# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Alan Welch' _publ_contact_author_email a.j.welch@hw.ac.uk loop_ _publ_author_name 'Alan Welch' 'Amelia McAnaw' 'Greig Scott' 'Lisa Elrick' 'Georgina Rosair' data_x82978 _database_code_depnum_ccdc_archive 'CCDC 891748' #TrackingRef '- compound 1 cif (modified).cif' _audit_update_record ; 2012-05-25 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common x82978 _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 B9 N O3 P Rh), 0.75(C H2 Cl2)' _chemical_formula_sum 'C20.75 H27.50 B9 Cl1.50 N O3 P Rh' _chemical_formula_weight 623.28 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 12.4890(9) _cell_length_b 14.5862(10) _cell_length_c 16.8809(12) _cell_angle_alpha 92.949(4) _cell_angle_beta 105.014(4) _cell_angle_gamma 107.242(4) _cell_volume 2809.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 640 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 17.07 _exptl_crystal_description PLATE _exptl_crystal_colour red _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1254 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6437 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'TWINABS (Bruker, 2008)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74270 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.89 _reflns_number_total 12876 _reflns_number_gt 9066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0750P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12876 _refine_ls_number_parameters 696 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _restr_distance_atom_site_label_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param _restr_distance_diff _restr_distance_details C2S CL4A 1_555 1.70 0.02 -0.047 'generated by SHELX DFIX' C2S CL3A 1_555 1.70 0.02 0.011 'generated by SHELX DFIX' C2S CL3B 1_555 1.70 0.02 0.011 'generated by SHELX DFIX' 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 C1A C 0.7370(6) 0.3431(5) 0.3291(4) 0.0146(15) Uani 1 1 d . . . H1A H 0.7268 0.3163 0.3810 0.017 Uiso 1 1 calc R . . C2A C 0.6477(6) 0.2893(5) 0.2439(4) 0.0156(15) Uani 1 1 d . . . H2A H 0.5825 0.2287 0.2416 0.019 Uiso 1 1 calc R . . Rh3A Rh 0.60135(5) 0.41454(4) 0.28951(3) 0.01221(13) Uani 1 1 d . . . B4A B 0.7904(7) 0.4693(6) 0.3316(5) 0.0153(17) Uani 1 1 d . . . H4A H 0.8152 0.5192 0.3814 0.018 Uiso 1 1 calc R . . B5A B 0.8750(7) 0.3883(6) 0.3243(5) 0.0191(18) Uani 1 1 d . . . H5A H 0.9466 0.3935 0.3702 0.023 Uiso 1 1 calc R . . B6A B 0.7824(7) 0.2749(6) 0.2688(5) 0.0192(18) Uani 1 1 d . . . H6A H 0.7999 0.2137 0.2813 0.023 Uiso 1 1 calc R . . B7A B 0.6250(7) 0.3727(6) 0.1742(5) 0.0163(17) Uani 1 1 d . . . H7A H 0.5509 0.3651 0.1299 0.020 Uiso 1 1 calc R . . B8A B 0.7274(7) 0.4918(6) 0.2268(5) 0.0143(17) Uani 1 1 d . . . H8A H 0.7185 0.5556 0.2131 0.017 Uiso 1 1 calc R . . B9A B 0.8695(8) 0.4780(6) 0.2545(5) 0.0186(19) Uani 1 1 d . . . H9A H 0.9401 0.5349 0.2587 0.022 Uiso 1 1 calc R . . B10A B 0.8610(7) 0.3584(6) 0.2150(5) 0.0175(18) Uani 1 1 d . . . H10A H 0.9248 0.3464 0.1947 0.021 Uiso 1 1 calc R . . B11A B 0.7129(8) 0.2930(6) 0.1691(6) 0.024(2) Uani 1 1 d . . . H11A H 0.6871 0.2401 0.1216 0.029 Uiso 1 1 calc R . . B12A B 0.7670(7) 0.4179(6) 0.1575(5) 0.0181(18) Uani 1 1 d . . . H12A H 0.7751 0.4387 0.1033 0.022 Uiso 1 1 calc R . . P1A P 0.55439(16) 0.55689(13) 0.29446(11) 0.0134(4) Uani 1 1 d . . . O1A O 0.4219(4) 0.3238(3) 0.2758(3) 0.0190(11) Uani 1 1 d . . . O2A O 0.5368(4) 0.3884(3) 0.3979(3) 0.0157(10) Uani 1 1 d . . . O3A O 0.3604(5) 0.2926(4) 0.3855(4) 0.0325(14) Uani 1 1 d . . . N1A N 0.4360(6) 0.3325(4) 0.3543(4) 0.0207(15) Uani 1 1 d . . . C10A C 0.6769(6) 0.6475(5) 0.3678(4) 0.0145(15) Uani 1 1 d . . . C11A C 0.7047(6) 0.6356(5) 0.4511(4) 0.0175(16) Uani 1 1 d . . . H11 H 0.6541 0.5789 0.4697 0.021 Uiso 1 1 calc R . . C12A C 0.8015(6) 0.7011(5) 0.5090(4) 0.0204(17) Uani 1 1 d . . . H12 H 0.8208 0.6915 0.5686 0.024 Uiso 1 1 calc R . . C13A C 0.8711(6) 0.7800(5) 0.4830(5) 0.0228(17) Uani 1 1 d . . . H13A H 0.9389 0.8290 0.5245 0.027 Uiso 1 1 calc R . . C14A C 0.8471(6) 0.7912(5) 0.4001(4) 0.0221(17) Uani 1 1 d . . . H14A H 0.8987 0.8473 0.3816 0.026 Uiso 1 1 calc R . . C15A C 0.7532(6) 0.7258(5) 0.3434(5) 0.0181(16) Uani 1 1 d . . . H15A H 0.7382 0.7336 0.2834 0.022 Uiso 1 1 calc R . . C16A C 0.5151(6) 0.6055(5) 0.1987(4) 0.0157(15) Uani 1 1 d . . . C17A C 0.4761(6) 0.5468(5) 0.1230(4) 0.0164(15) Uani 1 1 d . . . H17A H 0.4774 0.4785 0.1209 0.020 Uiso 1 1 calc R . . C18A C 0.4353(6) 0.5818(5) 0.0501(4) 0.0218(17) Uani 1 1 d . . . H18A H 0.4050 0.5383 -0.0040 0.026 Uiso 1 1 calc R . . C19A C 0.4368(6) 0.6773(5) 0.0526(4) 0.0192(16) Uani 1 1 d . . . H19A H 0.4109 0.7032 -0.0002 0.023 Uiso 1 1 calc R . . C20A C 0.4747(6) 0.7384(5) 0.1292(4) 0.0204(16) Uani 1 1 d . . . H20A H 0.4742 0.8069 0.1313 0.024 Uiso 1 1 calc R . . C21A C 0.5122(6) 0.7014(5) 0.2007(4) 0.0172(16) Uani 1 1 d . . . H21A H 0.5380 0.7435 0.2553 0.021 Uiso 1 1 calc R . . C22A C 0.4261(6) 0.5481(5) 0.3317(4) 0.0149(15) Uani 1 1 d . . . C23A C 0.4280(6) 0.6071(5) 0.4001(4) 0.0169(15) Uani 1 1 d . . . H23A H 0.5033 0.6544 0.4355 0.020 Uiso 1 1 calc R . . C24A C 0.3222(6) 0.5989(6) 0.4184(4) 0.0222(17) Uani 1 1 d . . . H24A H 0.3227 0.6416 0.4669 0.027 Uiso 1 1 calc R . . C25A C 0.2188(7) 0.5338(6) 0.3714(5) 0.0258(18) Uani 1 1 d . . . H25A H 0.1449 0.5288 0.3861 0.031 Uiso 1 1 calc R . . C26A C 0.2156(6) 0.4748(5) 0.3033(5) 0.0216(17) Uani 1 1 d . . . H26A H 0.1396 0.4274 0.2692 0.026 Uiso 1 1 calc R . . C27A C 0.3182(6) 0.4814(5) 0.2823(5) 0.0241(18) Uani 1 1 d . . . H27A H 0.3159 0.4393 0.2328 0.029 Uiso 1 1 calc R . . C1B C 0.1242(7) 1.1142(5) 0.2983(5) 0.0273(19) Uani 1 1 d . . . H1B H 0.1761 1.1608 0.3487 0.033 Uiso 1 1 calc R . . C2B C 0.1476(7) 1.1279(5) 0.2102(5) 0.0261(18) Uani 1 1 d . . . H2B H 0.2149 1.1830 0.2055 0.031 Uiso 1 1 calc R . . Rh3B Rh 0.22098(5) 1.01958(4) 0.26875(3) 0.01474(14) Uani 1 1 d . . . B4B B 0.0644(7) 0.9907(6) 0.3073(5) 0.0172(18) Uani 1 1 d . . . H4B H 0.0759 0.9610 0.3596 0.021 Uiso 1 1 calc R . . B5B B -0.0212(8) 1.0734(7) 0.2899(6) 0.031(2) Uani 1 1 d . . . H5B H -0.0568 1.0904 0.3328 0.037 Uiso 1 1 calc R . . B6B B 0.0352(8) 1.1616(7) 0.2279(7) 0.032(2) Uani 1 1 d . . . H6B H 0.0323 1.2294 0.2334 0.039 Uiso 1 1 calc R . . B7B B 0.1068(8) 1.0162(6) 0.1469(6) 0.024(2) Uani 1 1 d . . . H7B H 0.1431 1.0014 0.1036 0.029 Uiso 1 1 calc R . . B8B B 0.0444(7) 0.9246(6) 0.2076(5) 0.0163(18) Uani 1 1 d . . . H8B H 0.0402 0.8551 0.1995 0.020 Uiso 1 1 calc R . . B9B B -0.0738(8) 0.9583(6) 0.2298(5) 0.0216(19) Uani 1 1 d . . . H9B H -0.1434 0.9070 0.2363 0.026 Uiso 1 1 calc R . . B10B B -0.0895(8) 1.0597(7) 0.1825(6) 0.028(2) Uani 1 1 d . . . H10B H -0.1686 1.0669 0.1606 0.034 Uiso 1 1 calc R . . B11B B 0.0223(8) 1.0989(6) 0.1330(6) 0.028(2) Uani 1 1 d . . . H11B H 0.0123 1.1311 0.0819 0.033 Uiso 1 1 calc R . . B12B B -0.0466(8) 0.9742(7) 0.1319(5) 0.024(2) Uani 1 1 d . . . H12B