# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _publ_section_title ; The oxidative activation of a B-H bond: novel route to metallaboratrane complexes ; _publ_contact_author_name 'Professor Neil G Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; _publ_contact_author_email Neil.Connelly@bristol.ac.uk _publ_contact_author_phone '+44 117 928 8162' _publ_contact_author_fax '+44 117 925 1295' loop_ _publ_author_name _publ_author_address 'Adams, C.J.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; 'Blagg, R.J.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; 'Charmant, J.P.H.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; 'Connelly, N.G.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; 'Haddow, M.F.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; 'Orpen, A.G.' ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UK ; data_1 _database_code_depnum_ccdc_archive 'CCDC 603867' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C34 H40 B N9 O P Rh S3, C H2 Cl2' _chemical_formula_sum 'C35 H42 B Cl2 N9 O P Rh S3' _chemical_formula_weight 916.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.122(3) _cell_length_b 13.342(3) _cell_length_c 13.744(3) _cell_angle_alpha 76.38(3) _cell_angle_beta 79.99(3) _cell_angle_gamma 62.36(3) _cell_volume 2065.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4386 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.98 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.473 _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick, 2003)' _exptl_special_details ; A heavilly disordered dichloromethane molecule is present in the asymmetric unit attempts to sensibly model this molecule failed and a diffuse solvent correction has been applied to the intensity data using the SQUEEZE routine of the PLATON program suite. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23687 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9439 _reflns_number_gt 7144 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT v6.28A (Bruker-AXS, 2000)' _computing_data_reduction ; SAINT v6.28A and SHELXTL v6.1 (Bruker-AXS, 2000) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v6.1 (Bruker-AXS, 2000)' _computing_publication_material 'SHELXTL v6.1 (Bruker-AXS, 2000)' _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^)+(0.0656P)^2^] 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_number_reflns 9439 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 B1 B 0.8091(3) 0.4399(3) 0.2040(3) 0.0182(8) Uani 1 1 d . . . H1 H 0.7827 0.5229 0.2053 0.022 Uiso 1 1 calc R . . C1 C 0.7358(3) 0.7686(3) 0.3107(3) 0.0205(7) Uani 1 1 d . . . C2 C 0.9188(3) 0.3951(3) 0.3628(3) 0.0177(7) Uani 1 1 d . . . C3 C 1.0041(3) 0.2073(3) 0.3713(3) 0.0234(8) Uani 1 1 d . . . C4 C 1.0802(4) 0.0829(3) 0.4066(4) 0.0364(10) Uani 1 1 d . . . H4A H 1.0671 0.0359 0.3696 0.055 Uiso 1 1 calc R . . H4B H 1.0621 0.0622 0.4785 0.055 Uiso 1 1 calc R . . H4C H 1.1611 0.0690 0.3948 0.055 Uiso 1 1 calc R . . C5 C 1.0724(4) 0.2850(4) 0.4859(3) 0.0359(10) Uani 1 1 d . . . H5A H 1.0925 0.2117 0.5341 0.043 Uiso 1 1 calc R . . H5B H 1.0313 0.3490 0.5240 0.043 Uiso 1 1 calc R . . C6 C 1.1847(4) 0.2895(4) 0.4294(4) 0.0440(12) Uani 1 1 d . . . H6A H 1.2256 0.2254 0.3925 0.066 Uiso 1 1 calc R . . H6B H 1.2345 0.2836 0.4781 0.066 Uiso 1 1 calc R . . H6C H 1.1644 0.3624 0.3822 0.066 Uiso 1 1 calc R . . C7 C 0.8494(4) 0.4585(3) 0.0097(3) 0.0257(8) Uani 1 1 d . . . C8 C 1.0332(4) 0.3404(4) 0.0083(3) 0.0330(10) Uani 1 1 d . . . C9 C 1.1541(4) 0.2722(5) -0.0306(4) 0.0454(12) Uani 1 1 d . . . H9A H 1.1931 0.3219 -0.0517 0.068 Uiso 1 1 calc R . . H9B H 1.1533 0.2410 -0.0882 0.068 Uiso 1 1 calc R . . H9C H 1.1953 0.2089 0.0224 0.068 Uiso 1 1 calc R . . C10 C 0.9556(4) 0.4393(4) -0.1612(3) 0.0352(10) Uani 1 1 d . . . H10A H 1.0334 0.4340 -0.1843 0.042 Uiso 1 1 calc R . . H10B H 0.8983 0.5189 -0.1845 0.042 Uiso 1 1 calc R . . C11 C 0.9365(4) 0.3572(4) -0.2066(3) 0.0361(10) Uani 1 1 d . . . H11A H 0.9945 0.2784 -0.1851 0.054 Uiso 1 1 calc R . . H11B H 0.9434 0.3771 -0.2800 0.054 Uiso 1 1 calc R . . H11C H 0.8593 0.3627 -0.1843 0.054 Uiso 1 1 calc R . . C12 C 0.6227(3) 0.4442(3) 0.2971(2) 0.0157(7) Uani 1 1 d . . . C13 C 0.5977(3) 0.3340(3) 0.2170(3) 0.0189(7) Uani 1 1 d . . . C14 C 0.5474(4) 0.2655(3) 0.1904(3) 0.0280(9) Uani 1 1 d . . . H14A H 0.5959 0.2258 0.1357 0.042 Uiso 1 1 calc R . . H14B H 0.4695 0.3168 0.1688 0.042 Uiso 1 1 calc R . . H14C H 0.5435 0.2088 0.2491 0.042 Uiso 1 1 calc R . . C15 C 0.4541(3) 0.4006(3) 0.3659(3) 0.0231(8) Uani 1 1 d . . . H15A H 0.4643 0.4154 0.4300 0.028 Uiso 1 1 calc R . . H15B H 0.4511 0.3258 0.3797 0.028 Uiso 1 1 calc R . . C16 C 0.3412(4) 0.4943(3) 0.3266(3) 0.0327(9) Uani 1 1 d . . . H16A H 0.3442 0.5684 0.3115 0.049 Uiso 1 1 calc R . . H16B H 0.2778 0.4976 0.3775 0.049 Uiso 1 1 calc R . . H16C H 0.3283 0.4775 0.2653 0.049 Uiso 1 1 calc R . . C17 C 0.4320(3) 0.7540(3) 0.2103(3) 0.0207(8) Uani 1 1 d . . . C18 C 0.4945(4) 0.6724(3) 0.1487(3) 0.0220(8) Uani 1 1 d . . . H18 H 0.5763 0.6335 0.1484 0.026 Uiso 1 1 calc R . . C19 C 0.4384(4) 0.6471(3) 0.0875(3) 0.0297(9) Uani 1 1 d . . . H19 H 0.4816 0.5903 0.0467 0.036 Uiso 1 1 calc R . . C20 C 0.3199(4) 0.7050(4) 0.0863(3) 0.0383(11) Uani 1 1 d . . . H20 H 0.2813 0.6876 0.0451 0.046 Uiso 1 1 calc R . . C21 C 0.2573(4) 0.7884(4) 0.1452(4) 0.0390(11) Uani 1 1 d . . . H21 H 0.1758 0.8288 0.1436 0.047 Uiso 1 1 calc R . . C22 C 0.3129(4) 0.8134(4) 0.2066(3) 0.0310(9) Uani 1 1 d . . . H22 H 