data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Connelly, Neil' _publ_contact_author_email neil.connelly@bristol.ac.uk _publ_section_title ; Isomerism in rhodium(I) N,S-donor heteroscorpionates: ring substituent and ancillary ligand effects ; _publ_author_name N.Connelly data_10 _database_code_depnum_ccdc_archive 'CCDC 783349' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H24 B N8 O2 Rh S2' _chemical_formula_sum 'C17 H24 B N8 O2 Rh S2' _chemical_formula_weight 550.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P21/n _Symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6356(5) _cell_length_b 16.6124(7) _cell_length_c 13.7050(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.893(1) _cell_angle_gamma 90.00 _cell_volume 2377.81(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5888 _cell_measurement_theta_min 2.231 _cell_measurement_theta_max 27.5002 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.831 _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 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12253 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5463 _reflns_number_gt 4157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v5.054 (Bruker-AXS, 1997-1998)' _computing_cell_refinement 'SMART v5.054 (Bruker-AXS, 1997-1998)' _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 '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^)+(0.0338P)^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 5463 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.489348(18) 0.940413(12) 0.136805(14) 0.02710(7) Uani 1 1 d . . . S1 S 0.32143(7) 1.03043(4) 0.07481(5) 0.03744(17) Uani 1 1 d . . . S2 S 0.55886(6) 0.83486(4) 0.40725(5) 0.03652(17) Uani 1 1 d . . . N1 N 0.29221(17) 0.85789(11) 0.23351(14) 0.0260(4) Uani 1 1 d . . . N2 N 0.35938(18) 0.85172(12) 0.15757(14) 0.0274(5) Uani 1 1 d . . . N3 N 0.20741(17) 1.00111(11) 0.23882(14) 0.0259(4) Uani 1 1 d . . . N4 N 0.10702(19) 1.03347(12) 0.27891(16) 0.0323(5) Uani 1 1 d . . . N5 N 0.12138(18) 1.09508(12) 0.13886(15) 0.0288(5) Uani 1 1 d . . . N6 N 0.42678(18) 0.97000(11) 0.33471(14) 0.0247(4) Uani 1 1 d . . . N7 N 0.4443(2) 1.05342(11) 0.33273(15) 0.0292(5) Uani 1 1 d . . . N8 N 0.62181(18) 0.99347(12) 0.40786(14) 0.0252(4) Uani 1 1 d . . . O1 O 0.6616(2) 1.08144(13) 0.13886(16) 0.0622(6) Uani 1 1 d . . . O2 O 0.7093(2) 0.82347(14) 0.16736(17) 0.0625(6) Uani 1 1 d . . . B1 B 0.2909(3) 0.93345(17) 0.2982(2) 0.0266(6) Uani 1 1 d . . . H1 H 0.2533 0.9190 0.3575 0.032 Uiso 1 1 calc R . . C1 C 0.5980(3) 1.02579(18) 0.13270(19) 0.0394(7) Uani 1 1 d . . . C2 C 0.6260(3) 0.86789(18) 0.1592(2) 0.0404(7) Uani 1 1 d . . . C3 C 0.2245(2) 0.78882(14) 0.23778(18) 0.0292(6) Uani 1 1 d . . . C4 C 0.2482(2) 0.73903(15) 0.1637(2) 0.0359(6) Uani 1 1 d . . . H4 H 0.2133 0.6869 0.1484 0.043 Uiso 1 1 calc R . . C5 C 0.3328(2) 0.77927(15) 0.11518(19) 0.0340(6) Uani 1 1 d . . . C6 C 0.1386(3) 0.77522(16) 0.3109(2) 0.0421(7) Uani 1 1 d . . . H6A H 0.1871 0.7833 0.3784 0.063 Uiso 1 1 calc R . . H6B H 0.1054 0.7201 0.3041 0.063 Uiso 1 1 calc R . . H6C H 0.0671 0.8134 0.2980 0.063 Uiso 1 1 calc R . . C7 C 0.3901(3) 0.75295(17) 0.0289(2) 0.0471(7) Uani 1 1 d . . . H7A H 0.4376 0.7978 0.0068 0.071 Uiso 1 1 calc R . . H7B H 0.3218 0.7360 -0.0256 0.071 Uiso 1 1 calc R . . H7C H 0.4485 0.7078 0.0490 0.071 Uiso 1 1 calc R . . C8 C 0.2162(2) 1.03945(14) 0.15513(18) 0.0269(5) Uani 1 1 d . . . C9 C 0.0584(2) 1.08916(15) 0.2170(2) 0.0329(6) Uani 1 1 d . . . C10 C -0.0494(2) 1.14292(17) 0.2297(2) 0.0492(8) Uani 1 1 d . . . H10A H -0.0825 1.1264 0.2887 0.074 Uiso 1 1 calc R . . H10B H -0.1178 1.1391 0.1710 0.074 Uiso 1 1 calc R . . H10C H -0.0189 1.1986 0.2378 0.074 Uiso 1 1 calc R . . C11 C 0.0936(3) 1.14967(15) 0.0534(2) 0.0385(6) Uani 1 1 d . . . H11A H 0.1746 1.1633 0.0315 0.046 Uiso 1 1 calc R . . H11B H 0.0566 1.2002 0.0738 0.046 Uiso 1 1 calc R . . C12 C 0.0012(3) 1.11297(19) -0.0330(2) 0.0643(10) Uani 1 1 d . . . H12A H 0.0396 1.0646 -0.0561 0.096 Uiso 1 1 calc R . . H12B H -0.0172 1.1521 -0.0873 0.096 Uiso 1 1 calc R . . H12C H -0.0785 1.0985 -0.0113 0.096 Uiso 1 1 calc R . . C13 C 0.5334(2) 0.93332(14) 0.38213(16) 0.0255(5) Uani 1 1 d . . . C14 C 0.5635(2) 1.06469(14) 0.37657(17) 0.0285(5) Uani 1 1 d . . . C15 C 0.6263(3) 1.14522(15) 0.3902(2) 0.0402(7) Uani 1 1 d . . . H15A H 0.5650 1.1868 0.3615 0.060 Uiso 1 1 calc R . . H15B H 0.7000 1.1461 0.3567 0.060 Uiso 1 1 calc R . . H15C H 0.6552 1.1557 0.4612 0.060 Uiso 1 1 calc R . . C16 C 0.7546(2) 0.98072(16) 0.45761(19) 0.0347(6) Uani 1 1 d . . . H16A H 0.7570 0.9393 0.5098 0.042 Uiso 1 1 calc R . . H16B H 0.7888 1.0314 0.4904 0.042 Uiso 1 1 calc R . . C17 C 0.8391(2) 0.95427(16) 0.3862(2) 0.0438(7) Uani 1 1 d . . . H17A H 0.8079 0.9029 0.3558 0.066 Uiso 1 1 calc R . . H17B H 0.9273 0.9477 0.4224 0.066 Uiso 1 1 calc R . . H17C H 0.8369 0.9951 0.3343 0.066 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 0.02784(11) 0.02805(12) 0.02535(10) -0.00405(8) 0.00492(7) -0.00054(9) S1 0.0465(4) 0.0377(4) 0.0303(4) 0.0063(3) 0.0127(3) 0.0137(3) S2 0.0394(4) 0.0246(4) 0.0422(4) 0.0078(3) -0.0009(3) -0.0008(3) N1 0.0260(10) 0.0226(11) 0.0272(11) -0.0016(8) -0.0007(8) -0.0026(9) N2 0.0280(11) 0.0250(12) 0.0281(11) -0.0033(9) 0.0023(8) 0.0004(9) N3 0.0236(10) 0.0253(12) 0.0281(11) -0.0036(8) 0.0035(8) 0.0009(8) N4 0.0248(11) 0.0310(12) 0.0431(13) -0.0023(10) 0.0113(9) -0.0015(9) N5 0.0254(11) 0.0228(11) 0.0362(12) -0.0024(9) 0.0011(9) 0.0012(9) N6 0.0289(11) 0.0183(10) 0.0259(10) -0.0022(8) 0.0025(8) -0.0020(8) N7 0.0344(11) 0.0209(11) 0.0316(11) -0.0024(9) 0.0046(9) -0.0022(9) N8 0.0265(10) 0.0241(11) 0.0238(10) -0.0029(8) 0.0016(8) -0.0009(9) O1 0.0681(15) 0.0650(16) 0.0534(14) -0.0070(11) 0.0113(11) -0.0358(13) O2 0.0457(13) 0.0675(16) 0.0739(16) -0.0025(12) 0.0105(11) 0.0246(12) B1 0.0271(14) 0.0271(16) 0.0253(14) 0.0010(11) 0.0044(11) -0.0021(12) C1 0.0397(16) 0.0492(18) 0.0304(15) -0.0034(13) 0.0096(12) -0.0067(14) C2 0.0357(15) 0.0479(19) 0.0384(16) -0.0063(13) 0.0092(12) -0.0004(14) C3 0.0244(12) 0.0234(14) 0.0347(14) 0.0048(11) -0.0070(10) -0.0017(10) C4 0.0346(14) 0.0215(14) 0.0463(17) -0.0042(12) -0.0061(12) -0.0019(11) C5 0.0331(14) 0.0278(15) 0.0362(15) -0.0066(11) -0.0059(11) 0.0027(11) C6 0.0405(16) 0.0351(17) 0.0484(18) 0.0100(13) 0.0028(13) -0.0096(13) C7 0.0570(19) 0.0358(17) 0.0470(18) -0.0181(13) 0.0062(14) 0.0005(14) C8 0.0273(13) 0.0214(13) 0.0300(13) -0.0033(10) 0.0004(10) 0.0004(10) C9 0.0242(13) 0.0243(14) 0.0491(17) -0.0055(12) 0.0043(11) -0.0021(11) C10 0.0319(15) 0.0378(17) 0.081(2) 0.0026(16) 0.0193(15) 0.0066(13) C11 0.0417(15) 0.0257(15) 0.0449(16) 0.0042(12) 0.0000(13) 0.0062(12) C12 0.070(2) 0.047(2) 0.061(2) 0.0130(16) -0.0265(17) 0.0018(17) C13 0.0300(13) 0.0260(14) 0.0201(12) 0.0003(9) 0.0036(9) -0.0005(10) C14 0.0336(13) 0.0244(14) 0.0271(13) -0.0062(10) 0.0048(10) -0.0010(11) C15 0.0393(15) 0.0293(15) 0.0500(17) -0.0053(13) 0.0036(13) -0.0076(12) C16 0.0284(13) 0.0359(16) 0.0360(15) -0.0030(12) -0.0031(11) -0.0032(12) C17 0.0315(15) 0.0489(19) 0.0515(18) 0.0021(14) 0.0089(13) -0.0007(13) _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 1.837(3) . ? Rh1 C2 1.868(3) . ? Rh1 N2 2.0763(19) . ? Rh1 S1 2.3609(7) . ? S1 C8 1.718(2) . ? S2 C13 1.683(2) . ? N1 C3 1.362(3) . ? N1 N2 1.373(3) . ? N1 B1 1.539(3) . ? N2 C5 1.343(3) . ? N3 C8 1.331(3) . ? N3 N4 1.397(3) . ? N3 B1 1.562(3) . ? N4 C9 1.295(3) . ? N5 C8 1.355(3) . ? N5 C9 1.370(3) . ? N5 C11 1.467(3) . ? N6 C13 1.342(3) . ? N6 N7 1.399(3) . ? N6 B1 1.561(3) . ? N7 C14 1.309(3) . ? N8 C14 1.367(3) . ? N8 C13 1.372(3) . ? N8 C16 1.463(3) . ? O1 C1 1.140(3) . ? O2 C2 1.142(3) . ? B1 H1 1.0000 . ? C3 C4 1.369(3) . ? C3 C6 1.494(3) . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C7 1.494(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.489(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.516(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.491(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.513(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 C2 91.65(12) . . ? C1 Rh1 N2 172.29(10) . . ? C2 Rh1 N2 92.13(10) . . ? C1 Rh1 S1 86.40(9) . . ? C2 Rh1 S1 168.47(8) . . ? N2 Rh1 S1 91.20(6) . . ? C8 S1 Rh1 111.40(8) . . ? C3 N1 N2 108.96(19) . . ? C3 N1 B1 126.9(2) . . ? N2 N1 B1 124.10(19) . . ? C5 N2 N1 107.3(2) . . ? C5 N2 Rh1 131.89(17) . . ? N1 N2 Rh1 120.41(14) . . ? C8 N3 N4 109.75(19) . . ? C8 N3 B1 131.9(2) . . ? N4 N3 B1 118.24(19) . . ? C9 N4 N3 104.9(2) . . ? C8 N5 C9 106.3(2) . . ? C8 N5 C11 125.8(2) . . ? C9 N5 C11 127.9(2) . . ? C13 N6 N7 110.83(19) . . ? C13 N6 B1 128.7(2) . . ? N7 N6 B1 119.86(19) . . ? C14 N7 N6 104.69(19) . . ? C14 N8 C13 107.6(2) . . ? C14 N8 C16 127.8(2) . . ? C13 N8 C16 124.7(2) . . ? N1 B1 N6 113.1(2) . . ? N1 B1 N3 110.67(19) . . ? N6 B1 N3 106.72(19) . . ? N1 B1 H1 108.7 . . ? N6 B1 H1 108.7 . . ? N3 B1 H1 108.7 . . ? O1 C1 Rh1 173.0(2) . . ? O2 C2 Rh1 176.2(2) . . ? N1 C3 C4 107.7(2) . . ? N1 C3 C6 123.5(2) . . ? C4 C3 C6 128.8(2) . . ? C3 C4 C5 106.9(2) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N2 C5 C4 109.1(2) . . ? N2 C5 C7 121.4(2) . . ? C4 C5 C7 129.5(2) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N5 107.3(2) . . ? N3 C8 S1 132.11(18) . . ? N5 C8 S1 120.58(18) . . ? N4 C9 N5 111.7(2) . . ? N4 C9 C10 125.0(3) . . ? N5 C9 C10 123.3(2) . . ? 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 . . ? N5 C11 C12 112.2(2) . . ? N5 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N5 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 N8 105.6(2) . . ? N6 C13 S2 128.96(19) . . ? N8 C13 S2 125.43(17) . . ? N7 C14 N8 111.3(2) . . ? N7 C14 C15 123.9(2) . . ? N8 C14 C15 124.8(2) . . ? 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 . . ? N8 C16 C17 112.3(2) . . ? N8 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N8 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 C8 -120.01(12) . . . . ? C2 Rh1 S1 C8 159.4(4) . . . . ? N2 Rh1 S1 C8 52.66(10) . . . . ? C3 N1 N2 C5 0.2(2) . . . . ? B1 N1 N2 C5 -177.0(2) . . . . ? C3 N1 N2 Rh1 -173.56(14) . . . . ? B1 N1 N2 Rh1 9.3(3) . . . . ? C2 Rh1 N2 C5 -53.9(2) . . . . ? S1 Rh1 N2 C5 115.0(2) . . . . ? C2 Rh1 N2 N1 118.01(18) . . . . ? S1 Rh1 N2 N1 -73.03(16) . . . . ? C8 N3 N4 C9 0.9(3) . . . . ? B1 N3 N4 C9 177.7(2) . . . . ? C13 N6 N7 C14 2.0(3) . . . . ? B1 N6 N7 C14 173.9(2) . . . . ? C3 N1 B1 N6 137.6(2) . . . . ? N2 N1 B1 N6 -45.7(3) . . . . ? C3 N1 B1 N3 -102.6(3) . . . . ? N2 N1 B1 N3 74.0(3) . . . . ? C13 N6 B1 N1 -52.5(3) . . . . ? N7 N6 B1 N1 137.2(2) . . . . ? C13 N6 B1 N3 -174.5(2) . . . . ? N7 N6 B1 N3 15.3(3) . . . . ? C8 N3 B1 N1 -59.6(3) . . . . ? N4 N3 B1 N1 124.3(2) . . . . ? C8 N3 B1 N6 63.9(3) . . . . ? N4 N3 B1 N6 -112.2(2) . . . . ? N2 N1 C3 C4 -0.5(3) . . . . ? B1 N1 C3 C4 176.6(2) . . . . ? N2 N1 C3 C6 -179.0(2) . . . . ? B1 N1 C3 C6 -1.9(4) . . . . ? N1 C3 C4 C5 0.6(3) . . . . ? C6 C3 C4 C5 179.0(2) . . . . ? N1 N2 C5 C4 0.2(3) . . . . ? Rh1 N2 C5 C4 172.95(17) . . . . ? N1 N2 C5 C7 179.7(2) . . . . ? Rh1 N2 C5 C7 -7.6(4) . . . . ? C3 C4 C5 N2 -0.5(3) . . . . ? C3 C4 C5 C7 -179.9(2) . . . . ? N4 N3 C8 N5 -1.3(3) . . . . ? B1 N3 C8 N5 -177.6(2) . . . . ? N4 N3 C8 S1 177.42(18) . . . . ? B1 N3 C8 S1 1.1(4) . . . . ? C9 N5 C8 N3 1.2(3) . . . . ? C11 N5 C8 N3 -178.4(2) . . . . ? C9 N5 C8 S1 -177.68(17) . . . . ? C11 N5 C8 S1 2.7(3) . . . . ? Rh1 S1 C8 N3 -6.2(3) . . . . ? Rh1 S1 C8 N5 172.39(16) . . . . ? N3 N4 C9 N5 -0.1(3) . . . . ? N3 N4 C9 C10 -177.9(2) . . . . ? C8 N5 C9 N4 -0.7(3) . . . . ? C11 N5 C9 N4 178.9(2) . . . . ? C8 N5 C9 C10 177.1(2) . . . . ? C11 N5 C9 C10 -3.2(4) . . . . ? C8 N5 C11 C12 88.9(3) . . . . ? C9 N5 C11 C12 -90.7(3) . . . . ? N7 N6 C13 N8 -2.1(2) . . . . ? B1 N6 C13 N8 -173.0(2) . . . . ? N7 N6 C13 S2 177.72(17) . . . . ? B1 N6 C13 S2 6.8(4) . . . . ? C14 N8 C13 N6 1.3(2) . . . . ? C16 N8 C13 N6 -177.3(2) . . . . ? C14 N8 C13 S2 -178.48(18) . . . . ? C16 N8 C13 S2 2.9(3) . . . . ? N6 N7 C14 N8 -1.1(3) . . . . ? N6 N7 C14 C15 178.9(2) . . . . ? C13 N8 C14 N7 -0.1(3) . . . . ? C16 N8 C14 N7 178.5(2) . . . . ? C13 N8 C14 C15 179.9(2) . . . . ? C16 N8 C14 C15 -1.5(4) . . . . ? C14 N8 C16 C17 -98.3(3) . . . . ? C13 N8 C16 C17 80.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.072 # Attachment '- all.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 792567' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 B N8 Rh S2, C H2 Cl2' _chemical_formula_sum 'C24 H38 B Cl2 N8 Rh S2' _chemical_formula_weight 687.36 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 13.7606(14) _cell_length_b 10.0914(11) _cell_length_c 21.575(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.249(9) _cell_angle_gamma 90.00 _cell_volume 2991.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 315 _cell_measurement_theta_min 2.223 _cell_measurement_theta_max 27.482 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.830 _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 ? _diffrn_reflns_number 21548 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6839 _reflns_number_gt 6114 _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. The cyclooctadiene ligands is disordered and has been modelled as sitting over two positions. Rstraints on thermal parameters were used in order to ensure a smooth refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.5085P] 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 6839 _refine_ls_number_parameters 395 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.147 _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 0.933091(12) 0.183778(17) 0.885889(8) 0.01849(7) Uani 1 1 d . . . S1 S 0.85513(4) 0.38515(5) 0.85388(3) 0.01961(12) Uani 1 1 d . B . S2 S 0.68195(4) -0.08436(5) 0.93514(3) 0.02074(13) Uani 1 1 d . . . B1 B 0.76577(18) 0.2187(2) 0.97164(11) 0.0160(5) Uani 1 1 d . B . H1 H 0.7883 0.1598 0.9381 0.019 Uiso 1 1 calc R . . N1 N 0.85722(14) 0.26668(19) 1.00991(9) 0.0186(4) Uani 1 1 d . . . N2 N 0.94254(14) 0.24792(18) 0.98055(9) 0.0192(4) Uani 1 1 d . B . N3 N 0.71546(13) 0.34089(18) 0.93952(8) 0.0164(4) Uani 1 1 d . . . N4 N 0.62824(14) 0.39715(18) 0.95643(9) 0.0187(4) Uani 1 1 d . B . N5 N 0.69330(14) 0.51792(17) 0.88411(8) 0.0167(4) Uani 1 1 d . . . N6 N 0.69471(13) 0.13818(17) 1.00877(8) 0.0151(4) Uani 1 1 d . . . N7 N 0.66168(15) 0.18283(17) 1.06485(9) 0.0181(4) Uani 1 1 d . B . N8 N 0.60830(13) -0.01957(17) 1.04550(8) 0.0150(3) Uani 1 1 d . . . C3 C 0.87574(18) 0.3449(2) 1.06059(11) 0.0240(5) Uani 1 1 d . B . C4 C 0.97389(19) 0.3733(2) 1.06435(12) 0.0278(5) Uani 1 1 d . . . H4 H 1.0081 0.4244 1.0955 0.033 Uiso 1 1 calc R B . C5 C 1.01301(18) 0.3124(2) 1.01345(12) 0.0241(5) Uani 1 1 d . B . C6 C 0.8014(2) 0.3956(3) 1.10278(12) 0.0337(6) Uani 1 1 d . . . H6A H 0.7423 0.4211 1.0781 0.051 Uiso 1 1 calc R B . H6B H 0.8275 0.4729 1.1256 0.051 Uiso 1 1 calc R . . H6C H 0.7856 0.3260 1.1322 0.051 Uiso 1 1 calc R . . C7 C 1.11504(18) 0.3168(2) 0.99385(14) 0.0311(6) Uani 1 1 d . . . H7A H 1.1527 0.2452 1.0143 0.047 Uiso 1 1 calc R B . H7B H 1.1443 0.4023 1.0056 0.047 Uiso 1 1 calc R . . H7C H 1.1152 0.3058 0.9487 0.047 Uiso 1 1 calc R . . C8 C 0.75429(16) 0.4128(2) 0.89504(10) 0.0166(4) Uani 1 1 d . B . C9 C 0.61686(17) 0.5024(2) 0.92160(10) 0.0179(4) Uani 1 1 d . B . C10 C 0.53215(18) 0.5938(2) 0.92054(11) 0.0229(5) Uani 1 1 d . . . H10A H 0.4950 0.5861 0.8806 0.034 Uiso 1 1 calc R B . H10B H 0.5552 0.6851 0.9262 0.034 Uiso 1 1 calc R . . H10C H 0.4903 0.5705 0.9542 0.034 Uiso 1 1 calc R . . C11 C 0.70831(18) 0.6261(2) 0.83996(10) 0.0206(5) Uani 1 1 d . B . H11A H 0.7790 0.6425 0.8378 0.025 Uiso 1 1 calc R . . H11B H 0.6781 0.7081 0.8552 0.025 Uiso 1 1 calc R . . C13 C 0.66490(18) 0.5944(3) 0.77559(11) 0.0249(5) Uani 1 1 d . . . H13A H 0.6969 0.5158 0.7595 0.037 Uiso 1 1 calc R B . H13B H 0.6746 0.6698 0.7480 0.037 Uiso 1 1 calc R . . H13C H 0.5951 0.5772 0.7776 0.037 Uiso 1 1 calc R . . C14 C 0.66263(15) 0.0140(2) 0.99639(10) 0.0149(4) Uani 1 1 d . B . C15 C 0.61105(16) 0.0863(2) 1.08564(10) 0.0169(4) Uani 1 1 d . B . C16 C 0.56226(18) 0.0885(2) 1.14544(10) 0.0223(5) Uani 1 1 d . . . H16A H 0.5837 0.1667 1.1695 0.034 Uiso 1 1 calc R B . H16B H 0.5794 0.0082 1.1692 0.034 Uiso 1 1 calc R . . H16C H 0.4916 0.0920 1.1371 0.034 Uiso 1 1 calc R . . C17 C 0.55887(16) -0.1463(2) 1.05332(11) 0.0182(4) Uani 1 1 d . B . H17A H 0.5313 -0.1771 1.0124 0.022 Uiso 1 1 calc R . . H17B H 0.5042 -0.1335 1.0807 0.022 Uiso 1 1 calc R . . C18 C 0.62679(18) -0.2518(2) 1.08107(13) 0.0269(5) Uani 1 1 d . . . H18A H 0.6789 -0.2686 1.0529 0.040 Uiso 1 1 calc R B . H18B H 0.5902 -0.3337 1.0870 0.040 Uiso 1 1 calc R . . H18C H 0.6552 -0.2211 1.1212 0.040 Uiso 1 1 calc R . . C19 C 1.04204(19) 0.0359(2) 0.90970(12) 0.0273(5) Uani 1 1 d . B . H19 H 1.0673 0.0384 0.9541 0.033 Uiso 1 1 calc R A 1 C20A C 0.9515(2) -0.0236(2) 0.90040(12) 0.0280(5) Uani 0.744(6) 1 d PU B 1 H20A H 0.9237 -0.0572 0.9393 0.034 Uiso 0.744(6) 1 calc PR B 1 C21A C 0.9105(6) -0.0943(8) 0.8399(4) 0.0330(16) Uani 0.744(6) 1 d PU B 1 H21A H 0.9395 -0.1838 0.8377 0.040 Uiso 0.744(6) 1 calc PR B 1 H21B H 0.8392 -0.1050 0.8417 0.040 Uiso 0.744(6) 1 calc PR B 1 C22A C 0.9318(3) -0.0179(4) 0.78164(17) 0.0347(10) Uani 0.744(6) 1 d PU B 1 H22A H 0.9967 -0.0439 0.7682 0.042 Uiso 0.744(6) 1 calc PR B 1 H22B H 0.8830 -0.0418 0.7480 0.042 Uiso 0.744(6) 1 calc PR B 1 C23A C 0.9298(4) 0.1304(6) 0.7916(3) 0.0284(12) Uani 0.744(6) 1 d PU B 1 H23A H 0.8802 0.1788 0.7646 0.034 Uiso 0.744(6) 1 calc PR B 1 C24A C 1.0136(3) 0.2039(5) 0.8083(2) 0.0314(10) Uani 0.744(6) 1 d PU B 1 H24A H 1.0129 0.2956 0.7908 0.038 Uiso 0.744(6) 1 calc PR B 1 C25A C 1.1150(3) 0.1463(5) 0.8189(2) 0.0417(12) Uani 0.744(6) 1 d PU B 1 H25A H 1.1383 0.1171 0.7785 0.050 Uiso 0.744(6) 1 calc PR B 1 H25B H 1.1594 0.2169 0.8352 0.050 Uiso 0.744(6) 1 calc PR B 1 C26A C 1.1209(2) 0.0309(3) 0.86331(14) 0.0362(6) Uani 0.744(6) 1 d PU B 1 H26A H 1.1855 0.0311 0.8860 0.043 Uiso 0.744(6) 1 calc PR B 1 H26B H 1.1148 -0.0527 0.8394 0.043 Uiso 0.744(6) 1 calc PR B 1 C20B C 0.9515(2) -0.0236(2) 0.90040(12) 0.0280(5) Uani 0.256(6) 1 d PU B 2 H20B H 0.9248 -0.0538 0.9402 0.034 Uiso 0.256(6) 1 calc PR B 2 C21B C 0.9326(15) -0.116(2) 0.8513(10) 0.022(3) Uani 0.256(6) 1 d PU B 2 H21C H 0.8989 -0.1947 0.8671 0.027 Uiso 0.256(6) 1 calc PR B 2 H21D H 0.9946 -0.1453 0.8347 0.027 Uiso 0.256(6) 1 calc PR B 2 C22B C 0.8701(8) -0.0511(9) 0.8010(5) 0.024(2) Uani 0.256(6) 1 d PU B 2 H22C H 0.8009 -0.0573 0.8108 0.029 Uiso 0.256(6) 1 calc PR B 2 H22D H 0.8781 -0.0974 0.7611 0.029 Uiso 0.256(6) 1 calc PR B 2 C23B C 0.8988(11) 0.0940(13) 0.7949(8) 0.020(3) Uani 0.256(6) 1 d PU B 2 H23B H 0.8498 0.1463 0.7690 0.024 Uiso 0.256(6) 1 calc PR B 2 C24B C 0.9903(12) 0.1469(14) 0.7949(5) 0.022(2) Uani 0.256(6) 1 d PU B 2 H24B H 0.9940 0.2285 0.7689 0.026 Uiso 0.256(6) 1 calc PR B 2 C25B C 1.0843(8) 0.0634(13) 0.7969(5) 0.032(3) Uani 0.256(6) 1 d PU B 2 H25C H 1.0717 -0.0202 0.7738 0.039 Uiso 0.256(6) 1 calc PR B 2 H25D H 1.1354 0.1127 0.7760 0.039 Uiso 0.256(6) 1 calc PR B 2 C26B C 1.1209(2) 0.0309(3) 0.86331(14) 0.0362(6) Uani 0.256(6) 1 d PU B 2 H26C H 1.1500 -0.0588 0.8640 0.043 Uiso 0.256(6) 1 calc PR B 2 H26D H 1.1729 0.0945 0.8764 0.043 Uiso 0.256(6) 1 calc PR B 2 C27 C 0.6577(2) 0.1413(3) 0.80323(14) 0.0423(7) Uani 1 1 d . . . H27A H 0.6647 0.0945 0.8435 0.051 Uiso 1 1 calc R . . H27B H 0.7183 0.1918 0.7978 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.55892(6) 0.25211(7) 0.80407(3) 0.03895(17) Uani 1 1 d . . . Cl2 Cl 0.64121(7) 0.02378(10) 0.74259(4) 0.0587(2) 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 0.01465(11) 0.02119(11) 0.01975(11) 0.00626(6) 0.00210(7) -0.00005(6) S1 0.0162(3) 0.0203(3) 0.0223(3) 0.0077(2) 0.0013(2) -0.0024(2) S2 0.0214(3) 0.0185(3) 0.0227(3) -0.0053(2) 0.0053(2) -0.0034(2) B1 0.0174(12) 0.0148(11) 0.0159(11) 0.0021(9) 0.0009(9) -0.0017(9) N1 0.0170(9) 0.0203(9) 0.0184(9) 0.0026(7) -0.0011(7) -0.0030(7) N2 0.0157(9) 0.0167(9) 0.0246(10) 0.0063(7) -0.0030(7) -0.0002(7) N3 0.0162(9) 0.0161(9) 0.0170(9) 0.0007(7) 0.0007(7) -0.0023(7) N4 0.0202(10) 0.0168(9) 0.0192(9) -0.0012(7) 0.0016(7) 0.0007(7) N5 0.0208(10) 0.0127(8) 0.0165(9) 0.0014(7) 0.0003(7) -0.0028(7) N6 0.0158(9) 0.0147(8) 0.0147(8) 0.0000(7) 0.0006(7) -0.0005(7) N7 0.0220(10) 0.0176(9) 0.0148(9) 0.0006(7) 0.0013(7) -0.0008(7) N8 0.0147(9) 0.0131(8) 0.0170(9) 0.0017(7) 0.0002(7) -0.0014(7) C3 0.0263(13) 0.0203(11) 0.0247(12) -0.0011(9) -0.0051(10) -0.0057(9) C4 0.0269(13) 0.0228(12) 0.0323(13) -0.0001(10) -0.0108(10) -0.0054(10) C5 0.0204(12) 0.0172(11) 0.0337(13) 0.0073(9) -0.0067(10) -0.0025(9) C6 0.0382(16) 0.0326(14) 0.0306(14) -0.0131(11) 0.0038(11) -0.0140(12) C7 0.0167(12) 0.0255(13) 0.0499(17) 0.0053(11) -0.0077(11) -0.0026(9) C8 0.0186(11) 0.0138(10) 0.0168(10) 0.0003(8) -0.0030(8) -0.0042(8) C9 0.0237(12) 0.0137(10) 0.0162(10) -0.0028(8) 0.0012(8) -0.0034(8) C10 0.0278(13) 0.0180(11) 0.0234(11) 0.0010(9) 0.0048(9) 0.0052(9) C11 0.0286(12) 0.0121(10) 0.0215(11) 0.0044(8) 0.0045(9) -0.0011(9) C13 0.0238(12) 0.0297(13) 0.0213(11) 0.0056(9) 0.0016(9) 0.0033(10) C14 0.0135(10) 0.0145(10) 0.0167(10) 0.0015(8) 0.0002(8) 0.0002(8) C15 0.0155(10) 0.0193(10) 0.0157(10) 0.0010(8) -0.0003(8) 0.0004(8) C16 0.0267(13) 0.0249(12) 0.0158(11) 0.0011(9) 0.0039(9) -0.0020(9) C17 0.0148(10) 0.0160(10) 0.0240(11) 0.0028(8) 0.0022(8) -0.0040(8) C18 0.0223(13) 0.0191(12) 0.0393(14) 0.0100(10) 0.0024(10) 0.0001(9) C19 0.0290(13) 0.0237(12) 0.0293(13) 0.0063(10) 0.0020(10) 0.0100(10) C20A 0.0382(15) 0.0170(11) 0.0299(13) 0.0039(9) 0.0125(11) 0.0028(10) C21A 0.031(4) 0.032(3) 0.036(4) -0.005(2) 0.004(3) 0.001(2) C22A 0.031(2) 0.044(2) 0.0293(19) -0.0052(16) 0.0044(16) 0.0114(17) C23A 0.023(3) 0.041(3) 0.0226(19) 0.007(2) 0.006(2) 0.010(2) C24A 0.023(2) 0.039(3) 0.033(2) 0.013(2) 0.0119(17) 0.0076(18) C25A 0.024(2) 0.050(3) 0.054(3) 0.015(2) 0.0194(18) 0.0063(18) C26A 0.0233(13) 0.0393(15) 0.0464(16) 0.0059(12) 0.0060(12) 0.0118(11) C20B 0.0382(15) 0.0170(11) 0.0299(13) 0.0039(9) 0.0125(11) 0.0028(10) C21B 0.021(8) 0.026(7) 0.020(7) 0.002(4) 0.002(5) -0.008(6) C22B 0.027(5) 0.020(4) 0.027(5) -0.002(4) 0.002(4) 0.003(4) C23B 0.020(6) 0.021(6) 0.019(5) -0.002(4) 0.002(5) 0.004(4) C24B 0.027(6) 0.025(6) 0.014(5) 0.000(4) 0.003(4) -0.001(5) C25B 0.018(5) 0.041(6) 0.039(5) 0.001(5) 0.011(4) 0.003(4) C26B 0.0233(13) 0.0393(15) 0.0464(16) 0.0059(12) 0.0060(12) 0.0118(11) C27 0.0465(18) 0.0464(17) 0.0333(15) -0.0015(13) -0.0051(13) -0.0185(14) Cl1 0.0468(4) 0.0428(4) 0.0267(3) 0.0040(3) -0.0023(3) -0.0202(3) Cl2 0.0610(6) 0.0766(6) 0.0386(4) -0.0206(4) 0.0047(4) -0.0146(5) _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 C24A 2.070(4) . ? Rh1 C23A 2.102(6) . ? Rh1 C20A 2.129(2) . ? Rh1 N2 2.139(2) . ? Rh1 C19 2.156(2) . ? Rh1 C24B 2.188(11) . ? Rh1 C23B 2.190(16) . ? Rh1 S1 2.3818(6) . ? S1 C8 1.712(2) . ? S2 C14 1.685(2) . ? B1 N6 1.532(3) . ? B1 N1 1.543(3) . ? B1 N3 1.557(3) . ? B1 H1 1.0000 . ? N1 C3 1.361(3) . ? N1 N2 1.378(3) . ? N2 C5 1.338(3) . ? N3 C8 1.338(3) . ? N3 N4 1.395(3) . ? N4 C9 1.305(3) . ? N5 C8 1.365(3) . ? N5 C9 1.372(3) . ? N5 C11 1.471(3) . ? N6 C14 1.351(3) . ? N6 N7 1.391(2) . ? N7 C15 1.293(3) . ? N8 C14 1.373(3) . ? N8 C15 1.375(3) . ? N8 C17 1.463(3) . ? C3 C4 1.379(3) . ? C3 C6 1.498(4) . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C7 1.490(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.486(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.514(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.488(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.517(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20A 1.388(4) . ? C19 C26A 1.519(4) . ? C19 H19 1.0000 . ? C20A C21A 1.565(9) . ? C20A H20A 1.0000 . ? C21A C22A 1.517(8) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A C23A 1.513(7) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A C24A 1.401(7) . ? C23A H23A 1.0000 . ? C24A C25A 1.517(6) . ? C24A H24A 1.0000 . ? C25A C26A 1.507(5) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C21B C22B 1.497(17) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22B C23B 1.524(16) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C23B C24B 1.368(17) . ? C23B H23B 1.0000 . ? C24B C25B 1.542(17) . ? C24B H24B 1.0000 . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C27 Cl1 1.761(4) . ? C27 Cl2 1.771(3) . ? C27 H27A 0.9900 . ? C27 H27B 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 C24A Rh1 C23A 39.23(19) . . ? C24A Rh1 C20A 98.65(16) . . ? C23A Rh1 C20A 83.47(17) . . ? C24A Rh1 N2 137.42(18) . . ? C23A Rh1 N2 176.41(18) . . ? C20A Rh1 N2 99.02(8) . . ? C24A Rh1 C19 82.15(14) . . ? C23A Rh1 C19 91.71(16) . . ? C20A Rh1 C19 37.78(10) . . ? N2 Rh1 C19 88.75(9) . . ? C24A Rh1 C24B 19.0(3) . . ? C23A Rh1 C24B 22.7(4) . . ? C20A Rh1 C24B 85.3(4) . . ? N2 Rh1 C24B 154.5(4) . . ? C19 Rh1 C24B 79.3(4) . . ? C24A Rh1 C23B 54.1(4) . . ? C23A Rh1 C23B 15.1(3) . . ? C20A Rh1 C23B 75.1(4) . . ? N2 Rh1 C23B 168.4(4) . . ? C19 Rh1 C23B 92.2(4) . . ? C24B Rh1 C23B 36.4(4) . . ? C24A Rh1 S1 86.27(13) . . ? C23A Rh1 S1 87.33(15) . . ? C20A Rh1 S1 158.30(8) . . ? N2 Rh1 S1 91.18(5) . . ? C19 Rh1 S1 162.74(7) . . ? C24B Rh1 S1 93.7(3) . . ? C23B Rh1 S1 91.3(4) . . ? C8 S1 Rh1 110.71(7) . . ? N6 B1 N1 114.32(18) . . ? N6 B1 N3 111.84(18) . . ? N1 B1 N3 108.56(18) . . ? N6 B1 H1 107.3 . . ? N1 B1 H1 107.3 . . ? N3 B1 H1 107.3 . . ? C3 N1 N2 108.86(19) . . ? C3 N1 B1 136.2(2) . . ? N2 N1 B1 113.64(17) . . ? C5 N2 N1 107.46(19) . . ? C5 N2 Rh1 131.05(17) . . ? N1 N2 Rh1 118.23(14) . . ? C8 N3 N4 110.56(18) . . ? C8 N3 B1 124.26(19) . . ? N4 N3 B1 124.97(17) . . ? C9 N4 N3 104.92(17) . . ? C8 N5 C9 107.09(18) . . ? C8 N5 C11 125.53(18) . . ? C9 N5 C11 127.38(19) . . ? C14 N6 N7 110.69(17) . . ? C14 N6 B1 126.88(17) . . ? N7 N6 B1 122.17(17) . . ? C15 N7 N6 105.48(17) . . ? C14 N8 C15 107.33(17) . . ? C14 N8 C17 125.55(18) . . ? C15 N8 C17 127.10(17) . . ? N1 C3 C4 107.8(2) . . ? N1 C3 C6 125.7(2) . . ? C4 C3 C6 126.4(2) . . ? C3 C4 C5 106.4(2) . . ? C3 C4 H4 126.8 . . ? C5 C4 H4 126.8 . . ? N2 C5 C4 109.4(2) . . ? N2 C5 C7 122.0(2) . . ? C4 C5 C7 128.5(2) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N5 106.19(19) . . ? N3 C8 S1 130.67(17) . . ? N5 C8 S1 123.06(16) . . ? N4 C9 N5 111.19(19) . . ? N4 C9 C10 125.6(2) . . ? N5 C9 C10 123.18(19) . . ? 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 . . ? N5 C11 C13 112.00(19) . . ? N5 C11 H11A 109.2 . . ? C13 C11 H11A 109.2 . . ? N5 C11 H11B 109.2 . . ? C13 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 N8 105.21(17) . . ? N6 C14 S2 129.57(16) . . ? N8 C14 S2 125.22(16) . . ? N7 C15 N8 111.29(18) . . ? N7 C15 C16 124.6(2) . . ? N8 C15 C16 124.06(19) . . ? 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 . . ? N8 C17 C18 112.26(18) . . ? N8 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N8 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? 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 . . ? C20A C19 C26A 124.0(2) . . ? C20A C19 Rh1 70.06(14) . . ? C26A C19 Rh1 112.29(17) . . ? C20A C19 H19 114.2 . . ? C26A C19 H19 114.2 . . ? Rh1 C19 H19 114.2 . . ? C19 C20A C21A 126.6(4) . . ? C19 C20A Rh1 72.17(14) . . ? C21A C20A Rh1 106.9(3) . . ? C19 C20A H20A 114.1 . . ? C21A C20A H20A 114.1 . . ? Rh1 C20A H20A 114.1 . . ? C22A C21A C20A 112.4(6) . . ? C22A C21A H21A 109.1 . . ? C20A C21A H21A 109.1 . . ? C22A C21A H21B 109.1 . . ? C20A C21A H21B 109.1 . . ? H21A C21A H21B 107.8 . . ? C23A C22A C21A 112.3(5) . . ? C23A C22A H22A 109.2 . . ? C21A C22A H22A 109.2 . . ? C23A C22A H22B 109.2 . . ? C21A C22A H22B 109.2 . . ? H22A C22A H22B 107.9 . . ? C24A C23A C22A 122.6(4) . . ? C24A C23A Rh1 69.2(3) . . ? C22A C23A Rh1 113.1(3) . . ? C24A C23A H23A 114.6 . . ? C22A C23A H23A 114.6 . . ? Rh1 C23A H23A 114.6 . . ? C23A C24A C25A 125.0(5) . . ? C23A C24A Rh1 71.6(3) . . ? C25A C24A Rh1 111.7(3) . . ? C23A C24A H24A 113.7 . . ? C25A C24A H24A 113.7 . . ? Rh1 C24A H24A 113.7 . . ? C26A C25A C24A 114.1(3) . . ? C26A C25A H25A 108.7 . . ? C24A C25A H25A 108.7 . . ? C26A C25A H25B 108.7 . . ? C24A C25A H25B 108.7 . . ? H25A C25A H25B 107.6 . . ? C25A C26A C19 112.2(2) . . ? C25A C26A H26A 109.2 . . ? C19 C26A H26A 109.2 . . ? C25A C26A H26B 109.2 . . ? C19 C26A H26B 109.2 . . ? H26A C26A H26B 107.9 . . ? C22B C21B H21C 109.9 . . ? C22B C21B H21D 109.9 . . ? H21C C21B H21D 108.3 . . ? C21B C22B C23B 110.0(12) . . ? C21B C22B H22C 109.7 . . ? C23B C22B H22C 109.7 . . ? C21B C22B H22D 109.7 . . ? C23B C22B H22D 109.7 . . ? H22C C22B H22D 108.2 . . ? C24B C23B C22B 128.1(12) . . ? C24B C23B Rh1 71.7(9) . . ? C22B C23B Rh1 111.3(9) . . ? C24B C23B H23B 112.7 . . ? C22B C23B H23B 112.7 . . ? Rh1 C23B H23B 112.7 . . ? C23B C24B C25B 123.9(12) . . ? C23B C24B Rh1 71.9(9) . . ? C25B C24B Rh1 114.4(7) . . ? C23B C24B H24B 113.3 . . ? C25B C24B H24B 113.3 . . ? Rh1 C24B H24B 113.3 . . ? C24B C25B H25C 109.2 . . ? C24B C25B H25D 109.2 . . ? H25C C25B H25D 107.9 . . ? Cl1 C27 Cl2 111.49(17) . . ? Cl1 C27 H27A 109.3 . . ? Cl2 C27 H27A 109.3 . . ? Cl1 C27 H27B 109.3 . . ? Cl2 C27 H27B 109.3 . . ? H27A C27 H27B 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 C24A Rh1 S1 C8 168.16(19) . . . . ? C23A Rh1 S1 C8 128.88(19) . . . . ? C20A Rh1 S1 C8 64.03(19) . . . . ? N2 Rh1 S1 C8 -54.39(9) . . . . ? C19 Rh1 S1 C8 -144.0(2) . . . . ? C24B Rh1 S1 C8 150.7(4) . . . . ? C23B Rh1 S1 C8 114.3(4) . . . . ? N6 B1 N1 C3 -60.2(3) . . . . ? N3 B1 N1 C3 65.4(3) . . . . ? N6 B1 N1 N2 134.75(19) . . . . ? N3 B1 N1 N2 -99.6(2) . . . . ? C3 N1 N2 C5 0.9(2) . . . . ? B1 N1 N2 C5 170.04(18) . . . . ? C3 N1 N2 Rh1 -160.95(15) . . . . ? B1 N1 N2 Rh1 8.2(2) . . . . ? C24A Rh1 N2 C5 -6.2(3) . . . . ? C20A Rh1 N2 C5 107.2(2) . . . . ? C19 Rh1 N2 C5 70.7(2) . . . . ? C24B Rh1 N2 C5 9.1(8) . . . . ? C23B Rh1 N2 C5 165.8(19) . . . . ? S1 Rh1 N2 C5 -92.0(2) . . . . ? C24A Rh1 N2 N1 150.6(2) . . . . ? C20A Rh1 N2 N1 -95.98(16) . . . . ? C19 Rh1 N2 N1 -132.46(16) . . . . ? C24B Rh1 N2 N1 165.9(8) . . . . ? C23B Rh1 N2 N1 -37.4(19) . . . . ? S1 Rh1 N2 N1 64.80(14) . . . . ? N6 B1 N3 C8 -166.42(19) . . . . ? N1 B1 N3 C8 66.5(3) . . . . ? N6 B1 N3 N4 19.2(3) . . . . ? N1 B1 N3 N4 -107.8(2) . . . . ? C8 N3 N4 C9 -0.2(2) . . . . ? B1 N3 N4 C9 174.82(19) . . . . ? N1 B1 N6 C14 -123.0(2) . . . . ? N3 B1 N6 C14 113.1(2) . . . . ? N1 B1 N6 N7 50.6(3) . . . . ? N3 B1 N6 N7 -73.3(2) . . . . ? C14 N6 N7 C15 0.3(2) . . . . ? B1 N6 N7 C15 -174.28(19) . . . . ? N2 N1 C3 C4 -1.5(3) . . . . ? B1 N1 C3 C4 -167.0(2) . . . . ? N2 N1 C3 C6 176.0(2) . . . . ? B1 N1 C3 C6 10.4(4) . . . . ? N1 C3 C4 C5 1.5(3) . . . . ? C6 C3 C4 C5 -176.0(2) . . . . ? N1 N2 C5 C4 0.0(2) . . . . ? Rh1 N2 C5 C4 158.69(16) . . . . ? N1 N2 C5 C7 -178.1(2) . . . . ? Rh1 N2 C5 C7 -19.4(3) . . . . ? C3 C4 C5 N2 -0.9(3) . . . . ? C3 C4 C5 C7 177.0(2) . . . . ? N4 N3 C8 N5 1.5(2) . . . . ? B1 N3 C8 N5 -173.58(18) . . . . ? N4 N3 C8 S1 -175.30(16) . . . . ? B1 N3 C8 S1 9.7(3) . . . . ? C9 N5 C8 N3 -2.1(2) . . . . ? C11 N5 C8 N3 178.05(19) . . . . ? C9 N5 C8 S1 174.94(16) . . . . ? C11 N5 C8 S1 -4.9(3) . . . . ? Rh1 S1 C8 N3 -0.5(2) . . . . ? Rh1 S1 C8 N5 -176.81(15) . . . . ? N3 N4 C9 N5 -1.2(2) . . . . ? N3 N4 C9 C10 177.5(2) . . . . ? C8 N5 C9 N4 2.1(2) . . . . ? C11 N5 C9 N4 -178.0(2) . . . . ? C8 N5 C9 C10 -176.6(2) . . . . ? C11 N5 C9 C10 3.2(3) . . . . ? C8 N5 C11 C13 88.7(3) . . . . ? C9 N5 C11 C13 -91.0(3) . . . . ? N7 N6 C14 N8 0.2(2) . . . . ? B1 N6 C14 N8 174.43(19) . . . . ? N7 N6 C14 S2 -179.86(17) . . . . ? B1 N6 C14 S2 -5.6(3) . . . . ? C15 N8 C14 N6 -0.6(2) . . . . ? C17 N8 C14 N6 -179.41(19) . . . . ? C15 N8 C14 S2 179.49(16) . . . . ? C17 N8 C14 S2 0.6(3) . . . . ? N6 N7 C15 N8 -0.6(2) . . . . ? N6 N7 C15 C16 179.0(2) . . . . ? C14 N8 C15 N7 0.8(3) . . . . ? C17 N8 C15 N7 179.6(2) . . . . ? C14 N8 C15 C16 -178.9(2) . . . . ? C17 N8 C15 C16 -0.1(3) . . . . ? C14 N8 C17 C18 82.9(3) . . . . ? C15 N8 C17 C18 -95.7(3) . . . . ? C24A Rh1 C19 C20A -115.2(2) . . . . ? C23A Rh1 C19 C20A -77.0(2) . . . . ? N2 Rh1 C19 C20A 106.52(15) . . . . ? C24B Rh1 C19 C20A -96.2(5) . . . . ? C23B Rh1 C19 C20A -61.9(4) . . . . ? S1 Rh1 C19 C20A -163.53(18) . . . . ? C24A Rh1 C19 C26A 4.5(3) . . . . ? C23A Rh1 C19 C26A 42.6(3) . . . . ? C20A Rh1 C19 C26A 119.7(3) . . . . ? N2 Rh1 C19 C26A -133.8(2) . . . . ? C24B Rh1 C19 C26A 23.5(5) . . . . ? C23B Rh1 C19 C26A 57.7(4) . . . . ? S1 Rh1 C19 C26A -43.9(4) . . . . ? C26A C19 C20A C21A -5.8(5) . . . . ? Rh1 C19 C20A C21A 98.2(4) . . . . ? C26A C19 C20A Rh1 -104.0(2) . . . . ? C24A Rh1 C20A C19 65.1(2) . . . . ? C23A Rh1 C20A C19 101.3(2) . . . . ? N2 Rh1 C20A C19 -76.05(15) . . . . ? C24B Rh1 C20A C19 78.6(5) . . . . ? C23B Rh1 C20A C19 114.2(4) . . . . ? S1 Rh1 C20A C19 166.85(14) . . . . ? C24A Rh1 C20A C21A -58.8(4) . . . . ? C23A Rh1 C20A C21A -22.5(4) . . . . ? N2 Rh1 C20A C21A 160.1(4) . . . . ? C19 Rh1 C20A C21A -123.9(4) . . . . ? C24B Rh1 C20A C21A -45.3(6) . . . . ? C23B Rh1 C20A C21A -9.7(5) . . . . ? S1 Rh1 C20A C21A 43.0(4) . . . . ? C19 C20A C21A C22A -43.0(7) . . . . ? Rh1 C20A C21A C22A 37.1(6) . . . . ? C20A C21A C22A C23A -34.4(7) . . . . ? C21A C22A C23A C24A 93.5(6) . . . . ? C21A C22A C23A Rh1 14.3(6) . . . . ? C20A Rh1 C23A C24A -112.3(3) . . . . ? C19 Rh1 C23A C24A -75.4(3) . . . . ? C24B Rh1 C23A C24A -18.8(9) . . . . ? C23B Rh1 C23A C24A -167.7(19) . . . . ? S1 Rh1 C23A C24A 87.4(3) . . . . ? C24A Rh1 C23A C22A 117.7(5) . . . . ? C20A Rh1 C23A C22A 5.3(3) . . . . ? C19 Rh1 C23A C22A 42.3(4) . . . . ? C24B Rh1 C23A C22A 98.9(10) . . . . ? C23B Rh1 C23A C22A -50.0(17) . . . . ? S1 Rh1 C23A C22A -155.0(4) . . . . ? C22A C23A C24A C25A -0.6(8) . . . . ? Rh1 C23A C24A C25A 104.1(4) . . . . ? C22A C23A C24A Rh1 -104.7(5) . . . . ? C20A Rh1 C24A C23A 68.4(3) . . . . ? N2 Rh1 C24A C23A -178.0(2) . . . . ? C19 Rh1 C24A C23A 102.5(3) . . . . ? C24B Rh1 C24A C23A 22.5(12) . . . . ? C23B Rh1 C24A C23A 3.9(6) . . . . ? S1 Rh1 C24A C23A -90.3(3) . . . . ? C23A Rh1 C24A C25A -121.2(5) . . . . ? C20A Rh1 C24A C25A -52.8(4) . . . . ? N2 Rh1 C24A C25A 60.8(4) . . . . ? C19 Rh1 C24A C25A -18.7(4) . . . . ? C24B Rh1 C24A C25A -98.7(14) . . . . ? C23B Rh1 C24A C25A -117.2(6) . . . . ? S1 Rh1 C24A C25A 148.5(4) . . . . ? C23A C24A C25A C26A -51.5(6) . . . . ? Rh1 C24A C25A C26A 30.7(5) . . . . ? C24A C25A C26A C19 -26.9(5) . . . . ? C20A C19 C26A C25A 91.1(4) . . . . ? Rh1 C19 C26A C25A 10.8(4) . . . . ? C21B C22B C23B C24B 44(2) . . . . ? C21B C22B C23B Rh1 -39.0(15) . . . . ? C24A Rh1 C23B C24B 10.0(7) . . . . ? C23A Rh1 C23B C24B 19.6(15) . . . . ? C20A Rh1 C23B C24B -102.6(8) . . . . ? N2 Rh1 C23B C24B -163.3(15) . . . . ? C19 Rh1 C23B C24B -68.6(7) . . . . ? S1 Rh1 C23B C24B 94.5(7) . . . . ? C24A Rh1 C23B C22B 134.7(11) . . . . ? C23A Rh1 C23B C22B 144(2) . . . . ? C20A Rh1 C23B C22B 22.0(8) . . . . ? N2 Rh1 C23B C22B -39(3) . . . . ? C19 Rh1 C23B C22B 56.1(9) . . . . ? C24B Rh1 C23B C22B 124.7(13) . . . . ? S1 Rh1 C23B C22B -140.8(8) . . . . ? C22B C23B C24B C25B 5(2) . . . . ? Rh1 C23B C24B C25B 107.6(11) . . . . ? C22B C23B C24B Rh1 -103.1(16) . . . . ? C24A Rh1 C24B C23B -154.3(17) . . . . ? C23A Rh1 C24B C23B -13.1(9) . . . . ? C20A Rh1 C24B C23B 71.1(8) . . . . ? N2 Rh1 C24B C23B 172.3(7) . . . . ? C19 Rh1 C24B C23B 108.8(8) . . . . ? S1 Rh1 C24B C23B -87.1(8) . . . . ? C24A Rh1 C24B C25B 85.9(16) . . . . ? C23A Rh1 C24B C25B -132.8(15) . . . . ? C20A Rh1 C24B C25B -48.6(9) . . . . ? N2 Rh1 C24B C25B 52.6(14) . . . . ? C19 Rh1 C24B C25B -11.0(9) . . . . ? C23B Rh1 C24B C25B -119.7(14) . . . . ? S1 Rh1 C24B C25B 153.1(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.881 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.190 data_8 _database_code_depnum_ccdc_archive 'CCDC 792568' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H27 B N7 Rh S' _chemical_formula_sum 'C19 H27 B N7 Rh S' _chemical_formula_weight 499.26 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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6346(6) _cell_length_b 10.1088(4) _cell_length_c 15.1537(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.956(3) _cell_angle_gamma 90.00 _cell_volume 2165.87(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17942 _cell_measurement_theta_min 2.6423 _cell_measurement_theta_max 32.9161 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59330 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 33.00 _reflns_number_total 7787 _reflns_number_gt 4702 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruekr 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^)+(0.0648P)^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 7787 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 0.356653(14) -0.071783(19) 0.209424(13) 0.03843(8) Uani 1 1 d . . . S1 S 0.72905(6) 0.00335(8) 0.41082(5) 0.0578(2) Uani 1 1 d . . . B1 B 0.5725(2) -0.2004(3) 0.2808(2) 0.0436(7) Uani 1 1 d . . . H1B H 0.6310 -0.2539 0.3056 0.052 Uiso 1 1 calc R . . N1 N 0.51926(15) -0.1847(2) 0.35515(14) 0.0437(5) Uani 1 1 d . . . N2 N 0.43629(15) -0.1179(2) 0.34058(14) 0.0418(5) Uani 1 1 d . . . N3 N 0.50872(14) -0.2731(2) 0.19839(15) 0.0431(5) Uani 1 1 d . . . N4 N 0.41547(14) -0.24054(19) 0.16328(13) 0.0383(4) Uani 1 1 d . . . N5 N 0.60063(15) -0.06303(19) 0.25151(15) 0.0398(5) Uani 1 1 d . . . N6 N 0.56036(17) -0.0101(2) 0.16519(15) 0.0490(5) Uani 1 1 d . . . N7 N 0.65485(16) 0.1363(2) 0.25153(16) 0.0465(5) Uani 1 1 d . . . C3 C 0.5474(2) -0.2213(3) 0.44220(19) 0.0605(8) Uani 1 1 d . . . H3 H 0.6039 -0.2682 0.4692 0.073 Uiso 1 1 calc R . . C4 C 0.4825(2) -0.1808(3) 0.48656(19) 0.0642(9) Uani 1 1 d . . . H4 H 0.4841 -0.1947 0.5490 0.077 Uiso 1 1 calc R . . C5 C 0.4141(2) -0.1157(3) 0.42194(18) 0.0524(7) Uani 1 1 d . . . H5 H 0.3595 -0.0752 0.4327 0.063 Uiso 1 1 calc R . . C6 C 0.5286(2) -0.3825(3) 0.1567(2) 0.0521(7) Uani 1 1 d . . . H6 H 0.5887 -0.4244 0.1685 0.062 Uiso 1 1 calc R . . C7 C 0.4482(2) -0.4241(2) 0.0944(2) 0.0532(7) Uani 1 1 d . . . H7 H 0.4409 -0.4990 0.0554 0.064 Uiso 1 1 calc R . . C8 C 0.3797(2) -0.3321(2) 0.10106(16) 0.0421(6) Uani 1 1 d . . . H8 H 0.3158 -0.3345 0.0658 0.051 Uiso 1 1 calc R . . C9 C 0.65953(18) 0.0247(3) 0.30520(18) 0.0419(6) Uani 1 1 d . . . C10 C 0.5949(2) 0.1101(3) 0.1690(2) 0.0515(7) Uani 1 1 d . . . C11 C 0.5723(3) 0.2034(3) 0.0897(2) 0.0779(10) Uani 1 1 d . . . H11A H 0.5307 0.1594 0.0368 0.117 Uiso 1 1 calc R . . H11B H 0.6309 0.2302 0.0749 0.117 Uiso 1 1 calc R . . H11C H 0.5404 0.2818 0.1056 0.117 Uiso 1 1 calc R . . C12 C 0.7005(2) 0.2612(3) 0.2826(2) 0.0606(8) Uani 1 1 d . . . H12A H 0.7124 0.3092 0.2297 0.073 Uiso 1 1 calc R . . H12B H 0.7624 0.2436 0.3262 0.073 Uiso 1 1 calc R . . C13 C 0.6424(3) 0.3479(4) 0.3284(3) 0.0816(11) Uani 1 1 d . . . H13A H 0.5797 0.3618 0.2868 0.122 Uiso 1 1 calc R . . H13B H 0.6741 0.4333 0.3439 0.122 Uiso 1 1 calc R . . H13C H 0.6356 0.3047 0.3843 0.122 Uiso 1 1 calc R . . C14 C 0.3144(2) 0.0194(4) 0.0779(2) 0.0626(9) Uani 1 1 d . . . H14 H 0.3510 -0.0106 0.0342 0.075 Uiso 1 1 calc R . . C15 C 0.2454(2) -0.0689(3) 0.0883(2) 0.0597(9) Uani 1 1 d . . . H15 H 0.2419 -0.1508 0.0506 0.072 Uiso 1 1 calc R . . C16 C 0.1529(2) -0.0334(4) 0.1087(3) 0.0701(9) Uani 1 1 d . . . H16A H 0.1222 -0.1153 0.1226 0.084 Uiso 1 1 calc R . . H16B H 0.1106 0.0069 0.0535 0.084 Uiso 1 1 calc R . . C17 C 0.1639(2) 0.0617(3) 0.1879(2) 0.0617(8) Uani 1 1 d . . . H17A H 0.1137 0.0439 0.2194 0.074 Uiso 1 1 calc R . . H17B H 0.1552 0.1533 0.1640 0.074 Uiso 1 1 calc R . . C18 C 0.2596(2) 0.0508(3) 0.2563(2) 0.0551(7) Uani 1 1 d . . . H18 H 0.2562 0.0310 0.3200 0.066 Uiso 1 1 calc R . . C19 C 0.3391(2) 0.1230(3) 0.2514(2) 0.0580(8) Uani 1 1 d . . . H19 H 0.3815 0.1450 0.3127 0.070 Uiso 1 1 calc R . . C20 C 0.3451(3) 0.2203(3) 0.1797(3) 0.0736(10) Uani 1 1 d . . . H20A H 0.4121 0.2448 0.1872 0.088 Uiso 1 1 calc R . . H20B H 0.3103 0.3014 0.1881 0.088 Uiso 1 1 calc R . . C21 C 0.3046(3) 0.1681(4) 0.0831(3) 0.0832(11) Uani 1 1 d . . . H21A H 0.2369 0.1922 0.0623 0.100 Uiso 1 1 calc R . . H21B H 0.3379 0.2106 0.0414 0.100 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 0.04182(13) 0.03504(12) 0.03503(12) -0.00505(8) 0.00375(8) 0.00630(8) S1 0.0527(4) 0.0605(5) 0.0548(4) 0.0070(4) 0.0043(3) -0.0066(3) B1 0.0355(14) 0.0368(14) 0.0549(18) 0.0125(13) 0.0051(13) 0.0034(12) N1 0.0397(11) 0.0444(12) 0.0431(12) 0.0106(9) 0.0035(9) -0.0067(9) N2 0.0450(12) 0.0416(11) 0.0375(11) 0.0000(9) 0.0084(9) -0.0076(10) N3 0.0402(11) 0.0346(11) 0.0535(13) 0.0041(9) 0.0104(10) 0.0051(9) N4 0.0401(11) 0.0351(10) 0.0390(11) 0.0016(8) 0.0091(9) 0.0040(8) N5 0.0392(11) 0.0364(11) 0.0437(12) 0.0089(9) 0.0104(10) 0.0024(9) N6 0.0554(14) 0.0461(13) 0.0440(12) 0.0127(10) 0.0101(11) 0.0021(11) N7 0.0531(13) 0.0369(12) 0.0551(14) 0.0066(10) 0.0244(11) -0.0016(10) C3 0.0507(16) 0.0695(19) 0.0504(17) 0.0241(15) -0.0065(14) -0.0191(15) C4 0.0664(19) 0.084(2) 0.0363(14) 0.0111(15) 0.0030(14) -0.0265(17) C5 0.0562(17) 0.0617(16) 0.0394(14) -0.0057(13) 0.0123(13) -0.0174(14) C6 0.0556(17) 0.0369(13) 0.0706(19) 0.0057(13) 0.0286(15) 0.0110(13) C7 0.071(2) 0.0371(14) 0.0553(17) -0.0035(12) 0.0232(16) 0.0076(13) C8 0.0555(15) 0.0374(12) 0.0338(12) -0.0008(10) 0.0121(11) 0.0018(11) C9 0.0382(13) 0.0399(13) 0.0527(16) 0.0050(11) 0.0208(12) 0.0002(11) C10 0.0582(17) 0.0467(15) 0.0536(17) 0.0146(13) 0.0221(14) 0.0011(13) C11 0.107(3) 0.064(2) 0.062(2) 0.0266(17) 0.023(2) -0.008(2) C12 0.0674(19) 0.0486(16) 0.0692(19) 0.0061(15) 0.0238(16) -0.0126(14) C13 0.111(3) 0.056(2) 0.086(3) -0.0045(19) 0.039(2) -0.003(2) C14 0.071(2) 0.072(2) 0.0397(15) 0.0033(15) 0.0046(15) 0.0229(19) C15 0.0577(18) 0.0622(19) 0.0463(16) -0.0205(14) -0.0101(14) 0.0261(15) C16 0.0506(18) 0.072(2) 0.076(2) -0.0121(18) -0.0051(16) 0.0179(16) C17 0.0531(18) 0.0550(18) 0.077(2) -0.0116(15) 0.0171(17) 0.0130(14) C18 0.0608(18) 0.0519(16) 0.0510(17) -0.0127(13) 0.0117(14) 0.0130(14) C19 0.0648(19) 0.0408(15) 0.0607(19) -0.0153(14) 0.0022(15) 0.0089(14) C20 0.075(2) 0.0388(16) 0.101(3) -0.0014(17) 0.012(2) 0.0037(15) C21 0.094(3) 0.076(2) 0.076(2) 0.030(2) 0.017(2) 0.024(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 N2 2.081(2) . ? Rh1 C19 2.105(3) . ? Rh1 N4 2.1097(19) . ? Rh1 C15 2.116(3) . ? Rh1 C14 2.138(3) . ? Rh1 C18 2.139(3) . ? S1 C9 1.674(3) . ? B1 N1 1.535(4) . ? B1 N3 1.539(4) . ? B1 N5 1.546(3) . ? B1 H1B 1.0000 . ? N1 C3 1.329(3) . ? N1 N2 1.357(3) . ? N2 C5 1.353(4) . ? N3 C6 1.343(3) . ? N3 N4 1.371(3) . ? N4 C8 1.329(3) . ? N5 C9 1.353(4) . ? N5 N6 1.395(3) . ? N6 C10 1.312(4) . ? N7 C10 1.356(4) . ? N7 C9 1.382(4) . ? N7 C12 1.449(4) . ? C3 C4 1.360(5) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.371(4) . ? C6 H6 0.9500 . ? C7 C8 1.389(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C10 C11 1.495(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.509(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.387(5) . ? C14 C21 1.514(5) . ? C14 H14 1.0000 . ? C15 C16 1.508(5) . ? C15 H15 1.0000 . ? C16 C17 1.513(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.517(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.391(5) . ? C18 H18 1.0000 . ? C19 C20 1.485(5) . ? C19 H19 1.0000 . ? C20 C21 1.525(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 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 N2 Rh1 C19 90.18(11) . . ? N2 Rh1 N4 87.67(8) . . ? C19 Rh1 N4 161.54(11) . . ? N2 Rh1 C15 161.32(12) . . ? C19 Rh1 C15 97.04(11) . . ? N4 Rh1 C15 90.69(9) . . ? N2 Rh1 C14 160.60(12) . . ? C19 Rh1 C14 81.37(13) . . ? N4 Rh1 C14 94.83(10) . . ? C15 Rh1 C14 38.07(13) . . ? N2 Rh1 C18 93.94(11) . . ? C19 Rh1 C18 38.25(13) . . ? N4 Rh1 C18 160.21(10) . . ? C15 Rh1 C18 81.49(12) . . ? C14 Rh1 C18 90.17(13) . . ? N1 B1 N3 109.2(2) . . ? N1 B1 N5 109.9(2) . . ? N3 B1 N5 110.3(2) . . ? N1 B1 H1B 109.2 . . ? N3 B1 H1B 109.2 . . ? N5 B1 H1B 109.2 . . ? C3 N1 N2 109.6(2) . . ? C3 N1 B1 127.9(2) . . ? N2 N1 B1 122.35(19) . . ? C5 N2 N1 105.9(2) . . ? C5 N2 Rh1 131.3(2) . . ? N1 N2 Rh1 121.61(16) . . ? C6 N3 N4 109.3(2) . . ? C6 N3 B1 127.9(2) . . ? N4 N3 B1 122.4(2) . . ? C8 N4 N3 106.2(2) . . ? C8 N4 Rh1 132.78(17) . . ? N3 N4 Rh1 121.06(15) . . ? C9 N5 N6 111.2(2) . . ? C9 N5 B1 126.3(2) . . ? N6 N5 B1 122.3(2) . . ? C10 N6 N5 104.4(2) . . ? C10 N7 C9 107.8(2) . . ? C10 N7 C12 127.2(2) . . ? C9 N7 C12 124.8(3) . . ? N1 C3 C4 109.3(3) . . ? N1 C3 H3 125.4 . . ? C4 C3 H3 125.4 . . ? C3 C4 C5 105.3(3) . . ? C3 C4 H4 127.3 . . ? C5 C4 H4 127.3 . . ? N2 C5 C4 109.9(3) . . ? N2 C5 H5 125.1 . . ? C4 C5 H5 125.1 . . ? N3 C6 C7 108.9(2) . . ? N3 C6 H6 125.5 . . ? C7 C6 H6 125.5 . . ? C6 C7 C8 104.6(2) . . ? C6 C7 H7 127.7 . . ? C8 C7 H7 127.7 . . ? N4 C8 C7 111.0(2) . . ? N4 C8 H8 124.5 . . ? C7 C8 H8 124.5 . . ? N5 C9 N7 104.7(2) . . ? N5 C9 S1 128.8(2) . . ? N7 C9 S1 126.4(2) . . ? N6 C10 N7 111.8(2) . . ? N6 C10 C11 123.1(3) . . ? N7 C10 C11 125.0(3) . . ? 