# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email gxjin@fudan.edu.cn _publ_author_name 'Guo-Xin Jin' data_f90804c _database_code_depnum_ccdc_archive 'CCDC 770836' #TrackingRef '1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H47 B9 Cl3 Ir P2' _chemical_formula_weight 949.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.584(4) _cell_length_b 11.279(4) _cell_length_c 18.270(6) _cell_angle_alpha 76.059(4) _cell_angle_beta 74.745(4) _cell_angle_gamma 84.583(4) _cell_volume 2041.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 993 _cell_measurement_theta_min 2.538 _cell_measurement_theta_max 26.540 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 3.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6737 _exptl_absorpt_correction_T_max 0.7164 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.77 _diffrn_reflns_number 9254 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7782 _reflns_number_gt 6461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^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_number_reflns 7782 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir -0.02069(2) 0.87227(2) 0.712529(13) 0.03324(9) Uani 1 1 d . . . Cl1 Cl 0.08923(15) 0.94362(15) 0.57984(9) 0.0445(4) Uani 1 1 d . . . P1 P 0.17770(13) 0.87653(13) 0.74133(8) 0.0304(3) Uani 1 1 d . . . P2 P -0.05442(13) 1.06776(13) 0.73345(9) 0.0329(3) Uani 1 1 d . . . B1 B 0.3220(7) 1.2575(6) 0.6611(5) 0.0451(17) Uani 1 1 d . . . H1 H 0.3831 1.3167 0.6096 0.054 Uiso 1 1 calc R . . B2 B 0.3653(7) 1.1028(6) 0.6921(4) 0.0415(16) Uani 1 1 d . . . H2 H 0.4536 1.0599 0.6602 0.050 Uiso 1 1 calc R . . B3 B 0.2263(6) 1.1446(6) 0.6533(4) 0.0382(15) Uani 1 1 d . . . H3 H 0.2218 1.1271 0.5973 0.046 Uiso 1 1 calc R . . B4 B 0.1507(7) 1.2755(6) 0.6843(4) 0.0416(16) Uani 1 1 d . . . H4 H 0.0993 1.3440 0.6475 0.050 Uiso 1 1 calc R . . B5 B 0.2388(7) 1.3124(7) 0.7447(5) 0.0454(17) Uani 1 1 d . . . H5 H 0.2446 1.4080 0.7473 0.054 Uiso 1 1 calc R . . B6 B 0.3737(7) 1.2038(7) 0.7493(5) 0.0470(18) Uani 1 1 d . . . H6 H 0.4692 1.2260 0.7551 0.056 Uiso 1 1 calc R . . B9 B 0.0939(7) 1.2331(7) 0.7875(4) 0.0430(17) Uani 1 1 d . . . H9 H 0.006(5) 1.273(5) 0.816(3) 0.028(14) Uiso 1 1 d . . . B10 B 0.2340(8) 1.1975(7) 0.8293(5) 0.0449(17) Uani 1 1 d . . . H10A H 0.243(6) 1.219(6) 0.875(4) 0.052(19) Uiso 1 1 d . . . H10B H 0.178(6) 1.109(6) 0.836(4) 0.06(2) Uiso 1 1 d . . . B11 B 0.3053(7) 1.0607(7) 0.7953(5) 0.0442(17) Uani 1 1 d . . . H11' H 0.351(5) 0.997(5) 0.824(3) 0.032(14) Uiso 1 1 d . . . C1 C 0.3104(5) 0.8061(5) 0.6771(3) 0.0344(13) Uani 1 1 d . . . C2 C 0.3787(6) 0.8708(6) 0.6046(3) 0.0399(14) Uani 1 1 d . . . H2A H 0.3631 0.9545 0.5892 0.048 Uiso 1 1 calc R . . C3 C 0.4691(6) 0.8110(6) 0.5557(4) 0.0506(17) Uani 1 1 d . . . H3A H 0.5159 0.8556 0.5081 0.061 Uiso 1 1 calc R . . C4 C 0.4921(6) 0.6864(7) 0.5756(4) 0.0548(18) Uani 1 1 d . . . H4A H 0.5539 0.6472 0.5420 0.066 Uiso 1 1 calc R . . C5 C 0.4224(7) 0.6216(6) 0.6456(4) 0.0558(18) Uani 1 1 d . . . H5A H 0.4357 0.5373 0.6592 0.067 Uiso 1 1 calc R . . C6 C 0.3321(6) 0.6802(6) 0.6965(4) 0.0474(16) Uani 1 1 d . . . H6A H 0.2856 0.6348 0.7439 0.057 Uiso 1 1 calc R . . C7 C 0.2182(5) 1.0326(5) 0.7386(3) 0.0334(12) Uani 1 1 d . . . C8 C 0.0976(5) 1.1324(5) 0.7366(3) 0.0325(12) Uani 1 1 d . . . C9 C 0.1867(6) 0.7945(5) 0.8390(3) 0.0383(13) Uani 1 1 d . . . C10 C 0.3043(6) 0.7481(6) 0.8573(4) 0.0480(16) Uani 1 1 d . . . H10 H 0.3816 0.7552 0.8181 0.058 Uiso 1 1 calc R . . C11 C 0.3072(8) 0.6925(7) 0.9318(4) 0.065(2) Uani 1 1 d . . . H11 H 0.3861 0.6598 0.9425 0.079 Uiso 1 1 calc R . . C12 C 0.1958(10) 0.6842(7) 0.9911(5) 0.075(2) Uani 1 1 d . . . H12 H 0.1995 0.6486 1.0420 0.091 Uiso 1 1 calc R . . C13 C 0.0788(9) 0.7285(8) 0.9749(4) 0.072(2) Uani 1 1 d . . . H13 H 0.0019 0.7208 1.0144 0.086 Uiso 1 1 calc R . . C14 C 0.0765(6) 0.7846(6) 0.8992(4) 0.0499(16) Uani 1 1 d . . . H14 H -0.0027 0.8169 0.8888 0.060 Uiso 1 1 calc R . . C15 C -0.1326(5) 1.1818(5) 0.6678(3) 0.0380(13) Uani 1 1 d . . . C16 C -0.1696(6) 1.2959(6) 0.6839(4) 0.0464(15) Uani 1 1 d . . . H16 H -0.1500 1.3166 0.7258 0.056 Uiso 1 1 calc R . . C17 C -0.2364(7) 1.3792(7) 0.6366(5) 0.0600(19) Uani 1 1 d . . . H17 H -0.2580 1.4570 0.6458 0.072 Uiso 1 1 calc R . . C18 C -0.2708(8) 1.3482(8) 0.5766(5) 0.069(2) Uani 1 1 d . . . H18 H -0.3194 1.4032 0.5471 0.082 Uiso 1 1 calc R . . C19 C -0.2337(7) 1.2366(8) 0.5605(4) 0.064(2) Uani 1 1 d . . . H19 H -0.2548 1.2164 0.5188 0.076 Uiso 1 1 calc R . . C20 C -0.1633(6) 1.1514(6) 0.6064(4) 0.0479(16) Uani 1 1 d . . . H20 H -0.1380 1.0752 0.5952 0.057 Uiso 1 1 calc R . . C21 C -0.1660(6) 1.0735(5) 0.8281(3) 0.0396(14) Uani 1 1 d . . . C22 C -0.1209(7) 1.0408(6) 0.8953(4) 0.0553(18) Uani 1 1 d . . . H22 H -0.0322 1.0222 0.8914 0.066 Uiso 1 1 calc R . . C23 C -0.2039(9) 1.0354(8) 0.9667(5) 0.074(2) Uani 1 1 d . . . H23 H -0.1720 1.0123 1.0110 0.089 Uiso 1 1 calc R . . C24 C -0.3351(10) 1.0640(9) 0.9735(5) 0.084(3) Uani 1 1 d . . . H24 H -0.3919 1.0608 1.0224 0.101 Uiso 1 1 calc R . . C25 C -0.3817(8) 1.0975(8) 0.9076(6) 0.081(3) Uani 1 1 d . . . H25 H -0.4703 1.1172 0.9121 0.097 Uiso 1 1 calc R . . C26 C -0.2980(6) 1.1022(6) 0.8345(4) 0.0522(17) Uani 1 1 d . . . H26 H -0.3302 1.1244 0.7902 0.063 Uiso 1 1 calc R . . C27 C -0.0751(6) 0.6772(6) 0.7742(4) 0.0467(16) Uani 1 1 d . . . C28 C -0.1810(6) 0.7616(6) 0.7989(4) 0.0514(17) Uani 1 1 d . . . C29 C -0.2304(6) 0.8199(7) 0.7316(5) 0.059(2) Uani 1 1 d . . . C30 C -0.1530(6) 0.7756(5) 0.6684(4) 0.0494(17) Uani 1 1 d . . . C31 C -0.0539(6) 0.6906(5) 0.6935(4) 0.0464(15) Uani 1 1 d . . . C32 C -0.0158(7) 0.5798(6) 0.8267(4) 0.0558(18) Uani 1 1 d . . . H32A H -0.0617 0.5056 0.8379 0.084 Uiso 1 1 calc R . . H32B H -0.0220 0.6044 0.8744 0.084 Uiso 1 1 calc R . . H32C H 0.0746 0.5665 0.8019 0.084 Uiso 1 1 calc R . . C33 C -0.2518(7) 0.7635(8) 0.8816(4) 0.071(2) Uani 1 1 d . . . H33A H -0.2669 0.8466 0.8869 0.107 Uiso 1 1 calc R . . H33B H -0.1994 0.7206 0.9159 0.107 Uiso 1 1 calc R . . H33C H -0.3341 0.7247 0.8946 0.107 Uiso 1 1 calc R . . C34 C -0.3534(6) 0.8976(7) 0.7312(6) 0.077(3) Uani 1 1 d . . . H34A H -0.3456 0.9510 0.6808 0.115 Uiso 1 1 calc R . . H34B H -0.3668 0.9453 0.7697 0.115 Uiso 1 1 calc R . . H34C H -0.4266 0.8461 0.7429 0.115 Uiso 1 1 calc R . . C35 C -0.1741(8) 0.8028(8) 0.5869(5) 0.070(2) Uani 1 1 d . . . H35A H -0.2255 0.7402 0.5826 0.105 Uiso 1 1 calc R . . H35B H -0.0908 0.8048 0.5496 0.105 Uiso 1 1 calc R . . H35C H -0.2193 0.8806 0.5769 0.105 Uiso 1 1 calc R . . C36 C 0.0391(7) 0.6161(6) 0.6436(5) 0.064(2) Uani 1 1 d . . . H36A H -0.0060 0.5489 0.6395 0.095 Uiso 1 1 calc R . . H36B H 0.1108 0.5853 0.6666 0.095 Uiso 1 1 calc R . . H36C H 0.0720 0.6664 0.5926 0.095 Uiso 1 1 calc R . . C37 C 0.5074(14) 0.4263(10) 0.8386(6) 0.132(5) Uani 1 1 d . . . H37A H 0.4360 0.4595 0.8148 0.159 Uiso 1 1 calc R . . H37B H 0.5425 0.3538 0.8195 0.159 Uiso 1 1 calc R . . Cl2 Cl 0.4469(4) 0.3850(3) 0.9347(2) 0.1388(12) Uani 1 1 d . . . Cl3 Cl 0.6286(3) 0.5326(3) 0.8082(2) 0.1430(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02715(12) 0.02628(13) 0.04485(15) -0.00374(9) -0.00987(9) -0.00231(8) Cl1 0.0430(8) 0.0470(9) 0.0426(8) -0.0058(7) -0.0126(7) -0.0022(7) P1 0.0259(7) 0.0258(7) 0.0364(8) -0.0014(6) -0.0073(6) -0.0013(5) P2 0.0273(7) 0.0291(8) 0.0416(8) -0.0042(6) -0.0110(6) -0.0005(6) B1 0.042(4) 0.030(4) 0.058(5) -0.001(3) -0.010(3) -0.009(3) B2 0.032(3) 0.035(4) 0.055(4) -0.007(3) -0.006(3) -0.009(3) B3 0.036(3) 0.029(4) 0.043(4) -0.001(3) -0.005(3) -0.001(3) B4 0.042(4) 0.023(3) 0.058(4) -0.005(3) -0.014(3) -0.001(3) B5 0.044(4) 0.034(4) 0.061(5) -0.009(3) -0.016(4) -0.005(3) B6 0.040(4) 0.042(4) 0.060(5) -0.007(3) -0.016(3) -0.012(3) B9 0.040(4) 0.037(4) 0.051(4) -0.013(3) -0.006(3) -0.004(3) B10 0.053(4) 0.042(4) 0.047(4) -0.011(3) -0.020(4) -0.007(3) B11 0.043(4) 0.039(4) 0.054(5) -0.004(3) -0.023(4) -0.005(3) C1 0.028(3) 0.031(3) 0.043(3) -0.007(2) -0.009(2) 0.002(2) C2 0.041(3) 0.033(3) 0.043(3) -0.004(3) -0.010(3) -0.002(3) C3 0.045(4) 0.056(4) 0.043(4) -0.006(3) 0.001(3) -0.006(3) C4 0.045(4) 0.054(4) 0.060(4) -0.022(3) 0.002(3) 0.007(3) C5 0.052(4) 0.039(4) 0.072(5) -0.017(3) -0.008(4) 0.012(3) C6 0.042(3) 0.035(4) 0.056(4) -0.001(3) -0.005(3) -0.003(3) C7 0.023(3) 0.027(3) 0.045(3) 