Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Marcetta Darensbourg' _publ_contact_author_address ; Department of Chemistry Texas A & M University College Station Texas 77843-3225 UNITED STATES OF AMERICA ; _publ_contact_author_email MARCETTA@MAIL.CHEM.TAMU.EDU _publ_section_title ; NiN2S2 Complexes as Metallodithiolate Ligands to RhI, RhII, and RhIII ; loop_ _publ_author_name 'Marcetta Darensbourg' 'Kayla N. Green' 'Stephen P. Jeffery' 'Marilyn V. Rampersad' ; J.Reibenspies ; # Attachment 'CCDC291352.cif' data_mdm _database_code_depnum_ccdc_archive 'CCDC 291352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Cl N2 Ni O2 P Rh S2' _chemical_formula_weight 737.77 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.119(5) _cell_length_b 11.111(5) _cell_length_c 14.916(5) _cell_angle_alpha 82.768(5) _cell_angle_beta 79.333(5) _cell_angle_gamma 83.661(5) _cell_volume 1467.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6580 _exptl_absorpt_correction_T_max 0.7505 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9086 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6294 _reflns_number_gt 4954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.9705P] 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 6294 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.89980(4) 0.09555(3) 0.34021(2) 0.01969(12) Uani 1 1 d . . . Ni1 Ni 0.87855(6) 0.09222(5) 0.14254(4) 0.02015(15) Uani 1 1 d . . . O2 O 0.3417(4) 0.4865(4) 0.1147(3) 0.0405(9) Uani 1 1 d . . . H1O2 H 0.4129 0.5430 0.1054 0.061 Uiso 1 1 d R . . H2O2 H 0.2738 0.5603 0.1079 0.061 Uiso 1 1 d R . . S1 S 1.06727(12) 0.13552(11) 0.19772(7) 0.0232(2) Uani 1 1 d . . . S2 S 0.86246(12) -0.05726(10) 0.25117(7) 0.0219(2) Uani 1 1 d . . . P1 P 0.94390(12) 0.24952(10) 0.41562(7) 0.0181(2) Uani 1 1 d . . . O1 O 0.6579(4) 0.0138(3) 0.4909(2) 0.0353(8) Uani 1 1 d . . . Cl2 Cl 0.60170(13) 0.66735(11) 0.06070(8) 0.0293(3) Uani 1 1 d . . . N1 N 0.8933(4) 0.2371(4) 0.0530(2) 0.0237(8) Uani 1 1 d . . . N2 N 0.6923(4) 0.0564(4) 0.1064(2) 0.0229(8) Uani 1 1 d . . . C1 C 1.0659(6) 0.2957(4) 0.1466(3) 0.0272(10) Uani 1 1 d . . . H1A H 0.9868 0.3473 0.1825 0.033 Uiso 1 1 calc R . . H1B H 1.1639 0.3273 0.1448 0.033 Uiso 1 1 calc R . . C2 C 1.0351(5) 0.2955(4) 0.0506(3) 0.0263(10) Uani 1 1 d . . . H2A H 1.0257 0.3802 0.0210 0.032 Uiso 1 1 calc R . . H2B H 1.1200 0.2501 0.0138 0.032 Uiso 1 1 calc R . . C3 C 0.8986(5) 0.2058(5) -0.0428(3) 0.0265(10) Uani 1 1 d . . . H3A H 0.9866 0.1467 -0.0582 0.032 Uiso 1 1 calc R . . H3B H 0.9135 0.2805 -0.0860 0.032 Uiso 1 1 calc R . . C4 C 0.7596(5) 0.1523(5) -0.0571(3) 0.0286(10) Uani 1 1 d . . . H4A H 0.6738 0.2151 -0.0486 0.034 Uiso 1 1 calc R . . H4B H 0.7747 0.1328 -0.1213 0.034 Uiso 1 1 calc R . . C5 C 0.7196(5) 0.0394(5) 0.0058(3) 0.0273(10) Uani 1 1 d . . . H5A H 0.8017 -0.0258 -0.0061 0.033 Uiso 1 1 calc R . . H5B H 0.6283 0.0117 -0.0091 0.033 Uiso 1 1 calc R . . C6 C 0.7591(5) 0.3276(4) 0.0777(3) 0.0282(10) Uani 1 1 d . . . H6A H 0.7169 0.3582 0.0216 0.034 Uiso 1 1 calc R . . H6B H 0.7924 0.3978 0.1008 0.034 Uiso 1 1 calc R . . C7 C 0.6364(5) 0.2720(5) 0.1504(3) 0.0288(10) Uani 1 1 d . . . H7A H 0.6771 0.2491 0.2079 0.035 Uiso 1 1 calc R . . H7B H 0.5526 0.3356 0.1628 0.035 Uiso 1 1 calc R . . C8 C 0.5743(5) 0.1620(5) 0.1271(3) 0.0269(10) Uani 1 1 d . . . H8A H 0.5246 0.1860 0.0731 0.032 Uiso 1 1 calc R . . H8B H 0.4971 0.1341 0.1792 0.032 Uiso 1 1 calc R . . C9 C 0.6391(5) -0.0611(4) 0.1577(3) 0.0263(10) Uani 1 1 d . . . H9A H 0.6949 -0.1309 0.1274 0.032 Uiso 1 1 calc R . . H9B H 0.5313 -0.0633 0.1562 0.032 Uiso 1 1 calc R . . C10 C 0.6628(5) -0.0722(5) 0.2567(3) 0.0264(10) Uani 1 1 d . . . H10A H 0.6355 -0.1522 0.2890 0.032 Uiso 1 1 calc R . . H10B H 0.6008 -0.0071 0.2896 0.032 Uiso 1 1 calc R . . C11 C 0.7535(5) 0.0445(4) 0.4359(3) 0.0256(10) Uani 1 1 d . . . C12 C 0.8290(4) 0.2639(4) 0.5286(3) 0.0196(9) Uani 1 1 d . . . C13 C 0.7441(5) 0.3717(4) 0.5514(3) 0.0233(9) Uani 1 1 d . . . H13 H 0.7454 0.4414 0.5073 0.028 Uiso 1 1 calc R . . C14 C 0.6579(5) 0.3779(5) 0.6380(3) 0.0260(10) Uani 1 1 d . . . H14 H 0.6007 0.4517 0.6528 0.031 Uiso 1 1 calc R . . C15 C 0.6547(5) 0.2776(5) 0.7027(3) 0.0279(10) Uani 1 1 d . . . H15 H 0.5939 0.2818 0.7615 0.034 Uiso 1 1 calc R . . C16 C 0.7413(5) 0.1696(5) 0.6816(3) 0.0273(10) Uani 1 1 d . . . H16 H 0.7411 0.1009 0.7265 0.033 Uiso 1 1 calc R . . C17 C 0.8275(5) 0.1631(4) 0.5952(3) 0.0255(10) Uani 1 1 d . . . H17 H 0.8862 0.0897 0.5810 0.031 Uiso 1 1 calc R . . C18 C 1.1334(5) 0.2527(4) 0.4374(3) 0.0192(8) Uani 1 1 d . . . C19 C 1.1587(5) 0.2890(4) 0.5198(3) 0.0234(9) Uani 1 1 d . . . H19 H 1.0763 0.3071 0.5668 0.028 Uiso 1 1 calc R . . C20 C 1.3037(5) 0.2984(4) 0.5327(3) 0.0238(9) Uani 1 1 d . . . H20 H 1.3201 0.3246 0.5880 0.029 Uiso 1 1 calc R . . C21 C 1.4248(5) 0.2699(4) 0.4653(3) 0.0255(10) Uani 1 1 d . . . H21 H 1.5239 0.2754 0.4748 0.031 Uiso 1 1 calc R . . C22 C 1.4008(5) 0.2334(5) 0.3843(3) 0.0287(10) Uani 1 1 d . . . H22 H 1.4837 0.2152 0.3377 0.034 Uiso 1 1 calc R . . C23 C 1.2564(5) 0.2232(5) 0.3705(3) 0.0266(10) Uani 1 1 d . . . H23 H 1.2413 0.1961 0.3153 0.032 Uiso 1 1 calc R . . C24 C 0.9071(5) 0.3972(4) 0.3509(3) 0.0205(9) Uani 1 1 d . . . C25 C 0.7716(5) 0.4195(4) 0.3182(3) 0.0227(9) Uani 1 1 d . . . H25 H 0.6977 0.3631 0.3359 0.027 Uiso 1 1 calc R . . C26 C 0.7446(5) 0.5241(4) 0.2597(3) 0.0258(10) Uani 1 1 d . . . H26 H 0.6521 0.5391 0.2379 0.031 Uiso 1 1 calc R . . C27 C 0.8528(5) 0.6070(4) 0.2330(3) 0.0266(10) Uani 1 1 d . . . H27 H 0.8353 0.6774 0.1919 0.032 Uiso 1 1 calc R . . C28 C 0.9848(6) 0.5863(4) 0.2666(3) 0.0265(10) Uani 1 1 d . . . H28 H 1.0572 0.6441 0.2499 0.032 Uiso 1 1 calc R . . C29 C 1.0140(5) 0.4814(4) 0.3251(3) 0.0239(9) Uani 1 1 d . . . H29 H 1.1064 0.4675 0.3472 0.029 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 0.02168(19) 0.01867(19) 0.01941(19) -0.00152(13) -0.00518(13) -0.00273(13) Ni1 