H -0.0999 0.9325 0.0793 0.029 Uiso 1 1 calc R . . P1B P 0.27111(16) 0.87838(13) 0.27953(11) 0.0143(4) Uani 1 1 d . . . O1B O 0.3601(4) 1.0761(3) 0.3873(3) 0.0207(11) Uani 1 1 d . . . O2B O 0.4003(4) 1.1101(3) 0.2718(3) 0.0187(11) Uani 1 1 d . . . O3B O 0.5360(4) 1.1715(4) 0.3897(3) 0.0287(13) Uani 1 1 d . . . N1B N 0.4367(6) 1.1203(4) 0.3522(4) 0.0231(15) Uani 1 1 d . . . C10B C 0.4289(6) 0.9023(5) 0.3110(4) 0.0153(15) Uani 1 1 d . . . C11B C 0.4907(6) 0.8740(5) 0.3833(4) 0.0208(17) Uani 1 1 d . . . H11C H 0.4478 0.8398 0.4213 0.025 Uiso 1 1 calc R . . C12B C 0.6107(7) 0.8936(5) 0.4012(5) 0.0245(18) Uani 1 1 d . . . H12C H 0.6535 0.8729 0.4521 0.029 Uiso 1 1 calc R . . C13B C 0.6727(7) 0.9417(6) 0.3496(5) 0.0275(19) Uani 1 1 d . . . H13B H 0.7596 0.9572 0.3644 0.033 Uiso 1 1 calc R . . C14B C 0.6129(7) 0.9680(5) 0.2774(5) 0.0261(19) Uani 1 1 d . . . H14B H 0.6569 1.0014 0.2396 0.031 Uiso 1 1 calc R . . C15B C 0.4916(7) 0.9477(5) 0.2574(5) 0.0198(17) Uani 1 1 d . . . H15B H 0.4490 0.9655 0.2048 0.024 Uiso 1 1 calc R . . C16B C 0.2218(6) 0.7857(5) 0.1890(4) 0.0182(16) Uani 1 1 d . . . C17B C 0.2206(7) 0.6911(5) 0.1997(5) 0.0214(17) Uani 1 1 d . . . H17B H 0.2463 0.6736 0.2564 0.026 Uiso 1 1 calc R . . C18B C 0.1829(7) 0.6217(5) 0.1300(5) 0.0249(18) Uani 1 1 d . . . H18B H 0.1784 0.5531 0.1369 0.030 Uiso 1 1 calc R . . C19B C 0.1514(7) 0.6471(6) 0.0509(5) 0.032(2) Uani 1 1 d . . . H19B H 0.1252 0.5964 0.0015 0.038 Uiso 1 1 calc R . . C20B C 0.1557(7) 0.7404(6) 0.0397(5) 0.0260(18) Uani 1 1 d . . . H20B H 0.1335 0.7582 -0.0173 0.031 Uiso 1 1 calc R . . C21B C 0.1918(6) 0.8105(6) 0.1098(4) 0.0208(17) Uani 1 1 d . . . H21B H 0.1960 0.8790 0.1026 0.025 Uiso 1 1 calc R . . C22B C 0.2151(6) 0.8238(5) 0.3614(4) 0.0129(14) Uani 1 1 d . . . C23B C 0.1159(6) 0.7394(5) 0.3434(5) 0.0175(17) Uani 1 1 d . . . H23B H 0.0791 0.7048 0.2855 0.021 Uiso 1 1 calc R . . C24B C 0.0703(6) 0.7053(5) 0.4068(4) 0.0186(16) Uani 1 1 d . . . H24B H -0.0019 0.6476 0.3942 0.022 Uiso 1 1 calc R . . C25B C 0.1239(6) 0.7504(5) 0.4867(5) 0.0208(17) Uani 1 1 d . . . H25B H 0.0922 0.7231 0.5322 0.025 Uiso 1 1 calc R . . C26B C 0.2211(6) 0.8328(5) 0.5057(4) 0.0164(15) Uani 1 1 d . . . H26B H 0.2587 0.8655 0.5642 0.020 Uiso 1 1 calc R . . C27B C 0.2655(6) 0.8695(5) 0.4424(4) 0.0167(15) Uani 1 1 d . . . H27B H 0.3348 0.9297 0.4554 0.020 Uiso 1 1 calc R . . C1S C 0.8569(8) 0.6893(8) 1.0388(6) 0.062(3) Uani 1 1 d . . . H1S1 H 0.8930 0.6485 1.0759 0.074 Uiso 1 1 calc R . . H1S2 H 0.9136 0.7566 1.0513 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.8345(3) 0.6434(2) 0.93450(18) 0.0688(9) Uani 1 1 d . . . Cl2 Cl 0.7305(2) 0.6913(2) 1.0607(2) 0.0649(8) Uani 1 1 d . . . C2S C 0.3759(14) 0.0768(10) -0.0045(10) 0.060(6) Uani 0.50 1 d PD . . H2S1 H 0.4494 0.1041 -0.0207 0.071 Uiso 0.50 1 calc PR A 1 H2S2 H 0.3090 0.0860 -0.0472 0.071 Uiso 0.50 1 calc PR A 1 Cl3A Cl 0.3510(8) -0.0430(7) 0.0066(6) 0.051(3) Uani 0.25 1 d PD B 1 Cl3B Cl 0.4733(11) 0.0244(8) -0.0249(7) 0.063(3) Uani 0.25 1 d PD . 2 Cl4A Cl 0.3884(5) 0.1287(5) 0.0883(3) 0.085(2) Uani 0.50 1 d PD B . 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 C1A 0.014(4) 0.017(4) 0.013(4) 0.004(3) 0.004(3) 0.006(3) C2A 0.019(4) 0.016(4) 0.015(4) 0.004(3) 0.004(3) 0.012(3) Rh3A 0.0119(3) 0.0119(3) 0.0124(3) 0.0007(2) 0.0031(2) 0.0037(2) B4A 0.013(4) 0.007(4) 0.025(5) 0.001(3) 0.008(4) 0.001(3) B5A 0.015(4) 0.028(5) 0.021(4) 0.008(4) 0.010(4) 0.011(4) B6A 0.018(4) 0.014(4) 0.028(5) 0.004(4) 0.011(4) 0.006(3) B7A 0.014(4) 0.013(4) 0.025(5) 0.005(3) 0.006(4) 0.007(3) B8A 0.021(5) 0.011(4) 0.010(4) 0.002(3) 0.005(3) 0.003(3) B9A 0.024(5) 0.018(4) 0.014(4) 0.012(3) 0.007(4) 0.004(4) B10A 0.018(4) 0.019(4) 0.021(5) 0.007(3) 0.010(4) 0.010(4) B11A 0.031(5) 0.018(4) 0.027(5) 0.003(4) 0.009(4) 0.013(4) B12A 0.017(4) 0.019(4) 0.020(4) 0.004(3) 0.008(4) 0.004(3) P1A 0.0124(10) 0.0137(9) 0.0120(9) -0.0010(7) 0.0010(8) 0.0039(7) O1A 0.016(3) 0.020(3) 0.018(3) -0.002(2) 0.004(2) 0.004(2) O2A 0.013(3) 0.017(3) 0.019(3) 0.004(2) 0.005(2) 0.007(2) O3A 0.033(3) 0.023(3) 0.051(4) 0.010(3) 0.031(3) 0.006(3) N1A 0.023(4) 0.012(3) 0.033(4) 0.008(3) 0.018(3) 0.005(3) C10A 0.015(4) 0.011(3) 0.017(4) 0.000(3) 0.005(3) 0.003(3) C11A 0.016(4) 0.018(4) 0.020(4) -0.006(3) 0.007(3) 0.007(3) C12A 0.022(4) 0.024(4) 0.017(4) -0.005(3) 0.003(3) 0.014(3) C13A 0.010(4) 0.027(4) 0.028(4) -0.009(3) 0.003(3) 0.005(3) C14A 0.016(4) 0.024(4) 0.022(4) -0.001(3) 0.006(3) 0.003(3) C15A 0.018(4) 0.020(4) 0.019(4) 0.007(3) 0.007(3) 0.009(3) C16A 0.012(4) 0.012(4) 0.023(4) 0.000(3) 0.003(3) 0.006(3) C17A 0.014(4) 0.018(4) 0.019(4) 0.004(3) 0.002(3) 0.010(3) C18A 0.018(4) 0.030(4) 0.015(4) -0.001(3) -0.002(3) 0.011(3) C19A 0.035(5) 0.019(4) 0.008(3) 0.004(3) 0.006(3) 0.014(3) C20A 0.023(4) 0.016(4) 0.022(4) 0.004(3) 0.007(3) 0.005(3) C21A 0.021(4) 0.018(4) 0.018(4) 0.001(3) 0.010(3) 0.010(3) C22A 0.015(4) 0.017(4) 0.011(3) 0.002(3) 0.003(3) 0.005(3) C23A 0.017(4) 0.017(4) 0.018(4) 0.002(3) 0.002(3) 0.009(3) C24A 0.017(4) 0.039(5) 0.017(4) 0.006(3) 0.006(3) 0.016(4) C25A 0.023(4) 0.027(4) 0.039(5) 0.025(4) 0.019(4) 0.013(4) C26A 0.014(4) 0.018(4) 0.033(4) 0.003(3) 0.006(3) 0.005(3) C27A 0.017(4) 0.018(4) 0.036(5) 0.007(3) 0.003(4) 0.007(3) C1B 0.024(4) 0.013(4) 0.038(5) -0.009(3) 0.000(4) 0.006(3) C2B 0.023(4) 0.008(4) 0.047(5) 0.006(3) 0.006(4) 0.008(3) Rh3B 0.0133(3) 0.0114(3) 0.0188(3) 0.0018(2) 0.0033(3) 0.0042(2) B4B 0.021(5) 0.020(4) 0.014(4) 0.004(3) 0.004(3) 0.011(4) B5B 0.027(5) 0.028(5) 0.036(5) -0.012(4) 0.008(5) 0.009(4) B6B 0.018(5) 0.015(5) 0.064(7) 0.003(4) 0.009(5) 0.010(4) B7B 0.030(5) 0.024(5) 0.026(5) 0.007(4) 0.006(4) 0.019(4) B8B 0.021(5) 0.012(4) 0.012(4) 0.001(3) -0.002(3) 0.007(3) B9B 0.018(5) 0.022(5) 0.023(5) -0.001(4) 0.010(4) 0.001(4) B10B 0.022(5) 0.032(5) 0.031(5) -0.004(4) 0.001(4) 0.017(4) B11B 0.020(5) 0.024(5) 0.039(6) 0.006(4) -0.002(4) 0.016(4) B12B 0.025(5) 0.032(5) 0.017(4) 0.008(4) 0.000(4) 0.017(4) P1B 0.0147(10) 0.0115(9) 0.0164(10) 0.0007(7) 0.0037(8) 0.0048(7) O1B 0.025(3) 0.019(3) 0.019(3) 0.003(2) 0.005(2) 0.007(2) O2B 0.023(3) 0.014(3) 0.016(3) 0.005(2) 0.002(2) 0.003(2) O3B 0.013(3) 0.025(3) 0.038(3) 0.003(3) -0.004(3) 0.000(2) N1B 0.023(4) 0.012(3) 0.037(4) 0.004(3) 0.004(3) 0.013(3) C10B 0.015(4) 0.008(3) 0.020(4) -0.003(3) 0.005(3) 0.001(3) C11B 0.014(4) 0.027(4) 0.019(4) 0.001(3) 0.003(3) 0.004(3) C12B 0.023(4) 0.028(4) 0.019(4) -0.008(3) 0.000(3) 0.010(3) C13B 0.020(4) 0.024(4) 0.035(5) -0.006(4) 0.005(4) 0.006(3) C14B 0.026(5) 0.007(4) 0.047(5) -0.005(3) 0.023(4) 0.000(3) C15B 0.027(5) 0.014(4) 0.023(4) 0.002(3) 0.014(3) 0.008(3) C16B 0.015(4) 0.019(4) 0.021(4) -0.004(3) 0.004(3) 0.008(3) C17B 0.029(5) 0.015(4) 0.027(4) -0.001(3) 0.016(3) 0.010(3) C18B 0.028(5) 0.010(4) 0.034(5) -0.010(3) 0.008(4) 0.004(3) C19B 0.030(5) 0.041(5) 0.023(4) -0.015(4) 0.005(4) 0.015(4) C20B 0.026(4) 0.037(5) 0.022(4) -0.005(3) 0.009(3) 0.020(4) C21B 0.013(4) 