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 C13 112.8(3) . . ? N7 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N7 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? 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 . . ? C15 C14 C21 123.5(3) . . ? C15 C14 Rh1 70.12(18) . . ? C21 C14 Rh1 112.8(2) . . ? C15 C14 H14 114.2 . . ? C21 C14 H14 114.2 . . ? Rh1 C14 H14 114.2 . . ? C14 C15 C16 126.1(3) . . ? C14 C15 Rh1 71.81(17) . . ? C16 C15 Rh1 110.9(2) . . ? C14 C15 H15 113.5 . . ? C16 C15 H15 113.5 . . ? Rh1 C15 H15 113.5 . . ? C15 C16 C17 113.4(3) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C18 112.7(2) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 124.2(3) . . ? C19 C18 Rh1 69.56(18) . . ? C17 C18 Rh1 113.0(2) . . ? C19 C18 H18 114.0 . . ? C17 C18 H18 114.0 . . ? Rh1 C18 H18 114.0 . . ? C18 C19 C20 126.5(3) . . ? C18 C19 Rh1 72.20(17) . . ? C20 C19 Rh1 111.3(2) . . ? C18 C19 H19 113.2 . . ? C20 C19 H19 113.2 . . ? Rh1 C19 H19 113.2 . . ? C19 C20 C21 113.0(3) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C14 C21 C20 112.1(3) . . ? C14 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C14 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 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 N3 B1 N1 C3 126.1(3) . . . . ? N5 B1 N1 C3 -112.9(3) . . . . ? N3 B1 N1 N2 -59.9(3) . . . . ? N5 B1 N1 N2 61.2(3) . . . . ? C3 N1 N2 C5 -0.4(3) . . . . ? B1 N1 N2 C5 -175.5(2) . . . . ? C3 N1 N2 Rh1 -169.31(17) . . . . ? B1 N1 N2 Rh1 15.7(3) . . . . ? C19 Rh1 N2 C5 60.6(3) . . . . ? N4 Rh1 N2 C5 -137.8(3) . . . . ? C15 Rh1 N2 C5 -52.5(4) . . . . ? C14 Rh1 N2 C5 124.3(4) . . . . ? C18 Rh1 N2 C5 22.5(3) . . . . ? C19 Rh1 N2 N1 -133.7(2) . . . . ? N4 Rh1 N2 N1 27.94(18) . . . . ? C15 Rh1 N2 N1 113.2(3) . . . . ? C14 Rh1 N2 N1 -70.0(4) . . . . ? C18 Rh1 N2 N1 -171.81(19) . . . . ? N1 B1 N3 C6 -126.4(3) . . . . ? N5 B1 N3 C6 112.8(3) . . . . ? N1 B1 N3 N4 45.5(3) . . . . ? N5 B1 N3 N4 -75.3(3) . . . . ? C6 N3 N4 C8 0.6(3) . . . . ? B1 N3 N4 C8 -172.6(2) . . . . ? C6 N3 N4 Rh1 -178.92(17) . . . . ? B1 N3 N4 Rh1 7.8(3) . . . . ? N2 Rh1 N4 C8 141.0(2) . . . . ? C19 Rh1 N4 C8 -135.4(3) . . . . ? C15 Rh1 N4 C8 -20.4(2) . . . . ? C14 Rh1 N4 C8 -58.3(2) . . . . ? C18 Rh1 N4 C8 45.8(4) . . . . ? N2 Rh1 N4 N3 -39.58(18) . . . . ? C19 Rh1 N4 N3 44.0(4) . . . . ? C15 Rh1 N4 N3 159.0(2) . . . . ? C14 Rh1 N4 N3 121.1(2) . . . . ? C18 Rh1 N4 N3 -134.8(3) . . . . ? N1 B1 N5 C9 62.9(3) . . . . ? N3 B1 N5 C9 -176.7(2) . . . . ? N1 B1 N5 N6 -111.8(3) . . . . ? N3 B1 N5 N6 8.6(3) . . . . ? C9 N5 N6 C10 -1.0(3) . . . . ? B1 N5 N6 C10 174.4(2) . . . . ? N2 N1 C3 C4 0.9(3) . . . . ? B1 N1 C3 C4 175.6(3) . . . . ? N1 C3 C4 C5 -1.0(3) . . . . ? N1 N2 C5 C4 -0.2(3) . . . . ? Rh1 N2 C5 C4 167.2(2) . . . . ? C3 C4 C5 N2 0.7(3) . . . . ? N4 N3 C6 C7 -0.7(3) . . . . ? B1 N3 C6 C7 172.0(3) . . . . ? N3 C6 C7 C8 0.5(3) . . . . ? N3 N4 C8 C7 -0.3(3) . . . . ? Rh1 N4 C8 C7 179.18(18) . . . . ? C6 C7 C8 N4 -0.1(3) . . . . ? N6 N5 C9 N7 1.0(3) . . . . ? B1 N5 C9 N7 -174.2(2) . . . . ? N6 N5 C9 S1 -175.45(19) . . . . ? B1 N5 C9 S1 9.4(4) . . . . ? C10 N7 C9 N5 -0.6(3) . . . . ? C12 N7 C9 N5 174.7(3) . . . . ? C10 N7 C9 S1 175.9(2) . . . . ? C12 N7 C9 S1 -8.8(4) . . . . ? N5 N6 C10 N7 0.6(3) . . . . ? N5 N6 C10 C11 178.6(3) . . . . ? C9 N7 C10 N6 0.0(3) . . . . ? C12 N7 C10 N6 -175.1(3) . . . . ? C9 N7 C10 C11 -178.0(3) . . . . ? C12 N7 C10 C11 6.9(5) . . . . ? C10 N7 C12 C13 89.6(4) . . . . ? C9 N7 C12 C13 -84.7(4) . . . . ? N2 Rh1 C14 C15 -178.3(3) . . . . ? C19 Rh1 C14 C15 -113.3(2) . . . . ? N4 Rh1 C14 C15 84.94(18) . . . . ? C18 Rh1 C14 C15 -75.89(19) . . . . ? N2 Rh1 C14 C21 -59.4(5) . . . . ? C19 Rh1 C14 C21 5.7(3) . . . . ? N4 Rh1 C14 C21 -156.1(3) . . . . ? C15 Rh1 C14 C21 118.9(3) . . . . ? C18 Rh1 C14 C21 43.0(3) . . . . ? C21 C14 C15 C16 -1.8(5) . . . . ? Rh1 C14 C15 C16 103.0(3) . . . . ? C21 C14 C15 Rh1 -104.8(3) . . . . ? N2 Rh1 C15 C14 178.3(3) . . . . ? C19 Rh1 C15 C14 66.2(2) . . . . ? N4 Rh1 C15 C14 -96.95(18) . . . . ? C18 Rh1 C15 C14 101.3(2) . . . . ? N2 Rh1 C15 C16 55.7(4) . . . . ? C19 Rh1 C15 C16 -56.3(3) . . . . ? N4 Rh1 C15 C16 140.5(3) . . . . ? C14 Rh1 C15 C16 -122.5(3) . . . . ? C18 Rh1 C15 C16 -21.2(3) . . . . ? C14 C15 C16 C17 -49.4(5) . . . . ? Rh1 C15 C16 C17 32.8(4) . . . . ? C15 C16 C17 C18 -27.6(5) . . . . ? C16 C17 C18 C19 89.5(4) . . . . ? C16 C17 C18 Rh1 9.3(4) . . . . ? N2 Rh1 C18 C19 85.27(19) . . . . ? N4 Rh1 C18 C19 179.4(2) . . . . ? C15 Rh1 C18 C19 -113.0(2) . . . . ? C14 Rh1 C18 C19 -75.8(2) . . . . ? N2 Rh1 C18 C17 -155.1(2) . . . . ? C19 Rh1 C18 C17 119.6(3) . . . . ? N4 Rh1 C18 C17 -61.0(4) . . . . ? C15 Rh1 C18 C17 6.7(2) . . . . ? C14 Rh1 C18 C17 43.9(3) . . . . ? C17 C18 C19 C20 -0.8(5) . . . . ? Rh1 C18 C19 C20 103.7(3) . . . . ? C17 C18 C19 Rh1 -104.5(3) . . . . ? N2 Rh1 C19 C18 -96.16(19) . . . . ? N4 Rh1 C19 C18 -179.3(3) . . . . ? C15 Rh1 C19 C18 66.6(2) . . . . ? C14 Rh1 C19 C18 101.4(2) . . . . ? N2 Rh1 C19 C20 140.8(2) . . . . ? N4 Rh1 C19 C20 57.6(4) . . . . ? C15 Rh1 C19 C20 -56.5(3) . . . . ? C14 Rh1 C19 C20 -21.7(2) . . . . ? C18 Rh1 C19 C20 -123.0(3) . . . . ? C18 C19 C20 C21 -48.9(5) . . . . ? Rh1 C19 C20 C21 34.2(4) . . . . ? C15 C14 C21 C20 91.5(4) . . . . ? Rh1 C14 C21 C20 10.9(4) . . . . ? C19 C20 C21 C14 -29.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.480 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.127 data_16 _database_code_depnum_ccdc_archive 'CCDC 792569' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H35 B N8 O P Rh S2, 2(C H2 Cl2)' _chemical_formula_sum 'C34 H39 B Cl4 N8 O P Rh S2' _chemical_formula_weight 926.34 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 11.3740(3) _cell_length_b 13.0039(3) _cell_length_c 14.7214(3) _cell_angle_alpha 82.695(2) _cell_angle_beta 71.098(2) _cell_angle_gamma 81.534(2) _cell_volume 2030.17(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16185 _cell_measurement_theta_min 2.0064 _cell_measurement_theta_max 29.9974 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction - Gemini' _diffrn_measurement_method w/scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45489 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.1176 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.06 _reflns_number_total 10904 _reflns_number_gt 6363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxf Diff Ltd. V 1.171.32.5' _computing_cell_refinement 'CrysAlis RED, Oxf Diff Ltd. V 1.171.32.5' _computing_data_reduction 'CrysAlis RED, Oxf Diff Ltd. V 1.171.32.5' _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^)+(0.0403P)^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 10904 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 1.127458(18) 0.171281(16) 0.306372(14) 0.01551(6) Uani 1 1 d . . . N1 N 0.85302(18) 0.19047(15) 0.42521(14) 0.0147(5) Uani 1 1 d . . . N2 N 0.95443(18) 0.12073(15) 0.38755(13) 0.0138(4) Uani 1 1 d . . . N3 N 0.90492(18) 0.34712(15) 0.48361(13) 0.0137(4) Uani 1 1 d . . . N4 N 0.82718(18) 0.41543(15) 0.54958(14) 0.0152(5) Uani 1 1 d . . . N5 N 1.00427(18) 0.36572(15) 0.58207(14) 0.0145(5) Uani 1 1 d . . . N6 N 0.74462(18) 0.36912(15) 0.39398(14) 0.0152(5) Uani 1 1 d . . . N7 N 0.63104(18) 0.34878(16) 0.46276(14) 0.0178(5) Uani 1 1 d . . . N8 N 0.59752(19) 0.45236(16) 0.34112(15) 0.0183(5) Uani 1 1 d . . . S1 S 1.14453(6) 0.24063(5) 0.44410(4) 0.01728(15) Uani 1 1 d . . . S2 S 0.83066(6) 0.48177(5) 0.21883(5) 0.01977(15) Uani 1 1 d . . . P1 P 1.12495(6) 0.08821(5) 0.18144(5) 0.01461(15) Uani 1 1 d . . . O1 O 1.38311(18) 0.22816(15) 0.19988(13) 0.0318(5) Uani 1 1 d . . . B1 B 0.8670(3) 0.3085(2) 0.4021(2) 0.0157(6) Uani 1 1 d . . . H1 H 0.9345 0.3191 0.3395 0.019 Uiso 1 1 calc R . . C1 C 1.2833(2) 0.2071(2) 0.23938(18) 0.0187(6) Uani 1 1 d . . . C3 C 0.7586(2) 0.1379(2) 0.48287(17) 0.0193(6) Uani 1 1 d . . . H3 H 0.6778 0.1683 0.5177 0.023 Uiso 1 1 calc R . . C4 C 0.7990(2) 0.0324(2) 0.48272(18) 0.0201(6) Uani 1 1 d . . . H4 H 0.7529 -0.0234 0.5168 0.024 Uiso 1 1 calc R . . C5 C 0.9213(2) 0.0256(2) 0.42228(17) 0.0187(6) Uani 1 1 d . . . H5 H 0.9742 -0.0378 0.4076 0.022 Uiso 1 1 calc R . . C6 C 1.0130(2) 0.31751(19) 0.50332(17) 0.0146(5) Uani 1 1 d . . . C7 C 0.8909(2) 0.42559(19) 0.60692(17) 0.0165(5) Uani 1 1 d . . . C8 C 0.8478(2) 0.4915(2) 0.68906(17) 0.0197(6) Uani 1 1 d . . . H8A H 0.7635 0.5261 0.6943 0.030 Uiso 1 1 calc R . . H8B H 0.9051 0.5444 0.6786 0.030 Uiso 1 1 calc R . . H8C H 0.8462 0.4478 0.7487 0.030 Uiso 1 1 calc R . . C9 C 1.0984(2) 0.3508(2) 0.63325(18) 0.0209(6) Uani 1 1 d . . . H9A H 1.0882 0.4117 0.6703 0.025 Uiso 1 1 calc R . . H9B H 1.1832 0.3465 0.5857 0.025 Uiso 1 1 calc R . . C10 C 1.0853(3) 0.2523(2) 0.70123(19) 0.0287(7) Uani 1 1 d . . . H10A H 1.0015 0.2567 0.7485 0.043 Uiso 1 1 calc R . . H10B H 1.1482 0.2447 0.7347 0.043 Uiso 1 1 calc R . . H10C H 1.0978 0.1918 0.6644 0.043 Uiso 1 1 calc R . . C11 C 0.7258(2) 0.43233(19) 0.31827(17) 0.0161(6) Uani 1 1 d . . . C12 C 0.5456(2) 0.39820(19) 0.42841(19) 0.0188(6) Uani 1 1 d . . . C13 C 0.4099(2) 0.3943(2) 0.4754(2) 0.0266(7) Uani 1 1 d . . . H13A H 0.3771 0.3564 0.4371 0.040 Uiso 1 1 calc R . . H13B H 0.3671 0.4655 0.4801 0.040 Uiso 1 1 calc R . . H13C H 0.3954 0.3585 0.5401 0.040 Uiso 1 1 calc R . . C14 C 0.5310(3) 0.5185(2) 0.28121(19) 0.0254(6) Uani 1 1 d . . . H14A H 0.5774 0.5791 0.2506 0.030 Uiso 1 1 calc R . . H14B H 0.4472 0.5453 0.3225 0.030 Uiso 1 1 calc R . . C15 C 0.5165(3) 0.4596(2) 0.2033(2) 0.0337(7) Uani 1 1 d . . . H15A H 0.5994 0.4369 0.1597 0.051 Uiso 1 1 calc R . . H15B H 0.4683 0.5055 0.1667 0.051 Uiso 1 1 calc R . . H15C H 0.4727 0.3984 0.2331 0.051 Uiso 1 1 calc R . . C16 C 1.2174(2) 0.13665(19) 0.06130(17) 0.0172(6) Uani 1 1 d . . . C17 C 1.1653(2) 0.20733(19) 0.00155(18) 0.0201(6) Uani 1 1 d . . . H17 H 1.0778 0.2282 0.0216 0.024 Uiso 1 1 calc R . . C18 C 1.2392(3) 0.2475(2) -0.08663(18) 0.0235(6) Uani 1 1 d . . . H18 H 1.2026 0.2959 -0.1265 0.028 Uiso 1 1 calc R . . C19 C 1.3664(3) 0.2171(2) -0.11659(19) 0.0259(6) Uani 1 1 d . . . H19 H 1.4172 0.2444 -0.1772 0.031 Uiso 1 1 calc R . . C20 C 1.4199(3) 0.1471(2) -0.0587(2) 0.0279(7) Uani 1 1 d . . . H20 H 1.5073 0.1260 -0.0797 0.033 Uiso 1 1 calc R . . C21 C 1.3458(2) 0.1076(2) 0.03021(19) 0.0233(6) Uani 1 1 d . . . H21 H 1.3833 0.0602 0.0702 0.028 Uiso 1 1 calc R . . C22 C 1.1873(2) -0.04980(19) 0.18593(17) 0.0156(5) Uani 1 1 d . . . C23 C 1.2177(2) -0.0955(2) 0.26742(18) 0.0197(6) Uani 1 1 d . . . H23 H 1.2040 -0.0553 0.3202 0.024 Uiso 1 1 calc R . . C24 C 1.2681(2) -0.1998(2) 0.27218(19) 0.0243(6) Uani 1 1 d . . . H24 H 1.2879 -0.2307 0.3282 0.029 Uiso 1 1 calc R . . C25 C 1.2892(2) -0.2580(2) 0.1947(2) 0.0267(7) Uani 1 1 d . . . H25 H 1.3237 -0.3290 0.1975 0.032 Uiso 1 1 calc R . . C26 C 1.2602(2) -0.2128(2) 0.11377(19) 0.0237(6) Uani 1 1 d . . . H26 H 1.2748 -0.2530 0.0608 0.028 Uiso 1 1 calc R . . C27 C 1.2101(2) -0.1098(2) 0.10870(18) 0.0203(6) Uani 1 1 d . . . H27 H 1.1909 -0.0796 0.0522 0.024 Uiso 1 1 calc R . . C28 C 0.9683(2) 0.09397(19) 0.17063(16) 0.0143(5) Uani 1 1 d . . . C29 C 0.9212(2) 0.0102(2) 0.14924(17) 0.0201(6) Uani 1 1 d . . . H29 H 0.9696 -0.0561 0.1426 0.024 Uiso 1 1 calc R . . C30 C 0.8029(2) 0.0237(2) 0.13757(18) 0.0230(6) Uani 1 1 d . . . H30 H 0.7712 -0.0334 0.1225 0.028 Uiso 1 1 calc R . . C31 C 0.7314(2) 0.1199(2) 0.14782(18) 0.0243(6) Uani 1 1 d . . . H31 H 0.6511 0.1288 0.1393 0.029 Uiso 1 1 calc R . . C32 C 0.7770(2) 0.2030(2) 0.17044(18) 0.0227(6) Uani 1 1 d . . . H32 H 0.7280 0.2689 0.1783 0.027 Uiso 1 1 calc R . . C33 C 0.8947(2) 0.18912(19) 0.18144(17) 0.0166(6) Uani 1 1 d . . . H33 H 0.9258 0.2464 0.1968 0.020 Uiso 1 1 calc R . . C34 C 0.8491(3) 0.5283(2) 0.9568(2) 0.0311(7) Uani 1 1 d . . . H34A H 0.8436 0.5476 1.0211 0.037 Uiso 1 1 calc R . . H34B H 0.9080 0.5714 0.9077 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.90745(7) 0.39529(6) 0.94733(5) 0.03341(18) Uani 1 1 d . . . Cl2 Cl 0.70081(7) 0.55516(7) 0.94080(6) 0.0488(2) Uani 1 1 d . . . C35A C 0.4155(3) 0.9891(3) 0.6318(2) 0.0528(10) Uani 0.809(2) 1 d P A 1 H35A H 0.4085 1.0293 0.5717 0.063 Uiso 0.809(2) 1 calc PR A 1 H35B H 0.3302 0.9776 0.6742 0.063 Uiso 0.809(2) 1 calc PR A 1 Cl3A Cl 0.50850(9) 0.86436(8) 0.60412(7) 0.0393(3) Uani 0.809(2) 1 d P A 1 Cl4A Cl 0.4853(3) 1.0584(2) 0.6886(2) 0.0744(10) Uani 0.809(2) 1 d P A 1 C35B C 0.4155(3) 0.9891(3) 0.6318(2) 0.0528(10) Uani 0.191(2) 1 d P A 2 H35C H 0.3333 0.9739 0.6777 0.063 Uiso 0.191(2) 1 calc PR A 2 H35D H 0.4509 0.9335 0.5873 0.063 Uiso 0.191(2) 1 calc PR A 2 Cl3B Cl 0.4124(5) 1.1418(4) 0.5602(5) 0.074(2) Uani 0.191(2) 1 d P A 2 Cl4B Cl 0.5178(13) 1.0171(12) 0.6870(8) 0.105(5) Uani 0.191(2) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01613(11) 0.01420(12) 0.01725(12) -0.00199(8) -0.00622(8) -0.00212(8) N1 0.0140(11) 0.0151(12) 0.0163(11) -0.0002(9) -0.0073(9) -0.0007(9) N2 0.0151(11) 0.0124(12) 0.0152(11) -0.0023(9) -0.0068(9) 0.0004(9) N3 0.0150(11) 0.0119(11) 0.0141(11) -0.0008(9) -0.0042(9) -0.0023(9) N4 0.0160(11) 0.0132(11) 0.0146(11) -0.0010(9) -0.0027(9) -0.0012(9) N5 0.0150(11) 0.0131(11) 0.0164(11) -0.0010(9) -0.0065(9) -0.0010(9) N6 0.0155(11) 0.0131(12) 0.0175(11) -0.0007(9) -0.0058(9) -0.0022(9) N7 0.0131(11) 0.0169(12) 0.0226(12) -0.0004(10) -0.0045(9) -0.0028(9) N8 0.0183(11) 0.0131(12) 0.0272(13) -0.0004(10) -0.0135(10) 0.0000(9) S1 0.0151(3) 0.0183(4) 0.0207(4) -0.0060(3) -0.0083(3) 0.0007(3) S2 0.0257(4) 0.0170(4) 0.0184(3) 0.0022(3) -0.0101(3) -0.0038(3) P1 0.0159(3) 0.0125(4) 0.0156(3) -0.0011(3) -0.0053(3) -0.0016(3) O1 0.0241(11) 0.0381(13) 0.0341(12) -0.0020(10) -0.0063(9) -0.0133(10) B1 0.0126(14) 0.0195(17) 0.0159(15) -0.0021(13) -0.0057(12) -0.0014(12) C1 0.0243(15) 0.0166(15) 0.0191(14) -0.0049(11) -0.0113(12) -0.0018(12) C3 0.0166(14) 0.0227(16) 0.0171(14) 0.0020(12) -0.0044(11) -0.0027(12) C4 0.0211(14) 0.0139(14) 0.0255(15) 0.0027(11) -0.0082(12) -0.0043(11) C5 0.0237(14) 0.0143(14) 0.0227(15) -0.0009(11) -0.0137(12) -0.0023(11) C6 0.0192(14) 0.0131(14) 0.0135(13) 0.0008(11) -0.0067(11) -0.0058(11) C7 0.0190(13) 0.0123(14) 0.0161(13) 0.0029(11) -0.0040(11) -0.0025(11) C8 0.0228(14) 0.0172(15) 0.0198(14) -0.0051(12) -0.0067(12) -0.0014(11) C9 0.0154(13) 0.0289(17) 0.0213(14) -0.0046(12) -0.0090(11) -0.0017(12) C10 0.0327(17) 0.0328(18) 0.0238(16) 0.0016(13) -0.0171(13) 0.0016(14) C11 0.0185(13) 0.0149(14) 0.0209(14) -0.0035(11) -0.0138(11) -0.0017(11) C12 0.0176(14) 0.0099(14) 0.0310(16) -0.0049(12) -0.0099(12) -0.0003(11) C13 0.0170(14) 0.0212(16) 0.0433(18) -0.0071(14) -0.0107(13) -0.0004(12) C14 0.0270(15) 0.0190(15) 0.0364(17) 0.0002(13) -0.0215(13) 0.0027(12) C15 0.0376(18) 0.0306(18) 0.0416(18) -0.0074(15) -0.0279(15) 0.0079(14) C16 0.0221(14) 0.0117(14) 0.0183(14) -0.0037(11) -0.0055(11) -0.0035(11) C17 0.0246(15) 0.0137(14) 0.0221(15) -0.0034(12) -0.0084(12) 0.0013(11) C18 0.0332(17) 0.0161(15) 0.0209(15) -0.0006(12) -0.0092(13) -0.0014(12) C19 0.0316(17) 0.0180(15) 0.0198(15) 0.0035(12) 0.0029(12) -0.0063(13) C20 0.0234(15) 0.0212(16) 0.0336(17) -0.0007(13) -0.0024(13) -0.0017(12) C21 0.0231(15) 0.0175(15) 0.0264(16) 0.0026(12) -0.0063(12) -0.0005(12) C22 0.0138(13) 0.0127(14) 0.0211(14) -0.0005(11) -0.0059(11) -0.0038(10) C23 0.0180(14) 0.0182(15) 0.0214(14) -0.0008(12) -0.0035(11) -0.0041(11) C24 0.0204(15) 0.0237(16) 0.0272(16) 0.0058(13) -0.0067(12) -0.0060(12) C25 0.0212(15) 0.0130(15) 0.0412(18) 0.0024(13) -0.0058(13) -0.0009(12) C26 0.0246(15) 0.0179(16) 0.0291(16) -0.0085(13) -0.0059(13) -0.0042(12) C27 0.0203(14) 0.0206(15) 0.0206(14) 0.0008(12) -0.0070(11) -0.0047(12) C28 0.0172(13) 0.0151(14) 0.0110(12) 0.0001(10) -0.0052(10) -0.0025(11) C29 0.0229(15) 0.0184(15) 0.0187(14) -0.0017(11) -0.0062(12) -0.0016(12) C30 0.0249(15) 0.0249(16) 0.0234(15) -0.0057(12) -0.0099(12) -0.0073(13) C31 0.0165(14) 0.0317(17) 0.0263(15) -0.0037(13) -0.0090(12) -0.0012(12) C32 0.0205(14) 0.0195(15) 0.0288(16) -0.0064(12) -0.0094(12) 0.0031(12) C33 0.0206(14) 0.0151(14) 0.0178(14) 0.0007(11) -0.0105(11) -0.0045(11) C34 0.0338(17) 0.0260(17) 0.0386(18) -0.0072(14) -0.0180(14) -0.0001(14) Cl1 0.0385(4) 0.0236(4) 0.0403(4) -0.0016(3) -0.0160(4) -0.0025(3) Cl2 0.0361(5) 0.0726(7) 0.0422(5) -0.0191(5) -0.0227(4) 0.0162(4) C35A 0.047(2) 0.079(3) 0.0305(19) -0.0001(18) -0.0086(17) -0.014(2) Cl3A 0.0436(6) 0.0360(6) 0.0403(6) 0.0000(5) -0.0170(5) -0.0043(5) Cl4A 0.0752(19) 0.0904(14) 0.0548(13) -0.0385(12) 0.0152(11) -0.0541(12) C35B 0.047(2) 0.079(3) 0.0305(19) -0.0001(18) -0.0086(17) -0.014(2) Cl3B 0.051(3) 0.057(4) 0.111(5) 0.012(3) -0.027(3) -0.012(3) Cl4B 0.058(6) 0.241(16) 0.030(5) 0.032(7) -0.023(5) -0.077(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 1.824(3) . ? Rh1 N2 2.095(2) . ? Rh1 P1 2.2579(6) . ? Rh1 S1 2.3944(6) . ? N1 C3 1.349(3) . ? N1 N2 1.366(3) . ? N1 B1 1.550(3) . ? N2 C5 1.336(3) . ? N3 C6 1.345(3) . ? N3 N4 1.395(3) . ? N3 B1 1.559(3) . ? N4 C7 1.307(3) . ? N5 C6 1.356(3) . ? N5 C7 1.369(3) . ? N5 C9 1.475(3) . ? N6 C11 1.354(3) . ? N6 N7 1.396(3) . ? N6 B1 1.527(3) . ? N7 C12 1.290(3) . ? N8 C12 1.377(3) . ? N8 C11 1.379(3) . ? N8 C14 1.462(3) . ? S1 C6 1.713(2) . ? S2 C11 1.683(3) . ? P1 C16 1.827(3) . ? P1 C28 1.830(2) . ? P1 C22 1.831(2) . ? O1 C1 1.151(3) . ? B1 H1 1.0000 . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.481(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.516(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.479(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.521(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.391(3) . ? C16 C17 1.393(3) . ? C17 C18 1.384(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.377(4) . ? C19 H19 0.9500 . ? C20 C21 1.389(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.392(3) . ? C22 C27 1.395(3) . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 C27 1.379(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.384(3) . ? C28 C29 1.394(3) . ? C29 C30 1.393(3) . ? C29 H29 0.9500 . ? C30 C31 1.385(4) . ? C30 H30 0.9500 . ? C31 C32 1.385(3) . ? C31 H31 0.9500 . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 Cl2 1.757(3) . ? C34 Cl1 1.765(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35A Cl4A 1.724(4) . ? C35A Cl3A 1.817(4) . ? C35A H35A 0.9900 . ? C35A 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 N2 175.96(10) . . ? C1 Rh1 P1 90.62(7) . . ? N2 Rh1 P1 89.58(5) . . ? C1 Rh1 S1 88.39(7) . . ? N2 Rh1 S1 90.94(5) . . ? P1 Rh1 S1 173.06(2) . . ? C3 N1 N2 109.1(2) . . ? C3 N1 B1 132.4(2) . . ? N2 N1 B1 118.38(19) . . ? C5 N2 N1 106.9(2) . . ? C5 N2 Rh1 131.58(17) . . ? N1 N2 Rh1 121.06(15) . . ? C6 N3 N4 110.20(17) . . ? C6 N3 B1 125.95(19) . . ? N4 N3 B1 123.80(18) . . ? C7 N4 N3 105.01(19) . . ? C6 N5 C7 107.50(19) . . ? C6 N5 C9 125.3(2) . . ? C7 N5 C9 127.1(2) . . ? C11 N6 N7 111.02(19) . . ? C11 N6 B1 128.0(2) . . ? N7 N6 B1 120.2(2) . . ? C12 N7 N6 105.5(2) . . ? C12 N8 C11 107.8(2) . . ? C12 N8 C14 127.1(2) . . ? C11 N8 C14 125.1(2) . . ? C6 S1 Rh1 113.56(8) . . ? C16 P1 C28 103.16(11) . . ? C16 P1 C22 101.87(11) . . ? C28 P1 C22 106.80(11) . . ? C16 P1 Rh1 116.78(8) . . ? C28 P1 Rh1 112.98(8) . . ? C22 P1 Rh1 113.95(8) . . ? N6 B1 N1 110.36(19) . . ? N6 B1 N3 110.8(2) . . ? N1 B1 N3 108.5(2) . . ? N6 B1 H1 109.0 . . ? N1 B1 H1 109.0 . . ? N3 B1 H1 109.0 . . ? O1 C1 Rh1 177.5(2) . . ? N1 C3 C4 108.5(2) . . ? N1 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? C3 C4 C5 105.1(2) . . ? C3 C4 H4 127.4 . . ? C5 C4 H4 127.4 . . ? N2 C5 C4 110.4(2) . . ? N2 C5 H5 124.8 . . ? C4 C5 H5 124.8 . . ? N3 C6 N5 106.3(2) . . ? N3 C6 S1 130.79(17) . . ? N5 C6 S1 122.90(18) . . ? N4 C7 N5 111.0(2) . . ? N4 C7 C8 125.5(2) . . ? N5 C7 C8 123.5(2) . . ? 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 . . ? N5 C9 C10 111.2(2) . . ? N5 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N5 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? 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 . . ? N6 C11 N8 104.5(2) . . ? N6 C11 S2 129.69(18) . . ? N8 C11 S2 125.75(19) . . ? N7 C12 N8 111.1(2) . . ? N7 C12 C13 124.3(2) . . ? N8 C12 C13 124.6(2) . . ? 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 . . ? N8 C14 C15 111.9(2) . . ? N8 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N8 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 . . ? C21 C16 C17 118.3(2) . . ? C21 C16 P1 119.2(2) . . ? C17 C16 P1 122.35(19) . . ? C18 C17 C16 120.9(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 120.7(3) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C23 C22 C27 118.7(2) . . ? C23 C22 P1 119.14(18) . . ? C27 C22 P1 122.09(19) . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 120.0(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.7(2) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 120.4(2) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C33 C28 C29 118.7(2) . . ? C33 C28 P1 117.10(17) . . ? C29 C28 P1 124.16(19) . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.3(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 119.4(2) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C28 121.7(2) . . ? C32 C33 H33 119.2 . . ? C28 C33 H33 119.2 . . ? Cl2 C34 Cl1 111.89(15) . . ? Cl2 C34 H34A 109.2 . . ? Cl1 C34 H34A 109.2 . . ? Cl2 C34 H34B 109.2 . . ? Cl1 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? Cl4A C35A Cl3A 109.6(2) . . ? Cl4A C35A H35A 109.8 . . ? Cl3A C35A H35A 109.8 . . ? Cl4A C35A H35B 109.8 . . ? Cl3A C35A H35B 109.8 . . ? H35A C35A H35B 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 C3 N1 N2 C5 0.1(2) . . . . ? B1 N1 N2 C5 176.28(19) . . . . ? C3 N1 N2 Rh1 -173.05(14) . . . . ? B1 N1 N2 Rh1 3.1(2) . . . . ? P1 Rh1 N2 C5 66.6(2) . . . . ? S1 Rh1 N2 C5 -106.5(2) . . . . ? P1 Rh1 N2 N1 -122.12(15) . . . . ? S1 Rh1 N2 N1 64.79(15) . . . . ? C6 N3 N4 C7 0.4(3) . . . . ? B1 N3 N4 C7 178.0(2) . . . . ? C11 N6 N7 C12 0.6(2) . . . . ? B1 N6 N7 C12 -169.68(19) . . . . ? C1 Rh1 S1 C6 134.83(12) . . . . ? N2 Rh1 S1 C6 -49.16(11) . . . . ? C1 Rh1 P1 C16 -28.30(13) . . . . ? N2 Rh1 P1 C16 155.74(11) . . . . ? C1 Rh1 P1 C28 -147.71(12) . . . . ? N2 Rh1 P1 C28 36.33(10) . . . . ? C1 Rh1 P1 C22 90.15(12) . . . . ? N2 Rh1 P1 C22 -85.81(10) . . . . ? C11 N6 B1 N1 -122.9(2) . . . . ? N7 N6 B1 N1 45.6(3) . . . . ? C11 N6 B1 N3 116.9(2) . . . . ? N7 N6 B1 N3 -74.7(3) . . . . ? C3 N1 B1 N6 -39.0(3) . . . . ? N2 N1 B1 N6 145.90(19) . . . . ? C3 N1 B1 N3 82.6(3) . . . . ? N2 N1 B1 N3 -92.5(2) . . . . ? C6 N3 B1 N6 -173.1(2) . . . . ? N4 N3 B1 N6 9.6(3) . . . . ? C6 N3 B1 N1 65.6(3) . . . . ? N4 N3 B1 N1 -111.7(2) . . . . ? N2 N1 C3 C4 0.0(3) . . . . ? B1 N1 C3 C4 -175.4(2) . . . . ? N1 C3 C4 C5 -0.1(3) . . . . ? N1 N2 C5 C4 -0.2(3) . . . . ? Rh1 N2 C5 C4 171.98(16) . . . . ? C3 C4 C5 N2 0.2(3) . . . . ? N4 N3 C6 N5 0.6(3) . . . . ? B1 N3 C6 N5 -177.0(2) . . . . ? N4 N3 C6 S1 -176.49(19) . . . . ? B1 N3 C6 S1 5.9(4) . . . . ? C7 N5 C6 N3 -1.3(3) . . . . ? C9 N5 C6 N3 175.9(2) . . . . ? C7 N5 C6 S1 176.10(18) . . . . ? C9 N5 C6 S1 -6.7(3) . . . . ? Rh1 S1 C6 N3 -2.2(3) . . . . ? Rh1 S1 C6 N5 -178.82(17) . . . . ? N3 N4 C7 N5 -1.2(3) . . . . ? N3 N4 C7 C8 179.5(2) . . . . ? C6 N5 C7 N4 1.6(3) . . . . ? C9 N5 C7 N4 -175.6(2) . . . . ? C6 N5 C7 C8 -179.1(2) . . . . ? C9 N5 C7 C8 3.8(4) . . . . ? C6 N5 C9 C10 -80.8(3) . . . . ? C7 N5 C9 C10 95.8(3) . . . . ? N7 N6 C11 N8 0.5(2) . . . . ? B1 N6 C11 N8 169.8(2) . . . . ? N7 N6 C11 S2 178.41(17) . . . . ? B1 N6 C11 S2 -12.3(4) . . . . ? C12 N8 C11 N6 -1.4(2) . . . . ? C14 N8 C11 N6 179.4(2) . . . . ? C12 N8 C11 S2 -179.36(17) . . . . ? C14 N8 C11 S2 1.4(3) . . . . ? N6 N7 C12 N8 -1.5(3) . . . . ? N6 N7 C12 C13 176.8(2) . . . . ? C11 N8 C12 N7 1.9(3) . . . . ? C14 N8 C12 N7 -179.0(2) . . . . ? C11 N8 C12 C13 -176.4(2) . . . . ? C14 N8 C12 C13 2.8(4) . . . . ? C12 N8 C14 C15 -95.7(3) . . . . ? C11 N8 C14 C15 83.4(3) . . . . ? C28 P1 C16 C21 -155.51(19) . . . . ? C22 P1 C16 C21 -44.9(2) . . . . ? Rh1 P1 C16 C21 79.9(2) . . . . ? C28 P1 C16 C17 28.7(2) . . . . ? C22 P1 C16 C17 139.4(2) . . . . ? Rh1 P1 C16 C17 -95.82(19) . . . . ? C21 C16 C17 C18 0.2(4) . . . . ? P1 C16 C17 C18 175.95(18) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 -0.4(4) . . . . ? C19 C20 C21 C16 0.9(4) . . . . ? C17 C16 C21 C20 -0.8(4) . . . . ? P1 C16 C21 C20 -176.72(19) . . . . ? C16 P1 C22 C23 133.5(2) . . . . ? C28 P1 C22 C23 -118.6(2) . . . . ? Rh1 P1 C22 C23 6.9(2) . . . . ? C16 P1 C22 C27 -43.9(2) . . . . ? C28 P1 C22 C27 63.9(2) . . . . ? Rh1 P1 C22 C27 -170.58(17) . . . . ? C27 C22 C23 C24 -0.9(4) . . . . ? P1 C22 C23 C24 -178.50(19) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C23 C24 C25 C26 -0.1(4) . . . . ? C24 C25 C26 C27 0.0(4) . . . . ? C25 C26 C27 C22 -0.3(4) . . . . ? C23 C22 C27 C26 0.8(4) . . . . ? P1 C22 C27 C26 178.28(19) . . . . ? C16 P1 C28 C33 -83.1(2) . . . . ? C22 P1 C28 C33 169.93(18) . . . . ? Rh1 P1 C28 C33 43.9(2) . . . . ? C16 P1 C28 C29 94.6(2) . . . . ? C22 P1 C28 C29 -12.3(2) . . . . ? Rh1 P1 C28 C29 -138.36(19) . . . . ? C33 C28 C29 C30 1.1(4) . . . . ? P1 C28 C29 C30 -176.66(19) . . . . ? C28 C29 C30 C31 -0.5(4) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 0.8(4) . . . . ? C31 C32 C33 C28 -0.1(4) . . . . ? C29 C28 C33 C32 -0.8(4) . . . . ? P1 C28 C33 C32 177.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.981 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.102 data_17 _database_code_depnum_ccdc_archive 'CCDC 792570' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H57 B N8 O P Rh S2, 0.5(C6 H14), 2(C H Cl3) ' _chemical_formula_sum 'C39 H66 B Cl6 N8 O P Rh S2' _chemical_formula_weight 1084.51 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' 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' N N 0.0061 0.0033 '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 12.598(3) _cell_length_b 13.928(3) _cell_length_c 15.347(3) _cell_angle_alpha 78.64(3) _cell_angle_beta 72.48(3) _cell_angle_gamma 79.16(3) _cell_volume 2493.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8567 _cell_measurement_theta_min 2.1185 _cell_measurement_theta_max 27.4515 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6391 _exptl_absorpt_correction_T_max 0.8214 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28328 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11391 _reflns_number_gt 9714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _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^)+(0.0394P)^2^+2.0610P] 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 11391 _refine_ls_number_parameters 568 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.047 _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 0.227681(14) 0.279576(13) 0.422945(12) 0.01156(5) Uani 1 1 d . . . P1 P 0.24115(5) 0.34417(4) 0.27203(4) 0.01291(12) Uani 1 1 d . . . S1 S 0.40393(5) 0.17351(4) 0.38714(4) 0.01543(12) Uani 1 1 d . . . S2 S 0.14826(5) 0.44510(4) 0.66652(4) 0.01643(12) Uani 1 1 d . . . O1 O 0.00596(14) 0.40127(14) 0.48118(13) 0.0222(4) Uani 1 1 d . . . B1 B 0.3482(2) 0.26288(19) 0.60130(19) 0.0133(5) Uani 1 1 d . . . H1 H 0.3620 0.2697 0.6605 0.016 Uiso 1 1 calc R . . N1 N 0.24218(15) 0.21246(14) 0.62518(14) 0.0132(4) Uani 1 1 d . . . N2 N 0.19042(15) 0.20662(15) 0.56016(14) 0.0137(4) Uani 1 1 d . . . N3 N 0.45291(15) 0.19840(14) 0.54669(14) 0.0137(4) Uani 1 1 d . . . N4 N 0.54140(16) 0.16777(15) 0.58744(14) 0.0160(4) Uani 1 1 d . . . N5 N 0.57640(15) 0.10037(14) 0.46134(14) 0.0135(4) Uani 1 1 d . . . N6 N 0.33607(15) 0.36743(14) 0.54450(13) 0.0126(4) Uani 1 1 d . . . N7 N 0.42102(16) 0.39816(15) 0.46727(13) 0.0145(4) Uani 1 1 d . . . N8 N 0.29992(15) 0.52646(14) 0.51422(14) 0.0134(4) Uani 1 1 d . . . C1 C 0.09213(19) 0.35638(18) 0.45461(16) 0.0157(5) Uani 1 1 d . . . C3 C 0.10365(19) 0.15632(17) 0.60371(17) 0.0158(5) Uani 1 1 d . . . C4 C 0.09870(19) 0.13030(18) 0.69684(17) 0.0173(5) Uani 1 1 d . . . H4 H 0.0453 0.0946 0.7430 0.021 Uiso 1 1 calc R . . C5 C 0.18699(19) 0.16674(17) 0.70858(16) 0.0154(5) Uani 1 1 d . . . C6 C 0.0262(2) 0.1369(2) 0.55376(19) 0.0223(5) Uani 1 1 d . . . H6A H -0.0347 0.1923 0.5542 0.033 Uiso 1 1 calc R . . H6B H -0.0056 0.0759 0.5846 0.033 Uiso 1 1 calc R . . H6C H 0.0682 0.1296 0.4898 0.033 Uiso 1 1 calc R . . C7 C 0.2208(2) 0.1590(2) 0.79533(18) 0.0248(6) Uani 1 1 d . . . H7A H 0.2879 0.1099 0.7938 0.037 Uiso 1 1 calc R . . H7B H 0.1593 0.1386 0.8487 0.037 Uiso 1 1 calc R . . H7C H 0.2372 0.2234 0.8004 0.037 Uiso 1 1 calc R . . C8 C 0.47480(18) 0.15892(17) 0.46963(16) 0.0127(4) Uani 1 1 d . . . C9 C 0.61384(19) 0.10949(17) 0.53421(17) 0.0161(5) Uani 1 1 d . . . C10 C 0.7240(2) 0.0606(2) 0.54902(19) 0.0218(5) Uani 1 1 d . . . H10A H 0.7327 0.0790 0.6046 0.033 Uiso 1 1 calc R . . H10B H 0.7848 0.0818 0.4955 0.033 Uiso 1 1 calc R . . H10C H 0.7269 -0.0113 0.5567 0.033 Uiso 1 1 calc R . . C11 C 0.63415(19) 0.03974(17) 0.38791(17) 0.0165(5) Uani 1 1 d . . . H11A H 0.5775 0.0174 0.3664 0.020 Uiso 1 1 calc R . . H11B H 0.6787 -0.0196 0.4132 0.020 Uiso 1 1 calc R . . C12 C 0.7115(2) 0.0968(2) 0.30642(19) 0.0248(6) Uani 1 1 d . . . H12A H 0.6688 0.1584 0.2844 0.037 Uiso 1 1 calc R . . H12B H 0.7426 0.0566 0.2565 0.037 Uiso 1 1 calc R . . H12C H 0.7729 0.1123 0.3259 0.037 Uiso 1 1 calc R . . C13 C 0.26249(18) 0.44528(17) 0.57479(16) 0.0124(4) Uani 1 1 d . . . C14 C 0.39638(18) 0.49371(18) 0.45112(16) 0.0141(5) Uani 1 1 d . . . C15 C 0.4638(2) 0.55963(19) 0.37409(17) 0.0194(5) Uani 1 1 d . . . H15A H 0.5338 0.5211 0.3433 0.029 Uiso 1 1 calc R . . H15B H 0.4814 0.6126 0.3989 0.029 Uiso 1 1 calc R . . H15C H 0.4206 0.5885 0.3295 0.029 Uiso 1 1 calc R . . C16 C 0.2495(2) 0.62896(18) 0.52256(18) 0.0195(5) Uani 1 1 d . . . H16A H 0.1667 0.6328 0.5414 0.023 Uiso 1 1 calc R . . H16B H 0.2717 0.6705 0.4615 0.023 Uiso 1 1 calc R . . C17 C 0.2854(2) 0.66918(19) 0.59226(19) 0.0234(6) Uani 1 1 d . . . H17A H 0.2629 0.6287 0.6530 0.035 Uiso 1 1 calc R . . H17B H 0.2493 0.7376 0.5961 0.035 Uiso 1 1 calc R . . H17C H 0.3672 0.6674 0.5729 0.035 Uiso 1 1 calc R . . C18 C 0.16386(19) 0.27621(18) 0.22454(17) 0.0151(5) Uani 1 1 d . . . H18 H 0.1784 0.3012 0.1569 0.018 Uiso 1 1 calc R . . C19 C 0.03624(19) 0.29092(18) 0.26757(18) 0.0175(5) Uani 1 1 d . . . H19A H 0.0192 0.2682 0.3350 0.021 Uiso 1 1 calc R . . H19B H 0.0068 0.3621 0.2576 0.021 Uiso 1 1 calc R . . C20 C -0.0213(2) 0.23296(19) 0.22435(18) 0.0201(5) Uani 1 1 d . . . H20A H -0.1033 0.2420 0.2540 0.024 Uiso 1 1 calc R . . H20B H -0.0088 0.2591 0.1578 0.024 Uiso 1 1 calc R . . C21 C 0.0240(2) 0.12280(19) 0.2358(2) 0.0254(6) Uani 1 1 d . . . H21A H 0.0053 0.0951 0.3023 0.030 Uiso 1 1 calc R . . H21B H -0.0122 0.0877 0.2048 0.030 Uiso 1 1 calc R . . C22 C 0.1506(2) 0.1065(2) 0.1947(2) 0.0295(6) Uani 1 1 d . . . H22A H 0.1686 0.1267 0.1269 0.035 Uiso 1 1 calc R . . H22B H 0.1788 0.0352 0.2069 0.035 Uiso 1 1 calc R . . C23 C 0.2096(2) 0.16556(19) 0.2356(2) 0.0244(6) Uani 1 1 d . . . H23A H 0.2912 0.1567 0.2045 0.029 Uiso 1 1 calc R . . H23B H 0.1991 0.1397 0.3021 0.029 Uiso 1 1 calc R . . C24 C 0.38557(19) 0.32760(18) 0.19409(16) 0.0162(5) Uani 1 1 d . . . H24 H 0.4148 0.2567 0.2114 0.019 Uiso 1 1 calc R . . C25 C 0.4016(2) 0.3395(2) 0.08936(17) 0.0225(5) Uani 1 1 d . . . H25A H 0.3532 0.2986 0.0768 0.027 Uiso 1 1 calc R . . H25B H 0.3789 0.4094 0.0658 0.027 Uiso 1 1 calc R . . C26 C 0.5245(2) 0.3078(2) 0.03952(19) 0.0266(6) Uani 1 1 d . . . H26A H 0.5440 0.2358 0.0575 0.032 Uiso 1 1 calc R . . H26B H 0.5342 0.3205 -0.0280 0.032 Uiso 1 1 calc R . . C27 C 0.6038(2) 0.3626(2) 0.06224(19) 0.0273(6) Uani 1 1 d . . . H27A H 0.5906 0.4337 0.0377 0.033 Uiso 1 1 calc R . . H27B H 0.6825 0.3368 0.0322 0.033 Uiso 1 1 calc R . . C28 C 0.5860(2) 0.3501(2) 0.16649(19) 0.0238(6) Uani 1 1 d . . . H28A H 0.6052 0.2795 0.1903 0.029 Uiso 1 1 calc R . . H28B H 0.6366 0.3883 0.1798 0.029 Uiso 1 1 calc R . . C29 C 0.4647(2) 0.3858(2) 0.21532(18) 0.0199(5) Uani 1 1 d . . . H29A H 0.4464 0.4572 0.1941 0.024 Uiso 1 1 calc R . . H29B H 0.4546 0.3762 0.2828 0.024 Uiso 1 1 calc R . . C30 C 0.17423(19) 0.47415(17) 0.25251(16) 0.0142(5) Uani 1 1 d . . . H30 H 0.0930 0.4737 0.2866 0.017 Uiso 1 1 calc R . . C31 C 0.2159(2) 0.54514(19) 0.29563(18) 0.0195(5) Uani 1 1 d . . . H31A H 0.2104 0.5183 0.3613 0.023 Uiso 1 1 calc R . . H31B H 0.2959 0.5505 0.2633 0.023 Uiso 1 1 calc R . . C32 C 0.1470(2) 0.64754(19) 0.28911(18) 0.0212(5) Uani 1 1 d . . . H32A H 0.1776 0.6924 0.3151 0.025 Uiso 1 1 calc R . . H32B H 0.0683 0.6431 0.3262 0.025 Uiso 1 1 calc R . . C33 C 0.1494(2) 0.69014(19) 0.18860(18) 0.0219(5) Uani 1 1 d . . . H33A H 0.1012 0.7550 0.1865 0.026 Uiso 1 1 calc R . . H33B H 0.2272 0.7005 0.1527 0.026 Uiso 1 1 calc R . . C34 C 0.1077(2) 0.62003(19) 0.14534(18) 0.0196(5) Uani 1 1 d . . . H34A H 0.0276 0.6148 0.1776 0.024 Uiso 1 1 calc R . . H34B H 0.1134 0.6471 0.0797 0.024 Uiso 1 1 calc R . . C35 C 0.1763(2) 0.51743(18) 0.15169(17) 0.0177(5) Uani 1 1 d . . . H35A H 0.2549 0.5217 0.1145 0.021 Uiso 1 1 calc R . . H35B H 0.1453 0.4728 0.1257 0.021 Uiso 1 1 calc R . . C36 C 0.8019(2) 0.5859(2) 0.11924(19) 0.0232(5) Uani 1 1 d . . . H36 H 0.8198 0.5955 0.1759 0.028 Uiso 1 1 calc R . . C37 C 0.4908(2) 0.8735(2) 0.1836(2) 0.0311(6) Uani 1 1 d . . . H37 H 0.5332 0.8285 0.2249 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.65468(6) 0.60281(6) 0.13993(5) 0.03133(16) Uani 1 1 d . . . Cl2 Cl 0.86094(6) 0.67471(5) 0.02641(5) 0.02950(15) Uani 1 1 d . . . Cl3 Cl 0.86053(6) 0.46594(6) 0.09489(5) 0.03426(17) Uani 1 1 d . . . Cl4 Cl 0.47023(7) 0.99443(6) 0.21061(6) 0.03944(18) Uani 1 1 d . . . Cl5 Cl 0.36135(7) 0.83127(8) 0.20294(7) 0.0524(2) Uani 1 1 d . . . Cl6 Cl 0.57154(7) 0.87064(7) 0.06846(6) 0.0444(2) Uani 1 1 d . . . C38A C 0.2502(5) 0.9028(4) 0.9795(4) 0.0657(16) Uani 0.805(6) 1 d PDU A 1 H38A H 0.2335 0.8357 0.9846 0.098 Uiso 0.805(6) 1 calc PR A 1 H38B H 0.3055 0.9013 1.0132 0.098 Uiso 0.805(6) 1 calc PR A 1 H38C H 0.2806 0.9291 0.9143 0.098 Uiso 0.805(6) 1 calc PR A 1 C39A C 0.1465(4) 0.9664(4) 1.0193(3) 0.0582(15) Uani 0.805(6) 1 d PDU A 1 H39A H 0.1232 0.9459 1.0870 0.070 Uiso 0.805(6) 1 calc PR A 1 H39B H 0.1624 1.0355 1.0076 0.070 Uiso 0.805(6) 1 calc PR A 1 C40A C 0.0529(4) 0.9633(3) 0.9819(3) 0.0566(15) Uani 0.805(6) 1 d PDU . 1 H40A H 0.0327 0.8954 0.9981 0.068 Uiso 0.805(6) 1 calc PR A 1 H40B H 0.0781 0.9784 0.9136 0.068 Uiso 0.805(6) 1 calc PR A 1 C38B C 0.1691(13) 0.8742(19) 0.9670(18) 0.098(10) Uani 0.195(6) 1 d PDU A 2 H38D H 0.1749 0.9451 0.9531 0.147 Uiso 0.195(6) 1 calc PR A 2 H38E H 0.2161 0.8418 0.9144 0.147 Uiso 0.195(6) 1 calc PR A 2 H38F H 0.1946 0.8454 1.0220 0.147 Uiso 0.195(6) 1 calc PR A 2 C39B C 0.0485(14) 0.8595(7) 0.9845(11) 0.063(6) Uani 0.195(6) 1 d PDU A 2 H39C H 0.0223 0.8193 1.0457 0.075 Uiso 0.195(6) 1 calc PR A 2 H39D H 0.0410 0.8249 0.9366 0.075 Uiso 0.195(6) 1 calc PR A 2 C40B C -0.0216(15) 0.9639(9) 0.9813(17) 0.083(8) Uani 0.195(6) 1 d PDU . 2 H40C H -0.0214 0.9903 0.9165 0.100 Uiso 0.195(6) 1 calc PR A 2 H40D H -0.1003 0.9580 1.0174 0.100 Uiso 0.195(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00945(8) 0.01250(9) 0.01271(9) -0.00126(7) -0.00327(6) -0.00169(6) P1 0.0115(3) 0.0145(3) 0.0133(3) -0.0020(2) -0.0037(2) -0.0028(2) S1 0.0134(3) 0.0171(3) 0.0159(3) -0.0043(2) -0.0050(2) 0.0010(2) S2 0.0128(3) 0.0170(3) 0.0169(3) -0.0029(2) -0.0013(2) -0.0001(2) O1 0.0154(8) 0.0271(10) 0.0228(10) -0.0061(8) -0.0046(7) 0.0022(7) B1 0.0141(12) 0.0121(12) 0.0146(13) -0.0038(10) -0.0040(10) -0.0020(9) N1 0.0127(9) 0.0106(9) 0.0156(10) -0.0023(8) -0.0029(7) -0.0013(7) N2 0.0103(9) 0.0169(10) 0.0149(10) -0.0022(8) -0.0047(7) -0.0024(7) N3 0.0127(9) 0.0139(10) 0.0161(10) -0.0018(8) -0.0064(8) -0.0024(7) N4 0.0132(9) 0.0163(10) 0.0205(11) -0.0027(8) -0.0080(8) -0.0017(7) N5 0.0103(9) 0.0123(10) 0.0175(10) -0.0020(8) -0.0033(7) -0.0016(7) N6 0.0110(9) 0.0142(10) 0.0128(10) -0.0023(8) -0.0013(7) -0.0047(7) N7 0.0135(9) 0.0172(10) 0.0133(10) -0.0019(8) -0.0021(7) -0.0060(7) N8 0.0134(9) 0.0123(10) 0.0158(10) -0.0029(8) -0.0052(7) -0.0019(7) C1 0.0170(11) 0.0181(12) 0.0134(11) -0.0005(9) -0.0064(9) -0.0044(9) C3 0.0127(10) 0.0128(11) 0.0215(13) -0.0017(10) -0.0046(9) -0.0018(8) C4 0.0155(11) 0.0134(12) 0.0186(12) -0.0008(10) 0.0011(9) -0.0025(9) C5 0.0168(11) 0.0122(11) 0.0146(12) -0.0017(9) -0.0015(9) -0.0007(9) C6 0.0192(12) 0.0237(14) 0.0263(14) 0.0016(11) -0.0083(10) -0.0109(10) C7 0.0308(14) 0.0279(15) 0.0168(13) -0.0003(11) -0.0051(11) -0.0119(11) C8 0.0106(10) 0.0105(11) 0.0160(11) -0.0003(9) -0.0016(8) -0.0038(8) C9 0.0142(11) 0.0131(11) 0.0214(13) -0.0019(10) -0.0043(9) -0.0044(9) C10 0.0132(11) 0.0237(14) 0.0295(14) -0.0054(11) -0.0090(10) 0.0016(9) C11 0.0150(11) 0.0118(11) 0.0209(13) -0.0042(10) -0.0030(9) 0.0010(9) C12 0.0243(13) 0.0190(13) 0.0233(14) -0.0020(11) 0.0023(10) -0.0001(10) C13 0.0121(10) 0.0134(11) 0.0140(11) -0.0029(9) -0.0063(8) -0.0021(8) C14 0.0127(10) 0.0170(12) 0.0149(11) -0.0041(9) -0.0049(9) -0.0041(9) C15 0.0194(12) 0.0198(13) 0.0202(13) 0.0002(10) -0.0053(10) -0.0090(10) C16 0.0161(11) 0.0138(12) 0.0273(14) -0.0009(10) -0.0059(10) -0.0015(9) C17 0.0218(12) 0.0158(13) 0.0313(15) -0.0085(11) -0.0018(11) -0.0033(10) C18 0.0164(11) 0.0154(12) 0.0153(12) -0.0039(9) -0.0056(9) -0.0022(9) C19 0.0174(11) 0.0158(12) 0.0206(13) -0.0058(10) -0.0057(9) -0.0017(9) C20 0.0190(12) 0.0205(13) 0.0227(13) -0.0044(10) -0.0054(10) -0.0068(10) C21 0.0297(14) 0.0161(13) 0.0348(16) -0.0033(11) -0.0127(12) -0.0083(10) C22 0.0304(14) 0.0184(14) 0.0464(19) -0.0149(13) -0.0180(13) 0.0030(11) C23 0.0226(13) 0.0180(13) 0.0375(16) -0.0092(12) -0.0150(11) 0.0019(10) C24 0.0150(11) 0.0191(12) 0.0130(11) -0.0027(9) -0.0028(9) -0.0005(9) C25 0.0175(12) 0.0324(15) 0.0150(12) -0.0051(11) -0.0024(9) 0.0014(10) C26 0.0202(13) 0.0365(16) 0.0183(13) -0.0047(12) -0.0007(10) 0.0012(11) C27 0.0185(12) 0.0309(15) 0.0251(14) 0.0007(12) 0.0017(10) -0.0028(11) C28 0.0150(12) 0.0274(14) 0.0270(14) -0.0018(11) -0.0027(10) -0.0058(10) C29 0.0170(11) 0.0245(14) 0.0174(12) -0.0019(10) -0.0014(9) -0.0079(10) C30 0.0137(10) 0.0133(11) 0.0163(12) -0.0023(9) -0.0047(9) -0.0023(8) C31 0.0210(12) 0.0205(13) 0.0206(13) -0.0045(10) -0.0088(10) -0.0047(10) C32 0.0246(13) 0.0182(13) 0.0222(13) -0.0056(10) -0.0059(10) -0.0040(10) C33 0.0246(13) 0.0147(12) 0.0232(14) -0.0026(10) -0.0031(10) -0.0013(10) C34 0.0196(12) 0.0191(13) 0.0178(12) 0.0009(10) -0.0050(10) -0.0007(9) C35 0.0211(12) 0.0164(12) 0.0162(12) -0.0018(10) -0.0057(9) -0.0039(9) C36 0.0228(13) 0.0268(14) 0.0199(13) -0.0041(11) -0.0056(10) -0.0030(10) C37 0.0310(15) 0.0274(15) 0.0394(18) -0.0085(13) -0.0165(13) 0.0003(12) Cl1 0.0217(3) 0.0358(4) 0.0323(4) -0.0023(3) -0.0039(3) -0.0026(3) Cl2 0.0325(3) 0.0336(4) 0.0217(3) -0.0012(3) -0.0041(3) -0.0113(3) Cl3 0.0313(4) 0.0285(4) 0.0387(4) -0.0080(3) -0.0045(3) 0.0013(3) Cl4 0.0460(4) 0.0265(4) 0.0456(5) -0.0103(3) -0.0153(4) 0.0053(3) Cl5 0.0414(5) 0.0650(6) 0.0623(6) -0.0133(5) -0.0223(4) -0.0178(4) Cl6 0.0500(5) 0.0462(5) 0.0397(5) -0.0160(4) -0.0142(4) -0.0004(4) C38A 0.076(4) 0.081(4) 0.045(3) -0.007(3) -0.021(3) -0.020(3) C39A 0.107(4) 0.041(3) 0.032(2) -0.005(2) -0.030(3) -0.004(3) C40A 0.111(4) 0.033(3) 0.040(3) 0.007(2) -0.032(3) -0.038(3) C38B 0.064(10) 0.10(2) 0.068(16) 0.043(15) 0.018(12) 0.023(10) C39B 0.137(13) 0.042(9) 0.046(10) 0.043(7) -0.074(10) -0.073(9) C40B 0.061(12) 0.113(16) 0.063(14) 0.025(14) -0.019(12) -0.016(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 C1 1.821(2) . ? Rh1 N2 2.104(2) . ? Rh1 P1 2.2808(9) . ? Rh1 S1 2.4013(10) . ? P1 C18 1.850(2) . ? P1 C24 1.853(2) . ? P1 C30 1.855(2) . ? S1 C8 1.718(2) . ? S2 C13 1.683(2) . ? O1 C1 1.146(3) . ? B1 N1 1.539(3) . ? B1 N6 1.549(3) . ? B1 N3 1.560(3) . ? B1 H1 1.0000 . ? N1 C5 1.355(3) . ? N1 N2 1.368(3) . ? N2 C3 1.340(3) . ? N3 C8 1.334(3) . ? N3 N4 1.397(3) . ? N4 C9 1.301(3) . ? N5 C8 1.367(3) . ? N5 C9 1.373(3) . ? N5 C11 1.471(3) . ? N6 C13 1.346(3) . ? N6 N7 1.394(3) . ? N7 C14 1.300(3) . ? N8 C14 1.371(3) . ? N8 C13 1.374(3) . ? N8 C16 1.463(3) . ? C3 C4 1.389(3) . ? C3 C6 1.498(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 C7 1.494(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.488(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.520(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.491(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.511(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.534(3) . ? C18 C23 1.536(3) . ? C18 H18 1.0000 . ? C19 C20 1.529(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.528(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.518(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.530(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.536(3) . ? C24 C25 1.537(3) . ? C24 H24 1.0000 . ? C25 C26 1.529(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.518(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.526(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.522(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.534(3) . ? C30 C35 1.540(3) . ? C30 H30 1.0000 . ? C31 C32 1.526(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.533(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.526(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.526(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 Cl3 1.759(3) . ? C36 Cl1 1.762(3) . ? C36 Cl2 1.768(3) . ? C36 H36 1.0000 . ? C37 Cl6 1.757(3) . ? C37 Cl5 1.760(3) . ? C37 Cl4 1.767(3) . ? C37 H37 1.0000 . ? C38A C39A 1.470(6) . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A C40A 1.468(6) . ? C39A H39A 0.9900 . ? C39A H39B 0.9900 . ? C40A C40A 1.549(8) 2_577 ? C40A H40A 0.9900 . ? C40A H40B 0.9900 . ? C38B C39B 1.507(10) . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B C40B 1.554(10) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40B C40B 1.502(10) 2_577 ? C40B H40C 0.9900 . ? C40B H40D 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 N2 87.53(10) . . ? C1 Rh1 P1 88.54(8) . . ? N2 Rh1 P1 168.98(5) . . ? C1 Rh1 S1 177.56(8) . . ? N2 Rh1 S1 90.11(6) . . ? P1 Rh1 S1 93.67(4) . . ? C18 P1 C24 102.72(11) . . ? C18 P1 C30 103.25(11) . . ? C24 P1 C30 110.62(11) . . ? C18 P1 Rh1 109.68(8) . . ? C24 P1 Rh1 114.25(8) . . ? C30 P1 Rh1 115.00(8) . . ? C8 S1 Rh1 112.91(8) . . ? N1 B1 N6 112.78(19) . . ? N1 B1 N3 110.81(19) . . ? N6 B1 N3 108.98(19) . . ? N1 B1 H1 108.0 . . ? N6 B1 H1 108.0 . . ? N3 B1 H1 108.0 . . ? C5 N1 N2 109.58(19) . . ? C5 N1 B1 127.9(2) . . ? N2 N1 B1 122.48(19) . . ? C3 N2 N1 106.79(19) . . ? C3 N2 Rh1 126.85(16) . . ? N1 N2 Rh1 125.89(15) . . ? C8 N3 N4 110.35(18) . . ? C8 N3 B1 133.28(19) . . ? N4 N3 B1 116.19(18) . . ? C9 N4 N3 105.17(19) . . ? C8 N5 C9 106.91(19) . . ? C8 N5 C11 126.23(19) . . ? C9 N5 C11 126.86(19) . . ? C13 N6 N7 110.89(19) . . ? C13 N6 B1 125.12(19) . . ? N7 N6 B1 121.66(18) . . ? C14 N7 N6 105.14(19) . . ? C14 N8 C13 107.48(19) . . ? C14 N8 C16 127.4(2) . . ? C13 N8 C16 124.9(2) . . ? O1 C1 Rh1 174.9(2) . . ? N2 C3 C4 109.9(2) . . ? N2 C3 C6 121.7(2) . . ? C4 C3 C6 128.5(2) . . ? C5 C4 C3 106.0(2) . . ? C5 C4 H4 127.0 . . ? C3 C4 H4 127.0 . . ? N1 C5 C4 107.8(2) . . ? N1 C5 C7 124.0(2) . . ? C4 C5 C7 128.3(2) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N5 106.39(19) . . ? N3 C8 S1 132.37(17) . . ? N5 C8 S1 121.20(18) . . ? N4 C9 N5 111.1(2) . . ? N4 C9 C10 124.6(2) . . ? N5 C9 C10 124.2(2) . . ? 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 . . ? N5 C11 C12 111.7(2) . . ? N5 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N5 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 N8 105.24(19) . . ? N6 C13 S2 128.13(18) . . ? N8 C13 S2 126.63(18) . . ? N7 C14 N8 111.2(2) . . ? N7 C14 C15 124.7(2) . . ? N8 C14 C15 124.1(2) . . ? 