Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew S.Weller' _publ_contact_author_address ;Department of Chemistry University of Bath Bath, BA2 7AY United Kingdom ; _publ_contact_author_email a.s.weller@bath.ac.uk _publ_contact_author_phone '44 1225 38 3394' _publ_contact_author_fax '44 1225 82 6231' _publ_section_title ; Cationic Rhodium Mono-Phosphine Fragments Stabilised by Carborane Monoanions [closo-CB11H6X]- (X = H, Br). Synthesis, Structures and Reactivity with Alkenes. ; loop_ _publ_author_name _publ_author_address 'Eduardo Molinos' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Simon K. Brayshaw' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Gabriele Kociok-Kohn' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Andrew S. Weller' ;University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; data_k05asw13 _database_code_depnum_ccdc_archive 'CCDC 655388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4b' _chemical_melting_point ? _chemical_formula_moiety 'C19 H41 B11 Br6 P Rh, C6 H5 F' _chemical_formula_sum 'C25 H46 B11 Br6 F P Rh' _chemical_formula_weight 1097.87 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.7857(3) _cell_length_b 13.1635(2) _cell_length_c 23.1199(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.8460(10) _cell_angle_gamma 90.00 _cell_volume 7703.90(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55280 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 6.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0535 _exptl_absorpt_correction_T_max 0.0949 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '358 1.5 degree images with \f and \w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 42541 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8692 _reflns_number_gt 7863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+17.1805P] 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 8692 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.108733(7) 0.385111(16) 0.056755(8) 0.01757(5) Uani 1 1 d . . . H1A H 0.0808(15) 0.364(3) -0.0025(17) 0.049(11) Uiso 1 1 d . . . H1B H 0.0621(12) 0.448(3) 0.0572(14) 0.030(8) Uiso 1 1 d . . . P P 0.13409(2) 0.52143(5) 0.01311(3) 0.01651(13) Uani 1 1 d . . . C2 C 0.11895(10) 0.6458(2) 0.04399(11) 0.0207(5) Uani 1 1 d . . . H2 H 0.1452 0.6953 0.0337 0.025 Uiso 1 1 calc R . . C3 C 0.12738(11) 0.6434(2) 0.11213(11) 0.0260(6) Uani 1 1 d . . . H3A H 0.1024 0.5944 0.1244 0.031 Uiso 1 1 calc R . . H3B H 0.1637 0.6198 0.1282 0.031 Uiso 1 1 calc R . . C4 C 0.11896(12) 0.7484(3) 0.13760(14) 0.0322(7) Uani 1 1 d . . . H4A H 0.1232 0.7434 0.1810 0.039 Uiso 1 1 calc R . . H4B H 0.1460 0.7960 0.1285 0.039 Uiso 1 1 calc R . . C5 C 0.06438(12) 0.7895(3) 0.11228(14) 0.0334(7) Uani 1 1 d . . . H5A H 0.0605 0.8585 0.1279 0.040 Uiso 1 1 calc R . . H5B H 0.0372 0.7453 0.1242 0.040 Uiso 1 1 calc R . . C6 C 0.05641(13) 0.7934(3) 0.04520(14) 0.0361(7) Uani 1 1 d . . . H6A H 0.0818 0.8422 0.0335 0.043 Uiso 1 1 calc R . . H6B H 0.0203 0.8182 0.0291 0.043 Uiso 1 1 calc R . . C7 C 0.06412(11) 0.6895(3) 0.01878(13) 0.0288(6) Uani 1 1 d . . . H7A H 0.0600 0.6958 -0.0245 0.035 Uiso 1 1 calc R . . H7B H 0.0366 0.6423 0.0273 0.035 Uiso 1 1 calc R . . C8 C 0.20627(9) 0.5245(2) 0.01490(10) 0.0174(5) Uani 1 1 d . . . H8 H 0.2142 0.4621 -0.0065 0.021 Uiso 1 1 calc R . . C9 C 0.22405(10) 0.6142(2) -0.01919(11) 0.0221(5) Uani 1 1 d . . . H9A H 0.2015 0.6182 -0.0588 0.026 Uiso 1 1 calc R . . H9B H 0.2200 0.6784 0.0018 0.026 Uiso 1 1 calc R . . C10 C 0.28177(10) 0.6009(2) -0.02516(12) 0.0251(6) Uani 1 1 d . . . H10A H 0.2850 0.5399 -0.0492 0.030 Uiso 1 1 calc R . . H10B H 0.2930 0.6606 -0.0459 0.030 Uiso 1 1 calc R . . C11 C 0.31782(10) 0.5899(2) 0.03450(12) 0.0272(6) Uani 1 1 d . . . H11A H 0.3179 0.6540 0.0569 0.033 Uiso 1 1 calc R . . H11B H 0.3544 0.5766 0.0290 0.033 Uiso 1 1 calc R . . C12 C 0.29933(10) 0.5029(2) 0.06913(12) 0.0257(6) Uani 1 1 d . . . H12A H 0.3223 0.4987 0.1085 0.031 Uiso 1 1 calc R . . H12B H 0.3024 0.4380 0.0484 0.031 Uiso 1 1 calc R . . C13 C 0.24189(10) 0.5184(2) 0.07616(11) 0.0220(5) Uani 1 1 d . . . H13A H 0.2389 0.5819 0.0983 0.026 Uiso 1 1 calc R . . H13B H 0.2306 0.4611 0.0986 0.026 Uiso 1 1 calc R . . C14 C 0.10639(9) 0.5289(2) -0.06714(10) 0.0191(5) Uani 1 1 d . . . H14 H 0.1124 0.5998 -0.0800 0.023 Uiso 1 1 calc R . . C15 C 0.04651(10) 0.5081(2) -0.08387(11) 0.0249(6) Uani 1 1 d . . . H15A H 0.0393 0.4362 -0.0755 0.030 Uiso 1 1 calc R . . H15B H 0.0274 0.5515 -0.0598 0.030 Uiso 1 1 calc R . . C16 C 0.02673(11) 0.5304(3) -0.14945(12) 0.0330(7) Uani 1 1 d . . . H16A H -0.0117 0.5173 -0.1596 0.040 Uiso 1 1 calc R . . H16B H 0.0328 0.6029 -0.1574 0.040 Uiso 1 1 calc R . . C17 C 0.05505(12) 0.4645(3) -0.18739(12) 0.0390(8) Uani 1 1 d . . . H17A H 0.0440 0.4847 -0.2292 0.047 Uiso 1 1 calc R . . H17B H 0.0448 0.3927 -0.1837 0.047 Uiso 1 1 calc R . . C18 C 0.11492(11) 0.4741(3) -0.16978(12) 0.0322(7) Uani 1 1 d . . . H18A H 0.1258 0.5426 -0.1805 0.039 Uiso 1 1 calc R . . H18B H 0.1318 0.4237 -0.1921 0.039 Uiso 1 1 calc R . . C19 C 0.13453(10) 0.4571(2) -0.10372(11) 0.0236(5) Uani 1 1 d . . . H19A H 0.1731 0.4693 -0.0939 0.028 Uiso 1 1 calc R . . H19B H 0.1279 0.3858 -0.0937 0.028 Uiso 1 1 calc R . . C1 C 0.18430(11) 0.0221(2) 0.19986(11) 0.0241(5) Uani 1 1 d . . . H1 H 0.1904 -0.0619 0.2046 0.029 Uiso 1 1 calc R . . B2 B 0.12093(12) 0.0660(3) 0.19282(13) 0.0239(6) Uani 1 1 d . . . H2A H 0.0851 0.0180 0.1926 0.029 Uiso 1 1 calc R . . B3 B 0.15505(12) 0.0656(2) 0.13209(13) 0.0220(6) Uani 1 1 d . . . H3 H 0.1414 0.0175 0.0921 0.026 Uiso 1 1 calc R . . B4 B 0.22387(12) 0.0860(2) 0.16111(13) 0.0221(6) Uani 1 1 d . . . H4 H 0.2554 0.0509 0.1402 0.027 Uiso 1 1 calc R . . B5 B 0.23191(12) 0.0993(3) 0.23892(13) 0.0238(6) Uani 1 1 d . . . H5 H 0.2686 0.0727 0.2690 0.029 Uiso 1 1 calc R . . B6 B 0.16849(13) 0.0867(3) 0.25862(13) 0.0245(6) Uani 1 1 d . . . H6 H 0.1638 0.0516 0.3015 0.029 Uiso 1 1 calc R . . B7 B 0.12071(11) 0.1747(2) 0.14839(12) 0.0183(5) Uani 1 1 d . . . Br7 Br 0.059190(10) 0.22984(2) 0.093546(11) 0.02308(6) Uani 1 1 d . . . B8 B 0.18351(11) 0.1870(2) 0.12862(12) 0.0179(5) Uani 1 1 d . . . Br8 Br 0.188399(10) 0.25145(2) 0.052924(11) 0.02180(6) Uani 1 1 d . . . B9 B 0.23125(11) 0.2089(2) 0.19389(12) 0.0192(6) Uani 1 1 d . . . Br9 Br 0.293679(10) 0.29135(2) 0.192796(12) 0.02673(7) Uani 1 1 d . . . B10 B 0.19682(12) 0.2091(2) 0.25465(12) 0.0206(6) Uani 1 1 d . . . Br10 Br 0.221357(11) 0.29146(2) 0.324489(11) 0.02810(7) Uani 1 1 d . . . B11 B 0.12812(11) 0.1882(2) 0.22613(12) 0.0203(6) Uani 1 1 d . . . Br11 Br 0.072752(12) 0.24747(2) 0.261724(13) 0.03040(7) Uani 1 1 d . . . B12 B 0.16693(11) 0.2632(2) 0.18599(12) 0.0169(5) Uani 1 1 d . . . Br12 Br 0.152475(9) 0.407985(19) 0.172838(10) 0.01914(6) Uani 1 1 d . . . C21 C 0.04128(17) -0.0153(4) -0.1139(4) 0.089(2) Uani 1 1 d . . . H21 H 0.0273 -0.0790 -0.1051 0.106 Uiso 1 1 calc R . . C22 C 0.04536(18) 0.0131(4) -0.1725(3) 0.0730(16) Uani 1 1 d . B . H22 H 0.0346 -0.0329 -0.2042 0.088 Uiso 1 1 calc R . . C23 C 0.0641(2) 0.1036(4) -0.1826(2) 0.0682(13) Uani 1 1 d . . . C24 C 0.07994(16) 0.1687(4) -0.1402(3) 0.0685(14) Uani 1 1 d . B . H24 H 0.0931 0.2329 -0.1495 0.082 Uiso 1 1 calc R . . C25 C 0.07793(16) 0.1468(4) -0.0838(2) 0.0633(13) Uani 1 1 d . . . H25 H 0.0898 0.1952 -0.0537 0.076 Uiso 1 1 calc R B . C26 C 0.05944(18) 0.0579(5) -0.0700(2) 0.0652(13) Uani 1 1 d . A . F1 F 0.0592(2) 0.0394(5) -0.0150(2) 0.104(2) Uani 0.60 1 d P A 1 F1A F 0.0737(4) 0.1402(11) -0.2279(5) 0.140(5) Uani 0.40 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.01729(9) 0.01797(11) 0.01640(9) 0.00222(7) 0.00049(7) -0.00143(7) P 0.0156(3) 0.0175(3) 0.0157(3) 0.0017(2) 0.0011(2) -0.0003(2) C2 0.0191(11) 0.0198(13) 0.0232(12) 0.0018(10) 0.0040(9) 0.0018(10) C3 0.0291(13) 0.0264(15) 0.0211(12) -0.0024(11) 0.0015(10) 0.0040(12) C4 0.0327(15) 0.0307(17) 0.0309(15) -0.0104(12) 0.0005(12) 0.0044(13) C5 0.0309(14) 0.0327(18) 0.0364(16) -0.0086(13) 0.0056(12) 0.0096(13) C6 0.0376(16) 0.0318(18) 0.0377(16) -0.0025(14) 0.0044(13) 0.0163(14) C7 0.0244(13) 0.0334(17) 0.0274(14) 0.0004(12) 0.0018(10) 0.0092(12) C8 0.0166(10) 0.0184(13) 0.0165(11) -0.0015(9) 0.0011(8) -0.0004(9) C9 0.0194(11) 0.0248(15) 0.0218(12) 0.0045(10) 0.0036(9) -0.0018(10) C10 0.0235(12) 0.0304(16) 0.0230(12) 0.0005(11) 0.0088(10) -0.0025(11) C11 0.0181(11) 0.0350(17) 0.0280(14) -0.0035(12) 0.0031(10) -0.0043(11) C12 0.0193(11) 0.0330(16) 0.0227(12) -0.0008(11) -0.0016(10) 0.0029(11) C13 0.0192(11) 0.0301(15) 0.0154(11) 0.0005(10) 0.0001(9) -0.0031(11) C14 0.0175(11) 0.0237(14) 0.0152(11) 0.0035(10) 0.0004(8) -0.0018(10) C15 0.0181(11) 0.0340(16) 0.0213(12) 0.0030(11) 0.0004(9) -0.0028(11) C16 0.0222(12) 0.048(2) 0.0251(14) 0.0091(13) -0.0052(10) 0.0001(13) C17 0.0313(14) 0.061(2) 0.0201(13) -0.0031(14) -0.0060(11) -0.0022(15) C18 0.0305(14) 0.049(2) 0.0161(12) -0.0030(12) 0.0014(10) 0.0021(14) C19 0.0239(12) 0.0260(15) 0.0191(12) -0.0022(10) -0.0007(9) 0.0020(11) C1 0.0318(13) 0.0181(14) 0.0222(12) 0.0007(10) 0.0042(10) 0.0003(11) B2 0.0286(14) 0.0185(15) 0.0251(14) 0.0038(12) 0.0066(12) -0.0010(12) B3 0.0267(14) 0.0182(15) 0.0210(13) 0.0003(11) 0.0044(11) 0.0003(12) B4 0.0259(13) 0.0167(15) 0.0236(14) -0.0014(11) 0.0043(11) 0.0027(12) B5 0.0264(14) 0.0216(16) 0.0217(14) 0.0023(12) 0.0004(11) 0.0058(12) B6 0.0329(15) 0.0202(16) 0.0208(14) 0.0027(12) 0.0060(12) 0.0030(13) B7 0.0197(12) 0.0159(14) 0.0189(12) 0.0000(10) 0.0026(10) 0.0000(11) Br7 0.01858(11) 0.02341(14) 0.02523(13) 0.00469(10) -0.00110(9) -0.00408(10) B8 0.0217(12) 0.0171(14) 0.0152(12) 0.0010(10) 0.0040(10) 0.0014(11) Br8 0.02565(12) 0.02414(15) 0.01629(12) 0.00059(9) 0.00565(9) 0.00062(10) B9 0.0193(12) 0.0186(15) 0.0192(13) 0.0007(11) 0.0019(10) 0.0018(11) Br9 0.01969(12) 0.03054(16) 0.02880(14) -0.00059(11) 0.00161(10) -0.00282(11) B10 0.0249(13) 0.0185(15) 0.0177(13) -0.0004(11) 0.0020(10) 0.0009(12) Br10 0.03519(14) 0.03018(16) 0.01705(12) -0.00436(10) 0.00010(10) 0.00039(12) B11 0.0239(13) 0.0178(15) 0.0193(13) 0.0012(11) 0.0046(10) 0.0023(12) Br11 0.03139(14) 0.03049(17) 0.03332(15) 0.00024(12) 0.01629(12) 0.00277(12) B12 0.0199(12) 0.0144(14) 0.0160(12) 0.0005(10) 0.0019(10) 0.0009(11) Br12 0.02341(12) 0.01523(13) 0.01803(11) 0.00019(9) 0.00194(9) 0.00021(9) C21 0.037(2) 0.038(3) 0.194(7) 0.028(4) 0.027(3) 0.0068(19) C22 0.056(3) 0.066(4) 0.086(3) -0.044(3) -0.014(2) 0.014(2) C23 0.070(3) 0.065(3) 0.075(3) -0.001(3) 0.027(3) 0.025(3) C24 0.041(2) 0.048(3) 0.121(4) -0.010(3) 0.027(2) 0.005(2) C25 0.044(2) 0.061(3) 0.076(3) -0.030(3) -0.009(2) 0.015(2) C26 0.056(2) 0.076(4) 0.065(3) 0.014(3) 0.014(2) 0.038(3) F1 0.123(4) 0.119(5) 0.080(3) 0.045(3) 0.046(3) 0.065(4) F1A 0.135(9) 0.195(13) 0.104(7) 0.044(8) 0.062(7) 0.031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh P 2.2165(7) . ? Rh Br7 2.6346(3) . ? Rh Br8 2.7187(3) . ? Rh Br12 2.7241(3) . ? Rh H1A 1.45(4) . ? Rh H1B 1.46(3) . ? P C8 1.854(2) . ? P C2 1.856(3) . ? P C14 1.860(2) . ? C2 C7 1.536(3) . ? C2 C3 1.549(4) . ? C2 H2 1.0000 . ? C3 C4 1.533(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.519(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.526(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.526(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.536(4) . ? C8 C13 1.538(3) . ? C8 H8 1.0000 . ? C9 C10 1.530(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.524(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.534(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.538(4) . ? C14 C15 1.544(3) . ? C14 H14 1.0000 . ? C15 C16 