0.0224(3) 0.0196(3) 0.0190(3) -0.0017(2) -0.0054(2) -0.0017(2) O2 0.035(2) 0.041(2) 0.043(2) 0.0037(18) -0.0034(17) -0.0077(17) S1 0.0232(5) 0.0258(6) 0.0213(5) -0.0039(4) -0.0043(4) -0.0035(4) S2 0.0271(6) 0.0173(5) 0.0228(5) -0.0020(4) -0.0084(4) -0.0025(4) P1 0.0184(5) 0.0189(5) 0.0176(5) -0.0014(4) -0.0042(4) -0.0026(4) O1 0.0305(19) 0.037(2) 0.0358(19) 0.0022(16) 0.0002(16) -0.0104(16) Cl2 0.0273(6) 0.0294(6) 0.0324(6) -0.0008(5) -0.0096(5) -0.0022(5) N1 0.027(2) 0.026(2) 0.0171(17) -0.0017(15) -0.0007(15) -0.0012(16) N2 0.0240(19) 0.024(2) 0.0217(18) -0.0044(15) -0.0051(15) -0.0022(15) C1 0.033(3) 0.024(2) 0.024(2) -0.0023(19) -0.0001(19) -0.007(2) C2 0.030(2) 0.026(2) 0.022(2) -0.0019(19) -0.0004(18) -0.0055(19) C3 0.031(2) 0.030(3) 0.018(2) -0.0015(19) -0.0032(18) 0.000(2) C4 0.029(2) 0.035(3) 0.022(2) -0.007(2) -0.0063(19) 0.004(2) C5 0.026(2) 0.030(3) 0.027(2) -0.012(2) -0.0047(19) 0.001(2) C6 0.032(3) 0.023(2) 0.026(2) 0.0017(19) -0.0017(19) 0.004(2) C7 0.030(2) 0.029(3) 0.025(2) -0.004(2) -0.0019(19) 0.004(2) C8 0.024(2) 0.034(3) 0.022(2) -0.002(2) -0.0053(18) 0.000(2) C9 0.026(2) 0.028(2) 0.027(2) -0.0021(19) -0.0078(19) -0.0077(19) C10 0.028(2) 0.027(2) 0.027(2) -0.0001(19) -0.0072(19) -0.0114(19) C11 0.027(2) 0.022(2) 0.030(2) -0.0053(19) -0.011(2) -0.0008(19) C12 0.0151(19) 0.025(2) 0.019(2) -0.0030(17) -0.0034(16) -0.0022(17) C13 0.022(2) 0.023(2) 0.025(2) -0.0028(18) -0.0051(17) -0.0049(18) C14 0.019(2) 0.030(2) 0.029(2) -0.008(2) -0.0023(18) 0.0001(19) C15 0.024(2) 0.040(3) 0.021(2) -0.005(2) -0.0025(18) -0.008(2) C16 0.032(2) 0.029(3) 0.020(2) 0.0018(19) -0.0069(19) -0.001(2) C17 0.024(2) 0.025(2) 0.028(2) -0.0057(19) -0.0069(18) 0.0022(19) C18 0.021(2) 0.019(2) 0.0186(19) -0.0006(17) -0.0045(16) -0.0040(17) C19 0.023(2) 0.025(2) 0.023(2) -0.0015(18) -0.0070(17) -0.0024(18) C20 0.026(2) 0.024(2) 0.025(2) -0.0034(18) -0.0119(18) -0.0025(18) C21 0.021(2) 0.029(2) 0.026(2) 0.0018(19) -0.0043(18) -0.0050(19) C22 0.021(2) 0.038(3) 0.026(2) -0.004(2) 0.0005(18) -0.003(2) C23 0.023(2) 0.035(3) 0.022(2) -0.005(2) -0.0041(18) -0.008(2) C24 0.023(2) 0.018(2) 0.021(2) -0.0039(17) -0.0026(17) 0.0009(17) C25 0.028(2) 0.020(2) 0.019(2) -0.0019(17) -0.0030(17) 0.0003(18) C26 0.026(2) 0.026(2) 0.025(2) -0.0044(19) -0.0067(18) 0.0053(19) C27 0.034(2) 0.022(2) 0.022(2) -0.0010(18) -0.0035(19) 0.0018(19) C28 0.036(3) 0.022(2) 0.023(2) 0.0010(18) -0.0058(19) -0.0113(19) C29 0.025(2) 0.026(2) 0.023(2) -0.0034(18) -0.0065(18) -0.0036(18) _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 C11 1.843(5) . ? Rh1 P1 2.2710(13) . ? Rh1 S2 2.3719(13) . ? Rh1 S1 2.3994(13) . ? Rh1 Ni1 2.9955(12) . ? Ni1 N1 1.958(4) . ? Ni1 N2 1.968(4) . ? Ni1 S1 2.1628(15) . ? Ni1 S2 2.1665(14) . ? S1 C1 1.846(5) . ? S2 C10 1.832(5) . ? P1 C18 1.821(4) . ? P1 C24 1.826(5) . ? P1 C12 1.828(4) . ? O1 C11 1.132(6) . ? N1 C2 1.503(6) . ? N1 C3 1.503(6) . ? N1 C6 1.516(6) . ? N2 C5 1.508(6) . ? N2 C9 1.509(6) . ? N2 C8 1.524(6) . ? C1 C2 1.509(6) . ? C3 C4 1.518(7) . ? C4 C5 1.505(7) . ? C6 C7 1.531(7) . ? C7 C8 1.505(7) . ? C9 C10 1.520(6) . ? C12 C13 1.397(6) . ? C12 C17 1.399(6) . ? C13 C14 1.387(6) . ? C14 C15 1.378(7) . ? C15 C16 1.399(7) . ? C16 C17 1.386(6) . ? C18 C23 1.395(6) . ? C18 C19 1.407(6) . ? C19 C20 1.388(6) . ? C20 C21 1.386(6) . ? C21 C22 1.384(7) . ? C22 C23 1.388(6) . ? C24 C29 1.395(6) . ? C24 C25 1.398(6) . ? C25 C26 1.390(6) . ? C26 C27 1.394(7) . ? C27 C28 1.373(7) . ? C28 C29 1.397(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 P1 91.70(15) . . ? C11 Rh1 S2 92.33(15) . . ? P1 Rh1 S2 175.72(4) . . ? C11 Rh1 S1 167.87(15) . . ? P1 Rh1 S1 99.97(5) . . ? S2 Rh1 S1 75.92(5) . . ? C11 Rh1 Ni1 123.27(14) . . ? P1 Rh1 Ni1 130.26(3) . . ? S2 Rh1 Ni1 45.81(3) . . ? S1 Rh1 Ni1 45.63(4) . . ? N1 Ni1 N2 91.37(16) . . ? N1 Ni1 S1 91.35(12) . . ? N2 Ni1 S1 173.24(11) . . ? N1 Ni1 S2 174.76(12) . . ? N2 Ni1 S2 91.46(12) . . ? S1 Ni1 S2 85.37(5) . . ? N1 Ni1 Rh1 123.07(12) . . ? N2 Ni1 Rh1 121.09(11) . . ? S1 Ni1 Rh1 52.47(3) . . ? S2 Ni1 Rh1 51.72(4) . . ? C1 S1 Ni1 96.30(16) . . ? C1 S1 Rh1 116.32(16) . . ? Ni1 S1 Rh1 81.90(5) . . ? C10 S2 Ni1 95.99(16) . . ? C10 S2 Rh1 111.50(16) . . ? Ni1 S2 Rh1 82.47(5) . . ? C18 P1 C24 103.7(2) . . ? C18 P1 C12 102.89(19) . . ? C24 P1 C12 103.8(2) . . ? C18 P1 Rh1 117.44(15) . . ? C24 P1 Rh1 110.89(15) . . ? C12 P1 Rh1 116.45(15) . . ? C2 N1 C3 105.8(3) . . ? C2 N1 C6 109.7(4) . . ? C3 N1 C6 109.3(3) . . ? C2 N1 Ni1 111.3(3) . . ? C3 N1 Ni1 111.5(3) . . ? C6 N1 Ni1 109.2(3) . . ? C5 N2 C9 106.6(4) . . ? C5 N2 C8 110.8(3) . . ? C9 N2 C8 110.3(3) . . ? C5 N2 Ni1 110.1(3) . . ? C9 N2 Ni1 110.8(3) . . ? C8 N2 Ni1 108.2(3) . . ? C2 C1 S1 105.8(3) . . ? N1 C2 C1 110.5(4) . . ? N1 C3 C4 114.4(4) . . ? C5 C4 C3 115.0(4) . . ? C4 C5 N2 114.2(4) . . ? N1 C6 C7 112.6(4) . . ? C8 C7 C6 116.3(4) . . ? C7 C8 N2 113.7(4) . . ? N2 C9 C10 110.5(4) . . ? C9 C10 S2 105.8(3) . . ? O1 C11 Rh1 175.8(4) . . ? C13 C12 C17 118.8(4) . . ? C13 C12 P1 122.6(3) . . ? C17 C12 P1 118.6(3) . . ? C14 C13 C12 120.5(4) . . ? C15 C14 C13 120.5(4) . . ? C14 C15 C16 119.8(4) . . ? C17 C16 C15 119.9(4) . . ? C16 C17 C12 120.6(4) . . ? C23 C18 C19 118.8(4) . . ? C23 C18 P1 120.2(3) . . ? C19 C18 P1 121.0(3) . . ? C20 C19 C18 120.1(4) . . ? C21 C20 C19 120.4(4) . . ? C22 C21 C20 119.8(4) . . ? C21 C22 C23 120.5(4) . . ? C22 C23 C18 120.4(4) . . ? C29 C24 C25 119.3(4) . . ? C29 C24 P1 122.8(3) . . ? C25 C24 P1 117.5(3) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C27 120.2(4) . . ? C28 C27 C26 119.6(4) . . ? C27 C28 C29 120.9(4) . . ? C24 C29 C28 119.8(4) . . ? 