0.001(2) -0.009(2) 0.000(2) C8 0.026(3) 0.029(3) 0.039(3) -0.004(2) -0.006(2) -0.002(2) C9 0.041(3) 0.029(3) 0.042(3) 0.000(2) -0.013(3) -0.003(2) C10 0.044(3) 0.042(4) 0.056(4) -0.002(3) -0.018(3) 0.004(3) C11 0.082(6) 0.053(5) 0.065(5) -0.001(4) -0.039(5) 0.004(4) C12 0.112(7) 0.058(5) 0.051(5) 0.009(4) -0.026(5) -0.013(5) C13 0.086(6) 0.078(6) 0.047(4) -0.003(4) -0.012(4) -0.019(5) C14 0.046(4) 0.053(4) 0.045(4) -0.004(3) -0.006(3) -0.010(3) C15 0.030(3) 0.034(3) 0.048(4) -0.002(3) -0.012(3) 0.001(2) C16 0.044(3) 0.036(4) 0.059(4) -0.010(3) -0.017(3) 0.006(3) C17 0.060(4) 0.041(4) 0.080(5) -0.011(4) -0.026(4) 0.015(3) C18 0.068(5) 0.067(5) 0.073(5) -0.011(4) -0.036(4) 0.027(4) C19 0.064(5) 0.077(6) 0.057(4) -0.021(4) -0.032(4) 0.028(4) C20 0.041(3) 0.047(4) 0.059(4) -0.015(3) -0.020(3) 0.012(3) C21 0.038(3) 0.033(3) 0.045(3) -0.008(3) -0.003(3) -0.003(3) C22 0.061(4) 0.051(4) 0.048(4) -0.003(3) -0.008(3) -0.010(3) C23 0.094(7) 0.071(6) 0.051(5) -0.007(4) -0.008(4) -0.025(5) C24 0.093(7) 0.085(7) 0.055(5) -0.019(5) 0.030(5) -0.036(5) C25 0.053(5) 0.061(5) 0.109(7) -0.025(5) 0.021(5) -0.011(4) C26 0.037(3) 0.044(4) 0.066(4) -0.011(3) 0.001(3) 0.000(3) C27 0.036(3) 0.031(3) 0.066(4) 0.002(3) -0.008(3) -0.013(3) C28 0.033(3) 0.037(4) 0.072(5) 0.000(3) -0.001(3) -0.012(3) C29 0.028(3) 0.057(5) 0.090(6) -0.001(4) -0.020(4) -0.014(3) C30 0.044(4) 0.021(3) 0.083(5) -0.005(3) -0.021(4) -0.003(3) C31 0.047(4) 0.023(3) 0.067(4) -0.003(3) -0.014(3) -0.008(3) C32 0.056(4) 0.037(4) 0.070(5) 0.002(3) -0.019(4) -0.003(3) C33 0.050(4) 0.072(6) 0.075(5) -0.006(4) 0.011(4) -0.024(4) C34 0.033(4) 0.060(5) 0.140(8) -0.022(5) -0.027(4) 0.002(3) C35 0.076(5) 0.067(5) 0.079(6) -0.010(4) -0.043(4) -0.011(4) C36 0.069(5) 0.038(4) 0.087(5) -0.026(4) -0.014(4) 0.001(3) C37 0.237(15) 0.082(8) 0.108(8) -0.006(6) -0.091(9) -0.051(9) Cl2 0.181(3) 0.106(3) 0.117(2) -0.0207(19) -0.024(2) 0.006(2) Cl3 0.127(3) 0.136(3) 0.178(3) -0.078(3) -0.005(2) -0.052(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C28 2.229(6) . ? Ir1 C31 2.233(6) . ? Ir1 C30 2.259(7) . ? Ir1 C29 2.267(6) . ? Ir1 C27 2.268(6) . ? Ir1 P1 2.3025(15) . ? Ir1 P2 2.3066(17) . ? Ir1 Cl1 2.3730(16) . ? P1 C9 1.824(6) . ? P1 C1 1.830(6) . ? P1 C7 1.837(6) . ? P2 C21 1.831(6) . ? P2 C15 1.833(6) . ? P2 C8 1.848(6) . ? B1 B4 1.753(10) . ? B1 B3 1.754(10) . ? B1 B2 1.756(10) . ? B1 B5 1.770(11) . ? B1 B6 1.787(11) . ? B2 C7 1.727(8) . ? B2 B6 1.745(11) . ? B2 B3 1.773(10) . ? B2 B11 1.784(11) . ? B3 C7 1.742(8) . ? B3 C8 1.743(8) . ? B3 B4 1.756(10) . ? B4 C8 1.726(8) . ? B4 B5 1.759(11) . ? B4 B9 1.779(10) . ? B5 B9 1.748(10) . ? B5 B10 1.754(11) . ? B5 B6 1.797(10) . ? B6 B11 1.756(10) . ? B6 B10 1.777(11) . ? B9 C8 1.623(9) . ? B9 B10 1.812(11) . ? B10 B11 1.825(11) . ? B11 C7 1.654(9) . ? C1 C6 1.391(8) . ? C1 C2 1.394(8) . ? C2 C3 1.373(8) . ? C3 C4 1.379(9) . ? C4 C5 1.366(9) . ? C5 C6 1.387(9) . ? C7 C8 1.622(7) . ? C9 C14 1.369(8) . ? C9 C10 1.394(8) . ? C10 C11 1.362(9) . ? C11 C12 1.369(11) . ? C12 C13 1.369(11) . ? C13 C14 1.381(9) . ? C15 C20 1.371(9) . ? C15 C16 1.386(8) . ? C16 C17 1.390(9) . ? C17 C18 1.368(10) . ? C18 C19 1.361(11) . ? C19 C20 1.409(9) . ? C21 C26 1.385(8) . ? C21 C22 1.389(9) . ? C22 C23 1.358(10) . ? C23 C24 1.375(13) . ? C24 C25 1.377(13) . ? C25 C26 1.387(10) . ? C27 C31 1.403(9) . ? C27 C28 1.451(9) . ? C27 C32 1.483(8) . ? C28 C29 1.450(10) . ? C28 C33 1.504(10) . ? C29 C30 1.398(10) . ? C29 C34 1.500(9) . ? C30 C31 1.442(9) . ? C30 C35 1.518(10) . ? C31 C36 1.499(9) . ? C37 Cl2 1.667(12) . ? C37 Cl3 1.729(12) . ? 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 C28 Ir1 C31 62.3(3) . . ? C28 Ir1 C30 61.4(3) . . ? C31 Ir1 C30 37.5(2) . . ? C28 Ir1 C29 37.6(2) . . ? C31 Ir1 C29 62.1(3) . . ? C30 Ir1 C29 36.0(3) . . ? C28 Ir1 C27 37.6(2) . . ? C31 Ir1 C27 36.3(2) . . ? C30 Ir1 C27 61.0(2) . . ? C29 Ir1 C27 62.1(2) . . ? C28 Ir1 P1 119.80(19) . . ? C31 Ir1 P1 112.07(17) . . ? C30 Ir1 P1 148.30(17) . . ? C29 Ir1 P1 157.4(2) . . ? C27 Ir1 P1 99.75(16) . . ? C28 Ir1 P2 106.39(18) . . ? C31 Ir1 P2 162.24(17) . . ? C30 Ir1 P2 125.97(16) . . ? C29 Ir1 P2 100.4(2) . . ? C27 Ir1 P2 140.36(18) . . ? P1 Ir1 P2 85.26(5) . . ? C28 Ir1 Cl1 147.7(2) . . ? C31 Ir1 Cl1 92.38(18) . . ? C30 Ir1 Cl1 86.28(19) . . ? C29 Ir1 Cl1 114.1(2) . . ? C27 Ir1 Cl1 127.02(18) . . ? P1 Ir1 Cl1 87.21(5) . . ? P2 Ir1 Cl1 92.32(6) . . ? C9 P1 C1 103.9(3) . . ? C9 P1 C7 102.6(3) . . ? C1 P1 C7 110.4(3) . . ? C9 P1 Ir1 115.60(19) . . ? C1 P1 Ir1 111.94(19) . . ? C7 P1 Ir1 111.71(17) . . ? C21 P2 C15 101.1(3) . . ? C21 P2 C8 103.8(3) . . ? C15 P2 C8 107.9(3) . . ? C21 P2 Ir1 112.6(2) . . ? C15 P2 Ir1 117.8(2) . . ? C8 P2 Ir1 112.32(18) . . ? B4 B1 B3 60.1(4) . . ? B4 B1 B2 109.1(5) . . ? B3 B1 B2 60.7(4) . . ? B4 B1 B5 59.9(4) . . ? B3 B1 B5 107.5(5) . . ? B2 B1 B5 107.9(5) . . ? B4 B1 B6 108.8(5) . . ? B3 B1 B6 107.6(5) . . ? B2 B1 B6 59.0(4) . . ? B5 B1 B6 60.7(4) . . ? C7 B2 B6 103.4(5) . . ? C7 B2 B1 104.8(5) . . ? B6 B2 B1 61.4(4) . . ? C7 B2 B3 59.7(3) . . ? B6 B2 B3 108.6(5) . . ? B1 B2 B3 59.6(4) . . ? C7 B2 B11 56.2(4) . . ? B6 B2 B11 59.7(4) . . ? B1 B2 B11 107.9(5) . . ? B3 B2 B11 106.6(5) . . ? C7 B3 C8 55.5(3) . . ? C7 B3 B1 104.3(5) . . ? C8 B3 B1 103.2(5) . . ? C7 B3 B4 104.9(5) . . ? C8 B3 B4 59.1(4) . . ? B1 B3 B4 60.0(4) . . ? C7 B3 B2 58.8(3) . . ? C8 B3 B2 102.7(5) . . ? B1 B3 B2 59.7(4) . . ? B4 B3 B2 108.2(5) . . ? C8 B4 B1 103.9(5) . . ? C8 B4 B3 60.1(4) . . ? B1 B4 B3 60.0(4) . . ? C8 B4 B5 100.8(5) . . ? B1 B4 B5 60.5(4) . . ? B3 B4 B5 107.9(5) . . ? C8 B4 B9 55.1(4) . . ? B1 B4 B9 107.5(5) . . ? B3 B4 B9 107.0(5) . . ? B5 B4 B9 59.2(4) . . ? B9 B5 B10 62.3(4) . . ? B9 B5 B4 61.0(4) . . ? B10 B5 B4 112.5(5) . . ? B9 B5 B1 108.2(5) . . ? B10 B5 B1 110.4(5) . . ? B4 B5 B1 59.6(4) . . ? B9 B5 B6 107.8(5) . . ? B10 B5 B6 60.0(4) . . ? B4 B5 B6 108.1(5) . . ? B1 B5 B6 60.1(4) . . ? B2 B6 B11 61.3(4) . . ? B2 B6 B10 112.1(5) . . ? B11 B6 B10 62.2(4) . . ? B2 B6 B1 59.6(4) . . ? B11 B6 B1 107.7(5) . . ? B10 B6 B1 108.6(5) . . ? B2 B6 B5 107.2(5) . . ? B11 B6 B5 106.5(5) . . ? B10 B6 B5 58.8(4) . . ? B1 B6 B5 59.2(4) . . ? C8 B9 B5 105.5(5) . . ? C8 B9 B4 60.8(4) . . ? B5 B9 B4 59.8(4) . . ? C8 B9 B10 106.4(5) . . ? B5 B9 B10 59.0(4) . . ? B4 B9 B10 108.8(5) . . ? B5 B10 B6 61.2(4) . . ? B5 B10 B9 58.7(4) . . ? B6 B10 B9 105.9(5) . . ? B5 B10 B11 105.4(5) . . ? B6 B10 B11 58.3(4) . . ? B9 B10 B11 102.3(5) . . ? C7 B11 B6 106.1(5) . . ? C7 B11 B2 60.2(4) . . ? B6 B11 B2 59.1(4) . . ? C7 B11 B10 107.9(5) . . ? B6 B11 B10 59.5(4) . . ? B2 B11 B10 108.1(5) . . ? C6 C1 C2 118.2(5) . . ? C6 C1 P1 118.8(4) . . ? C2 C1 P1 122.4(4) . . ? C3 C2 C1 120.0(6) . . ? C2 C3 C4 121.6(6) . . ? C5 C4 C3 118.8(6) . . ? C4 C5 C6 120.7(6) . . ? C5 C6 C1 120.6(6) . . ? C8 C7 B11 109.0(5) . . ? C8 C7 B2 110.1(4) . . ? B11 C7 B2 63.6(4) . . ? C8 C7 B3 62.3(3) . . ? B11 C7 B3 114.2(5) . . ? B2 C7 B3 61.5(4) . . ? C8 C7 P1 114.8(4) . . ? B11 C7 P1 121.9(4) . . ? B2 C7 P1 127.0(4) . . ? B3 C7 P1 119.0(4) . . ? C7 C8 B9 114.3(5) . . ? C7 C8 B4 111.8(4) . . ? B9 C8 B4 64.1(4) . . ? C7 C8 B3 62.2(3) . . ? B9 C8 B3 115.2(5) . . ? B4 C8 B3 60.8(4) . . ? C7 C8 P2 113.2(4) . . ? B9 C8 P2 121.3(4) . . ? B4 C8 P2 123.7(4) . . ? B3 C8 P2 116.3(4) . . ? C14 C9 C10 117.2(6) . . ? C14 C9 P1 119.8(5) . . ? C10 C9 P1 122.8(5) . . ? C11 C10 C9 120.8(7) . . ? C10 C11 C12 120.9(7) . . ? C11 C12 C13 119.6(7) . . ? C12 C13 C14 119.1(8) . . ? C9 C14 C13 122.3(7) . . ? C20 C15 C16 120.1(6) . . ? C20 C15 P2 120.1(5) . . ? C16 C15 P2 119.7(5) . . ? C15 C16 C17 119.3(6) . . ? C18 C17 C16 121.0(7) . . ? C19 C18 C17 119.7(7) . . ? C18 C19 C20 120.5(7) . . ? C15 C20 C19 119.4(6) . . ? C26 C21 C22 119.0(6) . . ? C26 C21 P2 120.7(5) . . ? C22 C21 P2 120.2(5) . . ? C23 C22 C21 121.2(7) . . ? C22 C23 C24 120.2(8) . . ? C23 C24 C25 119.5(7) . . ? C24 C25 C26 120.8(8) . . ? C21 C26 C25 119.3(7) . . ? C31 C27 C28 108.0(6) . . ? C31 C27 C32 125.7(6) . . ? C28 C27 C32 125.5(6) . . ? C31 C27 Ir1 70.5(3) . . ? C28 C27 Ir1 69.7(3) . . ? C32 C27 Ir1 133.1(4) . . ? C29 C28 C27 107.4(6) . . ? C29 C28 C33 124.4(6) . . ? C27 C28 C33 126.2(6) . . ? C29 C28 Ir1 72.6(3) . . ? C27 C28 Ir1 72.6(3) . . ? C33 C28 Ir1 132.8(5) . . ? C30 C29 C28 107.1(6) . . ? C30 C29 C34 125.5(7) . . ? C28 C29 C34 126.8(7) . . ? C30 C29 Ir1 71.7(4) . . ? C28 C29 Ir1 69.8(3) . . ? C34 C29 Ir1 130.7(5) . . ? C29 C30 C31 109.6(6) . . ? C29 C30 C35 126.3(6) . . ? C31 C30 C35 123.9(7) . . ? C29 C30 Ir1 72.3(4) . . ? C31 C30 Ir1 70.3(4) . . ? C35 C30 Ir1 127.5(5) . . ? C27 C31 C30 107.6(6) . . ? C27 C31 C36 126.9(6) . . ? C30 C31 C36 124.7(7) . . ? C27 C31 Ir1 73.2(4) . . ? C30 C31 Ir1 72.3(4) . . ? C36 C31 Ir1 127.7(5) . . ? Cl2 C37 Cl3 115.2(6) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.076 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.133 # Attachment '1b.cif' data_f90908d _database_code_depnum_ccdc_archive 'CCDC 770837' #TrackingRef '1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H47 B9 Cl3 P2 Rh' _chemical_formula_weight 860.