# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'N. Connelly' _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_section_title ; A novel route to rhodaboratranes [Rh(CO)(PR3){B(taz)3}]+ via the redox activation of scorpionate complexes [RhLL'(Tt)] ; loop_ _publ_author_name 'N. Connelly' 'Chris Adams' 'Robin J. Blagg' 'Jonathan Charmant' 'Mairi F. Haddow' 'Alex Hamilton' ; J.Knight ; 'A. Orpen' 'Benjamin M. Ridgway' # Attachment 'Revised_cifs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 733499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 B N6 Rh S2' _chemical_formula_sum 'C18 H30 B N6 Rh S2' _chemical_formula_weight 508.32 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.548(2) _cell_length_b 13.774(2) _cell_length_c 24.862(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4297.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'SADABS V2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29091 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4925 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+2.8412P] 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 4925 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.235658(15) 0.097011(14) 0.695492(8) 0.00962(6) Uani 1 1 d . . . S1 S 0.10874(5) 0.21820(5) 0.66316(3) 0.01386(14) Uani 1 1 d . . . S2 S 0.14185(5) -0.03859(5) 0.66028(3) 0.01441(14) Uani 1 1 d . . . N1 N 0.20918(16) 0.21105(15) 0.56502(8) 0.0112(4) Uani 1 1 d . . . N2 N 0.20795(17) 0.25920(15) 0.51588(9) 0.0130(4) Uani 1 1 d . . . N3 N 0.09969(16) 0.33115(15) 0.57354(9) 0.0128(5) Uani 1 1 d . . . N4 N 0.19539(16) 0.02851(15) 0.55916(8) 0.0105(4) Uani 1 1 d . . . N5 N 0.17262(16) 0.00639(15) 0.50566(8) 0.0123(4) Uani 1 1 d . . . N6 N 0.09001(16) -0.09603(15) 0.55958(8) 0.0113(4) Uani 1 1 d . . . B1 B 0.2712(2) 0.1144(2) 0.57182(12) 0.0116(6) Uani 1 1 d . . . H1A H 0.3330 0.1131 0.5470 0.014 Uiso 1 1 calc R . . H1B H 0.2982 0.1088 0.6091 0.014 Uiso 1 1 calc R . . C2 C 0.14268(19) 0.25298(17) 0.59993(10) 0.0113(5) Uani 1 1 d . . . C3 C 0.1411(2) 0.33060(18) 0.52225(11) 0.0131(5) Uani 1 1 d . . . C4 C 0.1098(2) 0.40074(19) 0.47958(11) 0.0169(5) Uani 1 1 d . . . H4A H 0.1482 0.3856 0.4463 0.025 Uiso 1 1 calc R . . H4B H 0.1275 0.4668 0.4912 0.025 Uiso 1 1 calc R . . H4C H 0.0329 0.3960 0.4732 0.025 Uiso 1 1 calc R . . C5 C 0.0272(2) 0.40310(19) 0.59715(12) 0.0173(6) Uani 1 1 d . . . H5A H 0.0364 0.4656 0.5781 0.021 Uiso 1 1 calc R . . H5B H 0.0471 0.4134 0.6353 0.021 Uiso 1 1 calc R . . C6 C -0.0889(2) 0.3736(2) 0.59445(12) 0.0201(6) Uani 1 1 d . . . H6A H -0.1094 0.3633 0.5568 0.030 Uiso 1 1 calc R . . H6B H -0.1331 0.4251 0.6100 0.030 Uiso 1 1 calc R . . H6C H -0.0994 0.3134 0.6147 0.030 Uiso 1 1 calc R . . C7 C 0.14446(19) -0.03276(17) 0.59188(10) 0.0109(5) Uani 1 1 d . . . C8 C 0.1103(2) -0.06867(18) 0.50730(10) 0.0115(5) Uani 1 1 d . . . C9 C 0.0685(2) -0.1207(2) 0.45962(11) 0.0171(6) Uani 1 1 d . . . H9A H 0.0838 -0.0828 0.4271 0.026 Uiso 1 1 calc R . . H9B H -0.0087 -0.1292 0.4633 0.026 Uiso 1 1 calc R . . H9C H 0.1028 -0.1844 0.4569 0.026 Uiso 1 1 calc R . . C10 C 0.0295(2) -0.18091(19) 0.57793(11) 0.0151(5) Uani 1 1 d . . . H10A H 0.0712 -0.2152 0.6059 0.018 Uiso 1 1 calc R . . H10B H 0.0199 -0.2260 0.5473 0.018 Uiso 1 1 calc R . . C11 C -0.0796(2) -0.1548(2) 0.60081(12) 0.0205(6) Uani 1 1 d . . . H11A H -0.0708 -0.1106 0.6314 0.031 Uiso 1 1 calc R . . H11B H -0.1158 -0.2140 0.6128 0.031 Uiso 1 1 calc R . . H11C H -0.1225 -0.1231 0.5729 0.031 Uiso 1 1 calc R . . C12 C 0.3496(2) 0.00086(19) 0.72998(11) 0.0153(5) Uani 1 1 d . . . H12 H 0.3565 -0.0624 0.7106 0.018 Uiso 1 1 calc R . . C13 C 0.2593(2) 0.00667(19) 0.76367(10) 0.0143(5) Uani 1 1 d . . . H13 H 0.2145 -0.0534 0.7633 0.017 Uiso 1 1 calc R . . C14 C 0.2527(2) 0.0625(2) 0.81581(10) 0.0162(5) Uani 1 1 d . . . H14A H 0.2918 0.0266 0.8441 0.019 Uiso 1 1 calc R . . H14B H 0.1772 0.0673 0.8270 0.019 Uiso 1 1 calc R . . C15 C 0.2996(2) 0.1649(2) 0.81067(11) 0.0175(6) Uani 1 1 d . . . H15A H 0.2661 0.2080 0.8377 0.021 Uiso 1 1 calc R . . H15B H 0.3770 0.1626 0.8181 0.021 Uiso 1 1 calc R . . C16 C 0.2810(2) 0.20615(19) 0.75471(11) 0.0155(5) Uani 1 1 d . . . H16 H 0.2351 0.2655 0.7542 0.019 Uiso 1 1 calc R . . C17 C 0.3547(2) 0.20249(19) 0.71322(11) 0.0164(6) Uani 1 1 d . . . H17 H 0.3528 0.2604 0.6890 0.020 Uiso 1 1 calc R . . C18 C 0.4612(2) 0.1522(2) 0.71471(12) 0.0206(6) Uani 1 1 d . . . H18A H 0.5123 0.1928 0.7351 0.025 Uiso 1 1 calc R . . H18B H 0.4886 0.1454 0.6775 0.025 Uiso 1 1 calc R . . C19 C 0.4550(2) 0.0509(2) 0.74094(11) 0.0198(6) Uani 1 1 d . . . H19A H 0.5137 0.0100 0.7269 0.024 Uiso 1 1 calc R . . H19B H 0.4649 0.0575 0.7803 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00959(10) 0.00996(10) 0.00932(10) 0.00053(8) -0.00160(8) -0.00020(7) S1 0.0144(3) 0.0155(3) 0.0117(3) 0.0024(3) 0.0005(3) 0.0043(2) S2 0.0200(3) 0.0137(3) 0.0096(3) 0.0006(3) -0.0006(3) -0.0049(3) N1 0.0112(10) 0.0101(10) 0.0122(11) 0.0015(9) -0.0004(8) -0.0006(8) N2 0.0137(10) 0.0130(10) 0.0122(11) 0.0042(9) -0.0030(9) -0.0024(8) N3 0.0126(10) 0.0100(10) 0.0159(12) 0.0017(9) -0.0020(9) -0.0007(8) N4 0.0114(10) 0.0103(10) 0.0100(10) 0.0003(8) -0.0008(8) 0.0008(8) N5 0.0133(10) 0.0141(11) 0.0095(11) -0.0014(9) -0.0020(9) 0.0008(8) N6 0.0123(10) 0.0102(10) 0.0115(11) -0.0015(9) -0.0011(8) -0.0006(8) B1 0.0115(13) 0.0133(14) 0.0101(14) 0.0012(11) -0.0008(11) 0.0007(11) C2 0.0096(11) 0.0091(11) 0.0152(13) 0.0010(10) -0.0040(10) -0.0014(9) C3 0.0122(12) 0.0118(12) 0.0154(13) 0.0001(10) -0.0026(10) -0.0044(10) C4 0.0167(13) 0.0166(13) 0.0175(14) 0.0034(12) -0.0041(11) -0.0015(11) C5 0.0203(13) 0.0113(12) 0.0203(14) -0.0030(12) -0.0038(11) 0.0045(11) C6 0.0183(14) 0.0175(13) 0.0245(16) 0.0018(12) 0.0040(12) 0.0056(11) C7 0.0115(11) 0.0083(11) 0.0129(12) -0.0016(10) -0.0006(10) 0.0023(9) C8 0.0106(12) 0.0128(12) 0.0110(12) -0.0006(10) -0.0009(10) 0.0033(9) C9 0.0174(13) 0.0190(14) 0.0148(14) -0.0055(11) -0.0020(11) 0.0002(10) C10 0.0170(13) 0.0116(12) 0.0168(14) 0.0008(11) -0.0024(11) -0.0057(10) C11 0.0179(14) 0.0231(15) 0.0207(15) 0.0040(12) 0.0013(12) -0.0060(11) C12 0.0165(13) 0.0154(12) 0.0139(13) 0.0020(11) -0.0025(11) 0.0043(10) C13 0.0154(12) 0.0140(12) 0.0137(13) 0.0041(10) -0.0016(11) 0.0018(10) C14 0.0140(13) 0.0236(14) 0.0110(13) 0.0026(11) -0.0009(10) -0.0004(10) C15 0.0171(13) 0.0244(15) 0.0111(13) -0.0035(11) -0.0006(11) -0.0031(11) C16 0.0188(13) 0.0128(12) 0.0148(13) -0.0031(11) -0.0030(11) -0.0033(10) C17 0.0208(14) 0.0149(13) 0.0136(13) 0.0016(11) -0.0044(11) -0.0076(11) C18 0.0145(13) 0.0321(17) 0.0154(14) 0.0000(12) -0.0009(11) -0.0072(12) C19 0.0119(12) 0.0324(16) 0.0150(14) 0.0005(12) -0.0003(11) 0.0035(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 C13 2.124(3) . ? Rh1 C12 2.129(2) . ? Rh1 C17 2.130(3) . ? Rh1 C16 2.180(3) . ? Rh1 S2 2.3750(7) . ? Rh1 S1 2.4431(7) . ? S1 C2 1.698(3) . ? S2 C7 1.703(3) . ? N1 C2 1.335(3) . ? N1 N2 1.390(3) . ? N1 B1 1.552(3) . ? N2 C3 1.302(3) . ? N3 C2 1.371(3) . ? N3 C3 1.377(3) . ? N3 C5 1.468(3) . ? N4 C7 1.335(3) . ? N4 N5 1.394(3) . ? N4 B1 1.550(3) . ? N5 C8 1.297(3) . ? N6 C7 1.368(3) . ? N6 C8 1.377(3) . ? N6 C10 1.467(3) . ? B1 H1A 0.9900 . ? B1 H1B 0.9900 . ? C3 C4 1.488(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.514(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.481(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.526(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.410(4) . ? C12 C19 1.517(4) . ? C12 H12 1.0000 . ? C13 C14 1.509(4) . ? C13 H13 1.0000 . ? C14 C15 1.534(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.521(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.386(4) . ? C16 H16 1.0000 . ? C17 C18 1.507(4) . ? C17 H17 1.0000 . ? C18 C19 1.542(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 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 C13 Rh1 C12 38.74(10) . . ? C13 Rh1 C17 97.85(10) . . ? C12 Rh1 C17 82.55(11) . . ? C13 Rh1 C16 80.12(10) . . ? C12 Rh1 C16 88.95(10) . . ? C17 Rh1 C16 37.50(10) . . ? C13 Rh1 S2 84.42(7) . . ? C12 Rh1 S2 89.54(8) . . ? C17 Rh1 S2 163.81(8) . . ? C16 Rh1 S2 157.03(7) . . ? C13 Rh1 S1 138.95(7) . . ? C12 Rh1 S1 174.39(8) . . ? C17 Rh1 S1 93.38(8) . . ? C16 Rh1 S1 85.48(7) . . ? S2 Rh1 S1 95.34(3) . . ? C2 S1 Rh1 109.51(9) . . ? C7 S2 Rh1 108.76(9) . . ? C2 N1 N2 111.0(2) . . ? C2 N1 B1 127.9(2) . . ? N2 N1 B1 120.7(2) . . ? C3 N2 N1 105.1(2) . . ? C2 N3 C3 106.9(2) . . ? C2 N3 C5 125.6(2) . . ? C3 N3 C5 127.4(2) . . ? C7 N4 N5 110.2(2) . . ? C7 N4 B1 130.7(2) . . ? N5 N4 B1 119.1(2) . . ? C8 N5 N4 105.5(2) . . ? C7 N6 C8 106.7(2) . . ? C7 N6 C10 125.7(2) . . ? C8 N6 C10 127.4(2) . . ? N4 B1 N1 108.9(2) . . ? N4 B1 H1A 109.9 . . ? N1 B1 H1A 109.9 . . ? N4 B1 H1B 109.9 . . ? N1 B1 H1B 109.9 . . ? H1A B1 H1B 108.3 . . ? N1 C2 N3 105.9(2) . . ? N1 C2 S1 129.53(19) . . ? N3 C2 S1 124.46(19) . . ? N2 C3 N3 111.1(2) . . ? N2 C3 C4 125.0(2) . . ? N3 C3 C4 123.9(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 113.4(2) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 106.5(2) . . ? N4 C7 S2 130.36(19) . . ? N6 C7 S2 123.14(19) . . ? N5 C8 N6 111.0(2) . . ? N5 C8 C9 125.0(2) . . ? N6 C8 C9 123.9(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 113.1(2) . . ? N6 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N6 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C19 124.6(2) . . ? C13 C12 Rh1 70.43(14) . . ? C19 C12 Rh1 112.06(18) . . ? C13 C12 H12 114.0 . . ? C19 C12 H12 114.0 . . ? Rh1 C12 H12 114.0 . . ? C12 C13 C14 125.7(2) . . ? C12 C13 Rh1 70.82(15) . . ? C14 C13 Rh1 112.29(18) . . ? C12 C13 H13 113.5 . . ? C14 C13 H13 113.5 . . ? Rh1 C13 H13 113.5 . . ? C13 C14 C15 112.1(2) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 111.2(2) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 124.4(2) . . ? C17 C16 Rh1 69.28(15) . . ? C15 C16 Rh1 113.59(17) . . ? C17 C16 H16 113.9 . . ? C15 C16 H16 113.9 . . ? Rh1 C16 H16 113.9 . . ? C16 C17 C18 126.2(2) . . ? C16 C17 Rh1 73.22(15) . . ? C18 C17 Rh1 108.27(18) . . ? C16 C17 H17 113.8 . . ? C18 C17 H17 113.8 . . ? Rh1 C17 H17 113.8 . . ? C17 C18 C19 112.4(2) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C12 C19 C18 112.3(2) . . ? C12 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? C12 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Rh1 S1 C2 -176.03(14) . . . . ? C12 Rh1 S1 C2 121.3(8) . . . . ? C17 Rh1 S1 C2 77.94(12) . . . . ? C16 Rh1 S1 C2 114.64(11) . . . . ? S2 Rh1 S1 C2 -88.40(9) . . . . ? C13 Rh1 S2 C7 -154.89(11) . . . . ? C12 Rh1 S2 C7 -116.42(12) . . . . ? C17 Rh1 S2 C7 -55.9(3) . . . . ? C16 Rh1 S2 C7 157.4(2) . . . . ? S1 Rh1 S2 C7 66.35(9) . . . . ? C2 N1 N2 C3 0.7(3) . . . . ? B1 N1 N2 C3 173.6(2) . . . . ? C7 N4 N5 C8 -1.2(3) . . . . ? B1 N4 N5 C8 178.6(2) . . . . ? C7 N4 B1 N1 -102.6(3) . . . . ? N5 N4 B1 N1 77.6(3) . . . . ? C2 N1 B1 N4 80.7(3) . . . . ? N2 N1 B1 N4 -90.9(3) . . . . ? N2 N1 C2 N3 -1.6(3) . . . . ? B1 N1 C2 N3 -173.9(2) . . . . ? N2 N1 C2 S1 175.34(18) . . . . ? B1 N1 C2 S1 3.1(4) . . . . ? C3 N3 C2 N1 1.8(3) . . . . ? C5 N3 C2 N1 -175.7(2) . . . . ? C3 N3 C2 S1 -175.31(18) . . . . ? C5 N3 C2 S1 7.1(3) . . . . ? Rh1 S1 C2 N1 15.2(3) . . . . ? Rh1 S1 C2 N3 -168.39(18) . . . . ? N1 N2 C3 N3 0.5(3) . . . . ? N1 N2 C3 C4 -177.4(2) . . . . ? C2 N3 C3 N2 -1.5(3) . . . . ? C5 N3 C3 N2 176.0(2) . . . . ? C2 N3 C3 C4 176.5(2) . . . . ? C5 N3 C3 C4 -6.0(4) . . . . ? C2 N3 C5 C6 -86.7(3) . . . . ? C3 N3 C5 C6 96.2(3) . . . . ? N5 N4 C7 N6 1.1(3) . . . . ? B1 N4 C7 N6 -178.6(2) . . . . ? N5 N4 C7 S2 -179.07(19) . . . . ? B1 N4 C7 S2 1.2(4) . . . . ? C8 N6 C7 N4 -0.6(3) . . . . ? C10 N6 C7 N4 174.8(2) . . . . ? C8 N6 C7 S2 179.54(18) . . . . ? C10 N6 C7 S2 -5.0(3) . . . . ? Rh1 S2 C7 N4 5.7(3) . . . . ? Rh1 S2 C7 N6 -174.48(17) . . . . ? N4 N5 C8 N6 0.8(3) . . . . ? N4 N5 C8 C9 -177.4(2) . . . . ? C7 N6 C8 N5 -0.1(3) . . . . ? C10 N6 C8 N5 -175.5(2) . . . . ? C7 N6 C8 C9 178.1(2) . . . . ? C10 N6 C8 C9 2.8(4) . . . . ? C7 N6 C10 C11 78.4(3) . . . . ? C8 N6 C10 C11 -107.1(3) . . . . ? C17 Rh1 C12 C13 112.52(17) . . . . ? C16 Rh1 C12 C13 75.44(16) . . . . ? S2 Rh1 C12 C13 -81.64(15) . . . . ? S1 Rh1 C12 C13 68.8(8) . . . . ? C13 Rh1 C12 C19 -120.4(3) . . . . ? C17 Rh1 C12 C19 -7.90(19) . . . . ? C16 Rh1 C12 C19 -44.98(19) . . . . ? S2 Rh1 C12 C19 157.94(18) . . . . ? S1 Rh1 C12 C19 -51.6(9) . . . . ? C19 C12 C13 C14 -0.3(4) . . . . ? Rh1 C12 C13 C14 -104.2(3) . . . . ? C19 C12 C13 Rh1 103.8(3) . . . . ? C17 Rh1 C13 C12 -67.61(17) . . . . ? C16 Rh1 C13 C12 -100.80(17) . . . . ? S2 Rh1 C13 C12 96.25(15) . . . . ? S1 Rh1 C13 C12 -172.03(12) . . . . ? C12 Rh1 C13 C14 121.6(3) . . . . ? C17 Rh1 C13 C14 54.03(19) . . . . ? C16 Rh1 C13 C14 20.84(18) . . . . ? S2 Rh1 C13 C14 -142.10(18) . . . . ? S1 Rh1 C13 C14 -50.4(2) . . . . ? C12 C13 C14 C15 45.9(4) . . . . ? Rh1 C13 C14 C15 -35.9(3) . . . . ? C13 C14 C15 C16 33.3(3) . . . . ? C14 C15 C16 C17 -96.0(3) . . . . ? C14 C15 C16 Rh1 -15.7(3) . . . . ? C13 Rh1 C16 C17 117.04(17) . . . . ? C12 Rh1 C16 C17 79.10(17) . . . . ? S2 Rh1 C16 C17 165.44(15) . . . . ? S1 Rh1 C16 C17 -101.55(15) . . . . ? C13 Rh1 C16 C15 -2.58(19) . . . . ? C12 Rh1 C16 C15 -40.52(19) . . . . ? C17 Rh1 C16 C15 -119.6(3) . . . . ? S2 Rh1 C16 C15 45.8(3) . . . . ? S1 Rh1 C16 C15 138.83(19) . . . . ? C15 C16 C17 C18 4.4(4) . . . . ? Rh1 C16 C17 C18 -100.7(3) . . . . ? C15 C16 C17 Rh1 105.0(2) . . . . ? C13 Rh1 C17 C16 -62.35(17) . . . . ? C12 Rh1 C17 C16 -98.05(17) . . . . ? S2 Rh1 C17 C16 -159.4(2) . . . . ? S1 Rh1 C17 C16 78.07(15) . . . . ? C13 Rh1 C17 C18 61.0(2) . . . . ? C12 Rh1 C17 C18 25.29(19) . . . . ? C16 Rh1 C17 C18 123.3(3) . . . . ? S2 Rh1 C17 C18 -36.1(4) . . . . ? S1 Rh1 C17 C18 -158.59(18) . . . . ? C16 C17 C18 C19 43.5(4) . . . . ? Rh1 C17 C18 C19 -38.7(3) . . . . ? C13 C12 C19 C18 -91.9(3) . . . . ? Rh1 C12 C19 C18 -11.1(3) . . . . ? C17 C18 C19 C12 33.3(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.898 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.096 data_2 _database_code_depnum_ccdc_archive 'CCDC 733500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H37 B N9 Rh S3), H2 O' _chemical_formula_sum 'C46 H76 B2 N18 O1 Rh2 S6' _chemical_formula_weight 1317.11 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2629(8) _cell_length_b 15.5576(11) _cell_length_c 17.0557(12) _cell_angle_alpha 79.5750(10) _cell_angle_beta 89.8850(10) _cell_angle_gamma 89.5420(10) _cell_volume 2939.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'SADABS V2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_reflns_number 30872 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.1558 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.57 _reflns_number_total 13432 _reflns_number_gt 7255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Brukerr SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^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 13432 _refine_ls_number_parameters 694 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.005 _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 0.76356(3) 0.33614(2) 0.84154(2) 0.02067(11) Uani 1 1 d . . . S1 S 0.62200(10) 0.37140(8) 0.94144(7) 0.0253(3) Uani 1 1 d . . . S2 S 0.65791(11) 0.21329(8) 0.81361(7) 0.0269(3) Uani 1 1 d . . . S3 S 1.06031(10) 0.15003(8) 0.97415(7) 0.0219(3) Uani 1 1 d . . . N1 N 0.7402(3) 0.2551(2) 1.0558(2) 0.0182(9) Uani 1 1 d . . . N2 N 0.7642(3) 0.2410(2) 1.1374(2) 0.0225(9) Uani 1 1 d . . . N3 N 0.6540(3) 0.3596(2) 1.1024(2) 0.0212(9) Uani 1 1 d . . . N4 N 0.6496(3) 0.1562(2) 0.9764(2) 0.0191(9) Uani 1 1 d . . . N5 N 0.5685(3) 0.1203(2) 1.0340(2) 0.0204(9) Uani 1 1 d . . . N6 N 0.4890(3) 0.1327(2) 0.9147(2) 0.0212(9) Uani 1 1 d . . . N7 N 0.8442(3) 0.1142(2) 1.0479(2) 0.0183(9) Uani 1 1 d . . . N8 N 0.7953(3) 0.0573(2) 1.1131(2) 0.0198(9) Uani 1 1 d . . . N9 N 0.9888(3) 0.0357(2) 1.1067(2) 0.0176(9) Uani 1 1 d . . . B1 B 0.7709(4) 0.1887(4) 1.0016(3) 0.0205(13) Uani 1 1 d . . . H1 H 0.8157 0.2180 0.9535 0.025 Uiso 1 1 calc R . . C2 C 0.6743(4) 0.3281(3) 1.0341(3) 0.0191(11) Uani 1 1 d . . . C3 C 0.7108(4) 0.3054(3) 1.1637(3) 0.0222(11) Uani 1 1 d . . . C4 C 0.7116(4) 0.3177(3) 1.2478(3) 0.0313(13) Uani 1 1 d . . . H3A H 0.7619 0.2727 1.2794 0.047 Uiso 1 1 calc R . . H4B H 0.6305 0.3129 1.2689 0.047 Uiso 1 1 calc R . . H5C H 0.7430 0.3756 1.2506 0.047 Uiso 1 1 calc R . . C5 C 0.5891(4) 0.4405(3) 1.1089(3) 0.0266(12) Uani 1 1 d . . . H6A H 0.5436 0.4317 1.1594 0.032 Uiso 1 1 calc R . . H7B H 0.5320 0.4546 1.0643 0.032 Uiso 1 1 calc R . . C6 C 0.6737(4) 0.5160(3) 1.1069(3) 0.0386(14) Uani 1 1 d . . . H8A H 0.7225 0.5059 1.1553 0.058 Uiso 1 1 calc R . . H9B H 0.6283 0.5704 1.1042 0.058 Uiso 1 1 calc R . . H10C H 0.7252 0.5204 1.0600 0.058 Uiso 1 1 calc R . . C7 C 0.6009(4) 0.1665(3) 0.9040(3) 0.0207(11) Uani 1 1 d . . . C8 C 0.4730(4) 0.1067(3) 0.9945(3) 0.0255(12) Uani 1 1 d . . . C9 C 0.3623(4) 0.0676(3) 1.0310(3) 0.0318(13) Uani 1 1 d . . . H11A H 0.3751 0.0464 1.0881 0.048 Uiso 1 1 calc R . . H12B H 0.3396 0.0186 1.0054 0.048 Uiso 1 1 calc R . . H13C H 0.2989 0.1118 1.0237 0.048 Uiso 1 1 calc R . . C10 C 0.3996(4) 0.1348(3) 0.8523(3) 0.0299(13) Uani 1 1 d . . . H14A H 0.3424 0.0869 0.8684 0.036 Uiso 1 1 calc R . . H15B H 0.4387 0.1257 0.8024 0.036 Uiso 1 1 calc R . . C11 C 0.3340(4) 0.2219(3) 0.8379(3) 0.0402(14) Uani 1 1 d . . . H16A H 0.2871 0.2274 0.8852 0.060 Uiso 1 1 calc R . . H17B H 0.2810 0.2248 0.7919 0.060 Uiso 1 1 calc R . . H18C H 0.3914 0.2696 0.8272 0.060 Uiso 1 1 calc R . . C12 C 0.9641(4) 0.0999(3) 1.0438(3) 0.0188(11) Uani 1 1 d . . . C13 C 0.8844(4) 0.0124(3) 1.1461(3) 0.0199(11) Uani 1 1 d . . . C14 C 0.8771(4) -0.0562(3) 1.2188(3) 0.0283(12) Uani 1 1 d . . . H19A H 0.7945 -0.0624 1.2369 0.042 Uiso 1 1 calc R . . H20B H 0.9263 -0.0396 1.2610 0.042 Uiso 1 1 calc R . . H21C H 0.9059 -0.1120 1.2066 0.042 Uiso 1 1 calc R . . C15 C 1.1062(3) -0.0041(3) 1.1276(3) 0.0230(12) Uani 1 1 d . . . H22A H 1.1558 0.0013 1.0790 0.028 Uiso 1 1 calc R . . H23B H 1.0967 -0.0672 1.1494 0.028 Uiso 1 1 calc R . . C16 C 1.1681(4) 0.0393(3) 1.1885(3) 0.0333(13) Uani 1 1 d . . . H24A H 1.1810 0.1011 1.1661 0.050 Uiso 1 1 calc R . . H25B H 1.2448 0.0104 1.2024 0.050 Uiso 1 1 calc R . . H26C H 1.1188 0.0345 1.2364 0.050 Uiso 1 1 calc R . . C17 C 0.8241(4) 0.3443(3) 0.7223(3) 0.0280(12) Uani 1 1 d . . . H27 H 0.7841 0.3029 0.6926 0.034 Uiso 1 1 calc R . . C18 C 0.9124(4) 0.3059(3) 0.7744(3) 0.0297(13) Uani 1 1 d . . . H28 H 0.9234 0.2419 0.7751 0.036 Uiso 1 1 calc R . . C19 C 1.0240(4) 0.3512(3) 0.7927(3) 0.0399(15) Uani 1 1 d . . . H29A H 1.0447 0.3968 0.7464 0.048 Uiso 1 1 calc R . . H30B H 1.0901 0.3083 0.8015 0.048 Uiso 1 1 calc R . . C20 C 1.0095(4) 0.3935(3) 0.8667(3) 0.0415(15) Uani 1 1 d . . . H31A H 1.0332 0.3507 0.9144 0.050 Uiso 1 1 calc R . . H32B H 1.0637 0.4440 0.8621 0.050 Uiso 1 1 calc R . . C21 C 0.8847(4) 0.4242(3) 0.8779(3) 0.0289(12) Uani 1 1 d . . . H33 H 0.8685 0.4375 0.9322 0.035 Uiso 1 1 calc R . . C22 C 0.8128(4) 0.4700(3) 0.8184(3) 0.0292(12) Uani 1 1 d . . . H34 H 0.7538 0.5096 0.8381 0.035 Uiso 1 1 calc R . . C23 C 0.8541(4) 0.5024(3) 0.7331(3) 0.0337(13) Uani 1 1 d . . . H35A H 0.8161 0.5596 0.7123 0.040 Uiso 1 1 calc R . . H36B H 0.9412 0.5110 0.7326 0.040 Uiso 1 1 calc R . . C24 C 0.8230(4) 0.4378(3) 0.6794(3) 0.0332(13) Uani 1 1 d . . . H37A H 0.7431 0.4523 0.6564 0.040 Uiso 1 1 calc R . . H38B H 0.8805 0.4440 0.6347 0.040 Uiso 1 1 calc R . . Rh1' Rh 0.10740(3) 0.20034(3) 0.45056(2) 0.02314(11) Uani 1 1 d . . . S1' S 0.05064(10) 0.25100(9) 0.31618(7) 0.0307(3) Uani 1 1 d . . . S2' S 0.21764(11) 0.07385(8) 0.42134(8) 0.0291(3) Uani 1 1 d . . . S3' S 0.50756(12) 0.29025(9) 0.52268(8) 0.0352(3) Uani 1 1 d . . . N1' N 0.2894(3) 0.2761(2) 0.2816(2) 0.0210(9) Uani 1 1 d . . . N2' N 0.3628(3) 0.2861(3) 0.2147(2) 0.0257(10) Uani 1 1 d . . . N3' N 0.1750(3) 0.2790(2) 0.1789(2) 0.0199(9) Uani 1 1 d . . . N4' N 0.4111(3) 0.1800(2) 0.3820(2) 0.0230(9) Uani 1 1 d . . . N5' N 0.5312(3) 0.1740(3) 0.3664(2) 0.0252(10) Uani 1 1 d . . . N6' N 0.4531(3) 0.0425(2) 0.4005(2) 0.0226(9) Uani 1 1 d . . . N7' N 0.4275(3) 0.3444(2) 0.3695(2) 0.0202(9) Uani 1 1 d . . . N8' N 0.4315(3) 0.4181(2) 0.3094(2) 0.0242(10) Uani 1 1 d . . . N9' N 0.5437(3) 0.4369(2) 0.4107(2) 0.0228(9) Uani 1 1 d . . . B1' B 0.3430(5) 0.2678(4) 0.3653(3) 0.0235(13) Uani 1 1 d . . . H1' H 0.2779 0.2672 0.4053 0.028 Uiso 1 1 calc R . . C2' C 0.1753(4) 0.2692(3) 0.2595(3) 0.0219(11) Uani 1 1 d . . . C3' C 0.2916(4) 0.2885(3) 0.1544(3) 0.0270(12) Uani 1 1 d . . . C4' C 0.3298(5) 0.2996(3) 0.0693(3) 0.0397(14) Uani 1 1 d . . . H39' H 0.3078 0.3583 0.0415 0.060 Uiso 1 1 calc R . . H40' H 0.2906 0.2559 0.0437 0.060 Uiso 1 1 calc R . . H41' H 0.4161 0.2920 0.0668 0.060 Uiso 1 1 calc R . . C5' C 0.0697(4) 0.2778(3) 0.1298(3) 0.0293(12) Uani 1 1 d . . . H42' H 0.0107 0.2380 0.1600 0.035 Uiso 1 1 calc R . . H43' H 0.0915 0.2542 0.0815 0.035 Uiso 1 1 calc R . . C6' C 0.0130(4) 0.3681(3) 0.1046(3) 0.0402(14) Uani 1 1 d . . . H44' H -0.0106 0.3913 0.1521 0.060 Uiso 1 1 calc R . . H45' H -0.0571 0.3634 0.0717 0.060 Uiso 1 1 calc R . . H46' H 0.0705 0.4076 0.0737 0.060 Uiso 1 1 calc R . . C7' C 0.3625(4) 0.1017(3) 0.4009(3) 0.0222(11) Uani 1 1 d . . . C8' C 0.5535(4) 0.0908(3) 0.3774(3) 0.0280(12) Uani 1 1 d . . . C9' C 0.6723(4) 0.0515(3) 0.3670(3) 0.0414(15) Uani 1 1 d . . . H47' H 0.6671 0.0142 0.3266 0.062 Uiso 1 1 calc R . . H48' H 0.6983 0.0164 0.4177 0.062 Uiso 1 1 calc R . . H49' H 0.7297 0.0982 0.3497 0.062 Uiso 1 1 calc R . . C10' C 0.4431(4) -0.0528(3) 0.4150(3) 0.0304(13) Uani 1 1 d . . . H50C H 0.3843 -0.0710 0.4579 0.036 Uiso 1 1 calc R . . H51D H 0.5207 -0.0791 0.4335 0.036 Uiso 1 1 calc R . . C11' C 0.4058(5) -0.0864(3) 0.3413(3) 0.0448(15) Uani 1 1 d . . . H52D H 0.3233 -0.0691 0.3284 0.067 Uiso 1 1 calc R . . H53E H 0.4125 -0.1503 0.3511 0.067 Uiso 1 1 calc R . . H54F H 0.4573 -0.0617 0.2967 0.067 Uiso 1 1 calc R . . C12' C 0.4930(4) 0.3560(3) 0.4333(3) 0.0228(11) Uani 1 1 d . . . C13' C 0.5015(4) 0.4724(3) 0.3366(3) 0.0238(12) Uani 1 1 d . . . C14' C 0.5300(4) 0.5617(3) 0.2939(3) 0.0351(13) Uani 1 1 d . . . H55D H 0.4825 0.5753 0.2451 0.053 Uiso 1 1 calc R . . H56E H 0.6146 0.5646 0.2800 0.053 Uiso 1 1 calc R . . H57F H 0.5119 0.6041 0.3283 0.053 Uiso 1 1 calc R . . C15' C 0.6305(4) 0.4748(3) 0.4578(3) 0.0324(13) Uani 1 1 d . . . H58C H 0.6162 0.4528 0.5152 0.039 Uiso 1 1 calc R . . H59D H 0.6207 0.5391 0.4479 0.039 Uiso 1 1 calc R . . C16' C 0.7565(4) 0.4517(4) 0.4368(4) 0.0556(18) Uani 1 1 d . . . H60D H 0.7660 0.3880 0.4457 0.083 Uiso 1 1 calc R . . H61E H 0.8127 0.4762 0.4705 0.083 Uiso 1 1 calc R . . H62F H 0.7722 0.4760 0.3806 0.083 Uiso 1 1 calc R . . C17' C 0.1725(4) 0.1810(3) 0.5685(3) 0.0318(13) Uani 1 1 d . . . H63' H 0.2515 0.1508 0.5757 0.038 Uiso 1 1 calc R . . C18' C 0.0768(4) 0.1245(3) 0.5678(3) 0.0284(12) Uani 1 1 d . . . H64' H 0.1005 0.0617 0.5732 0.034 Uiso 1 1 calc R . . C19' C -0.0444(4) 0.1383(3) 0.6016(3) 0.0346(14) Uani 1 1 d . . . H65C H -0.0367 0.1730 0.6445 0.042 Uiso 1 1 calc R . . H66D H -0.0785 0.0809 0.6252 0.042 Uiso 1 1 calc R . . C20' C -0.1285(4) 0.1858(4) 0.5370(3) 0.0406(15) Uani 1 1 d . . . H67C H -0.1705 0.1420 0.5120 0.049 Uiso 1 1 calc R . . H68D H -0.1888 0.2187 0.5622 0.049 Uiso 1 1 calc R . . C21' C -0.0644(4) 0.2477(3) 0.4736(3) 0.0346(14) Uani 1 1 d . . . H69' H -0.1126 0.2668 0.4243 0.042 Uiso 1 1 calc R . . C22' C 0.0213(4) 0.3090(3) 0.4861(3) 0.0351(14) Uani 1 1 d . . . H70' H 0.0217 0.3635 0.4447 0.042 Uiso 1 1 calc R . . C23' C 0.0580(5) 0.3220(3) 0.5687(3) 0.0451(16) Uani 1 1 d . . . H71C H -0.0092 0.3065 0.6059 0.054 Uiso 1 1 calc R . . H72D H 0.0762 0.3845 0.5670 0.054 Uiso 1 1 calc R . . C24' C 0.1670(5) 0.2662(4) 0.6001(3) 0.0432(15) Uani 1 1 d . . . H73C H 0.2400 0.3000 0.5841 0.052 Uiso 1 1 calc R . . H74D H 0.1642 0.2531 0.6590 0.052 Uiso 1 1 calc R . . O1 O 0.5143(5) 0.0889(4) 0.2021(3) 0.0913(18) Uani 1 1 d D . . H1O H 0.520(6) 0.139(3) 0.221(4) 0.137 Uiso 1 1 d D . . H2O H 0.578(4) 0.085(4) 0.171(4) 0.137 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0187(2) 0.0202(2) 0.0231(2) -0.00409(18) 0.00198(17) 0.00273(16) S1 0.0233(7) 0.0314(8) 0.0204(7) -0.0033(6) -0.0008(5) 0.0132(6) S2 0.0305(7) 0.0292(8) 0.0219(7) -0.0069(6) -0.0011(6) -0.0021(6) S3 0.0167(6) 0.0247(7) 0.0242(7) -0.0041(6) 0.0013(5) 0.0011(5) N1 0.014(2) 0.022(2) 0.019(2) -0.0043(18) -0.0058(17) 0.0064(17) N2 0.020(2) 0.027(2) 0.020(2) -0.0049(19) -0.0051(18) 0.0046(18) N3 0.022(2) 0.020(2) 0.022(2) -0.0050(18) -0.0004(18) 0.0071(17) N4 0.015(2) 0.022(2) 0.020(2) -0.0018(18) -0.0002(17) -0.0047(16) N5 0.013(2) 0.024(2) 0.023(2) -0.0007(18) 0.0011(18) 0.0025(17) N6 0.015(2) 0.023(2) 0.027(2) -0.0075(19) -0.0062(18) 0.0010(17) N7 0.016(2) 0.018(2) 0.021(2) -0.0044(18) -0.0002(17) 0.0028(16) N8 0.017(2) 0.018(2) 0.023(2) -0.0006(18) 0.0002(18) 0.0003(17) N9 0.016(2) 0.017(2) 0.019(2) -0.0032(17) -0.0049(17) 0.0022(16) B1 0.011(3) 0.027(3) 0.024(3) -0.004(3) -0.003(2) 0.004(2) C2 0.011(2) 0.023(3) 0.023(3) -0.004(2) -0.001(2) 0.000(2) C3 0.017(2) 0.024(3) 0.024(3) -0.001(2) 0.002(2) -0.001(2) C4 0.038(3) 0.032(3) 0.024(3) -0.004(2) -0.005(2) 0.007(2) C5 0.028(3) 0.030(3) 0.022(3) -0.007(2) 0.001(2) 0.014(2) C6 0.037(3) 0.028(3) 0.048(4) -0.001(3) -0.001(3) 0.006(3) C7 0.018(2) 0.017(3) 0.028(3) -0.006(2) -0.003(2) 0.003(2) C8 0.014(3) 0.026(3) 0.035(3) -0.001(2) -0.001(2) 0.006(2) C9 0.015(3) 0.029(3) 0.049(4) 0.000(3) 0.000(2) 0.002(2) C10 0.021(3) 0.034(3) 0.036(3) -0.009(3) -0.015(2) 0.000(2) C11 0.030(3) 0.046(4) 0.042(4) -0.001(3) -0.016(3) 0.006(3) C12 0.012(2) 0.020(3) 0.027(3) -0.013(2) -0.001(2) 0.0026(19) C13 0.022(3) 0.020(3) 0.019(3) -0.008(2) 0.001(2) -0.001(2) C14 0.028(3) 0.030(3) 0.025(3) 0.001(2) -0.004(2) 0.001(2) C15 0.011(2) 0.021(3) 0.033(3) 0.006(2) -0.005(2) 0.007(2) C16 0.021(3) 0.046(4) 0.034(3) -0.008(3) -0.010(2) 0.001(2) C17 0.031(3) 0.027(3) 0.027(3) -0.010(2) 0.011(2) 0.005(2) C18 0.028(3) 0.025(3) 0.034(3) -0.003(2) 0.013(2) 0.010(2) C19 0.023(3) 0.035(4) 0.056(4) 0.006(3) 0.012(3) 0.010(2) C20 0.031(3) 0.031(3) 0.059(4) 0.001(3) -0.012(3) -0.002(3) C21 0.028(3) 0.024(3) 0.036(3) -0.007(2) 0.000(2) -0.001(2) C22 0.031(3) 0.021(3) 0.037(3) -0.009(2) 0.002(3) 0.002(2) C23 0.027(3) 0.024(3) 0.045(4) 0.006(3) 0.002(3) 0.004(2) C24 0.034(3) 0.035(3) 0.028(3) 0.002(3) 0.008(2) 0.011(2) Rh1' 0.0237(2) 0.0233(2) 0.0215(2) -0.00207(18) 0.00228(18) 0.00623(17) S1' 0.0214(7) 0.0447(9) 0.0232(7) 0.0012(6) -0.0006(6) 0.0021(6) S2' 0.0267(7) 0.0222(7) 0.0388(8) -0.0064(6) 0.0049(6) 0.0029(6) S3' 0.0478(9) 0.0285(8) 0.0273(8) 0.0003(6) -0.0103(7) 0.0034(6) N1' 0.022(2) 0.022(2) 0.020(2) -0.0070(18) 0.0025(18) 0.0002(17) N2' 0.024(2) 0.030(3) 0.023(2) -0.006(2) 0.002(2) 0.0005(18) N3' 0.023(2) 0.019(2) 0.018(2) -0.0055(18) -0.0031(18) -0.0005(17) N4' 0.022(2) 0.019(2) 0.026(2) -0.0009(19) 0.0006(18) 0.0067(18) N5' 0.019(2) 0.029(3) 0.029(2) -0.008(2) 0.0026(18) 0.0064(18) N6' 0.027(2) 0.019(2) 0.022(2) -0.0035(18) -0.0002(18) 0.0102(18) N7' 0.022(2) 0.018(2) 0.020(2) -0.0018(18) -0.0028(18) 0.0061(17) N8' 0.028(2) 0.017(2) 0.027(2) -0.0048(19) 0.0024(19) 0.0031(18) N9' 0.024(2) 0.018(2) 0.027(2) -0.0064(19) -0.0018(19) 0.0009(18) B1' 0.021(3) 0.026(3) 0.023(3) -0.002(3) 0.003(3) 0.004(2) C2' 0.027(3) 0.015(3) 0.022(3) 0.001(2) -0.002(2) 0.004(2) C3' 0.030(3) 0.023(3) 0.028(3) -0.003(2) 0.005(3) 0.001(2) C4' 0.046(3) 0.048(4) 0.024(3) -0.006(3) 0.009(3) -0.002(3) C5' 0.034(3) 0.033(3) 0.020(3) -0.005(2) -0.003(2) -0.005(2) C6' 0.044(3) 0.039(4) 0.035(3) 0.001(3) -0.017(3) -0.006(3) C7' 0.028(3) 0.021(3) 0.016(3) 0.000(2) -0.001(2) 0.007(2) C8' 0.025(3) 0.036(3) 0.024(3) -0.010(3) -0.002(2) 0.008(2) C9' 0.031(3) 0.042(4) 0.052(4) -0.010(3) 0.005(3) 0.017(3) C10' 0.037(3) 0.020(3) 0.035(3) -0.006(2) -0.002(3) 0.007(2) C11' 0.079(4) 0.024(3) 0.031(3) -0.005(3) -0.006(3) 0.004(3) C12' 0.016(2) 0.026(3) 0.026(3) -0.006(2) -0.005(2) 0.008(2) C13' 0.027(3) 0.016(3) 0.027(3) -0.001(2) 0.003(2) 0.005(2) C14' 0.045(3) 0.026(3) 0.032(3) 0.002(3) -0.002(3) 0.000(3) C15' 0.034(3) 0.024(3) 0.040(3) -0.009(3) -0.003(3) 0.000(2) C16' 0.030(3) 0.069(5) 0.072(5) -0.025(4) -0.009(3) 0.007(3) C17' 0.031(3) 0.039(3) 0.024(3) -0.003(3) 0.001(2) 0.015(3) C18' 0.032(3) 0.031(3) 0.018(3) 0.008(2) 0.001(2) 0.006(2) C19' 0.036(3) 0.040(4) 0.025(3) 0.004(3) 0.010(3) -0.001(3) C20' 0.035(3) 0.045(4) 0.039(4) 0.000(3) 0.009(3) 0.005(3) C21' 0.026(3) 0.034(3) 0.041(4) -0.001(3) -0.001(3) 0.019(3) C22' 0.041(3) 0.031(3) 0.031(3) 0.001(3) 0.009(3) 0.021(3) C23' 0.063(4) 0.024(3) 0.050(4) -0.014(3) 0.019(3) 0.001(3) C24' 0.040(3) 0.057(4) 0.039(4) -0.024(3) 0.005(3) -0.009(3) O1 0.116(4) 0.115(5) 0.043(3) -0.013(3) 0.024(3) -0.055(4) _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 C21 2.113(5) . ? Rh1 C18 2.125(4) . ? Rh1 C17 2.125(4) . ? Rh1 C22 2.126(5) . ? Rh1 S2 2.3798(13) . ? Rh1 S1 2.4615(12) . ? S1 C2 1.707(5) . ? S2 C7 1.708(5) . ? S3 C12 1.693(4) . ? N1 C2 1.346(5) . ? N1 N2 1.395(5) . ? N1 B1 1.544(6) . ? N2 C3 1.311(5) . ? N3 C2 1.360(5) . ? N3 C3 1.374(5) . ? N3 C5 1.472(5) . ? N4 C7 1.335(5) . ? N4 N5 1.385(4) . ? N4 B1 1.548(6) . ? N5 C8 1.309(6) . ? N6 C8 1.360(6) . ? N6 C7 1.368(5) . ? N6 C10 1.463(5) . ? N7 C12 1.371(5) . ? N7 N8 1.405(5) . ? N7 B1 1.518(6) . ? N8 C13 1.288(5) . ? N9 C12 1.355(5) . ? N9 C13 1.372(5) . ? N9 C15 1.474(5) . ? B1 H1 1.0000 . ? C3 C4 1.481(6) . ? C4 H3A 0.9800 . ? C4 H4B 0.9800 . ? C4 H5C 0.9800 . ? C5 C6 1.514(6) . ? C5 H6A 0.9900 . ? C5 H7B 0.9900 . ? C6 H8A 0.9800 . ? C6 H9B 0.9800 . ? C6 H10C 0.9800 . ? C8 C9 1.477(6) . ? C9 H11A 0.9800 . ? C9 H12B 0.9800 . ? C9 H13C 0.9800 . ? C10 C11 1.518(6) . ? C10 H14A 0.9900 . ? C10 H15B 0.9900 . ? C11 H16A 0.9800 . ? C11 H17B 0.9800 . ? C11 H18C 0.9800 . ? C13 C14 1.485(6) . ? C14 H19A 0.9800 . ? C14 H20B 0.9800 . ? C14 H21C 0.9800 . ? C15 C16 1.511(6) . ? C15 H22A 0.9900 . ? C15 H23B 0.9900 . ? C16 H24A 0.9800 . ? C16 H25B 0.9800 . ? C16 H26C 0.9800 . ? C17 C18 1.392(6) . ? C17 C24 1.505(6) . ? C17 H27 1.0000 . ? C18 C19 1.507(7) . ? C18 H28 1.0000 . ? C19 C20 1.533(7) . ? C19 H29A 0.9900 . ? C19 H30B 0.9900 . ? C20 C21 1.504(6) . ? C20 H31A 0.9900 . ? C20 H32B 0.9900 . ? C21 C22 1.388(6) . ? C21 H33 1.0000 . ? C22 C23 1.525(6) . ? C22 H34 1.0000 . ? C23 C24 1.522(7) . ? C23 H35A 0.9900 . ? C23 H36B 0.9900 . ? C24 H37A 0.9900 . ? C24 H38B 0.9900 . ? Rh1' C17' 2.112(5) . ? Rh1' C22' 2.122(5) . ? Rh1' C21' 2.126(4) . ? Rh1' C18' 2.159(4) . ? Rh1' S1' 2.3720(13) . ? Rh1' S2' 2.4446(13) . ? S1' C2' 1.699(4) . ? S2' C7' 1.711(5) . ? S3' C12' 1.683(5) . ? N1' C2' 1.350(5) . ? N1' N2' 1.394(5) . ? N1' B1' 1.534(6) . ? N2' C3' 1.301(6) . ? N3' C2' 1.357(5) . ? N3' C3' 1.378(5) . ? N3' C5' 1.454(5) . ? N4' C7' 1.325(5) . ? N4' N5' 1.384(4) . ? N4' B1' 1.541(6) . ? N5' C8' 1.296(6) . ? N6' C7' 1.369(5) . ? N6' C8' 1.379(6) . ? N6' C10' 1.463(5) . ? N7' C12' 1.355(5) . ? N7' N8' 1.394(5) . ? N7' B1' 1.544(6) . ? N8' C13' 1.306(6) . ? N9' C13' 1.370(5) . ? N9' C12' 1.375(5) . ? N9' C15' 1.460(6) . ? B1' H1' 1.0000 . ? C3' C4' 1.494(6) . ? C4' H39' 0.9800 . ? C4' H40' 0.9800 . ? C4' H41' 0.9800 . ? C5' C6' 1.529(6) . ? C5' H42' 0.9900 . ? C5' H43' 0.9900 . ? C6' H44' 0.9800 . ? C6' H45' 0.9800 . ? C6' H46' 0.9800 . ? C8' C9' 1.491(6) . ? C9' H47' 0.9800 . ? C9' H48' 0.9800 . ? C9' H49' 0.9800 . ? C10' C11' 1.509(6) . ? C10' H50C 0.9900 . ? C10' H51D 0.9900 . ? C11' H52D 0.9800 . ? C11' H53E 0.9800 . ? C11' H54F 0.9800 . ? C13' C14' 1.484(6) . ? C14' H55D 0.9800 . ? C14' H56E 0.9800 . ? C14' H57F 0.9800 . ? C15' C16' 1.519(6) . ? C15' H58C 0.9900 . ? C15' H59D 0.9900 . ? C16' H60D 0.9800 . ? C16' H61E 0.9800 . ? C16' H62F 0.9800 . ? C17' C18' 1.398(7) . ? C17' C24' 1.519(7) . ? C17' H63' 1.0000 . ? C18' C19' 1.509(6) . ? C18' H64' 1.0000 . ? C19' C20' 1.534(6) . ? C19' H65C 0.9900 . ? C19' H66D 0.9900 . ? C20' C21' 1.500(6) . ? C20' H67C 0.9900 . ? C20' H68D 0.9900 . ? C21' C22' 1.404(7) . ? C21' H69' 1.0000 . ? C22' C23' 1.518(7) . ? C22' H70' 1.0000 . ? C23' C24' 1.538(7) . ? C23' H71C 0.9900 . ? C23' H72D 0.9900 . ? C24' H73C 0.9900 . ? C24' H74D 0.9900 . ? O1 H1O 0.904(10) . ? O1 H2O 0.902(10) . ? 