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 C11 Rh1 Ni1 N1 124.0(2) . . . . ? P1 Rh1 Ni1 N1 -3.03(14) . . . . ? S2 Rh1 Ni1 N1 179.24(14) . . . . ? S1 Rh1 Ni1 N1 -62.30(14) . . . . ? C11 Rh1 Ni1 N2 8.8(2) . . . . ? P1 Rh1 Ni1 N2 -118.25(14) . . . . ? S2 Rh1 Ni1 N2 64.02(14) . . . . ? S1 Rh1 Ni1 N2 -177.52(14) . . . . ? C11 Rh1 Ni1 S1 -173.71(18) . . . . ? P1 Rh1 Ni1 S1 59.28(6) . . . . ? S2 Rh1 Ni1 S1 -118.46(6) . . . . ? C11 Rh1 Ni1 S2 -55.26(18) . . . . ? P1 Rh1 Ni1 S2 177.73(5) . . . . ? S1 Rh1 Ni1 S2 118.46(6) . . . . ? N1 Ni1 S1 C1 16.31(19) . . . . ? N2 Ni1 S1 C1 -97.4(10) . . . . ? S2 Ni1 S1 C1 -159.59(16) . . . . ? Rh1 Ni1 S1 C1 -115.77(16) . . . . ? N1 Ni1 S1 Rh1 132.08(11) . . . . ? N2 Ni1 S1 Rh1 18.3(10) . . . . ? S2 Ni1 S1 Rh1 -43.82(4) . . . . ? C11 Rh1 S1 C1 118.9(7) . . . . ? P1 Rh1 S1 C1 -45.18(18) . . . . ? S2 Rh1 S1 C1 133.59(18) . . . . ? Ni1 Rh1 S1 C1 93.05(18) . . . . ? C11 Rh1 S1 Ni1 25.8(7) . . . . ? P1 Rh1 S1 Ni1 -138.23(4) . . . . ? S2 Rh1 S1 Ni1 40.54(4) . . . . ? N1 Ni1 S2 C10 104.0(13) . . . . ? N2 Ni1 S2 C10 -18.68(19) . . . . ? S1 Ni1 S2 C10 155.35(16) . . . . ? Rh1 Ni1 S2 C10 110.96(16) . . . . ? N1 Ni1 S2 Rh1 -7.0(13) . . . . ? N2 Ni1 S2 Rh1 -129.64(11) . . . . ? S1 Ni1 S2 Rh1 44.39(4) . . . . ? C11 Rh1 S2 C10 43.1(2) . . . . ? P1 Rh1 S2 C10 -117.4(6) . . . . ? S1 Rh1 S2 C10 -133.89(17) . . . . ? Ni1 Rh1 S2 C10 -93.51(17) . . . . ? C11 Rh1 S2 Ni1 136.56(14) . . . . ? P1 Rh1 S2 Ni1 -23.9(6) . . . . ? S1 Rh1 S2 Ni1 -40.38(4) . . . . ? C11 Rh1 P1 C18 121.9(2) . . . . ? S2 Rh1 P1 C18 -77.7(6) . . . . ? S1 Rh1 P1 C18 -61.45(16) . . . . ? Ni1 Rh1 P1 C18 -100.05(16) . . . . ? C11 Rh1 P1 C24 -119.2(2) . . . . ? S2 Rh1 P1 C24 41.3(6) . . . . ? S1 Rh1 P1 C24 57.53(15) . . . . ? Ni1 Rh1 P1 C24 18.93(16) . . . . ? C11 Rh1 P1 C12 -0.8(2) . . . . ? S2 Rh1 P1 C12 159.7(5) . . . . ? S1 Rh1 P1 C12 175.93(15) . . . . ? Ni1 Rh1 P1 C12 137.32(15) . . . . ? N2 Ni1 N1 C2 -176.0(3) . . . . ? S1 Ni1 N1 C2 10.2(3) . . . . ? S2 Ni1 N1 C2 61.4(14) . . . . ? Rh1 Ni1 N1 C2 54.8(3) . . . . ? N2 Ni1 N1 C3 -58.1(3) . . . . ? S1 Ni1 N1 C3 128.1(3) . . . . ? S2 Ni1 N1 C3 179(90) . . . . ? Rh1 Ni1 N1 C3 172.7(2) . . . . ? N2 Ni1 N1 C6 62.8(3) . . . . ? S1 Ni1 N1 C6 -111.1(3) . . . . ? S2 Ni1 N1 C6 -59.9(14) . . . . ? Rh1 Ni1 N1 C6 -66.4(3) . . . . ? N1 Ni1 N2 C5 59.0(3) . . . . ? S1 Ni1 N2 C5 172.7(9) . . . . ? S2 Ni1 N2 C5 -125.4(3) . . . . ? Rh1 Ni1 N2 C5 -170.3(2) . . . . ? N1 Ni1 N2 C9 176.7(3) . . . . ? S1 Ni1 N2 C9 -69.6(11) . . . . ? S2 Ni1 N2 C9 -7.7(3) . . . . ? Rh1 Ni1 N2 C9 -52.6(3) . . . . ? N1 Ni1 N2 C8 -62.2(3) . . . . ? S1 Ni1 N2 C8 51.5(11) . . . . ? S2 Ni1 N2 C8 113.3(3) . . . . ? Rh1 Ni1 N2 C8 68.4(3) . . . . ? Ni1 S1 C1 C2 -40.9(3) . . . . ? Rh1 S1 C1 C2 -124.9(3) . . . . ? C3 N1 C2 C1 -162.6(4) . . . . ? C6 N1 C2 C1 79.7(5) . . . . ? Ni1 N1 C2 C1 -41.3(4) . . . . ? S1 C1 C2 N1 55.1(4) . . . . ? C2 N1 C3 C4 -176.4(4) . . . . ? C6 N1 C3 C4 -58.4(5) . . . . ? Ni1 N1 C3 C4 62.5(4) . . . . ? N1 C3 C4 C5 -56.8(5) . . . . ? C3 C4 C5 N2 58.7(5) . . . . ? C9 N2 C5 C4 174.5(4) . . . . ? C8 N2 C5 C4 54.4(5) . . . . ? Ni1 N2 C5 C4 -65.2(4) . . . . ? C2 N1 C6 C7 -134.4(4) . . . . ? C3 N1 C6 C7 110.1(4) . . . . ? Ni1 N1 C6 C7 -12.2(5) . . . . ? N1 C6 C7 C8 -57.7(6) . . . . ? C6 C7 C8 N2 58.0(5) . . . . ? C5 N2 C8 C7 -109.4(4) . . . . ? C9 N2 C8 C7 132.8(4) . . . . ? Ni1 N2 C8 C7 11.4(4) . . . . ? C5 N2 C9 C10 159.2(4) . . . . ? C8 N2 C9 C10 -80.5(4) . . . . ? Ni1 N2 C9 C10 39.3(4) . . . . ? N2 C9 C10 S2 -55.7(4) . . . . ? Ni1 S2 C10 C9 42.8(3) . . . . ? Rh1 S2 C10 C9 127.0(3) . . . . ? P1 Rh1 C11 O1 125(6) . . . . ? S2 Rh1 C11 O1 -53(6) . . . . ? S1 Rh1 C11 O1 -39(6) . . . . ? Ni1 Rh1 C11 O1 -17(6) . . . . ? C18 P1 C12 C13 105.0(4) . . . . ? C24 P1 C12 C13 -2.9(4) . . . . ? Rh1 P1 C12 C13 -125.1(3) . . . . ? C18 P1 C12 C17 -74.2(4) . . . . ? C24 P1 C12 C17 177.9(3) . . . . ? Rh1 P1 C12 C17 55.7(4) . . . . ? C17 C12 C13 C14 -1.2(6) . . . . ? P1 C12 C13 C14 179.6(3) . . . . ? C12 C13 C14 C15 -0.1(7) . . . . ? C13 C14 C15 C16 1.3(7) . . . . ? C14 C15 C16 C17 -1.3(7) . . . . ? C15 C16 C17 C12 0.1(7) . . . . ? C13 C12 C17 C16 1.2(7) . . . . ? P1 C12 C17 C16 -179.6(4) . . . . ? C24 P1 C18 C23 -82.9(4) . . . . ? C12 P1 C18 C23 169.1(4) . . . . ? Rh1 P1 C18 C23 39.8(4) . . . . ? C24 P1 C18 C19 94.7(4) . . . . ? C12 P1 C18 C19 -13.3(4) . . . . ? Rh1 P1 C18 C19 -142.6(3) . . . . ? C23 C18 C19 C20 1.8(7) . . . . ? P1 C18 C19 C20 -175.8(3) . . . . ? C18 C19 C20 C21 -1.3(7) . . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C20 C21 C22 C23 -1.1(8) . . . . ? C21 C22 C23 C18 1.6(8) . . . . ? C19 C18 C23 C22 -2.0(7) . . . . ? P1 C18 C23 C22 175.6(4) . . . . ? C18 P1 C24 C29 2.8(4) . . . . ? C12 P1 C24 C29 110.0(4) . . . . ? Rh1 P1 C24 C29 -124.2(3) . . . . ? C18 P1 C24 C25 175.7(3) . . . . ? C12 P1 C24 C25 -77.0(4) . . . . ? Rh1 P1 C24 C25 48.8(4) . . . . ? C29 C24 C25 C26 0.6(6) . . . . ? P1 C24 C25 C26 -172.6(3) . . . . ? C24 C25 C26 C27 0.3(7) . . . . ? C25 C26 C27 C28 -1.6(7) . . . . ? C26 C27 C28 C29 1.9(7) . . . . ? C25 C24 C29 C28 -0.3(6) . . . . ? P1 C24 C29 C28 172.5(3) . . . . ? C27 C28 C29 C24 -0.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 3.439 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.176 # Attachment 'CCDC291354.cif' data_rh _database_code_depnum_ccdc_archive 'CCDC 291354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H84 F12 N14 Ni4 O8 Rh2 S8' _chemical_formula_weight 1930.46 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.611(3) _cell_length_b 12.738(3) _cell_length_c 13.248(3) _cell_angle_alpha 102.397(4) _cell_angle_beta 94.325(4) _cell_angle_gamma 118.550(4) _cell_volume 1786.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 935 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 1.