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 . . ? N8 C16 C17 112.1(2) . . ? N8 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N8 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 109.9(2) . . ? C19 C18 P1 113.81(17) . . ? C23 C18 P1 109.89(16) . . ? C19 C18 H18 107.7 . . ? C23 C18 H18 107.7 . . ? P1 C18 H18 107.7 . . ? C20 C19 C18 110.5(2) . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 111.3(2) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 110.8(2) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 111.3(2) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C18 111.9(2) . . ? C22 C23 H23A 109.2 . . ? C18 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C18 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C29 C24 C25 110.7(2) . . ? C29 C24 P1 112.39(17) . . ? C25 C24 P1 119.01(16) . . ? C29 C24 H24 104.4 . . ? C25 C24 H24 104.4 . . ? P1 C24 H24 104.4 . . ? C26 C25 C24 110.4(2) . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 112.0(2) . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 110.8(2) . . ? 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 . . ? C29 C28 C27 110.9(2) . . ? C29 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C24 109.8(2) . . ? C28 C29 H29A 109.7 . . ? C24 C29 H29A 109.7 . . ? C28 C29 H29B 109.7 . . ? C24 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C35 110.11(19) . . ? C31 C30 P1 113.46(16) . . ? C35 C30 P1 115.92(17) . . ? C31 C30 H30 105.4 . . ? C35 C30 H30 105.4 . . ? P1 C30 H30 105.4 . . ? C32 C31 C30 111.1(2) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C33 111.1(2) . . ? 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 110.6(2) . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 111.1(2) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C30 111.3(2) . . ? C34 C35 H35A 109.4 . . ? C30 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C30 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? Cl3 C36 Cl1 110.97(15) . . ? Cl3 C36 Cl2 110.10(15) . . ? Cl1 C36 Cl2 109.92(15) . . ? Cl3 C36 H36 108.6 . . ? Cl1 C36 H36 108.6 . . ? Cl2 C36 H36 108.6 . . ? Cl6 C37 Cl5 110.82(16) . . ? Cl6 C37 Cl4 110.05(18) . . ? Cl5 C37 Cl4 110.88(16) . . ? Cl6 C37 H37 108.3 . . ? Cl5 C37 H37 108.3 . . ? Cl4 C37 H37 108.3 . . ? C40A C39A C38A 113.8(4) . . ? C40A C39A H39A 108.8 . . ? C38A C39A H39A 108.8 . . ? C40A C39A H39B 108.8 . . ? C38A C39A H39B 108.8 . . ? H39A C39A H39B 107.7 . . ? C39A C40A C40A 113.5(5) . 2_577 ? C39A C40A H40A 108.9 . . ? C40A C40A H40A 108.9 2_577 . ? C39A C40A H40B 108.9 . . ? C40A C40A H40B 108.9 2_577 . ? H40A C40A H40B 107.7 . . ? C39B C38B H38D 109.5 . . ? C39B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C39B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C38B C39B C40B 106.8(10) . . ? C38B C39B H39C 110.4 . . ? C40B C39B H39C 110.4 . . ? C38B C39B H39D 110.4 . . ? C40B C39B H39D 110.4 . . ? H39C C39B H39D 108.6 . . ? C40B C40B C39B 113.5(12) 2_577 . ? C40B C40B H40C 108.9 2_577 . ? C39B C40B H40C 108.9 . . ? C40B C40B H40D 108.9 2_577 . ? C39B C40B H40D 108.9 . . ? H40C C40B H40D 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 C1 Rh1 P1 C18 -83.42(11) . . . . ? N2 Rh1 P1 C18 -14.3(3) . . . . ? S1 Rh1 P1 C18 95.55(8) . . . . ? C1 Rh1 P1 C24 161.90(12) . . . . ? N2 Rh1 P1 C24 -129.0(3) . . . . ? S1 Rh1 P1 C24 -19.13(9) . . . . ? C1 Rh1 P1 C30 32.39(11) . . . . ? N2 Rh1 P1 C30 101.5(3) . . . . ? S1 Rh1 P1 C30 -148.64(8) . . . . ? N2 Rh1 S1 C8 -45.05(10) . . . . ? P1 Rh1 S1 C8 145.31(9) . . . . ? N6 B1 N1 C5 -131.3(2) . . . . ? N3 B1 N1 C5 106.2(3) . . . . ? N6 B1 N1 N2 49.9(3) . . . . ? N3 B1 N1 N2 -72.5(3) . . . . ? C5 N1 N2 C3 -0.5(2) . . . . ? B1 N1 N2 C3 178.4(2) . . . . ? C5 N1 N2 Rh1 171.95(15) . . . . ? B1 N1 N2 Rh1 -9.1(3) . . . . ? C1 Rh1 N2 C3 60.7(2) . . . . ? P1 Rh1 N2 C3 -8.5(4) . . . . ? S1 Rh1 N2 C3 -118.67(19) . . . . ? C1 Rh1 N2 N1 -110.28(19) . . . . ? P1 Rh1 N2 N1 -179.50(19) . . . . ? S1 Rh1 N2 N1 70.33(17) . . . . ? N1 B1 N3 C8 54.3(3) . . . . ? N6 B1 N3 C8 -70.4(3) . . . . ? N1 B1 N3 N4 -120.3(2) . . . . ? N6 B1 N3 N4 115.1(2) . . . . ? C8 N3 N4 C9 -0.8(3) . . . . ? B1 N3 N4 C9 175.01(19) . . . . ? N1 B1 N6 C13 64.1(3) . . . . ? N3 B1 N6 C13 -172.45(19) . . . . ? N1 B1 N6 N7 -134.9(2) . . . . ? N3 B1 N6 N7 -11.4(3) . . . . ? C13 N6 N7 C14 -1.1(2) . . . . ? B1 N6 N7 C14 -164.6(2) . . . . ? N1 N2 C3 C4 0.5(3) . . . . ? Rh1 N2 C3 C4 -171.93(16) . . . . ? N1 N2 C3 C6 179.1(2) . . . . ? Rh1 N2 C3 C6 6.7(3) . . . . ? N2 C3 C4 C5 -0.2(3) . . . . ? C6 C3 C4 C5 -178.7(2) . . . . ? N2 N1 C5 C4 0.4(3) . . . . ? B1 N1 C5 C4 -178.4(2) . . . . ? N2 N1 C5 C7 179.9(2) . . . . ? B1 N1 C5 C7 1.1(4) . . . . ? C3 C4 C5 N1 -0.1(3) . . . . ? C3 C4 C5 C7 -179.6(2) . . . . ? N4 N3 C8 N5 1.6(2) . . . . ? B1 N3 C8 N5 -173.2(2) . . . . ? N4 N3 C8 S1 -175.87(18) . . . . ? B1 N3 C8 S1 9.3(4) . . . . ? C9 N5 C8 N3 -1.7(2) . . . . ? C11 N5 C8 N3 178.5(2) . . . . ? C9 N5 C8 S1 176.05(17) . . . . ? C11 N5 C8 S1 -3.7(3) . . . . ? Rh1 S1 C8 N3 -3.4(3) . . . . ? Rh1 S1 C8 N5 179.45(15) . . . . ? N3 N4 C9 N5 -0.4(3) . . . . ? N3 N4 C9 C10 178.5(2) . . . . ? C8 N5 C9 N4 1.3(3) . . . . ? C11 N5 C9 N4 -178.9(2) . . . . ? C8 N5 C9 C10 -177.5(2) . . . . ? C11 N5 C9 C10 2.2(4) . . . . ? C8 N5 C11 C12 90.2(3) . . . . ? C9 N5 C11 C12 -89.5(3) . . . . ? N7 N6 C13 N8 1.5(2) . . . . ? B1 N6 C13 N8 164.35(19) . . . . ? N7 N6 C13 S2 -178.74(16) . . . . ? B1 N6 C13 S2 -15.9(3) . . . . ? C14 N8 C13 N6 -1.4(2) . . . . ? C16 N8 C13 N6 -176.4(2) . . . . ? C14 N8 C13 S2 178.91(17) . . . . ? C16 N8 C13 S2 3.8(3) . . . . ? N6 N7 C14 N8 0.2(2) . . . . ? N6 N7 C14 C15 -179.8(2) . . . . ? C13 N8 C14 N7 0.7(3) . . . . ? C16 N8 C14 N7 175.6(2) . . . . ? C13 N8 C14 C15 -179.3(2) . . . . ? C16 N8 C14 C15 -4.4(4) . . . . ? C14 N8 C16 C17 -94.6(3) . . . . ? C13 N8 C16 C17 79.5(3) . . . . ? C24 P1 C18 C19 -171.21(18) . . . . ? C30 P1 C18 C19 -56.1(2) . . . . ? Rh1 P1 C18 C19 66.93(18) . . . . ? C24 P1 C18 C23 65.0(2) . . . . ? C30 P1 C18 C23 -179.89(18) . . . . ? Rh1 P1 C18 C23 -56.84(19) . . . . ? C23 C18 C19 C20 -56.6(3) . . . . ? P1 C18 C19 C20 179.70(17) . . . . ? C18 C19 C20 C21 57.7(3) . . . . ? C19 C20 C21 C22 -56.6(3) . . . . ? C20 C21 C22 C23 55.0(3) . . . . ? C21 C22 C23 C18 -55.3(3) . . . . ? C19 C18 C23 C22 55.7(3) . . . . ? P1 C18 C23 C22 -178.3(2) . . . . ? C18 P1 C24 C29 175.27(17) . . . . ? C30 P1 C24 C29 65.6(2) . . . . ? Rh1 P1 C24 C29 -66.02(19) . . . . ? C18 P1 C24 C25 43.6(2) . . . . ? C30 P1 C24 C25 -66.1(2) . . . . ? Rh1 P1 C24 C25 162.27(17) . . . . ? C29 C24 C25 C26 56.1(3) . . . . ? P1 C24 C25 C26 -171.49(19) . . . . ? C24 C25 C26 C27 -54.8(3) . . . . ? C25 C26 C27 C28 55.3(3) . . . . ? C26 C27 C28 C29 -57.2(3) . . . . ? C27 C28 C29 C24 58.5(3) . . . . ? C25 C24 C29 C28 -58.1(3) . . . . ? P1 C24 C29 C28 166.13(18) . . . . ? C18 P1 C30 C31 173.96(17) . . . . ? C24 P1 C30 C31 -76.75(19) . . . . ? Rh1 P1 C30 C31 54.52(19) . . . . ? C18 P1 C30 C35 -57.15(19) . . . . ? C24 P1 C30 C35 52.1(2) . . . . ? Rh1 P1 C30 C35 -176.60(14) . . . . ? C35 C30 C31 C32 56.1(3) . . . . ? P1 C30 C31 C32 -172.15(17) . . . . ? C30 C31 C32 C33 -56.8(3) . . . . ? C31 C32 C33 C34 56.5(3) . . . . ? C32 C33 C34 C35 -56.3(3) . . . . ? C33 C34 C35 C30 56.5(3) . . . . ? C31 C30 C35 C34 -55.9(3) . . . . ? P1 C30 C35 C34 173.56(16) . . . . ? C38A C39A C40A C40A -175.3(5) . . . 2_577 ? C38B C39B C40B C40B -35(3) . . . 2_577 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.905 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.089 data_18 _database_code_depnum_ccdc_archive 'CCDC 792571' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H42 B N11 O P Rh S2, 1.5(C H2 Cl2)' _chemical_formula_sum 'C23.50 H45 B Cl3 N11 O P Rh S2' _chemical_formula_weight 812.86 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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.888(2) _cell_length_b 12.172(2) _cell_length_c 13.906(3) _cell_angle_alpha 92.35(3) _cell_angle_beta 93.44(3) _cell_angle_gamma 99.11(3) _cell_volume 1814.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6077 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.34 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.837 _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 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20298 _diffrn_reflns_av_R_equivalents 0.1923 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8295 _reflns_number_gt 6261 _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 '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^)+(0.0326P)^2^+0.1448P] 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 8295 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.56937(3) 0.813386(19) 0.738305(16) 0.01306(8) Uani 1 1 d . . . P1 P 0.76385(9) 0.89862(7) 0.78265(5) 0.0146(2) Uani 1 1 d . . . S1 S 0.64564(10) 0.66500(6) 0.65408(6) 0.0182(2) Uani 1 1 d . . . S2 S 0.24711(11) 0.74375(8) 0.90852(6) 0.0254(2) Uani 1 1 d . . . O1 O 0.4687(3) 1.0025(2) 0.8281(2) 0.0354(7) Uani 1 1 d . . . N1 N 0.3087(3) 0.6670(2) 0.69083(16) 0.0112(6) Uani 1 1 d . . . N2 N 0.3865(3) 0.7623(2) 0.67260(17) 0.0135(6) Uani 1 1 d . . . N3 N 0.4377(3) 0.5108(2) 0.69347(17) 0.0156(7) Uani 1 1 d . . . N4 N 0.3952(3) 0.3973(2) 0.67358(18) 0.0185(7) Uani 1 1 d . . . N5 N 0.5694(3) 0.4475(2) 0.60388(17) 0.0148(6) Uani 1 1 d . . . N6 N 0.4231(3) 0.6259(2) 0.84753(17) 0.0146(6) Uani 1 1 d . . . N7 N 0.5322(3) 0.5897(2) 0.88221(18) 0.0141(6) Uani 1 1 d . . . N8 N 0.4625(3) 0.6948(2) 0.99346(17) 0.0167(7) Uani 1 1 d . . . N9 N 0.8221(3) 0.9869(2) 0.69831(18) 0.0159(7) Uani 1 1 d . . . N10 N 0.7744(3) 0.9903(2) 0.87831(18) 0.0178(7) Uani 1 1 d . . . N11 N 0.8754(3) 0.8192(2) 0.78990(18) 0.0187(7) Uani 1 1 d . . . B1 B 0.3516(4) 0.5760(3) 0.7512(2) 0.0157(9) Uani 1 1 d . . . H1 H 0.2765 0.5227 0.7667 0.019 Uiso 1 1 calc R . . C1 C 0.5116(4) 0.9315(3) 0.7952(2) 0.0214(9) Uani 1 1 d . . . C3 C 0.1942(4) 0.6686(3) 0.6474(2) 0.0174(8) Uani 1 1 d . . . C4 C 0.2008(4) 0.7666(3) 0.6002(2) 0.0190(8) Uani 1 1 d . . . H4 H 0.1354 0.7909 0.5627 0.023 Uiso 1 1 calc R . . C5 C 0.3212(4) 0.8226(3) 0.6183(2) 0.0153(8) Uani 1 1 d . . . C6 C 0.0870(4) 0.5777(3) 0.6533(2) 0.0235(9) Uani 1 1 d . . . H6A H 0.1066 0.5085 0.6241 0.035 Uiso 1 1 calc R . . H6B H 0.0131 0.5975 0.6187 0.035 Uiso 1 1 calc R . . H6C H 0.0704 0.5673 0.7211 0.035 Uiso 1 1 calc R . . C7 C 0.3765(4) 0.9352(3) 0.5863(2) 0.0243(9) Uani 1 1 d . . . H7A H 0.3638 0.9928 0.6344 0.036 Uiso 1 1 calc R . . H7B H 0.3357 0.9485 0.5241 0.036 Uiso 1 1 calc R . . H7C H 0.4660 0.9378 0.5797 0.036 Uiso 1 1 calc R . . C8 C 0.5434(4) 0.5418(2) 0.6519(2) 0.0143(8) Uani 1 1 d . . . C9 C 0.4748(4) 0.3630(3) 0.6200(2) 0.0176(8) Uani 1 1 d . . . C10 C 0.4698(4) 0.2455(3) 0.5824(2) 0.0208(8) Uani 1 1 d . . . H10A H 0.3928 0.2001 0.6004 0.031 Uiso 1 1 calc R . . H10B H 0.5419 0.2158 0.6101 0.031 Uiso 1 1 calc R . . H10C H 0.4713 0.2436 0.5119 0.031 Uiso 1 1 calc R . . C11 C 0.6793(4) 0.4397(3) 0.5506(2) 0.0194(8) Uani 1 1 d . . . H11A H 0.7058 0.5115 0.5210 0.023 Uiso 1 1 calc R . . H11B H 0.6576 0.3813 0.4980 0.023 Uiso 1 1 calc R . . C12 C 0.7866(4) 0.4123(3) 0.6146(2) 0.0261(9) Uani 1 1 d . . . H12A H 0.8082 0.4697 0.6671 0.039 Uiso 1 1 calc R . . H12B H 0.8590 0.4099 0.5764 0.039 Uiso 1 1 calc R . . H12C H 0.7622 0.3397 0.6418 0.039 Uiso 1 1 calc R . . C13 C 0.3779(4) 0.6878(3) 0.9153(2) 0.0164(8) Uani 1 1 d . . . C14 C 0.5520(4) 0.6337(3) 0.9704(2) 0.0172(8) Uani 1 1 d . . . C15 C 0.6616(4) 0.6207(3) 1.0370(2) 0.0235(9) Uani 1 1 d . . . H15A H 0.7030 0.5613 1.0108 0.035 Uiso 1 1 calc R . . H15B H 0.6331 0.6016 1.1006 0.035 Uiso 1 1 calc R . . H15C H 0.7205 0.6909 1.0430 0.035 Uiso 1 1 calc R . . C16 C 0.4528(4) 0.7536(3) 1.0860(2) 0.0241(9) Uani 1 1 d . . . H16A H 0.4181 0.8226 1.0742 0.029 Uiso 1 1 calc R . . H16B H 0.5372 0.7753 1.1183 0.029 Uiso 1 1 calc R . . C17 C 0.3705(4) 0.6828(3) 1.1525(2) 0.0307(10) Uani 1 1 d . . . H17A H 0.2855 0.6649 1.1225 0.046 Uiso 1 1 calc R . . H17B H 0.3694 0.7242 1.2142 0.046 Uiso 1 1 calc R . . H17C H 0.4036 0.6137 1.1634 0.046 Uiso 1 1 calc R . . C18 C 0.8426(4) 0.9321(3) 0.6056(2) 0.0211(8) Uani 1 1 d . . . H18A H 0.7621 0.9050 0.5704 0.032 Uiso 1 1 calc R . . H18B H 0.8866 0.8691 0.6175 0.032 Uiso 1 1 calc R . . H18C H 0.8929 0.9856 0.5672 0.032 Uiso 1 1 calc R . . C19 C 0.7576(4) 1.0816(3) 0.6830(2) 0.0252(9) Uani 1 1 d . . . H19A H 0.8045 1.1329 0.6408 0.038 Uiso 1 1 calc R . . H19B H 0.7509 1.1204 0.7452 0.038 Uiso 1 1 calc R . . H19C H 0.6739 1.0551 0.6528 0.038 Uiso 1 1 calc R . . C20 C 0.8851(4) 1.0737(3) 0.9014(2) 0.0245(9) Uani 1 1 d . . . H20A H 0.8610 1.1403 0.9321 0.037 Uiso 1 1 calc R . . H20B H 0.9255 1.0936 0.8420 0.037 Uiso 1 1 calc R . . H20C H 0.9432 1.0434 0.9456 0.037 Uiso 1 1 calc R . . C21 C 0.7174(4) 0.9494(3) 0.9664(2) 0.0235(9) Uani 1 1 d . . . H21A H 0.7781 0.9165 1.0061 0.035 Uiso 1 1 calc R . . H21B H 0.6441 0.8929 0.9485 0.035 Uiso 1 1 calc R . . H21C H 0.6921 1.0116 1.0030 0.035 Uiso 1 1 calc R . . C22 C 1.0074(4) 0.8665(3) 0.7944(2) 0.0242(9) Uani 1 1 d . . . H22A H 1.0378 0.8843 0.8619 0.036 Uiso 1 1 calc R . . H22B H 1.0188 0.9345 0.7585 0.036 Uiso 1 1 calc R . . H22C H 1.0543 0.8123 0.7660 0.036 Uiso 1 1 calc R . . C23 C 0.8539(4) 0.7181(3) 0.8442(2) 0.0218(8) Uani 1 1 d . . . H23A H 0.8967 0.6612 0.8152 0.033 Uiso 1 1 calc R . . H23B H 0.7642 0.6902 0.8423 0.033 Uiso 1 1 calc R . . H23C H 0.8863 0.7353 0.9113 0.033 Uiso 1 1 calc R . . C24 C 0.8705(4) 0.7455(3) 0.2832(3) 0.0333(10) Uani 1 1 d . . . H24A H 0.8134 0.6739 0.2702 0.040 Uiso 1 1 calc R . . H24B H 0.9464 0.7416 0.2482 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.91157(14) 0.76432(11) 0.40758(8) 0.0532(4) Uani 1 1 d . . . Cl2 Cl 0.79706(13) 0.85502(9) 0.23965(8) 0.0437(3) Uani 1 1 d . . . C25 C 0.9396(14) 0.4867(11) 0.9844(9) 0.074(4) Uani 0.50 1 d P . . H25A H 0.8906 0.4301 1.0221 0.089 Uiso 0.50 1 calc PR . . H25B H 0.8965 0.5517 0.9750 0.089 Uiso 0.50 1 calc PR . . Cl3 Cl 1.0226(6) 0.5508(4) 1.0893(3) 0.0722(15) Uani 0.50 1 d P . . Cl4 Cl 1.0196(5) 0.4116(4) 0.9119(3) 0.0585(11) Uani 0.50 1 d P . . 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 0.01646(19) 0.00980(12) 0.01212(12) -0.00054(8) -0.00088(9) 0.00069(10) P1 0.0184(6) 0.0127(4) 0.0118(4) 0.0003(3) 0.0005(3) 0.0001(3) S1 0.0212(6) 0.0124(4) 0.0203(4) -0.0017(3) 0.0070(3) -0.0009(3) S2 0.0311(7) 0.0329(5) 0.0164(4) -0.0045(3) -0.0015(4) 0.0200(4) O1 0.028(2) 0.0260(14) 0.0503(17) -0.0159(12) -0.0035(13) 0.0044(13) N1 0.0094(18) 0.0141(12) 0.0104(11) -0.0005(9) -0.0006(10) 0.0035(11) N2 0.0149(19) 0.0118(12) 0.0126(12) 0.0013(9) -0.0026(11) -0.0009(11) N3 0.025(2) 0.0102(12) 0.0100(12) -0.0001(9) 0.0023(11) -0.0020(12) N4 0.030(2) 0.0088(12) 0.0141(13) -0.0001(10) 0.0005(12) -0.0032(12) N5 0.019(2) 0.0133(13) 0.0120(12) -0.0023(9) 0.0024(11) 0.0025(12) N6 0.019(2) 0.0127(12) 0.0127(12) 0.0017(10) -0.0013(11) 0.0046(12) N7 0.0091(18) 0.0164(13) 0.0174(13) 0.0045(10) 0.0007(11) 0.0026(11) N8 0.023(2) 0.0147(13) 0.0127(12) -0.0008(10) -0.0014(11) 0.0041(12) N9 0.018(2) 0.0153(13) 0.0146(13) 0.0031(10) 0.0007(11) 0.0029(12) N10 0.021(2) 0.0178(13) 0.0132(12) -0.0022(10) 0.0009(11) -0.0013(12) N11 0.020(2) 0.0157(13) 0.0197(13) 0.0037(10) -0.0008(12) 0.0001(12) B1 0.021(3) 0.0122(16) 0.0132(16) -0.0006(13) 0.0046(15) 0.0003(16) C1 0.026(3) 0.0131(16) 0.0242(17) -0.0068(13) -0.0003(15) 0.0017(15) C3 0.017(2) 0.0205(16) 0.0133(14) -0.0032(12) 0.0014(13) -0.0014(14) C4 0.024(3) 0.0201(16) 0.0127(14) 0.0002(12) -0.0023(14) 0.0052(15) C5 0.019(2) 0.0178(15) 0.0101(14) -0.0001(11) 0.0005(13) 0.0070(14) C6 0.012(2) 0.0284(19) 0.0290(18) 0.0025(14) -0.0034(15) 0.0006(16) C7 0.036(3) 0.0172(16) 0.0192(16) 0.0045(13) -0.0007(16) 0.0017(16) C8 0.020(2) 0.0140(15) 0.0098(13) 0.0009(11) -0.0012(13) 0.0052(14) C9 0.026(3) 0.0148(15) 0.0098(14) 0.0001(11) -0.0015(13) -0.0017(15) C10 0.027(3) 0.0131(15) 0.0208(16) -0.0025(12) -0.0012(15) 0.0012(15) C11 0.025(3) 0.0161(16) 0.0170(15) -0.0021(12) 0.0054(14) 0.0011(15) C12 0.025(3) 0.0247(18) 0.0274(18) -0.0028(14) 0.0029(16) 0.0000(17) C13 0.020(2) 0.0148(15) 0.0143(14) 0.0004(11) 0.0009(13) 0.0027(14) C14 0.020(2) 0.0142(15) 0.0167(15) 0.0045(12) -0.0003(14) -0.0008(14) C15 0.025(3) 0.0233(18) 0.0209(16) 0.0068(13) -0.0026(15) -0.0010(16) C16 0.036(3) 0.0222(17) 0.0145(15) -0.0068(13) -0.0059(15) 0.0100(17) C17 0.042(3) 0.040(2) 0.0142(16) 0.0000(14) 0.0047(16) 0.018(2) C18 0.025(3) 0.0209(17) 0.0175(16) 0.0015(13) 0.0033(14) 0.0018(16) C19 0.035(3) 0.0181(17) 0.0246(17) 0.0051(13) 0.0066(16) 0.0069(17) C20 0.028(3) 0.0214(17) 0.0217(17) -0.0041(13) 0.0001(15) -0.0020(16) C21 0.030(3) 0.0233(17) 0.0174(16) 0.0020(13) 0.0023(15) 0.0040(16) C22 0.027(3) 0.0210(17) 0.0246(18) -0.0024(13) 0.0025(16) 0.0028(16) C23 0.015(2) 0.0247(18) 0.0291(18) 0.0097(14) -0.0019(15) 0.0131(16) C24 0.030(3) 0.033(2) 0.034(2) -0.0049(16) 0.0058(18) -0.0037(19) Cl1 0.0485(10) 0.0638(8) 0.0423(6) -0.0146(5) -0.0154(6) 0.0055(7) Cl2 0.0485(9) 0.0337(5) 0.0447(6) 0.0057(4) 0.0051(5) -0.0081(5) C25 0.081(13) 0.084(8) 0.068(8) -0.011(6) -0.012(7) 0.060(9) Cl3 0.093(5) 0.062(3) 0.0554(19) 0.0013(19) 0.021(3) -0.012(2) Cl4 0.042(3) 0.085(3) 0.0514(17) -0.0048(19) 0.0043(14) 0.023(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 1.828(4) . ? Rh1 N2 2.128(3) . ? Rh1 P1 2.2441(12) . ? Rh1 S1 2.3962(12) . ? P1 N11 1.669(3) . ? P1 N10 1.688(3) . ? P1 N9 1.706(3) . ? S1 C8 1.718(3) . ? S2 C13 1.673(4) . ? O1 C1 1.138(5) . ? N1 C3 1.355(5) . ? N1 N2 1.366(4) . ? N1 B1 1.531(4) . ? N2 C5 1.327(4) . ? N3 C8 1.326(5) . ? N3 N4 1.397(3) . ? N3 B1 1.558(5) . ? N4 C9 1.284(5) . ? N5 C9 1.371(4) . ? N5 C8 1.382(4) . ? N5 C11 1.458(5) . ? N6 C13 1.346(4) . ? N6 N7 1.398(4) . ? N6 B1 1.558(4) . ? N7 C14 1.310(4) . ? N8 C14 1.361(5) . ? N8 C13 1.372(4) . ? N8 C16 1.465(4) . ? N9 C19 1.458(4) . ? N9 C18 1.473(4) . ? N10 C20 1.458(4) . ? N10 C21 1.475(5) . ? N11 C22 1.458(5) . ? N11 C23 1.464(4) . ? B1 H1 1.0000 . ? C3 C4 1.379(4) . ? C3 C6 1.484(5) . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C7 1.503(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.494(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.513(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.499(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? 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 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Cl1 1.757(4) . ? C24 Cl2 1.768(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 Cl3 1.226(14) 2_767 ? C25 C25 1.35(3) 2_767 ? C25 Cl4 1.702(14) . ? C25 Cl3 1.755(11) . ? C25 Cl4 1.847(12) 2_767 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Cl3 Cl4 0.698(5) 2_767 ? Cl3 C25 1.226(14) 2_767 ? Cl4 Cl3 0.698(5) 2_767 ? Cl4 C25 1.847(12) 2_767 ? 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 N2 87.65(14) . . ? C1 Rh1 P1 88.29(13) . . ? N2 Rh1 P1 166.56(7) . . ? C1 Rh1 S1 176.23(11) . . ? N2 Rh1 S1 91.57(8) . . ? P1 Rh1 S1 91.65(4) . . ? N11 P1 N10 111.96(15) . . ? N11 P1 N9 99.41(16) . . ? N10 P1 N9 99.35(13) . . ? N11 P1 Rh1 117.30(11) . . ? N10 P1 Rh1 114.48(13) . . ? N9 P1 Rh1 111.76(11) . . ? C8 S1 Rh1 112.05(13) . . ? C3 N1 N2 109.4(2) . . ? C3 N1 B1 128.1(3) . . ? N2 N1 B1 122.6(3) . . ? C5 N2 N1 107.5(3) . . ? C5 N2 Rh1 126.7(2) . . ? N1 N2 Rh1 125.19(18) . . ? C8 N3 N4 110.2(3) . . ? C8 N3 B1 133.1(3) . . ? N4 N3 B1 116.5(3) . . ? C9 N4 N3 105.7(3) . . ? C9 N5 C8 106.4(3) . . ? C9 N5 C11 127.4(3) . . ? C8 N5 C11 126.1(3) . . ? C13 N6 N7 111.5(2) . . ? C13 N6 B1 125.7(3) . . ? N7 N6 B1 121.5(3) . . ? C14 N7 N6 104.0(3) . . ? C14 N8 C13 107.7(3) . . ? C14 N8 C16 127.0(3) . . ? C13 N8 C16 125.2(3) . . ? C19 N9 C18 110.8(3) . . ? C19 N9 P1 115.5(3) . . ? C18 N9 P1 114.8(2) . . ? C20 N10 C21 111.5(2) . . ? C20 N10 P1 121.8(3) . . ? C21 N10 P1 117.1(2) . . ? C22 N11 C23 111.3(3) . . ? C22 N11 P1 122.1(2) . . ? C23 N11 P1 118.4(3) . . ? N1 B1 N6 111.4(2) . . ? N1 B1 N3 110.4(3) . . ? N6 B1 N3 109.1(3) . . ? N1 B1 H1 108.6 . . ? N6 B1 H1 108.6 . . ? N3 B1 H1 108.6 . . ? O1 C1 Rh1 175.8(3) . . ? N1 C3 C4 107.0(3) . . ? N1 C3 C6 123.4(3) . . ? C4 C3 C6 129.6(3) . . ? C3 C4 C5 106.6(3) . . ? C3 C4 H4 126.7 . . ? C5 C4 H4 126.7 . . ? N2 C5 C4 109.5(3) . . ? N2 C5 C7 122.2(3) . . ? C4 C5 C7 128.3(3) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N5 106.1(3) . . ? N3 C8 S1 133.2(3) . . ? N5 C8 S1 120.5(3) . . ? N4 C9 N5 111.5(3) . . ? N4 C9 C10 125.1(3) . . ? N5 C9 C10 123.4(4) . . ? 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 . . ? N5 C11 C12 112.2(3) . . ? N5 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N5 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 N8 104.9(3) . . ? N6 C13 S2 128.5(2) . . ? N8 C13 S2 126.6(3) . . ? N7 C14 N8 111.8(3) . . ? N7 C14 C15 124.1(4) . . ? N8 C14 C15 124.1(3) . . ? 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 . . ? N8 C16 C17 112.3(3) . . ? N8 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N8 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N9 C18 H18A 109.5 . . ? N9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N9 C19 H19A 109.5 . . ? N9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N10 C21 H21A 109.5 . . ? N10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N11 C22 H22A 109.5 . . ? N11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N11 C23 H23A 109.5 . . ? N11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl1 C24 Cl2 111.8(2) . . ? Cl1 C24 H24A 109.3 . . ? Cl2 C24 H24A 109.3 . . ? Cl1 C24 H24B 109.3 . . ? Cl2 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? Cl4 C25 Cl3 116.0(7) . . ? Cl4 C25 H25A 104.2 . . ? Cl3 C25 H25A 91.6 . . ? Cl4 C25 H25B 134.0 . . ? Cl3 C25 H25B 91.6 . . ? H25A C25 H25B 111.5 . . ? 