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.556(3) _cell_length_b 11.240(4) _cell_length_c 18.262(6) _cell_angle_alpha 76.758(4) _cell_angle_beta 74.904(4) _cell_angle_gamma 84.873(3) _cell_volume 2035.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 920 _cell_measurement_theta_min 2.689 _cell_measurement_theta_max 27.304 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8689 _exptl_absorpt_correction_T_max 0.9312 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.18 _diffrn_reflns_number 9221 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7761 _reflns_number_gt 6426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^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_number_reflns 7761 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.01929(2) 0.87101(2) 0.710771(14) 0.03134(9) Uani 1 1 d . . . Cl1 Cl 0.09157(8) 0.94271(7) 0.57943(5) 0.04344(19) Uani 1 1 d . . . P1 P 0.17967(7) 0.87611(6) 0.74061(4) 0.02943(17) Uani 1 1 d . . . P2 P -0.05264(7) 1.06717(7) 0.73389(5) 0.03169(17) Uani 1 1 d . . . B1 B 0.3253(3) 1.2566(3) 0.6614(2) 0.0409(8) Uani 1 1 d . . . H1 H 0.3868 1.3152 0.6101 0.049 Uiso 1 1 calc R . . B2 B 0.3665(3) 1.1022(3) 0.6920(2) 0.0389(8) Uani 1 1 d . . . H2 H 0.4544 1.0592 0.6596 0.047 Uiso 1 1 calc R . . B3 B 0.2283(3) 1.1431(3) 0.6535(2) 0.0374(8) Uani 1 1 d . . . H3 H 0.2234 1.1254 0.5975 0.045 Uiso 1 1 calc R . . B4 B 0.1524(3) 1.2743(3) 0.6862(2) 0.0394(8) Uani 1 1 d . . . H4 H 0.1002 1.3428 0.6502 0.047 Uiso 1 1 calc R . . B5 B 0.2403(4) 1.3126(3) 0.7462(2) 0.0436(9) Uani 1 1 d . . . H5 H 0.2455 1.4086 0.7493 0.052 Uiso 1 1 calc R . . B6 B 0.3765(4) 1.2034(3) 0.7504(2) 0.0445(9) Uani 1 1 d . . . H6 H 0.4720 1.2259 0.7566 0.053 Uiso 1 1 calc R . . B9 B 0.0955(4) 1.2319(3) 0.7888(2) 0.0414(8) Uani 1 1 d . . . H9 H -0.002(3) 1.267(3) 0.8165(18) 0.044(9) Uiso 1 1 d . . . B10 B 0.2373(4) 1.1972(4) 0.8303(2) 0.0459(9) Uani 1 1 d . . . H10A H 0.245(3) 1.222(3) 0.881(2) 0.056(10) Uiso 1 1 d . . . H10B H 0.180(3) 1.107(3) 0.839(2) 0.056(10) Uiso 1 1 d . . . B11 B 0.3089(4) 1.0589(4) 0.7952(2) 0.0418(8) Uani 1 1 d . . . H11' H 0.363(3) 0.982(3) 0.8256(19) 0.050(9) Uiso 1 1 d . . . C1 C 0.3119(3) 0.8053(3) 0.67606(17) 0.0329(6) Uani 1 1 d . . . C2 C 0.3802(3) 0.8686(3) 0.60443(18) 0.0374(7) Uani 1 1 d . . . H2A H 0.3650 0.9523 0.5894 0.045 Uiso 1 1 calc R . . C3 C 0.4713(3) 0.8080(3) 0.5549(2) 0.0482(8) Uani 1 1 d . . . H3A H 0.5180 0.8517 0.5073 0.058 Uiso 1 1 calc R . . C4 C 0.4932(3) 0.6845(3) 0.5753(2) 0.0550(9) Uani 1 1 d . . . H4A H 0.5550 0.6448 0.5418 0.066 Uiso 1 1 calc R . . C5 C 0.4243(3) 0.6194(3) 0.6449(2) 0.0535(9) Uani 1 1 d . . . H5A H 0.4378 0.5351 0.6583 0.064 Uiso 1 1 calc R . . C6 C 0.3341(3) 0.6791(3) 0.6956(2) 0.0441(8) Uani 1 1 d . . . H6A H 0.2879 0.6345 0.7430 0.053 Uiso 1 1 calc R . . C7 C 0.2199(3) 1.0331(2) 0.73857(17) 0.0300(6) Uani 1 1 d . . . C8 C 0.1003(3) 1.1301(2) 0.73722(17) 0.0311(6) Uani 1 1 d . . . C9 C 0.1875(3) 0.7941(3) 0.83815(17) 0.0361(7) Uani 1 1 d . . . C10 C 0.3049(3) 0.7471(3) 0.8564(2) 0.0468(8) Uani 1 1 d . . . H10 H 0.3826 0.7529 0.8176 0.056 Uiso 1 1 calc R . . C11 C 0.3060(5) 0.6919(4) 0.9319(2) 0.0639(11) Uani 1 1 d . . . H11 H 0.3846 0.6600 0.9434 0.077 Uiso 1 1 calc R . . C12 C 0.1925(5) 0.6836(4) 0.9903(3) 0.0760(13) Uani 1 1 d . . . H12 H 0.1946 0.6475 1.0412 0.091 Uiso 1 1 calc R . . C13 C 0.0766(5) 0.7288(4) 0.9731(2) 0.0686(11) Uani 1 1 d . . . H13 H -0.0007 0.7218 1.0122 0.082 Uiso 1 1 calc R . . C14 C 0.0742(3) 0.7849(3) 0.89754(19) 0.0485(8) Uani 1 1 d . . . H14 H -0.0048 0.8169 0.8866 0.058 Uiso 1 1 calc R . . C15 C -0.1317(3) 1.1806(3) 0.66955(19) 0.0370(7) Uani 1 1 d . . . C16 C -0.1690(3) 1.2950(3) 0.6856(2) 0.0460(8) Uani 1 1 d . . . H16 H -0.1485 1.3160 0.7275 0.055 Uiso 1 1 calc R . . C17 C -0.2361(4) 1.3777(3) 0.6402(3) 0.0603(10) Uani 1 1 d . . . H17 H -0.2584 1.4552 0.6506 0.072 Uiso 1 1 calc R . . C18 C -0.2703(4) 1.3465(4) 0.5796(3) 0.0665(11) Uani 1 1 d . . . H18 H -0.3189 1.4014 0.5503 0.080 Uiso 1 1 calc R . . C19 C -0.2328(4) 1.2347(4) 0.5624(2) 0.0631(11) Uani 1 1 d . . . H19 H -0.2541 1.2143 0.5206 0.076 Uiso 1 1 calc R . . C20 C -0.1627(3) 1.1511(3) 0.6073(2) 0.0473(8) Uani 1 1 d . . . H20 H -0.1368 1.0752 0.5952 0.057 Uiso 1 1 calc R . . C21 C -0.1635(3) 1.0717(3) 0.82856(19) 0.0393(7) Uani 1 1 d . . . C22 C -0.1179(4) 1.0398(3) 0.8955(2) 0.0518(9) Uani 1 1 d . . . H22 H -0.0292 1.0206 0.8918 0.062 Uiso 1 1 calc R . . C23 C -0.2021(5) 1.0363(4) 0.9669(2) 0.0733(13) Uani 1 1 d . . . H23 H -0.1705 1.0156 1.0113 0.088 Uiso 1 1 calc R . . C24 C -0.3324(5) 1.0631(4) 0.9729(3) 0.0848(16) Uani 1 1 d . . . H24 H -0.3894 1.0594 1.0217 0.102 Uiso 1 1 calc R . . C25 C -0.3808(4) 1.0957(4) 0.9073(3) 0.0697(12) Uani 1 1 d . . . H25 H -0.4697 1.1149 0.9116 0.084 Uiso 1 1 calc R . . C26 C -0.2964(3) 1.0993(3) 0.8361(2) 0.0500(8) Uani 1 1 d . . . H26 H -0.3285 1.1207 0.7919 0.060 Uiso 1 1 calc R . . C27 C -0.0753(3) 0.6769(3) 0.7715(2) 0.0432(8) Uani 1 1 d . . . C28 C -0.1801(3) 0.7607(3) 0.7961(2) 0.0459(8) Uani 1 1 d . . . C29 C -0.2272(3) 0.8181(3) 0.7286(2) 0.0487(9) Uani 1 1 d . . . C30 C -0.1505(3) 0.7749(3) 0.6648(2) 0.0463(8) Uani 1 1 d . . . C31 C -0.0522(3) 0.6895(3) 0.6906(2) 0.0441(8) Uani 1 1 d . . . C32 C -0.0163(4) 0.5783(3) 0.8239(2) 0.0573(9) Uani 1 1 d . . . H32A H -0.0529 0.5014 0.8275 0.086 Uiso 1 1 calc R . . H32B H -0.0352 0.5963 0.8747 0.086 Uiso 1 1 calc R . . H32C H 0.0770 0.5738 0.8033 0.086 Uiso 1 1 calc R . . C33 C -0.2512(4) 0.7630(4) 0.8775(2) 0.0626(10) Uani 1 1 d . . . H33A H -0.2696 0.8462 0.8828 0.094 Uiso 1 1 calc R . . H33B H -0.1979 0.7230 0.9118 0.094 Uiso 1 1 calc R . . H33C H -0.3322 0.7212 0.8905 0.094 Uiso 1 1 calc R . . C34 C -0.3518(3) 0.8955(4) 0.7293(3) 0.0715(13) Uani 1 1 d . . . H34A H -0.3383 0.9603 0.6838 0.107 Uiso 1 1 calc R . . H34B H -0.3749 0.9296 0.7748 0.107 Uiso 1 1 calc R . . H34C H -0.4214 0.8457 0.7298 0.107 Uiso 1 1 calc R . . C35 C -0.1705(4) 0.8027(4) 0.5846(3) 0.0727(12) Uani 1 1 d . . . H35A H -0.2229 0.7410 0.5794 0.109 Uiso 1 1 calc R . . H35B H -0.0869 0.8040 0.5476 0.109 Uiso 1 1 calc R . . H35C H -0.2146 0.8811 0.5751 0.109 Uiso 1 1 calc R . . C36 C 0.0425(4) 0.6166(3) 0.6405(2) 0.0609(10) Uani 1 1 d . . . H36A H -0.0040 0.5566 0.6288 0.091 Uiso 1 1 calc R . . H36B H 0.1067 0.5764 0.6673 0.091 Uiso 1 1 calc R . . H36C H 0.0855 0.6700 0.5931 0.091 Uiso 1 1 calc R . . C37 C 0.5059(7) 0.4255(5) 0.8408(3) 0.115(2) Uani 1 1 d . . . H37A H 0.5400 0.3526 0.8214 0.138 Uiso 1 1 calc R . . H37B H 0.4342 0.4589 0.8174 0.138 Uiso 1 1 calc R . . Cl2 Cl 0.4444(2) 0.38362(15) 0.93857(10) 0.1257(6) Uani 1 1 d . . . Cl3 Cl 0.62626(17) 0.52937(17) 0.81064(12) 0.1390(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02765(13) 0.02719(13) 0.03968(16) -0.00779(10) -0.00878(10) -0.00048(8) Cl1 0.0430(4) 0.0473(5) 0.0393(4) -0.0077(3) -0.0109(3) 0.0005(3) P1 0.0277(4) 0.0261(4) 0.0332(4) -0.0051(3) -0.0069(3) 0.0006(3) P2 0.0272(4) 0.0295(4) 0.0391(4) -0.0090(3) -0.0089(3) 0.0018(3) B1 0.0393(19) 0.0325(18) 0.050(2) -0.0077(16) -0.0074(17) -0.0071(14) B2 0.0293(17) 0.0376(19) 0.050(2) -0.0120(16) -0.0075(16) -0.0025(14) B3 0.0351(18) 0.0347(18) 0.042(2) -0.0077(15) -0.0079(16) -0.0037(14) B4 0.0403(19) 0.0266(17) 0.049(2) -0.0045(15) -0.0109(17) -0.0006(14) B5 0.044(2) 0.0340(19) 0.055(2) -0.0130(17) -0.0105(18) -0.0042(15) B6 0.0372(19) 0.041(2) 0.060(3) -0.0143(18) -0.0161(18) -0.0042(15) B9 0.0387(19) 0.0333(19) 0.053(2) -0.0155(17) -0.0073(17) -0.0003(15) B10 0.053(2) 0.045(2) 