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6131 _exptl_absorpt_correction_T_max 0.7138 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9336 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6143 _reflns_number_gt 5564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+3.4578P] 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 6143 _refine_ls_number_parameters 498 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.282 _refine_ls_shift/su_mean 0.018 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 0.03524(2) 0.41301(2) 0.02134(2) 0.02091(11) Uani 1 1 d . . . Ni1 Ni 0.27323(4) 0.65580(4) -0.08513(4) 0.02455(14) Uani 1 1 d . . . Ni2 Ni 0.14079(4) 0.69093(4) 0.25963(4) 0.02568(14) Uani 1 1 d . . . S1 S 0.17081(9) 0.73482(9) -0.01796(8) 0.0290(2) Uani 1 1 d . . . S2 S 0.24489(8) 0.55132(9) 0.02612(7) 0.0269(2) Uani 1 1 d . . . S3 S -0.00689(8) 0.67919(9) 0.16008(7) 0.0245(2) Uani 1 1 d . . . S4 S 0.06576(9) 0.49521(9) 0.20572(7) 0.0262(2) Uani 1 1 d . . . N1 N 0.3136(3) 0.7503(3) -0.1847(3) 0.0362(8) Uani 1 1 d . . . N2 N 0.3733(4) 0.5961(3) -0.1489(3) 0.0396(9) Uani 1 1 d . . . N3 N 0.2146(3) 0.8673(3) 0.3187(3) 0.0375(8) Uani 1 1 d . . . N4 N 0.2730(3) 0.7136(3) 0.3595(3) 0.0389(8) Uani 1 1 d . . . N5 N 0.0889(3) 0.2827(3) 0.0555(2) 0.0265(7) Uani 1 1 d . . . C1 C 0.1700(5) 0.8106(5) -0.1238(4) 0.0476(12) Uani 1 1 d . . . H1A H 0.1013 0.7503 -0.1845 0.057 Uiso 1 1 calc R . . H1B H 0.1584 0.8823 -0.0966 0.057 Uiso 1 1 calc R . . C2 C 0.2876(6) 0.8529(5) -0.1571(4) 0.0536(13) Uani 1 1 d . . . H2A H 0.3544 0.9226 -0.0993 0.064 Uiso 1 1 calc R . . H2B H 0.2853 0.8840 -0.2191 0.064 Uiso 1 1 calc R . . C3 C 0.2431(5) 0.6608(4) -0.2905(3) 0.0413(10) Uani 1 1 d . . . H3A H 0.2529 0.7082 -0.3428 0.050 Uiso 1 1 calc R . . H3B H 0.1543 0.6155 -0.2885 0.050 Uiso 1 1 calc R . . C4 C 0.2829(5) 0.5681(5) -0.3264(4) 0.0459(11) Uani 1 1 d . . . H4A H 0.2209 0.5027 -0.3893 0.055 Uiso 1 1 calc R . . H4B H 0.3617 0.6111 -0.3497 0.055 Uiso 1 1 calc R . . C5 C 0.3007(5) 0.5054(5) -0.2508(4) 0.0448(11) Uani 1 1 d . . . H5A H 0.2193 0.4430 -0.2416 0.054 Uiso 1 1 calc R . . H5B H 0.3436 0.4612 -0.2788 0.054 Uiso 1 1 calc R . . C6 C 0.4521(5) 0.8008(5) -0.1841(4) 0.0562(14) Uani 1 1 d . . . H6A H 0.5023 0.8826 -0.1300 0.067 Uiso 1 1 calc R . . H6B H 0.4691 0.8123 -0.2539 0.067 Uiso 1 1 calc R . . C7 C 0.4867(4) 0.7047(4) -0.1587(4) 0.0424(11) Uani 1 1 d . . . H7A H 0.5220 0.6776 -0.2161 0.051 Uiso 1 1 calc R . . H7B H 0.5490 0.7439 -0.0920 0.051 Uiso 1 1 calc R . . C8 C 0.4151(5) 0.5382(5) -0.0769(4) 0.0480(12) Uani 1 1 d . . . H8A H 0.4471 0.4885 -0.1171 0.058 Uiso 1 1 calc R . . H8B H 0.4823 0.6049 -0.0177 0.058 Uiso 1 1 calc R . . C9 C 0.3127(4) 0.4597(4) -0.0364(4) 0.0380(10) Uani 1 1 d . . . H9A H 0.3408 0.4288 0.0162 0.046 Uiso 1 1 calc R . . H9B H 0.2499 0.3869 -0.0946 0.046 Uiso 1 1 calc R . . C10 C 0.0604(4) 0.8492(4) 0.1838(3) 0.0323(9) Uani 1 1 d . . . H10A H 0.1180 0.8790 0.1361 0.039 Uiso 1 1 calc R . . H10B H -0.0057 0.8683 0.1697 0.039 Uiso 1 1 calc R . . C11 C 0.1272(5) 0.9120(4) 0.2955(4) 0.0422(10) Uani 1 1 d . . . H11A H 0.0676 0.8924 0.3429 0.051 Uiso 1 1 calc R . . H11B H 0.1737 1.0035 0.3078 0.051 Uiso 1 1 calc R . . C12 C 0.3274(4) 0.9250(4) 0.2757(4) 0.0415(10) Uani 1 1 d . . . H12A H 0.3605 1.0160 0.2932 0.050 Uiso 1 1 calc R . . H12B H 0.3055 0.8912 0.1978 0.050 Uiso 1 1 calc R . . C13 C 0.4250(4) 0.9024(5) 0.3177(4) 0.0483(12) Uani 1 1 d . . . H13A H 0.4627 0.9565 0.3913 0.058 Uiso 1 1 calc R . . H13B H 0.4902 0.9295 0.2760 0.058 Uiso 1 1 calc R . . C14 C 0.3867(4) 0.7721(5) 0.3176(4) 0.0418(11) Uani 1 1 d . . . H14A H 0.3724 0.7216 0.2445 0.050 Uiso 1 1 calc R . . H14B H 0.4543 0.7724 0.3611 0.050 Uiso 1 1 calc R . . C15 C 0.2502(5) 0.8967(4) 0.4367(4) 0.0460(12) Uani 1 1 d . . . H15A H 0.1809 0.8927 0.4696 0.055 Uiso 1 1 calc R . . H15B H 0.3223 0.9820 0.4659 0.055 Uiso 1 1 calc R . . C16 C 0.2825(4) 0.8001(5) 0.4619(3) 0.0433(11) Uani 1 1 d . . . H16A H 0.3673 0.8439 0.5049 0.052 Uiso 1 1 calc R . . H16B H 0.2247 0.7516 0.5029 0.052 Uiso 1 1 calc R . . C17 C 0.2470(5) 0.5923(5) 0.3782(4) 0.0426(11) Uani 1 1 d . . . H17A H 0.3237 0.6012 0.4144 0.051 Uiso 1 1 calc R . . H17B H 0.1857 0.5681 0.4238 0.051 Uiso 1 1 calc R . . C18 C 0.1984(4) 0.4949(4) 0.2749(3) 0.0344(9) Uani 1 1 d . . . H18A H 0.1719 0.4122 0.2859 0.041 Uiso 1 1 calc R . . H18B H 0.2631 0.5133 0.2325 0.041 Uiso 1 1 calc R . . C19 C 0.1153(3) 0.2177(4) 0.0775(3) 0.0250(8) Uani 1 1 d . . . C20 C 0.1468(4) 0.1296(4) 0.1090(3) 0.0329(9) Uani 1 1 d . . . H20A H 0.1479 0.0738 0.0458 0.049 Uiso 1 1 calc R . . H20B H 0.0850 0.0802 0.1457 0.049 Uiso 1 1 calc R . . H20C H 0.2284 0.1764 0.1561 0.049 Uiso 1 1 calc R . . C21 C 0.2472(4) 0.1121(4) 0.8608(4) 0.0404(10) Uani 1 1 d . . . O1 O 0.3351(4) 0.1419(4) 0.9305(3) 0.0730(12) Uani 1 1 d . A . O2 O 0.1354(3) 0.0470(3) 0.8568(3) 0.0428(7) Uani 1 1 d . A . C22A C 0.2774(5) 0.1542(5) 0.7609(5) 0.0532(13) Uani 0.58(9) 1 d PD A -1 F1A F 0.203(2) 0.191(3) 0.7280(18) 0.077(5) Uani 0.58(9) 1 d PD A -1 F2A F 0.265(3) 0.060(2) 0.6816(16) 0.055(4) Uani 0.58(9) 1 d PD A -1 F3A F 0.3902(11) 0.2495(19) 0.767(3) 0.075(5) Uani 0.58(9) 1 d PD A -1 C22B C 0.2774(5) 0.1542(5) 0.7609(5) 0.0532(13) Uani 0.42(9) 1 d PD A -2 F1B F 0.1886(17) 0.164(3) 0.708(3) 0.070(6) Uani 0.42(9) 1 d PD A -2 F2B F 0.297(4) 0.074(3) 0.693(3) 0.059(6) Uani 0.42(9) 1 d PD A -2 F3B F 0.3846(18) 0.262(2) 0.787(4) 0.083(8) Uani 0.42(9) 1 d PD A -2 C23 C 0.3993(4) 0.2533(4) 0.4199(3) 0.0331(9) Uani 1 1 d . . . O3 O 0.4793(3) 0.2274(3) 0.4436(3) 0.0426(7) Uani 1 1 d . B . O4 O 0.3302(3) 0.2219(3) 0.3354(2) 0.0426(7) Uani 1 1 d . B . C24A C 0.3753(6) 0.3289(7) 0.5122(4) 0.0616(16) Uani 0.41(5) 1 d PD B -1 F4A F 0.369(3) 0.425(2) 0.4930(15) 0.072(6) Uani 0.41(5) 1 d PD B -1 F5A F 0.2722(10) 0.270(2) 0.5505(13) 0.070(6) Uani 0.41(5) 1 d PD B -1 F6A F 0.460(2) 0.372(3) 0.5998(12) 0.117(10) Uani 0.41(5) 1 d PD B -1 C24B C 0.3753(6) 0.3289(7) 0.5122(4) 0.0616(16) Uani 0.59(5) 1 d PD B -2 F4B F 0.322(2) 0.388(2) 0.4828(12) 0.105(6) Uani 0.59(5) 1 d PD B -2 F5B F 0.2799(12) 0.237(2) 0.5426(13) 0.107(6) Uani 0.59(5) 1 d PD B -2 F6B F 0.4687(8) 0.4021(15) 0.5942(9) 0.078(4) Uani 0.59(5) 1 d PD B -2 N6 N -0.0059(5) 0.3254(6) 0.4556(5) 0.0759(16) Uani 1 1 d . . . C25 C 0.0143(5) 0.2488(6) 0.4178(4) 0.0506(12) Uani 1 1 d . . . C26 C 0.0406(5) 0.1535(6) 0.3712(5) 0.0701(18) Uani 1 1 d . . . H26A H 0.0333 0.1028 0.4194 0.105 Uiso 1 1 calc R . . H26B H 0.1247 0.1922 0.3583 0.105 Uiso 1 1 calc R . . H26C H -0.0183 0.1003 0.3042 0.105 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 0.02294(18) 0.02130(18) 0.02087(18) 0.00671(12) 0.00319(12) 0.01292(13) Ni1 0.0271(3) 0.0254(3) 0.0250(3) 0.0092(2) 0.00866(19) 0.0150(2) Ni2 0.0249(3) 0.0223(3) 0.0280(3) 0.0059(2) -0.0021(2) 0.0122(2) S1 0.0272(5) 0.0234(5) 0.0373(5) 0.0081(4) 0.0113(4) 0.0131(4) S2 0.0228(4) 0.0300(5) 0.0287(5) 0.0114(4) 0.0021(4) 0.0133(4) S3 0.0253(4) 0.0285(5) 0.0227(4) 0.0056(4) 0.0033(3) 0.0169(4) S4 0.0337(5) 0.0242(5) 0.0217(4) 0.0070(4) 0.0028(4) 0.0156(4) N1 0.045(2) 0.0303(18) 0.0324(18) 0.0153(15) 0.0134(16) 0.0152(16) N2 0.041(2) 0.036(2) 0.049(2) 0.0139(17) 0.0214(17) 0.0229(17) N3 0.0318(18) 0.0276(18) 0.047(2) 0.0041(16) -0.0025(16) 0.0146(15) N4 0.0354(19) 0.0331(19) 0.042(2) 0.0078(16) -0.0065(16) 0.0163(16) N5 0.0297(17) 0.0269(16) 0.0244(16) 0.0087(13) 0.0031(13) 0.0154(14) C1 0.056(3) 0.040(3) 0.064(3) 0.029(2) 0.017(2) 0.031(2) C2 0.078(4) 0.044(3) 0.054(3) 0.023(2) 0.026(3) 0.037(3) C3 0.056(3) 0.046(3) 0.030(2) 0.0140(19) 0.0069(19) 0.031(2) C4 0.042(2) 0.044(3) 0.053(3) 0.013(2) 0.019(2) 0.021(2) C5 0.044(3) 0.048(3) 0.044(3) 0.007(2) 0.014(2) 0.026(2) C6 0.069(3) 0.040(3) 0.046(3) 0.022(2) 0.022(3) 0.012(2) C7 0.026(2) 0.050(3) 0.045(3) 0.003(2) 0.0069(18) 0.020(2) C8 0.040(3) 0.061(3) 0.054(3) 0.023(2) 0.013(2) 0.032(2) C9 0.047(3) 0.047(3) 0.040(2) 0.016(2) 0.0041(19) 0.038(2) C10 0.038(2) 0.028(2) 0.041(2) 0.0103(17) 0.0078(18) 0.0245(18) C11 0.051(3) 0.039(2) 0.042(2) 0.008(2) 0.011(2) 0.028(2) C12 0.049(3) 0.027(2) 0.037(2) 0.0058(18) 0.011(2) 0.0122(19) C13 0.036(2) 0.052(3) 0.042(3) 0.008(2) 0.008(2) 0.014(2) C14 0.033(2) 0.056(3) 0.034(2) 0.006(2) 0.0015(18) 0.025(2) C15 0.049(3) 0.028(2) 0.047(3) -0.0040(19) 0.022(2) 0.013(2) C16 0.029(2) 0.070(3) 0.027(2) 0.016(2) 0.0010(17) 0.022(2) C17 0.049(3) 0.050(3) 0.037(2) 0.016(2) 0.002(2) 0.031(2) C18 0.044(2) 0.033(2) 0.039(2) 0.0149(18) 0.0020(18) 0.028(2) C19 0.0195(17) 0.0279(19) 0.0192(17) 0.0007(15) 0.0040(14) 0.0080(15) C20 0.035(2) 0.035(2) 0.038(2) 0.0171(18) 0.0065(17) 0.0216(18) C21 0.040(3) 0.030(2) 0.048(3) 0.0023(19) 0.006(2) 0.020(2) O1 0.046(2) 0.085(3) 0.058(2) -0.001(2) -0.0085(19) 0.022(2) O2 0.0413(18) 0.0426(18) 0.0499(19) 0.0159(15) 0.0114(14) 0.0240(15) C22A 0.057(3) 0.054(3) 0.073(4) 0.026(3) 0.034(3) 0.040(3) F1A 0.127(14) 0.103(9) 0.082(7) 0.067(6) 0.081(9) 0.094(10) F2A 0.059(11) 0.075(6) 0.038(5) 0.006(4) 0.016(5) 0.044(7) F3A 0.057(7) 0.063(7) 0.120(14) 0.037(7) 0.056(6) 0.031(5) C22B 0.057(3) 0.054(3) 0.073(4) 0.026(3) 0.034(3) 0.040(3) F1B 0.039(9) 0.089(11) 0.107(12) 0.057(9) 0.011(9) 0.039(8) F2B 0.056(14) 0.071(9) 0.067(10) 0.024(7) 0.023(8) 0.043(9) F3B 0.091(14) 0.049(8) 0.120(15) 0.028(7) 0.079(10) 0.034(7) C23 0.034(2) 0.034(2) 0.032(2) 0.0100(17) 0.0086(18) 0.0175(18) O3 0.0431(17) 0.0451(18) 0.0411(17) 0.0025(14) 0.0025(14) 0.0284(15) O4 0.0408(17) 0.0512(19) 0.0314(16) 0.0049(14) 0.0006(13) 0.0238(15) C24A 0.062(4) 0.093(5) 0.043(3) 0.002(3) 0.007(3) 0.056(4) F4A 0.090(14) 0.062(8) 0.065(7) -0.017(7) -0.029(8) 0.062(9) F5A 0.035(6) 0.117(11) 0.049(6) -0.005(8) 0.011(5) 0.043(7) F6A 0.18(2) 0.22(2) 0.024(7) -0.027(8) -0.024(8) 0.18(2) C24B 0.062(4) 0.093(5) 0.043(3) 0.002(3) 0.007(3) 0.056(4) F4B 0.071(9) 0.106(9) 0.108(8) -0.058(8) -0.029(6) 0.065(7) F5B 0.105(9) 0.233(17) 0.061(6) 0.073(9) 0.058(6) 0.125(11) F6B 0.049(5) 0.077(7) 0.070(8) -0.040(4) -0.006(4) 0.029(6) N6 0.067(3) 0.073(4) 0.106(5) 0.036(3) 0.033(3) 0.044(3) C25 0.040(3) 0.070(4) 0.052(3) 0.026(3) 0.017(2) 0.031(3) C26 0.051(3) 0.069(4) 0.068(4) -0.010(3) 0.009(3) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N5 2.183(3) . ? Rh1 S3 2.3540(11) 2_565 ? Rh1 S1 2.3600(11) 2_565 ? Rh1 S2 2.3606(11) . ? Rh1 S4 2.3635(11) . ? Rh1 Rh1 2.8925(8) 2_565 ? Ni1 N1 1.910(3) . ? Ni1 N2 1.920(4) . ? Ni1 S1 2.1224(11) . ? Ni1 S2 2.1302(11) . ? Ni2 N4 1.912(4) . ? Ni2 N3 1.913(4) . ? Ni2 S4 2.1211(12) . ? Ni2 S3 2.1234(11) . ? S1 C1 1.868(5) . ? S1 Rh1 2.3599(11) 2_565 ? S2 C9 1.851(4) . ? S3 C10 1.849(4) . ? S3 Rh1 2.3540(11) 2_565 ? S4 C18 1.848(4) . ? N1 C2 1.473(6) . ? N1 C3 1.488(6) . ? N1 C6 1.545(7) . ? N2 C5 1.458(6) . ? N2 C7 1.480(6) . ? N2 C8 1.527(6) . ? N3 C12 1.481(6) . ? N3 C11 1.502(6) . ? N3 C15 1.506(6) . ? N4 C14 1.481(6) . ? N4 C17 1.500(6) . ? N4 C16 1.509(6) . ? N5 C19 1.111(5) . ? C1 C2 1.457(8) . ? C3 C4 1.496(7) . ? C4 C5 1.474(7) . ? C6 C7 1.571(8) . ? C8 C9 1.434(7) . ? C10 C11 1.483(6) . ? C12 C13 1.487(7) . ? C13 C14 1.490(7) . ? C15 C16 1.558(7) . ? C17 C18 1.485(6) . ? C19 C20 1.482(6) . ? C21 O2 1.237(6) . ? C21 O1 1.232(6) . ? C21 C22A 1.540(7) . ? C22A F1A 1.321(11) . ? C22A F3A 1.339(12) . ? C22A F2A 1.349(11) . ? C23 O4 1.226(5) . ? C23 O3 1.240(5) . ? C23 C24A 1.530(7) . ? C24A F6A 1.325(12) . ? C24A F4A 1.345(12) . ? C24A F5A 1.357(13) . ? N6 C25 1.147(8) . ? C25 C26 1.434(8) . ? 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 N5 Rh1 S3 88.79(9) . 2_565 ? N5 Rh1 S1 88.31(9) . 2_565 ? S3 Rh1 S1 89.87(3) 2_565 2_565 ? N5 Rh1 S2 88.01(9) . . ? S3 Rh1 S2 89.75(3) 2_565 . ? S1 Rh1 S2 176.31(3) 2_565 . ? N5 Rh1 S4 87.50(9) . . ? S3 Rh1 S4 176.26(3) 2_565 . ? S1 Rh1 S4 89.56(4) 2_565 . ? S2 Rh1 S4 90.59(3) . . ? N5 Rh1 Rh1 179.35(8) . 2_565 ? S3 Rh1 Rh1 91.86(3) 2_565 2_565 ? S1 Rh1 Rh1 91.74(3) 2_565 2_565 ? S2 Rh1 Rh1 91.95(3) . 2_565 ? S4 Rh1 Rh1 91.85(3) . 2_565 ? N1 Ni1 N2 82.77(17) . . ? N1 Ni1 S1 93.24(12) . . ? N2 Ni1 S1 175.52(12) . . ? N1 Ni1 S2 174.49(12) . . ? N2 Ni1 S2 92.46(12) . . ? S1 Ni1 S2 91.43(4) . . ? N4 Ni2 N3 83.12(16) . . ? N4 Ni2 S4 92.65(12) . . ? N3 Ni2 S4 175.38(12) . . ? N4 Ni2 S3 174.42(12) . . ? N3 Ni2 S3 92.42(11) . . ? S4 Ni2 S3 91.69(4) . . ? C1 S1 Ni1 94.65(17) . . ? C1 S1 Rh1 108.12(17) . 