Electronic Supplementary Material 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 'Guo-Xin Jin' _publ_contact_author_address ; Department of Chemistry Fudan University Key Lab of Molecular Catalysis and Handan Road 220 Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis and Structure of Heterometallic Complexes (RhFe, CoFe) Containing Bridging 1,2-Dicarba-closo-dodecarborane-1,2-dichalcogenolato Ligand ; loop_ _publ_author_name 'Guo-Xin Jin' 'Shuyi Cai' 'Yin-Qiang Chen' 'Xiu-Feng Hou' # Attachment '5a.cif' data_f51110a _database_code_depnum_ccdc_archive 'CCDC 608150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 B10 Fe O3 Rh S2' _chemical_formula_weight 584.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.980(5) _cell_length_b 14.000(4) _cell_length_c 19.502(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4909(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 959 _cell_measurement_theta_min 2.376 _cell_measurement_theta_max 21.427 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.9310 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 3.80 _diffrn_reflns_number 19592 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4338 _reflns_number_gt 2349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4338 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 0.805 _refine_ls_restrained_S_all 0.805 _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 0.099352(17) 0.75184(3) 0.153745(14) 0.03621(9) Uani 1 1 d . . . Fe1 Fe 0.00300(3) 0.75526(5) 0.06034(3) 0.04235(16) Uani 1 1 d . . . O1 O -0.07636(17) 0.7353(3) -0.07117(15) 0.0831(12) Uani 1 1 d . . . O2 O -0.0259(2) 0.9588(2) 0.07957(19) 0.0881(13) Uani 1 1 d . . . O3 O -0.11768(19) 0.7021(2) 0.15213(17) 0.0780(11) Uani 1 1 d . . . S1 S 0.05988(6) 0.61435(7) 0.09468(5) 0.0411(3) Uani 1 1 d . . . S2 S 0.12438(6) 0.79755(7) 0.03977(5) 0.0373(3) Uani 1 1 d . . . C1 C 0.1332(2) 0.5938(3) 0.03283(18) 0.0356(10) Uani 1 1 d . . . C2 C 0.1678(2) 0.6921(3) 0.00207(19) 0.0355(10) Uani 1 1 d . . . C3 C -0.0439(2) 0.7406(4) -0.0214(2) 0.0559(12) Uani 1 1 d . . . C4 C -0.0154(3) 0.8792(4) 0.0709(2) 0.0617(15) Uani 1 1 d . . . C5 C -0.0713(3) 0.7235(3) 0.1154(2) 0.0536(14) Uani 1 1 d . . . C6 C 0.1295(3) 0.8688(3) 0.21995(19) 0.0423(12) Uani 1 1 d . . . C7 C 0.1874(3) 0.7994(3) 0.2242(2) 0.0449(12) Uani 1 1 d . . . C8 C 0.1559(3) 0.7147(3) 0.2497(2) 0.0463(13) Uani 1 1 d . . . C9 C 0.0781(3) 0.7314(3) 0.26234(19) 0.0424(12) Uani 1 1 d . . . C10 C 0.0625(3) 0.8288(3) 0.2463(2) 0.0434(12) Uani 1 1 d . . . C11 C 0.1386(3) 0.9713(3) 0.1971(2) 0.0633(15) Uani 1 1 d . . . H11A H 0.1518 1.0102 0.2358 0.095 Uiso 1 1 calc R . . H11B H 0.0926 0.9938 0.1779 0.095 Uiso 1 1 calc R . . H11C H 0.1771 0.9751 0.1631 0.095 Uiso 1 1 calc R . . C12 C 0.2681(3) 0.8161(4) 0.2100(2) 0.0731(16) Uani 1 1 d . . . H12A H 0.2923 0.8372 0.2512 0.110 Uiso 1 1 calc R . . H12B H 0.2732 0.8641 0.1752 0.110 Uiso 1 1 calc R . . H12C H 0.2906 0.7577 0.1946 0.110 Uiso 1 1 calc R . . C13 C 0.1959(3) 0.6231(3) 0.2654(2) 0.0753(17) Uani 1 1 d . . . H13A H 0.2151 0.6253 0.3113 0.113 Uiso 1 1 calc R . . H13B H 0.2362 0.6148 0.2336 0.113 Uiso 1 1 calc R . . H13C H 0.1619 0.5705 0.2612 0.113 Uiso 1 1 calc R . . C14 C 0.0253(3) 0.6613(3) 0.2943(2) 0.0734(17) Uani 1 1 d . . . H14A H 0.0269 0.6676 0.3433 0.110 Uiso 1 1 calc R . . H14B H 0.0394 0.5976 0.2817 0.110 Uiso 1 1 calc R . . H14C H -0.0243 0.6738 0.2784 0.110 Uiso 1 1 calc R . . C15 C -0.0089(3) 0.8805(3) 0.2592(2) 0.0652(15) Uani 1 1 d . . . H15A H -0.0083 0.9070 0.3046 0.098 Uiso 1 1 calc R . . H15B H -0.0497 0.8367 0.2551 0.098 Uiso 1 1 calc R . . H15C H -0.0145 0.9309 0.2263 0.098 Uiso 1 1 calc R . . B3 B 0.2215(3) 0.6272(3) 0.0590(2) 0.0396(13) Uani 1 1 d . . . H3 H 0.2363 0.6497 0.1113 0.048 Uiso 1 1 calc R . . B4 B 0.2603(3) 0.6826(4) -0.0137(2) 0.0437(14) Uani 1 1 d . . . H4 H 0.3001 0.7419 -0.0091 0.052 Uiso 1 1 calc R . . B5 B 0.1944(3) 0.6794(4) -0.0806(2) 0.0476(14) Uani 1 1 d . . . H5 H 0.1919 0.7369 -0.1190 0.057 Uiso 1 1 calc R . . B6 B 0.1133(3) 0.6232(3) -0.0516(2) 0.0433(14) Uani 1 1 d . . . H6 H 0.0581 0.6430 -0.0713 0.052 Uiso 1 1 calc R . . B7 B 0.2001(3) 0.5077(3) 0.0400(2) 0.0458(14) Uani 1 1 d . . . H7 H 0.2003 0.4522 0.0799 0.055 Uiso 1 1 calc R . . B8 B 0.2834(3) 0.5620(4) 0.0087(2) 0.0481(14) Uani 1 1 d . . . H8 H 0.3389 0.5416 0.0275 0.058 Uiso 1 1 calc R . . B9 B 0.2671(3) 0.5937(4) -0.0784(2) 0.0520(16) Uani 1 1 d . . . H9 H 0.3124 0.5938 -0.1163 0.062 Uiso 1 1 calc R . . B10 B 0.1764(3) 0.5584(3) -0.1005(3) 0.0509(15) Uani 1 1 d . . . H10 H 0.1628 0.5353 -0.1529 0.061 Uiso 1 1 calc R . . B11 B 0.1345(3) 0.5052(3) -0.0274(2) 0.0464(14) Uani 1 1 d . . . H11 H 0.0928 0.4480 -0.0309 0.056 Uiso 1 1 calc R . . B12 B 0.2300(3) 0.4862(4) -0.0449(2) 0.0505(16) Uani 1 1 d . . . H12 H 0.2511 0.4159 -0.0609 0.061 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 0.04108(18) 0.03657(17) 0.03097(16) -0.0020(2) -0.00074(15) -0.0024(2) Fe1 0.0377(4) 0.0457(4) 0.0437(4) -0.0007(4) -0.0039(3) -0.0013(4) O1 0.055(2) 0.146(4) 0.049(2) -0.002(3) -0.0139(16) 0.005(3) O2 0.080(3) 0.057(2) 0.127(3) -0.006(2) -0.007(2) 0.014(2) O3 0.060(3) 0.092(3) 0.082(3) 0.005(2) 0.025(2) -0.003(2) S1 0.0445(7) 0.0387(6) 0.0402(6) 0.0004(6) 0.0017(6) -0.0078(6) S2 0.0417(7) 0.0324(6) 0.0378(6) 0.0008(5) -0.0020(5) -0.0027(5) C1 0.043(3) 0.034(2) 0.029(2) 0.0017(19) -0.006(2) -0.007(2) C2 0.046(3) 0.030(2) 0.030(2) 0.000(2) -0.002(2) 0.001(2) C3 0.039(3) 0.072(3) 0.057(3) 0.005(3) 0.006(2) -0.006(3) C4 0.052(4) 0.067(4) 0.066(4) 0.003(3) -0.005(3) 0.003(3) C5 0.055(3) 0.048(3) 0.058(3) -0.002(2) -0.005(3) 0.003(2) C6 0.059(3) 0.041(3) 0.027(3) -0.006(2) -0.004(2) -0.011(3) C7 0.048(3) 0.058(3) 0.028(3) -0.011(2) -0.007(2) -0.001(3) C8 0.068(4) 0.047(3) 0.024(3) -0.004(2) -0.008(2) 0.010(3) C9 0.065(3) 0.036(3) 0.026(2) -0.0044(19) 0.003(2) -0.007(2) C10 0.061(3) 0.041(3) 0.028(3) -0.007(2) 0.001(2) 0.000(3) C11 0.090(4) 0.052(3) 0.048(3) 0.002(2) -0.002(3) -0.022(3) C12 0.054(4) 0.110(4) 0.055(3) -0.011(3) -0.008(3) -0.010(3) C13 0.112(5) 0.068(4) 0.046(3) -0.007(3) -0.010(3) 0.039(4) C14 0.106(5) 0.047(3) 0.067(4) 0.003(3) 0.024(3) -0.012(3) C15 0.077(4) 0.056(3) 0.063(3) -0.009(3) 0.012(3) 0.007(3) B3 0.039(3) 0.042(3) 0.039(3) 0.007(2) -0.009(2) 0.003(3) B4 0.044(3) 0.050(3) 0.038(3) -0.002(3) 0.004(3) -0.002(3) B5 0.064(4) 0.052(3) 0.027(3) 0.001(2) 0.001(3) 0.004(3) B6 0.059(4) 0.042(3) 0.029(3) -0.003(2) -0.013(3) -0.003(3) B7 0.059(4) 0.037(3) 0.041(3) 0.002(3) -0.007(3) 0.010(3) B8 0.047(4) 0.055(4) 0.042(3) 0.001(3) -0.001(3) 0.013(3) B9 0.061(4) 0.051(4) 0.044(4) 0.001(3) 0.009(3) 0.009(3) B10 0.074(4) 0.046(3) 0.033(3) -0.007(3) -0.004(3) 0.006(3) B11 0.067(4) 0.033(3) 0.038(3) -0.008(2) -0.009(3) -0.004(3) B12 0.063(5) 0.045(4) 0.043(3) -0.007(3) -0.002(3) 0.009(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 C6 2.155(4) . ? Rh1 C9 2.171(4) . ? Rh1 C8 2.193(4) . ? Rh1 C7 2.200(4) . ? Rh1 C10 2.205(4) . ? Rh1 S1 2.3529(12) . ? Rh1 S2 2.3564(12) . ? Rh1 Fe1 2.5143(8) . ? Fe1 C5 1.770(5) . ? Fe1 C4 1.778(5) . ? Fe1 C3 1.816(5) . ? Fe1 S2 2.2967(14) . ? Fe1 S1 2.3207(13) . ? O1 C3 1.134(5) . ? O2 C4 1.143(5) . ? O3 C5 1.140(5) . ? S1 C1 1.810(4) . ? S2 C2 1.825(4) . ? C1 C2 1.624(5) . ? C1 B11 1.708(6) . ? C1 B7 1.709(6) . ? C1 B3 1.731(6) . ? C1 B6 1.735(5) . ? C2 B5 1.691(6) . ? C2 B4 1.697(6) . ? C2 B6 1.728(6) . ? C2 B3 1.729(6) . ? C6 C10 1.424(6) . ? C6 C7 1.427(6) . ? C6 C11 1.512(5) . ? C7 C8 1.406(5) . ? C7 C12 1.495(6) . ? C8 C9 1.439(6) . ? C8 C13 1.501(5) . ? C9 C10 1.427(5) . ? C9 C14 1.502(5) . ? C10 C15 1.494(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? B3 B8 1.742(7) . ? B3 B7 1.755(6) . ? B3 B4 1.760(6) . ? B3 H3 1.1000 . ? B4 B5 1.763(7) . ? B4 B9 1.777(6) . ? B4 B8 1.793(7) . ? B4 H4 1.1000 . ? B5 B6 1.751(7) . ? B5 B10 1.768(7) . ? B5 B9 1.775(7) . ? B5 H5 1.1000 . ? B6 B10 1.737(7) . ? B6 B11 1.760(6) . ? B6 H6 1.1000 . ? B7 B11 1.766(7) . ? B7 B12 1.767(7) . ? B7 B8 1.787(7) . ? B7 H7 1.1000 . ? B8 B12 1.773(7) . ? B8 B9 1.781(7) . ? B8 H8 1.1000 . ? B9 B10 1.758(7) . ? B9 B12 1.770(7) . ? B9 H9 1.1000 . ? B10 B12 1.768(7) . ? B10 B11 1.776(7) . ? B10 H10 1.1000 . ? B11 B12 1.771(7) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? 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 C6 Rh1 C9 63.89(15) . . ? C6 Rh1 C8 63.40(15) . . ? C9 Rh1 C8 38.51(15) . . ? C6 Rh1 C7 38.24(15) . . ? C9 Rh1 C7 63.72(16) . . ? C8 Rh1 C7 37.34(14) . . ? C6 Rh1 C10 38.12(15) . . ? C9 Rh1 C10 38.07(14) . . ? C8 Rh1 C10 63.67(15) . . ? C7 Rh1 C10 63.70(17) . . ? C6 Rh1 S1 172.33(11) . . ? C9 Rh1 S1 108.46(11) . . ? C8 Rh1 S1 111.31(12) . . ? C7 Rh1 S1 140.40(13) . . ? C10 Rh1 S1 135.26(12) . . ? C6 Rh1 S2 108.11(11) . . ? C9 Rh1 S2 171.73(11) . . ? C8 Rh1 S2 141.37(14) . . ? C7 Rh1 S2 111.69(12) . . ? C10 Rh1 S2 134.19(12) . . ? S1 Rh1 S2 79.51(4) . . ? C6 Rh1 Fe1 126.38(12) . . ? C9 Rh1 Fe1 126.01(12) . . ? C8 Rh1 Fe1 160.45(14) . . ? C7 Rh1 Fe1 160.53(13) . . ? C10 Rh1 Fe1 112.14(13) . . ? S1 Rh1 Fe1 56.84(3) . . ? S2 Rh1 Fe1 56.16(3) . . ? C5 Fe1 C4 92.0(2) . . ? C5 Fe1 C3 98.83(19) . . ? C4 Fe1 C3 97.2(2) . . ? C5 Fe1 S2 152.59(15) . . ? C4 Fe1 S2 86.90(16) . . ? C3 Fe1 S2 108.49(13) . . ? C5 Fe1 S1 86.80(14) . . ? C4 Fe1 S1 151.42(16) . . ? C3 Fe1 S1 111.21(17) . . ? S2 Fe1 S1 81.42(4) . . ? C5 Fe1 Rh1 94.36(15) . . ? C4 Fe1 Rh1 93.63(16) . . ? C3 Fe1 Rh1 162.59(14) . . ? S2 Fe1 Rh1 58.45(3) . . ? S1 Fe1 Rh1 58.07(3) . . ? C1 S1 Fe1 105.29(13) . . ? C1 S1 Rh1 103.67(13) . . ? Fe1 S1 Rh1 65.09(4) . . ? C2 S2 Fe1 105.57(14) . . ? C2 S2 Rh1 104.00(13) . . ? Fe1 S2 Rh1 65.40(3) . . ? C2 C1 B11 110.8(3) . . ? C2 C1 B7 111.0(3) . . ? B11 C1 B7 62.2(3) . . ? C2 C1 B3 61.9(2) . . ? B11 C1 B3 112.7(3) . . ? B7 C1 B3 61.4(3) . . ? C2 C1 B6 61.8(2) . . ? B11 C1 B6 61.5(2) . . ? B7 C1 B6 113.0(3) . . ? B3 C1 B6 113.9(3) . . ? C2 C1 S1 113.0(3) . . ? B11 C1 S1 125.7(3) . . ? B7 C1 S1 124.7(3) . . ? B3 C1 S1 115.4(3) . . ? B6 C1 S1 116.4(3) . . ? C1 C2 B5 111.8(3) . . ? C1 C2 B4 112.1(3) . . ? B5 C2 B4 62.7(3) . . ? C1 C2 B6 62.3(2) . . ? B5 C2 B6 61.6(3) . . ? B4 C2 B6 113.7(3) . . ? C1 C2 B3 62.1(2) . . ? B5 C2 B3 113.5(3) . . ? B4 C2 B3 61.8(3) . . ? B6 C2 B3 114.4(3) . . ? C1 C2 S2 111.9(3) . . ? B5 C2 S2 126.1(3) . . ? B4 C2 S2 123.8(3) . . ? B6 C2 S2 116.9(3) . . ? B3 C2 S2 113.9(3) . . ? O1 C3 Fe1 175.8(5) . . ? O2 C4 Fe1 177.7(5) . . ? O3 C5 Fe1 178.0(4) . . ? C10 C6 C7 109.2(4) . . ? C10 C6 C11 124.8(4) . . ? C7 C6 C11 125.8(5) . . ? C10 C6 Rh1 72.8(2) . . ? C7 C6 Rh1 72.6(2) . . ? C11 C6 Rh1 124.9(3) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 C12 126.1(5) . . ? C6 C7 C12 126.2(5) . . ? C8 C7 Rh1 71.1(3) . . ? C6 C7 Rh1 69.2(2) . . ? C12 C7 Rh1 129.1(3) . . ? C7 C8 C9 108.4(4) . . ? C7 C8 C13 126.8(5) . . ? C9 C8 C13 124.8(4) . . ? C7 C8 Rh1 71.6(3) . . ? C9 C8 Rh1 69.9(2) . . ? C13 C8 Rh1 126.7(3) . . ? C10 C9 C8 108.0(4) . . ? C10 C9 C14 126.3(4) . . ? C8 C9 C14 125.4(4) . . ? C10 C9 Rh1 72.2(2) . . ? C8 C9 Rh1 71.6(2) . . ? C14 C9 Rh1 127.1(3) . . ? C6 C10 C9 106.8(4) . . ? C6 C10 C15 126.7(4) . . ? C9 C10 C15 126.5(4) . . ? C6 C10 Rh1 69.0(2) . . ? C9 C10 Rh1 69.7(2) . . ? C15 C10 Rh1 129.2(3) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C2 B3 C1 56.0(2) . . ? C2 B3 B8 105.7(3) . . ? C1 B3 B8 106.2(3) . . ? C2 B3 B7 104.1(3) . . ? C1 B3 B7 58.7(3) . . ? B8 B3 B7 61.5(3) . . ? C2 B3 B4 58.2(2) . . ? C1 B3 B4 104.2(3) . . ? B8 B3 B4 