0.047(2) -0.0170(18) -0.0168(19) -0.0075(17) B11 0.045(2) 0.041(2) 0.045(2) -0.0117(17) -0.0184(18) 0.0007(16) C1 0.0280(14) 0.0319(15) 0.0402(18) -0.0098(13) -0.0100(13) 0.0022(11) C2 0.0377(16) 0.0348(16) 0.0408(18) -0.0091(13) -0.0106(14) -0.0005(13) C3 0.0419(18) 0.058(2) 0.042(2) -0.0129(16) -0.0031(15) -0.0022(16) C4 0.048(2) 0.057(2) 0.058(2) -0.0264(19) -0.0028(18) 0.0107(17) C5 0.053(2) 0.0387(19) 0.066(3) -0.0193(18) -0.0058(19) 0.0120(16) C6 0.0445(18) 0.0336(17) 0.048(2) -0.0079(14) -0.0027(15) 0.0015(13) C7 0.0291(14) 0.0264(14) 0.0349(16) -0.0053(12) -0.0103(12) -0.0002(11) C8 0.0261(14) 0.0275(14) 0.0393(17) -0.0076(12) -0.0073(12) -0.0008(11) C9 0.0429(17) 0.0289(15) 0.0359(17) -0.0044(12) -0.0112(14) -0.0013(12) C10 0.0492(19) 0.0425(19) 0.048(2) -0.0041(15) -0.0174(16) 0.0047(15) C11 0.084(3) 0.052(2) 0.061(3) -0.0020(19) -0.040(2) 0.007(2) C12 0.117(4) 0.065(3) 0.042(2) 0.006(2) -0.028(3) -0.009(3) C13 0.080(3) 0.079(3) 0.040(2) -0.006(2) -0.003(2) -0.015(2) C14 0.050(2) 0.051(2) 0.042(2) -0.0087(16) -0.0069(16) -0.0043(16) C15 0.0320(15) 0.0347(16) 0.0443(19) -0.0072(13) -0.0124(14) 0.0047(12) C16 0.0451(18) 0.0408(18) 0.053(2) -0.0120(15) -0.0161(16) 0.0091(14) C17 0.061(2) 0.041(2) 0.077(3) -0.0122(19) -0.020(2) 0.0163(17) C18 0.065(3) 0.068(3) 0.067(3) -0.011(2) -0.029(2) 0.027(2) C19 0.066(2) 0.074(3) 0.059(2) -0.021(2) -0.033(2) 0.023(2) C20 0.0416(18) 0.049(2) 0.056(2) -0.0167(16) -0.0181(16) 0.0112(15) C21 0.0385(17) 0.0347(16) 0.0422(19) -0.0120(14) -0.0019(14) -0.0026(13) C22 0.057(2) 0.052(2) 0.045(2) -0.0089(16) -0.0081(18) -0.0127(17) C23 0.094(3) 0.079(3) 0.048(2) -0.014(2) -0.008(2) -0.032(3) C24 0.095(4) 0.078(3) 0.065(3) -0.030(3) 0.034(3) -0.038(3) C25 0.052(2) 0.064(3) 0.077(3) -0.020(2) 0.016(2) -0.0044(19) C26 0.0407(18) 0.045(2) 0.059(2) -0.0116(17) -0.0009(17) -0.0013(14) C27 0.0408(17) 0.0288(16) 0.059(2) -0.0065(14) -0.0101(16) -0.0069(13) C28 0.0374(17) 0.0370(18) 0.059(2) -0.0099(15) -0.0031(16) -0.0085(13) C29 0.0320(16) 0.0386(18) 0.078(3) -0.0104(17) -0.0171(17) -0.0064(13) C30 0.0427(18) 0.0379(18) 0.063(2) -0.0076(16) -0.0228(17) -0.0083(14) C31 0.0466(18) 0.0319(16) 0.057(2) -0.0109(15) -0.0158(16) -0.0076(13) C32 0.063(2) 0.0341(18) 0.069(3) 0.0029(17) -0.016(2) -0.0055(16) C33 0.049(2) 0.061(2) 0.067(3) -0.013(2) 0.0077(19) -0.0187(18) C34 0.0317(18) 0.057(2) 0.126(4) -0.017(2) -0.022(2) 0.0012(16) C35 0.080(3) 0.071(3) 0.082(3) -0.012(2) -0.046(3) -0.016(2) C36 0.070(2) 0.042(2) 0.076(3) -0.0265(19) -0.016(2) -0.0015(18) C37 0.183(6) 0.089(4) 0.096(4) -0.021(3) -0.062(4) -0.038(4) Cl2 0.1773(17) 0.0963(11) 0.1004(12) -0.0207(9) -0.0329(11) 0.0068(11) Cl3 0.1196(12) 0.1372(15) 0.1723(17) -0.0864(13) 0.0036(12) -0.0471(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 C31 2.226(3) . ? Rh1 C28 2.227(3) . ? Rh1 C29 2.247(3) . ? Rh1 C30 2.254(3) . ? Rh1 C27 2.263(3) . ? Rh1 P1 2.3114(10) . ? Rh1 P2 2.3181(10) . ? Rh1 Cl1 2.3649(11) . ? P1 C9 1.828(3) . ? P1 C1 1.829(3) . ? P1 C7 1.841(3) . ? P2 C21 1.827(3) . ? P2 C15 1.827(3) . ? P2 C8 1.840(3) . ? B1 B2 1.749(5) . ? B1 B3 1.758(5) . ? B1 B4 1.767(5) . ? B1 B5 1.795(5) . ? B1 B6 1.802(6) . ? B2 C7 1.717(4) . ? B2 B6 1.755(5) . ? B2 B3 1.761(5) . ? B2 B11 1.787(6) . ? B3 C7 1.738(5) . ? B3 C8 1.745(5) . ? B3 B4 1.765(5) . ? B4 C8 1.731(4) . ? B4 B5 1.751(5) . ? B4 B9 1.776(6) . ? B5 B9 1.752(5) . ? B5 B10 1.764(6) . ? B5 B6 1.811(5) . ? B6 B11 1.764(5) . ? B6 B10 1.775(6) . ? B9 C8 1.630(4) . ? B9 B10 1.821(5) . ? B10 B11 1.843(5) . ? B11 C7 1.651(4) . ? C1 C2 1.383(4) . ? C1 C6 1.395(4) . ? C2 C3 1.385(4) . ? C3 C4 1.367(5) . ? C4 C5 1.367(5) . ? C5 C6 1.387(4) . ? C7 C8 1.594(4) . ? C9 C14 1.383(4) . ? C9 C10 1.394(4) . ? C10 C11 1.378(5) . ? C11 C12 1.375(6) . ? C12 C13 1.367(6) . ? C13 C14 1.386(5) . ? C15 C20 1.377(4) . ? C15 C16 1.385(4) . ? C16 C17 1.374(5) . ? C17 C18 1.375(5) . ? C18 C19 1.363(5) . ? C19 C20 1.393(5) . ? C21 C26 1.387(4) . ? C21 C22 1.390(5) . ? C22 C23 1.367(6) . ? C23 C24 1.362(7) . ? C24 C25 1.385(7) . ? C25 C26 1.366(5) . ? C27 C31 1.409(5) . ? C27 C28 1.435(4) . ? C27 C32 1.494(5) . ? C28 C29 1.443(5) . ? C28 C33 1.486(5) . ? C29 C30 1.395(5) . ? C29 C34 1.509(5) . ? C30 C31 1.446(5) . ? C30 C35 1.493(5) . ? C31 C36 1.493(5) . ? C37 Cl3 1.699(6) . ? C37 Cl2 1.701(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 C31 Rh1 C28 62.47(13) . . ? C31 Rh1 C29 61.92(12) . . ? C28 Rh1 C29 37.62(13) . . ? C31 Rh1 C30 37.64(12) . . ? C28 Rh1 C30 61.93(13) . . ? C29 Rh1 C30 36.11(13) . . ? C31 Rh1 C27 36.59(12) . . ? C28 Rh1 C27 37.28(12) . . ? C29 Rh1 C27 61.61(12) . . ? C30 Rh1 C27 61.35(12) . . ? C31 Rh1 P1 112.17(9) . . ? C28 Rh1 P1 119.71(10) . . ? C29 Rh1 P1 157.32(10) . . ? C30 Rh1 P1 148.45(9) . . ? C27 Rh1 P1 100.00(8) . . ? C31 Rh1 P2 162.56(9) . . ? C28 Rh1 P2 106.15(9) . . ? C29 Rh1 P2 100.85(9) . . ? C30 Rh1 P2 126.29(9) . . ? C27 Rh1 P2 139.66(9) . . ? P1 Rh1 P2 84.75(3) . . ? C31 Rh1 Cl1 92.71(10) . . ? C28 Rh1 Cl1 148.09(9) . . ? C29 Rh1 Cl1 114.35(10) . . ? C30 Rh1 Cl1 86.15(10) . . ? C27 Rh1 Cl1 127.69(9) . . ? P1 Rh1 Cl1 87.09(3) . . ? P2 Rh1 Cl1 92.38(3) . . ? C9 P1 C1 104.31(14) . . ? C9 P1 C7 102.96(13) . . ? C1 P1 C7 110.73(13) . . ? C9 P1 Rh1 115.42(10) . . ? C1 P1 Rh1 111.35(9) . . ? C7 P1 Rh1 111.58(9) . . ? C21 P2 C15 101.29(15) . . ? C21 P2 C8 104.21(14) . . ? C15 P2 C8 108.47(14) . . ? C21 P2 Rh1 112.40(10) . . ? C15 P2 Rh1 117.43(10) . . ? C8 P2 Rh1 111.80(9) . . ? B2 B1 B3 60.25(19) . . ? B2 B1 B4 108.2(2) . . ? B3 B1 B4 60.10(19) . . ? B2 B1 B5 107.5(3) . . ? B3 B1 B5 106.9(3) . . ? B4 B1 B5 58.9(2) . . ? B2 B1 B6 59.2(2) . . ? B3 B1 B6 107.3(3) . . ? B4 B1 B6 107.6(3) . . ? B5 B1 B6 60.4(2) . . ? C7 B2 B1 105.3(2) . . ? C7 B2 B6 103.1(3) . . ? B1 B2 B6 61.9(2) . . ? C7 B2 B3 59.95(18) . . ? B1 B2 B3 60.1(2) . . ? B6 B2 B3 109.3(3) . . ? C7 B2 B11 56.20(19) . . ? B1 B2 B11 109.1(3) . . ? B6 B2 B11 59.7(2) . . ? B3 B2 B11 107.6(3) . . ? C7 B3 C8 54.50(17) . . ? C7 B3 B1 104.1(2) . . ? C8 B3 B1 103.5(2) . . ? C7 B3 B2 58.78(19) . . ? C8 B3 B2 102.1(2) . . ? B1 B3 B2 59.6(2) . . ? C7 B3 B4 103.8(2) . . ? C8 B3 B4 59.10(19) . . ? B1 B3 B4 60.2(2) . . ? B2 B3 B4 107.7(2) . . ? C8 B4 B5 101.2(2) . . ? C8 B4 B3 59.85(18) . . ? B5 B4 B3 108.5(3) . . ? C8 B4 B1 103.7(2) . . ? B5 B4 B1 61.3(2) . . ? B3 B4 B1 59.72(19) . . ? C8 B4 B9 55.37(18) . . ? B5 B4 B9 59.6(2) . . ? B3 B4 B9 107.4(3) . . ? B1 B4 B9 108.4(3) . . ? B4 B5 B9 60.9(2) . . ? B4 B5 B10 112.4(3) . . ? B9 B5 B10 62.4(2) . . ? B4 B5 B1 59.8(2) . . ? B9 B5 B1 108.2(2) . . ? B10 B5 B1 110.0(3) . . ? B4 B5 B6 107.9(3) . . ? B9 B5 B6 107.4(3) . . ? B10 B5 B6 59.5(2) . . ? B1 B5 B6 60.0(2) . . ? B2 B6 B11 61.0(2) . . ? B2 B6 B10 112.0(3) . . ? B11 B6 B10 62.8(2) . . ? B2 B6 B1 58.9(2) . . ? B11 B6 B1 107.7(2) . . ? B10 B6 B1 109.2(3) . . ? B2 B6 B5 106.5(3) . . ? B11 B6 B5 107.0(3) . . ? B10 B6 B5 58.9(2) . . ? B1 B6 B5 59.6(2) . . ? C8 B9 B5 105.4(3) . . ? C8 B9 B4 60.9(2) . . ? B5 B9 B4 59.5(2) . . ? C8 B9 B10 106.0(2) . . ? B5 B9 B10 59.1(2) . . ? B4 B9 B10 108.5(3) . . ? B5 B10 B6 61.5(2) . . ? B5 B10 B9 58.5(2) . . ? B6 B10 B9 105.9(3) . . ? B5 B10 B11 105.6(3) . . ? B6 B10 B11 58.3(2) . . ? B9 B10 B11 102.1(2) . . ? C7 B11 B6 105.4(3) . . ? C7 B11 B2 59.75(19) . . ? B6 B11 B2 59.2(2) . . ? C7 B11 B10 106.8(3) . . ? B6 B11 B10 58.9(2) . . ? B2 B11 B10 107.4(3) . . ? C2 C1 C6 118.2(3) . . ? C2 C1 P1 122.8(2) . . ? C6 C1 P1 118.5(2) . . ? C1 C2 C3 120.4(3) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C1 120.7(3) . . ? C8 C7 B11 110.6(2) . . ? C8 C7 B2 110.7(2) . . ? B11 C7 B2 64.1(2) . . ? C8 C7 B3 62.97(18) . . ? B11 C7 B3 115.3(2) . . ? B2 C7 B3 61.27(19) . . ? C8 C7 P1 114.59(18) . . ? B11 C7 P1 120.7(2) . . ? B2 C7 P1 126.4(2) . . ? B3 C7 P1 118.50(19) . . ? C7 C8 B9 114.4(2) . . ? C7 C8 B4 111.9(2) . . ? B9 C8 B4 63.7(2) . . ? C7 C8 B3 62.54(18) . . ? B9 C8 B3 115.4(2) . . ? B4 C8 B3 61.05(19) . . ? C7 C8 P2 114.35(18) . . ? B9 C8 P2 120.3(2) . . ? B4 C8 P2 123.0(2) . . ? B3 C8 P2 116.5(2) . . ? C14 C9 C10 118.3(3) . . ? C14 C9 P1 119.0(2) . . ? C10 C9 P1 122.6(3) . . ? C11 C10 C9 120.2(4) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 119.6(4) . . ? C12 C13 C14 120.1(4) . . ? C9 C14 C13 121.0(4) . . ? C20 C15 C16 119.0(3) . . ? C20 C15 P2 120.5(2) . . ? C16 