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 C21 Rh1 C18 82.22(19) . . ? C21 Rh1 C17 98.22(19) . . ? C18 Rh1 C17 38.24(17) . . ? C21 Rh1 C22 38.21(17) . . ? C18 Rh1 C22 89.67(19) . . ? C17 Rh1 C22 81.36(19) . . ? C21 Rh1 S2 167.38(13) . . ? C18 Rh1 S2 91.52(14) . . ? C17 Rh1 S2 83.20(14) . . ? C22 Rh1 S2 153.37(14) . . ? C21 Rh1 S1 88.80(13) . . ? C18 Rh1 S1 168.01(14) . . ? C17 Rh1 S1 152.33(13) . . ? C22 Rh1 S1 88.15(13) . . ? S2 Rh1 S1 95.71(4) . . ? C2 S1 Rh1 108.62(15) . . ? C7 S2 Rh1 103.73(17) . . ? C2 N1 N2 110.7(4) . . ? C2 N1 B1 125.2(4) . . ? N2 N1 B1 123.6(4) . . ? C3 N2 N1 105.1(4) . . ? C2 N3 C3 108.0(4) . . ? C2 N3 C5 126.2(4) . . ? C3 N3 C5 125.7(4) . . ? C7 N4 N5 110.4(3) . . ? C7 N4 B1 129.1(4) . . ? N5 N4 B1 120.0(4) . . ? C8 N5 N4 105.2(4) . . ? C8 N6 C7 107.1(4) . . ? C8 N6 C10 126.9(4) . . ? C7 N6 C10 125.6(4) . . ? C12 N7 N8 110.1(3) . . ? C12 N7 B1 128.3(4) . . ? N8 N7 B1 120.8(3) . . ? C13 N8 N7 104.7(3) . . ? C12 N9 C13 107.9(3) . . ? C12 N9 C15 126.1(4) . . ? C13 N9 C15 126.0(4) . . ? N7 B1 N1 109.6(4) . . ? N7 B1 N4 111.4(4) . . ? N1 B1 N4 105.1(3) . . ? N7 B1 H1 110.2 . . ? N1 B1 H1 110.2 . . ? N4 B1 H1 110.2 . . ? N1 C2 N3 105.7(4) . . ? N1 C2 S1 127.9(4) . . ? N3 C2 S1 126.4(3) . . ? N2 C3 N3 110.5(4) . . ? N2 C3 C4 124.6(4) . . ? N3 C3 C4 124.9(4) . . ? C3 C4 H3A 109.5 . . ? C3 C4 H4B 109.5 . . ? H3A C4 H4B 109.5 . . ? C3 C4 H5C 109.5 . . ? H3A C4 H5C 109.5 . . ? H4B C4 H5C 109.5 . . ? N3 C5 C6 111.0(4) . . ? N3 C5 H6A 109.4 . . ? C6 C5 H6A 109.4 . . ? N3 C5 H7B 109.4 . . ? C6 C5 H7B 109.4 . . ? H6A C5 H7B 108.0 . . ? C5 C6 H8A 109.5 . . ? C5 C6 H9B 109.5 . . ? H8A C6 H9B 109.5 . . ? C5 C6 H10C 109.5 . . ? H8A C6 H10C 109.5 . . ? H9B C6 H10C 109.5 . . ? N4 C7 N6 106.2(4) . . ? N4 C7 S2 129.7(3) . . ? N6 C7 S2 124.1(4) . . ? N5 C8 N6 111.0(4) . . ? N5 C8 C9 125.0(4) . . ? N6 C8 C9 124.0(4) . . ? C8 C9 H11A 109.5 . . ? C8 C9 H12B 109.5 . . ? H11A C9 H12B 109.5 . . ? C8 C9 H13C 109.5 . . ? H11A C9 H13C 109.5 . . ? H12B C9 H13C 109.5 . . ? N6 C10 C11 110.6(4) . . ? N6 C10 H14A 109.5 . . ? C11 C10 H14A 109.5 . . ? N6 C10 H15B 109.5 . . ? C11 C10 H15B 109.5 . . ? H14A C10 H15B 108.1 . . ? C10 C11 H16A 109.5 . . ? C10 C11 H17B 109.5 . . ? H16A C11 H17B 109.5 . . ? C10 C11 H18C 109.5 . . ? H16A C11 H18C 109.5 . . ? H17B C11 H18C 109.5 . . ? N9 C12 N7 105.1(4) . . ? N9 C12 S3 127.4(3) . . ? N7 C12 S3 127.5(4) . . ? N8 C13 N9 112.1(4) . . ? N8 C13 C14 124.8(4) . . ? N9 C13 C14 123.1(4) . . ? C13 C14 H19A 109.5 . . ? C13 C14 H20B 109.5 . . ? H19A C14 H20B 109.5 . . ? C13 C14 H21C 109.5 . . ? H19A C14 H21C 109.5 . . ? H20B C14 H21C 109.5 . . ? N9 C15 C16 111.3(4) . . ? N9 C15 H22A 109.4 . . ? C16 C15 H22A 109.4 . . ? N9 C15 H23B 109.4 . . ? C16 C15 H23B 109.4 . . ? H22A C15 H23B 108.0 . . ? C15 C16 H24A 109.5 . . ? C15 C16 H25B 109.5 . . ? H24A C16 H25B 109.5 . . ? C15 C16 H26C 109.5 . . ? H24A C16 H26C 109.5 . . ? H25B C16 H26C 109.5 . . ? C18 C17 C24 125.3(5) . . ? C18 C17 Rh1 70.9(3) . . ? C24 C17 Rh1 110.6(3) . . ? C18 C17 H27 114.0 . . ? C24 C17 H27 114.0 . . ? Rh1 C17 H27 114.0 . . ? C17 C18 C19 124.5(5) . . ? C17 C18 Rh1 70.9(3) . . ? C19 C18 Rh1 113.0(3) . . ? C17 C18 H28 113.7 . . ? C19 C18 H28 113.7 . . ? Rh1 C18 H28 113.7 . . ? C18 C19 C20 111.8(4) . . ? C18 C19 H29A 109.2 . . ? C20 C19 H29A 109.2 . . ? C18 C19 H30B 109.2 . . ? C20 C19 H30B 109.2 . . ? H29A C19 H30B 107.9 . . ? C21 C20 C19 113.1(4) . . ? C21 C20 H31A 109.0 . . ? C19 C20 H31A 109.0 . . ? C21 C20 H32B 109.0 . . ? C19 C20 H32B 109.0 . . ? H31A C20 H32B 107.8 . . ? C22 C21 C20 125.5(5) . . ? C22 C21 Rh1 71.4(3) . . ? C20 C21 Rh1 109.4(3) . . ? C22 C21 H33 114.1 . . ? C20 C21 H33 114.1 . . ? Rh1 C21 H33 114.1 . . ? C21 C22 C23 123.9(4) . . ? C21 C22 Rh1 70.4(3) . . ? C23 C22 Rh1 113.8(3) . . ? C21 C22 H34 113.8 . . ? C23 C22 H34 113.8 . . ? Rh1 C22 H34 113.8 . . ? C24 C23 C22 111.2(4) . . ? C24 C23 H35A 109.4 . . ? C22 C23 H35A 109.4 . . ? C24 C23 H36B 109.4 . . ? C22 C23 H36B 109.4 . . ? H35A C23 H36B 108.0 . . ? C17 C24 C23 113.1(4) . . ? C17 C24 H37A 109.0 . . ? C23 C24 H37A 109.0 . . ? C17 C24 H38B 109.0 . . ? C23 C24 H38B 109.0 . . ? H37A C24 H38B 107.8 . . ? C17' Rh1' C22' 82.4(2) . . ? C17' Rh1' C21' 97.68(19) . . ? C22' Rh1' C21' 38.60(18) . . ? C17' Rh1' C18' 38.19(17) . . ? C22' Rh1' C18' 89.56(19) . . ? C21' Rh1' C18' 80.28(19) . . ? C17' Rh1' S1' 168.29(15) . . ? C22' Rh1' S1' 90.71(14) . . ? C21' Rh1' S1' 82.49(15) . . ? C18' Rh1' S1' 151.88(14) . . ? C17' Rh1' S2' 92.22(14) . . ? C22' Rh1' S2' 174.54(15) . . ? C21' Rh1' S2' 144.20(15) . . ? C18' Rh1' S2' 86.86(13) . . ? S1' Rh1' S2' 94.40(5) . . ? C2' S1' Rh1' 108.62(17) . . ? C7' S2' Rh1' 109.68(17) . . ? C2' N1' N2' 109.8(4) . . ? C2' N1' B1' 129.7(4) . . ? N2' N1' B1' 120.4(4) . . ? C3' N2' N1' 105.3(4) . . ? C2' N3' C3' 106.8(4) . . ? C2' N3' C5' 125.1(4) . . ? C3' N3' C5' 128.0(4) . . ? C7' N4' N5' 111.5(4) . . ? C7' N4' B1' 125.7(4) . . ? N5' N4' B1' 122.1(4) . . ? C8' N5' N4' 104.7(4) . . ? C7' N6' C8' 106.2(4) . . ? C7' N6' C10' 126.8(4) . . ? C8' N6' C10' 126.9(4) . . ? C12' N7' N8' 111.0(4) . . ? C12' N7' B1' 126.5(4) . . ? N8' N7' B1' 121.9(4) . . ? C13' N8' N7' 105.1(4) . . ? C13' N9' C12' 107.9(4) . . ? C13' N9' C15' 127.2(4) . . ? C12' N9' C15' 124.8(4) . . ? N1' B1' N4' 106.8(4) . . ? N1' B1' N7' 110.7(4) . . ? N4' B1' N7' 110.6(4) . . ? N1' B1' H1' 109.6 . . ? N4' B1' H1' 109.6 . . ? N7' B1' H1' 109.6 . . ? N1' C2' N3' 106.7(4) . . ? N1' C2' S1' 130.0(4) . . ? N3' C2' S1' 123.4(4) . . ? N2' C3' N3' 111.3(4) . . ? N2' C3' C4' 125.0(4) . . ? N3' C3' C4' 123.7(5) . . ? C3' C4' H39' 109.5 . . ? C3' C4' H40' 109.5 . . ? H39' C4' H40' 109.5 . . ? C3' C4' H41' 109.5 . . ? H39' C4' H41' 109.5 . . ? H40' C4' H41' 109.5 . . ? N3' C5' C6' 113.0(4) . . ? N3' C5' H42' 109.0 . . ? C6' C5' H42' 109.0 . . ? N3' C5' H43' 109.0 . . ? C6' C5' H43' 109.0 . . ? H42' C5' H43' 107.8 . . ? C5' C6' H44' 109.5 . . ? C5' C6' H45' 109.5 . . ? H44' C6' H45' 109.5 . . ? C5' C6' H46' 109.5 . . ? H44' C6' H46' 109.5 . . ? H45' C6' H46' 109.5 . . ? N4' C7' N6' 106.1(4) . . ? N4' C7' S2' 129.7(4) . . ? N6' C7' S2' 124.2(4) . . ? N5' C8' N6' 111.5(4) . . ? N5' C8' C9' 124.6(5) . . ? N6' C8' C9' 123.8(5) . . ? C8' C9' H47' 109.5 . . ? C8' C9' H48' 109.5 . . ? H47' C9' H48' 109.5 . . ? C8' C9' H49' 109.5 . . ? H47' C9' H49' 109.5 . . ? H48' C9' H49' 109.5 . . ? N6' C10' C11' 112.1(4) . . ? N6' C10' H50C 109.2 . . ? C11' C10' H50C 109.2 . . ? N6' C10' H51D 109.2 . . ? C11' C10' H51D 109.2 . . ? H50C C10' H51D 107.9 . . ? C10' C11' H52D 109.5 . . ? C10' C11' H53E 109.5 . . ? H52D C11' H53E 109.5 . . ? C10' C11' H54F 109.5 . . ? H52D C11' H54F 109.5 . . ? H53E C11' H54F 109.5 . . ? N7' C12' N9' 104.7(4) . . ? N7' C12' S3' 129.2(4) . . ? N9' C12' S3' 126.1(4) . . ? N8' C13' N9' 111.1(4) . . ? N8' C13' C14' 124.8(5) . . ? N9' C13' C14' 124.2(5) . . ? C13' C14' H55D 109.5 . . ? C13' C14' H56E 109.5 . . ? H55D C14' H56E 109.5 . . ? C13' C14' H57F 109.5 . . ? H55D C14' H57F 109.5 . . ? H56E C14' H57F 109.5 . . ? N9' C15' C16' 111.3(4) . . ? N9' C15' H58C 109.4 . . ? C16' C15' H58C 109.4 . . ? N9' C15' H59D 109.4 . . ? C16' C15' H59D 109.4 . . ? H58C C15' H59D 108.0 . . ? C15' C16' H60D 109.5 . . ? C15' C16' H61E 109.5 . . ? H60D C16' H61E 109.5 . . ? C15' C16' H62F 109.5 . . ? H60D C16' H62F 109.5 . . ? H61E C16' H62F 109.5 . . ? C18' C17' C24' 124.6(4) . . ? C18' C17' Rh1' 72.7(3) . . ? C24' C17' Rh1' 110.1(3) . . ? C18' C17' H63' 114.0 . . ? C24' C17' H63' 114.0 . . ? Rh1' C17' H63' 114.0 . . ? C17' C18' C19' 124.4(5) . . ? C17' C18' Rh1' 69.1(3) . . ? C19' C18' Rh1' 114.1(3) . . ? C17' C18' H64' 113.8 . . ? C19' C18' H64' 113.8 . . ? Rh1' C18' H64' 113.8 . . ? C18' C19' C20' 111.4(4) . . ? C18' C19' H65C 109.4 . . ? C20' C19' H65C 109.4 . . ? C18' C19' H66D 109.4 . . ? C20' C19' H66D 109.4 . . ? H65C C19' H66D 108.0 . . ? C21' C20' C19' 112.5(4) . . ? C21' C20' H67C 109.1 . . ? C19' C20' H67C 109.1 . . ? C21' C20' H68D 109.1 . . ? C19' C20' H68D 109.1 . . ? H67C C20' H68D 107.8 . . ? C22' C21' C20' 126.3(5) . . ? C22' C21' Rh1' 70.6(3) . . ? C20' C21' Rh1' 112.0(3) . . ? C22' C21' H69' 113.4 . . ? C20' C21' H69' 113.4 . . ? Rh1' C21' H69' 113.4 . . ? C21' C22' C23' 122.6(5) . . ? C21' C22' Rh1' 70.8(3) . . ? C23' C22' Rh1' 112.9(3) . . ? C21' C22' H70' 114.4 . . ? C23' C22' H70' 114.4 . . ? Rh1' C22' H70' 114.4 . . ? C22' C23' C24' 112.3(4) . . ? C22' C23' H71C 109.1 . . ? C24' C23' H71C 109.1 . . ? C22' C23' H72D 109.1 . . ? C24' C23' H72D 109.1 . . ? H71C C23' H72D 107.9 . . ? C17' C24' C23' 112.1(4) . . ? C17' C24' H73C 109.2 . . ? C23' C24' H73C 109.2 . . ? C17' C24' H74D 109.2 . . ? C23' C24' H74D 109.2 . . ? H73C C24' H74D 107.9 . . ? H1O O1 H2O 108(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Rh1 S1 C2 -70.2(2) . . . . ? C18 Rh1 S1 C2 -28.8(7) . . . . ? C17 Rh1 S1 C2 -175.7(3) . . . . ? C22 Rh1 S1 C2 -108.4(2) . . . . ? S2 Rh1 S1 C2 98.00(17) . . . . ? C21 Rh1 S2 C7 74.3(6) . . . . ? C18 Rh1 S2 C7 134.2(2) . . . . ? C17 Rh1 S2 C7 171.6(2) . . . . ? C22 Rh1 S2 C7 -133.5(3) . . . . ? S1 Rh1 S2 C7 -36.20(16) . . . . ? C2 N1 N2 C3 0.8(5) . . . . ? B1 N1 N2 C3 -171.3(4) . . . . ? C7 N4 N5 C8 2.2(5) . . . . ? B1 N4 N5 C8 174.7(4) . . . . ? C12 N7 N8 C13 0.8(5) . . . . ? B1 N7 N8 C13 -169.6(4) . . . . ? C12 N7 B1 N1 -103.2(5) . . . . ? N8 N7 B1 N1 65.3(5) . . . . ? C12 N7 B1 N4 140.9(4) . . . . ? N8 N7 B1 N4 -50.6(5) . . . . ? C2 N1 B1 N7 -178.7(4) . . . . ? N2 N1 B1 N7 -7.7(5) . . . . ? C2 N1 B1 N4 -58.8(5) . . . . ? N2 N1 B1 N4 112.2(4) . . . . ? C7 N4 B1 N7 -126.1(5) . . . . ? N5 N4 B1 N7 63.0(5) . . . . ? C7 N4 B1 N1 115.2(5) . . . . ? N5 N4 B1 N1 -55.7(5) . . . . ? N2 N1 C2 N3 -1.3(5) . . . . ? B1 N1 C2 N3 170.7(4) . . . . ? N2 N1 C2 S1 -179.3(3) . . . . ? B1 N1 C2 S1 -7.3(6) . . . . ? C3 N3 C2 N1 1.3(5) . . . . ? C5 N3 C2 N1 177.7(4) . . . . ? C3 N3 C2 S1 179.4(3) . . . . ? C5 N3 C2 S1 -4.2(6) . . . . ? Rh1 S1 C2 N1 -31.2(4) . . . . ? Rh1 S1 C2 N3 151.2(3) . . . . ? N1 N2 C3 N3 0.1(5) . . . . ? N1 N2 C3 C4 180.0(4) . . . . ? C2 N3 C3 N2 -0.9(5) . . . . ? C5 N3 C3 N2 -177.3(4) . . . . ? C2 N3 C3 C4 179.2(4) . . . . ? C5 N3 C3 C4 2.8(7) . . . . ? C2 N3 C5 C6 -94.8(5) . . . . ? C3 N3 C5 C6 81.0(5) . . . . ? N5 N4 C7 N6 -3.0(5) . . . . ? B1 N4 C7 N6 -174.6(4) . . . . ? N5 N4 C7 S2 175.7(3) . . . . ? B1 N4 C7 S2 4.1(7) . . . . ? C8 N6 C7 N4 2.7(5) . . . . ? C10 N6 C7 N4 175.8(4) . . . . ? C8 N6 C7 S2 -176.1(3) . . . . ? C10 N6 C7 S2 -3.0(6) . . . . ? Rh1 S2 C7 N4 -39.1(5) . . . . ? Rh1 S2 C7 N6 139.4(3) . . . . ? N4 N5 C8 N6 -0.4(5) . . . . ? N4 N5 C8 C9 179.1(4) . . . . ? C7 N6 C8 N5 -1.4(5) . . . . ? C10 N6 C8 N5 -174.4(4) . . . . ? C7 N6 C8 C9 179.1(4) . . . . ? C10 N6 C8 C9 6.1(7) . . . . ? C8 N6 C10 C11 88.7(6) . . . . ? C7 N6 C10 C11 -83.1(5) . . . . ? C13 N9 C12 N7 0.8(5) . . . . ? C15 N9 C12 N7 178.9(4) . . . . ? C13 N9 C12 S3 -178.2(3) . . . . ? C15 N9 C12 S3 -0.1(7) . . . . ? N8 N7 C12 N9 -1.0(5) . . . . ? B1 N7 C12 N9 168.5(4) . . . . ? N8 N7 C12 S3 178.0(3) . . . . ? B1 N7 C12 S3 -12.5(7) . . . . ? N7 N8 C13 N9 -0.3(5) . . . . ? N7 N8 C13 C14 179.1(4) . . . . ? C12 N9 C13 N8 -0.3(5) . . . . ? C15 N9 C13 N8 -178.4(4) . . . . ? C12 N9 C13 C14 -179.7(4) . . . . ? C15 N9 C13 C14 2.2(7) . . . . ? C12 N9 C15 C16 95.1(5) . . . . ? C13 N9 C15 C16 -87.1(5) . . . . ? C21 Rh1 C17 C18 66.2(3) . . . . ? C22 Rh1 C17 C18 100.6(3) . . . . ? S2 Rh1 C17 C18 -101.2(3) . . . . ? S1 Rh1 C17 C18 169.5(3) . . . . ? C21 Rh1 C17 C24 -55.3(4) . . . . ? C18 Rh1 C17 C24 -121.5(5) . . . . ? C22 Rh1 C17 C24 -20.9(3) . . . . ? S2 Rh1 C17 C24 137.3(3) . . . . ? S1 Rh1 C17 C24 48.0(5) . . . . ? C24 C17 C18 C19 -3.1(7) . . . . ? Rh1 C17 C18 C19 -105.3(5) . . . . ? C24 C17 C18 Rh1 102.1(4) . . . . ? C21 Rh1 C18 C17 -114.0(3) . . . . ? C22 Rh1 C18 C17 -76.4(3) . . . . ? S2 Rh1 C18 C17 77.0(3) . . . . ? S1 Rh1 C18 C17 -155.9(5) . . . . ? C21 Rh1 C18 C19 6.3(3) . . . . ? C17 Rh1 C18 C19 120.3(5) . . . . ? C22 Rh1 C18 C19 43.9(4) . . . . ? S2 Rh1 C18 C19 -162.7(3) . . . . ? S1 Rh1 C18 C19 -35.6(9) . . . . ? C17 C18 C19 C20 93.3(6) . . . . ? Rh1 C18 C19 C20 11.3(5) . . . . ? C18 C19 C20 C21 -31.2(6) . . . . ? C19 C20 C21 C22 -44.8(7) . . . . ? C19 C20 C21 Rh1 35.8(5) . . . . ? C18 Rh1 C21 C22 99.5(3) . . . . ? C17 Rh1 C21 C22 64.6(3) . . . . ? S2 Rh1 C21 C22 160.2(5) . . . . ? S1 Rh1 C21 C22 -88.5(3) . . . . ? C18 Rh1 C21 C20 -22.7(3) . . . . ? C17 Rh1 C21 C20 -57.5(4) . . . . ? C22 Rh1 C21 C20 -122.1(5) . . . . ? S2 Rh1 C21 C20 38.1(9) . . . . ? S1 Rh1 C21 C20 149.3(3) . . . . ? C20 C21 C22 C23 -5.0(8) . . . . ? Rh1 C21 C22 C23 -106.0(5) . . . . ? C20 C21 C22 Rh1 101.0(5) . . . . ? C18 Rh1 C22 C21 -77.8(3) . . . . ? C17 Rh1 C22 C21 -115.3(3) . . . . ? S2 Rh1 C22 C21 -170.5(2) . . . . ? S1 Rh1 C22 C21 90.4(3) . . . . ? C21 Rh1 C22 C23 119.3(5) . . . . ? C18 Rh1 C22 C23 41.5(4) . . . . ? C17 Rh1 C22 C23 4.0(3) . . . . ? S2 Rh1 C22 C23 -51.2(5) . . . . ? S1 Rh1 C22 C23 -150.3(3) . . . . ? C21 C22 C23 C24 95.1(6) . . . . ? Rh1 C22 C23 C24 13.5(5) . . . . ? C18 C17 C24 C23 -45.7(6) . . . . ? Rh1 C17 C24 C23 34.9(5) . . . . ? C22 C23 C24 C17 -31.7(6) . . . . ? C17' Rh1' S1' C2' 66.0(7) . . . . ? C22' Rh1' S1' C2' 119.8(2) . . . . ? C21' Rh1' S1' C2' 157.6(2) . . . . ? C18' Rh1' S1' C2' -149.8(3) . . . . ? S2' Rh1' S1' C2' -58.27(17) . . . . ? C17' Rh1' S2' C7' -80.0(2) . . . . ? C22' Rh1' S2' C7' -68.7(15) . . . . ? C21' Rh1' S2' C7' 173.6(3) . . . . ? C18' Rh1' S2' C7' -117.8(2) . . . . ? S1' Rh1' S2' C7' 90.38(17) . . . . ? C2' N1' N2' C3' 2.3(5) . . . . ? B1' N1' N2' C3' 178.1(4) . . . . ? C7' N4' N5' C8' -0.9(5) . . . . ? B1' N4' N5' C8' -171.7(4) . . . . ? C12' N7' N8' C13' 1.6(5) . . . . ? B1' N7' N8' C13' 173.1(4) . . . . ? C2' N1' B1' N4' 107.6(5) . . . . ? N2' N1' B1' N4' -67.2(5) . . . . ? C2' N1' B1' N7' -132.0(5) . . . . ? N2' N1' B1' N7' 53.2(5) . . . . ? C7' N4' B1' N1' -75.9(5) . . . . ? N5' N4' B1' N1' 93.6(5) . . . . ? C7' N4' B1' N7' 163.6(4) . . . . ? N5' N4' B1' N7' -26.9(6) . . . . ? C12' N7' B1' N1' -177.5(4) . . . . ? N8' N7' B1' N1' 12.3(6) . . . . ? C12' N7' B1' N4' -59.4(6) . . . . ? N8' N7' B1' N4' 130.4(4) . . . . ? N2' N1' C2' N3' -2.8(5) . . . . ? B1' N1' C2' N3' -178.1(4) . . . . ? N2' N1' C2' S1' 176.6(3) . . . . ? B1' N1' C2' S1' 1.3(7) . . . . ? C3' N3' C2' N1' 2.2(5) . . . . ? C5' N3' C2' N1' -178.9(4) . . . . ? C3' N3' C2' S1' -177.2(3) . . . . ? C5' N3' C2' S1' 1.7(6) . . . . ? Rh1' S1' C2' N1' -14.9(5) . . . . ? Rh1' S1' C2' N3' 164.4(3) . . . . ? N1' N2' C3' N3' -0.9(5) . . . . ? N1' N2' C3' C4' 179.3(4) . . . . ? C2' N3' C3' N2' -0.8(5) . . . . ? C5' N3' C3' N2' -179.7(4) . . . . ? C2' N3' C3' C4' 179.0(4) . . . . ? C5' N3' C3' C4' 0.1(7) . . . . ? C2' N3' C5' C6' 89.4(5) . . . . ? C3' N3' C5' C6' -91.9(5) . . . . ? N5' N4' C7' N6' 2.1(5) . . . . ? B1' N4' C7' N6' 172.5(4) . . . . ? N5' N4' C7' S2' -177.2(3) . . . . ? B1' N4' C7' S2' -6.8(7) . . . . ? C8' N6' C7' N4' -2.4(5) . . . . ? C10' N6' C7' N4' -177.7(4) . . . . ? C8' N6' C7' S2' 177.0(3) . . . . ? C10' N6' C7' S2' 1.6(7) . . . . ? Rh1' S2' C7' N4' -16.7(5) . . . . ? Rh1' S2' C7' N6' 164.1(3) . . . . ? N4' N5' C8' N6' -0.7(5) . . . . ? N4' N5' C8' C9' 179.4(4) . . . . ? C7' N6' C8' N5' 2.0(5) . . . . ? C10' N6' C8' N5' 177.3(4) . . . . ? C7' N6' C8' C9' -178.2(4) . . . . ? C10' N6' C8' C9' -2.8(7) . . . . ? C7' N6' C10' C11' 82.6(6) . . . . ? C8' N6' C10' C11' -91.8(6) . . . . ? N8' N7' C12' N9' -3.1(4) . . . . ? B1' N7' C12' N9' -174.2(4) . . . . ? N8' N7' C12' S3' 174.6(3) . . . . ? B1' N7' C12' S3' 3.6(7) . . . . ? C13' N9' C12' N7' 3.4(5) . . . . ? C15' N9' C12' N7' -174.5(4) . . . . ? C13' N9' C12' S3' -174.4(3) . . . . ? C15' N9' C12' S3' 7.7(6) . . . . ? N7' N8' C13' N9' 0.7(5) . . . . ? N7' N8' C13' C14' -178.1(4) . . . . ? C12' N9' C13' N8' -2.6(5) . . . . ? C15' N9' C13' N8' 175.2(4) . . . . ? C12' N9' C13' C14' 176.2(4) . . . . ? C15' N9' C13' C14' -6.0(7) . . . . ? C13' N9' C15' C16' -86.8(6) . . . . ? C12' N9' C15' C16' 90.7(5) . . . . ? C22' Rh1' C17' C18' 99.0(3) . . . . ? C21' Rh1' C17' C18' 63.4(3) . . . . ? S1' Rh1' C17' C18' 153.5(5) . . . . ? S2' Rh1' C17' C18' -82.1(3) . . . . ? C22' Rh1' C17' C24' -22.2(3) . . . . ? C21' Rh1' C17' C24' -57.8(4) . . . . ? C18' Rh1' C17' C24' -121.3(5) . . . . ? S1' Rh1' C17' C24' 32.3(9) . . . . ? S2' Rh1' C17' C24' 156.7(3) . . . . ? C24' C17' C18' C19' -2.7(8) . . . . ? Rh1' C17' C18' C19' -105.6(4) . . . . ? C24' C17' C18' Rh1' 102.8(5) . . . . ? C22' Rh1' C18' C17' -78.3(3) . . . . ? C21' Rh1' C18' C17' -115.9(3) . . . . ? S1' Rh1' C18' C17' -168.9(2) . . . . ? S2' Rh1' C18' C17' 97.6(3) . . . . ? C17' Rh1' C18' C19' 119.5(5) . . . . ? C22' Rh1' C18' C19' 41.2(4) . . . . ? C21' Rh1' C18' C19' 3.5(4) . . . . ? S1' Rh1' C18' C19' -49.5(5) . . . . ? S2' Rh1' C18' C19' -142.9(4) . . . . ? C17' C18' C19' C20' 94.2(6) . . . . ? Rh1' C18' C19' C20' 13.8(6) . . . . ? C18' C19' C20' C21' -31.3(6) . . . . ? C19' C20' C21' C22' -46.9(7) . . . . ? C19' C20' C21' Rh1' 34.6(6) . . . . ? C17' Rh1' C21' C22' 67.5(3) . . . . ? C18' Rh1' C21' C22' 101.7(3) . . . . ? S1' Rh1' C21' C22' -100.7(3) . . . . ? S2' Rh1' C21' C22' 172.2(2) . . . . ? C17' Rh1' C21' C20' -54.8(4) . . . . ? C22' Rh1' C21' C20' -122.3(5) . . . . ? C18' Rh1' C21' C20' -20.7(4) . . . . ? S1' Rh1' C21' C20' 137.0(4) . . . . ? S2' Rh1' C21' C20' 49.9(5) . . . . ? C20' C21' C22' C23' -2.0(8) . . . . ? Rh1' C21' C22' C23' -105.4(5) . . . . ? C20' C21' C22' Rh1' 103.5(5) . . . . ? C17' Rh1' C22' C21' -112.5(3) . . . . ? C18' Rh1' C22' C21' -74.9(3) . . . . ? S1' Rh1' C22' C21' 77.0(3) . . . . ? S2' Rh1' C22' C21' -123.9(14) . . . . ? C17' Rh1' C22' C23' 5.7(4) . . . . ? C21' Rh1' C22' C23' 118.2(5) . . . . ? C18' Rh1' C22' C23' 43.3(4) . . . . ? S1' Rh1' C22' C23' -164.8(4) . . . . ? S2' Rh1' C22' C23' -5.7(18) . . . . ? C21' C22' C23' C24' 93.2(6) . . . . ? Rh1' C22' C23' C24' 12.0(6) . . . . ? C18' C17' C24' C23' -47.3(7) . . . . ? Rh1' C17' C24' C23' 35.1(5) . . . . ? C22' C23' C24' C17' -31.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.609 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.123 data_5 _database_code_depnum_ccdc_archive 'CCDC 733501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H50 B2 N18 O3 Rh2 S6' _chemical_formula_sum 'C33 H50 B2 N18 O3 Rh2 S6' _chemical_formula_weight 1166.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 hexagonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_int_tables_number 167 _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 12.8960(18) _cell_length_b 12.8960(18) _cell_length_c 74.468(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10725(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2673 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3564 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78890534 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34932 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -96 _diffrn_reflns_limit_l_max 96 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2673 _reflns_number_gt 2086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Briker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.310 -0.293 0.000 4374.4 -29.5 _platon_squeeze_details ; ? ; _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^)+(0.0783P)^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 2673 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.000 _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 0.6667 0.3333 0.066147(6) 0.0301(2) Uani 1 3 d S . . S1 S 0.68275(10) 0.17740(9) 0.048886(12) 0.0335(3) Uani 1 1 d . . . N1 N 0.5803(3) 0.2045(3) 0.01798(4) 0.0326(8) Uani 1 1 d . . . N2 N 0.4772(3) 0.1388(3) 0.00778(4) 0.0343(8) Uani 1 1 d . . . N3 N 0.4744(3) 0.0341(3) 0.03120(4) 0.0337(8) Uani 1 1 d . . . O1 O 0.8778(3) 0.3333 0.0833 0.0476(11) Uani 1 2 d S . . B1 B 0.6667 0.3333 0.01158(10) 0.0317(16) Uani 1 3 d S . . H1 H 0.6667 0.3333 -0.0018 0.038 Uiso 1 3 calc SR . . C1 C 0.7878(5) 0.3333 0.0833 0.0340(13) Uani 1 2 d S . . C2 C 0.5790(4) 0.1403(4) 0.03217(5) 0.0332(9) Uani 1 1 d . . . C3 C 0.4154(4) 0.0376(4) 0.01617(5) 0.0368(9) Uani 1 1 d . . . C4 C 0.2985(4) -0.0616(5) 0.01024(6) 0.0513(12) Uani 1 1 d . . . H4A H 0.2806 -0.0446 -0.0018 0.077 Uiso 1 1 calc R . . H4B H 0.2360 -0.0699 0.0186 0.077 Uiso 1 1 calc R . . H4C H 0.3011 -0.1362 0.0100 0.077 Uiso 1 1 calc R . . C5 C 0.4336(5) -0.0647(4) 0.04427(6) 0.0425(11) Uani 1 1 d . . . H5A H 0.3451 -0.1124 0.0441 0.051 Uiso 1 1 calc R . . H5B H 0.4586 -0.0310 0.0565 0.051 Uiso 1 1 calc R . . C6 C 0.4838(5) -0.1455(4) 0.04025(6) 0.0479(12) Uani 1 1 d . . . H6A H 0.4549 -0.1833 0.0285 0.072 Uiso 1 1 calc R . . H6B H 0.4577 -0.2074 0.0495 0.072 Uiso 1 1 calc R . . H6C H 0.5714 -0.0982 0.0401 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0351(2) 0.0351(2) 0.0201(3) 0.000 0.000 0.01757(12) S1 0.0419(6) 0.0346(6) 0.0272(5) -0.0009(4) -0.0035(4) 0.0214(5) N1 0.0325(18) 0.040(2) 0.0268(15) -0.0028(14) -0.0030(13) 0.0191(16) N2 0.0328(19) 0.038(2) 0.0321(16) -0.0109(14) -0.0072(14) 0.0182(16) N3 0.0364(19) 0.0296(18) 0.0347(17) -0.0057(14) -0.0013(15) 0.0161(16) O1 0.0429(18) 0.077(4) 0.034(2) -0.001(2) -0.0004(11) 0.0387(18) B1 0.035(2) 0.035(2) 0.026(3) 0.000 0.000 0.0174(12) C1 0.036(2) 0.041(4) 0.026(3) -0.001(2) -0.0004(12) 0.0205(18) C2 0.040(2) 0.032(2) 0.0305(18) -0.0029(15) 0.0009(17) 0.0205(19) C3 0.037(2) 0.036(2) 0.038(2) -0.0093(18) -0.0007(18) 0.019(2) C4 0.039(3) 0.047(3) 0.053(3) -0.011(2) -0.009(2) 0.011(2) C5 0.050(3) 0.032(2) 0.039(2) 0.0024(18) 0.007(2) 0.015(2) C6 0.065(3) 0.036(3) 0.047(2) -0.002(2) -0.005(2) 0.029(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 Rh1 C1 2.019(5) . ? Rh1 C1 2.019(5) 3_665 ? Rh1 C1 2.019(5) 2_655 ? Rh1 S1 2.4809(11) 2_655 ? Rh1 S1 2.4809(11) 3_665 ? Rh1 S1 2.4811(11) . ? Rh1 Rh1 2.5594(10) 16_544 ? S1 C2 1.711(4) . ? N1 C2 1.337(5) . ? N1 N2 1.392(4) . ? N1 B1 1.542(4) . ? N2 C3 1.300(6) . ? N3 C2 1.361(5) . ? N3 C3 1.367(5) . ? N3 C5 1.475(5) . ? O1 C1 1.161(7) . ? B1 N1 1.542(4) 2_655 ? B1 N1 1.542(4) 3_665 ? B1 H1 1.0000 . ? C1 Rh1 2.019(5) 16_544 ? C3 C4 1.475(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.505(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C1 84.11(17) . 3_665 ? C1 Rh1 C1 84.11(17) . 2_655 ? C1 Rh1 C1 84.10(17) 3_665 2_655 ? C1 Rh1 S1 92.71(8) . 2_655 ? C1 Rh1 S1 170.95(10) 3_665 2_655 ? C1 Rh1 S1 87.15(8) 2_655 2_655 ? C1 Rh1 S1 170.95(10) . 3_665 ? C1 Rh1 S1 87.15(8) 3_665 3_665 ? C1 Rh1 S1 92.71(8) 2_655 3_665 ? S1 Rh1 S1 95.60(3) 2_655 3_665 ? C1 Rh1 S1 87.15(8) . . ? C1 Rh1 S1 92.71(7) 3_665 . ? C1 Rh1 S1 170.96(10) 2_655 . ? S1 Rh1 S1 95.59(3) 2_655 . ? S1 Rh1 S1 95.59(3) 3_665 . ? C1 Rh1 Rh1 50.66(11) . 16_544 ? C1 Rh1 Rh1 50.66(11) 3_665 16_544 ? C1 Rh1 Rh1 50.66(11) 2_655 16_544 ? S1 Rh1 Rh1 121.20(2) 2_655 16_544 ? S1 Rh1 Rh1 121.20(2) 3_665 16_544 ? S1 Rh1 Rh1 121.20(2) . 16_544 ? C2 S1 Rh1 103.45(14) . . ? C2 N1 N2 110.0(3) . . ? C2 N1 B1 133.6(4) . . ? N2 N1 B1 116.3(3) . . ? C3 N2 N1 105.6(3) . . ? C2 N3 C3 107.3(3) . . ? C2 N3 C5 125.5(4) . . ? C3 N3 C5 127.2(4) . . ? N1 B1 N1 110.9(3) . 2_655 ? N1 B1 N1 110.9(3) . 3_665 ? N1 B1 N1 110.9(3) 2_655 3_665 ? N1 B1 H1 108.0 . . ? N1 B1 H1 108.0 2_655 . ? N1 B1 H1 108.0 3_665 . ? O1 C1 Rh1 140.67(11) . 16_544 ? O1 C1 Rh1 140.67(11) . . ? Rh1 C1 Rh1 78.7(2) 16_544 . ? N1 C2 N3 106.3(3) . . ? N1 C2 S1 129.5(3) . . ? N3 C2 S1 124.2(3) . . ? N2 C3 N3 110.8(4) . . ? N2 C3 C4 125.1(4) . . ? N3 C3 C4 124.1(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 112.1(4) . . ? N3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 S1 C2 176.30(17) . . . . ? C1 Rh1 S1 C2 92.34(17) 3_665 . . . ? C1 Rh1 S1 C2 161.4(4) 2_655 . . . ? S1 Rh1 S1 C2 -91.26(14) 2_655 . . . ? S1 Rh1 S1 C2 4.94(15) 3_665 . . . ? Rh1 Rh1 S1 C2 136.84(15) 16_544 . . . ? C2 N1 N2 C3 1.0(4) . . . . ? B1 N1 N2 C3 -176.2(3) . . . . ? C2 N1 B1 N1 28.7(7) . . . 2_655 ? N2 N1 B1 N1 -154.9(4) . . . 2_655 ? C2 N1 B1 N1 -94.9(4) . . . 3_665 ? N2 N1 B1 N1 81.4(6) . . . 3_665 ? C1 Rh1 C1 O1 137.67(7) 3_665 . . . ? C1 Rh1 C1 O1 -137.67(7) 2_655 . . . ? S1 Rh1 C1 O1 -50.82(2) 2_655 . . . ? S1 Rh1 C1 O1 152.6(4) 3_665 . . . ? S1 Rh1 C1 O1 44.65(3) . . . . ? Rh1 Rh1 C1 O1 179.998(2) 16_544 . . . ? C1 Rh1 C1 Rh1 -42.32(7) 3_665 . . 16_544 ? C1 Rh1 C1 Rh1 42.33(7) 2_655 . . 16_544 ? S1 Rh1 C1 Rh1 129.18(2) 2_655 . . 16_544 ? S1 Rh1 C1 Rh1 -27.4(4) 3_665 . . 16_544 ? S1 Rh1 C1 Rh1 -135.35(3) . . . 16_544 ? N2 N1 C2 N3 -0.8(4) . . . . ? B1 N1 C2 N3 175.7(4) . . . . ? N2 N1 C2 S1 179.8(3) . . . . ? B1 N1 C2 S1 -3.7(7) . . . . ? C3 N3 C2 N1 0.3(4) . . . . ? C5 N3 C2 N1 -179.1(4) . . . . ? C3 N3 C2 S1 179.8(3) . . . . ? C5 N3 C2 S1 0.4(6) . . . . ? Rh1 S1 C2 N1 69.7(4) . . . . ? Rh1 S1 C2 N3 -109.6(3) . . . . ? N1 N2 C3 N3 -0.8(4) . . . . ? N1 N2 C3 C4 -179.8(4) . . . . ? C2 N3 C3 N2 0.3(5) . . . . ? C5 N3 C3 N2 179.7(4) . . . . ? C2 N3 C3 C4 179.3(4) . . . . ? C5 N3 C3 C4 -1.3(7) . . . . ? C2 N3 C5 C6 -85.2(5) . . . . ? C3 N3 C5 C6 95.