61.6(3) . . ? B7 B3 B4 109.7(4) . . ? C2 B3 H3 125.4 . . ? C1 B3 H3 124.9 . . ? B8 B3 H3 121.1 . . ? B7 B3 H3 121.5 . . ? B4 B3 H3 121.6 . . ? C2 B4 B3 60.0(3) . . ? C2 B4 B5 58.5(3) . . ? B3 B4 B5 108.6(4) . . ? C2 B4 B9 104.5(4) . . ? B3 B4 B9 106.9(4) . . ? B5 B4 B9 60.2(3) . . ? C2 B4 B8 104.9(3) . . ? B3 B4 B8 58.7(3) . . ? B5 B4 B8 108.2(4) . . ? B9 B4 B8 59.9(3) . . ? C2 B4 H4 124.3 . . ? B3 B4 H4 121.7 . . ? B5 B4 H4 121.1 . . ? B9 B4 H4 122.8 . . ? B8 B4 H4 122.7 . . ? C2 B5 B6 60.3(3) . . ? C2 B5 B4 58.8(3) . . ? B6 B5 B4 109.4(3) . . ? C2 B5 B10 104.9(4) . . ? B6 B5 B10 59.1(3) . . ? B4 B5 B10 108.0(4) . . ? C2 B5 B9 104.8(3) . . ? B6 B5 B9 107.6(4) . . ? B4 B5 B9 60.3(3) . . ? B10 B5 B9 59.5(3) . . ? C2 B5 H5 124.1 . . ? B6 B5 H5 121.0 . . ? B4 B5 H5 120.9 . . ? B10 B5 H5 122.9 . . ? B9 B5 H5 122.7 . . ? C2 B6 C1 55.9(2) . . ? C2 B6 B10 104.7(4) . . ? C1 B6 B10 105.2(3) . . ? C2 B6 B5 58.2(3) . . ? C1 B6 B5 103.9(3) . . ? B10 B6 B5 60.9(3) . . ? C2 B6 B11 103.7(3) . . ? C1 B6 B11 58.5(2) . . ? B10 B6 B11 61.0(3) . . ? B5 B6 B11 109.1(4) . . ? C2 B6 H6 125.6 . . ? C1 B6 H6 125.2 . . ? B10 B6 H6 122.0 . . ? B5 B6 H6 121.8 . . ? B11 B6 H6 121.7 . . ? C1 B7 B3 59.9(2) . . ? C1 B7 B11 58.9(3) . . ? B3 B7 B11 108.8(3) . . ? C1 B7 B12 104.9(3) . . ? B3 B7 B12 107.0(4) . . ? B11 B7 B12 60.1(3) . . ? C1 B7 B8 105.2(3) . . ? B3 B7 B8 58.9(3) . . ? B11 B7 B8 108.3(3) . . ? B12 B7 B8 59.8(3) . . ? C1 B7 H7 124.0 . . ? B3 B7 H7 121.6 . . ? B11 B7 H7 121.0 . . ? B12 B7 H7 122.8 . . ? B8 B7 H7 122.6 . . ? B3 B8 B12 107.4(4) . . ? B3 B8 B9 107.5(4) . . ? B12 B8 B9 59.7(3) . . ? B3 B8 B7 59.6(3) . . ? B12 B8 B7 59.5(3) . . ? B9 B8 B7 107.1(4) . . ? B3 B8 B4 59.7(3) . . ? B12 B8 B4 107.1(4) . . ? B9 B8 B4 59.6(3) . . ? B7 B8 B4 106.8(4) . . ? B3 B8 H8 121.9 . . ? B12 B8 H8 122.2 . . ? B9 B8 H8 122.1 . . ? B7 B8 H8 122.4 . . ? B4 B8 H8 122.4 . . ? B10 B9 B12 60.1(3) . . ? B10 B9 B5 60.1(3) . . ? B12 B9 B5 107.8(4) . . ? B10 B9 B4 107.9(4) . . ? B12 B9 B4 107.9(4) . . ? B5 B9 B4 59.5(3) . . ? B10 B9 B8 108.5(4) . . ? B12 B9 B8 59.9(3) . . ? B5 B9 B8 108.2(3) . . ? B4 B9 B8 60.5(3) . . ? B10 B9 H9 121.5 . . ? B12 B9 H9 121.9 . . ? B5 B9 H9 121.9 . . ? B4 B9 H9 121.8 . . ? B8 B9 H9 121.3 . . ? B6 B10 B9 109.0(4) . . ? B6 B10 B12 108.6(4) . . ? B9 B10 B12 60.3(3) . . ? B6 B10 B5 59.9(3) . . ? B9 B10 B5 60.5(3) . . ? B12 B10 B5 108.3(4) . . ? B6 B10 B11 60.1(3) . . ? B9 B10 B11 108.3(4) . . ? B12 B10 B11 60.0(3) . . ? B5 B10 B11 107.7(3) . . ? B6 B10 H10 121.2 . . ? B9 B10 H10 121.1 . . ? B12 B10 H10 121.5 . . ? B5 B10 H10 121.8 . . ? B11 B10 H10 121.9 . . ? C1 B11 B6 60.0(2) . . ? C1 B11 B7 58.9(2) . . ? B6 B11 B7 109.0(3) . . ? C1 B11 B12 104.8(4) . . ? B6 B11 B12 107.4(4) . . ? B7 B11 B12 60.0(3) . . ? C1 B11 B10 104.6(3) . . ? B6 B11 B10 58.8(3) . . ? B7 B11 B10 107.8(4) . . ? B12 B11 B10 59.8(3) . . ? C1 B11 H11 124.2 . . ? B6 B11 H11 121.3 . . ? B7 B11 H11 121.1 . . ? B12 B11 H11 122.7 . . ? B10 B11 H11 123.0 . . ? B7 B12 B10 108.1(4) . . ? B7 B12 B9 108.4(4) . . ? B10 B12 B9 59.6(3) . . ? B7 B12 B11 59.9(3) . . ? B10 B12 B11 60.3(3) . . ? B9 B12 B11 108.0(4) . . ? B7 B12 B8 60.6(3) . . ? B10 B12 B8 108.4(4) . . ? B9 B12 B8 60.4(3) . . ? B11 B12 B8 108.8(4) . . ? B7 B12 H12 121.5 . . ? B10 B12 H12 121.8 . . ? B9 B12 H12 121.8 . . ? B11 B12 H12 121.5 . . ? B8 B12 H12 121.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.527 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.064 # Attachment '5b.cif' data_f51102d _database_code_depnum_ccdc_archive 'CCDC 608151' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 B10 Fe O3 Rh Se2' _chemical_formula_weight 678.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.114(5) _cell_length_b 13.980(4) _cell_length_c 19.704(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4990(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 614 _cell_measurement_theta_min 2.679 _cell_measurement_theta_max 19.264 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 4.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5731 _exptl_absorpt_correction_T_max 0.8183 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 4.92 _diffrn_reflns_number 18611 _diffrn_reflns_av_R_equivalents 0.1152 _diffrn_reflns_av_sigmaI/netI 0.1992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4913 _reflns_number_gt 1906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4913 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 0.588 _refine_ls_restrained_S_all 0.588 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.40015(2) 0.24559(4) 0.15522(3) 0.03928(14) Uani 1 1 d . . . Se1 Se 0.37418(3) 0.19517(5) 0.03889(3) 0.03949(18) Uani 1 1 d . . . Se2 Se 0.44025(3) 0.39063(5) 0.09707(4) 0.04427(19) Uani 1 1 d . . . Fe1 Fe 0.49846(5) 0.24302(8) 0.06261(4) 0.0458(3) Uani 1 1 d . . . O1 O 0.6168(2) 0.2962(4) 0.1539(3) 0.0765(17) Uani 1 1 d . . . O2 O 0.5275(2) 0.0406(4) 0.0818(3) 0.0878(19) Uani 1 1 d . . . O3 O 0.5747(2) 0.2658(4) -0.0679(2) 0.0843(19) Uani 1 1 d . . . C3 C 0.5701(4) 0.2750(5) 0.1163(4) 0.061(2) Uani 1 1 d . . . C4 C 0.5168(3) 0.1231(5) 0.0732(4) 0.056(2) Uani 1 1 d . . . C5 C 0.5433(3) 0.2603(6) -0.0182(4) 0.062(2) Uani 1 1 d . . . C6 C 0.3715(4) 0.1272(5) 0.2192(3) 0.0422(18) Uani 1 1 d . . . C7 C 0.4366(4) 0.1692(5) 0.2468(3) 0.048(2) Uani 1 1 d . . . C8 C 0.4200(4) 0.2646(5) 0.2635(3) 0.0448(19) Uani 1 1 d . . . C9 C 0.3424(4) 0.2807(5) 0.2488(3) 0.051(2) Uani 1 1 d . . . C10 C 0.3129(4) 0.1954(6) 0.2230(3) 0.046(2) Uani 1 1 d . . . C11 C 0.3635(3) 0.0266(4) 0.1974(3) 0.063(2) Uani 1 1 d . . . H9A H 0.3610 -0.0140 0.2367 0.094 Uiso 1 1 calc R . . H9B H 0.4052 0.0086 0.1702 0.094 Uiso 1 1 calc R . . H9C H 0.3190 0.0197 0.1713 0.094 Uiso 1 1 calc R . . C12 C 0.5077(3) 0.1188(5) 0.2610(3) 0.068(2) Uani 1 1 d . . . H10A H 0.5477 0.1638 0.2591 0.102 Uiso 1 1 calc R . . H10B H 0.5153 0.0696 0.2278 0.102 Uiso 1 1 calc R . . H10C H 0.5057 0.0906 0.3054 0.102 Uiso 1 1 calc R . . C13 C 0.4718(3) 0.3355(4) 0.2968(3) 0.072(2) Uani 1 1 d . . . H11A H 0.4705 0.3271 0.3451 0.108 Uiso 1 1 calc R . . H11B H 0.4567 0.3994 0.2857 0.108 Uiso 1 1 calc R . . H11C H 0.5212 0.3249 0.2807 0.108 Uiso 1 1 calc R . . C14 C 0.3024(4) 0.3731(5) 0.2641(3) 0.081(3) Uani 1 1 d . . . H12A H 0.2570 0.3751 0.2390 0.121 Uiso 1 1 calc R . . H12B H 0.3329 0.4262 0.2512 0.121 Uiso 1 1 calc R . . H12C H 0.2919 0.3765 0.3118 0.121 Uiso 1 1 calc R . . C15 C 0.2323(3) 0.1800(5) 0.2090(3) 0.078(3) Uani 1 1 d . . . H13A H 0.2087 0.1554 0.2490 0.117 Uiso 1 1 calc R . . H13B H 0.2268 0.1350 0.1726 0.117 Uiso 1 1 calc R . . H13C H 0.2100 0.2397 0.1966 0.117 Uiso 1 1 calc R . . C1 C 0.3301(3) 0.3107(4) -0.0001(3) 0.0366(17) Uani 1 1 d . . . C2 C 0.3617(3) 0.4093(4) 0.0300(3) 0.0396(18) Uani 1 1 d . . . B3 B 0.2736(4) 0.3749(6) 0.0532(4) 0.043(2) Uani 1 1 d . . . B4 B 0.2369(4) 0.3180(6) -0.0173(4) 0.043(2) Uani 1 1 d . . . B5 B 0.3034(5) 0.3235(6) -0.0824(4) 0.046(2) Uani 1 1 d . . . B6 B 0.3825(4) 0.3808(6) -0.0526(4) 0.043(2) Uani 1 1 d . . . B7 B 0.2940(5) 0.4937(6) 0.0357(5) 0.051(2) Uani 1 1 d . . . B8 B 0.2127(5) 0.4375(6) 0.0041(4) 0.048(2) Uani 1 1 d . . . B9 B 0.2298(5) 0.4057(6) -0.0814(4) 0.049(2) Uani 1 1 d . . . B10 B 0.3214(5) 0.4432(6) -0.1021(5) 0.055(3) Uani 1 1 d . . . B11 B 0.3612(5) 0.4985(6) -0.0301(4) 0.046(2) Uani 1 1 d . . . B12 B 0.2668(5) 0.5148(6) -0.0486(4) 0.054(3) Uani 1 1 d . . . H1 H 0.266(2) 0.347(3) 0.101(2) 0.024(15) Uiso 1 1 d . . . H2 H 0.205(2) 0.245(4) -0.007(2) 0.051(17) Uiso 1 1 d . . . H3 H 0.3140(19) 0.267(3) -0.1129(19) 0.011(13) Uiso 1 1 d . . . H4 H 0.438(2) 0.363(3) -0.066(2) 0.028(15) Uiso 1 1 d . . . H5 H 0.299(2) 0.545(3) 0.072(2) 0.029(16) Uiso 1 1 d . . . H6 H 0.152(2) 0.450(3) 0.020(2) 0.044(17) Uiso 1 1 d . . . H7 H 0.187(2) 0.413(4) -0.121(2) 0.059(19) Uiso 1 1 d . . . H8 H 0.344(2) 0.472(3) -0.145(2) 0.035(18) Uiso 1 1 d . . . H9 H 0.410(2) 0.552(4) -0.023(2) 0.056(18) Uiso 1 1 d . . . H10 H 0.256(2) 0.589(4) -0.056(2) 0.053(19) Uiso 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 0.0434(3) 0.0413(3) 0.0331(3) 0.0019(3) -0.0001(3) -0.0011(3) Se1 0.0442(4) 0.0361(4) 0.0381(4) -0.0008(4) 0.0015(4) -0.0020(4) Se2 0.0482(4) 0.0426(4) 0.0420(5) -0.0019(4) -0.0033(4) -0.0085(4) Fe1 0.0395(6) 0.0505(7) 0.0475(7) 0.0018(6) 0.0032(5) -0.0010(6) O1 0.064(4) 0.093(5) 0.072(4) 0.001(3) -0.015(3) 0.003(3) O2 0.070(4) 0.064(4) 0.129(5) 0.011(4) 0.005(3) 0.009(3) O3 0.051(3) 0.141(5) 0.061(4) 0.004(4) 0.019(2) 0.007(4) C3 0.050(5) 0.064(6) 0.069(7) 0.014(5) 0.003(4) -0.003(4) C4 0.040(5) 0.054(6) 0.073(6) -0.002(5) 0.009(4) -0.003(4) C5 0.029(4) 0.084(6) 0.074(7) -0.007(6) 0.002(4) 0.003(4) C6 0.053(5) 0.041(5) 0.033(5) 0.000(4) 0.004(4) -0.001(4) C7 0.062(5) 0.047(5) 0.034(5) 0.014(4) -0.003(4) 0.009(5) C8 0.058(5) 0.049(6) 0.027(4) 0.005(4) 0.001(3) 0.003(4) C9 0.073(6) 0.053(6) 0.028(5) 0.008(4) 0.011(4) 0.015(5) C10 0.050(5) 0.066(6) 0.023(5) 0.001(4) 0.005(4) -0.010(5) C11 0.099(6) 0.051(5) 0.038(5) 0.000(4) 0.008(4) -0.021(4) C12 0.071(5) 0.065(6) 0.067(6) 0.013(5) -0.013(5) 0.017(5) C13 0.110(7) 0.053(6) 0.053(5) -0.004(4) -0.031(5) -0.020(5) C14 0.123(7) 0.073(6) 0.046(6) 0.010(5) 0.019(5) 0.043(6) C15 0.059(5) 0.123(8) 0.052(6) 0.001(5) 0.012(4) -0.010(5) C1 0.045(4) 0.037(4) 0.028(4) -0.002(4) 0.004(3) 0.005(4) C2 0.046(4) 0.033(4) 0.039(5) -0.003(4) 0.009(4) -0.009(3) B3 0.048(6) 0.052(6) 0.030(6) -0.001(5) 0.002(5) 0.003(4) B4 0.053(6) 0.048(6) 0.030(6) -0.004(5) -0.006(4) -0.002(5) B5 0.083(7) 0.032(6) 0.023(6) -0.004(4) 0.006(5) 0.005(5) B6 0.043(6) 0.056(6) 0.031(6) 0.003(4) 0.003(4) -0.011(5) B7 0.072(7) 0.037(6) 0.043(7) -0.005(5) 0.000(5) 0.005(5) B8 0.057(6) 0.050(6) 0.038(6) 0.004(5) -0.003(5) 0.009(5) B9 0.063(6) 0.051(6) 0.034(6) -0.006(5) -0.007(5) 0.011(5) B10 0.074(7) 0.057(7) 0.034(6) 0.009(6) -0.001(6) 0.001(5) B11 0.067(6) 0.039(5) 0.033(6) 0.006(5) 0.007(5) 0.007(5) B12 0.079(7) 0.039(6) 0.043(6) 0.003(5) 0.006(5) 0.024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C6 2.144(6) . ? Rh1 C9 2.176(6) . ? Rh1 C8 2.180(6) . ? Rh1 C10 2.186(6) . ? Rh1 C7 2.198(6) . ? Rh1 Se2 2.4397(10) . ? Rh1 Se1 2.4439(10) . ? Rh1 Fe1 2.5500(11) . ? Se1 C1 1.959(6) . ? Se1 Fe1 2.3945(12) . ? Se2 C2 1.959(6) . ? Se2 Fe1 2.4148(13) . ? Fe1 C4 1.722(7) . ? Fe1 C3 1.733(7) . ? Fe1 C5 1.803(7) . ? O1 C3 1.163(6) . ? O2 C4 1.182(7) . ? O3 C5 1.135(7) . ? C6 C7 1.425(8) . ? C6 C10 1.428(8) . ? C6 C11 1.478(8) . ? C7 C8 1.408(9) . ? C7 C12 1.494(7) . ? C8 C9 1.453(8) . ? C8 C13 1.514(7) . ? C9 C10 1.402(8) . ? C9 C14 1.511(8) . ? C10 C15 1.501(7) . ? C11 H9A 0.9600 . ? C11 H9B 0.9600 . ? C11 H9C 0.9600 . ? C12 H10A 0.9600 . ? C12 H10B 0.9600 . ? C12 H10C 0.9600 . ? C13 H11A 0.9600 . ? C13 H11B 0.9600 . ? C13 H11C 0.9600 . ? C14 H12A 0.9600 . ? C14 H12B 0.9600 . ? C14 H12C 0.9600 . ? C15 H13A 0.9600 . ? C15 H13B 0.9600 . ? C15 H13C 0.9600 . ? C1 C2 1.606(7) . ? C1 B5 1.700(9) . ? C1 B6 1.711(9) . ? C1 B3 1.719(9) . ? C1 B4 1.725(8) . ? C2 B7 1.706(9) . ? C2 B6 1.718(9) . ? C2 B11 1.720(9) . ? C2 B3 1.728(9) . ? B3 B8 1.709(11) . ? B3 B4 1.734(10) . ? B3 B7 1.736(11) . ? B3 H1 1.02(4) . ? B4 B5 1.760(10) . ? B4 B9 1.765(11) . ? B4 B8 1.778(11) . ? B4 H2 1.19(5) . ? B5 B6 1.743(10) . ? B5 B10 1.748(11) . ? B5 B9 1.760(10) . ? B5 H3 1.02(4) . ? B6 B10 1.714(11) . ? B6 B11 1.748(10) . ? B6 H4 1.07(4) . ? B7 B12 1.757(12) . ? B7 B11 1.779(11) . ? B7 B8 1.783(11) . ? B7 H5 1.02(4) . ? B8 B9 1.768(10) . ? B8 B12 1.791(12) . ? B8 H6 1.16(4) . ? B9 