ? B5 B9 B4 60.53(16) . . ? B12 B9 B8 59.86(16) . . ? B10 B9 B8 109.83(19) . . ? B5 B9 B8 109.96(19) . . ? B4 B9 B8 61.08(15) . . ? B12 B9 H9 124.7(16) . . ? B10 B9 H9 124.9(15) . . ? B5 B9 H9 121.5(16) . . ? B4 B9 H9 117.1(15) . . ? B8 B9 H9 117.4(15) . . ? B6 B10 B12 108.87(19) . . ? B6 B10 B9 108.57(19) . . ? B12 B10 B9 59.87(15) . . ? B6 B10 B11 59.46(16) . . ? B12 B10 B11 60.63(16) . . ? B9 B10 B11 107.78(19) . . ? B6 B10 B5 59.47(16) . . ? B12 B10 B5 106.98(18) . . ? B9 B10 B5 59.77(15) . . ? B11 B10 B5 105.75(18) . . ? B6 B10 H10 112.3(17) . . ? B12 B10 H10 128.6(19) . . ? B9 B10 H10 128.5(17) . . ? B11 B10 H10 119.4(17) . . ? B5 B10 H10 119.9(19) . . ? C2 B11 B6 59.85(15) . . ? C2 B11 B10 106.16(19) . . ? B6 B11 B10 59.66(16) . . ? C2 B11 B12 107.09(19) . . ? B6 B11 B12 107.97(19) . . ? B10 B11 B12 59.31(16) . . ? C2 B11 B7 61.01(14) . . ? B6 B11 B7 109.93(18) . . ? B10 B11 B7 107.63(19) . . ? B12 B11 B7 59.73(16) . . ? C2 B11 H11 119.4(16) . . ? B6 B11 H11 121.8(16) . . ? B10 B11 H11 126.5(15) . . ? B12 B11 H11 123.6(16) . . ? B7 B11 H11 117.9(16) . . ? B9 B12 B10 60.09(16) . . ? B9 B12 B8 60.83(15) . . ? B10 B12 B8 110.7(2) . . ? B9 B12 B7 107.59(18) . . ? B10 B12 B7 108.76(19) . . ? B8 B12 B7 60.64(15) . . ? B9 B12 B11 107.50(19) . . ? B10 B12 B11 60.06(16) . . ? B8 B12 B11 110.10(19) . . ? B7 B12 B11 60.40(15) . . ? B9 B12 H12 123.0(17) . . ? B10 B12 H12 121.9(16) . . ? B8 B12 H12 118.9(16) . . ? B7 B12 H12 120.6(17) . . ? B11 B12 H12 121.4(16) . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.0(2) . . ? C15 C14 C2 122.7(2) . . ? C19 C14 C2 119.2(2) . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 119.3(2) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C14 121.2(3) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? C02 C01 Rh3 74.17(13) . . ? C02 C01 H01A 121(2) . . ? Rh3 C01 H01A 109.5(19) . . ? C02 C01 H01B 116.3(17) . . ? Rh3 C01 H01B 112.1(17) . . ? H01A C01 H01B 116(3) . . ? C03 C02 C01 121.3(2) . . ? C03 C02 C09 120.5(2) . . ? C01 C02 C09 117.9(2) . . ? C03 C02 Rh3 72.36(14) . . ? C01 C02 Rh3 67.89(13) . . ? C09 C02 Rh3 128.70(17) . . ? C02 C03 C04 123.2(2) . . ? C02 C03 C010 121.5(2) . . ? C04 C03 C010 115.2(2) . . ? C02 C03 Rh3 70.77(14) . . ? C04 C03 Rh3 70.83(13) . . ? C010 C03 Rh3 130.21(16) . . ? C05 C04 C03 129.6(2) . . ? C05 C04 Rh3 81.31(14) . . ? C03 C04 Rh3 71.40(14) . . ? C05 C04 H04 115(2) . . ? C03 C04 H04 115(2) . . ? Rh3 C04 H04 119.2(19) . . ? C04 C05 C06 123.1(2) . . ? C04 C05 Rh3 64.96(13) . . ? C06 C05 Rh3 130.37(16) . . ? C04 C05 H05 116(2) . . ? C06 C05 H05 120(2) . . ? Rh3 C05 H05 85(2) . . ? C07 C06 C05 120.1(2) . . ? C07 C06 C011 121.0(2) . . ? C05 C06 C011 118.6(2) . . ? C06 C07 C08 123.3(2) . . ? C06 C07 C012 123.0(2) . . ? C08 C07 C012 113.7(2) . . ? C07 C08 H08A 109.5 . . ? C07 C08 H08B 109.5 . . ? H08A C08 H08B 109.5 . . ? C07 C08 H08C 109.5 . . ? H08A C08 H08C 109.5 . . ? H08B C08 H08C 109.5 . . ? C02 C09 H09A 109.5 . . ? C02 C09 H09B 109.5 . . ? H09A C09 H09B 109.5 . . ? C02 C09 H09C 109.5 . . ? H09A C09 H09C 109.5 . . ? H09B C09 H09C 109.5 . . ? C03 C010 H01C 109.5 . . ? C03 C010 H01D 109.5 . . ? H01C C010 H01D 109.5 . . ? C03 C010 H01E 109.5 . . ? H01C C010 H01E 109.5 . . ? H01D C010 H01E 109.5 . . ? C06 C011 H01F 109.5 . . ? C06 C011 H01G 109.5 . . ? H01F C011 H01G 109.5 . . ? C06 C011 H01H 109.5 . . ? H01F C011 H01H 109.5 . . ? H01G C011 H01H 109.5 . . ? C07 C012 H01I 109.5 . . ? C07 C012 H01J 109.5 . . ? H01I C012 H01J 109.5 . . ? C07 C012 H01K 109.5 . . ? H01I C012 H01K 109.5 . . ? H01J C012 H01K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.795 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 965361'