0.031(4) 0.022(4) 0.002(3) 0.002(3) 0.016(3) C22B 0.010(4) 0.015(4) 0.015(3) 0.003(3) 0.002(3) 0.006(3) C23B 0.013(4) 0.015(4) 0.024(4) 0.002(3) 0.003(3) 0.007(3) C24B 0.009(4) 0.020(4) 0.029(4) 0.009(3) 0.006(3) 0.005(3) C25B 0.017(4) 0.022(4) 0.027(4) 0.011(3) 0.005(3) 0.013(3) C26B 0.020(4) 0.015(4) 0.017(4) 0.004(3) 0.005(3) 0.011(3) C27B 0.021(4) 0.012(4) 0.022(4) 0.010(3) 0.010(3) 0.007(3) C1S 0.025(5) 0.078(8) 0.060(7) -0.040(6) 0.005(5) -0.003(5) Cl1 0.0612(19) 0.0586(18) 0.0636(18) -0.0284(14) 0.0120(15) -0.0032(14) Cl2 0.0560(18) 0.0552(17) 0.091(2) 0.0151(15) 0.0378(16) 0.0140(14) C2S 0.016(10) 0.051(13) 0.103(19) 0.016(12) 0.020(11) -0.005(9) Cl3A 0.035(5) 0.052(6) 0.060(6) 0.033(5) 0.005(5) 0.006(4) Cl3B 0.079(8) 0.059(7) 0.060(7) 0.027(5) 0.027(6) 0.025(6) Cl4A 0.046(3) 0.113(5) 0.048(3) -0.017(3) 0.015(3) -0.042(3) _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 C1A C2A 1.569(9) . ? C1A B5A 1.678(11) . ? C1A B6A 1.697(10) . ? C1A B4A 1.756(10) . ? C1A Rh3A 2.221(7) . ? C1A H1A 1.0001 . ? C2A B11A 1.666(11) . ? C2A B6A 1.704(11) . ? C2A B7A 1.768(10) . ? C2A Rh3A 2.231(7) . ? C2A H2A 1.0001 . ? Rh3A B7A 2.128(8) . ? Rh3A B4A 2.161(8) . ? Rh3A O1A 2.184(5) . ? Rh3A O2A 2.190(5) . ? Rh3A B8A 2.192(8) . ? Rh3A P1A 2.3219(18) . ? B4A B9A 1.814(12) . ? B4A B5A 1.823(12) . ? B4A B8A 1.830(11) . ? B4A H4A 1.0001 . ? B5A B6A 1.759(12) . ? B5A B9A 1.809(11) . ? B5A B10A 1.825(12) . ? B5A H5A 1.0001 . ? B6A B11A 1.755(12) . ? B6A B10A 1.772(11) . ? B6A H6A 1.0001 . ? B7A B12A 1.801(11) . ? B7A B11A 1.833(11) . ? B7A B8A 1.838(11) . ? B7A H7A 1.0001 . ? B8A B9A 1.788(12) . ? B8A B12A 1.805(11) . ? B8A H8A 1.0001 . ? B9A B12A 1.785(12) . ? B9A B10A 1.799(12) . ? B9A H9A 1.0001 . ? B10A B11A 1.751(12) . ? B10A B12A 1.782(12) . ? B10A H10A 1.0001 . ? B11A B12A 1.786(12) . ? B11A H11A 1.0001 . ? B12A H12A 1.0001 . ? P1A C10A 1.809(7) . ? P1A C16A 1.809(7) . ? P1A C22A 1.840(7) . ? O1A N1A 1.286(7) . ? O2A N1A 1.281(7) . ? O3A N1A 1.213(7) . ? C10A C11A 1.391(9) . ? C10A C15A 1.410(10) . ? C11A C12A 1.392(10) . ? C11A H11 1.0000 . ? C12A C13A 1.388(10) . ? C12A H12 1.0000 . ? C13A C14A 1.383(10) . ? C13A H13A 1.0000 . ? C14A C15A 1.364(10) . ? C14A H14A 1.0000 . ? C15A H15A 1.0000 . ? C16A C17A 1.386(9) . ? C16A C21A 1.408(9) . ? C17A C18A 1.389(9) . ? C17A H17A 1.0000 . ? C18A C19A 1.385(9) . ? C18A H18A 1.0000 . ? C19A C20A 1.416(10) . ? C19A H19A 1.0000 . ? C20A C21A 1.375(10) . ? C20A H20A 1.0000 . ? C21A H21A 1.0000 . ? C22A C23A 1.394(9) . ? C22A C27A 1.420(10) . ? C23A C24A 1.407(10) . ? C23A H23A 1.0000 . ? C24A C25A 1.365(11) . ? C24A H24A 1.0000 . ? C25A C26A 1.384(11) . ? C25A H25A 1.0000 . ? C26A C27A 1.394(10) . ? C26A H26A 1.0000 . ? C27A H27A 1.0000 . ? C1B C2B 1.599(11) . ? C1B B5B 1.699(12) . ? C1B B6B 1.727(12) . ? C1B B4B 1.764(11) . ? C1B Rh3B 2.201(7) . ? C1B H1B 1.0001 . ? C2B B11B 1.679(11) . ? C2B B6B 1.707(12) . ? C2B B7B 1.762(11) . ? C2B Rh3B 2.205(7) . ? C2B H2B 1.0001 . ? Rh3B B4B 2.150(8) . ? Rh3B B7B 2.166(9) . ? Rh3B B8B 2.171(8) . ? Rh3B O1B 2.209(5) . ? Rh3B O2B 2.223(5) . ? Rh3B P1B 2.3261(19) . ? B4B B9B 1.788(12) . ? B4B B8B 1.816(11) . ? B4B B5B 1.823(12) . ? B4B H4B 1.0001 . ? B5B B9B 1.763(12) . ? B5B B10B 1.765(14) . ? B5B B6B 1.796(14) . ? B5B H5B 1.0001 . ? B6B B11B 1.749(14) . ? B6B B10B 1.765(13) . ? B6B H6B 1.0001 . ? B7B B12B 1.774(13) . ? B7B B11B 1.811(11) . ? B7B B8B 1.838(12) . ? B7B H7B 1.0001 . ? B8B B9B 1.804(12) . ? B8B B12B 1.810(11) . ? B8B H8B 1.0001 . ? B9B B10B 1.753(13) . ? B9B B12B 1.783(12) . ? B9B H9B 1.0001 . ? B10B B12B 1.759(13) . ? B10B B11B 1.776(14) . ? B10B H10B 1.0001 . ? B11B B12B 1.763(13) . ? B11B H11B 1.0001 . ? B12B H12B 1.0001 . ? P1B C22B 1.821(7) . ? P1B C10B 1.822(7) . ? P1B C16B 1.830(7) . ? O1B N1B 1.284(8) . ? O2B N1B 1.300(8) . ? O3B N1B 1.222(8) . ? C10B C15B 1.412(10) . ? C10B C11B 1.417(10) . ? C11B C12B 1.386(10) . ? C11B H11C 1.0000 . ? C12B C13B 1.393(11) . ? C12B H12C 1.0000 . ? C13B C14B 1.392(11) . ? C13B H13B 1.0000 . ? C14B C15B 1.398(10) . ? C14B H14B 1.0000 . ? C15B H15B 1.0000 . ? C16B C21B 1.389(10) . ? C16B C17B 1.397(10) . ? C17B C18B 1.392(10) . ? C17B H17B 1.0000 . ? C18B C19B 1.393(11) . ? C18B H18B 1.0000 . ? C19B C20B 1.371(11) . ? C19B H19B 1.0000 . ? C20B C21B 1.405(10) . ? C20B H20B 1.0000 . ? C21B H21B 1.0000 . ? C22B C27B 1.386(9) . ? C22B C23B 1.416(9) . ? C23B C24B 1.384(10) . ? C23B H23B 1.0000 . ? C24B C25B 1.372(10) . ? C24B H24B 1.0000 . ? C25B C26B 1.384(10) . ? C25B H25B 1.0000 . ? C26B C27B 1.388(9) . ? C26B H26B 1.0000 . ? C27B H27B 1.0000 . ? C1S Cl2 1.721(10) . ? C1S Cl1 1.771(10) . ? C1S H1S1 1.0000 . ? C1S H1S2 1.0000 . ? C2S Cl4A 1.653(15) . ? C2S Cl3B 1.711(15) . ? C2S Cl3A 1.711(14) . ? C2S H2S1 1.0000 . ? C2S H2S2 1.0000 . ? Cl3B Cl3B 1.31(2) 2_655 ? 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 C2A C1A B5A 113.2(6) . . ? C2A C1A B6A 62.8(5) . . ? B5A C1A B6A 62.8(5) . . ? C2A C1A B4A 113.2(5) . . ? B5A C1A B4A 64.1(5) . . ? B6A C1A B4A 116.8(5) . . ? C2A C1A Rh3A 69.7(3) . . ? B5A C1A Rh3A 124.1(5) . . ? B6A C1A Rh3A 128.0(5) . . ? B4A C1A Rh3A 64.6(3) . . ? C2A C1A H1A 118.9 . . ? B5A C1A H1A 116.5 . . ? B6A C1A H1A 113.8 . . ? B4A C1A H1A 119.1 . . ? Rh3A C1A H1A 106.5 . . ? C1A C2A B11A 111.7(6) . . ? C1A C2A B6A 62.3(4) . . ? B11A C2A B6A 62.8(5) . . ? C1A C2A B7A 110.8(5) . . ? B11A C2A B7A 64.5(4) . . ? B6A C2A B7A 116.6(6) . . ? C1A C2A Rh3A 69.0(3) . . ? B11A C2A Rh3A 122.8(4) . . ? B6A C2A Rh3A 126.9(5) . . ? B7A C2A Rh3A 63.1(3) . . ? C1A C2A H2A 120.4 . . ? B11A C2A H2A 116.8 . . ? B6A C2A H2A 113.8 . . ? B7A C2A H2A 119.9 . . ? Rh3A C2A H2A 108.0 . . ? B7A Rh3A B4A 84.7(3) . . ? B7A Rh3A O1A 101.8(3) . . ? B4A Rh3A O1A 160.3(2) . . ? B7A Rh3A O2A 154.5(2) . . ? B4A Rh3A O2A 108.2(2) . . ? O1A Rh3A O2A 59.15(17) . . ? B7A Rh3A B8A 50.3(3) . . ? B4A Rh3A B8A 49.7(3) . . ? O1A Rh3A B8A 146.4(2) . . ? O2A Rh3A B8A 153.1(2) . . ? B7A Rh3A C1A 78.4(3) . . ? B4A Rh3A C1A 47.2(3) . . ? O1A Rh3A C1A 115.4(2) . . ? O2A Rh3A C1A 94.2(2) . . ? B8A Rh3A C1A 80.5(3) . . ? B7A Rh3A C2A 47.8(3) . . ? B4A Rh3A C2A 78.5(3) . . ? O1A Rh3A C2A 92.1(2) . . ? O2A Rh3A C2A 112.0(2) . . ? B8A Rh3A C2A 81.3(3) . . ? C1A Rh3A C2A 41.3(2) . . ? B7A Rh3A P1A 113.7(2) . . ? B4A Rh3A P1A 101.5(2) . . ? O1A Rh3A P1A 92.92(13) . . ? O2A Rh3A P1A 85.88(13) . . ? B8A Rh3A P1A 84.7(2) . . ? C1A Rh3A P1A 147.02(18) . . ? C2A Rh3A P1A 161.42(18) . . ? C1A B4A B9A 101.0(5) . . ? C1A B4A B5A 55.9(4) . . ? B9A B4A B5A 59.6(4) . . ? C1A B4A B8A 105.3(5) . . ? B9A B4A B8A 58.8(4) . . ? B5A B4A B8A 107.9(6) . . ? C1A B4A Rh3A 68.2(3) . . ? B9A B4A Rh3A 118.1(5) . . ? B5A B4A Rh3A 120.0(5) . . ? B8A B4A Rh3A 66.0(4) . . ? C1A B4A H4A 126.2 . . ? B9A B4A H4A 123.0 . . ? B5A B4A H4A 120.2 . . ? B8A B4A H4A 122.7 . . ? Rh3A B4A H4A 108.8 . . ? C1A B5A B6A 59.1(4) . . ? C1A B5A B9A 104.4(6) . . ? B6A B5A B9A 107.8(6) . . ? C1A B5A B4A 60.1(4) . . ? B6A