0.2694 0.8714 0.2462 0.037 Uiso 1 1 calc R . . C23 C 0.4195(3) 0.8254(3) 0.3978(3) 0.0201(7) Uani 1 1 d . . . C24 C 0.3476(3) 0.7745(3) 0.4413(3) 0.0287(9) Uani 1 1 d . . . H24 H 0.3422 0.7214 0.4093 0.034 Uiso 1 1 calc R . . C25 C 0.2834(4) 0.8004(4) 0.5310(3) 0.0393(11) Uani 1 1 d . . . H25 H 0.2347 0.7646 0.5603 0.047 Uiso 1 1 calc R . . C26 C 0.2894(4) 0.8771(4) 0.5779(3) 0.0461(13) Uani 1 1 d . . . H26 H 0.2441 0.8955 0.6388 0.055 Uiso 1 1 calc R . . C27 C 0.3616(4) 0.9273(4) 0.5362(3) 0.0457(13) Uani 1 1 d . . . H27 H 0.3667 0.9797 0.5691 0.055 Uiso 1 1 calc R . . C28 C 0.4264(4) 0.9026(3) 0.4475(3) 0.0315(9) Uani 1 1 d . . . H28 H 0.4761 0.9377 0.4197 0.038 Uiso 1 1 calc R . . C29 C 0.4936(3) 0.9291(3) 0.2092(3) 0.0224(8) Uani 1 1 d . . . C30 C 0.3908(4) 1.0300(3) 0.2171(3) 0.0303(9) Uani 1 1 d . . . H30 H 0.3315 1.0277 0.2670 0.036 Uiso 1 1 calc R . . C31 C 0.3745(4) 1.1326(3) 0.1534(3) 0.0379(11) Uani 1 1 d . . . H31 H 0.3054 1.2007 0.1601 0.046 Uiso 1 1 calc R . . C32 C 0.4600(4) 1.1345(3) 0.0800(3) 0.0319(10) Uani 1 1 d . . . H32 H 0.4482 1.2040 0.0345 0.038 Uiso 1 1 calc R . . C33 C 0.5614(4) 1.0382(4) 0.0716(3) 0.0317(10) Uani 1 1 d . . . H33 H 0.6200 1.0418 0.0215 0.038 Uiso 1 1 calc R . . C34 C 0.5793(4) 0.9337(3) 0.1368(3) 0.0252(8) Uani 1 1 d . . . H34 H 0.6499 0.8668 0.1309 0.030 Uiso 1 1 calc R . . N1 N 0.8857(3) 0.3656(2) 0.2911(2) 0.0187(6) Uani 1 1 d . . . N2 N 0.9379(3) 0.2462(2) 0.2992(2) 0.0230(7) Uani 1 1 d . . . N3 N 0.9979(3) 0.2941(3) 0.4133(2) 0.0220(7) Uani 1 1 d . . . N4 N 0.8794(3) 0.4110(2) 0.1043(2) 0.0199(6) Uani 1 1 d . . . N5 N 0.9982(3) 0.3374(3) 0.1028(3) 0.0328(8) Uani 1 1 d . . . N6 N 0.9449(3) 0.4133(3) -0.0513(2) 0.0259(7) Uani 1 1 d . . . N7 N 0.7036(2) 0.4141(2) 0.2222(2) 0.0159(6) Uani 1 1 d . . . N8 N 0.6888(3) 0.3437(2) 0.1715(2) 0.0186(6) Uani 1 1 d . . . N9 N 0.5536(3) 0.3939(2) 0.2950(2) 0.0176(6) Uani 1 1 d . . . O1 O 0.7636(3) 0.8390(2) 0.3101(2) 0.0345(7) Uani 1 1 d . . . P1 P 0.51188(8) 0.78928(7) 0.28302(7) 0.01635(19) Uani 1 1 d . . . Rh1 Rh 0.69183(2) 0.65554(2) 0.32188(2) 0.01489(8) Uani 1 1 d . . . S1 S 0.87327(8) 0.52631(7) 0.39389(7) 0.0213(2) Uani 1 1 d . . . S2 S 0.60776(8) 0.52207(7) 0.38567(6) 0.01867(19) Uani 1 1 d . . . S3 S 0.71684(10) 0.55367(9) -0.02957(8) 0.0368(3) 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 B1 0.014(2) 0.0202(19) 0.022(2) -0.0097(16) 0.0040(16) -0.0079(16) C1 0.0206(19) 0.0202(17) 0.0222(19) -0.0009(14) -0.0051(15) -0.0103(15) C2 0.0184(18) 0.0196(16) 0.0158(17) -0.0029(13) -0.0008(14) -0.0091(14) C3 0.021(2) 0.0202(17) 0.028(2) -0.0058(15) -0.0005(16) -0.0088(15) C4 0.035(3) 0.0191(19) 0.049(3) 0.0000(18) -0.008(2) -0.0082(17) C5 0.039(3) 0.032(2) 0.030(2) -0.0038(18) -0.017(2) -0.0059(19) C6 0.047(3) 0.049(3) 0.040(3) -0.008(2) -0.011(2) -0.022(2) C7 0.035(2) 0.0260(19) 0.0180(19) -0.0059(15) 0.0039(16) -0.0162(17) C8 0.029(2) 0.046(2) 0.030(2) -0.0182(19) 0.0058(18) -0.019(2) C9 0.029(3) 0.067(3) 0.039(3) -0.026(2) 0.008(2) -0.017(2) C10 0.042(3) 0.042(2) 0.024(2) -0.0101(18) 0.0096(19) -0.022(2) C11 0.033(2) 0.056(3) 0.027(2) -0.011(2) 0.0011(19) -0.025(2) C12 0.0185(18) 0.0150(15) 0.0141(17) -0.0013(13) -0.0039(14) -0.0077(13) C13 0.026(2) 0.0184(16) 0.0163(18) -0.0005(13) -0.0055(15) -0.0133(15) C14 0.040(2) 0.033(2) 0.023(2) -0.0077(16) -0.0031(18) -0.0251(19) C15 0.027(2) 0.0291(19) 0.0221(19) -0.0036(15) 0.0024(16) -0.0218(17) C16 0.026(2) 0.033(2) 0.035(2) -0.0038(18) 0.0036(18) -0.0133(18) C17 0.026(2) 0.0254(18) 0.0170(18) -0.0013(14) -0.0002(15) -0.0184(16) C18 0.033(2) 0.0218(17) 0.0157(18) 0.0037(14) -0.0029(16) -0.0182(16) C19 0.052(3) 0.034(2) 0.0146(19) -0.0039(16) -0.0002(18) -0.030(2) C20 0.049(3) 0.060(3) 0.027(2) -0.002(2) -0.012(2) -0.041(2) C21 0.029(2) 0.056(3) 0.039(3) -0.003(2) -0.010(2) -0.025(2) C22 0.028(2) 0.038(2) 0.030(2) -0.0065(18) -0.0026(18) -0.0171(19) C23 0.0198(19) 0.0206(17) 0.0118(17) -0.0013(13) -0.0016(14) -0.0027(14) C24 0.022(2) 0.0231(19) 0.029(2) 0.0006(16) 0.0001(17) -0.0034(16) C25 0.022(2) 0.037(2) 0.030(2) 0.0142(19) -0.0008(18) 0.0006(18) C26 0.032(3) 0.049(3) 0.021(2) -0.003(2) 0.0020(19) 0.009(2) C27 0.050(3) 0.044(3) 0.028(2) -0.019(2) -0.003(2) -0.002(2) C28 0.032(2) 0.033(2) 0.026(2) -0.0074(17) -0.0079(18) -0.0083(18) C29 0.036(2) 0.0188(17) 0.0181(18) 0.0036(14) -0.0114(16) -0.0164(16) C30 0.036(2) 0.0239(19) 0.028(2) 0.0012(16) -0.0080(18) -0.0114(17) C31 0.051(3) 0.0207(19) 0.040(3) 0.0002(18) -0.018(2) -0.0113(19) C32 0.055(3) 0.0243(19) 0.027(2) -0.0007(16) -0.017(2) -0.023(2) C33 0.050(3) 0.042(2) 0.019(2) -0.0062(17) -0.0019(18) -0.034(2) C34 0.036(2) 0.030(2) 0.0183(19) -0.0016(15) -0.0042(17) -0.0221(18) N1 0.0193(16) 0.0171(14) 0.0209(16) -0.0067(12) 0.0017(12) -0.0086(12) N2 0.0207(17) 0.0168(14) 0.0305(18) -0.0050(13) -0.0029(14) -0.0067(13) N3 0.0208(17) 0.0211(15) 0.0233(17) -0.0022(12) -0.0056(13) -0.0082(13) N4 0.0195(16) 0.0234(15) 0.0194(16) -0.0073(12) 0.0014(13) -0.0110(13) N5 0.0242(19) 0.045(2) 0.0263(19) -0.0134(16) 0.0024(15) -0.0115(16) N6 0.0303(19) 0.0360(18) 0.0184(16) -0.0093(14) 0.0057(14) -0.0208(15) N7 0.0187(15) 0.0139(13) 0.0170(15) -0.0037(11) -0.0042(12) -0.0073(11) N8 0.0256(17) 0.0162(14) 0.0169(15) -0.0029(11) -0.0042(13) -0.0107(12) N9 0.0205(16) 0.0193(14) 0.0160(15) -0.0012(11) -0.0024(12) -0.0119(12) O1 0.0379(18) 0.0277(15) 0.0470(19) -0.0009(13) -0.0163(15) -0.0203(13) P1 0.0204(5) 0.0162(4) 0.0146(4) -0.0019(3) -0.0015(4) -0.0101(4) Rh1 0.01820(15) 0.01426(13) 