C15 P2 120.4(2) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C18 120.3(3) . . ? C19 C18 C17 119.8(3) . . ? C18 C19 C20 120.2(4) . . ? C15 C20 C19 120.1(3) . . ? C26 C21 C22 118.3(3) . . ? C26 C21 P2 121.1(3) . . ? C22 C21 P2 120.5(3) . . ? C23 C22 C21 120.6(4) . . ? C24 C23 C22 120.1(4) . . ? C23 C24 C25 120.7(4) . . ? C26 C25 C24 119.1(4) . . ? C25 C26 C21 121.2(4) . . ? C31 C27 C28 108.5(3) . . ? C31 C27 C32 125.0(3) . . ? C28 C27 C32 125.7(3) . . ? C31 C27 Rh1 70.30(18) . . ? C28 C27 Rh1 70.00(18) . . ? C32 C27 Rh1 133.4(2) . . ? C27 C28 C29 106.8(3) . . ? C27 C28 C33 126.3(3) . . ? C29 C28 C33 124.9(3) . . ? C27 C28 Rh1 72.72(18) . . ? C29 C28 Rh1 71.98(19) . . ? C33 C28 Rh1 133.2(2) . . ? C30 C29 C28 108.7(3) . . ? C30 C29 C34 125.2(4) . . ? C28 C29 C34 125.4(4) . . ? C30 C29 Rh1 72.21(18) . . ? C28 C29 Rh1 70.41(17) . . ? C34 C29 Rh1 130.8(2) . . ? C29 C30 C31 108.2(3) . . ? C29 C30 C35 126.9(3) . . ? C31 C30 C35 124.8(3) . . ? C29 C30 Rh1 71.68(18) . . ? C31 C30 Rh1 70.12(17) . . ? C35 C30 Rh1 127.4(2) . . ? C27 C31 C30 107.6(3) . . ? C27 C31 C36 127.5(3) . . ? C30 C31 C36 124.3(3) . . ? C27 C31 Rh1 73.12(17) . . ? C30 C31 Rh1 72.24(17) . . ? C36 C31 Rh1 126.7(2) . . ? Cl3 C37 Cl2 115.8(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.633 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.077 # Attachment '3b.cif' data_f91107c _database_code_depnum_ccdc_archive 'CCDC 770838' #TrackingRef '3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 B9 P2 Rh' _chemical_formula_weight 738.85 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 P2(1)/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 11.469(4) _cell_length_b 19.555(7) _cell_length_c 17.854(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.924(5) _cell_angle_gamma 90.00 _cell_volume 3869(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 831 _cell_measurement_theta_min 2.641 _cell_measurement_theta_max 24.406 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8311 _exptl_absorpt_correction_T_max 0.9522 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.32 _diffrn_reflns_number 18585 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8205 _reflns_number_gt 4930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^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_number_reflns 8205 _refine_ls_number_parameters 500 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh3 Rh 0.36044(3) 0.237960(17) 0.05073(2) 0.03352(12) Uani 1 1 d . . . P1 P 0.65617(11) 0.25721(7) 0.04637(8) 0.0475(3) Uani 1 1 d . . . P2 P 0.49056(11) 0.08681(6) 0.10971(7) 0.0414(3) Uani 1 1 d . . . B4 B 0.4453(4) 0.3296(3) 0.1110(3) 0.0389(12) Uani 1 1 d . A . H4A H 0.437(4) 0.372(2) 0.073(2) 0.047(12) Uiso 1 1 d . . . B5 B 0.5807(5) 0.3118(3) 0.1854(3) 0.0390(12) Uani 1 1 d . . . H5 H 0.6620 0.3441 0.1993 0.047 Uiso 1 1 calc R A . B6 B 0.5828(4) 0.2191(3) 0.1856(3) 0.0353(11) Uani 1 1 d . A . H6A H 0.660(4) 0.196(2) 0.194(2) 0.037(11) Uiso 1 1 d . . . B7 B 0.3328(5) 0.2035(3) 0.1615(3) 0.0386(12) Uani 1 1 d . A . H7A H 0.243(4) 0.173(2) 0.154(3) 0.053(13) Uiso 1 1 d . . . B8 B 0.3212(5) 0.2963(3) 0.1470(3) 0.0391(12) Uani 1 1 d . A . H8A H 0.232(4) 0.319(3) 0.133(3) 0.071(15) Uiso 1 1 d . . . B9 B 0.4459(4) 0.3355(3) 0.2110(3) 0.0421(13) Uani 1 1 d . A . H9 H 0.4372 0.3856 0.2371 0.051 Uiso 1 1 calc R . . B10 B 0.5400(5) 0.2705(3) 0.2619(3) 0.0426(12) Uani 1 1 d . A . H10A H 0.5970 0.2776 0.3212 0.051 Uiso 1 1 calc R . . B11 B 0.4708(4) 0.1902(3) 0.2339(3) 0.0384(12) Uani 1 1 d . . . H11A H 0.4857 0.1491 0.2774 0.046 Uiso 1 1 calc R A . B12 B 0.3801(5) 0.2629(3) 0.2407(3) 0.0413(12) Uani 1 1 d . A . H12A H 0.3300 0.2666 0.2855 0.050 Uiso 1 1 calc R . . C1 C 0.5464(4) 0.2704(2) 0.1050(3) 0.0354(10) Uani 1 1 d . A . C2 C 0.4574(4) 0.1716(2) 0.1448(2) 0.0337(10) Uani 1 1 d . A . C3 C 0.6251(4) 0.0545(2) 0.1809(3) 0.0494(12) Uani 1 1 d . A . C4 C 0.7284(5) 0.0501(3) 0.1573(4) 0.0676(16) Uani 1 1 d . . . H4 H 0.7276 0.0644 0.1075 0.081 Uiso 1 1 calc R A . C5 C 0.8346(6) 0.0251(3) 0.2046(5) 0.090(2) Uani 1 1 d . A . H5A H 0.9044 0.0230 0.1874 0.108 Uiso 1 1 calc R . . C6 C 0.8346(7) 0.0030(3) 0.2795(5) 0.097(3) Uani 1 1 d . . . H6 H 0.9058 -0.0126 0.3129 0.116 Uiso 1 1 calc R A . C7 C 0.7312(7) 0.0040(3) 0.3033(4) 0.091(2) Uani 1 1 d . A . H7 H 0.7309 -0.0125 0.3521 0.109 Uiso 1 1 calc R . . C8 C 0.6264(6) 0.0298(3) 0.2546(4) 0.0702(16) Uani 1 1 d . . . H8 H 0.5558 0.0307 0.2712 0.084 Uiso 1 1 calc R A . C9 C 0.3755(4) 0.0281(2) 0.1274(3) 0.0459(12) Uani 1 1 d . A . C10 C 0.3171(5) 0.0314(3) 0.1851(3) 0.0616(15) Uani 1 1 d . . . H10 H 0.3299 0.0686 0.2187 0.074 Uiso 1 1 calc R A . C11 C 0.2385(6) -0.0206(3) 0.1939(4) 0.0807(19) Uani 1 1 d . A . H11 H 0.1985 -0.0178 0.2330 0.097 Uiso 1 1 calc R . . C12 C 0.2198(7) -0.0762(3) 0.1449(4) 0.090(2) Uani 1 1 d . . . H12 H 0.1685 -0.1112 0.1515 0.108 Uiso 1 1 calc R A . C13 C 0.2765(6) -0.0797(3) 0.0869(4) 0.0751(18) Uani 1 1 d . A . H13 H 0.2624 -0.1169 0.0532 0.090 Uiso 1 1 calc R . . C14 C 0.3546(5) -0.0290(3) 0.0776(3) 0.0580(14) Uani 1 1 d . . . H14 H 0.3938 -0.0323 0.0381 0.070 Uiso 1 1 calc R A . C15 C 0.8061(4) 0.2663(3) 0.1144(3) 0.0522(13) Uani 1 1 d . A . C16 C 0.8603(5) 0.3274(3) 0.1412(3) 0.0664(15) Uani 1 1 d . . . H16 H 0.8202 0.3682 0.1249 0.080 Uiso 1 1 calc R A . C17 C 0.9758(6) 0.3289(5) 0.1928(4) 0.094(2) Uani 1 1 d . A . H17 H 1.0103 0.3706 0.2116 0.112 Uiso 1 1 calc R . . C18 C 1.0372(6) 0.2702(6) 0.2155(4) 0.103(3) Uani 1 1 d . . . H18 H 1.1139 0.2711 0.2493 0.124 Uiso 1 1 calc R A . C19 C 0.9847(6) 0.2096(5) 0.1879(5) 0.099(3) Uani 1 1 d . A . H19 H 1.0262 0.1690 0.2030 0.119 Uiso 1 1 calc R . . C20 C 0.8701(5) 0.2078(3) 0.1376(4) 0.0743(18) Uani 1 1 d . . . H20 H 0.8362 0.1658 0.1194 0.089 Uiso 1 1 calc R A . C21 C 0.6545(4) 0.3357(3) -0.0116(3) 0.0576(14) Uani 1 1 d . A . C22 C 0.6261(5) 0.4003(3) 0.0060(3) 0.0610(15) Uani 1 1 d . . . H22 H 0.6019 0.4075 0.0512 0.073 Uiso 1 1 calc R A . C23 C 0.6319(6) 0.4546(4) -0.0404(4) 0.091(2) Uani 1 1 d . A . H23 H 0.6106 0.4979 -0.0267 0.109 Uiso 1 1 calc R . . C24 C 0.6681(8) 0.4467(5) -0.1058(6) 0.119(3) Uani 1 1 d . . . H24 H 0.6718 0.4841 -0.1374 0.143 Uiso 1 1 calc R A . C25 C 0.6998(8) 0.3824(6) -0.1256(4) 0.125(4) Uani 1 1 d . A . H25 H 0.7248 0.3765 -0.1707 0.149 Uiso 1 1 calc R . . C26 C 0.6946(5) 0.3261(4) -0.0783(3) 0.0773(18) Uani 1 1 d . . . H26 H 0.7175 0.2830 -0.0911 0.093 Uiso 1 1 calc R A . C27 C 0.1992(4) 0.1826(3) -0.0254(2) 0.055(4) Uani 0.468(11) 1 d PGU A 1 C28 C 0.2953(5) 0.1751(2) -0.0609(2) 0.051(4) Uani 0.468(11) 1 d PGU A 1 C29 C 0.3296(3) 0.2410(3) -0.07972(18) 0.041(3) Uani 0.468(11) 1 d PGU A 1 C30 C 0.2546(4) 0.2892(2) -0.0559(2) 0.048(4) Uani 0.468(11) 1 d PGU A 1 C31 C 0.1741(3) 0.2531(3) -0.0224(2) 0.043(3) Uani 0.468(11) 1 d PGU A 1 C32 C 0.1350(8) 0.1256(5) 0.0038(4) 0.123(8) Uani 0.468(11) 1 d PGU A 1 H32A H 0.1594 0.0825 -0.0130 0.185 Uiso 0.468(11) 1 calc PR A 1 H32B H 0.0494 0.1311 -0.0162 0.185 Uiso 0.468(11) 1 calc PR A 1 H32C H 0.1551 0.1268 0.0595 0.185 Uiso 0.468(11) 1 calc PR A 1 C33 C 0.3512(9) 0.1087(4) -0.0759(4) 0.149(9) Uani 0.468(11) 1 d PGU A 1 H33A H 0.3095 0.0917 -0.1260 0.224 Uiso 0.468(11) 1 calc PR A 1 H33B H 0.3454 0.0760 -0.0369 0.224 Uiso 0.468(11) 1 calc PR A 1 H33C H 0.4346 0.1161 -0.0743 0.224 Uiso 0.468(11) 1 calc PR A 1 C34 C 0.4284(5) 0.2570(7) -0.1183(3) 0.152(9) Uani 0.468(11) 1 d PGU A 1 H34A H 0.3966 0.2556 -0.1735 0.228 Uiso 0.468(11) 1 calc PR A 1 H34B H 0.4917 0.2238 -0.1030 0.228 Uiso 0.468(11) 1 calc PR A 1 H34C H 0.4600 0.3017 -0.1029 0.228 Uiso 0.468(11) 1 calc PR A 1 C35 C 0.2598(9) 0.3655(3) -0.0648(4) 0.120(7) Uani 0.468(11) 1 d PGU A 1 H35A H 0.1852 0.3813 -0.0982 0.180 Uiso 0.468(11) 1 calc PR A 1 H35B H 0.3251 0.3770 -0.0869 0.180 Uiso 0.468(11) 1 calc PR A 1 H35C H 0.2723 0.3867 -0.0149 0.180 Uiso 0.468(11) 1 calc PR A 1 C36 C 0.0785(5) 0.2843(6) 0.0107(3) 0.114(7) Uani 0.468(11) 1 d PGU A 1 H36A H 0.0468 0.3245 -0.0183 0.171 Uiso 0.468(11) 1 calc PR A 1 H36B H 0.1129 0.2964 0.0639 0.171 Uiso 0.468(11) 1 calc PR A 1 H36C H 0.0146 0.2518 0.0076 0.171 Uiso 0.468(11) 1 calc PR A 1 C27' C 0.1716(3) 0.2286(3) -0.02332(19) 0.047(3) Uani 0.532(11) 1 d PGU A 2 C28' C 0.2224(4) 0.2883(2) -0.0469(2) 0.058(4) Uani 0.532(11) 