B5A B4A 110.3(6) . . ? B9A B5A B4A 60.0(5) . . ? C1A B5A B10A 103.2(6) . . ? B6A B5A B10A 59.2(5) . . ? B9A B5A B10A 59.4(5) . . ? B4A B5A B10A 107.9(6) . . ? C1A B5A H5A 124.9 . . ? B6A B5A H5A 120.8 . . ? B9A B5A H5A 122.9 . . ? B4A B5A H5A 120.1 . . ? B10A B5A H5A 123.6 . . ? C1A B6A C2A 54.9(4) . . ? C1A B6A B11A 101.7(6) . . ? C2A B6A B11A 57.5(5) . . ? C1A B6A B5A 58.1(4) . . ? C2A B6A B5A 103.1(6) . . ? B11A B6A B5A 108.1(6) . . ? C1A B6A B10A 104.7(6) . . ? C2A B6A B10A 103.8(6) . . ? B11A B6A B10A 59.5(5) . . ? B5A B6A B10A 62.2(5) . . ? C1A B6A H6A 126.2 . . ? C2A B6A H6A 126.2 . . ? B11A B6A H6A 123.3 . . ? B5A B6A H6A 121.5 . . ? B10A B6A H6A 122.1 . . ? C2A B7A B12A 101.3(5) . . ? C2A B7A B11A 55.1(4) . . ? B12A B7A B11A 58.9(4) . . ? C2A B7A B8A 106.0(5) . . ? B12A B7A B8A 59.5(4) . . ? B11A B7A B8A 106.9(6) . . ? C2A B7A Rh3A 69.2(4) . . ? B12A B7A Rh3A 119.8(5) . . ? B11A B7A Rh3A 119.9(5) . . ? B8A B7A Rh3A 66.6(4) . . ? C2A B7A H7A 125.8 . . ? B12A B7A H7A 122.4 . . ? B11A B7A H7A 121.5 . . ? B8A B7A H7A 122.5 . . ? Rh3A B7A H7A 107.7 . . ? B9A B8A B12A 59.6(5) . . ? B9A B8A B4A 60.2(4) . . ? B12A B8A B4A 106.5(6) . . ? B9A B8A B7A 105.9(6) . . ? B12A B8A B7A 59.3(4) . . ? B4A B8A B7A 104.0(5) . . ? B9A B8A Rh3A 117.8(5) . . ? B12A B8A Rh3A 116.4(5) . . ? B4A B8A Rh3A 64.3(3) . . ? B7A B8A Rh3A 63.0(3) . . ? B9A B8A H8A 120.0 . . ? B12A B8A H8A 120.7 . . ? B4A B8A H8A 123.8 . . ? B7A B8A H8A 125.0 . . ? Rh3A B8A H8A 112.7 . . ? B12A B9A B8A 60.7(5) . . ? B12A B9A B10A 59.6(5) . . ? B8A B9A B10A 110.3(6) . . ? B12A B9A B5A 107.8(6) . . ? B8A B9A B5A 110.3(6) . . ? B10A B9A B5A 60.8(5) . . ? B12A B9A B4A 108.0(6) . . ? B8A B9A B4A 61.0(5) . . ? B10A B9A B4A 109.4(5) . . ? B5A B9A B4A 60.4(4) . . ? B12A B9A H9A 122.4 . . ? B8A B9A H9A 119.7 . . ? B10A B9A H9A 120.7 . . ? B5A B9A H9A 121.0 . . ? B4A B9A H9A 121.3 . . ? B11A B10A B6A 59.8(5) . . ? B11A B10A B12A 60.7(5) . . ? B6A B10A B12A 109.0(6) . . ? B11A B10A B9A 107.5(6) . . ? B6A B10A B9A 107.7(6) . . ? B12A B10A B9A 59.8(5) . . ? B11A B10A B5A 105.4(6) . . ? B6A B10A B5A 58.5(5) . . ? B12A B10A B5A 107.2(6) . . ? B9A B10A B5A 59.9(4) . . ? B11A B10A H10A 122.5 . . ? B6A B10A H10A 121.7 . . ? B12A B10A H10A 121.0 . . ? B9A B10A H10A 121.8 . . ? B5A B10A H10A 123.4 . . ? C2A B11A B10A 106.4(6) . . ? C2A B11A B6A 59.7(5) . . ? B10A B11A B6A 60.7(5) . . ? C2A B11A B12A 106.1(6) . . ? B10A B11A B12A 60.5(5) . . ? B6A B11A B12A 109.6(6) . . ? C2A B11A B7A 60.5(4) . . ? B10A B11A B7A 109.2(6) . . ? B6A B11A B7A 110.8(6) . . ? B12A B11A B7A 59.7(4) . . ? C2A B11A H11A 123.4 . . ? B10A B11A H11A 121.7 . . ? B6A B11A H11A 120.0 . . ? B12A B11A H11A 122.0 . . ? B7A B11A H11A 120.2 . . ? B10A B12A B9A 60.6(5) . . ? B10A B12A B11A 58.8(5) . . ? B9A B12A B11A 106.5(6) . . ? B10A B12A B7A 109.3(6) . . ? B9A B12A B7A 107.6(6) . . ? B11A B12A B7A 61.5(5) . . ? B10A B12A B8A 110.4(6) . . ? B9A B12A B8A 59.7(5) . . ? B11A B12A B8A 110.4(6) . . ? B7A B12A B8A 61.3(4) . . ? B10A B12A H12A 120.9 . . ? B9A B12A H12A 122.9 . . ? B11A B12A H12A 121.7 . . ? B7A B12A H12A 120.8 . . ? B8A B12A H12A 119.8 . . ? C10A P1A C16A 109.3(3) . . ? C10A P1A C22A 106.2(3) . . ? C16A P1A C22A 100.9(3) . . ? C10A P1A Rh3A 107.4(2) . . ? C16A P1A Rh3A 118.2(2) . . ? C22A P1A Rh3A 114.2(2) . . ? N1A O1A Rh3A 93.2(4) . . ? N1A O2A Rh3A 93.0(4) . . ? O3A N1A O2A 122.0(6) . . ? O3A N1A O1A 123.5(6) . . ? O2A N1A O1A 114.5(5) . . ? C11A C10A C15A 117.7(6) . . ? C11A C10A P1A 119.3(5) . . ? C15A C10A P1A 122.8(5) . . ? C10A C11A C12A 121.2(7) . . ? C10A C11A H11 119.4 . . ? C12A C11A H11 119.4 . . ? C13A C12A C11A 119.3(7) . . ? C13A C12A H12 120.4 . . ? C11A C12A H12 120.4 . . ? C14A C13A C12A 120.3(7) . . ? C14A C13A H13A 119.9 . . ? C12A C13A H13A 119.9 . . ? C15A C14A C13A 120.1(7) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14A C15A C10A 121.3(7) . . ? C14A C15A H15A 119.3 . . ? C10A C15A H15A 119.3 . . ? C17A C16A C21A 119.0(6) . . ? C17A C16A P1A 120.8(5) . . ? C21A C16A P1A 119.9(5) . . ? C16A C17A C18A 120.7(7) . . ? C16A C17A H17A 119.7 . . ? C18A C17A H17A 119.7 . . ? C19A C18A C17A 119.8(7) . . ? C19A C18A H18A 120.1 . . ? C17A C18A H18A 120.1 . . ? C18A C19A C20A 120.6(6) . . ? C18A C19A H19A 119.7 . . ? C20A C19A H19A 119.7 . . ? C21A C20A C19A 118.5(7) . . ? C21A C20A H20A 120.7 . . ? C19A C20A H20A 120.7 . . ? C20A C21A C16A 121.4(6) . . ? C20A C21A H21A 119.3 . . ? C16A C21A H21A 119.3 . . ? C23A C22A C27A 119.6(7) . . ? C23A C22A P1A 124.2(5) . . ? C27A C22A P1A 116.0(5) . . ? C22A C23A C24A 118.9(7) . . ? C22A C23A H23A 120.6 . . ? C24A C23A H23A 120.6 . . ? C25A C24A C23A 121.4(7) . . ? C25A C24A H24A 119.3 . . ? C23A C24A H24A 119.3 . . ? C24A C25A C26A 120.4(7) . . ? C24A C25A H25A 119.8 . . ? C26A C25A H25A 119.8 . . ? C25A C26A C27A 120.2(7) . . ? C25A C26A H26A 119.9 . . ? C27A C26A H26A 119.9 . . ? C26A C27A C22A 119.6(7) . . ? C26A C27A H27A 120.2 . . ? C22A C27A H27A 120.2 . . ? C2B C1B B5B 111.8(6) . . ? C2B C1B B6B 61.6(5) . . ? B5B C1B B6B 63.2(5) . . ? C2B C1B B4B 111.7(5) . . ? B5B C1B B4B 63.5(5) . . ? B6B C1B B4B 116.1(6) . . ? C2B C1B Rh3B 68.9(4) . . ? B5B C1B Rh3B 123.2(5) . . ? B6B C1B Rh3B 126.2(6) . . ? B4B C1B Rh3B 64.6(3) . . ? C2B C1B H1B 120.4 . . ? B5B C1B H1B 116.8 . . ? B6B C1B H1B 114.4 . . ? B4B C1B H1B 119.5 . . ? Rh3B C1B H1B 107.5 . . ? C1B C2B B11B 111.9(6) . . ? C1B C2B B6B 62.9(5) . . ? B11B C2B B6B 62.2(5) . . ? C1B C2B B7B 112.0(6) . . ? B11B C2B B7B 63.5(5) . . ? B6B C2B B7B 115.8(6) . . ? C1B C2B Rh3B 68.6(4) . . ? B11B C2B Rh3B 123.5(5) . . ? B6B C2B Rh3B 127.1(6) . . ? B7B C2B Rh3B 65.1(3) . . ? C1B C2B H2B 119.9 . . ? B11B C2B H2B 117.3 . . ? B6B C2B H2B 114.2 . . ? B7B C2B H2B 119.5 . . ? Rh3B C2B H2B 107.0 . . ? B4B Rh3B B7B 84.8(3) . . ? B4B Rh3B B8B 49.7(3) . . ? B7B Rh3B B8B 50.1(3) . . ? B4B Rh3B C1B 47.8(3) . . ? B7B Rh3B C1B 79.3(3) . . ? B8B Rh3B C1B 81.4(3) . . ? B4B Rh3B C2B 79.5(3) . . ? B7B Rh3B C2B 47.5(3) . . ? B8B Rh3B C2B 81.4(3) . . ? C1B Rh3B C2B 42.6(3) . . ? B4B Rh3B O1B 102.3(2) . . ? B7B Rh3B O1B 160.2(3) . . ? B8B Rh3B O1B 146.4(3) . . ? C1B Rh3B O1B 91.7(2) . . ? C2B Rh3B O1B 115.0(2) . . ? B4B Rh3B O2B 152.8(2) . . ? B7B Rh3B O2B 107.2(3) . . ? B8B Rh3B O2B 154.0(2) . . ? C1B Rh3B O2B 109.3(2) . . ? C2B Rh3B O2B 90.7(2) . . ? O1B Rh3B O2B 58.97(18) . . ? B4B Rh3B P1B 105.0(2) . . ? B7B Rh3B P1B 111.4(2) . . ? B8B Rh3B P1B 85.8(2) . . ? C1B Rh3B P1B 151.2(2) . . ? C2B Rh3B P1B 158.6(2) . . ? O1B Rh3B P1B 84.87(14) . . ? O2B Rh3B P1B 93.39(13) . . ? C1B B4B B9B 101.2(6) . . ? C1B B4B B8B 105.5(6) . . ? B9B B4B B8B 60.1(4) . . ? C1B B4B B5B 56.5(5) . . ? B9B B4B B5B 58.4(5) . . ? B8B B4B B5B 107.8(6) . . ? C1B B4B Rh3B 67.6(4) . . ? B9B B4B Rh3B 118.7(5) . . ? B8B B4B Rh3B 65.7(4) . . ? B5B B4B Rh3B 119.7(5) . . ? C1B B4B H4B 126.1 . . ? B9B B4B H4B 122.6 . . ? B8B B4B H4B 122.3 . . ? B5B B4B H4B 120.7 . . ? Rh3B B4B H4B 109.0 . . ? C1B B5B B9B 