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.573 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.110 data_6 _database_code_depnum_ccdc_archive 'CCDC 733502' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H58 B N9 O P Rh S3, C H2 Cl2' _chemical_formula_sum 'C35 H60 B Cl2 N9 O P Rh S3' _chemical_formula_weight 934.69 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.530(2) _cell_length_b 13.237(3) _cell_length_c 14.645(3) _cell_angle_alpha 87.27(3) _cell_angle_beta 86.12(3) _cell_angle_gamma 79.85(3) _cell_volume 2193.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.133 _cell_measurement_theta_max 20.676 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24642 _diffrn_reflns_av_R_equivalents 0.1656 _diffrn_reflns_av_sigmaI/netI 0.2395 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9963 _reflns_number_gt 4810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^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 9963 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.874 _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 0.83730(5) 0.80815(5) 0.74264(4) 0.02089(17) Uani 1 1 d . . . P1 P 0.78269(16) 0.97830(17) 0.72355(12) 0.0228(5) Uani 1 1 d . . . S1 S 0.91433(17) 0.79662(18) 0.58482(12) 0.0336(5) Uani 1 1 d . . . S2 S 0.83798(16) 0.62860(17) 0.76682(13) 0.0291(5) Uani 1 1 d . . . S3 S 1.19189(18) 0.74958(18) 0.92964(12) 0.0336(5) Uani 1 1 d . . . O1 O 0.7354(5) 0.8213(5) 0.9346(3) 0.0401(15) Uani 1 1 d . . . N1 N 1.1039(5) 0.6495(5) 0.6339(4) 0.0220(14) Uani 1 1 d . . . N2 N 1.1836(5) 0.5723(5) 0.5930(4) 0.0285(16) Uani 1 1 d . . . N3 N 1.0700(5) 0.6586(5) 0.4901(4) 0.0241(15) Uani 1 1 d . . . N4 N 1.0759(5) 0.5817(5) 0.7948(4) 0.0223(14) Uani 1 1 d . . . N5 N 1.1567(5) 0.5061(5) 0.8373(4) 0.0279(16) Uani 1 1 d . . . N6 N 0.9725(5) 0.4814(5) 0.8659(4) 0.0237(15) Uani 1 1 d . . . N7 N 1.2392(5) 0.6838(5) 0.7540(4) 0.0213(14) Uani 1 1 d . . . N8 N 1.3346(5) 0.6677(5) 0.6894(4) 0.0249(15) Uani 1 1 d . . . N9 N 1.3945(5) 0.7140(5) 0.8181(4) 0.0242(15) Uani 1 1 d . . . B1 B 1.1130(7) 0.6725(7) 0.7360(5) 0.023(2) Uani 1 1 d . . . H1 H 1.0578 0.7374 0.7515 0.027 Uiso 1 1 calc R . . C1 C 0.7736(6) 0.8183(6) 0.8598(4) 0.0268(18) Uani 1 1 d . . . C2 C 1.0306(6) 0.7005(7) 0.5731(5) 0.031(2) Uani 1 1 d . . . C3 C 1.1618(6) 0.5797(7) 0.5061(5) 0.032(2) Uani 1 1 d . . . C4 C 1.2296(7) 0.5163(8) 0.4341(5) 0.048(3) Uani 1 1 d . . . H4A H 1.2873 0.4626 0.4622 0.071 Uiso 1 1 calc R . . H4B H 1.2708 0.5596 0.3918 0.071 Uiso 1 1 calc R . . H4C H 1.1756 0.4845 0.4004 0.071 Uiso 1 1 calc R . . C5 C 1.0236(7) 0.6954(7) 0.4000(5) 0.033(2) Uani 1 1 d . . . H5A H 1.0897 0.6881 0.3527 0.039 Uiso 1 1 calc R . . H5B H 0.9890 0.7692 0.4029 0.039 Uiso 1 1 calc R . . C6 C 0.9319(8) 0.6375(8) 0.3728(6) 0.052(3) Uani 1 1 d . . . H6A H 0.9677 0.5655 0.3638 0.078 Uiso 1 1 calc R . . H6B H 0.8995 0.6679 0.3156 0.078 Uiso 1 1 calc R . . H6C H 0.8684 0.6410 0.4212 0.078 Uiso 1 1 calc R . . C7 C 0.9654(6) 0.5665(6) 0.8094(4) 0.0218(17) Uani 1 1 d . . . C8 C 1.0906(6) 0.4468(6) 0.8792(5) 0.0267(18) Uani 1 1 d . . . C9 C 1.1375(7) 0.3542(6) 0.9335(5) 0.036(2) Uani 1 1 d . . . H9A H 1.2239 0.3437 0.9292 0.053 Uiso 1 1 calc R . . H9B H 1.1112 0.2946 0.9098 0.053 Uiso 1 1 calc R . . H9C H 1.1086 0.3625 0.9976 0.053 Uiso 1 1 calc R . . C10 C 0.8681(6) 0.4375(6) 0.9054(5) 0.0282(19) Uani 1 1 d . . . H10A H 0.8044 0.4941 0.9249 0.034 Uiso 1 1 calc R . . H10B H 0.8907 0.3936 0.9602 0.034 Uiso 1 1 calc R . . C11 C 0.8230(7) 0.3752(6) 0.8371(5) 0.0310(19) Uani 1 1 d . . . H11A H 0.8009 0.4184 0.7827 0.047 Uiso 1 1 calc R . . H11B H 0.7538 0.3488 0.8645 0.047 Uiso 1 1 calc R . . H11C H 0.8849 0.3175 0.8196 0.047 Uiso 1 1 calc R . . C12 C 1.2753(7) 0.7140(6) 0.8325(5) 0.0258(18) Uani 1 1 d . . . C13 C 1.4255(6) 0.6852(6) 0.7297(5) 0.0254(18) Uani 1 1 d . . . C14 C 1.5455(6) 0.6790(7) 0.6848(5) 0.031(2) Uani 1 1 d . . . H14A H 1.5454 0.6570 0.6219 0.046 Uiso 1 1 calc R . . H14B H 1.6014 0.6292 0.7189 0.046 Uiso 1 1 calc R . . H14C H 1.5691 0.7466 0.6840 0.046 Uiso 1 1 calc R . . C15 C 1.4744(7) 0.7288(7) 0.8879(5) 0.034(2) Uani 1 1 d . . . H15A H 1.4330 0.7808 0.9306 0.040 Uiso 1 1 calc R . . H15B H 1.5432 0.7553 0.8580 0.040 Uiso 1 1 calc R . . C16 C 1.5168(8) 0.6319(7) 0.9407(5) 0.042(2) Uani 1 1 d . . . H16A H 1.4489 0.6036 0.9680 0.063 Uiso 1 1 calc R . . H16B H 1.5655 0.6462 0.9892 0.063 Uiso 1 1 calc R . . H16C H 1.5639 0.5821 0.8995 0.063 Uiso 1 1 calc R . . C17 C 0.8908(6) 1.0485(6) 0.7665(4) 0.0255(18) Uani 1 1 d . . . H17 H 0.8663 1.1228 0.7489 0.031 Uiso 1 1 calc R . . C18 C 1.0164(6) 1.0128(6) 0.7216(5) 0.0272(18) Uani 1 1 d . . . H18A H 1.0389 0.9376 0.7321 0.033 Uiso 1 1 calc R . . H18B H 1.0148 1.0269 0.6547 0.033 Uiso 1 1 calc R . . C19 C 1.1094(7) 1.0657(7) 0.7589(5) 0.035(2) Uani 1 1 d . . . H19A H 1.0945 1.1393 0.7396 0.042 Uiso 1 1 calc R . . H19B H 1.1883 1.0348 0.7325 0.042 Uiso 1 1 calc R . . C20 C 1.1091(6) 1.0559(7) 0.8651(5) 0.033(2) Uani 1 1 d . . . H20A H 1.1345 0.9831 0.8845 0.039 Uiso 1 1 calc R . . H20B H 1.1657 1.0962 0.8869 0.039 Uiso 1 1 calc R . . C21 C 0.9863(6) 1.0948(6) 0.9073(5) 0.0275(18) Uani 1 1 d . . . H21A H 0.9865 1.0843 0.9746 0.033 Uiso 1 1 calc R . . H21B H 0.9650 1.1694 0.8933 0.033 Uiso 1 1 calc R . . C22 C 0.8946(6) 1.0401(7) 0.8714(4) 0.033(2) Uani 1 1 d . . . H22A H 0.8159 1.0695 0.8991 0.039 Uiso 1 1 calc R . . H22B H 0.9117 0.9666 0.8910 0.039 Uiso 1 1 calc R . . C23 C 0.7645(6) 1.0198(6) 0.6027(5) 0.0247(17) Uani 1 1 d . . . H23 H 0.8425 0.9927 0.5708 0.030 Uiso 1 1 calc R . . C24 C 0.7440(7) 1.1331(6) 0.5783(5) 0.034(2) Uani 1 1 d . . . H24A H 0.8033 1.1657 0.6061 0.041 Uiso 1 1 calc R . . H24B H 0.6647 1.1652 0.6030 0.041 Uiso 1 1 calc R . . C25 C 0.7530(7) 1.1509(7) 0.4741(5) 0.035(2) Uani 1 1 d . . . H25A H 0.7342 1.2255 0.4594 0.043 Uiso 1 1 calc R . . H25B H 0.8352 1.1261 0.4508 0.043 Uiso 1 1 calc R . . C26 C 0.6698(7) 1.0962(7) 0.4255(5) 0.035(2) Uani 1 1 d . . . H26A H 0.5870 1.1273 0.4420 0.042 Uiso 1 1 calc R . . H26B H 0.6839 1.1050 0.3584 0.042 Uiso 1 1 calc R . . C27 C 0.6893(7) 0.9839(6) 0.4520(5) 0.031(2) Uani 1 1 d . . . H27A H 0.7694 0.9513 0.4296 0.037 Uiso 1 1 calc R . . H27B H 0.6314 0.9506 0.4231 0.037 Uiso 1 1 calc R . . C28 C 0.6757(6) 0.9684(6) 0.5559(4) 0.0237(17) Uani 1 1 d . . . H28A H 0.6890 0.8940 0.5723 0.028 Uiso 1 1 calc R . . H28B H 0.5944 0.9983 0.5780 0.028 Uiso 1 1 calc R . . C29 C 0.6445(6) 1.0276(6) 0.7926(5) 0.0226(17) Uani 1 1 d . . . H29 H 0.6616 1.0043 0.8571 0.027 Uiso 1 1 calc R . . C30 C 0.6073(6) 1.1438(6) 0.7963(5) 0.0271(18) Uani 1 1 d . . . H30A H 0.6757 1.1752 0.8100 0.032 Uiso 1 1 calc R . . H30B H 0.5804 1.1719 0.7359 0.032 Uiso 1 1 calc R . . C31 C 0.5084(7) 1.1711(7) 0.8692(5) 0.036(2) Uani 1 1 d . . . H31A H 0.4842 1.2466 0.8693 0.044 Uiso 1 1 calc R . . H31B H 0.5379 1.1479 0.9300 0.044 Uiso 1 1 calc R . . C32 C 0.4019(7) 1.1224(7) 0.8539(5) 0.035(2) Uani 1 1 d . . . H32A H 0.3421 1.1378 0.9054 0.042 Uiso 1 1 calc R . . H32B H 0.3661 1.1518 0.7968 0.042 Uiso 1 1 calc R . . C33 C 0.4375(6) 1.0090(7) 0.8472(5) 0.037(2) Uani 1 1 d . . . H33A H 0.3684 0.9791 0.8325 0.045 Uiso 1 1 calc R . . H33B H 0.4638 0.9789 0.9071 0.045 Uiso 1 1 calc R . . C34 C 0.5379(6) 0.9815(7) 0.7729(5) 0.0294(19) Uani 1 1 d . . . H34A H 0.5604 0.9059 0.7708 0.035 Uiso 1 1 calc R . . H34B H 0.5100 1.0077 0.7124 0.035 Uiso 1 1 calc R . . C35 C 0.3950(7) 0.4159(8) 0.6873(6) 0.048(3) Uani 1 1 d . . . H35A H 0.3294 0.4020 0.7306 0.058 Uiso 1 1 calc R . . H35B H 0.3700 0.4840 0.6569 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.5205(2) 0.4201(2) 0.74968(18) 0.0585(7) Uani 1 1 d . . . Cl2 Cl 0.4206(3) 0.3235(3) 0.6056(2) 0.1024(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 Rh1 0.0203(3) 0.0331(4) 0.0088(3) -0.0001(2) -0.0020(2) -0.0029(2) P1 0.0166(9) 0.0389(14) 0.0126(9) 0.0015(9) -0.0039(7) -0.0032(9) S1 0.0344(11) 0.0473(15) 0.0131(9) -0.0007(9) -0.0003(8) 0.0084(10) S2 0.0208(9) 0.0359(14) 0.0308(11) 0.0010(9) -0.0071(8) -0.0041(9) S3 0.0451(12) 0.0415(15) 0.0145(9) -0.0052(9) 0.0039(8) -0.0090(10) O1 0.053(4) 0.050(4) 0.015(3) 0.003(3) 0.009(2) -0.005(3) N1 0.021(3) 0.037(4) 0.009(3) -0.006(3) -0.006(2) -0.007(3) N2 0.024(3) 0.042(5) 0.017(3) -0.006(3) 0.000(3) 0.003(3) N3 0.028(3) 0.028(4) 0.014(3) 0.000(3) -0.003(2) 0.002(3) N4 0.022(3) 0.034(4) 0.010(3) 0.001(3) -0.003(2) -0.002(3) N5 0.026(3) 0.034(4) 0.023(3) -0.003(3) -0.009(3) 0.000(3) N6 0.028(3) 0.034(4) 0.012(3) -0.005(3) 0.001(2) -0.012(3) N7 0.029(3) 0.023(4) 0.012(3) 0.001(3) -0.003(2) -0.005(3) N8 0.024(3) 0.032(4) 0.017(3) 0.002(3) 0.001(3) -0.002(3) N9 0.030(3) 0.030(4) 0.014(3) 0.000(3) -0.006(3) -0.006(3) B1 0.026(4) 0.033(6) 0.006(4) -0.006(4) 0.003(3) 0.006(4) C1 0.042(5) 0.026(5) 0.007(3) 0.001(3) 0.004(3) 0.006(4) C2 0.030(4) 0.048(6) 0.015(4) -0.004(4) -0.004(3) -0.005(4) C3 0.022(4) 0.054(6) 0.022(4) -0.004(4) -0.005(3) -0.008(4) C4 0.044(5) 0.067(8) 0.027(5) -0.007(5) -0.002(4) 0.004(5) C5 0.038(5) 0.042(6) 0.017(4) -0.001(4) -0.003(3) -0.005(4) C6 0.055(6) 0.066(8) 0.036(5) 0.002(5) -0.012(4) -0.013(5) C7 0.022(4) 0.033(5) 0.011(3) -0.006(3) 0.002(3) -0.006(3) C8 0.029(4) 0.033(5) 0.016(4) -0.003(3) -0.006(3) 0.001(4) C9 0.045(5) 0.035(6) 0.028(4) 0.001(4) -0.013(4) -0.006(4) C10 0.030(4) 0.040(6) 0.015(4) 0.001(4) 0.001(3) -0.010(4) C11 0.044(5) 0.025(5) 0.026(4) 0.003(4) -0.002(4) -0.011(4) C12 0.043(5) 0.016(4) 0.016(4) 0.001(3) 0.003(3) -0.002(3) C13 0.025(4) 0.027(5) 0.025(4) 0.002(3) -0.008(3) -0.007(3) C14 0.028(4) 0.044(6) 0.020(4) -0.005(4) -0.002(3) -0.005(4) C15 0.035(5) 0.039(6) 0.030(4) -0.004(4) -0.008(4) -0.010(4) C16 0.051(5) 0.041(6) 0.034(5) 0.001(4) -0.019(4) -0.002(5) C17 0.031(4) 0.030(5) 0.016(4) -0.002(3) -0.008(3) -0.004(4) C18 0.032(4) 0.037(5) 0.017(4) -0.004(3) -0.005(3) -0.015(4) C19 0.028(4) 0.054(6) 0.025(4) 0.002(4) -0.004(3) -0.014(4) C20 0.026(4) 0.052(6) 0.022(4) 0.001(4) -0.009(3) -0.010(4) C21 0.029(4) 0.035(5) 0.018(4) -0.004(3) -0.003(3) -0.004(4) C22 0.025(4) 0.065(7) 0.009(3) -0.008(4) -0.007(3) -0.008(4) C23 0.027(4) 0.027(5) 0.020(4) -0.005(3) -0.007(3) 0.000(3) C24 0.044(5) 0.037(6) 0.020(4) 0.008(4) -0.005(4) -0.008(4) C25 0.045(5) 0.033(6) 0.028(4) 0.007(4) -0.005(4) -0.004(4) C26 0.045(5) 0.039(6) 0.021(4) 0.003(4) -0.002(4) -0.007(4) C27 0.036(4) 0.041(6) 0.015(4) 0.003(4) -0.008(3) -0.002(4) C28 0.017(4) 0.033(5) 0.017(4) -0.003(3) 0.000(3) 0.005(3) C29 0.028(4) 0.024(5) 0.015(3) 0.001(3) -0.004(3) -0.002(3) C30 0.032(4) 0.029(5) 0.021(4) 0.003(3) -0.003(3) -0.007(4) C31 0.038(5) 0.044(6) 0.025(4) -0.006(4) 0.005(4) -0.003(4) C32 0.036(5) 0.044(6) 0.023(4) -0.001(4) 0.004(3) -0.001(4) C33 0.025(4) 0.063(7) 0.023(4) -0.010(4) 0.001(3) -0.006(4) C34 0.026(4) 0.043(6) 0.021(4) -0.004(4) -0.004(3) -0.011(4) C35 0.040(5) 0.053(7) 0.049(6) -0.012(5) -0.012(4) 0.004(5) Cl1 0.0566(15) 0.0530(18) 0.0695(17) 0.0169(14) -0.0332(13) -0.0136(13) Cl2 0.134(3) 0.087(3) 0.072(2) -0.0324(18) -0.056(2) 0.048(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 Rh1 C1 1.822(7) . ? Rh1 P1 2.239(2) . ? Rh1 S2 2.385(2) . ? Rh1 S1 2.421(2) . ? P1 C17 1.840(8) . ? P1 C23 1.843(7) . ? P1 C29 1.862(7) . ? S1 C2 1.684(8) . ? S2 C7 1.695(7) . ? S3 C12 1.700(7) . ? O1 C1 1.152(8) . ? N1 C2 1.344(8) . ? N1 N2 1.379(8) . ? N1 B1 1.553(9) . ? N2 C3 1.308(8) . ? N3 C3 1.373(9) . ? N3 C2 1.375(9) . ? N3 C5 1.485(8) . ? N4 C7 1.327(8) . ? N4 N5 1.396(7) . ? N4 B1 1.550(10) . ? N5 C8 1.294(9) . ? N6 C7 1.359(9) . ? N6 C8 1.382(9) . ? N6 C10 1.497(9) . ? N7 C12 1.350(9) . ? N7 N8 1.396(8) . ? N7 B1 1.531(10) . ? N8 C13 1.297(8) . ? N9 C13 1.373(9) . ? N9 C12 1.376(9) . ? N9 C15 1.463(9) . ? B1 H1 1.0000 . ? C3 C4 1.473(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.495(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.469(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.500(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.482(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.489(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.538(9) . ? C17 C18 1.553(10) . ? C17 H17 1.0000 . ? C18 C19 1.523(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.554(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.519(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.517(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.506(10) . ? C23 C28 1.538(10) . ? C23 H23 1.0000 . ? C24 C25 1.531(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.500(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.526(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.515(10) . ? C29 C30 1.525(10) . ? C29 H29 1.0000 . ? C30 C31 1.515(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.518(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.491(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.541(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 Cl2 1.727(9) . ? C35 Cl1 1.773(8) . ? C35 H35A 0.9900 . ? C35 H35B 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 C1 Rh1 P1 88.6(2) . . ? C1 Rh1 S2 85.0(3) . . ? P1 Rh1 S2 164.14(7) . . ? C1 Rh1 S1 177.8(2) . . ? P1 Rh1 S1 90.55(8) . . ? S2 Rh1 S1 95.38(8) . . ? C17 P1 C23 107.1(3) . . ? C17 P1 C29 103.1(3) . . ? C23 P1 C29 109.2(3) . . ? C17 P1 Rh1 111.8(3) . . ? C23 P1 Rh1 112.9(3) . . ? C29 P1 Rh1 112.2(3) . . ? C2 S1 Rh1 111.1(3) . . ? C7 S2 Rh1 112.1(3) . . ? C2 N1 N2 111.0(5) . . ? C2 N1 B1 128.7(6) . . ? N2 N1 B1 120.1(5) . . ? C3 N2 N1 105.6(6) . . ? C3 N3 C2 107.3(6) . . ? C3 N3 C5 127.0(6) . . ? C2 N3 C5 125.7(6) . . ? C7 N4 N5 112.8(6) . . ? C7 N4 B1 124.1(6) . . ? N5 N4 B1 123.1(6) . . ? C8 N5 N4 103.3(6) . . ? C7 N6 C8 107.4(6) . . ? C7 N6 C10 124.3(6) . . ? C8 N6 C10 128.3(6) . . ? C12 N7 N8 109.3(6) . . ? C12 N7 B1 126.1(6) . . ? N8 N7 B1 124.5(5) . . ? C13 N8 N7 106.3(6) . . ? C13 N9 C12 106.9(6) . . ? C13 N9 C15 126.8(6) . . ? C12 N9 C15 125.8(6) . . ? N7 B1 N4 110.3(6) . . ? N7 B1 N1 110.6(6) . . ? N4 B1 N1 107.5(6) . . ? N7 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? N1 B1 H1 109.5 . . ? O1 C1 Rh1 177.6(7) . . ? N1 C2 N3 105.3(6) . . ? N1 C2 S1 131.9(6) . . ? N3 C2 S1 122.8(5) . . ? N2 C3 N3 110.6(7) . . ? N2 C3 C4 125.2(7) . . ? N3 C3 C4 124.1(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 112.4(7) . . ? N3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 104.8(6) . . ? N4 C7 S2 131.4(6) . . ? N6 C7 S2 123.7(5) . . ? N5 C8 N6 111.7(7) . . ? N5 C8 C9 123.3(7) . . ? N6 C8 C9 125.1(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 111.5(6) . . ? N6 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N6 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 106.4(6) . . ? N7 C12 S3 127.8(6) . . ? N9 C12 S3 125.8(6) . . ? N8 C13 N9 111.0(6) . . ? N8 C13 C14 124.3(7) . . ? N9 C13 C14 124.7(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 112.3(7) . . ? N9 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N9 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 109.8(5) . . ? C22 C17 P1 112.8(5) . . ? C18 C17 P1 111.5(5) . . ? C22 C17 H17 107.5 . . ? C18 C17 H17 107.5 . . ? P1 C17 H17 107.5 . . ? C19 C18 C17 112.9(6) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 112.1(6) . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C19 110.2(6) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 111.8(7) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C17 113.1(6) . . ? C21 C22 H22A 108.9 . . ? C17 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C17 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C28 109.6(6) . . ? C24 C23 P1 118.5(5) . . ? C28 C23 P1 113.9(5) . . ? C24 C23 H23 104.4 . . ? C28 C23 H23 104.4 . . ? P1 C23 H23 104.4 . . ? C23 C24 C25 110.3(7) . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 112.7(7) . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 110.6(6) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 110.5(7) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C23 110.6(6) . . ? C27 C28 H28A 109.5 . . ? C23 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C34 C29 C30 108.5(6) . . ? C34 C29 P1 115.3(5) . . ? C30 C29 P1 117.3(5) . . ? C34 C29 H29 104.8 . . ? C30 C29 H29 104.8 . . ? P1 C29 H29 104.8 . . ? C31 C30 C29 110.5(6) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 112.3(7) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 110.3(7) . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C34 111.4(7) . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C29 C34 C33 110.8(6) . . ? C29 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? Cl2 C35 Cl1 113.0(5) . . ? Cl2 C35 H35A 109.0 . . ? Cl1 C35 H35A 109.0 . . ? Cl2 C35 H35B 109.0 . . ? Cl1 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 P1 C17 83.3(3) . . . . ? S2 Rh1 P1 C17 149.1(3) . . . . ? S1 Rh1 P1 C17 -98.7(3) . . . . ? C1 Rh1 P1 C23 -155.8(4) . . . . ? S2 Rh1 P1 C23 -90.0(4) . . . . ? S1 Rh1 P1 C23 22.1(3) . . . . ? C1 Rh1 P1 C29 -32.0(3) . . . . ? S2 Rh1 P1 C29 33.9(4) . . . . ? S1 Rh1 P1 C29 146.0(2) . . . . ? P1 Rh1 S1 C2 148.4(3) . . . . ? S2 Rh1 S1 C2 -46.3(3) . . . . ? C1 Rh1 S2 C7 -90.1(3) . . . . ? P1 Rh1 S2 C7 -156.3(3) . . . . ? S1 Rh1 S2 C7 92.1(3) . . . . ? C2 N1 N2 C3 2.8(8) . . . . ? B1 N1 N2 C3 -172.9(7) . . . . ? C7 N4 N5 C8 -1.3(8) . . . . ? B1 N4 N5 C8 179.4(6) . . . . ? C12 N7 N8 C13 1.7(8) . . . . ? B1 N7 N8 C13 179.5(7) . . . . ? C12 N7 B1 N4 -68.4(9) . . . . ? N8 N7 B1 N4 114.1(7) . . . . ? C12 N7 B1 N1 172.9(7) . . . . ? N8 N7 B1 N1 -4.6(10) . . . . ? C7 N4 B1 N7 164.7(6) . . . . ? N5 N4 B1 N7 -16.1(9) . . . . ? C7 N4 B1 N1 -74.6(8) . . . . ? N5 N4 B1 N1 104.6(7) . . . . ? C2 N1 B1 N7 -125.0(8) . . . . ? N2 N1 B1 N7 49.9(9) . . . . ? C2 N1 B1 N4 114.5(8) . . . . ? N2 N1 B1 N4 -70.6(8) . . . . ? N2 N1 C2 N3 -3.9(8) . . . . ? B1 N1 C2 N3 171.4(7) . . . . ? N2 N1 C2 S1 176.9(6) . . . . ? B1 N1 C2 S1 -7.8(13) . . . . ? C3 N3 C2 N1 3.4(8) . . . . ? C5 N3 C2 N1 -174.6(7) . . . . ? C3 N3 C2 S1 -177.3(6) . . . . ? C5 N3 C2 S1 4.7(11) . . . . ? Rh1 S1 C2 N1 -19.6(9) . . . . ? Rh1 S1 C2 N3 161.3(6) . . . . ? N1 N2 C3 N3 -0.5(9) . . . . ? N1 N2 C3 C4 176.5(8) . . . . ? C2 N3 C3 N2 -1.9(9) . . . . ? C5 N3 C3 N2 176.1(7) . . . . ? C2 N3 C3 C4 -178.9(8) . . . . ? C5 N3 C3 C4 -0.9(13) . . . . ? C3 N3 C5 C6 87.1(10) . . . . ? C2 N3 C5 C6 -95.3(10) . . . . ? N5 N4 C7 N6 2.5(8) . . . . ? B1 N4 C7 N6 -178.3(6) . . . . ? N5 N4 C7 S2 -174.1(6) . . . . ? B1 N4 C7 S2 5.2(11) . . . . ? C8 N6 C7 N4 -2.6(8) . . . . ? C10 N6 C7 N4 176.7(6) . . . . ? C8 N6 C7 S2 174.3(5) . . . . ? C10 N6 C7 S2 -6.4(10) . . . . ? Rh1 S2 C7 N4 -34.7(8) . . . . ? Rh1 S2 C7 N6 149.3(5) . . . . ? N4 N5 C8 N6 -0.4(8) . . . . ? N4 N5 C8 C9 179.3(7) . . . . ? C7 N6 C8 N5 1.9(9) . . . . ? C10 N6 C8 N5 -177.3(6) . . . . ? C7 N6 C8 C9 -177.7(7) . . . . ? C10 N6 C8 C9 3.0(12) . . . . ? C7 N6 C10 C11 79.7(9) . . . . ? C8 N6 C10 C11 -101.2(8) . . . . ? N8 N7 C12 N9 -1.7(8) . . . . ? B1 N7 C12 N9 -179.5(6) . . . . ? N8 N7 C12 S3 176.3(5) . . . . ? B1 N7 C12 S3 -1.5(11) . . . . ? C13 N9 C12 N7 1.1(8) . . . . ? C15 N9 C12 N7 -171.6(7) . . . . ? C13 N9 C12 S3 -176.9(6) . . . . ? C15 N9 C12 S3 10.4(11) . . . . ? N7 N8 C13 N9 -1.0(8) . . . . ? N7 N8 C13 C14 -178.7(7) . . . . ? C12 N9 C13 N8 -0.1(9) . . . . ? C15 N9 C13 N8 172.5(7) . . . . ? C12 N9 C13 C14 177.7(7) . . . . ? C15 N9 C13 C14 -9.7(12) . . . . ? C13 N9 C15 C16 -87.9(9) . . . . ? C12 N9 C15 C16 83.3(10) . . . . ? C23 P1 C17 C22 167.3(5) . . . . ? C29 P1 C17 C22 52.1(6) . . . . ? Rh1 P1 C17 C22 -68.6(6) . . . . ? C23 P1 C17 C18 -68.6(6) . . . . ? C29 P1 C17 C18 176.2(5) . . . . ? Rh1 P1 C17 C18 55.5(5) . . . . ? C22 C17 C18 C19 -51.5(9) . . . . ? P1 C17 C18 C19 -177.2(5) . . . . ? C17 C18 C19 C20 53.2(9) . . . . ? C18 C19 C20 C21 -54.3(10) . . . . ? C19 C20 C21 C22 55.6(9) . . . . ? C20 C21 C22 C17 -56.8(9) . . . . ? C18 C17 C22 C21 53.1(9) . . . . ? P1 C17 C22 C21 178.1(6) . . . . ? C17 P1 C23 C24 -48.5(7) . . . . ? C29 P1 C23 C24 62.6(7) . . . . ? Rh1 P1 C23 C24 -171.9(5) . . . . ? C17 P1 C23 C28 -179.7(5) . . . . ? C29 P1 C23 C28 -68.6(6) . . . . ? Rh1 P1 C23 C28 56.8(6) . . . . ? C28 C23 C24 C25 -56.8(8) . . . . ? P1 C23 C24 C25 170.1(5) . . . . ? C23 C24 C25 C26 55.2(9) . . . . ? C24 C25 C26 C27 -54.3(9) . . . . ? C25 C26 C27 C28 55.6(8) . . . . ? C26 C27 C28 C23 -59.0(8) . . . . ? C24 C23 C28 C27 59.6(8) . . . . ? P1 C23 C28 C27 -165.0(5) . . . . ? C17 P1 C29 C34 -179.2(5) . . . . ? C23 P1 C29 C34 67.2(6) . . . . ? Rh1 P1 C29 C34 -58.7(6) . . . . ? C17 P1 C29 C30 51.2(6) . . . . ? C23 P1 C29 C30 -62.5(6) . . . . ? Rh1 P1 C29 C30 171.6(4) . . . . ? C34 C29 C30 C31 58.4(7) . . . . ? P1 C29 C30 C31 -168.8(5) . . . . ? C29 C30 C31 C32 -57.3(8) . . . . ? C30 C31 C32 C33 55.0(9) . . . . ? C31 C32 C33 C34 -54.6(8) . . . . ? C30 C29 C34 C33 -58.7(8) . . . . ? P1 C29 C34 C33 167.5(5) . . . . ? C32 C33 C34 C29 58.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.114 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.152 data_7 _database_code_depnum_ccdc_archive 'CCDC 733503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H43 B N12 O P Rh S3, 2(C H2 Cl2)' _chemical_formula_sum 'C24 H47 B Cl4 N12 O P Rh S3' _chemical_formula_weight 902.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.697(2) _cell_length_b 13.580(3) _cell_length_c 14.533(3) _cell_angle_alpha 71.41(3) _cell_angle_beta 68.99(3) _cell_angle_gamma 74.88(3) _cell_volume 2014.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6118 _cell_measurement_theta_min 3.365 _cell_measurement_theta_max 70.012 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 8.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.153247 _exptl_absorpt_correction_T_max 0.450000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15056 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 70.04 _reflns_number_total 6792 _reflns_number_gt 6043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT V6.28 (Bruker, 2001)' _computing_structure_solution 'SHELXS V7.06 (Bruker 2003)' _computing_structure_refinement 'SHELXL V7.06 (Bruker 2003)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.1305P)^2^+1.6668P] 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 6792 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1795 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.79119(3) 0.85025(2) 0.17598(2) 0.01419(16) Uani 1 1 d . . . S1 S 0.91327(9) 0.67947(8) 0.21176(8) 0.0161(2) Uani 1 1 d . . . S2 S 0.84501(10) 0.91854(8) 0.29012(8) 0.0172(2) Uani 1 1 d . . . S3 S 0.41511(9) 0.70275(8) 0.42406(8) 0.0147(2) Uani 1 1 d . . . P1 P 0.77098(10) 0.81466(9) 0.04205(8) 0.0146(2) Uani 1 1 d . . . N1 N 0.8295(3) 0.6713(3) 0.4179(2) 0.0115(7) Uani 1 1 d . . . N2 N 0.8784(3) 0.6516(3) 0.4975(3) 0.0133(7) Uani 1 1 d . . . N3 N 1.0289(3) 0.6339(3) 0.3566(3) 0.0142(7) Uani 1 1 d . . . N4 N 0.6732(3) 0.8252(3) 0.4625(3) 0.0125(7) Uani 1 1 d . . . N5 N 0.5940(3) 0.8449(3) 0.5547(3) 0.0139(7) Uani 1 1 d . . . N6 N 0.6946(3) 0.9791(3) 0.4629(3) 0.0145(7) Uani 1 1 d . . . N7 N 0.6018(3) 0.6500(3) 0.5135(3) 0.0115(7) Uani 1 1 d . . . N8 N 0.6271(3) 0.5885(3) 0.6031(3) 0.0145(7) Uani 1 1 d . . . N9 N 0.4450(3) 0.5703(3) 0.6033(3) 0.0132(7) Uani 1 1 d . . . N10 N 0.8155(4) 0.9130(3) -0.0613(3) 0.0251(9) Uani 1 1 d . . . N11 N 0.8505(3) 0.7058(3) 0.0011(3) 0.0179(8) Uani 1 1 d . . . N12 N 0.6270(4) 0.7999(4) 0.0590(3) 0.0266(9) Uani 1 1 d . . . O1 O 0.6490(5) 1.0598(3) 0.1122(3) 0.0448(11) Uani 1 1 d . . . B1 B 0.6902(4) 0.7216(4) 0.4312(4) 0.0128(9) Uani 1 1 d . . . H1 H 0.6725 0.7385 0.3650 0.015 Uiso 1 1 calc R . . C1 C 0.7041(5) 0.9805(4) 0.1368(4) 0.0257(10) Uani 1 1 d . . . C2 C 0.9202(4) 0.6623(3) 0.3324(3) 0.0134(8) Uani 1 1 d . . . C3 C 0.9981(4) 0.6298(3) 0.4580(3) 0.0149(8) Uani 1 1 d . . . C4 C 1.0909(4) 0.6048(4) 0.5143(3) 0.0195(9) Uani 1 1 d . . . H4A H 1.0475 0.5996 0.5867 0.029 Uiso 1 1 calc R . . H4B H 1.1416 0.6607 0.4872 0.029 Uiso 1 1 calc R . . H4C H 1.1445 0.5375 0.5057 0.029 Uiso 1 1 calc R . . C5 C 1.1545(4) 0.6242(4) 0.2846(4) 0.0197(9) Uani 1 1 d . . . H5A H 1.1544 0.5981 0.2284 0.024 Uiso 1 1 calc R . . H5B H 1.2122 0.5726 0.3198 0.024 Uiso 1 1 calc R . . C6 C 1.1988(5) 0.7300(4) 0.2416(5) 0.0337(12) Uani 1 1 d . . . H6A H 1.1356 0.7835 0.2157 0.051 Uiso 1 1 calc R . . H6B H 1.2765 0.7248 0.1860 0.051 Uiso 1 1 calc R . . H6C H 1.2128 0.7500 0.2953 0.051 Uiso 1 1 calc R . . C7 C 0.7341(4) 0.9059(3) 0.4076(3) 0.0153(8) Uani 1 1 d . . . C8 C 0.6105(4) 0.9374(3) 0.5529(3) 0.0151(8) Uani 1 1 d . . . C9 C 0.5491(4) 0.9894(4) 0.6387(3) 0.0206(9) Uani 1 1 d . . . H9A H 0.4814 0.9528 0.6882 0.031 Uiso 1 1 calc R . . H9B H 0.5155 1.0631 0.6124 0.031 Uiso 1 1 calc R . . H9C H 0.6100 0.9865 0.6719 0.031 Uiso 1 1 calc R . . C10 C 0.7354(4) 1.0814(3) 0.4320(3) 0.0172(9) Uani 1 1 d . . . H10A H 0.6676 1.1317 0.4650 0.021 Uiso 1 1 calc R . . H10B H 0.7530 1.1092 0.3574 0.021 Uiso 1 1 calc R . . C11 C 0.8511(5) 1.0733(4) 0.4607(5) 0.0315(12) Uani 1 1 d . . . H11A H 0.8344 1.0451 0.5345 0.047 Uiso 1 1 calc R . . H11B H 0.8739 1.1433 0.4407 0.047 Uiso 1 1 calc R . . H11C H 0.9197 1.0262 0.4255 0.047 Uiso 1 1 calc R . . C12 C 0.4894(4) 0.6409(3) 0.5131(3) 0.0110(8) Uani 1 1 d . . . C13 C 0.5305(4) 0.5422(3) 0.6557(3) 0.0135(8) Uani 1 1 d . . . C14 C 0.5138(4) 0.4680(4) 0.7579(3) 0.0168(9) Uani 1 1 d . . . H14A H 0.5806 0.4669 0.7842 0.025 Uiso 1 1 calc R . . H14B H 0.5163 0.3971 0.7529 0.025 Uiso 1 1 calc R . . H14C H 0.4335 0.4909 0.8043 0.025 Uiso 1 1 calc R . . C15 C 0.3246(4) 0.5344(3) 0.6382(3) 0.0152(8) Uani 1 1 d . . . H15A H 0.3322 0.4609 0.6801 0.018 Uiso 1 1 calc R . . H15B H 0.3023 0.5351 0.5784 0.018 Uiso 1 1 calc R . . C16 C 0.2221(4) 0.6031(4) 0.7002(4) 0.0212(9) Uani 1 1 d . . . H16A H 0.2448 0.6041 0.7586 0.032 Uiso 1 1 calc R . . H16B H 0.1446 0.5746 0.7246 0.032 Uiso 1 1 calc R . . H16C H 0.2104 0.6750 0.6576 0.032 Uiso 1 1 calc R . . C17 C 0.9072(6) 0.9731(5) -0.0715(4) 0.0397(14) Uani 1 1 d . . . H17A H 0.9804 0.9614 -0.1292 0.060 Uiso 1 1 calc R . . H17B H 0.9313 0.9504 -0.0090 0.060 Uiso 1 1 calc R . . H17C H 0.8717 1.0482 -0.0834 0.060 Uiso 1 1 calc R . . C18 C 0.7987(7) 0.9218(5) -0.1589(4) 0.0437(15) Uani 1 1 d . . . H18A H 0.7977 0.9950 -0.1993 0.066 Uiso 1 1 calc R . . H18B H 0.7199 0.9000 -0.1467 0.066 Uiso 1 1 calc R . . H18C H 0.8673 0.8762 -0.1959 0.066 Uiso 1 1 calc R . . C19 C 0.9807(5) 0.7010(4) -0.0568(4) 0.0285(11) Uani 1 1 d . . . H19A H 1.0315 0.6654 -0.0109 0.043 Uiso 1 1 calc R . . H19B H 0.9988 0.7726 -0.0907 0.043 Uiso 1 1 calc R . . H19C H 0.9999 0.6617 -0.1080 0.043 Uiso 1 1 calc R . . C20 C 0.8181(5) 0.6020(4) 0.0593(4) 0.0243(10) Uani 1 1 d . . . H20A H 0.8115 0.5655 0.0136 0.036 Uiso 1 1 calc R . . H20B H 0.7384 0.6102 0.1123 0.036 Uiso 1 1 calc R . . H20C H 0.8827 0.5608 0.0910 0.036 Uiso 1 1 calc R . . C21 C 0.5939(5) 0.7583(5) -0.0091(4) 0.0368(13) Uani 1 1 d . . . H21A H 0.5330 0.7112 0.0317 0.055 Uiso 1 1 calc R . . H21B H 0.6686 0.7192 -0.0480 0.055 Uiso 1 1 calc R . . H21C H 0.5582 0.8170 -0.0561 0.055 Uiso 1 1 calc R . . C22 C 0.5197(5) 0.8488(5) 0.1277(4) 0.0325(12) Uani 1 1 d . . . H22A H 0.4957 0.9222 0.0931 0.049 Uiso 1 1 calc R . . H22B H 0.5404 0.8469 0.1880 0.049 Uiso 1 1 calc R . . H22C H 0.4506 0.8105 0.1485 0.049 Uiso 1 1 calc R . . C23 C 0.7611(5) 0.7137(4) 0.7073(4) 0.0237(10) Uani 1 1 d . . . H23A H 0.6811 0.7467 0.7479 0.028 Uiso 1 1 calc R . . H23B H 0.7437 0.6840 0.6606 0.028 Uiso 1 1 calc R . . Cl1 Cl 0.85814(11) 0.81049(9) 0.63522(9) 0.0273(3) Uani 1 1 d . . . Cl2 Cl 0.83373(14) 0.61139(11) 0.78936(10) 0.0373(3) Uani 1 1 d . . . C24 C 0.6859(6) 0.2857(6) 0.0743(6) 0.0529(18) Uani 1 1 d . . . H24A H 0.7730 0.2665 0.0758 0.063 Uiso 1 1 calc R . . H24B H 0.6720 0.2357 0.0441 0.063 Uiso 1 1 calc R . . Cl3 Cl 0.58526(14) 0.27179(12) 0.20135(12) 0.0433(4) Uani 1 1 d . . . Cl4 Cl 0.6647(2) 0.41250(15) -0.00292(14) 0.0674(6) 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 0.0192(2) 0.0125(2) 0.0113(2) 0.00069(15) -0.00701(15) -0.00427(14) S1 0.0188(5) 0.0165(6) 0.0136(5) -0.0028(4) -0.0086(4) 0.0001(4) S2 0.0220(5) 0.0190(6) 0.0135(5) -0.0027(4) -0.0032(4) -0.0128(4) S3 0.0148(5) 0.0148(5) 0.0167(5) 0.0010(4) -0.0108(4) -0.0037(4) P1 0.0174(5) 0.0150(6) 0.0121(5) 0.0005(4) -0.0071(4) -0.0046(4) N1 0.0126(17) 0.0125(18) 0.0100(15) 0.0013(14) -0.0066(13) -0.0037(12) N2 0.0132(17) 0.0160(18) 0.0141(16) 0.0012(14) -0.0090(14) -0.0073(13) N3 0.0137(18) 0.0104(18) 0.0191(18) 0.0010(14) -0.0072(15) -0.0055(13) N4 0.0096(16) 0.0151(18) 0.0134(16) -0.0021(14) -0.0032(13) -0.0051(12) N5 0.0135(17) 0.0148(19) 