1.534(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.514(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.526(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.531(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C1 B4 1.701(4) . ? C1 B3 1.704(4) . ? C1 B2 1.712(4) . ? C1 B5 1.714(4) . ? C1 B6 1.715(4) . ? C1 H1 1.1200 . ? B2 B7 1.760(4) . ? B2 B11 1.777(5) . ? B2 B6 1.786(4) . ? B2 B3 1.791(4) . ? B2 H2A 1.1200 . ? B3 B7 1.765(4) . ? B3 B8 1.767(4) . ? B3 B4 1.795(4) . ? B3 H3 1.1200 . ? B4 B8 1.766(4) . ? B4 B5 1.779(4) . ? B4 B9 1.781(4) . ? B4 H4 1.1200 . ? B5 B9 1.777(4) . ? B5 B10 1.778(4) . ? B5 B6 1.786(4) . ? B5 H5 1.1200 . ? B6 B11 1.771(4) . ? B6 B10 1.778(5) . ? B6 H6 1.1200 . ? B7 B8 1.771(4) . ? B7 B12 1.773(4) . ? B7 B11 1.779(4) . ? B7 Br7 1.973(3) . ? B8 B12 1.778(4) . ? B8 B9 1.782(4) . ? B8 Br8 1.970(3) . ? B9 B12 1.784(4) . ? B9 B10 1.797(4) . ? B9 Br9 1.946(3) . ? B10 B12 1.778(4) . ? B10 B11 1.791(4) . ? B10 Br10 1.949(3) . ? B11 B12 1.786(4) . ? B11 Br11 1.941(3) . ? B12 Br12 1.954(3) . ? C21 C26 1.414(8) . ? C21 C22 1.427(8) . ? C21 H21 0.9500 . ? C22 C23 1.322(8) . ? C22 H22 0.9500 . ? C23 F1A 1.218(10) . ? C23 C24 1.309(7) . ? C24 C25 1.347(7) . ? C24 H24 0.9500 . ? C25 C26 1.325(7) . ? C25 H25 0.9500 . ? C26 F1 1.294(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 P Rh Br7 167.786(18) . . ? P Rh Br8 102.689(18) . . ? Br7 Rh Br8 85.627(10) . . ? P Rh Br12 104.818(18) . . ? Br7 Rh Br12 84.491(9) . . ? Br8 Rh Br12 85.884(9) . . ? P Rh H1A 81.9(16) . . ? Br7 Rh H1A 88.5(16) . . ? Br8 Rh H1A 95.3(16) . . ? Br12 Rh H1A 172.8(16) . . ? P Rh H1B 82.0(13) . . ? Br7 Rh H1B 89.2(13) . . ? Br8 Rh H1B 173.9(14) . . ? Br12 Rh H1B 96.9(13) . . ? H1A Rh H1B 81(2) . . ? C8 P C2 104.76(12) . . ? C8 P C14 102.51(11) . . ? C2 P C14 105.52(12) . . ? C8 P Rh 112.86(9) . . ? C2 P Rh 115.94(9) . . ? C14 P Rh 113.93(9) . . ? C7 C2 C3 109.6(2) . . ? C7 C2 P 115.45(19) . . ? C3 C2 P 111.94(19) . . ? C7 C2 H2 106.4 . . ? C3 C2 H2 106.4 . . ? P C2 H2 106.4 . . ? C4 C3 C2 111.7(2) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 111.2(2) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 110.0(3) . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 C7 111.9(3) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C2 111.3(2) . . ? C6 C7 H7A 109.4 . . ? C2 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C2 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 109.2(2) . . ? C9 C8 P 113.62(17) . . ? C13 C8 P 116.27(17) . . ? C9 C8 H8 105.6 . . ? C13 C8 H8 105.6 . . ? P C8 H8 105.6 . . ? C10 C9 C8 110.4(2) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.6(2) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.5(2) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 111.0(2) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C8 109.3(2) . . ? C12 C13 H13A 109.8 . . ? C8 C13 H13A 109.8 . . ? C12 C13 H13B 109.8 . . ? C8 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C19 C14 C15 107.8(2) . . ? C19 C14 P 112.53(17) . . ? C15 C14 P 114.74(17) . . ? C19 C14 H14 107.1 . . ? C15 C14 H14 107.1 . . ? P C14 H14 107.1 . . ? C16 C15 C14 110.1(2) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 110.8(3) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.9(3) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 112.4(2) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C14 110.9(2) . . ? C18 C19 H19A 109.5 . . ? C14 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 108.0 . . ? B4 C1 B3 63.64(17) . . ? B4 C1 B2 116.1(2) . . ? B3 C1 B2 63.25(17) . . ? B4 C1 B5 62.80(18) . . ? B3 C1 B5 115.7(2) . . ? B2 C1 B5 115.2(2) . . ? B4 C1 B6 115.3(2) . . ? B3 C1 B6 115.6(2) . . ? B2 C1 B6 62.80(18) . . ? B5 C1 B6 62.79(18) . . ? B4 C1 H1 116.9 . . ? B3 C1 H1 116.8 . . ? B2 C1 H1 117.1 . . ? B5 C1 H1 117.5 . . ? B6 C1 H1 117.5 . . ? C1 B2 B7 103.2(2) . . ? C1 B2 B11 104.1(2) . . ? B7 B2 B11 60.41(17) . . ? C1 B2 B6 58.67(17) . . ? B7 B2 B6 107.4(2) . . ? B11 B2 B6 59.63(17) . . ? C1 B2 B3 58.16(16) . . ? B7 B2 B3 59.60(17) . . ? B11 B2 B3 108.4(2) . . ? B6 B2 B3 107.9(2) . . ? C1 B2 H2A 125.6 . . ? B7 B2 H2A 123.0 . . ? B11 B2 H2A 122.1 . . ? B6 B2 H2A 121.6 . . ? B3 B2 H2A 121.4 . . ? C1 B3 B7 103.3(2) . . ? C1 B3 B8 103.3(2) . . ? B7 B3 B8 60.18(17) . . ? C1 B3 B2 58.59(16) . . ? B7 B3 B2 59.32(17) . . ? B8 B3 B2 107.6(2) . . ? C1 B3 B4 58.11(16) . . ? B7 B3 B4 107.4(2) . . ? B8 B3 B4 59.43(17) . . ? B2 B3 B4 107.7(2) . . ? C1 B3 H3 125.8 . . ? B7 B3 H3 122.9 . . ? B8 B3 H3 122.8 . . ? B2 B3 H3 121.6 . . ? B4 B3 H3 121.8 . . ? C1 B4 B8 103.4(2) . . ? C1 B4 B5 58.94(17) . . ? B8 B4 B5 107.6(2) . . ? C1 B4 B9 104.6(2) . . ? B8 B4 B9 60.32(17) . . ? B5 B4 B9 59.87(17) . . ? C1 B4 B3 58.25(16) . . ? B8 B4 B3 59.48(17) . . ? B5 B4 B3 108.1(2) . . ? B9 B4 B3 108.3(2) . . ? C1 B4 H4 125.3 . . ? B8 B4 H4 123.0 . . ? B5 B4 H4 121.4 . . ? B9 B4 H4 122.1 . . ? B3 B4 H4 121.5 . . ? C1 B5 B9 104.2(2) . . ? C1 B5 B10 104.3(2) . . ? B9 B5 B10 60.72(17) . . ? C1 B5 B4 58.26(17) . . ? B9 B5 B4 60.10(17) . . ? B10 B5 B4 108.6(2) . . ? C1 B5 B6 58.64(17) . . ? B9 B5 B6 108.5(2) . . ? B10 B5 B6 59.86(18) . . ? B4 B5 B6 108.1(2) . . ? C1 B5 H5 125.4 . . ? B9 B5 H5 122.1 . . ? B10 B5 H5 122.1 . . ? B4 B5 H5 121.3 . . ? B6 B5 H5 121.4 . . ? C1 B6 B11 104.3(2) . . ? C1 B6 B10 104.3(2) . . ? B11 B6 B10 60.61(17) . . ? C1 B6 B2 58.52(17) . . ? B11 B6 B2 59.95(17) . . ? B10 B6 B2 108.5(2) . . ? C1 B6 B5 58.58(17) . . ? B11 B6 B5 108.4(2) . . ? B10 B6 B5 59.85(18) . . ? B2 B6 B5 108.2(2) . . ? C1 B6 H6 125.3 . . ? B11 B6 H6 122.2 . . ? B10 B6 H6 122.2 . . ? B2 B6 H6 121.3 . . ? B5 B6 H6 121.4 . . ? B2 B7 B3 61.08(17) . . ? B2 B7 B8 108.8(2) . . ? B3 B7 B8 59.96(17) . . ? B2 B7 B12 108.7(2) . . ? B3 B7 B12 108.8(2) . . ? B8 B7 B12 60.22(16) . . ? B2 B7 B11 60.27(17) . . ? B3 B7 B11 109.5(2) . . ? B8 B7 B11 108.77(19) . . ? B12 B7 B11 60.34(16) . . ? B2 B7 Br7 125.99(18) . . ? B3 B7 Br7 122.51(18) . . ? B8 B7 Br7 117.67(17) . . ? B12 B7 Br7 117.25(18) . . ? B11 B7 Br7 122.17(18) . . ? B7 Br7 Rh 96.47(9) . . ? B4 B8 B3 61.09(17) . . ? B4 B8 B7 108.4(2) . . ? B3 B8 B7 59.86(17) . . ? B4 B8 B12 108.23(19) . . ? B3 B8 B12 108.5(2) . . ? B7 B8 B12 59.96(16) . . ? B4 B8 B9 60.26(16) . . ? B3 B8 B9 109.6(2) . . ? B7 B8 B9 108.42(19) . . ? B12 B8 B9 60.14(16) . . ? B4 B8 Br8 124.80(18) . . ? B3 B8 Br8 121.78(18) . . ? B7 B8 Br8 118.88(17) . . ? B12 B8 Br8 118.92(18) . . ? B9 B8 Br8 122.19(18) . . ? B8 Br8 Rh 94.29(8) . . ? B5 B9 B4 60.02(17) . . ? B5 B9 B8 107.1(2) . . ? B4 B9 B8 59.43(16) . . ? B5 B9 B12 107.0(2) . . ? B4 B9 B12 107.3(2) . . ? B8 B9 B12 59.82(15) . . ? B5 B9 B10 59.68(17) . . ? B4 B9 B10 107.7(2) . . ? B8 B9 B10 107.30(19) . . ? B12 B9 B10 59.53(16) . . ? B5 B9 Br9 122.94(18) . . ? B4 B9 Br9 121.56(18) . . ? B8 B9 Br9 121.38(18) . . ? B12 B9 Br9 122.05(19) . . ? B10 B9 Br9 122.77(18) . . ? B12 B10 B5 107.2(2) . . ? B12 B10 B6 107.2(2) . . ? B5 B10 B6 60.29(18) . . ? B12 B10 B11 60.04(16) . . ? B5 B10 B11 107.8(2) . . ? B6 B10 B11 59.50(17) . . ? B12 B10 B9 59.87(16) . . ? B5 B10 B9 59.60(17) . . ? B6 B10 B9 107.9(2) . . ? B11 B10 B9 108.19(19) . . ? B12 B10 Br10 122.3(2) . . ? B5 B10 Br10 121.53(18) . . ? B6 B10 Br10 122.27(18) . . ? B11 B10 Br10 122.33(19) . . ? B9 B10 Br10 121.11(19) . . ? B6 B11 B2 60.43(18) . . ? B6 B11 B7 107.2(2) . . ? B2 B11 B7 59.32(17) . . ? B6 B11 B12 107.2(2) . . ? B2 B11 B12 107.4(2) . . ? B7 B11 B12 59.66(16) . . ? B6 B11 B10 59.89(17) . . ? B2 B11 B10 108.3(2) . . ? B7 B11 B10 107.3(2) . . ? B12 B11 B10 59.60(16) . . ? B6 B11 Br11 122.97(18) . . ? B2 B11 Br11 121.49(19) . . ? B7 B11 Br11 121.35(18) . . ? B12 B11 Br11 121.78(19) . . ? B10 B11 Br11 122.53(19) . . ? B7 B12 B10 108.2(2) . . ? B7 B12 B8 59.82(16) . . ? B10 B12 B8 108.3(2) . . ? B7 B12 B9 108.2(2) . . ? B10 B12 B9 60.60(16) . . ? B8 B12 B9 60.04(16) . . ? B7 B12 B11 60.00(16) . . ? B10 B12 B11 60.36(16) . . ? B8 B12 B11 108.2(2) . . ? B9 B12 B11 109.0(2) . . ? B7 B12 Br12 118.28(17) . . ? B10 B12 Br12 124.60(18) . . ? B8 B12 Br12 120.00(17) . . ? B9 B12 Br12 123.60(18) . . ? B11 B12 Br12 120.74(18) . . ? B12 Br12 Rh 94.41(8) . . ? C26 C21 C22 115.4(5) . . ? C26 C21 H21 122.3 . . ? C22 C21 H21 122.3 . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? F1A C23 C24 107.4(9) . . ? F1A C23 C22 130.4(9) . . ? C24 C23 C22 122.0(5) . . ? C23 C24 C25 121.5(5) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 120.2(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? F1 C26 C25 118.0(6) . . ? F1 C26 C21 121.0(6) . . ? C25 C26 C21 121.0(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.723 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.098 #===END data_k06asw11 _database_code_depnum_ccdc_archive 'CCDC 655389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5b' _chemical_melting_point ? _chemical_formula_moiety 'C38 H90 B22 P2 Rh2, C5 H12' _chemical_formula_sum 'C43 H102 B22 P2 Rh2' _chemical_formula_weight 1124.83 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 12.34430(10) _cell_length_b 20.10830(10) _cell_length_c 23.4143(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.35 _cell_angle_gamma 90.00 _cell_volume 5802.04(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 174804 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.508 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8533 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '723 1.0 degree images with \f and \w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 127863 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 30.51 _reflns_number_total 17673 _reflns_number_gt 14331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+7.9716P] 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 17673 _refine_ls_number_parameters 646 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 1.031849(14) 0.220352(8) 0.132071(7) 0.01703(5) Uani 1 1 d D . . Rh2 Rh 1.003350(15) 0.351990(9) 0.095744(8) 0.01884(5) Uani 1 1 d D . . P1 P 1.01820(5) 0.11231(3) 0.15240(3) 0.01892(12) Uani 1 1 d . . . P2 P 0.88186(5) 0.41486(3) 0.13985(3) 0.02041(12) Uani 1 1 d . . . C11 C 1.0227(2) 0.10781(12) 0.23214(10) 0.0239(5) Uani 1 1 d . . . H11 H 1.0860 0.1361 0.2453 0.029 Uiso 1 1 calc R . . C12 C 0.9243(2) 0.14051(16) 0.25768(11) 0.0337(6) Uani 1 1 d . . . H12A H 0.9089 0.1836 0.2385 0.040 Uiso 1 1 calc R . . H12B H 0.8599 0.1116 0.2510 0.040 Uiso 1 1 calc R . . C13 C 0.9458(3) 0.15188(19) 0.32205(13) 0.0484(9) Uani 1 1 d . . . H13A H 1.0082 0.1824 0.3288 0.058 Uiso 1 1 calc R . . H13B H 0.8814 0.1728 0.3379 0.058 Uiso 1 1 calc R . . C14 C 0.9700(3) 0.0858(2) 0.35205(13) 0.0473(8) Uani 1 1 d . . . H14A H 0.9888 0.0941 0.3931 0.057 Uiso 1 1 calc R . . H14B H 0.9044 0.0575 0.3491 0.057 Uiso 1 1 calc R . . C15 C 1.0628(3) 0.04970(17) 0.32608(12) 0.0413(7) Uani 1 1 d . . . H15A H 1.0723 0.0056 0.3445 0.050 Uiso 1 1 calc R . . H15B H 1.1306 0.0752 0.3340 0.050 Uiso 1 1 calc R . . C16 C 1.0439(3) 0.04018(15) 0.26126(12) 0.0360(6) Uani 1 1 d . . . H16A H 0.9809 0.0105 0.2532 0.043 Uiso 1 1 calc R . . H16B H 1.1084 0.0191 0.2458 0.043 Uiso 1 1 calc R . . C17 C 1.1297(2) 0.05562(12) 0.13353(10) 0.0217(5) Uani 1 1 d . . . H17 H 1.1213 0.0140 0.1562 0.026 Uiso 1 1 calc R . . C18 C 1.2415(2) 0.08433(14) 0.15184(13) 0.0314(6) Uani 1 1 d . . . H18A H 1.2515 0.1269 0.1316 0.038 Uiso 1 1 calc R . . H18B H 1.2445 0.0937 0.1934 0.038 Uiso 1 1 calc R . . C19 C 1.3341(2) 0.03715(15) 0.13899(14) 0.0356(6) Uani 1 1 d . . . H19A H 1.4044 0.0596 0.1482 0.043 Uiso 1 1 calc R . . H19B H 1.3307 -0.0027 0.1636 0.043 Uiso 1 1 calc R . . C20 C 1.3283(2) 0.01576(16) 0.07665(13) 0.0384(7) Uani 1 1 d . . . H20A H 1.3399 0.0547 0.0519 0.046 Uiso 1 1 calc R . . H20B H 1.3860 -0.0172 0.0704 0.046 Uiso 1 1 calc R . . C21 C 1.2181(2) -0.01465(15) 0.06114(12) 0.0339(6) Uani 1 1 d . . . H21A H 1.2083 -0.0547 0.0849 0.041 Uiso 1 1 calc R . . H21B H 1.2147 -0.0286 0.0205 0.041 Uiso 1 1 calc R . . C22 C 1.1267(2) 0.03486(13) 0.07058(11) 0.0282(5) Uani 1 1 d . . . H22A H 1.1353 0.0746 0.0462 0.034 Uiso 1 1 calc R . . H22B H 1.0558 0.0141 0.0596 0.034 Uiso 1 1 calc R . . C23 C 0.8952(2) 0.06942(12) 0.12103(11) 0.0229(5) Uani 1 1 d . . . H23 H 0.9020 0.0709 0.0787 0.027 Uiso 1 1 calc R . . C24 C 0.8862(2) -0.00527(13) 0.13598(13) 0.0330(6) Uani 1 1 d . . . H24A H 0.9560 -0.0278 0.1300 0.040 Uiso 1 1 calc R . . H24B H 0.8704 -0.0103 0.1767 0.040 Uiso 1 1 calc R . . C25 C 0.7953(3) -0.03760(14) 0.09798(14) 0.0375(7) Uani 1 1 d . . . H25A H 0.8143 -0.0354 0.0575 0.045 Uiso 1 1 calc R . . H25B H 0.7890 -0.0851 0.1085 0.045 Uiso 1 1 calc R . . C26 C 0.6866(2) -0.00338(15) 0.10413(14) 0.0390(7) Uani 1 1 d . . . H26A H 0.6619 -0.0118 0.1430 0.047 Uiso 1 1 calc R . . H26B H 0.6321 -0.0226 0.0761 0.047 Uiso 1 1 calc R . . C27 C 0.6938(2) 0.07142(14) 0.09438(13) 0.0331(6) Uani 1 1 d . . . H27A H 0.6244 0.0924 0.1035 0.040 Uiso 1 1 calc R . . H27B H 0.7050 0.0800 0.0535 0.040 Uiso 1 1 calc R . . C28 C 0.7865(2) 0.10327(14) 0.13111(12) 0.0290(5) Uani 1 1 d . . . H28A H 0.7711 0.0995 0.1720 0.035 Uiso 1 1 calc R . . H28B H 0.7912 0.1511 0.1216 0.035 Uiso 1 1 calc R . . C31 C 0.7965(2) 0.45868(14) 0.08334(12) 0.0329(6) Uani 1 1 d . . . H31 H 0.7685 0.4996 0.1018 0.040 Uiso 1 1 calc R . . C32 C 0.8650(3) 0.48300(15) 0.03476(12) 0.0376(7) Uani 1 1 d . . . H32A H 0.9276 0.5088 0.0512 0.045 Uiso 1 1 calc R . . H32B H 0.8935 0.4441 0.0145 0.045 Uiso 1 1 calc R . . C33 C 0.7987(4) 0.52635(18) -0.00774(15) 0.0572(10) Uani 1 1 d . . . H33A H 0.7769 0.5677 0.0114 0.069 Uiso 1 1 calc R . . H33B H 0.8438 0.5388 -0.0397 0.069 Uiso 1 1 calc R . . C34 C 0.6982(4) 0.4897(2) -0.03114(18) 0.0700(14) Uani 1 1 d . . . H34A H 0.6535 0.5200 -0.0561 0.084 Uiso 1 1 calc R . . H34B H 0.7203 0.4517 -0.0547 0.084 Uiso 1 1 calc R . . C35 C 0.6307(3) 0.4643(2) 0.01628(19) 0.0646(13) Uani 1 1 d . . . H35A H 0.5689 0.4382 -0.0007 0.078 Uiso 1 1 calc R . . H35B H 0.6008 0.5027 0.0367 0.078 Uiso 1 1 calc R . . C36 C 0.6965(3) 0.42083(17) 0.05910(16) 0.0462(8) Uani 1 1 d . . . H36A H 0.7196 0.3798 0.0399 0.055 Uiso 1 1 calc R . . H36B H 0.6508 0.4079 0.0907 0.055 Uiso 1 1 calc R . . C37 C 0.93932(18) 0.48418(11) 0.18423(10) 0.0197(4) Uani 1 1 d . . . H37 H 0.9783 0.4629 0.2181 0.024 Uiso 1 1 calc R . . C38 C 0.8542(2) 0.53115(13) 0.20866(12) 0.0277(5) Uani 1 1 d . . . H38A H 0.8177 0.5572 0.1772 0.033 Uiso 1 1 calc R . . H38B H 0.7984 0.5046 0.2271 0.033 Uiso 1 1 calc R . . C39 C 0.9097(2) 0.57825(14) 0.25240(12) 0.0314(6) Uani 1 1 d . . . H39A H 0.8551 0.6093 0.2666 0.038 Uiso 1 1 calc R . . H39B H 0.9402 0.5521 0.2854 0.038 Uiso 1 1 calc R . . C40 C 1.0002(2) 0.61809(13) 0.22699(13) 0.0328(6) Uani 1 1 d . . . H40A H 0.9684 0.6490 0.1977 0.039 Uiso 1 1 calc R . . H40B H 1.0380 0.6450 0.2575 0.039 Uiso 1 1 calc R . . C41 C 1.0816(2) 0.57289(13) 0.19996(12) 0.0280(5) Uani 1 1 d . . . H41A H 1.1203 0.5459 0.2301 0.034 Uiso 1 1 calc R . . H41B H 1.1358 0.6002 0.1811 0.034 Uiso 1 1 calc R . . C42 C 1.0242(2) 0.52677(12) 0.15584(11) 0.0231(5) Uani 1 1 d . . . H42A H 1.0782 0.4975 0.1388 0.028 Uiso 1 1 calc R . . H42B H 0.9883 0.5536 0.1248 0.028 Uiso 1 1 calc R . . C43 C 0.7847(2) 0.37365(12) 0.18594(12) 0.0272(5) Uani 1 1 d . . . H43 H 0.7193 0.4029 0.1865 0.033 Uiso 1 1 calc R . . C44 C 0.8276(2) 0.36384(15) 0.24834(13) 0.0354(6) Uani 1 1 d . . . H44A H 0.8526 0.4070 0.2646 0.042 Uiso 1 1 calc R . . H44B H 0.8903 0.3330 0.2497 0.042 Uiso 1 1 calc R . . C45 C 0.7378(3) 0.33528(16) 0.28416(17) 0.0485(9) Uani 1 1 d . . . H45A H 0.7675 0.3279 0.3239 0.058 Uiso 1 1 calc R . . H45B H 0.6781 0.3680 0.2854 0.058 Uiso 1 1 calc R . . C46 C 0.6930(3) 0.27024(16) 0.2599(2) 0.0559(11) Uani 1 1 d . . . H46A H 0.7494 0.2354 0.2646 0.067 Uiso 1 1 calc R . . H46B H 0.6303 0.2563 0.2816 0.067 Uiso 1 1 calc R . . C47 C 0.6575(3) 0.27641(16) 0.19738(19) 0.0523(10) Uani 1 1 d . . . H47A H 0.5924 0.3051 0.1934 0.063 Uiso 1 1 calc R . . H47B H 0.6374 0.2319 0.1821 0.063 Uiso 1 1 calc R . . C48 C 0.7465(2) 0.30586(14) 0.16205(16) 0.0381(7) Uani 1 1 d . . . H48A H 0.7183 0.3112 0.1219 0.046 Uiso 1 1 calc R . . H48B H 0.8089 0.2749 0.1625 0.046 Uiso 1 1 calc R . . C81 C 1.5120(7) 0.1504(4) -0.1146(3) 0.127(3) Uani 1 1 d . . . H81A H 1.5810 0.1404 -0.1314 0.191 Uiso 1 1 calc R . . H81B H 1.4736 0.1851 -0.1371 0.191 Uiso 1 1 calc R . . H81C H 1.4672 0.1101 -0.1146 0.191 Uiso 1 1 calc R . . C82 C 1.5322(8) 0.1728(5) -0.0578(4) 0.153(3) Uani 1 1 d . . . H82A H 1.5744 0.1383 -0.0361 0.183 Uiso 1 1 calc R . . H82B H 1.5778 0.2133 -0.0584 0.183 Uiso 1 1 calc R . . C83 C 1.4437(10) 0.1866(8) -0.0301(5) 0.270(9) Uani 1 1 d . . . H83A H 1.4043 0.1442 -0.0259 0.325 Uiso 1 1 calc R . . H83B H 1.3970 0.2151 -0.0557 0.325 Uiso 1 1 calc R . . C84 C 1.4501(10) 0.2186(5) 0.0263(4) 0.212(6) Uani 1 1 d . . . H84A H 1.3753 0.2241 0.0387 0.255 Uiso 1 1 calc R . . H84B H 1.4884 0.1880 0.0537 0.255 Uiso 1 1 calc R . . C85 C 1.5022(7) 0.2808(5) 0.0300(5) 0.193(5) Uani 1 1 d . . . H85A H 1.5025 0.2971 0.0694 0.290 Uiso 1 1 calc R . . H85B H 1.4632 0.3124 0.0044 0.290 Uiso 1 1 calc R . . H85C H 1.5770 0.2762 0.0187 0.290 Uiso 1 1 calc R . . C101 C 1.3435(2) 0.29735(14) 0.25297(13) 0.0350(6) Uani 1 1 d . . . H101 H 1.4114 0.2793 0.2828 0.042 Uiso 1 1 calc R . . C121 C 0.8920(3) 0.20066(14) -0.06343(12) 0.0334(6) Uani 1 1 d . . . H121 H 0.8330 0.1704 -0.0908 0.040 Uiso 1 1 calc R . . B102 B 1.2523(3) 0.24073(15) 0.22693(14) 0.0288(6) Uani 1 1 d . . . H102 H 1.2547 0.1865 0.2377 0.035 Uiso 1 1 calc R . . B103 B 1.3489(2) 0.27660(15) 0.18245(15) 0.0307(6) Uani 1 1 d . . . H103 H 1.4139 0.2460 0.1638 0.037 Uiso 1 1 calc R . . B104 B 1.3721(3) 0.35955(16) 0.20720(17) 0.0364(8) Uani 1 1 d . . . H104 H 1.4534 0.3838 0.2049 0.044 Uiso 1 1 calc R . . B105 B 1.2901(3) 0.37339(16) 0.26577(15) 0.0359(7) Uani 1 1 d . . . H105 H 1.3177 0.4066 0.3021 0.043 Uiso 1 1 calc R . . B106 B 1.2148(3) 0.30002(16) 0.27810(14) 0.0334(7) Uani 1 1 d . . . H106 H 1.1926 0.2850 0.3220 0.040 Uiso 1 1 calc R . . B107 B 1.1280(2) 0.28513(14) 0.21599(12) 0.0252(6) Uani 1 1 d . . . B108 B 1.2112(2) 0.27110(14) 0.15754(13) 0.0240(5) Uani 1 1 d . . . B109 B 1.2865(2) 0.34522(14) 0.14491(15) 0.0285(6) Uani 1 1 d . . . H109 H 1.3098 0.3600 0.1012 0.034 Uiso 1 1 calc R . . B110 B 1.2500(2) 0.40524(15) 0.19751(15) 0.0302(6) Uani 1 1 d . . . H110 H 1.2496 0.4599 0.1883 0.036 Uiso 1 1 calc R . . B111 B 1.1516(3) 0.36817(15) 0.24120(13) 0.0285(6) Uani 1 1 d . . . H111 H 1.0864 0.3981 0.2605 0.034 Uiso 1 1 calc R . . B112 B 1.1502(2) 0.35081(14) 0.16610(13) 0.0235(5) Uani 1 1 d D . . B122 B 0.8653(3) 0.21111(14) 0.00707(12) 0.0258(6) Uani 1 1 d . . . H122 H 0.7932 0.1904 0.0280 0.031 Uiso 1 1 calc R . . B123 B 0.8516(3) 0.27878(15) -0.04417(13) 0.0317(7) Uani 1 1 d . . . H123 H 0.7710 0.3018 -0.0564 0.038 Uiso 1 1 calc R . . B124 B 0.9534(3) 0.26741(16) -0.09364(14) 0.0359(7) Uani 1 1 d . . . H124 H 0.9387 0.2827 -0.1394 0.043 Uiso 1 1 calc R . . B125 B 1.0283(3) 0.19526(15) -0.07450(13) 0.0324(7) Uani 1 1 d . . . H125 H 1.0632 0.1631 -0.1079 0.039 Uiso 1 1 calc R . . B126 B 0.9747(3) 0.15952(14) -0.01291(12) 0.0262(6) Uani 1 1 d . . . H126 H 0.9741 0.1044 -0.0059 0.031 Uiso 1 1 calc R . . B127 B 0.9956(2) 0.21602(13) 0.04511(11) 0.0207(5) Uani 1 1 d . . . B128 B 0.9215(2) 0.29003(14) 0.02277(12) 0.0243(5) Uani 1 1 d . . . B129 B 0.9740(3) 0.32600(15) -0.03914(13) 0.0307(6) Uani 1 1 d . . . H129 H 0.9742 0.3808 -0.0478 0.037 Uiso 1 1 calc R . . B130 B 1.0839(3) 0.27421(16) -0.05815(14) 0.0334(7) Uani 1 1 d . . . H130 H 1.1557 0.2948 -0.0793 0.040 Uiso 1 1 calc R . . B131 B 1.0971(3) 0.20654(15) -0.00680(13) 0.0283(6) Uani 1 1 d . . . H131 H 1.1777 0.1833 0.0053 0.034 Uiso 1 1 calc R . . B132 B 1.0604(2) 0.28773(14) 0.01548(12) 0.0248(6) Uani 1 1 d . . . H107 H 1.048(2) 0.2587(14) 0.2160(12) 0.023(7) Uiso 1 1 d . . . H108 H 1.187(3) 0.2327(16) 0.1228(14) 0.037(9) Uiso 1 1 d . . . H128 H 0.880(2) 0.3249(14) 0.0595(12) 0.022(7) Uiso 1 1 d . . . H132 H 1.113(2) 0.3227(14) 0.0440(12) 0.024(7) Uiso 1 1 d . . . H100 H 0.9035(9) 0.2089(17) 0.1336(16) 0.051(10) Uiso 1 1 d D . . H112 H 1.092(2) 0.3932(6) 0.1382(11) 0.054(10) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01970(9) 0.01327(8) 0.01775(8) -0.00009(6) -0.00195(6) 0.00066(6) Rh2 0.02123(9) 0.01334(8) 0.02147(9) -0.00087(6) -0.00293(6) 0.00114(6) P1 0.0228(3) 0.0146(3) 0.0193(3) 0.0011(2) 0.0013(2) 0.0013(2) P2 0.0180(3) 0.0164(3) 0.0261(3) -0.0019(2) -0.0048(2) 0.0011(2) C11 0.0282(12) 0.0235(12) 0.0202(11) 0.0010(9) 0.0021(9) 0.0034(10) C12 0.0363(15) 0.0427(16) 0.0225(12) 0.0019(11) 0.0051(11) 0.0125(12) C13 0.058(2) 0.064(2) 0.0243(14) -0.0031(14) 0.0076(14) 0.0251(17) C14 0.052(2) 0.068(2) 0.0216(13) 0.0065(14) 0.0061(13) 0.0097(17) C15 0.0547(19) 0.0474(18) 0.0212(13) 0.0083(12) -0.0026(12) 0.0123(15) C16 0.0536(18) 0.0304(14) 0.0239(13) 0.0065(11) 0.0015(12) 0.0082(13) C17 0.0267(12) 0.0163(10) 0.0222(11) 0.0002(9) 0.0023(9) 0.0051(9) C18 0.0281(13) 0.0252(13) 0.0407(15) -0.0103(11) -0.0007(11) 0.0049(10) C19 0.0269(14) 0.0331(15) 0.0466(17) -0.0085(13) -0.0007(12) 0.0078(11) C20 0.0365(16) 0.0376(16) 0.0423(16) 0.0007(13) 0.0122(13) 0.0130(13) C21 0.0419(16) 0.0313(14) 0.0289(13) -0.0067(11) 0.0044(11) 0.0118(12) C22 0.0347(14) 0.0245(12) 0.0253(12) -0.0018(10) 0.0023(10) 0.0081(10) C23 0.0260(12) 0.0176(11) 0.0251(12) 0.0012(9) 0.0016(9) -0.0021(9) C24 0.0387(15) 0.0206(12) 0.0393(15) 0.0062(11) -0.0019(12) -0.0074(11) C25 0.0462(17) 0.0238(13) 0.0419(16) -0.0007(12) -0.0034(13) -0.0096(12) C26 0.0367(16) 0.0376(16) 0.0425(16) -0.0053(13) -0.0001(13) -0.0151(13) C27 0.0285(13) 0.0351(15) 0.0356(15) -0.0063(12) -0.0004(11) -0.0026(11) C28 0.0276(13) 0.0271(13) 0.0325(14) -0.0052(11) 0.0041(10) -0.0035(10) C31 0.0319(14) 0.0290(14) 0.0362(15) -0.0025(11) -0.0129(11) 0.0107(11) C32 0.0528(18) 0.0273(14) 0.0311(14) 0.0027(11) -0.0124(13) 0.0079(13) C33 0.092(3) 0.0367(18) 0.0391(18) 0.0034(14) -0.0236(18) 0.0175(18) C34 0.100(3) 0.050(2) 0.053(2) -0.0070(18) -0.049(2) 0.025(2) C35 0.055(2) 0.061(2) 0.072(3) -0.019(2) -0.044(2) 0.0275(19) C36 0.0347(16) 0.0454(18) 0.056(2) -0.0094(15) -0.0225(14) 0.0105(14) C37 0.0194(11) 0.0157(10) 0.0236(11) -0.0017(9) -0.0011(8) 0.0022(8) C38 0.0230(12) 0.0208(12) 0.0396(15) -0.0068(10) 0.0045(10) -0.0009(9) C39 0.0319(14) 0.0266(13) 0.0368(15) -0.0111(11) 0.0097(11) -0.0040(11) C40 0.0326(14) 0.0209(12) 0.0454(16) -0.0115(11) 0.0074(12) -0.0058(10) C41 0.0260(12) 0.0223(12) 0.0360(14) -0.0067(10) 0.0046(10) -0.0064(10) C42 0.0254(12) 0.0182(11) 0.0257(12) -0.0005(9) 0.0018(9) -0.0013(9) C43 0.0190(11) 0.0189(11) 0.0440(15) -0.0030(10) 0.0040(10) -0.0010(9) C44 0.0336(15) 0.0313(15) 0.0423(16) 0.0045(12) 0.0103(12) -0.0062(11) C45 0.051(2) 0.0346(16) 0.063(2) 0.0045(15) 0.0296(17) -0.0043(14) C46 0.047(2) 0.0288(16) 0.096(3) 0.0032(17) 0.039(2) -0.0040(14) C47 0.0266(15) 0.0263(15) 0.106(3) -0.0152(17) 0.0229(17) -0.0093(12) C48 0.0255(13) 0.0229(13) 0.067(2) -0.0105(13) 0.0086(13) -0.0055(10) C81 0.154(7) 0.110(6) 0.120(6) 0.011(5) 0.030(5) -0.036(5) C82 0.148(8) 0.147(8) 0.158(8) -0.060(7) -0.028(6) 0.003(6) C83 0.211(12) 0.43(2) 0.182(10) -0.160(12) 0.122(9) -0.210(13) C84 0.314(15) 0.224(12) 0.098(6) -0.046(7) 0.005(7) -0.156(11) C85 0.152(8) 0.197(10) 0.242(11) -0.083(8) 0.105(8) -0.112(7) C101 0.0320(14) 0.0282(14) 0.0425(16) -0.0066(12) -0.0173(12) 0.0068(11) C121 