B12 1.786(11) . ? B9 B10 1.787(11) . ? B9 H7 1.10(5) . ? B10 B12 1.758(12) . ? B10 B11 1.769(12) . ? B10 H8 1.02(4) . ? B11 B12 1.763(11) . ? B11 H9 1.16(4) . ? B12 H10 1.07(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 C6 Rh1 C9 63.9(2) . . ? C6 Rh1 C8 63.8(2) . . ? C9 Rh1 C8 39.0(2) . . ? C6 Rh1 C10 38.5(2) . . ? C9 Rh1 C10 37.5(2) . . ? C8 Rh1 C10 63.9(2) . . ? C6 Rh1 C7 38.3(2) . . ? C9 Rh1 C7 63.8(2) . . ? C8 Rh1 C7 37.5(2) . . ? C10 Rh1 C7 63.9(2) . . ? C6 Rh1 Se2 171.78(18) . . ? C9 Rh1 Se2 110.72(19) . . ? C8 Rh1 Se2 108.00(19) . . ? C10 Rh1 Se2 140.3(2) . . ? C7 Rh1 Se2 134.4(2) . . ? C6 Rh1 Se1 106.38(18) . . ? C9 Rh1 Se1 140.1(2) . . ? C8 Rh1 Se1 170.05(19) . . ? C10 Rh1 Se1 109.98(18) . . ? C7 Rh1 Se1 133.4(2) . . ? Se2 Rh1 Se1 81.75(3) . . ? C6 Rh1 Fe1 125.36(18) . . ? C9 Rh1 Fe1 161.0(2) . . ? C8 Rh1 Fe1 125.93(17) . . ? C10 Rh1 Fe1 159.7(2) . . ? C7 Rh1 Fe1 111.73(19) . . ? Se2 Rh1 Fe1 57.84(3) . . ? Se1 Rh1 Fe1 57.26(3) . . ? C1 Se1 Fe1 103.25(17) . . ? C1 Se1 Rh1 102.03(18) . . ? Fe1 Se1 Rh1 63.60(3) . . ? C2 Se2 Fe1 103.97(17) . . ? C2 Se2 Rh1 102.21(17) . . ? Fe1 Se2 Rh1 63.37(3) . . ? C4 Fe1 C3 91.9(3) . . ? C4 Fe1 C5 98.7(3) . . ? C3 Fe1 C5 99.6(3) . . ? C4 Fe1 Se1 86.1(2) . . ? C3 Fe1 Se1 153.5(2) . . ? C5 Fe1 Se1 106.8(2) . . ? C4 Fe1 Se2 151.9(2) . . ? C3 Fe1 Se2 86.3(2) . . ? C5 Fe1 Se2 109.3(3) . . ? Se1 Fe1 Se2 83.29(4) . . ? C4 Fe1 Rh1 93.6(2) . . ? C3 Fe1 Rh1 94.7(2) . . ? C5 Fe1 Rh1 160.8(2) . . ? Se1 Fe1 Rh1 59.14(3) . . ? Se2 Fe1 Rh1 58.79(3) . . ? O1 C3 Fe1 178.1(7) . . ? O2 C4 Fe1 177.9(7) . . ? O3 C5 Fe1 175.0(8) . . ? C7 C6 C10 108.7(6) . . ? C7 C6 C11 125.7(7) . . ? C10 C6 C11 125.3(7) . . ? C7 C6 Rh1 72.9(4) . . ? C10 C6 Rh1 72.3(4) . . ? C11 C6 Rh1 126.1(4) . . ? C8 C7 C6 107.6(6) . . ? C8 C7 C12 126.0(7) . . ? C6 C7 C12 126.2(7) . . ? C8 C7 Rh1 70.6(4) . . ? C6 C7 Rh1 68.8(4) . . ? C12 C7 Rh1 130.0(5) . . ? C7 C8 C9 107.9(6) . . ? C7 C8 C13 126.1(7) . . ? C9 C8 C13 125.8(7) . . ? C7 C8 Rh1 71.9(4) . . ? C9 C8 Rh1 70.4(4) . . ? C13 C8 Rh1 127.3(4) . . ? C10 C9 C8 108.0(6) . . ? C10 C9 C14 128.1(7) . . ? C8 C9 C14 123.8(7) . . ? C10 C9 Rh1 71.6(4) . . ? C8 C9 Rh1 70.7(4) . . ? C14 C9 Rh1 126.3(4) . . ? C9 C10 C6 107.7(6) . . ? C9 C10 C15 124.0(7) . . ? C6 C10 C15 128.1(7) . . ? C9 C10 Rh1 70.9(4) . . ? C6 C10 Rh1 69.2(4) . . ? C15 C10 Rh1 129.6(4) . . ? C6 C11 H9A 109.5 . . ? C6 C11 H9B 109.5 . . ? H9A C11 H9B 109.5 . . ? C6 C11 H9C 109.5 . . ? H9A C11 H9C 109.5 . . ? H9B C11 H9C 109.5 . . ? C7 C12 H10A 109.5 . . ? C7 C12 H10B 109.5 . . ? H10A C12 H10B 109.5 . . ? C7 C12 H10C 109.5 . . ? H10A C12 H10C 109.5 . . ? H10B C12 H10C 109.5 . . ? C8 C13 H11A 109.5 . . ? C8 C13 H11B 109.5 . . ? H11A C13 H11B 109.5 . . ? C8 C13 H11C 109.5 . . ? H11A C13 H11C 109.5 . . ? H11B C13 H11C 109.5 . . ? C9 C14 H12A 109.5 . . ? C9 C14 H12B 109.5 . . ? H12A C14 H12B 109.5 . . ? C9 C14 H12C 109.5 . . ? H12A C14 H12C 109.5 . . ? H12B C14 H12C 109.5 . . ? C10 C15 H13A 109.5 . . ? C10 C15 H13B 109.5 . . ? H13A C15 H13B 109.5 . . ? C10 C15 H13C 109.5 . . ? H13A C15 H13C 109.5 . . ? H13B C15 H13C 109.5 . . ? C2 C1 B5 111.3(5) . . ? C2 C1 B6 62.3(4) . . ? B5 C1 B6 61.4(4) . . ? C2 C1 B3 62.5(4) . . ? B5 C1 B3 111.0(5) . . ? B6 C1 B3 113.6(5) . . ? C2 C1 B4 111.8(5) . . ? B5 C1 B4 61.8(4) . . ? B6 C1 B4 113.0(5) . . ? B3 C1 B4 60.5(4) . . ? C2 C1 Se1 114.7(4) . . ? B5 C1 Se1 125.2(5) . . ? B6 C1 Se1 118.9(4) . . ? B3 C1 Se1 115.7(4) . . ? B4 C1 Se1 121.6(4) . . ? C1 C2 B7 111.2(5) . . ? C1 C2 B6 61.9(4) . . ? B7 C2 B6 112.3(5) . . ? C1 C2 B11 111.4(5) . . ? B7 C2 B11 62.6(4) . . ? B6 C2 B11 61.1(4) . . ? C1 C2 B3 61.9(4) . . ? B7 C2 B3 60.7(4) . . ? B6 C2 B3 112.8(5) . . ? B11 C2 B3 112.2(5) . . ? C1 C2 Se2 113.2(4) . . ? B7 C2 Se2 124.8(5) . . ? B6 C2 Se2 116.7(4) . . ? B11 C2 Se2 124.4(4) . . ? B3 C2 Se2 117.1(4) . . ? B8 B3 C1 107.8(6) . . ? B8 B3 C2 107.7(6) . . ? C1 B3 C2 55.5(3) . . ? B8 B3 B4 62.2(5) . . ? C1 B3 B4 59.9(4) . . ? C2 B3 B4 105.7(5) . . ? B8 B3 B7 62.3(5) . . ? C1 B3 B7 104.5(6) . . ? C2 B3 B7 59.0(4) . . ? B4 B3 B7 111.2(6) . . ? B8 B3 H1 129(3) . . ? C1 B3 H1 116(3) . . ? C2 B3 H1 118(2) . . ? B4 B3 H1 121(3) . . ? B7 B3 H1 125(3) . . ? C1 B4 B3 59.6(4) . . ? C1 B4 B5 58.4(4) . . ? B3 B4 B5 107.5(6) . . ? C1 B4 B9 104.6(5) . . ? B3 B4 B9 106.4(6) . . ? B5 B4 B9 59.9(4) . . ? C1 B4 B8 104.5(5) . . ? B3 B4 B8 58.2(5) . . ? B5 B4 B8 107.5(6) . . ? B9 B4 B8 59.9(4) . . ? C1 B4 H2 114(2) . . ? B3 B4 H2 116(2) . . ? B5 B4 H2 120(2) . . ? B9 B4 H2 133(2) . . ? B8 B4 H2 130(2) . . ? C1 B5 B6 59.6(4) . . ? C1 B5 B10 105.0(6) . . ? B6 B5 B10 58.8(5) . . ? C1 B5 B9 105.9(6) . . ? B6 B5 B9 108.6(6) . . ? B10 B5 B9 61.2(5) . . ? C1 B5 B4 59.8(4) . . ? B6 B5 B4 109.7(6) . . ? B10 B5 B4 109.4(6) . . ? B9 B5 B4 60.2(5) . . ? C1 B5 H3 115(2) . . ? B6 B5 H3 114(2) . . ? B10 B5 H3 126(2) . . ? B9 B5 H3 131(2) . . ? B4 B5 H3 122(2) . . ? C1 B6 B10 106.1(6) . . ? C1 B6 C2 55.9(3) . . ? B10 B6 C2 106.2(6) . . ? C1 B6 B5 59.0(4) . . ? B10 B6 B5 60.8(4) . . ? C2 B6 B5 104.2(5) . . ? C1 B6 B11 105.3(5) . . ? B10 B6 B11 61.5(5) . . ? C2 B6 B11 59.5(4) . . ? B5 B6 B11 109.7(6) . . ? C1 B6 H4 123(2) . . ? B10 B6 H4 126(2) . . ? C2 B6 H4 120(2) . . ? B5 B6 H4 125(2) . . ? B11 B6 H4 120(2) . . ? C2 B7 B3 60.3(4) . . ? C2 B7 B12 104.8(6) . . ? B3 B7 B12 106.8(6) . . ? C2 B7 B11 59.1(4) . . ? B3 B7 B11 109.0(6) . . ? B12 B7 B11 59.8(5) . . ? C2 B7 B8 105.5(6) . . ? B3 B7 B8 58.1(5) . . ? B12 B7 B8 60.8(5) . . ? B11 B7 B8 109.1(6) . . ? C2 B7 H5 118(3) . . ? B3 B7 H5 123(3) . . ? B12 B7 H5 125(3) . . ? B11 B7 H5 115(3) . . ? B8 B7 H5 129(3) . . ? B3 B8 B9 107.3(6) . . ? B3 B8 B4 59.6(4) . . ? B9 B8 B4 59.7(5) . . ? B3 B8 B7 59.6(4) . . ? B9 B8 B7 107.3(6) . . ? B4 B8 B7 107.0(6) . . ? B3 B8 B12 106.5(6) . . ? B9 B8 B12 60.2(5) . . ? B4 B8 B12 107.1(6) . . ? B7 B8 B12 58.9(5) . . ? B3 B8 H6 123(2) . . ? B9 B8 H6 117(2) . . ? B4 B8 H6 116(2) . . ? B7 B8 H6 129(2) . . ? B12 B8 H6 126(2) . . ? B5 B9 B4 59.9(4) . . ? B5 B9 B8 107.9(6) . . ? B4 B9 B8 60.4(4) . . ? B5 B9 B12 106.1(6) . . ? B4 B9 B12 107.9(6) . . ? B8 B9 B12 60.5(5) . . ? B5 B9 B10 59.1(4) . . ? B4 B9 B10 107.4(6) . . ? B8 B9 B10 107.9(6) . . ? B12 B9 B10 58.9(5) . . ? B5 B9 H7 126(3) . . ? B4 B9 H7 128(3) . . ? B8 B9 H7 121(3) . . ? B12 B9 H7 116(3) . . ? B10 B9 H7 118(3) . . ? B6 B10 B5 60.4(5) . . ? B6 B10 B12 108.2(7) . . ? B5 B10 B12 107.8(7) . . ? B6 B10 B11 60.2(5) . . ? B5 B10 B11 108.4(6) . . ? B12 B10 B11 60.0(5) . . ? B6 B10 B9 108.7(6) . . ? B5 B10 B9 59.7(5) . . ? B12 B10 B9 60.5(5) . . ? B11 B10 B9 108.9(7) . . ? B6 B10 H8 114(3) . . ? B5 B10 H8 129(3) . . ? B12 B10 H8 120(3) . . ? B11 B10 H8 109(3) . . ? B9 B10 H8 133(3) . . ? C2 B11 B6 59.4(4) . . ? C2 B11 B12 104.0(6) . . ? B6 B11 B12 106.4(6) . . ? C2 B11 B10 103.7(6) . . ? B6 B11 B10 58.3(4) . . ? B12 B11 B10 59.7(5) . . ? C2 B11 B7 58.3(4) . . ? B6 B11 B7 107.5(6) . . ? B12 B11 B7 59.5(5) . . ? B10 B11 B7 106.8(7) . . ? C2 B11 H9 112(3) . . ? B6 B11 H9 118(3) . . ? B12 B11 H9 133(2) . . ? B10 B11 H9 134(3) . . ? B7 B11 H9 117(3) . . ? B7 B12 B10 108.2(6) . . ? B7 B12 B11 60.7(5) . . ? B10 B12 B11 60.3(5) . . ? B7 B12 B9 107.7(6) . . ? B10 B12 B9 60.6(5) . . ? B11 B12 B9 109.2(6) . . ? B7 B12 B8 60.3(5) . . ? B10 B12 B8 108.2(6) . . ? B11 B12 B8 109.5(6) . . ? B9 B12 B8 59.3(5) . . ? B7 B12 H10 110(3) . . ? B10 B12 H10 125(3) . . ? B11 B12 H10 109(3) . . ? B9 B12 H10 135(3) . . ? B8 B12 H10 125(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.701 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.085 # Attachment '6a.cif' data_f51220e _database_code_depnum_ccdc_archive 'CCDC 608152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 B20 Fe2 O6 Rh2 S4' _chemical_formula_weight 1252.82 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 26.135(13) _cell_length_b 16.356(8) _cell_length_c 26.135(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11172(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 2.465 _cell_measurement_theta_max 19.072 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8827 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 3.79 _diffrn_reflns_number 45330 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.1501 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9862 _reflns_number_gt 4328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0156P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9862 _refine_ls_number_parameters 651 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 0.662 _refine_ls_restrained_S_all 0.662 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.004 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 0.617505(17) 0.86511(2) 0.112475(14) 0.04242(12) Uani 1 1 d . . . Fe1 Fe 0.58898(3) 0.71843(4) 0.11030(3) 0.0544(2) Uani 1 1 d . . . S1 S 0.64838(6) 0.76512(8) 0.16907(5) 0.0511(4) Uani 1 1 d . . . S2 S 0.65011(6) 0.76719(8) 0.05518(5) 0.0458(4) Uani 1 1 d . . . O1 O 0.5115(2) 0.7278(3) 0.18993(19) 0.115(2) Uani 1 1 d . . . O2 O 0.50892(19) 0.7598(3) 0.03713(18) 0.0957(17) Uani 1 1 d . . . O3 O 0.58514(19) 0.5400(3) 0.0976(2) 0.123(2) Uani 1 1 d . . . C1 C 0.7108(2) 0.7368(3) 0.14353(19) 0.0476(16) Uani 1 1 d . . . C2 C 0.7115(2) 0.7360(3) 0.08191(19) 0.0434(15) Uani 1 1 d . . . C3 C 0.5419(3) 0.7233(4) 0.1587(3) 0.078(2) Uani 1 1 d . . . C4 C 0.5405(3) 0.7432(4) 0.0650(2) 0.068(2) Uani 1 1 d . . . C5 C 0.5883(2) 0.6093(4) 0.1030(2) 0.074(2) Uani 1 1 d . . . C6 C 0.6093(2) 0.9788(3) 0.1565(2) 0.0415(14) Uani 1 1 d . . . C7 C 0.6368(2) 0.9963(3) 0.1109(2) 0.0425(14) Uani 1 1 d . . . H7A H 0.6715 1.0189 0.1093 0.051 Uiso 1 1 calc R . . C8 C 0.6055(3) 0.9780(3) 0.0682(2) 0.0451(15) Uani 1 1 d . . . C9 C 0.5582(2) 0.9489(3) 0.0874(2) 0.0539(17) Uani 1 1 d . . . H9A H 0.5283 0.9343 0.0667 0.065 Uiso 1 1 calc R . . C10 C 0.5602(2) 0.9488(3) 0.1415(2) 0.0527(16) Uani 1 1 d . . . H10A H 0.5320 0.9347 0.1646 0.063 Uiso 1 1 calc R . . C11 C 0.6251(2) 0.9983(3) 0.2110(2) 0.0497(16) Uani 1 1 d . . . C12 C 0.6069(2) 1.0861(3) 0.22241(18) 0.0702(18) Uani 1 1 d . . . H12A H 0.6229 1.1234 0.1990 0.105 Uiso 1 1 calc R . . H12B H 0.6160 1.1005 0.2568 0.105 Uiso 1 1 calc R . . H12C H 0.5704 1.0890 0.2186 0.105 Uiso 1 1 calc R . . C13 C 0.6832(2) 0.9934(3) 0.21678(19) 0.0704(19) Uani 1 1 d . . . H13A H 0.6944 0.9386 0.2100 0.106 Uiso 1 1 calc R . . H13B H 0.6926 1.0084 0.2510 0.106 Uiso 1 1 calc R . . H13C H 0.6992 1.0302 0.1930 0.106 Uiso 1 1 calc R . . C14 C 0.6002(2) 0.9394(3) 0.24992(18) 0.076(2) Uani 1 1 d . . . H14A H 0.6119 0.8846 0.2435 0.114 Uiso 1 1 calc R . . H14B H 0.5637 0.9415 0.2464 0.114 Uiso 1 1 calc R . . H14C H 0.6096 0.9553 0.2840 0.114 Uiso 1 1 calc R . . C15 C 0.6177(3) 0.9952(3) 0.0124(2) 0.0584(17) Uani 1 1 d . . . C16 C 0.5985(2) 1.0834(3) 0.00206(18) 0.088(2) Uani 1 1 d . . . H16A H 0.6161 1.1209 0.0241 0.132 Uiso 1 1 calc R . . H16B H 0.5624 1.0863 0.0087 0.132 Uiso 1 1 calc R . . H16C H 0.6049 1.0976 -0.0330 0.132 Uiso 1 1 calc R . . C17 C 0.6757(3) 0.9919(4) 0.00323(19) 0.080(2) Uani 1 1 d . . . H17A H 0.6879 0.9376 0.0099 0.121 Uiso 1 1 calc R . . H17B H 0.6925 1.0297 0.0257 0.121 Uiso 1 1 calc R . . H17C H 0.6829 1.0064 -0.0316 0.121 Uiso 1 1 calc R . . C18 C 0.5898(2) 0.9367(3) -0.02302(19) 0.082(2) Uani 1 1 d . . . H18A H 0.6021 0.8821 -0.0175 0.123 Uiso 1 1 calc R . . H18B H 0.5959 0.9522 -0.0579 0.123 Uiso 1 1 calc R . . H18C H 0.5538 0.9389 -0.0160 0.123 Uiso 1 1 calc R . . B3 B 0.7150(3) 0.6426(3) 0.1138(3) 0.0562(19) Uani 1 1 d . . . H3 