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 P1 N11 158.25(15) . . . . ? N2 Rh1 P1 N11 -129.3(4) . . . . ? S1 Rh1 P1 N11 -25.52(12) . . . . ? C1 Rh1 P1 N10 24.04(15) . . . . ? N2 Rh1 P1 N10 96.5(4) . . . . ? S1 Rh1 P1 N10 -159.73(11) . . . . ? C1 Rh1 P1 N9 -87.91(16) . . . . ? N2 Rh1 P1 N9 -15.5(4) . . . . ? S1 Rh1 P1 N9 88.32(12) . . . . ? N2 Rh1 S1 C8 -42.17(13) . . . . ? P1 Rh1 S1 C8 150.88(11) . . . . ? C3 N1 N2 C5 0.0(4) . . . . ? B1 N1 N2 C5 179.6(3) . . . . ? C3 N1 N2 Rh1 171.4(2) . . . . ? B1 N1 N2 Rh1 -9.1(4) . . . . ? C1 Rh1 N2 C5 55.3(3) . . . . ? P1 Rh1 N2 C5 -17.2(6) . . . . ? S1 Rh1 N2 C5 -121.0(3) . . . . ? C1 Rh1 N2 N1 -114.4(3) . . . . ? P1 Rh1 N2 N1 173.1(2) . . . . ? S1 Rh1 N2 N1 69.3(2) . . . . ? C8 N3 N4 C9 -0.7(3) . . . . ? B1 N3 N4 C9 175.2(3) . . . . ? C13 N6 N7 C14 -1.6(4) . . . . ? B1 N6 N7 C14 -168.8(3) . . . . ? N11 P1 N9 C19 -171.0(2) . . . . ? N10 P1 N9 C19 -56.7(3) . . . . ? Rh1 P1 N9 C19 64.5(2) . . . . ? N11 P1 N9 C18 58.1(3) . . . . ? N10 P1 N9 C18 172.4(3) . . . . ? Rh1 P1 N9 C18 -66.4(3) . . . . ? N11 P1 N10 C20 59.9(3) . . . . ? N9 P1 N10 C20 -44.3(3) . . . . ? Rh1 P1 N10 C20 -163.5(2) . . . . ? N11 P1 N10 C21 -83.3(3) . . . . ? N9 P1 N10 C21 172.5(3) . . . . ? Rh1 P1 N10 C21 53.3(3) . . . . ? N10 P1 N11 C22 -60.1(3) . . . . ? N9 P1 N11 C22 44.1(3) . . . . ? Rh1 P1 N11 C22 164.6(2) . . . . ? N10 P1 N11 C23 85.6(3) . . . . ? N9 P1 N11 C23 -170.2(2) . . . . ? Rh1 P1 N11 C23 -49.7(3) . . . . ? C3 N1 B1 N6 -131.9(3) . . . . ? N2 N1 B1 N6 48.6(4) . . . . ? C3 N1 B1 N3 106.7(4) . . . . ? N2 N1 B1 N3 -72.8(3) . . . . ? C13 N6 B1 N1 57.5(4) . . . . ? N7 N6 B1 N1 -137.2(3) . . . . ? C13 N6 B1 N3 179.7(3) . . . . ? N7 N6 B1 N3 -15.0(4) . . . . ? C8 N3 B1 N1 56.9(5) . . . . ? N4 N3 B1 N1 -117.8(3) . . . . ? C8 N3 B1 N6 -65.8(4) . . . . ? N4 N3 B1 N6 119.5(3) . . . . ? N2 N1 C3 C4 0.5(4) . . . . ? B1 N1 C3 C4 -179.1(3) . . . . ? N2 N1 C3 C6 -179.5(3) . . . . ? B1 N1 C3 C6 0.9(5) . . . . ? N1 C3 C4 C5 -0.7(4) . . . . ? C6 C3 C4 C5 179.3(4) . . . . ? N1 N2 C5 C4 -0.5(4) . . . . ? Rh1 N2 C5 C4 -171.7(2) . . . . ? N1 N2 C5 C7 178.3(3) . . . . ? Rh1 N2 C5 C7 7.1(5) . . . . ? C3 C4 C5 N2 0.8(4) . . . . ? C3 C4 C5 C7 -177.9(3) . . . . ? N4 N3 C8 N5 0.4(3) . . . . ? B1 N3 C8 N5 -174.6(3) . . . . ? N4 N3 C8 S1 -175.6(2) . . . . ? B1 N3 C8 S1 9.4(5) . . . . ? C9 N5 C8 N3 0.1(3) . . . . ? C11 N5 C8 N3 -177.4(3) . . . . ? C9 N5 C8 S1 176.7(2) . . . . ? C11 N5 C8 S1 -0.8(4) . . . . ? Rh1 S1 C8 N3 -6.5(4) . . . . ? Rh1 S1 C8 N5 177.94(19) . . . . ? N3 N4 C9 N5 0.8(3) . . . . ? N3 N4 C9 C10 178.4(3) . . . . ? C8 N5 C9 N4 -0.5(3) . . . . ? C11 N5 C9 N4 176.9(3) . . . . ? C8 N5 C9 C10 -178.3(3) . . . . ? C11 N5 C9 C10 -0.8(5) . . . . ? C9 N5 C11 C12 -88.9(4) . . . . ? C8 N5 C11 C12 88.0(4) . . . . ? N7 N6 C13 N8 2.3(4) . . . . ? B1 N6 C13 N8 168.9(3) . . . . ? N7 N6 C13 S2 -177.0(2) . . . . ? B1 N6 C13 S2 -10.4(5) . . . . ? C14 N8 C13 N6 -2.1(4) . . . . ? C16 N8 C13 N6 -179.5(3) . . . . ? C14 N8 C13 S2 177.2(3) . . . . ? C16 N8 C13 S2 -0.1(5) . . . . ? N6 N7 C14 N8 0.2(4) . . . . ? N6 N7 C14 C15 -178.4(3) . . . . ? C13 N8 C14 N7 1.2(4) . . . . ? C16 N8 C14 N7 178.5(3) . . . . ? C13 N8 C14 C15 179.8(3) . . . . ? C16 N8 C14 C15 -2.9(5) . . . . ? C14 N8 C16 C17 -93.1(5) . . . . ? C13 N8 C16 C17 83.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.669 _refine_diff_density_min -2.185 _refine_diff_density_rms 0.159 data_19 _database_code_depnum_ccdc_archive 'CCDC 792572' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H39 B N8 O P Rh S2, C H2 Cl2' _chemical_formula_sum 'C35 H41 B Cl2 N8 O P Rh S2' _chemical_formula_weight 869.47 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' Cl Cl 0.1484 0.1585 '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' _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 10.5053(14) _cell_length_b 12.4117(18) _cell_length_c 16.077(3) _cell_angle_alpha 80.982(13) _cell_angle_beta 74.946(14) _cell_angle_gamma 76.619(9) _cell_volume 1958.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.164 _cell_measurement_theta_max 25.603 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.95 _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_% 0 _diffrn_reflns_number 22642 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8958 _reflns_number_gt 7403 _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^)+(0.0542P)^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 8958 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.90013(2) 0.81985(2) 0.634075(15) 0.01098(8) Uani 1 1 d . . . S1 S 0.70474(8) 0.95845(7) 0.62178(5) 0.01631(17) Uani 1 1 d . . . S2 S 0.91692(8) 0.72350(7) 0.96925(5) 0.01803(18) Uani 1 1 d . . . P1 P 1.09663(8) 0.69532(7) 0.63061(5) 0.01235(17) Uani 1 1 d . . . N1 N 0.8785(2) 0.9497(2) 0.78685(16) 0.0120(5) Uani 1 1 d . . . N2 N 0.9441(2) 0.9299(2) 0.70311(16) 0.0124(5) Uani 1 1 d . . . N3 N 0.6285(2) 0.9534(2) 0.80220(16) 0.0135(5) Uani 1 1 d . . . N4 N 0.5102(3) 0.9818(2) 0.86542(17) 0.0153(6) Uani 1 1 d . . . N5 N 0.4701(2) 1.0238(2) 0.73495(17) 0.0145(5) Uani 1 1 d . . . N6 N 0.7777(2) 0.7735(2) 0.84188(16) 0.0124(5) Uani 1 1 d . . . N7 N 0.7105(3) 0.7226(2) 0.80008(16) 0.0151(6) Uani 1 1 d . . . N8 N 0.7987(3) 0.6003(2) 0.89519(17) 0.0143(5) Uani 1 1 d . . . O1 O 0.8177(3) 0.6884(2) 0.52523(17) 0.0316(6) Uani 1 1 d . . . B1 B 0.7558(3) 0.9011(3) 0.8386(2) 0.0137(7) Uani 1 1 d . . . H1 H 0.7358 0.9201 0.8994 0.016 Uiso 1 1 calc R . . C1 C 0.8527(3) 0.7369(3) 0.5681(2) 0.0194(7) Uani 1 1 d . . . C3 C 0.9261(3) 1.0306(3) 0.8103(2) 0.0150(6) Uani 1 1 d . . . C4 C 1.0213(3) 1.0636(3) 0.7401(2) 0.0172(7) Uani 1 1 d . . . H4 H 1.0710 1.1196 0.7371 0.021 Uiso 1 1 calc R . . C5 C 1.0307(3) 0.9993(3) 0.67471(19) 0.0130(6) Uani 1 1 d . . . C6 C 0.8822(4) 1.0687(3) 0.8989(2) 0.0256(8) Uani 1 1 d . . . H6A H 0.7866 1.1042 0.9100 0.038 Uiso 1 1 calc R . . H6B H 0.9353 1.1223 0.9028 0.038 Uiso 1 1 calc R . . H6C H 0.8958 1.0045 0.9420 0.038 Uiso 1 1 calc R . . C7 C 1.1185(3) 1.0010(3) 0.5855(2) 0.0172(7) Uani 1 1 d . . . H7A H 1.1971 0.9400 0.5836 0.026 Uiso 1 1 calc R . . H7B H 1.1484 1.0722 0.5697 0.026 Uiso 1 1 calc R . . H7C H 1.0679 0.9920 0.5446 0.026 Uiso 1 1 calc R . . C8 C 0.6039(3) 0.9772(3) 0.7231(2) 0.0137(6) Uani 1 1 d . . . C9 C 0.4178(3) 1.0239(3) 0.8229(2) 0.0149(6) Uani 1 1 d . . . C10 C 0.2745(3) 1.0685(3) 0.8637(2) 0.0223(7) Uani 1 1 d . . . H10A H 0.2638 1.0680 0.9261 0.033 Uiso 1 1 calc R . . H10B H 0.2176 1.0218 0.8535 0.033 Uiso 1 1 calc R . . H10C H 0.2478 1.1449 0.8383 0.033 Uiso 1 1 calc R . . C11 C 0.3970(3) 1.0617(3) 0.6668(2) 0.0205(7) Uani 1 1 d . . . H11A H 0.3025 1.0533 0.6900 0.025 Uiso 1 1 calc R . . H11B H 0.4372 1.0139 0.6190 0.025 Uiso 1 1 calc R . . C12 C 0.3993(4) 1.1817(3) 0.6315(3) 0.0337(9) Uani 1 1 d . . . H12A H 0.3592 1.2296 0.6785 0.051 Uiso 1 1 calc R . . H12B H 0.3476 1.2033 0.5867 0.051 Uiso 1 1 calc R . . H12C H 0.4924 1.1901 0.6064 0.051 Uiso 1 1 calc R . . C13 C 0.8312(3) 0.6991(3) 0.90118(19) 0.0143(6) Uani 1 1 d . . . C14 C 0.7250(3) 0.6193(3) 0.8334(2) 0.0156(7) Uani 1 1 d . . . C15 C 0.6660(4) 0.5337(3) 0.8103(2) 0.0238(8) Uani 1 1 d . . . H15A H 0.6168 0.5668 0.7653 0.036 Uiso 1 1 calc R . . H15B H 0.6041 0.5058 0.8617 0.036 Uiso 1 1 calc R . . H15C H 0.7380 0.4720 0.7885 0.036 Uiso 1 1 calc R . . C16 C 0.8276(3) 0.4973(3) 0.9514(2) 0.0205(7) Uani 1 1 d . . . H16A H 0.9171 0.4901 0.9635 0.025 Uiso 1 1 calc R . . H16B H 0.8310 0.4330 0.9209 0.025 Uiso 1 1 calc R . . C17 C 0.7235(4) 0.4945(3) 1.0358(2) 0.0264(8) Uani 1 1 d . . . H17A H 0.7233 0.5556 1.0677 0.040 Uiso 1 1 calc R . . H17B H 0.7449 0.4233 1.0704 0.040 Uiso 1 1 calc R . . H17C H 0.6345 0.5027 1.0241 0.040 Uiso 1 1 calc R . . C18 C 1.1947(3) 0.6634(3) 0.5223(2) 0.0153(6) Uani 1 1 d . . . C19 C 1.2820(3) 0.5610(3) 0.5086(2) 0.0230(8) Uani 1 1 d . . . H19 H 1.2868 0.5044 0.5556 0.028 Uiso 1 1 calc R . . C20 C 1.3619(4) 0.5415(3) 0.4267(2) 0.0281(8) Uani 1 1 d . . . H20 H 1.4209 0.4715 0.4178 0.034 Uiso 1 1 calc R . . C21 C 1.3558(4) 0.6234(3) 0.3583(2) 0.0243(8) Uani 1 1 d . . . H21 H 1.4113 0.6100 0.3025 0.029 Uiso 1 1 calc R . . C22 C 1.2689(3) 0.7250(3) 0.3708(2) 0.0230(8) Uani 1 1 d . . . H22 H 1.2641 0.7814 0.3237 0.028 Uiso 1 1 calc R . . C23 C 1.1887(3) 0.7441(3) 0.4527(2) 0.0183(7) Uani 1 1 d . . . H23 H 1.1287 0.8137 0.4610 0.022 Uiso 1 1 calc R . . C24 C 1.0798(3) 0.5565(3) 0.6862(2) 0.0153(6) Uani 1 1 d . . . C25 C 1.0114(3) 0.4940(3) 0.6557(2) 0.0252(8) Uani 1 1 d . . . H25 H 0.9754 0.5233 0.6065 0.030 Uiso 1 1 calc R . . C26 C 0.9948(4) 0.3891(3) 0.6960(3) 0.0286(8) Uani 1 1 d . . . H26 H 0.9494 0.3463 0.6739 0.034 Uiso 1 1 calc R . . C27 C 1.0450(4) 0.3472(3) 0.7689(2) 0.0268(8) Uani 1 1 d . . . H27 H 1.0315 0.2764 0.7977 0.032 Uiso 1 1 calc R . . C28 C 1.1141(4) 0.4079(3) 0.7996(2) 0.0270(8) Uani 1 1 d . . . H28 H 1.1497 0.3783 0.8489 0.032 Uiso 1 1 calc R . . C29 C 1.1318(3) 0.5122(3) 0.7586(2) 0.0209(7) Uani 1 1 d . . . H29 H 1.1796 0.5538 0.7801 0.025 Uiso 1 1 calc R . . C30 C 1.2176(3) 0.7324(2) 0.6788(2) 0.0131(6) Uani 1 1 d . . . C31 C 1.1742(3) 0.7606(3) 0.7641(2) 0.0157(7) Uani 1 1 d . . . H31 H 1.0826 0.7645 0.7936 0.019 Uiso 1 1 calc R . . C32 C 1.2636(3) 0.7827(3) 0.8057(2) 0.0184(7) Uani 1 1 d . . . H32 H 1.2336 0.8008 0.8639 0.022 Uiso 1 1 calc R . . C33 C 1.3976(3) 0.7786(3) 0.7626(2) 0.0208(7) Uani 1 1 d . . . H33 H 1.4594 0.7928 0.7915 0.025 Uiso 1 1 calc R . . C34 C 1.4405(3) 0.7539(3) 0.6777(2) 0.0237(8) Uani 1 1 d . . . H34 H 1.5316 0.7531 0.6480 0.028 Uiso 1 1 calc R . . C35 C 1.3524(3) 0.7301(3) 0.6350(2) 0.0172(7) Uani 1 1 d . . . H35 H 1.3831 0.7125 0.5768 0.021 Uiso 1 1 calc R . . C36 C 0.4875(4) 0.2053(3) 0.9578(2) 0.0233(8) Uani 1 1 d . . . H36A H 0.3896 0.2192 0.9840 0.028 Uiso 1 1 calc R . . H36B H 0.5225 0.1240 0.9648 0.028 Uiso 1 1 calc R . . Cl1 Cl 0.51564(11) 0.25350(8) 0.84627(6) 0.0360(2) Uani 1 1 d . . . Cl2 Cl 0.56742(9) 0.27286(8) 1.01190(6) 0.0288(2) 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 0.00954(12) 0.01301(13) 0.01100(13) -0.00227(9) -0.00348(9) -0.00152(9) S1 0.0124(4) 0.0219(4) 0.0123(4) -0.0008(3) -0.0032(3) 0.0010(3) S2 0.0188(4) 0.0203(4) 0.0172(4) 0.0007(3) -0.0098(3) -0.0036(3) P1 0.0115(4) 0.0142(4) 0.0114(4) -0.0019(3) -0.0029(3) -0.0019(3) N1 0.0103(12) 0.0149(14) 0.0097(12) -0.0018(10) -0.0017(10) -0.0006(10) N2 0.0110(12) 0.0161(14) 0.0103(12) -0.0016(10) -0.0034(10) -0.0019(10) N3 0.0103(12) 0.0148(14) 0.0134(13) -0.0020(11) -0.0006(10) -0.0009(10) N4 0.0113(13) 0.0178(14) 0.0155(13) -0.0046(11) -0.0005(11) -0.0017(11) N5 0.0098(12) 0.0183(14) 0.0152(13) -0.0008(11) -0.0038(11) -0.0018(11) N6 0.0097(12) 0.0162(14) 0.0120(12) -0.0010(10) -0.0048(10) -0.0018(10) N7 0.0141(13) 0.0183(15) 0.0137(13) -0.0027(11) -0.0043(11) -0.0029(11) N8 0.0160(13) 0.0120(13) 0.0152(13) 0.0013(11) -0.0058(11) -0.0026(11) O1 0.0370(15) 0.0278(15) 0.0391(16) -0.0123(12) -0.0239(13) -0.0015(12) B1 0.0104(16) 0.0178(19) 0.0137(17) -0.0009(14) -0.0033(14) -0.0044(14) C1 0.0168(16) 0.0200(18) 0.0209(17) -0.0014(14) -0.0069(14) -0.0002(14) C3 0.0138(15) 0.0164(16) 0.0167(16) -0.0050(13) -0.0061(13) -0.0017(13) C4 0.0155(16) 0.0169(17) 0.0217(17) -0.0029(13) -0.0071(14) -0.0043(13) C5 0.0095(14) 0.0142(16) 0.0132(15) 0.0021(12) -0.0024(12) -0.0006(12) C6 0.0253(18) 0.031(2) 0.0235(18) -0.0121(16) -0.0003(15) -0.0118(16) C7 0.0149(15) 0.0210(18) 0.0161(16) 0.0022(13) -0.0046(13) -0.0064(13) C8 0.0126(15) 0.0118(15) 0.0165(15) -0.0046(12) -0.0029(12) -0.0003(12) C9 0.0122(15) 0.0162(16) 0.0156(15) -0.0036(13) -0.0018(13) -0.0017(12) C10 0.0132(16) 0.033(2) 0.0191(17) -0.0047(15) -0.0034(14) -0.0007(14) C11 0.0106(15) 0.033(2) 0.0189(17) -0.0002(15) -0.0075(13) -0.0029(14) C12 0.033(2) 0.034(2) 0.035(2) 0.0049(18) -0.0190(19) -0.0012(18) C13 0.0111(14) 0.0173(17) 0.0120(15) -0.0013(12) -0.0017(12) 0.0010(12) C14 0.0120(15) 0.0183(17) 0.0138(15) -0.0033(13) -0.0004(12) 0.0002(12) C15 0.0260(18) 0.0196(18) 0.0287(19) -0.0034(15) -0.0126(16) -0.0029(15) C16 0.0231(17) 0.0157(17) 0.0227(18) 0.0026(14) -0.0099(15) -0.0018(14) C17 0.033(2) 0.0213(19) 0.0260(19) 0.0056(15) -0.0092(16) -0.0112(16) C18 0.0159(15) 0.0183(17) 0.0138(15) -0.0031(13) -0.0037(13) -0.0064(13) C19 0.0267(19) 0.0200(18) 0.0186(17) -0.0029(14) -0.0008(15) -0.0021(15) C20 0.032(2) 0.0211(19) 0.027(2) -0.0100(16) -0.0010(16) 0.0011(16) C21 0.0284(19) 0.030(2) 0.0151(16) -0.0098(15) 0.0036(14) -0.0125(16) C22 0.0252(18) 0.029(2) 0.0157(17) -0.0013(15) -0.0041(14) -0.0089(15) C23 0.0175(16) 0.0199(18) 0.0174(16) -0.0021(13) -0.0039(13) -0.0035(13) C24 0.0138(15) 0.0134(16) 0.0162(16) -0.0028(13) 0.0012(13) -0.0022(12) C25 0.0247(18) 0.0207(19) 0.033(2) -0.0029(16) -0.0129(16) -0.0030(15) C26 0.0273(19) 0.0187(19) 0.043(2) -0.0055(17) -0.0117(18) -0.0057(15) C27 0.034(2) 0.0143(18) 0.0271(19) -0.0010(15) 0.0018(16) -0.0064(15) C28 0.043(2) 0.0167(18) 0.0208(18) -0.0013(14) -0.0098(17) -0.0017(16) C29 0.0285(19) 0.0174(17) 0.0190(17) -0.0029(14) -0.0094(15) -0.0041(14) C30 0.0125(15) 0.0098(15) 0.0176(16) -0.0009(12) -0.0063(13) -0.0008(12) C31 0.0152(15) 0.0145(16) 0.0180(16) -0.0004(13) -0.0059(13) -0.0029(13) C32 0.0215(17) 0.0156(17) 0.0204(17) -0.0038(13) -0.0106(14) -0.0009(13) C33 0.0222(17) 0.0145(17) 0.0310(19) -0.0023(14) -0.0163(15) -0.0030(14) C34 0.0119(16) 0.0234(19) 0.035(2) 0.0010(16) -0.0058(15) -0.0056(14) C35 0.0161(16) 0.0149(16) 0.0205(17) -0.0017(13) -0.0049(13) -0.0025(13) C36 0.0291(19) 0.026(2) 0.0147(16) -0.0004(14) -0.0029(15) -0.0096(16) Cl1 0.0611(7) 0.0323(5) 0.0173(4) 0.0013(4) -0.0065(4) -0.0201(5) Cl2 0.0334(5) 0.0297(5) 0.0262(5) -0.0078(4) -0.0091(4) -0.0066(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 C1 1.813(3) . ? Rh1 N2 2.084(3) . ? Rh1 P1 2.2681(9) . ? Rh1 S1 2.3835(8) . ? S1 C8 1.715(3) . ? S2 C13 1.686(3) . ? P1 C30 1.823(3) . ? P1 C18 1.829(3) . ? P1 C24 1.837(3) . ? N1 C3 1.359(4) . ? N1 N2 1.375(3) . ? N1 B1 1.537(4) . ? N2 C5 1.342(4) . ? N3 C8 1.337(4) . ? N3 N4 1.398(3) . ? N3 B1 1.561(4) . ? N4 C9 1.296(4) . ? N5 C8 1.366(4) . ? N5 C9 1.378(4) . ? N5 C11 1.455(4) . ? N6 C13 1.356(4) . ? N6 N7 1.390(3) . ? N6 B1 1.541(4) . ? N7 C14 1.301(4) . ? N8 C13 1.370(4) . ? N8 C14 1.372(4) . ? N8 C16 1.464(4) . ? O1 C1 1.156(4) . ? B1 H1 1.0000 . ? C3 C4 1.379(5) . ? C3 C6 1.495(4) . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C7 1.490(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.489(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.512(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.483(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.506(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.384(4) . ? C18 C19 1.395(5) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.379(5) . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.388(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.385(5) . ? C24 C29 1.396(4) . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C27 1.387(5) . ? C26 H26 0.9500 . ? C27 C28 1.376(5) . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.401(4) . ? C30 C35 1.404(4) . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.390(5) . ? C32 H32 0.9500 . ? C33 C34 1.382(5) . ? C33 H33 0.9500 . ? C34 C35 1.391(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 Cl2 1.760(3) . ? C36 Cl1 1.769(3) . ? 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 N2 173.98(12) . . ? C1 Rh1 P1 89.81(10) . . ? N2 Rh1 P1 95.15(7) . . ? C1 Rh1 S1 88.83(10) . . ? N2 Rh1 S1 85.87(7) . . ? P1 Rh1 S1 173.62(3) . . ? C8 S1 Rh1 109.11(11) . . ? C30 P1 C18 103.39(14) . . ? C30 P1 C24 102.70(14) . . ? C18 P1 C24 102.30(14) . . ? C30 P1 Rh1 116.42(10) . . ? C18 P1 Rh1 115.02(10) . . ? C24 P1 Rh1 115.12(10) . . ? C3 N1 N2 109.1(2) . . ? C3 N1 B1 126.0(3) . . ? N2 N1 B1 124.2(2) . . ? C5 N2 N1 107.4(2) . . ? C5 N2 Rh1 128.2(2) . . ? N1 N2 Rh1 124.24(19) . . ? C8 N3 N4 110.5(2) . . ? C8 N3 B1 135.0(3) . . ? N4 N3 B1 114.5(2) . . ? C9 N4 N3 105.2(2) . . ? C8 N5 C9 107.0(2) . . ? C8 N5 C11 125.8(3) . . ? C9 N5 C11 127.1(3) . . ? C13 N6 N7 110.4(2) . . ? C13 N6 B1 125.3(3) . . ? N7 N6 B1 122.1(2) . . ? C14 N7 N6 105.6(2) . . ? C13 N8 C14 107.6(3) . . ? C13 N8 C16 125.0(3) . . ? C14 N8 C16 127.2(3) . . ? N1 B1 N6 114.0(3) . . ? N1 B1 N3 111.7(2) . . ? N6 B1 N3 108.0(2) . . ? N1 B1 H1 107.6 . . ? N6 B1 H1 107.6 . . ? N3 B1 H1 107.6 . . ? O1 C1 Rh1 176.6(3) . . ? N1 C3 C4 107.5(3) . . ? N1 C3 C6 123.5(3) . . ? C4 C3 C6 129.0(3) . . ? C3 C4 C5 106.8(3) . . ? C3 C4 H4 126.6 . . ? C5 C4 H4 126.6 . . ? N2 C5 C4 109.1(3) . . ? N2 C5 C7 122.0(3) . . ? C4 C5 C7 128.9(3) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N5 106.1(3) . . ? N3 C8 S1 132.4(2) . . ? N5 C8 S1 121.5(2) . . ? N4 C9 N5 111.1(3) . . ? N4 C9 C10 124.5(3) . . ? N5 C9 C10 124.4(3) . . ? 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 . . ? N5 C11 C12 112.8(3) . . ? N5 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N5 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 N8 105.4(3) . . ? N6 C13 S2 127.3(2) . . ? N8 C13 S2 127.2(2) . . ? N7 C14 N8 111.1(3) . . ? N7 C14 C15 124.7(3) . . ? N8 C14 C15 124.2(3) . . ? 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 . . ? N8 C16 C17 112.2(3) . . ? N8 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N8 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.7(3) . . ? C23 C18 P1 119.8(2) . . ? C19 C18 P1 121.4(2) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 119.5(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C18 C23 C22 121.2(3) . . ? C18 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C29 118.8(3) . . ? C25 C24 P1 118.7(2) . . ? C29 C24 P1 122.5(2) . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.6(3) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 120.4(3) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C31 C30 C35 119.2(3) . . ? C31 C30 P1 118.1(2) . . ? C35 C30 P1 122.6(2) . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 119.8(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 121.0(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C30 119.3(3) . . ? C34 C35 H35 120.3 . . ? C30 C35 H35 120.3 . . ? Cl2 C36 Cl1 110.97(19) . . ? Cl2 C36 H36A 109.4 . . ? Cl1 C36 H36A 109.4 . . ? Cl2 C36 H36B 109.4 . . ? Cl1 C36 H36B 109.4 . . ? H36A C36 H36B 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 C1 Rh1 S1 C8 119.69(16) . . . . ? N2 Rh1 S1 C8 -63.16(14) . . . . ? C1 Rh1 P1 C30 173.73(16) . . . . ? N2 Rh1 P1 C30 -2.85(13) . . . . ? C1 Rh1 P1 C18 52.58(16) . . . . ? N2 Rh1 P1 C18 -124.00(13) . . . . ? C1 Rh1 P1 C24 -66.00(16) . . . . ? N2 Rh1 P1 C24 117.41(13) . . . . ? C3 N1 N2 C5 -0.7(3) . . . . ? B1 N1 N2 C5 170.1(3) . . . . ? C3 N1 N2 Rh1 -176.25(19) . . . . ? B1 N1 N2 Rh1 -5.4(4) . . . . ? P1 Rh1 N2 C5 73.6(2) . . . . ? S1 Rh1 N2 C5 -100.1(2) . . . . ? P1 Rh1 N2 N1 -111.8(2) . . . . ? S1 Rh1 N2 N1 74.6(2) . . . . ? C8 N3 N4 C9 -1.1(3) . . . . ? B1 N3 N4 C9 179.6(3) . . . . ? C13 N6 N7 C14 -0.6(3) . . . . ? B1 N6 N7 C14 -164.3(3) . . . . ? C3 N1 B1 N6 -137.4(3) . . . . ? N2 N1 B1 N6 53.4(4) . . . . ? C3 N1 B1 N3 99.8(3) . . . . ? N2 N1 B1 N3 -69.4(4) . . . . ? C13 N6 B1 N1 87.2(4) . . . . ? N7 N6 B1 N1 -111.6(3) . . . . ? C13 N6 B1 N3 -148.1(3) . . . . ? N7 N6 B1 N3 13.1(4) . . . . ? C8 N3 B1 N1 44.6(5) . . . . ? N4 N3 B1 N1 -136.3(3) . . . . ? C8 N3 B1 N6 -81.5(4) . . . . ? N4 N3 B1 N6 97.6(3) . . . . ? N2 N1 C3 C4 0.9(3) . . . . ? B1 N1 C3 C4 -169.7(3) . . . . ? N2 N1 C3 C6 -176.6(3) . . . . ? B1 N1 C3 C6 12.8(5) . . . . ? N1 C3 C4 C5 -0.8(3) . . . . ? C6 C3 C4 C5 176.5(3) . . . . ? N1 N2 C5 C4 0.1(3) . . . . ? Rh1 N2 C5 C4 175.5(2) . . . . ? N1 N2 C5 C7 -179.6(3) . . . . ? Rh1 N2 C5 C7 -4.2(4) . . . . ? C3 C4 C5 N2 0.4(3) . . . . ? C3 C4 C5 C7 -179.9(3) . . . . ? N4 N3 C8 N5 1.5(3) . . . . ? B1 N3 C8 N5 -179.4(3) . . . . ? N4 N3 C8 S1 -178.0(3) . . . . ? B1 N3 C8 S1 1.1(6) . . . . ? C9 N5 C8 N3 -1.3(3) . . . . ? C11 N5 C8 N3 -179.1(3) . . . . ? C9 N5 C8 S1 178.3(2) . . . . ? C11 N5 C8 S1 0.5(4) . . . . ? Rh1 S1 C8 N3 20.0(3) . . . . ? Rh1 S1 C8 N5 -159.4(2) . . . . ? N3 N4 C9 N5 0.3(3) . . . . ? N3 N4 C9 C10 -178.7(3) . . . . ? C8 N5 C9 N4 0.6(4) . . . . ? C11 N5 C9 N4 178.4(3) . . . . ? C8 N5 C9 C10 179.6(3) . . . . ? C11 N5 C9 C10 -2.6(5) . . . . ? C8 N5 C11 C12 -89.0(4) . . . . ? C9 N5 C11 C12 93.6(4) . . . . ? N7 N6 C13 N8 0.9(3) . . . . ? B1 N6 C13 N8 164.0(3) . . . . ? N7 N6 C13 S2 -178.0(2) . . . . ? B1 N6 C13 S2 -14.9(4) . . . . ? C14 N8 C13 N6 -0.9(3) . . . . ? C16 N8 C13 N6 -175.5(3) . . . . ? C14 N8 C13 S2 178.0(2) . . . . ? C16 N8 C13 S2 3.4(5) . . . . ? N6 N7 C14 N8 0.0(3) . . . . ? N6 N7 C14 C15 178.0(3) . . . . ? C13 N8 C14 N7 0.6(4) . . . . ? C16 N8 C14 N7 175.0(3) . . . . ? C13 N8 C14 C15 -177.4(3) . . . . ? C16 N8 C14 C15 -3.0(5) . . . . ? C13 N8 C16 C17 82.6(4) . . . . ? C14 N8 C16 C17 -90.9(4) . . . . ? C30 P1 C18 C23 -96.7(3) . . . . ? C24 P1 C18 C23 156.8(3) . . . . ? Rh1 P1 C18 C23 31.3(3) . . . . ? C30 P1 C18 C19 79.5(3) . . . . ? C24 P1 C18 C19 -26.9(3) . . . . ? Rh1 P1 C18 C19 -152.5(2) . . . . ? C23 C18 C19 C20 0.5(5) . . . . ? P1 C18 C19 C20 -175.7(3) . . . . ? C18 C19 C20 C21 0.2(6) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? C20 C21 C22 C23 0.4(5) . . . . ? C19 C18 C23 C22 -0.9(5) . . . . ? P1 C18 C23 C22 175.5(2) . . . . ? C21 C22 C23 C18 0.4(5) . . . . ? C30 P1 C24 C25 -169.6(3) . . . . ? C18 P1 C24 C25 -62.6(3) . . . . ? Rh1 P1 C24 C25 62.9(3) . . . . ? C30 P1 C24 C29 11.2(3) . . . . ? C18 P1 C24 C29 118.2(3) . . . . ? Rh1 P1 C24 C29 -116.3(3) . . . . ? C29 C24 C25 C26 -0.1(5) . . . . ? P1 C24 C25 C26 -179.3(3) . . . . ? C24 C25 C26 C27 1.3(6) . . . . ? C25 C26 C27 C28 -1.8(6) . . . . ? C26 C27 C28 C29 1.2(6) . . . . ? C27 C28 C29 C24 0.0(5) . . . . ? C25 C24 C29 C28 -0.6(5) . . . . ? P1 C24 C29 C28 178.6(3) . . . . ? C18 P1 C30 C31 -179.2(2) . . . . ? C24 P1 C30 C31 -73.0(3) . . . . ? Rh1 P1 C30 C31 53.7(3) . . . . ? C18 P1 C30 C35 -1.3(3) . . . . ? C24 P1 C30 C35 104.8(3) . . . . ? Rh1 P1 C30 C35 -128.5(2) . . . . ? C35 C30 C31 C32 -1.9(5) . . . . ? P1 C30 C31 C32 176.0(2) . . . . ? C30 C31 C32 C33 0.8(5) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? C32 C33 C34 C35 -1.6(5) . . . . ? C33 C34 C35 C30 0.6(5) . . . . ? C31 C30 C35 C34 1.2(5) . . . . ? P1 C30 C35 C34 -176.6(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 0.563 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.155 data_21 _database_code_depnum_ccdc_archive 'CCDC 792573' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H39 B N8 O P Rh S2, 2(C H2 Cl2)' _chemical_formula_sum 'C40 H43 B Cl4 N8 O P Rh S2' _chemical_formula_weight 1002.