# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Neil Connelly' _publ_contact_author_email NEIL.CONNELLY@BRISTOL.AC.UK _publ_section_title ; Fluxional rhodium scorpionate complexes of the hydrotris(methimazolyl)borate (Tm) ligand and their static boratrane derivatives ; loop_ _publ_author_name 'N Connelly' 'Mairi F. Haddow' 'Alex Hamilton' 'Maria J. Lopez-Gomez' 'A Orpen' # Attachment 'all.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 761317' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 B N6 Rh S3, C H2 Cl2' _chemical_formula_sum 'C21 H30 B Cl2 N6 Rh S3' _chemical_formula_weight 647.31 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' 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.750(2) _cell_length_b 14.571(4) _cell_length_c 22.091(6) _cell_angle_alpha 102.325(10) _cell_angle_beta 90.215(10) _cell_angle_gamma 107.157(10) _cell_volume 2622.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7247 _cell_measurement_theta_min ? _cell_measurement_theta_max 29.985 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS - Bruker 2007' _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 Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 48121 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11979 _reflns_number_gt 8531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _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^)+(0.0887P)^2^+1.2976P] 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 11979 _refine_ls_number_parameters 761 _refine_ls_number_restraints 238 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.122 _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 -0.02581(4) 0.22334(3) 0.484791(17) 0.01833(11) Uani 1 1 d . . . S1 S 0.02769(15) 0.39791(9) 0.53080(6) 0.0239(3) Uani 1 1 d . A . B1A B 0.2359(7) 0.2846(4) 0.5895(3) 0.0258(14) Uani 0.57(3) 1 d P A 1 H1A H 0.1380 0.2362 0.5651 0.031 Uiso 0.57(3) 1 calc PR A 1 B1B B 0.2359(7) 0.2846(4) 0.5895(3) 0.0258(14) Uani 0.43(3) 1 d P A 2 H1B H 0.1442 0.2412 0.5596 0.031 Uiso 0.43(3) 1 calc PR A 2 N1 N 0.1919(5) 0.3726(3) 0.6289(2) 0.0260(10) Uani 1 1 d . . . N2 N 0.1156(6) 0.5052(3) 0.6482(2) 0.0328(11) Uani 1 1 d . . . C2 C 0.1111(6) 0.4233(3) 0.6042(2) 0.0244(11) Uani 1 1 d . A . C3 C 0.2482(7) 0.4241(4) 0.6889(3) 0.0364(15) Uani 1 1 d . A . H3 H 0.3090 0.4050 0.7169 0.044 Uiso 1 1 calc R . . C4 C 0.2016(8) 0.5062(4) 0.7006(3) 0.0407(16) Uani 1 1 d . A . H4 H 0.2242 0.5555 0.7381 0.049 Uiso 1 1 calc R . . C5 C 0.0461(8) 0.5814(4) 0.6387(3) 0.0428(16) Uani 1 1 d . A . H5A H 0.0819 0.6016 0.6002 0.064 Uiso 1 1 calc R . . H5B H 0.0811 0.6385 0.6738 0.064 Uiso 1 1 calc R . . H5C H -0.0711 0.5552 0.6356 0.064 Uiso 1 1 calc R . . S2A S 0.1994(15) 0.2358(9) 0.4297(5) 0.0279(16) Uani 0.57(3) 1 d PU A 1 S3A S 0.0439(12) 0.1793(5) 0.6908(3) 0.0245(12) Uani 0.57(3) 1 d PU A 1 N3A N 0.3733(18) 0.3210(13) 0.5422(7) 0.013(2) Uani 0.57(3) 1 d PU A 1 N4A N 0.4908(18) 0.3693(12) 0.4642(7) 0.019(2) Uani 0.57(3) 1 d PU A 1 N5A N 0.3161(18) 0.2311(18) 0.6292(10) 0.015(3) Uani 0.57(3) 1 d PU A 1 N6A N 0.327(2) 0.1375(10) 0.6915(6) 0.021(3) Uani 0.57(3) 1 d PU A 1 C6A C 0.354(2) 0.3096(16) 0.4805(8) 0.017(2) Uani 0.57(3) 1 d PU A 1 C7A C 0.519(2) 0.3926(15) 0.5638(8) 0.018(3) Uani 0.57(3) 1 d PU A 1 H7A H 0.5582 0.4177 0.6061 0.022 Uiso 0.57(3) 1 calc PR A 1 C8A C 0.593(2) 0.4197(13) 0.5158(8) 0.019(3) Uani 0.57(3) 1 d PU A 1 H8A H 0.6973 0.4650 0.5167 0.023 Uiso 0.57(3) 1 calc PR A 1 C9A C 0.519(3) 0.3728(12) 0.3981(7) 0.040(4) Uani 0.57(3) 1 d PU A 1 H9A1 H 0.5605 0.3189 0.3788 0.060 Uiso 0.57(3) 1 calc PR A 1 H9A2 H 0.5967 0.4360 0.3963 0.060 Uiso 0.57(3) 1 calc PR A 1 H9A3 H 0.4174 0.3658 0.3758 0.060 Uiso 0.57(3) 1 calc PR A 1 C10A C 0.2284(17) 0.1828(11) 0.6696(7) 0.015(2) Uani 0.57(3) 1 d PU A 1 C11A C 0.4589(18) 0.2085(13) 0.6246(7) 0.015(3) Uani 0.57(3) 1 d PU A 1 H11A H 0.5386 0.2298 0.5973 0.018 Uiso 0.57(3) 1 calc PR A 1 C12A C 0.469(2) 0.1530(13) 0.6635(7) 0.023(3) Uani 0.57(3) 1 d PU A 1 H12A H 0.5554 0.1289 0.6706 0.028 Uiso 0.57(3) 1 calc PR A 1 C13A C 0.278(2) 0.0779(10) 0.7385(7) 0.032(3) Uani 0.57(3) 1 d PU A 1 H13A H 0.3555 0.0420 0.7422 0.048 Uiso 0.57(3) 1 calc PR A 1 H13B H 0.1716 0.0308 0.7258 0.048 Uiso 0.57(3) 1 calc PR A 1 H13C H 0.2757 0.1215 0.7787 0.048 Uiso 0.57(3) 1 calc PR A 1 S2B S 0.2241(14) 0.2646(9) 0.4371(7) 0.0214(18) Uani 0.43(3) 1 d PU A 2 S3B S -0.013(2) 0.1820(6) 0.6896(4) 0.0249(18) Uani 0.43(3) 1 d PU A 2 N3B N 0.361(3) 0.3360(16) 0.5582(9) 0.014(3) Uani 0.43(3) 1 d PU A 2 N4B N 0.519(2) 0.3846(14) 0.4866(10) 0.018(3) Uani 0.43(3) 1 d PU A 2 N5B N 0.274(3) 0.230(2) 0.6353(15) 0.019(4) Uani 0.43(3) 1 d PU A 2 N6B N 0.266(3) 0.1343(15) 0.6993(10) 0.023(3) Uani 0.43(3) 1 d PU A 2 C6B C 0.369(3) 0.329(2) 0.4958(11) 0.017(2) Uani 0.43(3) 1 d PU A 2 C7B C 0.512(3) 0.3981(16) 0.5858(10) 0.018(4) Uani 0.43(3) 1 d PU A 2 H7B H 0.5438 0.4154 0.6288 0.022 Uiso 0.43(3) 1 calc PR A 2 C8B C 0.601(3) 0.4282(16) 0.5411(12) 0.023(4) Uani 0.43(3) 1 d PU A 2 H8B H 0.7066 0.4733 0.5472 0.028 Uiso 0.43(3) 1 calc PR A 2 C9B C 0.5714(18) 0.3882(12) 0.4224(10) 0.022(4) Uani 0.43(3) 1 d PU A 2 H9B1 H 0.6638 0.4468 0.4243 0.033 Uiso 0.43(3) 1 calc PR A 2 H9B2 H 0.4831 0.3914 0.3963 0.033 Uiso 0.43(3) 1 calc PR A 2 H9B3 H 0.6016 0.3290 0.4046 0.033 Uiso 0.43(3) 1 calc PR A 2 C10B C 0.172(3) 0.1842(14) 0.6761(9) 0.019(3) Uani 0.43(3) 1 d PU A 2 C11B C 0.419(3) 0.2125(17) 0.6396(11) 0.021(4) Uani 0.43(3) 1 d PU A 2 H11B H 0.5093 0.2397 0.6182 0.026 Uiso 0.43(3) 1 calc PR A 2 C12B C 0.418(3) 0.1530(14) 0.6772(11) 0.023(4) Uani 0.43(3) 1 d PU A 2 H12B H 0.5017 0.1284 0.6869 0.027 Uiso 0.43(3) 1 calc PR A 2 C13B C 0.194(3) 0.0696(13) 0.7411(8) 0.035(5) Uani 0.43(3) 1 d PU A 2 H13D H 0.1010 0.0164 0.7191 0.053 Uiso 0.43(3) 1 calc PR A 2 H13E H 0.1587 0.1080 0.7774 0.053 Uiso 0.43(3) 1 calc PR A 2 H13F H 0.2729 0.0414 0.7547 0.053 Uiso 0.43(3) 1 calc PR A 2 C14 C -0.0915(8) 0.0720(4) 0.4420(3) 0.0399(16) Uani 1 1 d . A . H14 H 0.0014 0.0472 0.4295 0.048 Uiso 1 1 calc R . . C15 C -0.1347(8) 0.1242(4) 0.4010(3) 0.0410(17) Uani 1 1 d . A . H15 H -0.0662 0.1295 0.3651 0.049 Uiso 1 1 calc R . . C16 C -0.3016(8) 0.1274(4) 0.3880(3) 0.0446(18) Uani 1 1 d . . . H16A H -0.2959 0.1812 0.3664 0.054 Uiso 1 1 calc R A . H16B H -0.3638 0.0646 0.3599 0.054 Uiso 1 1 calc R . . C17 C -0.3865(7) 0.1437(4) 0.4460(3) 0.0429(18) Uani 1 1 d . A . H17A H -0.4398 0.0793 0.4561 0.051 Uiso 1 1 calc R . . H17B H -0.4707 0.1739 0.4388 0.051 Uiso 1 1 calc R . . C18 C -0.2725(5) 0.2105(4) 0.5012(3) 0.0254(12) Uani 1 1 d . A . H18 H -0.2939 0.2745 0.5183 0.031 Uiso 1 1 calc R . . C19 C -0.2046(6) 0.1747(4) 0.5445(3) 0.0245(11) Uani 1 1 d . A . H19 H -0.1868 0.2172 0.5875 0.029 Uiso 1 1 calc R . . C20 C -0.2261(7) 0.0671(4) 0.5422(3) 0.0398(16) Uani 1 1 d . . . H20A H -0.3336 0.0370 0.5557 0.048 Uiso 1 1 calc R A . H20B H -0.1453 0.0623 0.5719 0.048 Uiso 1 1 calc R . . C21 C -0.2094(8) 0.0090(4) 0.4776(3) 0.053(2) Uani 1 1 d . A . H21A H -0.1732 -0.0478 0.4817 0.064 Uiso 1 1 calc R . . H21B H -0.3155 -0.0170 0.4540 0.064 Uiso 1 1 calc R . . Rh2 Rh 0.75190(4) 0.28286(3) 0.049349(18) 0.02080(12) Uani 1 1 d . . . S4 S 1.00375(16) 0.26914(11) 0.08718(7) 0.0332(3) Uani 1 1 d . . . S5 S 0.66499(18) 0.12233(10) -0.01328(7) 0.0321(3) Uani 1 1 d . . . S6 S 0.56619(17) 0.24533(10) 0.25671(9) 0.0403(4) Uani 1 1 d . . . N7 N 0.8569(5) 0.1801(3) 0.1787(2) 0.0280(10) Uani 1 1 d . . . N8 N 1.1028(5) 0.2707(4) 0.2041(3) 0.0432(14) Uani 1 1 d . . . N9 N 0.7324(6) 0.0497(3) 0.0857(2) 0.0349(12) Uani 1 1 d . . . N10 N 0.7697(5) -0.0313(3) -0.0055(2) 0.0265(10) Uani 1 1 d . . . N11 N 0.5695(6) 0.0752(3) 0.1783(2) 0.0309(11) Uani 1 1 d . . . N12 N 0.3892(5) 0.0550(3) 0.2458(2) 0.0300(11) Uani 1 1 d . . . B2 B 0.6986(8) 0.1269(4) 0.1388(3) 0.0319(15) Uani 1 1 d . . . H2 H 0.6612 0.1752 0.1215 0.038 Uiso 1 1 calc R . . C22 C 0.9839(7) 0.2400(4) 0.1582(3) 0.0310(13) Uani 1 1 d . . . C23 C 0.8986(6) 0.1742(4) 0.2377(3) 0.0275(12) Uani 1 1 d . . . H23 H 0.8305 0.1370 0.2630 0.033 Uiso 1 1 calc R . . C24 C 1.0501(6) 0.2291(4) 0.2533(3) 0.0355(14) Uani 1 1 d . . . H24 H 1.1101 0.2378 0.2911 0.043 Uiso 1 1 calc R . . C25 C 1.2621(8) 0.3322(8) 0.1987(5) 0.098(4) Uani 1 1 d . . . H25A H 1.3176 0.2945 0.1696 0.148 Uiso 1 1 calc R . . H25B H 1.3215 0.3547 0.2396 0.148 Uiso 1 1 calc R . . H25C H 1.2558 0.3894 0.1834 0.148 Uiso 1 1 calc R . . C26 C 0.7240(6) 0.0454(4) 0.0242(3) 0.0285(12) Uani 1 1 d . . . C27 C 0.7925(7) -0.0278(4) 0.0924(3) 0.0407(16) Uani 1 1 d . . . H27 H 0.8159 -0.0416 0.1309 0.049 Uiso 1 1 calc R . . C28 C 0.8117(7) -0.0786(4) 0.0372(3) 0.0327(14) Uani 1 1 d . . . H28 H 0.8468 -0.1356 0.0286 0.039 Uiso 1 1 calc R . . C29 C 0.7639(7) -0.0656(4) -0.0723(3) 0.0315(13) Uani 1 1 d . . . H29A H 0.6542 -0.1053 -0.0880 0.047 Uiso 1 1 calc R . . H29B H 0.8364 -0.1058 -0.0826 0.047 Uiso 1 1 calc R . . H29C H 0.7972 -0.0088 -0.0916 0.047 Uiso 1 1 calc R . . C30 C 0.5094(6) 0.1240(4) 0.2262(3) 0.0286(13) Uani 1 1 d . . . C31 C 0.4803(8) -0.0239(4) 0.1666(3) 0.0432(18) Uani 1 1 d . . . H31 H 0.4945 -0.0746 0.1342 0.052 Uiso 1 1 calc R . . C32 C 0.3721(8) -0.0357(4) 0.2084(3) 0.0389(16) Uani 1 1 d . . . H32 H 0.2965 -0.0961 0.2118 0.047 Uiso 1 1 calc R . . C33 C 0.2951(7) 0.0760(4) 0.2977(3) 0.0388(15) Uani 1 1 d . . . H33A H 0.2303 0.0140 0.3072 0.058 Uiso 1 1 calc R . . H33B H 0.2243 0.1121 0.2870 0.058 Uiso 1 1 calc R . . H33C H 0.3669 0.1161 0.3341 0.058 Uiso 1 1 calc R . . C34 C 0.5322(6) 0.3054(4) 0.0249(3) 0.0291(13) Uani 1 1 d . . . H34 H 0.4400 0.2435 0.0138 0.035 Uiso 1 1 calc R . . C35 C 0.6364(6) 0.3194(4) -0.0227(2) 0.0217(11) Uani 1 1 d . . . H35 H 0.6041 0.2657 -0.0612 0.026 Uiso 1 1 calc R . . C36 C 0.7322(6) 0.4169(3) -0.0340(2) 0.0198(10) Uani 1 1 d . . . H36A H 0.6616 0.4440 -0.0553 0.024 Uiso 1 1 calc R . . H36B H 0.8174 0.4074 -0.0618 0.024 Uiso 1 1 calc R . . C37 C 0.8090(6) 0.4907(3) 0.0262(2) 0.0196(10) Uani 1 1 d . . . H37A H 0.9036 0.5416 0.0170 0.024 Uiso 1 1 calc R . . H37B H 0.7312 0.5240 0.0449 0.024 Uiso 1 1 calc R . . C38 C 0.8604(6) 0.4394(3) 0.0722(2) 0.0178(10) Uani 1 1 d . . . H38 H 0.9785 0.4610 0.0831 0.021 Uiso 1 1 calc R . . C39 C 0.7673(6) 0.4093(4) 0.1190(2) 0.0235(11) Uani 1 1 d . . . H39 H 0.8316 0.4137 0.1576 0.028 Uiso 1 1 calc R . . C40 C 0.6039(6) 0.4188(5) 0.1307(3) 0.0350(14) Uani 1 1 d . . . H40A H 0.6138 0.4881 0.1507 0.042 Uiso 1 1 calc R . . H40B H 0.5539 0.3772 0.1596 0.042 Uiso 1 1 calc R . . C41 C 0.4953(6) 0.3879(5) 0.0705(3) 0.0344(14) Uani 1 1 d . . . H41A H 0.3818 0.3661 0.0804 0.041 Uiso 1 1 calc R . . H41B H 0.5107 0.4454 0.0515 0.041 Uiso 1 1 calc R . . C42 C 0.8822(7) 0.7029(5) 0.1455(3) 0.0404(15) Uani 1 1 d . . . H42A H 0.9153 0.7334 0.1899 0.048 Uiso 1 1 calc R . . H42B H 0.8863 0.6342 0.1374 0.048 Uiso 1 1 calc R . . Cl1 Cl 1.0149(2) 0.76845(12) 0.09936(8) 0.0437(4) Uani 1 1 d . . . Cl2 Cl 0.6846(2) 0.70268(14) 0.12939(12) 0.0738(7) Uani 1 1 d . . . Cl3 Cl 0.2681(3) 0.69261(15) 0.20042(9) 0.0663(6) Uani 1 1 d . . . C43A C 0.123(3) 0.6173(19) 0.2364(12) 0.043(6) Uani 0.291(6) 1 d PU B 1 H43A H 0.0806 0.5515 0.2082 0.051 Uiso 0.291(6) 1 calc PR B 1 H43B H 0.0336 0.6456 0.2448 0.051 Uiso 0.291(6) 1 calc PR B 1 Cl4A Cl 0.2038(6) 0.6045(4) 0.3086(3) 0.041(2) Uani 0.291(6) 1 d P B 1 C43B C 0.1929(16) 0.6427(9) 0.2627(6) 0.065(3) Uani 0.709(6) 1 d P B 2 H43C H 0.2182 0.6955 0.3012 0.079 Uiso 0.709(6) 1 calc PR B 2 H43D H 0.0748 0.6151 0.2560 0.079 Uiso 0.709(6) 1 calc PR B 2 Cl4B Cl 0.2735(4) 0.5511(2) 0.27171(16) 0.0751(13) Uani 0.709(6) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0146(2) 0.0207(2) 0.0180(2) -0.00159(15) -0.00531(14) 0.00720(15) S1 0.0241(7) 0.0156(6) 0.0271(7) 0.0066(5) -0.0091(5) -0.0027(5) B1A 0.026(3) 0.021(3) 0.024(3) 0.013(2) -0.013(2) -0.007(2) B1B 0.026(3) 0.021(3) 0.024(3) 0.013(2) -0.013(2) -0.007(2) N1 0.031(2) 0.016(2) 0.022(2) 0.0054(18) -0.0084(19) -0.0063(18) N2 0.045(3) 0.014(2) 0.029(3) 0.0014(19) -0.009(2) -0.004(2) C2 0.030(3) 0.014(2) 0.026(3) 0.009(2) -0.005(2) -0.002(2) C3 0.050(4) 0.021(3) 0.024(3) 0.003(2) -0.015(3) -0.009(3) C4 0.055(4) 0.022(3) 0.030(3) 0.003(2) -0.014(3) -0.009(3) C5 0.065(5) 0.018(3) 0.043(4) 0.005(3) -0.003(3) 0.011(3) S2A 0.030(4) 0.042(5) 0.0153(18) 0.004(3) -0.002(2) 0.019(3) S3A 0.019(3) 0.0300(17) 0.0172(14) 0.0060(11) 0.006(2) -0.003(2) N3A 0.009(4) 0.019(6) 0.014(5) 0.002(5) 0.006(4) 0.011(3) N4A 0.027(5) 0.019(6) 0.018(5) 0.008(5) 0.006(4) 0.014(4) N5A 0.009(6) 0.019(5) 0.016(5) 0.010(4) -0.003(5) -0.001(5) N6A 0.032(7) 0.012(4) 0.016(5) 0.004(3) -0.007(6) 0.002(6) C6A 0.018(3) 0.020(7) 0.017(6) 0.003(5) 0.003(4) 0.012(3) C7A 0.013(5) 0.027(6) 0.018(6) 0.007(6) 0.002(5) 0.010(4) C8A 0.020(5) 0.014(6) 0.026(7) 0.003(6) 0.012(5) 0.008(4) C9A 0.075(12) 0.023(7) 0.023(6) 0.011(6) 0.024(7) 0.012(8) C10A 0.013(5) 0.016(5) 0.011(5) -0.002(4) 0.000(4) -0.001(5) C11A 0.013(6) 0.015(5) 0.012(6) -0.001(4) -0.003(4) 0.001(5) C12A 0.029(7) 0.027(6) 0.016(6) 0.000(4) 0.000(5) 0.015(6) C13A 0.046(9) 0.020(6) 0.027(6) 0.011(4) 0.000(6) 0.003(6) S2B 0.011(2) 0.027(4) 0.026(4) 0.011(3) 0.003(2) 0.001(3) S3B 0.032(5) 0.0216(19) 0.0184(18) 0.0077(14) 0.001(3) 0.003(3) N3B 0.013(5) 0.010(6) 0.017(6) -0.003(5) 0.001(5) 0.006(4) N4B 0.014(6) 0.010(6) 0.029(8) 0.005(7) 0.007(6) 0.003(4) N5B 0.017(9) 0.016(6) 0.022(8) 0.005(5) -0.007(7) 0.001(8) N6B 0.034(8) 0.010(5) 0.022(7) 0.002(4) -0.009(6) 0.002(7) C6B 0.018(3) 0.020(7) 0.017(6) 0.003(5) 0.003(4) 0.012(3) C7B 0.016(7) 0.008(6) 0.026(7) -0.001(7) -0.009(7) 0.001(5) C8B 0.015(6) 0.013(6) 0.037(9) -0.005(8) 0.000(7) 0.004(5) C9B 0.015(7) 0.007(6) 0.040(9) 0.002(7) 0.010(6) 0.001(5) C10B 0.029(8) 0.012(5) 0.014(6) 0.004(5) -0.006(6) 0.002(7) C11B 0.014(8) 0.010(6) 0.033(10) -0.004(6) -0.003(6) -0.001(6) C12B 0.022(9) 0.012(6) 0.031(11) -0.002(6) -0.016(7) 0.005(8) C13B 0.064(13) 0.020(7) 0.021(7) 0.014(5) -0.017(8) 0.007(9) C14 0.052(4) 0.024(3) 0.039(4) -0.020(3) -0.030(3) 0.026(3) C15 0.054(4) 0.043(4) 0.027(3) -0.017(3) -0.029(3) 0.033(3) C16 0.049(4) 0.028(3) 0.050(4) -0.015(3) -0.040(3) 0.019(3) C17 0.020(3) 0.019(3) 0.085(5) 0.013(3) -0.031(3) -0.002(2) C18 0.010(2) 0.017(2) 0.047(3) 0.005(2) 0.001(2) 0.0015(19) C19 0.015(2) 0.015(2) 0.041(3) 0.005(2) 0.003(2) 0.0002(19) C20 0.027(3) 0.021(3) 0.068(5) 0.019(3) -0.016(3) -0.005(2) C21 0.059(4) 0.017(3) 0.074(5) -0.011(3) -0.051(4) 0.013(3) Rh2 0.0167(2) 0.0231(2) 0.0241(2) 0.01485(17) -0.00100(15) 0.00154(15) S4 0.0243(7) 0.0424(8) 0.0432(9) 0.0314(7) 0.0014(6) 0.0102(6) S5 0.0460(9) 0.0226(7) 0.0286(7) 0.0152(6) -0.0077(6) 0.0052(6) S6 0.0224(7) 