1 d PGU A 2 C29' C 0.3170(4) 0.2679(3) -0.07975(19) 0.055(3) Uani 0.532(11) 1 d PGU A 2 C30' C 0.3245(4) 0.1956(3) -0.0765(2) 0.051(4) Uani 0.532(11) 1 d PGU A 2 C31' C 0.2346(5) 0.17133(19) -0.0416(2) 0.053(4) Uani 0.532(11) 1 d PGU A 2 C32' C 0.0685(4) 0.2264(6) 0.0145(3) 0.093(5) Uani 0.532(11) 1 d PGU A 2 H32D H 0.0950 0.2438 0.0664 0.139 Uiso 0.532(11) 1 calc PR A 2 H32E H 0.0415 0.1801 0.0159 0.139 Uiso 0.532(11) 1 calc PR A 2 H32F H 0.0032 0.2540 -0.0146 0.139 Uiso 0.532(11) 1 calc PR A 2 C33' C 0.1830(9) 0.3607(3) -0.0385(4) 0.097(5) Uani 0.532(11) 1 d PGU A 2 H33D H 0.1495 0.3637 0.0054 0.145 Uiso 0.532(11) 1 calc PR A 2 H33E H 0.1231 0.3738 -0.0845 0.145 Uiso 0.532(11) 1 calc PR A 2 H33F H 0.2512 0.3907 -0.0311 0.145 Uiso 0.532(11) 1 calc PR A 2 C34' C 0.3957(7) 0.3148(6) -0.1124(3) 0.123(7) Uani 0.532(11) 1 d PGU A 2 H34D H 0.4563 0.3347 -0.0707 0.185 Uiso 0.532(11) 1 calc PR A 2 H34E H 0.3471 0.3504 -0.1419 0.185 Uiso 0.532(11) 1 calc PR A 2 H34F H 0.4339 0.2892 -0.1454 0.185 Uiso 0.532(11) 1 calc PR A 2 C35' C 0.4126(7) 0.1522(6) -0.1050(4) 0.103(6) Uani 0.532(11) 1 d PGU A 2 H35D H 0.4779 0.1389 -0.0620 0.154 Uiso 0.532(11) 1 calc PR A 2 H35E H 0.4439 0.1779 -0.1414 0.154 Uiso 0.532(11) 1 calc PR A 2 H35F H 0.3724 0.1121 -0.1300 0.154 Uiso 0.532(11) 1 calc PR A 2 C36' C 0.2104(9) 0.0976(3) -0.0266(4) 0.106(6) Uani 0.532(11) 1 d PGU A 2 H36D H 0.2478 0.0686 -0.0571 0.159 Uiso 0.532(11) 1 calc PR A 2 H36E H 0.1249 0.0896 -0.0405 0.159 Uiso 0.532(11) 1 calc PR A 2 H36F H 0.2430 0.0875 0.0274 0.159 Uiso 0.532(11) 1 calc PR A 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 Rh3 0.03315(18) 0.03755(19) 0.02705(19) 0.00020(16) 0.00270(13) 0.00193(16) P1 0.0430(7) 0.0562(8) 0.0467(8) -0.0045(6) 0.0177(6) 0.0025(6) P2 0.0467(7) 0.0403(7) 0.0381(7) -0.0023(5) 0.0127(6) 0.0036(5) B4 0.037(3) 0.036(3) 0.041(3) -0.005(2) 0.004(2) 0.002(2) B5 0.039(3) 0.037(3) 0.038(3) -0.008(2) 0.004(2) -0.002(2) B6 0.031(3) 0.037(3) 0.037(3) 0.004(2) 0.007(2) 0.005(2) B7 0.042(3) 0.037(3) 0.040(3) 0.004(2) 0.015(2) 0.003(2) B8 0.033(3) 0.040(3) 0.044(3) 0.001(2) 0.008(2) 0.007(2) B9 0.040(3) 0.044(3) 0.041(3) -0.008(2) 0.008(2) 0.006(2) B10 0.042(3) 0.049(3) 0.034(3) -0.007(2) 0.004(2) -0.001(2) B11 0.041(3) 0.040(3) 0.035(3) 0.004(2) 0.010(2) -0.003(2) B12 0.039(3) 0.049(3) 0.036(3) -0.006(2) 0.010(2) -0.001(2) C1 0.032(2) 0.035(2) 0.040(3) -0.0019(19) 0.0104(19) 0.0010(18) C2 0.035(2) 0.035(2) 0.031(3) 0.0050(18) 0.0072(19) 0.0041(18) C3 0.058(3) 0.031(3) 0.055(3) -0.004(2) 0.007(3) 0.005(2) C4 0.055(3) 0.059(4) 0.084(5) -0.007(3) 0.010(3) 0.007(3) C5 0.058(4) 0.077(5) 0.124(7) -0.009(4) 0.004(4) 0.013(3) C6 0.079(5) 0.063(4) 0.119(7) -0.013(4) -0.029(5) 0.026(4) C7 0.118(6) 0.056(4) 0.075(5) 0.008(3) -0.019(4) 0.013(4) C8 0.081(4) 0.055(3) 0.065(4) 0.012(3) 0.002(3) 0.015(3) C9 0.050(3) 0.040(3) 0.045(3) 0.002(2) 0.007(2) 0.000(2) C10 0.088(4) 0.050(3) 0.055(4) -0.007(3) 0.033(3) -0.014(3) C11 0.099(5) 0.077(4) 0.080(5) -0.003(4) 0.047(4) -0.025(4) C12 0.115(6) 0.057(4) 0.103(6) -0.010(4) 0.041(5) -0.033(4) C13 0.099(5) 0.050(4) 0.074(5) -0.019(3) 0.020(4) -0.019(3) C14 0.078(4) 0.043(3) 0.055(4) -0.007(2) 0.021(3) -0.002(3) C15 0.038(2) 0.068(3) 0.054(3) 0.007(3) 0.019(2) 0.004(3) C16 0.046(3) 0.081(4) 0.068(4) 0.005(3) 0.007(3) -0.005(3) C17 0.051(4) 0.144(7) 0.089(5) -0.008(5) 0.023(4) -0.034(4) C18 0.041(4) 0.198(10) 0.075(5) 0.050(6) 0.024(3) 0.020(5) C19 0.056(4) 0.146(8) 0.101(6) 0.052(6) 0.030(4) 0.032(4) C20 0.054(3) 0.089(4) 0.087(5) 0.027(4) 0.031(3) 0.020(3) C21 0.048(3) 0.083(4) 0.039(3) 0.009(3) 0.006(2) -0.011(3) C22 0.061(3) 0.065(4) 0.057(4) 0.017(3) 0.015(3) -0.005(3) C23 0.076(4) 0.096(5) 0.093(6) 0.039(4) 0.008(4) -0.009(4) C24 0.109(7) 0.148(9) 0.093(7) 0.063(7) 0.014(5) -0.029(6) C25 0.109(7) 0.220(11) 0.049(5) 0.021(7) 0.029(4) -0.058(7) C26 0.079(4) 0.105(5) 0.054(4) -0.003(4) 0.030(3) -0.019(4) C27 0.058(8) 0.077(10) 0.020(6) 0.008(7) -0.005(6) -0.020(7) C28 0.063(9) 0.044(7) 0.030(7) -0.012(6) -0.018(7) 0.011(7) C29 0.034(6) 0.077(10) 0.007(5) 0.015(5) -0.003(4) -0.006(6) C30 0.048(7) 0.035(8) 0.042(8) 0.004(6) -0.024(6) 0.010(5) C31 0.041(7) 0.062(8) 0.019(7) -0.008(5) -0.005(5) 0.006(5) C32 0.106(12) 0.117(13) 0.118(13) 0.043(10) -0.025(9) -0.073(10) C33 0.148(15) 0.127(13) 0.142(15) -0.094(11) -0.019(11) 0.040(11) C34 0.154(15) 0.217(19) 0.106(14) -0.025(12) 0.071(12) -0.045(13) C35 0.150(14) 0.078(10) 0.103(12) 0.036(9) -0.022(10) 0.002(10) C36 0.063(9) 0.179(16) 0.100(12) 0.031(11) 0.022(8) 0.064(10) C27' 0.041(7) 0.058(7) 0.040(7) -0.001(5) 0.005(5) 0.004(5) C28' 0.075(8) 0.062(9) 0.036(7) -0.002(6) 0.014(7) 0.017(6) C29' 0.053(7) 0.037(7) 0.056(8) 0.016(5) -0.019(6) -0.003(5) C30' 0.045(6) 0.060(8) 0.041(7) 0.001(6) 0.001(5) 0.009(6) C31' 0.053(7) 0.058(7) 0.039(7) 0.008(6) -0.001(6) -0.018(6) C32' 0.045(6) 0.151(13) 0.084(9) -0.031(8) 0.019(6) -0.021(7) C33' 0.104(10) 0.066(8) 0.090(10) 0.001(7) -0.031(8) 0.040(7) C34' 0.087(9) 0.191(14) 0.084(10) 0.091(10) 0.008(7) -0.025(9) C35' 0.109(10) 0.147(12) 0.053(7) -0.031(8) 0.021(7) 0.061(9) C36' 0.130(12) 0.081(9) 0.079(9) 0.003(7) -0.023(8) -0.051(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 Rh3 B4 2.185(5) . ? Rh3 C2 2.186(4) . ? Rh3 B7 2.188(5) . ? Rh3 C1 2.197(4) . ? Rh3 B8 2.203(5) . ? Rh3 C30 2.217(3) . ? Rh3 C31 2.219(3) . ? Rh3 C27' 2.236(3) . ? Rh3 C28' 2.256(3) . ? Rh3 C29 2.265(3) . ? Rh3 C27 2.269(3) . ? Rh3 C31' 2.296(3) . ? P1 C15 1.841(5) . ? P1 C21 1.848(6) . ? P1 C1 1.851(4) . ? P2 C9 1.837(5) . ? P2 C3 1.840(5) . ? P2 C2 1.847(4) . ? B4 C1 1.661(6) . ? B4 B9 1.789(8) . ? B4 B5 1.799(7) . ? B4 B8 1.826(7) . ? B5 C1 1.605(6) . ? B5 B10 1.751(7) . ? B5 B9 1.784(7) . ? B5 B6 1.811(7) . ? B6 C2 1.709(6) . ? B6 C1 1.716(7) . ? B6 B11 1.813(7) . ? B6 B10 1.857(7) . ? B7 C2 1.655(6) . ? B7 B11 1.786(7) . ? B7 B12 1.801(8) . ? B7 B8 1.832(8) . ? B8 B9 1.760(7) . ? B8 B12 1.761(8) . ? B9 B12 1.753(8) . ? B9 B10 1.760(7) . ? B10 B11 1.772(7) . ? B10 B12 1.781(7) . ? B11 C2 1.600(7) . ? B11 B12 1.783(7) . ? C3 C4 1.359(7) . ? C3 C8 1.398(7) . ? C4 C5 1.380(8) . ? C5 C6 1.405(10) . ? C6 C7 1.359(10) . ? C7 C8 1.384(8) . ? C9 C10 1.366(6) . ? C9 C14 1.409(7) . ? C10 C11 1.396(7) . ? C11 C12 1.376(8) . ? C12 C13 1.360(8) . ? C13 C14 1.376(7) . ? C15 C20 1.366(7) . ? C15 C16 1.373(7) . ? C16 C17 1.406(8) . ? C17 C18 1.353(10) . ? C18 C19 1.361(11) . ? C19 C20 1.389(9) . ? C21 C22 1.361(7) . ? C21 C26 1.396(7) . ? C22 C23 1.360(8) . ? C23 C24 1.346(10) . ? C24 C25 1.378(12) . ? C25 C26 1.398(11) . ? C27 C28 1.4128(17) . ? C27 C31 1.4130(17) . ? C27 C32 1.5018(18) . ? C28 C29 1.4128(17) . ? C28 C33 1.5019(18) . ? C29 C30 1.4130(17) . ? C29 C34 1.5019(18) . ? C30 C31 1.4128(17) . ? C30 C35 1.5018(18) . ? C31 C36 1.5019(18) . ? C27' C28' 1.4165(17) . ? C27' C31' 1.4165(17) . ? C27' C32' 1.5058(18) . ? C28' C29' 1.4166(17) . ? C28' C33' 1.5058(18) . ? C29' C30' 1.4166(17) . ? C29' C34' 1.5056(18) . ? C30' C31' 1.4165(17) . ? C30' C35' 1.5058(18) . ? C31' C36' 1.5058(18) . ? 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 B4 Rh3 C2 91.96(19) . . ? B4 Rh3 B7 87.6(2) . . ? C2 Rh3 B7 44.47(16) . . ? B4 Rh3 C1 44.55(16) . . ? C2 Rh3 C1 65.70(15) . . ? B7 Rh3 C1 92.32(18) . . ? B4 Rh3 B8 49.17(19) . . ? C2 Rh3 B8 82.73(18) . . ? B7 Rh3 B8 49.3(2) . . ? C1 Rh3 B8 82.91(17) . . ? B4 Rh3 C30 97.35(18) . . ? C2 Rh3 C30 170.44(15) . . ? B7 Rh3 C30 137.8(2) . . ? C1 Rh3 C30 120.17(17) . . ? B8 Rh3 C30 105.04(19) . . ? B4 Rh3 C31 114.8(2) . . ? C2 Rh3 C31 138.92(18) . . ? B7 Rh3 C31 103.37(18) . . ? C1 Rh3 C31 154.1(2) . . ? B8 Rh3 C31 91.74(17) . . ? C30 Rh3 C31 37.15(6) . . ? B4 Rh3 C27' 126.8(2) . . ? C2 Rh3 C27' 129.03(17) . . ? B7 Rh3 C27' 99.53(17) . . ? C1 Rh3 C27' 165.28(18) . . ? B8 Rh3 C27' 98.17(18) . . ? C30 Rh3 C27' 45.28(7) . . ? C31 Rh3 C27' 12.4 . . ? B4 Rh3 C28' 99.06(18) . . ? C2 Rh3 C28' 165.77(17) . . ? B7 Rh3 C28' 126.6(2) . . ? C1 Rh3 C28' 128.52(18) . . ? B8 Rh3 C28' 97.66(18) . . ? C30 Rh3 C28' 11.2 . . ? C31 Rh3 C28' 27.1 . . ? C27' Rh3 C28' 36.76(6) . . ? B4 Rh3 C29 114.6(2) . . ? C2 Rh3 C29 136.03(19) . . ? B7 Rh3 C29 156.5(2) . . ? C1 Rh3 C29 108.83(15) . . ? B8 Rh3 C29 141.2(2) . . ? C30 Rh3 C29 36.74(6) . . ? C31 Rh3 C29 61.30(9) . . ? C27' Rh3 C29 61.51(9) . . ? C28' Rh3 