0.0480(17) 0.0233(13) 0.0273(13) 0.0014(10) -0.0103(12) -0.0019(12) B102 0.0301(15) 0.0213(13) 0.0334(15) -0.0040(11) -0.0121(12) 0.0058(11) B103 0.0220(14) 0.0245(14) 0.0446(18) -0.0041(13) -0.0084(12) 0.0029(11) B104 0.0255(15) 0.0255(15) 0.056(2) -0.0049(14) -0.0129(14) 0.0052(12) B105 0.0362(17) 0.0256(15) 0.0437(19) -0.0102(13) -0.0175(14) 0.0069(13) B106 0.0386(17) 0.0275(15) 0.0324(16) -0.0059(12) -0.0122(13) 0.0077(13) B107 0.0286(14) 0.0211(13) 0.0251(13) -0.0003(11) -0.0060(11) 0.0028(11) B108 0.0230(13) 0.0188(12) 0.0294(14) -0.0025(11) -0.0056(10) 0.0031(10) B109 0.0223(13) 0.0192(13) 0.0433(17) -0.0023(12) -0.0034(12) 0.0003(10) B110 0.0234(14) 0.0201(13) 0.0455(18) -0.0064(12) -0.0120(12) 0.0012(11) B111 0.0300(15) 0.0230(14) 0.0312(15) -0.0062(11) -0.0104(12) 0.0055(11) B112 0.0208(12) 0.0184(12) 0.0304(14) -0.0039(11) -0.0054(10) 0.0028(10) B122 0.0319(15) 0.0209(13) 0.0233(13) 0.0006(10) -0.0093(11) -0.0013(11) B123 0.0467(18) 0.0221(14) 0.0246(14) 0.0000(11) -0.0117(13) 0.0011(13) B124 0.060(2) 0.0226(15) 0.0239(14) 0.0025(11) -0.0038(14) -0.0034(14) B125 0.050(2) 0.0216(14) 0.0253(14) -0.0015(11) 0.0044(13) -0.0007(13) B126 0.0380(16) 0.0181(13) 0.0219(13) -0.0007(10) -0.0045(11) 0.0002(11) B127 0.0275(13) 0.0157(12) 0.0183(11) 0.0014(9) -0.0037(10) -0.0010(10) B128 0.0312(14) 0.0180(12) 0.0232(13) -0.0004(10) -0.0037(11) 0.0004(10) B129 0.0492(19) 0.0206(14) 0.0216(13) 0.0006(11) -0.0029(12) -0.0013(13) B130 0.0495(19) 0.0242(15) 0.0273(15) 0.0006(12) 0.0087(13) -0.0033(13) B131 0.0375(16) 0.0202(13) 0.0276(14) -0.0026(11) 0.0054(12) -0.0003(11) B132 0.0335(15) 0.0180(13) 0.0225(13) -0.0007(10) -0.0006(11) -0.0034(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 B127 2.061(3) . ? Rh1 P1 2.2325(6) . ? Rh1 B108 2.479(3) . ? Rh1 B107 2.587(3) . ? Rh1 Rh2 2.7962(2) . ? Rh1 H107 2.11(3) . ? Rh1 H108 1.95(3) . ? Rh1 H100 1.604(10) . ? Rh2 P2 2.2572(6) . ? Rh2 B128 2.300(3) . ? Rh2 B112 2.378(3) . ? Rh2 B132 2.419(3) . ? Rh2 H128 1.78(3) . ? Rh2 H132 1.96(3) . ? Rh2 H112 1.653(10) . ? P1 C23 1.860(2) . ? P1 C17 1.860(2) . ? P1 C11 1.867(2) . ? P2 C37 1.855(2) . ? P2 C43 1.855(3) . ? P2 C31 1.864(3) . ? C11 C12 1.533(4) . ? C11 C16 1.537(4) . ? C11 H11 1.0000 . ? C12 C13 1.532(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.514(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.534(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.530(3) . ? C17 C18 1.534(4) . ? C17 H17 1.0000 . ? C18 C19 1.529(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.516(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.530(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.536(4) . ? C23 C24 1.547(3) . ? C23 H23 1.0000 . ? C24 C25 1.535(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.523(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.525(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.531(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C31 C36 1.531(4) . ? C31 C32 1.536(4) . ? C31 H31 1.0000 . ? C32 C33 1.525(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.515(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.528(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.534(3) . ? C37 C38 1.547(3) . ? C37 H37 1.0000 . ? C38 C39 1.527(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.524(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.520(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.531(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.537(4) . ? C43 C44 1.537(4) . ? C43 H43 1.0000 . ? C44 C45 1.539(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.518(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.508(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.532(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C81 C82 1.413(10) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.332(12) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.465(11) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.407(10) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C101 B102 1.690(4) . ? C101 B104 1.698(5) . ? C101 B105 1.699(4) . ? C101 B103 1.708(5) . ? C101 B106 1.727(5) . ? C101 H101 1.1200 . ? C121 B122 1.715(4) . ? C121 B124 1.715(4) . ? C121 B123 1.716(4) . ? C121 B125 1.721(5) . ? C121 B126 1.728(4) . ? C121 H121 1.1200 . ? B102 B106 1.771(4) . ? B102 B107 1.781(4) . ? B102 B103 1.781(5) . ? B102 B108 1.781(4) . ? B102 H102 1.1200 . ? B103 B108 1.768(4) . ? B103 B104 1.784(4) . ? B103 B109 1.786(4) . ? B103 H103 1.1200 . ? B104 B110 1.768(4) . ? B104 B105 1.773(5) . ? B104 B109 1.774(5) . ? B104 H104 1.1200 . ? B105 B110 1.765(5) . ? B105 B111 1.775(4) . ? B105 B106 1.776(5) . ? B105 H105 1.1200 . ? B106 B111 1.776(4) . ? B106 B107 1.781(4) . ? B106 H106 1.1200 . ? B107 B108 1.781(4) . ? B107 B111 1.789(4) . ? B107 B112 1.795(4) . ? B107 H107 1.12(3) . ? B108 B112 1.787(4) . ? B108 B109 1.790(4) . ? B108 H108 1.15(3) . ? B109 B112 1.785(4) . ? B109 B110 1.800(4) . ? B109 H109 1.1200 . ? B110 B112 1.775(4) . ? B110 B111 1.795(5) . ? B110 H110 1.1200 . ? B111 B112 1.792(4) . ? B111 H111 1.1200 . ? B112 H112 1.274(10) . ? B122 B128 1.762(4) . ? B122 B126 1.787(4) . ? B122 B127 1.796(4) . ? B122 B123 1.815(4) . ? B122 H122 1.1200 . ? B123 B128 1.759(4) . ? B123 B124 1.773(5) . ? B123 B129 1.783(5) . ? B123 H123 1.1200 . ? B124 B129 1.744(4) . ? B124 B125 1.764(5) . ? B124 B130 1.774(5) . ? B124 H124 1.1200 . ? B125 B130 1.763(4) . ? B125 B131 1.769(5) . ? B125 B126 1.773(4) . ? B125 H125 1.1200 . ? B126 B127 1.778(4) . ? B126 B131 1.781(4) . ? B126 H126 1.1200 . ? B127 B131 1.806(4) . ? B127 B132 1.807(4) . ? B127 B128 1.808(4) . ? B128 B132 1.734(4) . ? B128 B129 1.776(4) . ? B128 H128 1.24(3) . ? B129 B130 1.786(5) . ? B129 B132 1.790(4) . ? B129 H129 1.1200 . ? B130 B132 1.785(4) . ? B130 B131 1.817(4) . ? B130 H130 1.1200 . ? B131 B132 1.781(4) . ? B131 H131 1.1200 . ? B132 H132 1.15(3) . ? 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 B127 Rh1 P1 98.90(7) . . ? B127 Rh1 B108 113.23(11) . . ? P1 Rh1 B108 115.26(7) . . ? B127 Rh1 B107 146.63(10) . . ? P1 Rh1 B107 111.41(6) . . ? B108 Rh1 B107 41.10(10) . . ? B127 Rh1 Rh2 73.93(7) . . ? P1 Rh1 Rh2 167.506(18) . . ? B108 Rh1 Rh2 77.19(6) . . ? B107 Rh1 Rh2 78.37(6) . . ? B127 Rh1 H107 159.9(8) . . ? P1 Rh1 H107 99.3(8) . . ? B108 Rh1 H107 65.9(8) . . ? B107 Rh1 H107 25.1(8) . . ? Rh2 Rh1 H107 86.6(8) . . ? B127 Rh1 H108 93.0(9) . . ? P1 Rh1 H108 103.5(9) . . ? B108 Rh1 H108 26.9(9) . . ? B107 Rh1 H108 67.2(10) . . ? Rh2 Rh1 H108 87.3(9) . . ? H107 Rh1 H108 91.1(12) . . ? B127 Rh1 H100 81.8(13) . . ? P1 Rh1 H100 76.6(13) . . ? B108 Rh1 H100 157.5(13) . . ? B107 Rh1 H100 117.7(13) . . ? Rh2 Rh1 H100 92.0(13) . . ? H107 Rh1 H100 94.0(15) . . ? H108 Rh1 H100 174.8(16) . . ? P2 Rh2 B128 111.61(8) . . ? P2 Rh2 B112 100.88(7) . . ? B128 Rh2 B112 142.51(10) . . ? P2 Rh2 B132 152.37(7) . . ? B128 Rh2 B132 43.03(10) . . ? B112 Rh2 B132 106.75(10) . . ? P2 Rh2 Rh1 117.788(18) . . ? B128 Rh2 Rh1 75.83(7) . . ? B112 Rh2 Rh1 72.69(7) . . ? B132 Rh2 Rh1 72.15(7) . . ? P2 Rh2 H128 79.4(9) . . ? B128 Rh2 H128 32.4(9) . . ? B112 Rh2 H128 157.1(9) . . ? B132 Rh2 H128 75.3(9) . . ? Rh1 Rh2 H128 86.8(9) . . ? P2 Rh2 H132 162.3(8) . . ? B128 Rh2 H132 70.6(8) . . ? B112 Rh2 H132 84.2(8) . . ? B132 Rh2 H132 27.9(8) . . ? Rh1 Rh2 H132 79.9(8) . . ? H128 Rh2 H132 102.5(12) . . ? P2 Rh2 H112 82.9(10) . . ? B128 Rh2 H112 164.4(12) . . ? B112 Rh2 H112 30.6(4) . . ? B132 Rh2 H112 121.5(12) . . ? Rh1 Rh2 H112 103.0(4) . . ? H128 Rh2 H112 162.3(13) . . ? H132 Rh2 H112 93.8(15) . . ? C23 P1 C17 102.73(11) . . ? C23 P1 C11 110.40(12) . . ? C17 P1 C11 103.20(11) . . ? C23 P1 Rh1 115.93(8) . . ? C17 P1 Rh1 118.66(8) . . ? C11 P1 Rh1 105.20(8) . . ? C37 P2 C43 104.40(11) . . ? C37 P2 C31 102.97(12) . . ? C43 P2 C31 105.44(13) . . ? C37 P2 Rh2 115.77(8) . . ? C43 P2 Rh2 119.04(8) . . ? C31 P2 Rh2 107.65(10) . . ? C12 C11 C16 108.9(2) . . ? C12 C11 P1 113.02(17) . . ? C16 C11 P1 118.75(18) . . ? C12 C11 H11 104.9 . . ? C16 C11 H11 104.9 . . ? P1 C11 H11 104.9 . . ? C13 C12 C11 110.6(2) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 110.0(3) . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 111.5(3) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 112.5(3) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C11 109.9(2) . . ? C15 C16 H16A 109.7 . . ? C11 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? C11 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C22 C17 C18 110.0(2) . . ? C22 C17 P1 114.79(17) . . ? C18 C17 P1 111.67(16) . . ? C22 C17 H17 106.6 . . ? C18 C17 H17 106.6 . . ? P1 C17 H17 106.6 . . ? C19 C18 C17 112.5(2) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 111.8(2) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C19 109.6(2) . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 111.2(2) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C17 C22 C21 109.9(2) . . ? C17 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? C17 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C28 C23 C24 108.7(2) . . ? C28 C23 P1 115.76(17) . . ? C24 C23 P1 115.37(18) . . ? C28 C23 H23 105.3 . . ? C24 C23 H23 105.3 . . ? P1 C23 H23 105.3 . . ? C25 C24 C23 109.8(2) . . ? C25 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? C25 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 111.9(2) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C27 111.8(2) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 112.2(2) . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C23 111.1(2) . . ? C27 C28 H28A 109.4 . . ? C23 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C23 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C36 C31 C32 110.5(3) . . ? C36 C31 P2 116.0(2) . . ? C32 C31 P2 111.30(19) . . ? C36 C31 H31 106.1 . . ? C32 C31 H31 106.1 . . ? P2 C31 H31 106.1 . . ? C33 C32 C31 111.6(3) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 110.7(3) . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 111.8(3) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 112.3(3) . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 110.2(3) . . ? C35 C36 H36A 109.6 . . ? C31 C36 H36A 109.6 . . ? C35 C36 H36B 109.6 . . ? C31 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C42 C37 C38 108.37(19) . . ? C42 C37 P2 115.16(16) . . ? C38 C37 P2 114.83(16) . . ? C42 C37 H37 105.9 . . ? C38 C37 H37 105.9 . . ? P2 C37 H37 105.9 . . ? C39 C38 C37 109.8(2) . . ? C39 C38 H38A 109.7 . . ? C37 C38 H38A 109.7 . . ? C39 C38 H38B 109.7 . . ? C37 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C40 C39 C38 112.0(2) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C41 C40 C39 111.4(2) . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 110.6(2) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C41 C42 C37 110.3(2) . . ? C41 C42 H42A 109.6 . . ? C37 C42 H42A 109.6 . . ? C41 C42 H42B 109.6 . . ? C37 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C48 C43 C44 108.3(2) . . ? C48 C43 P2 112.3(2) . . ? C44 C43 P2 114.32(18) . . ? C48 C43 H43 107.2 . . ? C44 C43 H43 107.2 . . ? P2 C43 H43 107.2 . . ? C43 C44 C45 110.3(3) . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C44 112.1(3) . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45B 109.2 . . ? C44 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C47 C46 C45 111.8(3) . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46B 109.3 . . ? C45 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? C46 C47 C48 112.3(3) . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.9 . . ? C47 C48 C43 111.1(3) . . ? C47 C48 H48A 109.4 . . ? C43 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C43 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C81 114.8(9) . . ? C83 C82 H82A 108.6 . . ? C81 C82 H82A 108.6 . . ? C83 C82 H82B 108.6 . . ? C81 C82 H82B 108.6 . . ? H82A C82 H82B 107.5 . . ? C82 C83 C84 121.8(11) . . ? C82 C83 H83A 106.9 . . ? C84 C83 H83A 106.9 . . ? C82 C83 H83B 106.9 . . ? C84 C83 H83B 106.9 . . ? H83A C83 H83B 106.7 . . ? C85 C84 C83 116.5(9) . . ? C85 C84 H84A 108.2 . . ? C83 C84 H84A 108.2 . . ? C85 C84 H84B 108.2 . . ? C83 C84 H84B 108.2 . . ? H84A C84 H84B 107.3 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? B102 C101 B104 115.3(2) . . ? B102 C101 B105 114.4(2) . . ? B104 C101 B105 63.0(2) . . ? B102 C101 B103 63.21(18) . . ? B104 C101 B103 63.2(2) . . ? B105 C101 B103 115.3(2) . . ? B102 C101 B106 62.42(18) . . ? B104 C101 B106 114.9(2) . . ? B105 C101 B106 62.5(2) . . ? B103 C101 B106 115.2(2) . . ? B102 C101 H101 117.7 . . ? B104 C101 H101 117.2 . . ? B105 C101 H101 117.8 . . ? B103 C101 H101 117.0 . . ? B106 C101 H101 117.8 . . ? B122 C121 B124 114.6(2) . . ? B122 C121 B123 63.89(17) . . ? B124 C121 B123 62.24(19) . . ? B122 C121 B125 113.4(2) . . ? B124 C121 B125 61.8(2) . . ? B123 C121 B125 113.5(2) . . ? B122 C121 B126 62.55(17) . . ? B124 C121 B126 113.5(2) . . ? B123 C121 B126 115.3(2) . . ? B125 C121 B126 61.87(18) . . ? B122 C121 H121 117.5 . . ? B124 C121 H121 118.5 . . ? B123 C121 H121 117.3 . . ? B125 C121 H121 119.2 . . ? B126 C121 H121 118.0 . . ? C101 B102 B106 59.80(18) . . ? C101 B102 B107 105.3(2) . . ? B106 B102 B107 60.20(17) . . ? C101 B102 B103 58.89(19) . . ? B106 B102 B103 109.5(2) . . ? B107 B102 B103 108.3(2) . . ? C101 B102 B108 104.3(2) . . ? B106 B102 B108 108.3(2) . . ? B107 B102 B108 60.01(16) . . ? B103 B102 B108 59.50(17) . . ? C101 B102 H102 124.5 . . ? B106 B102 H102 120.5 . . ? B107 B102 H102 122.2 . . ? B103 B102 H102 121.1 . . ? B108 B102 H102 122.9 . . ? C101 B103 B108 104.1(2) . . ? C101 B103 B102 57.91(18) . . ? B108 B103 B102 60.26(17) . . ? C101 B103 B104 58.13(19) . . ? B108 B103 B104 107.4(2) . . ? B102 B103 B104 106.8(2) . . ? C101 B103 B109 104.3(2) . . ? B108 B103 B109 60.50(16) . . ? B102 B103 B109 108.5(2) . . ? B104 B103 B109 59.60(17) . . ? C101 B103 H103 125.4 . . ? B108 B103 H103 122.3 . . ? B102 B103 H103 121.7 . . ? B104 B103 H103 122.3 . . ? B109 B103 H103 122.0 . . ? C101 B104 B110 104.9(2) . . ? C101 B104 B105 58.5(2) . . ? B110 B104 B105 59.80(19) . . ? C101 B104 B109 105.3(2) . . ? B110 B104 B109 61.09(17) . . ? B105 B104 B109 108.8(2) . . ? C101 B104 B103 58.70(18) . . ? B110 B104 B103 108.9(2) . . ? B105 B104 B103 108.0(3) . . ? B109 B104 B103 60.27(17) . . ? C101 B104 H104 124.8 . . ? B110 B104 H104 121.8 . . ? B105 B104 H104 121.5 . . ? B109 B104 H104 121.6 . . ? B103 B104 H104 121.2 . . ? C101 B105 B110 105.0(2) . . ? C101 B105 B104 58.50(19) . . ? B110 B105 B104 59.96(19) . . ? C101 B105 B111 105.4(2) . . ? B110 B105 B111 60.94(18) . . ? B104 B105 B111 108.8(2) . . ? C101 B105 B106 59.54(19) . . ? B110 B105 B106 109.1(2) . . ? B104 B105 B106 108.9(2) . . ? B111 B105 B106 60.02(18) . . ? C101 B105 H105 124.6 . . ? B110 B105 H105 121.9 . . ? B104 B105 H105 121.3 . . ? B111 B105 H105 121.8 . . ? B106 B105 H105 120.8 . . ? C101 B106 B102 57.78(18) . . ? C101 B106 B105 57.99(19) . . ? B102 B106 B105 106.8(3) . . ? C101 B106 B111 104.2(2) . . ? B102 B106 B111 108.4(2) . . ? B105 B106 B111 59.96(18) . . ? C101 B106 B107 103.8(2) . . ? B102 B106 B107 60.18(17) . . ? B105 B106 B107 107.6(2) . . ? B111 B106 B107 60.40(17) . . ? C101 B106 H106 125.7 . . ? B102 B106 H106 121.8 . . ? B105 B106 H106 122.1 . . ? B111 B106 H106 122.0 . . ? B107 B106 H106 122.4 . . ? B102 B107 B106 59.62(17) . . ? B102 B107 B108 60.01(17) . . ? B106 B107 B108 107.9(2) . . ? B102 B107 B111 107.3(2) . . ? B106 B107 B111 59.67(17) . . ? B108 B107 B111 108.1(2) . . ? B102 B107 B112 107.4(2) . . ? B106 B107 B112 107.4(2) . . ? B108 B107 B112 59.96(16) . . ? B111 B107 B112 59.98(16) . . ? B102 B107 Rh1 102.11(15) . . ? B106 B107 Rh1 158.80(18) . . ? B108 B107 Rh1 66.19(13) . . ? B111 B107 Rh1 141.18(17) . . ? B112 B107 Rh1 87.54(14) . . ? B102 B107 H107 120.9(15) . . ? B106 B107 H107 124.6(14) . . ? B108 B107 H107 118.2(14) . . ? B111 B107 H107 124.6(15) . . ? B112 B107 H107 121.1(15) . . ? Rh1 B107 H107 52.9(14) . . ? B103 B108 B102 60.24(18) . . ? B103 B108 B107 108.9(2) . . ? B102 B108 B107 59.98(17) . . ? B103 B108 B112 108.1(2) . . ? B102 B108 B112 107.7(2) . . ? B107 B108 B112 60.40(16) . . ? B103 B108 B109 60.26(17) . . ? B102 B108 B109 108.3(2) . . ? B107 B108 B109 108.9(2) . . ? B112 B108 B109 59.86(16) . . ? B103 B108 Rh1 158.92(18) . . ? B102 B108 Rh1 106.31(17) . . ? B107 B108 Rh1 72.71(14) . . ? B112 B108 Rh1 91.15(14) . . ? B109 B108 Rh1 140.18(17) . . ? B103 B108 H108 118.9(16) . . ? B102 B108 H108 117.7(16) . . ? B107 B108 H108 120.7(16) . . ? B112 B108 H108 126.0(16) . . ? B109 B108 H108 124.1(16) . . ? Rh1 B108 H108 50.1(16) . . ? B104 B109 B112 106.7(2) . . ? B104 B109 B103 60.13(18) . . ? B112 B109 B103 107.3(2) . . ? B104 B109 B108 106.8(2) . . ? B112 B109 B108 59.98(16) . . ? B103 B109 B108 59.24(16) . . ? B104 B109 B110 59.30(17) . . ? B112 B109 B110 59.34(16) . . ? B103 B109 B110 107.4(2) . . ? B108 B109 B110 107.0(2) . . ? B104 B109 H109 122.4 . . ? B112 B109 H109 122.3 . . ? B103 B109 H109 121.9 . . ? B108 B109 H109 122.4 . . ? B110 B109 H109 122.4 . . ? B105 B110 B104 60.2(2) . . ? B105 B110 B112 107.6(2) . . ? B104 B110 B112 107.4(2) . . ? B105 B110 B111 59.80(19) . . ? B104 B110 B111 108.1(2) . . ? B112 B110 B111 60.24(17) . . ? B105 B110 B109 107.9(2) . . ? B104 B110 B109 59.61(18) . . ? B112 B110 B109 59.90(16) . . ? B111 B110 B109 108.4(2) . . ? B105 B110 H110 121.8 . . ? B104 B110 H110 121.9 . . ? B112 B110 H110 122.0 . . ? B111 B110 H110 121.4 . . ? B109 B110 H110 121.7 . . ? B105 B111 B106 60.02(19) . . ? B105 B111 B107 107.3(2) . . ? B106 B111 B107 59.94(17) . . ? B105 B111 B112 106.5(2) . . ? B106 B111 B112 107.8(2) . . ? B107 B111 B112 60.17(16) . . ? B105 B111 B110 59.27(19) . . ? B106 B111 B110 107.7(2) . . ? B107 B111 B110 107.6(2) . . ? B112 B111 B110 59.31(17) . . ? B105 B111 H111 122.6 . . ? B106 B111 H111 121.6 . . ? B107 B111 H111 121.8 . . ? B112 B111 H111 122.3 . . ? B110 B111 H111 122.2 . . ? B110 B112 B109 60.76(17) . . ? B110 B112 B108 108.24(19) . . ? B109 B112 B108 60.16(16) . . ? B110 B112 B111 60.44(18) . . ? B109 B112 B111 109.3(2) . . ? B108 B112 B111 107.8(2) . . ? B110 B112 B107 108.2(2) . . ? B109 B112 B107 108.5(2) . . ? B108 B112 B107 59.64(16) . . ? B111 B112 B107 59.85(17) . . ? B110 B112 Rh2 139.79(18) . . ? B109 B112 Rh2 120.06(18) . . ? B108 B112 Rh2 103.91(15) . . ? B111 B112 Rh2 129.87(17) . . ? B107 B112 Rh2 108.58(16) . . ? B110 B112 H112 99.2(6) . . ? B109 B112 H112 114.6(16) . . ? B108 B112 H112 140.6(11) . . ? B111 B112 H112 110.3(13) . . ? B107 B112 H112 136.3(15) . . ? Rh2 B112 H112 41.4(5) . . ? C121 B122 B128 102.5(2) . . ? C121 B122 B126 59.09(17) . . ? B128 B122 B126 106.4(2) . . ? C121 B122 B127 105.5(2) . . ? B128 B122 B127 61.10(15) . . ? B126 B122 B127 59.52(16) . . ? C121 B122 B123 58.09(16) . . ? B128 B122 B123 58.87(16) . . ? B126 B122 B123 107.7(2) . . ? B127 B122 B123 109.4(2) . . ? C121 B122 H122 125.3 . . ? B128 B122 H122 123.8 . . ? B126 B122 H122 122.1 . . ? B127 B122 H122 121.0 . . ? B123 B122 H122 121.4 . . ? C121 B123 B128 102.5(2) . . ? C121 B123 B124 58.85(18) . . ? B128 B123 B124 105.6(2) . . ? C121 B123 B129 104.3(2) . . ? B128 B123 B129 60.21(17) . . ? B124 B123 B129 58.75(19) . . ? C121 B123 B122 58.02(16) . . ? B128 B123 B122 59.05(16) . . ? B124 B123 B122 107.0(2) . . ? B129 B123 B122 108.0(2) . . ? C121 B123 H123 125.4 . . ? B128 B123 H123 123.9 . . ? B124 B123 H123 122.6 . . ? B129 B123 H123 122.2 . . ? B122 B123 H123 121.8 . . ? C121 B124 B129 106.0(2) . . ? C121 B124 B125 59.28(18) . . ? B129 B124 B125 108.5(2) . . ? C121 B124 B123 58.92(18) . . ? B129 B124 B123 60.90(19) . . ? B125 B124 B123 108.7(2) . . ? C121 B124 B130 106.2(2) . . ? B129 B124 B130 61.02(19) . . ? B125 B124 B130 59.77(19) . . ? B123 B124 B130 110.0(2) . . ? C121 B124 H124 124.0 . . ? B129 B124 H124 121.5 . . ? B125 B124 H124 121.5 . . ? B123 B124 H124 120.6 . . ? B130 B124 H124 121.3 . . ? C121 B125 B130 106.4(2) . . ? C121 B125 B124 58.95(19) . . ? B130 B125 B124 60.39(19) . . ? C121 B125 B131 106.3(2) . . ? B130 B125 B131 61.92(18) . . ? B124 B125 B131 109.8(2) . . ? C121 B125 B126 59.26(17) . . ? B130 B125 B126 110.3(2) . . ? B124 B125 B126 109.0(2) . . ? B131 B125 B126 60.38(17) . . ? C121 B125 H125 124.1 . . ? B130 B125 H125 120.7 . . ? B124 B125 H125 121.0 . . ? B131 B125 H125 121.0 . . ? B126 B125 H125 120.7 . . ? C121 B126 B125 58.87(18) . . ? C121 B126 B127 105.70(19) . . ? B125 B126 B127 108.5(2) . . ? C121 B126 B131 105.4(2) . . ? B125 B126 B131 59.69(18) . . ? B127 B126 B131 60.99(16) . . ? C121 B126 B122 58.36(16) . . ? B125 B126 B122 107.5(2) . . ? B127 B126 B122 60.47(16) . . ? B131 B126 B122 108.8(2) . . ? C121 B126 H126 124.4 . . ? B125 B126 H126 121.8 . . ? B127 B126 H126 121.4 . . ? B131 B126 H126 121.8 . . ? B122 B126 H126 121.6 . . ? B126 B127 B122 60.01(16) . . ? B126 B127 B131 59.58(17) . . ? B122 B127 B131 107.3(2) . . ? B126 B127 B132 105.32(19) . . ? B122 B127 B132 104.91(18) . . ? B131 B127 B132 59.05(16) . . ? B126 B127 B128 104.86(18) . . ? B122 B127 B128 58.53(15) . . ? B131 B127 B128 104.57(19) . . ? B132 B127 B128 57.33(16) . . ? B126 B127 Rh1 142.68(17) . . ? B122 B127 Rh1 128.97(18) . . ? B131 B127 Rh1 123.38(18) . . ? B132 B127 Rh1 105.68(15) . . ? B128 B127 Rh1 109.15(16) . . ? B132 B128 B123 110.2(2) . . ? B132 B128 B122 109.6(2) . . ? B123 B128 B122 62.08(16) . . ? B132 B128 B129 61.31(18) . . ? B123 B128 B129 60.57(18) . . ? B122 B128 B129 110.8(2) . . ? B132 B128 B127 61.29(16) . . ? B123 B128 B127 111.4(2) . . ? B122 B128 B127 60.37(15) . . ? B129 B128 B127 111.6(2) . . ? B132 B128 Rh2 72.14(13) . . ? B123 B128 Rh2 154.54(18) . . ? B122 B128 Rh2 142.49(18) . . ? B129 B128 Rh2 102.70(16) . . ? B127 B128 Rh2 92.16(14) . . ? B132 B128 H128 122.2(13) . . ? B123 B128 H128 119.3(13) . . ? B122 B128 H128 118.7(13) . . ? B129 B128 H128 121.3(13) . . ? B127 B128 H128 119.1(13) . . ? Rh2 B128 H128 50.3(13) . . ? B124 B129 B128 106.1(2) . . ? B124 B129 B123 60.35(19) . . ? B128 B129 B123 59.22(17) . . ? B124 B129 B130 60.3(2) . . ? B128 B129 B130 106.5(2) . . ? B123 B129 B130 109.0(2) . . ? B124 B129 B132 106.7(2) . . ? B128 B129 B132 58.18(16) . . ? B123 B129 B132 106.6(2) . . ? B130 B129 B132 59.90(18) . . ? B124 B129 H129 122.2 . . ? B128 B129 H129 123.6 . . ? B123 B129 H129 121.5 . . ? B130 B129 H129 121.3 . . ? B132 B129 H129 123.0 . . ? B125 B130 B124 59.84(19) . . ? B125 B130 B132 105.3(2) . . ? B124 B130 B132 105.7(2) . . ? B125 B130 B129 106.7(2) . . ? B124 B130 B129 58.68(19) . . ? B132 B130 B129 60.16(17) . . ? B125 B130 B131 59.21(17) . . ? B124 B130 B131 107.3(2) . . ? B132 B130 B131 59.24(16) . . ? B129 B130 B131 108.2(2) . . ? B125 B130 H130 123.0 . . ? B124 B130 H130 122.8 . . ? B132 B130 H130 123.3 . . ? B129 B130 H130 121.8 . . ? B131 B130 H130 121.8 . . ? B125 B131 B132 105.2(2) . . ? B125 B131 B126 59.93(17) . . ? B132 B131 B126 106.3(2) . . ? B125 B131 B127 107.5(2) . . ? B132 B131 B127 60.49(16) . . ? B126 B131 B127 59.43(16) . . ? B125 B131 B130 58.87(18) . . ? B132 B131 B130 59.50(17) . . ? B126 B131 B130 107.5(2) . . ? B127 B131 B130 109.1(2) . . ? B125 B131 H131 123.1 . . ? B132 B131 H131 123.1 . . ? B126 B131 H131 122.4 . . ? B127 B131 H131 121.0 . . ? B130 B131 H131 121.6 . . ? B128 B132 B131 108.9(2) . . ? B128 B132 B130 108.4(2) . . ? B131 B132 B130 61.26(17) . . ? B128 B132 B129 60.51(17) . . ? B131 B132 B129 109.6(2) . . ? B130 B132 B129 59.94(18) . . ? B128 B132 B127 61.38(16) . . ? B131 B132 B127 60.45(16) . . ? B130 B132 B127 110.5(2) . . ? B129 B132 B127 111.0(2) . . ? B128 B132 Rh2 64.84(13) . . ? B131 B132 Rh2 143.90(18) . . ? B130 B132 Rh2 154.48(19) . . ? B129 B132 Rh2 97.88(16) . . ? B127 B132 Rh2 88.42(14) . . ? B128 B132 H132 117.2(14) . . ? B131 B132 H132 126.0(14) . . ? B130 B132 H132 122.5(14) . . ? B129 B132 H132 116.5(14) . . ? B127 B132 H132 121.0(14) . . ? Rh2 B132 H132 53.2(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.072 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.104 #===END data_h06asw11 _database_code_depnum_ccdc_archive 'CCDC 655390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 6' _chemical_melting_point ? _chemical_formula_moiety 'C16 H39 B11 Br6 P Rh, C5 H12' _chemical_formula_sum 'C21 H51 B11 Br6 P Rh' _chemical_formula_weight 1035.87 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.6256(1) _cell_length_b 19.1042(1) _cell_length_c 13.7346(1) _cell_angle_alpha 90.00 _cell_angle_beta 121.2435(3) _cell_angle_gamma 90.00 _cell_volume 3729.87(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 78610 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 33.142 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 6.