0.01468(14) -0.00328(9) -0.00097(10) -0.00899(10) S1 0.0239(5) 0.0206(4) 0.0211(5) -0.0066(3) -0.0070(4) -0.0080(4) S2 0.0258(5) 0.0192(4) 0.0152(4) -0.0056(3) 0.0042(4) -0.0141(4) S3 0.0405(7) 0.0316(5) 0.0229(5) -0.0026(4) -0.0010(5) -0.0046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N4 1.536(5) . ? B1 N1 1.536(5) . ? B1 N7 1.542(5) . ? B1 H1 1.0000 . ? C1 O1 1.152(4) . ? C1 Rh1 1.817(3) . ? C2 N1 1.343(4) . ? C2 N3 1.373(5) . ? C2 S1 1.702(3) . ? C3 N2 1.282(5) . ? C3 N3 1.376(4) . ? C3 C4 1.496(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.462(5) . ? C5 C6 1.561(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N4 1.343(5) . ? C7 N6 1.345(5) . ? C7 S3 1.699(4) . ? C8 N5 1.298(5) . ? C8 N6 1.367(6) . ? C8 C9 1.492(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N6 1.465(5) . ? C10 C11 1.511(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N7 1.329(4) . ? C12 N9 1.364(4) . ? C12 S2 1.710(3) . ? C13 N8 1.298(5) . ? C13 N9 1.370(4) . ? C13 C14 1.485(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N9 1.467(5) . ? C15 C16 1.514(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.390(6) . ? C17 C18 1.393(5) . ? C17 P1 1.834(4) . ? C18 C19 1.393(5) . ? C18 H18 0.9500 . ? C19 C20 1.380(6) . ? C19 H19 0.9500 . ? C20 C21 1.382(7) . ? C20 H20 0.9500 . ? C21 C22 1.389(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.384(5) . ? C23 C28 1.405(5) . ? C23 P1 1.827(4) . ? C24 C25 1.386(6) . ? C24 H24 0.9500 . ? C25 C26 1.368(7) . ? C25 H25 0.9500 . ? C26 C27 1.376(8) . ? C26 H26 0.9500 . ? C27 C28 1.373(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.381(5) . ? C29 C30 1.406(6) . ? C29 P1 1.829(4) . ? C30 C31 1.385(6) . ? C30 H30 0.9500 . ? C31 C32 1.377(7) . ? C31 H31 0.9500 . ? C32 C33 1.366(6) . ? C32 H32 0.9500 . ? C33 C34 1.408(5) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? N1 N2 1.396(4) . ? N4 N5 1.405(5) . ? N7 N8 1.389(4) . ? P1 Rh1 2.2639(14) . ? Rh1 S1 2.4141(14) . ? Rh1 S2 2.4307(11) . ? 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 N4 B1 N1 109.1(3) . . ? N4 B1 N7 113.1(3) . . ? N1 B1 N7 106.6(3) . . ? N4 B1 H1 109.3 . . ? N1 B1 H1 109.3 . . ? N7 B1 H1 109.3 . . ? O1 C1 Rh1 175.7(3) . . ? N1 C2 N3 105.9(3) . . ? N1 C2 S1 130.0(3) . . ? N3 C2 S1 124.1(3) . . ? N2 C3 N3 111.9(3) . . ? N2 C3 C4 125.0(3) . . ? N3 C3 C4 123.1(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 109.5(4) . . ? N3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 107.0(3) . . ? N4 C7 S3 128.1(3) . . ? N6 C7 S3 124.9(3) . . ? N5 C8 N6 111.4(4) . . ? N5 C8 C9 124.4(4) . . ? N6 C8 C9 124.1(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 111.3(3) . . ? N6 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N6 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 106.1(3) . . ? N7 C12 S2 129.2(3) . . ? N9 C12 S2 124.6(3) . . ? N8 C13 N9 111.4(3) . . ? N8 C13 C14 125.0(3) . . ? N9 C13 C14 123.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 112.4(3) . . ? N9 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N9 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 118.8(3) . . ? C22 C17 P1 122.6(3) . . ? C18 C17 P1 118.3(3) . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.8(4) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.3(4) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? C24 C23 C28 118.3(4) . . ? C24 C23 P1 122.5(3) . . ? C28 C23 P1 119.0(3) . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 120.7(5) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.5(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C23 120.2(4) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C34 C29 C30 118.9(3) . . ? C34 C29 P1 118.7(3) . . ? C30 C29 P1 122.1(3) . . ? C31 C30 C29 121.1(4) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 119.0(4) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 121.2(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 120.3(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 119.6(4) . . ? C29 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C2 N1 N2 110.2(3) . . ? C2 N1 B1 131.0(3) . . ? N2 N1 B1 118.7(3) . . ? C3 N2 N1 105.4(3) . . ? C2 N3 C3 106.5(3) . . ? C2 N3 C5 125.4(3) . . ? C3 N3 C5 127.5(3) . . ? C7 N4 N5 109.3(3) . . ? C7 N4 B1 129.6(3) . . ? N5 N4 B1 120.4(3) . . ? C8 N5 N4 104.9(3) . . ? C7 N6 C8 107.3(3) . . ? C7 N6 C10 127.2(4) . . ? C8 N6 C10 125.5(4) . . ? C12 N7 N8 111.0(3) . . ? C12 N7 B1 124.0(3) . . ? N8 N7 B1 124.4(3) . . ? C13 N8 N7 104.7(3) . . ? C12 N9 C13 106.8(3) . . ? C12 N9 C15 125.5(3) . . ? C13 N9 C15 127.7(3) . . ? C23 P1 C29 103.60(17) . . ? C23 P1 C17 105.01(17) . . ? C29 P1 C17 99.73(16) . . ? C23 P1 Rh1 110.01(12) . . ? C29 P1 Rh1 118.46(14) . . ? C17 P1 Rh1 118.24(13) . . ? C1 Rh1 P1 90.12(12) . . ? C1 Rh1 S1 86.40(12) . . ? P1 Rh1 S1 168.86(3) . . ? C1 Rh1 S2 162.59(12) . . ? P1 Rh1 S2 86.55(4) . . ? S1 Rh1 S2 93.62(4) . . ? C2 S1 Rh1 108.41(13) . . ? C12 S2 Rh1 111.09(12) . . ? 