2_565 ? Ni1 S1 Rh1 114.14(5) . 2_565 ? C9 S2 Ni1 95.61(15) . . ? C9 S2 Rh1 108.65(16) . . ? Ni1 S2 Rh1 114.00(4) . . ? C10 S3 Ni2 96.16(14) . . ? C10 S3 Rh1 108.69(14) . 2_565 ? Ni2 S3 Rh1 115.58(4) . 2_565 ? C18 S4 Ni2 95.99(14) . . ? C18 S4 Rh1 110.13(14) . . ? Ni2 S4 Rh1 115.07(4) . . ? C2 N1 C3 113.1(4) . . ? C2 N1 C6 111.1(4) . . ? C3 N1 C6 107.5(4) . . ? C2 N1 Ni1 111.3(3) . . ? C3 N1 Ni1 106.8(3) . . ? C6 N1 Ni1 106.7(3) . . ? C5 N2 C7 112.7(4) . . ? C5 N2 C8 111.3(4) . . ? C7 N2 C8 106.4(4) . . ? C5 N2 Ni1 108.0(3) . . ? C7 N2 Ni1 108.1(3) . . ? C8 N2 Ni1 110.4(3) . . ? C12 N3 C11 113.0(4) . . ? C12 N3 C15 109.3(3) . . ? C11 N3 C15 108.4(4) . . ? C12 N3 Ni2 106.0(3) . . ? C11 N3 Ni2 112.1(3) . . ? C15 N3 Ni2 107.8(3) . . ? C14 N4 C17 112.5(4) . . ? C14 N4 C16 110.5(3) . . ? C17 N4 C16 108.6(4) . . ? C14 N4 Ni2 107.0(3) . . ? C17 N4 Ni2 111.2(3) . . ? C16 N4 Ni2 106.9(3) . . ? C19 N5 Rh1 176.7(3) . . ? C2 C1 S1 108.2(4) . . ? C1 C2 N1 110.6(4) . . ? N1 C3 C4 113.5(4) . . ? C5 C4 C3 118.1(4) . . ? N2 C5 C4 110.5(4) . . ? N1 C6 C7 108.6(4) . . ? N2 C7 C6 108.3(4) . . ? C9 C8 N2 109.3(4) . . ? C8 C9 S2 108.7(3) . . ? C11 C10 S3 108.2(3) . . ? C10 C11 N3 108.9(3) . . ? N3 C12 C13 112.9(4) . . ? C12 C13 C14 117.1(4) . . ? N4 C14 C13 112.4(4) . . ? N3 C15 C16 109.0(3) . . ? N4 C16 C15 108.9(3) . . ? C18 C17 N4 108.9(4) . . ? C17 C18 S4 107.5(3) . . ? N5 C19 C20 178.0(4) . . ? O2 C21 O1 129.0(5) . . ? O2 C21 C22A 113.8(4) . . ? O1 C21 C22A 117.1(5) . . ? F1A C22A F3A 103.6(13) . . ? F1A C22A F2A 107.9(12) . . ? F3A C22A F2A 104.5(13) . . ? F1A C22A C21 111.1(7) . . ? F3A C22A C21 118.2(17) . . ? F2A C22A C21 110.9(12) . . ? O4 C23 O3 130.6(4) . . ? O4 C23 C24A 113.8(4) . . ? O3 C23 C24A 115.4(4) . . ? F6A C24A F4A 107.9(13) . . ? F6A C24A F5A 99.0(13) . . ? F4A C24A F5A 103.0(12) . . ? F6A C24A C23 112.2(10) . . ? F4A C24A C23 114.2(10) . . ? F5A C24A C23 118.9(11) . . ? N6 C25 C26 179.5(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 S1 C1 11.0(2) . . . . ? N2 Ni1 S1 C1 38.0(17) . . . . ? S2 Ni1 S1 C1 -171.90(18) . . . . ? N1 Ni1 S1 Rh1 123.26(12) . . . 2_565 ? N2 Ni1 S1 Rh1 150.3(17) . . . 2_565 ? S2 Ni1 S1 Rh1 -59.67(5) . . . 2_565 ? N1 Ni1 S2 C9 -39.6(12) . . . . ? N2 Ni1 S2 C9 -9.73(19) . . . . ? S1 Ni1 S2 C9 172.51(15) . . . . ? N1 Ni1 S2 Rh1 -152.9(12) . . . . ? N2 Ni1 S2 Rh1 -123.02(13) . . . . ? S1 Ni1 S2 Rh1 59.22(5) . . . . ? N5 Rh1 S2 C9 38.79(17) . . . . ? S3 Rh1 S2 C9 -50.01(15) 2_565 . . . ? S1 Rh1 S2 C9 34.0(6) 2_565 . . . ? S4 Rh1 S2 C9 126.27(15) . . . . ? Rh1 Rh1 S2 C9 -141.86(15) 2_565 . . . ? N5 Rh1 S2 Ni1 144.05(9) . . . . ? S3 Rh1 S2 Ni1 55.25(5) 2_565 . . . ? S1 Rh1 S2 Ni1 139.3(5) 2_565 . . . ? S4 Rh1 S2 Ni1 -128.47(5) . . . . ? Rh1 Rh1 S2 Ni1 -36.60(4) 2_565 . . . ? N4 Ni2 S3 C10 47.4(13) . . . . ? N3 Ni2 S3 C10 10.68(19) . . . . ? S4 Ni2 S3 C10 -171.45(14) . . . . ? N4 Ni2 S3 Rh1 161.5(13) . . . 2_565 ? N3 Ni2 S3 Rh1 124.82(13) . . . 2_565 ? S4 Ni2 S3 Rh1 -57.30(5) . . . 2_565 ? N4 Ni2 S4 C18 -10.46(19) . . . . ? N3 Ni2 S4 C18 -34.3(15) . . . . ? S3 Ni2 S4 C18 173.03(15) . . . . ? N4 Ni2 S4 Rh1 -126.00(13) . . . . ? N3 Ni2 S4 Rh1 -149.8(15) . . . . ? S3 Ni2 S4 Rh1 57.49(5) . . . . ? N5 Rh1 S4 C18 36.46(17) . . . . ? S3 Rh1 S4 C18 43.6(5) 2_565 . . . ? S1 Rh1 S4 C18 124.79(15) 2_565 . . . ? S2 Rh1 S4 C18 -51.52(15) . . . . ? Rh1 Rh1 S4 C18 -143.49(15) 2_565 . . . ? N5 Rh1 S4 Ni2 143.57(10) . . . . ? S3 Rh1 S4 Ni2 150.7(5) 2_565 . . . ? S1 Rh1 S4 Ni2 -128.10(5) 2_565 . . . ? S2 Rh1 S4 Ni2 55.59(5) . . . . ? Rh1 Rh1 S4 Ni2 -36.38(5) 2_565 . . . ? N2 Ni1 N1 C2 -163.9(4) . . . . ? S1 Ni1 N1 C2 14.0(3) . . . . ? S2 Ni1 N1 C2 -133.8(11) . . . . ? N2 Ni1 N1 C3 72.2(3) . . . . ? S1 Ni1 N1 C3 -109.9(3) . . . . ? S2 Ni1 N1 C3 102.3(12) . . . . ? N2 Ni1 N1 C6 -42.5(3) . . . . ? S1 Ni1 N1 C6 135.4(3) . . . . ? S2 Ni1 N1 C6 -12.4(14) . . . . ? N1 Ni1 N2 C5 -76.7(3) . . . . ? S1 Ni1 N2 C5 -103.9(16) . . . . ? S2 Ni1 N2 C5 106.1(3) . . . . ? N1 Ni1 N2 C7 45.5(3) . . . . ? S1 Ni1 N2 C7 18.3(19) . . . . ? S2 Ni1 N2 C7 -131.7(3) . . . . ? N1 Ni1 N2 C8 161.4(3) . . . . ? S1 Ni1 N2 C8 134.2(15) . . . . ? S2 Ni1 N2 C8 -15.8(3) . . . . ? N4 Ni2 N3 C12 74.7(3) . . . . ? S4 Ni2 N3 C12 98.7(15) . . . . ? S3 Ni2 N3 C12 -108.6(3) . . . . ? N4 Ni2 N3 C11 -161.5(3) . . . . ? S4 Ni2 N3 C11 -137.5(14) . . . . ? S3 Ni2 N3 C11 15.1(3) . . . . ? N4 Ni2 N3 C15 -42.3(3) . . . . ? S4 Ni2 N3 C15 -18.3(17) . . . . ? S3 Ni2 N3 C15 134.4(3) . . . . ? N3 Ni2 N4 C14 -74.9(3) . . . . ? S4 Ni2 N4 C14 107.0(3) . . . . ? S3 Ni2 N4 C14 -111.9(12) . . . . ? N3 Ni2 N4 C17 161.9(3) . . . . ? S4 Ni2 N4 C17 -16.2(3) . . . . ? S3 Ni2 N4 C17 125.0(12) . . . . ? N3 Ni2 N4 C16 43.6(3) . . . . ? S4 Ni2 N4 C16 -134.6(3) . . . . ? S3 Ni2 N4 C16 6.6(15) . . . . ? S3 Rh1 N5 C19 -163(5) 2_565 . . . ? S1 Rh1 N5 C19 -73(5) 2_565 . . . ? S2 Rh1 N5 C19 107(5) . . . . ? S4 Rh1 N5 C19 16(5) . . . . ? Rh1 Rh1 N5 C19 21(12) 2_565 . . . ? Ni1 S1 C1 C2 -35.7(4) . . . . ? Rh1 S1 C1 C2 -153.0(3) 2_565 . . . ? S1 C1 C2 N1 52.3(5) . . . . ? C3 N1 C2 C1 77.7(5) . . . . ? C6 N1 C2 C1 -161.2(4) . . . . ? Ni1 N1 C2 C1 -42.5(5) . . . . ? C2 N1 C3 C4 171.0(4) . . . . ? C6 N1 C3 C4 47.9(5) . . . . ? Ni1 N1 C3 C4 -66.2(4) . . . . ? N1 C3 C4 C5 46.1(6) . . . . ? C7 N2 C5 C4 -49.0(5) . . . . ? C8 N2 C5 C4 -168.3(4) . . . . ? Ni1 N2 C5 C4 70.3(4) . . . . ? C3 C4 C5 N2 -47.2(6) . . . . ? C2 N1 C6 C7 152.8(4) . . . . ? C3 N1 C6 C7 -82.9(4) . . . . ? Ni1 N1 C6 C7 31.3(4) . . . . ? C5 N2 C7 C6 83.8(5) . . . . ? C8 N2 C7 C6 -154.0(4) . . . . ? Ni1 N2 C7 C6 -35.5(4) . . . . ? N1 C6 C7 N2 2.5(5) . . . . ? C5 N2 C8 C9 -75.4(5) . . . . ? C7 N2 C8 C9 161.6(4) . . . . ? Ni1 N2 C8 C9 44.6(5) . . . . ? N2 C8 C9 S2 -53.7(5) . . . . ? Ni1 S2 C9 C8 36.5(3) . . . . ? Rh1 S2 C9 C8 154.2(3) . . . . ? Ni2 S3 C10 C11 -35.9(3) . . . . ? Rh1 S3 C10 C11 -155.6(3) 2_565 . . . ? S3 C10 C11 N3 51.8(4) . . . . ? C12 N3 C11 C10 