0.0189(7) 0.0799(12) 0.0145(7) -0.0070(7) 0.0047(5) N7 0.034(3) 0.017(2) 0.033(3) 0.0139(19) -0.009(2) 0.0019(18) N8 0.019(2) 0.070(4) 0.052(3) 0.044(3) -0.005(2) 0.008(2) N9 0.047(3) 0.023(2) 0.031(3) 0.016(2) -0.011(2) 0.000(2) N10 0.024(2) 0.027(2) 0.031(3) 0.016(2) -0.0016(19) 0.0029(18) N11 0.039(3) 0.021(2) 0.025(2) 0.011(2) -0.011(2) -0.007(2) N12 0.025(2) 0.026(2) 0.034(3) 0.013(2) -0.014(2) -0.0042(19) B2 0.043(4) 0.018(3) 0.031(3) 0.015(3) -0.013(3) -0.003(3) C22 0.029(3) 0.034(3) 0.039(3) 0.023(3) -0.002(2) 0.011(2) C23 0.028(3) 0.027(3) 0.034(3) 0.018(2) -0.004(2) 0.009(2) C24 0.020(3) 0.050(4) 0.043(4) 0.025(3) -0.010(2) 0.010(3) C25 0.017(3) 0.178(10) 0.113(8) 0.118(8) -0.012(4) -0.012(5) C26 0.030(3) 0.021(3) 0.032(3) 0.015(2) -0.009(2) -0.002(2) C27 0.046(4) 0.023(3) 0.052(4) 0.024(3) -0.018(3) -0.001(3) C28 0.030(3) 0.026(3) 0.040(4) 0.018(3) -0.012(3) -0.001(2) C29 0.027(3) 0.033(3) 0.040(3) 0.017(3) 0.005(2) 0.012(2) C30 0.021(3) 0.022(3) 0.040(3) 0.015(2) -0.015(2) -0.004(2) C31 0.069(5) 0.023(3) 0.014(3) 0.006(2) -0.010(3) -0.022(3) C32 0.051(4) 0.029(3) 0.019(3) 0.009(2) -0.011(3) -0.017(3) C33 0.023(3) 0.035(3) 0.058(4) 0.014(3) -0.003(3) 0.005(2) C34 0.013(2) 0.044(3) 0.032(3) 0.026(3) -0.008(2) -0.002(2) C35 0.020(3) 0.025(3) 0.020(3) 0.009(2) -0.007(2) 0.002(2) C36 0.024(3) 0.021(2) 0.019(2) 0.010(2) 0.001(2) 0.009(2) C37 0.019(2) 0.020(2) 0.022(3) 0.008(2) 0.003(2) 0.0063(19) C38 0.014(2) 0.017(2) 0.019(2) 0.0038(19) -0.0034(18) -0.0006(18) C39 0.019(3) 0.034(3) 0.016(2) 0.007(2) 0.0012(19) 0.004(2) C40 0.022(3) 0.062(4) 0.026(3) 0.016(3) 0.009(2) 0.015(3) C41 0.018(3) 0.063(4) 0.030(3) 0.020(3) 0.010(2) 0.017(3) C42 0.028(3) 0.049(4) 0.034(3) -0.011(3) -0.006(3) 0.011(3) Cl1 0.0483(9) 0.0423(9) 0.0440(9) 0.0101(7) -0.0050(7) 0.0189(7) Cl2 0.0322(9) 0.0483(11) 0.1202(19) -0.0343(11) -0.0165(10) 0.0191(8) Cl3 0.0941(16) 0.0622(12) 0.0401(10) 0.0183(9) -0.0062(10) 0.0153(11) C43A 0.038(9) 0.048(10) 0.039(9) 0.011(7) -0.017(7) 0.007(7) Cl4A 0.033(3) 0.045(4) 0.045(4) 0.022(3) -0.001(2) 0.006(2) C43B 0.063(8) 0.059(8) 0.077(9) 0.038(7) -0.003(7) 0.007(6) Cl4B 0.102(3) 0.0535(18) 0.072(2) 0.0241(16) -0.0213(19) 0.0198(17) _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 C14 2.109(5) . ? Rh1 C19 2.109(5) . ? Rh1 C15 2.110(5) . ? Rh1 H1B 2.1401 . yes Rh1 C18 2.150(5) . ? Rh1 H1A 2.2173 . yes Rh1 S2A 2.302(12) . yes Rh1 S2B 2.401(13) . yes Rh1 S1 2.4315(15) . yes Rh1 S3B 4.694(8) . yes Rh1 S3A 4.791(8) . yes S1 C2 1.696(5) . yes B1A N1 1.538(8) . yes B1A N5A 1.57(2) . yes B1A N3A 1.639(15) . yes B1A H1A 1.0000 . ? N1 C2 1.350(6) . ? N1 C3 1.383(7) . ? N2 C2 1.358(7) . ? N2 C4 1.373(7) . ? N2 C5 1.465(7) . ? C3 C4 1.349(9) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? S2A C6A 1.693(14) . yes S3A C10A 1.671(11) . yes N3A C6A 1.341(16) . ? N3A C7A 1.39(2) . ? N4A C6A 1.35(2) . ? N4A C8A 1.375(16) . ? N4A C9A 1.491(14) . ? N5A C10A 1.356(17) . ? N5A C11A 1.382(15) . ? N6A C12A 1.363(15) . ? N6A C10A 1.375(16) . ? N6A C13A 1.479(15) . ? C7A C8A 1.318(17) . ? C7A H7A 0.9500 . ? C8A H8A 0.9500 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C11A C12A 1.319(19) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? S2B C6B 1.716(19) . yes S3B C10B 1.641(17) . yes N3B C6B 1.36(2) . ? N3B C7B 1.41(3) . ? N4B C8B 1.33(2) . ? N4B C6B 1.36(3) . ? N4B C9B 1.50(2) . ? N5B C11B 1.38(2) . ? N5B C10B 1.40(2) . ? N6B C12B 1.39(2) . ? N6B C10B 1.41(2) . ? N6B C13B 1.47(2) . ? C7B C8B 1.33(2) . ? C7B H7B 0.9500 . ? C8B H8B 0.9500 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C11B C12B 1.32(3) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14 C15 1.415(8) . ? C14 C21 1.510(10) . ? C14 H14 1.0000 . ? C15 C16 1.504(8) . ? C15 H15 1.0000 . ? C16 C17 1.495(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.531(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.390(7) . ? C18 H18 1.0000 . ? C19 C20 1.512(7) . ? C19 H19 1.0000 . ? C20 C21 1.529(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? Rh2 C39 2.103(5) . ? Rh2 C35 2.122(4) . ? Rh2 C34 2.130(5) . ? Rh2 C38 2.142(5) . ? Rh2 S5 2.3505(16) . yes Rh2 S4 2.4315(14) . yes Rh2 S6 4.952(2) . yes S4 C22 1.707(6) . yes S5 C26 1.715(5) . yes S6 C30 1.672(6) . yes N7 C22 1.343(7) . ? N7 C23 1.379(6) . ? N7 B2 1.537(7) . yes N8 C22 1.354(7) . ? N8 C24 1.372(7) . ? N8 C25 1.439(8) . ? N9 C26 1.347(7) . ? N9 C27 1.414(7) . ? N9 B2 1.538(9) . yes N10 C26 1.339(7) . ? N10 C28 1.387(6) . ? N10 C29 1.449(7) . ? N11 C30 1.344(8) . ? N11 C31 1.392(7) . ? N11 B2 1.545(8) . yes N12 C32 1.366(8) . ? N12 C30 1.368(7) . ? N12 C33 1.448(8) . ? B2 H2 1.0000 . ? C23 C24 1.329(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.324(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.326(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.402(7) . ? C34 C41 1.510(8) . ? C34 H34 1.0000 . ? C35 C36 1.494(6) . ? C35 H35 1.0000 . ? C36 C37 1.529(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.520(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.384(7) . ? C38 H38 1.0000 . ? C39 C40 1.495(7) . ? C39 H39 1.0000 . ? C40 C41 1.534(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 Cl1 1.752(7) . ? C42 Cl2 1.763(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? Cl3 C43B 1.735(12) . ? Cl3 C43A 1.73(3) . ? C43A Cl4A 1.81(2) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C43B Cl4B 1.729(12) . ? C43B H43C 0.9900 . ? C43B H43D 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 C14 Rh1 C19 82.8(3) . . ? C14 Rh1 C15 39.2(2) . . ? C19 Rh1 C15 98.7(3) . . ? C14 Rh1 H1B 104.6 . . ? C19 Rh1 H1B 86.4 . . ? C15 Rh1 H1B 141.1 . . ? C14 Rh1 C18 90.0(2) . . ? C19 Rh1 C18 38.1(2) . . ? C15 Rh1 C18 81.0(2) . . ? H1B Rh1 C18 120.8 . . ? C14 Rh1 H1A 103.2 . . ? C19 Rh1 H1A 83.0 . . ? C15 Rh1 H1A 140.6 . . ? H1B Rh1 H1A 3.6 . . ? C18 Rh1 H1A 117.7 . . ? C14 Rh1 S2A 85.3(4) . . ? C19 Rh1 S2A 160.3(3) . . ? C15 Rh1 S2A 81.6(3) . . ? H1B Rh1 S2A 81.4 . . ? C18 Rh1 S2A 157.7(3) . . ? H1A Rh1 S2A 84.5 . . yes C14 Rh1 S2B 94.9(4) . . ? C19 Rh1 S2B 163.1(3) . . ? C15 Rh1 S2B 89.7(4) . . ? H1B Rh1 S2B 77.9 . . yes C18 Rh1 S2B 158.7(3) . . ? H1A Rh1 S2B 81.3 . . ? C14 Rh1 S1 175.11(15) . . ? C19 Rh1 S1 95.40(14) . . ? C15 Rh1 S1 137.18(16) . . ? H1B Rh1 S1 79.8 . . yes C18 Rh1 S1 85.83(14) . . ? H1A Rh1 S1 81.1 . . yes S2A Rh1 S1 97.6(3) . . yes S2B Rh1 S1 88.1(3) . . yes C14 Rh1 S3B 95.9(2) . . ? C19 Rh1 S3B 46.2(2) . . ? C15 Rh1 S3B 131.4(2) . . ? H1B Rh1 S3B 40.2 . . ? C18 Rh1 S3B 82.0(3) . . ? H1A Rh1 S3B 36.8 . . ? S2A Rh1 S3B 120.1(3) . . ? S2B Rh1 S3B 117.9(3) . . ? S1 Rh1 S3B 86.06(10) . . ? C14 Rh1 S3A 95.23(19) . . ? C19 Rh1 S3A 51.95(18) . . ? C15 Rh1 S3A 132.4(2) . . ? H1B Rh1 S3A 34.6 . . ? C18 Rh1 S3A 88.07(19) . . ? H1A Rh1 S3A 31.1 . . ? S2A Rh1 S3A 114.0(3) . . ? S2B Rh1 S3A 112.0(3) . . ? S1 Rh1 S3A 87.21(9) . . ? S3B Rh1 S3A 6.12(11) . . ? C2 S1 Rh1 109.36(17) . . ? N1 B1A N5A 113.3(10) . . yes N1 B1A N3A 111.0(7) . . yes N5A B1A N3A 103.3(9) . . yes N1 B1A H1A 109.7 . . ? N5A B1A H1A 109.7 . . ? N3A B1A H1A 109.7 . . ? C2 N1 C3 108.2(5) . . ? C2 N1 B1A 122.4(4) . . ? C3 N1 B1A 128.4(5) . . ? C2 N2 C4 109.0(5) . . ? C2 N2 C5 124.3(5) . . ? C4 N2 C5 126.6(5) . . ? N1 C2 N2 107.5(4) . . ? N1 C2 S1 128.2(4) . . ? N2 C2 S1 124.2(4) . . ? C4 C3 N1 108.1(5) . . ? C4 C3 H3 126.0 . . ? N1 C3 H3 126.0 . . ? C3 C4 N2 107.2(5) . . ? C3 C4 H4 126.4 . . ? N2 C4 H4 126.4 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6A S2A Rh1 105.4(8) . . yes C10A S3A Rh1 82.7(5) . . yes C6A N3A C7A 108.5(12) . . ? C6A N3A B1A 127.7(13) . . ? C7A N3A B1A 121.7(9) . . ? C6A N4A C8A 110.6(10) . . ? C6A N4A C9A 121.8(11) . . ? C8A N4A C9A 127.6(11) . . ? C10A N5A C11A 108.3(13) . . ? C10A N5A B1A 119.2(10) . . ? C11A N5A B1A 131.5(11) . . ? C12A N6A C10A 111.8(11) . . ? C12A N6A C13A 126.3(12) . . ? C10A N6A C13A 121.9(12) . . ? N3A C6A N4A 105.8(11) . . ? N3A C6A S2A 129.8(14) . . ? N4A C6A S2A 124.3(12) . . ? C8A C7A N3A 108.7(11) . . ? C8A C7A H7A 125.6 . . ? N3A C7A H7A 125.6 . . ? C7A C8A N4A 106.2(12) . . ? C7A C8A H8A 126.9 . . ? N4A C8A H8A 126.9 . . ? N5A C10A N6A 104.2(10) . . ? N5A C10A S3A 129.2(11) . . ? N6A C10A S3A 126.6(10) . . ? C12A C11A N5A 110.3(11) . . ? C12A C11A H11A 124.9 . . ? N5A C11A H11A 124.9 . . ? C11A C12A N6A 105.2(11) . . ? C11A C12A H12A 127.4 . . ? N6A C12A H12A 127.4 . . ? C6B S2B Rh1 106.7(11) . . yes C10B S3B Rh1 82.5(7) . . yes C6B N3B C7B 105.8(17) . . ? C8B N4B C6B 109.7(15) . . ? C8B N4B C9B 129.2(16) . . ? C6B N4B C9B 121.1(15) . . ? C11B N5B C10B 108.9(18) . . ? C12B N6B C10B 112.8(15) . . ? C12B N6B C13B 129.1(15) . . ? C10B N6B C13B 118.1(14) . . ? N3B C6B N4B 107.5(15) . . ? N3B C6B S2B 129(2) . . ? N4B C6B S2B 123.8(17) . . ? C8B C7B N3B 108.4(15) . . ? C8B C7B H7B 125.8 . . ? N3B C7B H7B 125.8 . . ? C7B C8B N4B 108.5(16) . . ? C7B C8B H8B 125.7 . . ? N4B C8B H8B 125.7 . . ? N4B C9B H9B1 109.5 . . ? N4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? N4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N5B C10B N6B 101.8(15) . . ? N5B C10B S3B 129.3(14) . . ? N6B C10B S3B 128.8(13) . . ? C12B C11B N5B 111.8(17) . . ? C12B C11B H11B 124.1 . . ? N5B C11B H11B 124.1 . . ? C11B C12B N6B 104.6(15) . . ? C11B C12B H12B 127.7 . . ? N6B C12B H12B 127.7 . . ? N6B C13B H13D 109.5 . . ? N6B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? N6B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C15 C14 C21 124.1(6) . . ? C15 C14 Rh1 70.5(3) . . ? C21 C14 Rh1 112.7(4) . . ? C15 C14 H14 114.0 . . ? C21 C14 H14 114.0 . . ? Rh1 C14 H14 114.0 . . ? C14 C15 C16 125.4(7) . . ? C14 C15 Rh1 70.4(3) . . ? C16 C15 Rh1 111.6(4) . . ? C14 C15 H15 113.8 . . ? C16 C15 H15 113.8 . . ? Rh1 C15 H15 113.8 . . ? C17 C16 C15 112.1(5) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 112.3(5) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C17 123.2(5) . . ? C19 C18 Rh1 69.4(3) . . ? C17 C18 Rh1 112.1(4) . . ? C19 C18 H18 114.6 . . ? C17 C18 H18 114.6 . . ? Rh1 C18 H18 114.6 . . ? C18 C19 C20 125.5(5) . . ? C18 C19 Rh1 72.5(3) . . ? C20 C19 Rh1 108.5(4) . . ? C18 C19 H19 114.1 . . ? C20 C19 H19 114.1 . . ? Rh1 C19 H19 114.1 . . ? C19 C20 C21 113.0(5) . . ? 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 111.8(5) . . ? C14 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C14 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C39 Rh2 C35 98.0(2) . . ? C39 Rh2 C34 81.5(2) . . ? C35 Rh2 C34 38.49(19) . . ? C39 Rh2 C38 38.05(18) . . ? C35 Rh2 C38 81.01(18) . . ? C34 Rh2 C38 88.9(2) . . ? C39 Rh2 S5 162.62(14) . . ? C35 Rh2 S5 84.27(14) . . ? C34 Rh2 S5 89.96(17) . . ? C38 Rh2 S5 157.68(13) . . ? C39 Rh2 S4 92.81(14) . . ? C35 Rh2 S4 144.78(14) . . ? C34 Rh2 S4 174.17(17) . . ? C38 Rh2 S4 87.39(13) . . ? S5 Rh2 S4 95.18(6) . . ? C39 Rh2 S6 60.59(14) . . ? C35 Rh2 S6 128.51(14) . . ? C34 Rh2 S6 90.22(15) . . ? C38 Rh2 S6 97.68(13) . . ? S5 Rh2 S6 104.61(4) . . ? S4 Rh2 S6 85.83(4) . . ? C22 S4 Rh2 109.9(2) . . yes C26 S5 Rh2 108.45(19) . . yes C30 S6 Rh2 85.9(2) . . ? C22 N7 C23 108.3(4) . . ? C22 N7 B2 122.7(4) . . ? C23 N7 B2 128.9(4) . . ? C22 N8 C24 109.6(5) . . ? C22 N8 C25 123.8(5) . . ? C24 N8 C25 126.5(5) . . ? C26 N9 C27 105.5(5) . . ? C26 N9 B2 128.3(4) . . ? C27 N9 B2 126.0(5) . . ? C26 N10 C28 109.8(5) . . ? C26 N10 C29 125.6(4) . . ? C28 N10 C29 124.4(5) . . ? C30 N11 C31 108.1(5) . . ? C30 N11 B2 123.5(4) . . ? C31 N11 B2 127.8(5) . . ? C32 N12 C30 109.3(5) . . ? C32 N12 C33 125.9(5) . . ? C30 N12 C33 124.7(5) . . ? N9 B2 N7 107.1(5) . . ? N9 B2 N11 109.8(4) . . ? N7 B2 N11 110.2(4) . . ? N9 B2 H2 109.9 . . ? N7 B2 H2 109.9 . . ? N11 B2 H2 109.9 . . ? N7 C22 N8 106.7(5) . . ? N7 C22 S4 128.6(4) . . ? N8 C22 S4 124.5(4) . . ? C24 C23 N7 108.7(5) . . ? C24 C23 H23 125.7 . . ? N7 C23 H23 125.7 . . ? C23 C24 N8 106.7(5) . . ? C23 C24 H24 126.7 . . ? N8 C24 H24 126.7 . . ? N8 C25 H25A 109.5 . . ? N8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N10 C26 N9 108.9(4) . . ? N10 C26 S5 123.2(4) . . ? N9 C26 S5 127.9(5) . . ? C28 C27 N9 110.2(5) . . ? C28 C27 H27 124.9 . . ? N9 C27 H27 124.9 . . ? C27 C28 N10 105.6(5) . . ? C27 C28 H28 127.2 . . ? N10 C28 H28 127.2 . . ? N10 C29 H29A 109.5 . . ? N10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N11 C30 N12 106.6(5) . . ? N11 C30 S6 127.8(4) . . ? N12 C30 S6 125.6(5) . . ? C32 C31 N11 108.4(6) . . ? C32 C31 H31 125.8 . . ? N11 C31 H31 125.8 . . ? C31 C32 N12 107.4(5) . . ? C31 C32 H32 126.3 . . ? N12 C32 H32 126.3 . . ? N12 C33 H33A 109.5 . . ? N12 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N12 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C41 124.3(5) . . ? C35 C34 Rh2 70.5(3) . . ? C41 C34 Rh2 113.0(3) . . ? C35 C34 H34 113.9 . . ? C41 C34 H34 113.9 . . ? Rh2 C34 H34 113.9 . . ? C34 C35 C36 125.6(5) . . ? C34 C35 Rh2 71.1(3) . . ? C36 C35 Rh2 110.6(3) . . ? C34 C35 H35 113.9 . . ? C36 C35 H35 113.9 . . ? Rh2 C35 H35 113.9 . . ? C35 C36 C37 112.1(4) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C36 110.9(4) . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C37 123.2(4) . . ? C39 C38 Rh2 69.5(3) . . ? C37 C38 Rh2 113.1(3) . . ? C39 C38 H38 114.3 . . ? C37 C38 H38 114.3 . . ? Rh2 C38 H38 114.3 . . ? C38 C39 C40 126.1(5) . . ? C38 C39 Rh2 72.5(3) . . ? C40 C39 Rh2 110.3(4) . . ? C38 C39 H39 113.5 . . ? C40 C39 H39 113.5 . . ? Rh2 C39 H39 113.5 . . ? C39 C40 C41 112.0(5) . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40B 109.2 . . ? C41 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C34 C41 C40 111.3(5) . . ? C34 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? C34 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? Cl1 C42 Cl2 110.7(4) . . ? Cl1 C42 H42A 109.5 . . ? Cl2 C42 H42A 109.5 . . ? Cl1 C42 H42B 109.5 . . ? Cl2 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C43B Cl3 C43A 26.2(7) . . ? Cl3 C43A Cl4A 111.5(13) . . ? Cl3 C43A H43A 109.3 . . ? Cl4A C43A H43A 109.3 . . ? Cl3 C43A H43B 109.3 . . ? Cl4A C43A H43B 109.3 . . ? H43A C43A H43B 108.0 . . ? Cl4B C43B Cl3 111.3(8) . . ? Cl4B C43B H43C 109.4 . . ? Cl3 C43B H43C 109.4 . . ? Cl4B C43B H43D 109.4 . . ? Cl3 C43B H43D 109.4 . . ? H43C C43B H43D 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 C14 Rh1 S1 C2 136(2) . . . . ? C19 Rh1 S1 C2 66.9(3) . . . . ? C15 Rh1 S1 C2 175.9(4) . . . . ? H1B Rh1 S1 C2 -18.5 . . . . ? C18 Rh1 S1 C2 103.8(3) . . . . ? H1A Rh1 S1 C2 -15.1 . . . . ? S2A Rh1 S1 C2 -98.3(3) . . . . ? S2B Rh1 S1 C2 -96.6(4) . . . . ? S3B Rh1 S1 C2 21.6(3) . . . . ? S3A Rh1 S1 C2 15.5(2) . . . . ? N5A B1A N1 C2 -174.8(7) . . . . ? N3A B1A N1 C2 69.5(8) . . . . ? N5A B1A N1 C3 18.1(10) . . . . ? N3A B1A N1 C3 -97.6(8) . . . . ? C3 N1 C2 N2 -0.4(6) . . . . ? B1A N1 C2 N2 -169.8(4) . . . . ? C3 N1 C2 S1 175.7(4) . . . . ? B1A N1 C2 S1 6.3(7) . . . . ? C4 N2 C2 N1 0.8(6) . . . . ? C5 N2 C2 N1 177.7(5) . . . . ? C4 N2 C2 S1 -175.6(4) . . . . ? C5 N2 C2 S1 1.4(8) . . . . ? Rh1 S1 C2 N1 23.2(5) . . . . ? Rh1 S1 C2 N2 -161.3(4) . . . . ? C2 N1 C3 C4 0.0(7) . . . . ? B1A N1 C3 C4 168.5(5) . . . . ? N1 C3 C4 N2 0.5(7) . . . . ? C2 N2 C4 C3 -0.8(7) . . . . ? C5 N2 C4 C3 -177.6(6) . . . . ? C14 Rh1 S2A C6A -136.1(9) . . . . ? C19 Rh1 S2A C6A -83.0(13) . . . . ? C15 Rh1 S2A C6A -175.4(10) . . . . ? H1B Rh1 S2A C6A -30.5 . . . . ? C18 Rh1 S2A C6A 145.4(10) . . . . ? H1A Rh1 S2A C6A -32.3 . . . . ? S2B Rh1 S2A C6A 38(3) . . . . ? S1 Rh1 S2A C6A 47.9(9) . . . . ? S3B Rh1 S2A C6A -42.0(10) . . . . ? S3A Rh1 S2A C6A -42.4(10) . . . . ? C14 Rh1 S3A C10A 86.5(6) . . . . ? C19 Rh1 S3A C10A 163.1(6) . . . . ? C15 Rh1 S3A C10A 100.3(6) . . . . ? H1B Rh1 S3A C10A -21.8 . . . . ? C18 Rh1 S3A C10A 176.3(6) . . . . ? H1A Rh1 S3A C10A -20.5 . . . . ? S2A Rh1 S3A C10A -0.7(7) . . . . ? S2B Rh1 S3A C10A -10.9(7) . . . . ? S1 Rh1 S3A C10A -97.8(5) . . . . ? S3B Rh1 S3A C10A -176.7(18) . . . . ? N1 B1A N3A C6A -106.6(17) . . . . ? N5A B1A N3A C6A 131.6(19) . . . . ? N1 B1A N3A C7A 55.1(17) . . . . ? N5A B1A N3A C7A -66.6(19) . . . . ? N1 B1A N5A C10A 66(2) . . . . ? N3A B1A N5A C10A -173.6(17) . . . . ? N1 B1A N5A C11A -126(2) . . . . ? N3A B1A N5A C11A -6(3) . . . . ? C7A N3A C6A N4A 3(2) . . . . ? B1A N3A C6A N4A 167.1(15) . . . . ? C7A N3A C6A S2A -178.1(19) . . . . ? B1A N3A C6A S2A -14(3) . . . . ? C8A N4A C6A N3A -1(2) . . . . ? C9A N4A C6A N3A 176.7(16) . . . . ? C8A N4A C6A S2A 180.0(17) . . . . ? C9A N4A C6A S2A -2(3) . . . . ? Rh1 S2A C6A N3A 31(2) . . . . ? Rh1 S2A C6A N4A -150.4(17) . . . . ? C6A N3A C7A C8A -4(2) . . . . ? B1A N3A C7A C8A -169.2(15) . . . . ? N3A C7A C8A N4A 3(2) . . . . ? C6A N4A C8A C7A -1(2) . . . . ? C9A N4A C8A C7A -179.2(17) . . . . ? C11A N5A C10A N6A 4(2) . . . . ? B1A N5A C10A N6A 174.4(17) . . . . ? C11A N5A C10A S3A -177.3(13) . . . . ? B1A N5A C10A S3A -7(3) . . . . ? C12A N6A C10A N5A -2.8(18) . . . . ? C13A N6A C10A N5A 178.6(16) . . . . ? C12A N6A C10A S3A 178.5(12) . . . . ? C13A N6A C10A S3A 0(2) . . . . ? Rh1 S3A C10A N5A 29.9(17) . . . . ? Rh1 S3A C10A N6A -151.7(13) . . . . ? C10A N5A C11A C12A -4(2) . . . . ? B1A N5A C11A C12A -173(2) . . . . ? N5A C11A C12A N6A 2.1(19) . . . . ? C10A N6A C12A C11A 0.4(17) . . . . ? C13A N6A C12A C11A 179.0(14) . . . . ? C14 Rh1 S2B C6B -128.2(13) . . . . ? C19 Rh1 S2B C6B -46.8(19) . . . . ? C15 Rh1 S2B C6B -167.1(13) . . . . ? H1B Rh1 S2B C6B -24.3 . . . . ? C18 Rh1 S2B C6B 129.1(14) . . . . ? H1A Rh1 S2B C6B -25.5 . . . . ? S2A Rh1 S2B C6B -135(4) . . . . ? S1 Rh1 S2B C6B 55.7(13) . . . . ? S3B Rh1 S2B C6B -28.8(13) . . . . ? S3A Rh1 S2B C6B -30.5(13) . . . . ? C14 Rh1 S3B C10B 87.2(7) . . . . ? C19 Rh1 S3B C10B 161.4(8) . . . . ? C15 Rh1 S3B C10B 105.9(8) . . . . ? H1B Rh1 S3B C10B -18.4 . . . . ? C18 Rh1 S3B C10B 176.4(7) . . . . ? H1A Rh1 S3B C10B -16.9 . . . . ? S2A Rh1 S3B C10B -0.8(8) . . . . ? S2B Rh1 S3B C10B -11.5(8) . . . . ? S1 Rh1 S3B C10B -97.3(7) . . . . ? S3A Rh1 S3B C10B 3.4(16) . . . . ? C7B N3B C6B N4B -1(3) . . . . ? C7B N3B C6B S2B -179(3) . . . . ? C8B N4B C6B N3B -2(3) . . . . ? C9B N4B C6B N3B 177(2) . . . . ? C8B N4B C6B S2B 177(2) . . . . ? C9B N4B C6B S2B -4(4) . . . . ? Rh1 S2B C6B N3B 15(3) . . . . ? Rh1 S2B C6B N4B -164(2) . . . . ? C6B N3B C7B C8B 2(3) . . . . ? N3B C7B C8B N4B -3(3) . . . . ? C6B N4B C8B C7B 3(3) . . . . ? C9B N4B C8B C7B -175(2) . . . . ? C11B N5B C10B N6B -4(3) . . . . ? C11B N5B C10B S3B 179.8(18) . . . . ? C12B N6B C10B N5B 3(2) . . . . ? C13B N6B C10B N5B -175(2) . . . . ? C12B N6B C10B S3B 179.3(17) . . . . ? C13B N6B C10B S3B 1(3) . . . . ? Rh1 S3B C10B N5B 27(2) . . . . ? Rh1 S3B C10B N6B -147.6(19) . . . . ? C10B N5B C11B C12B 4(3) . . . . ? N5B C11B C12B N6B -2(3) . . . . ? C10B N6B C12B C11B -1(2) . . . . ? C13B N6B C12B C11B 177(2) . . . . ? C19 Rh1 C14 C15 113.2(4) . . . . ? H1B Rh1 C14 C15 -162.3 . . . . ? C18 Rh1 C14 C15 75.7(4) . . . . ? H1A Rh1 C14 C15 -165.7 . . . . ? S2A Rh1 C14 C15 -82.5(5) . . . . ? S2B Rh1 C14 C15 -83.6(5) . . . . ? S1 Rh1 C14 C15 44(3) . . . . ? S3B Rh1 C14 C15 157.7(4) . . . . ? S3A Rh1 C14 C15 163.8(4) . . . . ? C19 Rh1 C14 C21 -6.5(4) . . . . ? C15 Rh1 C14 C21 -119.7(6) . . . . ? H1B Rh1 C14 C21 77.9 . . . . ? C18 Rh1 C14 C21 -44.0(4) . . . . ? H1A Rh1 C14 C21 74.5 . . . . ? S2A Rh1 C14 C21 157.8(4) . . . . ? S2B Rh1 C14 C21 156.7(5) . . . . ? S1 Rh1 C14 C21 -76(2) . . . . ? S3B Rh1 C14 C21 38.0(4) . . . . ? S3A Rh1 C14 C21 44.1(4) . . . . ? C21 C14 C15 C16 1.8(9) . . . . ? Rh1 C14 C15 C16 -103.0(6) . . . . ? C21 C14 C15 Rh1 104.8(6) . . . . ? C19 Rh1 C15 C14 -67.3(4) . . . . ? H1B Rh1 C15 C14 27.8 . . . . ? C18 Rh1 C15 C14 -101.2(4) . . . . ? H1A Rh1 C15 C14 22.2 . . . . ? S2A Rh1 C15 C14 92.9(5) . . . . ? S2B Rh1 C15 C14 98.1(5) . . . . ? S1 Rh1 C15 C14 -175.0(3) . . . . ? S3B Rh1 C15 C14 -30.2(6) . . . . ? S3A Rh1 C15 C14 -22.1(5) . . . . ? C14 Rh1 C15 C16 121.4(7) . . . . ? C19 Rh1 C15 C16 54.1(5) . . . . ? H1B Rh1 C15 C16 149.2 . . . . ? C18 Rh1 C15 C16 20.2(5) . . . . ? H1A Rh1 C15 C16 143.6 . . . . ? S2A Rh1 C15 C16 -145.7(6) . . . . ? S2B Rh1 C15 C16 -140.5(6) . . . . ? S1 Rh1 C15 C16 -53.6(6) . . . . ? S3B Rh1 C15 C16 91.2(5) . . . . ? S3A Rh1 C15 C16 99.3(5) . . . . ? C14 C15 C16 C17 44.9(8) . . . . ? Rh1 C15 C16 C17 -35.8(7) . . . . ? C15 C16 C17 C18 34.2(7) . . . . ? C16 C17 C18 C19 -96.0(6) . . . . ? C16 C17 C18 Rh1 -16.9(6) . . . . ? C14 Rh1 C18 C19 78.3(3) . . . . ? C15 Rh1 C18 C19 116.6(3) . . . . ? H1B Rh1 C18 C19 -28.7 . . . . ? H1A Rh1 C18 C19 -26.6 . . . . ? S2A Rh1 C18 C19 155.9(9) . . . . ? S2B Rh1 C18 C19 -178.1(10) . . . . ? S1 Rh1 C18 C19 -104.2(3) . . . . ? S3B Rh1 C18 C19 -17.7(3) . . . . ? S3A Rh1 C18 C19 -16.9(3) . . . . ? C14 Rh1 C18 C17 -40.3(4) . . . . ? C19 Rh1 C18 C17 -118.6(5) . . . . ? C15 Rh1 C18 C17 -1.9(4) . . . . ? H1B Rh1 C18 C17 -147.3 . . . . ? H1A Rh1 C18 C17 -145.2 . . . . ? S2A Rh1 C18 C17 37.3(10) . . . . ? S2B Rh1 C18 C17 63.3(11) . . . . ? S1 Rh1 C18 C17 137.2(4) . . . . ? S3B Rh1 C18 C17 -136.2(4) . . . . ? S3A Rh1 C18 C17 -135.5(4) . . . . ? C17 C18 C19 C20 2.9(9) . . . . ? Rh1 C18 C19 C20 -100.6(6) . . . . ? C17 C18 C19 Rh1 103.5(5) . . . . ? C14 Rh1 C19 C18 -99.2(3) . . . . ? C15 Rh1 C19 C18 -63.3(3) . . . . ? H1B Rh1 C19 C18 155.5 . . . . ? H1A Rh1 C19 C18 156.4 . . . . ? S2A Rh1 C19 C18 -152.6(9) . . . . ? S2B Rh1 C19 C18 177.6(12) . . . . ? S1 Rh1 C19 C18 76.2(3) . . . . ? S3B Rh1 C19 C18 155.4(4) . . . . ? S3A Rh1 C19 C18 158.3(4) . . . . ? C14 Rh1 C19 C20 23.2(4) . . . . ? C15 Rh1 C19 C20 59.2(4) . . . . ? H1B Rh1 C19 C20 -82.0 . . . . ? C18 Rh1 C19 C20 122.4(5) . . . . ? H1A Rh1 C19 C20 -81.1 . . . . ? S2A Rh1 C19 C20 -30.2(11) . . . . ? S2B Rh1 C19 C20 -60.0(13) . . . . ? S1 Rh1 C19 C20 -161.4(3) . . . . ? S3B Rh1 C19 C20 -82.1(4) . . . . ? S3A Rh1 C19 C20 -79.2(4) . . . . ? C18 C19 C20 C21 44.8(8) . . . . ? Rh1 C19 C20 C21 -36.6(5) . . . . ? C15 C14 C21 C20 -92.9(6) . . . . ? Rh1 C14 C21 C20 -11.7(6) . . . . ? C19 C20 C21 C14 32.2(7) . . . . ? C39 Rh2 S4 C22 67.3(3) . . . . ? C35 Rh2 S4 C22 175.3(3) . . . . ? C34 Rh2 S4 C22 54.5(14) . . . . ? C38 Rh2 S4 C22 104.9(3) . . . . ? S5 Rh2 S4 C22 -97.3(2) . . . . ? S6 Rh2 S4 C22 7.0(2) . . . . ? C39 Rh2 S5 C26 -80.3(5) . . . . ? C35 Rh2 S5 C26 -178.7(3) . . . . ? C34 Rh2 S5 C26 -140.5(3) . . . . ? C38 Rh2 S5 C26 132.5(4) . . . . ? S4 Rh2 S5 C26 36.7(2) . . . . ? S6 Rh2 S5 C26 -50.3(2) . . . . ? C39 Rh2 S6 C30 176.2(2) . . . . ? C35 Rh2 S6 C30 100.4(2) . . . . ? C34 Rh2 S6 C30 96.1(2) . . . . ? C38 Rh2 S6 C30 -175.0(2) . . . . ? S5 Rh2 S6 C30 6.10(18) . . . . ? S4 Rh2 S6 C30 -88.18(18) . . . . ? C26 N9 B2 N7 -116.1(6) . . . . ? C27 N9 B2 N7 58.2(7) . . . . ? C26 N9 B2 N11 124.2(6) . . . . ? C27 N9 B2 N11 -61.4(7) . . . . ? C22 N7 B2 N9 68.2(6) . . . . ? C23 N7 B2 N9 -109.0(6) . . . . ? C22 N7 B2 N11 -172.4(5) . . . . ? C23 N7 B2 N11 10.4(8) . . . . ? C30 N11 B2 N9 -176.5(4) . . . . ? C31 N11 B2 N9 -6.4(8) . . . . ? C30 N11 B2 N7 65.7(7) . . . . ? C31 N11 B2 N7 -124.2(6) . . . . ? C23 N7 C22 N8 0.0(6) . . . . ? B2 N7 C22 N8 -177.7(5) . . . . ? C23 N7 C22 S4 176.4(4) . . . . ? B2 N7 C22 S4 -1.3(8) . . . . ? C24 N8 C22 N7 0.5(7) . . . . ? C25 N8 C22 N7 176.6(7) . . . . ? C24 N8 C22 S4 -176.1(5) . . . . ? C25 N8 C22 S4 0.0(10) . . . . ? Rh2 S4 C22 N7 37.2(6) . . . . ? Rh2 S4 C22 N8 -147.0(5) . . . . ? C22 N7 C23 C24 -0.5(7) . . . . ? B2 N7 C23 C24 177.0(6) . . . . ? N7 C23 C24 N8 0.8(7) . . . . ? C22 N8 C24 C23 -0.8(7) . . . . ? C25 N8 C24 C23 -176.8(8) . . . . ? C28 N10 C26 N9 -0.8(6) . . . . ? C29 N10 C26 N9 174.4(5) . . . . ? C28 N10 C26 S5 179.4(4) . . . . ? C29 N10 C26 S5 -5.4(7) . . . . ? C27 N9 C26 N10 2.1(6) . . . . ? B2 N9 C26 N10 177.4(5) . . . . ? C27 N9 C26 S5 -178.1(4) . . . . ? B2 N9 C26 S5 -2.9(9) . . . . ? Rh2 S5 C26 N10 -144.8(4) . . . . ? Rh2 S5 C26 N9 35.5(5) . . . . ? C26 N9 C27 C28 -2.8(6) . . . . ? B2 N9 C27 C28 -178.2(5) . . . . ? N9 C27 C28 N10 2.3(6) . . . . ? C26 N10 C28 C27 -1.0(6) . . . . ? C29 N10 C28 C27 -176.2(5) . . . . ? C31 N11 C30 N12 2.8(6) . . . . ? B2 N11 C30 N12 174.6(4) . . . . ? C31 N11 C30 S6 -176.7(4) . . . . ? B2 N11 C30 S6 -4.9(7) . . . . ? C32 N12 C30 N11 -2.1(6) . . . . ? C33 N12 C30 N11 178.4(5) . . . . ? C32 N12 C30 S6 177.4(4) . . . . ? C33 N12 C30 S6 -2.1(7) . . . . ? Rh2 S6 C30 N11 25.8(4) . . . . ? Rh2 S6 C30 N12 -153.7(4) . . . . ? C30 N11 C31 C32 -2.6(7) . . . . ? B2 N11 C31 C32 -173.9(5) . . . . ? N11 C31 C32 N12 1.2(7) . . . . ? C30 N12 C32 C31 0.6(6) . . . . ? C33 N12 C32 C31 -179.9(5) . . . . ? C39 Rh2 C34 C35 114.4(3) . . . . ? C38 Rh2 C34 C35 76.9(3) . . . . ? S5 Rh2 C34 C35 -80.8(3) . . . . ? S4 Rh2 C34 C35 127.3(13) . . . . ? S6 Rh2 C34 C35 174.6(3) . . . . ? C39 Rh2 C34 C41 -5.5(4) . . . . ? C35 Rh2 C34 C41 -119.9(5) . . . . ? C38 Rh2 C34 C41 -43.0(4) . . . . ? S5 Rh2 C34 C41 159.3(4) . . . . ? S4 Rh2 C34 C41 7.4(16) . . . . ? S6 Rh2 C34 C41 54.7(4) . . . . ? C41 C34 C35 C36 2.9(7) . . . . ? Rh2 C34 C35 C36 -102.2(5) . . . . ? C41 C34 C35 Rh2 105.1(5) . . . . ? C39 Rh2 C35 C34 -65.5(3) . . . . ? C38 Rh2 C35 C34 -99.6(3) . . . . ? S5 Rh2 C35 C34 97.2(3) . . . . ? S4 Rh2 C35 C34 -171.9(3) . . . . ? S6 Rh2 C35 C34 -6.9(4) . . . . ? C39 Rh2 C35 C36 56.4(4) . . . . ? C34 Rh2 C35 C36 121.9(5) . . . . ? C38 Rh2 C35 C36 22.2(4) . . . . ? S5 Rh2 C35 C36 -140.9(4) . . . . ? S4 Rh2 C35 C36 -50.1(5) . . . . ? S6 Rh2 C35 C36 114.9(3) . . . . ? C34 C35 C36 C37 42.8(6) . . . . ? Rh2 C35 C36 C37 -38.1(5) . . . . ? C35 C36 C37 C38 35.6(6) . . . . ? C36 C37 C38 C39 -96.2(6) . . . . ? C36 C37 C38 Rh2 -16.4(5) . . . . ? C35 Rh2 C38 C39 115.4(3) . . . . ? C34 Rh2 C38 C39 77.6(3) . . . . ? S5 Rh2 C38 C39 164.8(3) . . . . ? S4 Rh2 C38 C39 -97.9(3) . . . . ? S6 Rh2 C38 C39 -12.5(3) . . . . ? C39 Rh2 C38 C37 -118.4(5) . . . . ? C35 Rh2 C38 C37 -3.0(3) . . . . ? C34 Rh2 C38 C37 -40.9(4) . . . . ? S5 Rh2 C38 C37 46.3(6) . . . . ? S4 Rh2 C38 C37 143.6(3) . . . . ? S6 Rh2 C38 C37 -130.9(3) . . . . ? C37 C38 C39 C40 2.1(8) . . . . ? Rh2 C38 C39 C40 -102.8(5) . . . . ? C37 C38 C39 Rh2 104.8(4) . . . . ? C35 Rh2 C39 C38 -64.2(3) . . . . ? C34 Rh2 C39 C38 -99.2(3) . . . . ? S5 Rh2 C39 C38 -160.5(4) . . . . ? S4 Rh2 C39 C38 82.2(3) . . . . ? S6 Rh2 C39 C38 165.8(3) . . . . ? C35 Rh2 C39 C40 58.5(4) . . . . ? C34 Rh2 C39 C40 23.6(4) . . . . ? C38 Rh2 C39 C40 122.8(5) . . . . ? S5 Rh2 C39 C40 -37.7(7) . . . . ? S4 Rh2 C39 C40 -155.1(3) . . . . ? S6 Rh2 C39 C40 -71.5(3) . . . . ? C38 C39 C40 C41 44.8(8) . . . . ? Rh2 C39 C40 C41 -37.9(6) . . . . ? C35 C34 C41 C40 -94.6(6) . . . . ? Rh2 C34 C41 C40 -13.3(6) . . . . ? C39 C40 C41 C34 33.5(7) . . . . ? C43B Cl3 C43A Cl4A -13.7(13) . . . . ? C43A Cl3 C43B Cl4B 102(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.631 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.297 data_3 _database_code_depnum_ccdc_archive 'CCDC 761318' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H31 B N6 O P Rh S3, C H2 Cl2' _chemical_formula_sum 'C32 H33 B Cl2 N6 O P Rh S3' _chemical_formula_weight 829.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7020(19) _cell_length_b 11.763(2) _cell_length_c 16.687(3) _cell_angle_alpha 85.91(3) _cell_angle_beta 85.18(3) _cell_angle_gamma 67.44(3) _cell_volume 1750.