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 C22 C17 C18 C19 -2.7(5) . . . . ? P1 C17 C18 C19 -176.3(3) . . . . ? C17 C18 C19 C20 1.2(5) . . . . ? C18 C19 C20 C21 0.5(6) . . . . ? C19 C20 C21 C22 -0.8(7) . . . . ? C20 C21 C22 C17 -0.7(7) . . . . ? C18 C17 C22 C21 2.4(6) . . . . ? P1 C17 C22 C21 175.8(3) . . . . ? C28 C23 C24 C25 0.7(6) . . . . ? P1 C23 C24 C25 176.8(3) . . . . ? C23 C24 C25 C26 0.3(6) . . . . ? C24 C25 C26 C27 -1.2(7) . . . . ? C25 C26 C27 C28 0.9(7) . . . . ? C26 C27 C28 C23 0.2(7) . . . . ? C24 C23 C28 C27 -1.0(6) . . . . ? P1 C23 C28 C27 -177.2(3) . . . . ? C34 C29 C30 C31 0.3(6) . . . . ? P1 C29 C30 C31 -173.4(3) . . . . ? C29 C30 C31 C32 1.3(6) . . . . ? C30 C31 C32 C33 -2.3(6) . . . . ? C31 C32 C33 C34 1.6(6) . . . . ? C30 C29 C34 C33 -1.0(5) . . . . ? P1 C29 C34 C33 172.9(3) . . . . ? C32 C33 C34 C29 0.1(6) . . . . ? N3 C2 N1 N2 3.5(4) . . . . ? S1 C2 N1 N2 -174.1(3) . . . . ? N3 C2 N1 B1 -173.0(3) . . . . ? S1 C2 N1 B1 9.5(6) . . . . ? N4 B1 N1 C2 119.8(4) . . . . ? N7 B1 N1 C2 -117.8(4) . . . . ? N4 B1 N1 N2 -56.4(4) . . . . ? N7 B1 N1 N2 66.0(4) . . . . ? N3 C3 N2 N1 1.0(4) . . . . ? C4 C3 N2 N1 -178.8(4) . . . . ? C2 N1 N2 C3 -2.8(4) . . . . ? B1 N1 N2 C3 174.1(3) . . . . ? N1 C2 N3 C3 -2.8(4) . . . . ? S1 C2 N3 C3 174.9(3) . . . . ? N1 C2 N3 C5 168.6(4) . . . . ? S1 C2 N3 C5 -13.7(5) . . . . ? N2 C3 N3 C2 1.1(4) . . . . ? C4 C3 N3 C2 -179.1(4) . . . . ? N2 C3 N3 C5 -170.0(4) . . . . ? C4 C3 N3 C5 9.7(6) . . . . ? C6 C5 N3 C2 -86.4(5) . . . . ? C6 C5 N3 C3 83.2(5) . . . . ? N6 C7 N4 N5 2.5(4) . . . . ? S3 C7 N4 N5 -179.6(3) . . . . ? N6 C7 N4 B1 172.7(3) . . . . ? S3 C7 N4 B1 -9.5(6) . . . . ? N1 B1 N4 C7 -176.3(3) . . . . ? N7 B1 N4 C7 65.3(5) . . . . ? N1 B1 N4 N5 -7.1(4) . . . . ? N7 B1 N4 N5 -125.5(3) . . . . ? N6 C8 N5 N4 1.4(5) . . . . ? C9 C8 N5 N4 -178.1(4) . . . . ? C7 N4 N5 C8 -2.5(4) . . . . ? B1 N4 N5 C8 -173.6(3) . . . . ? N4 C7 N6 C8 -1.6(4) . . . . ? S3 C7 N6 C8 -179.6(3) . . . . ? N4 C7 N6 C10 -179.5(3) . . . . ? S3 C7 N6 C10 2.6(6) . . . . ? N5 C8 N6 C7 0.1(5) . . . . ? C9 C8 N6 C7 179.6(4) . . . . ? N5 C8 N6 C10 178.0(4) . . . . ? C9 C8 N6 C10 -2.5(6) . . . . ? C11 C10 N6 C7 -92.4(5) . . . . ? C11 C10 N6 C8 90.2(5) . . . . ? N9 C12 N7 N8 -0.5(4) . . . . ? S2 C12 N7 N8 175.7(3) . . . . ? N9 C12 N7 B1 -172.4(3) . . . . ? S2 C12 N7 B1 3.8(5) . . . . ? N4 B1 N7 C12 -171.9(3) . . . . ? N1 B1 N7 C12 68.3(4) . . . . ? N4 B1 N7 N8 17.3(5) . . . . ? N1 B1 N7 N8 -102.5(3) . . . . ? N9 C13 N8 N7 -0.5(4) . . . . ? C14 C13 N8 N7 -179.5(3) . . . . ? C12 N7 N8 C13 0.7(4) . . . . ? B1 N7 N8 C13 172.5(3) . . . . ? N7 C12 N9 C13 0.2(4) . . . . ? S2 C12 N9 C13 -176.3(3) . . . . ? N7 C12 N9 C15 178.2(3) . . . . ? S2 C12 N9 C15 1.7(5) . . . . ? N8 C13 N9 C12 0.2(4) . . . . ? C14 C13 N9 C12 179.2(3) . . . . ? N8 C13 N9 C15 -177.7(3) . . . . ? C14 C13 N9 C15 1.3(6) . . . . ? C16 C15 N9 C12 96.2(4) . . . . ? C16 C15 N9 C13 -86.2(4) . . . . ? C24 C23 P1 C29 136.4(3) . . . . ? C28 C23 P1 C29 -47.6(3) . . . . ? C24 C23 P1 C17 32.2(3) . . . . ? C28 C23 P1 C17 -151.8(3) . . . . ? C24 C23 P1 Rh1 -96.0(3) . . . . ? C28 C23 P1 Rh1 79.9(3) . . . . ? C34 C29 P1 C23 156.6(3) . . . . ? C30 C29 P1 C23 -29.7(4) . . . . ? C34 C29 P1 C17 -95.2(3) . . . . ? C30 C29 P1 C17 78.5(3) . . . . ? C34 C29 P1 Rh1 34.5(3) . . . . ? C30 C29 P1 Rh1 -151.8(3) . . . . ? C22 C17 P1 C23 38.2(4) . . . . ? C18 C17 P1 C23 -148.4(3) . . . . ? C22 C17 P1 C29 -68.8(4) . . . . ? C18 C17 P1 C29 104.6(3) . . . . ? C22 C17 P1 Rh1 161.3(3) . . . . ? C18 C17 P1 Rh1 -25.3(3) . . . . ? C23 P1 Rh1 C1 -93.64(18) . . . . ? C29 P1 Rh1 C1 25.18(18) . . . . ? C17 P1 Rh1 C1 145.80(18) . . . . ? C23 P1 Rh1 S1 -21.9(2) . . . . ? C29 P1 Rh1 S1 96.9(2) . . . . ? C17 P1 Rh1 S1 -142.5(2) . . . . ? C23 P1 Rh1 S2 69.27(13) . . . . ? C29 P1 Rh1 S2 -171.92(14) . . . . ? C17 P1 Rh1 S2 -51.30(13) . . . . ? N1 C2 S1 Rh1 17.3(4) . . . . ? N3 C2 S1 Rh1 -159.8(3) . . . . ? C1 Rh1 S1 C2 -148.26(18) . . . . ? P1 Rh1 S1 C2 139.7(2) . . . . ? S2 Rh1 S1 C2 49.19(13) . . . . ? N7 C12 S2 Rh1 28.2(4) . . . . ? N9 C12 S2 Rh1 -156.2(3) . . . . ? C1 Rh1 S2 C12 174.9(4) . . . . ? P1 Rh1 S2 C12 95.55(13) . . . . ? S1 Rh1 S2 C12 -95.61(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.677 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.112 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 603868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H39 B N9 O P Rh S3, F6 P, 2(C H2 Cl2)' _chemical_formula_sum 'C36 H43 B Cl4 F6 N9 O P2 Rh S3' _chemical_formula_weight 1145.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.8991(19) _cell_length_b 14.035(2) _cell_length_c 14.286(2) _cell_angle_alpha 68.377(5) _cell_angle_beta 88.304(6) _cell_angle_gamma 87.738(5) _cell_volume 2402.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6931 _cell_measurement_theta_min 2.184 _cell_measurement_theta_max 26.959 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773343 _exptl_absorpt_correction_T_max 0.980000 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25690 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10972 _reflns_number_gt 7390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.02 (Bruker, 2001)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.4341P] 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 10972 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.74646(3) 0.64432(2) 0.63886(3) 0.02077(10) Uani 1 1 d . . . Cl1 Cl 0.59144(14) 0.81414(13) 0.89214(11) 0.0657(4) Uani 1 1 d . . . Cl2 Cl 0.6310(2) 1.03210(15) 0.82160(16) 0.1027(8) Uani 1 1 d . . . Cl3 Cl 0.84704(16) 0.34635(16) 0.13170(15) 0.0854(6) Uani 1 1 d . . . Cl4 Cl 0.63743(15) 0.41447(13) 0.06252(13) 0.0708(5) Uani 1 1 d . . . S1 S 0.90853(10) 0.67777(9) 0.54801(9) 0.0343(3) Uani 1 1 d . . . S2 S 0.82356(10) 0.58725(9) 0.80089(9) 0.0342(3) Uani 1 1 d . . . S3 S 0.57485(9) 0.65557(9) 0.70180(10) 0.0360(3) Uani 1 1 d . . . C1 C 0.6881(4) 0.7001(4) 0.5121(4) 0.0358(11) Uani 1 1 d . . . C2 C 0.8934(3) 0.8088(3) 0.5030(3) 0.0256(9) Uani 1 1 d . . . C3 C 0.9046(3) 0.9745(3) 0.4243(3) 