76.9(5) . . . . ? C15 N3 C11 C10 -161.7(4) . . . . ? Ni2 N3 C11 C10 -42.9(4) . . . . ? C11 N3 C12 C13 167.6(4) . . . . ? C15 N3 C12 C13 46.8(5) . . . . ? Ni2 N3 C12 C13 -69.1(4) . . . . ? N3 C12 C13 C14 47.4(6) . . . . ? C17 N4 C14 C13 -169.5(4) . . . . ? C16 N4 C14 C13 -47.9(5) . . . . ? Ni2 N4 C14 C13 68.1(4) . . . . ? C12 C13 C14 N4 -46.4(6) . . . . ? C12 N3 C15 C16 -84.3(4) . . . . ? C11 N3 C15 C16 152.1(4) . . . . ? Ni2 N3 C15 C16 30.6(4) . . . . ? C14 N4 C16 C15 81.5(4) . . . . ? C17 N4 C16 C15 -154.7(4) . . . . ? Ni2 N4 C16 C15 -34.6(4) . . . . ? N3 C15 C16 N4 2.7(5) . . . . ? C14 N4 C17 C18 -75.3(5) . . . . ? C16 N4 C17 C18 162.1(4) . . . . ? Ni2 N4 C17 C18 44.7(4) . . . . ? N4 C17 C18 S4 -53.5(4) . . . . ? Ni2 S4 C18 C17 36.4(3) . . . . ? Rh1 S4 C18 C17 155.9(3) . . . . ? Rh1 N5 C19 C20 41(16) . . . . ? O2 C21 C22A F1A 43.3(16) . . . . ? O1 C21 C22A F1A -139.8(16) . . . . ? O2 C21 C22A F3A 162.8(15) . . . . ? O1 C21 C22A F3A -20.3(16) . . . . ? O2 C21 C22A F2A -76.7(17) . . . . ? O1 C21 C22A F2A 100.2(17) . . . . ? O4 C23 C24A F6A -173.4(18) . . . . ? O3 C23 C24A F6A 10.8(19) . . . . ? O4 C23 C24A F4A -50.1(17) . . . . ? O3 C23 C24A F4A 134.0(16) . . . . ? O4 C23 C24A F5A 71.9(14) . . . . ? O3 C23 C24A F5A -103.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.051 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.118 # Attachment 'CCDC291356.cif' data_md257a _database_code_depnum_ccdc_archive 'CCDC 291356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H108 B6 F24 N12 Ni6 Rh2 S12' #'C27 H54 B3 F12 N6 Ni3 Rh S6' _chemical_formula_weight 1194.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 21.507(2) _cell_length_b 21.507(2) _cell_length_c 15.769(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6316.6(12) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 757 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 49.50 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 8.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4955 _exptl_absorpt_correction_T_max 0.9228 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MWPC area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7075 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_sigmaI/netI 0.1043 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 58.74 _reflns_number_total 1893 _reflns_number_gt 1459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0300P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 1893 _refine_ls_number_parameters 173 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.005 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 0.0000 0.0000 -0.00596(7) 0.0284(3) Uani 1 3 d S . . Ni1 Ni -0.10210(8) 0.06325(9) -0.02862(10) 0.0329(4) Uani 1 1 d . . . S1 S -0.07490(15) 0.02416(16) 0.08228(14) 0.0363(7) Uani 1 1 d . . . S2 S 0.00363(14) 0.09860(15) -0.07947(14) 0.0316(7) Uani 1 1 d . . . N1 N -0.2013(5) 0.0179(4) 0.0038(6) 0.042(2) Uani 1 1 d . . . N2 N -0.1369(5) 0.0800(4) -0.1338(5) 0.038(2) Uani 1 1 d . . . C1 C -0.1653(7) -0.0528(7) 0.0935(7) 0.055(3) Uani 1 1 d . . . H1A H -0.1756 -0.0884 0.0481 0.067 Uiso 1 1 calc R . . H1B H -0.1712 -0.0764 0.1492 0.067 Uiso 1 1 calc R . . C2 C -0.2143(6) -0.0215(6) 0.0864(7) 0.047(3) Uani 1 1 d . . . H2A H -0.2650 -0.0604 0.0896 0.056 Uiso 1 1 calc R . . H2B H -0.2051 0.0120 0.1341 0.056 Uiso 1 1 calc R . . C3 C -0.2263(8) 0.0697(7) 0.0131(9) 0.065(4) Uani 1 1 d . . . H3A H -0.1933 0.1089 0.0515 0.078 Uiso 1 1 calc R . . H3B H -0.2746 0.0456 0.0394 0.078 Uiso 1 1 calc R . . C4 C -0.2295(7) 0.1005(7) -0.0694(12) 0.084(5) Uani 1 1 d . . . H4A H -0.2686 0.0623 -0.1035 0.101 Uiso 1 1 calc R . . H4B H -0.2423 0.1382 -0.0592 0.101 Uiso 1 1 calc R . . C5 C -0.1631(6) 0.1318(6) -0.1194(8) 0.047(3) Uani 1 1 d . . . H5A H -0.1254 0.1746 -0.0896 0.056 Uiso 1 1 calc R . . H5B H -0.1716 0.1477 -0.1750 0.056 Uiso 1 1 calc R . . C6 C -0.2376(6) -0.0322(5) -0.0692(6) 0.039(3) Uani 1 1 d . . . H6A H -0.2888 -0.0456 -0.0713 0.047 Uiso 1 1 calc R . . H6B H -0.2351 -0.0766 -0.0615 0.047 Uiso 1 1 calc R . . C7 C -0.1990(7) 0.0062(5) -0.1550(7) 0.053(3) Uani 1 1 d . . . H7A H -0.1810 -0.0224 -0.1845 0.064 Uiso 1 1 calc R . . H7B H -0.2333 0.0105 -0.1929 0.064 Uiso 1 1 calc R . . C8 C -0.0785(6) 0.1096(6) -0.1994(6) 0.046(3) Uani 1 1 d . . . H8A H -0.1003 0.0977 -0.2567 0.056 Uiso 1 1 calc R . . H8B H -0.0505 0.1626 -0.1943 0.056 Uiso 1 1 calc R . . C9 C -0.0296(5) 0.0800(6) -0.1895(5) 0.038(3) Uani 1 1 d . . . H9A H 0.0110 0.1033 -0.2299 0.045 Uiso 1 1 calc R . . H9B H -0.0557 0.0276 -0.2004 0.045 Uiso 1 1 calc R . . B1A B 0.0816(13) 0.3046(15) -0.1962(16) 0.076(4) Uani 0.576(14) 1 d PD A -1 F1A F 0.1030(10) 0.2574(10) -0.2162(14) 0.076(4) Uani 0.576(14) 1 d PD A -1 F2A F 0.0506(7) 0.2856(7) -0.1116(9) 0.076(4) Uani 0.576(14) 1 d PD A -1 F3A F 0.0269(7) 0.2942(7) -0.2450(9) 0.076(4) Uani 0.576(14) 1 d PD A -1 F4A F 0.1344(7) 0.3758(7) -0.1919(9) 0.076(4) Uani 0.576(14) 1 d PD A -1 B1B B 0.0873(17) 0.3070(15) -0.2021(16) 0.073(5) Uani 0.424(14) 1 d PD A -2 F1B F 0.0902(14) 0.2476(12) -0.2238(16) 0.073(5) Uani 0.424(14) 1 d PD A -2 F2B F 0.0228(9) 0.2897(10) -0.1564(12) 0.073(5) Uani 0.424(14) 1 d PD A -2 F3B F 0.0911(11) 0.3445(10) -0.2710(10) 0.073(5) Uani 0.424(14) 1 d PD A -2 F4B F 0.1466(9) 0.3501(9) -0.1524(10) 0.073(5) Uani 0.424(14) 1 d PD A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0357(5) 0.0357(5) 0.0137(5) 0.000 0.000 0.0179(2) Ni1 0.0305(10) 0.0354(10) 0.0315(9) -0.0026(8) 0.0019(8) 0.0156(9) S1 0.0365(17) 0.0434(18) 0.0239(14) -0.0027(12) 0.0062(11) 0.0162(14) S2 0.0320(16) 0.0379(16) 0.0243(13) 0.0016(11) -0.0006(11) 0.0170(14) N1 0.049(6) 0.031(6) 0.048(6) -0.017(5) -0.008(4) 0.022(5) N2 0.031(5) 0.028(5) 0.049(6) -0.004(4) -0.003(4) 0.011(4) C1 0.051(8) 0.062(9) 0.045(8) 0.009(6) 0.012(6) 0.021(7) C2 0.022(6) 0.055(8) 0.040(7) -0.004(6) 0.013(5) 0.002(6) C3 0.067(9) 0.053(9) 0.083(11) -0.014(8) 0.002(7) 0.037(8) C4 