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 908 _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6943 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17529 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0883 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 30.44 _reflns_number_total 9636 _reflns_number_gt 7615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.1158P)^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 9636 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.89674(3) 0.68604(3) 0.716328(17) 0.02496(11) Uani 1 1 d . . . P1 P 0.81900(11) 0.82074(9) 0.81748(6) 0.0253(2) Uani 1 1 d . . . S1 S 1.02659(11) 0.52650(9) 0.62282(6) 0.0302(2) Uani 1 1 d . . . S2 S 0.78289(11) 0.55688(9) 0.79375(6) 0.0298(2) Uani 1 1 d . . . S3 S 0.36863(15) 0.94244(11) 0.61619(8) 0.0457(3) Uani 1 1 d . . . O1 O 1.0573(4) 0.8201(3) 0.6156(2) 0.0461(8) Uani 1 1 d . . . B1 B 0.6457(5) 0.6611(4) 0.6175(3) 0.0277(8) Uani 1 1 d . . . H1 H 0.7068 0.7081 0.6309 0.033 Uiso 1 1 calc R . . N1 N 0.7489(4) 0.5277(3) 0.5945(2) 0.0268(6) Uani 1 1 d . . . N2 N 0.9355(4) 0.3533(3) 0.5735(2) 0.0313(7) Uani 1 1 d . . . N3 N 0.5469(4) 0.6451(3) 0.6930(2) 0.0308(7) Uani 1 1 d . . . N4 N 0.4914(4) 0.5864(3) 0.8145(2) 0.0343(7) Uani 1 1 d . . . N5 N 0.5489(4) 0.7259(3) 0.5449(2) 0.0298(7) Uani 1 1 d . . . N6 N 0.3987(4) 0.8663(3) 0.4644(2) 0.0368(8) Uani 1 1 d . . . C1 C 0.9959(4) 0.7705(4) 0.6582(2) 0.0298(8) Uani 1 1 d . . . C2 C 0.8986(4) 0.4705(3) 0.5959(2) 0.0275(7) Uani 1 1 d . . . C3 C 0.8074(5) 0.3360(4) 0.5577(3) 0.0360(9) Uani 1 1 d . . . H3 H 0.8016 0.2631 0.5400 0.043 Uiso 1 1 calc R . . C4 C 0.6917(5) 0.4440(4) 0.5725(3) 0.0355(9) Uani 1 1 d . . . H4 H 0.5889 0.4595 0.5685 0.043 Uiso 1 1 calc R . . C5 C 1.0875(5) 0.2609(4) 0.5615(3) 0.0412(10) Uani 1 1 d . . . H5A H 1.1245 0.2671 0.5056 0.062 Uiso 1 1 calc R . . H5B H 1.0866 0.1784 0.5734 0.062 Uiso 1 1 calc R . . H5C H 1.1532 0.2755 0.5976 0.062 Uiso 1 1 calc R . . C6 C 0.6022(4) 0.6002(4) 0.7650(2) 0.0293(8) Uani 1 1 d . . . C7 C 0.3634(5) 0.6222(5) 0.7718(3) 0.0413(10) Uani 1 1 d . . . H7 H 0.2691 0.6211 0.7914 0.050 Uiso 1 1 calc R . . C8 C 0.3987(5) 0.6587(4) 0.6975(3) 0.0371(9) Uani 1 1 d . . . H8 H 0.3326 0.6889 0.6552 0.045 Uiso 1 1 calc R . . C9 C 0.5024(6) 0.5469(5) 0.8990(3) 0.0475(12) Uani 1 1 d . . . H9A H 0.5429 0.4566 0.9039 0.071 Uiso 1 1 calc R . . H9B H 0.4030 0.5793 0.9269 0.071 Uiso 1 1 calc R . . H9C H 0.5689 0.5780 0.9233 0.071 Uiso 1 1 calc R . . C10 C 0.4398(5) 0.8420(4) 0.5422(3) 0.0326(8) Uani 1 1 d . . . C11 C 0.4861(5) 0.7682(4) 0.4177(3) 0.0383(9) Uani 1 1 d . . . H11 H 0.4815 0.7628 0.3615 0.046 Uiso 1 1 calc R . . C12 C 0.5787(5) 0.6825(4) 0.4667(3) 0.0342(9) Uani 1 1 d . . . H12 H 0.6519 0.6055 0.4511 0.041 Uiso 1 1 calc R . . C13 C 0.2834(6) 0.9797(5) 0.4345(3) 0.0555(14) Uani 1 1 d . . . H13A H 0.1930 1.0002 0.4706 0.083 Uiso 1 1 calc R . . H13B H 0.2602 0.9681 0.3804 0.083 Uiso 1 1 calc R . . H13C H 0.3198 1.0470 0.4324 0.083 Uiso 1 1 calc R . . C14 C 0.8186(5) 0.9756(4) 0.7939(2) 0.0292(8) Uani 1 1 d . . . C15 C 0.6899(5) 1.0827(4) 0.8000(3) 0.0350(9) Uani 1 1 d . . . H15 H 0.5965 1.0776 0.8172 0.042 Uiso 1 1 calc R . . C16 C 0.6986(6) 1.1975(4) 0.7808(3) 0.0441(11) Uani 1 1 d . . . H16 H 0.6106 1.2701 0.7846 0.053 Uiso 1 1 calc R . . C17 C 0.8328(7) 1.2064(4) 0.7566(3) 0.0468(12) Uani 1 1 d . . . H17 H 0.8382 1.2848 0.7443 0.056 Uiso 1 1 calc R . . C18 C 0.9608(6) 1.0998(5) 0.7503(3) 0.0463(11) Uani 1 1 d . . . H18 H 1.0538 1.1053 0.7326 0.056 Uiso 1 1 calc R . . C19 C 0.9543(5) 0.9865(4) 0.7694(3) 0.0388(9) Uani 1 1 d . . . H19 H 1.0433 0.9146 0.7659 0.047 Uiso 1 1 calc R . . C20 C 0.9307(4) 0.7746(4) 0.9064(2) 0.0271(7) Uani 1 1 d . . . C21 C 0.9277(5) 0.8612(4) 0.9599(3) 0.0366(9) Uani 1 1 d . . . H21 H 0.8712 0.9460 0.9486 0.044 Uiso 1 1 calc R . . C22 C 1.0060(5) 0.8259(4) 1.0294(3) 0.0401(10) Uani 1 1 d . . . H22 H 1.0021 0.8863 1.0654 0.048 Uiso 1 1 calc R . . C23 C 1.0892(5) 0.7030(5) 1.0460(3) 0.0412(10) Uani 1 1 d . . . H23 H 1.1438 0.6788 1.0931 0.049 Uiso 1 1 calc R . . C24 C 1.0931(5) 0.6151(4) 0.9941(3) 0.0403(10) Uani 1 1 d . . . H24 H 1.1485 0.5304 1.0062 0.048 Uiso 1 1 calc R . . C25 C 1.0157(5) 0.6511(4) 0.9238(3) 0.0337(9) Uani 1 1 d . . . H25 H 1.0211 0.5907 0.8875 0.040 Uiso 1 1 calc R . . C26 C 0.6298(4) 0.8491(3) 0.8602(2) 0.0286(8) Uani 1 1 d . . . C27 C 0.5193(5) 0.8755(4) 0.8057(3) 0.0356(9) Uani 1 1 d . . . H27 H 0.5435 0.8817 0.7496 0.043 Uiso 1 1 calc R . . C28 C 0.3732(5) 0.8927(4) 0.8333(3) 0.0428(10) Uani 1 1 d . . . H28 H 0.2981 0.9108 0.7960 0.051 Uiso 1 1 calc R . . C29 C 0.3372(5) 0.8836(5) 0.9149(3) 0.0485(12) Uani 1 1 d . . . H29 H 0.2383 0.8931 0.9336 0.058 Uiso 1 1 calc R . . C30 C 0.4464(6) 0.8604(6) 0.9691(3) 0.0541(13) Uani 1 1 d . . . H30 H 0.4212 0.8562 1.0252 0.065 Uiso 1 1 calc R . . C31 C 0.5932(5) 0.8431(5) 0.9423(3) 0.0418(10) Uani 1 1 d . . . H31 H 0.6673 0.8273 0.9799 0.050 Uiso 1 1 calc R . . C32 C 0.1950(8) 0.3345(7) 0.8006(4) 0.076(2) Uani 1 1 d . . . H32A H 0.0948 0.3401 0.8227 0.091 Uiso 1 1 calc R . . H32B H 0.1811 0.4034 0.7603 0.091 Uiso 1 1 calc R . . Cl1 Cl 0.2829(2) 0.19697(17) 0.75349(14) 0.0808(5) Uani 1 1 d . . . Cl2 Cl 0.2943(2) 0.35053(17) 0.87787(11) 0.0802(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02235(16) 0.02680(16) 0.02371(17) -0.00375(11) -0.00147(10) -0.00664(11) P1 0.0228(4) 0.0270(4) 0.0240(5) -0.0037(3) -0.0022(3) -0.0065(3) S1 0.0233(4) 0.0325(5) 0.0309(5) -0.0085(4) -0.0004(4) -0.0054(4) S2 0.0278(5) 0.0308(5) 0.0285(5) 0.0017(4) -0.0060(4) -0.0081(4) S3 0.0469(7) 0.0370(6) 0.0398(6) -0.0077(5) -0.0099(5) 0.0014(5) O1 0.0396(18) 0.054(2) 0.047(2) -0.0026(16) 0.0050(15) -0.0221(16) B1 0.026(2) 0.0284(19) 0.025(2) -0.0026(16) -0.0031(15) -0.0059(16) N1 0.0254(15) 0.0248(14) 0.0295(16) -0.0025(12) -0.0060(12) -0.0077(12) N2 0.0357(18) 0.0263(15) 0.0265(16) -0.0041(12) -0.0007(13) -0.0057(13) N3 0.0244(16) 0.0336(16) 0.0311(17) -0.0012(13) -0.0030(13) -0.0069(13) N4 0.0268(17) 0.0427(19) 0.0341(18) 0.0036(15) 0.0019(14) -0.0158(14) N5 0.0250(16) 0.0339(16) 0.0272(16) -0.0044(13) -0.0049(12) -0.0064(13) N6 0.0357(19) 0.0383(18) 0.0310(18) 0.0010(14) -0.0105(15) -0.0067(15) C1 0.0204(17) 0.0339(19) 0.032(2) -0.0041(15) -0.0006(14) -0.0066(14) C2 0.0244(17) 0.0284(17) 0.0236(17) -0.0042(14) -0.0006(13) -0.0030(14) C3 0.040(2) 0.0326(19) 0.038(2) -0.0043(17) -0.0055(18) -0.0160(17) C4 0.039(2) 0.035(2) 0.035(2) -0.0019(17) -0.0073(17) -0.0147(17) C5 0.036(2) 0.034(2) 0.043(3) -0.0124(18) 0.0013(19) -0.0012(17) C6 0.0267(18) 0.0309(18) 0.0276(19) -0.0036(15) 0.0002(14) -0.0078(14) C7 0.025(2) 0.054(3) 0.043(3) 0.004(2) 0.0004(17) -0.0144(19) C8 0.028(2) 0.043(2) 0.039(2) 0.0005(18) -0.0045(17) -0.0119(17) C9 0.050(3) 0.063(3) 0.031(2) 0.007(2) 0.003(2) -0.026(2) C10 0.030(2) 0.0316(19) 0.033(2) -0.0019(16) -0.0066(16) -0.0073(15) C11 0.038(2) 0.046(2) 0.029(2) -0.0036(17) -0.0072(17) -0.0120(19) C12 0.032(2) 0.036(2) 0.030(2) -0.0068(16) -0.0044(16) -0.0067(16) C13 0.056(3) 0.046(3) 0.045(3) 0.007(2) -0.024(2) 0.004(2) C14 0.035(2) 0.0294(18) 0.0223(17) -0.0026(14) -0.0050(14) -0.0100(15) C15 0.036(2) 0.0325(19) 0.031(2) -0.0045(16) -0.0031(16) -0.0070(16) C16 0.058(3) 0.0282(19) 0.042(3) -0.0043(18) -0.013(2) -0.0091(19) C17 0.076(4) 0.038(2) 0.036(2) 0.0016(19) -0.012(2) -0.031(2) C18 0.050(3) 0.053(3) 0.042(3) -0.006(2) -0.001(2) -0.026(2) C19 0.037(2) 0.038(2) 0.041(2) -0.0064(18) -0.0039(18) -0.0136(18) C20 0.0249(17) 0.0320(18) 0.0229(17) -0.0013(14) -0.0039(13) -0.0084(14) C21 0.044(2) 0.0324(19) 0.031(2) -0.0031(16) -0.0097(18) -0.0107(17) C22 0.045(3) 0.046(2) 0.033(2) -0.0073(18) -0.0094(18) -0.019(2) C23 0.038(2) 0.053(3) 0.031(2) 0.0041(19) -0.0134(18) -0.015(2) C24 0.039(2) 0.038(2) 0.036(2) 0.0028(18) -0.0095(18) -0.0059(18) C25 0.032(2) 0.034(2) 0.030(2) -0.0049(16) -0.0049(16) -0.0068(16) C26 0.0251(18) 0.0278(17) 0.032(2) -0.0053(15) 0.0031(14) -0.0091(14) C27 0.029(2) 0.037(2) 0.036(2) -0.0047(17) -0.0008(16) -0.0067(16) C28 0.027(2) 0.046(2) 0.050(3) -0.008(2) -0.0008(19) -0.0073(18) C29 0.029(2) 0.057(3) 0.055(3) -0.012(2) 0.011(2) -0.013(2) C30 0.046(3) 0.074(4) 0.041(3) -0.013(3) 0.016(2) -0.023(3) C31 0.036(2) 0.057(3) 0.029(2) -0.0067(19) 0.0018(17) -0.014(2) C32 0.059(4) 0.074(4) 0.070(4) 0.000(3) -0.019(3) 0.003(3) Cl1 0.0603(10) 0.0741(11) 0.1092(15) -0.0254(10) -0.0177(10) -0.0206(8) Cl2 0.0862(12) 0.0709(10) 0.0698(11) -0.0181(8) -0.0143(9) -0.0100(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 1.815(4) . yes Rh1 P1 2.2757(13) . yes Rh1 H1 2.3488 . yes Rh1 S1 2.4118(13) . yes Rh1 S2 2.4424(13) . yes P1 C26 1.825(4) . ? P1 C14 1.834(4) . ? P1 C20 1.837(4) . ? S1 C2 1.715(4) . yes S2 C6 1.728(4) . yes S3 C10 1.684(4) . yes O1 C1 1.156(5) . yes B1 N1 1.558(5) . yes B1 N5 1.562(5) . yes B1 N3 1.562(6) . yes B1 H1 1.0000 . ? N1 C2 1.347(5) . ? N1 C4 1.385(5) . ? N2 C2 1.357(5) . ? N2 C3 1.383(6) . ? N2 C5 1.466(5) . ? N3 C6 1.345(5) . ? N3 C8 1.381(5) . ? N4 C6 1.353(5) . ? N4 C7 1.390(6) . ? N4 C9 1.453(6) . ? N5 C10 1.371(5) . ? N5 C12 1.401(5) . ? N6 C10 1.369(5) . ? N6 C11 1.387(6) . ? N6 C13 1.461(6) . ? C3 C4 1.356(6) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.342(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.343(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.396(5) . ? C14 C19 1.396(6) . ? C15 C16 1.398(6) . ? C15 H15 0.9500 . ? C16 C17 1.371(8) . ? C16 H16 0.9500 . ? C17 C18 1.389(8) . ? C17 H17 0.9500 . ? C18 C19 1.371(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.390(5) . ? C20 C21 1.392(6) . ? C21 C22 1.390(6) . ? C21 H21 0.9500 . ? C22 C23 1.380(7) . ? C22 H22 0.9500 . ? C23 C24 1.382(7) . ? C23 H23 0.9500 . ? C24 C25 1.398(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.390(6) . ? C26 C27 1.393(6) . ? C27 C28 1.395(6) . ? C27 H27 0.9500 . ? C28 C29 1.384(7) . ? C28 H28 0.9500 . ? C29 C30 1.385(8) . ? C29 H29 0.9500 . ? C30 C31 1.398(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 Cl1 1.724(7) . ? C32 Cl2 1.735(7) . ? C32 H32A 0.9900 . ? C32 H32B 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 93.93(13) . . yes C1 Rh1 H1 101.1 . . ? P1 Rh1 H1 113.1 . . yes C1 Rh1 S1 84.25(13) . . yes P1 Rh1 S1 168.23(4) . . yes H1 Rh1 S1 78.6 . . yes C1 Rh1 S2 175.15(12) . . yes P1 Rh1 S2 88.98(4) . . yes H1 Rh1 S2 81.2 . . yes S1 Rh1 S2 92.12(4) . . yes C26 P1 C14 103.92(18) . . ? C26 P1 C20 102.88(19) . . ? C14 P1 C20 101.09(18) . . ? C26 P1 Rh1 114.45(13) . . ? C14 P1 Rh1 116.97(13) . . ? C20 P1 Rh1 115.57(13) . . ? C2 S1 Rh1 106.81(13) . . yes C6 S2 Rh1 107.94(15) . . yes N1 B1 N5 108.4(3) . . yes N1 B1 N3 105.3(3) . . yes N5 B1 N3 111.7(3) . . yes N1 B1 H1 110.4 . . ? N5 B1 H1 110.4 . . ? N3 B1 H1 110.4 . . ? C2 N1 C4 108.3(3) . . ? C2 N1 B1 129.6(3) . . ? C4 N1 B1 121.9(3) . . ? C2 N2 C3 109.5(3) . . ? C2 N2 C5 126.0(4) . . ? C3 N2 C5 124.4(4) . . ? C6 N3 C8 107.9(4) . . ? C6 N3 B1 123.2(3) . . ? C8 N3 B1 128.5(4) . . ? C6 N4 C7 108.4(4) . . ? C6 N4 C9 125.7(4) . . ? C7 N4 C9 125.9(4) . . ? C10 N5 C12 108.1(3) . . ? C10 N5 B1 126.6(3) . . ? C12 N5 B1 124.4(3) . . ? C10 N6 C11 109.7(3) . . ? C10 N6 C13 125.2(4) . . ? C11 N6 C13 125.1(4) . . ? O1 C1 Rh1 174.4(4) . . ? N1 C2 N2 107.5(3) . . ? N1 C2 S1 129.0(3) . . ? N2 C2 S1 123.5(3) . . ? C4 C3 N2 106.3(4) . . ? C4 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? C3 C4 N1 108.4(4) . . ? C3 C4 H4 125.8 . . ? N1 C4 H4 125.8 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N4 108.3(4) . . ? N3 C6 S2 129.0(3) . . ? N4 C6 S2 122.6(3) . . ? C8 C7 N4 106.8(4) . . ? C8 C7 H7 126.6 . . ? N4 C7 H7 126.6 . . ? C7 C8 N3 108.7(4) . . ? C7 C8 H8 125.7 . . ? N3 C8 H8 125.7 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 N5 106.5(3) . . ? N6 C10 S3 124.2(3) . . ? N5 C10 S3 129.2(3) . . ? C12 C11 N6 107.1(4) . . ? C12 C11 H11 126.4 . . ? N6 C11 H11 126.4 . . ? C11 C12 N5 108.5(4) . . ? C11 C12 H12 125.8 . . ? N5 C12 H12 125.8 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.5(4) . . ? C15 C14 P1 123.3(3) . . ? C19 C14 P1 118.2(3) . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.3(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C14 120.8(4) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 118.2(4) . . ? C25 C20 P1 120.6(3) . . ? C21 C20 P1 121.1(3) . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 119.9(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 120.7(4) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C31 C26 C27 119.7(4) . . ? C31 C26 P1 123.7(3) . . ? C27 C26 P1 116.6(3) . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.2(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.6(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C31 120.8(5) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C26 C31 C30 119.5(5) . . ? C26 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? Cl1 C32 Cl2 112.9(3) . . ? Cl1 C32 H32A 109.0 . . ? Cl2 C32 H32A 109.0 . . ? Cl1 C32 H32B 109.0 . . ? Cl2 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 P1 C26 142.09(19) . . . . ? H1 Rh1 P1 C26 38.2 . . . . ? S1 Rh1 P1 C26 -137.3(2) . . . . ? S2 Rh1 P1 C26 -41.80(15) . . . . ? C1 Rh1 P1 C14 20.22(19) . . . . ? H1 Rh1 P1 C14 -83.6 . . . . ? S1 Rh1 P1 C14 100.9(2) . . . . ? S2 Rh1 P1 C14 -163.67(15) . . . . ? C1 Rh1 P1 C20 -98.65(19) . . . . ? H1 Rh1 P1 C20 157.5 . . . . ? S1 Rh1 P1 C20 -18.0(3) . . . . ? S2 Rh1 P1 C20 77.46(15) . . . . ? C1 Rh1 S1 C2 -136.27(19) . . . . ? P1 Rh1 S1 C2 142.1(2) . . . . ? H1 Rh1 S1 C2 -33.7 . . . . ? S2 Rh1 S1 C2 46.96(15) . . . . ? C1 Rh1 S2 C6 -141.2(15) . . . . ? P1 Rh1 S2 C6 91.93(15) . . . . ? H1 Rh1 S2 C6 -21.7 . . . . ? S1 Rh1 S2 C6 -99.79(15) . . . . ? N5 B1 N1 C2 125.9(4) . . . . ? N3 B1 N1 C2 -114.4(4) . . . . ? N5 B1 N1 C4 -58.1(5) . . . . ? N3 B1 N1 C4 61.5(5) . . . . ? N1 B1 N3 C6 67.6(5) . . . . ? N5 B1 N3 C6 -174.9(4) . . . . ? N1 B1 N3 C8 -104.3(4) . . . . ? N5 B1 N3 C8 13.2(6) . . . . ? N1 B1 N5 C10 177.0(4) . . . . ? N3 B1 N5 C10 61.5(5) . . . . ? N1 B1 N5 C12 -15.1(5) . . . . ? N3 B1 N5 C12 -130.6(4) . . . . ? P1 Rh1 C1 O1 -154(4) . . . . ? H1 Rh1 C1 O1 -39.9 . . . . ? S1 Rh1 C1 O1 37(4) . . . . ? S2 Rh1 C1 O1 79(4) . . . . ? C4 N1 C2 N2 1.2(4) . . . . ? B1 N1 C2 N2 177.6(4) . . . . ? C4 N1 C2 S1 -177.1(3) . . . . ? B1 N1 C2 S1 -0.7(6) . . . . ? C3 N2 C2 N1 0.0(5) . . . . ? C5 N2 C2 N1 175.6(4) . . . . ? C3 N2 C2 S1 178.4(3) . . . . ? C5 N2 C2 S1 -6.0(6) . . . . ? Rh1 S1 C2 N1 26.7(4) . . . . ? Rh1 S1 C2 N2 -151.3(3) . . . . ? C2 N2 C3 C4 -1.3(5) . . . . ? C5 N2 C3 C4 -176.9(4) . . . . ? N2 C3 C4 N1 2.0(5) . . . . ? C2 N1 C4 C3 -2.1(5) . . . . ? B1 N1 C4 C3 -178.8(4) . . . . ? C8 N3 C6 N4 -0.4(5) . . . . ? B1 N3 C6 N4 -173.7(3) . . . . ? C8 N3 C6 S2 176.2(3) . . . . ? B1 N3 C6 S2 2.9(6) . . . . ? C7 N4 C6 N3 0.8(5) . . . . ? C9 N4 C6 N3 -176.3(4) . . . . ? C7 N4 C6 S2 -176.1(3) . . . . ? C9 N4 C6 S2 6.8(6) . . . . ? Rh1 S2 C6 N3 31.2(4) . . . . ? Rh1 S2 C6 N4 -152.6(3) . . . . ? C6 N4 C7 C8 -0.8(5) . . . . ? C9 N4 C7 C8 176.2(4) . . . . ? N4 C7 C8 N3 0.6(5) . . . . ? C6 N3 C8 C7 -0.1(5) . . . . ? B1 N3 C8 C7 172.8(4) . . . . ? C11 N6 C10 N5 -2.7(5) . . . . ? C13 N6 C10 N5 179.1(5) . . . . ? C11 N6 C10 S3 175.5(3) . . . . ? C13 N6 C10 S3 -2.8(7) . . . . ? C12 N5 C10 N6 2.9(5) . . . . ? B1 N5 C10 N6 172.4(4) . . . . ? C12 N5 C10 S3 -175.1(4) . . . . ? B1 N5 C10 S3 -5.6(7) . . . . ? C10 N6 C11 C12 1.4(5) . . . . ? C13 N6 C11 C12 179.6(5) . . . . ? N6 C11 C12 N5 0.5(5) . . . . ? C10 N5 C12 C11 -2.1(5) . . . . ? B1 N5 C12 C11 -171.9(4) . . . . ? C26 P1 C14 C15 -7.4(4) . . . . ? C20 P1 C14 C15 -113.8(4) . . . . ? Rh1 P1 C14 C15 119.8(3) . . . . ? C26 P1 C14 C19 171.9(3) . . . . ? C20 P1 C14 C19 65.5(4) . . . . ? Rh1 P1 C14 C19 -60.9(4) . . . . ? C19 C14 C15 C16 0.8(6) . . . . ? P1 C14 C15 C16 -179.9(3) . . . . ? C14 C15 C16 C17 -0.6(7) . . . . ? C15 C16 C17 C18 0.8(7) . . . . ? C16 C17 C18 C19 -1.2(7) . . . . ? C17 C18 C19 C14 1.4(7) . . . . ? C15 C14 C19 C18 -1.2(6) . . . . ? P1 C14 C19 C18 179.5(4) . . . . ? C26 P1 C20 C25 101.8(4) . . . . ? C14 P1 C20 C25 -150.9(3) . . . . ? Rh1 P1 C20 C25 -23.6(4) . . . . ? C26 P1 C20 C21 -75.4(4) . . . . ? C14 P1 C20 C21 31.8(4) . . . . ? Rh1 P1 C20 C21 159.1(3) . . . . ? C25 C20 C21 C22 -0.7(7) . . . . ? P1 C20 C21 C22 176.6(4) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C21 C22 C23 C24 -0.8(8) . . . . ? C22 C23 C24 C25 1.6(7) . . . . ? C21 C20 C25 C24 1.4(7) . . . . ? P1 C20 C25 C24 -175.9(4) . . . . ? C23 C24 C25 C20 -1.9(7) . . . . ? C14 P1 C26 C31 -100.8(4) . . . . ? C20 P1 C26 C31 4.3(4) . . . . ? Rh1 P1 C26 C31 130.5(4) . . . . ? C14 P1 C26 C27 80.6(3) . . . . ? C20 P1 C26 C27 -174.3(3) . . . . ? Rh1 P1 C26 C27 -48.1(3) . . . . ? C31 C26 C27 C28 -1.6(6) . . . . ? P1 C26 C27 C28 177.1(3) . . . . ? C26 C27 C28 C29 -0.1(7) . . . . ? C27 C28 C29 C30 1.7(8) . . . . ? C28 C29 C30 C31 -1.6(9) . . . . ? C27 C26 C31 C30 1.7(7) . . . . ? P1 C26 C31 C30 -176.9(4) . . . . ? C29 C30 C31 C26 -0.