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 14.9460(5) _cell_length_b 16.7773(3) _cell_length_c 17.6339(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.065(2) _cell_angle_gamma 90.00 _cell_volume 4404.50(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22385 _cell_measurement_theta_min 2.0953 _cell_measurement_theta_max 29.9999 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'Crysalis RED' _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 'Oxford Diffraction Gemini' _diffrn_measurement_method w/scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52164 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.1467 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.09 _reflns_number_total 12074 _reflns_number_gt 6382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxf Diff Ltd. V 1.171.32.5' _computing_cell_refinement 'CrysAlis RED, Oxf Diff Ltd. V 1.171.32.5' _computing_data_reduction 'CrysAlis RED, Oxf Diff Ltd. V 1.171.32.5' _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^)+(0.0424P)^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 12074 _refine_ls_number_parameters 586 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.941 _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 0.610971(15) 0.403111(15) 0.425555(11) 0.02792(8) Uani 1 1 d . A . P1 P 0.72137(5) 0.48687(5) 0.39748(4) 0.02820(19) Uani 1 1 d . . . S1 S 0.47512(5) 0.33396(5) 0.44555(4) 0.0378(2) Uani 1 1 d . . . S2 S 0.58768(5) 0.37882(5) 0.28853(3) 0.02982(19) Uani 1 1 d . . . O1 O 0.61163(13) 0.46884(13) 0.58194(10) 0.0386(5) Uani 1 1 d . A . N1 N 0.56314(16) 0.19828(14) 0.39967(11) 0.0306(6) Uani 1 1 d . . . N2 N 0.54049(17) 0.12022(14) 0.37793(11) 0.0335(6) Uani 1 1 d . A . N3 N 0.41955(17) 0.18565(17) 0.40520(12) 0.0380(7) Uani 1 1 d . . . N4 N 0.67942(15) 0.23778(14) 0.31312(11) 0.0279(6) Uani 1 1 d . . . N5 N 0.72767(15) 0.18250(14) 0.27382(11) 0.0280(6) Uani 1 1 d . A . N6 N 0.68246(14) 0.28334(15) 0.19898(11) 0.0260(5) Uani 1 1 d . . . N7 N 0.72850(15) 0.16977(14) 0.43815(11) 0.0252(5) Uani 1 1 d . . . N8 N 0.80704(15) 0.20207(14) 0.46882(11) 0.0250(5) Uani 1 1 d . A . B1 B 0.6605(2) 0.2268(2) 0.39764(16) 0.0299(8) Uani 1 1 d . A . H1 H 0.6666 0.2798 0.4235 0.036 Uiso 1 1 calc R . . C1 C 0.61197(18) 0.44436(18) 0.52108(15) 0.0304(7) Uani 1 1 d . . . C3 C 0.4901(2) 0.2381(2) 0.41603(13) 0.0352(8) Uani 1 1 d . A . C4 C 0.4545(2) 0.1144(2) 0.38290(14) 0.0409(9) Uani 1 1 d . A . C5 C 0.4007(2) 0.0413(2) 0.36458(16) 0.0475(9) Uani 1 1 d . . . H5A H 0.3596 0.0508 0.3190 0.071 Uiso 1 1 calc R A . H5B H 0.3659 0.0281 0.4075 0.071 Uiso 1 1 calc R . . H5C H 0.4409 -0.0030 0.3552 0.071 Uiso 1 1 calc R . . C6 C 0.3265(2) 0.2030(2) 0.41475(15) 0.0468(9) Uani 1 1 d . A . H6A H 0.2877 0.1701 0.3787 0.056 Uiso 1 1 calc R . . H6B H 0.3143 0.2597 0.4021 0.056 Uiso 1 1 calc R . . C7 C 0.3023(2) 0.1868(2) 0.49561(16) 0.0585(11) Uani 1 1 d . . . H7A H 0.3142 0.1308 0.5084 0.088 Uiso 1 1 calc R A . H7B H 0.2385 0.1984 0.4990 0.088 Uiso 1 1 calc R . . H7C H 0.3387 0.2210 0.5314 0.088 Uiso 1 1 calc R . . C8 C 0.65125(17) 0.29844(18) 0.26818(14) 0.0265(7) Uani 1 1 d . A . C9 C 0.72786(18) 0.21275(19) 0.20521(14) 0.0295(7) Uani 1 1 d . A . C10 C 0.77237(19) 0.17588(18) 0.14169(14) 0.0333(7) Uani 1 1 d . . . H10A H 0.7936 0.1224 0.1567 0.050 Uiso 1 1 calc R A . H10B H 0.8235 0.2088 0.1300 0.050 Uiso 1 1 calc R . . H10C H 0.7293 0.1721 0.0966 0.050 Uiso 1 1 calc R . . C11 C 0.66919(17) 0.33576(19) 0.13214(13) 0.0306(7) Uani 1 1 d . A . H11A H 0.7156 0.3243 0.0969 0.037 Uiso 1 1 calc R . . H11B H 0.6759 0.3920 0.1485 0.037 Uiso 1 1 calc R . . C12 C 0.57624(19) 0.3235(2) 0.09081(15) 0.0443(9) Uani 1 1 d . . . H12A H 0.5714 0.2690 0.0709 0.066 Uiso 1 1 calc R A . H12B H 0.5672 0.3614 0.0486 0.066 Uiso 1 1 calc R . . H12C H 0.5304 0.3320 0.1264 0.066 Uiso 1 1 calc R . . C13 C 0.7294(2) 0.08996(18) 0.44673(14) 0.0337(8) Uani 1 1 d . A . H13 H 0.6823 0.0546 0.4294 0.040 Uiso 1 1 calc R . . C14 C 0.8093(2) 0.06837(18) 0.48445(14) 0.0316(7) Uani 1 1 d . . . H14 H 0.8286 0.0163 0.4994 0.038 Uiso 1 1 calc R A . C15 C 0.85713(18) 0.14070(17) 0.49646(14) 0.0247(6) Uani 1 1 d . A . C16 C 0.94709(19) 0.15413(17) 0.53504(15) 0.0282(7) Uani 1 1 d . . . C17 C 0.99920(19) 0.09073(18) 0.56471(14) 0.0291(7) Uani 1 1 d . A . H17 H 0.9769 0.0378 0.5592 0.035 Uiso 1 1 calc R . . C18 C 1.08350(19) 0.10410(19) 0.60224(16) 0.0361(8) Uani 1 1 d . . . H18 H 1.1181 0.0606 0.6231 0.043 Uiso 1 1 calc R A . C19 C 1.11685(19) 0.1802(2) 0.60915(18) 0.0409(8) Uani 1 1 d . A . H19 H 1.1744 0.1891 0.6351 0.049 Uiso 1 1 calc R . . C20 C 1.0677(2) 0.2436(2) 0.57893(18) 0.0440(8) Uani 1 1 d . . . H20 H 1.0916 0.2961 0.5831 0.053 Uiso 1 1 calc R A . C21 C 0.98301(18) 0.23076(18) 0.54233(16) 0.0335(7) Uani 1 1 d . A . H21 H 0.9489 0.2748 0.5219 0.040 Uiso 1 1 calc R . . C22 C 0.79771(17) 0.43999(18) 0.33482(14) 0.0268(7) Uani 1 1 d . A . C23 C 0.81538(18) 0.47089(19) 0.26416(15) 0.0321(7) Uani 1 1 d . . . H23 H 0.7907 0.5209 0.2479 0.038 Uiso 1 1 calc R A . C24 C 0.86868(19) 0.42908(19) 0.21758(15) 0.0344(8) Uani 1 1 d . A . H24 H 0.8798 0.4505 0.1694 0.041 Uiso 1 1 calc R . . C25 C 0.90570(18) 0.35692(19) 0.24015(15) 0.0323(7) Uani 1 1 d . . . H25 H 0.9432 0.3291 0.2083 0.039 Uiso 1 1 calc R A . C26 C 0.88781(18) 0.32533(18) 0.30947(15) 0.0308(7) Uani 1 1 d . A . H26 H 0.9126 0.2753 0.3254 0.037 Uiso 1 1 calc R . . C27 C 0.83352(19) 0.36664(19) 0.35592(14) 0.0311(7) Uani 1 1 d . . . H27 H 0.8208 0.3440 0.4032 0.037 Uiso 1 1 calc R A . C28 C 0.67749(18) 0.57685(17) 0.34963(13) 0.0263(7) Uani 1 1 d . A . C29 C 0.58463(19) 0.58808(18) 0.34120(14) 0.0301(7) Uani 1 1 d . . . H29 H 0.5465 0.5484 0.3593 0.036 Uiso 1 1 calc R A . C30 C 0.5468(2) 0.65623(19) 0.30678(14) 0.0355(8) Uani 1 1 d . A . H30 H 0.4835 0.6630 0.3016 0.043 Uiso 1 1 calc R . . C31 C 0.6022(2) 0.7142(2) 0.28010(14) 0.0386(8) Uani 1 1 d . . . H31 H 0.5769 0.7609 0.2565 0.046 Uiso 1 1 calc R A . C32 C 0.6940(2) 0.7041(2) 0.28787(15) 0.0404(8) Uani 1 1 d . A . H32 H 0.7317 0.7438 0.2691 0.049 Uiso 1 1 calc R . . C34A C 0.7938(3) 0.5349(3) 0.4778(2) 0.0199(15) Uani 0.601(10) 1 d PGU A 1 C35A C 0.8702(3) 0.4934(4) 0.5058(2) 0.0419(19) Uani 0.601(10) 1 d PGU A 1 H35A H 0.8849 0.4441 0.4834 0.050 Uiso 0.601(10) 1 calc PR A 1 C36A C 0.9250(2) 0.5238(5) 0.5668(2) 0.043(2) Uani 0.601(10) 1 d PGU A 1 H36A H 0.9772 0.4955 0.5859 0.052 Uiso 0.601(10) 1 calc PR A 1 C37A C 0.9035(3) 0.5958(4) 0.59968(19) 0.0324(16) Uani 0.601(10) 1 d PGU A 1 H37A H 0.9410 0.6167 0.6413 0.039 Uiso 0.601(10) 1 calc PR A 1 C38A C 0.8271(4) 0.6373(2) 0.5717(2) 0.0344(16) Uani 0.601(10) 1 d PGU A 1 H38A H 0.8124 0.6865 0.5942 0.041 Uiso 0.601(10) 1 calc PR A 1 C39A C 0.7723(4) 0.6069(3) 0.5108(2) 0.0290(14) Uani 0.601(10) 1 d PGU A 1 H39A H 0.7201 0.6352 0.4916 0.035 Uiso 0.601(10) 1 calc PR A 1 C33 C 0.7320(2) 0.63637(19) 0.32288(14) 0.0355(8) Uani 1 1 d . . . H33 H 0.7954 0.6305 0.3286 0.043 Uiso 1 1 calc R A . C34B C 0.8052(4) 0.5101(4) 0.4759(3) 0.022(2) Uani 0.399(10) 1 d PGU A 2 C35B C 0.8559(5) 0.4523(5) 0.5165(3) 0.031(2) Uani 0.399(10) 1 d PGU A 2 H35B H 0.8486 0.3977 0.5031 0.037 Uiso 0.399(10) 1 calc PR A 2 C36B C 0.9171(4) 0.4743(6) 0.5768(3) 0.039(2) Uani 0.399(10) 1 d PGU A 2 H36B H 0.9517 0.4348 0.6045 0.047 Uiso 0.399(10) 1 calc PR A 2 C37B C 0.9277(5) 0.5542(6) 0.5964(3) 0.035(3) Uani 0.399(10) 1 d PGU A 2 H37B H 0.9695 0.5693 0.6376 0.042 Uiso 0.399(10) 1 calc PR A 2 C38B C 0.8770(7) 0.6121(5) 0.5558(4) 0.040(3) Uani 0.399(10) 1 d PGU A 2 H38B H 0.8843 0.6667 0.5692 0.048 Uiso 0.399(10) 1 calc PR A 2 C39B C 0.8158(6) 0.5900(4) 0.4955(4) 0.032(2) Uani 0.399(10) 1 d PGU A 2 H39B H 0.7812 0.6295 0.4678 0.039 Uiso 0.399(10) 1 calc PR A 2 C40 C 0.3471(2) 0.4784(2) 0.24236(16) 0.0465(9) Uani 1 1 d . B 2 H40A H 0.3972 0.4692 0.2819 0.056 Uiso 1 1 calc R B 2 H40B H 0.3474 0.5355 0.2282 0.056 Uiso 1 1 calc R B 2 Cl1 Cl 0.24478(6) 0.45488(6) 0.27899(5) 0.0642(3) Uani 1 1 d . B 2 Cl2 Cl 0.36274(5) 0.41950(5) 0.16171(4) 0.0404(2) Uani 1 1 d . B 2 C41A C 0.0151(9) 0.5965(7) 0.1987(7) 0.044(3) Uani 0.540(18) 1 d PU C 3 H41A H 0.0767 0.6095 0.1862 0.053 Uiso 0.540(18) 1 calc PR C 3 H41B H 0.0113 0.5381 0.2056 0.053 Uiso 0.540(18) 1 calc PR C 3 Cl3A Cl -0.0621(10) 0.62627(19) 0.1239(3) 0.062(2) Uani 0.540(18) 1 d PU C 3 Cl4A Cl -0.0067(3) 0.6452(3) 0.2849(5) 0.0465(11) Uani 0.540(18) 1 d PU C 3 C41B C -0.0009(10) 0.6102(9) 0.1721(7) 0.039(3) Uani 0.460(18) 1 d PU C 4 H41C H 0.0156 0.5538 0.1825 0.046 Uiso 0.460(18) 1 calc PR C 4 H41D H 0.0469 0.6347 0.1444 0.046 Uiso 0.460(18) 1 calc PR C 4 Cl3B Cl -0.1056(5) 0.6144(4) 0.1143(2) 0.0378(12) Uani 0.460(18) 1 d PU C 4 Cl4B Cl -0.0083(4) 0.6596(5) 0.2568(5) 0.0547(12) Uani 0.460(18) 1 d PU C 4 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 0.02256(12) 0.04802(17) 0.01305(10) 0.00192(10) 0.00091(8) -0.01688(12) P1 0.0214(4) 0.0471(5) 0.0158(3) 0.0052(3) 0.0001(3) -0.0155(4) S1 0.0305(4) 0.0611(6) 0.0228(4) -0.0048(4) 0.0082(3) -0.0267(4) S2 0.0200(4) 0.0556(5) 0.0135(3) 0.0015(3) -0.0007(3) -0.0081(3) O1 0.0365(12) 0.0607(16) 0.0184(10) -0.0025(10) 0.0014(9) -0.0157(11) N1 0.0382(15) 0.0407(17) 0.0130(11) 0.0000(10) 0.0030(10) -0.0270(13) N2 0.0404(15) 0.0436(17) 0.0155(11) 0.0041(10) -0.0037(10) -0.0300(13) N3 0.0389(16) 0.059(2) 0.0158(12) -0.0004(12) 0.0040(11) -0.0350(14) N4 0.0312(14) 0.0361(16) 0.0158(11) 0.0043(11) -0.0002(10) -0.0174(12) N5 0.0284(13) 0.0392(16) 0.0157(11) 0.0031(10) -0.0019(10) -0.0158(12) N6 0.0195(12) 0.0459(16) 0.0124(10) 0.0053(10) 0.0003(9) -0.0066(12) N7 0.0328(14) 0.0299(16) 0.0124(10) -0.0025(10) -0.0005(10) -0.0188(11) N8 0.0274(13) 0.0330(15) 0.0152(11) -0.0047(10) 0.0046(10) -0.0122(11) B1 0.040(2) 0.035(2) 0.0147(15) -0.0047(14) 0.0016(14) -0.0249(17) C1 0.0234(15) 0.046(2) 0.0219(15) 0.0028(13) 0.0022(12) -0.0186(14) C3 0.0339(17) 0.061(2) 0.0104(12) 0.0003(13) 0.0014(12) -0.0324(17) C4 0.052(2) 0.059(3) 0.0107(13) 0.0018(14) -0.0012(13) -0.0371(19) C5 0.052(2) 0.061(2) 0.0276(16) 0.0005(15) -0.0017(15) -0.0411(19) C6 0.044(2) 0.076(3) 0.0220(15) -0.0069(15) 0.0082(14) -0.0392(19) C7 0.058(2) 0.093(3) 0.0268(16) -0.0075(17) 0.0147(16) -0.039(2) C8 0.0196(14) 0.045(2) 0.0151(13) -0.0006(13) 0.0024(11) -0.0159(13) C9 0.0210(15) 0.049(2) 0.0183(14) 0.0070(13) 0.0001(11) -0.0121(15) C10 0.0284(16) 0.049(2) 0.0233(14) 0.0101(14) 0.0042(12) -0.0012(15) C11 0.0212(15) 0.055(2) 0.0157(13) 0.0128(13) 0.0017(11) 0.0035(14) C12 0.0264(17) 0.090(3) 0.0162(14) 0.0038(15) -0.0015(12) 0.0074(17) C13 0.050(2) 0.034(2) 0.0169(13) 0.0000(13) -0.0003(13) -0.0217(16) C14 0.0438(19) 0.0276(18) 0.0243(14) -0.0062(12) 0.0086(14) -0.0108(15) C15 0.0279(16) 0.0278(18) 0.0207(13) -0.0073(12) 0.0145(12) -0.0078(14) C16 0.0280(16) 0.0300(19) 0.0295(15) -0.0067(13) 0.0182(13) -0.0062(14) C17 0.0291(16) 0.0283(18) 0.0328(15) -0.0043(13) 0.0185(13) -0.0006(14) C18 0.0260(16) 0.042(2) 0.0431(17) -0.0036(15) 0.0168(14) 0.0065(16) C19 0.0154(15) 0.052(2) 0.056(2) -0.0116(17) 0.0084(14) -0.0014(16) C20 0.0271(17) 0.035(2) 0.071(2) -0.0131(17) 0.0135(16) -0.0092(16) C21 0.0193(15) 0.032(2) 0.0503(18) -0.0071(14) 0.0108(13) -0.0030(14) C22 0.0170(14) 0.0433(19) 0.0197(13) 0.0096(13) 0.0000(11) -0.0111(13) C23 0.0203(15) 0.045(2) 0.0305(15) 0.0156(14) 0.0025(12) -0.0005(14) C24 0.0226(16) 0.051(2) 0.0301(15) 0.0157(14) 0.0085(13) -0.0015(15) C25 0.0178(15) 0.042(2) 0.0363(16) 0.0047(15) -0.0006(13) -0.0080(14) C26 0.0273(16) 0.0325(18) 0.0303(15) 0.0070(13) -0.0105(13) -0.0123(14) C27 0.0267(16) 0.047(2) 0.0177(13) 0.0095(13) -0.0076(12) -0.0154(15) C28 0.0274(15) 0.0386(19) 0.0126(12) -0.0013(11) 0.0000(11) -0.0125(13) C29 0.0303(16) 0.041(2) 0.0194(13) -0.0097(13) 0.0053(12) -0.0096(15) C30 0.0382(18) 0.046(2) 0.0222(14) -0.0082(14) 0.0027(13) -0.0031(16) C31 0.052(2) 0.045(2) 0.0173(14) 0.0002(13) -0.0058(14) -0.0029(17) C32 0.045(2) 0.056(2) 0.0196(15) 0.0065(14) -0.0061(14) -0.0193(18) C34A 0.014(3) 0.030(4) 0.016(3) 0.010(2) 0.001(2) -0.008(3) C35A 0.044(4) 0.035(5) 0.044(4) -0.009(3) -0.014(3) 0.008(3) C36A 0.031(3) 0.062(6) 0.032(4) -0.008(4) -0.017(3) 0.006(3) C37A 0.029(3) 0.044(4) 0.023(3) 0.004(3) -0.005(2) -0.015(3) C38A 0.038(4) 0.039(3) 0.026(3) -0.011(2) 0.002(2) -0.005(3) C39A 0.023(3) 0.037(3) 0.026(3) -0.002(2) -0.006(2) 0.001(3) C33 0.0296(17) 0.054(2) 0.0220(14) 0.0086(14) -0.0055(13) -0.0145(16) C34B 0.027(5) 0.014(5) 0.027(5) -0.003(3) 0.011(4) -0.007(4) C35B 0.036(5) 0.035(5) 0.020(4) -0.001(4) -0.006(3) 0.001(4) C36B 0.042(5) 0.048(6) 0.026(4) 0.007(4) -0.008(3) -0.010(5) C37B 0.038(6) 0.051(7) 0.015(4) 0.000(5) -0.007(4) -0.022(5) C38B 0.060(7) 0.027(5) 0.033(5) -0.002(4) -0.002(4) -0.020(5) C39B 0.038(6) 0.019(5) 0.038(4) 0.012(4) -0.008(4) -0.001(4) C40 0.052(2) 0.051(2) 0.0357(17) -0.0069(15) 0.0002(15) -0.0231(18) Cl1 0.0626(6) 0.0806(7) 0.0513(5) -0.0223(5) 0.0156(5) -0.0363(6) Cl2 0.0469(5) 0.0439(5) 0.0290(4) 0.0070(3) -0.0048(3) -0.0035(4) C41A 0.062(6) 0.022(5) 0.053(7) 0.014(5) 0.036(5) -0.003(4) Cl3A 0.113(6) 0.0416(13) 0.0342(14) 0.0039(10) 0.024(2) -0.007(2) Cl4A 0.0423(12) 0.0555(18) 0.043(2) -0.0144(17) 0.0105(15) -0.0142(11) C41B 0.061(6) 0.023(7) 0.033(7) 0.015(5) 0.016(5) 0.001(5) Cl3B 0.039(2) 0.042(2) 0.0324(12) 0.0011(11) 0.0070(12) 0.0079(14) Cl4B 0.0607(17) 0.069(3) 0.036(2) -0.018(2) 0.0145(18) -0.0342(16) _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 1.820(3) . ? Rh1 P1 2.2554(7) . ? Rh1 S1 2.3915(7) . ? Rh1 S2 2.4449(6) . ? P1 C28 1.823(3) . ? P1 C34B 1.824(4) . ? P1 C22 1.834(3) . ? P1 C34A 1.886(3) . ? S1 C3 1.712(3) . ? S2 C8 1.706(3) . ? O1 C1 1.150(3) . ? N1 C3 1.333(4) . ? N1 N2 1.398(3) . ? N1 B1 1.535(4) . ? N2 C4 1.299(4) . ? N3 C3 1.374(3) . ? N3 C4 1.376(4) . ? N3 C6 1.445(4) . ? N4 C8 1.335(3) . ? N4 N5 1.396(3) . ? N4 B1 1.552(3) . ? N5 C9 1.312(3) . ? N6 C9 1.365(4) . ? N6 C8 1.368(3) . ? N6 C11 1.470(3) . ? N7 C13 1.347(4) . ? N7 N8 1.361(3) . ? N7 B1 1.526(4) . ? N8 C15 1.339(3) . ? B1 H1 1.0000 . ? C4 C5 1.486(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.526(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.487(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.364(4) . ? C13 H13 0.9500 . ? C14 C15 1.415(4) . ? C14 H14 0.9500 . ? C15 C16 1.470(4) . ? C16 C17 1.393(4) . ? C16 C21 1.395(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.372(4) . ? C18 H18 0.9500 . ? C19 C20 1.374(4) . ? C19 H19 0.9500 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.380(4) . ? C22 C23 1.396(3) . ? C23 C24 1.384(4) . ? C23 H23 0.9500 . ? C24 C25 1.375(4) . ? C24 H24 0.9500 . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 C27 1.388(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.396(4) . ? C28 C33 1.397(4) . ? C29 C30 1.391(4) . ? C29 H29 0.9500 . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.376(4) . ? C31 H31 0.9500 . ? C32 C33 1.391(4) . ? C32 H32 0.9500 . ? C34A C35A 1.3900 . ? C34A C39A 1.3900 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A C38A 1.3900 . ? C37A H37A 0.9500 . ? C38A C39A 1.3900 . ? C38A H38A 0.9500 . ? C39A H39A 0.9500 . ? C33 H33 0.9500 . ? C34B C35B 1.3900 . ? C34B C39B 1.3900 . ? C35B C36B 1.3900 . ? C35B H35B 0.9500 . ? C36B C37B 1.3900 . ? C36B H36B 0.9500 . ? C37B C38B 1.3900 . ? C37B H37B 0.9500 . ? C38B C39B 1.3900 . ? C38B H38B 0.9500 . ? C39B H39B 0.9500 . ? C40 Cl1 1.757(3) . ? C40 Cl2 1.765(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41A Cl3A 1.748(9) . ? C41A Cl4A 1.780(12) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C41B Cl4B 1.719(14) . ? C41B Cl3B 1.793(13) . ? C41B H41C 0.9900 . ? C41B H41D 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 91.14(8) . . ? C1 Rh1 S1 89.18(8) . . ? P1 Rh1 S1 169.03(3) . . ? C1 Rh1 S2 165.23(10) . . ? P1 Rh1 S2 85.99(2) . . ? S1 Rh1 S2 90.93(2) . . ? C28 P1 C34B 111.6(3) . . ? C28 P1 C22 107.09(12) . . ? C34B P1 C22 97.2(2) . . ? C28 P1 C34A 98.82(19) . . ? C22 P1 C34A 106.82(17) . . ? C28 P1 Rh1 112.17(9) . . ? C34B P1 Rh1 115.7(2) . . ? C22 P1 Rh1 111.79(9) . . ? C34A P1 Rh1 118.92(14) . . ? C3 S1 Rh1 105.99(10) . . ? C8 S2 Rh1 107.84(9) . . ? C3 N1 N2 110.2(2) . . ? C3 N1 B1 130.2(3) . . ? N2 N1 B1 119.5(2) . . ? C4 N2 N1 105.6(3) . . ? C3 N3 C4 106.8(3) . . ? C3 N3 C6 126.1(3) . . ? C4 N3 C6 127.0(3) . . ? C8 N4 N5 111.2(2) . . ? C8 N4 B1 125.9(2) . . ? N5 N4 B1 122.9(2) . . ? C9 N5 N4 104.1(2) . . ? C9 N6 C8 107.2(2) . . ? C9 N6 C11 127.9(2) . . ? C8 N6 C11 124.9(2) . . ? C13 N7 N8 110.6(2) . . ? C13 N7 B1 132.4(2) . . ? N8 N7 B1 116.9(2) . . ? C15 N8 N7 105.9(2) . . ? N7 B1 N1 112.8(2) . . ? N7 B1 N4 110.7(2) . . ? N1 B1 N4 108.2(2) . . ? N7 B1 H1 108.3 . . ? N1 B1 H1 108.3 . . ? N4 B1 H1 108.3 . . ? O1 C1 Rh1 178.4(3) . . ? N1 C3 N3 106.4(3) . . ? N1 C3 S1 131.9(2) . . ? N3 C3 S1 121.6(3) . . ? N2 C4 N3 110.9(3) . . ? N2 C4 C5 124.6(3) . . ? N3 C4 C5 124.5(3) . . ? 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 . . ? N3 C6 C7 112.5(3) . . ? N3 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N3 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 N6 105.9(2) . . ? N4 C8 S2 129.05(19) . . ? N6 C8 S2 125.0(2) . . ? N5 C9 N6 111.6(2) . . ? N5 C9 C10 124.8(3) . . ? N6 C9 C10 123.5(2) . . ? 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 . . ? N6 C11 C12 110.8(2) . . ? N6 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N6 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 C14 108.6(3) . . ? N7 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? C13 C14 C15 104.7(3) . . ? C13 C14 H14 127.6 . . ? C15 C14 H14 127.6 . . ? N8 C15 C14 110.3(2) . . ? N8 C15 C16 120.6(2) . . ? C14 C15 C16 129.1(3) . . ? C17 C16 C21 118.1(3) . . ? C17 C16 C15 121.0(3) . . ? C21 C16 C15 120.9(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C16 121.0(3) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? C27 C22 C23 118.2(3) . . ? C27 C22 P1 117.84(19) . . ? C23 C22 P1 123.7(2) . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.8(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.3(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C22 C27 C26 121.3(2) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C33 118.1(3) . . ? C29 C28 P1 118.3(2) . . ? C33 C28 P1 123.5(2) . . ? C30 C29 C28 121.3(3) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 119.6(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C30 120.0(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C35A C34A C39A 120.0 . . ? C35A C34A P1 116.9(2) . . ? C39A C34A P1 123.1(2) . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C38A C37A C36A 120.0 . . ? C38A C37A H37A 120.0 . . ? C36A C37A H37A 120.0 . . ? C37A C38A C39A 120.0 . . ? C37A C38A H38A 120.0 . . ? C39A C38A H38A 120.0 . . ? C38A C39A C34A 120.0 . . ? C38A C39A H39A 120.0 . . ? C34A C39A H39A 120.0 . . ? C32 C33 C28 120.5(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35B C34B C39B 120.0 . . ? C35B C34B P1 123.2(3) . . ? C39B C34B P1 116.8(3) . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C37B C36B C35B 120.0 . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B C37B C38B 120.0 . . ? C36B C37B H37B 120.0 . . ? C38B C37B H37B 120.0 . . ? C39B C38B C37B 120.0 . . ? C39B C38B H38B 120.0 . . ? C37B C38B H38B 120.0 . . ? C38B C39B C34B 120.0 . . ? C38B C39B H39B 120.0 . . ? C34B C39B H39B 120.0 . . ? Cl1 C40 Cl2 110.57(16) . . ? Cl1 C40 H40A 109.5 . . ? Cl2 C40 H40A 109.5 . . ? Cl1 C40 H40B 109.5 . . ? Cl2 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? Cl3A C41A Cl4A 110.8(7) . . ? Cl3A C41A H41A 109.5 . . ? Cl4A C41A H41A 109.5 . . ? Cl3A C41A H41B 109.5 . . ? Cl4A C41A H41B 109.5 . . ? H41A C41A H41B 108.1 . . ? Cl4B C41B Cl3B 110.8(8) . . ? Cl4B C41B H41C 109.5 . . ? Cl3B C41B H41C 109.5 . . ? Cl4B C41B H41D 109.5 . . ? Cl3B C41B H41D 109.5 . . ? H41C C41B H41D 108.1 . . ? 