0.049(10) 0.045(9) 0.166(16) -0.014(10) 0.021(10) 0.030(7) C5 0.049(8) 0.029(7) 0.069(8) -0.003(5) -0.014(6) 0.023(7) C6 0.034(7) 0.032(7) 0.052(7) -0.011(5) -0.010(5) 0.016(5) C7 0.061(9) 0.028(7) 0.060(9) 0.001(6) -0.007(7) 0.013(7) C8 0.049(8) 0.055(8) 0.039(7) 0.018(5) -0.008(5) 0.029(7) C9 0.037(7) 0.059(8) 0.024(6) 0.005(5) 0.002(4) 0.029(6) B1A 0.067(6) 0.078(5) 0.098(7) -0.040(4) -0.027(4) 0.048(4) F1A 0.067(6) 0.078(5) 0.098(7) -0.040(4) -0.027(4) 0.048(4) F2A 0.067(6) 0.078(5) 0.098(7) -0.040(4) -0.027(4) 0.048(4) F3A 0.067(6) 0.078(5) 0.098(7) -0.040(4) -0.027(4) 0.048(4) F4A 0.067(6) 0.078(5) 0.098(7) -0.040(4) -0.027(4) 0.048(4) B1B 0.111(10) 0.088(8) 0.057(7) 0.010(5) -0.001(5) 0.078(7) F1B 0.111(10) 0.088(8) 0.057(7) 0.010(5) -0.001(5) 0.078(7) F2B 0.111(10) 0.088(8) 0.057(7) 0.010(5) -0.001(5) 0.078(7) F3B 0.111(10) 0.088(8) 0.057(7) 0.010(5) -0.001(5) 0.078(7) F4B 0.111(10) 0.088(8) 0.057(7) 0.010(5) -0.001(5) 0.078(7) _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 S1 2.374(3) 3 ? Rh1 S1 2.374(3) 2 ? Rh1 S1 2.374(3) . ? Rh1 S2 2.383(3) 2 ? Rh1 S2 2.383(3) 3 ? Rh1 S2 2.383(3) . ? Ni1 N1 1.919(9) . ? Ni1 N2 1.927(9) . ? Ni1 S1 2.144(3) . ? Ni1 S2 2.159(3) . ? S1 C1 1.826(12) . ? S2 C9 1.842(9) . ? N1 C3 1.466(14) . ? N1 C6 1.502(12) . ? N1 C2 1.502(13) . ? N2 C5 1.495(13) . ? N2 C8 1.502(13) . ? N2 C7 1.515(13) . ? C1 C2 1.511(16) . ? C3 C4 1.48(2) . ? C4 C5 1.469(17) . ? C6 C7 1.588(15) . ? C8 C9 1.487(13) . ? B1A F3A 1.33(2) . ? B1A F1A 1.35(2) . ? B1A F4A 1.38(3) . ? B1A F2A 1.46(3) . ? B1B F3B 1.33(2) . ? B1B F1B 1.35(2) . ? B1B F4B 1.38(3) . ? B1B F2B 1.44(3) . ? 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 S1 Rh1 S1 89.14(10) 3 2 ? S1 Rh1 S1 89.14(10) 3 . ? S1 Rh1 S1 89.14(10) 2 . ? S1 Rh1 S2 168.07(9) 3 2 ? S1 Rh1 S2 79.30(9) 2 2 ? S1 Rh1 S2 93.57(9) . 2 ? S1 Rh1 S2 79.30(9) 3 3 ? S1 Rh1 S2 93.57(9) 2 3 ? S1 Rh1 S2 168.07(9) . 3 ? S2 Rh1 S2 98.35(8) 2 3 ? S1 Rh1 S2 93.57(9) 3 . ? S1 Rh1 S2 168.07(9) 2 . ? S1 Rh1 S2 79.30(9) . . ? S2 Rh1 S2 98.35(8) 2 . ? S2 Rh1 S2 98.35(8) 3 . ? N1 Ni1 N2 83.5(4) . . ? N1 Ni1 S1 92.0(3) . . ? N2 Ni1 S1 169.5(3) . . ? N1 Ni1 S2 170.1(3) . . ? N2 Ni1 S2 93.1(3) . . ? S1 Ni1 S2 89.72(11) . . ? C1 S1 Ni1 93.4(4) . . ? C1 S1 Rh1 113.0(4) . . ? Ni1 S1 Rh1 87.47(9) . . ? C9 S2 Ni1 92.7(3) . . ? C9 S2 Rh1 115.3(4) . . ? Ni1 S2 Rh1 86.90(10) . . ? C3 N1 C6 111.5(9) . . ? C3 N1 C2 107.8(9) . . ? C6 N1 C2 112.1(8) . . ? C3 N1 Ni1 112.2(8) . . ? C6 N1 Ni1 102.0(6) . . ? C2 N1 Ni1 111.3(7) . . ? C5 N2 C8 109.6(8) . . ? C5 N2 C7 110.6(9) . . ? C8 N2 C7 113.8(8) . . ? C5 N2 Ni1 109.6(7) . . ? C8 N2 Ni1 110.6(6) . . ? C7 N2 Ni1 102.4(6) . . ? C2 C1 S1 104.6(8) . . ? N1 C2 C1 110.0(8) . . ? N1 C3 C4 111.7(11) . . ? C5 C4 C3 115.1(13) . . ? C4 C5 N2 112.5(10) . . ? N1 C6 C7 109.3(8) . . ? N2 C7 C6 108.3(8) . . ? C9 C8 N2 111.5(8) . . ? C8 C9 S2 106.7(7) . . ? F3A B1A F1A 110.3(18) . . ? F3A B1A F4A 112(2) . . ? F1A B1A F4A 116.6(19) . . ? F3A B1A F2A 103.9(18) . . ? F1A B1A F2A 107(2) . . ? F4A B1A F2A 105.9(16) . . ? F3B B1B F1B 110(2) . . ? F3B B1B F4B 107(2) . . ? F1B B1B F4B 108(2) . . ? F3B B1B F2B 109(2) . . ? F1B B1B F2B 112(2) . . ? F4B B1B F2B 110(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 S1 C1 25.8(5) . . . . ? N2 Ni1 S1 C1 -38.8(16) . . . . ? S2 Ni1 S1 C1 -144.5(4) . . . . ? N1 Ni1 S1 Rh1 138.7(2) . . . . ? N2 Ni1 S1 Rh1 74.0(16) . . . . ? S2 Ni1 S1 Rh1 -31.59(10) . . . . ? S1 Rh1 S1 C1 -144.7(4) 3 . . . ? S1 Rh1 S1 C1 -55.6(5) 2 . . . ? S2 Rh1 S1 C1 23.6(4) 2 . . . ? S2 Rh1 S1 C1 -158.9(6) 3 . . . ? S2 Rh1 S1 C1 121.5(4) . . . . ? S1 Rh1 S1 Ni1 122.67(14) 3 . . . ? S1 Rh1 S1 Ni1 -148.18(14) 2 . . . ? S2 Rh1 S1 Ni1 -68.95(11) 2 . . . ? S2 Rh1 S1 Ni1 108.5(5) 3 . . . ? S2 Rh1 S1 Ni1 28.88(10) . . . . ? N1 Ni1 S2 C9 46.3(18) . . . . ? N2 Ni1 S2 C9 -23.1(4) . . . . ? S1 Ni1 S2 C9 146.7(4) . . . . ? N1 Ni1 S2 Rh1 -68.9(18) . . . . ? N2 Ni1 S2 Rh1 -138.4(3) . . . . ? S1 Ni1 S2 Rh1 31.47(10) . . . . ? S1 Rh1 S2 C9 151.3(4) 3 . . . ? S1 Rh1 S2 C9 -105.8(6) 2 . . . ? S1 Rh1 S2 C9 -120.2(4) . . . . ? S2 Rh1 S2 C9 -28.2(4) 2 . . . ? S2 Rh1 S2 C9 71.6(3) 3 . . . ? S1 Rh1 S2 Ni1 -117.12(10) 3 . . . ? S1 Rh1 S2 Ni1 -14.3(6) 2 . . . ? S1 Rh1 S2 Ni1 -28.68(10) . . . . ? S2 Rh1 S2 Ni1 63.40(13) 2 . . . ? S2 Rh1 S2 Ni1 163.19(8) 3 . . . ? N2 Ni1 N1 C3 -68.5(8) . . . . ? S1 Ni1 N1 C3 121.1(8) . . . . ? S2 Ni1 N1 C3 -138.7(16) . . . . ? N2 Ni1 N1 C6 50.9(6) . . . . ? S1 Ni1 N1 C6 -119.5(6) . . . . ? S2 Ni1 N1 C6 -19(2) . . . . ? N2 Ni1 N1 C2 170.6(7) . . . . ? S1 Ni1 N1 C2 0.2(6) . . . . ? S2 Ni1 N1 C2 100.4(18) . . . . ? N1 Ni1 N2 C5 67.4(7) . . . . ? S1 Ni1 N2 C5 132.7(14) . . . . ? S2 Ni1 N2 C5 -121.9(7) . . . . ? N1 Ni1 N2 C8 -171.8(7) . . . . ? S1 Ni1 N2 C8 -106.4(15) . . . . ? S2 Ni1 N2 C8 -1.1(7) . . . . ? N1 Ni1 N2 C7 -50.2(7) . . . . ? S1 Ni1 N2 C7 15(2) . . . . ? S2 Ni1 N2 C7 120.5(7) . . . . ? Ni1 S1 C1 C2 -48.7(8) . . . . ? Rh1 S1 C1 C2 -137.4(7) . . . . ? C3 N1 C2 C1 -157.8(10) . . . . ? C6 N1 C2 C1 79.1(11) . . . . ? Ni1 N1 C2 C1 -34.4(11) . . . . ? S1 C1 C2 N1 57.1(10) . . . . ? C6 N1 C3 C4 -44.9(14) . . . . ? C2 N1 C3 C4 -168.4(10) . . . . ? Ni1 N1 C3 C4 68.8(12) . . . . ? N1 C3 C4 C5 -53.1(16) . . . . ? C3 C4 C5 N2 54.8(15) . . . . ? C8 N2 C5 C4 168.4(11) . . . . ? C7 N2 C5 C4 42.1(14) . . . . ? Ni1 N2 C5 C4 -70.1(12) . . . . ? C3 N1 C6 C7 81.1(12) . . . . ? C2 N1 C6 C7 -157.9(9) . . . . ? Ni1 N1 C6 C7 -38.8(9) . . . . ? C5 N2 C7 C6 -80.5(11) . . . . ? C8 N2 C7 C6 155.6(9) . . . . ? Ni1 N2 C7 C6 36.2(10) . . . . ? N1 C6 C7 N2 1.6(12) . . . . ? C5 N2 C8 C9 154.6(9) . . . . ? C7 N2 C8 C9 -81.0(11) . . . . ? Ni1 N2 C8 C9 33.7(11) . . . . ? N2 C8 C9 S2 -55.0(10) . . . . ? Ni1 S2 C9 C8 45.5(7) . . . . ? Rh1 S2 C9 C8 133.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 58.74 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.667 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.098