104.9(6) . . ? C1B B5B B10B 104.0(7) . . ? B9B B5B B10B 59.6(5) . . ? C1B B5B B6B 59.1(5) . . ? B9B B5B B6B 108.0(7) . . ? B10B B5B B6B 59.4(6) . . ? C1B B5B B4B 60.0(5) . . ? B9B B5B B4B 59.8(5) . . ? B10B B5B B4B 107.9(6) . . ? B6B B5B B4B 109.8(6) . . ? C1B B5B H5B 124.5 . . ? B9B B5B H5B 122.6 . . ? B10B B5B H5B 123.2 . . ? B6B B5B H5B 120.9 . . ? B4B B5B H5B 120.5 . . ? C2B B6B C1B 55.5(5) . . ? C2B B6B B11B 58.1(5) . . ? C1B B6B B11B 102.8(6) . . ? C2B B6B B10B 103.8(6) . . ? C1B B6B B10B 102.9(6) . . ? B11B B6B B10B 60.7(5) . . ? C2B B6B B5B 102.5(6) . . ? C1B B6B B5B 57.6(5) . . ? B11B B6B B5B 107.5(6) . . ? B10B B6B B5B 59.4(5) . . ? C2B B6B H6B 125.8 . . ? C1B B6B H6B 126.2 . . ? B11B B6B H6B 122.2 . . ? B10B B6B H6B 123.3 . . ? B5B B6B H6B 123.0 . . ? C2B B7B B12B 101.2(6) . . ? C2B B7B B11B 56.0(5) . . ? B12B B7B B11B 58.9(5) . . ? C2B B7B B8B 104.9(6) . . ? B12B B7B B8B 60.1(5) . . ? B11B B7B B8B 107.8(6) . . ? C2B B7B Rh3B 67.4(4) . . ? B12B B7B Rh3B 118.2(5) . . ? B11B B7B Rh3B 119.0(5) . . ? B8B B7B Rh3B 65.1(4) . . ? C2B B7B H7B 126.3 . . ? B12B B7B H7B 122.4 . . ? B11B B7B H7B 120.7 . . ? B8B B7B H7B 122.7 . . ? Rh3B B7B H7B 109.7 . . ? B9B B8B B12B 59.1(5) . . ? B9B B8B B4B 59.2(4) . . ? B12B B8B B4B 105.7(6) . . ? B9B B8B B7B 105.3(6) . . ? B12B B8B B7B 58.2(5) . . ? B4B B8B B7B 105.6(6) . . ? B9B B8B Rh3B 116.9(5) . . ? B12B B8B Rh3B 116.3(5) . . ? B4B B8B Rh3B 64.6(4) . . ? B7B B8B Rh3B 64.8(4) . . ? B9B B8B H8B 121.1 . . ? B12B B8B H8B 121.6 . . ? B4B B8B H8B 123.6 . . ? B7B B8B H8B 124.1 . . ? Rh3B B8B H8B 112.2 . . ? B10B B9B B5B 60.2(5) . . ? B10B B9B B12B 59.6(5) . . ? B5B B9B B12B 107.7(7) . . ? B10B B9B B4B 109.9(6) . . ? B5B B9B B4B 61.8(5) . . ? B12B B9B B4B 108.0(6) . . ? B10B B9B B8B 110.3(6) . . ? B5B B9B B8B 111.0(6) . . ? B12B B9B B8B 60.6(4) . . ? B4B B9B B8B 60.7(4) . . ? B10B B9B H9B 120.8 . . ? B5B B9B H9B 120.6 . . ? B12B B9B H9B 122.6 . . ? B4B B9B H9B 120.8 . . ? B8B B9B H9B 119.8 . . ? B9B B10B B12B 61.0(5) . . ? B9B B10B B5B 60.1(5) . . ? B12B B10B B5B 108.7(6) . . ? B9B B10B B6B 109.8(6) . . ? B12B B10B B6B 108.5(7) . . ? B5B B10B B6B 61.2(6) . . ? B9B B10B B11B 108.6(6) . . ? B12B B10B B11B 59.9(5) . . ? B5B B10B B11B 107.7(7) . . ? B6B B10B B11B 59.2(5) . . ? B9B B10B H10B 120.6 . . ? B12B B10B H10B 121.3 . . ? B5B B10B H10B 121.4 . . ? B6B B10B H10B 121.0 . . ? B11B B10B H10B 122.3 . . ? C2B B11B B6B 59.7(5) . . ? C2B B11B B12B 105.0(6) . . ? B6B B11B B12B 109.0(7) . . ? C2B B11B B10B 104.4(7) . . ? B6B B11B B10B 60.1(5) . . ? B12B B11B B10B 59.6(5) . . ? C2B B11B B7B 60.5(5) . . ? B6B B11B B7B 111.2(6) . . ? B12B B11B B7B 59.5(5) . . ? B10B B11B B7B 107.9(6) . . ? C2B B11B H11B 124.2 . . ? B6B B11B H11B 119.8 . . ? B12B B11B H11B 122.7 . . ? B10B B11B H11B 123.1 . . ? B7B B11B H11B 120.2 . . ? B10B B12B B11B 60.6(5) . . ? B10B B12B B7B 110.4(7) . . ? B11B B12B B7B 61.6(5) . . ? B10B B12B B9B 59.3(5) . . ? B11B B12B B9B 107.8(6) . . ? B7B B12B B9B 108.9(6) . . ? B10B B12B B8B 109.8(6) . . ? B11B B12B B8B 111.2(6) . . ? B7B B12B B8B 61.7(5) . . ? B9B B12B B8B 60.3(5) . . ? B10B B12B H12B 120.9 . . ? B11B B12B H12B 120.6 . . ? B7B B12B H12B 120.0 . . ? B9B B12B H12B 122.5 . . ? B8B B12B H12B 119.8 . . ? C22B P1B C10B 107.5(3) . . ? C22B P1B C16B 108.4(3) . . ? C10B P1B C16B 102.4(3) . . ? C22B P1B Rh3B 105.5(2) . . ? C10B P1B Rh3B 112.5(2) . . ? C16B P1B Rh3B 119.9(2) . . ? N1B O1B Rh3B 93.5(4) . . ? N1B O2B Rh3B 92.4(4) . . ? O3B N1B O1B 124.1(6) . . ? O3B N1B O2B 120.7(7) . . ? O1B N1B O2B 115.1(6) . . ? C15B C10B C11B 118.5(7) . . ? C15B C10B P1B 117.3(5) . . ? C11B C10B P1B 124.1(5) . . ? C12B C11B C10B 120.0(7) . . ? C12B C11B H11C 120.0 . . ? C10B C11B H11C 120.0 . . ? C11B C12B C13B 121.2(7) . . ? C11B C12B H12C 119.4 . . ? C13B C12B H12C 119.4 . . ? C14B C13B C12B 119.6(7) . . ? C14B C13B H13B 120.2 . . ? C12B C13B H13B 120.2 . . ? C13B C14B C15B 120.2(7) . . ? C13B C14B H14B 119.9 . . ? C15B C14B H14B 119.9 . . ? C14B C15B C10B 120.5(7) . . ? C14B C15B H15B 119.8 . . ? C10B C15B H15B 119.8 . . ? C21B C16B C17B 120.1(7) . . ? C21B C16B P1B 120.1(6) . . ? C17B C16B P1B 119.7(5) . . ? C18B C17B C16B 118.8(7) . . ? C18B C17B H17B 120.6 . . ? C16B C17B H17B 120.6 . . ? C17B C18B C19B 120.5(7) . . ? C17B C18B H18B 119.8 . . ? C19B C18B H18B 119.8 . . ? C20B C19B C18B 121.1(7) . . ? C20B C19B H19B 119.5 . . ? C18B C19B H19B 119.5 . . ? C19B C20B C21B 118.8(7) . . ? C19B C20B H20B 120.6 . . ? C21B C20B H20B 120.6 . . ? C16B C21B C20B 120.7(7) . . ? C16B C21B H21B 119.7 . . ? C20B C21B H21B 119.7 . . ? C27B C22B C23B 119.1(6) . . ? C27B C22B P1B 119.3(5) . . ? C23B C22B P1B 121.4(5) . . ? C24B C23B C22B 119.4(7) . . ? C24B C23B H23B 120.3 . . ? C22B C23B H23B 120.3 . . ? C25B C24B C23B 120.2(7) . . ? C25B C24B H24B 119.9 . . ? C23B C24B H24B 119.9 . . ? C24B C25B C26B 121.3(7) . . ? C24B C25B H25B 119.3 . . ? C26B C25B H25B 119.3 . . ? C25B C26B C27B 118.9(7) . . ? C25B C26B H26B 120.5 . . ? C27B C26B H26B 120.5 . . ? C22B C27B C26B 120.9(7) . . ? C22B C27B H27B 119.5 . . ? C26B C27B H27B 119.5 . . ? Cl2 C1S Cl1 113.5(5) . . ? Cl2 C1S H1S1 108.9 . . ? Cl1 C1S H1S1 108.9 . . ? Cl2 C1S H1S2 108.9 . . ? Cl1 C1S H1S2 108.9 . . ? H1S1 C1S H1S2 107.7 . . ? Cl4A C2S Cl3B 123.8(12) . . ? Cl4A C2S Cl3A 103.8(10) . . ? Cl3B C2S Cl3A 62.7(7) . . ? Cl4A C2S H2S1 111.0 . . ? Cl3B C2S H2S1 48.4 . . ? Cl3A C2S H2S1 111.0 . . ? Cl4A C2S H2S2 111.0 . . ? Cl3B C2S H2S2 125.0 . . ? Cl3A C2S H2S2 111.0 . . ? H2S1 C2S H2S2 109.0 . . ? Cl3B Cl3B C2S 125.1(14) 2_655 . ? _diffrn_measured_fraction_theta_max 0.752 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.770 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.154 # Attachment '- compound 2.cif' data_2886 _database_code_depnum_ccdc_archive 'CCDC 891749' #TrackingRef '- compound 2.cif' _audit_update_record ; 2010-03-01 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common x82886 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H44 B9 Cl2 P2 Rh' _chemical_formula_weight 845.78 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' 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 9.7670(6) _cell_length_b 12.1220(7) _cell_length_c 19.3752(12) _cell_angle_alpha 75.731(3) _cell_angle_beta 80.599(3) _cell_angle_gamma 71.411(3) _cell_volume 2098.