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0873 _exptl_absorpt_correction_T_max 0.1755 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '718 1.0 degree images with \f and \w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 48929 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.75 _diffrn_reflns_theta_max 33.18 _reflns_number_total 13829 _reflns_number_gt 12572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; DIRDIF-99 program system P.T. Beurskens, G. Beurskens, R. de Gelder, S. Garcia-Granda, R.O. Gould, R. Israel and J.M.M. Smits (1999). Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The platon program 'SQUEEZE' was used to account for disordered solvent residues; the contents of the asymmetric unit are assumed to contain one molecule of pentane. The hydrogen atoms H11A, H11B and H12 were located and refined with a restrained C-H distance of 0.95 A. ; _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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(4) _refine_ls_number_reflns 13829 _refine_ls_number_parameters 328 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.006528(14) 0.156615(11) 0.006298(17) 0.02185(4) Uani 1 1 d . . . P P -0.09388(5) 0.17889(4) 0.06429(6) 0.02346(13) Uani 1 1 d . . . C1 C -0.0420(3) 0.0999(3) 0.2639(3) 0.0470(9) Uani 1 1 d . . . H1A H -0.0986 0.0721 0.2155 0.070 Uiso 1 1 calc R . . H1B H -0.0302 0.1013 0.3416 0.070 Uiso 1 1 calc R . . H1C H 0.0120 0.0786 0.2647 0.070 Uiso 1 1 calc R . . C2 C -0.0563(2) 0.1743(2) 0.2170(3) 0.0327(6) Uani 1 1 d . . . H2 H -0.1084 0.1952 0.2237 0.039 Uiso 1 1 calc R . . C3 C 0.0305(3) 0.2177(3) 0.2919(3) 0.0499(10) Uani 1 1 d . . . H3A H 0.0214 0.2652 0.2609 0.075 Uiso 1 1 calc R . . H3B H 0.0850 0.1962 0.2942 0.075 Uiso 1 1 calc R . . H3C H 0.0414 0.2197 0.3691 0.075 Uiso 1 1 calc R . . C4 C -0.2673(3) 0.1307(2) 0.0400(4) 0.0396(8) Uani 1 1 d . . . H4A H -0.2312 0.1231 0.1225 0.059 Uiso 1 1 calc R . . H4B H -0.3171 0.0954 0.0038 0.059 Uiso 1 1 calc R . . H4C H -0.2956 0.1775 0.0236 0.059 Uiso 1 1 calc R . . C5 C -0.2018(2) 0.12466(17) -0.0069(3) 0.0279(5) Uani 1 1 d . . . H5 H -0.1804 0.0748 0.0045 0.033 Uiso 1 1 calc R . . C6 C -0.2586(2) 0.13659(19) -0.1347(3) 0.0341(6) Uani 1 1 d . . . H6A H -0.2175 0.1318 -0.1658 0.051 Uiso 1 1 calc R . . H6B H -0.2857 0.1837 -0.1506 0.051 Uiso 1 1 calc R . . H6C H -0.3093 0.1019 -0.1703 0.051 Uiso 1 1 calc R . . C7 C -0.2007(3) 0.3019(2) 0.0527(4) 0.0410(8) Uani 1 1 d . . . H7A H -0.1851 0.2881 0.1293 0.062 Uiso 1 1 calc R . . H7B H -0.2625 0.2829 -0.0036 0.062 Uiso 1 1 calc R . . H7C H -0.2022 0.3531 0.0471 0.062 Uiso 1 1 calc R . . C8 C -0.1262(2) 0.27306(17) 0.0297(3) 0.0305(6) Uani 1 1 d . . . H8 H -0.0675 0.2994 0.0829 0.037 Uiso 1 1 calc R . . C9 C -0.1482(3) 0.2932(2) -0.0895(3) 0.0387(7) Uani 1 1 d . . . H9A H -0.0993 0.2744 -0.1019 0.058 Uiso 1 1 calc R . . H9B H -0.1499 0.3443 -0.0964 0.058 Uiso 1 1 calc R . . H9C H -0.2094 0.2738 -0.1466 0.058 Uiso 1 1 calc R . . C11 C -0.0464(2) 0.05657(16) -0.0610(3) 0.0288(6) Uani 1 1 d D . . C12 C 0.0183(2) 0.05058(16) 0.0585(3) 0.0302(6) Uani 1 1 d D . . C13 C 0.1165(2) 0.01829(18) 0.1174(3) 0.0342(7) Uani 1 1 d . . . C14 C 0.1039(4) -0.0558(2) 0.1497(6) 0.0619(14) Uani 1 1 d . . . H14A H 0.0610 -0.0821 0.0806 0.093 Uiso 1 1 calc R . . H14B H 0.0776 -0.0533 0.1990 0.093 Uiso 1 1 calc R . . H14C H 0.1650 -0.0794 0.1903 0.093 Uiso 1 1 calc R . . C15 C 0.1825(3) 0.0605(3) 0.2218(4) 0.0545(11) Uani 1 1 d . . . H15A H 0.1888 0.1078 0.1989 0.082 Uiso 1 1 calc R . . H15B H 0.2443 0.0378 0.2621 0.082 Uiso 1 1 calc R . . H15C H 0.1573 0.0633 0.2722 0.082 Uiso 1 1 calc R . . C16 C 0.1587(3) 0.0119(2) 0.0414(4) 0.0443(8) Uani 1 1 d . . . H16A H 0.1162 -0.0153 -0.0267 0.066 Uiso 1 1 calc R . . H16B H 0.2198 -0.0117 0.0836 0.066 Uiso 1 1 calc R . . H16C H 0.1670 0.0588 0.0188 0.066 Uiso 1 1 calc R . . C21 C 0.3533(3) 0.2512(3) 0.0439(3) 0.0418(8) Uani 1 1 d . . . H21 H 0.4256 0.2281 0.0933 0.050 Uiso 1 1 calc R . . B22 B 0.2665(2) 0.2100(2) 0.0522(3) 0.0335(7) Uani 1 1 d . . . H22 H 0.2761 0.1617 0.1034 0.040 Uiso 1 1 calc R . . B23 B 0.2712(3) 0.2066(2) -0.0746(4) 0.0347(7) Uani 1 1 d . . . H23 H 0.2835 0.1563 -0.1066 0.042 Uiso 1 1 calc R . . B24 B 0.3196(3) 0.2878(2) -0.0849(4) 0.0358(8) Uani 1 1 d . . . H24 H 0.3645 0.2906 -0.1236 0.043 Uiso 1 1 calc R . . B25 B 0.3445(3) 0.3400(2) 0.0342(3) 0.0373(9) Uani 1 1 d . . . H25 H 0.4056 0.3770 0.0739 0.045 Uiso 1 1 calc R . . B26 B 0.3113(3) 0.2925(2) 0.1193(3) 0.0355(8) Uani 1 1 d . . . H26 H 0.3499 0.2983 0.2142 0.043 Uiso 1 1 calc R . . B27 B 0.1880(2) 0.27834(18) 0.0354(3) 0.0242(5) Uani 1 1 d . . . B28 B 0.1651(2) 0.22656(17) -0.0817(3) 0.0239(5) Uani 1 1 d . . . B29 B 0.1963(3) 0.27337(19) -0.1686(3) 0.0267(6) Uani 1 1 d . . . B30 B 0.2422(3) 0.3559(2) -0.1014(3) 0.0298(7) Uani 1 1 d . . . B31 B 0.2366(3) 0.3593(2) 0.0256(3) 0.0316(7) Uani 1 1 d . . . B32 B 0.1439(2) 0.31870(17) -0.1001(3) 0.0234(5) Uani 1 1 d . . . Br7 Br 0.10726(2) 0.268868(16) 0.10074(2) 0.02743(6) Uani 1 1 d . . . Br8 Br 0.05791(2) 0.161423(15) -0.14500(2) 0.02584(6) Uani 1 1 d . . . Br9 Br 0.12722(3) 0.260428(19) -0.33263(3) 0.03553(7) Uani 1 1 d . . . Br10 Br 0.23030(3) 0.439867(19) -0.18743(3) 0.03944(8) Uani 1 1 d . . . Br11 Br 0.21967(4) 0.44592(2) 0.08691(4) 0.04966(11) Uani 1 1 d . . . Br12 Br 0.01888(2) 0.357906(18) -0.18612(3) 0.03227(7) Uani 1 1 d . . . H12 H -0.013(2) 0.0452(19) 0.101(3) 0.015(8) Uiso 1 1 d D . . H11A H -0.030(3) 0.038(2) -0.113(3) 0.027(10) Uiso 1 1 d D . . H11B H -0.106(2) 0.043(3) -0.077(5) 0.051(14) Uiso 1 1 d 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 Rh 0.02330(9) 0.02185(9) 0.02351(9) -0.00175(7) 0.01434(8) -0.00297(7) P 0.0249(3) 0.0269(3) 0.0218(3) 0.0013(3) 0.0144(3) -0.0007(3) C1 0.049(2) 0.063(3) 0.0325(17) 0.0201(17) 0.0237(16) 0.0115(19) C2 0.0332(15) 0.0451(17) 0.0240(13) 0.0000(12) 0.0177(12) -0.0014(13) C3 0.046(2) 0.075(3) 0.0283(17) -0.0080(18) 0.0194(16) -0.011(2) C4 0.0354(17) 0.0449(19) 0.052(2) 0.0055(16) 0.0321(16) -0.0011(14) C5 0.0261(13) 0.0298(14) 0.0316(14) 0.0022(11) 0.0176(11) 0.0016(11) C6 0.0299(14) 0.0365(17) 0.0305(15) 0.0000(13) 0.0118(12) -0.0017(12) C7 0.0404(18) 0.0384(18) 0.052(2) 0.0010(16) 0.0297(17) 0.0081(14) C8 0.0319(15) 0.0251(14) 0.0370(16) -0.0005(11) 0.0197(13) -0.0007(11) C9 0.0442(18) 0.0329(16) 0.0402(18) 0.0092(14) 0.0228(15) 0.0066(14) C11 0.0293(14) 0.0244(13) 0.0359(16) -0.0054(11) 0.0191(12) -0.0035(10) C12 0.0331(15) 0.0237(13) 0.0382(16) 0.0048(11) 0.0216(13) 0.0000(11) C13 0.0308(15) 0.0260(14) 0.0455(19) 0.0064(12) 0.0197(14) 0.0007(11) C14 0.049(2) 0.039(2) 0.098(4) 0.027(2) 0.038(3) 0.0089(18) C15 0.0363(19) 0.068(3) 0.045(2) -0.002(2) 0.0109(17) 0.0053(19) C16 0.0353(17) 0.043(2) 0.056(2) 0.0024(17) 0.0248(17) 0.0079(15) C21 0.0249(14) 0.059(2) 0.0385(18) 0.0139(16) 0.0141(13) -0.0041(14) B22 0.0234(14) 0.044(2) 0.0330(17) 0.0118(15) 0.0144(13) 0.0002(13) B23 0.0292(16) 0.0375(19) 0.044(2) 0.0063(15) 0.0234(15) 0.0046(14) B24 0.0287(16) 0.046(2) 0.0379(18) 0.0059(16) 0.0207(15) -0.0057(15) B25 0.0271(16) 0.050(2) 0.0303(17) 0.0020(15) 0.0115(14) -0.0159(15) B26 0.0243(15) 0.047(2) 0.0313(16) 0.0024(15) 0.0119(13) -0.0104(15) B27 0.0252(13) 0.0279(14) 0.0197(12) 0.0015(10) 0.0118(11) -0.0033(11) B28 0.0225(13) 0.0251(14) 0.0268(14) 0.0005(11) 0.0148(12) -0.0030(10) B29 0.0284(15) 0.0302(15) 0.0260(14) -0.0028(12) 0.0173(12) -0.0051(12) B30 0.0317(16) 0.0309(16) 0.0247(14) -0.0005(12) 0.0131(13) -0.0102(13) B31 0.0381(18) 0.0332(17) 0.0237(14) -0.0055(12) 0.0161(13) -0.0143(14) B32 0.0244(13) 0.0239(13) 0.0225(13) -0.0002(10) 0.0125(11) -0.0035(10) Br7 0.03264(13) 0.02990(14) 0.02443(12) -0.00654(10) 0.01810(11) -0.01041(11) Br8 0.03004(13) 0.02557(13) 0.02800(13) -0.00586(10) 0.01934(11) -0.00691(10) Br9 0.04434(17) 0.04171(18) 0.02878(14) -0.00672(13) 0.02476(14) -0.01120(14) Br10 0.0547(2) 0.03373(16) 0.03381(16) 0.00111(13) 0.02576(16) -0.01498(15) Br11 0.0821(3) 0.03435(18) 0.0414(2) -0.01550(15) 0.0382(2) -0.02404(19) Br12 0.03220(15) 0.03237(15) 0.03152(14) 0.00415(12) 0.01602(12) 0.00507(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C11 2.107(3) . ? Rh C12 2.124(3) . ? Rh P 2.2319(7) . ? Rh Br7 2.6140(3) . ? Rh Br8 2.6264(3) . ? P C5 1.852(3) . ? P C2 1.854(3) . ? P C8 1.867(3) . ? C1 C2 1.527(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.513(6) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.530(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.519(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.530(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.531(5) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.426(5) . ? C11 H11A 0.950(18) . ? C11 H11B 0.929(19) . ? C12 C13 1.526(5) . ? C12 H12 0.969(18) . ? C13 C15 1.510(6) . ? C13 C14 1.530(5) . ? C13 C16 1.535(6) . ? 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 . ? C21 B22 1.698(5) . ? C21 B25 1.701(6) . ? C21 B24 1.703(6) . ? C21 B23 1.712(6) . ? C21 B26 1.713(7) . ? C21 H21 1.1200 . ? B22 B28 1.764(5) . ? B22 B27 1.776(5) . ? B22 B26 1.782(6) . ? B22 B23 1.783(6) . ? B22 H22 1.1200 . ? B23 B28 1.757(5) . ? B23 B29 1.782(5) . ? B23 B24 1.786(6) . ? B23 H23 1.1200 . ? B24 B30 1.760(6) . ? B24 B25 1.771(6) . ? B24 B29 1.777(5) . ? B24 H24 1.1200 . ? B25 B31 1.775(6) . ? B25 B26 1.779(5) . ? B25 B30 1.780(6) . ? B25 H25 1.1200 . ? B26 B27 1.776(5) . ? B26 B31 1.781(6) . ? B26 H26 1.1200 . ? B27 B28 1.755(5) . ? B27 B31 1.782(5) . ? B27 B32 1.784(4) . ? B27 Br7 1.972(3) . ? B28 B29 1.770(5) . ? B28 B32 1.787(5) . ? B28 Br8 1.968(3) . ? B29 B30 1.785(5) . ? B29 B32 1.800(5) . ? B29 Br9 1.943(3) . ? B30 B32 1.791(5) . ? B30 B31 1.796(5) . ? B30 Br10 1.941(4) . ? B31 B32 1.788(5) . ? B31 Br11 1.943(4) . ? B32 Br12 1.931(3) . ? 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 C11 Rh C12 39.40(14) . . ? C11 Rh P 96.32(9) . . ? C12 Rh P 90.94(9) . . ? C11 Rh Br7 167.52(9) . . ? C12 Rh Br7 133.78(10) . . ? P Rh Br7 94.12(2) . . ? C11 Rh Br8 85.28(9) . . ? C12 Rh Br8 106.84(9) . . ? P Rh Br8 152.39(2) . . ? Br7 Rh Br8 88.642(10) . . ? C5 P C2 103.67(15) . . ? C5 P C8 109.43(15) . . ? C2 P C8 102.53(17) . . ? C5 P Rh 113.85(10) . . ? C2 P Rh 121.27(12) . . ? C8 P Rh 105.23(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 109.7(3) . . ? C3 C2 P 112.7(2) . . ? C1 C2 P 114.1(3) . . ? C3 C2 H2 106.6 . . ? C1 C2 H2 106.6 . . ? P C2 H2 106.