0.0248(9) Uani 1 1 d . . . C4 C 0.9392(4) 1.0738(3) 0.3511(4) 0.0342(11) Uani 1 1 d . . . H4A H 0.9096 1.1296 0.3702 0.051 Uiso 1 1 calc R . . H4B H 0.9158 1.0824 0.2837 0.051 Uiso 1 1 calc R . . H4C H 1.0151 1.0752 0.3509 0.051 Uiso 1 1 calc R . . C5 C 1.0247(4) 0.8589(4) 0.3612(4) 0.0369(12) Uani 1 1 d . . . H5A H 1.0184 0.9124 0.2930 0.044 Uiso 1 1 calc R . . H5B H 1.0107 0.7922 0.3559 0.044 Uiso 1 1 calc R . . C6 C 1.1334(4) 0.8557(4) 0.3959(4) 0.0429(13) Uani 1 1 d . . . H6A H 1.1496 0.9229 0.3971 0.064 Uiso 1 1 calc R . . H6B H 1.1815 0.8387 0.3496 0.064 Uiso 1 1 calc R . . H6C H 1.1402 0.8035 0.4637 0.064 Uiso 1 1 calc R . . C7 C 0.8334(3) 0.7069(3) 0.8056(3) 0.0283(10) Uani 1 1 d . . . C8 C 0.8634(3) 0.8381(3) 0.8481(3) 0.0279(10) Uani 1 1 d . . . C9 C 0.8960(4) 0.8986(4) 0.9072(3) 0.0381(12) Uani 1 1 d . . . H9A H 0.8837 0.9718 0.8683 0.057 Uiso 1 1 calc R . . H9B H 0.9700 0.8852 0.9219 0.057 Uiso 1 1 calc R . . H9C H 0.8559 0.8789 0.9704 0.057 Uiso 1 1 calc R . . C10 C 0.8981(4) 0.6595(4) 0.9814(3) 0.0397(12) Uani 1 1 d . . . H10A H 0.9548 0.6877 1.0075 0.048 Uiso 1 1 calc R . . H10B H 0.9240 0.5943 0.9761 0.048 Uiso 1 1 calc R . . C11 C 0.8076(5) 0.6389(5) 1.0535(4) 0.0522(15) Uani 1 1 d . . . H11A H 0.7813 0.7035 1.0582 0.078 Uiso 1 1 calc R . . H11B H 0.8296 0.5918 1.1201 0.078 Uiso 1 1 calc R . . H11C H 0.7525 0.6080 1.0294 0.078 Uiso 1 1 calc R . . C12 C 0.5681(3) 0.7868(3) 0.6623(3) 0.0286(10) Uani 1 1 d . . . C13 C 0.5202(4) 0.9460(3) 0.6306(3) 0.0276(10) Uani 1 1 d . . . C14 C 0.4521(4) 1.0372(4) 0.6217(4) 0.0381(12) Uani 1 1 d . . . H14A H 0.4908 1.0999 0.5883 0.057 Uiso 1 1 calc R . . H14B H 0.4296 1.0337 0.6890 0.057 Uiso 1 1 calc R . . H14C H 0.3912 1.0381 0.5819 0.057 Uiso 1 1 calc R . . C15 C 0.3773(4) 0.8136(4) 0.6890(4) 0.0475(14) Uani 1 1 d . . . H15A H 0.3375 0.8618 0.7136 0.057 Uiso 1 1 calc R . . H15B H 0.3779 0.7450 0.7435 0.057 Uiso 1 1 calc R . . C16 C 0.3260(4) 0.8086(4) 0.5981(5) 0.0565(17) Uani 1 1 d . . . H16A H 0.3229 0.8772 0.5453 0.085 Uiso 1 1 calc R . . H16B H 0.2555 0.7838 0.6162 0.085 Uiso 1 1 calc R . . H16C H 0.3662 0.7617 0.5733 0.085 Uiso 1 1 calc R . . C17 C 0.8499(3) 0.3794(3) 0.7177(3) 0.0270(10) Uani 1 1 d . . . C18 C 0.9519(4) 0.4114(3) 0.6889(4) 0.0317(11) Uani 1 1 d . . . H18 H 0.9629 0.4758 0.6365 0.038 Uiso 1 1 calc R . . C19 C 1.0363(4) 0.3506(4) 0.7357(4) 0.0381(12) Uani 1 1 d . . . H19 H 1.1047 0.3724 0.7143 0.046 Uiso 1 1 calc R . . C20 C 1.0208(4) 0.2585(4) 0.8133(4) 0.0396(12) Uani 1 1 d . . . H20 H 1.0788 0.2171 0.8461 0.047 Uiso 1 1 calc R . . C21 C 0.9223(4) 0.2260(4) 0.8438(3) 0.0367(12) Uani 1 1 d . . . H21 H 0.9126 0.1625 0.8978 0.044 Uiso 1 1 calc R . . C22 C 0.8362(4) 0.2851(3) 0.7965(3) 0.0319(11) Uani 1 1 d . . . H22 H 0.7683 0.2615 0.8176 0.038 Uiso 1 1 calc R . . C23 C 0.6291(3) 0.3910(3) 0.7186(3) 0.0258(9) Uani 1 1 d . . . C24 C 0.5914(4) 0.4071(3) 0.8044(3) 0.0290(10) Uani 1 1 d . . . H24 H 0.6231 0.4556 0.8254 0.035 Uiso 1 1 calc R . . C25 C 0.5085(4) 0.3533(4) 0.8590(4) 0.0393(12) Uani 1 1 d . . . H25 H 0.4836 0.3648 0.9173 0.047 Uiso 1 1 calc R . . C26 C 0.4620(4) 0.2829(4) 0.8292(4) 0.0433(13) Uani 1 1 d . . . H26 H 0.4044 0.2466 0.8665 0.052 Uiso 1 1 calc R . . C27 C 0.4988(4) 0.2648(4) 0.7449(4) 0.0398(12) Uani 1 1 d . . . H27 H 0.4668 0.2156 0.7249 0.048 Uiso 1 1 calc R . . C28 C 0.5822(4) 0.3185(3) 0.6901(3) 0.0305(10) Uani 1 1 d . . . H28 H 0.6076 0.3057 0.6325 0.037 Uiso 1 1 calc R . . C29 C 0.7386(3) 0.4541(3) 0.5291(3) 0.0232(9) Uani 1 1 d . . . C30 C 0.6495(3) 0.4921(3) 0.4722(3) 0.0283(10) Uani 1 1 d . . . H30 H 0.5930 0.5187 0.5002 0.034 Uiso 1 1 calc R . . C31 C 0.6421(4) 0.4917(3) 0.3770(3) 0.0324(11) Uani 1 1 d . . . H31 H 0.5801 0.5162 0.3403 0.039 Uiso 1 1 calc R . . C32 C 0.7251(4) 0.4555(3) 0.3341(4) 0.0336(11) Uani 1 1 d . . . H32 H 0.7201 0.4550 0.2680 0.040 Uiso 1 1 calc R . . C33 C 0.8144(4) 0.4204(4) 0.3874(4) 0.0350(11) Uani 1 1 d . . . H33 H 0.8717 0.3971 0.3576 0.042 Uiso 1 1 calc R . . C34 C 0.8216(3) 0.4187(3) 0.4850(3) 0.0265(10) Uani 1 1 d . . . H34 H 0.8834 0.3933 0.5216 0.032 Uiso 1 1 calc R . . C35 C 0.5846(5) 0.9284(6) 0.9207(5) 0.075(2) Uani 1 1 d . . . H35A H 0.5117 0.9431 0.9358 0.090 Uiso 1 1 calc R . . H35B H 0.6259 0.9175 0.9814 0.090 Uiso 1 1 calc R . . C36 C 0.7508(7) 0.3501(5) 0.0451(5) 0.080(2) Uani 1 1 d . . . H36A H 0.7779 0.3850 -0.0243 0.096 Uiso 1 1 calc R . . H36B H 0.7344 0.2792 0.0531 0.096 Uiso 1 1 calc R . . P1 P 0.74170(9) 0.46183(8) 0.65354(8) 0.0225(2) Uani 1 1 d . . . P2 P 0.76713(12) 0.00226(15) 0.13150(12) 0.0537(4) Uani 1 1 d . . . F1 F 0.783(2) -0.071(2) 0.239(2) 0.114(8) Uani 0.47(5) 1 d P A 1 F2 F 0.7539(15) -0.1091(16) 0.1147(18) 0.059(4) Uani 0.47(5) 1 d P A 1 F3 F 0.6392(15) -0.012(3) 0.1530(17) 0.102(8) Uani 0.47(5) 1 d P A 1 F4 F 0.765(4) 0.089(3) 0.161(3) 0.111(10) Uani 0.47(5) 1 d P A 1 F5 F 0.885(2) -0.011(3) 0.121(4) 0.088(9) Uani 0.47(5) 1 d P A 1 F6 F 0.742(4) 0.074(3) 0.019(3) 0.080(8) Uani 0.47(5) 1 d P A 1 F7 F 0.882(2) -0.027(2) 0.108(3) 0.083(7) Uani 0.53(5) 1 d P A 2 F8 F 0.6621(18) 0.054(4) 0.1445(15) 0.134(11) Uani 0.53(5) 1 d P A 2 F9 F 0.821(2) 0.1134(10) 0.1297(14) 0.075(5) Uani 0.53(5) 1 d P A 2 F10 F 0.724(3) -0.089(3) 0.124(2) 0.137(10) Uani 0.53(5) 1 d P A 2 F11 F 0.7809(13) -0.044(2) 0.2530(14) 0.083(6) Uani 0.53(5) 1 d P A 2 F12 F 0.760(3) 0.052(3) 0.012(3) 0.069(6) Uani 0.53(5) 1 d P A 2 O1 O 0.6533(3) 0.7381(3) 0.4336(3) 0.0561(11) Uani 1 1 d . . . B1 B 0.7571(4) 0.7990(3) 0.6333(4) 0.0212(10) Uani 