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 30.44 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.667 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.182 data_5 _database_code_depnum_ccdc_archive 'CCDC 761319' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H34 B N9 O P Rh S3' _chemical_formula_sum 'C19 H34 B N9 O P Rh S3' _chemical_formula_weight 645.42 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' _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 7.8254(16) _cell_length_b 12.527(3) _cell_length_c 14.475(3) _cell_angle_alpha 75.837(7) _cell_angle_beta 89.881(8) _cell_angle_gamma 85.536(8) _cell_volume 1371.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4094 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.2835 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details 'SADABS - BRUKER 2007' _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 Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23639 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.85 _reflns_number_total 6403 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _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^)+(0.0373P)^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 6403 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.64018(3) 0.82530(2) 0.791780(19) 0.01110(9) Uani 1 1 d . . . P1 P 0.43724(11) 0.79142(7) 0.90348(6) 0.0119(2) Uani 1 1 d . . . S1 S 0.69644(11) 0.63005(7) 0.80681(6) 0.01421(19) Uani 1 1 d . . . S2 S 0.88346(10) 0.87080(7) 0.68927(6) 0.01375(19) Uani 1 1 d . . . S3 S 0.75666(11) 0.73297(7) 0.33910(6) 0.0157(2) Uani 1 1 d . . . O1 O 0.6184(3) 1.0635(2) 0.7875(2) 0.0276(6) Uani 1 1 d . . . N1 N 0.7930(3) 0.6643(2) 0.61655(19) 0.0104(6) Uani 1 1 d . . . N2 N 0.9452(3) 0.5341(2) 0.71793(19) 0.0116(6) Uani 1 1 d . . . N3 N 0.7018(3) 0.8649(2) 0.52770(19) 0.0116(6) Uani 1 1 d . . . N4 N 0.7971(3) 1.0248(2) 0.5245(2) 0.0118(6) Uani 1 1 d . . . N5 N 0.5460(3) 0.7021(2) 0.4969(2) 0.0124(6) Uani 1 1 d . . . N6 N 0.4570(4) 0.6377(2) 0.3799(2) 0.0167(7) Uani 1 1 d . . . N7 N 0.3144(3) 0.9036(2) 0.9165(2) 0.0155(6) Uani 1 1 d . . . N8 N 0.5162(4) 0.7450(2) 1.01689(19) 0.0135(6) Uani 1 1 d . . . N9 N 0.3175(4) 0.6891(2) 0.8955(2) 0.0159(7) Uani 1 1 d . . . B1 B 0.6414(5) 0.7481(3) 0.5711(3) 0.0122(8) Uani 1 1 d . . . H1 H 0.5593 0.7544 0.6228 0.015 Uiso 1 1 calc R . . C1 C 0.6205(5) 0.9703(3) 0.7911(2) 0.0172(8) Uani 1 1 d . . . C2 C 0.8117(4) 0.6118(3) 0.7104(2) 0.0107(7) Uani 1 1 d . . . C3 C 1.0127(4) 0.5392(3) 0.6287(2) 0.0131(7) Uani 1 1 d . . . H3 H 1.1067 0.4938 0.6140 0.016 Uiso 1 1 calc R . . C4 C 0.9205(4) 0.6201(3) 0.5669(2) 0.0125(7) Uani 1 1 d . . . H4 H 0.9392 0.6434 0.5003 0.015 Uiso 1 1 calc R . . C5 C 0.9998(4) 0.4539(3) 0.8053(2) 0.0160(8) Uani 1 1 d . . . H5A H 1.0141 0.4919 0.8561 0.024 Uiso 1 1 calc R . . H5B H 1.1091 0.4150 0.7952 0.024 Uiso 1 1 calc R . . H5C H 0.9130 0.4006 0.8237 0.024 Uiso 1 1 calc R . . C6 C 0.7897(4) 0.9209(3) 0.5784(2) 0.0123(7) Uani 1 1 d . . . C7 C 0.7106(4) 1.0354(3) 0.4398(3) 0.0161(8) Uani 1 1 d . . . H7 H 0.6956 1.1001 0.3891 0.019 Uiso 1 1 calc R . . C8 C 0.6518(4) 0.9375(3) 0.4421(2) 0.0132(7) Uani 1 1 d . . . H8 H 0.5864 0.9207 0.3931 0.016 Uiso 1 1 calc R . . C9 C 0.8749(4) 1.1130(3) 0.5557(3) 0.0187(8) Uani 1 1 d . . . H9A H 0.7968 1.1419 0.5984 0.028 Uiso 1 1 calc R . . H9B H 0.8967 1.1726 0.5001 0.028 Uiso 1 1 calc R . . H9C H 0.9833 1.0835 0.5896 0.028 Uiso 1 1 calc R . . C10 C 0.5851(4) 0.6914(3) 0.4072(2) 0.0139(7) Uani 1 1 d . . . C11 C 0.3418(4) 0.6123(3) 0.4518(3) 0.0201(8) Uani 1 1 d . . . H11 H 0.2417 0.5742 0.4507 0.024 Uiso 1 1 calc R . . C12 C 0.3965(4) 0.6511(3) 0.5240(3) 0.0159(8) Uani 1 1 d . . . H12 H 0.3421 0.6447 0.5836 0.019 Uiso 1 1 calc R . . C13 C 0.4467(5) 0.6121(3) 0.2872(3) 0.0267(9) Uani 1 1 d . . . H13A H 0.4550 0.6797 0.2368 0.040 Uiso 1 1 calc R . . H13B H 0.3371 0.5815 0.2808 0.040 Uiso 1 1 calc R . . H13C H 0.5412 0.5580 0.2818 0.040 Uiso 1 1 calc R . . C14 C 0.2063(5) 0.8987(3) 0.9999(3) 0.0203(8) Uani 1 1 d . . . H14A H 0.1848 0.9729 1.0104 0.031 Uiso 1 1 calc R . . H14B H 0.2647 0.8498 1.0561 0.031 Uiso 1 1 calc R . . H14C H 0.0970 0.8701 0.9891 0.031 Uiso 1 1 calc R . . C15 C 0.2269(5) 0.9709(3) 0.8293(3) 0.0210(8) Uani 1 1 d . . . H15A H 0.1166 0.9418 0.8216 0.032 Uiso 1 1 calc R . . H15B H 0.2983 0.9682 0.7741 0.032 Uiso 1 1 calc R . . H15C H 0.2075 1.0475 0.8342 0.032 Uiso 1 1 calc R . . C16 C 0.6190(5) 0.8232(3) 1.0491(3) 0.0200(8) Uani 1 1 d . . . H16A H 0.6364 0.7992 1.1184 0.030 Uiso 1 1 calc R . . H16B H 0.5584 0.8970 1.0325 0.030 Uiso 1 1 calc R . . H16C H 0.7304 0.8255 1.0179 0.030 Uiso 1 1 calc R . . C17 C 0.6059(5) 0.6349(3) 1.0387(3) 0.0201(8) Uani 1 1 d . . . H17A H 0.7185 0.6385 1.0088 0.030 Uiso 1 1 calc R . . H17B H 0.5386 0.5848 1.0141 0.030 Uiso 1 1 calc R . . H17C H 0.6208 0.6076 1.1079 0.030 Uiso 1 1 calc R . . C18 C 0.1963(5) 0.6434(3) 0.9710(3) 0.0218(9) Uani 1 1 d . . . H18A H 0.0809 0.6788 0.9533 0.033 Uiso 1 1 calc R . . H18B H 0.2324 0.6576 1.0314 0.033 Uiso 1 1 calc R . . H18C H 0.1955 0.5636 0.9782 0.033 Uiso 1 1 calc R . . C19 C 0.2678(4) 0.6765(3) 0.8017(2) 0.0171(8) Uani 1 1 d . . . H19A H 0.2833 0.5984 0.8008 0.026 Uiso 1 1 calc R . . H19B H 0.3396 0.7194 0.7530 0.026 Uiso 1 1 calc R . . H19C H 0.1472 0.7033 0.7883 0.026 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 0.01391(15) 0.00991(14) 0.00982(14) -0.00303(11) 0.00148(10) -0.00120(10) P1 0.0148(4) 0.0103(4) 0.0107(5) -0.0030(4) 0.0003(4) -0.0001(4) S1 0.0189(5) 0.0112(4) 0.0119(4) -0.0019(4) 0.0041(4) 0.0002(3) S2 0.0133(4) 0.0157(5) 0.0123(4) -0.0028(4) -0.0003(3) -0.0037(3) S3 0.0188(5) 0.0165(5) 0.0116(4) -0.0029(4) 0.0030(4) -0.0006(4) O1 0.0385(17) 0.0136(14) 0.0328(16) -0.0091(12) 0.0078(13) -0.0042(12) N1 0.0108(14) 0.0095(14) 0.0108(14) -0.0029(12) 0.0013(11) 0.0004(11) N2 0.0122(14) 0.0104(15) 0.0117(15) -0.0021(12) -0.0003(11) 0.0000(11) N3 0.0112(14) 0.0118(15) 0.0118(15) -0.0031(12) 0.0005(12) 0.0000(11) N4 0.0137(14) 0.0064(14) 0.0143(15) -0.0009(12) 0.0023(12) 0.0004(11) N5 0.0106(14) 0.0116(15) 0.0142(15) -0.0017(12) 0.0007(12) -0.0012(11) N6 0.0214(16) 0.0135(15) 0.0170(16) -0.0058(13) -0.0021(13) -0.0054(12) N7 0.0167(15) 0.0162(16) 0.0118(15) -0.0023(13) 0.0004(12) 0.0052(12) N8 0.0199(15) 0.0119(15) 0.0085(15) -0.0023(12) -0.0015(12) -0.0007(12) N9 0.0183(16) 0.0169(16) 0.0138(16) -0.0055(13) 0.0021(12) -0.0043(12) B1 0.0108(19) 0.0114(19) 0.013(2) -0.0022(16) 0.0013(15) 0.0017(15) C1 0.024(2) 0.017(2) 0.0108(18) -0.0040(15) 0.0028(15) -0.0018(15) C2 0.0114(16) 0.0102(17) 0.0119(17) -0.0046(14) -0.0007(13) -0.0028(13) C3 0.0098(16) 0.0155(18) 0.0154(18) -0.0061(15) 0.0021(14) -0.0033(13) C4 0.0130(17) 0.0129(18) 0.0118(18) -0.0031(14) 0.0045(14) -0.0029(13) C5 0.0155(17) 0.0167(19) 0.0143(18) -0.0015(15) -0.0027(15) 0.0014(14) C6 0.0096(16) 0.0131(18) 0.0142(18) -0.0034(15) 0.0040(14) 0.0003(13) C7 0.0174(18) 0.0124(18) 0.0160(19) -0.0005(15) 0.0028(15) 0.0052(14) C8 0.0133(17) 0.0141(18) 0.0099(17) 0.0005(14) 0.0001(14) 0.0029(14) C9 0.0200(19) 0.0125(18) 0.024(2) -0.0059(16) 0.0048(16) -0.0022(15) C10 0.0145(17) 0.0127(18) 0.0129(18) -0.0014(15) -0.0026(14) 0.0029(14) C11 0.0150(18) 0.0179(19) 0.027(2) -0.0035(17) 0.0026(16) -0.0063(15) C12 0.0125(17) 0.0132(18) 0.020(2) 0.0001(16) 0.0038(15) -0.0043(14) C13 0.037(2) 0.031(2) 0.018(2) -0.0141(18) -0.0023(18) -0.0114(19) C14 0.022(2) 0.019(2) 0.022(2) -0.0101(17) 0.0065(16) 0.0030(15) C15 0.0216(19) 0.017(2) 0.023(2) -0.0060(17) -0.0064(16) 0.0056(15) C16 0.027(2) 0.021(2) 0.0138(19) -0.0065(16) -0.0030(16) -0.0050(16) C17 0.027(2) 0.0165(19) 0.0142(19) -0.0002(16) -0.0023(16) 0.0051(16) C18 0.025(2) 0.021(2) 0.020(2) -0.0059(17) 0.0078(16) -0.0058(16) C19 0.0153(18) 0.0153(18) 0.020(2) -0.0032(16) -0.0064(15) -0.0025(14) _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 1.809(4) . yes Rh1 P1 2.2527(10) . yes Rh1 S1 2.4075(10) . yes Rh1 S2 2.4279(10) . yes Rh1 H1 2.8859 . yes P1 N9 1.672(3) . ? P1 N7 1.689(3) . ? P1 N8 1.702(3) . ? S1 C2 1.713(3) . yes S2 C6 1.717(3) . yes S3 C10 1.703(3) . yes O1 C1 1.154(4) . yes N1 C2 1.359(4) . ? N1 C4 1.387(4) . ? N1 B1 1.553(4) . yes N2 C2 1.357(4) . ? N2 C3 1.384(4) . ? N2 C5 1.451(4) . ? N3 C6 1.354(4) . ? N3 C8 1.382(4) . ? N3 B1 1.554(4) . yes N4 C6 1.350(4) . ? N4 C7 1.375(4) . ? N4 C9 1.464(4) . ? N5 C10 1.369(4) . ? N5 C12 1.387(4) . ? N5 B1 1.554(5) . yes N6 C10 1.360(4) . ? N6 C11 1.370(4) . ? N6 C13 1.457(5) . ? N7 C14 1.465(4) . ? N7 C15 1.471(4) . ? N8 C17 1.460(4) . ? N8 C16 1.474(4) . ? N9 C19 1.461(4) . ? N9 C18 1.482(4) . ? B1 H1 1.0000 . ? C3 C4 1.340(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.335(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.340(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 . ? 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 90.60(11) . . yes C1 Rh1 S1 172.67(12) . . yes P1 Rh1 S1 90.11(3) . . yes C1 Rh1 S2 85.31(11) . . yes P1 Rh1 S2 171.34(3) . . yes S1 Rh1 S2 92.98(3) . . yes C1 Rh1 H1 120.6 . . yes P1 Rh1 H1 112.9 . . yes S1 Rh1 H1 65.6 . . yes S2 Rh1 H1 75.7 . . yes N9 P1 N7 111.37(15) . . ? N9 P1 N8 101.04(14) . . ? N7 P1 N8 99.15(14) . . ? N9 P1 Rh1 114.07(11) . . ? N7 P1 Rh1 115.26(11) . . ? N8 P1 Rh1 114.13(10) . . ? C2 S1 Rh1 108.31(12) . . yes C6 S2 Rh1 103.15(11) . . yes C2 N1 C4 108.2(3) . . ? C2 N1 B1 125.8(3) . . ? C4 N1 B1 125.6(3) . . ? C2 N2 C3 109.3(3) . . ? C2 N2 C5 124.8(3) . . ? C3 N2 C5 125.8(3) . . ? C6 N3 C8 107.5(3) . . ? C6 N3 B1 123.1(3) . . ? C8 N3 B1 128.2(3) . . ? C6 N4 C7 109.1(3) . . ? C6 N4 C9 124.5(3) . . ? C7 N4 C9 126.3(3) . . ? C10 N5 C12 108.1(3) . . ? C10 N5 B1 133.2(3) . . ? C12 N5 B1 118.4(3) . . ? C10 N6 C11 110.0(3) . . ? C10 N6 C13 124.1(3) . . ? C11 N6 C13 125.9(3) . . ? C14 N7 C15 111.2(3) . . ? C14 N7 P1 121.0(2) . . ? C15 N7 P1 115.6(2) . . ? C17 N8 C16 110.5(3) . . ? C17 N8 P1 115.3(2) . . ? C16 N8 P1 114.3(2) . . ? C19 N9 C18 113.0(3) . . ? C19 N9 P1 119.6(2) . . ? C18 N9 P1 121.7(2) . . ? N1 B1 N5 109.4(3) . . yes N1 B1 N3 111.8(3) . . yes N5 B1 N3 112.5(3) . . yes N1 B1 H1 107.7 . . ? N5 B1 H1 107.7 . . ? N3 B1 H1 107.7 . . ? O1 C1 Rh1 175.3(3) . . ? N2 C2 N1 107.0(3) . . ? N2 C2 S1 122.5(3) . . ? N1 C2 S1 130.5(3) . . ? C4 C3 N2 107.1(3) . . ? C4 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C3 C4 N1 108.4(3) . . ? C3 C4 H4 125.8 . . ? N1 C4 H4 125.8 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N3 107.6(3) . . ? N4 C6 S2 124.8(3) . . ? N3 C6 S2 127.5(2) . . ? C8 C7 N4 107.0(3) . . ? C8 C7 H7 126.5 . . ? N4 C7 H7 126.5 . . ? C7 C8 N3 108.7(3) . . ? C7 C8 H8 125.6 . . ? N3 C8 H8 125.6 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 N5 106.2(3) . . ? N6 C10 S3 124.3(3) . . ? N5 C10 S3 129.5(3) . . ? C12 C11 N6 107.2(3) . . ? C12 C11 H11 126.4 . . ? N6 C11 H11 126.4 . . ? C11 C12 N5 108.4(3) . . ? C11 C12 H12 125.8 . . ? N5 C12 H12 125.8 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N7 C14 H14A 109.5 . . ? N7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N7 C15 H15A 109.5 . . ? N7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 H16A 109.5 . . ? N8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N8 C17 H17A 109.5 . . ? N8 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N8 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 . . ? 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 N9 147.80(16) . . . . ? S1 Rh1 P1 N9 -39.50(12) . . . . ? S2 Rh1 P1 N9 -150.5(2) . . . . ? H1 Rh1 P1 N9 23.9 . . . . ? C1 Rh1 P1 N7 17.10(16) . . . . ? S1 Rh1 P1 N7 -170.19(12) . . . . ? S2 Rh1 P1 N7 78.8(3) . . . . ? H1 Rh1 P1 N7 -106.8 . . . . ? C1 Rh1 P1 N8 -96.74(16) . . . . ? S1 Rh1 P1 N8 75.97(11) . . . . ? S2 Rh1 P1 N8 -35.0(3) . . . . ? H1 Rh1 P1 N8 139.4 . . . . ? C1 Rh1 S1 C2 -99.9(9) . . . . ? P1 Rh1 S1 C2 164.47(12) . . . . ? S2 Rh1 S1 C2 -23.62(12) . . . . ? H1 Rh1 S1 C2 49.2 . . . . ? C1 Rh1 S2 C6 -82.68(17) . . . . ? P1 Rh1 S2 C6 -144.7(2) . . . . ? S1 Rh1 S2 C6 104.46(12) . . . . ? H1 Rh1 S2 C6 40.5 . . . . ? N9 P1 N7 C14 62.5(3) . . . . ? N8 P1 N7 C14 -43.2(3) . . . . ? Rh1 P1 N7 C14 -165.5(2) . . . . ? N9 P1 N7 C15 -76.6(3) . . . . ? N8 P1 N7 C15 177.6(2) . . . . ? Rh1 P1 N7 C15 55.4(3) . . . . ? N9 P1 N8 C17 55.0(3) . . . . ? N7 P1 N8 C17 169.0(2) . . . . ? Rh1 P1 N8 C17 -67.9(2) . . . . ? N9 P1 N8 C16 -175.3(2) . . . . ? N7 P1 N8 C16 -61.3(3) . . . . ? Rh1 P1 N8 C16 61.8(3) . . . . ? N7 P1 N9 C19 94.6(3) . . . . ? N8 P1 N9 C19 -160.9(3) . . . . ? Rh1 P1 N9 C19 -38.0(3) . . . . ? N7 P1 N9 C18 -57.1(3) . . . . ? N8 P1 N9 C18 47.4(3) . . . . ? Rh1 P1 N9 C18 170.3(2) . . . . ? C2 N1 B1 N5 -118.4(3) . . . . ? C4 N1 B1 N5 53.1(4) . . . . ? C2 N1 B1 N3 116.4(3) . . . . ? C4 N1 B1 N3 -72.2(4) . . . . ? C10 N5 B1 N1 -74.0(4) . . . . ? C12 N5 B1 N1 99.2(3) . . . . ? C10 N5 B1 N3 50.9(5) . . . . ? C12 N5 B1 N3 -135.9(3) . . . . ? C6 N3 B1 N1 -55.5(4) . . . . ? C8 N3 B1 N1 138.0(3) . . . . ? C6 N3 B1 N5 -179.0(3) . . . . ? C8 N3 B1 N5 14.5(5) . . . . ? P1 Rh1 C1 O1 165(4) . . . . ? S1 Rh1 C1 O1 69(4) . . . . ? S2 Rh1 C1 O1 -8(4) . . . . ? H1 Rh1 C1 O1 -78.2 . . . . ? C3 N2 C2 N1 1.1(4) . . . . ? C5 N2 C2 N1 -175.1(3) . . . . ? C3 N2 C2 S1 -179.9(2) . . . . ? C5 N2 C2 S1 3.9(5) . . . . ? C4 N1 C2 N2 -1.9(4) . . . . ? B1 N1 C2 N2 170.8(3) . . . . ? C4 N1 C2 S1 179.2(3) . . . . ? B1 N1 C2 S1 -8.1(5) . . . . ? Rh1 S1 C2 N2 138.7(3) . . . . ? Rh1 S1 C2 N1 -42.6(3) . . . . ? C2 N2 C3 C4 0.1(4) . . . . ? C5 N2 C3 C4 176.3(3) . . . . ? N2 C3 C4 N1 -1.3(4) . . . . ? C2 N1 C4 C3 2.0(4) . . . . ? B1 N1 C4 C3 -170.7(3) . . . . ? C7 N4 C6 N3 1.0(4) . . . . ? C9 N4 C6 N3 177.1(3) . . . . ? C7 N4 C6 S2 179.0(2) . . . . ? C9 N4 C6 S2 -4.9(5) . . . . ? C8 N3 C6 N4 -1.3(3) . . . . ? B1 N3 C6 N4 -170.2(3) . . . . ? C8 N3 C6 S2 -179.2(2) . . . . ? B1 N3 C6 S2 11.9(5) . . . . ? Rh1 S2 C6 N4 117.1(3) . . . . ? Rh1 S2 C6 N3 -65.3(3) . . . . ? C6 N4 C7 C8 -0.3(4) . . . . ? C9 N4 C7 C8 -176.3(3) . . . . ? N4 C7 C8 N3 -0.5(4) . . . . ? C6 N3 C8 C7 1.1(4) . . . . ? B1 N3 C8 C7 169.2(3) . . . . ? C11 N6 C10 N5 -1.6(4) . . . . ? C13 N6 C10 N5 178.3(3) . . . . ? C11 N6 C10 S3 177.8(3) . . . . ? C13 N6 C10 S3 -2.3(5) . . . . ? C12 N5 C10 N6 1.9(4) . . . . ? B1 N5 C10 N6 175.6(3) . . . . ? C12 N5 C10 S3 -177.5(3) . . . . ? B1 N5 C10 S3 -3.8(5) . . . . ? C10 N6 C11 C12 0.6(4) . . . . ? C13 N6 C11 C12 -179.2(3) . . . . ? N6 C11 C12 N5 0.6(4) . . . . ? C10 N5 C12 C11 -1.6(4) . . . . ? B1 N5 C12 C11 -176.