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 30.42 _exptl_crystal_description BLOCK _exptl_crystal_colour orange _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details 'SADABS (Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49055 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 31.07 _reflns_number_total 13335 _reflns_number_gt 10888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0421P)^2^+0.0772P] 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 13335 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 P1 P 0.42880(5) 0.24081(4) 0.16400(2) 0.01262(9) Uani 1 1 d . . . C1 C 0.3239(2) 0.52132(17) 0.22600(10) 0.0169(4) Uani 1 1 d . . . H2 H 0.4385 0.4806 0.2403 0.020 Uiso 1 1 calc R . . P2 P 0.23859(5) 0.22875(4) 0.33143(2) 0.01319(10) Uani 1 1 d . . . C2 C 0.2783(2) 0.52528(17) 0.14896(10) 0.0174(4) Uani 1 1 d . . . H1 H 0.3624 0.4843 0.1086 0.021 Uiso 1 1 calc R . . Rh3 Rh 0.238231(15) 0.365675(12) 0.225729(7) 0.01102(4) Uani 1 1 d . . . B4 B 0.1855(2) 0.50814(19) 0.28918(11) 0.0148(4) Uani 1 1 d . . . H11 H 0.2007 0.4614 0.3462 0.018 Uiso 1 1 calc R . . B5 B 0.2274(3) 0.64696(19) 0.25632(12) 0.0188(4) Uani 1 1 d . . . H10 H 0.2679 0.6881 0.2916 0.023 Uiso 1 1 calc R . . B6 B 0.2945(3) 0.6555(2) 0.16589(13) 0.0237(5) Uani 1 1 d . . . H6 H 0.3799 0.7003 0.1406 0.028 Uiso 1 1 calc R . . B7 B 0.1048(2) 0.5218(2) 0.14993(12) 0.0182(4) Uani 1 1 d . . . H4 H 0.0646 0.4858 0.1117 0.022 Uiso 1 1 calc R . . B8 B 0.0326(2) 0.5134(2) 0.24268(11) 0.0153(4) Uani 1 1 d . . . H7 H -0.0578 0.4742 0.2678 0.018 Uiso 1 1 calc R . . B9 B 0.0450(2) 0.64427(19) 0.26567(11) 0.0164(4) Uani 1 1 d . . . H12 H -0.0357 0.6842 0.3075 0.020 Uiso 1 1 calc R . . B10 B 0.1128(3) 0.7349(2) 0.18907(12) 0.0218(5) Uani 1 1 d . . . H9 H 0.0758 0.8345 0.1795 0.026 Uiso 1 1 calc R . . B11 B 0.1530(3) 0.6572(2) 0.11817(12) 0.0228(5) Uani 1 1 d . . . H5 H 0.1464 0.7043 0.0608 0.027 Uiso 1 1 calc R . . B12 B -0.0023(3) 0.6529(2) 0.17939(12) 0.0214(5) Uani 1 1 d . . . H8 H -0.1145 0.6997 0.1629 0.026 Uiso 1 1 calc R . . H31 H 0.148(3) 0.301(2) 0.2127(13) 0.036(7) Uiso 1 1 d . . . C101 C 0.3904(2) 0.22959(17) 0.07710(10) 0.0170(4) Uani 1 1 d . . . C102 C 0.5037(2) 0.16638(19) 0.03427(11) 0.0224(4) Uani 1 1 d . . . H102 H 0.5984 0.1332 0.0498 0.027 Uiso 1 1 calc R . . C103 C 0.4772(3) 0.1525(2) -0.03079(11) 0.0285(5) Uani 1 1 d . . . H103 H 0.5540 0.1102 -0.0599 0.034 Uiso 1 1 calc R . . C104 C 0.3391(3) 0.1999(2) -0.05336(12) 0.0384(6) Uani 1 1 d . . . H104 H 0.3216 0.1900 -0.0979 0.046 Uiso 1 1 calc R . . C105 C 0.2272(3) 0.2613(2) -0.01163(13) 0.0399(7) Uani 1 1 d . . . H105 H 0.1326 0.2935 -0.0273 0.048 Uiso 1 1 calc R . . C106 C 0.2530(3) 0.2764(2) 0.05430(12) 0.0269(5) Uani 1 1 d . . . H106 H 0.1758 0.3188 0.0832 0.032 Uiso 1 1 calc R . . C107 C 0.5119(2) 0.08224(17) 0.19921(10) 0.0159(4) Uani 1 1 d . . . C108 C 0.6559(2) 0.03336(18) 0.21595(11) 0.0224(4) Uani 1 1 d . . . H108 H 0.7154 0.0839 0.2113 0.027 Uiso 1 1 calc R . . C109 C 0.7121(2) -0.0884(2) 0.23929(12) 0.0287(5) Uani 1 1 d . . . H109 H 0.8104 -0.1208 0.2500 0.034 Uiso 1 1 calc R . . C110 C 0.6275(3) -0.16296(19) 0.24714(12) 0.0299(5) Uani 1 1 d . . . H110 H 0.6663 -0.2461 0.2645 0.036 Uiso 1 1 calc R . . C111 C 0.4841(3) -0.11591(19) 0.22948(11) 0.0260(5) Uani 1 1 d . . . H111 H 0.4256 -0.1671 0.2339 0.031 Uiso 1 1 calc R . . C112 C 0.4274(2) 0.00622(17) 0.20531(10) 0.0192(4) Uani 1 1 d . . . H112 H 0.3302 0.0380 0.1929 0.023 Uiso 1 1 calc R . . C113 C 0.5785(2) 0.30712(17) 0.14340(10) 0.0160(4) Uani 1 1 d . . . C114 C 0.6121(2) 0.36831(18) 0.07469(11) 0.0217(4) Uani 1 1 d . . . H114 H 0.5667 0.3662 0.0355 0.026 Uiso 1 1 calc R . . C115 C 0.7123(3) 0.4325(2) 0.06378(14) 0.0333(5) Uani 1 1 d . . . H115 H 0.7332 0.4755 0.0173 0.040 Uiso 1 1 calc R . . C116 C 0.7810(3) 0.4338(2) 0.12001(15) 0.0387(6) Uani 1 1 d . . . H116 H 0.8490 0.4778 0.1122 0.046 Uiso 1 1 calc R . . C117 C 0.7512(2) 0.3712(2) 0.18806(14) 0.0348(6) Uani 1 1 d . . . H117 H 0.8004 0.3708 0.2266 0.042 Uiso 1 1 calc R . . C118 C 0.6497(2) 0.30919(19) 0.19988(11) 0.0225(4) Uani 1 1 d . . . H118 H 0.6283 0.2677 0.2468 0.027 Uiso 1 1 calc R . . C201 C 0.1680(2) 0.10346(17) 0.33624(11) 0.0190(4) Uani 1 1 d . . . C202 C 0.0985(2) 0.09530(18) 0.28164(11) 0.0210(4) Uani 1 1 d . . . H202 H 0.0884 0.1553 0.2391 0.025 Uiso 1 1 calc R . . C203 C 0.0433(2) 0.00021(19) 0.28839(13) 0.0271(5) Uani 1 1 d . . . H203 H -0.0038 -0.0045 0.2504 0.032 Uiso 1 1 calc R . . C204 C 0.0566(3) -0.0872(2) 0.34978(14) 0.0317(5) Uani 1 1 d . . . H204 H 0.0220 -0.1535 0.3536 0.038 Uiso 1 1 calc R . . C205 C 0.1207(3) -0.0779(2) 0.40620(13) 0.0352(6) Uani 1 1 d . . . H205 H 0.1273 -0.1366 0.4493 0.042 Uiso 1 1 calc R . . C206 C 0.1750(3) 0.0169(2) 0.39964(12) 0.0314(5) Uani 1 1 d . . . H206 H 0.2175 0.0234 0.4386 0.038 Uiso 1 1 calc R . . C207 C 0.1263(2) 0.28285(16) 0.40906(10) 0.0147(4) Uani 1 1 d . . . C208 C -0.0234(2) 0.32626(18) 0.40648(10) 0.0187(4) Uani 1 1 d . . . H208 H -0.0646 0.3267 0.3652 0.022 Uiso 1 1 calc R . . C209 C -0.1136(2) 0.36891(18) 0.46337(11) 0.0212(4) Uani 1 1 d . . . H209 H -0.2156 0.3987 0.4608 0.025 Uiso 1 1 calc R . . C210 C -0.0540(2) 0.36783(18) 0.52405(11) 0.0204(4) Uani 1 1 d . . . H210 H -0.1149 0.3979 0.5629 0.025 Uiso 1 1 calc R . . C211 C 0.0940(2) 0.32283(18) 0.52761(10) 0.0201(4) Uani 1 1 d . . . H211 H 0.1347 0.3211 0.5693 0.024 Uiso 1 1 calc R . . C212 C 0.1838(2) 0.28016(18) 0.47098(10) 0.0174(4) Uani 1 1 d . . . H212 H 0.2855 0.2488 0.4743 0.021 Uiso 1 1 calc R . . C214 C 0.4935(3) 0.0430(2) 0.37667(12) 0.0310(5) Uani 1 1 d . . . H214 H 0.4496 -0.0125 0.3697 0.037 Uiso 1 1 calc R . . C215 C 0.6324(3) 0.0029(2) 0.39998(13) 0.0422(7) Uani 1 1 d . . . H215 H 0.6822 -0.0798 0.4087 0.051 Uiso 1 1 calc R . . C216 C 0.6981(3) 0.0817(3) 0.41047(12) 0.0401(7) Uani 1 1 d . . . H216 H 0.7922 0.0535 0.4268 0.048 Uiso 1 1 calc R . . C217 C 0.6261(2) 0.2027(2) 0.39706(11) 0.0314(5) Uani 1 1 d . . . H217 H 0.6711 0.2576 0.4039 0.038 Uiso 1 1 calc R . . C218 C 0.4881(2) 0.2434(2) 0.37357(11) 0.0228(4) Uani 1 1 d . . . H218 H 0.4397 0.3263 0.3641 0.027 Uiso 1 1 calc R . . C219 C 0.4193(2) 0.16365(18) 0.36364(10) 0.0189(4) Uani 1 1 d . . . Cl1S Cl 0.54222(8) 0.64849(7) 0.46271(4) 0.05118(19) Uani 1 1 d . . . C1S C 0.4625(3) 0.6246(3) 0.39473(13) 0.0406(7) Uani 1 1 d . . . H2S H 0.4150 0.7023 0.3647 0.049 Uiso 1 1 calc R . . H1S H 0.3869 0.5850 0.4166 0.049 Uiso 1 1 calc R . . Cl2S Cl 0.59127(6) 0.53612(5) 0.34015(3) 0.03246(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 P1 0.0151(2) 0.0114(2) 0.0112(2) -0.00364(17) -0.00128(17) -0.00265(18) C1 0.0179(9) 0.0123(9) 0.0213(9) -0.0040(7) -0.0034(7) -0.0044(7) P2 0.0173(2) 0.0112(2) 0.0107(2) -0.00303(17) -0.00074(17) -0.00329(18) C2 0.0222(10) 0.0112(9) 0.0154(9) -0.0004(7) 0.0001(7) -0.0030(7) Rh3 0.01227(7) 0.01042(7) 0.01049(7) -0.00269(5) -0.00163(5) -0.00277(5) B4 0.0181(10) 0.0122(10) 0.0143(10) -0.0026(8) -0.0040(8) -0.0036(8) B5 0.0227(11) 0.0109(10) 0.0230(11) -0.0040(8) -0.0047(9) -0.0035(8) B6 0.0295(13) 0.0149(11) 0.0267(12) -0.0031(9) 0.0020(10) -0.0094(10) B7 0.0186(11) 0.0169(11) 0.0169(10) -0.0054(8) -0.0055(8) 0.0012(8) B8 0.0155(10) 0.0179(11) 0.0138(10) -0.0064(8) -0.0011(8) -0.0043(8) B9 0.0197(10) 0.0131(10) 0.0151(10) -0.0046(8) -0.0023(8) -0.0013(8) B10 0.0300(13) 0.0107(10) 0.0199(11) -0.0016(8) -0.0027(9) -0.0002(9) B11 0.0310(13) 0.0142(11) 0.0152(10) -0.0002(8) 0.0002(9) 0.0013(9) B12 0.0205(11) 0.0203(11) 0.0184(11) -0.0067(9) -0.0074(9) 0.0055(9) C101 0.0278(10) 0.0116(9) 