0.0144(17) -0.0020(14) -0.0059(14) -0.0035(13) N6 0.0170(18) 0.0128(19) 0.0146(17) 0.0004(14) -0.0051(14) -0.0080(13) N7 0.0154(17) 0.0113(18) 0.0100(16) 0.0010(13) -0.0083(13) -0.0042(12) N8 0.0200(18) 0.0110(18) 0.0153(17) 0.0027(14) -0.0123(15) -0.0047(13) N9 0.0125(17) 0.0119(18) 0.0184(17) -0.0008(14) -0.0095(14) -0.0041(13) N10 0.041(2) 0.024(2) 0.0134(18) 0.0034(16) -0.0121(17) -0.0148(18) N11 0.0193(19) 0.017(2) 0.0191(18) -0.0036(16) -0.0074(15) -0.0051(14) N12 0.019(2) 0.038(3) 0.032(2) -0.013(2) -0.0133(17) -0.0077(16) O1 0.069(3) 0.027(2) 0.037(2) -0.0136(19) -0.023(2) 0.014(2) B1 0.012(2) 0.009(2) 0.019(2) 0.0012(19) -0.0088(18) -0.0039(16) C1 0.043(3) 0.015(3) 0.017(2) -0.0022(19) -0.015(2) 0.003(2) C2 0.016(2) 0.009(2) 0.018(2) 0.0014(17) -0.0123(17) -0.0036(14) C3 0.021(2) 0.009(2) 0.016(2) 0.0020(16) -0.0110(17) -0.0038(15) C4 0.019(2) 0.023(2) 0.022(2) -0.0012(19) -0.0146(18) -0.0071(17) C5 0.012(2) 0.021(2) 0.022(2) -0.0013(19) -0.0048(17) -0.0013(16) C6 0.021(3) 0.029(3) 0.043(3) 0.002(2) -0.005(2) -0.010(2) C7 0.014(2) 0.015(2) 0.020(2) -0.0010(18) -0.0097(17) -0.0044(15) C8 0.015(2) 0.014(2) 0.016(2) 0.0021(17) -0.0080(17) -0.0046(15) C9 0.025(2) 0.019(2) 0.018(2) -0.0052(18) -0.0034(18) -0.0068(17) C10 0.023(2) 0.007(2) 0.022(2) 0.0019(17) -0.0092(18) -0.0067(16) C11 0.031(3) 0.023(3) 0.048(3) 0.000(2) -0.021(2) -0.014(2) C12 0.0113(19) 0.010(2) 0.0134(19) -0.0017(16) -0.0055(15) -0.0029(14) C13 0.016(2) 0.013(2) 0.0130(19) 0.0005(16) -0.0092(16) -0.0038(15) C14 0.017(2) 0.016(2) 0.015(2) 0.0043(17) -0.0074(17) -0.0051(15) C15 0.013(2) 0.017(2) 0.017(2) 0.0022(17) -0.0057(16) -0.0101(15) C16 0.019(2) 0.024(3) 0.022(2) -0.0032(19) -0.0072(18) -0.0081(17) C17 0.066(4) 0.029(3) 0.026(3) 0.007(2) -0.010(3) -0.032(3) C18 0.078(5) 0.040(4) 0.017(3) 0.006(2) -0.022(3) -0.022(3) C19 0.024(3) 0.037(3) 0.025(2) -0.013(2) -0.003(2) -0.006(2) C20 0.039(3) 0.014(2) 0.027(2) 0.0004(19) -0.017(2) -0.0118(19) C21 0.030(3) 0.059(4) 0.034(3) -0.012(3) -0.020(2) -0.014(2) C22 0.021(2) 0.035(3) 0.037(3) -0.004(2) -0.004(2) -0.008(2) C23 0.029(3) 0.026(3) 0.019(2) -0.002(2) -0.0119(19) -0.0091(19) Cl1 0.0334(6) 0.0240(6) 0.0311(6) -0.0055(5) -0.0144(5) -0.0109(4) Cl2 0.0573(8) 0.0312(7) 0.0285(6) 0.0015(5) -0.0247(6) -0.0102(6) C24 0.033(3) 0.041(4) 0.063(4) 0.004(3) -0.002(3) -0.010(3) Cl3 0.0487(8) 0.0365(8) 0.0483(8) -0.0135(7) -0.0099(7) -0.0160(6) Cl4 0.1171(17) 0.0444(10) 0.0452(9) -0.0059(8) -0.0242(10) -0.0277(10) _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 C1 1.823(5) . ? Rh1 P1 2.2511(12) . ? Rh1 S1 2.3925(14) . ? Rh1 S2 2.4581(11) . ? S1 C2 1.723(4) . ? S2 C7 1.723(5) . ? S3 C12 1.693(4) . ? P1 N12 1.669(4) . ? P1 N10 1.683(4) . ? P1 N11 1.688(4) . ? N1 C2 1.330(6) . ? N1 N2 1.390(5) . ? N1 B1 1.561(5) . ? N2 C3 1.301(6) . ? N3 C2 1.366(5) . ? N3 C3 1.372(6) . ? N3 C5 1.468(6) . ? N4 C7 1.337(5) . ? N4 N5 1.391(5) . ? N4 B1 1.557(6) . ? N5 C8 1.309(6) . ? N6 C7 1.360(6) . ? N6 C8 1.377(6) . ? N6 C10 1.468(5) . ? N7 C12 1.356(5) . ? N7 N8 1.390(5) . ? N7 B1 1.530(6) . ? N8 C13 1.305(5) . ? N9 C12 1.370(5) . ? N9 C13 1.373(5) . ? N9 C15 1.472(5) . ? N10 C17 1.450(7) . ? N10 C18 1.464(7) . ? N11 C19 1.447(6) . ? N11 C20 1.461(6) . ? N12 C22 1.450(7) . ? N12 C21 1.482(6) . ? O1 C1 1.122(7) . ? B1 H1 1.0000 . ? C3 C4 1.493(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.519(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.492(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.522(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.484(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.516(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Cl2 1.769(5) . ? C23 Cl1 1.778(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 Cl4 1.741(7) . ? C24 Cl3 1.779(7) . ? C24 H24A 0.9900 . ? C24 H24B 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 C1 Rh1 P1 86.33(16) . . ? C1 Rh1 S1 174.94(15) . . ? P1 Rh1 S1 89.44(5) . . ? C1 Rh1 S2 88.32(16) . . ? P1 Rh1 S2 166.18(4) . . ? S1 Rh1 S2 95.18(4) . . ? C2 S1 Rh1 104.17(15) . . ? C7 S2 Rh1 111.35(14) . . ? N12 P1 N10 110.3(2) . . ? N12 P1 N11 99.3(2) . . ? N10 P1 N11 102.8(2) . . ? N12 P1 Rh1 113.22(16) . . ? N10 P1 Rh1 108.03(15) . . ? N11 P1 Rh1 122.37(14) . . ? C2 N1 N2 110.3(3) . . ? C2 N1 B1 128.4(3) . . ? N2 N1 B1 119.8(3) . . ? C3 N2 N1 105.3(3) . . ? C2 N3 C3 106.7(4) . . ? C2 N3 C5 126.1(4) . . ? C3 N3 C5 126.7(4) . . ? C7 N4 N5 110.2(3) . . ? C7 N4 B1 125.8(4) . . ? N5 N4 B1 124.0(3) . . ? C8 N5 N4 104.9(3) . . ? C7 N6 C8 106.3(3) . . ? C7 N6 C10 126.2(4) . . ? C8 N6 C10 127.5(4) . . ? C12 N7 N8 111.2(3) . . ? C12 N7 B1 126.4(3) . . ? N8 N7 B1 122.3(3) . . ? C13 N8 N7 105.1(3) . . ? C12 N9 C13 108.1(3) . . ? C12 N9 C15 125.3(3) . . ? C13 N9 C15 126.6(4) . . ? C17 N10 C18 112.7(4) . . ? C17 N10 P1 122.1(3) . . ? C18 N10 P1 122.2(4) . . ? C19 N11 C20 112.6(4) . . ? C19 N11 P1 119.8(3) . . ? C20 N11 P1 120.8(3) . . ? C22 N12 C21 113.1(4) . . ? C22 N12 P1 121.8(3) . . ? C21 N12 P1 123.7(4) . . ? N7 B1 N4 109.8(3) . . ? N7 B1 N1 112.4(3) . . ? N4 B1 N1 105.4(3) . . ? N7 B1 H1 109.7 . . ? N4 B1 H1 109.7 . . ? N1 B1 H1 109.7 . . ? O1 C1 Rh1 178.6(5) . . ? N1 C2 N3 106.6(3) . . ? N1 C2 S1 130.1(3) . . ? N3 C2 S1 123.3(3) . . ? N2 C3 N3 111.0(4) . . ? N2 C3 C4 125.1(4) . . ? N3 C3 C4 123.9(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 110.5(4) . . ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 107.2(4) . . ? N4 C7 S2 128.3(3) . . ? N6 C7 S2 124.5(3) . . ? N5 C8 N6 111.4(4) . . ? N5 C8 C9 124.4(4) . . ? N6 C8 C9 124.2(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 112.0(4) . . ? N6 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N6 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 104.7(3) . . ? N7 C12 S3 129.1(3) . . ? N9 C12 S3 126.2(3) . . ? N8 C13 N9 110.9(4) . . ? N8 C13 C14 125.3(4) . . ? N9 C13 C14 123.7(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 112.1(4) . . ? N9 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N9 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N10 C17 H17A 109.5 . . ? N10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C18 H18A 109.5 . . ? N10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N11 C19 H19A 109.5 . . ? N11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N11 C20 H20A 109.5 . . ? N11 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N11 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N12 C21 H21A 109.5 . . ? N12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N12 C22 H22A 109.5 . . ? N12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Cl2 C23 Cl1 110.5(3) . . ? Cl2 C23 H23A 109.5 . . ? Cl1 C23 H23A 109.5 . . ? Cl2 C23 H23B 109.5 . . ? Cl1 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? Cl4 C24 Cl3 113.4(4) . . ? Cl4 C24 H24A 108.9 . . ? Cl3 C24 H24A 108.9 . . ? Cl4 C24 H24B 108.9 . . ? Cl3 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Rh1 S1 C2 -166.52(14) . . . . ? S2 Rh1 S1 C2 26.52(14) . . . . ? C1 Rh1 S2 C7 88.1(2) . . . . ? P1 Rh1 S2 C7 155.3(2) . . . . ? S1 Rh1 S2 C7 -95.55(17) . . . . ? C1 Rh1 P1 N12 -72.3(2) . . . . ? S1 Rh1 P1 N12 110.52(18) . . . . ? S2 Rh1 P1 N12 -139.7(2) . . . . ? C1 Rh1 P1 N10 50.2(2) . . . . ? S1 Rh1 P1 N10 -127.00(18) . . . . ? S2 Rh1 P1 N10 -17.2(3) . . . . ? C1 Rh1 P1 N11 169.1(2) . . . . ? S1 Rh1 P1 N11 -8.13(16) . . . . ? S2 Rh1 P1 N11 101.6(2) . . . . ? C2 N1 N2 C3 -0.8(4) . . . . ? B1 N1 N2 C3 -168.0(4) . . . . ? C7 N4 N5 C8 -0.5(4) . . . . ? B1 N4 N5 C8 177.5(4) . . . . ? C12 N7 N8 C13 0.5(4) . . . . ? B1 N7 N8 C13 177.5(4) . . . . ? N12 P1 N10 C17 153.2(5) . . . . ? N11 P1 N10 C17 -101.7(5) . . . . ? Rh1 P1 N10 C17 29.0(5) . . . . ? N12 P1 N10 C18 -47.6(5) . . . . ? N11 P1 N10 C18 57.5(5) . . . . ? Rh1 P1 N10 C18 -171.8(5) . . . . ? N12 P1 N11 C19 158.5(4) . . . . ? N10 P1 N11 C19 45.0(4) . . . . ? Rh1 P1 N11 C19 -76.3(4) . . . . ? N12 P1 N11 C20 -52.3(4) . . . . ? N10 P1 N11 C20 -165.8(3) . . . . ? Rh1 P1 N11 C20 72.9(4) . . . . ? N10 P1 N12 C22 -95.8(4) . . . . ? N11 P1 N12 C22 156.7(4) . . . . ? Rh1 P1 N12 C22 25.4(5) . . . . ? N10 P1 N12 C21 69.8(5) . . . . ? N11 P1 N12 C21 -37.7(5) . . . . ? Rh1 P1 N12 C21 -169.0(4) . . . . ? C12 N7 B1 N4 97.3(5) . . . . ? N8 N7 B1 N4 -79.3(4) . . . . ? C12 N7 B1 N1 -145.7(4) . . . . ? N8 N7 B1 N1 37.7(5) . . . . ? C7 N4 B1 N7 -178.9(3) . . . . ? N5 N4 B1 N7 3.4(5) . . . . ? C7 N4 B1 N1 59.9(5) . . . . ? N5 N4 B1 N1 -117.8(4) . . . . ? C2 N1 B1 N7 130.9(4) . . . . ? N2 N1 B1 N7 -64.4(5) . . . . ? C2 N1 B1 N4 -109.5(4) . . . . ? N2 N1 B1 N4 55.1(4) . . . . ? N2 N1 C2 N3 1.6(4) . . . . ? B1 N1 C2 N3 167.4(4) . . . . ? N2 N1 C2 S1 -179.2(3) . . . . ? B1 N1 C2 S1 -13.4(6) . . . . ? C3 N3 C2 N1 -1.7(4) . . . . ? C5 N3 C2 N1 -174.1(4) . . . . ? C3 N3 C2 S1 179.0(3) . . . . ? C5 N3 C2 S1 6.6(6) . . . . ? Rh1 S1 C2 N1 52.8(4) . . . . ? Rh1 S1 C2 N3 -128.1(3) . . . . ? N1 N2 C3 N3 -0.3(4) . . . . ? N1 N2 C3 C4 179.0(4) . . . . ? C2 N3 C3 N2 1.3(5) . . . . ? C5 N3 C3 N2 173.6(4) . . . . ? C2 N3 C3 C4 -178.0(4) . . . . ? C5 N3 C3 C4 -5.7(7) . . . . ? C2 N3 C5 C6 86.2(5) . . . . ? C3 N3 C5 C6 -84.6(5) . . . . ? N5 N4 C7 N6 -0.5(4) . . . . ? B1 N4 C7 N6 -178.4(3) . . . . ? N5 N4 C7 S2 178.1(3) . . . . ? B1 N4 C7 S2 0.2(6) . . . . ? C8 N6 C7 N4 1.2(4) . . . . ? C10 N6 C7 N4 -179.3(4) . . . . ? C8 N6 C7 S2 -177.5(3) . . . . ? C10 N6 C7 S2 2.1(6) . . . . ? Rh1 S2 C7 N4 40.6(4) . . . . ? Rh1 S2 C7 N6 -141.1(3) . . . . ? N4 N5 C8 N6 1.3(4) . . . . ? N4 N5 C8 C9 -176.9(4) . . . . ? C7 N6 C8 N5 -1.6(5) . . . . ? C10 N6 C8 N5 178.9(4) . . . . ? C7 N6 C8 C9 176.6(4) . . . . ? C10 N6 C8 C9 -3.0(7) . . . . ? C7 N6 C10 C11 -87.5(5) . . . . ? C8 N6 C10 C11 91.9(5) . . . . ? N8 N7 C12 N9 -1.4(4) . . . . ? B1 N7 C12 N9 -178.3(4) . . . . ? N8 N7 C12 S3 177.5(3) . . . . ? B1 N7 C12 S3 0.6(6) . . . . ? C13 N9 C12 N7 1.7(4) . . . . ? C15 N9 C12 N7 180.0(4) . . . . ? C13 N9 C12 S3 -177.2(3) . . . . ? C15 N9 C12 S3 1.1(6) . . . . ? N7 N8 C13 N9 0.7(5) . . . . ? N7 N8 C13 C14 -179.9(4) . . . . ? C12 N9 C13 N8 -1.5(5) . . . . ? C15 N9 C13 N8 -179.8(4) . . . . ? C12 N9 C13 C14 179.0(4) . . . . ? C15 N9 C13 C14 0.8(7) . . . . ? C12 N9 C15 C16 -90.6(5) . . . . ? C13 N9 C15 C16 87.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 70.04 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 3.037 _refine_diff_density_min -2.603 _refine_diff_density_rms 0.177 data_10 _database_code_depnum_ccdc_archive 'CCDC 733505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C51 H55 B N9 O6 P2 Rh S3), 3(C H2 Cl2) ' _chemical_formula_sum 'C105 H116 B2 Cl6 N18 O12 P4 Rh2 S6' _chemical_formula_weight 2578.54 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.309(2) _cell_length_b 14.935(3) _cell_length_c 19.807(4) _cell_angle_alpha 102.89(3) _cell_angle_beta 91.48(3) _cell_angle_gamma 94.73(3) _cell_volume 2959.8(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2588 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.28 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1326 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Crystal was twinned, GEMINI was used to resolve the two sets of reflections. It was not possible to model one CH2Cl2 solvent molecule. ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29160 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.3239 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.53 _reflns_number_total 29161 _reflns_number_gt 10919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1282P)^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 29161 _refine_ls_number_parameters 721 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.2733 _refine_ls_R_factor_gt 0.1098 _refine_ls_wR_factor_ref 0.2990 _refine_ls_wR_factor_gt 0.2278 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.980 _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 0.96353(6) 0.54820(5) 0.73423(4) 0.0279(2) Uani 1 1 d . . . S1 S 0.99617(19) 0.48419(14) 0.61413(11) 0.0313(5) Uani 1 1 d . . . S2 S 1.1236(2) 0.46695(14) 0.77945(12) 0.0346(5) Uani 1 1 d . . . S3 S 0.6628(2) 0.19378(15) 0.62122(12) 0.0373(6) Uani 1 1 d . . . P1 P 0.9015(2) 0.60136(16) 0.83892(12) 0.0327(6) Uani 1 1 d . . . P2 P 0.87024(19) 0.65646(15) 0.69815(11) 0.0281(5) Uani 1 1 d . . . O1 O 0.8960(5) 0.5379(4) 0.8971(3) 0.0398(15) Uani 1 1 d . . . O2 O 0.7524(5) 0.6289(4) 0.8379(3) 0.0359(14) Uani 1 1 d . . . O3 O 0.9743(5) 0.6884(4) 0.8917(3) 0.0387(15) Uani 1 1 d . . . O4 O 0.9269(5) 0.6924(4) 0.6331(3) 0.0310(14) Uani 1 1 d . . . O5 O 0.8683(5) 0.7494(4) 0.7561(3) 0.0338(14) Uani 1 1 d . . . O6 O 0.7231(4) 0.6400(4) 0.6643(3) 0.0354(14) Uani 1 1 d . . . N1 N 1.0877(6) 0.3157(4) 0.6245(3) 0.0261(15) Uani 1 1 d . . . N2 N 1.1920(6) 0.2644(4) 0.5998(3) 0.0304(16) Uani 1 1 d . . . N3 N 1.1983(6) 0.3912(4) 0.5599(4) 0.0343(18) Uani 1 1 d . . . N4 N 1.0344(6) 0.2817(4) 0.7409(3) 0.0248(15) Uani 1 1 d . . . N5 N 1.0275(7) 0.2034(5) 0.7690(4) 0.0368(18) Uani 1 1 d . . . N6 N 1.1177(7) 0.3248(5) 0.8451(3) 0.0377(19) Uani 1 1 d . . . N7 N 0.9294(6) 0.1773(4) 0.6304(3) 0.0250(15) Uani 1 1 d . . . N8 N 1.0143(6) 0.1064(4) 0.6181(3) 0.0287(16) Uani 1 1 d . . . N9 N 0.8104(6) 0.0480(4) 0.5883(3) 0.0278(16) Uani 1 1 d . . . B1 B 0.9754(8) 0.2763(6) 0.6666(5) 0.029(2) Uani 1 1 d . . . H1 H 0.9021 0.3145 0.6695 0.034 Uiso 1 1 calc R . . C1 C 1.0963(7) 0.3956(5) 0.6011(4) 0.028(2) Uani 1 1 d . . . C2 C 1.2573(7) 0.3119(6) 0.5614(5) 0.036(2) Uani 1 1 d . . . C3 C 1.3737(8) 0.2812(6) 0.5209(5) 0.053(3) Uani 1 1 d . . . H3A H 1.4016 0.2273 0.5337 0.080 Uiso 1 1 calc R . . H3B H 1.4433 0.3297 0.5310 0.080 Uiso 1 1 calc R . . H3C H 1.3504 0.2671 0.4722 0.080 Uiso 1 1 calc R . . C4 C 1.2359(8) 0.4582(6) 0.5149(5) 0.046(2) Uani 1 1 d . . . H4A H 1.2719 0.4253 0.4727 0.055 Uiso 1 1 calc R . . H4B H 1.1587 0.4847 0.5020 0.055 Uiso 1 1 calc R . . C5 C 1.3323(9) 0.5326(6) 0.5514(5) 0.060(3) Uani 1 1 d . . . H5A H 1.2947 0.5677 0.5916 0.090 Uiso 1 1 calc R . . H5B H 1.3574 0.5722 0.5210 0.090 Uiso 1 1 calc R . . H5C H 1.4076 0.5063 0.5655 0.090 Uiso 1 1 calc R . . C6 C 1.0852(7) 0.3560(6) 0.7861(4) 0.030(2) Uani 1 1 d . . . C7 C 1.0787(8) 0.2347(6) 0.8325(5) 0.039(2) Uani 1 1 d . . . C8 C 1.0954(11) 0.1718(7) 0.8819(5) 0.073(4) Uani 1 1 d . . . H8A H 1.0710 0.2017 0.9273 0.109 Uiso 1 1 calc R . . H8B H 1.1848 0.1587 0.8840 0.109 Uiso 1 1 calc R . . H8C H 1.0410 0.1153 0.8659 0.109 Uiso 1 1 calc R . . C9 C 1.1825(10) 0.3855(6) 0.9080(5) 0.054(3) Uani 1 1 d . . . H9A H 1.1688 0.3566 0.9469 0.065 Uiso 1 1 calc R . . H9B H 1.1426 0.4433 0.9180 0.065 Uiso 1 1 calc R . . C10 C 1.3281(10) 0.4055(8) 0.9015(5) 0.072(3) Uani 1 1 d . . . H10A H 1.3706 0.3504 0.9003 0.108 Uiso 1 1 calc R . . H10B H 1.3624 0.4527 0.9405 0.108 Uiso 1 1 calc R . . H10C H 1.3430 0.4261 0.8595 0.108 Uiso 1 1 calc R . . C11 C 0.8037(7) 0.1407(6) 0.6134(4) 0.030(2) Uani 1 1 d . . . C12 C 0.9398(7) 0.0318(5) 0.5924(4) 0.0243(18) Uani 1 1 d . . . C13 C 0.9857(8) -0.0625(5) 0.5724(4) 0.039(2) Uani 1 1 d . . . H13A H 0.9781 -0.0839 0.5229 0.058 Uiso 1 1 calc R . . H13B H 0.9334 -0.1040 0.5935 0.058 Uiso 1 1 calc R . . H13C H 1.0752 -0.0603 0.5879 0.058 Uiso 1 1 calc R . . C14 C 0.7006(7) -0.0176(5) 0.5619(4) 0.034(2) Uani 1 1 d . . . H14A H 0.6243 0.0015 0.5870 0.040 Uiso 1 1 calc R . . H14B H 0.7179 -0.0774 0.5700 0.040 Uiso 1 1 calc R . . C15 C 0.6729(9) -0.0265(6) 0.4869(4) 0.047(2) Uani 1 1 d . . . H15A H 0.6641 0.0334 0.4781 0.071 Uiso 1 1 calc R . . H15B H 0.5934 -0.0651 0.4727 0.071 Uiso 1 1 calc R . . H15C H 0.7432 -0.0535 0.4613 0.071 Uiso 1 1 calc R . . C16 C 0.8384(8) 0.4487(6) 0.8849(4) 0.034(2) Uani 1 1 d . . . C17 C 0.7759(9) 0.4026(7) 0.8229(5) 0.052(3) Uani 1 1 d . . . H17 H 0.7678 0.4320 0.7864 0.062 Uiso 1 1 calc R . . C18 C 0.7252(9) 0.3117(7) 0.8158(5) 0.056(3) Uani 1 1 d . . . H18 H 0.6822 0.2799 0.7745 0.067 Uiso 1 1 calc R . . C19 C 0.7385(11) 0.2687(7) 0.8696(6) 0.071(3) Uani 1 1 d . . . H19 H 0.7072 0.2072 0.8643 0.085 Uiso 1 1 calc R . . C20 C 0.7994(12) 0.3177(7) 0.9322(5) 0.069(3) Uani 1 1 d . . . H20 H 0.8050 0.2887 0.9690 0.083 Uiso 1 1 calc R . . C21 C 0.8516(9) 0.4077(6) 0.9412(5) 0.049(3) Uani 1 1 d . . . H21 H 0.8935 0.4396 0.9828 0.059 Uiso 1 1 calc R . . C22 C 0.6835(8) 0.6657(7) 0.8925(4) 0.039(2) Uani 1 1 d . . . C23 C 0.5833(9) 0.6089(7) 0.9112(5) 0.051(3) Uani 1 1 d . . . H23 H 0.5671 0.5471 0.8889 0.061 Uiso 1 1 calc R . . C24 C 0.5092(13) 0.6499(11) 0.9651(7) 0.087(4) Uani 1 1 d . . . H24 H 0.4420 0.6132 0.9786 0.104 Uiso 1 1 calc R . . C25 C 0.5278(12) 0.7402(11) 0.9996(6) 0.075(4) Uani 1 1 d . . . H25 H 0.4764 0.7632 1.0363 0.090 Uiso 1 1 calc R . . C26 C 0.6245(11) 0.7964(10) 0.9791(6) 0.079(4) Uani 1 1 d . . . H26 H 0.6382 0.8587 1.0006 0.094 Uiso 1 1 calc R . . C27 C 0.7013(9) 0.7575(8) 0.9252(5) 0.062(3) Uani 1 1 d . . . H27 H 0.7667 0.7949 0.9109 0.075 Uiso 1 1 calc R . . C28 C 1.0871(8) 0.7406(6) 0.8790(4) 0.037(2) Uani 1 1 d . . . C29 C 1.2040(8) 0.7013(6) 0.8695(4) 0.041(2) Uani 1 1 d . . . H29 H 1.2076 0.6393 0.8698 0.049 Uiso 1 1 calc R . . C30 C 1.3190(9) 0.7554(7) 0.8593(5) 0.055(3) Uani 1 1 d . . . H30 H 1.3988 0.7305 0.8536 0.066 Uiso 1 1 calc R . . C31 C 1.3069(11) 0.8478(8) 0.8583(5) 0.069(3) Uani 1 1 d . . . H31 H 1.3800 0.8848 0.8513 0.083 Uiso 1 1 calc R . . C32 C 1.1920(11) 0.8840(7) 0.8673(6) 0.071(3) Uani 1 1 d . . . H32 H 1.1870 0.9459 0.8673 0.086 Uiso 1 1 calc R . . C33 C 1.0818(9) 0.8307(6) 0.8763(5) 0.047(2) Uani 1 1 d . . . H33 H 1.0024 0.8563 0.8807 0.056 Uiso 1 1 calc R . . C34 C 1.0619(7) 0.7177(5) 0.6246(4) 0.033(2) Uani 1 1 d . . . C35 C 1.1534(8) 0.7430(6) 0.6790(4) 0.036(2) Uani 1 1 d . . . H35 H 1.1327 0.7402 0.7239 0.043 Uiso 1 1 calc R . . C36 C 1.2781(8) 0.7728(6) 0.6635(5) 0.050(3) Uani 1 1 d . . . H36 H 1.3408 0.7913 0.6996 0.060 Uiso 1 1 calc R . . C37 C 1.3131(9) 0.7764(6) 0.5991(5) 0.046(3) Uani 1 1 d . . . H37 H 1.3976 0.7974 0.5912 0.056 Uiso 1 1 calc R . . C38 C 1.2221(10) 0.7485(6) 0.5454(5) 0.053(3) Uani 1 1 d . . . H38 H 1.2459 0.7481 0.5004 0.063 Uiso 1 1 calc R . . C39 C 1.0949(8) 0.7208(5) 0.5575(4) 0.034(2) Uani 1 1 d . . . H39 H 1.0323 0.7044 0.5211 0.041 Uiso 1 1 calc R . . C40 C 0.8223(8) 0.8336(5) 0.7490(4) 0.034(2) Uani 1 1 d . . . C41 C 0.9084(8) 0.9064(6) 0.7441(4) 0.037(2) Uani 1 1 d . . . H41 H 0.9970 0.8988 0.7424 0.045 Uiso 1 1 calc R . . C42 C 0.8650(12) 0.9931(7) 0.7418(5) 0.060(3) Uani 1 1 d . . . H42 H 0.9247 1.0423 0.7391 0.072 Uiso 1 1 calc R . . C43 C 0.7333(11) 1.0043(7) 0.7434(5) 0.062(3) Uani 1 1 d . . . H43 H 0.7032 1.0604 0.7406 0.074 Uiso 1 1 calc R . . C44 C 0.6467(11) 0.9304(7) 0.7493(6) 0.072(3) Uani 1 1 d . . . H44 H 0.5581 0.9379 0.7504 0.086 Uiso 1 1 calc R . . C45 C 0.6883(9) 0.8456(6) 0.7536(5) 0.057(3) Uani 1 1 d . . . H45 H 0.6290 0.7978 0.7594 0.069 Uiso 1 1 calc R . . C46 C 0.6297(7) 0.5729(6) 0.6804(4) 0.034(2) Uani 1 1 d . . . C47 C 0.5182(8) 0.6060(6) 0.7096(4) 0.041(2) Uani 1 1 d . . . H47 H 0.5081 0.6688 0.7186 0.049 Uiso 1 1 calc R . . C48 C 0.4219(8) 0.5457(6) 0.7254(5) 0.049(3) Uani 1 1 d . . . H48 H 0.3475 0.5676 0.7463 0.058 Uiso 1 1 calc R . . C49 C 0.4364(9) 0.4528(7) 0.7102(5) 0.053(3) Uani 1 1 d . . . H49 H 0.3710 0.4119 0.7206 0.064 Uiso 1 1 calc R . . C50 C 0.5480(8) 0.4193(7) 0.6794(5) 0.054(3) Uani 1 1 d . . . H50 H 0.5586 0.3565 0.6702 0.064 Uiso 1 1 calc R . . C51 C 0.6450(8) 0.4821(6) 0.6623(5) 0.048(3) Uani 1 1 d . . . H51 H 0.7177 0.4611 0.6390 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.3830(3) 0.2074(2) 0.76840(17) 0.0931(11) Uani 1 1 d . . . Cl2 Cl 0.2872(3) 0.0157(2) 0.7173(2) 0.1086(14) Uani 1 1 d . . . C52 C 0.3279(9) 0.1217(6) 0.6963(5) 0.056(3) Uani 1 1 d . . . H52A H 0.3952 0.1146 0.6626 0.067 Uiso 1 1 calc R . . H52B H 0.2520 0.1405 0.6750 0.067 Uiso 1 1 calc R . . C53 C 0.7488(11) 0.0706(10) 0.9486(10) 0.100(10) Uani 0.50 1 d PDU A 1 H53A H 0.7748 0.1011 0.9120 0.120 Uiso 0.50 1 calc PR A 1 H53B H 0.7532 0.1179 0.9912 0.120 Uiso 0.50 1 calc PR A 1 Cl3 Cl 0.8626(8) -0.0007(4) 0.9568(4) 0.107(3) Uani 0.50 1 d PD A 1 Cl4 Cl 0.5899(8) 0.0308(5) 0.9315(5) 0.142(4) Uani 0.50 1 d PD . . 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 0.0194(3) 0.0298(4) 0.0388(4) 0.0171(3) 0.0004(3) 0.0010(3) S1 0.0290(12) 0.0310(13) 0.0406(13) 0.0194(11) 0.0059(10) 0.0103(10) S2 0.0250(12) 0.0278(13) 0.0536(15) 0.0169(11) -0.0069(11) -0.0011(9) S3 0.0217(11) 0.0414(14) 0.0522(15) 0.0170(12) 0.0002(10) 0.0045(10) P1 0.0309(13) 0.0326(14) 0.0363(13) 0.0134(11) -0.0037(11) -0.0010(10) P2 0.0202(11) 0.0316(13) 0.0357(13) 0.0149(11) 0.0006(10) 0.0014(10) O1 0.039(4) 0.038(4) 0.047(4) 0.025(3) -0.009(3) -0.011(3) O2 0.022(3) 0.054(4) 0.032(3) 0.011(3) 0.004(3) 0.000(3) O3 0.050(4) 0.037(4) 0.033(3) 0.013(3) 0.005(3) 0.007(3) O4 0.019(3) 0.038(4) 0.043(3) 0.027(3) 0.000(3) -0.002(2) O5 0.021(3) 0.049(4) 0.042(3) 0.033(3) -0.004(3) 0.003(3) O6 0.010(3) 0.051(4) 0.053(4) 0.027(3) 0.002(3) 0.002(3) N1 0.023(4) 0.024(4) 0.035(4) 0.015(3) 0.003(3) -0.001(3) N2 0.018(3) 0.036(4) 0.045(4) 0.022(4) 0.009(3) 0.008(3) N3 0.030(4) 0.029(4) 0.053(5) 0.023(4) 0.024(4) 0.015(3) N4 0.021(4) 0.020(4) 0.038(4) 0.016(3) 0.005(3) 0.000(3) N5 0.040(4) 0.035(5) 0.041(5) 0.024(4) 0.006(4) -0.006(4) N6 0.043(5) 0.043(5) 0.033(4) 0.023(4) -0.006(4) 0.001(4) N7 0.016(3) 0.025(4) 0.038(4) 0.013(3) 0.002(3) 0.005(3) N8 0.025(4) 0.021(4) 0.044(4) 0.015(3) -0.007(3) 0.005(3) N9 0.018(4) 0.026(4) 0.041(4) 0.013(3) 0.004(3) -0.001(3) B1 0.018(5) 0.038(6) 0.038(6) 0.027(5) 0.002(4) 0.003(4) C1 0.020(4) 0.028(5) 0.045(5) 0.025(4) -0.003(4) 0.000(3) C2 0.023(5) 0.034(5) 0.061(6) 0.027(5) 0.012(4) 0.005(4) C3 0.036(6) 0.042(6) 0.091(8) 0.030(6) 0.024(6) 0.009(5) C4 0.029(5) 0.053(6) 0.067(6) 0.038(6) 0.010(5) 0.008(5) C5 0.037(6) 0.058(7) 0.096(8) 0.045(6) -0.008(6) 0.001(5) C6 0.023(4) 0.029(5) 0.038(5) 0.008(4) -0.002(4) 0.005(4) C7 0.032(5) 0.044(6) 0.047(6) 0.022(5) 0.012(5) -0.004(4) C8 0.095(9) 0.074(8) 0.059(7) 0.045(6) -0.010(6) -0.017(7) C9 0.084(8) 0.040(6) 0.040(6) 0.019(5) -0.016(6) -0.008(6) C10 0.073(8) 0.081(9) 0.061(7) 0.024(6) -0.038(6) 0.000(7) C11 0.016(4) 0.042(6) 0.032(5) 0.011(4) -0.010(4) -0.005(4) C12 0.024(4) 0.022(5) 0.027(5) 0.007(4) 0.003(4) 0.001(4) C13 0.032(5) 0.028(5) 0.059(6) 0.015(5) 0.000(4) 0.006(4) C14 0.024(5) 0.030(5) 0.044(6) 0.004(4) 0.000(4) -0.002(4) C15 0.046(6) 0.041(6) 0.052(6) 0.007(5) -0.003(5) -0.002(5) C16 0.029(5) 0.041(6) 0.034(5) 0.012(5) 0.012(4) -0.002(4) C17 0.042(6) 0.063(7) 0.051(6) 0.020(6) 0.010(5) -0.025(5) C18 0.051(6) 0.067(8) 0.046(6) 0.010(6) 0.016(5) -0.016(6) C19 0.086(9) 0.049(7) 0.072(8) 0.007(7) 0.037(7) -0.027(6) C20 0.124(11) 0.039(7) 0.048(7) 0.020(6) 0.020(7) -0.010(7) C21 0.067(7) 0.036(6) 0.043(6) 0.005(5) 0.016(5) 0.009(5) C22 0.035(5) 0.057(7) 0.024(5) 0.010(5) -0.002(4) 0.010(5) C23 0.039(6) 0.057(7) 0.063(7) 0.024(6) 0.017(5) 0.010(5) C24 0.082(10) 0.112(12) 0.087(10) 0.063(9) 0.007(8) 0.021(9) C25 0.063(9) 0.131(13) 0.038(7) 0.024(8) 0.006(6) 0.034(9) C26 0.053(8) 0.115(11) 0.055(7) -0.007(7) -0.002(6) 0.004(8) C27 0.029(6) 0.097(10) 0.051(7) -0.009(7) 0.007(5) 0.017(6) C28 0.027(5) 0.038(6) 0.049(6) 0.026(5) -0.006(4) -0.013(4) C29 0.035(5) 0.039(6) 0.052(6) 0.017(5) -0.005(5) -0.003(4) C30 0.030(6) 0.070(8) 0.069(7) 0.025(6) 0.001(5) 0.001(5) C31 0.060(8) 0.080(9) 0.075(8) 0.047(7) -0.026(6) -0.030(7) C32 0.062(8) 0.042(7) 0.117(10) 0.038(7) -0.020(7) -0.007(6) C33 0.035(5) 0.034(6) 0.074(7) 0.017(5) -0.006(5) 0.005(4) C34 0.023(5) 0.032(5) 0.045(6) 0.017(4) -0.003(4) -0.003(4) C35 0.039(5) 0.037(5) 0.039(5) 0.021(4) 0.008(4) 0.010(4) C36 0.025(5) 0.047(6) 0.076(7) 0.014(6) -0.003(5) -0.002(4) C37 0.028(5) 0.056(7) 0.067(7) 0.037(6) 0.014(5) -0.001(5) C38 0.055(7) 0.053(7) 0.064(7) 0.035(6) 0.032(6) 0.013(5) C39 0.041(5) 0.029(5) 0.034(5) 0.013(4) -0.001(4) 0.002(4) C40 0.032(5) 0.024(5) 0.046(6) 0.006(4) 0.000(4) 0.012(4) C41 0.037(5) 0.034(6) 0.043(5) 0.017(5) 0.011(4) -0.005(4) C42 0.104(10) 0.036(6) 0.039(6) 0.018(5) 0.000(6) -0.019(6) C43 0.071(8) 0.044(7) 0.075(8) 0.024(6) -0.001(7) 0.004(6) C44 0.053(7) 0.055(8) 0.112(10) 0.023(7) 0.000(7) 0.026(6) C45 0.046(6) 0.040(6) 0.091(8) 0.017(6) 0.014(6) 0.017(5) C46 0.019(4) 0.045(6) 0.039(5) 0.016(5) -0.007(4) 0.000(4) C47 0.035(5) 0.029(5) 0.055(6) 0.002(5) 0.015(5) -0.005(4) C48 0.026(5) 0.041(6) 0.070(7) -0.005(5) -0.001(5) -0.003(5) C49 0.036(6) 0.040(6) 0.085(8) 0.024(6) -0.001(5) -0.014(5) C50 0.027(5) 0.050(7) 0.087(8) 0.026(6) 0.000(5) -0.001(5) C51 0.020(5) 0.041(6) 0.083(7) 0.015(6) 0.006(5) 0.009(4) Cl1 0.058(2) 0.101(3) 0.101(2) -0.010(2) 0.0033(18) -0.0157(18) Cl2 0.079(2) 0.067(2) 0.196(4) 0.072(3) -0.031(2) -0.0020(18) C52 0.039(6) 0.061(7) 0.075(7) 0.039(6) -0.022(5) -0.010(5) C53 0.20(3) 0.061(16) 0.045(13) 0.041(12) -0.073(15) -0.040(17) Cl3 0.149(7) 0.052(4) 0.098(5) -0.030(4) 0.062(5) -0.015(4) Cl4 0.122(6) 0.067(5) 0.200(8) -0.053(5) 0.111(6) -0.010(4) _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 P1 2.181(3) . ? Rh1 P2 2.188(2) . ? Rh1 S2 2.395(2) . ? Rh1 S1 2.401(2) . ? S1 C1 1.723(8) . ? S2 C6 1.707(8) . ? S3 C11 1.706(8) . ? P1 O3 1.594(6) . ? P1 O2 1.624(6) . ? P1 O1 1.647(5) . ? P2 O5 1.594(6) . ? P2 O4 1.609(5) . ? P2 O6 1.620(5) . ? O1 C16 1.380(9) . ? O2 C22 1.347(10) . ? O3 C28 1.405(9) . ? O4 C34 1.436(9) . ? O5 C40 1.414(8) . ? O6 C46 1.426(9) . ? N1 C1 1.370(8) . ? N1 N2 1.407(8) . ? N1 B1 1.593(10) . ? N2 C2 1.313(9) . ? N3 C1 1.345(9) . ? N3 C2 1.381(9) . ? N3 C4 1.515(9) . ? N4 C6 1.321(9) . ? N4 N5 1.400(8) . ? N4 B1 1.560(10) . ? N5 C7 1.319(10) . ? N6 C7 1.339(10) . ? N6 C6 1.393(9) . ? N6 C9 1.475(11) . ? N7 C11 1.368(9) . ? N7 N8 1.413(8) . ? N7 B1 1.522(11) . ? N8 C12 1.294(9) . ? N9 C11 1.370(9) . ? N9 C12 1.379(9) . ? N9 C14 1.440(9) . ? B1 H1 0.9800 . ? C2 C3 1.507(11) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.472(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 C8 1.516(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.520(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 C13 1.496(10) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.480(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.382(12) . ? C16 C21 1.395(11) . ? C17 C18 1.390(12) . ? C17 H17 0.9300 . ? C18 C19 1.369(13) . ? C18 H18 0.9300 . ? C19 C20 1.397(14) . ? C19 H19 0.9300 . ? C20 C21 1.377(12) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.374(13) . ? C22 C23 1.392(12) . ? C23 C24 1.388(15) . ? C23 H23 0.9300 . ? C24 C25 1.364(16) . ? C24 H24 0.9300 . ? C25 C26 1.379(15) . ? C25 H25 0.9300 . ? C26 C27 1.395(13) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.364(11) . ? C28 C29 1.383(11) . ? C29 C30 1.424(12) . ? C29 H29 0.9300 . ? C30 C31 1.399(13) . ? C30 H30 0.9300 . ? C31 C32 1.342(14) . ? C31 H31 0.9300 . ? C32 C33 1.371(13) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.378(11) . ? C34 C39 1.391(10) . ? C35 C36 1.389(11) . ? C35 H35 0.9300 . ? C36 C37 1.346(11) . ? C36 H36 0.9300 . ? C37 C38 1.367(13) . ? C37 H37 0.9300 . ? C38 C39 1.385(12) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.369(11) . ? C40 C45 1.411(11) . ? C41 C42 1.415(12) . ? C41 H41 0.9300 . ? C42 C43 1.382(14) . ? C42 H42 0.9300 . ? C43 C44 1.389(14) . ? C43 H43 0.9300 . ? C44 C45 1.389(12) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.348(11) . ? C46 C47 1.379(11) . ? C47 C48 1.374(11) . ? C47 H47 0.9300 . ? C48 C49 1.373(12) . ? C48 H48 0.9300 . ? C49 C50 1.395(12) . ? C49 H49 0.9300 . ? C50 C51 1.413(12) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? Cl1 C52 1.740(10) . ? Cl2 C52 1.746(9) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 Cl3 1.676(9) . ? C53 Cl4 1.694(9) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? 