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.577 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.137 data_7 _database_code_depnum_ccdc_archive 'CCDC 761320' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 B N6 P Rh S3, F6 P, C H2 Cl2' _chemical_formula_sum 'C31 H32 B Cl2 F6 N6 P2 Rh S3' _chemical_formula_weight 945.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _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 13.7550(7) _cell_length_b 27.5304(13) _cell_length_c 9.7544(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.643(3) _cell_angle_gamma 90.00 _cell_volume 3686.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5010 _cell_measurement_theta_min 2.5625 _cell_measurement_theta_max 22.289 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS - Bruker 2007' _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 Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 80297 _diffrn_reflns_av_R_equivalents 0.1409 _diffrn_reflns_av_sigmaI/netI 0.1360 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.60 _reflns_number_total 10342 _reflns_number_gt 5792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _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^)+(0.0290P)^2^+2.4156P] 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 10342 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.73797(2) 0.818127(10) 0.09260(3) 0.01035(7) Uani 1 1 d . . . P1 P 0.62965(7) 0.88234(3) 0.08510(10) 0.0120(2) Uani 1 1 d . . . S1 S 0.81088(7) 0.85217(3) -0.09668(10) 0.0140(2) Uani 1 1 d . . . S2 S 0.84047(7) 0.74850(3) 0.07805(10) 0.0149(2) Uani 1 1 d . . . S3 S 0.68138(7) 0.78961(3) 0.30200(10) 0.0138(2) Uani 1 1 d . . . N1 N 0.8943(2) 0.89072(10) 0.1388(3) 0.0104(6) Uani 1 1 d . . . N2 N 0.9477(2) 0.92343(11) -0.0460(3) 0.0131(7) Uani 1 1 d . . . N3 N 0.9235(2) 0.81159(10) 0.2619(3) 0.0120(7) Uani 1 1 d . . . N4 N 1.0031(2) 0.74331(11) 0.2564(3) 0.0161(7) Uani 1 1 d . . . N5 N 0.7974(2) 0.86773(10) 0.3498(3) 0.0112(7) Uani 1 1 d . . . N6 N 0.7059(2) 0.85352(11) 0.5208(3) 0.0129(7) Uani 1 1 d . . . B1 B 0.8462(3) 0.85027(15) 0.2203(4) 0.0122(9) Uani 1 1 d . . . C2 C 0.8853(3) 0.89034(13) 0.0003(4) 0.0117(8) Uani 1 1 d . . . C3 C 0.9977(3) 0.94410(13) 0.0658(4) 0.0149(8) Uani 1 1 d . . . H3 H 1.0469 0.9682 0.0622 0.018 Uiso 1 1 calc R . . C4 C 0.9658(3) 0.92469(13) 0.1803(4) 0.0143(8) Uani 1 1 d . . . H4 H 0.9874 0.9325 0.2721 0.017 Uiso 1 1 calc R . . C5 C 0.9539(3) 0.93637(14) -0.1910(4) 0.0200(9) Uani 1 1 d . . . H5A H 0.9484 0.9069 -0.2474 0.030 Uiso 1 1 calc R . . H5B H 1.0167 0.9521 -0.2036 0.030 Uiso 1 1 calc R . . H5C H 0.9009 0.9587 -0.2190 0.030 Uiso 1 1 calc R . . C6 C 0.9242(3) 0.76708(13) 0.2034(4) 0.0131(8) Uani 1 1 d . . . C7 C 1.0541(3) 0.77307(14) 0.3508(4) 0.0187(9) Uani 1 1 d . . . H7 H 1.1126 0.7652 0.4031 0.022 Uiso 1 1 calc R . . C8 C 1.0044(3) 0.81551(14) 0.3537(4) 0.0171(8) Uani 1 1 d . . . H8 H 1.0217 0.8430 0.4087 0.021 Uiso 1 1 calc R . . C9 C 1.0295(3) 0.69365(13) 0.2218(4) 0.0216(9) Uani 1 1 d . . . H9A H 0.9844 0.6815 0.1479 0.032 Uiso 1 1 calc R . . H9B H 1.0260 0.6729 0.3029 0.032 Uiso 1 1 calc R . . H9C H 1.0961 0.6932 0.1913 0.032 Uiso 1 1 calc R . . C10 C 0.7284(3) 0.83804(13) 0.3966(4) 0.0124(8) Uani 1 1 d . . . C11 C 0.7625(3) 0.89400(13) 0.5555(4) 0.0141(8) Uani 1 1 d . . . H11 H 0.7615 0.9122 0.6383 0.017 Uiso 1 1 calc R . . C12 C 0.8190(3) 0.90278(13) 0.4505(4) 0.0122(8) Uani 1 1 d . . . H12 H 0.8652 0.9283 0.4458 0.015 Uiso 1 1 calc R . . C13 C 0.5282(3) 0.86332(14) -0.0315(4) 0.0156(8) Uani 1 1 d . . . C14 C 0.6377(3) 0.82998(13) 0.6074(4) 0.0158(9) Uani 1 1 d . . . H14A H 0.5893 0.8118 0.5498 0.024 Uiso 1 1 calc R . . H14B H 0.6046 0.8546 0.6600 0.024 Uiso 1 1 calc R . . H14C H 0.6731 0.8076 0.6708 0.024 Uiso 1 1 calc R . . C15 C 0.5304(3) 0.81719(14) -0.0898(4) 0.0155(8) Uani 1 1 d . . . H15 H 0.5844 0.7965 -0.0683 0.019 Uiso 1 1 calc R . . C16 C 0.4546(3) 0.80123(15) -0.1785(4) 0.0252(10) Uani 1 1 d . . . H16 H 0.4564 0.7697 -0.2178 0.030 Uiso 1 1 calc R . . C17 C 0.3764(3) 0.83162(16) -0.2096(5) 0.0282(11) Uani 1 1 d . . . H17 H 0.3246 0.8209 -0.2713 0.034 Uiso 1 1 calc R . . C18 C 0.3724(3) 0.87720(15) -0.1523(4) 0.0228(10) Uani 1 1 d . . . H18 H 0.3181 0.8978 -0.1740 0.027 Uiso 1 1 calc R . . C19 C 0.4477(3) 0.89272(15) -0.0631(4) 0.0199(9) Uani 1 1 d . . . H19 H 0.4447 0.9240 -0.0225 0.024 Uiso 1 1 calc R . . C20 C 0.6684(3) 0.94045(13) 0.0120(4) 0.0140(8) Uani 1 1 d . . . C21 C 0.7339(3) 0.97034(12) 0.0878(4) 0.0159(8) Uani 1 1 d . . . H21 H 0.7563 0.9612 0.1783 0.019 Uiso 1 1 calc R . . C22 C 0.7667(3) 1.01324(14) 0.0321(4) 0.0197(9) Uani 1 1 d . . . H22 H 0.8091 1.0339 0.0859 0.024 Uiso 1 1 calc R . . C23 C 0.7379(3) 1.02601(14) -0.1012(5) 0.0246(10) Uani 1 1 d . . . H23 H 0.7615 1.0551 -0.1397 0.030 Uiso 1 1 calc R . . C24 C 0.6745(3) 0.99630(14) -0.1783(4) 0.0231(10) Uani 1 1 d . . . H24 H 0.6551 1.0049 -0.2703 0.028 Uiso 1 1 calc R . . C25 C 0.6391(3) 0.95399(14) -0.1226(4) 0.0174(9) Uani 1 1 d . . . H25 H 0.5947 0.9341 -0.1760 0.021 Uiso 1 1 calc R . . C26 C 0.5655(3) 0.89845(14) 0.2380(4) 0.0155(8) Uani 1 1 d . . . C27 C 0.5907(3) 0.93742(14) 0.3239(4) 0.0187(9) Uani 1 1 d . . . H27 H 0.6411 0.9589 0.3004 0.022 Uiso 1 1 calc R . . C28 C 0.5433(3) 0.94528(16) 0.4436(4) 0.0274(11) Uani 1 1 d . . . H28 H 0.5630 0.9713 0.5029 0.033 Uiso 1 1 calc R . . C29 C 0.4679(3) 0.91556(18) 0.4767(5) 0.0322(12) Uani 1 1 d . . . H29 H 0.4345 0.9215 0.5573 0.039 Uiso 1 1 calc R . . C30 C 0.4409(3) 0.87688(17) 0.3918(5) 0.0293(11) Uani 1 1 d . . . H30 H 0.3887 0.8564 0.4142 0.035 Uiso 1 1 calc R . . C31 C 0.4898(3) 0.86786(15) 0.2737(4) 0.0200(9) Uani 1 1 d . . . H31 H 0.4717 0.8408 0.2172 0.024 Uiso 1 1 calc R . . C32 C 0.2353(3) 0.66130(16) 0.6578(5) 0.0362(12) Uani 1 1 d . . . H32A H 0.2884 0.6397 0.6307 0.043 Uiso 1 1 calc R . . H32B H 0.2137 0.6497 0.7470 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.13861(10) 0.65821(5) 0.53482(15) 0.0576(4) Uani 1 1 d . . . Cl2 Cl 0.27938(10) 0.72067(5) 0.6763(2) 0.0874(7) Uani 1 1 d . . . P2 P 0.16059(8) 0.94282(4) 0.53655(12) 0.0219(3) Uani 1 1 d . . . F1 F 0.26850(18) 0.96204(11) 0.5652(3) 0.0556(9) Uani 1 1 d . . . F2 F 0.12217(17) 0.98500(8) 0.6312(3) 0.0300(6) Uani 1 1 d . . . F3 F 0.1717(2) 0.90867(9) 0.6697(3) 0.0515(8) Uani 1 1 d . . . F4 F 0.05140(16) 0.92273(8) 0.5099(2) 0.0268(6) Uani 1 1 d . . . F5 F 0.1457(2) 0.97732(11) 0.4065(3) 0.0571(9) Uani 1 1 d . . . F6 F 0.1977(2) 0.90052(12) 0.4428(4) 0.0756(12) 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 0.01003(14) 0.01021(14) 0.01080(14) -0.00088(14) 0.00048(11) -0.00090(13) P1 0.0112(5) 0.0120(5) 0.0129(5) -0.0002(4) 0.0007(4) -0.0004(4) S1 0.0160(5) 0.0154(5) 0.0108(5) -0.0012(4) 0.0009(4) -0.0027(4) S2 0.0156(5) 0.0119(5) 0.0171(5) -0.0036(4) -0.0006(4) 0.0016(4) S3 0.0153(5) 0.0120(5) 0.0141(5) 0.0000(4) 0.0023(4) -0.0033(4) N1 0.0113(16) 0.0109(16) 0.0088(15) 0.0015(13) -0.0009(13) -0.0024(13) N2 0.0156(17) 0.0139(17) 0.0101(16) 0.0002(14) 0.0024(13) -0.0021(13) N3 0.0127(16) 0.0095(16) 0.0139(16) -0.0002(13) 0.0032(13) -0.0021(13) N4 0.0151(17) 0.0133(17) 0.0195(18) 0.0026(14) -0.0016(14) 0.0052(14) N5 0.0119(16) 0.0120(16) 0.0097(16) -0.0004(13) 0.0006(13) -0.0021(13) N6 0.0148(17) 0.0143(17) 0.0098(16) 0.0016(14) 0.0028(13) 0.0004(13) B1 0.015(2) 0.010(2) 0.012(2) -0.0009(18) 0.0032(18) 0.0003(17) C2 0.0106(19) 0.0095(19) 0.0153(19) 0.0006(16) 0.0036(16) 0.0004(15) C3 0.014(2) 0.014(2) 0.017(2) 0.0001(17) 0.0013(17) -0.0053(16) C4 0.012(2) 0.014(2) 0.017(2) -0.0043(17) -0.0012(16) -0.0022(16) C5 0.027(2) 0.021(2) 0.012(2) 0.0020(18) 0.0045(18) -0.0048(18) C6 0.0111(19) 0.0116(19) 0.017(2) 0.0012(16) 0.0045(16) 0.0028(15) C7 0.015(2) 0.018(2) 0.021(2) 0.0011(18) -0.0071(18) 0.0001(17) C8 0.017(2) 0.018(2) 0.0156(19) 0.0013(18) -0.0027(16) -0.0027(18) C9 0.025(2) 0.014(2) 0.026(2) -0.0006(18) -0.0003(19) 0.0101(17) C10 0.0114(18) 0.0133(19) 0.0123(19) 0.0025(16) -0.0018(16) 0.0028(15) C11 0.017(2) 0.014(2) 0.0105(19) -0.0021(16) -0.0049(16) -0.0001(16) C12 0.0130(19) 0.0117(19) 0.0112(19) 0.0000(16) -0.0049(16) -0.0013(15) C13 0.014(2) 0.019(2) 0.014(2) 0.0030(17) 0.0014(16) -0.0036(16) C14 0.019(2) 0.015(2) 0.014(2) 0.0018(16) 0.0064(17) -0.0005(16) C15 0.0097(18) 0.016(2) 0.020(2) 0.0016(19) -0.0005(16) -0.0015(17) C16 0.021(2) 0.023(2) 0.031(3) -0.008(2) -0.002(2) -0.0028(19) C17 0.016(2) 0.036(3) 0.031(3) -0.007(2) -0.0087(19) -0.005(2) C18 0.016(2) 0.028(2) 0.024(2) -0.002(2) -0.0035(19) 0.0035(18) C19 0.019(2) 0.019(2) 0.021(2) 0.0003(18) -0.0008(18) 0.0031(18) C20 0.014(2) 0.0120(19) 0.016(2) -0.0010(16) 0.0026(16) 0.0043(16) C21 0.0152(19) 0.0117(18) 0.021(2) -0.0009(18) 0.0019(16) 0.0001(17) C22 0.015(2) 0.016(2) 0.029(2) -0.0037(19) -0.0002(19) -0.0034(17) C23 0.026(2) 0.012(2) 0.036(3) 0.004(2) 0.007(2) -0.0029(17) C24 0.027(2) 0.022(2) 0.020(2) 0.0032(19) 0.0030(19) -0.0013(19) C25 0.017(2) 0.018(2) 0.017(2) -0.0025(18) 0.0023(17) 0.0018(17) C26 0.014(2) 0.018(2) 0.014(2) 0.0017(17) -0.0019(16) 0.0082(16) C27 0.018(2) 0.017(2) 0.020(2) -0.0019(18) -0.0025(18) 0.0058(17) C28 0.033(3) 0.028(3) 0.021(2) -0.006(2) -0.002(2) 0.017(2) C29 0.026(3) 0.051(3) 0.021(2) 0.001(2) 0.006(2) 0.019(2) C30 0.016(2) 0.045(3) 0.028(3) 0.007(2) 0.007(2) 0.004(2) C31 0.012(2) 0.028(2) 0.019(2) -0.0003(19) -0.0010(17) 0.0050(18) C32 0.034(3) 0.025(3) 0.047(3) -0.002(2) -0.010(2) 0.001(2) Cl1 0.0557(9) 0.0633(10) 0.0503(9) 0.0189(8) -0.0231(7) -0.0222(8) Cl2 0.0359(8) 0.0345(8) 0.191(2) -0.0340(11) -0.0014(11) -0.0103(7) P2 0.0145(6) 0.0248(6) 0.0263(6) -0.0086(5) 0.0000(5) 0.0003(5) F1 0.0145(14) 0.060(2) 0.091(3) -0.0304(18) -0.0017(15) -0.0079(13) F2 0.0325(14) 0.0204(13) 0.0390(16) -0.0076(12) 0.0163(12) -0.0078(11) F3 0.0534(19) 0.0291(16) 0.066(2) 0.0190(15) -0.0387(16) -0.0057(14) F4 0.0190(13) 0.0351(15) 0.0256(14) -0.0053(12) -0.0047(11) -0.0052(11) F5 0.068(2) 0.076(2) 0.0272(16) 0.0181(16) 0.0045(15) -0.0268(18) F6 0.0397(18) 0.071(2) 0.120(3) -0.072(2) 0.0330(19) -0.0075(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 B1 2.077(4) . yes Rh1 P1 2.3101(10) . yes Rh1 S1 2.3514(10) . yes Rh1 S3 2.3657(10) . yes Rh1 S2 2.3892(10) . yes P1 C13 1.821(4) . ? P1 C26 1.835(4) . ? P1 C20 1.844(4) . ? S1 C2 1.710(4) . yes S2 C6 1.704(4) . yes S3 C10 1.724(4) . yes N1 C2 1.349(4) . ? N1 C4 1.398(4) . ? N1 B1 1.541(5) . yes N2 C2 1.349(4) . ? N2 C3 1.375(5) . ? N2 C5 1.466(5) . ? N3 C6 1.352(4) . ? N3 C8 1.387(5) . ? N3 B1 1.541(5) . yes N4 C6 1.342(5) . ? N4 C7 1.389(5) . ? N4 C9 1.460(4) . ? N5 C10 1.354(4) . ? N5 C12 1.395(4) . ? N5 B1 1.545(5) . yes N6 C10 1.339(4) . ? N6 C11 1.389(5) . ? N6 C14 1.455(4) . ? C3 C4 1.338(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.356(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.347(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C19 1.389(5) . ? C13 C15 1.392(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.382(6) . ? C16 H16 0.9500 . ? C17 C18 1.376(6) . ? C17 H17 0.9500 . ? C18 C19 1.378(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.397(5) . ? C20 C25 1.399(5) . ? C21 C22 1.387(5) . ? C21 H21 0.9500 . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.383(6) . ? C23 H23 0.9500 . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.392(5) . ? C26 C31 1.401(5) . ? C27 C28 1.391(5) . ? C27 H27 0.9500 . ? C28 C29 1.375(6) . ? C28 H28 0.9500 . ? C29 C30 1.385(6) . ? C29 H29 0.9500 . ? C30 C31 1.392(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 Cl1 1.735(5) . ? C32 Cl2 1.749(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? P2 F1 1.584(3) . ? P2 F6 1.585(3) . ? P2 F5 1.588(3) . ? P2 F2 1.594(2) . ? P2 F3 1.602(3) . ? P2 F4 1.606(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Rh1 P1 97.42(12) . . yes B1 Rh1 S1 88.61(12) . . yes P1 Rh1 S1 88.65(3) . . yes B1 Rh1 S3 83.47(12) . . yes P1 Rh1 S3 91.97(3) . . yes S1 Rh1 S3 172.07(4) . . yes B1 Rh1 S2 88.52(12) . . yes P1 Rh1 S2 173.71(4) . . yes S1 Rh1 S2 89.45(3) . . yes S3 Rh1 S2 90.73(3) . . yes C13 P1 C26 100.84(17) . . ? C13 P1 C20 103.69(17) . . ? C26 P1 C20 105.68(17) . . ? C13 P1 Rh1 105.48(13) . . ? C26 P1 Rh1 120.12(12) . . ? C20 P1 Rh1 118.33(12) . . ? C2 S1 Rh1 94.63(13) . . yes C6 S2 Rh1 95.22(13) . . yes C10 S3 Rh1 94.16(13) . . yes C2 N1 C4 108.3(3) . . ? C2 N1 B1 119.7(3) . . ? C4 N1 B1 130.6(3) . . ? C2 N2 C3 108.1(3) . . ? C2 N2 C5 124.4(3) . . ? C3 N2 C5 127.4(3) . . ? C6 N3 C8 108.4(3) . . ? C6 N3 B1 122.6(3) . . ? C8 N3 B1 128.9(3) . . ? C6 N4 C7 109.3(3) . . ? C6 N4 C9 125.1(3) . . ? C7 N4 C9 125.6(3) . . ? C10 N5 C12 107.6(3) . . ? C10 N5 B1 116.0(3) . . ? C12 N5 B1 135.0(3) . . ? C10 N6 C11 108.6(3) . . ? C10 N6 C14 125.4(3) . . ? C11 N6 C14 126.0(3) . . ? N3 B1 N1 108.9(3) . . ? N3 B1 N5 109.1(3) . . ? N1 B1 N5 114.8(3) . . ? N3 B1 Rh1 108.7(2) . . ? N1 B1 Rh1 108.3(3) . . ? N5 B1 Rh1 106.9(2) . . ? N1 C2 N2 108.1(3) . . ? N1 C2 S1 124.9(3) . . ? N2 C2 S1 126.9(3) . . ? C4 C3 N2 108.9(3) . . ? C4 C3 H3 125.6 . . ? N2 C3 H3 125.6 . . ? C3 C4 N1 106.7(3) . . ? C3 C4 H4 126.6 . . ? N1 C4 H4 126.6 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N3 107.8(3) . . ? N4 C6 S2 128.5(3) . . ? N3 C6 S2 123.5(3) . . ? C8 C7 N4 106.7(3) . . ? C8 C7 H7 126.7 . . ? N4 C7 H7 126.7 . . ? C7 C8 N3 107.8(3) . . ? C7 C8 H8 126.1 . . ? N3 C8 H8 126.1 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 N5 108.7(3) . . ? N6 C10 S3 129.1(3) . . ? N5 C10 S3 122.3(3) . . ? C12 C11 N6 107.4(3) . . ? C12 C11 H11 126.3 . . ? N6 C11 H11 126.3 . . ? C11 C12 N5 107.7(3) . . ? C11 C12 H12 126.1 . . ? N5 C12 H12 126.1 . . ? C19 C13 C15 118.6(4) . . ? C19 C13 P1 122.6(3) . . ? C15 C13 P1 118.8(3) . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C13 120.7(4) . . ? C16 C15 H15 119.7 . . ? C13 C15 H15 119.7 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.4(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C13 121.0(4) . . ? C18 C19 H19 119.5 . . ? C13 C19 H19 119.5 . . ? C21 C20 C25 118.5(3) . . ? C21 C20 P1 119.9(3) . . ? C25 C20 P1 121.4(3) . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.4(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 120.3(4) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C27 C26 C31 118.3(4) . . ? C27 C26 P1 124.1(3) . . ? C31 C26 P1 117.4(3) . . ? C28 C27 C26 120.9(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 119.6(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C31 120.4(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 120.3(4) . . ? C30 C31 H31 119.9 . . ? C26 C31 H31 119.9 . . ? Cl1 C32 Cl2 111.3(3) . . ? Cl1 C32 H32A 109.4 . . ? Cl2 C32 H32A 109.4 . . ? Cl1 C32 H32B 109.4 . . ? Cl2 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? F1 P2 F6 90.82(15) . . ? F1 P2 F5 90.75(17) . . ? F6 P2 F5 90.5(2) . . ? F1 P2 F2 89.77(14) . . ? F6 P2 F2 179.34(16) . . ? F5 P2 F2 89.78(16) . . ? F1 P2 F3 90.75(17) . . ? F6 P2 F3 91.1(2) . . ? F5 P2 F3 177.81(18) . . ? F2 P2 F3 88.64(15) . . ? F1 P2 F4 179.00(18) . . ? F6 P2 F4 89.19(14) . . ? F5 P2 F4 90.25(15) . . ? F2 P2 F4 90.21(13) . . ? F3 P2 F4 88.25(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 Rh1 P1 C13 177.15(17) . . . . ? S1 Rh1 P1 C13 88.72(13) . . . . ? S3 Rh1 P1 C13 -99.18(13) . . . . ? S2 Rh1 P1 C13 16.2(4) . . . . ? B1 Rh1 P1 C26 -70.12(19) . . . . ? S1 Rh1 P1 C26 -158.54(15) . . . . ? S3 Rh1 P1 C26 13.55(15) . . . . ? S2 Rh1 P1 C26 129.0(3) . . . . ? B1 Rh1 P1 C20 61.78(19) . . . . ? S1 Rh1 P1 C20 -26.64(15) . . . . ? S3 Rh1 P1 C20 145.45(15) . . . . ? S2 Rh1 P1 C20 -99.1(4) . . . . ? B1 Rh1 S1 C2 -12.56(17) . . . . ? P1 Rh1 S1 C2 84.90(12) . . . . ? S3 Rh1 S1 C2 -9.7(3) . . . . ? S2 Rh1 S1 C2 -101.10(12) . . . . ? B1 Rh1 S2 C6 9.57(17) . . . . ? P1 Rh1 S2 C6 170.6(3) . . . . ? S1 Rh1 S2 C6 98.20(13) . . . . ? S3 Rh1 S2 C6 -73.88(13) . . . . ? B1 Rh1 S3 C10 28.32(17) . . . . ? P1 Rh1 S3 C10 -68.93(13) . . . . ? S1 Rh1 S3 C10 25.5(3) . . . . ? S2 Rh1 S3 C10 116.75(13) . . . . ? C6 N3 B1 N1 -108.1(4) . . . . ? C8 N3 B1 N1 67.7(5) . . . . ? C6 N3 B1 N5 125.8(3) . . . . ? C8 N3 B1 N5 -58.4(5) . . . . ? C6 N3 B1 Rh1 9.6(4) . . . . ? C8 N3 B1 Rh1 -174.6(3) . . . . ? C2 N1 B1 N3 98.1(4) . . . . ? C4 N1 B1 N3 -66.6(5) . . . . ? C2 N1 B1 N5 -139.2(3) . . . . ? C4 N1 B1 N5 56.1(5) . . . . ? C2 N1 B1 Rh1 -19.8(4) . . . . ? C4 N1 B1 Rh1 175.4(3) . . . . ? C10 N5 B1 N3 -79.0(4) . . . . ? C12 N5 B1 N3 85.6(5) . . . . ? C10 N5 B1 N1 158.5(3) . . . . ? C12 N5 B1 N1 -37.0(6) . . . . ? C10 N5 B1 Rh1 38.4(4) . . . . ? C12 N5 B1 Rh1 -157.1(3) . . . . ? P1 Rh1 B1 N3 171.3(2) . . . . ? S1 Rh1 B1 N3 -100.3(2) . . . . ? S3 Rh1 B1 N3 80.1(2) . . . . ? S2 Rh1 B1 N3 -10.8(2) . . . . ? P1 Rh1 B1 N1 -70.6(2) . . . . ? S1 Rh1 B1 N1 17.8(2) . . . . ? S3 Rh1 B1 N1 -161.8(2) . . . . ? S2 Rh1 B1 N1 107.3(2) . . . . ? P1 Rh1 B1 N5 53.6(2) . . . . ? S1 Rh1 B1 N5 142.1(2) . . . . ? S3 Rh1 B1 N5 -37.5(2) . . . . ? S2 Rh1 B1 N5 -128.4(2) . . . . ? C4 N1 C2 N2 -0.9(4) . . . . ? B1 N1 C2 N2 -168.7(3) . . . . ? C4 N1 C2 S1 176.5(3) . . . . ? B1 N1 C2 S1 8.7(5) . . . . ? C3 N2 C2 N1 1.1(4) . . . . ? C5 N2 C2 N1 -175.1(3) . . . . ? C3 N2 C2 S1 -176.2(3) . . . . ? C5 N2 C2 S1 7.6(5) . . . . ? Rh1 S1 C2 N1 5.8(3) . . . . ? Rh1 S1 C2 N2 -177.3(3) . . . . ? C2 N2 C3 C4 -0.9(4) . . . . ? C5 N2 C3 C4 175.1(3) . . . . ? N2 C3 C4 N1 0.4(4) . . . . ? C2 N1 C4 C3 0.3(4) . . . . ? B1 N1 C4 C3 166.3(3) . . . . ? C7 N4 C6 N3 0.0(4) . . . . ? C9 N4 C6 N3 178.9(3) . . . . ? C7 N4 C6 S2 176.5(3) . . . . ? C9 N4 C6 S2 -4.6(6) . . . . ? C8 N3 C6 N4 0.1(4) . . . . ? B1 N3 C6 N4 176.6(3) . . . . ? C8 N3 C6 S2 -176.7(3) . . . . ? B1 N3 C6 S2 -0.1(5) . . . . ? Rh1 S2 C6 N4 176.2(3) . . . . ? Rh1 S2 C6 N3 -7.8(3) . . . . ? C6 N4 C7 C8 0.0(4) . . . . ? C9 N4 C7 C8 -178.9(3) . . . . ? N4 C7 C8 N3 0.1(4) . . . . ? C6 N3 C8 C7 -0.1(4) . . . . ? B1 N3 C8 C7 -176.4(3) . . . . ? C11 N6 C10 N5 -0.5(4) . . . . ? C14 N6 C10 N5 -177.2(3) . . . . ? C11 N6 C10 S3 -179.9(3) . . . . ? C14 N6 C10 S3 3.4(6) . . . . ? C12 N5 C10 N6 0.6(4) . . . . ? B1 N5 C10 N6 169.2(3) . . . . ? C12 N5 C10 S3 180.0(3) . . . . ? B1 N5 C10 S3 -11.4(4) . . . . ? Rh1 S3 C10 N6 162.2(3) . . . . ? Rh1 S3 C10 N5 -17.0(3) . . . . ? C10 N6 C11 C12 0.2(4) . . . . ? C14 N6 C11 C12 176.9(3) . . . . ? N6 C11 C12 N5 0.1(4) . . . . ? C10 N5 C12 C11 -0.4(4) . . . . ? B1 N5 C12 C11 -165.8(4) . . . . ? C26 P1 C13 C19 54.6(3) . . . . ? C20 P1 C13 C19 -54.7(3) . . . . ? Rh1 P1 C13 C19 -179.7(3) . . . . ? C26 P1 C13 C15 -124.3(3) . . . . ? C20 P1 C13 C15 126.4(3) . . . . ? Rh1 P1 C13 C15 1.3(3) . . . . ? C19 C13 C15 C16 0.8(6) . . . . ? P1 C13 C15 C16 179.8(3) . . . . ? C13 C15 C16 C17 0.2(6) . . . . ? C15 C16 C17 C18 -0.7(7) . . . . ? C16 C17 C18 C19 0.2(6) . . . . ? C17 C18 C19 C13 0.8(6) . . . . ? C15 C13 C19 C18 -1.3(6) . . . . ? P1 C13 C19 C18 179.8(3) . . . . ? C13 P1 C20 C21 168.6(3) . . . . ? C26 P1 C20 C21 62.9(3) . . . . ? Rh1 P1 C20 C21 -75.1(3) . . . . ? C13 P1 C20 C25 -16.1(3) . . . . ? C26 P1 C20 C25 -121.8(3) . . . . ? Rh1 P1 C20 C25 100.2(3) . . . . ? C25 C20 C21 C22 2.0(5) . . . . ? P1 C20 C21 C22 177.5(3) . . . . ? C20 C21 C22 C23 -2.6(6) . . . . ? C21 C22 C23 C24 1.4(6) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C23 C24 C25 C20 -1.0(6) . . . . ? C21 C20 C25 C24 -0.2(5) . . . . ? P1 C20 C25 C24 -175.6(3) . . . . ? C13 P1 C26 C27 -142.5(3) . . . . ? C20 P1 C26 C27 -34.7(4) . . . . ? Rh1 P1 C26 C27 102.4(3) . . . . ? C13 P1 C26 C31 41.1(3) . . . . ? C20 P1 C26 C31 148.8(3) . . . . ? Rh1 P1 C26 C31 -74.0(3) . . . . ? C31 C26 C27 C28 1.2(6) . . . . ? P1 C26 C27 C28 -175.2(3) . . . . ? C26 C27 C28 C29 -2.4(6) . . . . ? C27 C28 C29 C30 1.6(6) . . . . ? C28 C29 C30 C31 0.2(6) . . . . ? C29 C30 C31 C26 -1.4(6) . . . . ? C27 C26 C31 C30 0.6(6) . . . . ? P1 C26 C31 C30 177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.152 data_9 _database_code_depnum_ccdc_archive 'CCDC 761321' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 B2 F2 N12 Rh S6, 3(C H2 Cl2), F6 P' _chemical_formula_sum 'C27 H36 B2 Cl6 F8 N12 P Rh S6' _chemical_formula_weight 1241.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0886(4) _cell_length_b 10.6024(4) _cell_length_c 23.2459(8) _cell_angle_alpha 102.385(2) _cell_angle_beta 95.605(2) _cell_angle_gamma 100.385(2) _cell_volume 2364.64(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9414 _cell_measurement_theta_min 2.787 _cell_measurement_theta_max 30.5495 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details 'Sadabs - Bruker 2007' _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 Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 93913 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.59 _reflns_number_total 14420 _reflns_number_gt 11975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _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^)+(0.0368P)^2^+6.8049P] 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 14420 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 1.0000 0.0000 1.0000 0.01039(6) Uani 1 2 d S . . S1 S 1.09295(6) 0.21530(6) 0.98905(3) 0.01310(11) Uani 1 1 d . . . S2 S 0.92679(6) -0.09163(6) 0.89669(3) 0.01361(11) Uani 1 1 d . . . S3 S 0.78539(6) 0.04789(6) 1.02106(3) 0.01373(11) Uani 1 1 d . . . B1 B 0.7908(3) 0.1848(3) 0.89867(12) 0.0134(5) Uani 1 1 d . . . F1 F 0.71973(17) 0.24867(17) 0.86325(8) 0.0222(3) Uani 1 1 d . . . N1 N 0.8474(2) 0.2851(2) 0.95851(9) 0.0135(4) Uani 1 1 d . . . N2 N 0.9543(2) 0.3907(2) 1.04636(10) 0.0148(4) Uani 1 1 d . . . N3 N 0.9057(2) 0.1421(2) 0.86419(9) 0.0131(4) Uani 1 1 d . . . N4 N 1.0660(2) 0.0494(2) 0.82848(10) 0.0168(4) Uani 1 1 d . . . N5 N 0.6879(2) 0.0650(2) 0.90699(10) 0.0145(4) Uani 1 1 d . . . N6 N 0.5747(2) -0.0974(2) 0.93789(10) 0.0170(4) Uani 1 1 d . . . C2 C 0.9608(2) 0.2978(2) 0.99750(11) 0.0125(4) Uani 1 1 d . . . C3 C 0.8368(3) 0.4377(3) 1.03874(12) 0.0184(5) Uani 1 1 d . . . H3 H 0.8084 0.5040 1.0663 0.022 Uiso 1 1 calc R . . C4 C 0.7699(3) 0.3715(3) 0.98450(12) 0.0174(5) Uani 1 1 d . . . H4 H 0.6847 0.3821 0.9671 0.021 Uiso 1 1 calc R . . C5 C 1.0537(3) 0.4316(3) 1.10037(11) 0.0189(5) Uani 1 1 d . . . H5A H 1.0984 0.3586 1.1045 0.028 Uiso 1 1 calc R . . H5B H 1.0073 0.4557 1.1350 0.028 Uiso 1 1 calc R . . H5C H 1.1220 0.5079 1.0978 0.028 Uiso 1 1 calc R . . C6 C 0.9658(3) 0.0375(2) 0.86289(11) 0.0137(4) Uani 1 1 d . . . C7 C 1.0700(3) 0.1630(3) 0.80817(12) 0.0180(5) Uani 1 1 d . . . H7 H 1.1304 0.1944 0.7831 0.022 Uiso 1 1 calc R . . C8 C 0.9716(3) 0.2209(2) 0.83081(11) 0.0158(5) Uani 1 1 d . . . H8 H 0.9511 0.3016 0.8249 0.019 Uiso 1 1 calc R . . C9 C 1.1547(3) -0.0434(3) 0.81433(14) 0.0260(6) Uani 1 1 d . . . H9A H 1.2119 -0.0443 0.8507 0.039 Uiso 1 1 calc R . . H9B H 1.2126 -0.0165 0.7858 0.039 Uiso 1 1 calc R . . H9C H 1.0993 -0.1319 0.7969 0.039 Uiso 1 1 calc R . . C10 C 0.6827(2) 0.0057(2) 0.95325(11) 0.0139(4) Uani 1 1 d . . . C11 C 0.5126(3) -0.1051(3) 0.88128(13) 0.0206(5) Uani 1 1 d . . . H11 H 0.4351 -0.1687 0.8598 0.025 Uiso 1 1 calc R . . C12 C 0.5833(3) -0.0048(3) 0.86232(12) 0.0192(5) Uani 1 1 d . . . H12 H 0.5643 0.0145 0.8247 0.023 Uiso 1 1 calc R . . C13 C 0.5330(3) -0.1872(3) 0.97537(14) 0.0216(5) Uani 1 1 d . . . H13A H 0.6015 -0.2407 0.9794 0.032 Uiso 1 1 calc R . . H13B H 0.4452 -0.2451 0.9571 0.032 Uiso 1 1 calc R . . H13C H 0.5242 -0.1361 1.0148 0.032 Uiso 1 1 calc R . . C14 C 0.4466(3) 1.1404(3) 0.38852(11) 0.0157(5) Uani 1 1 d . . . Rh2 Rh 0.5000 1.0000 0.5000 0.01146(6) Uani 1 2 d S . . S4 S 0.35054(6) 1.08157(6) 0.43825(3) 0.01496(11) Uani 1 1 d . . . S5 S 0.44565(6) 0.77817(6) 0.44147(3) 0.01455(11) Uani 1 1 d . . . S6 S 0.69957(6) 1.06450(6) 0.45726(3) 0.01449(11) Uani 1 1 d . . . B2 B 0.4956(3) 0.9225(3) 0.32305(13) 0.0174(5) Uani 1 1 d . . . F2 F 0.49578(19) 0.89489(18) 0.26138(7) 0.0249(4) Uani 1 1 d . . . N7 N 0.4999(2) 1.0718(2) 0.34367(10) 0.0159(4) Uani 1 1 d . . . N8 N 0.4806(2) 1.2693(2) 0.38802(10) 0.0189(4) Uani 1 1 d . . . N9 N 0.3631(2) 0.8395(2) 0.33455(10) 0.0171(4) Uani 1 1 d . . . N10 N 0.2049(2) 0.7176(2) 0.36804(10) 0.0187(4) Uani 1 1 d . . . N11 N 0.6214(2) 0.8797(2) 0.34960(10) 0.0167(4) Uani 1 1 d . . . N12 N 0.7861(2) 0.8414(2) 0.40681(10) 0.0194(4) Uani 1 1 d . . . C15 C 0.5571(3) 1.2829(3) 0.34276(13) 0.0229(5) Uani 1 1 d . . . H15 H 0.5939 1.3630 0.3327 0.028 Uiso 1 1 calc R . . C16 C 0.5694(3) 1.1604(3) 0.31547(12) 0.0210(5) Uani 1 1 d . . . H16 H 0.6173 1.1388 0.2827 0.025 Uiso 1 1 calc R . . C17 C 0.4404(4) 1.3769(3) 0.42820(15) 0.0304(7) Uani 1 1 d . . . H17A H 0.3420 1.3702 0.4194 0.046 Uiso 1 1 calc R . . H17B H 0.4887 1.4615 0.4228 0.046 Uiso 1 1 calc R . . H17C H 0.4635 1.3714 0.4694 0.046 Uiso 1 1 calc R . . C18 C 0.3370(3) 0.7797(2) 0.37937(11) 0.0154(4) Uani 1 1 d . . . C19 C 0.1455(3) 0.7398(3) 0.31583(13) 0.0237(6) Uani 1 1 d . . . H19 H 0.0535 0.7077 0.2977 0.028 Uiso 1 1 calc R . . C20 C 0.2438(3) 0.8157(3) 0.29582(13) 0.0228(5) Uani 1 1 d . . . H20 H 0.2329 0.8476 0.2608 0.027 Uiso 1 1 calc R . . C21 C 0.1381(3) 0.6340(3) 0.40342(14) 0.0252(6) Uani 1 1 d . . . H21A H 0.1798 0.5569 0.4017 0.038 Uiso 1 1 calc R . . H21B H 0.0411 0.6049 0.3876 0.038 Uiso 1 1 calc R . . H21C H 0.1485 0.6841 0.4448 0.038 Uiso 1 1 calc R . . C22 C 0.7020(3) 0.9256(2) 0.40278(11) 0.0150(4) Uani 1 1 d . . . C23 C 0.7579(3) 0.7403(3) 0.35623(13) 0.0245(6) Uani 1 1 d . . . H23 H 0.8021 0.6679 0.3478 0.029 Uiso 1 1 calc R . . C24 C 0.6555(3) 0.7638(3) 0.32101(13) 0.0224(5) Uani 1 1 d . . . H24 H 0.6139 0.7101 0.2831 0.027 Uiso 1 1 calc R . . C25 C 0.8918(3) 0.8521(3) 0.45589(14) 0.0272(6) Uani 1 1 d . . . H25A H 0.9810 0.8841 0.4450 0.041 Uiso 1 1 calc R . . H25B H 0.8890 0.7652 0.4645 0.041 Uiso 1 1 calc R . . H25C H 0.8765 0.9142 0.4912 0.041 Uiso 1 1 calc R . . P1 P 0.80012(7) 0.42789(7) 0.23485(3) 0.01656(13) Uani 1 1 d . . . F3 F 0.7521(2) 0.3932(2) 0.16483(8) 0.0312(4) Uani 1 1 d . . . F4 F 0.8583(2) 0.57818(18) 0.23335(9) 0.0335(4) Uani 1 1 d . . . F5 F 0.94414(19) 0.3922(2) 0.22458(9) 0.0317(4) Uani 1 1 d . . . F6 F 0.8469(2) 0.46354(19) 0.30562(8) 0.0296(4) Uani 1 1 d . . . F7 F 0.7398(2) 0.27877(17) 0.23653(9) 0.0288(4) Uani 1 1 d . . . F8 F 0.65589(19) 0.46487(19) 0.24666(8) 0.0279(4) Uani 1 1 d . . . C26 C 0.2885(5) 0.3188(4) 0.23436(17) 0.0458(10) Uani 1 1 d . . . H26A H 0.3722 0.2963 0.2197 0.055 Uiso 1 1 calc R . . H26B H 0.2238 0.3193 0.1996 0.055 Uiso 1 1 calc R . . Cl3 Cl 0.21559(10) 0.19762(11) 0.27021(4) 0.0457(2) Uani 1 1 d . . . Cl4 Cl 0.32873(11) 0.47664(10) 0.28268(5) 0.0497(2) Uani 1 1 d . . . C27 C 0.5339(3) 0.6190(3) 0.15437(14) 0.0286(6) Uani 1 1 d . . . H27A H 0.4849 0.6813 0.1772 0.034 Uiso 1 1 calc R . . H27B H 0.6052 0.6026 0.1826 0.034 Uiso 1 1 calc R . . Cl5 Cl 0.41850(10) 0.46883(9) 0.12073(4) 0.0404(2) Uani 1 1 d . . . Cl6 Cl 0.61094(10) 0.69043(12) 0.10078(5) 0.0471(2) Uani 1 1 d . . . C28 C 0.9312(5) 0.2304(6) 0.3691(3) 0.0665(16) Uani 1 1 d . . . H28A H 0.9515 0.2741 0.3365 0.080 Uiso 1 1 calc R . . H28B H 0.8312 0.2105 0.3681 0.080 Uiso 1 1 calc R . . Cl7 Cl 0.99072(16) 0.07926(19) 0.35692(10) 0.1002(7) Uani 1 1 d . . . Cl8 Cl 1.0049(2) 0.3373(2) 0.43639(8) 0.1139(8) 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 0.01017(11) 0.00929(11) 0.01209(11) 0.00398(8) 0.00074(9) 0.00175(9) S1 0.0118(3) 0.0111(2) 0.0168(3) 0.0053(2) 0.0011(2) 0.0013(2) S2 0.0173(3) 0.0100(2) 0.0138(3) 0.0041(2) 0.0007(2) 0.0025(2) S3 0.0121(3) 0.0154(3) 0.0154(3) 0.0064(2) 0.0024(2) 0.0037(2) B1 0.0121(12) 0.0130(11) 0.0159(12) 0.0061(9) 0.0003(9) 0.0023(9) F1 0.0219(8) 0.0226(8) 0.0240(8) 0.0095(6) -0.0006(6) 0.0073(7) N1 0.0145(10) 0.0110(9) 0.0165(9) 0.0053(7) 0.0026(8) 0.0041(7) N2 0.0188(10) 0.0101(9) 0.0158(9) 0.0048(7) 0.0037(8) 0.0013(8) N3 0.0142(9) 0.0108(9) 0.0141(9) 0.0037(7) -0.0001(7) 0.0019(7) N4 0.0200(11) 0.0157(10) 0.0177(10) 0.0070(8) 0.0062(8) 0.0058(8) N5 0.0113(9) 0.0143(9) 0.0173(10) 0.0053(8) -0.0012(8) 0.0008(8) N6 0.0123(10) 0.0150(10) 0.0244(11) 0.0075(8) 0.0015(8) 0.0013(8) C2 0.0127(10) 0.0100(10) 0.0152(10) 0.0048(8) 0.0024(8) 0.0007(8) C3 0.0206(12) 0.0157(11) 0.0224(12) 0.0069(9) 0.0092(10) 0.0070(10) C4 0.0180(12) 0.0167(11) 0.0216(12) 0.0090(9) 0.0070(10) 0.0070(9) C5 0.0256(13) 0.0143(11) 0.0150(11) 0.0029(9) 0.0013(10) 0.0011(10) C6 0.0147(11) 0.0124(10) 0.0127(10) 0.0027(8) -0.0001(8) 0.0011(8) C7 0.0207(12) 0.0170(11) 0.0184(11) 0.0080(9) 0.0055(10) 0.0038(10) C8 0.0180(12) 0.0137(11) 0.0164(11) 0.0063(9) 0.0008(9) 0.0025(9) C9 0.0308(16) 0.0266(14) 0.0304(15) 0.0132(12) 0.0157(12) 0.0169(12) C10 0.0120(10) 0.0128(10) 0.0187(11) 0.0053(9) 0.0034(9) 0.0044(8) C11 0.0160(12) 0.0191(12) 0.0248(13) 0.0056(10) -0.0031(10) 0.0012(10) C12 0.0165(12) 0.0203(12) 0.0194(12) 0.0054(10) -0.0037(9) 0.0021(10) C13 0.0160(12) 0.0196(12) 0.0321(15) 0.0129(11) 0.0067(11) 0.0013(10) C14 0.0138(11) 0.0188(12) 0.0154(11) 0.0064(9) 0.0000(9) 0.0037(9) Rh2 0.01159(12) 0.01197(12) 0.01065(11) 0.00316(9) 0.00111(9) 0.00172(9) S4 0.0142(3) 0.0176(3) 0.0146(3) 0.0061(2) 0.0019(2) 0.0044(2) S5 0.0162(3) 0.0133(3) 0.0137(3) 0.0035(2) 0.0004(2) 0.0023(2) S6 0.0137(3) 0.0146(3) 0.0142(3) 0.0025(2) 