0.0124(8) -0.0025(7) -0.0037(7) -0.0062(8) C102 0.0282(11) 0.0216(11) 0.0183(10) -0.0081(8) -0.0007(8) -0.0065(9) C103 0.0446(14) 0.0242(11) 0.0179(10) -0.0105(9) 0.0020(9) -0.0092(10) C104 0.0625(18) 0.0317(13) 0.0197(11) -0.0115(10) -0.0155(11) -0.0018(12) C105 0.0508(16) 0.0372(14) 0.0291(12) -0.0163(11) -0.0231(12) 0.0071(12) C106 0.0351(12) 0.0233(11) 0.0222(10) -0.0109(9) -0.0112(9) 0.0004(9) C107 0.0204(9) 0.0131(9) 0.0119(8) -0.0034(7) 0.0022(7) -0.0028(7) C108 0.0218(10) 0.0165(10) 0.0244(10) -0.0019(8) -0.0005(8) -0.0022(8) C109 0.0226(11) 0.0228(11) 0.0288(12) 0.0004(9) 0.0004(9) 0.0039(9) C110 0.0408(14) 0.0124(10) 0.0254(11) -0.0031(8) 0.0052(10) 0.0029(9) C111 0.0370(13) 0.0166(10) 0.0227(11) -0.0052(8) 0.0050(9) -0.0086(9) C112 0.0246(10) 0.0147(9) 0.0174(9) -0.0045(7) 0.0014(8) -0.0051(8) C113 0.0152(9) 0.0145(9) 0.0185(9) -0.0066(7) 0.0013(7) -0.0036(7) C114 0.0222(10) 0.0219(11) 0.0213(10) -0.0067(8) 0.0031(8) -0.0075(8) C115 0.0346(13) 0.0342(13) 0.0347(13) -0.0096(10) 0.0131(10) -0.0213(11) C116 0.0297(13) 0.0456(16) 0.0539(17) -0.0260(13) 0.0110(11) -0.0243(12) C117 0.0230(11) 0.0507(16) 0.0431(15) -0.0303(13) 0.0019(10) -0.0146(11) C118 0.0187(10) 0.0285(11) 0.0222(10) -0.0122(9) 0.0003(8) -0.0051(8) C201 0.0250(10) 0.0125(9) 0.0196(9) -0.0065(7) 0.0054(8) -0.0069(8) C202 0.0214(10) 0.0191(10) 0.0241(10) -0.0070(8) 0.0020(8) -0.0081(8) C203 0.0259(11) 0.0233(11) 0.0370(13) -0.0134(10) 0.0042(9) -0.0121(9) C204 0.0349(13) 0.0182(11) 0.0454(14) -0.0147(10) 0.0135(11) -0.0148(10) C205 0.0577(17) 0.0196(11) 0.0269(12) -0.0034(9) 0.0100(11) -0.0172(11) C206 0.0571(16) 0.0199(11) 0.0198(10) -0.0047(9) 0.0036(10) -0.0178(11) C207 0.0196(9) 0.0115(9) 0.0124(8) -0.0030(7) 0.0019(7) -0.0051(7) C208 0.0211(10) 0.0203(10) 0.0143(9) -0.0035(7) -0.0013(7) -0.0057(8) C209 0.0186(10) 0.0210(10) 0.0219(10) -0.0031(8) 0.0039(8) -0.0066(8) C210 0.0252(10) 0.0172(10) 0.0177(9) -0.0060(8) 0.0058(8) -0.0066(8) C211 0.0267(11) 0.0218(10) 0.0135(9) -0.0058(8) -0.0004(8) -0.0085(8) C212 0.0186(9) 0.0202(10) 0.0143(9) -0.0049(7) -0.0008(7) -0.0061(8) C214 0.0398(13) 0.0223(11) 0.0223(11) -0.0078(9) -0.0090(10) 0.0081(10) C215 0.0428(15) 0.0392(15) 0.0274(12) -0.0128(11) -0.0146(11) 0.0217(12) C216 0.0248(12) 0.0660(19) 0.0171(11) -0.0153(11) -0.0089(9) 0.0124(12) C217 0.0200(10) 0.0548(16) 0.0163(10) -0.0052(10) -0.0038(8) -0.0074(10) C218 0.0176(10) 0.0289(11) 0.0175(10) -0.0019(8) -0.0010(8) -0.0030(8) C219 0.0186(9) 0.0220(10) 0.0108(8) -0.0041(7) -0.0001(7) 0.0012(8) Cl1S 0.0507(4) 0.0749(5) 0.0412(4) -0.0293(4) -0.0089(3) -0.0212(4) C1S 0.0280(13) 0.0679(19) 0.0304(13) -0.0232(13) -0.0034(10) -0.0101(13) Cl2S 0.0333(3) 0.0349(3) 0.0293(3) -0.0091(2) -0.0039(2) -0.0077(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 P1 C113 1.8285(19) . ? P1 C101 1.8293(18) . ? P1 C107 1.8327(19) . ? P1 Rh3 2.3568(5) . ? C1 C2 1.612(3) . ? C1 B4 1.689(3) . ? C1 B5 1.702(3) . ? C1 B6 1.721(3) . ? C1 Rh3 2.2964(18) . ? C1 H2 1.1200 . ? P2 C219 1.832(2) . ? P2 C201 1.835(2) . ? P2 C207 1.8394(18) . ? P2 Rh3 2.2961(5) . ? C2 B7 1.705(3) . ? C2 B11 1.712(3) . ? C2 B6 1.748(3) . ? C2 Rh3 2.2320(19) . ? C2 H1 1.1200 . ? Rh3 B4 2.243(2) . ? Rh3 B7 2.262(2) . ? Rh3 B8 2.265(2) . ? Rh3 H31 1.44(2) . ? B4 B9 1.790(3) . ? B4 B5 1.797(3) . ? B4 B8 1.843(3) . ? B4 H11 1.1200 . ? B5 B6 1.758(3) . ? B5 B10 1.766(3) . ? B5 B9 1.771(3) . ? B5 H10 1.1200 . ? B6 B10 1.773(3) . ? B6 B11 1.777(4) . ? B6 H6 1.1200 . ? B7 B12 1.772(3) . ? B7 B11 1.788(3) . ? B7 B8 1.811(3) . ? B7 H4 1.1200 . ? B8 B9 1.794(3) . ? B8 B12 1.796(3) . ? B8 H7 1.1200 . ? B9 B12 1.776(3) . ? B9 B10 1.785(3) . ? B9 H12 1.1200 . ? B10 B11 1.776(3) . ? B10 B12 1.778(4) . ? B10 H9 1.1200 . ? B11 B12 1.773(3) . ? B11 H5 1.1200 . ? B12 H8 1.1200 . ? C101 C106 1.379(3) . ? C101 C102 1.405(3) . ? C102 C103 1.387(3) . ? C102 H102 0.9500 . ? C103 C104 1.383(3) . ? C103 H103 0.9500 . ? C104 C105 1.376(4) . ? C104 H104 0.9500 . ? C105 C106 1.406(3) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C112 1.394(3) . ? C107 C108 1.399(3) . ? C108 C109 1.386(3) . ? C108 H108 0.9500 . ? C109 C110 1.375(3) . ? C109 H109 0.9500 . ? C110 C111 1.398(3) . ? C110 H110 0.9500 . ? C111 C112 1.392(3) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C113 C118 1.398(3) . ? C113 C114 1.399(3) . ? C114 C115 1.394(3) . ? C114 H114 0.9500 . ? C115 C116 1.376(4) . ? C115 H115 0.9500 . ? C116 C117 1.386(4) . ? C116 H116 0.9500 . ? C117 C118 1.384(3) . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C201 C202 1.385(3) . ? C201 C206 1.400(3) . ? C202 C203 1.391(3) . ? C202 H202 0.9500 . ? C203 C204 1.377(3) . ? C203 H203 0.9500 . ? C204 C205 1.389(3) . ? C204 H204 0.9500 . ? C205 C206 1.383(3) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C207 C208 1.392(3) . ? C207 C212 1.395(2) . ? C208 C209 1.390(3) . ? C208 H208 0.9500 . ? C209 C210 1.390(3) . ? C209 H209 0.9500 . ? C210 C211 1.380(3) . ? C210 H210 0.9500 . ? C211 C212 1.385(3) . ? C211 H211 0.9500 . ? C212 H212 0.9500 . ? C214 C219 1.389(3) . ? C214 C215 1.398(3) . ? C214 H214 0.9500 . ? C215 C216 1.377(4) . ? C215 H215 0.9500 . ? C216 C217 1.388(4) . ? C216 H216 0.9500 . ? C217 C218 1.390(3) . ? C217 H217 0.9500 . ? C218 C219 1.403(3) . ? C218 H218 0.9500 . ? Cl1S C1S 1.758(2) . ? C1S Cl2S 1.765(3) . ? C1S H2S 0.9900 . ? C1S H1S 0.9900 . ? 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 C113 P1 C101 104.60(9) . . ? C113 P1 C107 105.30(9) . . ? C101 P1 C107 98.36(8) . . ? C113 P1 Rh3 106.98(6) . . ? C101 P1 Rh3 115.43(7) . . ? C107 P1 Rh3 124.29(6) . . ? C2 C1 B4 109.66(14) . . ? C2 C1 B5 110.94(15) . . ? B4 C1 B5 64.00(13) . . ? C2 C1 B6 63.18(13) . . ? B4 C1 B6 115.41(16) . . ? B5 C1 B6 61.78(13) . . ? C2 C1 Rh3 67.03(9) . . ? B4 C1 Rh3 66.49(9) . . ? B5 C1 Rh3 125.70(13) . . ? B6 C1 Rh3 127.11(13) . . ? C2 C1 H2 122.0 . . ? B4 C1 H2 119.7 . . ? B5 C1 H2 116.6 . . ? B6 C1 H2 114.3 . . ? Rh3 C1 H2 106.2 . . ? C219 P2 C201 106.17(10) . . ? C219 P2 C207 102.67(9) . . ? C201 P2 C207 97.62(9) . . ? C219 P2 Rh3 112.30(7) . . ? C201 P2 Rh3 118.92(7) . . ? C207 P2 Rh3 117.02(6) . . ? C1 C2 B7 114.36(15) . . ? C1 C2 B11 111.54(15) . . ? B7 C2 B11 63.09(13) . . ? C1 C2 B6 61.46(12) . . ? B7 C2 B6 115.25(16) . . ? B11 C2 B6 61.77(13) . . ? C1 C2 Rh3 71.31(10) . . ? B7 C2 Rh3 68.65(10) . . ? B11 C2 Rh3 127.69(14) . . ? B6 C2 Rh3 129.52(13) . . ? C1 C2 H1 119.5 . . ? B7 C2 H1 118.2 . . ? B11 C2 H1 117.3 . . ? B6 C2 H1 115.5 . . ? Rh3 C2 H1 102.2 . . ? C2 Rh3 B4 74.17(7) . . ? C2 Rh3 B7 44.59(8) . . ? B4 Rh3 B7 79.61(8) . . ? C2 Rh3 B8 76.46(8) . . ? B4 Rh3 B8 48.25(7) . . ? B7 Rh3 B8 47.15(8) . . ? C2 Rh3 P2 157.82(5) . . ? B4 Rh3 P2 88.65(6) . . ? B7 Rh3 P2 146.70(6) . . ? B8 Rh3 P2 102.71(6) . . ? C2 Rh3 C1 41.67(7) . . ? B4 Rh3 C1 43.67(7) . . ? B7 Rh3 C1 75.40(8) . . ? B8 Rh3 C1 77.03(7) . . ? P2 Rh3 C1 116.21(5) . . ? C2 Rh3 P1 90.07(5) . . ? B4 Rh3 P1 143.75(6) . . ? B7 Rh3 P1 