H 0.6849 0.5956 0.1143 0.067 Uiso 1 1 calc R . . B4 B 0.7514(3) 0.6635(4) 0.1683(3) 0.061(2) Uani 1 1 d . . . H4 H 0.7450 0.6311 0.2046 0.074 Uiso 1 1 calc R . . B5 B 0.7689(3) 0.7687(4) 0.1678(2) 0.053(2) Uani 1 1 d . . . H5 H 0.7734 0.8035 0.2035 0.064 Uiso 1 1 calc R . . B6 B 0.7443(2) 0.8145(4) 0.1128(2) 0.0463(17) Uani 1 1 d . . . H6 H 0.7334 0.8794 0.1125 0.056 Uiso 1 1 calc R . . B7 B 0.7515(3) 0.6623(4) 0.0587(3) 0.061(2) Uani 1 1 d . . . H7 H 0.7448 0.6289 0.0227 0.073 Uiso 1 1 calc R . . B8 B 0.7787(3) 0.6166(4) 0.1135(3) 0.072(2) Uani 1 1 d . . . H8 H 0.7908 0.5522 0.1137 0.086 Uiso 1 1 calc R . . B9 B 0.8128(3) 0.6922(4) 0.1470(3) 0.064(2) Uani 1 1 d . . . H9 H 0.8471 0.6771 0.1695 0.077 Uiso 1 1 calc R . . B10 B 0.8080(3) 0.7845(4) 0.1132(2) 0.0560(19) Uani 1 1 d . . . H10 H 0.8392 0.8295 0.1131 0.067 Uiso 1 1 calc R . . B11 B 0.7694(3) 0.7662(4) 0.0587(2) 0.0496(19) Uani 1 1 d . . . H11 H 0.7742 0.7999 0.0225 0.059 Uiso 1 1 calc R . . B12 B 0.8139(3) 0.6912(4) 0.0794(3) 0.059(2) Uani 1 1 d . . . H12 H 0.8485 0.6758 0.0574 0.071 Uiso 1 1 calc R . . Rh2 Rh 0.393707(16) 0.40425(2) 0.125489(15) 0.04143(12) Uani 1 1 d . . . Fe2 Fe 0.39312(4) 0.55345(4) 0.10249(3) 0.0556(2) Uani 1 1 d . . . O4 O 0.4798(2) 0.5595(3) 0.03207(18) 0.116(2) Uani 1 1 d . . . O5 O 0.3219(2) 0.5210(3) 0.01955(18) 0.115(2) Uani 1 1 d . . . O6 O 0.3853(2) 0.7326(2) 0.09856(16) 0.1090(18) Uani 1 1 d . . . S3 S 0.44821(6) 0.50215(8) 0.16333(5) 0.0478(4) Uani 1 1 d . . . S4 S 0.33320(6) 0.49773(8) 0.15715(5) 0.0492(4) Uani 1 1 d . . . C21 C 0.4180(2) 0.5241(3) 0.22468(18) 0.0416(15) Uani 1 1 d . . . C22 C 0.3562(2) 0.5206(3) 0.22106(19) 0.0427(15) Uani 1 1 d . . . C23 C 0.4461(3) 0.5566(4) 0.0594(2) 0.075(2) Uani 1 1 d . . . C24 C 0.3495(3) 0.5344(4) 0.0519(3) 0.079(2) Uani 1 1 d . . . C25 C 0.3880(3) 0.6632(3) 0.1028(2) 0.0724(19) Uani 1 1 d . . . C26 C 0.4405(2) 0.2944(3) 0.1109(2) 0.0443(15) Uani 1 1 d . . . C27 C 0.3960(2) 0.2705(3) 0.13882(18) 0.0435(14) Uani 1 1 d . . . H27A H 0.3962 0.2442 0.1725 0.052 Uiso 1 1 calc R . . C28 C 0.3516(2) 0.2900(3) 0.1103(2) 0.0448(15) Uani 1 1 d . . . C29 C 0.3687(2) 0.3266(3) 0.0638(2) 0.0472(16) Uani 1 1 d . . . H29A H 0.3468 0.3434 0.0352 0.057 Uiso 1 1 calc R . . C30 C 0.4224(2) 0.3288(3) 0.0642(2) 0.0496(16) Uani 1 1 d . . . H30A H 0.4441 0.3478 0.0360 0.060 Uiso 1 1 calc R . . C31 C 0.4959(2) 0.2780(3) 0.1257(2) 0.0563(17) Uani 1 1 d . . . C32 C 0.5076(2) 0.1904(3) 0.1069(2) 0.081(2) Uani 1 1 d . . . H32A H 0.5422 0.1764 0.1156 0.122 Uiso 1 1 calc R . . H32B H 0.5034 0.1879 0.0705 0.122 Uiso 1 1 calc R . . H32C H 0.4845 0.1526 0.1230 0.122 Uiso 1 1 calc R . . C33 C 0.5034(2) 0.2802(3) 0.1833(2) 0.075(2) Uani 1 1 d . . . H33A H 0.4966 0.3344 0.1957 0.113 Uiso 1 1 calc R . . H33B H 0.5380 0.2653 0.1914 0.113 Uiso 1 1 calc R . . H33C H 0.4803 0.2423 0.1993 0.113 Uiso 1 1 calc R . . C34 C 0.5328(2) 0.3377(4) 0.0997(2) 0.089(2) Uani 1 1 d . . . H34A H 0.5261 0.3922 0.1117 0.134 Uiso 1 1 calc R . . H34B H 0.5281 0.3355 0.0633 0.134 Uiso 1 1 calc R . . H34C H 0.5674 0.3229 0.1079 0.134 Uiso 1 1 calc R . . C35 C 0.2964(2) 0.2686(3) 0.1232(2) 0.0471(15) Uani 1 1 d . . . C36 C 0.2854(2) 0.1842(3) 0.0986(2) 0.077(2) Uani 1 1 d . . . H36A H 0.2893 0.1881 0.0622 0.115 Uiso 1 1 calc R . . H36B H 0.2511 0.1676 0.1067 0.115 Uiso 1 1 calc R . . H36C H 0.3091 0.1445 0.1118 0.115 Uiso 1 1 calc R . . C37 C 0.2891(2) 0.2619(3) 0.1818(2) 0.077(2) Uani 1 1 d . . . H37A H 0.2957 0.3140 0.1973 0.116 Uiso 1 1 calc R . . H37B H 0.3125 0.2220 0.1953 0.116 Uiso 1 1 calc R . . H37C H 0.2546 0.2453 0.1891 0.116 Uiso 1 1 calc R . . C38 C 0.2582(2) 0.3302(3) 0.1018(2) 0.081(2) Uani 1 1 d . . . H38A H 0.2623 0.3339 0.0654 0.122 Uiso 1 1 calc R . . H38B H 0.2643 0.3829 0.1169 0.122 Uiso 1 1 calc R . . H38C H 0.2240 0.3127 0.1096 0.122 Uiso 1 1 calc R . . B13 B 0.3849(3) 0.6151(3) 0.2299(2) 0.0525(19) Uani 1 1 d . . . H13 H 0.3855 0.6649 0.2016 0.063 Uiso 1 1 calc R . . B14 B 0.4382(3) 0.5935(4) 0.2686(2) 0.057(2) Uani 1 1 d . . . H14 H 0.4739 0.6285 0.2656 0.069 Uiso 1 1 calc R . . B15 B 0.4391(3) 0.4881(4) 0.2817(2) 0.0489(19) Uani 1 1 d . . . H15 H 0.4754 0.4552 0.2869 0.059 Uiso 1 1 calc R . . B16 B 0.3875(2) 0.4413(3) 0.2518(2) 0.0421(16) Uani 1 1 d . . . H16 H 0.3899 0.3779 0.2379 0.051 Uiso 1 1 calc R . . B17 B 0.3283(3) 0.5892(4) 0.2620(2) 0.056(2) Uani 1 1 d . . . H17 H 0.2920 0.6213 0.2546 0.067 Uiso 1 1 calc R . . B18 B 0.3809(3) 0.6344(4) 0.2941(2) 0.065(2) Uani 1 1 d . . . H18 H 0.3789 0.6975 0.3086 0.078 Uiso 1 1 calc R . . B19 B 0.4146(3) 0.5576(4) 0.3274(2) 0.060(2) Uani 1 1 d . . . H19 H 0.4346 0.5701 0.3636 0.072 Uiso 1 1 calc R . . B20 B 0.3828(3) 0.4642(3) 0.3163(2) 0.0497(19) Uani 1 1 d . . . H20 H 0.3818 0.4158 0.3455 0.060 Uiso 1 1 calc R . . B21 B 0.3298(3) 0.4823(4) 0.2756(2) 0.051(2) Uani 1 1 d . . . H21 H 0.2944 0.4459 0.2768 0.061 Uiso 1 1 calc R . . B22 B 0.3472(3) 0.5543(4) 0.3239(3) 0.064(2) Uani 1 1 d . . . H22 H 0.3232 0.5646 0.3578 0.077 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 0.0492(3) 0.0403(2) 0.0378(3) -0.0026(2) 0.0011(2) 0.0017(2) Fe1 0.0549(6) 0.0472(5) 0.0610(6) -0.0040(5) 0.0035(5) -0.0076(4) S1 0.0645(13) 0.0475(9) 0.0414(9) 0.0037(7) 0.0027(8) -0.0016(9) S2 0.0494(12) 0.0475(9) 0.0405(9) -0.0077(7) -0.0032(7) 0.0018(8) O1 0.119(6) 0.113(4) 0.111(5) 0.001(4) 0.052(4) -0.010(4) O2 0.071(4) 0.126(4) 0.090(4) -0.007(3) -0.020(3) 0.001(3) O3 0.103(4) 0.061(3) 0.206(6) -0.023(4) -0.009(4) -0.014(3) C1 0.054(5) 0.042(3) 0.047(4) 0.001(3) -0.005(3) -0.001(3) C2 0.050(4) 0.037(3) 0.043(4) -0.003(3) -0.007(3) -0.003(3) C3 0.088(7) 0.073(5) 0.074(5) 0.007(4) 0.006(5) -0.010(5) C4 0.062(6) 0.078(5) 0.063(5) -0.011(4) 0.006(4) -0.013(4) C5 0.055(5) 0.068(5) 0.098(5) -0.011(4) -0.006(4) -0.012(4) C6 0.048(4) 0.034(3) 0.043(4) -0.005(2) -0.003(4) 0.006(3) C7 0.052(4) 0.036(3) 0.040(3) 0.002(3) 0.002(3) 0.000(3) C8 0.053(4) 0.036(3) 0.046(4) -0.001(3) -0.003(4) 0.008(3) C9 0.051(5) 0.058(4) 0.053(4) -0.010(3) -0.012(4) 0.004(4) C10 0.052(5) 0.055(4) 0.051(4) -0.008(3) 0.007(3) 0.000(3) C11 0.053(5) 0.050(4) 0.046(4) -0.005(3) -0.005(3) 0.005(3) C12 0.088(5) 0.069(4) 0.054(4) -0.023(3) -0.008(4) 0.011(4) C13 0.078(6) 0.080(5) 0.053(4) -0.011(3) -0.019(4) 0.010(4) C14 0.107(6) 0.084(4) 0.037(3) -0.003(3) 0.003(4) -0.007(4) C15 0.086(6) 0.052(4) 0.038(4) 0.005(3) -0.002(4) 0.007(4) C16 0.152(8) 0.058(4) 0.055(4) 0.013(3) -0.007(4) 0.031(5) C17 0.105(7) 0.091(5) 0.046(4) 0.005(3) 0.021(4) 0.004(5) C18 0.108(7) 0.094(5) 0.044(4) -0.010(4) -0.013(4) -0.007(4) B3 0.057(5) 0.033(4) 0.078(5) 0.006(4) -0.011(4) 0.000(4) B4 0.078(6) 0.045(4) 0.060(5) 0.024(4) -0.014(4) 0.007(5) B5 0.057(6) 0.059(5) 0.044(4) -0.001(4) -0.021(4) -0.006(4) B6 0.048(5) 0.042(4) 0.048(4) 0.001(3) 0.000(4) -0.013(3) B7 0.064(6) 0.047(4) 0.071(6) -0.017(4) 0.002(4) 0.010(4) B8 0.066(6) 0.037(4) 0.111(7) -0.008(5) -0.012(5) 0.004(4) B9 0.046(6) 0.058(5) 0.090(6) 0.023(5) -0.016(4) 0.006(4) B10 0.054(5) 0.054(4) 0.060(5) 0.000(4) -0.013(4) -0.007(4) B11 0.050(5) 0.052(4) 0.047(4) 0.001(4) 0.007(4) -0.004(4) B12 0.054(6) 0.048(5) 0.076(6) -0.002(4) 0.003(4) 0.008(4) Rh2 0.0435(3) 0.0388(2) 0.0420(3) -0.0047(2) -0.0015(2) 0.0032(2) Fe2 0.0733(7) 0.0451(5) 0.0483(5) 0.0028(4) -0.0014(5) 0.0025(5) O4 0.134(6) 0.137(4) 0.079(4) 0.000(3) 0.050(3) 0.009(4) O5 0.149(6) 0.105(4) 0.091(4) 0.023(3) -0.063(4) -0.011(4) O6 0.184(5) 0.049(3) 0.094(3) 0.007(3) 0.018(4) 0.006(4) S3 0.0479(11) 0.0489(9) 0.0466(10) -0.0038(8) 0.0062(8) -0.0049(8) S4 0.0487(11) 0.0447(9) 0.0543(10) -0.0041(8) -0.0049(8) 0.0075(8) C21 0.051(4) 0.033(3) 0.040(4) 0.001(3) 0.004(3) -0.005(3) C22 0.045(4) 0.033(3) 0.050(4) -0.004(3) 0.002(3) 0.000(3) C23 0.100(7) 0.075(5) 0.051(5) -0.006(4) 0.011(4) 0.009(5) C24 0.110(7) 0.070(5) 0.058(5) 0.007(4) -0.014(5) 0.016(5) C25 0.096(6) 0.061(4) 0.060(4) 0.004(4) 0.006(4) -0.004(4) C26 0.050(4) 0.037(3) 0.046(4) -0.009(3) -0.002(4) 0.005(3) C27 0.054(4) 0.039(3) 0.038(3) -0.003(2) -0.004(3) 0.003(3) C28 0.057(5) 0.035(3) 0.043(4) -0.010(3) 0.001(4) 0.001(3) C29 0.050(5) 0.049(4) 0.043(4) -0.012(3) -0.010(3) 0.009(3) C30 0.057(5) 0.053(4) 0.038(4) -0.002(3) 0.004(3) 0.003(4) C31 0.042(4) 0.060(4) 0.067(5) -0.009(4) 0.000(4) 0.019(3) C32 0.069(5) 0.083(5) 0.092(5) -0.018(4) -0.017(4) 0.041(4) C33 0.054(5) 0.099(5) 0.071(5) -0.013(4) -0.024(4) 0.017(4) C34 0.041(5) 0.102(5) 0.125(6) 0.008(5) 0.011(4) -0.001(4) C35 0.046(4) 0.041(3) 0.054(4) -0.013(3) -0.001(3) 0.006(3) C36 0.060(5) 0.067(4) 0.103(5) -0.019(4) -0.010(4) -0.012(4) C37 0.054(5) 0.095(5) 0.083(5) -0.008(4) 0.024(4) -0.017(4) C38 0.045(4) 0.070(4) 0.129(6) -0.005(4) -0.006(4) 0.002(4) B13 0.066(5) 0.029(4) 0.062(5) -0.004(3) 0.001(4) 0.001(4) B14 0.069(6) 0.057(5) 0.045(4) -0.016(4) -0.002(4) -0.025(4) B15 0.046(5) 0.051(4) 0.049(5) 0.003(4) -0.010(4) -0.001(4) B16 0.037(4) 0.043(4) 0.047(4) 0.010(3) 0.004(4) -0.006(4) B17 0.061(6) 0.046(4) 0.060(5) -0.005(4) 0.011(4) 0.018(4) B18 0.097(7) 0.045(4) 0.053(4) -0.013(4) 0.006(5) 0.001(5) B19 0.083(7) 0.056(5) 0.042(4) -0.008(4) 0.004(4) -0.011(4) B20 0.065(6) 0.043(4) 0.041(4) 0.007(3) 0.013(4) -0.008(4) B21 0.055(5) 0.046(4) 0.052(5) 0.004(3) 0.019(4) -0.002(4) B22 0.080(7) 0.065(5) 0.048(5) -0.002(4) 0.017(4) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C10 2.166(5) . ? Rh1 C9 2.171(5) . ? Rh1 C6 2.198(5) . ? Rh1 C8 2.202(5) . ? Rh1 C7 2.204(4) . ? Rh1 S1 2.3481(16) . ? Rh1 S2 2.3523(15) . ? Rh1 Fe1 2.5128(14) . ? Fe1 C3 1.767(7) . ? Fe1 C4 1.780(7) . ? Fe1 C5 1.795(6) . ? Fe1 S2 2.2944(18) . ? Fe1 S1 2.3134(18) . ? S1 C1 1.824(6) . ? S2 C2 1.824(5) . ? O1 C3 1.140(7) . ? O2 C4 1.134(7) . ? O3 C5 1.145(6) . ? C1 C2 1.611(6) . ? C1 B5 1.725(8) . ? C1 B4 1.726(8) . ? C1 B3 1.729(7) . ? C1 B6 1.739(7) . ? C2 B11 1.703(8) . ? C2 B7 1.706(8) . ? C2 B3 1.741(7) . ? C2 B6 1.742(7) . ? C6 C7 1.421(6) . ? C6 C10 1.428(7) . ? C6 C11 1.516(6) . ? C7 C8 1.417(6) . ? C7 H7A 0.9800 . ? C8 C9 1.416(7) . ? C8 C15 1.521(7) . ? C9 C10 1.416(6) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 C13 1.529(7) . ? C11 C12 1.542(6) . ? C11 C14 1.545(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C18 1.518(7) . ? C15 C17 1.534(7) . ? C15 C16 1.551(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? B3 B8 1.719(9) . ? B3 B4 1.747(9) . ? B3 B7 1.756(9) . ? B3 H3 1.1000 . ? B4 B9 1.760(10) . ? B4 B8 1.773(9) . ? B4 B5 1.780(8) . ? B4 H4 1.1000 . ? B5 B6 1.743(8) . ? B5 B10 1.774(9) . ? B5 B9 1.781(9) . ? B5 H5 1.1000 . ? B6 B10 1.735(9) . ? B6 B11 1.747(8) . ? B6 H6 1.1000 . ? B7 B11 1.764(8) . ? B7 B8 1.767(9) . ? B7 B12 1.782(10) . ? B7 H7 1.1000 . ? B8 B9 1.757(9) . ? B8 B12 1.769(9) . ? B8 H8 1.1000 . ? B9 B10 1.755(8) . ? B9 B12 1.769(9) . ? B9 H9 1.1000 . ? B10 B12 1.770(8) . ? B10 B11 1.770(8) . ? B10 H10 1.1000 . ? B11 B12 1.776(9) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? Rh2 C29 2.154(5) . ? Rh2 C30 2.157(5) . ? Rh2 C28 2.205(5) . ? Rh2 C26 2.207(5) . ? Rh2 C27 2.216(5) . ? Rh2 S4 2.3501(16) . ? Rh2 S3 2.3603(16) . ? Rh2 Fe2 2.5133(14) . ? Fe2 C24 1.773(7) . ? Fe2 C23 1.785(7) . ? Fe2 C25 1.801(6) . ? Fe2 S3 2.3034(18) . ? Fe2 S4 2.3074(18) . ? O4 C23 1.135(7) . ? O5 C24 1.133(7) . ? O6 C25 1.142(5) . ? S3 C21 1.824(5) . ? S4 C22 1.814(5) . ? C21 C22 1.619(7) . ? C21 B15 1.694(7) . ? C21 B14 1.697(7) . ? C21 B16 1.724(7) . ? C21 B13 1.726(7) . ? C22 B21 1.702(7) . ? C22 B17 1.713(7) . ? C22 B16 1.732(7) . ? C22 B13 1.732(7) . ? C26 C30 1.424(6) . ? C26 C27 1.428(7) . ? C26 C31 1.521(7) . ? C27 C28 1.416(7) . ? C27 H27A 0.9800 . ? C28 C29 1.428(6) . ? C28 C35 1.521(7) . ? C29 C30 1.405(7) . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C31 C33 1.520(6) . ? C31 C34 1.532(7) . ? C31 C32 1.544(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C38 1.526(6) . ? C35 C37 1.546(6) . ? C35 C36 1.550(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? B13 B18 1.712(8) . ? B13 B17 1.752(9) . ? B13 B14 1.758(9) . ? B13 H13 1.1000 . ? B14 B15 1.757(8) . ? B14 B19 1.757(8) . ? B14 B18 1.770(10) . ? B14 H14 1.1000 . ? B15 B16 1.737(8) . ? B15 B19 1.770(8) . ? B15 B20 1.772(9) . ? B15 H15 1.1000 . ? B16 B20 1.733(7) . ? B16 B21 1.763(8) . ? B16 H16 1.1000 . ? B17 B18 1.773(9) . ? B17 B22 1.786(9) . ? B17 B21 1.786(8) . ? B17 H17 1.1000 . ? B18 B22 1.761(9) . ? B18 B19 1.764(9) . ? B18 H18 1.1000 . ? B19 B20 1.763(8) . ? B19 B22 1.764(9) . ? B19 H19 1.1000 . ? B20 B22 1.753(9) . ? B20 B21 1.771(9) . ? B20 H20 1.1000 . ? B21 B22 1.786(9) . ? B21 H21 1.1000 . ? B22 H22 1.1000 . ? 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 C10 Rh1 C9 38.11(16) . . ? C10 Rh1 C6 38.19(18) . . ? C9 Rh1 C6 63.5(2) . . ? C10 Rh1 C8 63.6(2) . . ? C9 Rh1 C8 37.77(18) . . ? C6 Rh1 C8 63.35(17) . . ? C10 Rh1 C7 63.23(19) . . ? C9 Rh1 C7 62.82(19) . . ? C6 Rh1 C7 37.66(16) . . ? C8 Rh1 C7 37.51(16) . . ? C10 Rh1 S1 117.16(15) . . ? C9 Rh1 S1 151.09(17) . . ? C6 Rh1 S1 107.03(14) . . ? C8 Rh1 S1 164.63(17) . . ? C7 Rh1 S1 127.64(14) . . ? C10 Rh1 S2 154.68(16) . . ? C9 Rh1 S2 119.79(15) . . ? C6 Rh1 S2 160.91(16) . . ? C8 Rh1 S2 106.78(14) . . ? C7 Rh1 S2 124.62(14) . . ? S1 Rh1 S2 78.60(6) . . ? C10 Rh1 Fe1 113.96(15) . . ? C9 Rh1 Fe1 112.61(16) . . ? C6 Rh1 Fe1 142.25(15) . . ? C8 Rh1 Fe1 138.30(16) . . ? C7 Rh1 Fe1 175.35(14) . . ? S1 Rh1 Fe1 56.72(5) . . ? S2 Rh1 Fe1 56.16(5) . . ? C3 Fe1 C4 88.2(3) . . ? C3 Fe1 C5 96.5(3) . . ? C4 Fe1 C5 98.5(3) . . ? C3 Fe1 S2 156.8(2) . . ? C4 Fe1 S2 90.0(2) . . ? C5 Fe1 S2 106.6(2) . . ? C3 Fe1 S1 88.7(2) . . ? C4 Fe1 S1 147.5(2) . . ? C5 Fe1 S1 113.9(2) . . ? S2 Fe1 S1 80.49(6) . . ? C3 Fe1 Rh1 98.5(2) . . ? C4 Fe1 Rh1 90.5(2) . . ? C5 Fe1 Rh1 162.7(2) . . ? S2 Fe1 Rh1 58.38(4) . . ? S1 Fe1 Rh1 58.05(4) . . ? C1 S1 Fe1 105.90(18) . . ? C1 S1 Rh1 104.70(17) . . ? Fe1 S1 Rh1 65.24(5) . . ? C2 S2 Fe1 105.97(18) . . ? C2 S2 Rh1 105.41(16) . . ? Fe1 S2 Rh1 65.46(5) . . ? C2 C1 B5 111.1(4) . . ? C2 C1 B4 111.2(4) . . ? B5 C1 B4 62.1(4) . . ? C2 C1 B3 62.7(3) . . ? B5 C1 B3 112.3(4) . . ? B4 C1 B3 60.7(3) . . ? C2 C1 B6 62.5(3) . . ? B5 C1 B6 60.4(3) . . ? B4 C1 B6 111.8(5) . . ? B3 C1 B6 114.3(4) . . ? C2 C1 S1 112.2(4) . . ? B5 C1 S1 125.2(4) . . ? B4 C1 S1 126.1(4) . . ? B3 C1 S1 116.6(4) . . ? B6 C1 S1 115.7(4) . . ? C1 C2 B11 111.4(4) . . ? C1 C2 B7 111.7(4) . . ? B11 C2 B7 62.3(4) . . ? C1 C2 B3 62.0(3) . . ? B11 C2 B3 112.3(4) . . ? B7 C2 B3 61.3(3) . . ? C1 C2 B6 62.4(3) . . ? B11 C2 B6 60.9(3) . . ? B7 C2 B6 112.7(5) . . ? B3 C2 B6 113.6(4) . . ? C1 C2 S2 111.7(4) . . ? B11 C2 S2 124.3(4) . . ? B7 C2 S2 126.9(4) . . ? B3 C2 S2 118.3(4) . . ? B6 C2 S2 113.8(3) . . ? O1 C3 Fe1 178.9(7) . . ? O2 C4 Fe1 178.3(7) . . ? O3 C5 Fe1 176.4(6) . . ? C7 C6 C10 107.1(5) . . ? C7 C6 C11 127.4(5) . . ? C10 C6 C11 125.1(5) . . ? C7 C6 Rh1 71.4(3) . . ? C10 C6 Rh1 69.7(3) . . ? C11 C6 Rh1 130.0(3) . . ? C8 C7 C6 109.0(5) . . ? C8 C7 Rh1 71.2(3) . . ? C6 C7 Rh1 70.9(3) . . ? C8 C7 H7A 125.5 . . ? C6 C7 H7A 125.5 . . ? Rh1 C7 H7A 125.5 . . ? C9 C8 C7 107.2(5) . . ? C9 C8 C15 125.9(6) . . ? C7 C8 C15 126.5(6) . . ? C9 C8 Rh1 69.9(3) . . ? C7 C8 Rh1 71.3(3) . . ? C15 C8 Rh1 129.0(3) . . ? C8 C9 C10 108.8(5) . . ? C8 C9 Rh1 72.3(3) . . ? C10 C9 Rh1 70.7(3) . . ? C8 C9 H9A 125.6 . . ? C10 C9 H9A 125.6 . . ? Rh1 C9 H9A 125.6 . . ? C9 C10 C6 107.9(5) . . ? C9 C10 Rh1 71.1(3) . . ? C6 C10 Rh1 72.1(3) . . ? C9 C10 H10A 126.0 . . ? C6 C10 H10A 126.0 . . ? Rh1 C10 H10A 126.0 . . ? C6 C11 C13 110.7(5) . . ? C6 C11 C12 107.0(4) . . ? C13 C11 C12 109.7(5) . . ? C6 C11 C14 111.8(5) . . ? C13 C11 C14 108.7(5) . . ? C12 C11 C14 108.8(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C8 111.6(5) . . ? C18 C15 C17 111.0(5) . . ? C8 C15 C17 110.6(5) . . ? C18 C15 C16 108.9(5) . . ? C8 C15 C16 105.7(4) . . ? C17 C15 C16 109.0(5) . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? B8 B3 C1 106.5(4) . . ? B8 B3 C2 105.4(5) . . ? C1 B3 C2 55.3(3) . . ? B8 B3 B4 61.5(4) . . ? C1 B3 B4 59.5(3) . . ? C2 B3 B4 104.3(4) . . ? B8 B3 B7 61.1(4) . . ? C1 B3 B7 103.9(4) . . ? C2 B3 B7 58.4(3) . . ? B4 B3 B7 109.7(5) . . ? B8 B3 H3 121.3 . . ? C1 B3 H3 124.9 . . ? C2 B3 H3 125.6 . . ? B4 B3 H3 121.0 . . ? B7 B3 H3 121.8 . . ? C1 B4 B3 59.7(3) . . ? C1 B4 B9 104.9(4) . . ? B3 B4 B9 106.9(5) . . ? C1 B4 B8 104.2(4) . . ? B3 B4 B8 58.4(4) . . ? B9 B4 B8 59.6(4) . . ? C1 B4 B5 58.9(3) . . ? B3 B4 B5 108.8(4) . . ? B9 B4 B5 60.4(4) . . ? B8 B4 B5 108.0(5) . . ? C1 B4 H4 124.4 . . ? B3 B4 H4 121.7 . . ? B9 B4 H4 122.7 . . ? B8 B4 H4 123.2 . . ? B5 B4 H4 120.8 . . ? C1 B5 B6 60.2(3) . . ? C1 B5 B10 104.8(4) . . ? B6 B5 B10 59.1(3) . . ? C1 B5 B4 59.0(3) . . ? B6 B5 B4 109.1(4) . . ? B10 B5 B4 107.2(5) . . ? C1 B5 B9 104.0(4) . . ? B6 B5 B9 106.8(5) . . ? B10 B5 B9 59.2(4) . . ? B4 B5 B9 59.3(4) . . ? C1 B5 H5 124.2 . . ? B6 B5 H5 121.1 . . ? B10 B5 H5 123.2 . . ? B4 B5 H5 121.4 . . ? B9 B5 H5 123.6 . . ? B10 B6 C1 105.8(4) . . ? B10 B6 C2 105.4(4) . . ? C1 B6 C2 55.1(3) . . ? B10 B6 B5 61.3(4) . . ? C1 B6 B5 59.4(3) . . ? C2 B6 B5 104.2(4) . . ? B10 B6 B11 61.1(4) . . ? C1 B6 B11 103.4(4) . . ? C2 B6 B11 58.4(3) . . ? B5 B6 B11 109.5(5) . . ? B10 B6 H6 121.5 . . ? C1 B6 H6 125.3 . . ? C2 B6 H6 125.5 . . ? B5 B6 H6 121.1 . . ? B11 B6 H6 121.9 . . ? C2 B7 B3 60.3(3) . . ? C2 B7 B11 58.8(3) . . ? B3 B7 B11 108.7(4) . . ? C2 B7 B8 104.8(5) . . ? B3 B7 B8 58.4(4) . . ? B11 B7 B8 107.5(5) . . ? C2 B7 B12 105.3(4) . . ? B3 B7 B12 107.2(5) . . ? B11 B7 B12 60.1(4) . . ? B8 B7 B12 59.8(4) . . ? C2 B7 H7 123.8 . . ? B3 B7 H7 121.5 . . ? B11 B7 H7 121.3 . . ? B8 B7 H7 123.2 . . ? B12 B7 H7 122.5 . . ? B3 B8 B9 108.3(5) . . ? B3 B8 B7 60.5(4) . . ? B9 B8 B7 108.1(4) . . ? B3 B8 B12 109.5(5) . . ? B9 B8 B12 60.2(4) . . ? B7 B8 B12 60.5(4) . . ? B3 B8 B4 60.0(4) . . ? B9 B8 B4 59.8(4) . . ? B7 B8 B4 108.0(4) . . ? B12 B8 B4 108.5(4) . . ? B3 B8 H8 121.0 . . ? B9 B8 H8 121.8 . . ? B7 B8 H8 121.6 . . ? B12 B8 H8 120.9 . . ? B4 B8 H8 121.9 . . ? B10 B9 B8 108.5(5) . . ? B10 B9 B4 108.9(5) . . ? B8 B9 B4 60.5(4) . . ? B10 B9 B12 60.3(4) . . ? B8 B9 B12 60.2(4) . . ? B4 B9 B12 109.1(5) . . ? B10 B9 B5 60.2(4) . . ? B8 B9 B5 108.7(5) . . ? B4 B9 B5 60.3(4) . . ? B12 B9 B5 108.7(5) . . ? B10 B9 H9 121.4 . . ? B8 B9 H9 121.4 . . ? B4 B9 H9 121.0 . . ? B12 B9 H9 121.2 . . ? B5 B9 H9 121.4 . . ? B6 B10 B9 108.3(5) . . ? B6 B10 B12 109.0(5) . . ? B9 B10 B12 60.2(3) . . ? B6 B10 B11 59.8(4) . . ? B9 B10 B11 107.6(4) . . ? B12 B10 B11 60.2(3) . . ? B6 B10 B5 59.6(4) . . ? B9 B10 B5 60.6(4) . . ? B12 B10 B5 109.0(5) . . ? B11 B10 B5 107.1(5) . . ? B6 B10 H10 121.5 . . ? B9 B10 H10 121.6 . . ? B12 B10 H10 120.8 . . ? B11 B10 H10 122.4 . . ? B5 B10 H10 121.7 . . ? C2 B11 B6 60.6(3) . . ? C2 B11 B7 58.9(3) . . ? B6 B11 B7 109.6(5) . . ? C2 B11 B10 105.5(4) . . ? B6 B11 B10 59.1(3) . . ? B7 B11 B10 108.3(5) . . ? C2 B11 B12 105.8(4) . . ? B6 B11 B12 108.1(5) . . ? B7 B11 B12 60.5(4) . . ? B10 B11 B12 59.9(4) . . ? C2 B11 H11 123.6 . . ? B6 B11 H11 120.8 . . ? B7 B11 H11 120.8 . . ? B10 B11 H11 122.7 . . ? B12 B11 H11 122.2 . . ? B8 B12 B9 59.6(4) . . ? B8 B12 B10 107.3(5) . . ? B9 B12 B10 59.5(4) . . ? B8 B12 B11 106.9(5) . . ? B9 B12 B11 106.7(5) . . ? B10 B12 B11 59.9(3) . . ? B8 B12 B7 59.7(4) . . ? B9 B12 B7 106.9(5) . . ? B10 B12 B7 107.5(5) . . ? B11 B12 B7 59.4(4) . . ? B8 B12 H12 122.2 . . ? B9 B12 H12 122.6 . . ? B10 B12 H12 121.9 . . ? B11 B12 H12 122.5 . . ? B7 B12 H12 122.2 . . ? C29 Rh2 C30 38.05(17) . . ? C29 Rh2 C28 38.22(17) . . ? C30 Rh2 C28 63.6(2) . . ? C29 Rh2 C26 63.8(2) . . ? C30 Rh2 C26 38.08(17) . . ? C28 Rh2 C26 63.6(2) . . ? C29 Rh2 C27 62.87(18) . . ? C30 Rh2 C27 62.78(18) . . ? C28 Rh2 C27 37.37(17) . . ? C26 Rh2 C27 37.67(17) . . ? C29 Rh2 S4 116.29(16) . . ? C30 Rh2 S4 150.22(16) . . ? C28 Rh2 S4 106.17(15) . . ? C26 Rh2 S4 164.49(16) . . ? C27 Rh2 S4 127.25(15) . . ? C29 Rh2 S3 153.73(17) . . ? C30 Rh2 S3 119.28(16) . . ? C28 Rh2 S3 162.11(16) . . ? C26 Rh2 S3 106.86(15) . . ? C27 Rh2 S3 125.97(15) . . ? S4 Rh2 S3 79.47(6) . . ? C29 Rh2 Fe2 113.05(15) . . ? C30 Rh2 Fe2 112.32(15) . . ? C28 Rh2 Fe2 140.98(16) . . ? C26 Rh2 Fe2 138.80(15) . . ? C27 Rh2 Fe2 175.06(13) . . ? S4 Rh2 Fe2 56.52(5) . . ? S3 Rh2 Fe2 56.30(5) . . ? C24 Fe2 C23 91.9(3) . . ? C24 Fe2 C25 97.5(3) . . ? C23 Fe2 C25 91.8(3) . . ? C24 Fe2 S3 148.5(2) . . ? C23 Fe2 S3 87.8(2) . . ? C25 Fe2 S3 114.0(2) . . ? C24 Fe2 S4 87.5(2) . . ? C23 Fe2 S4 158.2(2) . . ? C25 Fe2 S4 109.9(2) . . ? S3 Fe2 S4 81.54(6) . . ? C24 Fe2 Rh2 90.7(2) . . ? C23 Fe2 Rh2 100.0(2) . . ? C25 Fe2 Rh2 165.36(18) . . ? S3 Fe2 Rh2 58.49(4) . . ? S4 Fe2 Rh2 58.17(4) . . ? C21 S3 Fe2 105.31(18) . . ? C21 S3 Rh2 103.92(17) . . ? Fe2 S3 Rh2 65.21(5) . . ? C22 S4 Fe2 105.31(18) . . ? C22 S4 Rh2 103.65(18) . . ? Fe2 S4 Rh2 65.31(5) . . ? C22 C21 B15 111.4(4) . . ? C22 C21 B14 111.9(4) . . ? B15 C21 B14 62.4(3) . . ? C22 C21 B16 62.3(3) . . ? B15 C21 B16 61.1(3) . . ? B14 C21 B16 113.0(4) . . ? C22 C21 B13 62.3(3) . . ? B15 C21 B13 113.2(4) . . ? B14 C21 B13 61.8(3) . . ? B16 C21 B13 114.4(4) . . ? C22 C21 S3 112.0(4) . . ? B15 C21 S3 124.2(4) . . ? B14 C21 S3 126.3(4) . . ? B16 C21 S3 114.0(3) . . ? B13 C21 S3 117.2(3) . . ? C21 C22 B21 111.6(4) . . ? C21 C22 B17 111.4(4) . . ? B21 C22 B17 63.1(3) . . ? C21 C22 B16 61.8(3) . . ? B21 C22 B16 61.8(3) . . ? B17 C22 B16 113.8(4) . . ? C21 C22 B13 61.9(3) . . ? B21 C22 B13 113.1(4) . . ? B17 C22 B13 61.1(3) . . ? B16 C22 B13 113.7(4) . . ? C21 C22 S4 113.0(4) . . ? B21 C22 S4 124.1(4) . . ? B17 C22 S4 124.7(4) . . ? B16 C22 S4 115.4(3) . . ? B13 C22 S4 116.7(3) . . ? O4 C23 Fe2 179.3(7) . . ? O5 C24 Fe2 178.9(7) . . ? O6 C25 Fe2 174.1(5) . . ? C30 C26 C27 106.0(5) . . ? C30 C26 C31 127.1(6) . . ? C27 C26 C31 126.6(5) . . ? C30 C26 Rh2 69.0(3) . . ? C27 C26 Rh2 71.5(3) . . ? C31 C26 Rh2 128.8(4) . . ? C28 C27 C26 109.7(5) . . ? C28 C27 Rh2 70.9(3) . . ? C26 C27 Rh2 70.8(3) . . ? C28 C27 H27A 125.1 . . ? C26 C27 H27A 125.1 . . ? Rh2 C27 H27A 125.1 . . ? C27 C28 C29 106.6(5) . . ? C27 C28 C35 127.5(5) . . ? C29 C28 C35 125.6(6) . . ? C27 C28 Rh2 71.7(3) . . ? C29 C28 Rh2 69.0(3) . . ? C35 C28 Rh2 128.9(3) . . ? C30 C29 C28 108.5(5) . . ? C30 C29 Rh2 71.1(3) . . ? C28 C29 Rh2 72.8(3) . . ? C30 C29 H29A 125.6 . . ? C28 C29 H29A 125.7 . . ? Rh2 C29 H29A 125.6 . . ? C29 C30 C26 109.2(5) . . ? C29 C30 Rh2 70.9(3) . . ? C26 C30 Rh2 72.9(3) . . ? C29 C30 H30A 125.4 . . ? C26 C30 H30A 125.4 . . ? Rh2 C30 H30A 125.4 . . ? C33 C31 C26 111.8(5) . . ? C33 C31 C34 110.0(5) . . ? C26 C31 C34 112.0(5) . . ? C33 C31 C32 108.2(5) . . ? C26 C31 C32 105.7(5) . . ? C34 C31 C32 109.0(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C28 C35 C38 112.8(5) . . ? C28 C35 C37 110.7(5) . . ? C38 C35 C37 109.2(5) . . ? C28 C35 C36 106.8(4) . . ? C38 C35 C36 108.4(5) . . ? C37 C35 C36 108.9(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? B18 B13 C21 105.5(4) . . ? B18 B13 C22 105.6(4) . . ? C21 B13 C22 55.8(3) . . ? B18 B13 B17 61.6(4) . . ? C21 B13 B17 104.7(4) . . ? C22 B13 B17 