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C4 108.9(3) . . ? C6 C5 P 112.2(2) . . ? C4 C5 P 116.2(3) . . ? C6 C5 H5 106.3 . . ? C4 C5 H5 106.3 . . ? P C5 H5 106.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C9 111.1(3) . . ? C7 C8 P 116.8(3) . . ? C9 C8 P 113.1(2) . . ? C7 C8 H8 104.8 . . ? C9 C8 H8 104.8 . . ? P C8 H8 104.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 Rh 70.94(18) . . ? C12 C11 H11A 119(3) . . ? Rh C11 H11A 117(3) . . ? C12 C11 H11B 109(3) . . ? Rh C11 H11B 121(3) . . ? H11A C11 H11B 113(4) . . ? C11 C12 C13 127.1(3) . . ? C11 C12 Rh 69.66(18) . . ? C13 C12 Rh 116.8(2) . . ? C11 C12 H12 113(2) . . ? C13 C12 H12 113(2) . . ? Rh C12 H12 109(2) . . ? C15 C13 C12 109.8(3) . . ? C15 C13 C14 111.1(4) . . ? C12 C13 C14 104.9(3) . . ? C15 C13 C16 108.9(3) . . ? C12 C13 C16 114.4(3) . . ? C14 C13 C16 107.7(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 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 . . ? B22 C21 B25 115.2(3) . . ? B22 C21 B24 115.2(3) . . ? B25 C21 B24 62.7(3) . . ? B22 C21 B23 63.0(2) . . ? B25 C21 B23 115.3(3) . . ? B24 C21 B23 63.1(2) . . ? B22 C21 B26 63.0(2) . . ? B25 C21 B26 62.8(3) . . ? B24 C21 B26 114.9(3) . . ? B23 C21 B26 115.4(3) . . ? B22 C21 H21 117.3 . . ? B25 C21 H21 117.5 . . ? B24 C21 H21 117.6 . . ? B23 C21 H21 117.1 . . ? B26 C21 H21 117.5 . . ? C21 B22 B28 103.5(3) . . ? C21 B22 B27 104.1(3) . . ? B28 B22 B27 59.43(19) . . ? C21 B22 B26 58.9(3) . . ? B28 B22 B26 107.3(3) . . ? B27 B22 B26 59.9(2) . . ? C21 B22 B23 58.9(2) . . ? B28 B22 B23 59.4(2) . . ? B27 B22 B23 107.6(3) . . ? B26 B22 B23 108.6(3) . . ? C21 B22 H22 125.1 . . ? B28 B22 H22 123.4 . . ? B27 B22 H22 122.8 . . ? B26 B22 H22 121.2 . . ? B23 B22 H22 121.3 . . ? C21 B23 B28 103.2(3) . . ? C21 B23 B29 104.2(3) . . ? B28 B23 B29 60.00(19) . . ? C21 B23 B22 58.1(2) . . ? B28 B23 B22 59.8(2) . . ? B29 B23 B22 108.3(3) . . ? C21 B23 B24 58.2(2) . . ? B28 B23 B24 106.7(3) . . ? B29 B23 B24 59.7(2) . . ? B22 B23 B24 107.2(3) . . ? C21 B23 H23 125.6 . . ? B28 B23 H23 123.2 . . ? B29 B23 H23 122.1 . . ? B22 B23 H23 121.6 . . ? B24 B23 H23 122.2 . . ? C21 B24 B30 105.2(3) . . ? C21 B24 B25 58.6(3) . . ? B30 B24 B25 60.6(2) . . ? C21 B24 B29 104.8(2) . . ? B30 B24 B29 60.6(2) . . ? B25 B24 B29 108.9(3) . . ? C21 B24 B23 58.7(2) . . ? B30 B24 B23 108.8(3) . . ? B25 B24 B23 108.4(3) . . ? B29 B24 B23 60.0(2) . . ? C21 B24 H24 124.9 . . ? B30 B24 H24 121.7 . . ? B25 B24 H24 121.1 . . ? B29 B24 H24 122.0 . . ? B23 B24 H24 121.3 . . ? C21 B25 B24 58.7(2) . . ? C21 B25 B31 104.8(3) . . ? B24 B25 B31 108.1(3) . . ? C21 B25 B26 58.9(2) . . ? B24 B25 B26 108.4(3) . . ? B31 B25 B26 60.1(2) . . ? C21 B25 B30 104.4(3) . . ? B24 B25 B30 59.4(2) . . ? B31 B25 B30 60.7(2) . . ? B26 B25 B30 108.7(3) . . ? C21 B25 H25 124.9 . . ? B24 B25 H25 121.6 . . ? B31 B25 H25 122.1 . . ? B26 B25 H25 121.0 . . ? B30 B25 H25 122.3 . . ? C21 B26 B27 103.5(3) . . ? C21 B26 B25 58.3(2) . . ? B27 B26 B25 107.4(3) . . ? C21 B26 B31 104.1(3) . . ? B27 B26 B31 60.1(2) . . ? B25 B26 B31 59.8(2) . . ? C21 B26 B22 58.1(2) . . ? B27 B26 B22 59.9(2) . . ? B25 B26 B22 107.4(3) . . ? B31 B26 B22 108.2(3) . . ? C21 B26 H26 125.6 . . ? B27 B26 H26 122.8 . . ? B25 B26 H26 121.9 . . ? B31 B26 H26 122.2 . . ? B22 B26 H26 121.6 . . ? B28 B27 B26 108.0(3) . . ? B28 B27 B22 59.9(2) . . ? B26 B27 B22 60.2(2) . . ? B28 B27 B31 108.1(2) . . ? B26 B27 B31 60.1(2) . . ? B22 B27 B31 108.4(3) . . ? B28 B27 B32 60.66(18) . . ? B26 B27 B32 108.8(2) . . ? B22 B27 B32 109.2(2) . . ? B31 B27 B32 60.17(19) . . ? B28 B27 Br7 119.4(2) . . ? B26 B27 Br7 123.2(2) . . ? B22 B27 Br7 120.1(2) . . ? B31 B27 Br7 123.8(2) . . ? B32 B27 Br7 120.4(2) . . ? B27 B28 B23 109.7(3) . . ? B27 B28 B22 60.6(2) . . ? B23 B28 B22 60.9(2) . . ? B27 B28 B29 109.5(2) . . ? B23 B28 B29 60.7(2) . . ? B22 B28 B29 109.7(2) . . ? B27 B28 B32 60.49(18) . . ? B23 B28 B32 109.9(2) . . ? B22 B28 B32 109.7(2) . . ? B29 B28 B32 60.81(19) . . ? B27 B28 Br8 118.5(2) . . ? B23 B28 Br8 122.7(2) . . ? B22 B28 Br8 120.3(2) . . ? B29 B28 Br8 122.5(2) . . ? B32 B28 Br8 119.56(19) . . ? B28 B29 B24 106.6(3) . . ? B28 B29 B23 59.28(19) . . ? B24 B29 B23 60.2(2) . . ? B28 B29 B30 107.1(2) . . ? B24 B29 B30 59.2(2) . . ? B23 B29 B30 107.9(3) . . ? B28 B29 B32 60.08(18) . . ? B24 B29 B32 107.2(3) . . ? B23 B29 B32 108.2(2) . . ? B30 B29 B32 59.93(19) . . ? B28 B29 Br9 120.9(2) . . ? B24 B29 Br9 124.0(2) . . ? B23 B29 Br9 121.3(2) . . ? B30 B29 Br9 123.3(2) . . ? B32 B29 Br9 120.8(2) . . ? B24 B30 B25 60.0(2) . . ? B24 B30 B29 60.2(2) . . ? B25 B30 B29 108.1(3) . . ? B24 B30 B32 108.4(3) . . ? B25 B30 B32 107.7(2) . . ? B29 B30 B32 60.46(19) . . ? B24 B30 B31 107.7(3) . . ? B25 B30 B31 59.5(2) . . ? B29 B30 B31 108.0(2) . . ? B32 B30 B31 59.79(19) . . ? B24 B30 Br10 121.8(2) . . ? B25 B30 Br10 121.2(2) . . ? B29 B30 Br10 122.3(2) . . ? B32 B30 Br10 121.9(2) . . ? B31 B30 Br10 121.4(3) . . ? B25 B31 B26 60.0(2) . . ? B25 B31 B27 107.3(3) . . ? B26 B31 B27 59.8(2) . . ? B25 B31 B32 108.0(3) . . ? B26 B31 B32 108.4(3) . . ? B27 B31 B32 59.98(18) . . ? B25 B31 B30 59.8(2) . . ? B26 B31 B30 107.9(3) . . ? B27 B31 B30 107.2(2) . . ? B32 B31 B30 59.96(19) . . ? B25 B31 Br11 121.1(2) . . ? B26 B31 Br11 120.0(2) . . ? B27 B31 Br11 122.2(2) . . ? B32 B31 Br11 122.8(3) . . ? B30 B31 Br11 123.0(2) . . ? B27 B32 B28 58.85(18) . . ? B27 B32 B31 59.85(19) . . ? B28 B32 B31 106.4(2) . . ? B27 B32 B30 107.4(2) . . ? B28 B32 B30 106.1(2) . . ? B31 B32 B30 60.25(19) . . ? B27 B32 B29 106.8(2) . . ? B28 B32 B29 59.12(18) . . ? B31 B32 B29 107.7(2) . . ? B30 B32 B29 59.61(19) . . ? B27 B32 Br12 122.4(2) . . ? B28 B32 Br12 122.63(19) . . ? B31 B32 Br12 122.5(2) . . ? B30 B32 Br12 122.6(2) . . ? B29 B32 Br12 121.7(2) . . ? B27 Br7 Rh 105.17(10) . . ? B28 Br8 Rh 105.34(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.792 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.123 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.052 0.500 -0.030 347.5 4.1 2 0.448 0.000 0.070 347.5 4.1 _platon_squeeze_details ; ? ; #===END data_h06asw15 _database_code_depnum_ccdc_archive 'CCDC 624749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 9' _chemical_melting_point ? _chemical_formula_moiety 'C16 H31 B11 Br6 P Rh' _chemical_formula_sum 'C16 H31 B11 Br6 P Rh' _chemical_formula_weight 955.66 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.9014(1) _cell_length_b 13.8202(1) _cell_length_c 16.3616(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2917.23(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 119804 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 29.131 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 8.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2152 _exptl_absorpt_correction_T_max 0.3497 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '588 1.0 degree images with \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61703 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.32 _diffrn_reflns_theta_max 29.13 _reflns_number_total 7799 _reflns_number_gt 7004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms H1' - H6' were modelled with a constrained X-H vector direction, Uiso=1.2 Ueq, and with a refined X-H distance. The B-H bond distances for H2' - H6' were restrained to be equal. H3 and H4 were located and refined with their C-H distances restrained to be equal. ; _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^)+(0.0276P)^2^+3.7753P] 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 -0.014(6) _refine_ls_number_reflns 7799 _refine_ls_number_parameters 330 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.63779(3) -0.12634(2) 0.85410(2) 0.02610(8) Uani 1 1 d . . . P P 0.59280(9) -0.27460(8) 0.82103(7) 0.0272(2) Uani 1 1 d . . . C1 C 0.4666(4) -0.2777(3) 0.8731(3) 0.0341(10) Uani 1 1 d . . . H1 H 0.4266 -0.3393 0.8670 0.041 Uiso 1 1 calc R . . C2 C 0.4901(4) -0.2467(4) 0.9618(3) 0.0383(11) Uani 1 1 d . . . H2A H 0.4271 -0.2484 0.9963 0.046 Uiso 1 1 calc R . . H2B H 0.5443 -0.2878 0.9868 0.046 Uiso 1 1 calc R . . C3 C 0.5282(4) -0.1434(3) 0.9487(3) 0.0323(10) Uani 1 1 d D . . C4 C 0.4807(4) -0.1076(3) 0.8768(3) 0.0302(9) Uani 1 1 d D . . C5 C 0.4109(3) -0.1852(3) 0.8421(3) 0.0331(10) Uani 1 1 d . . . H5A H 0.4087 -0.1827 0.7816 0.040 Uiso 1 1 calc R . . H5B H 0.3395 -0.1802 0.8640 0.040 Uiso 1 1 calc R . . C6 C 0.6796(4) -0.3717(3) 0.8544(3) 0.0323(9) Uani 1 1 d . . . H6 H 0.7446 -0.3626 0.8220 0.039 Uiso 1 1 calc R . . C7 C 0.7151(5) -0.3766(4) 0.9446(3) 0.0442(12) Uani 1 1 d . . . H7A H 0.7628 -0.3225 0.9575 0.053 Uiso 1 1 calc R . . H7B H 0.6549 -0.3737 0.9820 0.053 Uiso 1 1 calc R . . C8 C 0.7700(5) -0.4726(4) 0.9517(4) 0.0485(14) Uani 1 1 d . . . H8A H 0.7662 -0.4974 1.0084 0.058 Uiso 1 1 calc R . . H8B H 0.8438 -0.4663 0.9359 0.058 Uiso 1 1 calc R . . C9 C 0.7130(5) -0.5403(4) 0.8930(3) 0.0443(13) Uani 1 1 d . . . H9A H 0.6693 -0.5864 0.9240 0.053 Uiso 1 1 calc R . . H9B H 0.7633 -0.5776 0.8600 0.053 Uiso 1 1 calc R . . C10 C 0.6452(4) -0.4772(3) 0.8374(3) 0.0358(10) Uani 1 1 d . . . H10A H 0.5709 -0.4860 0.8506 0.043 Uiso 1 1 calc R . . H10B H 0.6565 -0.4941 0.7793 0.043 Uiso 1 1 calc R . . C11 C 0.5779(4) -0.3087(3) 0.7126(3) 0.0302(9) Uani 1 1 d . . . H11 H 0.5517 -0.3768 0.7115 0.036 Uiso 1 1 calc R . . C12 C 0.5069(4) -0.2495(3) 0.6570(3) 0.0336(10) Uani 1 1 d . . . H12A H 0.4332 -0.2671 0.6652 0.040 Uiso 1 1 calc R . . H12B H 0.5156 -0.1792 0.6666 0.040 Uiso 1 1 calc R . . C13 C 0.5443(4) -0.2781(4) 0.5718(3) 0.0385(11) Uani 1 1 d . . . H13A H 0.5196 -0.3436 0.5569 0.046 Uiso 1 1 calc R . . H13B H 0.5202 -0.2313 0.5301 0.046 Uiso 1 1 calc R . . C14 C 0.6614(4) -0.2761(4) 0.5797(3) 0.0379(11) Uani 1 1 d . . . H14A H 0.6883 -0.2100 0.5699 0.045 Uiso 1 1 calc R . . H14B H 0.6938 -0.3208 0.5399 0.045 Uiso 1 1 calc R . . C15 C 0.6842(4) -0.3086(4) 0.6678(3) 0.0369(10) Uani 1 1 d . . . H15A H 0.7328 -0.2632 0.6946 0.044 Uiso 1 1 calc R . . H15B H 0.7152 -0.3741 0.6683 0.044 Uiso 1 1 calc R . . C1' C 0.9286(4) 0.1965(3) 0.7643(3) 0.0295(9) Uani 1 1 d . . . H1' H 0.9426(9) 0.259(4) 0.7508(9) 0.035 Uiso 1 1 d R . . B2 B 1.0111(4) 0.1421(3) 0.8315(3) 0.0265(10) Uani 1 1 d D . . H2' H 1.0785(15) 0.1756(8) 0.8595(7) 0.032 Uiso 1 1 d RD . . B3 B 1.0094(4) 0.1107(4) 0.7258(3) 0.0299(10) Uani 1 1 d D . . H3' H 1.0757(15) 0.1247(5) 0.6865(9) 0.036 Uiso 1 1 d RD . . B4 B 0.8803(4) 0.1248(4) 0.6892(3) 0.0310(11) Uani 1 1 d D . . H4' H 0.8643(5) 0.1476(6) 0.6264(14) 0.037 Uiso 1 1 d RD . . B5 B 0.8015(4) 0.1649(3) 0.7724(3) 0.0268(10) Uani 1 1 d D . . H5' H 0.7357(15) 0.2127(11) 0.7628(4) 0.032 Uiso 1 1 d RD . . B6 B 0.8820(4) 0.1763(3) 0.8603(3) 0.0260(9) Uani 1 1 d D . . H6' H 0.8673(5) 0.2313(13) 0.9061(11) 0.031 Uiso 1 1 d RD . . B7 B 0.9312(4) 0.0592(3) 0.8855(3) 0.0249(9) Uani 1 1 d . . . B8 B 1.0106(4) 0.0178(3) 0.8018(3) 0.0249(9) Uani 1 1 d . . . B9 B 0.9294(4) 0.0075(3) 0.7133(3) 0.0261(10) Uani 1 1 d . . . B10 B 0.8003(4) 0.0406(3) 0.7422(3) 0.0253(10) Uani 1 1 d . . . B11 B 0.8026(4) 0.0733(3) 0.8477(3) 0.0242(9) Uani 1 1 d . . . B12 B 0.8807(3) -0.0235(3) 0.8114(3) 0.0213(9) Uani 1 1 d . . . Br7 Br 0.95581(4) 0.01861(3) 0.99697(3) 0.03490(11) Uani 1 1 d . . . Br8 Br 1.13101(3) -0.06348(3) 0.82072(3) 0.03244(10) Uani 1 1 d . . . Br9 Br 0.95457(4) -0.08834(3) 0.62812(3) 0.03363(11) Uani 1 1 d . . . Br10 Br 0.67791(4) -0.02389(3) 0.69902(3) 0.03457(11) Uani 1 1 d . . . Br11 Br 0.68231(3) 0.04567(3) 