C29 45.68(7) . . ? B4 Rh3 C27 151.3(2) . . ? C2 Rh3 C27 110.64(15) . . ? B7 Rh3 C27 96.29(19) . . ? C1 Rh3 C27 162.0(2) . . ? B8 Rh3 C27 114.6(2) . . ? C30 Rh3 C27 61.28(9) . . ? C31 Rh3 C27 36.68(6) . . ? C27' Rh3 C27 24.5 . . ? C28' Rh3 C27 56.20(8) . . ? C29 Rh3 C27 60.57(8) . . ? B4 Rh3 C31' 159.48(17) . . ? C2 Rh3 C31' 108.44(14) . . ? B7 Rh3 C31' 105.3(2) . . ? C1 Rh3 C31' 147.1(2) . . ? B8 Rh3 C31' 129.6(2) . . ? C30 Rh3 C31' 62.36(9) . . ? C31 Rh3 C31' 47.27(7) . . ? C27' Rh3 C31' 36.40(6) . . ? C28' Rh3 C31' 60.45(9) . . ? C29 Rh3 C31' 51.22(7) . . ? C27 Rh3 C31' 15.0 . . ? C15 P1 C21 99.3(2) . . ? C15 P1 C1 105.6(2) . . ? C21 P1 C1 106.9(2) . . ? C9 P2 C3 100.3(2) . . ? C9 P2 C2 106.4(2) . . ? C3 P2 C2 106.4(2) . . ? C1 B4 B9 106.6(4) . . ? C1 B4 B5 55.1(3) . . ? B9 B4 B5 59.6(3) . . ? C1 B4 B8 113.2(4) . . ? B9 B4 B8 58.3(3) . . ? B5 B4 B8 105.9(4) . . ? C1 B4 Rh3 68.1(2) . . ? B9 B4 Rh3 115.5(3) . . ? B5 B4 Rh3 113.3(3) . . ? B8 B4 Rh3 65.9(2) . . ? C1 B5 B10 114.4(4) . . ? C1 B5 B9 109.4(4) . . ? B10 B5 B9 59.7(3) . . ? C1 B5 B4 58.1(3) . . ? B10 B5 B4 108.2(4) . . ? B9 B5 B4 59.9(3) . . ? C1 B5 B6 59.9(3) . . ? B10 B5 B6 62.8(3) . . ? B9 B5 B6 105.7(4) . . ? B4 B5 B6 101.8(3) . . ? C2 B6 C1 87.9(3) . . ? C2 B6 B5 122.2(4) . . ? C1 B6 B5 54.1(3) . . ? C2 B6 B11 54.0(3) . . ? C1 B6 B11 122.2(3) . . ? B5 B6 B11 107.6(3) . . ? C2 B6 B10 104.7(3) . . ? C1 B6 B10 104.2(3) . . ? B5 B6 B10 57.0(3) . . ? B11 B6 B10 57.7(3) . . ? C2 B7 B11 55.3(3) . . ? C2 B7 B12 106.5(4) . . ? B11 B7 B12 59.6(3) . . ? C2 B7 B8 112.5(4) . . ? B11 B7 B8 105.4(4) . . ? B12 B7 B8 58.0(3) . . ? C2 B7 Rh3 67.7(2) . . ? B11 B7 Rh3 113.1(3) . . ? B12 B7 Rh3 115.3(3) . . ? B8 B7 Rh3 65.8(2) . . ? B9 B8 B12 59.7(3) . . ? B9 B8 B4 59.8(3) . . ? B12 B8 B4 108.9(4) . . ? B9 B8 B7 108.8(4) . . ? B12 B8 B7 60.1(3) . . ? B4 B8 B7 111.6(3) . . ? B9 B8 Rh3 115.9(3) . . ? B12 B8 Rh3 116.3(3) . . ? B4 B8 Rh3 64.9(2) . . ? B7 B8 Rh3 64.9(2) . . ? B12 B9 B8 60.2(3) . . ? B12 B9 B10 60.9(3) . . ? B8 B9 B10 108.0(4) . . ? B12 B9 B5 109.7(4) . . ? B8 B9 B5 109.5(4) . . ? B10 B9 B5 59.2(3) . . ? B12 B9 B4 111.0(4) . . ? B8 B9 B4 61.9(3) . . ? B10 B9 B4 108.3(4) . . ? B5 B9 B4 60.5(3) . . ? B5 B10 B9 61.1(3) . . ? B5 B10 B11 112.2(4) . . ? B9 B10 B11 108.9(4) . . ? B5 B10 B12 109.9(4) . . ? B9 B10 B12 59.3(3) . . ? B11 B10 B12 60.2(3) . . ? B5 B10 B6 60.2(3) . . ? B9 B10 B6 104.8(4) . . ? B11 B10 B6 59.9(3) . . ? B12 B10 B6 104.5(4) . . ? C2 B11 B10 113.7(4) . . ? C2 B11 B12 109.9(4) . . ? B10 B11 B12 60.1(3) . . ? C2 B11 B7 58.2(3) . . ? B10 B11 B7 108.9(4) . . ? B12 B11 B7 60.6(3) . . ? C2 B11 B6 59.7(3) . . ? B10 B11 B6 62.4(3) . . ? B12 B11 B6 106.3(4) . . ? B7 B11 B6 102.4(3) . . ? B9 B12 B8 60.1(3) . . ? B9 B12 B10 59.7(3) . . ? B8 B12 B10 107.0(4) . . ? B9 B12 B11 108.7(3) . . ? B8 B12 B11 108.6(4) . . ? B10 B12 B11 59.7(3) . . ? B9 B12 B7 110.5(4) . . ? B8 B12 B7 61.9(3) . . ? B10 B12 B7 107.8(4) . . ? B11 B12 B7 59.8(3) . . ? B5 C1 B4 66.8(3) . . ? B5 C1 B6 66.0(3) . . ? B4 C1 B6 112.1(4) . . ? B5 C1 P1 122.0(3) . . ? B4 C1 P1 136.2(3) . . ? B6 C1 P1 109.8(3) . . ? B5 C1 Rh3 121.7(3) . . ? B4 C1 Rh3 67.3(2) . . ? B6 C1 Rh3 101.5(2) . . ? P1 C1 Rh3 115.8(2) . . ? B11 C2 B7 66.5(3) . . ? B11 C2 B6 66.3(3) . . ? B7 C2 B6 112.9(3) . . ? B11 C2 P2 124.5(3) . . ? B7 C2 P2 131.5(3) . . ? B6 C2 P2 114.1(3) . . ? B11 C2 Rh3 121.9(3) . . ? B7 C2 Rh3 67.8(2) . . ? B6 C2 Rh3 102.2(3) . . ? P2 C2 Rh3 112.3(2) . . ? C4 C3 C8 118.2(5) . . ? C4 C3 P2 116.7(4) . . ? C8 C3 P2 124.9(4) . . ? C3 C4 C5 122.3(7) . . ? C4 C5 C6 118.4(7) . . ? C7 C6 C5 120.4(7) . . ? C6 C7 C8 119.8(7) . . ? C7 C8 C3 120.9(6) . . ? C10 C9 C14 118.5(5) . . ? C10 C9 P2 127.8(4) . . ? C14 C9 P2 113.5(4) . . ? C9 C10 C11 120.5(5) . . ? C12 C11 C10 120.2(6) . . ? C13 C12 C11 119.9(6) . . ? C12 C13 C14 120.6(5) . . ? C13 C14 C9 120.4(5) . . ? C20 C15 C16 117.6(5) . . ? C20 C15 P1 117.1(5) . . ? C16 C15 P1 125.2(4) . . ? C15 C16 C17 120.8(6) . . ? C18 C17 C16 120.5(7) . . ? C17 C18 C19 118.9(7) . . ? C18 C19 C20 120.9(7) . . ? C15 C20 C19 121.3(7) . . ? C22 C21 C26 118.2(5) . . ? C22 C21 P1 127.6(4) . . ? C26 C21 P1 114.1(5) . . ? C23 C22 C21 122.2(6) . . ? C24 C23 C22 120.9(8) . . ? C23 C24 C25 119.2(8) . . ? C24 C25 C26 120.6(8) . . ? C21 C26 C25 119.0(7) . . ? C28 C27 C31 108.0 . . ? C28 C27 C32 126.0 . . ? C31 C27 C32 126.0 . . ? C28 C27 Rh3 73.04(12) . . ? C31 C27 Rh3 69.75(12) . . ? C32 C27 Rh3 122.85(11) . . ? C27 C28 C29 108.0 . . ? C27 C28 C33 126.0 . . ? C29 C28 C33 126.0 . . ? C27 C28 Rh3 70.91(12) . . ? C29 C28 Rh3 70.75(12) . . ? C33 C28 Rh3 123.98(11) . . ? C28 C29 C30 108.0 . . ? C28 C29 C34 126.0 . . ? C30 C29 C34 126.0 . . ? C28 C29 Rh3 73.17(12) . . ? C30 C29 Rh3 69.78(11) . . ? C34 C29 Rh3 122.69(11) . . ? C31 C30 C29 108.0 . . ? C31 C30 C35 126.0 . . ? C29 C30 C35 126.0 . . ? C31 C30 Rh3 71.52(12) . . ? C29 C30 Rh3 73.49(12) . . ? C35 C30 Rh3 120.77(11) . . ? C30 C31 C27 108.0 . . ? C30 C31 C36 126.0 . . ? C27 C31 C36 126.0 . . ? C30 C31 Rh3 71.34(12) . . ? C27 C31 Rh3 73.57(12) . . ? C36 C31 Rh3 120.87(11) . . ? C28' C27' C31' 108.0 . . ? C28' C27' C32' 126.0 . . ? C31' C27' C32' 126.0 . . ? C28' C27' Rh3 72.40(12) . . ? C31' C27' Rh3 74.11(12) . . ? C32' C27' Rh3 119.35(11) . . ? C27' C28' C29' 108.0 . . ? C27' C28' C33' 126.0 . . ? C29' C28' C33' 126.0 . . ? C27' C28' Rh3 70.84(12) . . ? C29' C28' Rh3 74.79(12) . . ? C33' C28' Rh3 120.16(11) . . ? C28' C29' C30' 108.0 . . ? C28' C29' C34' 126.0 . . ? C30' C29' C34' 126.0 . . ? C28' C29' Rh3 69.25(11) . . ? C30' C29' Rh3 73.30(11) . . ? C34' C29' Rh3 123.07(11) . . ? C31' C30' C29' 108.0 . . ? C31' C30' C35' 126.0 . . ? C29' C30' C35' 126.0 . . ? C31' C30' Rh3 70.11(11) . . ? C29' C30' Rh3 71.47(11) . . ? C35' C30' Rh3 124.04(10) . . ? C27' C31' C30' 108.0 . . ? C27' C31' C36' 126.0 . . ? C30' C31' C36' 126.0 . . ? C27' C31' Rh3 69.49(11) . . ? C30' C31' Rh3 74.43(12) . . ? C36' C31' Rh3 121.76(11) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.126 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.095 # Attachment '4b.cif' data_f90929c _database_code_depnum_ccdc_archive 'CCDC 770839' #TrackingRef '4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 B9 P2 Rh' _chemical_formula_weight 740.87 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' 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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.646(3) _cell_length_b 19.419(6) _cell_length_c 10.436(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.175(3) _cell_angle_gamma 90.00 _cell_volume 1835.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.328 _cell_measurement_theta_max 26.927 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8230 _exptl_absorpt_correction_T_max 0.9390 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.02 _diffrn_reflns_number 8864 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4022 _reflns_number_gt 3315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+1.0297P] 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 4022 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.55263(4) 0.2500 0.63006(3) 0.03790(15) Uani 1 2 d S . . H1A H 0.714(6) 0.2500 0.632(5) 0.047(14) Uiso 1 2 d S . . P1 P 0.66070(8) 0.33056(4) 0.78817(8) 0.0322(2) Uani 1 1 d . . . B1 B 1.0811(6) 0.2500 1.0684(6) 0.0440(13) Uani 1 2 d S . . H1 H 1.1983 0.2500 1.0781 0.053 Uiso 1 2 calc SR . . B2 B 1.0150(4) 0.2969(2) 1.1841(4) 0.0449(9) Uani 1 1 d . . . H2 H 1.0885 0.3283 1.2678 0.054 Uiso 1 1 calc R . . B3 B 0.8707(7) 0.2500 1.2127(6) 0.0496(14) Uani 1 2 d S . . H3A H 0.864(6) 0.2500 1.320(6) 0.053(15) Uiso 1 2 d S . . H3B H 0.772(10) 0.2500 1.136(9) 0.11(3) Uiso 1 2 d S . . B4 B 0.9364(5) 0.2500 0.9076(6) 0.0378(11) Uani 1 2 d S . . H4 H 0.9538 0.2500 0.8088 0.045 Uiso 1 2 calc SR . . B5 B 0.9712(4) 0.3231(2) 1.0147(4) 0.0405(9) Uani 1 1 d . . . H5 H 1.0166 0.3705 0.9870 0.049 Uiso 1 1 calc R . . B6 B 0.8325(4) 0.3236(2) 1.0929(4) 0.0418(9) Uani 1 1 d . . . H6A H 0.789(4) 0.3650(19) 1.108(3) 0.034(9) Uiso 1 1 d . . . C1 C 0.7935(3) 0.29107(16) 0.9411(3) 0.0316(6) Uani 1 1 d . . . C2 C 0.5312(3) 0.37969(18) 0.8446(3) 0.0390(7) Uani 1 1 d . . . C3 C 0.4714(4) 0.3504(2) 0.9339(4) 0.0514(9) Uani 1 1 d . . . H3 H 0.5075 0.3085 0.9750 0.062 Uiso 1 1 calc