111.84(6) . . ? B8 Rh3 P1 158.55(5) . . ? P2 Rh3 P1 96.043(18) . . ? C1 Rh3 P1 103.99(5) . . ? C2 Rh3 H31 123.2(10) . . ? B4 Rh3 H31 129.8(10) . . ? B7 Rh3 H31 85.3(10) . . ? B8 Rh3 H31 87.3(10) . . ? P2 Rh3 H31 78.5(10) . . ? C1 Rh3 H31 160.3(10) . . ? P1 Rh3 H31 86.3(10) . . ? C1 B4 B9 104.06(15) . . ? C1 B4 B5 58.36(12) . . ? B9 B4 B5 59.16(12) . . ? C1 B4 B8 107.00(14) . . ? B9 B4 B8 59.18(12) . . ? B5 B4 B8 107.80(15) . . ? C1 B4 Rh3 69.84(10) . . ? B9 B4 Rh3 120.53(12) . . ? B5 B4 Rh3 123.69(13) . . ? B8 B4 Rh3 66.49(9) . . ? C1 B4 H11 123.7 . . ? B9 B4 H11 122.0 . . ? B5 B4 H11 119.3 . . ? B8 B4 H11 123.1 . . ? Rh3 B4 H11 106.5 . . ? C1 B5 B6 59.62(13) . . ? C1 B5 B10 105.59(16) . . ? B6 B5 B10 60.41(14) . . ? C1 B5 B9 104.32(15) . . ? B6 B5 B9 108.86(16) . . ? B10 B5 B9 60.63(13) . . ? C1 B5 B4 57.64(12) . . ? B6 B5 B4 108.35(15) . . ? B10 B5 B4 108.85(16) . . ? B9 B5 B4 60.20(12) . . ? C1 B5 H10 124.9 . . ? B6 B5 H10 120.7 . . ? B10 B5 H10 121.5 . . ? B9 B5 H10 122.1 . . ? B4 B5 H10 121.6 . . ? C1 B6 C2 55.36(11) . . ? C1 B6 B5 58.59(13) . . ? C2 B6 B5 102.33(16) . . ? C1 B6 B10 104.52(16) . . ? C2 B6 B10 103.24(16) . . ? B5 B6 B10 60.03(13) . . ? C1 B6 B11 103.60(16) . . ? C2 B6 B11 58.12(12) . . ? B5 B6 B11 107.50(17) . . ? B10 B6 B11 60.05(14) . . ? C1 B6 H6 125.1 . . ? C2 B6 H6 126.4 . . ? B5 B6 H6 122.7 . . ? B10 B6 H6 123.0 . . ? B11 B6 H6 122.3 . . ? C2 B7 B12 103.61(16) . . ? C2 B7 B11 58.65(13) . . ? B12 B7 B11 59.73(13) . . ? C2 B7 B8 104.60(14) . . ? B12 B7 B8 60.18(13) . . ? B11 B7 B8 108.68(15) . . ? C2 B7 Rh3 66.76(9) . . ? B12 B7 Rh3 120.95(13) . . ? B11 B7 Rh3 121.87(13) . . ? B8 B7 Rh3 66.49(10) . . ? C2 B7 H4 125.9 . . ? B12 B7 H4 120.9 . . ? B11 B7 H4 118.9 . . ? B8 B7 H4 122.9 . . ? Rh3 B7 H4 108.0 . . ? B9 B8 B12 59.29(12) . . ? B9 B8 B7 105.52(15) . . ? B12 B8 B7 58.83(12) . . ? B9 B8 B4 58.94(11) . . ? B12 B8 B4 105.12(15) . . ? B7 B8 B4 104.27(14) . . ? B9 B8 Rh3 119.20(13) . . ? B12 B8 Rh3 119.64(13) . . ? B7 B8 Rh3 66.35(9) . . ? B4 B8 Rh3 65.26(9) . . ? B9 B8 H7 120.7 . . ? B12 B8 H7 120.7 . . ? B7 B8 H7 124.3 . . ? B4 B8 H7 124.9 . . ? Rh3 B8 H7 109.6 . . ? B5 B9 B12 107.64(16) . . ? B5 B9 B10 59.55(13) . . ? B12 B9 B10 59.89(13) . . ? B5 B9 B4 60.64(12) . . ? B12 B9 B4 108.26(15) . . ? B10 B9 B4 108.34(16) . . ? B5 B9 B8 111.18(15) . . ? B12 B9 B8 60.41(12) . . ? B10 B9 B8 110.06(15) . . ? B4 B9 B8 61.88(12) . . ? B5 B9 H12 121.1 . . ? B12 B9 H12 122.3 . . ? B10 B9 H12 121.6 . . ? B4 B9 H12 121.1 . . ? B8 B9 H12 119.2 . . ? B5 B10 B6 59.56(13) . . ? B5 B10 B11 107.15(16) . . ? B6 B10 B11 60.08(14) . . ? B5 B10 B12 107.78(16) . . ? B6 B10 B12 108.27(16) . . ? B11 B10 B12 59.84(14) . . ? B5 B10 B9 59.82(13) . . ? B6 B10 B9 107.53(16) . . ? B11 B10 B9 107.08(16) . . ? B12 B10 B9 59.80(13) . . ? B5 B10 H9 122.2 . . ? B6 B10 H9 121.7 . . ? B11 B10 H9 122.2 . . ? B12 B10 H9 121.6 . . ? B9 B10 H9 122.2 . . ? C2 B11 B12 103.28(16) . . ? C2 B11 B10 104.60(16) . . ? B12 B11 B10 60.13(13) . . ? C2 B11 B6 60.11(13) . . ? B12 B11 B6 108.34(16) . . ? B10 B11 B6 59.87(14) . . ? C2 B11 B7 58.26(12) . . ? B12 B11 B7 59.68(13) . . ? B10 B11 B7 108.56(16) . . ? B6 B11 B7 109.82(16) . . ? C2 B11 H5 125.2 . . ? B12 B11 H5 123.1 . . ? B10 B11 H5 122.3 . . ? B6 B11 H5 120.2 . . ? B7 B11 H5 120.9 . . ? B7 B12 B11 60.59(13) . . ? B7 B12 B9 107.98(15) . . ? B11 B12 B9 107.63(16) . . ? B7 B12 B10 109.21(17) . . ? B11 B12 B10 60.03(14) . . ? B9 B12 B10 60.31(13) . . ? B7 B12 B8 60.99(12) . . ? B11 B12 B8 110.03(15) . . ? B9 B12 B8 60.29(12) . . ? B10 B12 B8 110.31(15) . . ? B7 B12 H8 121.2 . . ? B11 B12 H8 121.4 . . ? B9 B12 H8 122.3 . . ? B10 B12 H8 120.7 . . ? B8 B12 H8 120.0 . . ? C106 C101 C102 119.57(18) . . ? C106 C101 P1 121.97(15) . . ? C102 C101 P1 118.39(15) . . ? C103 C102 C101 119.9(2) . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C104 C103 C102 120.2(2) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C105 C104 C103 120.4(2) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C104 C105 C106 119.9(2) . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C101 C106 C105 120.0(2) . . ? C101 C106 H106 120.0 . . ? C105 C106 H106 120.0 . . ? C112 C107 C108 118.87(18) . . ? C112 C107 P1 117.04(15) . . ? C108 C107 P1 123.98(15) . . ? C109 C108 C107 120.2(2) . . ? C109 C108 H108 119.9 . . ? C107 C108 H108 119.9 . . ? C110 C109 C108 120.8(2) . . ? C110 C109 H109 119.6 . . ? C108 C109 H109 119.6 . . ? C109 C110 C111 119.7(2) . . ? C109 C110 H110 120.2 . . ? C111 C110 H110 120.2 . . ? C112 C111 C110 119.8(2) . . ? C112 C111 H111 120.1 . . ? C110 C111 H111 120.1 . . ? C111 C112 C107 120.56(19) . . ? C111 C112 H112 119.7 . . ? C107 C112 H112 119.7 . . ? C118 C113 C114 118.83(19) . . ? C118 C113 P1 118.52(15) . . ? C114 C113 P1 122.17(15) . . ? C115 C114 C113 120.0(2) . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C116 C115 C114 120.3(2) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C117 120.2(2) . . ? C115 C116 H116 119.9 . . ? C117 C116 H116 119.9 . . ? C118 C117 C116 120.0(2) . . ? C118 C117 H117 120.0 . . ? C116 C117 H117 120.0 . . ? C117 C118 C113 120.6(2) . . ? C117 C118 H118 119.7 . . ? C113 C118 H118 119.7 . . ? C202 C201 C206 118.34(19) . . ? C202 C201 P2 122.68(15) . . ? C206 C201 P2 118.80(16) . . ? C201 C202 C203 120.7(2) . . ? C201 C202 H202 119.6 . . ? C203 C202 H202 119.6 . . ? C204 C203 C202 120.3(2) . . ? C204 C203 H203 119.8 . . ? C202 C203 H203 119.8 . . ? C203 C204 C205 119.7(2) . . ? C203 C204 H204 120.1 . . ? C205 C204 H204 120.1 . . ? C206 C205 C204 119.9(2) . . ? C206 C205 H205 120.0 . . ? C204 C205 H205 120.0 . . ? C205 C206 C201 120.8(2) . . ? C205 C206 H206 119.6 . . ? C201 C206 H206 119.6 . . ? C208 C207 C212 118.43(17) . . ? C208 C207 P2 118.46(14) . . ? C212 C207 P2 123.10(15) . . ? C209 C208 C207 121.01(18) . . ? C209 C208 H208 119.5 . . ? C207 C208 H208 119.5 . . ? C208 C209 C210 119.74(19) . . ? C208 C209 H209 120.1 . . ? C210 C209 H209 120.1 . . ? C211 C210 C209 119.63(18) . . ? C211 C210 H210 120.2 . . ? C209 C210 H210 120.2 . . ? C210 C211 C212 120.63(18) . . ? C210 C211 H211 119.7 . . ? C212 C211 H211 119.7 . . ? C211 C212 C207 120.54(18) . . ? C211 C212 H212 119.7 . . ? C207 C212 H212 119.7 . . ? C219 C214 C215 120.3(2) . . ? C219 C214 H214 119.8 . . ? C215 C214 H214 119.8 . . ? C216 C215 C214 120.8(2) . . ? C216 C215 H215 119.6 . . ? C214 C215 H215 119.6 . . ? C215 C216 C217 119.6(2) . . ? C215 C216 H216 120.2 . . ? C217 C216 H216 120.2 . . ? C216 C217 C218 119.9(2) . . ? C216 C217 H217 120.1 . . ? C218 C217 H217 120.1 . . ? C217 C218 C219 121.0(2) . . ? C217 C218 H218 119.5 . . ? C219 C218 H218 119.5 . . ? C214 C219 C218 118.38(19) . . ? C214 C219 P2 124.94(17) . . ? C218 C219 P2 116.65(15) . . ? Cl1S C1S Cl2S 112.00(14) . . ? Cl1S C1S H2S 109.2 . . ? Cl2S C1S H2S 109.2 . . ? Cl1S C1S H1S 109.2 . . ? Cl2S C1S H1S 109.2 . . ? H2S C1S H1S 107.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.094