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 P1 Rh1 P2 90.19(9) . . ? P1 Rh1 S2 90.04(9) . . ? P2 Rh1 S2 161.51(8) . . ? P1 Rh1 S1 171.04(8) . . ? P2 Rh1 S1 86.05(8) . . ? S2 Rh1 S1 96.10(8) . . ? C1 S1 Rh1 113.5(3) . . ? C6 S2 Rh1 119.8(3) . . ? O3 P1 O2 102.2(3) . . ? O3 P1 O1 93.0(3) . . ? O2 P1 O1 101.0(3) . . ? O3 P1 Rh1 123.8(2) . . ? O2 P1 Rh1 111.3(2) . . ? O1 P1 Rh1 121.7(2) . . ? O5 P2 O4 102.8(3) . . ? O5 P2 O6 103.2(3) . . ? O4 P2 O6 92.3(3) . . ? O5 P2 Rh1 113.5(2) . . ? O4 P2 Rh1 119.3(2) . . ? O6 P2 Rh1 122.1(2) . . ? C16 O1 P1 124.1(5) . . ? C22 O2 P1 127.6(5) . . ? C28 O3 P1 126.0(5) . . ? C34 O4 P2 125.1(5) . . ? C40 O5 P2 127.9(5) . . ? C46 O6 P2 121.6(4) . . ? C1 N1 N2 109.0(6) . . ? C1 N1 B1 129.0(6) . . ? N2 N1 B1 121.8(6) . . ? C2 N2 N1 106.0(6) . . ? C1 N3 C2 108.7(6) . . ? C1 N3 C4 125.6(6) . . ? C2 N3 C4 125.6(6) . . ? C6 N4 N5 111.8(6) . . ? C6 N4 B1 127.4(6) . . ? N5 N4 B1 120.5(6) . . ? C7 N5 N4 103.6(7) . . ? C7 N6 C6 107.5(7) . . ? C7 N6 C9 129.4(7) . . ? C6 N6 C9 123.1(7) . . ? C11 N7 N8 109.9(6) . . ? C11 N7 B1 127.2(7) . . ? N8 N7 B1 122.5(6) . . ? C12 N8 N7 104.9(6) . . ? C11 N9 C12 107.1(6) . . ? C11 N9 C14 125.0(6) . . ? C12 N9 C14 127.9(7) . . ? N7 B1 N4 111.2(6) . . ? N7 B1 N1 109.9(7) . . ? N4 B1 N1 106.9(6) . . ? N7 B1 H1 109.6 . . ? N4 B1 H1 109.6 . . ? N1 B1 H1 109.6 . . ? N3 C1 N1 106.3(6) . . ? N3 C1 S1 123.7(5) . . ? N1 C1 S1 129.9(6) . . ? N2 C2 N3 109.9(7) . . ? N2 C2 C3 125.0(7) . . ? N3 C2 C3 125.0(7) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 N3 111.3(7) . . ? C5 C4 H4A 109.4 . . ? N3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? N3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N6 105.0(7) . . ? N4 C6 S2 132.2(6) . . ? N6 C6 S2 122.6(6) . . ? N5 C7 N6 112.0(7) . . ? N5 C7 C8 122.0(9) . . ? N6 C7 C8 125.9(8) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 113.1(8) . . ? N6 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N6 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 N9 105.8(6) . . ? N7 C11 S3 129.6(7) . . ? N9 C11 S3 124.6(6) . . ? N8 C12 N9 112.4(7) . . ? N8 C12 C13 124.6(7) . . ? N9 C12 C13 122.9(7) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N9 C14 C15 112.2(7) . . ? N9 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N9 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 124.0(8) . . ? O1 C16 C21 113.5(8) . . ? C17 C16 C21 122.5(9) . . ? C16 C17 C18 118.9(9) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.2(10) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.6(10) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 122.0(9) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C16 116.8(9) . . ? C20 C21 H21 121.6 . . ? C16 C21 H21 121.6 . . ? O2 C22 C27 122.4(9) . . ? O2 C22 C23 117.3(9) . . ? C27 C22 C23 120.0(9) . . ? C24 C23 C22 116.1(11) . . ? C24 C23 H23 121.9 . . ? C22 C23 H23 121.9 . . ? C25 C24 C23 124.8(12) . . ? C25 C24 H24 117.6 . . ? C23 C24 H24 117.6 . . ? C24 C25 C26 118.6(12) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C25 C26 C27 118.2(12) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C22 C27 C26 122.3(11) . . ? C22 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C33 C28 C29 119.6(8) . . ? C33 C28 O3 120.0(8) . . ? C29 C28 O3 120.4(7) . . ? C28 C29 C30 120.1(8) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 117.2(9) . . ? C31 C30 H30 121.4 . . ? C29 C30 H30 121.4 . . ? C32 C31 C30 121.4(10) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 120.7(10) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C28 C33 C32 120.9(9) . . ? C28 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C39 120.9(7) . . ? C35 C34 O4 123.5(7) . . ? C39 C34 O4 115.5(7) . . ? C34 C35 C36 116.9(8) . . ? C34 C35 H35 121.5 . . ? C36 C35 H35 121.5 . . ? C37 C36 C35 123.6(9) . . ? C37 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C36 C37 C38 118.7(8) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C37 C38 C39 120.7(9) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 119.1(8) . . ? C38 C39 H39 120.4 . . ? C34 C39 H39 120.4 . . ? C41 C40 C45 119.6(8) . . ? C41 C40 O5 120.2(7) . . ? C45 C40 O5 120.0(7) . . ? C40 C41 C42 121.1(9) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C43 C42 C41 119.6(9) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 118.9(10) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C45 C44 C43 122.1(10) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C44 C45 C40 118.6(9) . . ? C44 C45 H45 120.7 . . ? C40 C45 H45 120.7 . . ? C51 C46 C47 122.3(8) . . ? C51 C46 O6 121.5(8) . . ? C47 C46 O6 115.9(7) . . ? C48 C47 C46 119.7(8) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C49 C48 C47 119.6(9) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.7(8) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C51 119.0(9) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C46 C51 C50 118.6(9) . . ? C46 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? Cl1 C52 Cl2 112.4(5) . . ? Cl1 C52 H52A 109.1 . . ? Cl2 C52 H52A 109.1 . . ? Cl1 C52 H52B 109.1 . . ? Cl2 C52 H52B 109.1 . . ? H52A C52 H52B 107.9 . . ? Cl3 C53 Cl4 121.2(10) . . ? Cl3 C53 H53A 107.0 . . ? Cl4 C53 H53A 107.0 . . ? Cl3 C53 H53B 107.0 . . ? Cl4 C53 H53B 107.0 . . ? H53A C53 H53B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Rh1 S1 C1 -124.3(6) . . . . ? P2 Rh1 S1 C1 170.4(3) . . . . ? S2 Rh1 S1 C1 8.8(3) . . . . ? P1 Rh1 S2 C6 91.5(3) . . . . ? P2 Rh1 S2 C6 -177.8(4) . . . . ? S1 Rh1 S2 C6 -82.0(3) . . . . ? P2 Rh1 P1 O3 -79.8(3) . . . . ? S2 Rh1 P1 O3 81.7(3) . . . . ? S1 Rh1 P1 O3 -144.9(5) . . . . ? P2 Rh1 P1 O2 42.4(2) . . . . ? S2 Rh1 P1 O2 -156.1(2) . . . . ? S1 Rh1 P1 O2 -22.6(7) . . . . ? P2 Rh1 P1 O1 161.1(3) . . . . ? S2 Rh1 P1 O1 -37.4(3) . . . . ? S1 Rh1 P1 O1 96.0(6) . . . . ? P1 Rh1 P2 O5 30.4(2) . . . . ? S2 Rh1 P2 O5 -60.3(4) . . . . ? S1 Rh1 P2 O5 -157.8(2) . . . . ? P1 Rh1 P2 O4 151.8(3) . . . . ? S2 Rh1 P2 O4 61.1(4) . . . . ? S1 Rh1 P2 O4 -36.3(3) . . . . ? P1 Rh1 P2 O6 -94.2(3) . . . . ? S2 Rh1 P2 O6 175.1(3) . . . . ? S1 Rh1 P2 O6 77.7(3) . . . . ? O3 P1 O1 C16 178.3(6) . . . . ? O2 P1 O1 C16 75.2(7) . . . . ? Rh1 P1 O1 C16 -48.4(7) . . . . ? O3 P1 O2 C22 -44.4(8) . . . . ? O1 P1 O2 C22 51.2(8) . . . . ? Rh1 P1 O2 C22 -178.3(7) . . . . ? O2 P1 O3 C28 -127.6(6) . . . . ? O1 P1 O3 C28 130.5(6) . . . . ? Rh1 P1 O3 C28 -1.4(7) . . . . ? O5 P2 O4 C34 78.8(6) . . . . ? O6 P2 O4 C34 -177.0(6) . . . . ? Rh1 P2 O4 C34 -47.8(7) . . . . ? O4 P2 O5 C40 46.0(6) . . . . ? O6 P2 O5 C40 -49.5(6) . . . . ? Rh1 P2 O5 C40 176.3(5) . . . . ? O5 P2 O6 C46 -103.4(6) . . . . ? O4 P2 O6 C46 152.8(6) . . . . ? Rh1 P2 O6 C46 25.7(7) . . . . ? C1 N1 N2 C2 -1.9(9) . . . . ? B1 N1 N2 C2 173.1(7) . . . . ? C6 N4 N5 C7 -1.1(9) . . . . ? B1 N4 N5 C7 -176.2(7) . . . . ? C11 N7 N8 C12 2.3(8) . . . . ? B1 N7 N8 C12 174.6(6) . . . . ? C11 N7 B1 N4 111.7(8) . . . . ? N8 N7 B1 N4 -59.2(9) . . . . ? C11 N7 B1 N1 -130.2(7) . . . . ? N8 N7 B1 N1 58.9(8) . . . . ? C6 N4 B1 N7 178.9(7) . . . . ? N5 N4 B1 N7 -6.8(9) . . . . ? C6 N4 B1 N1 58.9(10) . . . . ? N5 N4 B1 N1 -126.8(7) . . . . ? C1 N1 B1 N7 127.8(8) . . . . ? N2 N1 B1 N7 -46.0(9) . . . . ? C1 N1 B1 N4 -111.4(8) . . . . ? N2 N1 B1 N4 74.8(8) . . . . ? C2 N3 C1 N1 -3.8(9) . . . . ? C4 N3 C1 N1 171.8(7) . . . . ? C2 N3 C1 S1 179.8(6) . . . . ? C4 N3 C1 S1 -4.5(12) . . . . ? N2 N1 C1 N3 3.5(8) . . . . ? B1 N1 C1 N3 -170.9(7) . . . . ? N2 N1 C1 S1 179.6(6) . . . . ? B1 N1 C1 S1 5.1(12) . . . . ? Rh1 S1 C1 N3 -130.3(6) . . . . ? Rh1 S1 C1 N1 54.3(8) . . . . ? N1 N2 C2 N3 -0.5(9) . . . . ? N1 N2 C2 C3 -176.6(8) . . . . ? C1 N3 C2 N2 2.8(10) . . . . ? C4 N3 C2 N2 -172.8(8) . . . . ? C1 N3 C2 C3 178.8(8) . . . . ? C4 N3 C2 C3 3.2(14) . . . . ? C1 N3 C4 C5 93.3(10) . . . . ? C2 N3 C4 C5 -91.8(10) . . . . ? N5 N4 C6 N6 2.4(8) . . . . ? B1 N4 C6 N6 177.2(7) . . . . ? N5 N4 C6 S2 176.4(6) . . . . ? B1 N4 C6 S2 -8.9(12) . . . . ? C7 N6 C6 N4 -2.9(9) . . . . ? C9 N6 C6 N4 177.5(8) . . . . ? C7 N6 C6 S2 -177.5(6) . . . . ? C9 N6 C6 S2 2.9(11) . . . . ? Rh1 S2 C6 N4 52.1(9) . . . . ? Rh1 S2 C6 N6 -134.8(6) . . . . ? N4 N5 C7 N6 -0.8(9) . . . . ? N4 N5 C7 C8 -177.9(8) . . . . ? C6 N6 C7 N5 2.3(10) . . . . ? C9 N6 C7 N5 -178.1(8) . . . . ? C6 N6 C7 C8 179.3(8) . . . . ? C9 N6 C7 C8 -1.1(15) . . . . ? C7 N6 C9 C10 102.1(10) . . . . ? C6 N6 C9 C10 -78.4(10) . . . . ? N8 N7 C11 N9 -2.2(8) . . . . ? B1 N7 C11 N9 -174.0(6) . . . . ? N8 N7 C11 S3 177.0(6) . . . . ? B1 N7 C11 S3 5.2(11) . . . . ? C12 N9 C11 N7 1.3(8) . . . . ? C14 N9 C11 N7 -177.9(6) . . . . ? C12 N9 C11 S3 -178.0(6) . . . . ? C14 N9 C11 S3 2.9(11) . . . . ? N7 N8 C12 N9 -1.5(8) . . . . ? N7 N8 C12 C13 -178.6(7) . . . . ? C11 N9 C12 N8 0.2(8) . . . . ? C14 N9 C12 N8 179.3(7) . . . . ? C11 N9 C12 C13 177.4(7) . . . . ? C14 N9 C12 C13 -3.5(11) . . . . ? C11 N9 C14 C15 88.4(9) . . . . ? C12 N9 C14 C15 -90.5(9) . . . . ? P1 O1 C16 C17 -1.5(12) . . . . ? P1 O1 C16 C21 177.1(6) . . . . ? O1 C16 C17 C18 177.9(8) . . . . ? C21 C16 C17 C18 -0.7(14) . . . . ? C16 C17 C18 C19 -0.6(15) . . . . ? C17 C18 C19 C20 2.1(16) . . . . ? C18 C19 C20 C21 -2.5(18) . . . . ? C19 C20 C21 C16 1.3(16) . . . . ? O1 C16 C21 C20 -178.3(8) . . . . ? C17 C16 C21 C20 0.3(14) . . . . ? P1 O2 C22 C27 77.6(10) . . . . ? P1 O2 C22 C23 -108.3(8) . . . . ? O2 C22 C23 C24 -176.5(8) . . . . ? C27 C22 C23 C24 -2.3(13) . . . . ? C22 C23 C24 C25 0.3(16) . . . . ? C23 C24 C25 C26 1.8(18) . . . . ? C24 C25 C26 C27 -1.9(16) . . . . ? O2 C22 C27 C26 176.2(9) . . . . ? C23 C22 C27 C26 2.3(14) . . . . ? C25 C26 C27 C22 -0.1(16) . . . . ? P1 O3 C28 C33 114.9(8) . . . . ? P1 O3 C28 C29 -65.3(9) . . . . ? C33 C28 C29 C30 2.1(14) . . . . ? O3 C28 C29 C30 -177.6(8) . . . . ? C28 C29 C30 C31 -1.0(14) . . . . ? C29 C30 C31 C32 0.6(16) . . . . ? C30 C31 C32 C33 -1.3(18) . . . . ? C29 C28 C33 C32 -2.8(15) . . . . ? O3 C28 C33 C32 177.0(9) . . . . ? C31 C32 C33 C28 2.4(17) . . . . ? P2 O4 C34 C35 -21.8(11) . . . . ? P2 O4 C34 C39 161.9(5) . . . . ? C39 C34 C35 C36 1.1(12) . . . . ? O4 C34 C35 C36 -175.0(7) . . . . ? C34 C35 C36 C37 -1.3(13) . . . . ? C35 C36 C37 C38 -0.6(14) . . . . ? C36 C37 C38 C39 2.7(14) . . . . ? C37 C38 C39 C34 -2.9(13) . . . . ? C35 C34 C39 C38 0.9(12) . . . . ? O4 C34 C39 C38 177.3(7) . . . . ? P2 O5 C40 C41 -102.9(8) . . . . ? P2 O5 C40 C45 83.2(9) . . . . ? C45 C40 C41 C42 -1.7(13) . . . . ? O5 C40 C41 C42 -175.6(7) . . . . ? C40 C41 C42 C43 -0.9(14) . . . . ? C41 C42 C43 C44 1.8(15) . . . . ? C42 C43 C44 C45 0.0(17) . . . . ? C43 C44 C45 C40 -2.6(17) . . . . ? C41 C40 C45 C44 3.4(14) . . . . ? O5 C40 C45 C44 177.3(9) . . . . ? P2 O6 C46 C51 -65.2(10) . . . . ? P2 O6 C46 C47 120.6(7) . . . . ? C51 C46 C47 C48 4.5(13) . . . . ? O6 C46 C47 C48 178.6(7) . . . . ? C46 C47 C48 C49 -1.7(14) . . . . ? C47 C48 C49 C50 0.4(14) . . . . ? C48 C49 C50 C51 -1.6(15) . . . . ? C47 C46 C51 C50 -5.6(13) . . . . ? O6 C46 C51 C50 -179.4(7) . . . . ? C49 C50 C51 C46 4.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.537 _refine_diff_density_min -2.657 _refine_diff_density_rms 0.253 data_11+ _database_code_depnum_ccdc_archive 'CCDC 733506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H57 B N9 O P Rh S3, F6 P, 3(C H2 Cl2)' _chemical_formula_sum 'C37 H63 B Cl6 F6 N9 O P2 Rh S3' _chemical_formula_weight 1248.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.339(5) _cell_length_b 15.281(3) _cell_length_c 28.840(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10726(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14543 _cell_measurement_theta_min 3.632 _cell_measurement_theta_max 69.936 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 7.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.212097 _exptl_absorpt_correction_T_max 0.860000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75672 _diffrn_reflns_av_R_equivalents 0.0951 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 70.06 _reflns_number_total 10147 _reflns_number_gt 7987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT V6.41 (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.0557P)^2^+41.7467P] 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 10147 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.568352(14) 0.34079(2) 0.166052(10) 0.01934(11) Uani 1 1 d . . . S3 S 0.48744(5) 0.26858(8) 0.19282(4) 0.0244(2) Uani 1 1 d . . . S2 S 0.63586(5) 0.42040(8) 0.12325(4) 0.0276(3) Uani 1 1 d . . . S1 S 0.62309(5) 0.21040(8) 0.16071(4) 0.0292(3) Uani 1 1 d . . . P1 P 0.60512(5) 0.35893(8) 0.24829(4) 0.0199(2) Uani 1 1 d . . . N1 N 0.56430(15) 0.2219(3) 0.08247(12) 0.0206(8) Uani 1 1 d . . . N2 N 0.55424(17) 0.1795(3) 0.04072(13) 0.0261(9) Uani 1 1 d . . . N3 N 0.61799(18) 0.1104(3) 0.08095(14) 0.0339(10) Uani 1 1 d . . . N4 N 0.55410(15) 0.3818(2) 0.06371(12) 0.0195(8) Uani 1 1 d . . . N5 N 0.53628(16) 0.3966(3) 0.01839(12) 0.0248(8) Uani 1 1 d . . . N6 N 0.61369(17) 0.4668(3) 0.03233(13) 0.0256(9) Uani 1 1 d . . . N7 N 0.47438(16) 0.2942(3) 0.10110(12) 0.0213(8) Uani 1 1 d . . . N8 N 0.43709(16) 0.2818(3) 0.06512(13) 0.0252(9) Uani 1 1 d . . . N9 N 0.40096(16) 0.2406(3) 0.13218(12) 0.0230(8) Uani 1 1 d . . . O1 O 0.50357(17) 0.5062(3) 0.15683(12) 0.0388(9) Uani 1 1 d . . . B1 B 0.5367(2) 0.3085(4) 0.09773(16) 0.0221(11) Uani 1 1 d . . . C1 C 0.5267(2) 0.4451(3) 0.16224(15) 0.0265(10) Uani 1 1 d . . . C2 C 0.60195(19) 0.1804(3) 0.10661(16) 0.0253(10) Uani 1 1 d . A . C3 C 0.5877(2) 0.1133(3) 0.04085(15) 0.0280(11) Uani 1 1 d . A . C4 C 0.5924(3) 0.0481(4) 0.00240(18) 0.0379(13) Uani 1 1 d . . . H4A H 0.5818 -0.0099 0.0138 0.057 Uiso 1 1 calc R A . H4B H 0.6305 0.0463 -0.0087 0.057 Uiso 1 1 calc R . . H4C H 0.5681 0.0652 -0.0231 0.057 Uiso 1 1 calc R . . C5A C 0.6511(4) 0.0349(8) 0.0998(3) 0.034(3) Uani 0.68(2) 1 d P A 1 H5A1 H 0.6492 0.0337 0.1341 0.041 Uiso 0.68(2) 1 calc PR A 1 H5A2 H 0.6368 -0.0213 0.0877 0.041 Uiso 0.68(2) 1 calc PR A 1 C6A C 0.7095(5) 0.0487(8) 0.0839(3) 0.055(3) Uani 0.68(2) 1 d P A 1 H6A1 H 0.7101 0.0578 0.0503 0.083 Uiso 0.68(2) 1 calc PR A 1 H6A2 H 0.7315 -0.0029 0.0918 0.083 Uiso 0.68(2) 1 calc PR A 1 H6A3 H 0.7248 0.1003 0.0995 0.083 Uiso 0.68(2) 1 calc PR A 1 C5B C 0.6747(8) 0.0681(10) 0.0862(5) 0.017(5) Uani 0.32(2) 1 d P A 2 H5B1 H 0.7004 0.1072 0.1028 0.020 Uiso 0.32(2) 1 calc PR A 2 H5B2 H 0.6905 0.0528 0.0556 0.020 Uiso 0.32(2) 1 calc PR A 2 C6B C 0.6618(7) -0.0149(13) 0.1149(6) 0.029(5) Uani 0.32(2) 1 d P A 2 H6B1 H 0.6439 0.0020 0.1440 0.044 Uiso 0.32(2) 1 calc PR A 2 H6B2 H 0.6960 -0.0460 0.1218 0.044 Uiso 0.32(2) 1 calc PR A 2 H6B3 H 0.6372 -0.0532 0.0972 0.044 Uiso 0.32(2) 1 calc PR A 2 C7 C 0.60050(19) 0.4239(3) 0.07172(15) 0.0239(10) Uani 1 1 d . . . C8 C 0.57299(19) 0.4489(3) 0.00098(15) 0.0226(10) Uani 1 1 d . . . C9 C 0.5725(2) 0.4855(3) -0.04699(16) 0.0289(11) Uani 1 1 d . . . H9A H 0.5413 0.4613 -0.0642 0.043 Uiso 1 1 calc R . . H9B H 0.6068 0.4700 -0.0628 0.043 Uiso 1 1 calc R . . H9C H 0.5691 0.5494 -0.0455 0.043 Uiso 1 1 calc R . . C10 C 0.6632(2) 0.5201(4) 0.02509(18) 0.0354(12) Uani 1 1 d . . . H10A H 0.6734 0.5187 -0.0081 0.043 Uiso 1 1 calc R . . H10B H 0.6941 0.4948 0.0430 0.043 Uiso 1 1 calc R . . C11 C 0.6544(3) 0.6131(4) 0.0399(2) 0.0493(16) Uani 1 1 d . . . H11A H 0.6251 0.6391 0.0211 0.074 Uiso 1 1 calc R . . H11B H 0.6884 0.6463 0.0355 0.074 Uiso 1 1 calc R . . H11C H 0.6438 0.6145 0.0727 0.074 Uiso 1 1 calc R . . C12 C 0.45270(19) 0.2689(3) 0.14116(15) 0.0215(9) Uani 1 1 d . . . C13 C 0.3936(2) 0.2499(3) 0.08485(15) 0.0258(10) Uani 1 1 d . . . C14 C 0.3411(2) 0.2264(4) 0.06097(17) 0.0365(13) Uani 1 1 d . . . H14A H 0.3115 0.2645 0.0721 0.055 Uiso 1 1 calc R . . H14B H 0.3319 0.1653 0.0677 0.055 Uiso 1 1 calc R . . H14C H 0.3454 0.2340 0.0274 0.055 Uiso 1 1 calc R . . C15 C 0.3603(2) 0.2132(3) 0.16702(16) 0.0280(11) Uani 1 1 d . . . H15A H 0.3794 0.1844 0.1932 0.034 Uiso 1 1 calc R . . H15B H 0.3349 0.1700 0.1530 0.034 Uiso 1 1 calc R . . C16 C 0.3277(2) 0.2901(4) 0.18491(19) 0.0400(13) Uani 1 1 d . . . H16A H 0.3529 0.3335 0.1982 0.060 Uiso 1 1 calc R . . H16B H 0.3021 0.2702 0.2089 0.060 Uiso 1 1 calc R . . H16C H 0.3071 0.3167 0.1593 0.060 Uiso 1 1 calc R . . C17 C 0.66641(18) 0.4300(3) 0.25266(15) 0.0230(9) Uani 1 1 d . . . H17 H 0.6764 0.4343 0.2862 0.028 Uiso 1 1 calc R . . C18 C 0.71610(19) 0.3921(3) 0.22696(16) 0.0270(10) Uani 1 1 d . . . H18A H 0.7257 0.3345 0.2404 0.032 Uiso 1 1 calc R . . H18B H 0.7066 0.3832 0.1939 0.032 Uiso 1 1 calc R . . C19 C 0.7656(2) 0.4537(4) 0.23058(17) 0.0313(11) Uani 1 1 d . . . H19A H 0.7777 0.4568 0.2633 0.038 Uiso 1 1 calc R . . H19B H 0.7963 0.4298 0.2120 0.038 Uiso 1 1 calc R . . C20 C 0.7521(2) 0.5448(4) 0.21367(17) 0.0337(12) Uani 1 1 d . . . H20A H 0.7431 0.5429 0.1802 0.040 Uiso 1 1 calc R . . H20B H 0.7845 0.5832 0.2177 0.040 Uiso 1 1 calc R . . C21 C 0.7034(2) 0.5822(3) 0.24070(17) 0.0312(11) Uani 1 1 d . . . H21A H 0.7133 0.5877 0.2739 0.037 Uiso 1 1 calc R . . H21B H 0.6945 0.6413 0.2288 0.037 Uiso 1 1 calc R . . C22 C 0.6534(2) 0.5226(3) 0.23565(16) 0.0271(10) Uani 1 1 d . . . H22A H 0.6421 0.5204 0.2027 0.033 Uiso 1 1 calc R . . H22B H 0.6224 0.5468 0.2538 0.033 Uiso 1 1 calc R . . C23 C 0.55691(19) 0.4011(3) 0.29394(15) 0.0235(10) Uani 1 1 d . . . H23 H 0.5392 0.3480 0.3076 0.028 Uiso 1 1 calc R . . C24 C 0.5096(2) 0.4572(3) 0.27584(16) 0.0293(11) Uani 1 1 d . . . H24A H 0.4903 0.4254 0.2508 0.035 Uiso 1 1 calc R . . H24B H 0.5245 0.5122 0.2627 0.035 Uiso 1 1 calc R . . C25 C 0.4690(2) 0.4789(4) 0.31460(17) 0.0331(12) Uani 1 1 d . . . H25A H 0.4402 0.5183 0.3023 0.040 Uiso 1 1 calc R . . H25B H 0.4509 0.4243 0.3251 0.040 Uiso 1 1 calc R . . C26 C 0.4970(2) 0.5224(4) 0.35570(17) 0.0351(12) Uani 1 1 d . . . H26A H 0.5108 0.5807 0.3463 0.042 Uiso 1 1 calc R . . H26B H 0.4700 0.5309 0.3809 0.042 Uiso 1 1 calc R . . C27 C 0.5443(2) 0.4680(4) 0.37339(15) 0.0301(11) Uani 1 1 d . . . H27A H 0.5299 0.4126 0.3864 0.036 Uiso 1 1 calc R . . H27B H 0.5631 0.5000 0.3987 0.036 Uiso 1 1 calc R . . C28 C 0.5858(2) 0.4473(3) 0.33494(15) 0.0275(10) Uani 1 1 d . . . H28A H 0.6151 0.4090 0.3474 0.033 Uiso 1 1 calc R . . H28B H 0.6030 0.5022 0.3240 0.033 Uiso 1 1 calc R . . C29 C 0.62897(19) 0.2522(3) 0.27219(15) 0.0221(9) Uani 1 1 d . . . H29 H 0.6568 0.2295 0.2497 0.027 Uiso 1 1 calc R . . C30 C 0.6581(2) 0.2557(3) 0.31941(15) 0.0257(10) Uani 1 1 d . . . H30A H 0.6883 0.2991 0.3183 0.031 Uiso 1 1 calc R . . H30B H 0.6318 0.2744 0.3436 0.031 Uiso 1 1 calc R . . C31 C 0.6812(2) 0.1661(3) 0.33156(16) 0.0316(11) Uani 1 1 d . . . H31A H 0.7096 0.1498 0.3085 0.038 Uiso 1 1 calc R . . H31B H 0.6991 0.1689 0.3624 0.038 Uiso 1 1 calc R . . C32 C 0.6374(2) 0.0969(4) 0.33235(16) 0.0326(12) Uani 1 1 d . . . H32A H 0.6112 0.1094 0.3578 0.039 Uiso 1 1 calc R . . H32B H 0.6544 0.0392 0.3384 0.039 Uiso 1 1 calc R . . C33 C 0.6065(2) 0.0938(3) 0.28635(16) 0.0281(10) Uani 1 1 d . . . H33A H 0.6317 0.0741 0.2615 0.034 Uiso 1 1 calc R . . H33B H 0.5761 0.0509 0.2886 0.034 Uiso 1 1 calc R . . C34 C 0.5831(2) 0.1833(3) 0.27380(15) 0.0257(10) Uani 1 1 d . . . H34A H 0.5553 0.2007 0.2971 0.031 Uiso 1 1 calc R . . H34B H 0.5648 0.1801 0.2432 0.031 Uiso 1 1 calc R . . C37 C 0.3688(3) 0.2145(6) 0.3446(2) 0.064(2) Uani 1 1 d . . . H37A H 0.3652 0.1500 0.3442 0.077 Uiso 1 1 calc R . . H37B H 0.3910 0.2305 0.3721 0.077 Uiso 1 1 calc R . . Cl5 Cl 0.40380(10) 0.24836(16) 0.29408(6) 0.0844(7) Uani 1 1 d . . . Cl6 Cl 0.30313(12) 0.26123(16) 0.35009(7) 0.0908(7) Uani 1 1 d . . . P2 P 0.73617(5) 0.46973(9) 0.41126(4) 0.0280(3) Uani 1 1 d . . . F1 F 0.67562(14) 0.5078(3) 0.41188(12) 0.0575(10) Uani 1 1 d . . . F2 F 0.71315(17) 0.3759(2) 0.39758(12) 0.0586(10) Uani 1 1 d . . . F3 F 0.74140(15) 0.4929(3) 0.35782(10) 0.0565(10) Uani 1 1 d . . . F4 F 0.76037(16) 0.5627(2) 0.42536(12) 0.0545(9) Uani 1 1 d . . . F5 F 0.73103(14) 0.4458(2) 0.46511(10) 0.0467(9) Uani 1 1 d . . . F6 F 0.79778(14) 0.4331(3) 0.41108(12) 0.0558(10) Uani 1 1 d . . . C35 C 0.4832(3) 0.2529(4) 0.45355(19) 0.0474(15) Uani 1 1 d . . . H35A H 0.5155 0.2856 0.4654 0.057 Uiso 1 1 calc R . . H35B H 0.4740 0.2068 0.4764 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.42711(8) 0.32488(11) 0.44763(6) 0.0570(4) Uani 1 1 d . . . Cl2 Cl 0.49977(8) 0.20440(13) 0.40047(5) 0.0638(5) Uani 1 1 d . . . C36 C 0.7023(3) 0.2351(4) 0.4760(2) 0.0470(15) Uani 1 1 d . . . H36A H 0.7261 0.1917 0.4604 0.056 Uiso 1 1 calc R . . H36B H 0.7171 0.2941 0.4692 0.056 Uiso 1 1 calc R . . Cl3 Cl 0.63448(7) 0.22685(11) 0.45368(6) 0.0559(4) Uani 1 1 d . . . Cl4 Cl 0.70405(9) 0.21704(12) 0.53609(6) 0.0643(5) 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 0.01898(18) 0.02578(19) 0.01326(16) 0.00145(13) -0.00034(12) -0.00056(13) S3 0.0202(6) 0.0372(6) 0.0157(5) 0.0046(5) 0.0004(4) -0.0013(5) S2 0.0233(6) 0.0400(7) 0.0196(5) 0.0004(5) 0.0011(4) -0.0067(5) S1 0.0301(7) 0.0371(7) 0.0204(5) -0.0051(5) -0.0078(5) 0.0109(5) P1 0.0185(6) 0.0263(6) 0.0149(5) -0.0005(4) -0.0013(4) 0.0013(5) N1 0.020(2) 0.027(2) 0.0144(16) 0.0028(15) 0.0017(14) -0.0016(16) N2 0.032(2) 0.027(2) 0.0189(18) -0.0004(16) 0.0004(16) 0.0007(18) N3 0.037(3) 0.039(2) 0.026(2) -0.0073(19) -0.0074(18) 0.014(2) N4 0.0181(18) 0.027(2) 0.0132(16) 0.0009(15) 0.0009(14) -0.0004(16) N5 0.031(2) 0.029(2) 0.0147(16) 0.0026(16) -0.0008(16) 0.0009(18) N6 0.026(2) 0.029(2) 0.0212(18) 0.0000(16) 0.0053(16) -0.0035(17) N7 0.021(2) 0.028(2) 0.0144(16) 0.0038(15) -0.0006(14) -0.0029(16) N8 0.022(2) 0.036(2) 0.0179(17) 0.0011(17) -0.0065(15) -0.0057(17) N9 0.021(2) 0.030(2) 0.0186(17) 0.0053(16) 0.0004(15) -0.0009(16) O1 0.047(2) 0.039(2) 0.0307(18) 0.0026(17) 0.0056(17) 0.0152(19) B1 0.021(3) 0.032(3) 0.013(2) 0.001(2) 0.0020(19) -0.002(2) C1 0.028(3) 0.033(3) 0.018(2) 0.000(2) -0.0005(19) 0.002(2) C2 0.022(2) 0.033(3) 0.021(2) -0.002(2) -0.0002(18) 0.000(2) C3 0.032(3) 0.035(3) 0.017(2) 0.000(2) -0.0012(19) -0.004(2) C4 0.052(4) 0.035(3) 0.027(2) -0.005(2) -0.006(2) 0.009(3) C5A 0.033(5) 0.035(7) 0.033(5) -0.009(5) -0.001(4) 0.006(5) C6A 0.036(7) 0.091(8) 0.038(5) 0.005(5) 0.004(4) 0.022(6) C5B 0.018(13) 0.015(8) 0.017(7) -0.004(6) -0.001(6) 0.000(7) C6B 0.034(10) 0.015(9) 0.039(9) 0.011(7) -0.019(7) 0.003(7) C7 0.024(2) 0.027(2) 0.021(2) 0.0030(19) 0.0038(18) -0.002(2) C8 0.022(2) 0.030(2) 0.016(2) 0.0008(19) 0.0039(17) 0.005(2) C9 0.035(3) 0.033(3) 0.019(2) 0.005(2) 0.0061(19) 0.002(2) C10 0.032(3) 0.045(3) 0.029(2) 0.004(2) 0.006(2) -0.012(2) C11 0.054(4) 0.043(3) 0.051(3) -0.001(3) 0.007(3) -0.017(3) C12 0.023(2) 0.023(2) 0.018(2) 0.0020(18) 0.0021(18) 0.0047(19) C13 0.025(3) 0.032(3) 0.020(2) 0.0018(19) -0.0007(18) -0.006(2) C14 0.029(3) 0.053(3) 0.028(2) 0.003(2) -0.006(2) -0.011(2) C15 0.022(2) 0.038(3) 0.024(2) 0.009(2) 0.0062(19) -0.003(2) C16 0.029(3) 0.055(4) 0.037(3) 0.010(3) 0.010(2) 0.010(3) C17 0.018(2) 0.034(3) 0.0172(19) -0.0024(19) -0.0031(17) 0.000(2) C18 0.023(2) 0.037(3) 0.021(2) -0.001(2) -0.0007(18) -0.002(2) C19 0.022(3) 0.044(3) 0.028(2) -0.001(2) 0.002(2) -0.002(2) C20 0.031(3) 0.044(3) 0.026(2) -0.001(2) 0.002(2) -0.010(2) C21 0.034(3) 0.035(3) 0.025(2) -0.004(2) -0.004(2) -0.004(2) C22 0.026(3) 0.030(3) 0.025(2) -0.002(2) -0.0017(19) 0.000(2) C23 0.023(2) 0.030(2) 0.018(2) -0.0030(19) 0.0004(18) 0.004(2) C24 0.030(3) 0.038(3) 0.021(2) -0.005(2) -0.0016(19) 0.008(2) C25 0.028(3) 0.042(3) 0.029(2) -0.003(2) 0.001(2) 0.009(2) C26 0.039(3) 0.041(3) 0.025(2) -0.006(2) 0.006(2) 0.009(2) C27 0.034(3) 0.040(3) 0.016(2) -0.002(2) 0.0011(19) 0.003(2) C28 0.025(2) 0.035(3) 0.023(2) -0.002(2) -0.0017(19) 0.003(2) C29 0.022(2) 0.027(2) 0.017(2) 0.0031(18) -0.0004(17) 0.0038(19) C30 0.023(2) 0.036(3) 0.018(2) 0.0014(19) -0.0050(18) 0.002(2) C31 0.032(3) 0.042(3) 0.022(2) 0.004(2) -0.005(2) 0.007(2) C32 0.032(3) 0.041(3) 0.025(2) 0.007(2) -0.003(2) 0.008(2) C33 0.027(3) 0.032(3) 0.025(2) 0.007(2) 0.001(2) 0.000(2) C34 0.024(2) 0.036(3) 0.017(2) 0.0036(19) -0.0015(18) 0.002(2) C37 0.075(5) 0.084(5) 0.034(3) 0.008(3) -0.012(3) -0.017(4) Cl5 0.1011(16) 0.1139(17) 0.0381(8) 0.0103(9) -0.0102(9) -0.0601(14) Cl6 0.125(2) 0.0916(16) 0.0561(11) 0.0029(11) 0.0001(12) 0.0414(14) P2 0.0273(7) 0.0361(7) 0.0208(5) 0.0000(5) -0.0026(5) -0.0058(5) F1 0.0371(19) 0.088(3) 0.0472(19) -0.004(2) -0.0082(16) 0.0105(19) F2 0.079(3) 0.051(2) 0.0457(19) -0.0031(17) -0.0189(19) -0.026(2) F3 0.050(2) 0.096(3) 0.0235(15) 0.0071(17) -0.0029(14) -0.023(2) F4 0.067(2) 0.048(2) 0.0481(19) 0.0040(17) -0.0070(18) -0.0218(18) F5 0.046(2) 0.071(2) 0.0233(14) 0.0039(15) -0.0063(13) -0.0203(17) F6 0.041(2) 0.079(3) 0.0480(19) -0.0176(19) -0.0077(16) 0.0147(18) C35 0.055(4) 0.057(4) 0.030(3) -0.011(3) -0.014(3) 0.014(3) Cl1 0.0769(12) 0.0479(9) 0.0462(8) 0.0007(7) 0.0021(8) 0.0265(8) Cl2 0.0793(12) 0.0785(12) 0.0335(7) -0.0069(8) -0.0018(7) 0.0352(10) C36 0.048(4) 0.048(4) 0.046(3) -0.003(3) 0.020(3) -0.011(3) Cl3 0.0469(9) 0.0541(9) 0.0669(10) -0.0093(8) 0.0218(8) -0.0105(7) Cl4 0.0892(14) 0.0591(10) 0.0447(8) -0.0029(8) 0.0183(8) -0.0164(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.892(5) . ? Rh1 B1 2.173(5) . ? Rh1 S3 2.3857(12) . ? Rh1 S2 2.3881(12) . ? Rh1 S1 2.4017(13) . ? Rh1 P1 2.5500(12) . ? S3 C12 1.713(5) . ? S2 C7 1.718(5) . ? S1 C2 1.705(5) . ? P1 C17 1.850(5) . ? P1 C29 1.863(5) . ? P1 C23 1.878(4) . ? N1 C2 1.314(6) . ? N1 N2 1.389(5) . ? N1 B1 1.548(7) . ? N2 C3 1.299(7) . ? N3 C2 1.358(6) . ? N3 C3 1.372(6) . ? N3 C5A 1.509(12) . ? N3 C5B 1.531(19) . ? N4 C7 1.320(6) . ? N4 N5 1.396(5) . ? N4 B1 1.548(6) . ? N5 C8 1.299(6) . ? N6 C7 1.350(6) . ? N6 C8 1.369(6) . ? N6 C10 1.470(6) . ? N7 C12 1.328(5) . ? N7 N8 1.391(5) . ? N7 B1 1.535(6) . ? N8 C13 1.297(6) . ? N9 C12 1.356(6) . ? N9 C13 1.384(6) . ? N9 C15 1.472(6) . ? O1 C1 1.101(6) . ? C3 C4 1.495(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5A C6A 1.507(15) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C5B C6B 1.55(2) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C8 C9 1.492(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.499(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.495(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.509(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.530(7) . ? C17 C18 1.532(6) . ? C17 H17 1.0000 . ? C18 C19 1.532(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.511(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.529(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.528(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.526(6) . ? C23 C28 1.546(6) . ? C23 H23 1.0000 . ? C24 C25 1.529(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.521(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.507(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.533(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.535(7) . ? C29 C30 1.536(6) . ? C29 H29 1.0000 . ? C30 C31 1.521(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.502(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.526(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.525(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C37 Cl6 1.757(9) . ? C37 Cl5 1.767(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? P2 F1 1.585(4) . ? P2 F3 1.587(3) . ? P2 F2 1.589(4) . ? P2 F4 1.591(4) . ? P2 F5 1.600(3) . ? P2 F6 1.601(4) . ? C35 Cl2 1.748(6) . ? C35 Cl1 1.762(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 Cl4 1.755(6) . ? C36 Cl3 1.777(7) . ? C36 H36A 0.9900 . ? C36 H36B 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 C1 Rh1 B1 87.0(2) . . ? C1 Rh1 S3 88.05(15) . . ? B1 Rh1 S3 84.00(14) . . ? C1 Rh1 S2 84.82(15) . . ? B1 Rh1 S2 83.75(14) . . ? S3 Rh1 S2 166.12(4) . . ? C1 Rh1 S1 172.87(14) . . ? B1 Rh1 S1 87.15(15) . . ? S3 Rh1 S1 95.44(5) . . ? S2 Rh1 S1 90.45(5) . . ? C1 Rh1 P1 98.66(14) . . ? B1 Rh1 P1 173.08(15) . . ? S3 Rh1 P1 92.23(4) . . ? S2 Rh1 P1 100.60(4) . . ? S1 Rh1 P1 87.43(4) . . ? C12 S3 Rh1 97.17(16) . . ? C7 S2 Rh1 96.80(16) . . ? C2 S1 Rh1 96.56(17) . . ? C17 P1 C29 103.8(2) . . ? C17 P1 C23 104.7(2) . . ? C29 P1 C23 103.6(2) . . ? C17 P1 Rh1 114.22(14) . . ? C29 P1 Rh1 111.00(15) . . ? C23 P1 Rh1 118.04(14) . . ? C2 N1 N2 110.9(4) . . ? C2 N1 B1 124.4(4) . . ? N2 N1 B1 124.6(4) . . ? C3 N2 N1 104.5(4) . . ? C2 N3 C3 106.2(4) . . ? C2 N3 C5A 124.1(5) . . ? C3 N3 C5A 127.9(5) . . ? C2 N3 C5B 122.6(6) . . ? C3 N3 C5B 125.5(6) . . ? C7 N4 N5 110.5(4) . . ? C7 N4 B1 118.4(4) . . ? N5 N4 B1 128.7(4) . . ? C8 N5 N4 104.4(4) . . ? C7 N6 C8 106.7(4) . . ? C7 N6 C10 125.7(4) . . ? C8 N6 C10 127.6(4) . . ? C12 N7 N8 110.5(4) . . ? C12 N7 B1 119.3(4) . . ? N8 N7 B1 128.1(3) . . ? C13 N8 N7 104.9(4) . . ? C12 N9 C13 106.1(4) . . ? C12 N9 C15 125.8(4) . . ? C13 N9 C15 128.0(4) . . ? N7 B1 N4 114.5(4) . . ? N7 B1 N1 109.0(4) . . ? N4 B1 N1 108.6(3) . . ? N7 B1 Rh1 109.0(3) . . ? N4 B1 Rh1 108.3(3) . . ? N1 B1 Rh1 107.3(3) . . ? O1 C1 Rh1 175.0(4) . . ? N1 C2 N3 107.0(4) . . ? N1 C2 S1 124.4(4) . . ? N3 C2 S1 128.6(4) . . ? N2 C3 N3 111.4(4) . . ? N2 C3 C4 124.4(4) . . ? N3 C3 C4 124.2(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6A C5A N3 106.7(10) . . ? C6A C5A H5A1 110.4 . . ? N3 C5A H5A1 110.4 . . ? C6A C5A H5A2 110.4 . . ? N3 C5A H5A2 110.4 . . ? H5A1 C5A H5A2 108.6 . . ? N3 C5B C6B 102.5(15) . . ? N3 C5B H5B1 111.3 . . ? C6B C5B H5B1 111.3 . . ? N3 C5B H5B2 111.3 . . ? C6B C5B H5B2 111.3 . . ? H5B1 C5B H5B2 109.2 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? N4 C7 N6 107.0(4) . . ? N4 C7 S2 124.4(3) . . ? N6 C7 S2 128.6(4) . . ? N5 C8 N6 111.4(4) . . ? N5 C8 C9 125.7(4) . . ? N6 C8 C9 122.9(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 111.5(5) . . ? N6 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N6 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 107.2(4) . . ? N7 C12 S3 124.1(4) . . ? N9 C12 S3 128.6(3) . . ? N8 C13 N9 111.4(4) . . ? N8 C13 C14 125.9(4) . . ? N9 C13 C14 122.7(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 111.3(4) . . ? N9 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N9 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 111.0(4) . . ? C22 C17 P1 110.8(3) . . ? C18 C17 P1 112.4(3) . . ? C22 C17 H17 107.5 . . ? C18 C17 H17 107.5 . . ? P1 C17 H17 107.5 . . ? C19 C18 C17 110.8(4) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 112.0(4) . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 110.4(4) . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 110.2(4) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C17 110.9(4) . . ? C21 C22 H22A 109.5 . . ? C17 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 110.4(4) . . ? C24 C23 P1 115.1(3) . . ? C28 C23 P1 114.2(3) . . ? C24 C23 H23 105.4 . . ? C28 C23 H23 105.4 . . ? P1 C23 H23 105.4 . . ? C23 C24 C25 111.0(4) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 112.0(4) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 111.4(4) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 111.8(4) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C23 110.4(4) . . ? C27 C28 H28A 109.6 . . ? C23 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C23 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C34 C29 C30 109.4(4) . . ? C34 C29 P1 112.6(3) . . ? C30 C29 P1 116.2(3) . . ? C34 C29 H29 105.9 . . ? C30 C29 H29 105.9 . . ? P1 C29 H29 105.9 . . ? C31 C30 C29 110.1(4) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? C32 C31 C30 112.0(4) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 111.1(4) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.2(4) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C29 110.6(4) . . ? C33 C34 H34A 109.5 . . ? C29 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? Cl6 C37 Cl5 113.2(4) . . ? Cl6 C37 H37A 108.9 . . ? Cl5 C37 H37A 108.9 . . ? Cl6 C37 H37B 108.9 . . ? Cl5 C37 H37B 108.9 . . ? H37A C37 H37B 107.8 . . ? F1 P2 F3 90.2(2) . . ? F1 P2 F2 90.4(2) . . ? F3 P2 F2 89.3(2) . . ? F1 P2 F4 90.7(2) . . ? F3 P2 F4 91.1(2) . . ? F2 P2 F4 178.8(2) . . ? F1 P2 F5 90.02(19) . . ? F3 P2 F5 179.7(3) . . ? F2 P2 F5 90.41(19) . . ? F4 P2 F5 89.16(19) . . ? F1 P2 F6 178.8(2) . . ? F3 P2 F6 90.0(2) . . ? F2 P2 F6 90.8(2) . . ? F4 P2 F6 88.1(2) . . ? F5 P2 F6 89.80(19) . . ? Cl2 C35 Cl1 111.0(3) . . ? Cl2 C35 H35A 109.4 . . ? Cl1 C35 H35A 109.4 . . ? Cl2 C35 H35B 109.4 . . ? Cl1 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? Cl4 C36 Cl3 111.7(3) . . ? Cl4 C36 H36A 109.3 . . ? Cl3 C36 H36A 109.3 . . ? Cl4 C36 H36B 109.3 . . ? Cl3 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 S3 C12 71.6(2) . . . . ? B1 Rh1 S3 C12 -15.6(2) . . . . ? S2 Rh1 S3 C12 12.6(3) . . . . ? S1 Rh1 S3 C12 -102.16(16) . . . . ? P1 Rh1 S3 C12 170.20(16) . . . . ? C1 Rh1 S2 C7 -70.2(2) . . . . ? B1 Rh1 S2 C7 17.3(2) . . . . ? S3 Rh1 S2 C7 -10.9(3) . . . . ? S1 Rh1 S2 C7 104.42(17) . . . . ? P1 Rh1 S2 C7 -168.11(17) . . . . ? B1 Rh1 S1 C2 1.2(2) . . . . ? S3 Rh1 S1 C2 84.90(17) . . . . ? S2 Rh1 S1 C2 -82.51(17) . . . . ? P1 Rh1 S1 C2 176.90(17) . . . . ? C1 Rh1 P1 C17 -82.3(2) . . . . ? S3 Rh1 P1 C17 -170.69(17) . . . . ? S2 Rh1 P1 C17 3.98(17) . . . . ? S1 Rh1 P1 C17 93.96(17) . . . . ? C1 Rh1 P1 C29 160.8(2) . . . . ? S3 Rh1 P1 C29 72.44(16) . . . . ? S2 Rh1 P1 C29 -112.88(16) . . . . ? S1 Rh1 P1 C29 -22.91(16) . . . . ? C1 Rh1 P1 C23 41.4(2) . . . . ? S3 Rh1 P1 C23 -46.94(18) . . . . ? S2 Rh1 P1 C23 127.73(18) . . . . ? S1 Rh1 P1 C23 -142.29(18) . . . . ? C2 N1 N2 C3 -1.1(5) . . . . ? B1 N1 N2 C3 176.6(4) . . . . ? C7 N4 N5 C8 -0.8(5) . . . . ? B1 N4 N5 C8 -163.1(4) . . . . ? C12 N7 N8 C13 0.6(5) . . . . ? B1 N7 N8 C13 163.5(5) . . . . ? C12 N7 B1 N4 -147.4(4) . . . . ? N8 N7 B1 N4 51.0(6) . . . . ? C12 N7 B1 N1 90.8(5) . . . . ? N8 N7 B1 N1 -70.8(5) . . . . ? C12 N7 B1 Rh1 -26.0(5) . . . . ? N8 N7 B1 Rh1 172.4(3) . . . . ? C7 N4 B1 N7 151.9(4) . . . . ? N5 N4 B1 N7 -47.0(6) . . . . ? C7 N4 B1 N1 -86.1(5) . . . . ? N5 N4 B1 N1 75.0(5) . . . . ? C7 N4 B1 Rh1 30.1(5) . . . . ? N5 N4 B1 Rh1 -168.8(3) . . . . ? C2 N1 B1 N7 -121.1(4) . . . . ? N2 N1 B1 N7 61.6(5) . . . . ? C2 N1 B1 N4 113.6(5) . . . . ? N2 N1 B1 N4 -63.7(5) . . . . ? C2 N1 B1 Rh1 -3.2(5) . . . . ? N2 N1 B1 Rh1 179.5(3) . . . . ? C1 Rh1 B1 N7 -65.7(3) . . . . ? S3 Rh1 B1 N7 22.7(3) . . . . ? S2 Rh1 B1 N7 -150.8(3) . . . . ? S1 Rh1 B1 N7 118.4(3) . . . . ? C1 Rh1 B1 N4 59.4(3) . . . . ? S3 Rh1 B1 N4 147.7(3) . . . . ? S2 Rh1 B1 N4 -25.7(3) . . . . ? S1 Rh1 B1 N4 -116.5(3) . . . . ? C1 Rh1 B1 N1 176.4(3) . . . . ? S3 Rh1 B1 N1 -95.2(3) . . . . ? S2 Rh1 B1 N1 91.3(3) . . . . ? S1 Rh1 B1 N1 0.6(3) . . . . ? N2 N1 C2 N3 0.8(5) . . . . ? B1 N1 C2 N3 -176.9(4) . . . . ? N2 N1 C2 S1 -177.2(3) . . . . ? B1 N1 C2 S1 5.1(7) . . . . ? C3 N3 C2 N1 -0.1(6) . . . . ? C5A N3 C2 N1 -166.0(7) . . . . ? C5B N3 C2 N1 154.4(9) . . . . ? C3 N3 C2 S1 177.7(4) . . . . ? C5A N3 C2 S1 11.9(9) . . . . ? C5B N3 C2 S1 -27.7(11) . . . . ? Rh1 S1 C2 N1 -3.6(4) . . . . ? Rh1 S1 C2 N3 178.8(5) . . . . ? N1 N2 C3 N3 1.0(5) . . . . ? N1 N2 C3 C4 -179.3(5) . . . . ? C2 N3 C3 N2 -0.6(6) . . . . ? C5A N3 C3 N2 164.6(7) . . . . ? C5B N3 C3 N2 -154.2(9) . . . . ? C2 N3 C3 C4 179.7(5) . . . . ? C5A N3 C3 C4 -15.1(10) . . . . ? C5B N3 C3 C4 26.1(12) . . . . ? C2 N3 C5A C6A -101.9(8) . . . . ? C3 N3 C5A C6A 95.3(9) . . . . ? C5B N3 C5A C6A -3.3(10) . . . . ? C2 N3 C5B C6B 102.6(10) . . . . ? C3 N3 C5B C6B -107.8(11) . . . . ? C5A N3 C5B C6B -1.1(8) . . . . ? N5 N4 C7 N6 0.1(5) . . . . ? B1 N4 C7 N6 164.5(4) . . . . ? N5 N4 C7 S2 -178.9(3) . . . . ? B1 N4 C7 S2 -14.6(6) . . . . ? C8 N6 C7 N4 0.5(5) . . . . ? C10 N6 C7 N4 -178.0(4) . . . . ? C8 N6 C7 S2 179.5(4) . . . . ? C10 N6 C7 S2 1.0(7) . . . . ? Rh1 S2 C7 N4 -7.1(4) . . . . ? Rh1 S2 C7 N6 174.0(4) . . . . ? N4 N5 C8 N6 1.2(5) . . . . ? N4 N5 C8 C9 -179.3(4) . . . . ? C7 N6 C8 N5 -1.1(5) . . . . ? C10 N6 C8 N5 177.4(5) . . . . ? C7 N6 C8 C9 179.3(4) . . . . ? C10 N6 C8 C9 -2.2(7) . . . . ? C7 N6 C10 C11 -87.9(6) . . . . ? C8 N6 C10 C11 93.8(6) . . . . ? N8 N7 C12 N9 -0.7(5) . . . . ? B1 N7 C12 N9 -165.3(4) . . . . ? N8 N7 C12 S3 176.3(3) . . . . ? B1 N7 C12 S3 11.7(6) . . . . ? C13 N9 C12 N7 0.5(5) . . . . ? C15 N9 C12 N7 -174.8(4) . . . . ? C13 N9 C12 S3 -176.4(4) . . . . ? C15 N9 C12 S3 8.3(7) . . . . ? Rh1 S3 C12 N7 7.3(4) . . . . ? Rh1 S3 C12 N9 -176.3(4) . . . . ? N7 N8 C13 N9 -0.3(5) . . . . ? N7 N8 C13 C14 179.0(5) . . . . ? C12 N9 C13 N8 -0.2(6) . . . . ? C15 N9 C13 N8 175.1(4) . . . . ? C12 N9 C13 C14 -179.5(5) . . . . ? C15 N9 C13 C14 -4.3(8) . . . . ? C12 N9 C15 C16 87.1(6) . . . . ? C13 N9 C15 C16 -87.3(6) . . . . ? C29 P1 C17 C22 -178.2(3) . . . . ? C23 P1 C17 C22 -69.8(3) . . . . ? Rh1 P1 C17 C22 60.8(3) . . . . ? C29 P1 C17 C18 57.0(4) . . . . ? C23 P1 C17 C18 165.4(3) . . . . ? Rh1 P1 C17 C18 -63.9(3) . . . . ? C22 C17 C18 C19 54.2(5) . . . . ? P1 C17 C18 C19 178.9(3) . . . . ? C17 C18 C19 C20 -55.1(5) . . . . ? C18 C19 C20 C21 56.9(5) . . . . ? C19 C20 C21 C22 -58.0(5) . . . . ? C20 C21 C22 C17 57.9(5) . . . . ? C18 C17 C22 C21 -56.3(5) . . . . ? P1 C17 C22 C21 178.2(3) . . . . ? C17 P1 C23 C24 102.8(4) . . . . ? C29 P1 C23 C24 -148.8(4) . . . . ? Rh1 P1 C23 C24 -25.6(4) . . . . ? C17 P1 C23 C28 -26.4(4) . . . . ? C29 P1 C23 C28 82.1(4) . . . . ? Rh1 P1 C23 C28 -154.7(3) . . . . ? C28 C23 C24 C25 -56.0(6) . . . . ? P1 C23 C24 C25 173.0(4) . . . . ? C23 C24 C25 C26 55.2(6) . . . . ? C24 C25 C26 C27 -54.5(6) . . . . ? C25 C26 C27 C28 55.1(6) . . . . ? C26 C27 C28 C23 -56.3(6) . . . . ? C24 C23 C28 C27 56.4(5) . . . . ? P1 C23 C28 C27 -172.2(3) . . . . ? C17 P1 C29 C34 177.6(3) . . . . ? C23 P1 C29 C34 68.4(3) . . . . ? Rh1 P1 C29 C34 -59.3(3) . . . . ? C17 P1 C29 C30 50.2(4) . . . . ? C23 P1 C29 C30 -59.0(4) . . . . ? Rh1 P1 C29 C30 173.3(3) . . . . ? C34 C29 C30 C31 58.0(5) . . . . ? P1 C29 C30 C31 -173.1(3) . . . . ? C29 C30 C31 C32 -57.5(5) . . . . ? C30 C31 C32 C33 55.6(6) . . . . ? C31 C32 C33 C34 -54.9(6) . . . . ? C32 C33 C34 C29 56.5(5) . . . . ? C30 C29 C34 C33 -58.0(5) . . . . ? P1 C29 C34 C33 171.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 70.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.615 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.110 data_12+ _database_code_depnum_ccdc_archive 'CCDC 733507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H42 B N12 O P Rh S3, F6 P' _chemical_formula_sum 'C22 H42 B F6 N12 O P2 Rh S3' _chemical_formula_weight 876.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.254(4) _cell_length_b 13.158(3) _cell_length_c 13.214(13) _cell_angle_alpha 113.91(2) _cell_angle_beta 90.917(19) _cell_angle_gamma 95.449(16) _cell_volume 1777.5(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 315 _cell_measurement_theta_min 2.352 _cell_measurement_theta_max 27.482 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details 'SADABS V2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20527 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8130 _reflns_number_gt 7531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.628 (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART V5.628 (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT V6.41 (Bruker, 2003)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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^)+(0.0427P)^2^+1.1213P] 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 8130 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 Rh1 Rh 0.670896(14) 0.704465(13) 0.735418(12) 0.01011(6) Uani 1 1 d . . . S1 S 0.73056(5) 0.58489(5) 0.55523(4) 0.01588(11) Uani 1 1 d . . . S2 S 0.47980(5) 0.60020(5) 0.70380(4) 0.01556(11) Uani 1 1 d . . . S3 S 0.86308(5) 0.80452(5) 0.80585(4) 0.01514(11) Uani 1 1 d . . . P1 P 0.60564(5) 0.84383(5) 0.66988(4) 0.01214(11) Uani 1 1 d . . . P2 P 0.15116(6) 0.07986(5) 0.73003(5) 0.02040(13) Uani 1 1 d . . . O1 O 0.59975(16) 0.82144(14) 0.96747(13) 0.0227(4) Uani 1 1 d . . . N1 N 0.78648(16) 0.49185(15) 0.69408(15) 0.0126(3) Uani 1 1 d . . . N2 N 0.83818(17) 0.40184(15) 0.69846(16) 0.0163(4) Uani 1 1 d . . . N3 N 0.82575(17) 0.38971(15) 0.52583(15) 0.0153(4) Uani 1 1 d . . . N4 N 0.62007(16) 0.52738(15) 0.82354(15) 0.0132(4) Uani 1 1 d . . . N5 N 0.61592(18) 0.45163(16) 0.87314(15) 0.0165(4) Uani 1 1 d . . . N6 N 0.43684(17) 0.45118(16) 0.80032(15) 0.0159(4) Uani 1 1 d . . . N7 N 0.82980(16) 0.64426(15) 0.88505(15) 0.0129(4) Uani 1 1 d . . . N8 N 0.88321(17) 0.60550(15) 0.95636(15) 0.0154(4) Uani 1 1 d . . . N9 N 0.98684(17) 0.76018(16) 0.96322(15) 0.0150(4) Uani 1 1 d . . . N10 N 0.71817(17) 0.91639(16) 0.63900(17) 0.0183(4) Uani 1 1 d . . . N11 N 0.54357(17) 0.95044(16) 0.76747(15) 0.0164(4) Uani 1 1 d . . . N12 N 0.49023(17) 0.79611(16) 0.57308(15) 0.0168(4) Uani 1 1 d . . . F1 F 0.01683(14) 0.06770(13) 0.76547(13) 0.0316(4) Uani 1 1 d . . . F2 F 0.10269(15) 0.03898(14) 0.60457(12) 0.0319(4) Uani 1 1 d . . . F3 F 0.28563(14) 0.09381(15) 0.69530(15) 0.0411(4) Uani 1 1 d . . . F4 F 0.16285(16) -0.04710(13) 0.70957(13) 0.0350(4) Uani 1 1 d . . . F5 F 0.13875(15) 0.20686(13) 0.75023(15) 0.0378(4) Uani 1 1 d . . . F6 F 0.19869(17) 0.12081(16) 0.85629(14) 0.0443(5) Uani 1 1 d . . . B1 B 0.7319(2) 0.5832(2) 0.79207(19) 0.0124(4) Uani 1 1 d . . . C1 C 0.6261(2) 0.78029(18) 0.88008(19) 0.0160(4) Uani 1 1 d . . . C2 C 0.78138(19) 0.48550(18) 0.59113(18) 0.0143(4) Uani 1 1 d . . . C3 C 0.8619(2) 0.34189(19) 0.59563(19) 0.0172(4) Uani 1 1 d . . . C4 C 0.9228(2) 0.2391(2) 0.5585(2) 0.0242(5) Uani 1 1 d . . . H4A H 0.9437 0.2234 0.6227 0.036 Uiso 1 1 calc R . . H4B H 0.9957 0.2496 0.5227 0.036 Uiso 1 1 calc R . . H4C H 0.8693 0.1761 0.5056 0.036 Uiso 1 1 calc R . . C5 C 0.8256(2) 0.3443(2) 0.40393(18) 0.0182(5) Uani 1 1 d . . . H5A H 0.7475 0.3521 0.3739 0.022 Uiso 1 1 calc R . . H5B H 0.8352 0.2635 0.3748 0.022 Uiso 1 1 calc R . . C6 C 0.9244(2) 0.4029(2) 0.3642(2) 0.0252(5) Uani 1 1 d . . . H6A H 0.9185 0.4836 0.3968 0.038 Uiso 1 1 calc R . . H6B H 0.9164 0.3745 0.2831 0.038 Uiso 1 1 calc R . . H6C H 1.0022 0.3886 0.3868 0.038 Uiso 1 1 calc R . . C7 C 0.51213(19) 0.52555(18) 0.77871(17) 0.0134(4) Uani 1 1 d . . . C8 C 0.5048(2) 0.40802(18) 0.85807(18) 0.0165(4) Uani 1 1 d . . . C9 C 0.4551(2) 0.3223(2) 0.8970(2) 0.0229(5) Uani 1 1 d . . . H9A H 0.4332 0.2512 0.8330 0.034 Uiso 1 1 calc R . . H9B H 0.3839 0.3469 0.9380 0.034 Uiso 1 1 calc R . . H9C H 0.5153 0.3124 0.9456 0.034 Uiso 1 1 calc R . . C10 C 0.3079(2) 0.4246(2) 0.7677(2) 0.0229(5) Uani 1 1 d . . . H10A H 0.2817 0.3475 0.7594 0.027 Uiso 1 1 calc R . . H10B H 0.2935 0.4279 0.6950 0.027 Uiso 1 1 calc R . . C11 C 0.2347(2) 0.5056(3) 0.8529(2) 0.0303(6) Uani 1 1 d . . . H11A H 0.2441 0.4985 0.9236 0.045 Uiso 1 1 calc R . . H11B H 0.1502 0.4883 0.8268 0.045 Uiso 1 1 calc R . . H11C H 0.2625 0.5823 0.8634 0.045 Uiso 1 1 calc R . . C12 C 0.89372(19) 0.73599(18) 0.88833(17) 0.0136(4) Uani 1 1 d . . . C13 C 0.9766(2) 0.67754(18) 1.00277(18) 0.0155(4) Uani 1 1 d . . . C14 C 1.0631(2) 0.6730(2) 1.08718(19) 0.0199(5) Uani 1 1 d . . . H14A H 1.0561 0.7357 1.1586 0.030 Uiso 1 1 calc R . . H14B H 1.1446 0.6780 1.0633 0.030 Uiso 1 1 calc R . . H14C H 1.0453 0.6023 1.0951 0.030 Uiso 1 1 calc R . . C15 C 1.0727(2) 0.8614(2) 1.00007(19) 0.0199(5) Uani 1 1 d . . . H15A H 1.1168 0.8703 1.0691 0.024 Uiso 1 1 calc R . . H15B H 1.0283 0.9273 1.0173 0.024 Uiso 1 1 calc R . . C16 C 1.1613(2) 0.8583(3) 0.9145(2) 0.0318(6) Uani 1 1 d . . . H16A H 1.2106 0.7972 0.9019 0.048 Uiso 1 1 calc R . . H16B H 1.2127 0.9295 0.9411 0.048 Uiso 1 1 calc R . . H16C H 1.1181 0.8461 0.8448 0.048 Uiso 1 1 calc R . . C17 C 0.8168(2) 0.8599(2) 0.5781(2) 0.0204(5) Uani 1 1 d . . . H17A H 0.8001 0.8375 0.4985 0.031 Uiso 1 1 calc R . . H17B H 0.8256 0.7934 0.5924 0.031 Uiso 1 1 calc R . . H17C H 0.8910 0.9109 0.6026 0.031 Uiso 1 1 calc R . . C18 C 0.7068(2) 1.0201(2) 0.6260(2) 0.0275(6) Uani 1 1 d . . . H18A H 0.7778 1.0733 0.6609 0.041 Uiso 1 1 calc R . . H18B H 0.6354 1.0523 0.6615 0.041 Uiso 1 1 calc R . . H18C H 0.6997 1.0044 0.5469 0.041 Uiso 1 1 calc R . . C19 C 0.6214(2) 1.0296(2) 0.8605(2) 0.0228(5) Uani 1 1 d . . . H19A H 0.5887 1.1018 0.8906 0.034 Uiso 1 1 calc R . . H19B H 0.7013 1.0393 0.8352 0.034 Uiso 1 1 calc R . . H19C H 0.6264 1.0012 0.9182 0.034 Uiso 1 1 calc R . . C20 C 0.4261(2) 0.9250(2) 0.8029(2) 0.0215(5) Uani 1 1 d . . . H20A H 0.4353 0.8894 0.8544 0.032 Uiso 1 1 calc R . . H20B H 0.3749 0.8742 0.7380 0.032 Uiso 1 1 calc R . . H20C H 0.3894 0.9944 0.8400 0.032 Uiso 1 1 calc R . . C21 C 0.4377(2) 0.8745(2) 0.5366(2) 0.0241(5) Uani 1 1 d . . . H21A H 0.4865 0.8860 0.4805 0.036 Uiso 1 1 calc R . . H21B H 0.4353 0.9462 0.6002 0.036 Uiso 1 1 calc R . . H21C H 0.3563 0.8437 0.5046 0.036 Uiso 1 1 calc R . . C22 C 0.4970(2) 0.68936(19) 0.47945(19) 0.0200(5) Uani 1 1 d . . . H22A H 0.4198 0.6645 0.4368 0.030 Uiso 1 1 calc R . . H22B H 0.5163 0.6336 0.5068 0.030 Uiso 1 1 calc R . . H22C H 0.5593 0.6982 0.4318 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01106(9) 0.00988(9) 0.00944(9) 0.00401(6) -0.00008(6) 0.00120(6) S1 0.0206(3) 0.0166(3) 0.0116(2) 0.0060(2) 0.0027(2) 0.0067(2) S2 0.0133(3) 0.0178(3) 0.0170(2) 0.0091(2) -0.00208(19) -0.0006(2) S3 0.0139(3) 0.0167(3) 0.0170(3) 0.0099(2) -0.0019(2) -0.0014(2) P1 0.0121(3) 0.0122(3) 0.0127(2) 0.0056(2) 0.0005(2) 0.0019(2) P2 0.0205(3) 0.0164(3) 0.0211(3) 0.0047(2) 0.0007(2) 0.0014(2) O1 0.0280(9) 0.0227(9) 0.0164(8) 0.0060(7) 0.0059(7) 0.0062(7) N1 0.0130(9) 0.0116(8) 0.0138(8) 0.0055(7) 0.0012(7) 0.0023(7) N2 0.0177(9) 0.0125(9) 0.0195(9) 0.0067(7) 0.0025(7) 0.0048(7) N3 0.0158(9) 0.0140(9) 0.0150(9) 0.0045(7) 0.0032(7) 0.0034(7) N4 0.0147(9) 0.0127(9) 0.0127(8) 0.0059(7) 0.0013(7) 0.0011(7) N5 0.0210(10) 0.0139(9) 0.0167(9) 0.0085(7) 0.0028(7) 0.0010(7) N6 0.0167(9) 0.0146(9) 0.0147(9) 0.0050(7) 0.0022(7) -0.0011(7) N7 0.0149(9) 0.0123(8) 0.0126(8) 0.0059(7) -0.0003(7) 0.0026(7) N8 0.0189(9) 0.0140(9) 0.0144(9) 0.0068(7) -0.0024(7) 0.0034(7) N9 0.0150(9) 0.0150(9) 0.0144(9) 0.0057(7) -0.0012(7) 0.0007(7) N10 0.0171(9) 0.0176(10) 0.0254(10) 0.0134(8) 0.0048(8) 0.0036(8) N11 0.0152(9) 0.0148(9) 0.0161(9) 0.0031(7) -0.0004(7) 0.0025(7) N12 0.0191(9) 0.0158(9) 0.0141(9) 0.0042(7) -0.0031(7) 0.0049(7) F1 0.0265(8) 0.0291(8) 0.0341(8) 0.0085(7) 0.0084(7) -0.0017(6) F2 0.0381(9) 0.0358(9) 0.0241(8) 0.0157(7) -0.0020(7) -0.0009(7) F3 0.0216(8) 0.0378(10) 0.0478(10) 0.0011(8) 0.0092(7) 0.0021(7) F4 0.0487(10) 0.0223(8) 0.0349(9) 0.0116(7) -0.0022(8) 0.0093(7) F5 0.0335(9) 0.0178(8) 0.0590(11) 0.0126(8) 0.0097(8) 0.0023(7) F6 0.0458(11) 0.0487(11) 0.0243(8) 0.0007(8) -0.0106(7) 0.0063(9) B1 0.0135(11) 0.0121(11) 0.0117(10) 0.0049(9) 0.0011(9) 0.0018(9) C1 0.0140(10) 0.0135(10) 0.0222(11) 0.0094(9) -0.0020(8) 0.0006(8) C2 0.0121(10) 0.0155(10) 0.0140(10) 0.0050(8) 0.0017(8) -0.0001(8) C3 0.0169(11) 0.0158(11) 0.0186(11) 0.0067(9) 0.0014(8) 0.0005(8) C4 0.0289(13) 0.0200(12) 0.0240(12) 0.0072(10) 0.0057(10) 0.0122(10) C5 0.0189(11) 0.0189(11) 0.0128(10) 0.0021(8) -0.0004(8) 0.0037(9) C6 0.0267(13) 0.0273(13) 0.0185(11) 0.0065(10) 0.0047(10) 0.0010(10) C7 0.0140(10) 0.0134(10) 0.0110(9) 0.0033(8) 0.0016(8) -0.0003(8) C8 0.0208(11) 0.0125(10) 0.0144(10) 0.0043(8) 0.0029(8) -0.0006(8) C9 0.0292(13) 0.0175(11) 0.0240(12) 0.0115(10) 0.0043(10) -0.0027(10) C10 0.0151(11) 0.0266(13) 0.0266(12) 0.0123(10) 0.0001(9) -0.0052(9) C11 0.0223(13) 0.0457(17) 0.0299(13) 0.0213(12) 0.0074(10) 0.0082(12) C12 0.0140(10) 0.0134(10) 0.0125(9) 0.0040(8) 0.0015(8) 0.0025(8) C13 0.0168(11) 0.0159(10) 0.0134(10) 0.0048(8) 0.0012(8) 0.0047(8) C14 0.0209(12) 0.0207(11) 0.0177(11) 0.0072(9) -0.0045(9) 0.0040(9) C15 0.0172(11) 0.0186(11) 0.0207(11) 0.0066(9) -0.0059(9) -0.0054(9) C16 0.0223(13) 0.0434(17) 0.0270(13) 0.0152(12) -0.0032(10) -0.0129(12) C17 0.0179(11) 0.0224(12) 0.0231(11) 0.0113(10) 0.0053(9) 0.0030(9) C18 0.0251(13) 0.0239(13) 0.0445(16) 0.0243(12) 0.0096(11) 0.0057(10) C19 0.0244(12) 0.0190(12) 0.0197(11) 0.0025(9) -0.0028(9) 0.0022(10) C20 0.0192(12) 0.0234(12) 0.0209(11) 0.0073(10) 0.0051(9) 0.0048(9) C21 0.0263(13) 0.0224(12) 0.0243(12) 0.0100(10) -0.0086(10) 0.0052(10) C22 0.0201(11) 0.0186(11) 0.0174(11) 0.0034(9) -0.0034(9) 0.0033(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.867(3) . ? Rh1 B1 2.176(2) . ? Rh1 S2 2.3723(9) . ? Rh1 S3 2.3830(10) . ? Rh1 S1 2.4105(19) . ? Rh1 P1 2.4849(9) . ? S1 C2 1.702(2) . ? S2 C7 1.709(2) . ? S3 C12 1.721(2) . ? P1 N10 1.669(2) . ? P1 N12 1.691(2) . ? P1 N11 1.693(2) . ? P2 F2 1.590(2) . ? P2 F6 1.596(2) . ? P2 F4 1.5994(17) . ? P2 F5 1.6021(17) . ? P2 F1 1.6025(17) . ? P2 F3 1.6038(18) . ? O1 C1 1.118(3) . ? N1 C2 1.329(3) . ? N1 N2 1.389(2) . ? N1 B1 1.550(3) . ? N2 C3 1.312(3) . ? N3 C2 1.354(3) . ? N3 C3 1.385(3) . ? N3 C5 1.473(3) . ? N4 C7 1.337(3) . ? N4 N5 1.395(3) . ? N4 B1 1.545(3) . ? N5 C8 1.303(3) . ? N6 C7 1.354(3) . ? N6 C8 1.380(3) . ? N6 C10 1.475(3) . ? N7 C12 1.330(3) . ? N7 N8 1.392(3) . ? N7 B1 1.535(3) . ? N8 C13 1.303(3) . ? N9 C12 1.352(3) . ? N9 C13 1.381(3) . ? N9 C15 1.469(3) . ? N10 C18 1.460(3) . ? N10 C17 1.460(3) . ? N11 C19 1.455(3) . ? N11 C20 1.464(3) . ? N12 C22 1.457(3) . ? N12 C21 1.468(3) . ? C3 C4 1.480(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.514(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.486(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.519(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.492(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.511(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 B1 86.19(10) . . ? C1 Rh1 S2 85.47(7) . . ? B1 Rh1 S2 86.24(7) . . ? C1 Rh1 S3 84.78(8) . . ? B1 Rh1 S3 84.58(7) . . ? S2 Rh1 S3 167.01(2) . . ? C1 Rh1 S1 172.09(7) . . ? B1 Rh1 S1 86.19(8) . . ? S2 Rh1 S1 91.93(3) . . ? S3 Rh1 S1 96.59(4) . . ? C1 Rh1 P1 94.36(8) . . ? B1 Rh1 P1 178.79(7) . . ? S2 Rh1 P1 94.88(3) . . ? S3 Rh1 P1 94.40(3) . . ? S1 Rh1 P1 93.29(6) . . ? C2 S1 Rh1 97.54(9) . . ? C7 S2 Rh1 95.93(8) . . ? C12 S3 Rh1 96.03(8) . . ? N10 P1 N12 113.40(11) . . ? N10 P1 N11 99.67(10) . . ? N12 P1 N11 98.51(10) . . ? N10 P1 Rh1 113.77(7) . . ? N12 P1 Rh1 115.22(8) . . ? N11 P1 Rh1 114.24(9) . . ? F2 P2 F6 179.51(11) . . ? F2 P2 F4 89.67(9) . . ? F6 P2 F4 90.34(10) . . ? F2 P2 F5 90.14(10) . . ? F6 P2 F5 89.86(10) . . ? F4 P2 F5 179.70(11) . . ? F2 P2 F1 89.83(10) . . ? F6 P2 F1 89.68(11) . . ? F4 P2 F1 90.09(9) . . ? F5 P2 F1 89.69(9) . . ? F2 P2 F3 90.39(10) . . ? F6 P2 F3 90.10(11) . . ? F4 P2 F3 90.64(10) . . ? F5 P2 F3 89.59(10) . . ? F1 P2 F3 179.24(10) . . ? C2 N1 N2 110.73(17) . . ? C2 N1 B1 123.28(18) . . ? N2 N1 B1 125.82(18) . . ? C3 N2 N1 104.73(18) . . ? C2 N3 C3 106.36(19) . . ? C2 N3 C5 125.24(19) . . ? C3 N3 C5 128.26(19) . . ? C7 N4 N5 110.17(18) . . ? C7 N4 B1 120.13(18) . . ? N5 N4 B1 127.70(18) . . ? C8 N5 N4 104.79(18) . . ? C7 N6 C8 106.37(18) . . ? C7 N6 C10 125.35(19) . . ? C8 N6 C10 128.28(19) . . ? C12 N7 N8 110.21(17) . . ? C12 N7 B1 119.45(18) . . ? N8 N7 B1 128.71(18) . . ? C13 N8 N7 104.87(18) . . ? C12 N9 C13 106.29(18) . . ? C12 N9 C15 124.89(19) . . ? C13 N9 C15 128.58(19) . . ? C18 N10 C17 111.33(19) . . ? C18 N10 P1 123.76(17) . . ? C17 N10 P1 120.20(16) . . ? C19 N11 C20 111.6(2) . . ? C19 N11 P1 117.57(16) . . ? C20 N11 P1 117.73(16) . . ? C22 N12 C21 110.56(19) . . ? C22 N12 P1 117.30(15) . . ? C21 N12 P1 119.40(16) . . ? N7 B1 N4 116.14(18) . . ? N7 B1 N1 108.88(18) . . ? N4 B1 N1 108.04(17) . . ? N7 B1 Rh1 108.03(14) . . ? N4 B1 Rh1 106.92(14) . . ? N1 B1 Rh1 108.61(15) . . ? O1 C1 Rh1 176.8(2) . . ? N1 C2 N3 107.24(19) . . ? N1 C2 S1 123.96(17) . . ? N3 C2 S1 128.78(18) . . ? N2 C3 N3 110.9(2) . . ? N2 C3 C4 125.1(2) . . ? N3 C3 C4 123.9(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 112.43(19) . . ? N3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 107.17(19) . . ? N4 C7 S2 125.31(17) . . ? N6 C7 S2 127.48(17) . . ? N5 C8 N6 111.50(19) . . ? N5 C8 C9 125.2(2) . . ? N6 C8 C9 123.3(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 111.6(2) . . ? N6 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N6 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 107.39(18) . . ? N7 C12 S3 124.64(16) . . ? N9 C12 S3 127.91(17) . . ? N8 C13 N9 111.21(19) . . ? N8 C13 C14 125.4(2) . . ? N9 C13 C14 123.4(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 112.9(2) . . ? N9 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N9 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N10 C17 H17A 109.5 . . ? N10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C18 H18A 109.5 . . ? N10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N11 C19 H19A 109.5 . . ? N11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N11 C20 H20A 109.5 . . ? N11 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N11 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N12 C21 H21A 109.5 . . ? N12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N12 C22 H22A 109.5 . . ? N12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 Rh1 S1 C2 -0.27(10) . . . . ? S2 Rh1 S1 C2 -86.37(8) . . . . ? S3 Rh1 S1 C2 83.82(8) . . . . ? P1 Rh1 S1 C2 178.63(8) . . . . ? C1 Rh1 S2 C7 -71.98(11) . . . . ? B1 Rh1 S2 C7 14.50(10) . . . . ? S3 Rh1 S2 C7 -30.54(13) . . . . ? S1 Rh1 S2 C7 100.55(10) . . . . ? P1 Rh1 S2 C7 -165.98(7) . . . . ? C1 Rh1 S3 C12 68.64(11) . . . . ? B1 Rh1 S3 C12 -18.02(10) . . . . ? S2 Rh1 S3 C12 27.14(13) . . . . ? S1 Rh1 S3 C12 -103.54(9) . . . . ? P1 Rh1 S3 C12 162.63(7) . . . . ? C1 Rh1 P1 N10 111.93(11) . . . . ? S2 Rh1 P1 N10 -162.25(8) . . . . ? S3 Rh1 P1 N10 26.85(9) . . . . ? S1 Rh1 P1 N10 -70.03(8) . . . . ? C1 Rh1 P1 N12 -114.66(11) . . . . ? S2 Rh1 P1 N12 -28.85(8) . . . . ? S3 Rh1 P1 N12 160.25(8) . . . . ? S1 Rh1 P1 N12 63.37(9) . . . . ? C1 Rh1 P1 N11 -1.62(10) . . . . ? S2 Rh1 P1 N11 84.20(8) . . . . ? S3 Rh1 P1 N11 -86.70(8) . . . . ? S1 Rh1 P1 N11 176.42(8) . . . . ? C2 N1 N2 C3 -0.7(2) . . . . ? B1 N1 N2 C3 174.56(19) . . . . ? C7 N4 N5 C8 -1.1(2) . . . . ? B1 N4 N5 C8 -164.8(2) . . . . ? C12 N7 N8 C13 1.7(2) . . . . ? B1 N7 N8 C13 166.8(2) . . . . ? N12 P1 N10 C18 61.7(2) . . . . ? N11 P1 N10 C18 -42.0(2) . . . . ? Rh1 P1 N10 C18 -164.01(18) . . . . ? N12 P1 N10 C17 -91.83(19) . . . . ? N11 P1 N10 C17 164.44(17) . . . . ? Rh1 P1 N10 C17 42.4(2) . . . . ? N10 P1 N11 C19 -53.43(19) . . . . ? N12 P1 N11 C19 -169.08(18) . . . . ? Rh1 P1 N11 C19 68.25(19) . . . . ? N10 P1 N11 C20 168.54(17) . . . . ? N12 P1 N11 C20 52.88(18) . . . . ? Rh1 P1 N11 C20 -69.79(17) . . . . ? N10 P1 N12 C22 86.04(19) . . . . ? N11 P1 N12 C22 -169.49(17) . . . . ? Rh1 P1 N12 C22 -47.53(19) . . . . ? N10 P1 N12 C21 -52.1(2) . . . . ? N11 P1 N12 C21 52.4(2) . . . . ? Rh1 P1 N12 C21 174.35(16) . . . . ? C12 N7 B1 N4 -145.9(2) . . . . ? N8 N7 B1 N4 50.2(3) . . . . ? C12 N7 B1 N1 91.9(2) . . . . ? N8 N7 B1 N1 -72.0(3) . . . . ? C12 N7 B1 Rh1 -25.8(2) . . . . ? N8 N7 B1 Rh1 170.22(17) . . . . ? C7 N4 B1 N7 144.5(2) . . . . ? N5 N4 B1 N7 -53.2(3) . . . . ? C7 N4 B1 N1 -92.9(2) . . . . ? N5 N4 B1 N1 69.4(3) . . . . ? C7 N4 B1 Rh1 23.9(2) . . . . ? N5 N4 B1 Rh1 -173.87(16) . . . . ? C2 N1 B1 N7 -124.6(2) . . . . ? N2 N1 B1 N7 60.6(3) . . . . ? C2 N1 B1 N4 108.4(2) . . . . ? N2 N1 B1 N4 -66.3(2) . . . . ? C2 N1 B1 Rh1 -7.2(2) . . . . ? N2 N1 B1 Rh1 178.02(16) . . . . ? C1 Rh1 B1 N7 -60.80(15) . . . . ? S2 Rh1 B1 N7 -146.50(14) . . . . ? S3 Rh1 B1 N7 24.31(13) . . . . ? S1 Rh1 B1 N7 121.31(14) . . . . ? C1 Rh1 B1 N4 64.89(15) . . . . ? S2 Rh1 B1 N4 -20.81(13) . . . . ? S3 Rh1 B1 N4 150.00(14) . . . . ? S1 Rh1 B1 N4 -113.00(13) . . . . ? C1 Rh1 B1 N1 -178.75(15) . . . . ? S2 Rh1 B1 N1 95.55(14) . . . . ? S3 Rh1 B1 N1 -93.64(14) . . . . ? S1 Rh1 B1 N1 3.37(13) . . . . ? N2 N1 C2 N3 2.0(2) . . . . ? B1 N1 C2 N3 -173.45(18) . . . . ? N2 N1 C2 S1 -176.54(15) . . . . ? B1 N1 C2 S1 8.0(3) . . . . ? C3 N3 C2 N1 -2.4(2) . . . . ? C5 N3 C2 N1 173.56(19) . . . . ? C3 N3 C2 S1 176.06(18) . . . . ? C5 N3 C2 S1 -8.0(3) . . . . ? Rh1 S1 C2 N1 -3.9(2) . . . . ? Rh1 S1 C2 N3 177.92(19) . . . . ? N1 N2 C3 N3 -0.8(2) . . . . ? N1 N2 C3 C4 177.2(2) . . . . ? C2 N3 C3 N2 2.0(3) . . . . ? C5 N3 C3 N2 -173.8(2) . . . . ? C2 N3 C3 C4 -176.1(2) . . . . ? C5 N3 C3 C4 8.2(4) . . . . ? C2 N3 C5 C6 78.9(3) . . . . ? C3 N3 C5 C6 -106.1(3) . . . . ? N5 N4 C7 N6 1.2(2) . . . . ? B1 N4 C7 N6 166.35(18) . . . . ? N5 N4 C7 S2 -176.42(15) . . . . ? B1 N4 C7 S2 -11.3(3) . . . . ? C8 N6 C7 N4 -0.9(2) . . . . ? C10 N6 C7 N4 178.7(2) . . . . ? C8 N6 C7 S2 176.69(17) . . . . ? C10 N6 C7 S2 -3.7(3) . . . . ? Rh1 S2 C7 N4 -6.6(2) . . . . ? Rh1 S2 C7 N6 176.28(19) . . . . ? N4 N5 C8 N6 0.5(2) . . . . ? N4 N5 C8 C9 -179.7(2) . . . . ? C7 N6 C8 N5 0.2(3) . . . . ? C10 N6 C8 N5 -179.4(2) . . . . ? C7 N6 C8 C9 -179.6(2) . . . . ? C10 N6 C8 C9 0.8(4) . . . . ? C7 N6 C10 C11 -86.0(3) . . . . ? C8 N6 C10 C11 93.5(3) . . . . ? N8 N7 C12 N9 -1.7(2) . . . . ? B1 N7 C12 N9 -168.40(18) . . . . ? N8 N7 C12 S3 175.70(15) . . . . ? B1 N7 C12 S3 9.0(3) . . . . ? C13 N9 C12 N7 1.1(2) . . . . ? C15 N9 C12 N7 -173.7(2) . . . . ? C13 N9 C12 S3 -176.22(17) . . . . ? C15 N9 C12 S3 9.0(3) . . . . ? Rh1 S3 C12 N7 10.9(2) . . . . ? Rh1 S3 C12 N9 -172.27(19) . . . . ? N7 N8 C13 N9 -1.0(2) . . . . ? N7 N8 C13 C14 179.5(2) . . . . ? C12 N9 C13 N8 0.0(3) . . . . ? C15 N9 C13 N8 174.4(2) . . . . ? C12 N9 C13 C14 179.6(2) . . . . ? C15 N9 C13 C14 -6.0(4) . . . . ? C12 N9 C15 C16 -74.9(3) . . . . ? C13 N9 C15 C16 111.