1 1 d . . . N1 N 0.8245(3) 0.8580(2) 0.5415(2) 0.0210(7) Uani 1 1 d . . . N3 N 0.9452(3) 0.8801(3) 0.4283(3) 0.0275(8) Uani 1 1 d . . . N2 N 0.8323(3) 0.9632(3) 0.4922(3) 0.0268(8) Uani 1 1 d . . . N4 N 0.8082(3) 0.7936(3) 0.7318(3) 0.0231(8) Uani 1 1 d . . . N6 N 0.8697(3) 0.7323(3) 0.8809(3) 0.0288(9) Uani 1 1 d . . . N5 N 0.8281(3) 0.8770(3) 0.7573(3) 0.0250(8) Uani 1 1 d . . . N7 N 0.6472(3) 0.8464(2) 0.6287(2) 0.0202(7) Uani 1 1 d . . . N9 N 0.4844(3) 0.8480(3) 0.6635(3) 0.0326(9) Uani 1 1 d . . . N8 N 0.6175(3) 0.9478(3) 0.6100(3) 0.0285(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 0.01962(18) 0.01713(16) 0.02545(18) -0.00777(13) -0.00054(12) 0.00035(12) Cl1 0.0706(11) 0.0757(11) 0.0444(8) -0.0150(8) 0.0065(7) -0.0029(9) Cl2 0.152(2) 0.0633(12) 0.0982(15) -0.0344(11) -0.0669(15) 0.0328(13) Cl3 0.0806(13) 0.0837(13) 0.0879(13) -0.0284(11) 0.0071(11) 0.0057(11) Cl4 0.0849(13) 0.0656(11) 0.0590(10) -0.0187(8) -0.0039(9) -0.0080(9) S1 0.0328(7) 0.0271(6) 0.0403(7) -0.0101(5) 0.0084(5) 0.0021(5) S2 0.0469(8) 0.0267(6) 0.0284(6) -0.0091(5) -0.0093(5) 0.0035(5) S3 0.0267(6) 0.0251(6) 0.0522(8) -0.0099(6) 0.0061(5) -0.0018(5) C1 0.041(3) 0.027(2) 0.042(3) -0.015(2) -0.008(2) 0.002(2) C2 0.025(2) 0.027(2) 0.026(2) -0.0124(19) 0.0024(18) -0.0012(19) C3 0.024(2) 0.026(2) 0.022(2) -0.0063(18) -0.0016(17) -0.0045(18) C4 0.031(3) 0.028(2) 0.040(3) -0.008(2) 0.006(2) -0.008(2) C5 0.043(3) 0.037(3) 0.031(3) -0.013(2) 0.012(2) -0.009(2) C6 0.036(3) 0.032(3) 0.062(3) -0.019(3) 0.014(3) -0.002(2) C7 0.030(2) 0.032(2) 0.023(2) -0.0096(19) -0.0023(18) -0.002(2) C8 0.027(2) 0.033(2) 0.026(2) -0.013(2) 0.0038(18) -0.009(2) C9 0.048(3) 0.039(3) 0.029(3) -0.013(2) -0.004(2) -0.013(2) C10 0.050(3) 0.037(3) 0.031(3) -0.012(2) -0.012(2) 0.003(2) C11 0.063(4) 0.060(4) 0.030(3) -0.012(3) -0.002(3) -0.014(3) C12 0.024(2) 0.026(2) 0.035(2) -0.010(2) -0.0028(19) 0.0038(19) C13 0.033(3) 0.023(2) 0.026(2) -0.0088(18) 0.0001(19) 0.0031(19) C14 0.042(3) 0.034(3) 0.036(3) -0.013(2) -0.002(2) 0.014(2) C15 0.028(3) 0.045(3) 0.060(4) -0.010(3) 0.007(3) 0.001(2) C16 0.040(3) 0.033(3) 0.087(5) -0.010(3) -0.014(3) -0.003(2) C17 0.030(2) 0.023(2) 0.030(2) -0.0110(19) -0.0082(19) 0.0056(19) C18 0.032(3) 0.024(2) 0.038(3) -0.010(2) -0.012(2) 0.004(2) C19 0.031(3) 0.042(3) 0.050(3) -0.027(3) -0.014(2) 0.006(2) C20 0.047(3) 0.036(3) 0.038(3) -0.017(2) -0.020(2) 0.015(2) C21 0.053(3) 0.024(2) 0.029(3) -0.005(2) -0.014(2) 0.012(2) C22 0.040(3) 0.027(2) 0.029(2) -0.012(2) -0.003(2) 0.004(2) C23 0.022(2) 0.021(2) 0.032(2) -0.0077(19) -0.0027(18) 0.0018(18) C24 0.033(3) 0.026(2) 0.026(2) -0.0073(19) -0.0010(19) -0.004(2) C25 0.043(3) 0.037(3) 0.034(3) -0.008(2) 0.006(2) -0.005(2) C26 0.037(3) 0.042(3) 0.039(3) -0.001(2) 0.004(2) -0.009(2) C27 0.043(3) 0.030(3) 0.044(3) -0.009(2) -0.010(2) -0.009(2) C28 0.034(3) 0.026(2) 0.032(2) -0.011(2) -0.001(2) -0.004(2) C29 0.024(2) 0.020(2) 0.024(2) -0.0070(17) -0.0002(17) -0.0018(17) C30 0.025(2) 0.029(2) 0.031(2) -0.011(2) -0.0017(19) 0.0012(19) C31 0.032(3) 0.026(2) 0.035(3) -0.007(2) -0.008(2) -0.001(2) C32 0.042(3) 0.029(2) 0.032(3) -0.014(2) 0.001(2) -0.005(2) C33 0.036(3) 0.036(3) 0.035(3) -0.016(2) 0.007(2) -0.001(2) C34 0.021(2) 0.026(2) 0.033(2) -0.0111(19) -0.0033(18) 0.0004(18) C35 0.066(5) 0.103(6) 0.061(4) -0.037(4) -0.009(3) 0.035(4) C36 0.139(7) 0.058(4) 0.040(4) -0.015(3) 0.006(4) -0.004(4) P1 0.0230(6) 0.0184(5) 0.0256(6) -0.0075(4) -0.0029(4) 0.0010(4) P2 0.0372(8) 0.0878(13) 0.0498(9) -0.0422(9) -0.0065(7) 0.0118(8) F1 0.189(19) 0.119(13) 0.048(9) -0.050(8) -0.047(9) 0.039(11) F2 0.053(7) 0.060(7) 0.071(8) -0.032(6) -0.007(5) -0.003(7) F3 0.029(7) 0.20(2) 0.090(9) -0.065(13) 0.010(6) 0.012(10) F4 0.13(2) 0.096(14) 0.146(17) -0.089(13) -0.065(16) 0.052(14) F5 0.025(8) 0.090(18) 0.165(18) -0.065(12) 0.009(8) -0.018(9) F6 0.091(14) 0.096(18) 0.060(10) -0.038(10) -0.018(9) 0.016(11) F7 0.068(12) 0.049(7) 0.136(14) -0.043(9) 0.012(9) 0.011(7) F8 0.039(9) 0.26(3) 0.095(8) -0.061(15) -0.003(7) 0.052(13) F9 0.094(12) 0.049(5) 0.101(9) -0.047(6) -0.042(8) 0.015(6) F10 0.17(2) 0.142(18) 0.105(11) -0.037(12) -0.004(14) -0.124(16) F11 0.074(8) 0.158(17) 0.035(5) -0.053(7) -0.012(4) -0.014(8) F12 0.091(15) 0.071(11) 0.048(7) -0.025(8) 0.000(7) -0.004(11) O1 0.086(3) 0.037(2) 0.043(2) -0.0102(18) -0.028(2) 0.009(2) B1 0.023(3) 0.016(2) 0.023(2) -0.0047(19) -0.0013(19) -0.0010(19) N1 0.0228(18) 0.0171(17) 0.0220(17) -0.0056(14) -0.0025(14) -0.0014(14) N3 0.034(2) 0.0249(19) 0.0224(18) -0.0076(15) 0.0068(16) -0.0048(16) N2 0.028(2) 0.0190(18) 0.031(2) -0.0057(16) -0.0001(16) -0.0038(15) N4 0.0230(19) 0.0223(18) 0.0235(18) -0.0075(15) -0.0012(14) -0.0041(15) N6 0.034(2) 0.028(2) 0.0235(19) -0.0089(16) -0.0048(16) -0.0003(17) N5 0.027(2) 0.0270(19) 0.0246(19) -0.0126(16) 0.0016(15) -0.0087(16) N7 0.0223(18) 0.0156(16) 0.0226(18) -0.0069(14) -0.0010(14) 0.0002(14) N9 0.024(2) 0.027(2) 0.042(2) -0.0082(18) 0.0029(17) 0.0003(16) N8 0.031(2) 0.0205(18) 0.035(2) -0.0113(16) -0.0054(16) 0.0085(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.857(5) . ? Rh1 B1 2.153(5) . ? Rh1 S3 2.3860(13) . ? Rh1 S2 2.3866(12) . ? Rh1 S1 2.3965(12) . ? Rh1 P1 2.4947(12) . ? Cl1 C35 1.794(7) . ? Cl2 C35 1.727(7) . ? Cl3 C36 1.765(8) . ? Cl4 C36 1.748(8) . ? S1 C2 1.714(4) . ? S2 C7 1.715(5) . ? S3 C12 1.716(4) . ? C1 O1 1.146(6) . ? C2 N1 1.332(5) . ? C2 N3 1.346(5) . ? C3 N2 1.297(5) . ? C3 N3 1.387(6) . ? C3 C4 1.477(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.480(6) . ? C5 