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 C28 -94.91(13) . . . . ? S1 Rh1 P1 C28 -3.34(18) . . . . ? S2 Rh1 P1 C28 70.59(9) . . . . ? C1 Rh1 P1 C34B 34.7(3) . . . . ? S1 Rh1 P1 C34B 126.3(3) . . . . ? S2 Rh1 P1 C34B -159.8(3) . . . . ? C1 Rh1 P1 C22 144.80(13) . . . . ? S1 Rh1 P1 C22 -123.63(16) . . . . ? S2 Rh1 P1 C22 -49.70(9) . . . . ? C1 Rh1 P1 C34A 19.6(2) . . . . ? S1 Rh1 P1 C34A 111.1(2) . . . . ? S2 Rh1 P1 C34A -174.94(19) . . . . ? C1 Rh1 S1 C3 -132.73(13) . . . . ? P1 Rh1 S1 C3 135.51(16) . . . . ? S2 Rh1 S1 C3 62.04(9) . . . . ? C1 Rh1 S2 C8 171.3(3) . . . . ? P1 Rh1 S2 C8 92.17(10) . . . . ? S1 Rh1 S2 C8 -98.37(10) . . . . ? C3 N1 N2 C4 -1.0(3) . . . . ? B1 N1 N2 C4 -177.9(2) . . . . ? C8 N4 N5 C9 0.7(3) . . . . ? B1 N4 N5 C9 179.3(2) . . . . ? C13 N7 N8 C15 0.2(3) . . . . ? B1 N7 N8 C15 -176.2(2) . . . . ? C13 N7 B1 N1 32.5(4) . . . . ? N8 N7 B1 N1 -152.0(2) . . . . ? C13 N7 B1 N4 -88.9(3) . . . . ? N8 N7 B1 N4 86.6(3) . . . . ? C3 N1 B1 N7 133.7(3) . . . . ? N2 N1 B1 N7 -50.1(3) . . . . ? C3 N1 B1 N4 -103.4(3) . . . . ? N2 N1 B1 N4 72.7(3) . . . . ? C8 N4 B1 N7 -159.6(2) . . . . ? N5 N4 B1 N7 22.0(3) . . . . ? C8 N4 B1 N1 76.3(3) . . . . ? N5 N4 B1 N1 -102.1(3) . . . . ? N2 N1 C3 N3 0.2(3) . . . . ? B1 N1 C3 N3 176.7(2) . . . . ? N2 N1 C3 S1 179.88(19) . . . . ? B1 N1 C3 S1 -3.7(4) . . . . ? C4 N3 C3 N1 0.6(3) . . . . ? C6 N3 C3 N1 -178.8(2) . . . . ? C4 N3 C3 S1 -179.10(18) . . . . ? C6 N3 C3 S1 1.5(4) . . . . ? Rh1 S1 C3 N1 13.5(3) . . . . ? Rh1 S1 C3 N3 -166.89(18) . . . . ? N1 N2 C4 N3 1.4(3) . . . . ? N1 N2 C4 C5 179.6(2) . . . . ? C3 N3 C4 N2 -1.3(3) . . . . ? C6 N3 C4 N2 178.1(2) . . . . ? C3 N3 C4 C5 -179.5(2) . . . . ? C6 N3 C4 C5 -0.1(4) . . . . ? C3 N3 C6 C7 -90.0(3) . . . . ? C4 N3 C6 C7 90.7(3) . . . . ? N5 N4 C8 N6 -0.9(3) . . . . ? B1 N4 C8 N6 -179.4(2) . . . . ? N5 N4 C8 S2 177.98(19) . . . . ? B1 N4 C8 S2 -0.6(4) . . . . ? C9 N6 C8 N4 0.7(3) . . . . ? C11 N6 C8 N4 -178.5(2) . . . . ? C9 N6 C8 S2 -178.2(2) . . . . ? C11 N6 C8 S2 2.6(4) . . . . ? Rh1 S2 C8 N4 26.3(3) . . . . ? Rh1 S2 C8 N6 -155.04(19) . . . . ? N4 N5 C9 N6 -0.2(3) . . . . ? N4 N5 C9 C10 179.2(2) . . . . ? C8 N6 C9 N5 -0.3(3) . . . . ? C11 N6 C9 N5 178.8(2) . . . . ? C8 N6 C9 C10 -179.7(2) . . . . ? C11 N6 C9 C10 -0.6(4) . . . . ? C9 N6 C11 C12 100.0(3) . . . . ? C8 N6 C11 C12 -81.0(3) . . . . ? N8 N7 C13 C14 0.7(3) . . . . ? B1 N7 C13 C14 176.4(2) . . . . ? N7 C13 C14 C15 -1.2(3) . . . . ? N7 N8 C15 C14 -1.0(3) . . . . ? N7 N8 C15 C16 -179.2(2) . . . . ? C13 C14 C15 N8 1.4(3) . . . . ? C13 C14 C15 C16 179.4(2) . . . . ? N8 C15 C16 C17 179.3(2) . . . . ? C14 C15 C16 C17 1.5(4) . . . . ? N8 C15 C16 C21 -1.3(4) . . . . ? C14 C15 C16 C21 -179.1(2) . . . . ? C21 C16 C17 C18 1.7(4) . . . . ? C15 C16 C17 C18 -178.9(2) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 1.1(5) . . . . ? C19 C20 C21 C16 -0.6(4) . . . . ? C17 C16 C21 C20 -0.8(4) . . . . ? C15 C16 C21 C20 179.8(3) . . . . ? C28 P1 C22 C27 -174.4(2) . . . . ? C34B P1 C22 C27 70.2(3) . . . . ? C34A P1 C22 C27 80.5(3) . . . . ? Rh1 P1 C22 C27 -51.2(2) . . . . ? C28 P1 C22 C23 -0.2(3) . . . . ? C34B P1 C22 C23 -115.5(3) . . . . ? C34A P1 C22 C23 -105.3(3) . . . . ? Rh1 P1 C22 C23 123.0(2) . . . . ? C27 C22 C23 C24 -1.0(4) . . . . ? P1 C22 C23 C24 -175.2(2) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C23 C24 C25 C26 1.3(4) . . . . ? C24 C25 C26 C27 -0.5(4) . . . . ? C23 C22 C27 C26 1.8(4) . . . . ? P1 C22 C27 C26 176.4(2) . . . . ? C25 C26 C27 C22 -1.1(4) . . . . ? C34B P1 C28 C29 -126.5(3) . . . . ? C22 P1 C28 C29 128.2(2) . . . . ? C34A P1 C28 C29 -121.1(2) . . . . ? Rh1 P1 C28 C29 5.2(2) . . . . ? C34B P1 C28 C33 51.5(3) . . . . ? C22 P1 C28 C33 -53.8(2) . . . . ? C34A P1 C28 C33 57.0(3) . . . . ? Rh1 P1 C28 C33 -176.7(2) . . . . ? C33 C28 C29 C30 0.4(4) . . . . ? P1 C28 C29 C30 178.55(19) . . . . ? C28 C29 C30 C31 0.1(4) . . . . ? C29 C30 C31 C32 -0.1(4) . . . . ? C30 C31 C32 C33 -0.5(4) . . . . ? C28 P1 C34A C35A -149.6(3) . . . . ? C34B P1 C34A C35A 8.7(12) . . . . ? C22 P1 C34A C35A -38.7(3) . . . . ? Rh1 P1 C34A C35A 88.9(3) . . . . ? C28 P1 C34A C39A 32.6(3) . . . . ? C34B P1 C34A C39A -169.0(14) . . . . ? C22 P1 C34A C39A 143.6(3) . . . . ? Rh1 P1 C34A C39A -88.8(4) . . . . ? C39A C34A C35A C36A 0.0 . . . . ? P1 C34A C35A C36A -177.8(3) . . . . ? C34A C35A C36A C37A 0.0 . . . . ? C35A C36A C37A C38A 0.0 . . . . ? C36A C37A C38A C39A 0.0 . . . . ? C37A C38A C39A C34A 0.0 . . . . ? C35A C34A C39A C38A 0.0 . . . . ? P1 C34A C39A C38A 177.7(3) . . . . ? C31 C32 C33 C28 1.0(4) . . . . ? C29 C28 C33 C32 -1.0(4) . . . . ? P1 C28 C33 C32 -179.0(2) . . . . ? C28 P1 C34B C35B -173.0(4) . . . . ? C22 P1 C34B C35B -61.4(4) . . . . ? C34A P1 C34B C35B 163.9(15) . . . . ? Rh1 P1 C34B C35B 57.1(5) . . . . ? C28 P1 C34B C39B 8.4(5) . . . . ? C22 P1 C34B C39B 120.1(4) . . . . ? C34A P1 C34B C39B -14.6(11) . . . . ? Rh1 P1 C34B C39B -121.5(4) . . . . ? C39B C34B C35B C36B 0.0 . . . . ? P1 C34B C35B C36B -178.5(5) . . . . ? C34B C35B C36B C37B 0.0 . . . . ? C35B C36B C37B C38B 0.0 . . . . ? C36B C37B C38B C39B 0.0 . . . . ? C37B C38B C39B C34B 0.0 . . . . ? C35B C34B C39B C38B 0.0 . . . . ? P1 C34B C39B C38B 178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.687 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.084 data_23 _database_code_depnum_ccdc_archive 'CCDC 792574' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H55 B2 Cl8 N16 Rh1 S4' _chemical_formula_weight 1224.34 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' 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 P2(1)/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 20.179(4) _cell_length_b 15.811(3) _cell_length_c 17.133(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.57(3) _cell_angle_gamma 90.00 _cell_volume 5418.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49779 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.1899 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _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 1.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11043 _reflns_number_gt 6226 _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^)+(0.0586P)^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 11043 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.74260(2) 0.93997(3) 0.37421(3) 0.01280(12) Uani 1 1 d . . . B1 B 0.7345(3) 0.9422(4) 0.2487(4) 0.0150(13) Uani 1 1 d . . . N1 N 0.7519(2) 1.0253(3) 0.2073(3) 0.0143(10) Uani 1 1 d . . . N2 N 0.8189(3) 1.0420(3) 0.2062(3) 0.0170(11) Uani 1 1 d . . . C1 C 0.8211(3) 1.1190(4) 0.1758(4) 0.0220(14) Uani 1 1 d . . . C2 C 0.7577(4) 1.1501(4) 0.1551(4) 0.0252(15) Uani 1 1 d . . . H2 H 0.7466 1.2016 0.1306 0.030 Uiso 1 1 calc R . . C3 C 0.7135(3) 1.0912(4) 0.1771(4) 0.0208(14) Uani 1 1 d . . . C4 C 0.8864(4) 1.1613(4) 0.1693(4) 0.0335(18) Uani 1 1 d . . . H4A H 0.9036 1.1860 0.2191 0.050 Uiso 1 1 calc R . . H4B H 0.8800 1.2048 0.1299 0.050 Uiso 1 1 calc R . . H4C H 0.9177 1.1204 0.1548 0.050 Uiso 1 1 calc R . . C5 C 0.6398(3) 1.0975(4) 0.1745(4) 0.0286(16) Uani 1 1 d . . . H5A H 0.6184 1.0629 0.1325 0.043 Uiso 1 1 calc R . . H5B H 0.6262 1.1553 0.1657 0.043 Uiso 1 1 calc R . . H5C H 0.6272 1.0784 0.2237 0.043 Uiso 1 1 calc R . . N3 N 0.7794(2) 0.8710(3) 0.2252(3) 0.0146(10) Uani 1 1 d . . . N4 N 0.7976(3) 0.8566(3) 0.1504(3) 0.0189(11) Uani 1 1 d . . . C6 C 0.8215(3) 0.7810(4) 0.1528(3) 0.0167(12) Uani 1 1 d . . . N5 N 0.8205(3) 0.7448(3) 0.2251(3) 0.0227(12) Uani 1 1 d . . . C7 C 0.7914(3) 0.8023(4) 0.2694(4) 0.0175(13) Uani 1 1 d . . . C8 C 0.8509(5) 0.6623(4) 0.2545(5) 0.042(2) Uani 1 1 d . . . H8A H 0.8912 0.6524 0.2306 0.051 Uiso 1 1 calc R . . H8B H 0.8635 0.6658 0.3111 0.051 Uiso 1 1 calc R . . C9 C 0.8058(5) 0.5925(6) 0.2368(5) 0.053(2) Uani 1 1 d . . . H9A H 0.7665 0.6012 0.2617 0.079 Uiso 1 1 calc R . . H9B H 0.8274 0.5410 0.2559 0.079 Uiso 1 1 calc R . . H9C H 0.7935 0.5886 0.1808 0.079 Uiso 1 1 calc R . . C10 C 0.8488(4) 0.7388(4) 0.0861(4) 0.0300(16) Uani 1 1 d . . . H10A H 0.8416 0.7742 0.0403 0.045 Uiso 1 1 calc R . . H10B H 0.8266 0.6856 0.0751 0.045 Uiso 1 1 calc R . . H10C H 0.8959 0.7293 0.1001 0.045 Uiso 1 1 calc R . . S1 S 0.77227(8) 0.79621(9) 0.36332(9) 0.0177(3) Uani 1 1 d . . . N6 N 0.6616(3) 0.9164(3) 0.2177(3) 0.0179(11) Uani 1 1 d . . . N7 N 0.6377(3) 0.9015(3) 0.1385(3) 0.0201(11) Uani 1 1 d . . . C11 C 0.5750(3) 0.8835(4) 0.1393(4) 0.0229(14) Uani 1 1 d . . . N8 N 0.5577(2) 0.8860(3) 0.2142(3) 0.0179(11) Uani 1 1 d . . . C12 C 0.6139(3) 0.9055(4) 0.2618(4) 0.0183(13) Uani 1 1 d . . . C13 C 0.4913(3) 0.8717(4) 0.2385(4) 0.0256(15) Uani 1 1 d . . . H13A H 0.4966 0.8457 0.2903 0.031 Uiso 1 1 calc R . . H13B H 0.4663 0.8328 0.2019 0.031 Uiso 1 1 calc R . . C14 C 0.4522(4) 0.9536(5) 0.2409(5) 0.0365(18) Uani 1 1 d . . . H14A H 0.4794 0.9949 0.2711 0.055 Uiso 1 1 calc R . . H14B H 0.4126 0.9434 0.2650 0.055 Uiso 1 1 calc R . . H14C H 0.4399 0.9741 0.1883 0.055 Uiso 1 1 calc R . . C15 C 0.5268(4) 0.8646(5) 0.0676(4) 0.0319(17) Uani 1 1 d . . . H15A H 0.5492 0.8685 0.0217 0.048 Uiso 1 1 calc R . . H15B H 0.4907 0.9046 0.0635 0.048 Uiso 1 1 calc R . . H15C H 0.5094 0.8084 0.0714 0.048 Uiso 1 1 calc R . . S2 S 0.62595(8) 0.91299(10) 0.36197(9) 0.0186(3) Uani 1 1 d . . . B2 B 0.8235(4) 1.0546(4) 0.5518(4) 0.0187(14) Uani 1 1 d . . . H2A H 0.8362 1.0799 0.6038 0.022 Uiso 1 1 calc R . . N9 N 0.7461(3) 0.9281(3) 0.5203(3) 0.0220(12) Uani 1 1 d . . . N10 N 0.7569(3) 1.0067(3) 0.5533(3) 0.0196(11) Uani 1 1 d . . . C16 C 0.7074(4) 1.0272(5) 0.5921(5) 0.0355(18) Uani 1 1 d . . . C17 C 0.6639(4) 0.9581(5) 0.5885(5) 0.0366(18) Uani 1 1 d . . . H17 H 0.6245 0.9536 0.6108 0.044 Uiso 1 1 calc R . . C18 C 0.6914(3) 0.8994(4) 0.5457(4) 0.0193(13) Uani 1 1 d . . . C19 C 0.7043(5) 1.1108(5) 0.6327(6) 0.056(3) Uani 1 1 d . . . H19A H 0.7352 1.1108 0.6804 0.083 Uiso 1 1 calc R . . H19B H 0.6598 1.1200 0.6452 0.083 Uiso 1 1 calc R . . H19C H 0.7159 1.1551 0.5987 0.083 Uiso 1 1 calc R . . C20 C 0.6682(3) 0.8093(4) 0.5283(4) 0.0240(14) Uani 1 1 d . . . H20A H 0.6904 0.7866 0.4867 0.036 Uiso 1 1 calc R . . H20B H 0.6207 0.8088 0.5125 0.036 Uiso 1 1 calc R . . H20C H 0.6787 0.7754 0.5748 0.036 Uiso 1 1 calc R . . N11 N 0.8162(2) 1.1274(3) 0.4895(3) 0.0163(11) Uani 1 1 d . . . N12 N 0.8586(3) 1.1980(3) 0.5069(3) 0.0186(11) Uani 1 1 d . . . C21 C 0.8397(3) 1.2522(4) 0.4519(3) 0.0189(13) Uani 1 1 d . . . N13 N 0.7875(3) 1.2213(3) 0.4007(3) 0.0177(11) Uani 1 1 d . . . C22 C 0.7742(3) 1.1418(4) 0.4260(4) 0.0171(13) Uani 1 1 d . . . C23 C 0.8720(4) 1.3365(4) 0.4430(5) 0.0319(17) Uani 1 1 d . . . H23A H 0.9031 1.3483 0.4891 0.048 Uiso 1 1 calc R . . H23B H 0.8382 1.3797 0.4365 0.048 Uiso 1 1 calc R . . H23C H 0.8952 1.3355 0.3976 0.048 Uiso 1 1 calc R . . C24 C 0.7520(3) 1.2640(4) 0.3315(4) 0.0277(16) Uani 1 1 d . . . H24A H 0.7428 1.2235 0.2889 0.033 Uiso 1 1 calc R . . H24B H 0.7804 1.3079 0.3144 0.033 Uiso 1 1 calc R . . C25 C 0.6885(5) 1.3020(6) 0.3482(5) 0.054(2) Uani 1 1 d . . . H25A H 0.6636 1.2610 0.3738 0.081 Uiso 1 1 calc R . . H25B H 0.6628 1.3195 0.2998 0.081 Uiso 1 1 calc R . . H25C H 0.6978 1.3501 0.3820 0.081 Uiso 1 1 calc R . . S3 S 0.70958(8) 1.08157(9) 0.37931(9) 0.0186(3) Uani 1 1 d . . . N14 N 0.8791(3) 0.9921(3) 0.5361(3) 0.0165(11) Uani 1 1 d . . . N15 N 0.9236(3) 0.9642(3) 0.6006(3) 0.0195(11) Uani 1 1 d . . . C26 C 0.9635(3) 0.9146(4) 0.5712(4) 0.0172(13) Uani 1 1 d . . . N16 N 0.9491(2) 0.9081(3) 0.4914(3) 0.0160(10) Uani 1 1 d . . . C27 C 0.8931(3) 0.9578(3) 0.4705(3) 0.0145(12) Uani 1 1 d . . . C28 C 0.9832(3) 0.8576(4) 0.4368(4) 0.0193(13) Uani 1 1 d . . . H28A H 1.0311 0.8627 0.4513 0.023 Uiso 1 1 calc R . . H28B H 0.9722 0.8800 0.3840 0.023 Uiso 1 1 calc R . . C29 C 0.9643(3) 0.7658(4) 0.4368(4) 0.0265(15) Uani 1 1 d . . . H29A H 0.9803 0.7414 0.4871 0.040 Uiso 1 1 calc R . . H29B H 0.9840 0.7368 0.3964 0.040 Uiso 1 1 calc R . . H29C H 0.9165 0.7606 0.4270 0.040 Uiso 1 1 calc R . . C30 C 1.0195(3) 0.8686(4) 0.6183(4) 0.0228(14) Uani 1 1 d . . . H30A H 1.0182 0.8786 0.6733 0.034 Uiso 1 1 calc R . . H30B H 1.0613 0.8885 0.6041 0.034 Uiso 1 1 calc R . . H30C H 1.0152 0.8091 0.6077 0.034 Uiso 1 1 calc R . . S4 S 0.85656(7) 0.97372(9) 0.37522(8) 0.0148(3) Uani 1 1 d . . . C100 C 0.7312(4) 0.9758(5) 1.0128(4) 0.0395(19) Uani 1 1 d . . . H10D H 0.7535 1.0216 1.0433 0.047 Uiso 1 1 calc R . . H10E H 0.7257 0.9293 1.0483 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.77991(14) 0.94296(15) 0.94180(13) 0.0575(6) Uani 1 1 d . . . Cl2 Cl 0.65034(13) 1.01094(15) 0.96689(14) 0.0604(7) Uani 1 1 d . . . C200 C 0.4351(5) 0.8995(6) 0.5364(6) 0.056(3) Uani 1 1 d . . . H20D H 0.3913 0.8737 0.5250 0.067 Uiso 1 1 calc R . . H20E H 0.4290 0.9602 0.5400 0.067 Uiso 1 1 calc R . . Cl3 Cl 0.48105(15) 0.8776(2) 0.46175(16) 0.0810(9) Uani 1 1 d . . . Cl4 Cl 0.47513(11) 0.86092(14) 0.62720(14) 0.0520(6) Uani 1 1 d . . . C300 C 0.3822(4) 0.1814(5) 0.1634(4) 0.0362(18) Uani 1 1 d . . . H30D H 0.3650 0.2332 0.1378 0.043 Uiso 1 1 calc R . . H30E H 0.3564 0.1346 0.1387 0.043 Uiso 1 1 calc R . . Cl5 Cl 0.46781(10) 0.16871(13) 0.15010(12) 0.0413(5) Uani 1 1 d . . . Cl6 Cl 0.37234(11) 0.18543(14) 0.26327(12) 0.0460(5) Uani 1 1 d . . . C400 C 0.9677(5) 0.9425(5) 0.2077(6) 0.059(3) Uani 1 1 d . . . H40A H 0.9196 0.9498 0.2026 0.071 Uiso 1 1 calc R . . H40B H 0.9875 0.9755 0.2525 0.071 Uiso 1 1 calc R . . Cl7 Cl 0.98715(11) 0.83584(12) 0.22404(12) 0.0412(5) Uani 1 1 d . . . Cl8 Cl 0.9966(3) 0.9787(3) 0.1241(4) 0.229(4) 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 0.0109(2) 0.0098(2) 0.0176(2) -0.00082(18) 0.00110(16) -0.00045(18) B1 0.013(3) 0.008(3) 0.023(3) 0.001(3) 0.002(3) 0.000(3) N1 0.015(2) 0.010(2) 0.018(3) 0.0004(19) 0.004(2) 0.003(2) N2 0.020(3) 0.013(3) 0.017(2) 0.0017(19) -0.001(2) -0.004(2) C1 0.031(4) 0.015(3) 0.018(3) 0.001(2) -0.002(3) 0.002(3) C2 0.039(4) 0.014(3) 0.022(3) 0.006(3) -0.001(3) 0.004(3) C3 0.028(4) 0.013(3) 0.021(3) -0.003(2) -0.001(3) 0.006(3) C4 0.031(4) 0.023(4) 0.043(4) 0.017(3) -0.004(3) -0.007(3) C5 0.025(4) 0.020(3) 0.038(4) 0.001(3) -0.006(3) 0.011(3) N3 0.016(3) 0.010(2) 0.017(2) 0.0009(19) 0.003(2) 0.000(2) N4 0.021(3) 0.018(3) 0.019(3) 0.000(2) 0.006(2) 0.000(2) C6 0.019(3) 0.010(3) 0.022(3) -0.003(2) 0.003(3) 0.001(2) N5 0.030(3) 0.014(3) 0.025(3) -0.004(2) 0.008(2) 0.007(2) C7 0.017(3) 0.009(3) 0.027(3) 0.000(2) 0.003(3) 0.001(2) C8 0.076(6) 0.014(3) 0.040(4) 0.001(3) 0.018(4) 0.011(4) C9 0.055(6) 0.055(6) 0.049(5) -0.002(4) 0.006(4) 0.000(5) C10 0.037(4) 0.023(4) 0.031(4) -0.003(3) 0.009(3) 0.005(3) S1 0.0217(8) 0.0109(7) 0.0206(8) 0.0019(6) 0.0031(6) 0.0001(6) N6 0.020(3) 0.012(2) 0.021(3) 0.001(2) 0.002(2) 0.000(2) N7 0.020(3) 0.015(3) 0.024(3) -0.002(2) -0.002(2) 0.000(2) C11 0.026(4) 0.010(3) 0.030(4) 0.000(2) -0.005(3) 0.001(3) N8 0.014(3) 0.018(3) 0.022(3) -0.001(2) 0.000(2) -0.001(2) C12 0.020(3) 0.010(3) 0.025(3) 0.002(2) 0.002(3) 0.004(2) C13 0.010(3) 0.027(4) 0.038(4) 0.000(3) -0.001(3) -0.004(3) C14 0.020(4) 0.032(4) 0.057(5) -0.011(3) 0.003(3) -0.001(3) C15 0.029(4) 0.034(4) 0.031(4) -0.009(3) -0.004(3) -0.005(3) S2 0.0142(7) 0.0197(8) 0.0222(8) -0.0021(6) 0.0031(6) -0.0024(6) B2 0.024(4) 0.012(3) 0.021(3) -0.003(3) 0.002(3) 0.000(3) N9 0.026(3) 0.017(3) 0.022(3) -0.002(2) 0.001(2) -0.004(2) N10 0.026(3) 0.011(2) 0.023(3) -0.001(2) 0.008(2) 0.004(2) C16 0.042(5) 0.021(4) 0.046(5) -0.004(3) 0.017(4) -0.007(3) C17 0.034(4) 0.030(4) 0.050(5) 0.000(3) 0.022(4) -0.007(3) C18 0.022(3) 0.015(3) 0.021(3) 0.003(2) 0.006(3) 0.001(3) C19 0.062(6) 0.029(5) 0.082(7) -0.022(4) 0.033(5) -0.005(4) C20 0.025(4) 0.017(3) 0.031(4) 0.004(3) 0.006(3) -0.005(3) N11 0.017(3) 0.011(2) 0.021(3) -0.0034(19) 0.003(2) -0.001(2) N12 0.016(3) 0.013(2) 0.026(3) -0.004(2) 0.001(2) -0.002(2) C21 0.021(3) 0.012(3) 0.023(3) -0.005(2) 0.001(3) -0.003(3) N13 0.019(3) 0.010(2) 0.024(3) 0.000(2) 0.001(2) 0.003(2) C22 0.017(3) 0.010(3) 0.025(3) -0.006(2) 0.006(3) 0.002(2) C23 0.033(4) 0.013(3) 0.049(4) 0.005(3) 0.002(3) -0.005(3) C24 0.030(4) 0.018(3) 0.031(4) 0.007(3) -0.008(3) 0.005(3) C25 0.059(6) 0.042(5) 0.057(6) 0.014(4) -0.003(5) 0.026(5) S3 0.0150(7) 0.0136(7) 0.0259(8) -0.0036(6) -0.0017(6) 0.0021(6) N14 0.019(3) 0.011(2) 0.018(3) -0.0005(19) -0.002(2) -0.003(2) N15 0.018(3) 0.015(3) 0.023(3) 0.006(2) -0.006(2) -0.004(2) C26 0.015(3) 0.011(3) 0.025(3) 0.001(2) -0.001(3) -0.006(2) N16 0.011(2) 0.014(2) 0.023(3) 0.004(2) -0.003(2) -0.001(2) C27 0.012(3) 0.009(3) 0.022(3) 0.001(2) -0.001(2) -0.003(2) C28 0.012(3) 0.023(3) 0.022(3) 0.003(3) 0.003(2) 0.005(3) C29 0.024(3) 0.025(4) 0.032(4) -0.001(3) 0.005(3) -0.002(3) C30 0.020(3) 0.021(3) 0.026(3) 0.007(3) -0.004(3) -0.005(3) S4 0.0129(7) 0.0139(7) 0.0171(7) 0.0011(6) 0.0006(6) -0.0004(6) C100 0.043(5) 0.044(5) 0.029(4) 0.005(3) -0.001(4) 0.002(4) Cl1 0.0845(18) 0.0493(13) 0.0434(12) -0.0146(10) 0.0262(12) -0.0063(12) Cl2 0.0685(16) 0.0576(15) 0.0503(13) 0.0215(11) -0.0103(12) 0.0084(12) C200 0.065(6) 0.039(5) 0.070(6) 0.000(4) 0.029(5) 0.017(5) Cl3 0.0675(18) 0.120(3) 0.0608(16) 0.0033(15) 0.0286(14) 0.0427(17) Cl4 0.0445(13) 0.0444(12) 0.0636(14) -0.0066(10) -0.0054(11) 0.0085(10) C300 0.042(5) 0.031(4) 0.034(4) 0.004(3) 0.000(4) 0.008(3) Cl5 0.0383(11) 0.0435(11) 0.0432(11) -0.0030(9) 0.0098(9) 0.0028(9) Cl6 0.0478(13) 0.0541(13) 0.0375(11) 0.0158(9) 0.0113(9) 0.0051(10) C400 0.063(6) 0.030(4) 0.095(7) 0.011(5) 0.051(6) 0.024(4) Cl7 0.0491(12) 0.0277(9) 0.0468(11) -0.0086(8) 0.0065(9) 0.0050(9) Cl8 0.320(7) 0.158(4) 0.268(6) 0.159(4) 0.261(6) 0.182(5) _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 2.136(7) . ? Rh1 S3 2.3408(16) . ? Rh1 S4 2.3586(16) . ? Rh1 S1 2.3641(16) . ? Rh1 S2 2.3741(16) . ? Rh1 N9 2.501(5) . ? B1 N3 1.531(8) . ? B1 N6 1.551(8) . ? B1 N1 1.555(8) . ? N1 C3 1.360(7) . ? N1 N2 1.380(7) . ? N2 C1 1.327(7) . ? C1 C2 1.373(9) . ? C1 C4 1.497(10) . ? C2 C3 1.376(10) . ? C2 H2 0.9300 . ? C3 C5 1.486(9) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? N3 C7 1.329(7) . ? N3 N4 1.397(7) . ? N4 C6 1.286(8) . ? C6 N5 1.368(8) . ? C6 C10 1.491(9) . ? N5 C7 1.366(8) . ? N5 C8 1.499(9) . ? C7 S1 1.706(7) . ? C8 C9 1.438(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? N6 C12 1.312(8) . ? N6 N7 1.399(7) . ? N7 C11 1.297(8) . ? C11 N8 1.375(8) . ? C11 C15 1.494(9) . ? N8 C12 1.342(8) . ? N8 C13 1.472(8) . ? C12 S2 1.706(6) . ? C13 C14 1.520(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? B2 N10 1.545(9) . ? B2 N14 1.546(9) . ? B2 N11 1.564(8) . ? B2 H2A 0.9800 . ? N9 C18 1.318(8) . ? N9 N10 1.371(7) . ? N10 C16 1.313(9) . ? C16 C17 1.397(10) . ? C16 C19 1.498(10) . ? C17 C18 1.346(10) . ? C17 H17 0.9300 . ? C18 C20 1.517(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N11 C22 1.308(8) . ? N11 N12 1.415(7) . ? N12 C21 1.293(8) . ? C21 N13 1.370(7) . ? C21 C23 1.501(9) . ? N13 C22 1.368(8) . ? N13 C24 1.466(7) . ? C22 S3 1.723(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.477(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? N14 C27 1.310(8) . ? N14 N15 1.401(7) . ? N15 C26 1.274(8) . ? C26 N16 1.363(8) . ? C26 C30 1.488(8) . ? N16 C27 1.385(7) . ? N16 C28 1.469(8) . ? C27 S4 1.719(6) . ? C28 C29 1.500(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C100 Cl1 1.740(8) . ? C100 Cl2 1.803(8) . ? C100 H10D 0.9700 . ? C100 H10E 0.9700 . ? C200 Cl3 1.712(9) . ? C200 Cl4 1.764(10) . ? C200 H20D 0.9700 . ? C200 H20E 0.9700 . ? C300 Cl6 1.750(8) . ? C300 Cl5 1.784(8) . ? C300 H30D 0.9700 . ? C300 H30E 0.9700 . ? C400 Cl8 1.715(10) . ? C400 Cl7 1.745(8) . ? C400 H40A 0.9700 . ? C400 H40B 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 B1 Rh1 S3 92.16(18) . . ? B1 Rh1 S4 87.07(19) . . ? S3 Rh1 S4 93.75(6) . . ? B1 Rh1 S1 85.57(18) . . ? S3 Rh1 S1 177.20(6) . . ? S4 Rh1 S1 87.78(5) . . ? B1 Rh1 S2 88.31(19) . . ? S3 Rh1 S2 83.76(6) . . ? S4 Rh1 S2 174.67(6) . . ? S1 Rh1 S2 94.52(6) . . ? B1 Rh1 N9 175.7(2) . . ? S3 Rh1 N9 90.27(13) . . ? S4 Rh1 N9 96.37(14) . . ? S1 Rh1 N9 91.89(12) . . ? S2 Rh1 N9 88.37(14) . . ? N3 B1 N6 106.5(5) . . ? N3 B1 N1 108.9(5) . . ? N6 B1 N1 109.1(5) . . ? N3 B1 Rh1 106.5(4) . . ? N6 B1 Rh1 106.5(4) . . ? N1 B1 Rh1 118.8(4) . . ? C3 N1 N2 111.0(5) . . ? C3 N1 B1 132.0(5) . . ? N2 N1 B1 116.7(4) . . ? C1 N2 N1 105.3(5) . . ? N2 C1 C2 110.7(6) . . ? N2 C1 C4 121.0(6) . . ? C2 C1 C4 128.3(6) . . ? C1 C2 C3 107.5(5) . . ? C1 C2 H2 126.2 . . ? C3 C2 H2 126.2 . . ? N1 C3 C2 105.4(6) . . ? N1 C3 C5 125.6(6) . . ? C2 C3 C5 129.0(6) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N3 N4 109.8(5) . . ? C7 N3 B1 121.4(5) . . ? N4 N3 B1 126.7(5) . . ? C6 N4 N3 105.4(5) . . ? N4 C6 N5 111.6(5) . . ? N4 C6 C10 124.5(6) . . ? N5 C6 C10 123.9(5) . . ? C7 N5 C6 106.4(5) . . ? C7 N5 C8 125.4(5) . . ? C6 N5 C8 127.9(5) . . ? N3 C7 N5 106.7(5) . . ? N3 C7 S1 122.5(5) . . ? N5 C7 S1 130.8(5) . . ? C9 C8 N5 112.1(7) . . ? C9 C8 H8A 109.2 . . ? N5 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? N5 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? 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 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 S1 Rh1 96.4(2) . . ? C12 N6 N7 110.5(5) . . ? C12 N6 B1 124.9(5) . . ? N7 N6 B1 124.6(5) . . ? C11 N7 N6 103.8(5) . . ? N7 C11 N8 111.8(5) . . ? N7 C11 C15 124.5(6) . . ? N8 C11 C15 123.7(6) . . ? C12 N8 C11 106.0(5) . . ? C12 N8 C13 126.2(5) . . ? C11 N8 C13 127.8(5) . . ? N6 C12 N8 107.8(5) . . ? N6 C12 S2 123.5(5) . . ? N8 C12 S2 128.6(5) . . ? N8 C13 C14 111.9(6) . . ? N8 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N8 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? 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 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 S2 Rh1 96.3(2) . . ? N10 B2 N14 110.1(5) . . ? N10 B2 N11 111.6(5) . . ? N14 B2 N11 110.9(5) . . ? N10 B2 H2A 108.1 . . ? N14 B2 H2A 108.1 . . ? N11 B2 H2A 108.1 . . ? C18 N9 N10 105.7(5) . . ? C18 N9 Rh1 116.2(4) . . ? N10 N9 Rh1 109.1(4) . . ? C16 N10 N9 110.0(5) . . ? C16 N10 B2 127.5(5) . . ? N9 N10 B2 122.0(5) . . ? N10 C16 C17 107.4(6) . . ? N10 C16 C19 122.3(7) . . ? C17 C16 C19 130.3(8) . . ? C18 C17 C16 105.2(7) . . ? C18 C17 H17 127.4 . . ? C16 C17 H17 127.4 . . ? N9 C18 C17 111.4(6) . . ? N9 C18 C20 120.6(6) . . ? C17 C18 C20 128.0(6) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 N11 N12 110.2(5) . . ? C22 N11 B2 133.5(5) . . ? N12 N11 B2 115.9(5) . . ? C21 N12 N11 104.9(5) . . ? N12 C21 N13 111.1(5) . . ? N12 C21 C23 125.0(5) . . ? N13 C21 C23 123.9(5) . . ? C22 N13 C21 106.9(5) . . ? C22 N13 C24 125.7(5) . . ? C21 N13 C24 127.4(5) . . ? N11 C22 N13 106.9(5) . . ? N11 C22 S3 131.1(5) . . ? N13 C22 S3 122.0(4) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N13 C24 C25 112.0(6) . . ? N13 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N13 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? 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 . . ? C22 S3 Rh1 110.1(2) . . ? C27 N14 N15 111.0(5) . . ? C27 N14 B2 131.1(5) . . ? N15 N14 B2 117.9(5) . . ? C26 N15 N14 104.8(5) . . ? N15 C26 N16 112.3(5) . . ? N15 C26 C30 124.1(6) . . ? N16 C26 C30 123.6(6) . . ? C26 N16 C27 106.0(5) . . ? C26 N16 C28 128.6(5) . . ? C27 N16 C28 125.4(5) . . ? N14 C27 N16 105.9(5) . . ? N14 C27 S4 129.8(5) . . ? N16 C27 S4 124.2(5) . . ? N16 C28 C29 112.7(5) . . ? N16 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? N16 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 S4 Rh1 105.6(2) . . ? Cl1 C100 Cl2 110.5(4) . . ? Cl1 C100 H10D 109.6 . . ? Cl2 C100 H10D 109.6 . . ? Cl1 C100 H10E 109.6 . . ? Cl2 C100 H10E 109.6 . . ? H10D C100 H10E 108.1 . . ? Cl3 C200 Cl4 111.0(5) . . ? Cl3 C200 H20D 109.4 . . ? Cl4 C200 H20D 109.4 . . ? Cl3 C200 H20E 109.4 . . ? Cl4 C200 H20E 109.4 . . ? H20D C200 H20E 108.0 . . ? Cl6 C300 Cl5 111.4(4) . . ? Cl6 C300 H30D 109.3 . . ? Cl5 C300 H30D 109.3 . . ? Cl6 C300 H30E 109.3 . . ? Cl5 C300 H30E 109.3 . . ? H30D C300 H30E 108.0 . . ? Cl8 C400 Cl7 111.3(5) . . ? Cl8 C400 H40A 109.4 . . ? Cl7 C400 H40A 109.4 . . ? Cl8 C400 H40B 109.4 . . ? Cl7 C400 H40B 109.4 . . ? H40A C400 H40B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 1.983 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.123