0.91654(3) 0.03029(10) Uani 1 1 d . . . Br12 Br 0.84176(3) -0.15595(3) 0.84225(3) 0.02706(9) Uani 1 1 d . . . H3 H 0.539(4) -0.097(3) 0.992(3) 0.028(12) Uiso 1 1 d D . . H4 H 0.469(4) -0.040(3) 0.870(3) 0.035(13) Uiso 1 1 d 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 Rh 0.02519(15) 0.02567(15) 0.02743(16) 0.00014(13) 0.00180(13) -0.00291(13) P 0.0263(5) 0.0268(5) 0.0286(5) 0.0020(4) 0.0004(4) -0.0025(4) C1 0.030(2) 0.033(2) 0.040(3) 0.000(2) 0.007(2) -0.0054(19) C2 0.037(3) 0.044(3) 0.034(2) 0.005(2) 0.010(2) -0.005(2) C3 0.032(2) 0.036(2) 0.029(2) -0.0026(19) 0.0050(18) -0.0037(19) C4 0.028(2) 0.030(2) 0.032(2) -0.0022(18) 0.0021(18) -0.0049(17) C5 0.024(2) 0.037(2) 0.038(3) -0.002(2) 0.0002(19) -0.0019(18) C6 0.031(2) 0.029(2) 0.037(2) 0.0025(19) 0.0022(19) -0.0037(18) C7 0.050(3) 0.039(3) 0.044(3) 0.004(2) -0.010(2) 0.003(2) C8 0.047(3) 0.051(3) 0.048(3) 0.017(3) -0.003(2) 0.005(3) C9 0.054(3) 0.035(3) 0.044(3) 0.005(2) 0.005(2) 0.013(2) C10 0.041(3) 0.029(2) 0.037(2) 0.0026(19) 0.007(2) 0.001(2) C11 0.034(2) 0.029(2) 0.027(2) 0.0002(18) -0.0028(18) -0.0047(18) C12 0.034(2) 0.033(2) 0.034(2) 0.0014(19) 0.000(2) -0.0026(18) C13 0.046(3) 0.041(3) 0.029(2) 0.001(2) -0.003(2) -0.007(2) C14 0.041(3) 0.040(2) 0.032(2) -0.002(2) 0.006(2) 0.001(2) C15 0.037(3) 0.040(2) 0.033(2) -0.002(2) 0.001(2) 0.002(2) C1' 0.031(2) 0.0195(19) 0.038(2) 0.0015(18) 0.0054(19) -0.0022(17) B2 0.029(2) 0.024(2) 0.027(2) 0.0002(19) 0.0004(18) 0.0001(18) B3 0.032(3) 0.026(2) 0.032(3) 0.0028(19) 0.007(2) -0.002(2) B4 0.036(3) 0.027(2) 0.029(2) 0.001(2) 0.003(2) 0.002(2) B5 0.032(3) 0.024(2) 0.024(2) 0.0012(18) -0.0010(19) 0.0013(19) B6 0.030(2) 0.023(2) 0.025(2) -0.0028(18) -0.0005(19) -0.0008(18) B7 0.029(2) 0.021(2) 0.024(2) -0.0015(18) -0.0043(18) -0.0002(18) B8 0.021(2) 0.0199(19) 0.034(2) 0.0021(19) 0.0034(18) 0.0002(17) B9 0.031(3) 0.021(2) 0.026(2) -0.0008(18) 0.0005(19) 0.0000(18) B10 0.022(2) 0.026(2) 0.028(2) 0.0056(19) -0.0070(18) -0.0006(18) B11 0.023(2) 0.025(2) 0.024(2) -0.0011(18) 0.0035(18) -0.0010(17) B12 0.019(2) 0.0218(19) 0.023(2) 0.0013(17) 0.0012(17) 0.0023(16) Br7 0.0459(3) 0.0345(2) 0.0243(2) 0.00026(18) -0.00672(19) 0.0053(2) Br8 0.0260(2) 0.0285(2) 0.0428(2) -0.00400(18) -0.00261(19) 0.00358(17) Br9 0.0464(3) 0.0292(2) 0.0253(2) -0.00383(17) 0.00247(19) 0.00424(19) Br10 0.0322(2) 0.0347(2) 0.0368(2) -0.00347(19) -0.01104(19) -0.00073(19) Br11 0.0286(2) 0.0286(2) 0.0336(2) -0.00290(17) 0.00706(18) -0.00059(17) Br12 0.0276(2) 0.02100(17) 0.0326(2) 0.00297(16) 0.00011(16) -0.00086(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 Rh C4 2.077(5) . ? Rh C3 2.109(5) . ? Rh P 2.1973(11) . ? Rh Br11 2.6504(5) . ? Rh Br12 2.6702(5) . ? Rh Br10 2.9514(6) . ? P C6 1.831(5) . ? P C1 1.839(5) . ? P C11 1.846(5) . ? C1 C2 1.544(7) . ? C1 C5 1.552(7) . ? C1 H1 1.0000 . ? C2 C3 1.526(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.415(7) . ? C3 H3 0.96(4) . ? C4 C5 1.511(6) . ? C4 H4 0.95(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.546(7) . ? C6 C10 1.549(6) . ? C6 H6 1.0000 . ? C7 C8 1.509(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.529(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.534(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.529(6) . ? C11 C15 1.554(7) . ? C11 H11 1.0000 . ? C12 C13 1.528(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.516(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.539(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C1' B4 1.697(7) . ? C1' B3 1.699(7) . ? C1' B5 1.703(7) . ? C1' B6 1.705(7) . ? C1' B2 1.706(7) . ? C1' H1' 0.9070 . ? B2 B7 1.776(7) . ? B2 B3 1.784(7) . ? B2 B8 1.785(6) . ? B2 B6 1.794(7) . ? B2 H2' 1.0863 . ? B3 B9 1.773(7) . ? B3 B4 1.780(8) . ? B3 B8 1.788(7) . ? B3 H3' 1.0880 . ? B4 B10 1.780(7) . ? B4 B9 1.784(7) . ? B4 B5 1.787(7) . ? B4 H4' 1.0939 . ? B5 B11 1.767(6) . ? B5 B6 1.781(7) . ? B5 B10 1.788(7) . ? B5 H5' 1.0867 . ? B6 B11 1.766(6) . ? B6 B7 1.787(6) . ? B6 H6' 1.0834 . ? B7 B11 1.781(7) . ? B7 B12 1.789(6) . ? B7 B8 1.803(7) . ? B7 Br7 1.935(5) . ? B8 B12 1.777(6) . ? B8 B9 1.793(7) . ? B8 Br8 1.942(5) . ? B9 B12 1.776(7) . ? B9 B10 1.791(7) . ? B9 Br9 1.950(5) . ? B10 B12 1.774(6) . ? B10 B11 1.786(7) . ? B10 Br10 1.946(5) . ? B11 B12 1.778(6) . ? B11 Br11 1.955(5) . ? B12 Br12 1.964(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 C4 Rh C3 39.51(18) . . ? C4 Rh P 84.40(13) . . ? C3 Rh P 84.24(13) . . ? C4 Rh Br11 91.76(12) . . ? C3 Rh Br11 87.85(13) . . ? P Rh Br11 171.32(4) . . ? C4 Rh Br12 173.66(13) . . ? C3 Rh Br12 134.16(13) . . ? P Rh Br12 95.71(3) . . ? Br11 Rh Br12 87.243(16) . . ? C4 Rh Br10 105.38(13) . . ? C3 Rh Br10 143.31(13) . . ? P Rh Br10 106.38(3) . . ? Br11 Rh Br10 82.133(15) . . ? Br12 Rh Br10 80.691(15) . . ? C6 P C1 112.7(2) . . ? C6 P C11 99.4(2) . . ? C1 P C11 110.3(2) . . ? C6 P Rh 116.64(15) . . ? C1 P Rh 98.14(15) . . ? C11 P Rh 120.16(16) . . ? C2 C1 C5 99.8(4) . . ? C2 C1 P 104.8(3) . . ? C5 C1 P 103.9(3) . . ? C2 C1 H1 115.5 . . ? C5 C1 H1 115.5 . . ? P C1 H1 115.5 . . ? C3 C2 C1 101.0(4) . . ? C3 C2 H2A 111.6 . . ? C1 C2 H2A 111.6 . . ? C3 C2 H2B 111.6 . . ? C1 C2 H2B 111.6 . . ? H2A C2 H2B 109.4 . . ? C4 C3 C2 107.7(4) . . ? C4 C3 Rh 69.0(3) . . ? C2 C3 Rh 115.1(3) . . ? C4 C3 H3 116(3) . . ? C2 C3 H3 125(3) . . ? Rh C3 H3 111(3) . . ? C3 C4 C5 108.9(4) . . ? C3 C4 Rh 71.4(3) . . ? C5 C4 Rh 115.2(3) . . ? C3 C4 H4 121(3) . . ? C5 C4 H4 124(3) . . ? Rh C4 H4 105(3) . . ? C4 C5 C1 100.7(4) . . ? C4 C5 H5A 111.6 . . ? C1 C5 H5A 111.6 . . ? C4 C5 H5B 111.6 . . ? C1 C5 H5B 111.6 . . ? H5A C5 H5B 109.4 . . ? C7 C6 C10 102.5(4) . . ? C7 C6 P 119.9(3) . . ? C10 C6 P 117.4(3) . . ? C7 C6 H6 105.2 . . ? C10 C6 H6 105.2 . . ? P C6 H6 105.2 . . ? C8 C7 C6 104.5(4) . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7B 110.8 . . ? C6 C7 H7B 110.8 . . ? H7A C7 H7B 108.9 . . ? C7 C8 C9 105.3(4) . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C8 C9 C10 107.4(4) . . ? C8 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? C8 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C9 C10 C6 105.4(4) . . ? C9 C10 H10A 110.7 . . ? C6 C10 H10A 110.7 . . ? C9 C10 H10B 110.7 . . ? C6 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? C12 C11 C15 104.4(4) . . ? C12 C11 P 119.8(3) . . ? C15 C11 P 111.1(3) . . ? C12 C11 H11 107.0 . . ? C15 C11 H11 107.0 . . ? P C11 H11 107.0 . . ? C13 C12 C11 102.4(4) . . ? C13 C12 H12A 111.3 . . ? C11 C12 H12A 111.3 . . ? C13 C12 H12B 111.3 . . ? C11 C12 H12B 111.3 . . ? H12A C12 H12B 109.2 . . ? C14 C13 C12 103.4(4) . . ? C14 C13 H13A 111.1 . . ? C12 C13 H13A 111.1 . . ? C14 C13 H13B 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.0 . . ? C13 C14 C15 105.4(4) . . ? C13 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? C13 C14 H14B 110.7 . . ? C15 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C14 C15 C11 105.9(4) . . ? C14 C15 H15A 110.6 . . ? C11 C15 H15A 110.6 . . ? C14 C15 H15B 110.6 . . ? C11 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? B4 C1' B3 63.2(3) . . ? B4 C1' B5 63.4(3) . . ? B3 C1' B5 116.1(3) . . ? B4 C1' B6 116.2(3) . . ? B3 C1' B6 116.3(3) . . ? B5 C1' B6 63.0(3) . . ? B4 C1' B2 116.0(3) . . ? B3 C1' B2 63.2(3) . . ? B5 C1' B2 115.9(3) . . ? B6 C1' B2 63.5(3) . . ? B4 C1' H1' 116.8 . . ? B3 C1' H1' 116.8 . . ? B5 C1' H1' 117.0 . . ? B6 C1' H1' 116.7 . . ? B2 C1' H1' 116.9 . . ? C1' B2 B7 104.1(3) . . ? C1' B2 B3 58.2(3) . . ? B7 B2 B3 108.6(3) . . ? C1' B2 B8 104.2(3) . . ? B7 B2 B8 60.8(3) . . ? B3 B2 B8 60.1(3) . . ? C1' B2 B6 58.2(3) . . ? B7 B2 B6 60.1(3) . . ? B3 B2 B6 107.9(3) . . ? B8 B2 B6 108.8(3) . . ? C1' B2 H2' 125.6 . . ? B7 B2 H2' 122.1 . . ? B3 B2 H2' 121.4 . . ? B8 B2 H2' 121.9 . . ? B6 B2 H2' 121.4 . . ? C1' B3 B9 104.3(4) . . ? C1' B3 B4 58.3(3) . . ? B9 B3 B4 60.3(3) . . ? C1' B3 B2 58.6(3) . . ? B9 B3 B2 108.3(3) . . ? B4 B3 B2 108.1(3) . . ? C1' B3 B8 104.4(3) . . ? B9 B3 B8 60.5(3) . . ? B4 B3 B8 108.7(3) . . ? B2 B3 B8 60.0(3) . . ? C1' B3 H3' 125.3 . . ? B9 B3 H3' 122.2 . . ? B4 B3 H3' 121.2 . . ? B2 B3 H3' 121.4 . . ? B8 B3 H3' 122.1 . . ? C1' B4 B10 104.0(3) . . ? C1' B4 B3 58.4(3) . . ? B10 B4 B3 107.9(3) . . ? C1' B4 B9 103.9(4) . . ? B10 B4 B9 60.3(3) . . ? B3 B4 B9 59.7(3) . . ? C1' B4 B5 58.4(3) . . ? B10 B4 B5 60.1(3) . . ? B3 B4 B5 108.1(4) . . ? B9 B4 B5 108.4(3) . . ? C1' B4 H4' 125.5 . . ? B10 B4 H4' 122.4 . . ? B3 B4 H4' 121.6 . . ? B9 B4 H4' 122.4 . . ? B5 B4 H4' 121.2 . . ? C1' B5 B11 103.3(3) . . ? C1' B5 B6 58.6(3) . . ? B11 B5 B6 59.7(3) . . ? C1' B5 B4 58.2(3) . . ? B11 B5 B4 107.7(3) . . ? B6 B5 B4 108.1(4) . . ? C1' B5 B10 103.5(3) . . ? B11 B5 B10 60.3(3) . . ? B6 B5 B10 108.3(3) . . ? B4 B5 B10 59.7(3) . . ? C1' B5 H5' 125.9 . . ? B11 B5 H5' 122.8 . . ? B6 B5 H5' 121.2 . . ? B4 B5 H5' 121.6 . . ? B10 B5 H5' 122.5 . . ? C1' B6 B11 103.3(3) . . ? C1' B6 B5 58.4(3) . . ? B11 B6 B5 59.8(3) . . ? C1' B6 B7 103.6(3) . . ? B11 B6 B7 60.2(3) . . ? B5 B6 B7 108.2(3) . . ? C1' B6 B2 58.3(3) . . ? B11 B6 B2 107.2(3) . . ? B5 B6 B2 107.8(3) . . ? B7 B6 B2 59.4(3) . . ? C1' B6 H6' 125.7 . . ? B11 B6 H6' 123.0 . . ? B5 B6 H6' 121.3 . . ? B7 B6 H6' 122.5 . . ? B2 B6 H6' 121.9 . . ? B2 B7 B11 107.3(3) . . ? B2 B7 B6 60.5(3) . . ? B11 B7 B6 59.3(3) . . ? B2 B7 B12 106.7(3) . . ? B11 B7 B12 59.7(3) . . ? B6 B7 B12 107.1(3) . . ? B2 B7 B8 59.8(3) . . ? B11 B7 B8 107.5(3) . . ? B6 B7 B8 108.3(3) . . ? B12 B7 B8 59.3(3) . . ? B2 B7 Br7 124.1(3) . . ? B11 B7 Br7 120.8(3) . . ? B6 B7 Br7 122.6(3) . . ? B12 B7 Br7 120.9(3) . . ? B8 B7 Br7 122.1(3) . . ? B12 B8 B2 106.8(3) . . ? B12 B8 B3 106.5(3) . . ? B2 B8 B3 59.9(3) . . ? B12 B8 B9 59.7(3) . . ? B2 B8 B9 107.4(3) . . ? B3 B8 B9 59.3(3) . . ? B12 B8 B7 60.0(3) . . ? B2 B8 B7 59.3(3) . . ? B3 B8 B7 107.2(3) . . ? B9 B8 B7 107.9(3) . . ? B12 B8 Br8 123.7(3) . . ? B2 B8 Br8 120.6(3) . . ? B3 B8 Br8 122.2(3) . . ? B9 B8 Br8 123.4(3) . . ? B7 B8 Br8 121.1(3) . . ? B3 B9 B12 107.2(3) . . ? B3 B9 B4 60.1(3) . . ? B12 B9 B4 107.1(3) . . ? B3 B9 B10 107.8(3) . . ? B12 B9 B10 59.6(3) . . ? B4 B9 B10 59.7(3) . . ? B3 B9 B8 60.2(3) . . ? B12 B9 B8 59.7(3) . . ? B4 B9 B8 108.3(3) . . ? B10 B9 B8 108.0(3) . . ? B3 B9 Br9 122.1(3) . . ? B12 B9 Br9 122.7(3) . . ? B4 B9 Br9 121.3(3) . . ? B10 B9 Br9 121.2(3) . . ? B8 B9 Br9 122.2(3) . . ? B12 B10 B4 107.4(3) . . ? B12 B10 B11 59.9(3) . . ? B4 B10 B11 107.2(3) . . ? B12 B10 B5 107.4(3) . . ? B4 B10 B5 60.1(3) . . ? B11 B10 B5 59.3(3) . . ? B12 B10 B9 59.8(3) . . ? B4 B10 B9 59.9(3) . . ? B11 B10 B9 107.7(3) . . ? B5 B10 B9 108.1(3) . . ? B12 B10 Br10 118.5(3) . . ? B4 B10 Br10 126.4(3) . . ? B11 B10 Br10 118.7(3) . . ? B5 B10 Br10 123.2(3) . . ? B9 B10 Br10 122.8(3) . . ? B6 B11 B5 60.5(3) . . ? B6 B11 B12 108.5(3) . . ? B5 B11 B12 108.1(3) . . ? B6 B11 B7 60.5(3) . . ? B5 B11 B7 109.2(3) . . ? B12 B11 B7 60.4(3) . . ? B6 B11 B10 109.0(3) . . ? B5 B11 B10 60.4(3) . . ? B12 B11 B10 59.7(3) . . ? B7 B11 B10 108.9(3) . . ? B6 B11 Br11 123.5(3) . . ? B5 B11 Br11 122.4(3) . . ? B12 B11 Br11 119.7(3) . . ? B7 B11 Br11 121.2(3) . . ? B10 B11 Br11 119.6(3) . . ? B10 B12 B9 60.6(3) . . ? B10 B12 B8 109.5(3) . . ? B9 B12 B8 60.6(3) . . ? B10 B12 B11 60.4(3) . . ? B9 B12 B11 108.7(3) . . ? B8 B12 B11 108.8(3) . . ? B10 B12 B7 109.0(3) . . ? B9 B12 B7 109.2(3) . . ? B8 B12 B7 60.7(3) . . ? B11 B12 B7 59.9(3) . . ? B10 B12 Br12 118.7(3) . . ? B9 B12 Br12 123.2(3) . . ? B8 B12 Br12 124.3(3) . . ? B11 B12 Br12 118.1(3) . . ? B7 B12 Br12 121.0(3) . . ? B10 Br10 Rh 92.88(14) . . ? B11 Br11 Rh 97.21(14) . . ? B12 Br12 Rh 97.36(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.021 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.113