58.9(3) . . ? B18 B13 B14 61.3(4) . . ? C21 B13 B14 58.3(3) . . ? C22 B13 B14 103.9(4) . . ? B17 B13 B14 110.2(5) . . ? B18 B13 H13 121.5 . . ? C21 B13 H13 125.3 . . ? C22 B13 H13 125.3 . . ? B17 B13 H13 120.9 . . ? B14 B13 H13 121.5 . . ? C21 B14 B15 58.7(3) . . ? C21 B14 B19 105.0(4) . . ? B15 B14 B19 60.5(3) . . ? C21 B14 B13 59.9(3) . . ? B15 B14 B13 108.7(5) . . ? B19 B14 B13 107.0(5) . . ? C21 B14 B18 104.2(5) . . ? B15 B14 B18 108.1(5) . . ? B19 B14 B18 60.0(4) . . ? B13 B14 B18 58.1(4) . . ? C21 B14 H14 124.3 . . ? B15 B14 H14 120.9 . . ? B19 B14 H14 122.4 . . ? B13 B14 H14 121.8 . . ? B18 B14 H14 123.2 . . ? C21 B15 B16 60.3(3) . . ? C21 B15 B14 58.9(3) . . ? B16 B15 B14 109.5(5) . . ? C21 B15 B19 104.6(4) . . ? B16 B15 B19 107.8(5) . . ? B14 B15 B19 59.8(3) . . ? C21 B15 B20 104.8(5) . . ? B16 B15 B20 59.2(3) . . ? B14 B15 B20 107.7(5) . . ? B19 B15 B20 59.7(4) . . ? C21 B15 H15 124.2 . . ? B16 B15 H15 120.7 . . ? B14 B15 H15 121.1 . . ? B19 B15 H15 122.8 . . ? B20 B15 H15 123.0 . . ? C21 B16 C22 55.9(3) . . ? C21 B16 B20 105.2(4) . . ? C22 B16 B20 104.8(4) . . ? C21 B16 B15 58.6(3) . . ? C22 B16 B15 104.2(4) . . ? B20 B16 B15 61.4(4) . . ? C21 B16 B21 103.9(4) . . ? C22 B16 B21 58.3(3) . . ? B20 B16 B21 60.9(4) . . ? B15 B16 B21 109.7(4) . . ? C21 B16 H16 125.3 . . ? C22 B16 H16 125.5 . . ? B20 B16 H16 122.0 . . ? B15 B16 H16 121.2 . . ? B21 B16 H16 121.7 . . ? C22 B17 B13 60.0(3) . . ? C22 B17 B18 103.8(5) . . ? B13 B17 B18 58.1(4) . . ? C22 B17 B22 103.8(4) . . ? B13 B17 B22 106.1(5) . . ? B18 B17 B22 59.3(4) . . ? C22 B17 B21 58.2(3) . . ? B13 B17 B21 108.2(4) . . ? B18 B17 B21 107.3(5) . . ? B22 B17 B21 60.0(3) . . ? C22 B17 H17 124.8 . . ? B13 B17 H17 121.9 . . ? B18 B17 H17 123.5 . . ? B22 B17 H17 123.3 . . ? B21 B17 H17 121.4 . . ? B13 B18 B22 109.0(5) . . ? B13 B18 B19 108.8(5) . . ? B22 B18 B19 60.1(4) . . ? B13 B18 B14 60.6(4) . . ? B22 B18 B14 107.9(5) . . ? B19 B18 B14 59.7(4) . . ? B13 B18 B17 60.3(4) . . ? B22 B18 B17 60.7(4) . . ? B19 B18 B17 108.9(5) . . ? B14 B18 B17 108.6(4) . . ? B13 B18 H18 121.0 . . ? B22 B18 H18 121.4 . . ? B19 B18 H18 121.5 . . ? B14 B18 H18 121.8 . . ? B17 B18 H18 121.1 . . ? B14 B19 B20 108.1(4) . . ? B14 B19 B18 60.3(4) . . ? B20 B19 B18 107.5(5) . . ? B14 B19 B22 108.3(5) . . ? B20 B19 B22 59.6(4) . . ? B18 B19 B22 59.9(4) . . ? B14 B19 B15 59.7(4) . . ? B20 B19 B15 60.2(3) . . ? B18 B19 B15 107.7(4) . . ? B22 B19 B15 107.8(5) . . ? B14 B19 H19 121.5 . . ? B20 B19 H19 121.9 . . ? B18 B19 H19 121.9 . . ? B22 B19 H19 121.8 . . ? B15 B19 H19 121.9 . . ? B16 B20 B22 109.2(4) . . ? B16 B20 B19 108.3(4) . . ? B22 B20 B19 60.2(4) . . ? B16 B20 B21 60.4(3) . . ? B22 B20 B21 60.9(4) . . ? B19 B20 B21 108.9(4) . . ? B16 B20 B15 59.4(3) . . ? B22 B20 B15 108.2(4) . . ? B19 B20 B15 60.1(3) . . ? B21 B20 B15 107.8(4) . . ? B16 B20 H20 121.4 . . ? B22 B20 H20 120.9 . . ? B19 B20 H20 121.4 . . ? B21 B20 H20 121.2 . . ? B15 B20 H20 122.2 . . ? C22 B21 B16 59.9(3) . . ? C22 B21 B20 104.4(5) . . ? B16 B21 B20 58.7(3) . . ? C22 B21 B22 104.2(4) . . ? B16 B21 B22 106.4(5) . . ? B20 B21 B22 59.0(4) . . ? C22 B21 B17 58.8(3) . . ? B16 B21 B17 108.8(4) . . ? B20 B21 B17 107.5(5) . . ? B22 B21 B17 60.0(3) . . ? C22 B21 H21 124.3 . . ? B16 B21 H21 121.6 . . ? B20 B21 H21 123.3 . . ? B22 B21 H21 123.4 . . ? B17 B21 H21 121.1 . . ? B20 B22 B18 108.1(5) . . ? B20 B22 B19 60.2(4) . . ? B18 B22 B19 60.1(4) . . ? B20 B22 B17 108.3(4) . . ? B18 B22 B17 60.0(4) . . ? B19 B22 B17 108.3(5) . . ? B20 B22 B21 60.1(3) . . ? B18 B22 B21 107.8(4) . . ? B19 B22 B21 108.2(5) . . ? B17 B22 B21 60.0(3) . . ? B20 B22 H22 121.5 . . ? B18 B22 H22 121.8 . . ? B19 B22 H22 121.5 . . ? B17 B22 H22 121.5 . . ? B21 B22 H22 121.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.711 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.067 # Attachment '7a.cif' data_f51214b _database_code_depnum_ccdc_archive 'CCDC 608153' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 B10 Co Fe O3 S2' _chemical_formula_weight 540.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.965(7) _cell_length_b 14.114(5) _cell_length_c 19.098(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4843(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 920 _cell_measurement_theta_min 2.267 _cell_measurement_theta_max 21.248 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8667 _exptl_absorpt_correction_T_max 0.9300 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 7.32 _diffrn_reflns_number 19294 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4265 _reflns_number_gt 2171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4265 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.779 _refine_ls_restrained_S_all 0.779 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.09773(3) 0.74925(4) 0.34722(2) 0.03648(14) Uani 1 1 d . . . Fe1 Fe 0.00148(3) 0.75687(4) 0.43589(3) 0.04363(16) Uani 1 1 d . . . O1 O -0.02895(19) 0.9601(2) 0.41992(19) 0.0868(12) Uani 1 1 d . . . O2 O -0.12208(18) 0.7027(2) 0.34526(17) 0.0785(11) Uani 1 1 d . . . O3 O -0.07802(16) 0.7386(3) 0.57091(17) 0.0857(11) Uani 1 1 d . . . S1 S 0.12316(6) 0.79803(7) 0.45607(5) 0.0386(3) Uani 1 1 d . . . S2 S 0.05866(6) 0.61823(7) 0.40020(5) 0.0416(3) Uani 1 1 d . . . C1 C 0.1650(2) 0.6929(3) 0.49692(19) 0.0371(10) Uani 1 1 d . . . C2 C 0.1301(2) 0.5957(2) 0.46523(18) 0.0373(10) Uani 1 1 d . . . C3 C -0.0185(2) 0.8808(4) 0.4268(2) 0.0599(13) Uani 1 1 d . . . C4 C -0.0749(2) 0.7244(3) 0.3809(2) 0.0553(13) Uani 1 1 d . . . C5 C -0.0454(2) 0.7431(3) 0.5196(2) 0.0585(12) Uani 1 1 d . . . C6 C 0.1265(2) 0.8624(3) 0.28560(19) 0.0411(11) Uani 1 1 d . . . C7 C 0.0588(2) 0.8223(3) 0.2592(2) 0.0419(11) Uani 1 1 d . . . C8 C 0.0738(2) 0.7256(2) 0.2436(2) 0.0445(12) Uani 1 1 d . . . C9 C 0.1521(3) 0.7078(3) 0.2561(2) 0.0462(12) Uani 1 1 d . . . C10 C 0.1842(2) 0.7917(3) 0.2813(2) 0.0441(11) Uani 1 1 d . . . C11 C 0.1376(2) 0.9634(2) 0.3090(2) 0.0583(13) Uani 1 1 d . . . H11A H 0.1507 1.0019 0.2694 0.087 Uiso 1 1 calc R . . H11B H 0.1768 0.9660 0.3431 0.087 Uiso 1 1 calc R . . H11C H 0.0924 0.9868 0.3294 0.087 Uiso 1 1 calc R . . C12 C -0.0120(2) 0.8753(3) 0.2446(2) 0.0614(13) Uani 1 1 d . . . H12A H -0.0109 0.8997 0.1977 0.092 Uiso 1 1 calc R . . H12B H -0.0167 0.9269 0.2771 0.092 Uiso 1 1 calc R . . H12C H -0.0536 0.8333 0.2498 0.092 Uiso 1 1 calc R . . C13 C 0.0202(3) 0.6559(3) 0.2117(2) 0.0734(16) Uani 1 1 d . . . H13A H 0.0212 0.6619 0.1616 0.110 Uiso 1 1 calc R . . H13B H -0.0291 0.6687 0.2285 0.110 Uiso 1 1 calc R . . H13C H 0.0344 0.5927 0.2247 0.110 Uiso 1 1 calc R . . C14 C 0.1908(3) 0.6152(3) 0.2402(2) 0.0700(14) Uani 1 1 d . . . H14A H 0.2104 0.6169 0.1934 0.105 Uiso 1 1 calc R . . H14B H 0.1558 0.5640 0.2442 0.105 Uiso 1 1 calc R . . H14C H 0.2307 0.6057 0.2728 0.105 Uiso 1 1 calc R . . C15 C 0.2653(2) 0.8086(3) 0.2967(2) 0.0654(14) Uani 1 1 d . . . H15A H 0.2903 0.8275 0.2546 0.098 Uiso 1 1 calc R . . H15B H 0.2873 0.7513 0.3142 0.098 Uiso 1 1 calc R . . H15C H 0.2700 0.8576 0.3312 0.098 Uiso 1 1 calc R . . B3 B 0.1091(3) 0.6252(3) 0.5511(2) 0.0465(13) Uani 1 1 d . . . H3 H 0.0536 0.6455 0.5702 0.056 Uiso 1 1 calc R . . B4 B 0.1898(3) 0.6809(4) 0.5823(2) 0.0511(14) Uani 1 1 d . . . H4 H 0.1867 0.7380 0.6214 0.061 Uiso 1 1 calc R . . B5 B 0.2575(3) 0.6831(3) 0.5147(2) 0.0444(13) Uani 1 1 d . . . H5 H 0.2979 0.7414 0.5105 0.053 Uiso 1 1 calc R . . B6 B 0.2197(2) 0.6286(3) 0.4404(2) 0.0404(12) Uani 1 1 d . . . H6 H 0.2359 0.6510 0.3873 0.049 Uiso 1 1 calc R . . B7 B 0.1306(3) 0.5074(3) 0.5267(2) 0.0511(14) Uani 1 1 d . . . H7 H 0.0888 0.4507 0.5294 0.061 Uiso 1 1 calc R . . B8 B 0.1706(3) 0.5600(3) 0.6016(3) 0.0562(15) Uani 1 1 d . . . H8 H 0.1554 0.5368 0.6547 0.067 Uiso 1 1 calc R . . B9 B 0.2625(3) 0.5953(3) 0.5815(2) 0.0519(15) Uani 1 1 d . . . H9 H 0.3069 0.5954 0.6211 0.062 Uiso 1 1 calc R . . B10 B 0.2796(3) 0.5638(3) 0.4927(2) 0.0497(14) Uani 1 1 d . . . H10 H 0.3354 0.5434 0.4745 0.060 Uiso 1 1 calc R . . B11 B 0.1975(3) 0.5098(3) 0.4593(3) 0.0456(13) Uani 1 1 d . . . H11 H 0.1985 0.4547 0.4186 0.055 Uiso 1 1 calc R . . B12 B 0.2257(3) 0.4878(4) 0.5465(3) 0.0554(16) Uani 1 1 d . . . H12 H 0.2464 0.4180 0.5632 0.067 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 Co1 0.0402(3) 0.0375(3) 0.0317(3) 0.0010(3) 0.0004(2) -0.0029(3) Fe1 0.0369(3) 0.0478(4) 0.0462(3) 0.0008(4) 0.0034(3) 0.0003(4) O1 0.089(3) 0.052(2) 0.119(3) 0.007(2) 0.011(2) 0.017(2) O2 0.057(2) 0.098(3) 0.081(3) 0.001(2) -0.023(2) -0.003(2) O3 0.054(2) 0.144(3) 0.060(2) 0.004(3) 0.0137(16) 0.013(2) S1 0.0428(6) 0.0346(5) 0.0383(6) -0.0014(5) 0.0008(5) -0.0014(5) S2 0.0420(6) 0.0392(6) 0.0437(7) -0.0004(6) -0.0009(6) -0.0075(5) C1 0.043(3) 0.037(2) 0.032(2) -0.003(2) 0.001(2) -0.002(2) C2 0.044(3) 0.036(2) 0.032(2) -0.0049(19) 0.005(2) -0.003(2) C3 0.045(3) 0.073(3) 0.062(3) 0.000(3) 0.004(2) 0.000(3) C4 0.049(3) 0.059(3) 0.058(3) 0.008(2) 0.008(2) 0.003(2) C5 0.040(3) 0.074(3) 0.061(3) 0.004(3) 0.000(2) 0.002(3) C6 0.057(3) 0.036(3) 0.030(2) 0.0034(19) 0.000(2) -0.007(2) C7 0.052(3) 0.039(3) 0.034(3) 0.009(2) -0.006(2) -0.001(2) C8 0.071(3) 0.033(3) 0.030(2) 0.0026(19) -0.003(2) -0.004(2) C9 0.064(3) 0.047(3) 0.028(3) 0.003(2) 0.009(2) 0.006(3) C10 0.050(3) 0.054(3) 0.028(3) 0.007(2) 0.008(2) 0.000(3) C11 0.075(4) 0.047(3) 0.053(3) 0.002(2) -0.001(3) -0.017(2) C12 0.068(4) 0.051(3) 0.065(3) 0.008(2) -0.017(3) 0.002(3) C13 0.102(4) 0.050(3) 0.068(3) -0.005(3) -0.030(3) -0.011(3) C14 0.102(4) 0.063(3) 0.045(3) -0.004(3) 0.009(3) 0.030(3) C15 0.049(3) 0.083(3) 0.064(3) 0.005(3) 0.008(2) -0.009(3) B3 0.055(4) 0.050(3) 0.035(3) 0.003(3) 0.017(3) -0.003(3) B4 0.063(4) 0.055(3) 0.035(3) -0.003(3) 0.001(3) 0.007(3) B5 0.036(3) 0.052(3) 0.045(3) -0.005(3) -0.004(3) -0.003(3) B6 0.038(3) 0.046(3) 0.037(3) -0.004(3) 0.007(2) 0.001(2) B7 0.065(4) 0.035(3) 0.053(4) 0.010(3) 0.011(3) -0.003(3) B8 0.079(4) 0.053(3) 0.036(3) 0.011(3) 0.004(3) 0.010(3) B9 0.058(4) 0.052(3) 0.045(4) 0.002(3) -0.006(3) 0.008(3) B10 0.046(3) 0.059(3) 0.044(3) -0.002(3) 0.000(3) 0.012(3) B11 0.059(4) 0.033(3) 0.044(3) -0.004(3) 0.001(3) 0.009(3) B12 0.067(4) 0.050(3) 0.049(4) 0.011(3) 0.001(3) 0.016(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 Co1 C6 2.051(4) . ? Co1 C8 2.053(4) . ? Co1 C9 2.080(4) . ? Co1 C10 2.087(4) . ? Co1 C7 2.093(4) . ? Co1 S2 2.2217(13) . ? Co1 S1 2.2371(13) . ? Co1 Fe1 2.4227(10) . ? Fe1 C4 1.788(5) . ? Fe1 C3 1.794(5) . ? Fe1 C5 1.817(5) . ? Fe1 S1 2.2946(14) . ? Fe1 S2 2.3128(13) . ? O1 C3 1.142(5) . ? O2 C4 1.129(5) . ? O3 C5 1.144(4) . ? S1 C1 1.837(4) . ? S2 C2 1.815(4) . ? C1 C2 1.626(5) . ? C1 B4 1.699(6) . ? C1 B5 1.702(5) . ? C1 B6 1.720(5) . ? C1 B3 1.729(5) . ? C2 B7 1.711(5) . ? C2 B11 1.716(5) . ? C2 B3 1.734(5) . ? C2 B6 1.741(5) . ? C6 C7 1.434(5) . ? C6 C10 1.442(5) . ? C6 C11 1.507(5) . ? C7 C8 1.423(5) . ? C7 C12 1.502(5) . ? C8 C9 1.448(5) . ? C8 C13 1.505(5) . ? C9 C10 1.403(5) . ? C9 C14 1.511(5) . ? C10 C15 1.505(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? B3 B8 1.731(7) . ? B3 B4 1.754(7) . ? B3 B7 1.770(6) . ? B3 H3 1.1000 . ? B4 B5 1.774(6) . ? B4 B8 1.779(7) . ? B4 B9 1.780(6) . ? B4 H4 1.1000 . ? B5 B6 1.752(6) . ? B5 B10 1.779(6) . ? B5 B9 1.781(6) . ? B5 H5 1.1000 . ? B6 B10 1.730(6) . ? B6 B11 1.761(6) . ? B6 H6 1.1000 . ? B7 B11 1.760(6) . ? B7 B8 1.765(7) . ? B7 B12 1.771(7) . ? B7 H7 1.1000 . ? B8 B9 1.766(7) . ? B8 B12 1.768(7) . ? B8 H8 1.1000 . ? B9 B10 1.779(6) . ? B9 B12 1.785(7) . ? B9 H9 1.1000 . ? B10 B12 1.774(7) . ? B10 B11 1.778(7) . ? B10 H10 1.1000 . ? B11 B12 1.768(6) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? 