R . . C4 C 0.3574(5) 0.3831(3) 0.9632(5) 0.0676(13) Uani 1 1 d . . . H4A H 0.3159 0.3624 1.0219 0.081 Uiso 1 1 calc R . . C5 C 0.3059(5) 0.4461(3) 0.9054(5) 0.0737(15) Uani 1 1 d . . . H5A H 0.2303 0.4680 0.9256 0.088 Uiso 1 1 calc R . . C6 C 0.3660(5) 0.4763(3) 0.8179(5) 0.0701(13) Uani 1 1 d . . . H6 H 0.3312 0.5189 0.7791 0.084 Uiso 1 1 calc R . . C7 C 0.4783(4) 0.4439(2) 0.7872(4) 0.0537(10) Uani 1 1 d . . . H7 H 0.5189 0.4648 0.7282 0.064 Uiso 1 1 calc R . . C8 C 0.7638(3) 0.39718(19) 0.7378(3) 0.0407(8) Uani 1 1 d . . . C9 C 0.8108(4) 0.4562(2) 0.8171(4) 0.0516(9) Uani 1 1 d . . . H9 H 0.7852 0.4621 0.8946 0.062 Uiso 1 1 calc R . . C10 C 0.8935(5) 0.5058(2) 0.7838(5) 0.0671(13) Uani 1 1 d . . . H10 H 0.9240 0.5446 0.8387 0.081 Uiso 1 1 calc R . . C11 C 0.9305(6) 0.4983(3) 0.6710(7) 0.0846(17) Uani 1 1 d . . . H11 H 0.9859 0.5322 0.6479 0.102 Uiso 1 1 calc R . . C12 C 0.8879(6) 0.4420(3) 0.5918(6) 0.0889(18) Uani 1 1 d . . . H12 H 0.9150 0.4378 0.5148 0.107 Uiso 1 1 calc R . . C13 C 0.8027(5) 0.3888(3) 0.6223(4) 0.0609(11) Uani 1 1 d . . . H13 H 0.7741 0.3500 0.5672 0.073 Uiso 1 1 calc R . . C14 C 0.3131(4) 0.2858(2) 0.5297(3) 0.0504(9) Uani 1 1 d . . . C15 C 0.4039(4) 0.3094(2) 0.4528(3) 0.0507(9) Uani 1 1 d . . . C16 C 0.4538(6) 0.2500 0.4038(5) 0.0564(15) Uani 1 2 d S . . C17 C 0.2180(5) 0.3297(3) 0.5828(5) 0.0776(16) Uani 1 1 d . . . H17A H 0.1173 0.3265 0.5226 0.116 Uiso 1 1 calc R . . H17B H 0.2503 0.3767 0.5879 0.116 Uiso 1 1 calc R . . H17C H 0.2252 0.3141 0.6722 0.116 Uiso 1 1 calc R . . C18 C 0.4172(6) 0.3806(3) 0.4121(6) 0.0833(16) Uani 1 1 d . . . H18A H 0.5090 0.3861 0.3964 0.125 Uiso 1 1 calc R . . H18B H 0.4148 0.4113 0.4834 0.125 Uiso 1 1 calc R . . H18C H 0.3367 0.3910 0.3299 0.125 Uiso 1 1 calc R . . C19 C 0.5356(8) 0.2500 0.3039(6) 0.092(3) Uani 1 2 d S . . H19A H 0.4658 0.2500 0.2124 0.137 Uiso 1 2 calc SR . . H19B H 0.5965 0.2096 0.3179 0.137 Uiso 0.50 1 calc PR . . H19C H 0.5965 0.2904 0.3179 0.137 Uiso 0.50 1 calc PR . . 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 0.0277(2) 0.0493(3) 0.0289(2) 0.000 -0.00011(14) 0.000 P1 0.0249(4) 0.0378(5) 0.0298(4) 0.0032(3) 0.0041(3) 0.0019(3) B1 0.023(2) 0.050(3) 0.049(3) 0.000 0.000(2) 0.000 B2 0.0342(19) 0.049(2) 0.0378(19) -0.0035(17) -0.0056(15) -0.0028(16) B3 0.038(3) 0.069(4) 0.034(3) 0.000 0.002(2) 0.000 B4 0.023(2) 0.044(3) 0.041(3) 0.000 0.0046(19) 0.000 B5 0.0259(18) 0.042(2) 0.044(2) 0.0001(16) -0.0004(15) -0.0026(14) B6 0.0351(19) 0.044(2) 0.0374(19) -0.0077(16) 0.0014(15) 0.0031(16) C1 0.0231(14) 0.0348(17) 0.0310(14) 0.0010(12) 0.0016(11) 0.0003(12) C2 0.0287(15) 0.045(2) 0.0376(16) -0.0013(14) 0.0046(13) 0.0045(13) C3 0.0385(19) 0.062(3) 0.054(2) 0.0050(18) 0.0169(16) 0.0062(17) C4 0.047(2) 0.100(4) 0.061(2) -0.004(2) 0.026(2) 0.006(2) C5 0.044(2) 0.104(4) 0.069(3) -0.023(3) 0.014(2) 0.021(2) C6 0.055(3) 0.062(3) 0.083(3) -0.005(2) 0.010(2) 0.025(2) C7 0.045(2) 0.057(2) 0.056(2) 0.0046(18) 0.0124(17) 0.0145(17) C8 0.0301(16) 0.047(2) 0.0425(17) 0.0122(15) 0.0089(13) 0.0026(14) C9 0.047(2) 0.043(2) 0.060(2) 0.0095(17) 0.0129(17) -0.0001(16) C10 0.052(2) 0.047(3) 0.095(4) 0.022(2) 0.016(2) -0.0044(19) C11 0.073(3) 0.069(4) 0.119(5) 0.033(3) 0.041(3) -0.007(3) C12 0.085(4) 0.112(5) 0.093(4) 0.036(4) 0.059(3) 0.009(3) C13 0.054(2) 0.075(3) 0.059(2) 0.013(2) 0.027(2) 0.005(2) C14 0.0293(17) 0.078(3) 0.0321(16) -0.0022(16) -0.0048(13) 0.0070(16) C15 0.0387(19) 0.067(3) 0.0332(17) 0.0083(17) -0.0047(14) 0.0045(17) C16 0.032(3) 0.099(5) 0.030(2) 0.000 0.0004(19) 0.000 C17 0.041(2) 0.115(4) 0.063(3) -0.020(3) 0.0010(19) 0.023(2) C18 0.058(3) 0.086(4) 0.079(3) 0.036(3) -0.010(2) 0.001(2) C19 0.054(4) 0.179(9) 0.041(3) 0.000 0.015(3) 0.000 _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 C16 2.221(5) . ? Rh1 C15 2.232(3) 4_565 ? Rh1 C15 2.232(3) . ? Rh1 P1 2.2517(10) . ? Rh1 P1 2.2517(9) 4_565 ? Rh1 C14 2.291(3) 4_565 ? Rh1 C14 2.291(3) . ? P1 C8 1.817(3) . ? P1 C2 1.823(3) . ? P1 C1 1.834(3) . ? B1 B5 1.745(5) 4_565 ? B1 B5 1.745(5) . ? B1 B4 1.775(7) . ? B1 B2 1.796(7) 4_565 ? B1 B2 1.796(7) . ? B2 B5 1.746(6) . ? B2 B6 1.765(5) . ? B2 B3 1.773(7) . ? B2 B2 1.822(9) 4_565 ? B3 B2 1.773(7) 4_565 ? B3 B6 1.851(6) 4_565 ? B3 B6 1.851(6) . ? B4 C1 1.730(5) 4_565 ? B4 C1 1.730(5) . ? B4 B5 1.767(5) . ? B4 B5 1.767(5) 4_565 ? B5 C1 1.735(5) . ? B5 B6 1.791(6) . ? B6 C1 1.624(5) . ? C1 C1 1.595(6) 4_565 ? C2 C3 1.377(5) . ? C2 C7 1.401(5) . ? C3 C4 1.392(6) . ? C4 C5 1.379(7) . ? C5 C6 1.371(7) . ? C6 C7 1.383(6) . ? C8 C13 1.390(5) . ? C8 C9 1.395(5) . ? C9 C10 1.370(6) . ? C10 C11 1.352(8) . ? C11 C12 1.346(9) . ? C12 C13 1.424(7) . ? C14 C14 1.392(8) 4_565 ? C14 C15 1.451(5) . ? C14 C17 1.492(6) . ? C15 C16 1.412(5) . ? C15 C18 1.464(6) . ? C16 C15 1.412(5) 4_565 ? C16 C19 1.509(8) . ? 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 C16 Rh1 C15 36.98(13) . 4_565 ? C16 Rh1 C15 36.98(13) . . ? C15 Rh1 C15 62.3(2) 4_565 . ? C16 Rh1 P1 134.40(4) . . ? C15 Rh1 P1 165.79(11) 4_565 . ? C15 Rh1 P1 104.54(11) . . ? C16 Rh1 P1 134.40(4) . 4_565 ? C15 Rh1 P1 104.54(11) 4_565 4_565 ? C15 Rh1 P1 165.79(11) . 4_565 ? P1 Rh1 P1 88.01(5) . 4_565 ? C16 Rh1 C14 61.21(16) . 4_565 ? C15 Rh1 C14 37.40(14) 4_565 4_565 ? C15 Rh1 C14 61.29(14) . 4_565 ? P1 Rh1 C14 133.24(11) . 4_565 ? P1 Rh1 C14 105.25(10) 4_565 4_565 ? C16 Rh1 C14 61.21(16) . . ? C15 Rh1 C14 61.29(14) 4_565 . ? C15 Rh1 C14 37.40(14) . . ? P1 Rh1 C14 105.25(10) . . ? P1 Rh1 C14 133.24(11) 4_565 . ? C14 Rh1 C14 35.4(2) 4_565 . ? C8 P1 C2 103.01(17) . . ? C8 P1 C1 105.16(14) . . ? C2 P1 C1 106.77(14) . . ? C8 P1 Rh1 116.37(12) . . ? C2 P1 Rh1 113.86(11) . . ? C1 P1 Rh1 110.79(10) . . ? B5 B1 B5 109.0(4) 4_565 . ? B5 B1 B4 60.3(2) 4_565 . ? B5 B1 B4 60.3(2) . . ? B5 B1 B2 59.0(2) 4_565 4_565 ? B5 B1 B2 108.1(4) . 4_565 ? B4 B1 B2 106.9(3) . 4_565 ? B5 B1 B2 108.1(4) 4_565 . ? B5 B1 B2 59.0(2) . . ? B4 B1 B2 106.9(3) . . ? B2 B1 B2 61.0(3) 4_565 . ? B5 B2 B6 61.3(2) . . ? B5 B2 B3 113.0(3) . . ? B6 B2 B3 63.1(2) . . ? B5 B2 B1 59.0(2) . . ? B6 B2 B1 107.8(3) . . ? B3 B2 B1 109.5(3) . . ? B5 B2 B2 106.96(19) . 4_565 ? B6 B2 B2 107.0(2) . 4_565 ? B3 B2 B2 59.07(18) . 4_565 ? B1 B2 B2 59.51(17) . 4_565 ? B2 B3 B2 61.9(4) . 4_565 ? B2 B3 B6 105.5(4) . 4_565 ? B2 B3 B6 58.3(2) 4_565 4_565 ? B2 B3 B6 58.3(2) . . ? B2 B3 B6 105.5(4) 4_565 . ? B6 B3 B6 101.1(4) 4_565 . ? C1 B4 C1 54.9(3) 4_565 . ? C1 B4 B5 103.5(3) 4_565 . ? C1 B4 B5 59.5(2) . . ? C1 B4 B5 59.5(2) 4_565 4_565 ? C1 B4 B5 103.5(3) . 4_565 ? B5 B4 B5 107.0(4) . 4_565 ? C1 B4 B1 103.3(3) 4_565 . ? C1 B4 B1 103.3(3) . . ? B5 B4 B1 59.0(2) . . ? B5 B4 B1 59.0(2) 4_565 . ? C1 B5 B1 104.4(3) . . ? C1 B5 B2 101.6(3) . . ? B1 B5 B2 61.9(3) . . ? C1 B5 B4 59.2(2) . . ? B1 B5 B4 60.7(3) . . ? B2 B5 B4 109.5(3) . . ? C1 B5 B6 54.84(19) . . ? B1 B5 B6 108.9(3) . . ? B2 B5 B6 59.9(2) . . ? B4 B5 B6 106.4(3) . . ? C1 B6 B2 105.4(3) . . ? C1 B6 B5 60.8(2) . . ? B2 B6 B5 58.8(2) . . ? C1 B6 B3 106.5(3) . . ? B2 B6 B3 58.7(3) . . ? B5 B6 B3 107.4(3) . . ? C1 C1 B6 112.87(19) 4_565 . ? C1 C1 B4 62.54(13) 4_565 . ? B6 C1 B4 116.3(3) . . ? C1 C1 B5 111.04(17) 4_565 . ? B6 C1 B5 64.3(2) . . ? B4 C1 B5 61.3(2) . . ? C1 C1 P1 114.71(10) 4_565 . ? B6 C1 P1 122.9(2) . . ? B4 C1 P1 112.5(2) . . ? B5 C1 P1 121.5(2) . . ? C3 C2 C7 118.7(3) . . ? C3 C2 P1 119.7(3) . . ? C7 C2 P1 121.2(3) . . ? C2 C3 C4 120.5(4) . . ? C5 C4 C3 120.0(4) . . ? C6 C5 C4 120.0(4) . . ? C5 C6 C7 120.3(4) . . ? C6 C7 C2 120.4(4) . . ? C13 C8 C9 118.8(4) . . ? C13 C8 P1 120.4(3) . . ? C9 C8 P1 120.8(3) . . ? C10 C9 C8 121.7(4) . . ? C11 C10 C9 119.8(5) . . ? C12 C11 C10 120.5(5) . . ? C11 C12 C13 121.9(5) . . ? C8 C13 C12 117.3(5) . . ? C14 C14 C15 108.4(2) 4_565 . ? C14 C14 C17 124.8(3) 4_565 . ? C15 C14 C17 126.2(4) . . ? C14 C14 Rh1 72.32(11) 4_565 . ? C15 C14 Rh1 69.08(19) . . ? C17 C14 Rh1 131.0(3) . . ? C16 C15 C14 106.7(4) . . ? C16 C15 C18 126.3(4) . . ? C14 C15 C18 126.0(4) . . ? C16 C15 Rh1 71.1(2) . . ? C14 C15 Rh1 73.52(19) . . ? C18 C15 Rh1 129.3(3) . . ? C15 C16 C15 109.6(5) 4_565 . ? C15 C16 C19 125.1(2) 4_565 . ? C15 C16 C19 125.1(2) . . ? C15 C16 Rh1 71.9(2) 4_565 . ? C15 C16 Rh1 71.9(2) . . ? C19 C16 Rh1 126.8(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 3.865 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.097