C6 1.494(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N4 1.320(5) . ? C7 N6 1.352(5) . ? C8 N5 1.297(6) . ? C8 N6 1.383(6) . ? C8 C9 1.478(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N6 1.469(6) . ? C10 C11 1.499(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N7 1.309(5) . ? C12 N9 1.357(6) . ? C13 N8 1.279(6) . ? C13 N9 1.374(6) . ? C13 C14 1.492(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N9 1.473(6) . ? C15 C16 1.500(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.400(6) . ? C17 C18 1.406(6) . ? C17 P1 1.815(4) . ? C18 C19 1.382(6) . ? C18 H18 0.9500 . ? C19 C20 1.376(7) . ? C19 H19 0.9500 . ? C20 C21 1.371(7) . ? C20 H20 0.9500 . ? C21 C22 1.391(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.393(6) . ? C23 C24 1.396(6) . ? C23 P1 1.821(4) . ? C24 C25 1.379(6) . ? C24 H24 0.9500 . ? C25 C26 1.374(7) . ? C25 H25 0.9500 . ? C26 C27 1.387(7) . ? C26 H26 0.9500 . ? C27 C28 1.385(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.392(6) . ? C29 C30 1.397(6) . ? C29 P1 1.823(4) . ? C30 C31 1.367(6) . ? C30 H30 0.9500 . ? C31 C32 1.389(7) . ? C31 H31 0.9500 . ? C32 C33 1.371(7) . ? C32 H32 0.9500 . ? C33 C34 1.390(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? P2 F4 1.43(2) . ? P2 F10 1.46(3) . ? P2 F1 1.51(3) . ? P2 F5 1.53(3) . ? P2 F8 1.548(18) . ? P2 F12 1.59(4) . ? P2 F6 1.58(5) . ? P2 F7 1.58(3) . ? P2 F11 1.626(19) . ? P2 F3 1.68(2) . ? P2 F2 1.68(2) . ? P2 F9 1.726(16) . ? B1 N7 1.533(6) . ? B1 N1 1.533(6) . ? B1 N4 1.546(6) . ? N1 N2 1.389(4) . ? N4 N5 1.383(5) . ? N7 N8 1.389(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 B1 87.10(19) . . ? C1 Rh1 S3 85.58(16) . . ? B1 Rh1 S3 84.37(13) . . ? C1 Rh1 S2 175.11(15) . . ? B1 Rh1 S2 88.02(13) . . ? S3 Rh1 S2 94.29(5) . . ? C1 Rh1 S1 84.53(16) . . ? B1 Rh1 S1 84.14(13) . . ? S3 Rh1 S1 165.19(4) . . ? S2 Rh1 S1 94.62(5) . . ? C1 Rh1 P1 96.15(15) . . ? B1 Rh1 P1 176.60(13) . . ? S3 Rh1 P1 96.83(4) . . ? S2 Rh1 P1 88.72(4) . . ? S1 Rh1 P1 95.17(4) . . ? C2 S1 Rh1 95.80(15) . . ? C7 S2 Rh1 95.92(15) . . ? C12 S3 Rh1 95.97(15) . . ? O1 C1 Rh1 177.4(4) . . ? N1 C2 N3 107.4(4) . . ? N1 C2 S1 123.0(3) . . ? N3 C2 S1 129.6(3) . . ? N2 C3 N3 110.9(4) . . ? N2 C3 C4 125.2(4) . . ? N3 C3 C4 123.9(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 113.8(4) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N6 106.9(4) . . ? N4 C7 S2 124.7(3) . . ? N6 C7 S2 128.4(3) . . ? N5 C8 N6 110.6(4) . . ? N5 C8 C9 124.8(4) . . ? N6 C8 C9 124.6(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 C11 111.6(4) . . ? N6 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N6 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N9 107.2(4) . . ? N7 C12 S3 124.7(3) . . ? N9 C12 S3 128.1(3) . . ? N8 C13 N9 111.6(4) . . ? N8 C13 C14 125.5(4) . . ? N9 C13 C14 122.9(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 C16 110.0(4) . . ? N9 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N9 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 118.2(4) . . ? C22 C17 P1 122.5(4) . . ? C18 C17 P1 119.3(3) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 119.9(5) . . ? C21 C22 H22 120.1 . . ? C17 C22 H22 120.1 . . ? C28 C23 C24 118.6(4) . . ? C28 C23 P1 123.4(3) . . ? C24 C23 P1 117.9(3) . . ? C25 C24 C23 120.8(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 120.1(5) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.9(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 120.4(4) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? C34 C29 C30 118.1(4) . . ? C34 C29 P1 124.1(3) . . ? C30 C29 P1 117.6(3) . . ? C31 C30 C29 121.3(4) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 119.7(4) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.5(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 120.3(4) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? Cl2 C35 Cl1 111.4(4) . . ? Cl2 C35 H35A 109.4 . . ? Cl1 C35 H35A 109.4 . . ? Cl2 C35 H35B 109.4 . . ? Cl1 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? Cl4 C36 Cl3 111.8(4) . . ? Cl4 C36 H36A 109.3 . . ? Cl3 C36 H36A 109.3 . . ? Cl4 C36 H36B 109.3 . . ? Cl3 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C17 P1 C23 103.1(2) . . ? C17 P1 C29 106.1(2) . . ? C23 P1 C29 103.8(2) . . ? C17 P1 Rh1 115.96(15) . . ? C23 P1 Rh1 116.31(15) . . ? C29 P1 Rh1 110.41(13) . . ? F4 P2 F1 91.6(11) . . ? F4 P2 F5 98.8(19) . . ? F1 P2 F5 84(2) . . ? F10 P2 F8 96.6(10) . . ? F10 P2 F12 86.4(17) . . ? F8 P2 F12 91.7(15) . . ? F4 P2 F6 91.1(16) . . ? F1 P2 F6 175(2) . . ? F5 P2 F6 99(3) . . ? F10 P2 F7 94(2) . . ? F8 P2 F7 168(2) . . ? F12 P2 F7 83(2) . . ? F10 P2 F11 96.8(13) . . ? F8 P2 F11 89.9(11) . . ? F12 P2 F11 176.3(17) . . ? F7 P2 F11 94.7(18) . . ? F4 P2 F3 91.3(13) . . ? F1 P2 F3 87.8(14) . . ? F5 P2 F3 167.4(16) . . ? F6 P2 F3 88(2) . . ? F4 P2 F2 169(2) . . ? F1 P2 F2 81.1(14) . . ? F5 P2 F2 88.7(17) . . ? F6 P2 F2 95.7(18) . . ? F3 P2 F2 80.3(13) . . ? F10 P2 F9 174.8(11) . . ? F8 P2 F9 85.5(13) . . ? F12 P2 F9 88.9(14) . . ? F7 P2 F9 83.7(13) . . ? F11 P2 F9 87.9(9) . . ? N7 B1 N1 112.7(3) . . ? N7 B1 N4 109.0(3) . . ? N1 B1 N4 110.7(3) . . ? N7 B1 Rh1 108.8(3) . . ? N1 B1 Rh1 107.9(3) . . ? N4 B1 Rh1 107.5(3) . . ? C2 N1 N2 110.1(3) . . ? C2 N1 B1 120.8(3) . . ? N2 N1 B1 128.9(3) . . ? C2 N3 C3 106.4(3) . . ? C2 N3 C5 125.5(4) . . ? C3 N3 C5 128.1(4) . . ? C3 N2 N1 105.2(3) . . ? C7 N4 N5 110.9(3) . . ? C7 N4 B1 123.7(4) . . ? N5 N4 B1 125.3(3) . . ? C7 N6 C8 106.5(4) . . ? C7 N6 C10 125.5(4) . . ? C8 N6 C10 127.6(4) . . ? C8 N5 N4 105.1(3) . . ? C12 N7 N8 110.4(3) . . ? C12 N7 B1 119.9(3) . . ? N8 N7 B1 128.6(3) . . ? C12 N9 C13 105.7(4) . . ? C12 N9 C15 125.4(4) . . ? C13 N9 C15 128.8(4) . . ? C13 N8 N7 105.