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 C6 Co1 C8 68.04(14) . . ? C6 Co1 C9 67.69(15) . . ? C8 Co1 C9 41.00(15) . . ? C6 Co1 C10 40.77(14) . . ? C8 Co1 C10 67.74(16) . . ? C9 Co1 C10 39.36(14) . . ? C6 Co1 C7 40.47(14) . . ? C8 Co1 C7 40.13(14) . . ? C9 Co1 C7 67.84(15) . . ? C10 Co1 C7 67.84(16) . . ? C6 Co1 S2 171.71(11) . . ? C8 Co1 S2 103.75(10) . . ? C9 Co1 S2 107.17(12) . . ? C10 Co1 S2 138.46(12) . . ? C7 Co1 S2 132.12(12) . . ? C6 Co1 S1 104.00(11) . . ? C8 Co1 S1 171.43(10) . . ? C9 Co1 S1 140.22(13) . . ? C10 Co1 S1 108.65(12) . . ? C7 Co1 S1 131.55(12) . . ? S2 Co1 S1 84.12(4) . . ? C6 Co1 Fe1 123.15(12) . . ? C8 Co1 Fe1 122.14(13) . . ? C9 Co1 Fe1 158.83(13) . . ? C10 Co1 Fe1 160.06(13) . . ? C7 Co1 Fe1 107.55(12) . . ? S2 Co1 Fe1 59.55(3) . . ? S1 Co1 Fe1 58.84(4) . . ? C4 Fe1 C3 92.30(19) . . ? C4 Fe1 C5 97.64(19) . . ? C3 Fe1 C5 95.5(2) . . ? C4 Fe1 S1 153.52(14) . . ? C3 Fe1 S1 87.71(14) . . ? C5 Fe1 S1 108.72(13) . . ? C4 Fe1 S2 87.18(14) . . ? C3 Fe1 S2 152.31(14) . . ? C5 Fe1 S2 111.98(16) . . ? S1 Fe1 S2 80.82(4) . . ? C4 Fe1 Co1 97.26(14) . . ? C3 Fe1 Co1 96.82(14) . . ? C5 Fe1 Co1 160.19(13) . . ? S1 Fe1 Co1 56.54(4) . . ? S2 Fe1 Co1 55.90(3) . . ? C1 S1 Co1 103.28(12) . . ? C1 S1 Fe1 104.88(12) . . ? Co1 S1 Fe1 64.62(3) . . ? C2 S2 Co1 103.54(12) . . ? C2 S2 Fe1 105.13(12) . . ? Co1 S2 Fe1 64.55(4) . . ? C2 C1 B4 112.0(3) . . ? C2 C1 B5 112.4(3) . . ? B4 C1 B5 62.9(3) . . ? C2 C1 B6 62.7(2) . . ? B4 C1 B6 113.6(3) . . ? B5 C1 B6 61.6(2) . . ? C2 C1 B3 62.1(2) . . ? B4 C1 B3 61.5(3) . . ? B5 C1 B3 113.8(3) . . ? B6 C1 B3 114.6(3) . . ? C2 C1 S1 111.5(2) . . ? B4 C1 S1 126.5(3) . . ? B5 C1 S1 123.4(3) . . ? B6 C1 S1 113.2(3) . . ? B3 C1 S1 117.5(3) . . ? C1 C2 B7 110.9(3) . . ? C1 C2 B11 110.4(3) . . ? B7 C2 B11 61.8(3) . . ? C1 C2 B3 61.9(2) . . ? B7 C2 B3 61.8(2) . . ? B11 C2 B3 112.7(3) . . ? C1 C2 B6 61.3(2) . . ? B7 C2 B6 112.1(3) . . ? B11 C2 B6 61.2(2) . . ? B3 C2 B6 113.3(3) . . ? C1 C2 S2 112.3(2) . . ? B7 C2 S2 126.9(3) . . ? B11 C2 S2 125.3(3) . . ? B3 C2 S2 116.8(3) . . ? B6 C2 S2 114.9(3) . . ? O1 C3 Fe1 177.7(4) . . ? O2 C4 Fe1 178.4(4) . . ? O3 C5 Fe1 175.7(4) . . ? C7 C6 C10 108.4(3) . . ? C7 C6 C11 126.2(4) . . ? C10 C6 C11 125.3(4) . . ? C7 C6 Co1 71.4(2) . . ? C10 C6 Co1 71.0(2) . . ? C11 C6 Co1 126.9(3) . . ? C8 C7 C6 107.0(4) . . ? C8 C7 C12 126.8(4) . . ? C6 C7 C12 126.0(4) . . ? C8 C7 Co1 68.4(2) . . ? C6 C7 Co1 68.2(2) . . ? C12 C7 Co1 132.6(3) . . ? C7 C8 C9 108.4(4) . . ? C7 C8 C13 126.2(4) . . ? C9 C8 C13 125.1(4) . . ? C7 C8 Co1 71.4(2) . . ? C9 C8 Co1 70.5(2) . . ? C13 C8 Co1 129.0(3) . . ? C10 C9 C8 108.0(4) . . ? C10 C9 C14 127.5(4) . . ? C8 C9 C14 124.3(4) . . ? C10 C9 Co1 70.6(2) . . ? C8 C9 Co1 68.5(2) . . ? C14 C9 Co1 128.9(3) . . ? C9 C10 C6 107.9(4) . . ? C9 C10 C15 126.8(4) . . ? C6 C10 C15 125.1(4) . . ? C9 C10 Co1 70.1(2) . . ? C6 C10 Co1 68.3(2) . . ? C15 C10 Co1 130.4(3) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 B3 B8 104.8(3) . . ? C1 B3 C2 56.0(2) . . ? B8 B3 C2 105.1(3) . . ? C1 B3 B4 58.4(2) . . ? B8 B3 B4 61.4(3) . . ? C2 B3 B4 104.4(3) . . ? C1 B3 B7 103.6(3) . . ? B8 B3 B7 60.5(3) . . ? C2 B3 B7 58.5(2) . . ? B4 B3 B7 109.3(4) . . ? C1 B3 H3 125.6 . . ? B8 B3 H3 122.1 . . ? C2 B3 H3 125.1 . . ? B4 B3 H3 121.3 . . ? B7 B3 H3 122.0 . . ? C1 B4 B3 60.1(2) . . ? C1 B4 B5 58.6(2) . . ? B3 B4 B5 109.1(3) . . ? C1 B4 B8 104.1(3) . . ? B3 B4 B8 58.7(3) . . ? B5 B4 B8 107.5(4) . . ? C1 B4 B9 104.6(3) . . ? B3 B4 B9 107.4(3) . . ? B5 B4 B9 60.1(3) . . ? B8 B4 B9 59.5(3) . . ? C1 B4 H4 124.5 . . ? B3 B4 H4 121.1 . . ? B5 B4 H4 121.1 . . ? B8 B4 H4 123.5 . . ? B9 B4 H4 122.7 . . ? C1 B5 B6 59.7(2) . . ? C1 B5 B4 58.5(2) . . ? B6 B5 B4 108.4(3) . . ? C1 B5 B10 104.3(3) . . ? B6 B5 B10 58.7(3) . . ? B4 B5 B10 107.9(3) . . ? C1 B5 B9 104.4(3) . . ? B6 B5 B9 107.1(3) . . ? B4 B5 B9 60.1(3) . . ? B10 B5 B9 60.0(3) . . ? C1 B5 H5 124.6 . . ? B6 B5 H5 121.6 . . ? B4 B5 H5 121.2 . . ? B10 B5 H5 122.9 . . ? B9 B5 H5 122.7 . . ? C1 B6 B10 105.7(3) . . ? C1 B6 C2 56.0(2) . . ? B10 B6 C2 106.0(3) . . ? C1 B6 B5 58.7(2) . . ? B10 B6 B5 61.4(3) . . ? C2 B6 B5 104.7(3) . . ? C1 B6 B11 104.1(3) . . ? B10 B6 B11 61.2(3) . . ? C2 B6 B11 58.7(2) . . ? B5 B6 B11 109.8(3) . . ? C1 B6 H6 125.2 . . ? B10 B6 H6 121.4 . . ? C2 B6 H6 124.8 . . ? B5 B6 H6 121.2 . . ? B11 B6 H6 121.6 . . ? C2 B7 B11 59.2(2) . . ? C2 B7 B8 104.6(3) . . ? B11 B7 B8 107.8(4) . . ? C2 B7 B3 59.7(2) . . ? B11 B7 B3 108.9(3) . . ? B8 B7 B3 58.7(3) . . ? C2 B7 B12 105.4(3) . . ? B11 B7 B12 60.1(3) . . ? B8 B7 B12 60.0(3) . . ? B3 B7 B12 107.5(4) . . ? C2 B7 H7 124.0 . . ? B11 B7 H7 121.0 . . ? B8 B7 H7 123.1 . . ? B3 B7 H7 121.5 . . ? B12 B7 H7 122.3 . . ? B3 B8 B7 60.8(3) . . ? B3 B8 B9 109.0(3) . . ? B7 B8 B9 108.8(4) . . ? B3 B8 B12 109.4(4) . . ? B7 B8 B12 60.2(3) . . ? B9 B8 B12 60.7(3) . . ? B3 B8 B4 59.9(3) . . ? B7 B8 B4 108.3(3) . . ? B9 B8 B4 60.3(3) . . ? B12 B8 B4 108.8(4) . . ? B3 B8 H8 120.9 . . ? B7 B8 H8 121.3 . . ? B9 B8 H8 121.1 . . ? B12 B8 H8 121.0 . . ? B4 B8 H8 121.7 . . ? B8 B9 B10 107.3(4) . . ? B8 B9 B4 60.2(3) . . ? B10 B9 B4 107.7(3) . . ? B8 B9 B5 107.7(3) . . ? B10 B9 B5 60.0(3) . . ? B4 B9 B5 59.8(2) . . ? B8 B9 B12 59.7(3) . . ? B10 B9 B12 59.7(3) . . ? B4 B9 B12 108.0(4) . . ? B5 B9 B12 107.8(3) . . ? B8 B9 H9 122.0 . . ? B10 B9 H9 122.1 . . ? B4 B9 H9 121.7 . . ? B5 B9 H9 121.9 . . ? B12 B9 H9 121.9 . . ? B6 B10 B12 108.4(3) . . ? B6 B10 B11 60.2(3) . . ? B12 B10 B11 59.7(3) . . ? B6 B10 B5 59.9(3) . . ? B12 B10 B5 108.3(3) . . ? B11 B10 B5 107.8(3) . . ? B6 B10 B9 108.2(3) . . ? B12 B10 B9 60.3(3) . . ? B11 B10 B9 107.8(4) . . ? B5 B10 B9 60.1(3) . . ? B6 B10 H10 121.5 . . ? B12 B10 H10 121.5 . . ? B11 B10 H10 122.0 . . ? B5 B10 H10 121.7 . . ? B9 B10 H10 121.6 . . ? C2 B11 B7 59.0(2) . . ? C2 B11 B6 60.1(2) . . ? B7 B11 B6 108.9(3) . . ? C2 B11 B12 105.3(3) . . ? B7 B11 B12 60.3(3) . . ? B6 B11 B12 107.3(3) . . ? C2 B11 B10 105.0(3) . . ? B7 B11 B10 108.2(3) . . ? B6 B11 B10 58.5(3) . . ? B12 B11 B10 60.0(3) . . ? C2 B11 H11 123.9 . . ? B7 B11 H11 120.9 . . ? B6 B11 H11 121.6 . . ? B12 B11 H11 122.4 . . ? B10 B11 H11 122.8 . . ? B8 B12 B11 107.3(3) . . ? B8 B12 B7 59.8(3) . . ? B11 B12 B7 59.6(3) . . ? B8 B12 B10 107.5(4) . . ? B11 B12 B10 60.3(3) . . ? B7 B12 B10 107.9(3) . . ? B8 B12 B9 59.6(3) . . ? B11 B12 B9 108.0(3) . . ? B7 B12 B9 107.7(4) . . ? B10 B12 B9 60.0(3) . . ? B8 B12 H12 122.2 . . ? B11 B12 H12 121.9 . . ? B7 B12 H12 121.9 . . ? B10 B12 H12 121.7 . . ? B9 B12 H12 121.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.267 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.060 # Attachment '8a.cif' data_f60110c _database_code_depnum_ccdc_archive 'CCDC 608154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H15 B10 Co Fe O3 S2' _chemical_formula_weight 470.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.314(6) _cell_length_b 10.717(7) _cell_length_c 19.450(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1941(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 715 _cell_measurement_theta_min 2.425 _cell_measurement_theta_max 21.316 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 3.78 _diffrn_reflns_number 8952 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.01 _reflns_number_total 3824 _reflns_number_gt 2596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0181P)^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 -0.02(2) _refine_ls_number_reflns 3824 _refine_ls_number_parameters 300 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.813 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21049(6) 0.47207(6) 0.15829(4) 0.03794(17) Uani 1 1 d . A . Fe2 Fe 0.42391(7) 0.39457(7) 0.21249(4) 0.0458(2) Uani 1 1 d . . . S3 S 0.41114(12) 0.58261(11) 0.15677(7) 0.0393(3) Uani 1 1 d . A . S4 S 0.34304(12) 0.32734(12) 0.10784(7) 0.0401(3) Uani 1 1 d . A . C1 C 0.3360(6) 0.2649(6) 0.2479(3) 0.0635(17) Uani 1 1 d . A . O1 O 0.2731(4) 0.1779(4) 0.2702(2) 0.0926(15) Uani 1 1 d . . . C2 C 0.4169(7) 0.4704(7) 0.2921(3) 0.0794(18) Uani 1 1 d . A . O2 O 0.4102(6) 0.5250(5) 0.3433(2) 0.1239(18) Uani 1 1 d . . . C3 C 0.6051(6) 0.3422(6) 0.2253(3) 0.0693(19) Uani 1 1 d . A . O3 O 0.7165(4) 0.3069(5) 0.2366(2) 0.1129(19) Uani 1 1 d . . . C4 C 0.057(3) 0.565(4) 0.202(2) 0.073(15) Uani 0.48(3) 1 d P A 1 H4 H 0.0799 0.6341 0.2283 0.087 Uiso 0.48(3) 1 calc PR A 1 C5 C 0.032(3) 0.573(2) 0.1383(16) 0.038(11) Uani 0.48(3) 1 d P A 1 H5 H 0.0282 0.6456 0.1121 0.045 Uiso 0.48(3) 1 calc PR A 1 C6 C 0.008(4) 0.445(6) 0.1142(17) 0.066(13) Uani 0.48(3) 1 d P A 1 H6 H -0.0115 0.4194 0.0695 0.079 Uiso 0.48(3) 1 calc PR A 1 C7 C 0.022(4) 0.372(3) 0.170(2) 0.060(9) Uani 0.48(3) 1 d PU A 1 H7 H 0.0152 0.2859 0.1728 0.072 Uiso 0.48(3) 1 calc PR A 1 C8 C 0.050(2) 0.462(3) 0.2258(13) 0.040(6) Uani 0.48(3) 1 d PU A 1 H8 H 0.0612 0.4415 0.2720 0.048 Uiso 0.48(3) 1 calc PR A 1 C4' C 0.058(3) 0.619(2) 0.174(2) 0.042(7) Uani 0.52(3) 1 d P A 2 H4' H 0.0711 0.7048 0.1689 0.051 Uiso 0.52(3) 1 calc PR A 2 C5' C 0.015(3) 0.530(3) 0.1191(13) 0.040(9) Uani 0.52(3) 1 d P A 2 H5' H -0.0015 0.5471 0.0729 0.047 Uiso 0.52(3) 1 calc PR A 2 C6' C 0.004(3) 0.420(4) 0.150(2) 0.08(2) Uani 0.52(3) 1 d PU A 2 H6' H -0.0253 0.3493 0.1262 0.092 Uiso 0.52(3) 1 calc PR A 2 C7' C 0.037(2) 0.412(2) 0.2197(15) 0.043(6) Uani 0.52(3) 1 d PU A 2 H7' H 0.0364 0.3440 0.2491 0.052 Uiso 0.52(3) 1 calc PR A 2 C8' C 0.076(2) 0.551(2) 0.2342(9) 0.033(5) Uani 0.52(3) 1 d P A 2 H8' H 0.1062 0.5832 0.2762 0.039 Uiso 0.52(3) 1 calc PR A 2 C10 C 0.4826(4) 0.5553(4) 0.0720(2) 0.0326(12) Uani 1 1 d . . . C11 C 0.4456(4) 0.4157(4) 0.0447(2) 0.0343(11) Uani 1 1 d . A . B3 B 0.6220(5) 0.4467(5) 0.0656(3) 0.0440(16) Uani 1 1 d . A . H3 H 0.6807 0.4062 0.1093 0.053 Uiso 1 1 calc R . . B4 B 0.6462(5) 0.6034(5) 0.0411(3) 0.0439(15) Uani 1 1 d . A . H4A H 0.7200 0.6653 0.0691 0.053 Uiso 1 1 calc R . . B5 B 0.4829(6) 0.6598(6) 0.0060(3) 0.0463(16) Uani 1 1 d . A . H5A H 0.4524 0.7584 0.0116 0.056 Uiso 1 1 calc R . . B6 B 0.3536(5) 0.5399(5) 0.0085(3) 0.0420(14) Uani 1 1 d . A . H6A H 0.2384 0.5591 0.0150 0.050 Uiso 1 1 calc R . . B7 B 0.5755(6) 0.3572(5) -0.0078(3) 0.0455(15) Uani 1 1 d . . . H7A H 0.6029 0.2576 -0.0119 0.055 Uiso 1 1 calc R A . B8 B 0.7061(6) 0.4783(5) -0.0125(3) 0.0494(15) Uani 1 1 d . A . H8A H 0.8209 0.4586 -0.0204 0.059 Uiso 1 1 calc R . . B9 B 0.6227(5) 0.6103(6) -0.0497(3) 0.0499(16) Uani 1 1 d . . . H9 H 0.6833 0.6764 -0.0818 0.060 Uiso 1 1 calc R A . B10 B 0.4421(6) 0.5720(5) -0.0676(3) 0.0493(17) Uani 1 1 d . A . H10 H 0.3852 0.6135 -0.1116 0.059 Uiso 1 1 calc R . . B11 B 0.4136(6) 0.4150(6) -0.0412(3) 0.0491(16) Uani 1 1 d . A . H11 H 0.3369 0.3523 -0.0668 0.059 Uiso 1 1 calc R . . B12 B 0.5796(6) 0.4585(6) -0.0788(3) 0.0533(17) Uani 1 1 d . A . H12 H 0.6119 0.4255 -0.1301 0.064 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 Co1 0.0237(3) 0.0499(4) 0.0402(4) 0.0029(3) 0.0011(3) 0.0011(3) Fe2 0.0297(3) 0.0645(5) 0.0433(5) 0.0089(4) -0.0035(4) -0.0012(4) S3 0.0337(6) 0.0468(8) 0.0374(7) -0.0069(7) 0.0029(7) -0.0035(6) S4 0.0332(6) 0.0402(7) 0.0469(8) 0.0009(6) -0.0012(6) -0.0025(6) C1 0.045(3) 0.089(5) 0.057(4) 0.024(3) -0.007(3) 0.014(3) O1 0.061(3) 0.111(3) 0.105(4) 0.059(3) -0.008(3) -0.013(3) C2 0.069(4) 0.127(5) 0.042(4) 0.003(4) 0.000(4) -0.020(4) O2 0.146(4) 0.165(5) 