0.0026(2) 0.0011(2) B2 0.0192(13) 0.0193(13) 0.0131(12) 0.0039(10) 0.0017(10) 0.0031(11) F2 0.0297(9) 0.0299(9) 0.0141(7) 0.0046(6) 0.0031(6) 0.0045(7) N7 0.0153(10) 0.0188(10) 0.0150(9) 0.0074(8) 0.0025(8) 0.0025(8) N8 0.0222(11) 0.0163(10) 0.0193(10) 0.0071(8) 0.0028(9) 0.0031(9) N9 0.0182(11) 0.0169(10) 0.0144(10) 0.0036(8) -0.0017(8) 0.0010(8) N10 0.0154(10) 0.0189(10) 0.0208(11) 0.0051(8) 0.0000(8) 0.0018(8) N11 0.0181(10) 0.0177(10) 0.0144(9) 0.0024(8) 0.0043(8) 0.0050(8) N12 0.0175(11) 0.0205(11) 0.0201(11) 0.0027(9) 0.0027(8) 0.0058(9) C15 0.0235(14) 0.0225(13) 0.0244(13) 0.0125(11) 0.0035(11) 0.0006(11) C16 0.0191(13) 0.0256(13) 0.0197(12) 0.0114(10) 0.0032(10) 0.0010(10) C17 0.046(2) 0.0183(13) 0.0293(15) 0.0064(11) 0.0103(14) 0.0085(13) C18 0.0155(11) 0.0128(10) 0.0171(11) 0.0021(8) 0.0009(9) 0.0031(9) C19 0.0171(13) 0.0272(14) 0.0243(13) 0.0067(11) -0.0041(10) 0.0010(11) C20 0.0208(13) 0.0274(14) 0.0183(12) 0.0064(10) -0.0044(10) 0.0026(11) C21 0.0175(13) 0.0272(14) 0.0311(15) 0.0125(12) 0.0032(11) -0.0014(11) C22 0.0141(11) 0.0146(11) 0.0170(11) 0.0052(9) 0.0047(9) 0.0017(9) C23 0.0257(14) 0.0213(13) 0.0248(14) -0.0016(11) 0.0034(11) 0.0092(11) C24 0.0252(14) 0.0203(13) 0.0190(12) -0.0017(10) 0.0040(10) 0.0048(11) C25 0.0221(14) 0.0296(15) 0.0290(15) 0.0031(12) -0.0032(11) 0.0118(12) P1 0.0188(3) 0.0137(3) 0.0173(3) 0.0055(2) 0.0031(2) 0.0013(2) F3 0.0314(10) 0.0408(11) 0.0174(8) 0.0055(7) 0.0024(7) -0.0008(8) F4 0.0370(11) 0.0181(8) 0.0429(11) 0.0160(8) -0.0042(9) -0.0055(7) F5 0.0213(9) 0.0414(11) 0.0385(11) 0.0169(9) 0.0115(8) 0.0101(8) F6 0.0412(11) 0.0300(9) 0.0178(8) 0.0040(7) -0.0014(7) 0.0131(8) F7 0.0348(10) 0.0149(8) 0.0394(10) 0.0085(7) 0.0171(8) 0.0031(7) F8 0.0264(9) 0.0318(9) 0.0317(9) 0.0123(8) 0.0088(7) 0.0141(8) C26 0.067(3) 0.0331(19) 0.0280(17) 0.0068(14) -0.0002(17) -0.0085(18) Cl3 0.0386(5) 0.0564(6) 0.0362(4) 0.0200(4) -0.0061(4) -0.0104(4) Cl4 0.0494(6) 0.0338(5) 0.0623(6) -0.0019(4) 0.0101(5) 0.0140(4) C27 0.0320(16) 0.0321(16) 0.0234(14) 0.0069(12) 0.0003(12) 0.0128(13) Cl5 0.0406(5) 0.0308(4) 0.0475(5) 0.0092(4) -0.0038(4) 0.0072(4) Cl6 0.0339(5) 0.0636(6) 0.0503(5) 0.0315(5) 0.0047(4) 0.0061(4) C28 0.039(2) 0.084(4) 0.083(4) 0.055(3) -0.012(2) -0.001(2) Cl7 0.0704(9) 0.1234(14) 0.1701(18) 0.1185(14) 0.0735(11) 0.0531(9) Cl8 0.1181(14) 0.1148(14) 0.0868(11) 0.0762(11) -0.0404(10) -0.0663(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 S2 2.3771(6) 2_757 ? Rh1 S2 2.3772(6) . yes Rh1 S1 2.3831(6) 2_757 ? Rh1 S1 2.3831(6) . yes Rh1 S3 2.3837(6) . yes Rh1 S3 2.3837(6) 2_757 ? S1 C2 1.726(2) . yes S2 C6 1.725(3) . yes S3 C10 1.723(3) . yes B1 F1 1.397(3) . yes B1 N1 1.544(3) . yes B1 N5 1.548(3) . yes B1 N3 1.551(3) . yes N1 C2 1.356(3) . ? N1 C4 1.388(3) . ? N2 C2 1.350(3) . ? N2 C3 1.376(3) . ? N2 C5 1.461(3) . ? N3 C6 1.353(3) . ? N3 C8 1.386(3) . ? N4 C6 1.353(3) . ? N4 C7 1.380(3) . ? N4 C9 1.454(3) . ? N5 C10 1.358(3) . ? N5 C12 1.384(3) . ? N6 C10 1.354(3) . ? N6 C11 1.380(4) . ? N6 C13 1.458(3) . ? C3 C4 1.350(4) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.350(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.350(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N8 1.350(3) . ? C14 N7 1.353(3) . ? C14 S4 1.725(3) . yes Rh2 S4 2.3794(6) 2_676 ? Rh2 S4 2.3794(6) . yes Rh2 S6 2.3862(6) . yes Rh2 S6 2.3863(6) 2_676 ? Rh2 S5 2.3875(6) 2_676 ? Rh2 S5 2.3875(6) . yes S5 C18 1.730(3) . yes S6 C22 1.730(3) . yes B2 F2 1.400(3) . yes B2 N11 1.540(4) . yes B2 N9 1.543(4) . yes B2 N7 1.543(4) . yes N7 C16 1.386(3) . ? N8 C15 1.381(4) . ? N8 C17 1.457(4) . ? N9 C18 1.355(3) . ? N9 C20 1.380(3) . ? N10 C18 1.349(3) . ? N10 C19 1.385(4) . ? N10 C21 1.456(4) . ? N11 C22 1.352(3) . ? N11 C24 1.385(3) . ? N12 C22 1.349(3) . ? N12 C23 1.378(4) . ? N12 C25 1.454(4) . ? C15 C16 1.351(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.346(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.347(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? P1 F5 1.5933(19) . ? P1 F3 1.5949(19) . ? P1 F7 1.5988(18) . ? P1 F4 1.6047(18) . ? P1 F8 1.6075(19) . ? P1 F6 1.6093(19) . ? C26 Cl4 1.757(4) . ? C26 Cl3 1.768(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 Cl6 1.764(3) . ? C27 Cl5 1.767(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 Cl8 1.730(6) . ? C28 Cl7 1.787(6) . ? C28 H28A 0.9900 . ? C28 H28B 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 S2 Rh1 S2 180.0 2_757 . yes S2 Rh1 S1 95.13(2) 2_757 2_757 ? S2 Rh1 S1 84.87(2) . 2_757 ? S2 Rh1 S1 84.87(2) 2_757 . ? S2 Rh1 S1 95.13(2) . . yes S1 Rh1 S1 179.999(12) 2_757 . ? S2 Rh1 S3 85.03(2) 2_757 . ? S2 Rh1 S3 94.97(2) . . yes S1 Rh1 S3 84.94(2) 2_757 . ? S1 Rh1 S3 95.06(2) . . yes S2 Rh1 S3 94.96(2) 2_757 2_757 ? S2 Rh1 S3 85.04(2) . 2_757 ? S1 Rh1 S3 95.06(2) 2_757 2_757 ? S1 Rh1 S3 84.94(2) . 2_757 ? S3 Rh1 S3 180.00(3) . 2_757 ? C2 S1 Rh1 104.03(8) . . yes C6 S2 Rh1 105.47(8) . . yes C10 S3 Rh1 105.53(9) . . yes F1 B1 N1 107.2(2) . . ? F1 B1 N5 107.1(2) . . ? N1 B1 N5 111.6(2) . . yes F1 B1 N3 106.2(2) . . ? N1 B1 N3 112.2(2) . . yes N5 B1 N3 112.2(2) . . yes C2 N1 C4 108.2(2) . . ? C2 N1 B1 130.9(2) . . ? C4 N1 B1 120.4(2) . . ? C2 N2 C3 109.8(2) . . ? C2 N2 C5 125.3(2) . . ? C3 N2 C5 124.8(2) . . ? C6 N3 C8 108.3(2) . . ? C6 N3 B1 130.7(2) . . ? C8 N3 B1 120.9(2) . . ? C6 N4 C7 109.4(2) . . ? C6 N4 C9 125.6(2) . . ? C7 N4 C9 125.1(2) . . ? C10 N5 C12 108.2(2) . . ? C10 N5 B1 130.3(2) . . ? C12 N5 B1 121.4(2) . . ? C10 N6 C11 109.6(2) . . ? C10 N6 C13 124.8(2) . . ? C11 N6 C13 125.6(2) . . ? N2 C2 N1 107.1(2) . . ? N2 C2 S1 124.32(19) . . ? N1 C2 S1 128.53(19) . . ? C4 C3 N2 106.7(2) . . ? C4 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C3 C4 N1 108.1(2) . . ? C3 C4 H4 125.9 . . ? N1 C4 H4 125.9 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N4 107.4(2) . . ? N3 C6 S2 128.6(2) . . ? N4 C6 S2 123.99(19) . . ? C8 C7 N4 106.8(2) . . ? C8 C7 H7 126.6 . . ? N4 C7 H7 126.6 . . ? C7 C8 N3 108.1(2) . . ? C7 C8 H8 126.0 . . ? N3 C8 H8 126.0 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 N5 107.2(2) . . ? N6 C10 S3 123.28(19) . . ? N5 C10 S3 129.51(19) . . ? C12 C11 N6 106.6(2) . . ? C12 C11 H11 126.7 . . ? N6 C11 H11 126.7 . . ? C11 C12 N5 108.4(2) . . ? C11 C12 H12 125.8 . . ? N5 C12 H12 125.8 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N8 C14 N7 107.4(2) . . ? N8 C14 S4 124.0(2) . . ? N7 C14 S4 128.6(2) . . ? S4 Rh2 S4 180.0 2_676 . yes S4 Rh2 S6 83.77(2) 2_676 . ? S4 Rh2 S6 96.23(2) . . yes S4 Rh2 S6 96.23(2) 2_676 2_676 ? S4 Rh2 S6 83.77(2) . 2_676 ? S6 Rh2 S6 179.999(1) . 2_676 ? S4 Rh2 S5 95.63(2) 2_676 2_676 ? S4 Rh2 S5 84.37(2) . 2_676 ? S6 Rh2 S5 84.69(2) . 2_676 ? S6 Rh2 S5 95.31(2) 2_676 2_676 ? S4 Rh2 S5 84.37(2) 2_676 . ? S4 Rh2 S5 95.63(2) . . yes S6 Rh2 S5 95.31(2) . . yes S6 Rh2 S5 84.69(2) 2_676 . ? S5 Rh2 S5 179.999(1) 2_676 . ? C14 S4 Rh2 105.96(9) . . yes C18 S5 Rh2 105.71(9) . . yes C22 S6 Rh2 103.37(9) . . yes F2 B2 N11 106.3(2) . . ? F2 B2 N9 107.2(2) . . ? N11 B2 N9 110.9(2) . . yes F2 B2 N7 106.9(2) . . ? N11 B2 N7 113.6(2) . . yes N9 B2 N7 111.5(2) . . yes C14 N7 C16 108.4(2) . . ? C14 N7 B2 130.9(2) . . ? C16 N7 B2 120.7(2) . . ? C14 N8 C15 109.4(2) . . ? C14 N8 C17 125.3(2) . . ? C15 N8 C17 125.3(2) . . ? C18 N9 C20 108.0(2) . . ? C18 N9 B2 131.0(2) . . ? C20 N9 B2 121.0(2) . . ? C18 N10 C19 109.3(2) . . ? C18 N10 C21 125.0(2) . . ? C19 N10 C21 125.6(2) . . ? C22 N11 C24 108.1(2) . . ? C22 N11 B2 131.6(2) . . ? C24 N11 B2 119.6(2) . . ? C22 N12 C23 109.5(2) . . ? C22 N12 C25 126.9(2) . . ? C23 N12 C25 123.6(2) . . ? C16 C15 N8 106.8(2) . . ? C16 C15 H15 126.6 . . ? N8 C15 H15 126.6 . . ? C15 C16 N7 108.0(2) . . ? C15 C16 H16 126.0 . . ? N7 C16 H16 126.0 . . ? N8 C17 H17A 109.5 . . ? N8 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N8 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C18 N9 107.5(2) . . ? N10 C18 S5 123.4(2) . . ? N9 C18 S5 129.0(2) . . ? C20 C19 N10 106.5(2) . . ? C20 C19 H19 126.8 . . ? N10 C19 H19 126.8 . . ? C19 C20 N9 108.7(2) . . ? C19 C20 H20 125.6 . . ? N9 C20 H20 125.6 . . ? 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 . . ? N12 C22 N11 107.4(2) . . ? N12 C22 S6 125.0(2) . . ? N11 C22 S6 127.6(2) . . ? C24 C23 N12 106.8(2) . . ? C24 C23 H23 126.6 . . ? N12 C23 H23 126.6 . . ? C23 C24 N11 108.2(2) . . ? C23 C24 H24 125.9 . . ? N11 C24 H24 125.9 . . ? N12 C25 H25A 109.5 . . ? N12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? F5 P1 F3 90.98(11) . . ? F5 P1 F7 90.46(11) . . ? F3 P1 F7 90.22(11) . . ? F5 P1 F4 90.51(11) . . ? F3 P1 F4 89.78(11) . . ? F7 P1 F4 179.04(12) . . ? F5 P1 F8 178.81(11) . . ? F3 P1 F8 90.20(11) . . ? F7 P1 F8 89.63(10) . . ? F4 P1 F8 89.41(11) . . ? F5 P1 F6 89.70(11) . . ? F3 P1 F6 179.31(12) . . ? F7 P1 F6 89.86(11) . . ? F4 P1 F6 90.13(11) . . ? F8 P1 F6 89.12(10) . . ? Cl4 C26 Cl3 111.5(2) . . ? Cl4 C26 H26A 109.3 . . ? Cl3 C26 H26A 109.3 . . ? Cl4 C26 H26B 109.3 . . ? Cl3 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? Cl6 C27 Cl5 111.37(18) . . ? Cl6 C27 H27A 109.4 . . ? Cl5 C27 H27A 109.4 . . ? Cl6 C27 H27B 109.4 . . ? Cl5 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? Cl8 C28 Cl7 112.6(3) . . ? Cl8 C28 H28A 109.1 . . ? Cl7 C28 H28A 109.1 . . ? Cl8 C28 H28B 109.1 . . ? Cl7 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Rh1 S1 C2 -87.52(9) 2_757 . . . ? S2 Rh1 S1 C2 92.48(9) . . . . ? S1 Rh1 S1 C2 64(14) 2_757 . . . ? S3 Rh1 S1 C2 -2.98(9) . . . . ? S3 Rh1 S1 C2 177.02(9) 2_757 . . . ? S2 Rh1 S2 C6 -139(34) 2_757 . . . ? S1 Rh1 S2 C6 177.23(9) 2_757 . . . ? S1 Rh1 S2 C6 -2.76(9) . . . . ? S3 Rh1 S2 C6 92.79(9) . . . . ? S3 Rh1 S2 C6 -87.21(9) 2_757 . . . ? S2 Rh1 S3 C10 176.24(9) 2_757 . . . ? S2 Rh1 S3 C10 -3.76(9) . . . . ? S1 Rh1 S3 C10 -88.15(9) 2_757 . . . ? S1 Rh1 S3 C10 91.85(9) . . . . ? S3 Rh1 S3 C10 -149(10) 2_757 . . . ? F1 B1 N1 C2 -150.1(2) . . . . ? N5 B1 N1 C2 93.0(3) . . . . ? N3 B1 N1 C2 -33.8(3) . . . . ? F1 B1 N1 C4 39.0(3) . . . . ? N5 B1 N1 C4 -77.9(3) . . . . ? N3 B1 N1 C4 155.3(2) . . . . ? F1 B1 N3 C6 -149.1(2) . . . . ? N1 B1 N3 C6 94.1(3) . . . . ? N5 B1 N3 C6 -32.4(3) . . . . ? F1 B1 N3 C8 36.0(3) . . . . ? N1 B1 N3 C8 -80.8(3) . . . . ? N5 B1 N3 C8 152.6(2) . . . . ? F1 B1 N5 C10 -149.0(2) . . . . ? N1 B1 N5 C10 -32.0(3) . . . . ? N3 B1 N5 C10 94.9(3) . . . . ? F1 B1 N5 C12 34.3(3) . . . . ? N1 B1 N5 C12 151.3(2) . . . . ? N3 B1 N5 C12 -81.8(3) . . . . ? C3 N2 C2 N1 -0.1(3) . . . . ? C5 N2 C2 N1 177.6(2) . . . . ? C3 N2 C2 S1 179.47(18) . . . . ? C5 N2 C2 S1 -2.9(3) . . . . ? C4 N1 C2 N2 -0.5(3) . . . . ? B1 N1 C2 N2 -172.2(2) . . . . ? C4 N1 C2 S1 -179.99(19) . . . . ? B1 N1 C2 S1 8.3(4) . . . . ? Rh1 S1 C2 N2 106.0(2) . . . . ? Rh1 S1 C2 N1 -74.6(2) . . . . ? C2 N2 C3 C4 0.6(3) . . . . ? C5 N2 C3 C4 -177.0(2) . . . . ? N2 C3 C4 N1 -0.9(3) . . . . ? C2 N1 C4 C3 0.9(3) . . . . ? B1 N1 C4 C3 173.6(2) . . . . ? C8 N3 C6 N4 -1.0(3) . . . . ? B1 N3 C6 N4 -176.5(2) . . . . ? C8 N3 C6 S2 179.7(2) . . . . ? B1 N3 C6 S2 4.3(4) . . . . ? C7 N4 C6 N3 0.5(3) . . . . ? C9 N4 C6 N3 -178.8(3) . . . . ? C7 N4 C6 S2 179.72(19) . . . . ? C9 N4 C6 S2 0.4(4) . . . . ? Rh1 S2 C6 N3 -71.7(2) . . . . ? Rh1 S2 C6 N4 109.2(2) . . . . ? C6 N4 C7 C8 0.3(3) . . . . ? C9 N4 C7 C8 179.6(3) . . . . ? N4 C7 C8 N3 -0.9(3) . . . . ? C6 N3 C8 C7 1.3(3) . . . . ? B1 N3 C8 C7 177.2(2) . . . . ? C11 N6 C10 N5 1.1(3) . . . . ? C13 N6 C10 N5 -179.9(2) . . . . ? C11 N6 C10 S3 179.55(19) . . . . ? C13 N6 C10 S3 -1.4(4) . . . . ? C12 N5 C10 N6 -1.3(3) . . . . ? B1 N5 C10 N6 -178.4(2) . . . . ? C12 N5 C10 S3 -179.6(2) . . . . ? B1 N5 C10 S3 3.3(4) . . . . ? Rh1 S3 C10 N6 111.6(2) . . . . ? Rh1 S3 C10 N5 -70.3(2) . . . . ? C10 N6 C11 C12 -0.5(3) . . . . ? C13 N6 C11 C12 -179.4(3) . . . . ? N6 C11 C12 N5 -0.3(3) . . . . ? C10 N5 C12 C11 1.0(3) . . . . ? B1 N5 C12 C11 178.4(2) . . . . ? N8 C14 S4 Rh2 -112.4(2) . . . . ? N7 C14 S4 Rh2 68.5(2) . . . . ? S4 Rh2 S4 C14 -16(23) 2_676 . . . ? S6 Rh2 S4 C14 3.40(10) . . . . ? S6 Rh2 S4 C14 -176.60(10) 2_676 . . . ? S5 Rh2 S4 C14 87.42(10) 2_676 . . . ? S5 Rh2 S4 C14 -92.58(10) . . . . ? S4 Rh2 S5 C18 -175.16(10) 2_676 . . . ? S4 Rh2 S5 C18 4.84(10) . . . . ? S6 Rh2 S5 C18 -91.97(9) . . . . ? S6 Rh2 S5 C18 88.03(9) 2_676 . . . ? S5 Rh2 S5 C18 -20(13) 2_676 . . . ? S4 Rh2 S6 C22 87.20(9) 2_676 . . . ? S4 Rh2 S6 C22 -92.80(9) . . . . ? S6 Rh2 S6 C22 134(5) 2_676 . . . ? S5 Rh2 S6 C22 -176.53(9) 2_676 . . . ? S5 Rh2 S6 C22 3.47(9) . . . . ? N8 C14 N7 C16 0.7(3) . . . . ? S4 C14 N7 C16 180.0(2) . . . . ? N8 C14 N7 B2 179.4(2) . . . . ? S4 C14 N7 B2 -1.3(4) . . . . ? F2 B2 N7 C14 148.1(3) . . . . ? N11 B2 N7 C14 -95.0(3) . . . . ? N9 B2 N7 C14 31.3(4) . . . . ? F2 B2 N7 C16 -33.3(3) . . . . ? N11 B2 N7 C16 83.6(3) . . . . ? N9 B2 N7 C16 -150.1(2) . . . . ? N7 C14 N8 C15 -0.5(3) . . . . ? S4 C14 N8 C15 -179.8(2) . . . . ? N7 C14 N8 C17 178.4(3) . . . . ? S4 C14 N8 C17 -0.9(4) . . . . ? F2 B2 N9 C18 145.0(3) . . . . ? N11 B2 N9 C18 29.4(4) . . . . ? N7 B2 N9 C18 -98.3(3) . . . . ? F2 B2 N9 C20 -35.3(3) . . . . ? N11 B2 N9 C20 -151.0(2) . . . . ? N7 B2 N9 C20 81.3(3) . . . . ? F2 B2 N11 C22 149.9(3) . . . . ? N9 B2 N11 C22 -93.9(3) . . . . ? N7 B2 N11 C22 32.7(4) . . . . ? F2 B2 N11 C24 -40.5(3) . . . . ? N9 B2 N11 C24 75.7(3) . . . . ? N7 B2 N11 C24 -157.8(2) . . . . ? C14 N8 C15 C16 0.0(3) . . . . ? C17 N8 C15 C16 -178.8(3) . . . . ? N8 C15 C16 N7 0.4(3) . . . . ? C14 N7 C16 C15 -0.7(3) . . . . ? B2 N7 C16 C15 -179.5(2) . . . . ? C19 N10 C18 N9 -0.9(3) . . . . ? C21 N10 C18 N9 175.7(3) . . . . ? C19 N10 C18 S5 178.8(2) . . . . ? C21 N10 C18 S5 -4.6(4) . . . . ? C20 N9 C18 N10 1.3(3) . . . . ? B2 N9 C18 N10 -179.0(3) . . . . ? C20 N9 C18 S5 -178.4(2) . . . . ? B2 N9 C18 S5 1.2(4) . . . . ? Rh2 S5 C18 N10 -113.0(2) . . . . ? Rh2 S5 C18 N9 66.7(2) . . . . ? C18 N10 C19 C20 0.2(3) . . . . ? C21 N10 C19 C20 -176.4(3) . . . . ? N10 C19 C20 N9 0.6(3) . . . . ? C18 N9 C20 C19 -1.2(3) . . . . ? B2 N9 C20 C19 179.1(3) . . . . ? C23 N12 C22 N11 -0.8(3) . . . . ? C25 N12 C22 N11 179.0(3) . . . . ? C23 N12 C22 S6 178.4(2) . . . . ? C25 N12 C22 S6 -1.8(4) . . . . ? C24 N11 C22 N12 1.0(3) . . . . ? B2 N11 C22 N12 171.5(3) . . . . ? C24 N11 C22 S6 -178.1(2) . . . . ? B2 N11 C22 S6 -7.7(4) . . . . ? Rh2 S6 C22 N12 -104.9(2) . . . . ? Rh2 S6 C22 N11 74.2(2) . . . . ? C22 N12 C23 C24 0.2(3) . . . . ? C25 N12 C23 C24 -179.6(3) . . . . ? N12 C23 C24 N11 0.5(3) . . . . ? C22 N11 C24 C23 -0.9(3) . . . . ? B2 N11 C24 C23 -172.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.187 _refine_diff_density_min -2.031 _refine_diff_density_rms 0.117