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.662 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.130 data_14++ _database_code_depnum_ccdc_archive 'CCDC 733508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B2 N18 P Rh2 S6, 2(F6 P), 4(C H2 Cl)' _chemical_formula_sum 'C52 H89 B2 Cl8 F12 N18 P3 Rh2 S6' _chemical_formula_weight 1990.72 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.412(3) _cell_length_b 14.307(3) _cell_length_c 24.049(5) _cell_angle_alpha 90.85(3) _cell_angle_beta 101.11(3) _cell_angle_gamma 107.75(3) _cell_volume 4299.3(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10882 _cell_measurement_theta_min 2.378 _cell_measurement_theta_max 27.399 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.755208 _exptl_absorpt_correction_T_max 0.850000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49319 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 27.48 _reflns_number_total 19642 _reflns_number_gt 15817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.628 (Bruker, 2005)' _computing_cell_refinement 'Bruker SMART V5.628 (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT V7.06A (Bruker, 2003)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.500 214.9 58.2 2 0.389 0.472 0.175 7.3 -0.2 3 0.611 0.528 0.825 7.3 -0.2 _platon_squeeze_details ; ? ; _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^)+(0.0803P)^2^+4.5935P] 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 19642 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_restrained_S_all 1.263 _refine_ls_shift/su_max 0.007 _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 0.19058(2) 0.30729(2) 0.281598(13) 0.01232(9) Uani 1 1 d . . . Rh2 Rh -0.05648(3) 0.34836(2) 0.227140(14) 0.01525(9) Uani 1 1 d . . . P1 P 0.30851(9) 0.34227(8) 0.37123(4) 0.0153(2) Uani 1 1 d . . . S1 S 0.07957(8) 0.30934(7) 0.18984(4) 0.0142(2) Uani 1 1 d . . . S2 S 0.04200(8) 0.30269(8) 0.32344(4) 0.0169(2) Uani 1 1 d . . . S3 S 0.32233(8) 0.28513(8) 0.23445(4) 0.0166(2) Uani 1 1 d . . . S4 S 0.07645(9) 0.50666(8) 0.24019(4) 0.0192(2) Uani 1 1 d . . . S5 S -0.16855(10) 0.40473(9) 0.27421(5) 0.0241(2) Uani 1 1 d . . . S6 S -0.19013(9) 0.19489(8) 0.19709(5) 0.0210(2) Uani 1 1 d . . . N1 N 0.0636(3) 0.1227(2) 0.21188(15) 0.0155(7) Uani 1 1 d . . . N2 N 0.0223(3) 0.0256(3) 0.18889(15) 0.0197(7) Uani 1 1 d . . . N3 N -0.0152(3) 0.1273(3) 0.12575(14) 0.0166(7) Uani 1 1 d . . . N4 N 0.0589(3) 0.1203(3) 0.31514(15) 0.0172(7) Uani 1 1 d . . . N5 N 0.0184(3) 0.0248(3) 0.33110(16) 0.0242(8) Uani 1 1 d . . . N6 N -0.0638(3) 0.1233(3) 0.36051(16) 0.0242(8) Uani 1 1 d . . . N7 N 0.2292(3) 0.1174(3) 0.27803(15) 0.0168(7) Uani 1 1 d . . . N8 N 0.2371(3) 0.0244(3) 0.28888(15) 0.0215(8) Uani 1 1 d . . . N9 N 0.3717(3) 0.1103(3) 0.25060(15) 0.0218(8) Uani 1 1 d . . . N10 N -0.0293(3) 0.4732(3) 0.13100(14) 0.0165(7) Uani 1 1 d . . . N11 N -0.0309(3) 0.5124(3) 0.07832(15) 0.0183(7) Uani 1 1 d . . . N12 N 0.1081(3) 0.6042(3) 0.14287(15) 0.0192(7) Uani 1 1 d . . . N13 N -0.1960(3) 0.4572(3) 0.16770(15) 0.0180(7) Uani 1 1 d . . . N14 N -0.2495(3) 0.5087(3) 0.13045(16) 0.0211(8) Uani 1 1 d . . . N15 N -0.2903(3) 0.5120(3) 0.21563(17) 0.0238(8) Uani 1 1 d . . . N16 N -0.1926(3) 0.3112(3) 0.11009(15) 0.0173(7) Uani 1 1 d . . . N17 N -0.2508(3) 0.3154(3) 0.05562(15) 0.0192(7) Uani 1 1 d . . . N18 N -0.3196(3) 0.1719(3) 0.08945(16) 0.0210(8) Uani 1 1 d . . . B1 B 0.1328(4) 0.1540(3) 0.2732(2) 0.0161(9) Uani 1 1 d . . . B2 B -0.1227(4) 0.3999(4) 0.1522(2) 0.0167(9) Uani 1 1 d . . . C1 C 0.0411(3) 0.1827(3) 0.17399(17) 0.0155(8) Uani 1 1 d . . . C2 C -0.0249(3) 0.0306(3) 0.13624(19) 0.0194(9) Uani 1 1 d . . . C3 C -0.0805(4) -0.0561(3) 0.0947(2) 0.0259(10) Uani 1 1 d . . . H3A H -0.0999 -0.1156 0.1150 0.039 Uiso 1 1 calc R . . H3B H -0.0330 -0.0626 0.0696 0.039 Uiso 1 1 calc R . . H3C H -0.1455 -0.0472 0.0719 0.039 Uiso 1 1 calc R . . C4 C -0.0439(4) 0.1649(3) 0.07043(17) 0.0203(9) Uani 1 1 d . . . H4A H -0.0523 0.2304 0.0764 0.024 Uiso 1 1 calc R . . H4B H -0.1131 0.1200 0.0491 0.024 Uiso 1 1 calc R . . C5 C 0.0419(4) 0.1730(4) 0.0360(2) 0.0275(10) Uani 1 1 d . . . H5A H 0.1101 0.2186 0.0568 0.041 Uiso 1 1 calc R . . H5B H 0.0212 0.1978 -0.0008 0.041 Uiso 1 1 calc R . . H5C H 0.0499 0.1080 0.0299 0.041 Uiso 1 1 calc R . . C6 C 0.0088(3) 0.1781(3) 0.33243(17) 0.0190(9) Uani 1 1 d . . . C7 C -0.0547(4) 0.0303(4) 0.3584(2) 0.0291(11) Uani 1 1 d . . . C8 C -0.1205(5) -0.0540(4) 0.3851(3) 0.0473(16) Uani 1 1 d . . . H8A H -0.1963 -0.0680 0.3676 0.071 Uiso 1 1 calc R . . H8B H -0.1093 -0.0369 0.4260 0.071 Uiso 1 1 calc R . . H8C H -0.0988 -0.1124 0.3793 0.071 Uiso 1 1 calc R . . C9 C -0.1381(4) 0.1581(4) 0.3874(2) 0.0326(11) Uani 1 1 d . . . H9A H -0.1009 0.2259 0.4049 0.039 Uiso 1 1 calc R . . H9B H -0.1590 0.1154 0.4179 0.039 Uiso 1 1 calc R . . C10 C -0.2368(5) 0.1571(5) 0.3450(2) 0.0382(13) Uani 1 1 d . . . H10A H -0.2164 0.1994 0.3148 0.057 Uiso 1 1 calc R . . H10B H -0.2833 0.1815 0.3642 0.057 Uiso 1 1 calc R . . H10C H -0.2753 0.0896 0.3286 0.057 Uiso 1 1 calc R . . C11 C 0.3095(3) 0.1683(3) 0.25427(17) 0.0163(8) Uani 1 1 d . . . C12 C 0.3233(4) 0.0230(3) 0.27216(18) 0.0244(10) Uani 1 1 d . . . C13 C 0.3669(5) -0.0614(4) 0.2764(2) 0.0352(13) Uani 1 1 d . . . H13A H 0.4392 -0.0401 0.3002 0.053 Uiso 1 1 calc R . . H13B H 0.3696 -0.0846 0.2384 0.053 Uiso 1 1 calc R . . H13C H 0.3206 -0.1149 0.2935 0.053 Uiso 1 1 calc R . . C14 C 0.4637(4) 0.1328(4) 0.2219(2) 0.0275(10) Uani 1 1 d . . . H14A H 0.4388 0.1441 0.1818 0.033 Uiso 1 1 calc R . . H14B H 0.4890 0.0747 0.2218 0.033 Uiso 1 1 calc R . . C15 C 0.5569(5) 0.2212(6) 0.2487(3) 0.057(2) Uani 1 1 d . . . H15A H 0.5360 0.2810 0.2437 0.085 Uiso 1 1 calc R . . H15B H 0.6174 0.2261 0.2305 0.085 Uiso 1 1 calc R . . H15C H 0.5778 0.2140 0.2894 0.085 Uiso 1 1 calc R . . C16 C 0.0531(3) 0.5292(3) 0.16972(18) 0.0156(8) Uani 1 1 d . . . C17 C 0.0540(4) 0.5901(3) 0.08688(18) 0.0183(8) Uani 1 1 d . . . C18 C 0.0894(4) 0.6558(3) 0.04213(19) 0.0238(10) Uani 1 1 d . . . H18A H 0.1616 0.6571 0.0390 0.036 Uiso 1 1 calc R . . H18B H 0.0899 0.7225 0.0523 0.036 Uiso 1 1 calc R . . H18C H 0.0400 0.6308 0.0056 0.036 Uiso 1 1 calc R . . C19 C 0.2065(4) 0.6846(3) 0.1693(2) 0.0275(10) Uani 1 1 d . . . H19A H 0.2048 0.6988 0.2095 0.033 Uiso 1 1 calc R . . H19B H 0.2081 0.7450 0.1494 0.033 Uiso 1 1 calc R . . C20 C 0.3066(4) 0.6588(5) 0.1669(3) 0.0451(15) Uani 1 1 d . . . H20A H 0.3071 0.6012 0.1883 0.068 Uiso 1 1 calc R . . H20B H 0.3695 0.7146 0.1837 0.068 Uiso 1 1 calc R . . H20C H 0.3082 0.6440 0.1273 0.068 Uiso 1 1 calc R . . C21 C -0.2202(3) 0.4598(3) 0.21868(19) 0.0189(8) Uani 1 1 d . . . C22 C -0.3049(4) 0.5404(3) 0.16091(19) 0.0219(9) Uani 1 1 d . . . C23 C -0.3753(4) 0.6003(4) 0.1398(2) 0.0325(11) Uani 1 1 d . . . H23A H -0.3739 0.6112 0.0998 0.049 Uiso 1 1 calc R . . H23B H -0.3498 0.6638 0.1623 0.049 Uiso 1 1 calc R . . H23C H -0.4488 0.5653 0.1433 0.049 Uiso 1 1 calc R . . C24 C -0.3351(4) 0.5360(4) 0.2631(2) 0.0325(12) Uani 1 1 d . . . H24A H -0.3530 0.4781 0.2857 0.039 Uiso 1 1 calc R . . H24B H -0.4021 0.5510 0.2479 0.039 Uiso 1 1 calc R . . C25 C -0.2589(6) 0.6215(6) 0.3006(3) 0.059(2) Uani 1 1 d . . . H25A H -0.1922 0.6072 0.3154 0.089 Uiso 1 1 calc R . . H25B H -0.2904 0.6342 0.3323 0.089 Uiso 1 1 calc R . . H25C H -0.2437 0.6797 0.2788 0.089 Uiso 1 1 calc R . . C26 C -0.2354(3) 0.2254(3) 0.13014(19) 0.0194(9) Uani 1 1 d . . . C27 C -0.3253(4) 0.2299(3) 0.04473(19) 0.0218(9) Uani 1 1 d . . . C28 C -0.4096(4) 0.1994(4) -0.0085(2) 0.0284(10) Uani 1 1 d . . . H28A H -0.4022 0.2544 -0.0329 0.043 Uiso 1 1 calc R . . H28B H -0.4804 0.1807 0.0011 0.043 Uiso 1 1 calc R . . H28C H -0.4012 0.1431 -0.0287 0.043 Uiso 1 1 calc R . . C29 C -0.3888(4) 0.0720(3) 0.0941(2) 0.0283(10) Uani 1 1 d . . . H29A H -0.4585 0.0603 0.0676 0.034 Uiso 1 1 calc R . . H29B H -0.4021 0.0664 0.1332 0.034 Uiso 1 1 calc R . . C30 C -0.3399(4) -0.0061(4) 0.0805(2) 0.0297(11) Uani 1 1 d . . . H30A H -0.3268 -0.0011 0.0418 0.045 Uiso 1 1 calc R . . H30B H -0.3892 -0.0715 0.0835 0.045 Uiso 1 1 calc R . . H30C H -0.2721 0.0037 0.1075 0.045 Uiso 1 1 calc R . . C31 C 0.3607(4) 0.4789(3) 0.37270(18) 0.0184(8) Uani 1 1 d . . . H31 H 0.4207 0.5026 0.4066 0.022 Uiso 1 1 calc R . . C32 C 0.4064(4) 0.5107(3) 0.3196(2) 0.0247(10) Uani 1 1 d . . . H32A H 0.4613 0.4789 0.3164 0.030 Uiso 1 1 calc R . . H32B H 0.3485 0.4890 0.2853 0.030 Uiso 1 1 calc R . . C33 C 0.4567(5) 0.6232(3) 0.3232(2) 0.0340(12) Uani 1 1 d . . . H33A H 0.5176 0.6445 0.3562 0.041 Uiso 1 1 calc R . . H33B H 0.4844 0.6427 0.2884 0.041 Uiso 1 1 calc R . . C34 C 0.3739(5) 0.6732(4) 0.3295(3) 0.0431(15) Uani 1 1 d . . . H34A H 0.3162 0.6561 0.2949 0.052 Uiso 1 1 calc R . . H34B H 0.4079 0.7455 0.3332 0.052 Uiso 1 1 calc R . . C35 C 0.3259(5) 0.6412(4) 0.3815(3) 0.0396(14) Uani 1 1 d . . . H35A H 0.2704 0.6727 0.3837 0.048 Uiso 1 1 calc R . . H35B H 0.3826 0.6637 0.4163 0.048 Uiso 1 1 calc R . . C36 C 0.2760(4) 0.5286(3) 0.3788(2) 0.0259(10) Uani 1 1 d . . . H36A H 0.2489 0.5097 0.4138 0.031 Uiso 1 1 calc R . . H36B H 0.2150 0.5064 0.3459 0.031 Uiso 1 1 calc R . . C37 C 0.2503(4) 0.3238(3) 0.43562(17) 0.0199(9) Uani 1 1 d . . . H37 H 0.1897 0.3518 0.4273 0.024 Uiso 1 1 calc R . . C38 C 0.3208(4) 0.3814(4) 0.49150(19) 0.0281(11) Uani 1 1 d . . . H38A H 0.3761 0.3505 0.5068 0.034 Uiso 1 1 calc R . . H38B H 0.3573 0.4500 0.4841 0.034 Uiso 1 1 calc R . . C39 C 0.2504(5) 0.3813(4) 0.5352(2) 0.0346(12) Uani 1 1 d . . . H39A H 0.2964 0.4161 0.5715 0.042 Uiso 1 1 calc R . . H39B H 0.1995 0.4174 0.5211 0.042 Uiso 1 1 calc R . . C40 C 0.1876(5) 0.2761(4) 0.5462(2) 0.0327(12) Uani 1 1 d . . . H40A H 0.2381 0.2433 0.5658 0.039 Uiso 1 1 calc R . . H40B H 0.1381 0.2791 0.5713 0.039 Uiso 1 1 calc R . . C41 C 0.1238(4) 0.2157(4) 0.4906(2) 0.0293(11) Uani 1 1 d . . . H41A H 0.0668 0.2434 0.4734 0.035 Uiso 1 1 calc R . . H41B H 0.0892 0.1470 0.4986 0.035 Uiso 1 1 calc R . . C42 C 0.1974(4) 0.2167(3) 0.44856(18) 0.0226(9) Uani 1 1 d . . . H42A H 0.1551 0.1771 0.4129 0.027 Uiso 1 1 calc R . . H42B H 0.2533 0.1873 0.4652 0.027 Uiso 1 1 calc R . . C43 C 0.4303(4) 0.3031(3) 0.38318(18) 0.0205(9) Uani 1 1 d . . . H43 H 0.4478 0.2968 0.3450 0.025 Uiso 1 1 calc R . . C44 C 0.5310(4) 0.3758(4) 0.4208(2) 0.0299(11) Uani 1 1 d . . . H44A H 0.5176 0.3845 0.4593 0.036 Uiso 1 1 calc R . . H44B H 0.5466 0.4407 0.4046 0.036 Uiso 1 1 calc R . . C45 C 0.6285(4) 0.3383(4) 0.4251(2) 0.0357(12) Uani 1 1 d . . . H45A H 0.6463 0.3359 0.3871 0.043 Uiso 1 1 calc R . . H45B H 0.6911 0.3848 0.4510 0.043 Uiso 1 1 calc R . . C46 C 0.6058(4) 0.2359(4) 0.4472(2) 0.0302(11) Uani 1 1 d . . . H46A H 0.6683 0.2125 0.4478 0.036 Uiso 1 1 calc R . . H46B H 0.5947 0.2394 0.4866 0.036 Uiso 1 1 calc R . . C47 C 0.5063(4) 0.1631(4) 0.4095(2) 0.0289(11) Uani 1 1 d . . . H47A H 0.4911 0.0979 0.4254 0.035 Uiso 1 1 calc R . . H47B H 0.5195 0.1552 0.3709 0.035 Uiso 1 1 calc R . . C48 C 0.4100(4) 0.2003(3) 0.4062(2) 0.0240(10) Uani 1 1 d . . . H48A H 0.3940 0.2033 0.4446 0.029 Uiso 1 1 calc R . . H48B H 0.3468 0.1532 0.3811 0.029 Uiso 1 1 calc R . . P2 P 0.75781(9) 0.03350(8) 0.91006(5) 0.0197(2) Uani 1 1 d D . . F1 F 0.6799(3) 0.0695(3) 0.86249(14) 0.0435(8) Uani 1 1 d D . . F2 F 0.8355(2) -0.0020(2) 0.95808(12) 0.0310(6) Uani 1 1 d D . . F3 F 0.8596(2) 0.1090(2) 0.89166(13) 0.0346(7) Uani 1 1 d D . . F4 F 0.6554(2) -0.0417(2) 0.92801(13) 0.0328(7) Uani 1 1 d D . . F5 F 0.7568(2) 0.1164(2) 0.95535(12) 0.0308(6) Uani 1 1 d D . . F6 F 0.7596(2) -0.0509(2) 0.86573(12) 0.0338(7) Uani 1 1 d D . . P3 P 0.58926(18) 0.90123(17) 0.42402(9) 0.0193(4) Uani 0.50 1 d PD A 1 F7 F 0.4657(4) 0.8825(5) 0.3967(2) 0.0352(14) Uani 0.50 1 d PD A 1 F8 F 0.7123(4) 0.9195(4) 0.4521(2) 0.0305(12) Uani 0.50 1 d PD A 1 F9 F 0.6067(6) 0.8581(5) 0.3653(2) 0.0409(11) Uani 0.50 1 d PD A 1 F10 F 0.5782(6) 0.9468(5) 0.4816(2) 0.0409(11) Uani 0.50 1 d PD A 1 F11 F 0.6206(5) 1.0077(4) 0.4015(3) 0.0426(16) Uani 0.50 1 d PD A 1 F12 F 0.5603(5) 0.7922(4) 0.4452(2) 0.0325(13) Uani 0.50 1 d PD A 1 C54 C 0.6748(11) 0.9301(13) 0.2395(6) 0.046(3) Uani 0.50 1 d P B 1 H54A H 0.6941 1.0022 0.2371 0.056 Uiso 0.50 1 calc PR B 1 H54B H 0.6694 0.9164 0.2792 0.056 Uiso 0.50 1 calc PR B 1 Cl9 Cl 0.7751(3) 0.8899(4) 0.22233(19) 0.0787(15) Uani 0.50 1 d P B 1 Cl10 Cl 0.5480(4) 0.8725(5) 0.1938(3) 0.074(2) Uani 0.50 1 d P B 1 P4 P 0.6586(3) 0.8724(3) 0.23907(16) 0.0421(8) Uani 0.50 1 d PD C 2 F13 F 0.5772(7) 0.7642(6) 0.2266(4) 0.085(3) Uani 0.50 1 d PD C 2 F14 F 0.7529(8) 0.9757(6) 0.2553(5) 0.081(3) Uani 0.50 1 d PD C 2 F15 F 0.6201(7) 0.8869(7) 0.2964(3) 0.064(2) Uani 0.50 1 d PD C 2 F16 F 0.7002(8) 0.8557(6) 0.1825(4) 0.065(2) Uani 0.50 1 d PD C 2 F17 F 0.5793(10) 0.9224(12) 0.2055(5) 0.095(6) Uani 0.50 1 d PD C 2 F18 F 0.7431(8) 0.8254(7) 0.2729(4) 0.085(3) Uani 0.50 1 d PD C 2 C50 C 0.2178(7) 0.9447(6) 0.4242(4) 0.032(2) Uani 0.50 1 d PD D 2 H50A H 0.1878 0.9595 0.3857 0.039 Uiso 0.50 1 calc PR D 2 H50B H 0.2607 1.0082 0.4459 0.039 Uiso 0.50 1 calc PR D 2 Cl3 Cl 0.3010(3) 0.8780(2) 0.41815(11) 0.0395(6) Uani 0.50 1 d PD D 2 Cl4 Cl 0.1145(2) 0.8904(2) 0.45643(9) 0.0415(7) Uani 0.50 1 d PD D 2 C49 C 0.2472(4) 0.4734(4) 0.0038(2) 0.0273(10) Uani 1 1 d . . . H49A H 0.2271 0.4155 -0.0239 0.033 Uiso 1 1 calc R . . H49B H 0.2169 0.5231 -0.0144 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.19283(10) 0.43716(9) 0.06518(5) 0.0321(3) Uani 1 1 d . . . Cl2 Cl 0.38855(10) 0.52333(11) 0.02235(6) 0.0402(3) Uani 1 1 d . . . C51 C 0.6421(4) 0.7293(4) 0.9229(2) 0.0279(10) Uani 1 1 d . . . H51A H 0.6733 0.7911 0.9057 0.033 Uiso 1 1 calc R . . H51B H 0.6738 0.6798 0.9115 0.033 Uiso 1 1 calc R . . Cl5 Cl 0.50207(11) 0.68662(11) 0.89693(6) 0.0385(3) Uani 1 1 d . . . Cl6 Cl 0.67506(11) 0.75107(10) 0.99848(6) 0.0344(3) Uani 1 1 d . . . C52 C 0.0158(10) 0.8187(5) 0.2432(4) 0.118(5) Uani 1 1 d . . . H52A H 0.0746 0.8657 0.2289 0.142 Uiso 1 1 calc R . . H52B H -0.0291 0.8557 0.2550 0.142 Uiso 1 1 calc R . . Cl7 Cl -0.06189(12) 0.72861(10) 0.18858(7) 0.0435(3) Uani 1 1 d . . . Cl8 Cl 0.0697(3) 0.76662(14) 0.30168(10) 0.1080(11) 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 0.01343(16) 0.01153(15) 0.01218(15) 0.00195(11) 0.00227(11) 0.00438(12) Rh2 0.01518(16) 0.01674(16) 0.01711(16) 0.00603(12) 0.00634(12) 0.00771(13) P1 0.0177(5) 0.0127(5) 0.0137(5) 0.0014(4) 0.0008(4) 0.0037(4) S1 0.0150(5) 0.0143(5) 0.0144(4) 0.0036(4) 0.0032(4) 0.0060(4) S2 0.0176(5) 0.0191(5) 0.0164(5) 0.0044(4) 0.0055(4) 0.0077(4) S3 0.0161(5) 0.0168(5) 0.0181(5) 0.0025(4) 0.0045(4) 0.0063(4) S4 0.0245(6) 0.0169(5) 0.0167(5) 0.0039(4) 0.0051(4) 0.0067(4) S5 0.0273(6) 0.0315(6) 0.0238(5) 0.0117(5) 0.0139(5) 0.0183(5) S6 0.0167(5) 0.0211(5) 0.0265(6) 0.0100(4) 0.0073(4) 0.0059(4) N1 0.0160(17) 0.0129(16) 0.0162(17) 0.0005(13) 0.0003(13) 0.0042(13) N2 0.0229(19) 0.0153(17) 0.0191(18) -0.0020(14) 0.0017(15) 0.0050(15) N3 0.0162(17) 0.0225(18) 0.0126(16) -0.0001(14) 0.0013(13) 0.0093(15) N4 0.0192(18) 0.0144(17) 0.0154(17) 0.0056(14) -0.0001(14) 0.0038(14) N5 0.024(2) 0.0185(18) 0.024(2) 0.0089(16) 0.0023(16) -0.0010(15) N6 0.021(2) 0.029(2) 0.0192(18) 0.0082(16) 0.0062(15) 0.0028(16) N7 0.0200(18) 0.0143(16) 0.0170(17) 0.0019(14) 0.0001(14) 0.0089(14) N8 0.032(2) 0.0136(17) 0.0184(18) 0.0002(14) -0.0024(16) 0.0111(16) N9 0.028(2) 0.028(2) 0.0150(17) 0.0008(15) 0.0022(15) 0.0187(17) N10 0.0185(18) 0.0188(17) 0.0154(16) 0.0063(14) 0.0055(14) 0.0091(14) N11 0.0188(18) 0.0206(18) 0.0195(18) 0.0091(15) 0.0083(14) 0.0089(15) N12 0.0238(19) 0.0128(17) 0.0215(18) 0.0031(14) 0.0060(15) 0.0054(15) N13 0.0171(18) 0.0195(18) 0.0207(18) 0.0031(15) 0.0031(14) 0.0110(15) N14 0.0201(19) 0.0201(18) 0.0241(19) 0.0036(15) -0.0007(15) 0.0109(15) N15 0.024(2) 0.027(2) 0.026(2) 0.0033(16) 0.0076(16) 0.0160(17) N16 0.0158(17) 0.0205(18) 0.0186(17) 0.0049(14) 0.0058(14) 0.0086(14) N17 0.0169(18) 0.0255(19) 0.0178(17) 0.0011(15) 0.0031(14) 0.0109(15) N18 0.0158(18) 0.0230(19) 0.027(2) 0.0029(16) 0.0074(15) 0.0076(15) B1 0.019(2) 0.012(2) 0.015(2) 0.0022(17) 0.0010(18) 0.0037(18) B2 0.016(2) 0.020(2) 0.018(2) 0.0071(18) 0.0063(18) 0.0089(19) C1 0.0133(19) 0.021(2) 0.0137(18) -0.0002(16) 0.0013(15) 0.0080(16) C2 0.017(2) 0.019(2) 0.021(2) -0.0010(17) 0.0010(17) 0.0064(17) C3 0.030(3) 0.024(2) 0.021(2) -0.0077(19) -0.0041(19) 0.013(2) C4 0.023(2) 0.028(2) 0.0115(19) 0.0006(17) -0.0003(16) 0.0139(19) C5 0.034(3) 0.036(3) 0.021(2) 0.006(2) 0.009(2) 0.020(2) C6 0.018(2) 0.023(2) 0.0139(19) 0.0051(17) 0.0006(16) 0.0048(17) C7 0.030(3) 0.025(2) 0.027(2) 0.013(2) 0.002(2) 0.002(2) C8 0.046(4) 0.040(3) 0.046(3) 0.025(3) 0.012(3) -0.004(3) C9 0.029(3) 0.043(3) 0.028(3) 0.008(2) 0.016(2) 0.008(2) C10 0.044(3) 0.050(3) 0.032(3) 0.012(3) 0.014(2) 0.027(3) C11 0.021(2) 0.0167(19) 0.0127(18) -0.0016(15) -0.0012(16) 0.0108(17) C12 0.038(3) 0.024(2) 0.014(2) -0.0010(17) -0.0008(19) 0.017(2) C13 0.059(4) 0.037(3) 0.025(2) 0.011(2) 0.012(2) 0.035(3) C14 0.035(3) 0.034(3) 0.023(2) 0.002(2) 0.011(2) 0.021(2) C15 0.026(3) 0.104(6) 0.040(3) -0.024(4) 0.004(3) 0.024(3) C16 0.017(2) 0.0149(19) 0.020(2) 0.0029(16) 0.0056(16) 0.0099(16) C17 0.021(2) 0.018(2) 0.019(2) 0.0050(17) 0.0080(17) 0.0091(17) C18 0.029(2) 0.020(2) 0.022(2) 0.0077(18) 0.0083(19) 0.0053(19) C19 0.033(3) 0.018(2) 0.023(2) 0.0014(18) 0.003(2) -0.0045(19) C20 0.027(3) 0.055(4) 0.040(3) -0.008(3) 0.007(2) -0.006(3) C21 0.018(2) 0.019(2) 0.024(2) 0.0040(17) 0.0086(17) 0.0085(17) C22 0.019(2) 0.024(2) 0.024(2) 0.0012(18) 0.0012(18) 0.0101(18) C23 0.036(3) 0.039(3) 0.030(3) -0.001(2) 0.002(2) 0.026(2) C24 0.038(3) 0.042(3) 0.035(3) 0.011(2) 0.024(2) 0.026(3) C25 0.055(4) 0.099(6) 0.027(3) -0.018(3) 0.008(3) 0.030(4) C26 0.015(2) 0.023(2) 0.025(2) 0.0032(18) 0.0078(17) 0.0096(17) C27 0.017(2) 0.026(2) 0.025(2) 0.0010(18) 0.0047(18) 0.0099(18) C28 0.020(2) 0.033(3) 0.030(3) -0.002(2) 0.0012(19) 0.009(2) C29 0.015(2) 0.023(2) 0.044(3) 0.004(2) 0.007(2) 0.0004(18) C30 0.029(3) 0.021(2) 0.037(3) -0.001(2) 0.006(2) 0.005(2) C31 0.022(2) 0.0127(19) 0.019(2) 0.0007(16) 0.0050(17) 0.0030(16) C32 0.034(3) 0.019(2) 0.026(2) 0.0035(18) 0.012(2) 0.0100(19) C33 0.043(3) 0.016(2) 0.045(3) 0.010(2) 0.021(3) 0.004(2) C34 0.062(4) 0.020(2) 0.060(4) 0.018(3) 0.035(3) 0.017(3) C35 0.054(4) 0.016(2) 0.059(4) 0.002(2) 0.030(3) 0.014(2) C36 0.030(3) 0.018(2) 0.034(3) 0.0047(19) 0.014(2) 0.0094(19) C37 0.028(2) 0.016(2) 0.0142(19) 0.0022(16) 0.0038(17) 0.0053(18) C38 0.035(3) 0.023(2) 0.018(2) 0.0036(18) 0.005(2) -0.002(2) C39 0.050(3) 0.028(3) 0.016(2) -0.0032(19) 0.011(2) -0.005(2) C40 0.044(3) 0.027(3) 0.020(2) 0.002(2) 0.012(2) -0.002(2) C41 0.035(3) 0.026(2) 0.021(2) 0.0069(19) 0.008(2) 0.000(2) C42 0.027(2) 0.020(2) 0.015(2) -0.0001(17) 0.0005(17) 0.0006(18) C43 0.020(2) 0.022(2) 0.018(2) 0.0017(17) -0.0013(17) 0.0089(18) C44 0.025(2) 0.021(2) 0.038(3) -0.004(2) -0.007(2) 0.0062(19) C45 0.024(3) 0.035(3) 0.042(3) -0.006(2) -0.010(2) 0.012(2) C46 0.033(3) 0.040(3) 0.022(2) -0.003(2) -0.004(2) 0.025(2) C47 0.038(3) 0.026(2) 0.026(2) -0.001(2) 0.000(2) 0.019(2) C48 0.029(2) 0.021(2) 0.022(2) -0.0004(18) -0.0015(19) 0.0117(19) P2 0.0180(5) 0.0203(5) 0.0198(5) 0.0015(4) 0.0020(4) 0.0059(4) F1 0.0408(19) 0.051(2) 0.0374(18) 0.0145(15) -0.0060(14) 0.0206(16) F2 0.0335(16) 0.0340(16) 0.0270(14) 0.0015(12) -0.0039(12) 0.0188(13) F3 0.0308(16) 0.0282(15) 0.0448(18) 0.0052(13) 0.0177(14) 0.0029(13) F4 0.0270(15) 0.0276(15) 0.0421(17) 0.0018(13) 0.0130(13) 0.0028(12) F5 0.0321(16) 0.0235(14) 0.0395(16) -0.0042(12) 0.0110(13) 0.0108(12) F6 0.0368(17) 0.0341(16) 0.0275(15) -0.0104(13) 0.0066(13) 0.0073(13) P3 0.0213(11) 0.0203(11) 0.0161(10) 0.0037(9) 0.0043(9) 0.0061(9) F7 0.028(3) 0.049(4) 0.027(3) 0.001(3) -0.003(2) 0.015(3) F8 0.019(3) 0.035(3) 0.031(3) 0.000(2) 0.000(2) 0.004(2) F9 0.066(3) 0.042(3) 0.019(2) -0.0047(18) 0.005(2) 0.027(2) F10 0.066(3) 0.042(3) 0.019(2) -0.0047(18) 0.005(2) 0.027(2) F11 0.046(4) 0.026(3) 0.061(4) 0.018(3) 0.022(3) 0.010(3) F12 0.038(3) 0.023(3) 0.035(3) 0.009(2) 0.006(3) 0.009(3) C54 0.032(7) 0.048(8) 0.051(8) -0.007(7) 0.004(6) 0.003(7) Cl9 0.046(2) 0.141(4) 0.070(3) 0.059(3) 0.0272(19) 0.048(2) Cl10 0.0340(19) 0.109(4) 0.059(3) 0.012(3) 0.0124(17) -0.009(2) P4 0.0399(19) 0.0362(18) 0.051(2) 0.0154(17) 0.0109(15) 0.0114(17) F13 0.066(6) 0.073(6) 0.088(7) -0.004(5) 0.024(5) -0.021(5) F14 0.074(7) 0.045(5) 0.124(9) 0.001(5) 0.050(6) 0.002(5) F15 0.059(5) 0.086(6) 0.058(5) 0.018(4) 0.025(4) 0.031(5) F16 0.088(7) 0.052(5) 0.072(6) 0.021(4) 0.042(5) 0.028(5) F17 0.085(10) 0.190(16) 0.073(9) 0.077(11) 0.047(8) 0.114(11) F18 0.095(8) 0.088(7) 0.079(6) -0.002(5) -0.015(5) 0.058(6) C50 0.044(6) 0.017(4) 0.039(6) -0.004(4) 0.036(5) -0.001(4) Cl3 0.0591(18) 0.0318(13) 0.0315(13) -0.0015(11) 0.0004(12) 0.0258(13) Cl4 0.0396(14) 0.0652(18) 0.0087(9) 0.0094(11) 0.0089(9) -0.0022(13) C49 0.024(2) 0.033(3) 0.026(2) 0.006(2) 0.0017(19) 0.012(2) Cl1 0.0351(7) 0.0346(6) 0.0344(6) 0.0069(5) 0.0119(5) 0.0194(5) Cl2 0.0214(6) 0.0468(8) 0.0504(8) 0.0113(6) 0.0020(5) 0.0108(6) C51 0.024(2) 0.027(2) 0.035(3) 0.006(2) 0.008(2) 0.010(2) Cl5 0.0266(6) 0.0480(8) 0.0392(7) -0.0022(6) 0.0055(5) 0.0103(6) Cl6 0.0355(7) 0.0356(7) 0.0338(6) 0.0032(5) 0.0052(5) 0.0149(6) C52 0.197(12) 0.024(4) 0.085(6) -0.002(4) -0.069(7) 0.026(5) Cl7 0.0422(8) 0.0307(7) 0.0579(9) 0.0030(6) 0.0103(7) 0.0122(6) Cl8 0.171(3) 0.0318(9) 0.0815(15) 0.0032(9) -0.0520(16) 0.0223(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 B1 2.084(5) . ? Rh1 P1 2.3601(14) . ? Rh1 S3 2.3688(12) . ? Rh1 S2 2.3837(12) . ? Rh1 S1 2.4186(13) . ? Rh2 B2 2.098(5) . ? Rh2 S5 2.3576(13) . ? Rh2 S6 2.3687(15) . ? Rh2 S1 2.3837(12) . ? Rh2 S4 2.3892(15) . ? Rh2 S2 2.6320(13) . ? P1 C37 1.852(4) . ? P1 C43 1.857(4) . ? P1 C31 1.862(4) . ? S1 C1 1.740(4) . ? S2 C6 1.729(4) . ? S3 C11 1.712(4) . ? S4 C16 1.717(4) . ? S5 C21 1.701(4) . ? S6 C26 1.720(4) . ? N1 C1 1.318(5) . ? N1 N2 1.390(5) . ? N1 B1 1.560(6) . ? N2 C2 1.316(6) . ? N3 C1 1.347(5) . ? N3 C2 1.381(5) . ? N3 C4 1.468(5) . ? N4 C6 1.321(6) . ? N4 N5 1.396(5) . ? N4 B1 1.531(6) . ? N5 C7 1.300(7) . ? N6 C6 1.350(6) . ? N6 C7 1.374(6) . ? N6 C9 1.482(6) . ? N7 C11 1.336(6) . ? N7 N8 1.390(5) . ? N7 B1 1.522(6) . ? N8 C12 1.301(6) . ? N9 C11 1.357(5) . ? N9 C12 1.380(6) . ? N9 C14 1.481(6) . ? N10 C16 1.331(6) . ? N10 N11 1.392(5) . ? N10 B2 1.545(6) . ? N11 C17 1.307(6) . ? N12 C16 1.354(5) . ? N12 C17 1.381(6) . ? N12 C19 1.483(6) . ? N13 C21 1.330(5) . ? N13 N14 1.398(5) . ? N13 B2 1.549(6) . ? N14 C22 1.304(6) . ? N15 C21 1.360(6) . ? N15 C22 1.378(6) . ? N15 C24 1.470(6) . ? N16 C26 1.328(5) . ? N16 N17 1.402(5) . ? N16 B2 1.546(6) . ? N17 C27 1.307(6) . ? N18 C26 1.358(6) . ? N18 C27 1.373(6) . ? N18 C29 1.466(6) . ? C2 C3 1.485(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.520(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.497(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.503(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.489(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.510(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.490(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.508(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 C23 1.485(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.485(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.494(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.518(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.539(6) . ? C31 C32 1.536(6) . ? C31 H31 1.0000 . ? C32 C33 1.538(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.521(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.529(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.540(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.543(6) . ? C37 C42 1.544(6) . ? C37 H37 1.0000 . ? C38 C39 1.542(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.538(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.529(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.541(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.539(6) . ? C43 C48 1.544(6) . ? C43 H43 1.0000 . ? C44 C45 1.545(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.529(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.532(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.529(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? P2 F2 1.598(3) . ? P2 F1 1.597(3) . ? P2 F4 1.603(3) . ? P2 F5 1.604(3) . ? P2 F3 1.605(3) . ? P2 F6 1.607(3) . ? P3 F11 1.585(6) . ? P3 F10 1.574(6) . ? P3 F8 1.597(5) . ? P3 F12 1.605(5) . ? P3 F7 1.599(6) . ? P3 F9 1.618(6) . ? C54 Cl9 1.728(15) . ? C54 Cl10 1.782(14) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? P4 F17 1.563(9) . ? P4 F13 1.584(8) . ? P4 F18 1.589(8) . ? P4 F15 1.595(8) . ? P4 F14 1.609(8) . ? P4 F16 1.607(8) . ? C50 Cl3 1.700(7) . ? C50 Cl4 1.702(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C49 Cl2 1.772(5) . ? C49 Cl1 1.785(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C51 Cl5 1.768(5) . ? C51 Cl6 1.784(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 Cl8 1.738(8) . ? C52 Cl7 1.754(8) . ? C52 H52A 0.9900 . ? C52 H52B 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 B1 Rh1 P1 103.27(13) . . ? B1 Rh1 S3 83.90(14) . . ? P1 Rh1 S3 93.02(4) . . ? B1 Rh1 S2 87.21(14) . . ? P1 Rh1 S2 91.68(4) . . ? S3 Rh1 S2 170.70(4) . . ? B1 Rh1 S1 88.99(13) . . ? P1 Rh1 S1 167.72(4) . . ? S3 Rh1 S1 88.82(4) . . ? S2 Rh1 S1 88.29(4) . . ? B2 Rh2 S5 88.52(13) . . ? B2 Rh2 S6 86.71(14) . . ? S5 Rh2 S6 92.39(5) . . ? B2 Rh2 S1 95.77(13) . . ? S5 Rh2 S1 170.94(4) . . ? S6 Rh2 S1 95.81(4) . . ? B2 Rh2 S4 84.68(14) . . ? S5 Rh2 S4 92.43(5) . . ? S6 Rh2 S4 170.01(4) . . ? S1 Rh2 S4 80.07(4) . . ? B2 Rh2 S2 173.80(14) . . ? S5 Rh2 S2 91.38(4) . . ? S6 Rh2 S2 99.49(5) . . ? S1 Rh2 S2 83.50(4) . . ? S4 Rh2 S2 89.13(5) . . ? C37 P1 C43 108.9(2) . . ? C37 P1 C31 102.30(19) . . ? C43 P1 C31 104.3(2) . . ? C37 P1 Rh1 118.23(15) . . ? C43 P1 Rh1 120.04(15) . . ? C31 P1 Rh1 99.80(15) . . ? C1 S1 Rh2 108.98(14) . . ? C1 S1 Rh1 94.79(14) . . ? Rh2 S1 Rh1 95.21(4) . . ? C6 S2 Rh1 94.55(16) . . ? C6 S2 Rh2 114.87(15) . . ? Rh1 S2 Rh2 89.86(4) . . ? C11 S3 Rh1 94.85(15) . . ? C16 S4 Rh2 94.72(15) . . ? C21 S5 Rh2 96.64(15) . . ? C26 S6 Rh2 96.16(16) . . ? C1 N1 N2 110.7(3) . . ? C1 N1 B1 125.8(3) . . ? N2 N1 B1 123.4(3) . . ? C2 N2 N1 104.8(3) . . ? C1 N3 C2 106.9(3) . . ? C1 N3 C4 125.6(4) . . ? C2 N3 C4 126.8(4) . . ? C6 N4 N5 110.6(4) . . ? C6 N4 B1 120.9(3) . . ? N5 N4 B1 127.3(4) . . ? C7 N5 N4 103.9(4) . . ? C6 N6 C7 105.9(4) . . ? C6 N6 C9 126.2(4) . . ? C7 N6 C9 127.9(4) . . ? C11 N7 N8 110.4(3) . . ? C11 N7 B1 117.5(3) . . ? N8 N7 B1 129.3(4) . . ? C12 N8 N7 104.6(4) . . ? C11 N9 C12 105.9(4) . . ? C11 N9 C14 125.8(4) . . ? C12 N9 C14 127.8(4) . . ? C16 N10 N11 110.8(3) . . ? C16 N10 B2 118.0(3) . . ? N11 N10 B2 128.1(3) . . ? C17 N11 N10 104.3(3) . . ? C16 N12 C17 106.2(4) . . ? C16 N12 C19 126.0(4) . . ? C17 N12 C19 127.8(4) . . ? C21 N13 N14 110.6(3) . . ? C21 N13 B2 123.6(3) . . ? N14 N13 B2 125.7(3) . . ? C22 N14 N13 104.3(4) . . ? C21 N15 C22 106.1(4) . . ? C21 N15 C24 125.4(4) . . ? C22 N15 C24 128.5(4) . . ? C26 N16 N17 110.0(4) . . ? C26 N16 B2 119.2(4) . . ? N17 N16 B2 126.4(3) . . ? C27 N17 N16 104.6(3) . . ? C26 N18 C27 106.3(4) . . ? C26 N18 C29 125.4(4) . . ? C27 N18 C29 128.3(4) . . ? N7 B1 N4 118.2(3) . . ? N7 B1 N1 107.9(3) . . ? N4 B1 N1 107.8(3) . . ? N7 B1 Rh1 107.1(3) . . ? N4 B1 Rh1 108.1(3) . . ? N1 B1 Rh1 107.3(3) . . ? N10 B2 N16 115.9(4) . . ? N10 B2 N13 108.2(3) . . ? N16 B2 N13 108.2(3) . . ? N10 B2 Rh2 107.3(3) . . ? N16 B2 Rh2 109.2(3) . . ? N13 B2 Rh2 107.7(3) . . ? N1 C1 N3 107.4(4) . . ? N1 C1 S1 122.1(3) . . ? N3 C1 S1 130.4(3) . . ? N2 C2 N3 110.2(4) . . ? N2 C2 C3 124.2(4) . . ? N3 C2 C3 125.5(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 110.7(3) . . ? N3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N6 107.5(4) . . ? N4 C6 S2 123.7(3) . . ? N6 C6 S2 128.7(4) . . ? N5 C7 N6 112.1(4) . . ? N5 C7 C8 124.3(5) . . ? N6 C7 C8 123.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 111.8(4) . . ? N6 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N6 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 N9 107.2(4) . . ? N7 C11 S3 122.4(3) . . ? N9 C11 S3 130.4(3) . . ? N8 C12 N9 111.9(4) . . ? N8 C12 C13 124.7(5) . . ? N9 C12 C13 123.4(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N9 C14 C15 114.6(4) . . ? N9 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N9 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N10 C16 N12 107.1(4) . . ? N10 C16 S4 123.6(3) . . ? N12 C16 S4 129.2(3) . . ? N11 C17 N12 111.6(4) . . ? N11 C17 C18 124.7(4) . . ? N12 C17 C18 123.7(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 C20 112.1(4) . . ? N12 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N12 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N13 C21 N15 107.1(4) . . ? N13 C21 S5 122.9(3) . . ? N15 C21 S5 130.0(3) . . ? N14 C22 N15 111.9(4) . . ? N14 C22 C23 124.5(4) . . ? N15 C22 C23 123.5(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N15 C24 C25 111.7(5) . . ? N15 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? N15 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N16 C26 N18 107.6(4) . . ? N16 C26 S6 123.8(4) . . ? N18 C26 S6 128.6(3) . . ? N17 C27 N18 111.6(4) . . ? N17 C27 C28 124.8(4) . . ? N18 C27 C28 123.6(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N18 C29 C30 112.3(4) . . ? N18 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? N18 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 110.3(4) . . ? C36 C31 P1 112.8(3) . . ? C32 C31 P1 110.8(3) . . ? C36 C31 H31 107.6 . . ? C32 C31 H31 107.6 . . ? P1 C31 H31 107.6 . . ? C33 C32 C31 110.5(4) . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 110.2(4) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C33 C34 C35 111.1(5) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 111.4(4) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 109.7(4) . . ? C31 C36 H36A 109.7 . . ? C35 C36 H36A 109.7 . . ? C31 C36 H36B 109.7 . . ? C35 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C38 C37 C42 108.1(3) . . ? C38 C37 P1 117.2(3) . . ? C42 C37 P1 117.4(3) . . ? C38 C37 H37 104.1 . . ? C42 C37 H37 104.1 . . ? P1 C37 H37 104.1 . . ? C39 C38 C37 109.6(4) . . ? C39 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? C39 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? C40 C39 C38 111.8(4) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C41 C40 C39 111.3(4) . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 110.7(4) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C41 C42 C37 109.5(4) . . ? C41 C42 H42A 109.8 . . ? C37 C42 H42A 109.8 . . ? C41 C42 H42B 109.8 . . ? C37 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C48 109.4(4) . . ? C44 C43 P1 115.7(3) . . ? C48 C43 P1 112.1(3) . . ? C44 C43 H43 106.3 . . ? C48 C43 H43 106.3 . . ? P1 C43 H43 106.3 . . ? C43 C44 C45 111.2(4) . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 111.2(5) . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C47 C46 C45 110.8(4) . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C46 C47 C48 110.2(4) . . ? C46 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? C46 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? C47 C48 C43 112.0(4) . . ? C47 C48 H48A 109.2 . . ? C43 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C43 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? F2 P2 F1 179.49(19) . . ? F2 P2 F4 90.38(17) . . ? F1 P2 F4 89.48(18) . . ? F2 P2 F5 89.23(16) . . ? F1 P2 F5 90.28(18) . . ? F4 P2 F5 89.90(16) . . ? F2 P2 F3 90.12(17) . . ? F1 P2 F3 90.02(18) . . ? F4 P2 F3 179.50(19) . . ? F5 P2 F3 90.13(17) . . ? F2 P2 F6 89.67(16) . . ? F1 P2 F6 90.82(18) . . ? F4 P2 F6 89.67(17) . . ? F5 P2 F6 178.82(17) . . ? F3 P2 F6 90.31(17) . . ? F11 P3 F10 89.7(4) . . ? F11 P3 F8 89.3(3) . . ? F10 P3 F8 87.4(3) . . ? F11 P3 F12 177.7(4) . . ? F10 P3 F12 92.3(3) . . ? F8 P3 F12 89.7(3) . . ? F11 P3 F7 91.2(4) . . ? F10 P3 F7 92.0(4) . . ? F8 P3 F7 179.3(3) . . ? F12 P3 F7 89.9(3) . . ? F11 P3 F9 88.7(4) . . ? F10 P3 F9 177.1(4) . . ? F8 P3 F9 90.2(3) . . ? F12 P3 F9 89.3(3) . . ? F7 P3 F9 90.4(3) . . ? Cl9 C54 Cl10 112.7(9) . . ? Cl9 C54 H54A 109.1 . . ? Cl10 C54 H54A 109.1 . . ? Cl9 C54 H54B 109.1 . . ? Cl10 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? F17 P4 F13 94.9(7) . . ? F17 P4 F18 177.7(7) . . ? F13 P4 F18 87.2(6) . . ? F17 P4 F15 91.1(6) . . ? F13 P4 F15 91.2(5) . . ? F18 P4 F15 89.7(5) . . ? F17 P4 F14 92.5(7) . . ? F13 P4 F14 172.5(6) . . ? F18 P4 F14 85.3(6) . . ? F15 P4 F14 89.7(5) . . ? F17 P4 F16 91.0(6) . . ? F13 P4 F16 88.5(5) . . ? F18 P4 F16 88.2(5) . . ? F15 P4 F16 177.9(5) . . ? F14 P4 F16 90.4(5) . . ? Cl3 C50 Cl4 115.6(5) . . ? Cl3 C50 H50A 108.4 . . ? Cl4 C50 H50A 108.4 . . ? Cl3 C50 H50B 108.4 . . ? Cl4 C50 H50B 108.4 . . ? H50A C50 H50B 107.4 . . ? Cl2 C49 Cl1 110.8(3) . . ? Cl2 C49 H49A 109.5 . . ? Cl1 C49 H49A 109.5 . . ? Cl2 C49 H49B 109.5 . . ? Cl1 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? Cl5 C51 Cl6 111.7(3) . . ? Cl5 C51 H51A 109.3 . . ? Cl6 C51 H51A 109.3 . . ? Cl5 C51 H51B 109.3 . . ? Cl6 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? Cl8 C52 Cl7 111.5(4) . . ? Cl8 C52 H52A 109.3 . . ? Cl7 C52 H52A 109.3 . . ? Cl8 C52 H52B 109.3 . . ? Cl7 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 Rh1 P1 C37 -73.2(2) . . . . ? S3 Rh1 P1 C37 -157.66(16) . . . . ? S2 Rh1 P1 C37 14.31(16) . . . . ? S1 Rh1 P1 C37 104.0(2) . . . . ? B1 Rh1 P1 C43 64.1(2) . . . . ? S3 Rh1 P1 C43 -20.33(17) . . . . ? S2 Rh1 P1 C43 151.64(17) . . . . ? S1 Rh1 P1 C43 -118.7(2) . . . . ? B1 Rh1 P1 C31 177.0(2) . . . . ? S3 Rh1 P1 C31 92.58(15) . . . . ? S2 Rh1 P1 C31 -95.44(15) . . . . ? S1 Rh1 P1 C31 -5.8(2) . . . . ? B2 Rh2 S1 C1 -102.4(2) . . . . ? S6 Rh2 S1 C1 -15.10(15) . . . . ? S4 Rh2 S1 C1 174.09(15) . . . . ? S2 Rh2 S1 C1 83.83(15) . . . . ? B2 Rh2 S1 Rh1 160.75(14) . . . . ? S6 Rh2 S1 Rh1 -111.99(5) . . . . ? S4 Rh2 S1 Rh1 77.20(5) . . . . ? S2 Rh2 S1 Rh1 -13.06(3) . . . . ? B1 Rh1 S1 C1 -7.99(19) . . . . ? P1 Rh1 S1 C1 174.7(2) . . . . ? S3 Rh1 S1 C1 75.93(14) . . . . ? S2 Rh1 S1 C1 -95.23(14) . . . . ? B1 Rh1 S1 Rh2 101.60(14) . . . . ? P1 Rh1 S1 Rh2 -75.68(18) . . . . ? S3 Rh1 S1 Rh2 -174.48(4) . . . . ? S2 Rh1 S1 Rh2 14.36(4) . . . . ? B1 Rh1 S2 C6 12.94(19) . . . . ? P1 Rh1 S2 C6 -90.27(15) . . . . ? S1 Rh1 S2 C6 102.01(15) . . . . ? B1 Rh1 S2 Rh2 -102.00(13) . . . . ? P1 Rh1 S2 Rh2 154.79(4) . . . . ? S1 Rh1 S2 Rh2 -12.93(3) . . . . ? S5 Rh2 S2 C6 105.74(17) . . . . ? S6 Rh2 S2 C6 13.08(17) . . . . ? S1 Rh2 S2 C6 -81.75(17) . . . . ? S4 Rh2 S2 C6 -161.86(17) . . . . ? S5 Rh2 S2 Rh1 -159.31(4) . . . . ? S6 Rh2 S2 Rh1 108.03(5) . . . . ? S1 Rh2 S2 Rh1 13.20(4) . . . . ? S4 Rh2 S2 Rh1 -66.91(4) . . . . ? B1 Rh1 S3 C11 -23.71(19) . . . . ? P1 Rh1 S3 C11 79.32(15) . . . . ? S1 Rh1 S3 C11 -112.83(15) . . . . ? B2 Rh2 S4 C16 -21.35(19) . . . . ? S5 Rh2 S4 C16 -109.64(14) . . . . ? S1 Rh2 S4 C16 75.47(14) . . . . ? S2 Rh2 S4 C16 159.02(14) . . . . ? B2 Rh2 S5 C21 -5.2(2) . . . . ? S6 Rh2 S5 C21 -91.85(16) . . . . ? S4 Rh2 S5 C21 79.40(16) . . . . ? S2 Rh2 S5 C21 168.59(16) . . . . ? B2 Rh2 S6 C26 8.94(19) . . . . ? S5 Rh2 S6 C26 97.32(15) . . . . ? S1 Rh2 S6 C26 -86.53(15) . . . . ? S2 Rh2 S6 C26 -170.89(14) . . . . ? C1 N1 N2 C2 0.2(5) . . . . ? B1 N1 N2 C2 -176.4(4) . . . . ? C6 N4 N5 C7 -0.8(5) . . . . ? B1 N4 N5 C7 -168.3(4) . . . . ? C11 N7 N8 C12 1.1(5) . . . . ? B1 N7 N8 C12 161.6(4) . . . . ? C16 N10 N11 C17 2.1(4) . . . . ? B2 N10 N11 C17 161.2(4) . . . . ? C21 N13 N14 C22 -0.2(5) . . . . ? B2 N13 N14 C22 176.9(4) . . . . ? C26 N16 N17 C27 -1.5(5) . . . . ? B2 N16 N17 C27 -157.3(4) . . . . ? C11 N7 B1 N4 -160.1(4) . . . . ? N8 N7 B1 N4 40.5(6) . . . . ? C11 N7 B1 N1 77.5(4) . . . . ? N8 N7 B1 N1 -81.9(5) . . . . ? C11 N7 B1 Rh1 -37.9(4) . . . . ? N8 N7 B1 Rh1 162.8(3) . . . . ? C6 N4 B1 N7 147.8(4) . . . . ? N5 N4 B1 N7 -45.8(6) . . . . ? C6 N4 B1 N1 -89.7(4) . . . . ? N5 N4 B1 N1 76.7(5) . . . . ? C6 N4 B1 Rh1 26.0(5) . . . . ? N5 N4 B1 Rh1 -167.6(3) . . . . ? C1 N1 B1 N7 -118.9(4) . . . . ? N2 N1 B1 N7 57.1(5) . . . . ? C1 N1 B1 N4 112.4(4) . . . . ? N2 N1 B1 N4 -71.5(5) . . . . ? C1 N1 B1 Rh1 -3.7(5) . . . . ? N2 N1 B1 Rh1 172.3(3) . . . . ? P1 Rh1 B1 N7 -57.9(3) . . . . ? S3 Rh1 B1 N7 33.8(3) . . . . ? S2 Rh1 B1 N7 -149.0(3) . . . . ? S1 Rh1 B1 N7 122.7(3) . . . . ? P1 Rh1 B1 N4 70.4(3) . . . . ? S3 Rh1 B1 N4 162.1(3) . . . . ? S2 Rh1 B1 N4 -20.6(3) . . . . ? S1 Rh1 B1 N4 -109.0(3) . . . . ? P1 Rh1 B1 N1 -173.6(2) . . . . ? S3 Rh1 B1 N1 -81.9(3) . . . . ? S2 Rh1 B1 N1 95.3(3) . . . . ? S1 Rh1 B1 N1 7.0(3) . . . . ? C16 N10 B2 N16 -157.1(4) . . . . ? N11 N10 B2 N16 45.0(6) . . . . ? C16 N10 B2 N13 81.2(4) . . . . ? N11 N10 B2 N13 -76.7(5) . . . . ? C16 N10 B2 Rh2 -34.8(4) . . . . ? N11 N10 B2 Rh2 167.3(3) . . . . ? C26 N16 B2 N10 147.0(4) . . . . ? N17 N16 B2 N10 -59.2(5) . . . . ? C26 N16 B2 N13 -91.3(4) . . . . ? N17 N16 B2 N13 62.5(5) . . . . ? C26 N16 B2 Rh2 25.7(5) . . . . ? N17 N16 B2 Rh2 179.5(3) . . . . ? C21 N13 B2 N10 -123.4(4) . . . . ? N14 N13 B2 N10 59.8(5) . . . . ? C21 N13 B2 N16 110.3(4) . . . . ? N14 N13 B2 N16 -66.5(5) . . . . ? C21 N13 B2 Rh2 -7.6(5) . . . . ? N14 N13 B2 Rh2 175.5(3) . . . . ? S5 Rh2 B2 N10 123.2(3) . . . . ? S6 Rh2 B2 N10 -144.3(3) . . . . ? S1 Rh2 B2 N10 -48.8(3) . . . . ? S4 Rh2 B2 N10 30.6(3) . . . . ? S5 Rh2 B2 N16 -110.4(3) . . . . ? S6 Rh2 B2 N16 -17.9(3) . . . . ? S1 Rh2 B2 N16 77.6(3) . . . . ? S4 Rh2 B2 N16 157.0(3) . . . . ? S5 Rh2 B2 N13 6.9(3) . . . . ? S6 Rh2 B2 N13 99.3(3) . . . . ? S1 Rh2 B2 N13 -165.2(3) . . . . ? S4 Rh2 B2 N13 -85.7(3) . . . . ? N2 N1 C1 N3 0.2(5) . . . . ? B1 N1 C1 N3 176.7(4) . . . . ? N2 N1 C1 S1 178.8(3) . . . . ? B1 N1 C1 S1 -4.7(6) . . . . ? C2 N3 C1 N1 -0.5(5) . . . . ? C4 N3 C1 N1 -170.9(4) . . . . ? C2 N3 C1 S1 -179.0(3) . . . . ? C4 N3 C1 S1 10.6(6) . . . . ? Rh2 S1 C1 N1 -88.4(3) . . . . ? Rh1 S1 C1 N1 8.8(4) . . . . ? Rh2 S1 C1 N3 89.9(4) . . . . ? Rh1 S1 C1 N3 -172.9(4) . . . . ? N1 N2 C2 N3 -0.5(5) . . . . ? N1 N2 C2 C3 179.6(4) . . . . ? C1 N3 C2 N2 0.6(5) . . . . ? C4 N3 C2 N2 170.9(4) . . . . ? C1 N3 C2 C3 -179.5(4) . . . . ? C4 N3 C2 C3 -9.2(7) . . . . ? C1 N3 C4 C5 90.4(5) . . . . ? C2 N3 C4 C5 -78.2(5) . . . . ? N5 N4 C6 N6 0.9(5) . . . . ? B1 N4 C6 N6 169.3(4) . . . . ? N5 N4 C6 S2 176.6(3) . . . . ? B1 N4 C6 S2 -14.9(6) . . . . ? C7 N6 C6 N4 -0.6(5) . . . . ? C9 N6 C6 N4 179.9(4) . . . . ? C7 N6 C6 S2 -176.1(4) . . . . ? C9 N6 C6 S2 4.4(7) . . . . ? Rh1 S2 C6 N4 -3.0(4) . . . . ? Rh2 S2 C6 N4 89.0(4) . . . . ? Rh1 S2 C6 N6 171.8(4) . . . . ? Rh2 S2 C6 N6 -96.2(4) . . . . ? N4 N5 C7 N6 0.4(5) . . . . ? N4 N5 C7 C8 -178.8(5) . . . . ? C6 N6 C7 N5 0.1(5) . . . . ? C9 N6 C7 N5 179.6(4) . . . . ? C6 N6 C7 C8 179.3(5) . . . . ? C9 N6 C7 C8 -1.2(8) . . . . ? C6 N6 C9 C10 83.2(6) . . . . ? C7 N6 C9 C10 -96.2(6) . . . . ? N8 N7 C11 N9 -1.4(5) . . . . ? B1 N7 C11 N9 -164.5(3) . . . . ? N8 N7 C11 S3 178.9(3) . . . . ? B1 N7 C11 S3 15.8(5) . . . . ? C12 N9 C11 N7 1.1(5) . . . . ? C14 N9 C11 N7 173.6(4) . . . . ? C12 N9 C11 S3 -179.3(3) . . . . ? C14 N9 C11 S3 -6.7(7) . . . . ? Rh1 S3 C11 N7 11.3(4) . . . . ? Rh1 S3 C11 N9 -168.3(4) . . . . ? N7 N8 C12 N9 -0.4(5) . . . . ? N7 N8 C12 C13 178.5(4) . . . . ? C11 N9 C12 N8 -0.5(5) . . . . ? C14 N9 C12 N8 -172.8(4) . . . . ? C11 N9 C12 C13 -179.4(4) . . . . ? C14 N9 C12 C13 8.3(7) . . . . ? C11 N9 C14 C15 64.9(6) . . . . ? C12 N9 C14 C15 -124.2(5) . . . . ? N11 N10 C16 N12 -1.6(5) . . . . ? B2 N10 C16 N12 -163.1(3) . . . . ? N11 N10 C16 S4 176.7(3) . . . . ? B2 N10 C16 S4 15.2(5) . . . . ? C17 N12 C16 N10 0.4(4) . . . . ? C19 N12 C16 N10 -179.7(4) . . . . ? C17 N12 C16 S4 -177.8(3) . . . . ? C19 N12 C16 S4 2.2(7) . . . . ? Rh2 S4 C16 N10 9.6(4) . . . . ? Rh2 S4 C16 N12 -172.5(4) . . . . ? N10 N11 C17 N12 -1.8(5) . . . . ? N10 N11 C17 C18 177.9(4) . . . . ? C16 N12 C17 N11 0.9(5) . . . . ? C19 N12 C17 N11 -179.0(4) . . . . ? C16 N12 C17 C18 -178.7(4) . . . . ? C19 N12 C17 C18 1.3(7) . . . . ? C16 N12 C19 C20 89.8(6) . . . . ? C17 N12 C19 C20 -90.3(6) . . . . ? N14 N13 C21 N15 0.5(5) . . . . ? B2 N13 C21 N15 -176.7(4) . . . . ? N14 N13 C21 S5 -179.8(3) . . . . ? B2 N13 C21 S5 3.0(6) . . . . ? C22 N15 C21 N13 -0.6(5) . . . . ? C24 N15 C21 N13 -177.7(4) . . . . ? C22 N15 C21 S5 179.7(4) . . . . ? C24 N15 C21 S5 2.6(7) . . . . ? Rh2 S5 C21 N13 2.8(4) . . . . ? Rh2 S5 C21 N15 -177.6(4) . . . . ? N13 N14 C22 N15 -0.1(5) . . . . ? N13 N14 C22 C23 179.6(4) . . . . ? C21 N15 C22 N14 0.4(5) . . . . ? C24 N15 C22 N14 177.5(5) . . . . ? C21 N15 C22 C23 -179.3(5) . . . . ? C24 N15 C22 C23 -2.3(8) . . . . ? C21 N15 C24 C25 80.3(6) . . . . ? C22 N15 C24 C25 -96.2(6) . . . . ? N17 N16 C26 N18 1.3(5) . . . . ? B2 N16 C26 N18 159.0(4) . . . . ? N17 N16 C26 S6 -176.8(3) . . . . ? B2 N16 C26 S6 -19.1(5) . . . . ? C27 N18 C26 N16 -0.5(5) . . . . ? C29 N18 C26 N16 179.5(4) . . . . ? C27 N18 C26 S6 177.5(3) . . . . ? C29 N18 C26 S6 -2.5(7) . . . . ? Rh2 S6 C26 N16 2.7(4) . . . . ? Rh2 S6 C26 N18 -175.0(4) . . . . ? N16 N17 C27 N18 1.2(5) . . . . ? N16 N17 C27 C28 178.9(4) . . . . ? C26 N18 C27 N17 -0.5(5) . . . . ? C29 N18 C27 N17 179.5(4) . . . . ? C26 N18 C27 C28 -178.2(4) . . . . ? C29 N18 C27 C28 1.8(7) . . . . ? C26 N18 C29 C30 -81.9(6) . . . . ? C27 N18 C29 C30 98.1(5) . . . . ? C37 P1 C31 C36 -52.0(4) . . . . ? C43 P1 C31 C36 -165.4(3) . . . . ? Rh1 P1 C31 C36 69.9(3) . . . . ? C37 P1 C31 C32 -176.1(3) . . . . ? C43 P1 C31 C32 70.5(4) . . . . ? Rh1 P1 C31 C32 -54.2(3) . . . . ? C36 C31 C32 C33 58.6(5) . . . . ? P1 C31 C32 C33 -175.9(3) . . . . ? C31 C32 C33 C34 -58.0(6) . . . . ? C32 C33 C34 C35 56.9(7) . . . . ? C33 C34 C35 C36 -56.8(7) . . . . ? C32 C31 C36 C35 -57.3(5) . . . . ? P1 C31 C36 C35 178.3(4) . . . . ? C34 C35 C36 C31 56.5(6) . . . . ? C43 P1 C37 C38 60.8(4) . . . . ? C31 P1 C37 C38 -49.1(4) . . . . ? Rh1 P1 C37 C38 -157.5(3) . . . . ? C43 P1 C37 C42 -70.4(4) . . . . ? C31 P1 C37 C42 179.6(3) . . . . ? Rh1 P1 C37 C42 71.2(4) . . . . ? C42 C37 C38 C39 -61.0(5) . . . . ? P1 C37 C38 C39 163.6(3) . . . . ? C37 C38 C39 C40 56.8(6) . . . . ? C38 C39 C40 C41 -53.3(6) . . . . ? C39 C40 C41 C42 54.4(6) . . . . ? C40 C41 C42 C37 -59.8(5) . . . . ? C38 C37 C42 C41 62.8(5) . . . . ? P1 C37 C42 C41 -161.9(3) . . . . ? C37 P1 C43 C44 -77.1(4) . . . . ? C31 P1 C43 C44 31.6(4) . . . . ? Rh1 P1 C43 C44 142.1(3) . . . . ? C37 P1 C43 C48 49.3(4) . . . . ? C31 P1 C43 C48 157.9(3) . . . . ? Rh1 P1 C43 C48 -91.6(3) . . . . ? C48 C43 C44 C45 55.4(5) . . . . ? P1 C43 C44 C45 -176.8(4) . . . . ? C43 C44 C45 C46 -56.3(6) . . . . ? C44 C45 C46 C47 56.5(6) . . . . ? C45 C46 C47 C48 -56.9(6) . . . . ? C46 C47 C48 C43 57.8(5) . . . . ? C44 C43 C48 C47 -56.9(5) . . . . ? P1 C43 C48 C47 173.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.603 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.200 data_15 _database_code_depnum_ccdc_archive 'CCDC 733509' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H39 B1 I1 N9 P1 Rh1 S3, 3(C H2 Cl2)' _chemical_formula_sum 'C36 H45 B1 Cl6 I1 N9 P1 Rh1 S3' _chemical_formula_weight 1184.33 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4896(4) _cell_length_b 20.7416(8) _cell_length_c 21.9597(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.1850(10) _cell_angle_gamma 90.00 _cell_volume 4774.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 12006 _cell_measurement_theta_min 2.173 _cell_measurement_theta_max 26.908 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.663733 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50648 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10955 _reflns_number_gt 7895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction 'SAINT v7.06A (Bruker-AXS, 1997-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0374P)^2^+13.1239P] 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 10955 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.005 _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 0.28278(3) 0.235595(16) 0.280717(15) 0.01584(8) Uani 1 1 d . . . I1 I 0.47336(3) 0.173117(15) 0.205985(15) 0.02663(9) Uani 1 1 d . . . S1 S 0.38570(11) 0.32846(5) 0.23893(5) 0.0231(2) Uani 1 1 d . . . S2 S 0.43151(10) 0.23282(6) 0.36479(5) 0.0231(2) Uani 1 1 d . . . S3 S 0.10649(11) 0.24993(5) 0.21061(5) 0.0246(3) Uani 1 1 d . . . P1 P 0.18010(11) 0.14211(5) 0.31206(5) 0.0194(2) Uani 1 1 d . . . N1 N 0.2325(3) 0.36847(16) 0.32569(16) 0.0174(8) Uani 1 1 d . . . N2 N 0.1920(4) 0.42379(17) 0.35581(18) 0.0245(9) Uani 1 1 d . . . N3 N 0.3294(4) 0.44896(17) 0.28557(17) 0.0216(8) Uani 1 1 d . . . N4 N 0.2138(3) 0.28149(16) 0.40426(16) 0.0187(8) Uani 1 1 d . . . N5 N 0.1520(4) 0.29927(18) 0.45668(18) 0.0264(9) Uani 1 1 d . . . N6 N 0.3422(4) 0.25856(19) 0.47982(18) 0.0278(9) Uani 1 1 d . . . N7 N 0.0403(3) 0.29731(17) 0.31866(18) 0.0204(8) Uani 1 1 d . . . N8 N -0.0642(4) 0.31863(19) 0.3503(2) 0.0309(10) Uani 1 1 d . . . N9 N -0.1231(4) 0.29049(19) 0.2561(2) 0.0310(10) Uani 1 1 d . . . B1 B 0.1821(5) 0.2989(2) 0.3372(2) 0.0169(10) Uani 1 1 d . . . C1 C 0.3149(4) 0.3836(2) 0.2836(2) 0.0191(9) Uani 1 1 d . . . C2 C 0.2524(4) 0.4712(2) 0.3298(2) 0.0246(10) Uani 1 1 d . . . C3 C 0.2405(5) 0.5405(2) 0.3458(3) 0.0368(13) Uani 1 1 d . . . H3A H 0.1894 0.5448 0.3809 0.055 Uiso 1 1 calc R . . H3B H 0.2006 0.5633 0.3121 0.055 Uiso 1 1 calc R . . H3C H 0.3237 0.5582 0.3546 0.055 Uiso 1 1 calc R . . C4 C 0.4202(5) 0.4854(2) 0.2493(2) 0.0305(12) Uani 1 1 d . . . H4A H 0.3900 0.5293 0.2441 0.037 Uiso 1 1 calc R . . H4B H 0.4245 0.4660 0.2092 0.037 Uiso 1 1 calc R . . C5 C 0.5517(5) 0.4862(3) 0.2796(3) 0.0450(15) Uani 1 1 d . . . H5A H 0.5475 0.5045 0.3196 0.068 Uiso 1 1 calc R . . H5B H 0.6077 0.5116 0.2557 0.068 Uiso 1 1 calc R . . H5C H 0.5838 0.4429 0.2827 0.068 Uiso 1 1 calc R . . C6 C 0.3291(4) 0.2573(2) 0.4179(2) 0.0221(10) Uani 1 1 d . . . C7 C 0.2303(5) 0.2836(2) 0.5012(2) 0.0297(11) Uani 1 1 d . . . C8 C 0.2032(6) 0.2888(3) 0.5669(2) 0.0449(15) Uani 1 1 d . . . H8A H 0.1296 0.3156 0.5716 0.067 Uiso 1 1 calc R . . H8B H 0.2754 0.3076 0.5885 0.067 Uiso 1 1 calc R . . H8C H 0.1871 0.2467 0.5829 0.067 Uiso 1 1 calc R . . C9 C 0.4559(6) 0.2368(3) 0.5148(3) 0.0453(15) Uani 1 1 d . . . H9A H 0.4642 0.2613 0.5523 0.054 Uiso 1 1 calc R . . H9B H 0.5309 0.2451 0.4915 0.054 Uiso 1 1 calc R . . C10 C 0.4500(9) 0.1663(3) 0.5296(4) 0.087(3) Uani 1 1 d . . . H10A H 0.3796 0.1584 0.5553 0.130 Uiso 1 1 calc R . . H10B H 0.5280 0.1534 0.5505 0.130 Uiso 1 1 calc R . . H10C H 0.4387 0.1419 0.4926 0.130 Uiso 1 1 calc R . . C11 C 0.0044(4) 0.2805(2) 0.2618(2) 0.0221(10) Uani 1 1 d . . . C12 C -0.1598(5) 0.3128(2) 0.3111(3) 0.0343(13) Uani 1 1 d . . . C13 C -0.2941(5) 0.3270(3) 0.3258(4) 0.060(2) Uani 1 1 d . . . H13A H -0.3221 0.2964 0.3554 0.091 Uiso 1 1 calc R . . H13B H -0.3475 0.3238 0.2895 0.091 Uiso 1 1 calc R . . H13C H -0.2995 0.3698 0.3422 0.091 Uiso 1 1 calc R . . C14 C -0.2033(5) 0.2750(3) 0.2016(3) 0.0515(17) Uani 1 1 d . . . H14A H -0.2831 0.2566 0.2142 0.062 Uiso 1 1 calc R . . H14B H -0.1604 0.2428 0.1778 0.062 Uiso 1 1 calc R . . C15 C -0.2310(8) 0.3328(4) 0.1627(4) 0.077(2) Uani 1 1 d . . . H15A H -0.2798 0.3633 0.1850 0.116 Uiso 1 1 calc R . . H15B H -0.2788 0.3199 0.1266 0.116 Uiso 1 1 calc R . . H15C H -0.1522 0.3523 0.1515 0.116 Uiso 1 1 calc R . . C16 C 0.2634(5) 0.0896(2) 0.3680(2) 0.0253(10) Uani 1 1 d . . . C17 C 0.3929(5) 0.0776(2) 0.3604(2) 0.0311(12) Uani 1 1 d . . . H17 H 0.4370 0.1003 0.3313 0.037 Uiso 1 1 calc R . . C18 C 0.4553(6) 0.0316(3) 0.3962(3) 0.0446(15) Uani 1 1 d . . . H18 H 0.5415 0.0239 0.3910 0.054 Uiso 1 1 calc R . . C19 C 0.3929(7) -0.0029(3) 0.4392(3) 0.0535(18) Uani 1 1 d . . . H19 H 0.4365 -0.0338 0.4626 0.064 Uiso 1 1 calc R . . C20 C 0.2649(7) 0.0083(3) 0.4478(3) 0.0494(16) Uani 1 1 d . . . H20 H 0.2222 -0.0147 0.4771 0.059 Uiso 1 1 calc R . . C21 C 0.2005(6) 0.0543(2) 0.4124(2) 0.0373(13) Uani 1 1 d . . . H21 H 0.1144 0.0618 0.4182 0.045 Uiso 1 1 calc R . . C22 C 0.1462(4) 0.0809(2) 0.2525(2) 0.0233(10) Uani 1 1 d . . . C23 C 0.0983(5) 0.0213(2) 0.2692(2) 0.0309(11) Uani 1 1 d . . . H23 H 0.0838 0.0133 0.3101 0.037 Uiso 1 1 calc R . . C24 C 0.0717(5) -0.0260(2) 0.2270(3) 0.0338(12) Uani 1 1 d . . . H24 H 0.0404 -0.0657 0.2392 0.041 Uiso 1 1 calc R . . C25 C 0.0920(5) -0.0140(2) 0.1655(2) 0.0313(12) Uani 1 1 d . . . H25 H 0.0741 -0.0456 0.1363 0.038 Uiso 1 1 calc R . . C26 C 0.1389(5) 0.0452(2) 0.1485(2) 0.0322(12) Uani 1 1 d . . . H26 H 0.1524 0.0535 0.1076 0.039 Uiso 1 1 calc R . . C27 C 0.1658(5) 0.0918(2) 0.1912(2) 0.0263(11) Uani 1 1 d . . . H27 H 0.1976 0.1314 0.1789 0.032 Uiso 1 1 calc R . . C28 C 0.0209(4) 0.1513(2) 0.3430(2) 0.0231(10) Uani 1 1 d . . . C29 C 0.0058(5) 0.1684(2) 0.4038(2) 0.0286(11) Uani 1 1 d . . . H29 H 0.0774 0.1755 0.4292 0.034 Uiso 1 1 calc R . . C30 C -0.1152(5) 0.1749(2) 0.4268(3) 0.0373(13) Uani 1 1 d . . . H30 H -0.1239 0.1859 0.4675 0.045 Uiso 1 1 calc R . . C31 C -0.2225(5) 0.1651(2) 0.3897(3) 0.0422(15) Uani 1 1 d . . . H31 H -0.3032 0.1688 0.4054 0.051 Uiso 1 1 calc R . . C32 C -0.2092(5) 0.1499(2) 0.3293(3) 0.0369(13) Uani 1 1 d . . . H32 H -0.2813 0.1445 0.3038 0.044 Uiso 1 1 calc R . . C33 C -0.0885(5) 0.1427(2) 0.3059(2) 0.0292(11) Uani 1 1 d . . . H33 H -0.0808 0.1321 0.2650 0.035 Uiso 1 1 calc R . . C34 C 0.3798(6) 0.4386(3) 0.4798(3) 0.0461(15) Uani 1 1 d . . . H34A H 0.2945 0.4229 0.4697 0.055 Uiso 1 1 calc R . . H34B H 0.3790 0.4852 0.4759 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.42207(18) 0.41764(9) 0.55526(7) 0.0605(5) Uani 1 1 d . . . Cl2 Cl 0.48699(16) 0.40594(8) 0.42893(7) 0.0526(4) Uani 1 1 d . . . C35 C 0.1429(10) 0.8536(5) 0.0122(4) 0.103(3) Uani 1 1 d . . . H35A H 0.2134 0.8521 0.0420 0.124 Uiso 1 1 calc R . . H35B H 0.0713 0.8317 0.0298 0.124 Uiso 1 1 calc R . . Cl3 Cl 0.1848(3) 0.81202(12) -0.04935(12) 0.1078(9) Uani 1 1 d . . . Cl4 Cl 0.1019(4) 0.93234(14) 0.00071(13) 0.1538(15) Uani 1 1 d . . . C36 C 0.8602(9) 0.9084(4) 0.3727(4) 0.088(3) Uani 1 1 d . . . H36A H 0.9124 0.8977 0.3385 0.106 Uiso 1 1 calc R . . H36B H 0.7804 0.8850 0.3674 0.106 Uiso 1 1 calc R . . Cl6 Cl 0.82871(17) 0.98892(9) 0.37099(9) 0.0677(5) Uani 1 1 d . . . Cl7 Cl 0.9382(2) 0.88219(10) 0.43962(9) 0.0841(6) 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 0.01438(17) 0.01542(16) 0.01760(18) -0.00156(13) -0.00096(13) 0.00004(13) I1 0.02092(16) 0.02874(17) 0.03043(18) -0.00800(13) 0.00364(13) 0.00187(13) S1 0.0227(6) 0.0224(6) 0.0246(6) -0.0008(5) 0.0066(5) -0.0038(5) S2 0.0159(5) 0.0286(6) 0.0245(6) -0.0030(5) -0.0035(5) 0.0012(5) S3 0.0255(6) 0.0245(6) 0.0232(6) 0.0003(5) -0.0069(5) -0.0007(5) P1 0.0193(6) 0.0177(6) 0.0210(6) -0.0004(5) -0.0022(5) 0.0010(5) N1 0.0134(18) 0.0150(18) 0.024(2) -0.0019(15) 0.0020(15) -0.0013(14) N2 0.023(2) 0.0176(19) 0.033(2) -0.0031(17) 0.0032(18) 0.0009(16) N3 0.023(2) 0.0137(18) 0.028(2) 0.0014(15) 0.0006(17) -0.0048(15) N4 0.0197(19) 0.0153(18) 0.021(2) -0.0015(14) 0.0028(16) -0.0012(14) N5 0.034(2) 0.023(2) 0.022(2) -0.0054(17) 0.0088(19) -0.0049(18) N6 0.034(2) 0.027(2) 0.022(2) 0.0014(17) -0.0097(18) -0.0050(18) N7 0.0109(18) 0.0194(19) 0.031(2) 0.0042(16) 0.0013(16) 0.0009(15) N8 0.022(2) 0.025(2) 0.046(3) 0.0037(19) 0.013(2) 0.0016(17) N9 0.017(2) 0.024(2) 0.050(3) 0.006(2) -0.009(2) -0.0013(17) B1 0.013(2) 0.013(2) 0.024(3) -0.0012(19) 0.001(2) 0.0031(18) C1 0.017(2) 0.017(2) 0.023(2) 0.0020(18) -0.0042(19) -0.0029(17) C2 0.022(2) 0.019(2) 0.033(3) 0.001(2) -0.005(2) 0.0001(19) C3 0.043(3) 0.014(2) 0.053(4) -0.002(2) 0.005(3) -0.001(2) C4 0.030(3) 0.024(3) 0.038(3) 0.009(2) 0.004(2) -0.008(2) C5 0.027(3) 0.036(3) 0.072(4) 0.012(3) 0.000(3) -0.011(2) C6 0.023(2) 0.020(2) 0.024(2) 0.0018(18) -0.0033(19) -0.0081(19) C7 0.042(3) 0.025(3) 0.023(3) -0.004(2) 0.005(2) -0.007(2) C8 0.064(4) 0.046(3) 0.026(3) -0.005(3) 0.010(3) -0.013(3) C9 0.047(4) 0.052(4) 0.035(3) -0.004(3) -0.022(3) 0.007(3) C10 0.117(7) 0.046(4) 0.094(6) 0.004(4) -0.053(6) 0.016(4) C11 0.017(2) 0.016(2) 0.033(3) 0.0054(19) -0.006(2) -0.0028(17) C12 0.014(2) 0.025(3) 0.063(4) 0.008(2) -0.001(2) -0.002(2) C13 0.013(3) 0.056(4) 0.112(6) 0.019(4) 0.012(3) 0.007(3) C14 0.025(3) 0.058(4) 0.070(5) -0.001(3) -0.023(3) -0.009(3) C15 0.069(5) 0.086(6) 0.074(5) 0.021(4) -0.033(4) 0.004(4) C16 0.030(3) 0.020(2) 0.026(3) -0.0010(19) -0.005(2) 0.000(2) C17 0.031(3) 0.030(3) 0.031(3) -0.004(2) -0.006(2) 0.007(2) C18 0.048(4) 0.043(3) 0.042(4) -0.008(3) -0.016(3) 0.023(3) C19 0.079(5) 0.034(3) 0.046(4) 0.005(3) -0.022(4) 0.022(3) C20 0.065(4) 0.039(3) 0.043(4) 0.015(3) -0.009(3) 0.008(3) C21 0.046(3) 0.031(3) 0.035(3) 0.009(2) 0.001(3) 0.006(2) C22 0.018(2) 0.020(2) 0.032(3) -0.004(2) -0.001(2) 0.0011(18) C23 0.034(3) 0.026(3) 0.032(3) 0.003(2) 0.003(2) -0.006(2) C24 0.035(3) 0.016(2) 0.051(4) -0.008(2) 0.007(3) -0.009(2) C25 0.031(3) 0.027(3) 0.037(3) -0.013(2) 0.000(2) 0.000(2) C26 0.031(3) 0.035(3) 0.031(3) -0.003(2) 0.000(2) -0.009(2) C27 0.030(3) 0.020(2) 0.029(3) 0.001(2) 0.003(2) 0.001(2) C28 0.022(2) 0.019(2) 0.028(3) 0.0020(19) 0.003(2) -0.0001(18) C29 0.028(3) 0.023(2) 0.035(3) 0.002(2) 0.005(2) 0.002(2) C30 0.042(3) 0.030(3) 0.041(3) 0.006(2) 0.017(3) 0.001(2) C31 0.032(3) 0.028(3) 0.068(4) 0.006(3) 0.016(3) 0.006(2) C32 0.022(3) 0.027(3) 0.061(4) 0.009(3) -0.002(3) 0.001(2) C33 0.026(3) 0.024(2) 0.038(3) 0.004(2) -0.001(2) 0.003(2) C34 0.061(4) 0.036(3) 0.042(4) -0.002(3) 0.007(3) -0.003(3) Cl1 0.0787(12) 0.0624(10) 0.0400(9) -0.0021(8) -0.0005(8) -0.0207(9) Cl2 0.0552(10) 0.0558(9) 0.0468(9) -0.0039(7) 0.0022(8) 0.0010(8) C35 0.125(8) 0.108(7) 0.079(6) 0.009(5) 0.036(6) -0.048(6) Cl3 0.150(2) 0.0886(16) 0.0875(17) 0.0105(13) 0.0451(17) 0.0087(16) Cl4 0.288(5) 0.0909(19) 0.0894(19) -0.0056(15) 0.096(2) -0.014(2) C36 0.129(8) 0.052(5) 0.080(6) 0.000(4) -0.039(5) 0.000(5) Cl6 0.0553(11) 0.0573(11) 0.0902(14) 0.0116(10) -0.0015(10) 0.0024(8) Cl7 0.1130(18) 0.0759(13) 0.0618(12) 0.0113(10) -0.0179(12) 0.0123(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 B1 2.117(5) . ? Rh1 P1 2.3346(12) . ? Rh1 S1 2.4070(12) . ? Rh1 S2 2.3720(12) . ? Rh1 S3 2.3794(12) . ? Rh1 I1 2.9359(5) . ? S1 C1 1.696(5) . ? S2 C6 1.693(5) . ? S3 C11 1.705(5) . ? P1 C16 1.838(5) . ? P1 C22 1.849(5) . ? P1 C28 1.837(5) . ? N1 B1 1.561(6) . ? N1 C1 1.327(5) . ? N2 C2 1.312(6) . ? N2 N1 1.399(5) . ? N3 C1 1.365(5) . ? N3 C2 1.368(6) . ? N3 C4 1.473(6) . ? N4 C6 1.333(6) . ? N4 B1 1.539(6) . ? N5 C7 1.295(6) . ? N5 N4 1.393(5) . ? N6 C6 1.362(6) . ? N6 C7 1.382(6) . ? N6 C9 1.465(6) . ? N7 C11 1.336(6) . ? N7 N8 1.392(5) . ? N7 B1 1.527(6) . ? N8 C12 1.301(7) . ? N9 C11 1.355(6) . ? N9 C12 1.364(7) . ? N9 C14 1.470(7) . ? C2 C3 1.486(6) . ? C4 C5 1.508(7) . ? C7 C8 1.484(7) . ? C10 C9 1.500(9) . ? Cl1 C34 1.753(6) . ? C12 C13 1.486(7) . ? Cl2 C34 1.752(6) . ? Cl3 C35 1.675(9) . ? C14 C15 1.496(9) . ? Cl4 C35 1.705(10) . ? C16 C21 1.403(7) . ? C17 C18 1.386(7) . ? C17 C16 1.398(7) . ? Cl6 C36 1.703(8) . ? Cl7 C36 1.742(8) . ? C18 C19 1.370(9) . ? C19 C20 1.383(9) . ? C21 C20 1.389(7) . ? C23 C24 1.372(7) . ? C23 C22 1.389(6) . ? C24 C25 1.398(7) . ? C26 C25 1.380(7) . ? C27 C26 1.368(7) . ? C27 C22 1.388(7) . ? C29 C28 1.397(7) . ? C30 C31 1.378(8) . ? C30 C29 1.390(7) . ? C32 C31 1.376(8) . ? C33 C32 1.392(7) . ? C33 C28 1.394(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Rh1 P1 95.53(14) . . ? B1 Rh1 S2 83.49(14) . . ? P1 Rh1 S2 92.72(4) . . ? B1 Rh1 S3 84.79(14) . . ? P1 Rh1 S3 86.48(4) . . ? S2 Rh1 S3 168.12(4) . . ? B1 Rh1 S1 88.18(14) . . ? P1 Rh1 S1 174.73(4) . . ? S2 Rh1 S1 91.42(4) . . ? S3 Rh1 S1 90.13(4) . . ? B1 Rh1 I1 165.29(13) . . ? P1 Rh1 I1 97.46(3) . . ? S2 Rh1 I1 89.01(3) . . ? S3 Rh1 I1 102.85(3) . . ? S1 Rh1 I1 79.35(3) . . ? C1 S1 Rh1 96.10(15) . . ? C6 S2 Rh1 96.49(16) . . ? C11 S3 Rh1 96.42(16) . . ? C28 P1 C16 103.3(2) . . ? C28 P1 C22 100.4(2) . . ? C16 P1 C22 98.0(2) . . ? C28 P1 Rh1 117.34(15) . . ? C16 P1 Rh1 118.47(16) . . ? C22 P1 Rh1 116.14(16) . . ? N7 B1 N4 115.0(4) . . ? N7 B1 N1 108.0(3) . . ? N4 B1 N1 108.1(3) . . ? N7 B1 Rh1 109.4(3) . . ? N4 B1 Rh1 108.7(3) . . ? N1 B1 Rh1 107.4(3) . . ? C1 N1 N2 110.7(3) . . ? C1 N1 B1 124.4(4) . . ? N2 N1 B1 124.8(3) . . ? C2 N2 N1 104.4(4) . . ? C1 N3 C2 106.8(4) . . ? C1 N3 C4 124.5(4) . . ? C2 N3 C4 128.5(4) . . ? C6 N4 N5 111.2(4) . . ? C6 N4 B1 117.7(4) . . ? N5 N4 B1 129.6(4) . . ? C7 N5 N4 104.8(4) . . ? C6 N6 C7 107.0(4) . . ? C6 N6 C9 124.5(4) . . ? C7 N6 C9 128.5(4) . . ? C11 N7 N8 110.4(4) . . ? C11 N7 B1 119.5(4) . . ? N8 N7 B1 129.6(4) . . ? C12 N8 N7 104.1(4) . . ? C11 N9 C12 106.3(4) . . ? C11 N9 C14 125.1(5) . . ? C12 N9 C14 128.5(5) . . ? N1 C1 N3 106.7(4) . . ? N1 C1 S1 123.7(3) . . ? N3 C1 S1 129.6(3) . . ? N2 C2 N3 111.4(4) . . ? N2 C2 C3 125.2(5) . . ? N3 C2 C3 123.4(4) . . ? N3 C4 C5 111.5(4) . . ? N4 C6 N6 105.8(4) . . ? N4 C6 S2 123.5(3) . . ? N6 C6 S2 130.6(4) . . ? N5 C7 N6 111.2(4) . . ? N5 C7 C8 125.1(5) . . ? N6 C7 C8 123.7(5) . . ? N5 C9 C10 112.1(5) . . ? N7 C11 N9 106.8(4) . . ? N7 C11 S3 123.5(3) . . ? N9 C11 S3 129.6(4) . . ? N8 C12 N9 112.3(4) . . ? N8 C12 C13 123.5(6) . . ? N9 C12 C13 124.2(5) . . ? N9 C14 C15 112.5(5) . . ? C17 C16 C21 118.4(5) . . ? C17 C16 P1 117.7(4) . . ? C21 C16 P1 123.3(4) . . ? C18 C17 C16 119.6(5) . . ? C19 C18 C17 121.5(6) . . ? C18 C19 C20 119.9(5) . . ? C19 C20 C21 119.5(6) . . ? C20 C21 C16 121.1(6) . . ? C27 C22 C23 118.1(4) . . ? C27 C22 P1 122.9(4) . . ? C23 C22 P1 119.1(4) . . ? C24 C23 C22 121.6(5) . . ? C23 C24 C25 119.4(5) . . ? C26 C25 C24 119.3(5) . . ? C27 C26 C25 120.6(5) . . ? C26 C27 C22 121.0(5) . . ? C33 C28 C29 118.1(4) . . ? C33 C28 P1 120.7(4) . . ? C29 C28 P1 121.2(4) . . ? C30 C29 C28 120.6(5) . . ? C31 C30 C29 120.5(5) . . ? C32 C31 C30 119.5(5) . . ? C31 C32 C33 120.5(5) . . ? C32 C33 C28 120.7(5) . . ? Cl2 C34 Cl1 111.2(3) . . ? Cl3 C35 Cl4 116.5(5) . . ? Cl6 C36 Cl7 114.1(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.193 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.124