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 S1 C2 66.2(2) . . . . ? B1 Rh1 S1 C2 -21.4(2) . . . . ? S3 Rh1 S1 C2 17.9(3) . . . . ? S2 Rh1 S1 C2 -108.96(16) . . . . ? P1 Rh1 S1 C2 161.91(16) . . . . ? B1 Rh1 S2 C7 1.1(2) . . . . ? S3 Rh1 S2 C7 -83.08(16) . . . . ? S1 Rh1 S2 C7 85.07(16) . . . . ? P1 Rh1 S2 C7 -179.84(16) . . . . ? C1 Rh1 S3 C12 -70.2(2) . . . . ? B1 Rh1 S3 C12 17.4(2) . . . . ? S2 Rh1 S3 C12 104.94(16) . . . . ? S1 Rh1 S3 C12 -21.9(3) . . . . ? P1 Rh1 S3 C12 -165.83(16) . . . . ? Rh1 S1 C2 N1 16.8(4) . . . . ? Rh1 S1 C2 N3 -164.7(4) . . . . ? Rh1 S2 C7 N4 -3.8(4) . . . . ? Rh1 S2 C7 N6 178.2(4) . . . . ? Rh1 S3 C12 N7 -11.5(4) . . . . ? Rh1 S3 C12 N9 171.7(4) . . . . ? C22 C17 C18 C19 1.2(7) . . . . ? P1 C17 C18 C19 -179.7(4) . . . . ? C17 C18 C19 C20 -1.6(7) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? C20 C21 C22 C17 -0.8(7) . . . . ? C18 C17 C22 C21 0.0(7) . . . . ? P1 C17 C22 C21 -179.0(4) . . . . ? C28 C23 C24 C25 -0.9(7) . . . . ? P1 C23 C24 C25 -177.8(4) . . . . ? C23 C24 C25 C26 0.0(7) . . . . ? C24 C25 C26 C27 0.8(8) . . . . ? C25 C26 C27 C28 -0.6(8) . . . . ? C26 C27 C28 C23 -0.4(7) . . . . ? C24 C23 C28 C27 1.1(7) . . . . ? P1 C23 C28 C27 177.8(4) . . . . ? C34 C29 C30 C31 2.1(6) . . . . ? P1 C29 C30 C31 178.2(3) . . . . ? C29 C30 C31 C32 -1.7(7) . . . . ? C30 C31 C32 C33 -0.1(7) . . . . ? C31 C32 C33 C34 1.4(7) . . . . ? C32 C33 C34 C29 -0.9(7) . . . . ? C30 C29 C34 C33 -0.8(6) . . . . ? P1 C29 C34 C33 -176.6(3) . . . . ? C22 C17 P1 C23 0.8(4) . . . . ? C18 C17 P1 C23 -178.2(4) . . . . ? C22 C17 P1 C29 -107.9(4) . . . . ? C18 C17 P1 C29 73.1(4) . . . . ? C22 C17 P1 Rh1 129.1(3) . . . . ? C18 C17 P1 Rh1 -49.9(4) . . . . ? C28 C23 P1 C17 -88.8(4) . . . . ? C24 C23 P1 C17 87.9(4) . . . . ? C28 C23 P1 C29 21.7(4) . . . . ? C24 C23 P1 C29 -161.6(3) . . . . ? C28 C23 P1 Rh1 143.1(3) . . . . ? C24 C23 P1 Rh1 -40.1(4) . . . . ? C34 C29 P1 C17 -18.0(4) . . . . ? C30 C29 P1 C17 166.2(3) . . . . ? C34 C29 P1 C23 -126.3(4) . . . . ? C30 C29 P1 C23 57.9(4) . . . . ? C34 C29 P1 Rh1 108.4(3) . . . . ? C30 C29 P1 Rh1 -67.4(3) . . . . ? C1 Rh1 P1 C17 144.1(2) . . . . ? S3 Rh1 P1 C17 -129.65(17) . . . . ? S2 Rh1 P1 C17 -35.48(17) . . . . ? S1 Rh1 P1 C17 59.05(17) . . . . ? C1 Rh1 P1 C23 -94.5(2) . . . . ? S3 Rh1 P1 C23 -8.19(16) . . . . ? S2 Rh1 P1 C23 85.98(16) . . . . ? S1 Rh1 P1 C23 -179.49(16) . . . . ? C1 Rh1 P1 C29 23.4(2) . . . . ? S3 Rh1 P1 C29 109.65(15) . . . . ? S2 Rh1 P1 C29 -156.18(15) . . . . ? S1 Rh1 P1 C29 -61.65(15) . . . . ? C1 Rh1 B1 N7 63.2(3) . . . . ? S3 Rh1 B1 N7 -22.6(3) . . . . ? S2 Rh1 B1 N7 -117.1(3) . . . . ? S1 Rh1 B1 N7 148.0(3) . . . . ? C1 Rh1 B1 N1 -59.4(3) . . . . ? S3 Rh1 B1 N1 -145.2(3) . . . . ? S2 Rh1 B1 N1 120.3(3) . . . . ? S1 Rh1 B1 N1 25.4(3) . . . . ? C1 Rh1 B1 N4 -178.8(3) . . . . ? S3 Rh1 B1 N4 95.3(3) . . . . ? S2 Rh1 B1 N4 0.8(3) . . . . ? S1 Rh1 B1 N4 -94.0(3) . . . . ? N3 C2 N1 N2 -0.8(5) . . . . ? S1 C2 N1 N2 178.0(3) . . . . ? N3 C2 N1 B1 -176.0(4) . . . . ? S1 C2 N1 B1 2.9(6) . . . . ? N7 B1 N1 C2 -144.2(4) . . . . ? N4 B1 N1 C2 93.4(5) . . . . ? Rh1 B1 N1 C2 -24.0(5) . . . . ? N7 B1 N1 N2 41.7(6) . . . . ? N4 B1 N1 N2 -80.7(5) . . . . ? Rh1 B1 N1 N2 161.9(3) . . . . ? N1 C2 N3 C3 0.4(5) . . . . ? S1 C2 N3 C3 -178.4(4) . . . . ? N1 C2 N3 C5 -176.2(4) . . . . ? S1 C2 N3 C5 5.0(7) . . . . ? N2 C3 N3 C2 0.2(5) . . . . ? C4 C3 N3 C2 -179.1(4) . . . . ? N2 C3 N3 C5 176.7(4) . . . . ? C4 C3 N3 C5 -2.6(7) . . . . ? C6 C5 N3 C2 -94.3(5) . . . . ? C6 C5 N3 C3 89.9(6) . . . . ? N3 C3 N2 N1 -0.7(5) . . . . ? C4 C3 N2 N1 178.7(4) . . . . ? C2 N1 N2 C3 1.0(5) . . . . ? B1 N1 N2 C3 175.6(4) . . . . ? N6 C7 N4 N5 0.3(5) . . . . ? S2 C7 N4 N5 -178.0(3) . . . . ? N6 C7 N4 B1 -176.1(4) . . . . ? S2 C7 N4 B1 5.5(6) . . . . ? N7 B1 N4 C7 114.2(4) . . . . ? N1 B1 N4 C7 -121.3(4) . . . . ? Rh1 B1 N4 C7 -3.6(5) . . . . ? N7 B1 N4 N5 -61.7(5) . . . . ? N1 B1 N4 N5 62.8(5) . . . . ? Rh1 B1 N4 N5 -179.5(3) . . . . ? N4 C7 N6 C8 0.7(5) . . . . ? S2 C7 N6 C8 179.0(4) . . . . ? N4 C7 N6 C10 174.3(4) . . . . ? S2 C7 N6 C10 -7.4(7) . . . . ? N5 C8 N6 C7 -1.6(5) . . . . ? C9 C8 N6 C7 -179.5(4) . . . . ? N5 C8 N6 C10 -175.0(4) . . . . ? C9 C8 N6 C10 7.1(7) . . . . ? C11 C10 N6 C7 -90.1(6) . . . . ? C11 C10 N6 C8 82.1(6) . . . . ? N6 C8 N5 N4 1.8(5) . . . . ? C9 C8 N5 N4 179.6(4) . . . . ? C7 N4 N5 C8 -1.3(5) . . . . ? B1 N4 N5 C8 175.1(4) . . . . ? N9 C12 N7 N8 1.7(5) . . . . ? S3 C12 N7 N8 -175.6(3) . . . . ? N9 C12 N7 B1 170.7(4) . . . . ? S3 C12 N7 B1 -6.6(6) . . . . ? N1 B1 N7 C12 143.0(4) . . . . ? N4 B1 N7 C12 -93.7(4) . . . . ? Rh1 B1 N7 C12 23.3(5) . . . . ? N1 B1 N7 N8 -50.2(6) . . . . ? N4 B1 N7 N8 73.1(5) . . . . ? Rh1 B1 N7 N8 -169.9(3) . . . . ? N7 C12 N9 C13 -1.2(5) . . . . ? S3 C12 N9 C13 176.0(4) . . . . ? N7 C12 N9 C15 175.2(4) . . . . ? S3 C12 N9 C15 -7.6(7) . . . . ? N8 C13 N9 C12 0.2(5) . . . . ? C14 C13 N9 C12 -179.5(4) . . . . ? N8 C13 N9 C15 -176.1(5) . . . . ? C14 C13 N9 C15 4.3(8) . . . . ? C16 C15 N9 C12 -84.0(6) . . . . ? C16 C15 N9 C13 91.5(6) . . . . ? N9 C13 N8 N7 0.8(5) . . . . ? C14 C13 N8 N7 -179.5(4) . . . . ? C12 N7 N8 C13 -1.6(5) . . . . ? B1 N7 N8 C13 -169.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.571 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.106