0.061(3) -0.011(3) 0.008(4) -0.025(4) C3 0.036(3) 0.103(5) 0.069(4) 0.046(4) -0.007(3) 0.002(3) O3 0.044(2) 0.165(5) 0.130(5) 0.089(4) 0.003(3) 0.016(3) C4 0.041(10) 0.09(3) 0.09(3) -0.08(3) -0.029(19) 0.008(16) C5 0.029(12) 0.006(13) 0.08(4) -0.013(11) -0.001(17) 0.001(10) C6 0.028(10) 0.12(4) 0.050(15) -0.06(2) -0.012(11) -0.011(14) C7 0.041(12) 0.053(19) 0.09(2) 0.019(17) 0.023(11) 0.007(11) C8 0.040(8) 0.042(11) 0.038(7) 0.010(9) 0.002(6) -0.004(9) C4' 0.031(8) 0.017(9) 0.08(2) 0.004(10) 0.018(10) 0.012(8) C5' 0.025(8) 0.07(3) 0.025(10) -0.034(19) -0.010(6) -0.001(17) C6' 0.015(8) 0.06(3) 0.15(6) -0.06(4) 0.01(2) -0.004(14) C7' 0.031(7) 0.011(10) 0.089(16) 0.010(11) 0.028(9) -0.007(7) C8' 0.024(7) 0.059(13) 0.015(8) -0.016(9) 0.001(7) -0.006(7) C10 0.029(2) 0.028(3) 0.041(3) 0.000(2) 0.001(2) 0.002(2) C11 0.025(2) 0.033(3) 0.044(3) -0.002(2) 0.001(2) 0.002(2) B3 0.019(3) 0.058(4) 0.056(4) 0.000(3) -0.003(3) 0.005(3) B4 0.029(3) 0.048(4) 0.054(4) 0.009(3) 0.003(3) -0.008(3) B5 0.044(3) 0.046(4) 0.049(4) 0.007(3) 0.005(3) 0.000(3) B6 0.032(3) 0.047(4) 0.047(4) -0.002(3) -0.009(3) 0.011(3) B7 0.044(3) 0.051(4) 0.043(4) -0.006(3) 0.000(3) 0.013(3) B8 0.029(3) 0.071(4) 0.048(4) 0.009(3) 0.007(3) 0.006(3) B9 0.039(3) 0.068(4) 0.043(4) 0.017(3) 0.007(3) -0.004(3) B10 0.043(3) 0.068(5) 0.037(4) 0.010(3) -0.001(3) 0.012(3) B11 0.039(3) 0.073(4) 0.036(4) -0.007(3) -0.007(3) -0.004(3) B12 0.042(3) 0.084(5) 0.034(4) -0.008(3) 0.007(3) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C4 1.93(3) . ? Co1 C8 1.99(2) . ? Co1 C6' 2.01(3) . ? Co1 C5 2.02(2) . ? Co1 C7 2.07(4) . ? Co1 C5' 2.07(2) . ? Co1 C6 2.09(3) . ? Co1 C7' 2.107(19) . ? Co1 C8' 2.113(19) . ? Co1 C4' 2.14(2) . ? Co1 S4 2.2119(17) . ? Co1 S3 2.2128(16) . ? Fe2 C2 1.750(7) . ? Fe2 C1 1.754(6) . ? Fe2 C3 1.796(5) . ? Fe2 S4 2.2867(19) . ? Fe2 S3 2.2911(18) . ? S3 C10 1.802(5) . ? S4 C11 1.822(5) . ? C1 O1 1.183(6) . ? C2 O2 1.158(7) . ? C3 O3 1.126(5) . ? C4 C8 1.20(3) . ? C4 C5 1.26(4) . ? C4 H4 0.9300 . ? C5 C6 1.47(5) . ? C5 H5 0.9300 . ? C6 C7 1.34(7) . ? C6 H6 0.9300 . ? C7 C8 1.47(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C4' C8' 1.39(4) . ? C4' C5' 1.49(4) . ? C4' H4' 0.9300 . ? C5' C6' 1.33(4) . ? C5' H5' 0.9300 . ? C6' C7' 1.39(4) . ? C6' H6' 0.9300 . ? C7' C8' 1.56(3) . ? C7' H7' 0.9300 . ? C8' H8' 0.9300 . ? C10 C11 1.625(6) . ? C10 B5 1.703(7) . ? C10 B4 1.717(6) . ? C10 B6 1.732(6) . ? C10 B3 1.747(6) . ? C11 B11 1.697(7) . ? C11 B7 1.702(7) . ? C11 B3 1.724(6) . ? C11 B6 1.733(6) . ? B3 B8 1.743(8) . ? B3 B4 1.760(8) . ? B3 B7 1.773(8) . ? B3 H3 1.1000 . ? B4 B5 1.772(7) . ? B4 B9 1.780(8) . ? B4 B8 1.788(8) . ? B4 H4A 1.1000 . ? B5 B10 1.756(8) . ? B5 B6 1.762(7) . ? B5 B9 1.775(8) . ? B5 H5A 1.1000 . ? B6 B10 1.729(8) . ? B6 B11 1.743(8) . ? B6 H6A 1.1000 . ? B7 B11 1.755(8) . ? B7 B12 1.758(8) . ? B7 B8 1.781(7) . ? B7 H7A 1.1000 . ? B8 B12 1.760(8) . ? B8 B9 1.768(8) . ? B8 H8A 1.1000 . ? B9 B10 1.766(8) . ? B9 B12 1.769(9) . ? B9 H9 1.1000 . ? B10 B12 1.779(8) . ? B10 B11 1.779(8) . ? B10 H10 1.1000 . ? B11 B12 1.772(8) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? 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 C4 Co1 C8 35.7(10) . . ? C4 Co1 C6' 58.0(14) . . ? C8 Co1 C6' 47.0(12) . . ? C4 Co1 C5 37.0(10) . . ? C8 Co1 C5 62.6(10) . . ? C6' Co1 C5 49.2(12) . . ? C4 Co1 C7 65.8(14) . . ? C8 Co1 C7 42.4(14) . . ? C6' Co1 C7 18.5(12) . . ? C5 Co1 C7 66.4(9) . . ? C4 Co1 C5' 50.0(8) . . ? C8 Co1 C5' 66.4(9) . . ? C6' Co1 C5' 38.0(12) . . ? C5 Co1 C5' 17.3(5) . . ? C7 Co1 C5' 56.4(10) . . ? C4 Co1 C6 65.5(13) . . ? C8 Co1 C6 65.6(12) . . ? C6' Co1 C6 21.1(14) . . ? C5 Co1 C6 41.8(14) . . ? C7 Co1 C6 37.7(19) . . ? C5' Co1 C6 25.4(14) . . ? C4 Co1 C7' 48.9(11) . . ? C8 Co1 C7' 15.2(7) . . ? C6' Co1 C7' 39.2(12) . . ? C5 Co1 C7' 69.0(10) . . ? C7 Co1 C7' 29.6(14) . . ? C5' Co1 C7' 67.9(10) . . ? C6 Co1 C7' 60.0(12) . . ? C4 Co1 C8' 18.4(10) . . ? C8 Co1 C8' 28.1(11) . . ? C6' Co1 C8' 66.3(13) . . ? C5 Co1 C8' 55.4(9) . . ? C7 Co1 C8' 68.1(12) . . ? C5' Co1 C8' 67.4(7) . . ? C6 Co1 C8' 79.0(9) . . ? C7' Co1 C8' 43.3(9) . . ? C4 Co1 C4' 21.7(13) . . ? C8 Co1 C4' 56.7(9) . . ? C6' Co1 C4' 65.3(12) . . ? C5 Co1 C4' 24.4(9) . . ? C7 Co1 C4' 78.6(11) . . ? C5' Co1 C4' 41.4(10) . . ? C6 Co1 C4' 64.2(13) . . ? C7' Co1 C4' 68.6(8) . . ? C8' Co1 C4' 38.1(12) . . ? C4 Co1 S4 165.1(11) . . ? C8 Co1 S4 132.1(9) . . ? C6' Co1 S4 107.7(11) . . ? C5 Co1 S4 138.5(9) . . ? C7 Co1 S4 99.2(10) . . ? C5' Co1 S4 122.5(8) . . ? C6 Co1 S4 102.9(12) . . ? C7' Co1 S4 117.8(6) . . ? C8' Co1 S4 157.2(7) . . ? C4' Co1 S4 161.6(11) . . ? C4 Co1 S3 110.8(10) . . ? C8 Co1 S3 132.2(9) . . ? C6' Co1 S3 163.1(12) . . ? C5 Co1 S3 114.0(7) . . ? C7 Co1 S3 174.3(13) . . ? C5' Co1 S3 125.4(9) . . ? C6 Co1 S3 146.1(15) . . ? C7' Co1 S3 144.8(9) . . ? C8' Co1 S3 107.2(6) . . ? C4' Co1 S3 99.6(8) . . ? S4 Co1 S3 84.15(6) . . ? C2 Fe2 C1 90.2(3) . . ? C2 Fe2 C3 93.3(3) . . ? C1 Fe2 C3 97.8(2) . . ? C2 Fe2 S4 157.2(2) . . ? C1 Fe2 S4 86.9(2) . . ? C3 Fe2 S4 109.5(2) . . ? C2 Fe2 S3 90.5(2) . . ? C1 Fe2 S3 149.15(17) . . ? C3 Fe2 S3 112.92(18) . . ? S4 Fe2 S3 80.74(6) . . ? C2 Fe2 Co1 101.4(2) . . ? C1 Fe2 Co1 93.46(17) . . ? C3 Fe2 Co1 161.4(2) . . ? S4 Fe2 Co1 56.28(4) . . ? S3 Fe2 Co1 56.26(4) . . ? C10 S3 Co1 103.73(14) . . ? C10 S3 Fe2 105.72(15) . . ? Co1 S3 Fe2 64.32(5) . . ? C11 S4 Co1 103.16(15) . . ? C11 S4 Fe2 105.30(15) . . ? Co1 S4 Fe2 64.41(5) . . ? O1 C1 Fe2 177.8(5) . . ? O2 C2 Fe2 177.1(7) . . ? O3 C3 Fe2 176.3(5) . . ? C8 C4 C5 116(3) . . ? C8 C4 Co1 74.7(16) . . ? C5 C4 Co1 75.4(16) . . ? C8 C4 H4 122.1 . . ? C5 C4 H4 122.1 . . ? Co1 C4 H4 119.1 . . ? C4 C5 C6 106(3) . . ? C4 C5 Co1 67.6(15) . . ? C6 C5 Co1 71.4(19) . . ? C4 C5 H5 127.0 . . ? C6 C5 H5 127.0 . . ? Co1 C5 H5 125.5 . . ? C7 C6 C5 106(3) . . ? C7 C6 Co1 70(2) . . ? C5 C6 Co1 66.8(18) . . ? C7 C6 H6 127.2 . . ? C5 C6 H6 127.2 . . ? Co1 C6 H6 127.2 . . ? C6 C7 C8 104(3) . . ? C6 C7 Co1 72(3) . . ? C8 C7 Co1 66.0(16) . . ? C6 C7 H7 128.2 . . ? C8 C7 H7 128.2 . . ? Co1 C7 H7 125.5 . . ? C4 C8 C7 109(2) . . ? C4 C8 Co1 69.6(15) . . ? C7 C8 Co1 71.6(17) . . ? C4 C8 H8 125.6 . . ? C7 C8 H8 125.6 . . ? Co1 C8 H8 124.7 . . ? C8' C4' C5' 107.3(19) . . ? C8' C4' Co1 69.8(13) . . ? C5' C4' Co1 66.7(14) . . ? C8' C4' H4' 126.3 . . ? C5' C4' H4' 126.3 . . ? Co1 C4' H4' 128.7 . . ? C6' C5' C4' 105(3) . . ? C6' C5' Co1 68.5(17) . . ? C4' C5' Co1 71.9(16) . . ? C6' C5' H5' 127.3 . . ? C4' C5' H5' 127.3 . . ? Co1 C5' H5' 123.9 . . ? C5' C6' C7' 119(3) . . ? C5' C6' Co1 73.5(17) . . ? C7' C6' Co1 74.2(14) . . ? C5' C6' H6' 120.7 . . ? C7' C6' H6' 120.7 . . ? Co1 C6' H6' 123.1 . . ? C6' C7' C8' 100(2) . . ? C6' C7' Co1 66.6(15) . . ? C8' C7' Co1 68.5(10) . . ? C6' C7' H7' 130.0 . . ? C8' C7' H7' 130.0 . . ? Co1 C7' H7' 126.4 . . ? C4' C8' C7' 108.8(18) . . ? C4' C8' Co1 72.1(13) . . ? C7' C8' Co1 68.2(11) . . ? C4' C8' H8' 125.6 . . ? C7' C8' H8' 125.6 . . ? Co1 C8' H8' 125.6 . . ? C11 C10 B5 111.0(4) . . ? C11 C10 B4 110.5(3) . . ? B5 C10 B4 62.4(3) . . ? C11 C10 B6 62.0(3) . . ? B5 C10 B6 61.7(3) . . ? B4 C10 B6 113.2(4) . . ? C11 C10 B3 61.4(3) . . ? B5 C10 B3 112.5(4) . . ? B4 C10 B3 61.1(3) . . ? B6 C10 B3 113.6(3) . . ? C11 C10 S3 111.7(3) . . ? B5 C10 S3 125.7(3) . . ? B4 C10 S3 126.9(3) . . ? B6 C10 S3 114.3(3) . . ? B3 C10 S3 116.6(3) . . ? C10 C11 B11 111.3(4) . . ? C10 C11 B7 112.6(3) . . ? B11 C11 B7 62.2(3) . . ? C10 C11 B3 62.8(3) . . ? B11 C11 B3 113.6(4) . . ? B7 C11 B3 62.3(3) . . ? C10 C11 B6 62.0(3) . . ? B11 C11 B6 61.1(3) . . ? B7 C11 B6 113.0(4) . . ? B3 C11 B6 114.8(4) . . ? C10 C11 S4 111.6(3) . . ? B11 C11 S4 124.7(3) . . ? B7 C11 S4 125.9(3) . . ? B3 C11 S4 116.1(3) . . ? B6 C11 S4 114.4(3) . . ? C11 B3 B8 105.1(4) . . ? C11 B3 C10 55.8(2) . . ? B8 B3 C10 105.5(4) . . ? C11 B3 B4 104.0(4) . . ? B8 B3 B4 61.4(3) . . ? C10 B3 B4 58.6(3) . . ? C11 B3 B7 58.2(3) . . ? B8 B3 B7 60.9(3) . . ? C10 B3 B7 103.7(4) . . ? B4 B3 B7 109.2(4) . . ? C11 B3 H3 125.4 . . ? B8 B3 H3 121.7 . . ? C10 B3 H3 125.3 . . ? B4 B3 H3 121.5 . . ? B7 B3 H3 121.9 . . ? C10 B4 B3 60.3(3) . . ? C10 B4 B5 58.4(3) . . ? B3 B4 B5 108.6(4) . . ? C10 B4 B9 104.5(4) . . ? B3 B4 B9 107.0(4) . . ? B5 B4 B9 59.9(3) . . ? C10 B4 B8 104.9(4) . . ? B3 B4 B8 58.8(3) . . ? B5 B4 B8 107.4(4) . . ? B9 B4 B8 59.4(3) . . ? C10 B4 H4A 124.1 . . ? B3 B4 H4A 121.3 . . ? B5 B4 H4A 121.5 . . ? B9 B4 H4A 123.0 . . ? B8 B4 H4A 123.1 . . ? C10 B5 B10 105.2(4) . . ? C10 B5 B6 59.9(3) . . ? B10 B5 B6 58.9(3) . . ? C10 B5 B4 59.2(3) . . ? B10 B5 B4 108.5(4) . . ? B6 B5 B4 109.1(4) . . ? C10 B5 B9 105.3(4) . . ? B10 B5 B9 60.0(3) . . ? B6 B5 B9 107.4(4) . . ? B4 B5 B9 60.2(3) . . ? C10 B5 H5A 123.9 . . ? B10 B5 H5A 122.6 . . ? B6 B5 H5A 121.4 . . ? B4 B5 H5A 120.8 . . ? B9 B5 H5A 122.5 . . ? B10 B6 C10 105.1(4) . . ? B10 B6 C11 105.4(4) . . ? C10 B6 C11 56.0(2) . . ? B10 B6 B11 61.7(3) . . ? C10 B6 B11 104.3(3) . . ? C11 B6 B11 58.4(3) . . ? B10 B6 B5 60.4(3) . . ? C10 B6 B5 58.3(3) . . ? C11 B6 B5 103.5(3) . . ? B11 B6 B5 109.0(4) . . ? B10 B6 H6A 121.8 . . ? C10 B6 H6A 125.2 . . ? C11 B6 H6A 125.4 . . ? B11 B6 H6A 121.4 . . ? B5 B6 H6A 122.2 . . ? C11 B7 B11 58.8(3) . . ? C11 B7 B12 105.0(4) . . ? B11 B7 B12 60.6(3) . . ? C11 B7 B3 59.5(3) . . ? B11 B7 B3 108.5(4) . . ? B12 B7 B3 107.0(4) . . ? C11 B7 B8 104.4(4) . . ? B11 B7 B8 108.1(4) . . ? B12 B7 B8 59.6(3) . . ? B3 B7 B8 58.7(3) . . ? C11 B7 H7A 124.4 . . ? B11 B7 H7A 120.9 . . ? B12 B7 H7A 122.5 . . ? B3 B7 H7A 121.8 . . ? B8 B7 H7A 123.0 . . ? B3 B8 B12 108.3(4) . . ? B3 B8 B9 108.3(4) . . ? B12 B8 B9 60.2(3) . . ? B3 B8 B7 60.4(3) . . ? B12 B8 B7 59.5(3) . . ? B9 B8 B7 107.7(4) . . ? B3 B8 B4 59.8(3) . . ? B12 B8 B4 108.0(4) . . ? B9 B8 B4 60.1(3) . . ? B7 B8 B4 107.6(4) . . ? B3 B8 H8A 121.4 . . ? B12 B8 H8A 121.7 . . ? B9 B8 H8A 121.6 . . ? B7 B8 H8A 122.0 . . ? B4 B8 H8A 121.9 . . ? B10 B9 B8 108.3(4) . . ? B10 B9 B12 60.4(3) . . ? B8 B9 B12 59.7(3) . . ? B10 B9 B5 59.5(3) . . ? B8 B9 B5 108.2(4) . . ? B12 B9 B5 107.7(4) . . ? B10 B9 B4 107.7(4) . . ? B8 B9 B4 60.5(3) . . ? B12 B9 B4 107.9(4) . . ? B5 B9 B4 59.8(3) . . ? B10 B9 H9 121.8 . . ? B8 B9 H9 121.4 . . ? B12 B9 H9 121.8 . . ? B5 B9 H9 122.0 . . ? B4 B9 H9 121.7 . . ? B6 B10 B5 60.8(3) . . ? B6 B10 B9 109.3(4) . . ? B5 B10 B9 60.5(3) . . ? B6 B10 B12 108.2(4) . . ? B5 B10 B12 108.1(4) . . ? B9 B10 B12 59.8(3) . . ? B6 B10 B11 59.6(3) . . ? B5 B10 B11 107.7(4) . . ? B9 B10 B11 107.7(4) . . ? B12 B10 B11 59.7(3) . . ? B6 B10 H10 121.1 . . ? B5 B10 H10 121.4 . . ? B9 B10 H10 121.2 . . ? B12 B10 H10 121.9 . . ? B11 B10 H10 122.4 . . ? C11 B11 B6 60.5(3) . . ? C11 B11 B7 59.1(3) . . ? B6 B11 B7 110.0(4) . . ? C11 B11 B12 104.6(4) . . ? B6 B11 B12 107.8(4) . . ? B7 B11 B12 59.8(3) . . ? C11 B11 B10 104.7(4) . . ? B6 B11 B10 58.8(3) . . ? B7 B11 B10 108.2(4) . . ? B12 B11 B10 60.1(3) . . ? C11 B11 H11 124.2 . . ? B6 B11 H11 120.7 . . ? B7 B11 H11 120.7 . . ? B12 B11 H11 122.7 . . ? B10 B11 H11 122.9 . . ? B7 B12 B8 60.9(3) . . ? B7 B12 B9 108.7(4) . . ? B8 B12 B9 60.2(3) . . ? B7 B12 B11 59.6(3) . . ? B8 B12 B11 108.3(4) . . ? B9 B12 B11 107.9(4) . . ? B7 B12 B10 108.1(4) . . ? B8 B12 B10 108.1(4) . . ? B9 B12 B10 59.7(3) . . ? B11 B12 B10 60.1(3) . . ? B7 B12 H12 121.3 . . ? B8 B12 H12 121.3 . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 121.9 . . ? B10 B12 H12 121.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.637 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.061